data_Underoil
#==============================================================================
# PROCESSING SUMMARY (IUCr Office Use Only)
_journal_date_recd_electronic 2018-11-08
_journal_date_to_coeditor ?
_journal_date_from_coeditor ?
_journal_date_accepted 2018-12-18
_journal_date_printers_first ?
_journal_date_printers_final ?
_journal_date_proofs_out ?
_journal_date_proofs_in ?
_journal_coeditor_name ?
_journal_coeditor_code LT5016SUP1
_journal_coeditor_notes
; ?
;
_journal_paper_category FA
_journal_techeditor_code M181787
_iucr_compatibility_tag ACTA95
_journal_techeditor_notes
;
;
_journal_coden_ASTM ?
_journal_name_full ?
_journal_year ?
_journal_volume ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
#==============================================================================
_audit_creation_date "2018-06-15"
_audit_creation_method CRYSTALS_ver_14.61_build_6236
_oxford_structure_analysis_title 'xcalibur in C:\Users\novy2\Desk At 13:38 on '
_chemical_name_systematic ?
_chemical_melting_point ?
#looking for refcif
# Check this file using the IUCr facility at:
# http://checkcif.iucr.org/
# The content below is held in the file 'script/refcif.dat'. This is a text
# file which you may edit to reflect local conditions.
# Items which need looking at are represented by a '?'.
# Items for which there are choices are prefixed with 'choose from'.
_publ_contact_letter
;
Please consider this CIF submission for
publication as a Short Format Paper in Acta
Crystallographica E.
;
_publ_contact_author_name 'Anthony Other'
_publ_contact_author_address
;
Chemical Crystallography Laboratory,
Department of Chemistry,
University of Nowhere,
Nowhere, NO1 4T, UK.
;
_publ_contact_author_phone '+44 1865 000000'
_publ_contact_author_fax '+44 1865 000000'
_publ_contact_author_email 'a.n.other@chem.no.ac.uk'
_publ_requested_journal 'Section E'
_publ_requested_category EO # choose from: FI FM FO CI CM CO AD
_publ_requested_coeditor_name 'Prof William Clegg'
_publ_section_title
# Title of paper - generally just the systematic or trivial name
; ?
;
# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.
loop_
_publ_author_name
_publ_author_address
_publ_author_footnote
'Other, Anthony N.' # Author 1
;
? # Address for author 1
;
;
? # Footnote for author 1
;
'Else, S. O.' # Author 2
;
? # Address 2
;
;
? # Footnote 2
;
_publ_section_abstract
# Text of the abstract
# (a) The Abstract must be self-contained and comprehensible
# without the rest of the paper. This means no references
# to atom names or to compound numbers; compounds must be
# identified as the title compound, or by name or by some other
# means such as derivatives of each other (e.g. "the
# corresponding ketone").
# (b) The chemical formula of "the title compound" must be given.
# (c) Any crystallographic molecular symmetry should be
# mentioned, and also the presence of more than one molecule
# in the asymmetric unit (i.e. anything other than Z'=1).
;
?
;
_publ_section_related_literature # Not in version 2.3.1
###############################################################
# Essential references (e.g. to the origin of the material studied, related
# structural studies, and to information supporting the reported structure)
# should be cited in this section, with appropriate very brief explanatory
# text, for example `The synthesis of the complex is described by Jones
# (2001). The anhydrous complex has essentially the same coordination
# geometry (Smith, 2003).' In addition, all references included in the
# supplementary materials, but not elsewhere in the published article,
# should be given here. The simple text `For related literature, see:...'
# may be used, but further details should be provided in the Comment
# section, which forms part of the supplementary material.
###############################################################
;
?
;
_publ_section_comment
# Text of the paper
# Note that atoms are referenced as N2, not N(2) or N~2~
# If text containing () occur within (), the outer ones should be []
# Figures should be referenced as Fig.
;
?
;
_publ_section_acknowledgements # Acknowledgments
;
?
;
_publ_section_figure_captions
# Captions to figures - Start each caption on a new line after a blank line
;
Fig. 1.
The title compound with displacement ellipsoids drawn at the 50%
probability level. H atoms are shown as spheres of
arbitary radius.
;
_publ_section_exptl_refinement
# Some potentially useful phrases are donated by Bill Clegg:
;
In the absence of significant anomalous scattering, Friedel pairs were
merged.
The absolute configuration was arbitrarily assigned.
The relatively large ratio of minimum to maximum corrections applied
in the multiscan process (1:nnn) reflect changes in the illuminated
volume of the crystal.
Changes in illuminated volume were kept to a minimum, and were
taken into account (G\"orbitz, 1999) by the multi-scan inter-frame
scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997).
G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098.
The H atoms were all located in a difference map, but those
attached to carbon atoms were repositioned geometrically.
The H atoms were initially refined with soft restraints on the
bond lengths and angles to regularise their geometry
(C---H in the range 0.93--0.98,
N---H in the range 0.86--0.89
N---H to 0.86
O---H = 0.82
\%A)
and
U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom),
after which the positions were refined with riding constraints
(Cooper et al, 2010).
Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst.
43, 1100-1107.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
# Hand-made tables can be put in the cif. The number of columns
# is set in the loop header.
# The contants of each column can either be a piece of text
# without any spaces (eg a number) or other text enclosed in " "
# Remove the leading # in the following example
#_geom_extra_table_head_A
#;
#Table 2.
#Molecular parameters deviating most from MOGUL averages
#;
#
#loop_
#_geom_extra_tableA_col_1
#_geom_extra_tableA_col_2
#_geom_extra_tableA_col_3
#_geom_extra_tableA_col_4
#
#Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d"
#N5-C6-C4 129 124 "7 (\%)"
#C3-O10-C2 105 109 "2 (\%)"
#C6-O7 1.25 1.22 ".02 (\%A)"
#
data_RScarnitinenitrilechloride
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 7.2588(3)
_cell_length_b 8.9399(4)
_cell_length_c 22.7927(9)
_cell_angle_alpha 90
_cell_angle_beta 95.818(4)
_cell_angle_gamma 90
_cell_volume 1471.47(11)
_symmetry_cell_setting 'monoclinic'
_symmetry_space_group_name_H-M 'P 21 '
_symmetry_space_group_name_Hall 'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x,y+1/2,-z'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687
0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424
0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975
1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194
1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 6
# Given Formula = C8.17 H17.50 Cl1.17 N2.33 O1.17
# Dc = 1.41 Fooo = 672.00 Mu = 3.99 M = 208.44
# Found Formula = C7 H15 Cl1 N2 O1
# Dc = 1.21 FOOO = 576.00 Mu = 3.42 M = 178.66
_chemical_formula_sum 'C7 H15 Cl N2 O'
_chemical_formula_moiety 'C7 H15 N2 O, Cl'
_chemical_compound_source ?
_chemical_formula_weight 178.66
_cell_measurement_reflns_used 7637
_cell_measurement_theta_min 3
_cell_measurement_theta_max 33
_cell_measurement_temperature 183
_exptl_crystal_description 'block'
_exptl_crystal_colour 'yellow'
_exptl_crystal_size_min 0.062
_exptl_crystal_size_mid 0.081
_exptl_crystal_size_max 0.125
_exptl_crystal_density_diffrn 1.210
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 576
_exptl_absorpt_coefficient_mu 0.342
# Sheldrick geometric approximatio 0.97 0.98
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)'
_exptl_absorpt_correction_T_min 0.77
_exptl_absorpt_correction_T_max 0.98
_diffrn_measurement_device_type 'Oxford Diffraction SuperNova'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'graphite'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction 'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 183
_diffrn_reflns_number 23769
_reflns_number_total 10401
_diffrn_reflns_av_R_equivalents 0.032
# Number of reflections without Friedels Law is 10401
# Number of reflections with Friedels Law is 5645
# Theoretical number of reflections is about 5360
_diffrn_reflns_theta_min 2.449
_diffrn_reflns_theta_max 32.576
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 32.576
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -34
_diffrn_reflns_limit_l_max 30
_reflns_limit_h_min -10
_reflns_limit_h_max 10
_reflns_limit_k_min -13
_reflns_limit_k_max 13
_reflns_limit_l_min 0
_reflns_limit_l_max 34
_oxford_diffrn_Wilson_B_factor 1.97
_oxford_diffrn_Wilson_scale 10.15
_atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.43
_refine_diff_density_max 0.75
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns 10401
_refine_ls_number_restraints 1
_refine_ls_number_parameters 299
_oxford_refine_ls_R_factor_ref 0.0735
_refine_ls_wR_factor_ref 0.1277
_refine_ls_goodness_of_fit_ref 0.9968
_refine_ls_shift/su_max 0.0004225
_refine_ls_shift/su_mean 0.0000285
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 10401
_refine_ls_R_factor_all 0.0735
_refine_ls_wR_factor_all 0.1277
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 7769
_refine_ls_R_factor_gt 0.0517
_refine_ls_wR_factor_gt 0.1171
_refine_ls_abs_structure_Flack -0.03(4)
_refine_ls_abs_structure_details 'Flack (1983), 4756 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration 'ad'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 0.23P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Agilent (2011). CrysAlisPro.
Oxford Diffraction, (2010). Supernova User Manual.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
N1 N 0.2393(4) 0.4065(3) 0.12418(11) 0.0559 1.0000 Uani . . . . . .
C2 C 0.2157(3) 0.2895(3) 0.10570(9) 0.0342 1.0000 Uani . . . . . .
C3 C 0.1838(3) 0.1392(3) 0.08215(8) 0.0296 1.0000 Uani . . . . . .
C4 C 0.1255(3) 0.1376(2) 0.01532(8) 0.0257 1.0000 Uani . . . . . .
O5 O -0.03223(19) 0.2299(2) 0.00070(6) 0.0340 1.0000 Uani . . . . . .
C6 C 0.2840(3) 0.1967(2) -0.01686(8) 0.0252 1.0000 Uani . . . . . .
N7 N 0.2810(2) 0.1497(2) -0.08098(7) 0.0241 1.0000 Uani . . . . . .
C8 C 0.4525(3) 0.2129(3) -0.10372(10) 0.0325 1.0000 Uani . . . . . .
C9 C 0.1145(3) 0.2128(3) -0.11692(8) 0.0305 1.0000 Uani . . . . . .
C10 C 0.2841(4) -0.0149(3) -0.08814(13) 0.0402 1.0000 Uani . . . . . .
N11 N 1.2671(3) 0.9068(3) 0.20806(11) 0.0549 1.0000 Uani . . . . . .
C12 C 1.2555(3) 0.7904(3) 0.22713(9) 0.0343 1.0000 Uani . . . . . .
C13 C 1.2383(3) 0.6400(3) 0.25102(8) 0.0303 1.0000 Uani . . . . . .
C14 C 1.2224(3) 0.6390(2) 0.31816(8) 0.0255 1.0000 Uani . . . . . .
O15 O 1.07428(19) 0.73225(19) 0.33227(6) 0.0322 1.0000 Uani . . . . . .
C16 C 1.4029(3) 0.6991(2) 0.35002(8) 0.0238 1.0000 Uani . . . . . .
N17 N 1.4408(2) 0.6523(2) 0.41398(7) 0.0245 1.0000 Uani . . . . . .
C18 C 1.6277(3) 0.7165(3) 0.43570(10) 0.0323 1.0000 Uani . . . . . .
C19 C 1.2992(3) 0.7148(3) 0.45062(8) 0.0279 1.0000 Uani . . . . . .
C20 C 1.4500(4) 0.4874(3) 0.42137(13) 0.0394 1.0000 Uani . . . . . .
N21 N 0.9535(3) 0.4159(3) 0.45514(11) 0.0531 1.0000 Uani . . . . . .
C22 C 0.9660(3) 0.2977(3) 0.43772(10) 0.0338 1.0000 Uani . . . . . .
C23 C 0.9810(3) 0.1461(3) 0.41538(9) 0.0306 1.0000 Uani . . . . . .
C24 C 0.9950(3) 0.1403(2) 0.34836(8) 0.0253 1.0000 Uani . . . . . .
O25 O 1.14212(19) 0.23254(19) 0.33271(6) 0.0326 1.0000 Uani . . . . . .
C26 C 0.8145(3) 0.1984(2) 0.31640(8) 0.0247 1.0000 Uani . . . . . .
N27 N 0.7760(2) 0.1497(2) 0.25248(7) 0.0245 1.0000 Uani . . . . . .
C28 C 0.9175(3) 0.2127(3) 0.21587(8) 0.0304 1.0000 Uani . . . . . .
C29 C 0.5882(3) 0.2126(3) 0.23068(10) 0.0326 1.0000 Uani . . . . . .
C30 C 0.7678(4) -0.0158(3) 0.24591(13) 0.0417 1.0000 Uani . . . . . .
Cl31 Cl 0.68275(6) 0.08879(8) 0.073991(18) 0.0267 1.0000 Uani . . . . . .
Cl32 Cl 0.74341(6) 0.58876(8) 0.259692(19) 0.0267 1.0000 Uani . . . . . .
Cl33 Cl 0.46947(6) 0.09158(9) 0.407349(19) 0.0277 1.0000 Uani . . . . . .
H293 H 0.5566 0.1906 0.1890 0.0481 1.0000 Uiso R . . . . .
H292 H 0.5951 0.3196 0.2370 0.0484 1.0000 Uiso R . . . . .
H291 H 0.4959 0.1695 0.2544 0.0492 1.0000 Uiso R . . . . .
H281 H 0.8819 0.1926 0.1769 0.0451 1.0000 Uiso R . . . . .
H283 H 1.0383 0.1666 0.2293 0.0450 1.0000 Uiso R . . . . .
H282 H 0.9206 0.3147 0.2216 0.0451 1.0000 Uiso R . . . . .
H302 H 0.7309 -0.0444 0.2060 0.0649 1.0000 Uiso R . . . . .
H303 H 0.8890 -0.0600 0.2561 0.0647 1.0000 Uiso R . . . . .
H301 H 0.6752 -0.0617 0.2693 0.0648 1.0000 Uiso R . . . . .
H262 H 0.8159 0.3074 0.3193 0.0312 1.0000 Uiso R . . . . .
H261 H 0.7105 0.1663 0.3372 0.0307 1.0000 Uiso R . . . . .
H232 H 1.0923 0.0953 0.4311 0.0367 1.0000 Uiso R . . . . .
H231 H 0.8639 0.0916 0.4204 0.0354 1.0000 Uiso R . . . . .
H241 H 1.0101 0.0345 0.3369 0.0327 1.0000 Uiso R . . . . .
H251 H 1.2353 0.1987 0.3511 0.0485 1.0000 Uiso R . . . . .
H193 H 1.3319 0.6890 0.4898 0.0429 1.0000 Uiso R . . . . .
H192 H 1.2947 0.8205 0.4465 0.0420 1.0000 Uiso R . . . . .
H191 H 1.1789 0.6672 0.4354 0.0422 1.0000 Uiso R . . . . .
H181 H 1.6529 0.6904 0.4755 0.0467 1.0000 Uiso R . . . . .
H183 H 1.6263 0.8204 0.4318 0.0468 1.0000 Uiso R . . . . .
H182 H 1.7204 0.6742 0.4135 0.0473 1.0000 Uiso R . . . . .
H202 H 1.4901 0.4617 0.4609 0.0606 1.0000 Uiso R . . . . .
H203 H 1.5372 0.4438 0.3963 0.0602 1.0000 Uiso R . . . . .
H201 H 1.3317 0.4398 0.4123 0.0603 1.0000 Uiso R . . . . .
H162 H 1.4006 0.8051 0.3463 0.0294 1.0000 Uiso R . . . . .
H161 H 1.5100 0.6644 0.3309 0.0282 1.0000 Uiso R . . . . .
H132 H 1.3439 0.5794 0.2418 0.0365 1.0000 Uiso R . . . . .
H131 H 1.1140 0.5917 0.2392 0.0315 1.0000 Uiso R . . . . .
H141 H 1.2051 0.5324 0.3288 0.0317 1.0000 Uiso R . . . . .
H151 H 0.9725 0.7015 0.3139 0.0483 1.0000 Uiso R . . . . .
H93 H 0.1222 0.1904 -0.1558 0.0451 1.0000 Uiso R . . . . .
H92 H 0.1139 0.3161 -0.1120 0.0453 1.0000 Uiso R . . . . .
H91 H 0.0002 0.1658 -0.1018 0.0441 1.0000 Uiso R . . . . .
H81 H 0.4568 0.1851 -0.1445 0.0478 1.0000 Uiso R . . . . .
H83 H 0.4507 0.3195 -0.1005 0.0483 1.0000 Uiso R . . . . .
H82 H 0.5592 0.1745 -0.0800 0.0489 1.0000 Uiso R . . . . .
H102 H 0.3088 -0.0433 -0.1273 0.0618 1.0000 Uiso R . . . . .
H103 H 0.3918 -0.0555 -0.0634 0.0618 1.0000 Uiso R . . . . .
H101 H 0.1701 -0.0634 -0.0775 0.0618 1.0000 Uiso R . . . . .
H62 H 0.2846 0.3043 -0.0146 0.0306 1.0000 Uiso R . . . . .
H61 H 0.4010 0.1728 0.0028 0.0289 1.0000 Uiso R . . . . .
H32 H 0.2906 0.0744 0.0922 0.0365 1.0000 Uiso R . . . . .
H31 H 0.0627 0.0930 0.0923 0.0311 1.0000 Uiso R . . . . .
H41 H 0.0979 0.0323 0.0038 0.0318 1.0000 Uiso R . . . . .
H51 H -0.1290 0.1987 0.0180 0.0509 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0578(15) 0.0637(16) 0.0464(13) -0.0177(12) 0.0065(11) -0.0085(12)
C2 0.0269(10) 0.0507(14) 0.0255(10) 0.0002(9) 0.0055(8) -0.0002(9)
C3 0.0281(10) 0.0406(11) 0.0205(8) 0.0044(8) 0.0044(7) 0.0037(8)
C4 0.0259(9) 0.0288(9) 0.0226(8) 0.0014(7) 0.0026(7) 0.0016(7)
O5 0.0223(7) 0.0475(9) 0.0325(7) 0.0093(7) 0.0043(5) 0.0070(6)
C6 0.0259(9) 0.0298(10) 0.0195(8) 0.0007(7) 0.0010(6) -0.0006(7)
N7 0.0263(8) 0.0263(8) 0.0202(7) -0.0006(6) 0.0040(6) 0.0017(7)
C8 0.0271(10) 0.0351(11) 0.0368(11) -0.0008(9) 0.0104(8) -0.0006(9)
C9 0.0300(10) 0.0415(12) 0.0195(8) -0.0020(8) 0.0008(7) -0.0005(9)
C10 0.0523(16) 0.0245(11) 0.0467(14) -0.0066(10) 0.0191(12) -0.0042(10)
N11 0.0514(14) 0.0638(16) 0.0486(13) 0.0177(12) 0.0008(10) -0.0051(12)
C12 0.0268(10) 0.0511(14) 0.0244(9) 0.0016(9) 0.0003(8) -0.0003(9)
C13 0.0271(10) 0.0442(11) 0.0192(8) -0.0064(8) -0.0002(7) 0.0036(8)
C14 0.0230(9) 0.0288(9) 0.0244(8) -0.0021(7) 0.0008(6) 0.0012(7)
O15 0.0220(7) 0.0446(9) 0.0299(7) -0.0074(7) 0.0016(5) 0.0063(6)
C16 0.0212(8) 0.0275(9) 0.0221(8) -0.0016(7) 0.0001(6) -0.0006(7)
N17 0.0214(8) 0.0287(8) 0.0225(7) -0.0004(6) -0.0023(6) 0.0048(7)
C18 0.0229(9) 0.0354(11) 0.0372(11) 0.0014(9) -0.0035(8) -0.0003(8)
C19 0.0278(9) 0.0381(11) 0.0183(8) -0.0012(8) 0.0055(7) 0.0013(8)
C20 0.0461(15) 0.0217(10) 0.0483(14) 0.0011(10) -0.0057(11) 0.0037(9)
N21 0.0530(14) 0.0560(15) 0.0518(13) -0.0167(12) 0.0135(11) -0.0055(12)
C22 0.0271(10) 0.0469(14) 0.0277(10) -0.0005(9) 0.0045(8) -0.0019(9)
C23 0.0289(10) 0.0392(11) 0.0234(8) 0.0056(8) 0.0010(7) -0.0036(8)
C24 0.0242(9) 0.0291(9) 0.0224(8) 0.0008(7) 0.0015(6) 0.0012(7)
O25 0.0209(7) 0.0479(9) 0.0286(7) 0.0086(7) 0.0006(5) -0.0038(6)
C26 0.0232(9) 0.0296(10) 0.0213(8) -0.0007(7) 0.0028(6) 0.0020(7)
N27 0.0238(8) 0.0279(8) 0.0212(7) -0.0027(7) -0.0007(6) -0.0015(7)
C28 0.0290(10) 0.0415(12) 0.0213(8) -0.0025(8) 0.0048(7) -0.0012(9)
C29 0.0234(9) 0.0359(12) 0.0377(11) -0.0022(9) -0.0009(8) 0.0016(8)
C30 0.0455(15) 0.0235(11) 0.0530(15) -0.0051(10) -0.0106(11) 0.0020(9)
Cl31 0.02254(18) 0.0283(2) 0.0287(2) 0.0018(2) 0.00047(14) -0.0005(2)
Cl32 0.02404(19) 0.0278(2) 0.02883(19) -0.0023(2) 0.00502(14) -0.0006(2)
Cl33 0.02406(18) 0.0287(2) 0.03004(19) 0.0019(2) 0.00127(14) -0.0012(2)
_refine_ls_extinction_method
'None'
_oxford_refine_ls_scale 0.3571(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 . C2 . 1.134(3) yes
C2 . C3 . 1.456(3) yes
C3 . C4 . 1.539(3) yes
C3 . H32 . 0.977 no
C3 . H31 . 1.019 no
C4 . O5 . 1.423(2) yes
C4 . C6 . 1.521(3) yes
C4 . H41 . 0.992 no
O5 . H51 . 0.884 no
C6 . N7 . 1.518(2) yes
C6 . H62 . 0.963 no
C6 . H61 . 0.943 no
N7 . C8 . 1.506(3) yes
N7 . C9 . 1.499(3) yes
N7 . C10 . 1.481(3) yes
C8 . H81 . 0.966 no
C8 . H83 . 0.956 no
C8 . H82 . 0.962 no
C9 . H93 . 0.914 no
C9 . H92 . 0.931 no
C9 . H91 . 1.020 no
C10 . H102 . 0.962 no
C10 . H103 . 0.986 no
C10 . H101 . 0.986 no
N11 . C12 . 1.134(3) yes
C12 . C13 . 1.461(3) yes
C13 . C14 . 1.546(3) yes
C13 . H132 . 0.979 no
C13 . H131 . 1.012 no
C14 . O15 . 1.423(2) yes
C14 . C16 . 1.530(3) yes
C14 . H141 . 0.994 no
O15 . H151 . 0.856 no
C16 . N17 . 1.515(2) yes
C16 . H162 . 0.952 no
C16 . H161 . 0.980 no
N17 . C18 . 1.509(3) yes
N17 . C19 . 1.497(3) yes
N17 . C20 . 1.485(3) yes
C18 . H181 . 0.937 no
C18 . H183 . 0.933 no
C18 . H182 . 0.959 no
C19 . H193 . 0.930 no
C19 . H192 . 0.950 no
C19 . H191 . 1.001 no
C20 . H202 . 0.947 no
C20 . H203 . 0.976 no
C20 . H201 . 0.962 no
N21 . C22 . 1.136(3) yes
C22 . C23 . 1.456(4) yes
C23 . C24 . 1.542(3) yes
C23 . H232 . 0.964 no
C23 . H231 . 0.996 no
C24 . O25 . 1.423(2) yes
C24 . C26 . 1.524(3) yes
C24 . H241 . 0.990 no
O25 . H251 . 0.817 no
C26 . N27 . 1.519(2) yes
C26 . H262 . 0.977 no
C26 . H261 . 0.975 no
N27 . C28 . 1.498(3) yes
N27 . C29 . 1.511(3) yes
N27 . C30 . 1.488(3) yes
C28 . H281 . 0.917 no
C28 . H283 . 0.989 no
C28 . H282 . 0.921 no
C29 . H293 . 0.975 no
C29 . H292 . 0.968 no
C29 . H291 . 0.982 no
C30 . H302 . 0.957 no
C30 . H303 . 0.971 no
C30 . H301 . 0.989 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . C2 . C3 . 179.5(2) yes
C2 . C3 . C4 . 113.03(18) yes
C2 . C3 . H32 . 111.6 no
C4 . C3 . H32 . 111.0 no
C2 . C3 . H31 . 113.5 no
C4 . C3 . H31 . 93.7 no
H32 . C3 . H31 . 112.8 no
C3 . C4 . O5 . 111.10(16) yes
C3 . C4 . C6 . 109.16(16) yes
O5 . C4 . C6 . 108.40(16) yes
C3 . C4 . H41 . 107.4 no
O5 . C4 . H41 . 110.7 no
C6 . C4 . H41 . 110.1 no
C4 . O5 . H51 . 111.6 no
C4 . C6 . N7 . 115.48(16) yes
C4 . C6 . H62 . 108.7 no
N7 . C6 . H62 . 109.1 no
C4 . C6 . H61 . 112.4 no
N7 . C6 . H61 . 108.6 no
H62 . C6 . H61 . 101.6 no
C6 . N7 . C8 . 107.20(16) yes
C6 . N7 . C9 . 110.76(15) yes
C8 . N7 . C9 . 108.65(16) yes
C6 . N7 . C10 . 112.44(17) yes
C8 . N7 . C10 . 108.18(19) yes
C9 . N7 . C10 . 109.5(2) yes
N7 . C8 . H81 . 110.1 no
N7 . C8 . H83 . 109.2 no
H81 . C8 . H83 . 109.4 no
N7 . C8 . H82 . 108.6 no
H81 . C8 . H82 . 110.3 no
H83 . C8 . H82 . 109.2 no
N7 . C9 . H93 . 108.8 no
N7 . C9 . H92 . 108.7 no
H93 . C9 . H92 . 109.6 no
N7 . C9 . H91 . 107.4 no
H93 . C9 . H91 . 111.6 no
H92 . C9 . H91 . 110.7 no
N7 . C10 . H102 . 111.7 no
N7 . C10 . H103 . 108.8 no
H102 . C10 . H103 . 102.9 no
N7 . C10 . H101 . 112.8 no
H102 . C10 . H101 . 110.7 no
H103 . C10 . H101 . 109.5 no
N11 . C12 . C13 . 179.2(2) yes
C12 . C13 . C14 . 113.09(18) yes
C12 . C13 . H132 . 109.4 no
C14 . C13 . H132 . 110.4 no
C12 . C13 . H131 . 113.6 no
C14 . C13 . H131 . 96.1 no
H132 . C13 . H131 . 113.8 no
C13 . C14 . O15 . 110.75(16) yes
C13 . C14 . C16 . 108.73(17) yes
O15 . C14 . C16 . 108.50(16) yes
C13 . C14 . H141 . 105.8 no
O15 . C14 . H141 . 112.9 no
C16 . C14 . H141 . 110.1 no
C14 . O15 . H151 . 109.6 no
C14 . C16 . N17 . 115.06(16) yes
C14 . C16 . H162 . 107.5 no
N17 . C16 . H162 . 111.1 no
C14 . C16 . H161 . 111.0 no
N17 . C16 . H161 . 105.4 no
H162 . C16 . H161 . 106.5 no
C16 . N17 . C18 . 106.30(17) yes
C16 . N17 . C19 . 111.46(15) yes
C18 . N17 . C19 . 108.69(17) yes
C16 . N17 . C20 . 112.63(18) yes
C18 . N17 . C20 . 108.16(19) yes
C19 . N17 . C20 . 109.4(2) yes
N17 . C18 . H181 . 107.7 no
N17 . C18 . H183 . 110.3 no
H181 . C18 . H183 . 109.9 no
N17 . C18 . H182 . 109.4 no
H181 . C18 . H182 . 109.5 no
H183 . C18 . H182 . 110.0 no
N17 . C19 . H193 . 108.7 no
N17 . C19 . H192 . 109.6 no
H193 . C19 . H192 . 110.1 no
N17 . C19 . H191 . 105.8 no
H193 . C19 . H191 . 110.9 no
H192 . C19 . H191 . 111.7 no
N17 . C20 . H202 . 110.8 no
N17 . C20 . H203 . 110.8 no
H202 . C20 . H203 . 107.8 no
N17 . C20 . H201 . 112.7 no
H202 . C20 . H201 . 106.2 no
H203 . C20 . H201 . 108.4 no
N21 . C22 . C23 . 179.7(3) yes
C22 . C23 . C24 . 113.12(18) yes
C22 . C23 . H232 . 113.5 no
C24 . C23 . H232 . 102.4 no
C22 . C23 . H231 . 108.7 no
C24 . C23 . H231 . 103.9 no
H232 . C23 . H231 . 114.9 no
C23 . C24 . O25 . 110.82(16) yes
C23 . C24 . C26 . 108.79(17) yes
O25 . C24 . C26 . 108.26(16) yes
C23 . C24 . H241 . 108.3 no
O25 . C24 . H241 . 112.4 no
C26 . C24 . H241 . 108.2 no
C24 . O25 . H251 . 105.1 no
C24 . C26 . N27 . 115.26(16) yes
C24 . C26 . H262 . 107.8 no
N27 . C26 . H262 . 110.5 no
C24 . C26 . H261 . 109.8 no
N27 . C26 . H261 . 107.8 no
H262 . C26 . H261 . 105.3 no
C26 . N27 . C28 . 110.88(15) yes
C26 . N27 . C29 . 106.33(16) yes
C28 . N27 . C29 . 108.88(16) yes
C26 . N27 . C30 . 112.52(18) yes
C28 . N27 . C30 . 109.9(2) yes
C29 . N27 . C30 . 108.16(19) yes
N27 . C28 . H281 . 108.9 no
N27 . C28 . H283 . 107.9 no
H281 . C28 . H283 . 111.8 no
N27 . C28 . H282 . 107.5 no
H281 . C28 . H282 . 109.5 no
H283 . C28 . H282 . 111.2 no
N27 . C29 . H293 . 111.1 no
N27 . C29 . H292 . 106.7 no
H293 . C29 . H292 . 110.4 no
N27 . C29 . H291 . 108.4 no
H293 . C29 . H291 . 110.6 no
H292 . C29 . H291 . 109.5 no
N27 . C30 . H302 . 111.5 no
N27 . C30 . H303 . 110.8 no
H302 . C30 . H303 . 106.1 no
N27 . C30 . H301 . 112.4 no
H302 . C30 . H301 . 105.1 no
H303 . C30 . H301 . 110.6 no
_iucr_refine_instructions_details
;
#
# Punched on 15/06/18 at 10:47:25
#
#LIST 12
BLOCK SCALE X'S U'S
CONT ENANTIO
RIDE C ( 3,X'S) H ( 32,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE O ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 62,X'S) H ( 61,X'S)
RIDE C ( 8,X'S) H ( 81,X'S) H ( 83,X'S) H ( 82,X'S)
RIDE C ( 9,X'S) H ( 93,X'S) H ( 92,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 102,X'S) H ( 103,X'S) H ( 101,X'S)
RIDE C ( 13,X'S) H ( 132,X'S) H ( 131,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE O ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 162,X'S) H ( 161,X'S)
RIDE C ( 18,X'S) H ( 181,X'S) H ( 183,X'S) H ( 182,X'S)
RIDE C ( 19,X'S) H ( 193,X'S) H ( 192,X'S) H ( 191,X'S)
RIDE C ( 20,X'S) H ( 202,X'S) H ( 203,X'S) H ( 201,X'S)
RIDE C ( 23,X'S) H ( 232,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE O ( 25,X'S) H ( 251,X'S)
RIDE C ( 26,X'S) H ( 262,X'S) H ( 261,X'S)
RIDE C ( 28,X'S) H ( 281,X'S) H ( 283,X'S) H ( 282,X'S)
RIDE C ( 29,X'S) H ( 293,X'S) H ( 292,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 302,X'S) H ( 303,X'S) H ( 301,X'S)
END
#
# Punched on 15/06/18 at 10:47:25
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
data_RScarnitinenitrileiodide
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 13.4725(2)
_cell_length_b 9.85510(10)
_cell_length_c 32.7259(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 4345.11(9)
_symmetry_cell_setting 'orthorhombic'
_symmetry_space_group_name_H-M 'P b c a '
_symmetry_space_group_name_Hall '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x,-y,-z'
'x,-y+1/2,z+1/2'
'-x,y+1/2,-z+1/2'
'-x+1/2,-y,z+1/2'
'x+1/2,y,-z+1/2'
'x+1/2,-y+1/2,-z'
'-x+1/2,y+1/2,z'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687
0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424
0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975
1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
I -0.3257 6.8362 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660
2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 16
# Given Formula = C7 H14 I1 N2 O1
# Dc = 1.65 Fooo = 2096.00 Mu = 228.26 M = 269.11
# Found Formula = C7 H15 I1 N2 O1
# Dc = 1.65 FOOO = 2112.00 Mu = 228.26 M = 270.11
_chemical_formula_sum 'C7 H15 I N2 O'
_chemical_formula_moiety 'C7 H15 N2 O, I'
_chemical_compound_source ?
_chemical_formula_weight 270.11
_cell_measurement_reflns_used 9526
_cell_measurement_theta_min 5
_cell_measurement_theta_max 79
_cell_measurement_temperature 160
_exptl_crystal_description 'plate'
_exptl_crystal_colour 'colorless'
_exptl_crystal_size_min 0.047
_exptl_crystal_size_mid 0.102
_exptl_crystal_size_max 0.115
_exptl_crystal_density_diffrn 1.652
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 2112
_exptl_absorpt_coefficient_mu 22.826
# Sheldrick geometric approximatio 0.10 0.34
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro (Rigaku Oxford Diffraction, 2017)
;
_exptl_absorpt_correction_T_min 0.12
_exptl_absorpt_correction_T_max 0.34
_diffrn_measurement_device_type 'Oxford Diffraction SuperNova'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'focussing mirrors'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54180
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement
;
CrysAlisPro (Rigaku Oxford Diffraction, 2017)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku Oxford Diffraction, 2017)
;
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 160
_diffrn_reflns_number 17435
_reflns_number_total 4437
_diffrn_reflns_av_R_equivalents 0.032
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 4437
# Theoretical number of reflections is about 8887
_diffrn_reflns_theta_min 4.251
_diffrn_reflns_theta_max 74.495
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 74.495
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -39
_diffrn_reflns_limit_l_max 40
_reflns_limit_h_min 0
_reflns_limit_h_max 16
_reflns_limit_k_min 0
_reflns_limit_k_max 12
_reflns_limit_l_min 0
_reflns_limit_l_max 40
_oxford_diffrn_Wilson_B_factor 3.86
_oxford_diffrn_Wilson_scale 0.90
_atom_sites_solution_primary other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.61
_refine_diff_density_max 1.97
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_restraints 2
_refine_ls_number_parameters 209
_refine_ls_number_reflns 4437
_oxford_refine_ls_R_factor_ref 0.0529
_refine_ls_wR_factor_ref 0.1128
_refine_ls_goodness_of_fit_ref 1.0124
_refine_ls_shift/su_max 0.0019919
_refine_ls_shift/su_mean 0.0000353
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 4437
_refine_ls_R_factor_all 0.0529
_refine_ls_wR_factor_all 0.1128
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 4082
_refine_ls_R_factor_gt 0.0492
_refine_ls_wR_factor_gt 0.1105
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +31.74P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Oxford Diffraction, (2010). Supernova User Manual.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Rigaku Oxford Diffraction (2017). CrysAlisPro.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
N1 N 0.7558(6) 0.4679(8) 0.54891(18) 0.0775 1.0000 Uani . . . . . .
C2 C 0.7749(5) 0.3800(8) 0.56924(18) 0.0528 1.0000 Uani . . . . . .
C3 C 0.7980(5) 0.2617(7) 0.59428(19) 0.0499 1.0000 Uani . . . . . .
C4 C 0.8279(4) 0.3040(6) 0.63764(17) 0.0403 1.0000 Uani . . . . . .
O5 O 0.7493(3) 0.3766(4) 0.65652(12) 0.0477 1.0000 Uani . . . . . .
C6 C 0.8555(4) 0.1739(6) 0.65983(17) 0.0417 1.0000 Uani . . . . . .
N7 N 0.9104(4) 0.1897(5) 0.70008(13) 0.0369 1.0000 Uani . . . . . .
C8 C 0.8546(5) 0.2769(6) 0.73039(18) 0.0457 1.0000 Uani . . . . . .
C9 C 1.0121(4) 0.2486(7) 0.69398(18) 0.0457 1.0000 Uani . . . . . .
C10 C 0.9205(5) 0.0500(7) 0.7174(2) 0.0527 1.0000 Uani . . . . . .
N11 N 0.2629(5) 0.5423(7) 0.70320(18) 0.0660 1.0000 Uani . . . . . .
C12 C 0.2715(5) 0.4543(8) 0.68075(17) 0.0485 1.0000 Uani . . . . . .
C13 C 0.2856(5) 0.3405(7) 0.65267(18) 0.0501 1.0000 Uani . . . . . .
C14 C 0.3472(4) 0.3832(6) 0.61548(17) 0.0478 1.0000 Uani D . . . . .
C16 C 0.3621(5) 0.2517(6) 0.59102(16) 0.0396 1.0000 Uani . . . . . .
N17 N 0.4157(3) 0.2668(4) 0.55040(13) 0.0343 1.0000 Uani . . . . . .
C18 C 0.3600(5) 0.3542(7) 0.52138(17) 0.0484 1.0000 Uani . . . . . .
C19 C 0.5179(5) 0.3217(8) 0.5561(2) 0.0543 1.0000 Uani . . . . . .
C20 C 0.4229(6) 0.1255(6) 0.5330(2) 0.0554 1.0000 Uani . . . . . .
I21 I 0.07520(3) 0.24189(4) 0.567724(13) 0.0539 1.0000 Uani . . . . . .
I22 I 0.55599(3) 0.15399(4) 0.677831(12) 0.0495 1.0000 Uani . . . . . .
H31 H 0.8520 0.2128 0.5817 0.0599 1.0000 Uiso R . . . . .
H32 H 0.7403 0.2038 0.5957 0.0599 1.0000 Uiso R . . . . .
H41 H 0.8866 0.3641 0.6360 0.0480 1.0000 Uiso R . . . . .
H61 H 0.7953 0.1226 0.6650 0.0497 1.0000 Uiso R . . . . .
H62 H 0.8993 0.1222 0.6425 0.0499 1.0000 Uiso R . . . . .
H82 H 0.8890 0.2746 0.7561 0.0677 1.0000 Uiso R . . . . .
H81 H 0.7882 0.2414 0.7332 0.0680 1.0000 Uiso R . . . . .
H83 H 0.8521 0.3682 0.7204 0.0680 1.0000 Uiso R . . . . .
H92 H 1.0480 0.2473 0.7192 0.0677 1.0000 Uiso R . . . . .
H93 H 1.0476 0.1988 0.6737 0.0679 1.0000 Uiso R . . . . .
H91 H 1.0065 0.3399 0.6848 0.0681 1.0000 Uiso R . . . . .
H102 H 0.9553 0.0556 0.7429 0.0789 1.0000 Uiso R . . . . .
H101 H 0.8556 0.0121 0.7220 0.0792 1.0000 Uiso R . . . . .
H103 H 0.9572 -0.0065 0.6989 0.0788 1.0000 Uiso R . . . . .
H132 H 0.3215 0.2697 0.6668 0.0602 1.0000 Uiso R . . . . .
H131 H 0.2217 0.3065 0.6442 0.0600 1.0000 Uiso R . . . . .
H161 H 0.4015 0.1909 0.6076 0.0479 1.0000 Uiso R . . . . .
H162 H 0.2981 0.2106 0.5852 0.0480 1.0000 Uiso R . . . . .
H182 H 0.3903 0.3494 0.4948 0.0727 1.0000 Uiso R . . . . .
H183 H 0.3611 0.4471 0.5310 0.0729 1.0000 Uiso R . . . . .
H181 H 0.2918 0.3227 0.5194 0.0728 1.0000 Uiso R . . . . .
H191 H 0.5530 0.3146 0.5308 0.0819 1.0000 Uiso R . . . . .
H193 H 0.5510 0.2681 0.5766 0.0818 1.0000 Uiso R . . . . .
H192 H 0.5141 0.4154 0.5649 0.0818 1.0000 Uiso R . . . . .
H51 H 0.7061 0.3177 0.6592 0.0721 1.0000 Uiso R . . . . .
H203 H 0.4584 0.1286 0.5077 0.0839 1.0000 Uiso R . . . . .
H202 H 0.4581 0.0693 0.5523 0.0840 1.0000 Uiso R . . . . .
H201 H 0.3573 0.0909 0.5287 0.0839 1.0000 Uiso R . . . . .
O151 O 0.4397(5) 0.4364(10) 0.6315(3) 0.0800 0.647(11) Uani D . P 1 1 .
O152 O 0.2671(9) 0.4530(15) 0.5946(4) 0.0782 0.353(11) Uani D . P 1 2 .
H141 H 0.3140 0.4534 0.5993 0.0582 0.647(11) Uiso R . P 1 1 .
H142 H 0.4063 0.4390 0.6206 0.0581 0.353(11) Uiso R . P 1 2 .
H1511 H 0.4663 0.3705 0.6422 0.0918 0.647(11) Uiso R . P 1 1 .
H1521 H 0.2221 0.4010 0.5883 0.0812 0.353(11) Uiso R . P 1 2 .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.107(6) 0.079(5) 0.046(3) -0.002(3) -0.006(4) 0.032(4)
C2 0.059(4) 0.064(4) 0.035(3) -0.006(3) -0.009(3) 0.014(3)
C3 0.056(4) 0.051(4) 0.043(3) -0.007(3) -0.011(3) 0.008(3)
C4 0.043(3) 0.040(3) 0.037(3) -0.003(2) -0.001(2) 0.004(3)
O5 0.048(2) 0.044(2) 0.051(2) -0.0053(19) 0.004(2) 0.0083(19)
C6 0.044(3) 0.043(3) 0.038(3) -0.003(2) 0.001(2) 0.002(3)
N7 0.042(2) 0.040(3) 0.028(2) -0.0022(19) 0.0054(19) 0.004(2)
C8 0.054(3) 0.046(3) 0.037(3) -0.005(3) 0.010(3) 0.012(3)
C9 0.039(3) 0.054(4) 0.044(3) 0.003(3) 0.002(2) -0.005(3)
C10 0.071(4) 0.042(3) 0.045(3) 0.003(3) -0.004(3) 0.006(3)
N11 0.085(4) 0.067(4) 0.047(3) 0.001(3) 0.016(3) 0.019(4)
C12 0.046(3) 0.068(4) 0.032(3) 0.004(3) 0.009(2) 0.006(3)
C13 0.052(3) 0.063(4) 0.035(3) -0.001(3) 0.005(3) -0.013(3)
C14 0.070(4) 0.039(3) 0.034(3) 0.004(2) 0.011(3) 0.007(3)
C16 0.052(3) 0.034(3) 0.032(3) 0.007(2) 0.002(2) -0.002(3)
N17 0.045(2) 0.028(2) 0.031(2) -0.0010(18) -0.0007(19) -0.0002(19)
C18 0.060(4) 0.052(4) 0.032(3) 0.009(3) -0.001(3) 0.003(3)
C19 0.050(4) 0.066(4) 0.047(4) 0.007(3) -0.002(3) -0.008(3)
C20 0.079(5) 0.036(3) 0.051(4) -0.010(3) 0.011(3) 0.001(3)
I21 0.0656(3) 0.0482(2) 0.0478(2) 0.00067(18) -0.01535(19) 0.0117(2)
I22 0.0469(2) 0.0507(2) 0.0510(2) 0.00087(18) 0.00861(17) 0.00453(18)
O151 0.061(5) 0.092(7) 0.087(6) -0.055(5) 0.021(4) -0.041(5)
O152 0.135(15) 0.054(9) 0.045(7) 0.008(6) 0.007(8) 0.038(10)
_refine_ls_extinction_method
'None'
_oxford_refine_ls_scale 1.055(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 . C2 . 1.123(9) yes
C2 . C3 . 1.459(9) yes
C3 . C4 . 1.532(8) yes
C3 . H31 . 0.964 no
C3 . H32 . 0.965 no
C4 . O5 . 1.420(7) yes
C4 . C6 . 1.519(8) yes
C4 . H41 . 0.989 no
O5 . H51 . 0.827 no
C6 . N7 . 1.518(7) yes
C6 . H61 . 0.972 no
C6 . H62 . 0.965 no
N7 . C8 . 1.511(7) yes
N7 . C9 . 1.502(7) yes
N7 . C10 . 1.496(8) yes
C8 . H82 . 0.961 no
C8 . H81 . 0.966 no
C8 . H83 . 0.958 no
C9 . H92 . 0.956 no
C9 . H93 . 0.954 no
C9 . H91 . 0.952 no
C10 . H102 . 0.959 no
C10 . H101 . 0.962 no
C10 . H103 . 0.960 no
N11 . C12 . 1.143(9) yes
C12 . C13 . 1.462(9) yes
C13 . C14 . 1.532(8) yes
C13 . H132 . 0.967 no
C13 . H131 . 0.965 no
C14 . C16 . 1.537(8) yes
C14 . O151 . 1.4508(10) yes
C14 . H141 . 0.979 no
C14 . C16 . 1.537(8) yes
C14 . O152 . 1.4506(10) yes
C14 . H142 . 0.982 no
C16 . N17 . 1.520(7) yes
C16 . H161 . 0.967 no
C16 . H162 . 0.971 no
N17 . C18 . 1.486(7) yes
N17 . C19 . 1.491(8) yes
N17 . C20 . 1.508(7) yes
C18 . H182 . 0.961 no
C18 . H183 . 0.968 no
C18 . H181 . 0.971 no
C19 . H191 . 0.958 no
C19 . H193 . 0.963 no
C19 . H192 . 0.968 no
C20 . H203 . 0.958 no
C20 . H202 . 0.964 no
C20 . H201 . 0.959 no
O151 . H1511 . 0.820 no
O152 . H1521 . 0.820 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . C2 . C3 . 177.5(7) yes
C2 . C3 . C4 . 111.0(5) yes
C2 . C3 . H31 . 108.6 no
C4 . C3 . H31 . 109.5 no
C2 . C3 . H32 . 109.1 no
C4 . C3 . H32 . 109.2 no
H31 . C3 . H32 . 109.4 no
C3 . C4 . O5 . 110.1(5) yes
C3 . C4 . C6 . 106.1(5) yes
O5 . C4 . C6 . 113.6(5) yes
C3 . C4 . H41 . 108.8 no
O5 . C4 . H41 . 108.5 no
C6 . C4 . H41 . 109.6 no
C4 . O5 . H51 . 102.5 no
C4 . C6 . N7 . 116.6(5) yes
C4 . C6 . H61 . 108.5 no
N7 . C6 . H61 . 107.9 no
C4 . C6 . H62 . 108.3 no
N7 . C6 . H62 . 105.6 no
H61 . C6 . H62 . 109.8 no
C6 . N7 . C8 . 112.7(5) yes
C6 . N7 . C9 . 111.6(4) yes
C8 . N7 . C9 . 108.7(5) yes
C6 . N7 . C10 . 106.2(5) yes
C8 . N7 . C10 . 108.6(4) yes
C9 . N7 . C10 . 108.8(5) yes
N7 . C8 . H82 . 108.8 no
N7 . C8 . H81 . 108.6 no
H82 . C8 . H81 . 110.7 no
N7 . C8 . H83 . 109.1 no
H82 . C8 . H83 . 109.8 no
H81 . C8 . H83 . 109.8 no
N7 . C9 . H92 . 110.0 no
N7 . C9 . H93 . 110.6 no
H92 . C9 . H93 . 109.8 no
N7 . C9 . H91 . 109.6 no
H92 . C9 . H91 . 108.9 no
H93 . C9 . H91 . 107.9 no
N7 . C10 . H102 . 108.7 no
N7 . C10 . H101 . 109.4 no
H102 . C10 . H101 . 109.4 no
N7 . C10 . H103 . 109.9 no
H102 . C10 . H103 . 109.4 no
H101 . C10 . H103 . 110.0 no
N11 . C12 . C13 . 178.0(7) yes
C12 . C13 . C14 . 111.1(5) yes
C12 . C13 . H132 . 108.5 no
C14 . C13 . H132 . 107.9 no
C12 . C13 . H131 . 109.3 no
C14 . C13 . H131 . 110.4 no
H132 . C13 . H131 . 109.5 no
C13 . C14 . C16 . 104.7(5) yes
C13 . C14 . O151 . 106.1(5) yes
C16 . C14 . O151 . 112.3(5) yes
C13 . C14 . H141 . 112.2 no
C16 . C14 . H141 . 112.0 no
O151 . C14 . H141 . 109.4 no
C13 . C14 . C16 . 104.7(5) yes
C13 . C14 . O152 . 95.9(7) yes
C16 . C14 . O152 . 104.6(7) yes
C13 . C14 . H142 . 117.3 no
C16 . C14 . H142 . 117.0 no
O152 . C14 . H142 . 114.6 no
C14 . C16 . N17 . 115.8(4) yes
C14 . C16 . H161 . 107.5 no
N17 . C16 . H161 . 107.0 no
C14 . C16 . H162 . 109.6 no
N17 . C16 . H162 . 107.0 no
H161 . C16 . H162 . 109.8 no
C16 . N17 . C18 . 112.1(4) yes
C16 . N17 . C19 . 111.3(4) yes
C18 . N17 . C19 . 109.7(5) yes
C16 . N17 . C20 . 105.6(4) yes
C18 . N17 . C20 . 109.1(5) yes
C19 . N17 . C20 . 108.9(5) yes
N17 . C18 . H182 . 109.5 no
N17 . C18 . H183 . 109.4 no
H182 . C18 . H183 . 109.5 no
N17 . C18 . H181 . 109.5 no
H182 . C18 . H181 . 109.0 no
H183 . C18 . H181 . 109.8 no
N17 . C19 . H191 . 108.7 no
N17 . C19 . H193 . 108.4 no
H191 . C19 . H193 . 109.5 no
N17 . C19 . H192 . 109.6 no
H191 . C19 . H192 . 110.7 no
H193 . C19 . H192 . 110.0 no
N17 . C20 . H203 . 109.2 no
N17 . C20 . H202 . 108.4 no
H203 . C20 . H202 . 109.9 no
N17 . C20 . H201 . 109.0 no
H203 . C20 . H201 . 110.0 no
H202 . C20 . H201 . 110.3 no
C14 . O151 . H1511 . 104.1 no
C14 . O152 . H1521 . 111.7 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C6 . H61 . O5 8_645 133 0.97 2.51 3.254(9) yes
_iucr_refine_instructions_details
;
#
# Punched on 11/06/18 at 15:14:00
#
#LIST 12
BLOCK SCALE X'S U'S
EQUIVALENCE PART(1001, OCC)
CONTINUE PART(1002, OCC)
WEIGHT -1 PART(1002, OCC)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE O ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S)
RIDE C ( 8,X'S) H ( 82,X'S) H ( 81,X'S) H ( 83,X'S)
RIDE C ( 9,X'S) H ( 92,X'S) H ( 93,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 102,X'S) H ( 101,X'S) H ( 103,X'S)
RIDE C ( 13,X'S) H ( 132,X'S) H ( 131,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
CONT H ( 142,X'S)
RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S)
RIDE C ( 18,X'S) H ( 182,X'S) H ( 183,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S) H ( 193,X'S) H ( 192,X'S)
RIDE C ( 20,X'S) H ( 203,X'S) H ( 202,X'S) H ( 201,X'S)
RIDE O ( 151,X'S) H (1511,X'S)
RIDE O ( 152,X'S) H (1521,X'S)
END
#
# Punched on 11/06/18 at 15:14:00
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
DISTANCE 1.450000 , 0.0010000 = C(14) TO O(151)
DISTANCE 1.450000 , 0.0010000 = C(14) TO O(152)
END
;
data_Rcarnitinenitrilechloride
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 7.2902(2)
_cell_length_b 8.9099(3)
_cell_length_c 7.8789(3)
_cell_angle_alpha 90
_cell_angle_beta 107.024(3)
_cell_angle_gamma 90
_cell_volume 489.35(3)
_symmetry_cell_setting 'monoclinic'
_symmetry_space_group_name_H-M 'P 1 21 1 '
_symmetry_space_group_name_Hall 'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x,y+1/2,-z'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687
0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424
0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975
1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194
1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C7 H15 Cl1 N2 O1
# Dc = 1.21 Fooo = 192.00 Mu = 3.43 M = 178.66
# Found Formula = C7 H15.00 Cl1 N2 O1
# Dc = 1.21 FOOO = 192.00 Mu = 3.43 M = 178.66
_chemical_formula_sum 'C7 H15 Cl N2 O'
_chemical_formula_moiety 'C7 H15 N2 O, Cl'
_chemical_compound_source ?
_chemical_formula_weight 178.66
_cell_measurement_reflns_used 10124
_cell_measurement_theta_min 3
_cell_measurement_theta_max 34
_cell_measurement_temperature 160
_exptl_crystal_description 'plate'
_exptl_crystal_colour 'colorless'
_exptl_crystal_size_min 0.067
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.302
_exptl_crystal_density_diffrn 1.212
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 191.998
_exptl_absorpt_coefficient_mu 0.343
# Sheldrick geometric approximatio 0.93 0.98
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)'
_exptl_absorpt_correction_T_min 0.59
_exptl_absorpt_correction_T_max 0.98
_diffrn_measurement_device_type 'Oxford Diffraction SuperNova'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'graphite'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction 'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 160
_diffrn_reflns_number 15361
_reflns_number_total 3726
_diffrn_reflns_av_R_equivalents 0.039
# Number of reflections without Friedels Law is 3726
# Number of reflections with Friedels Law is 1969
# Theoretical number of reflections is about 1865
_diffrn_reflns_theta_min 2.704
_diffrn_reflns_theta_max 33.133
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 33.133
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 11
_reflns_limit_h_min -11
_reflns_limit_h_max 10
_reflns_limit_k_min -13
_reflns_limit_k_max 13
_reflns_limit_l_min 0
_reflns_limit_l_max 12
_oxford_diffrn_Wilson_B_factor 1.79
_oxford_diffrn_Wilson_scale 0.08
_atom_sites_solution_primary direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.29
_refine_diff_density_max 0.39
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns 3726
_refine_ls_number_restraints 1
_refine_ls_number_parameters 101
_oxford_refine_ls_R_factor_ref 0.0358
_refine_ls_wR_factor_ref 0.0814
_refine_ls_goodness_of_fit_ref 0.9528
_refine_ls_shift/su_max 0.0033784
_refine_ls_shift/su_mean 0.0003128
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 3726
_refine_ls_R_factor_all 0.0358
_refine_ls_wR_factor_all 0.0814
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 3428
_refine_ls_R_factor_gt 0.0318
_refine_ls_wR_factor_gt 0.0785
_refine_ls_abs_structure_Flack -0.01(4)
_refine_ls_abs_structure_details 'Flack (1983), 1757 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration 'ad'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment noref #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.02P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Agilent (2011). CrysAlisPro.
Oxford Diffraction, (2010). Supernova User Manual.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
N1 N 0.4227(2) 0.29988(19) 0.86539(19) 0.0439 1.0000 Uani . . . . . .
C2 C 0.42518(18) 0.4188(2) 0.81389(17) 0.0298 1.0000 Uani . . . . . .
C3 C 0.42895(18) 0.57227(19) 0.74730(15) 0.0264 1.0000 Uani . . . . . .
C4 C 0.39881(15) 0.57640(17) 0.54599(14) 0.0216 1.0000 Uani . . . . . .
O5 O 0.53528(11) 0.48579(16) 0.49785(11) 0.0269 1.0000 Uani . . . . . .
C6 C 0.19831(15) 0.51844(17) 0.45120(14) 0.0204 1.0000 Uani . . . . . .
N7 N 0.11690(14) 0.56477(17) 0.25902(13) 0.0210 1.0000 Uani . . . . . .
C8 C 0.1055(2) 0.73162(19) 0.2394(2) 0.0339 1.0000 Uani . . . . . .
C9 C -0.08373(15) 0.50281(19) 0.19391(17) 0.0278 1.0000 Uani . . . . . .
C10 C 0.23296(17) 0.50150(19) 0.14668(15) 0.0262 1.0000 Uani . . . . . .
Cl11 Cl -0.09007(3) 0.62594(13) 0.72235(3) 0.0245 1.0000 Uani . . . . . .
H41 H 0.4069 0.6826 0.5146 0.0286 1.0000 Uiso . . . . . .
H61 H 0.2012 0.4142 0.4560 0.0265 1.0000 Uiso . . . . . .
H62 H 0.1084 0.5534 0.5132 0.0239 1.0000 Uiso . . . . . .
H93 H -0.1391 0.5301 0.0690 0.0411 1.0000 Uiso . . . . . .
H91 H -0.0787 0.3985 0.2056 0.0429 1.0000 Uiso . . . . . .
H92 H -0.1576 0.5456 0.2667 0.0421 1.0000 Uiso . . . . . .
H82 H 0.0367 0.7548 0.1145 0.0544 1.0000 Uiso . . . . . .
H83 H 0.0350 0.7684 0.3209 0.0555 1.0000 Uiso . . . . . .
H81 H 0.2340 0.7716 0.2709 0.0551 1.0000 Uiso . . . . . .
H101 H 0.1672 0.5260 0.0228 0.0388 1.0000 Uiso . . . . . .
H103 H 0.2411 0.3969 0.1621 0.0421 1.0000 Uiso . . . . . .
H102 H 0.3616 0.5437 0.1864 0.0402 1.0000 Uiso . . . . . .
H32 H 0.3304 0.6272 0.7801 0.0334 1.0000 Uiso . . . . . .
H31 H 0.5602 0.6057 0.8065 0.0319 1.0000 Uiso . . . . . .
H51 H 0.6362 0.5188 0.5584 0.0422 1.0000 Uiso . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0468(7) 0.0446(7) 0.0429(7) 0.0121(6) 0.0173(6) 0.0060(6)
C2 0.0267(5) 0.0396(7) 0.0232(5) 0.0027(5) 0.0073(4) 0.0039(5)
C3 0.0271(5) 0.0281(5) 0.0231(4) -0.0046(4) 0.0060(4) -0.0001(4)
C4 0.0209(4) 0.0206(4) 0.0224(4) -0.0019(4) 0.0050(3) -0.0012(4)
O5 0.0197(3) 0.0333(4) 0.0270(4) -0.0073(3) 0.0058(3) 0.0001(3)
C6 0.0204(4) 0.0197(4) 0.0211(4) -0.0004(3) 0.0059(3) -0.0009(4)
N7 0.0200(4) 0.0179(4) 0.0234(4) 0.0019(3) 0.0037(3) 0.0009(3)
C8 0.0352(7) 0.0171(5) 0.0429(7) 0.0038(5) 0.0013(5) 0.0010(5)
C9 0.0191(5) 0.0253(6) 0.0347(6) -0.0003(4) 0.0012(4) -0.0004(4)
C10 0.0265(5) 0.0305(6) 0.0216(5) 0.0012(4) 0.0071(4) 0.0010(4)
Cl11 0.02216(10) 0.02147(11) 0.02860(11) -0.00162(10) 0.00535(8) 0.00025(10)
_refine_ls_extinction_method
'None'
_oxford_refine_ls_scale 3.71(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 . C2 . 1.1370(19) yes
C2 . C3 . 1.467(2) yes
C3 . C4 . 1.5366(16) yes
C3 . H32 . 0.965 no
C3 . H31 . 0.980 no
C4 . O5 . 1.4165(14) yes
C4 . C6 . 1.5237(15) yes
C4 . H41 . 0.984 no
O5 . H51 . 0.806 no
C6 . N7 . 1.5130(14) yes
C6 . H61 . 0.929 no
C6 . H62 . 0.976 no
N7 . C8 . 1.4944(18) yes
N7 . C9 . 1.5060(15) yes
N7 . C10 . 1.5019(17) yes
C8 . H82 . 0.987 no
C8 . H83 . 0.988 no
C8 . H81 . 0.964 no
C9 . H93 . 0.979 no
C9 . H91 . 0.934 no
C9 . H92 . 0.972 no
C10 . H101 . 0.978 no
C10 . H103 . 0.940 no
C10 . H102 . 0.973 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . C2 . C3 . 179.82(14) yes
C2 . C3 . C4 . 112.30(10) yes
C2 . C3 . H32 . 106.4 no
C4 . C3 . H32 . 111.8 no
C2 . C3 . H31 . 103.4 no
C4 . C3 . H31 . 108.0 no
H32 . C3 . H31 . 114.7 no
C3 . C4 . O5 . 111.31(9) yes
C3 . C4 . C6 . 108.94(10) yes
O5 . C4 . C6 . 108.89(9) yes
C3 . C4 . H41 . 106.3 no
O5 . C4 . H41 . 112.5 no
C6 . C4 . H41 . 108.8 no
C4 . O5 . H51 . 102.9 no
C4 . C6 . N7 . 115.92(9) yes
C4 . C6 . H61 . 108.2 no
N7 . C6 . H61 . 108.1 no
C4 . C6 . H62 . 109.6 no
N7 . C6 . H62 . 106.8 no
H61 . C6 . H62 . 108.0 no
C6 . N7 . C8 . 111.62(10) yes
C6 . N7 . C9 . 107.35(9) yes
C8 . N7 . C9 . 108.08(10) yes
C6 . N7 . C10 . 111.33(9) yes
C8 . N7 . C10 . 109.66(12) yes
C9 . N7 . C10 . 108.67(9) yes
N7 . C8 . H82 . 107.9 no
N7 . C8 . H83 . 106.6 no
H82 . C8 . H83 . 111.7 no
N7 . C8 . H81 . 108.7 no
H82 . C8 . H81 . 110.6 no
H83 . C8 . H81 . 111.2 no
N7 . C9 . H93 . 109.0 no
N7 . C9 . H91 . 109.0 no
H93 . C9 . H91 . 109.8 no
N7 . C9 . H92 . 107.8 no
H93 . C9 . H92 . 111.1 no
H91 . C9 . H92 . 110.2 no
N7 . C10 . H101 . 108.0 no
N7 . C10 . H103 . 108.8 no
H101 . C10 . H103 . 110.2 no
N7 . C10 . H102 . 108.7 no
H101 . C10 . H102 . 112.3 no
H103 . C10 . H102 . 108.9 no
_iucr_refine_instructions_details
;
#
# Punched on 15/06/18 at 11:21:22
#
#LIST 12
BLOCK SCALE X'S U'S
CONT ENANTIO
END
#
# Punched on 15/06/18 at 11:21:22
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
data_Rcarnitinenitrilebromide
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 7.5269(2)
_cell_length_b 9.1017(3)
_cell_length_c 7.9300(3)
_cell_angle_alpha 90
_cell_angle_beta 107.161(4)
_cell_angle_gamma 90
_cell_volume 519.08(3)
_symmetry_cell_setting 'monoclinic'
_symmetry_space_group_name_H-M 'P 1 21 1 '
_symmetry_space_group_name_Hall 'P 2yb '
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x,y+1/2,-z'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687
0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424
0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609
3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975
1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194
1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C7 H15 Br1 Cl1 N2 O1
# Dc = 1.65 Fooo = 262.00 Mu = 41.76 M = 258.57
# Found Formula = C7 H15 Br1 N2 O1
# Dc = 1.43 FOOO = 228.00 Mu = 39.15 M = 223.11
_chemical_formula_sum 'C7 H15 Br N2 O'
_chemical_formula_moiety 'C7 H15 N2 O, Br'
_chemical_compound_source ?
_chemical_formula_weight 223.11
_cell_measurement_reflns_used 9220
_cell_measurement_theta_min 3
_cell_measurement_theta_max 30
_cell_measurement_temperature 160
_exptl_crystal_description 'plate'
_exptl_crystal_colour 'colorless'
_exptl_crystal_size_min 0.026
_exptl_crystal_size_mid 0.103
_exptl_crystal_size_max 0.120
_exptl_crystal_density_diffrn 1.427
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 228
_exptl_absorpt_coefficient_mu 3.915
# Sheldrick geometric approximatio 0.67 0.90
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)'
_exptl_absorpt_correction_T_min 0.64
_exptl_absorpt_correction_T_max 0.90
_diffrn_measurement_device_type 'Oxford Diffraction SuperNova'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'graphite'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction 'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 160
_diffrn_reflns_number 16508
_reflns_number_total 3402
_diffrn_reflns_av_R_equivalents 0.034
# Number of reflections without Friedels Law is 3402
# Number of reflections with Friedels Law is 1821
# Theoretical number of reflections is about 1727
_diffrn_reflns_theta_min 2.688
_diffrn_reflns_theta_max 31.495
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 31.495
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_limit_l_max 11
_reflns_limit_h_min -11
_reflns_limit_h_max 10
_reflns_limit_k_min -13
_reflns_limit_k_max 13
_reflns_limit_l_min 0
_reflns_limit_l_max 11
_oxford_diffrn_Wilson_B_factor 1.94
_oxford_diffrn_Wilson_scale 0.44
_atom_sites_solution_primary direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.53
_refine_diff_density_max 0.47
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns 3402
_refine_ls_number_restraints 1
_refine_ls_number_parameters 101
_oxford_refine_ls_R_factor_ref 0.0338
_refine_ls_wR_factor_ref 0.0720
_refine_ls_goodness_of_fit_ref 0.9715
_refine_ls_shift/su_max 0.0009162
_refine_ls_shift/su_mean 0.0000235
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 3402
_refine_ls_R_factor_all 0.0338
_refine_ls_wR_factor_all 0.0720
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 3118
_refine_ls_R_factor_gt 0.0293
_refine_ls_wR_factor_gt 0.0703
_refine_ls_abs_structure_Flack 0.043(10)
_refine_ls_abs_structure_details 'Flack (1983), 1581 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration 'ad'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.27P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Agilent (2011). CrysAlisPro.
Oxford Diffraction, (2010). Supernova User Manual.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
N1 N 0.9125(4) 0.2003(3) 1.3586(4) 0.0451 1.0000 Uani . . . . . .
C2 C 0.9201(4) 0.3168(3) 1.3109(3) 0.0296 1.0000 Uani . . . . . .
C3 C 0.9332(4) 0.4668(3) 1.2495(3) 0.0262 1.0000 Uani . . . . . .
C4 C 0.9026(3) 0.4744(3) 1.0483(3) 0.0202 1.0000 Uani . . . . . .
O5 O 1.0304(2) 0.3826(2) 0.9981(2) 0.0255 1.0000 Uani . . . . . .
C6 C 0.7066(3) 0.4236(3) 0.9531(3) 0.0193 1.0000 Uani . . . . . .
N7 N 0.6291(3) 0.4722(3) 0.7627(3) 0.0192 1.0000 Uani . . . . . .
C8 C 0.6234(5) 0.6354(3) 0.7463(5) 0.0339 1.0000 Uani . . . . . .
C9 C 0.4325(3) 0.4158(3) 0.6981(3) 0.0270 1.0000 Uani . . . . . .
C10 C 0.7395(3) 0.4081(3) 0.6498(3) 0.0255 1.0000 Uani . . . . . .
Br11 Br 0.41054(3) 0.53206(11) 1.21779(3) 0.0266 1.0000 Uani . . . . . .
H103 H 0.6766 0.4333 0.5370 0.0387 1.0000 Uiso R . . . . .
H102 H 0.8563 0.4509 0.6782 0.0382 1.0000 Uiso R . . . . .
H101 H 0.7481 0.3060 0.6655 0.0373 1.0000 Uiso R . . . . .
H83 H 0.5601 0.6727 0.8257 0.0512 1.0000 Uiso R . . . . .
H82 H 0.7459 0.6682 0.7737 0.0506 1.0000 Uiso R . . . . .
H81 H 0.5524 0.6600 0.6280 0.0496 1.0000 Uiso R . . . . .
H93 H 0.3631 0.4540 0.7700 0.0388 1.0000 Uiso R . . . . .
H92 H 0.4381 0.3096 0.7057 0.0385 1.0000 Uiso R . . . . .
H91 H 0.3805 0.4450 0.5821 0.0407 1.0000 Uiso R . . . . .
H32 H 1.0522 0.5041 1.3078 0.0319 1.0000 Uiso R . . . . .
H31 H 0.8461 0.5271 1.2816 0.0331 1.0000 Uiso R . . . . .
H41 H 0.9192 0.5751 1.0231 0.0230 1.0000 Uiso R . . . . .
H62 H 0.6260 0.4620 1.0122 0.0230 1.0000 Uiso R . . . . .
H61 H 0.7016 0.3199 0.9544 0.0218 1.0000 Uiso R . . . . .
H51 H 1.1098 0.4279 1.0403 0.0381 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0471(16) 0.0515(16) 0.0373(14) 0.0120(12) 0.0136(12) 0.0049(13)
C2 0.0242(11) 0.0437(16) 0.0213(11) 0.0024(10) 0.0075(9) 0.0044(10)
C3 0.0256(12) 0.0331(12) 0.0192(10) -0.0051(9) 0.0052(9) 0.0006(9)
C4 0.0202(10) 0.0214(9) 0.0189(9) -0.0029(8) 0.0059(8) -0.0009(8)
O5 0.0176(8) 0.0341(9) 0.0244(8) -0.0071(7) 0.0054(6) 0.0010(7)
C6 0.0181(9) 0.0230(10) 0.0167(9) -0.0002(8) 0.0051(8) 0.0004(8)
N7 0.0185(9) 0.0167(10) 0.0214(9) 0.0008(8) 0.0045(7) 0.0021(8)
C8 0.0377(16) 0.0136(13) 0.0454(16) 0.0051(12) 0.0047(13) 0.0017(11)
C9 0.0176(10) 0.0302(13) 0.0297(12) -0.0001(10) 0.0015(9) -0.0007(9)
C10 0.0237(11) 0.0365(13) 0.0183(10) 0.0018(9) 0.0091(8) 0.0029(10)
Br11 0.02418(10) 0.02568(10) 0.02912(10) -0.00089(14) 0.00641(7) 0.00152(14)
_refine_ls_extinction_method
'None'
_oxford_refine_ls_scale 1.565(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 . C2 . 1.133(4) yes
C2 . C3 . 1.463(4) yes
C3 . C4 . 1.545(3) yes
C3 . H32 . 0.942 no
C3 . H31 . 0.946 no
C4 . O5 . 1.417(3) yes
C4 . C6 . 1.518(3) yes
C4 . H41 . 0.954 no
O5 . H51 . 0.722 no
C6 . N7 . 1.515(3) yes
C6 . H62 . 0.937 no
C6 . H61 . 0.944 no
N7 . C8 . 1.491(4) yes
N7 . C9 . 1.506(3) yes
N7 . C10 . 1.507(3) yes
C8 . H83 . 0.957 no
C8 . H82 . 0.932 no
C8 . H81 . 0.959 no
C9 . H93 . 0.946 no
C9 . H92 . 0.968 no
C9 . H91 . 0.926 no
C10 . H103 . 0.909 no
C10 . H102 . 0.926 no
C10 . H101 . 0.938 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . C2 . C3 . 179.0(3) yes
C2 . C3 . C4 . 112.4(2) yes
C2 . C3 . H32 . 108.7 no
C4 . C3 . H32 . 108.7 no
C2 . C3 . H31 . 109.4 no
C4 . C3 . H31 . 110.4 no
H32 . C3 . H31 . 107.0 no
C3 . C4 . O5 . 110.93(19) yes
C3 . C4 . C6 . 109.06(19) yes
O5 . C4 . C6 . 108.75(19) yes
C3 . C4 . H41 . 105.7 no
O5 . C4 . H41 . 111.5 no
C6 . C4 . H41 . 110.9 no
C4 . O5 . H51 . 94.0 no
C4 . C6 . N7 . 115.99(19) yes
C4 . C6 . H62 . 108.4 no
N7 . C6 . H62 . 105.9 no
C4 . C6 . H61 . 109.6 no
N7 . C6 . H61 . 107.3 no
H62 . C6 . H61 . 109.5 no
C6 . N7 . C8 . 111.7(2) yes
C6 . N7 . C9 . 106.8(2) yes
C8 . N7 . C9 . 108.0(3) yes
C6 . N7 . C10 . 111.21(19) yes
C8 . N7 . C10 . 109.9(3) yes
C9 . N7 . C10 . 108.9(2) yes
N7 . C8 . H83 . 107.7 no
N7 . C8 . H82 . 107.3 no
H83 . C8 . H82 . 112.6 no
N7 . C8 . H81 . 108.1 no
H83 . C8 . H81 . 108.6 no
H82 . C8 . H81 . 112.3 no
N7 . C9 . H93 . 109.4 no
N7 . C9 . H92 . 107.4 no
H93 . C9 . H92 . 110.6 no
N7 . C9 . H91 . 109.0 no
H93 . C9 . H91 . 110.2 no
H92 . C9 . H91 . 110.3 no
N7 . C10 . H103 . 105.6 no
N7 . C10 . H102 . 110.0 no
H103 . C10 . H102 . 108.4 no
N7 . C10 . H101 . 109.4 no
H103 . C10 . H101 . 112.1 no
H102 . C10 . H101 . 111.2 no
_iucr_refine_instructions_details
;
#
# Punched on 15/06/18 at 11:23:44
#
#LIST 12
BLOCK SCALE X'S U'S
CONT ENANTIO
RIDE C ( 3,X'S) H ( 32,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE O ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 62,X'S) H ( 61,X'S)
RIDE C ( 8,X'S) H ( 83,X'S) H ( 82,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 93,X'S) H ( 92,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 103,X'S) H ( 102,X'S) H ( 101,X'S)
END
#
# Punched on 15/06/18 at 11:23:44
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
data_Rcarnitinenitrileiodide
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 7.58500(10)
_cell_length_b 10.8242(2)
_cell_length_c 13.0468(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1071.16(3)
_symmetry_cell_setting 'orthorhombic'
_symmetry_space_group_name_H-M 'P 21 21 21 '
_symmetry_space_group_name_Hall 'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x+1/2,-y,z+1/2'
'x+1/2,-y+1/2,-z'
'-x,y+1/2,-z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687
0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424
0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660
2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975
1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C8.75 H18.75 I1.25 N2.50 O1.25
# Dc = 2.09 Fooo = 660.00 Mu = 36.84 M = 337.64
# Found Formula = C7 H15 I1 N2 O1
# Dc = 1.67 FOOO = 528.00 Mu = 29.47 M = 270.11
_chemical_formula_sum 'C7 H15 I N2 O'
_chemical_formula_moiety 'CC7 H15 N2 O, I'
_chemical_compound_source ?
_chemical_formula_weight 270.11
_cell_measurement_reflns_used 14266
_cell_measurement_theta_min 2
_cell_measurement_theta_max 33
_cell_measurement_temperature 160
_exptl_crystal_description 'prism'
_exptl_crystal_colour 'colorless'
_exptl_crystal_size_min 0.099
_exptl_crystal_size_mid 0.118
_exptl_crystal_size_max 0.253
_exptl_crystal_density_diffrn 1.675
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 528
_exptl_absorpt_coefficient_mu 2.947
# Sheldrick geometric approximatio 0.71 0.75
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)'
_exptl_absorpt_correction_T_min 0.47
_exptl_absorpt_correction_T_max 0.75
_diffrn_measurement_device_type 'Oxford Diffraction SuperNova'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'graphite'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction 'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 160
_diffrn_reflns_number 17375
_reflns_number_total 3606
_diffrn_reflns_av_R_equivalents 0.021
# Number of reflections without Friedels Law is 3606
# Number of reflections with Friedels Law is 2125
# Theoretical number of reflections is about 1997
_diffrn_reflns_theta_min 2.445
_diffrn_reflns_theta_max 32.865
_diffrn_measured_fraction_theta_max 0.932
_diffrn_reflns_theta_full 27.935
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_reflns_limit_h_min -11
_reflns_limit_h_max 11
_reflns_limit_k_min 0
_reflns_limit_k_max 16
_reflns_limit_l_min 0
_reflns_limit_l_max 19
_oxford_diffrn_Wilson_B_factor 2.01
_oxford_diffrn_Wilson_scale 0.27
_atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.41
_refine_diff_density_max 0.39
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns 3606
_refine_ls_number_restraints 0
_refine_ls_number_parameters 101
_oxford_refine_ls_R_factor_ref 0.0138
_refine_ls_wR_factor_ref 0.0296
_refine_ls_goodness_of_fit_ref 0.9879
_refine_ls_shift/su_max 0.0015685
_refine_ls_shift/su_mean 0.0000754
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 3606
_refine_ls_R_factor_all 0.0138
_refine_ls_wR_factor_all 0.0296
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 3544
_refine_ls_R_factor_gt 0.0133
_refine_ls_wR_factor_gt 0.0294
_refine_ls_abs_structure_Flack -0.018(12)
_refine_ls_abs_structure_details 'Flack (1983), 1481 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration 'ad'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 0.25P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Agilent (2011). CrysAlisPro.
Oxford Diffraction, (2010). Supernova User Manual.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
N1 N -0.09118(19) 0.85547(11) 0.76082(10) 0.0321 1.0000 Uani . . . . . .
C2 C -0.03026(17) 0.76975(13) 0.72543(11) 0.0231 1.0000 Uani . . . . . .
C3 C 0.04857(17) 0.65622(13) 0.68432(12) 0.0256 1.0000 Uani . . . . . .
C4 C 0.24273(15) 0.64097(11) 0.71711(9) 0.0177 1.0000 Uani . . . . . .
O5 O 0.34704(13) 0.73213(9) 0.66875(8) 0.0245 1.0000 Uani . . . . . .
C6 C 0.25703(16) 0.65378(11) 0.83324(10) 0.0182 1.0000 Uani . . . . . .
N7 N 0.42553(14) 0.60624(9) 0.88085(8) 0.0172 1.0000 Uani . . . . . .
C8 C 0.58628(19) 0.67126(13) 0.84080(10) 0.0250 1.0000 Uani . . . . . .
C9 C 0.4143(2) 0.63029(12) 0.99430(9) 0.0243 1.0000 Uani . . . . . .
C10 C 0.44722(19) 0.46984(12) 0.86448(12) 0.0296 1.0000 Uani . . . . . .
I11 I 0.591822(11) 0.514611(8) 0.538035(7) 0.0274 1.0000 Uani . . . . . .
H41 H 0.2808 0.5608 0.6970 0.0205 1.0000 Uiso R . . . . .
H61 H 0.2542 0.7404 0.8497 0.0208 1.0000 Uiso R . . . . .
H62 H 0.1619 0.6123 0.8660 0.0208 1.0000 Uiso R . . . . .
H91 H 0.5174 0.5966 1.0255 0.0358 1.0000 Uiso R . . . . .
H92 H 0.4064 0.7183 1.0036 0.0359 1.0000 Uiso R . . . . .
H93 H 0.3086 0.5918 1.0192 0.0363 1.0000 Uiso R . . . . .
H101 H 0.5534 0.4450 0.9010 0.0438 1.0000 Uiso R . . . . .
H103 H 0.4634 0.4529 0.7911 0.0438 1.0000 Uiso R . . . . .
H102 H 0.3458 0.4280 0.8921 0.0449 1.0000 Uiso R . . . . .
H83 H 0.6895 0.6415 0.8779 0.0385 1.0000 Uiso R . . . . .
H82 H 0.5973 0.6486 0.7698 0.0380 1.0000 Uiso R . . . . .
H81 H 0.5707 0.7585 0.8497 0.0399 1.0000 Uiso R . . . . .
H32 H 0.0436 0.6590 0.6116 0.0329 1.0000 Uiso R . . . . .
H31 H -0.0220 0.5883 0.7047 0.0328 1.0000 Uiso R . . . . .
H51 H 0.4046 0.6968 0.6261 0.0374 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0290(6) 0.0308(6) 0.0366(6) -0.0007(5) -0.0039(6) 0.0099(6)
C2 0.0185(6) 0.0252(6) 0.0257(6) 0.0017(5) -0.0038(5) 0.0028(5)
C3 0.0205(6) 0.0238(6) 0.0326(7) -0.0072(5) -0.0084(5) 0.0041(4)
C4 0.0168(5) 0.0139(5) 0.0223(5) -0.0011(4) -0.0013(5) 0.0009(4)
O5 0.0290(5) 0.0190(4) 0.0255(5) 0.0039(3) 0.0042(4) -0.0002(4)
C6 0.0137(5) 0.0184(5) 0.0224(6) -0.0006(4) 0.0012(4) 0.0028(4)
N7 0.0157(4) 0.0160(4) 0.0198(4) -0.0016(3) -0.0012(4) 0.0019(4)
C8 0.0153(5) 0.0344(6) 0.0253(6) 0.0018(5) -0.0007(5) -0.0036(6)
C9 0.0251(6) 0.0295(6) 0.0184(5) 0.0000(4) -0.0008(5) 0.0017(6)
C10 0.0339(7) 0.0153(5) 0.0396(7) -0.0037(5) -0.0150(6) 0.0063(5)
I11 0.02249(4) 0.02995(4) 0.02973(4) -0.00501(3) 0.00702(3) 0.00090(3)
_refine_ls_extinction_coef 31.271
_refine_ls_extinction_method
'Larson (1970), Equation 22'
_oxford_refine_ls_scale 2.243(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 . C2 . 1.1348(18) yes
C2 . C3 . 1.4681(18) yes
C3 . C4 . 1.5424(17) yes
C3 . H32 . 0.950 no
C3 . H31 . 0.948 no
C4 . O5 . 1.4134(15) yes
C4 . C6 . 1.5253(18) yes
C4 . H41 . 0.951 no
O5 . H51 . 0.804 no
C6 . N7 . 1.5114(15) yes
C6 . H61 . 0.962 no
C6 . H62 . 0.952 no
N7 . C8 . 1.5017(17) yes
N7 . C9 . 1.5053(16) yes
N7 . C10 . 1.5008(16) yes
C8 . H83 . 0.975 no
C8 . H82 . 0.961 no
C8 . H81 . 0.959 no
C9 . H91 . 0.954 no
C9 . H92 . 0.963 no
C9 . H93 . 0.960 no
C10 . H101 . 0.974 no
C10 . H103 . 0.982 no
C10 . H102 . 0.962 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . C2 . C3 . 177.37(15) yes
C2 . C3 . C4 . 112.16(11) yes
C2 . C3 . H32 . 108.8 no
C4 . C3 . H32 . 108.6 no
C2 . C3 . H31 . 108.5 no
C4 . C3 . H31 . 112.2 no
H32 . C3 . H31 . 106.4 no
C3 . C4 . O5 . 109.63(10) yes
C3 . C4 . C6 . 109.49(10) yes
O5 . C4 . C6 . 109.89(10) yes
C3 . C4 . H41 . 108.1 no
O5 . C4 . H41 . 110.1 no
C6 . C4 . H41 . 109.6 no
C4 . O5 . H51 . 106.3 no
C4 . C6 . N7 . 115.94(10) yes
C4 . C6 . H61 . 107.9 no
N7 . C6 . H61 . 105.0 no
C4 . C6 . H62 . 110.5 no
N7 . C6 . H62 . 107.2 no
H61 . C6 . H62 . 110.0 no
C6 . N7 . C8 . 112.58(9) yes
C6 . N7 . C9 . 107.30(10) yes
C8 . N7 . C9 . 107.89(10) yes
C6 . N7 . C10 . 111.66(9) yes
C8 . N7 . C10 . 108.82(10) yes
C9 . N7 . C10 . 108.44(10) yes
N7 . C8 . H83 . 108.9 no
N7 . C8 . H82 . 106.6 no
H83 . C8 . H82 . 108.9 no
N7 . C8 . H81 . 108.6 no
H83 . C8 . H81 . 111.4 no
H82 . C8 . H81 . 112.2 no
N7 . C9 . H91 . 107.9 no
N7 . C9 . H92 . 107.4 no
H91 . C9 . H92 . 112.0 no
N7 . C9 . H93 . 107.8 no
H91 . C9 . H93 . 112.0 no
H92 . C9 . H93 . 109.6 no
N7 . C10 . H101 . 107.0 no
N7 . C10 . H103 . 109.6 no
H101 . C10 . H103 . 108.8 no
N7 . C10 . H102 . 108.8 no
H101 . C10 . H102 . 110.4 no
H103 . C10 . H102 . 112.2 no
_iucr_refine_instructions_details
;
#
# Punched on 15/06/18 at 11:24:41
#
#LIST 12
BLOCK SCALE X'S U'S
CONT ENANTIO
RIDE C ( 3,X'S) H ( 32,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE O ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S)
RIDE C ( 8,X'S) H ( 83,X'S) H ( 82,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) H ( 93,X'S)
RIDE C ( 10,X'S) H ( 101,X'S) H ( 103,X'S) H ( 102,X'S)
END
#
# Punched on 15/06/18 at 11:24:41
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
data_Rcarnitinenitrile2tetrafluoroborate1chloride1
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 9.40060(10)
_cell_length_b 13.2619(2)
_cell_length_c 16.6581(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2076.76(5)
_symmetry_cell_setting 'orthorhombic'
_symmetry_space_group_name_H-M 'P 21 21 21 '
_symmetry_space_group_name_Hall 'P 2ac 2ab '
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x+1/2,-y,z+1/2'
'x+1/2,-y+1/2,-z'
'-x,y+1/2,-z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687
0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424
0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194
1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975
1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498
0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615
1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C14 H30 B1 Cl1 F4 N4 O2
# Dc = 1.31 Fooo = 864.00 Mu = 20.90 M = 408.67
# Found Formula = C14 H30 B1 Cl1 F4 N4 O2
# Dc = 1.31 FOOO = 864.00 Mu = 20.90 M = 408.67
_chemical_formula_sum 'C14 H30 B Cl F4 N4 O2'
_chemical_formula_moiety '2(C7 H15 N2 O), B F4, Cl'
_chemical_compound_source ?
_chemical_formula_weight 408.67
_cell_measurement_reflns_used 13634
_cell_measurement_theta_min 4
_cell_measurement_theta_max 79
_cell_measurement_temperature 160
_exptl_crystal_description 'block'
_exptl_crystal_colour 'colorless'
_exptl_crystal_size_min 0.049
_exptl_crystal_size_mid 0.073
_exptl_crystal_size_max 0.128
_exptl_crystal_density_diffrn 1.307
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 864.000
_exptl_absorpt_coefficient_mu 2.090
# Sheldrick geometric approximatio 0.86 0.90
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)'
_exptl_absorpt_correction_T_min 0.75
_exptl_absorpt_correction_T_max 0.90
_diffrn_measurement_device_type 'Oxford Diffraction SuperNova'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'graphite'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction 'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 160
_diffrn_reflns_number 22105
_reflns_number_total 4175
_diffrn_reflns_av_R_equivalents 0.037
# Number of reflections without Friedels Law is 4175
# Number of reflections with Friedels Law is 2378
# Theoretical number of reflections is about 2123
_diffrn_reflns_theta_min 4.261
_diffrn_reflns_theta_max 74.484
_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full 74.484
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_limit_l_max 20
_reflns_limit_h_min -10
_reflns_limit_h_max 11
_reflns_limit_k_min 0
_reflns_limit_k_max 16
_reflns_limit_l_min 0
_reflns_limit_l_max 20
_oxford_diffrn_Wilson_B_factor 2.91
_oxford_diffrn_Wilson_scale 0.10
_atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.19
_refine_diff_density_max 0.34
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns 4175
_refine_ls_number_restraints 19
_refine_ls_number_parameters 264
_oxford_refine_ls_R_factor_ref 0.0349
_refine_ls_wR_factor_ref 0.0903
_refine_ls_goodness_of_fit_ref 0.9960
_refine_ls_shift/su_max 0.0003280
_refine_ls_shift/su_mean 0.0000404
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 4175
_refine_ls_R_factor_all 0.0349
_refine_ls_wR_factor_all 0.0903
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 3958
_refine_ls_R_factor_gt 0.0329
_refine_ls_wR_factor_gt 0.0888
_refine_ls_abs_structure_Flack 0.015(13)
_refine_ls_abs_structure_details 'Flack (1983), 1797 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration 'ad'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.47P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Agilent (2011). CrysAlisPro.
Oxford Diffraction, (2010). Supernova User Manual.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F -0.06770(15) 0.67840(12) 0.47040(8) 0.0544 1.0000 Uani . . . . . .
F2 F 0.0796(3) 0.75743(13) 0.38243(17) 0.0813 0.853(3) Uani . U P 1 2 .
F3 F -0.0505(2) 0.62500(17) 0.34243(10) 0.0647 0.853(3) Uani . U P 1 2 .
F4 F 0.1322(2) 0.60123(17) 0.42603(15) 0.0609 0.853(3) Uani . U P 1 2 .
N1 N 0.2576(2) 0.47251(18) 0.66214(12) 0.0550 1.0000 Uani . . . . . .
C2 C 0.1678(2) 0.45723(15) 0.61760(11) 0.0369 1.0000 Uani . . . . . .
C3 C 0.0521(2) 0.43916(14) 0.56122(10) 0.0328 1.0000 Uani . . . . . .
C4 C 0.10122(19) 0.37465(13) 0.48955(10) 0.0262 1.0000 Uani . . . . . .
O5 O 0.15963(15) 0.28203(10) 0.51708(8) 0.0350 1.0000 Uani . . . . . .
C6 C -0.02928(18) 0.36130(13) 0.43668(9) 0.0259 1.0000 Uani . . . . . .
N7 N -0.00343(14) 0.32273(11) 0.35235(8) 0.0242 1.0000 Uani . . . . . .
C8 C 0.0882(2) 0.39228(15) 0.30472(11) 0.0340 1.0000 Uani . . . . . .
C9 C 0.0626(3) 0.21973(14) 0.35305(12) 0.0422 1.0000 Uani . . . . . .
C10 C -0.1463(2) 0.31701(19) 0.31252(12) 0.0416 1.0000 Uani . . . . . .
N11 N 0.7337(2) 0.50357(16) 0.64934(12) 0.0511 1.0000 Uani . . . . . .
C12 C 0.6470(2) 0.51886(15) 0.60329(11) 0.0376 1.0000 Uani . . . . . .
C13 C 0.5363(2) 0.54103(14) 0.54405(11) 0.0332 1.0000 Uani . . . . . .
C14 C 0.60284(19) 0.57765(12) 0.46486(10) 0.0252 1.0000 Uani . . . . . .
O15 O 0.67869(14) 0.49861(10) 0.42738(8) 0.0333 1.0000 Uani . . . . . .
C16 C 0.48206(18) 0.61990(13) 0.41427(10) 0.0243 1.0000 Uani . . . . . .
N17 N 0.52589(15) 0.67854(11) 0.34012(8) 0.0249 1.0000 Uani . . . . . .
C18 C 0.6206(2) 0.76546(15) 0.36065(12) 0.0362 1.0000 Uani . . . . . .
C19 C 0.3921(2) 0.71857(19) 0.30362(13) 0.0432 1.0000 Uani . . . . . .
C20 C 0.5990(2) 0.61400(16) 0.27927(11) 0.0365 1.0000 Uani . . . . . .
Cl21 Cl 0.45198(5) 0.33936(3) 0.37601(3) 0.0355 1.0000 Uani . . . . . .
B22 B 0.0246(2) 0.66776(16) 0.40679(12) 0.0324 1.0000 Uani D . . . . .
H41 H 0.1742 0.4090 0.4611 0.0315 1.0000 Uiso R . . . . .
H61 H -0.0728 0.4292 0.4330 0.0312 1.0000 Uiso R . . . . .
H62 H -0.0952 0.3168 0.4658 0.0317 1.0000 Uiso R . . . . .
H82 H 0.0911 0.3673 0.2491 0.0503 1.0000 Uiso R . . . . .
H81 H 0.0435 0.4587 0.3062 0.0504 1.0000 Uiso R . . . . .
H83 H 0.1846 0.3946 0.3270 0.0496 1.0000 Uiso R . . . . .
H101 H -0.1346 0.2929 0.2564 0.0628 1.0000 Uiso R . . . . .
H103 H -0.1911 0.3834 0.3103 0.0625 1.0000 Uiso R . . . . .
H102 H -0.2073 0.2725 0.3423 0.0629 1.0000 Uiso R . . . . .
H93 H 0.0708 0.1954 0.2973 0.0631 1.0000 Uiso R . . . . .
H91 H 0.0038 0.1768 0.3810 0.0634 1.0000 Uiso R . . . . .
H92 H 0.1570 0.2201 0.3786 0.0637 1.0000 Uiso R . . . . .
H32 H -0.0251 0.4059 0.5898 0.0406 1.0000 Uiso R . . . . .
H31 H 0.0210 0.5000 0.5394 0.0405 1.0000 Uiso R . . . . .
H141 H 0.6714 0.6321 0.4776 0.0323 1.0000 Uiso R . . . . .
H161 H 0.4194 0.5614 0.3965 0.0304 1.0000 Uiso R . . . . .
H162 H 0.4253 0.6655 0.4495 0.0293 1.0000 Uiso R . . . . .
H181 H 0.6337 0.8063 0.3143 0.0520 1.0000 Uiso R . . . . .
H182 H 0.7147 0.7407 0.3749 0.0532 1.0000 Uiso R . . . . .
H183 H 0.5851 0.8020 0.4046 0.0529 1.0000 Uiso R . . . . .
H202 H 0.6117 0.6511 0.2291 0.0541 1.0000 Uiso R . . . . .
H201 H 0.5423 0.5543 0.2682 0.0546 1.0000 Uiso R . . . . .
H203 H 0.6905 0.5897 0.2983 0.0545 1.0000 Uiso R . . . . .
H193 H 0.4184 0.7545 0.2548 0.0657 1.0000 Uiso R . . . . .
H192 H 0.3260 0.6641 0.2927 0.0656 1.0000 Uiso R . . . . .
H191 H 0.3471 0.7638 0.3413 0.0655 1.0000 Uiso R . . . . .
H131 H 0.4761 0.4822 0.5324 0.0404 1.0000 Uiso R . . . . .
H132 H 0.4796 0.5955 0.5694 0.0402 1.0000 Uiso R . . . . .
H151 H 0.6130 0.4604 0.4099 0.0541 1.0000 Uiso R . . . . .
H51 H 0.0943 0.2563 0.5466 0.0556 1.0000 Uiso R . . . . .
F5 F 0.1456(10) 0.7275(8) 0.4392(7) 0.0542 0.147(3) Uani . U P 1 1 .
F6 F 0.069(2) 0.5855(10) 0.3898(10) 0.0841 0.147(3) Uani D U P 1 1 .
F7 F -0.0210(18) 0.7259(12) 0.3509(8) 0.0848 0.147(3) Uani . U P 1 1 .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
F1 0.0428(7) 0.0784(9) 0.0419(6) -0.0156(6) 0.0102(5) -0.0138(7)
F2 0.1003(19) 0.0321(8) 0.111(2) 0.0077(10) 0.0503(18) -0.0077(10)
F3 0.0564(10) 0.0951(15) 0.0425(8) -0.0237(8) -0.0081(7) 0.0105(10)
F4 0.0402(10) 0.0664(12) 0.0761(13) 0.0189(10) -0.0053(8) 0.0114(8)
N1 0.0565(12) 0.0704(14) 0.0379(10) -0.0102(10) -0.0041(9) -0.0164(10)
C2 0.0461(11) 0.0384(10) 0.0261(8) -0.0029(8) 0.0042(8) -0.0072(8)
C3 0.0364(10) 0.0365(9) 0.0255(8) -0.0020(7) -0.0005(8) 0.0003(8)
C4 0.0255(8) 0.0293(8) 0.0237(7) 0.0008(6) 0.0010(6) 0.0011(7)
O5 0.0318(7) 0.0373(7) 0.0358(7) 0.0049(6) -0.0024(5) 0.0078(5)
C6 0.0237(9) 0.0296(8) 0.0243(7) -0.0013(6) 0.0017(6) 0.0009(6)
N7 0.0222(7) 0.0256(7) 0.0248(6) -0.0009(5) -0.0017(5) -0.0014(5)
C8 0.0356(10) 0.0393(10) 0.0272(8) 0.0024(7) 0.0040(7) -0.0070(8)
C9 0.0604(14) 0.0263(8) 0.0398(10) -0.0046(8) -0.0028(9) 0.0072(9)
C10 0.0250(9) 0.0663(14) 0.0336(9) -0.0050(9) -0.0064(7) -0.0063(9)
N11 0.0621(13) 0.0528(11) 0.0386(9) 0.0094(9) -0.0110(9) 0.0115(10)
C12 0.0503(12) 0.0331(9) 0.0293(9) 0.0065(7) -0.0004(8) 0.0029(8)
C13 0.0365(11) 0.0344(8) 0.0286(8) 0.0055(7) -0.0004(8) 0.0004(8)
C14 0.0249(8) 0.0236(7) 0.0269(8) 0.0019(6) -0.0014(7) 0.0006(6)
O15 0.0264(7) 0.0323(7) 0.0413(7) -0.0015(5) 0.0003(5) 0.0070(5)
C16 0.0204(8) 0.0271(7) 0.0254(7) 0.0030(6) 0.0021(6) 0.0007(6)
N17 0.0228(7) 0.0290(7) 0.0228(6) 0.0014(5) 0.0004(5) 0.0041(6)
C18 0.0432(11) 0.0322(9) 0.0331(9) 0.0037(7) 0.0023(8) -0.0076(8)
C19 0.0288(10) 0.0609(13) 0.0400(10) 0.0190(10) -0.0017(8) 0.0135(9)
C20 0.0418(11) 0.0429(10) 0.0247(8) -0.0048(8) 0.0028(7) 0.0078(9)
Cl21 0.0320(2) 0.0345(2) 0.0401(2) -0.00389(18) -0.00299(17) 0.00079(17)
B22 0.0340(11) 0.031(1) 0.0319(9) 0.0036(8) 0.0033(8) -0.0033(9)
F5 0.032(5) 0.060(5) 0.070(6) -0.006(5) 0.008(4) -0.013(4)
F6 0.111(8) 0.057(6) 0.084(7) -0.014(6) 0.013(7) 0.009(6)
F7 0.104(8) 0.086(7) 0.065(6) 0.048(5) 0.008(6) 0.013(6)
_refine_ls_extinction_method
'None'
_oxford_refine_ls_scale 3.22(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
F1 . B22 . 1.377(2) yes
F2 . B22 . 1.359(3) yes
F3 . B22 . 1.403(3) yes
F4 . B22 . 1.380(3) yes
N1 . C2 . 1.142(3) yes
C2 . C3 . 1.457(3) yes
C3 . C4 . 1.540(2) yes
C3 . H32 . 0.974 no
C3 . H31 . 0.931 no
C4 . O5 . 1.421(2) yes
C4 . C6 . 1.520(2) yes
C4 . H41 . 0.949 no
O5 . H51 . 0.857 no
C6 . N7 . 1.515(2) yes
C6 . H61 . 0.991 no
C6 . H62 . 0.984 no
N7 . C8 . 1.491(2) yes
N7 . C9 . 1.501(2) yes
N7 . C10 . 1.500(2) yes
C8 . H82 . 0.984 no
C8 . H81 . 0.976 no
C8 . H83 . 0.980 no
C9 . H93 . 0.986 no
C9 . H91 . 0.920 no
C9 . H92 . 0.984 no
C10 . H101 . 0.995 no
C10 . H103 . 0.977 no
C10 . H102 . 0.961 no
N11 . C12 . 1.137(3) yes
C12 . C13 . 1.464(3) yes
C13 . C14 . 1.539(2) yes
C13 . H131 . 0.983 no
C13 . H132 . 0.992 no
C14 . O15 . 1.413(2) yes
C14 . C16 . 1.521(2) yes
C14 . H141 . 0.991 no
O15 . H151 . 0.851 no
C16 . N17 . 1.517(2) yes
C16 . H161 . 1.018 no
C16 . H162 . 0.997 no
N17 . C18 . 1.496(2) yes
N17 . C19 . 1.494(2) yes
N17 . C20 . 1.494(2) yes
C18 . H181 . 0.951 no
C18 . H182 . 0.973 no
C18 . H183 . 0.939 no
C19 . H193 . 0.974 no
C19 . H192 . 0.970 no
C19 . H191 . 0.966 no
C20 . H202 . 0.977 no
C20 . H201 . 0.972 no
C20 . H203 . 0.972 no
B22 . F5 . 1.488(10) yes
B22 . F6 . 1.201(13) yes
B22 . F7 . 1.282(11) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . C2 . C3 . 179.1(2) yes
C2 . C3 . C4 . 111.56(17) yes
C2 . C3 . H32 . 108.4 no
C4 . C3 . H32 . 110.5 no
C2 . C3 . H31 . 110.1 no
C4 . C3 . H31 . 105.9 no
H32 . C3 . H31 . 110.4 no
C3 . C4 . O5 . 110.22(14) yes
C3 . C4 . C6 . 105.78(14) yes
O5 . C4 . C6 . 113.45(14) yes
C3 . C4 . H41 . 109.7 no
O5 . C4 . H41 . 107.2 no
C6 . C4 . H41 . 110.5 no
C4 . O5 . H51 . 104.6 no
C4 . C6 . N7 . 116.55(14) yes
C4 . C6 . H61 . 105.2 no
N7 . C6 . H61 . 108.4 no
C4 . C6 . H62 . 107.0 no
N7 . C6 . H62 . 110.8 no
H61 . C6 . H62 . 108.5 no
C6 . N7 . C8 . 112.17(13) yes
C6 . N7 . C9 . 111.51(13) yes
C8 . N7 . C9 . 109.16(15) yes
C6 . N7 . C10 . 106.48(13) yes
C8 . N7 . C10 . 108.26(14) yes
C9 . N7 . C10 . 109.15(16) yes
N7 . C8 . H82 . 108.0 no
N7 . C8 . H81 . 107.2 no
H82 . C8 . H81 . 109.8 no
N7 . C8 . H83 . 110.7 no
H82 . C8 . H83 . 110.0 no
H81 . C8 . H83 . 111.1 no
N7 . C9 . H93 . 108.9 no
N7 . C9 . H91 . 108.6 no
H93 . C9 . H91 . 108.7 no
N7 . C9 . H92 . 111.9 no
H93 . C9 . H92 . 109.8 no
H91 . C9 . H92 . 108.9 no
N7 . C10 . H101 . 109.4 no
N7 . C10 . H103 . 110.9 no
H101 . C10 . H103 . 107.5 no
N7 . C10 . H102 . 109.7 no
H101 . C10 . H102 . 110.8 no
H103 . C10 . H102 . 108.5 no
N11 . C12 . C13 . 178.7(2) yes
C12 . C13 . C14 . 110.59(16) yes
C12 . C13 . H131 . 112.5 no
C14 . C13 . H131 . 108.4 no
C12 . C13 . H132 . 104.0 no
C14 . C13 . H132 . 110.7 no
H131 . C13 . H132 . 110.7 no
C13 . C14 . O15 . 110.48(14) yes
C13 . C14 . C16 . 106.72(14) yes
O15 . C14 . C16 . 113.89(14) yes
C13 . C14 . H141 . 108.1 no
O15 . C14 . H141 . 107.9 no
C16 . C14 . H141 . 109.6 no
C14 . O15 . H151 . 103.1 no
C14 . C16 . N17 . 115.94(14) yes
C14 . C16 . H161 . 108.2 no
N17 . C16 . H161 . 108.2 no
C14 . C16 . H162 . 107.2 no
N17 . C16 . H162 . 108.3 no
H161 . C16 . H162 . 108.8 no
C16 . N17 . C18 . 111.75(13) yes
C16 . N17 . C19 . 106.56(13) yes
C18 . N17 . C19 . 108.66(16) yes
C16 . N17 . C20 . 112.57(14) yes
C18 . N17 . C20 . 108.82(14) yes
C19 . N17 . C20 . 108.34(15) yes
N17 . C18 . H181 . 109.3 no
N17 . C18 . H182 . 109.7 no
H181 . C18 . H182 . 105.8 no
N17 . C18 . H183 . 111.4 no
H181 . C18 . H183 . 112.6 no
H182 . C18 . H183 . 107.9 no
N17 . C19 . H193 . 107.4 no
N17 . C19 . H192 . 110.6 no
H193 . C19 . H192 . 111.7 no
N17 . C19 . H191 . 109.0 no
H193 . C19 . H191 . 110.4 no
H192 . C19 . H191 . 107.7 no
N17 . C20 . H202 . 110.4 no
N17 . C20 . H201 . 110.1 no
H202 . C20 . H201 . 108.3 no
N17 . C20 . H203 . 112.1 no
H202 . C20 . H203 . 109.7 no
H201 . C20 . H203 . 106.1 no
F1 . B22 . F5 . 98.5(4) yes
F1 . B22 . F6 . 119.5(7) yes
F5 . B22 . F6 . 107.8(11) yes
F1 . B22 . F7 . 106.6(7) yes
F5 . B22 . F7 . 101.5(10) yes
F6 . B22 . F7 . 119.4(11) yes
F3 . B22 . F4 . 106.7(2) yes
F3 . B22 . F1 . 108.21(17) yes
F4 . B22 . F1 . 110.41(18) yes
F3 . B22 . F2 . 108.5(2) yes
F4 . B22 . F2 . 110.5(2) yes
F1 . B22 . F2 . 112.34(19) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C6 . H61 . O15 1_455 136 0.99 2.51 3.298(3) yes
_iucr_refine_instructions_details
;
#
# Punched on 15/06/18 at 12:34:18
#
#LIST 12
BLOCK SCALE X'S U'S
CONT ENANTIO
EQUIVALENCE PART(1001, OCC)
CONTINUE PART(1002, OCC)
WEIGHT -1 PART(1002, OCC)
RIDE C ( 3,X'S) H ( 32,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE O ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S)
RIDE C ( 8,X'S) H ( 82,X'S) H ( 81,X'S) H ( 83,X'S)
RIDE C ( 9,X'S) H ( 93,X'S) H ( 91,X'S) H ( 92,X'S)
RIDE C ( 10,X'S) H ( 101,X'S) H ( 103,X'S) H ( 102,X'S)
RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE O ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S)
RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S)
RIDE C ( 19,X'S) H ( 193,X'S) H ( 192,X'S) H ( 191,X'S)
RIDE C ( 20,X'S) H ( 202,X'S) H ( 201,X'S) H ( 203,X'S)
END
#
# Punched on 15/06/18 at 12:34:18
#
#LIST 16
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
U(IJ)'S 0.0, 0.010000 = F(2) TO F(7)
U(IJ)'S 0.0, 0.010000 = F(5) TO F(4)
U(IJ)'S 0.0, 0.010000 = F(6) TO F(3)
DISTANCE 1.380000 , 0.050000 = B(22) TO F(6)
END
;
data_Diltiazembromide
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 6.1060(3)
_cell_length_b 9.0317(6)
_cell_length_c 42.330(4)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2334.4(3)
_symmetry_cell_setting 'orthorhombic'
_symmetry_space_group_name_H-M 'P 21 21 21 '
_symmetry_space_group_name_Hall 'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x+1/2,-y,z+1/2'
'x+1/2,-y+1/2,-z'
'-x,y+1/2,-z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687
0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424
0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975
1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536
1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Br -0.6763 1.2805 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609
3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194
1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C22 H27 Br1 Cl1 N2 O4 S1
# Dc = 1.51 Fooo = 1092.00 Mu = 45.52 M = 530.89
# Found Formula = C22 H27 Br1 N2 O4 S1
# Dc = 1.41 FOOO = 1024.00 Mu = 34.83 M = 495.44
_chemical_formula_sum 'C22 H27 Br1 N2 O4 S1'
_chemical_formula_moiety 'C22 H27 N2 O4 S, Br'
_chemical_compound_source ?
_chemical_formula_weight 495.44
_cell_measurement_reflns_used 5919
_cell_measurement_theta_min 5
_cell_measurement_theta_max 78
_cell_measurement_temperature 160
_exptl_crystal_description 'plate'
_exptl_crystal_colour 'colorless'
_exptl_crystal_size_min 0.014
_exptl_crystal_size_mid 0.042
_exptl_crystal_size_max 0.066
_exptl_crystal_density_diffrn 1.410
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1024
_exptl_absorpt_coefficient_mu 3.483
# Sheldrick geometric approximatio 0.86 0.95
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)'
_exptl_absorpt_correction_T_min 0.69
_exptl_absorpt_correction_T_max 0.95
_diffrn_measurement_device_type 'Oxford Diffraction SuperNova'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'graphite'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54180
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction 'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 160
_diffrn_reflns_number 24363
_reflns_number_total 4772
_diffrn_reflns_av_R_equivalents 0.102
# Number of reflections without Friedels Law is 4772
# Number of reflections with Friedels Law is 2795
# Theoretical number of reflections is about 2387
_diffrn_reflns_theta_min 4.178
_diffrn_reflns_theta_max 74.486
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 74.486
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -52
_diffrn_reflns_limit_l_max 52
_reflns_limit_h_min -7
_reflns_limit_h_max 7
_reflns_limit_k_min 0
_reflns_limit_k_max 11
_reflns_limit_l_min 0
_reflns_limit_l_max 52
_oxford_diffrn_Wilson_B_factor 2.85
_oxford_diffrn_Wilson_scale 3.39
_atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.72
_refine_diff_density_max 0.93
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns 4772
_refine_ls_number_restraints 0
_refine_ls_number_parameters 272
_oxford_refine_ls_R_factor_ref 0.0768
_refine_ls_wR_factor_ref 0.0915
_refine_ls_goodness_of_fit_ref 1.0929
_refine_ls_shift/su_max 0.0017776
_refine_ls_shift/su_mean 0.0000981
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 4772
_refine_ls_R_factor_all 0.0768
_refine_ls_wR_factor_all 0.0915
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 4199
_refine_ls_R_factor_gt 0.0669
_refine_ls_wR_factor_gt 0.0899
_refine_ls_abs_structure_Flack -0.04(3)
_refine_ls_abs_structure_details 'Flack (1983), 1977 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration 'ad'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
29.0 23.1 9.35
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Agilent (2011). CrysAlisPro.
Oxford Diffraction, (2010). Supernova User Manual.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
S1 S -0.0196(3) 0.16071(18) 0.58505(4) 0.0428 1.0000 Uani . . . . . .
C2 C 0.1067(9) 0.1066(8) 0.62127(14) 0.0374 1.0000 Uani . . . . . .
C3 C 0.1757(11) -0.0332(8) 0.62539(18) 0.0442 1.0000 Uani . . . . . .
C4 C 0.2736(12) -0.0799(8) 0.65363(16) 0.0483 1.0000 Uani . . . . . .
C5 C 0.2981(12) 0.0226(8) 0.67763(18) 0.0478 1.0000 Uani . . . . . .
C6 C 0.2283(11) 0.1644(8) 0.67375(17) 0.0394 1.0000 Uani . . . . . .
C7 C 0.1299(10) 0.2103(7) 0.64579(15) 0.0321 1.0000 Uani . . . . . .
N8 N 0.0507(7) 0.3563(5) 0.64275(10) 0.0290 1.0000 Uani . . . . . .
C9 C -0.0934(9) 0.4188(7) 0.66718(13) 0.0294 1.0000 Uani . . . . . .
C10 C 0.0286(10) 0.5280(6) 0.68756(13) 0.0312 1.0000 Uani . . . . . .
N11 N -0.1185(7) 0.6150(6) 0.70871(10) 0.0275 1.0000 Uani . . . . . .
C12 C -0.2436(11) 0.7306(7) 0.69168(16) 0.0385 1.0000 Uani . . . . . .
C13 C 0.0065(12) 0.6818(6) 0.73561(14) 0.0452 1.0000 Uani . . . . . .
C14 C 0.0917(9) 0.4459(7) 0.61721(14) 0.0306 1.0000 Uani . . . . . .
O15 O 0.0096(8) 0.5654(4) 0.61337(8) 0.0353 1.0000 Uani . . . . . .
C16 C 0.2702(9) 0.3849(8) 0.59466(14) 0.0321 1.0000 Uani . . . . . .
O17 O 0.3822(6) 0.5117(5) 0.58050(10) 0.0374 1.0000 Uani . . . . . .
C18 C 0.4840(10) 0.6029(8) 0.60184(13) 0.0365 1.0000 Uani . . . . . .
O19 O 0.4773(8) 0.5760(5) 0.62998(9) 0.0408 1.0000 Uani . . . . . .
C20 C 0.5967(10) 0.7309(7) 0.58725(15) 0.0403 1.0000 Uani . . . . . .
C21 C 0.1802(10) 0.2881(7) 0.56829(15) 0.0374 1.0000 Uani . . . . . .
C22 C 0.0745(10) 0.3688(8) 0.54052(15) 0.0367 1.0000 Uani . . . . . .
C23 C -0.1281(10) 0.4362(7) 0.54301(15) 0.0347 1.0000 Uani . . . . . .
C24 C -0.2245(10) 0.5101(8) 0.51794(15) 0.0347 1.0000 Uani . . . . . .
C25 C -0.1192(10) 0.5144(6) 0.48912(14) 0.0246 1.0000 Uani . . . . . .
C26 C 0.0829(9) 0.4457(6) 0.48617(15) 0.0270 1.0000 Uani . . . . . .
C27 C 0.1755(9) 0.3733(7) 0.51119(15) 0.0324 1.0000 Uani . . . . . .
O28 O -0.1984(6) 0.5869(6) 0.46312(9) 0.0388 1.0000 Uani . . . . . .
C29 C -0.3813(11) 0.6810(7) 0.46722(16) 0.0426 1.0000 Uani . . . . . .
Br30 Br 0.52050(10) 0.39795(8) 0.736573(16) 0.0398 1.0000 Uani . . . . . .
H293 H -0.4059 0.7362 0.4482 0.0628 1.0000 Uiso R . . . . .
H292 H -0.5079 0.6224 0.4720 0.0628 1.0000 Uiso R . . . . .
H291 H -0.3538 0.7486 0.4840 0.0629 1.0000 Uiso R . . . . .
H231 H -0.2024 0.4307 0.5623 0.0398 1.0000 Uiso R . . . . .
H241 H -0.3601 0.5565 0.5205 0.0408 1.0000 Uiso R . . . . .
H261 H 0.1532 0.4486 0.4669 0.0372 1.0000 Uiso R . . . . .
H271 H 0.3100 0.3252 0.5087 0.0413 1.0000 Uiso R . . . . .
H211 H 0.3022 0.2291 0.5601 0.0421 1.0000 Uiso R . . . . .
H203 H 0.5795 0.8166 0.6003 0.0632 1.0000 Uiso R . . . . .
H202 H 0.7487 0.7094 0.5848 0.0631 1.0000 Uiso R . . . . .
H201 H 0.5336 0.7494 0.5670 0.0631 1.0000 Uiso R . . . . .
H161 H 0.3775 0.3285 0.6069 0.0409 1.0000 Uiso R . . . . .
H133 H -0.0917 0.7331 0.7493 0.0719 1.0000 Uiso R . . . . .
H132 H 0.1124 0.7505 0.7276 0.0718 1.0000 Uiso R . . . . .
H131 H 0.0790 0.6058 0.7472 0.0718 1.0000 Uiso R . . . . .
H123 H -0.3501 0.7737 0.7058 0.0591 1.0000 Uiso R . . . . .
H122 H -0.3167 0.6887 0.6738 0.0590 1.0000 Uiso R . . . . .
H121 H -0.1439 0.8067 0.6848 0.0588 1.0000 Uiso R . . . . .
H111 H -0.2151 0.5524 0.7170 0.0421 1.0000 Uiso R . . . . .
H102 H 0.1035 0.5980 0.6739 0.0370 1.0000 Uiso R . . . . .
H101 H 0.1329 0.4752 0.7002 0.0371 1.0000 Uiso R . . . . .
H92 H -0.2162 0.4669 0.6572 0.0360 1.0000 Uiso R . . . . .
H91 H -0.1442 0.3371 0.6802 0.0360 1.0000 Uiso R . . . . .
H31 H 0.1577 -0.1011 0.6090 0.0510 1.0000 Uiso R . . . . .
H41 H 0.3202 -0.1767 0.6561 0.0571 1.0000 Uiso R . . . . .
H51 H 0.3646 -0.0047 0.6966 0.0598 1.0000 Uiso R . . . . .
H61 H 0.2472 0.2329 0.6900 0.0501 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0438(10) 0.0469(10) 0.0376(8) -0.0077(7) -0.0078(10) 0.0019(10)
C2 0.033(3) 0.037(4) 0.043(4) -0.001(4) 0.001(3) 0.008(3)
C3 0.046(4) 0.032(4) 0.055(5) -0.006(4) 0.002(4) 0.004(3)
C4 0.058(5) 0.034(5) 0.052(5) -0.006(4) 0.002(4) 0.012(4)
C5 0.053(5) 0.046(5) 0.044(4) 0.004(4) -0.005(4) 0.025(4)
C6 0.043(4) 0.037(4) 0.038(4) -0.007(3) -0.001(3) 0.001(3)
C7 0.032(3) 0.034(4) 0.031(4) -0.002(3) 0.002(3) 0.006(3)
N8 0.025(3) 0.035(3) 0.026(2) -0.005(2) -0.003(2) 0.010(2)
C9 0.026(3) 0.028(4) 0.035(3) -0.004(3) -0.002(2) 0.009(3)
C10 0.024(3) 0.029(3) 0.041(3) -0.005(3) 0.005(3) 0.007(3)
N11 0.026(2) 0.025(3) 0.032(3) -0.005(3) 0.000(2) 0.003(2)
C12 0.043(4) 0.026(4) 0.047(4) -0.003(3) -0.001(3) 0.015(3)
C13 0.035(3) 0.061(4) 0.040(3) -0.023(3) -0.009(4) 0.014(4)
C14 0.018(3) 0.041(4) 0.032(3) -0.012(3) -0.004(2) 0.006(3)
O15 0.030(2) 0.039(3) 0.037(2) 0.0013(18) 0.003(2) 0.016(3)
C16 0.029(3) 0.030(4) 0.037(3) -0.005(3) 0.000(3) 0.010(3)
O17 0.027(2) 0.045(3) 0.041(3) -0.008(2) 0.000(2) 0.009(2)
C18 0.020(3) 0.045(3) 0.044(3) -0.012(3) -0.002(3) 0.014(4)
O19 0.032(2) 0.050(3) 0.040(2) 0.000(2) -0.003(2) 0.004(3)
C20 0.030(4) 0.042(4) 0.049(4) 0.007(4) -0.002(3) 0.008(3)
C21 0.035(4) 0.041(4) 0.036(4) -0.009(3) -0.001(3) 0.016(3)
C22 0.032(4) 0.049(5) 0.029(3) -0.009(3) -0.005(3) 0.011(3)
C23 0.034(3) 0.041(4) 0.029(4) -0.006(3) 0.002(3) 0.009(3)
C24 0.025(3) 0.039(4) 0.041(4) 0.000(3) -0.002(3) 0.005(3)
C25 0.030(3) 0.012(3) 0.031(3) 0.001(3) -0.003(3) -0.001(2)
C26 0.027(3) 0.015(3) 0.038(4) -0.003(3) 0.007(3) -0.003(2)
C27 0.023(3) 0.030(4) 0.044(4) -0.006(3) -0.002(3) 0.006(3)
O28 0.037(2) 0.047(3) 0.033(2) 0.009(2) 0.0041(19) 0.008(2)
C29 0.038(4) 0.046(5) 0.044(4) 0.007(4) -0.004(3) 0.009(4)
Br30 0.0287(3) 0.0486(4) 0.0422(3) 0.0052(4) -0.0020(3) -0.0043(4)
_refine_ls_extinction_method
'None'
_oxford_refine_ls_scale 0.5919(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 . C2 . 1.785(6) yes
S1 . C21 . 1.820(7) yes
C2 . C3 . 1.342(9) yes
C2 . C7 . 1.405(9) yes
C3 . C4 . 1.402(9) yes
C3 . H31 . 0.933 no
C4 . C5 . 1.382(9) yes
C4 . H41 . 0.925 no
C5 . C6 . 1.360(9) yes
C5 . H51 . 0.932 no
C6 . C7 . 1.390(9) yes
C6 . H61 . 0.933 no
C7 . N8 . 1.411(7) yes
N8 . C9 . 1.470(6) yes
N8 . C14 . 1.373(7) yes
C9 . C10 . 1.507(7) yes
C9 . H92 . 0.964 no
C9 . H91 . 0.972 no
C10 . N11 . 1.492(6) yes
C10 . H102 . 0.970 no
C10 . H101 . 0.958 no
N11 . C12 . 1.481(7) yes
N11 . C13 . 1.497(7) yes
N11 . H111 . 0.889 no
C12 . H123 . 0.966 no
C12 . H122 . 0.956 no
C12 . H121 . 0.963 no
C13 . H133 . 0.953 no
C13 . H132 . 0.958 no
C13 . H131 . 0.954 no
C14 . O15 . 1.202(7) yes
C14 . C16 . 1.550(7) yes
C16 . O17 . 1.462(7) yes
C16 . C21 . 1.521(8) yes
C16 . H161 . 0.979 no
O17 . C18 . 1.372(7) yes
C18 . O19 . 1.216(6) yes
C18 . C20 . 1.480(9) yes
C20 . H203 . 0.956 no
C20 . H202 . 0.954 no
C20 . H201 . 0.953 no
C21 . C22 . 1.527(9) yes
C21 . H211 . 0.980 no
C22 . C23 . 1.382(8) yes
C22 . C27 . 1.387(8) yes
C23 . C24 . 1.385(9) yes
C23 . H231 . 0.936 no
C24 . C25 . 1.380(8) yes
C24 . H241 . 0.934 no
C25 . C26 . 1.387(7) yes
C25 . O28 . 1.369(7) yes
C26 . C27 . 1.367(8) yes
C26 . H261 . 0.924 no
C27 . H271 . 0.935 no
O28 . C29 . 1.414(7) yes
C29 . H293 . 0.958 no
C29 . H292 . 0.958 no
C29 . H291 . 0.952 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . S1 . C21 . 102.6(3) yes
S1 . C2 . C3 . 120.3(6) yes
S1 . C2 . C7 . 119.7(5) yes
C3 . C2 . C7 . 120.0(6) yes
C2 . C3 . C4 . 121.8(7) yes
C2 . C3 . H31 . 119.0 no
C4 . C3 . H31 . 119.2 no
C3 . C4 . C5 . 118.1(7) yes
C3 . C4 . H41 . 120.8 no
C5 . C4 . H41 . 121.1 no
C4 . C5 . C6 . 120.6(7) yes
C4 . C5 . H51 . 120.1 no
C6 . C5 . H51 . 119.3 no
C5 . C6 . C7 . 121.2(7) yes
C5 . C6 . H61 . 119.8 no
C7 . C6 . H61 . 119.0 no
C2 . C7 . C6 . 118.3(6) yes
C2 . C7 . N8 . 121.4(6) yes
C6 . C7 . N8 . 120.3(6) yes
C7 . N8 . C9 . 120.0(5) yes
C7 . N8 . C14 . 124.0(5) yes
C9 . N8 . C14 . 115.9(5) yes
N8 . C9 . C10 . 111.0(4) yes
N8 . C9 . H92 . 109.2 no
C10 . C9 . H92 . 109.9 no
N8 . C9 . H91 . 107.4 no
C10 . C9 . H91 . 109.3 no
H92 . C9 . H91 . 110.0 no
C9 . C10 . N11 . 113.0(5) yes
C9 . C10 . H102 . 108.6 no
N11 . C10 . H102 . 107.3 no
C9 . C10 . H101 . 108.8 no
N11 . C10 . H101 . 109.1 no
H102 . C10 . H101 . 110.0 no
C10 . N11 . C12 . 112.9(4) yes
C10 . N11 . C13 . 111.2(4) yes
C12 . N11 . C13 . 110.4(5) yes
C10 . N11 . H111 . 107.5 no
C12 . N11 . H111 . 107.3 no
C13 . N11 . H111 . 107.1 no
N11 . C12 . H123 . 109.2 no
N11 . C12 . H122 . 110.3 no
H123 . C12 . H122 . 109.5 no
N11 . C12 . H121 . 108.9 no
H123 . C12 . H121 . 109.1 no
H122 . C12 . H121 . 109.7 no
N11 . C13 . H133 . 109.7 no
N11 . C13 . H132 . 109.6 no
H133 . C13 . H132 . 108.9 no
N11 . C13 . H131 . 109.9 no
H133 . C13 . H131 . 109.2 no
H132 . C13 . H131 . 109.6 no
N8 . C14 . O15 . 124.0(5) yes
N8 . C14 . C16 . 113.8(5) yes
O15 . C14 . C16 . 122.0(6) yes
C14 . C16 . O17 . 107.7(5) yes
C14 . C16 . C21 . 113.7(5) yes
O17 . C16 . C21 . 108.6(5) yes
C14 . C16 . H161 . 109.2 no
O17 . C16 . H161 . 108.1 no
C21 . C16 . H161 . 109.4 no
C16 . O17 . C18 . 114.3(5) yes
O17 . C18 . O19 . 120.6(6) yes
O17 . C18 . C20 . 113.9(5) yes
O19 . C18 . C20 . 125.5(6) yes
C18 . C20 . H203 . 109.9 no
C18 . C20 . H202 . 109.8 no
H203 . C20 . H202 . 109.5 no
C18 . C20 . H201 . 108.9 no
H203 . C20 . H201 . 109.4 no
H202 . C20 . H201 . 109.4 no
C16 . C21 . S1 . 108.6(4) yes
C16 . C21 . C22 . 116.3(6) yes
S1 . C21 . C22 . 108.6(4) yes
C16 . C21 . H211 . 107.4 no
S1 . C21 . H211 . 107.8 no
C22 . C21 . H211 . 107.9 no
C21 . C22 . C23 . 122.0(6) yes
C21 . C22 . C27 . 121.0(5) yes
C23 . C22 . C27 . 117.0(6) yes
C22 . C23 . C24 . 122.3(7) yes
C22 . C23 . H231 . 118.5 no
C24 . C23 . H231 . 119.2 no
C23 . C24 . C25 . 119.5(6) yes
C23 . C24 . H241 . 120.2 no
C25 . C24 . H241 . 120.2 no
C24 . C25 . C26 . 118.8(6) yes
C24 . C25 . O28 . 124.0(5) yes
C26 . C25 . O28 . 117.1(6) yes
C25 . C26 . C27 . 120.8(6) yes
C25 . C26 . H261 . 118.7 no
C27 . C26 . H261 . 120.4 no
C22 . C27 . C26 . 121.6(6) yes
C22 . C27 . H271 . 118.6 no
C26 . C27 . H271 . 119.9 no
C25 . O28 . C29 . 117.9(5) yes
O28 . C29 . H293 . 109.5 no
O28 . C29 . H292 . 109.3 no
H293 . C29 . H292 . 109.8 no
O28 . C29 . H291 . 109.8 no
H293 . C29 . H291 . 108.7 no
H292 . C29 . H291 . 109.8 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C20 . H202 . O15 1_655 135 0.95 2.38 3.132(9) yes
C20 . H201 . O28 3_566 145 0.95 2.41 3.241(9) yes
C12 . H122 . O19 1_455 177 0.96 2.46 3.417(9) yes
C9 . H92 . O19 1_455 177 0.96 2.41 3.372(9) yes
_iucr_refine_instructions_details
;
#
# Punched on 15/06/18 at 12:40:04
#
#LIST 12
BLOCK SCALE X'S U'S
CONT ENANTIO
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 9,X'S) H ( 92,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 102,X'S) H ( 101,X'S)
RIDE N ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 123,X'S) H ( 122,X'S) H ( 121,X'S)
RIDE C ( 13,X'S) H ( 133,X'S) H ( 132,X'S) H ( 131,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 20,X'S) H ( 203,X'S) H ( 202,X'S) H ( 201,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 26,X'S) H ( 261,X'S)
RIDE C ( 27,X'S) H ( 271,X'S)
RIDE C ( 29,X'S) H ( 293,X'S) H ( 292,X'S) H ( 291,X'S)
END
#
# Punched on 15/06/18 at 12:40:04
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
data_Diltiazemiodide
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 6.22190(10)
_cell_length_b 9.02280(10)
_cell_length_c 43.0569(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2417.17(5)
_symmetry_cell_setting 'orthorhombic'
_symmetry_space_group_name_H-M 'P 21 21 21 '
_symmetry_space_group_name_Hall 'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'x+1/2,-y+1/2,-z'
'-x,y+1/2,-z+1/2'
'-x+1/2,-y,z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687
0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424
0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975
1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536
1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
I -0.3257 6.8362 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660
2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C22 H27 I1 N2 O4 S1
# Dc = 1.49 Fooo = 1096.00 Mu = 114.56 M = 542.44
# Found Formula = C22 H27 I1 N2 O4 S1
# Dc = 1.49 FOOO = 1096.00 Mu = 114.56 M = 542.44
_chemical_formula_sum 'C22 H27 I N2 O4 S'
_chemical_formula_moiety 'C22 H27 N2 O4 S, I'
_chemical_compound_source ?
_chemical_formula_weight 542.44
_cell_measurement_reflns_used 13159
_cell_measurement_theta_min 4
_cell_measurement_theta_max 79
_cell_measurement_temperature 160
_exptl_crystal_description 'prism'
_exptl_crystal_colour 'colorless'
_exptl_crystal_size_min 0.031
_exptl_crystal_size_mid 0.050
_exptl_crystal_size_max 0.390
_exptl_crystal_density_diffrn 1.490
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1096
_exptl_absorpt_coefficient_mu 11.456
# Sheldrick geometric approximatio 0.56 0.70
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)'
_exptl_absorpt_correction_T_min 0.47
_exptl_absorpt_correction_T_max 0.70
_diffrn_measurement_device_type 'Oxford Diffraction SuperNova'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'graphite'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54180
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction 'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 160
_diffrn_reflns_number 15587
_reflns_number_total 4935
_diffrn_reflns_av_R_equivalents 0.030
# Number of reflections without Friedels Law is 4935
# Number of reflections with Friedels Law is 2885
# Theoretical number of reflections is about 2472
_diffrn_reflns_theta_min 4.107
_diffrn_reflns_theta_max 74.491
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 74.491
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -53
_diffrn_reflns_limit_l_max 52
_reflns_limit_h_min -7
_reflns_limit_h_max 7
_reflns_limit_k_min 0
_reflns_limit_k_max 11
_reflns_limit_l_min 0
_reflns_limit_l_max 53
_oxford_diffrn_Wilson_B_factor 2.13
_oxford_diffrn_Wilson_scale 0.02
_atom_sites_solution_primary direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.37
_refine_diff_density_max 0.36
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns 4935
_refine_ls_number_restraints 0
_refine_ls_number_parameters 272
_oxford_refine_ls_R_factor_ref 0.0209
_refine_ls_wR_factor_ref 0.0525
_refine_ls_goodness_of_fit_ref 0.9845
_refine_ls_shift/su_max 0.0015102
_refine_ls_shift/su_mean 0.0000579
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 4935
_refine_ls_R_factor_all 0.0209
_refine_ls_wR_factor_all 0.0525
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 4860
_refine_ls_R_factor_gt 0.0206
_refine_ls_wR_factor_gt 0.0524
_refine_ls_abs_structure_Flack -0.013(3)
_refine_ls_abs_structure_details 'Flack (1983), 2050 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration 'ad'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 1.04P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Agilent (2011). CrysAlisPro.
Oxford Diffraction, (2010). Supernova User Manual.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
S1 S 1.02427(11) 0.15951(6) 0.417600(13) 0.0276 1.0000 Uani . . . . . .
C2 C 0.8985(4) 0.1108(3) 0.38217(5) 0.0254 1.0000 Uani . . . . . .
C3 C 0.8229(5) -0.0332(3) 0.37791(6) 0.0303 1.0000 Uani . . . . . .
C4 C 0.7301(5) -0.0752(3) 0.34987(6) 0.0343 1.0000 Uani . . . . . .
C5 C 0.7125(5) 0.0256(3) 0.32594(6) 0.0337 1.0000 Uani . . . . . .
C6 C 0.7876(4) 0.1698(3) 0.32967(6) 0.0289 1.0000 Uani . . . . . .
C7 C 0.8805(4) 0.2134(3) 0.35759(6) 0.0237 1.0000 Uani . . . . . .
N8 N 0.9596(3) 0.3606(2) 0.36116(4) 0.0214 1.0000 Uani . . . . . .
C9 C 1.1007(4) 0.4238(3) 0.33715(5) 0.0221 1.0000 Uani . . . . . .
C10 C 0.9747(4) 0.5365(3) 0.31811(5) 0.0243 1.0000 Uani . . . . . .
N11 N 1.1161(3) 0.6262(2) 0.29716(4) 0.0218 1.0000 Uani . . . . . .
C12 C 0.9878(5) 0.6990(3) 0.27228(6) 0.0353 1.0000 Uani . . . . . .
C13 C 1.2474(5) 0.7371(3) 0.31425(6) 0.0321 1.0000 Uani . . . . . .
C14 C 0.9148(4) 0.4476(3) 0.38623(5) 0.0207 1.0000 Uani . . . . . .
O15 O 0.9969(3) 0.56815(16) 0.39033(3) 0.0245 1.0000 Uani . . . . . .
C16 C 0.7398(4) 0.3879(3) 0.40823(5) 0.0220 1.0000 Uani . . . . . .
O17 O 0.6276(3) 0.51100(19) 0.42194(4) 0.0234 1.0000 Uani . . . . . .
C18 C 0.5268(3) 0.5996(3) 0.40072(5) 0.0236 1.0000 Uani . . . . . .
O19 O 0.5332(3) 0.57361(18) 0.37324(4) 0.0276 1.0000 Uani . . . . . .
C20 C 0.4120(4) 0.7260(3) 0.41545(6) 0.0289 1.0000 Uani . . . . . .
C21 C 0.8276(4) 0.2897(3) 0.43445(5) 0.0240 1.0000 Uani . . . . . .
C22 C 0.9387(4) 0.3693(3) 0.46107(5) 0.0226 1.0000 Uani . . . . . .
C23 C 0.8368(4) 0.3766(3) 0.49003(5) 0.0225 1.0000 Uani . . . . . .
C24 C 0.9325(4) 0.4498(3) 0.51471(5) 0.0223 1.0000 Uani . . . . . .
C25 C 1.1323(4) 0.5170(3) 0.51102(5) 0.0207 1.0000 Uani . . . . . .
C26 C 1.2378(4) 0.5077(3) 0.48268(6) 0.0230 1.0000 Uani . . . . . .
C27 C 1.1405(4) 0.4332(3) 0.45812(5) 0.0242 1.0000 Uani . . . . . .
O28 O 1.2105(3) 0.5890(2) 0.53656(4) 0.0271 1.0000 Uani . . . . . .
C29 C 1.3943(4) 0.6818(3) 0.53234(6) 0.0312 1.0000 Uani . . . . . .
I30 I 1.48132(2) 0.394832(17) 0.264191(3) 0.0283 1.0000 Uani . . . . . .
H31 H 0.8293 -0.1014 0.3946 0.0364 1.0000 Uiso R . . . . .
H41 H 0.6792 -0.1716 0.3475 0.0405 1.0000 Uiso R . . . . .
H51 H 0.6519 -0.0015 0.3067 0.0405 1.0000 Uiso R . . . . .
H61 H 0.7702 0.2375 0.3135 0.0339 1.0000 Uiso R . . . . .
H92 H 1.2271 0.4704 0.3467 0.0270 1.0000 Uiso R . . . . .
H91 H 1.1486 0.3436 0.3237 0.0273 1.0000 Uiso R . . . . .
H101 H 0.9003 0.6034 0.3321 0.0296 1.0000 Uiso R . . . . .
H102 H 0.8718 0.4869 0.3050 0.0292 1.0000 Uiso R . . . . .
H121 H 1.0820 0.7558 0.2597 0.0529 1.0000 Uiso R . . . . .
H122 H 0.8828 0.7612 0.2820 0.0533 1.0000 Uiso R . . . . .
H123 H 0.9229 0.6244 0.2602 0.0531 1.0000 Uiso R . . . . .
H131 H 1.3391 0.7860 0.2995 0.0488 1.0000 Uiso R . . . . .
H132 H 1.3316 0.6882 0.3300 0.0487 1.0000 Uiso R . . . . .
H133 H 1.1536 0.8087 0.3234 0.0492 1.0000 Uiso R . . . . .
H161 H 0.6379 0.3309 0.3960 0.0259 1.0000 Uiso R . . . . .
H201 H 0.3910 0.8033 0.4007 0.0463 1.0000 Uiso R . . . . .
H202 H 0.4869 0.7638 0.4331 0.0467 1.0000 Uiso R . . . . .
H203 H 0.2762 0.6905 0.4218 0.0457 1.0000 Uiso R . . . . .
H211 H 0.7095 0.2310 0.4428 0.0290 1.0000 Uiso R . . . . .
H231 H 0.7014 0.3318 0.4926 0.0267 1.0000 Uiso R . . . . .
H241 H 0.8651 0.4560 0.5339 0.0265 1.0000 Uiso R . . . . .
H261 H 1.3700 0.5509 0.4796 0.0276 1.0000 Uiso R . . . . .
H271 H 1.2169 0.4250 0.4391 0.0286 1.0000 Uiso R . . . . .
H292 H 1.4171 0.7329 0.5514 0.0459 1.0000 Uiso R . . . . .
H291 H 1.5169 0.6195 0.5279 0.0458 1.0000 Uiso R . . . . .
H293 H 1.3691 0.7492 0.5154 0.0458 1.0000 Uiso R . . . . .
H111 H 1.2089 0.5655 0.2883 0.0328 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0344(3) 0.0262(2) 0.0222(2) 0.00463(19) -0.0066(3) -0.0002(3)
C2 0.0295(11) 0.0249(11) 0.0219(11) 0.0038(10) -0.0027(9) -0.0026(10)
C3 0.0368(14) 0.0221(12) 0.0322(13) 0.0060(10) 0.0018(11) -0.0049(10)
C4 0.0432(15) 0.0249(13) 0.0347(14) -0.0033(11) 0.0001(11) -0.0076(11)
C5 0.0391(15) 0.0319(14) 0.0300(13) -0.0065(11) -0.0050(12) -0.0075(12)
C6 0.0374(14) 0.0292(13) 0.0201(11) 0.0015(10) -0.0038(10) -0.0036(11)
C7 0.0289(12) 0.0214(11) 0.0207(11) 0.0011(9) -0.0011(9) -0.0032(9)
N8 0.0264(9) 0.0210(8) 0.0167(8) 0.0042(6) 0.0009(7) -0.0051(7)
C9 0.0225(10) 0.0245(11) 0.0193(10) 0.0045(9) 0.0021(8) -0.0016(9)
C10 0.0200(11) 0.0300(11) 0.0230(10) 0.0080(8) -0.0012(9) -0.0055(10)
N11 0.0209(9) 0.0260(10) 0.0185(9) 0.0046(8) 0.0004(7) -0.0017(8)
C12 0.0323(13) 0.0429(14) 0.0307(12) 0.0174(10) -0.0088(11) -0.0072(12)
C13 0.0352(14) 0.0305(13) 0.0304(13) 0.0052(11) -0.0038(11) -0.0111(11)
C14 0.0187(10) 0.0254(11) 0.0181(10) 0.0049(8) -0.0037(8) -0.0019(8)
O15 0.0246(8) 0.0255(7) 0.0234(7) 0.0009(6) -0.0005(7) -0.0090(7)
C16 0.0223(10) 0.0253(11) 0.0183(10) 0.0025(9) -0.0009(8) -0.0046(10)
O17 0.0235(8) 0.0291(8) 0.0176(7) 0.0029(6) -0.0012(6) -0.0023(7)
C18 0.0185(10) 0.0284(10) 0.0240(10) 0.0043(8) -0.0014(8) -0.0075(11)
O19 0.0277(8) 0.0336(8) 0.0213(7) 0.0017(6) -0.0038(7) -0.0007(7)
C20 0.0251(12) 0.0295(12) 0.0320(13) -0.0001(10) -0.0010(10) -0.0043(10)
C21 0.0245(11) 0.0271(12) 0.0204(11) 0.0054(9) -0.0024(9) -0.0067(9)
C22 0.0248(11) 0.0253(11) 0.0178(10) 0.0052(9) -0.0025(8) -0.0038(9)
C23 0.0197(10) 0.0249(11) 0.0229(11) 0.0066(9) 0.0011(8) -0.0004(9)
C24 0.0229(11) 0.0244(10) 0.0195(10) 0.0036(8) 0.0045(8) 0.0029(9)
C25 0.0238(11) 0.0189(10) 0.0195(10) 0.0022(9) -0.0023(9) 0.0034(9)
C26 0.0179(10) 0.0284(12) 0.0227(11) 0.0045(9) -0.0007(9) -0.0028(8)
C27 0.0261(11) 0.0302(12) 0.0162(10) 0.0035(9) 0.0022(9) -0.0041(9)
O28 0.0286(8) 0.0312(9) 0.0214(8) -0.0034(7) 0.0001(6) -0.0043(8)
C29 0.0296(13) 0.0334(13) 0.0306(13) -0.0011(11) -0.0025(10) -0.0068(11)
I30 0.02538(7) 0.03403(8) 0.02551(7) -0.00578(6) -0.00250(6) 0.00332(6)
_refine_ls_extinction_method
'None'
_oxford_refine_ls_scale 3.276(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 . C2 . 1.770(2) yes
S1 . C21 . 1.845(3) yes
C2 . C3 . 1.394(4) yes
C2 . C7 . 1.411(3) yes
C3 . C4 . 1.391(4) yes
C3 . H31 . 0.947 no
C4 . C5 . 1.379(4) yes
C4 . H41 . 0.931 no
C5 . C6 . 1.392(4) yes
C5 . H51 . 0.943 no
C6 . C7 . 1.391(3) yes
C6 . H61 . 0.933 no
C7 . N8 . 1.425(3) yes
N8 . C9 . 1.471(3) yes
N8 . C14 . 1.364(3) yes
C9 . C10 . 1.524(3) yes
C9 . H92 . 0.981 no
C9 . H91 . 0.974 no
C10 . N11 . 1.497(3) yes
C10 . H101 . 0.970 no
C10 . H102 . 0.965 no
N11 . C12 . 1.489(3) yes
N11 . C13 . 1.487(3) yes
N11 . H111 . 0.884 no
C12 . H121 . 0.948 no
C12 . H122 . 0.958 no
C12 . H123 . 0.942 no
C13 . H131 . 0.959 no
C13 . H132 . 0.964 no
C13 . H133 . 0.957 no
C14 . O15 . 1.214(3) yes
C14 . C16 . 1.540(3) yes
C16 . O17 . 1.439(3) yes
C16 . C21 . 1.535(3) yes
C16 . H161 . 0.971 no
O17 . C18 . 1.367(3) yes
C18 . O19 . 1.207(3) yes
C18 . C20 . 1.488(3) yes
C20 . H201 . 0.953 no
C20 . H202 . 0.953 no
C20 . H203 . 0.944 no
C21 . C22 . 1.519(3) yes
C21 . H211 . 0.975 no
C22 . C23 . 1.400(3) yes
C22 . C27 . 1.387(3) yes
C23 . C24 . 1.385(3) yes
C23 . H231 . 0.941 no
C24 . C25 . 1.392(3) yes
C24 . H241 . 0.928 no
C25 . C26 . 1.388(3) yes
C25 . O28 . 1.367(3) yes
C26 . C27 . 1.391(3) yes
C26 . H261 . 0.920 no
C27 . H271 . 0.949 no
O28 . C29 . 1.429(3) yes
C29 . H292 . 0.953 no
C29 . H291 . 0.966 no
C29 . H293 . 0.963 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . S1 . C21 . 101.76(11) yes
S1 . C2 . C3 . 119.62(19) yes
S1 . C2 . C7 . 121.22(19) yes
C3 . C2 . C7 . 119.1(2) yes
C2 . C3 . C4 . 120.5(2) yes
C2 . C3 . H31 . 119.4 no
C4 . C3 . H31 . 120.0 no
C3 . C4 . C5 . 120.1(2) yes
C3 . C4 . H41 . 119.3 no
C5 . C4 . H41 . 120.5 no
C4 . C5 . C6 . 120.3(2) yes
C4 . C5 . H51 . 121.2 no
C6 . C5 . H51 . 118.5 no
C5 . C6 . C7 . 120.2(2) yes
C5 . C6 . H61 . 119.1 no
C7 . C6 . H61 . 120.6 no
C2 . C7 . C6 . 119.7(2) yes
C2 . C7 . N8 . 120.3(2) yes
C6 . C7 . N8 . 120.0(2) yes
C7 . N8 . C9 . 119.45(18) yes
C7 . N8 . C14 . 123.46(19) yes
C9 . N8 . C14 . 117.08(18) yes
N8 . C9 . C10 . 109.24(18) yes
N8 . C9 . H92 . 110.5 no
C10 . C9 . H92 . 110.6 no
N8 . C9 . H91 . 108.2 no
C10 . C9 . H91 . 109.5 no
H92 . C9 . H91 . 108.8 no
C9 . C10 . N11 . 112.48(19) yes
C9 . C10 . H101 . 109.0 no
N11 . C10 . H101 . 108.6 no
C9 . C10 . H102 . 110.3 no
N11 . C10 . H102 . 106.7 no
H101 . C10 . H102 . 109.7 no
C10 . N11 . C12 . 110.91(18) yes
C10 . N11 . C13 . 112.86(18) yes
C12 . N11 . C13 . 110.7(2) yes
C10 . N11 . H111 . 108.1 no
C12 . N11 . H111 . 108.2 no
C13 . N11 . H111 . 105.8 no
N11 . C12 . H121 . 108.5 no
N11 . C12 . H122 . 108.1 no
H121 . C12 . H122 . 110.7 no
N11 . C12 . H123 . 108.3 no
H121 . C12 . H123 . 109.6 no
H122 . C12 . H123 . 111.6 no
N11 . C13 . H131 . 108.0 no
N11 . C13 . H132 . 109.8 no
H131 . C13 . H132 . 110.6 no
N11 . C13 . H133 . 108.9 no
H131 . C13 . H133 . 109.0 no
H132 . C13 . H133 . 110.5 no
N8 . C14 . O15 . 123.0(2) yes
N8 . C14 . C16 . 115.46(19) yes
O15 . C14 . C16 . 121.4(2) yes
C14 . C16 . O17 . 108.97(19) yes
C14 . C16 . C21 . 113.77(19) yes
O17 . C16 . C21 . 108.44(17) yes
C14 . C16 . H161 . 108.3 no
O17 . C16 . H161 . 108.3 no
C21 . C16 . H161 . 109.0 no
C16 . O17 . C18 . 113.60(17) yes
O17 . C18 . O19 . 121.8(2) yes
O17 . C18 . C20 . 112.58(19) yes
O19 . C18 . C20 . 125.7(2) yes
C18 . C20 . H201 . 110.0 no
C18 . C20 . H202 . 112.2 no
H201 . C20 . H202 . 109.7 no
C18 . C20 . H203 . 107.0 no
H201 . C20 . H203 . 108.6 no
H202 . C20 . H203 . 109.2 no
C16 . C21 . S1 . 108.29(16) yes
C16 . C21 . C22 . 116.4(2) yes
S1 . C21 . C22 . 107.21(16) yes
C16 . C21 . H211 . 108.5 no
S1 . C21 . H211 . 107.4 no
C22 . C21 . H211 . 108.7 no
C21 . C22 . C23 . 119.2(2) yes
C21 . C22 . C27 . 122.6(2) yes
C23 . C22 . C27 . 118.1(2) yes
C22 . C23 . C24 . 120.7(2) yes
C22 . C23 . H231 . 119.2 no
C24 . C23 . H231 . 120.0 no
C23 . C24 . C25 . 120.3(2) yes
C23 . C24 . H241 . 121.1 no
C25 . C24 . H241 . 118.6 no
C24 . C25 . C26 . 119.7(2) yes
C24 . C25 . O28 . 115.7(2) yes
C26 . C25 . O28 . 124.6(2) yes
C25 . C26 . C27 . 119.4(2) yes
C25 . C26 . H261 . 121.5 no
C27 . C26 . H261 . 119.0 no
C26 . C27 . C22 . 121.7(2) yes
C26 . C27 . H271 . 118.4 no
C22 . C27 . H271 . 120.0 no
C25 . O28 . C29 . 117.46(19) yes
O28 . C29 . H292 . 107.0 no
O28 . C29 . H291 . 108.4 no
H292 . C29 . H291 . 109.5 no
O28 . C29 . H293 . 109.7 no
H292 . C29 . H293 . 111.9 no
H291 . C29 . H293 . 110.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C9 . H92 . O19 1_655 176 0.98 2.41 3.388(4) yes
C13 . H132 . O19 1_655 176 0.96 2.47 3.434(4) yes
C20 . H202 . O28 2_466 161 0.95 2.33 3.241(4) yes
C20 . H203 . O15 1_455 129 0.94 2.46 3.142(4) yes
_iucr_refine_instructions_details
;
#
# Punched on 15/06/18 at 12:41:51
#
#LIST 12
BLOCK SCALE X'S U'S
CONT ENANTIO
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 9,X'S) H ( 92,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S)
RIDE N ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) H ( 123,X'S)
RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S) H ( 133,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) H ( 203,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 26,X'S) H ( 261,X'S)
RIDE C ( 27,X'S) H ( 271,X'S)
RIDE C ( 29,X'S) H ( 292,X'S) H ( 291,X'S) H ( 293,X'S)
END
#
# Punched on 15/06/18 at 12:41:51
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
data_Diltiazemnitrate
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 6.37650(10)
_cell_length_b 8.81740(10)
_cell_length_c 42.9420(7)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2414.38(6)
_symmetry_cell_setting 'orthorhombic'
_symmetry_space_group_name_H-M 'P 21 21 21 '
_symmetry_space_group_name_Hall 'P 2ac 2ab '
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x+1/2,-y,z+1/2'
'x+1/2,-y+1/2,-z'
'-x,y+1/2,-z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687
0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424
0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975
1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536
1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C22 H27 N3 O7 S1
# Dc = 1.31 Fooo = 1008.00 Mu = 15.93 M = 477.54
# Found Formula = C22 H27 N3 O7 S1
# Dc = 1.31 FOOO = 1008.00 Mu = 15.93 M = 477.54
_chemical_formula_sum 'C22 H27 N3 O7 S'
_chemical_formula_moiety 'C22 H27 N2 O4 S, N O3'
_chemical_compound_source ?
_chemical_formula_weight 477.54
_cell_measurement_reflns_used 11950
_cell_measurement_theta_min 4
_cell_measurement_theta_max 78
_cell_measurement_temperature 160
_exptl_crystal_description 'prism'
_exptl_crystal_colour 'colorless'
_exptl_crystal_size_min 0.027
_exptl_crystal_size_mid 0.048
_exptl_crystal_size_max 0.621
_exptl_crystal_density_diffrn 1.314
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1008
_exptl_absorpt_coefficient_mu 1.593
# Sheldrick geometric approximatio 0.93 0.96
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)'
_exptl_absorpt_correction_T_min 0.58
_exptl_absorpt_correction_T_max 0.96
_diffrn_measurement_device_type 'Oxford Diffraction SuperNova'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'graphite'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction 'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 160
_diffrn_reflns_number 25295
_reflns_number_total 4925
_diffrn_reflns_av_R_equivalents 0.051
# Number of reflections without Friedels Law is 4925
# Number of reflections with Friedels Law is 2874
# Theoretical number of reflections is about 2467
_diffrn_reflns_theta_min 4.118
_diffrn_reflns_theta_max 74.459
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 74.459
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -53
_diffrn_reflns_limit_l_max 53
_reflns_limit_h_min -7
_reflns_limit_h_max 7
_reflns_limit_k_min 0
_reflns_limit_k_max 11
_reflns_limit_l_min 0
_reflns_limit_l_max 53
_oxford_diffrn_Wilson_B_factor 2.32
_oxford_diffrn_Wilson_scale 0.06
_atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.26
_refine_diff_density_max 0.35
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns 4925
_refine_ls_number_restraints 0
_refine_ls_number_parameters 299
_oxford_refine_ls_R_factor_ref 0.0417
_refine_ls_wR_factor_ref 0.0928
_refine_ls_goodness_of_fit_ref 0.9931
_refine_ls_shift/su_max 0.0008641
_refine_ls_shift/su_mean 0.0000413
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 4925
_refine_ls_R_factor_all 0.0417
_refine_ls_wR_factor_all 0.0928
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 4641
_refine_ls_R_factor_gt 0.0389
_refine_ls_wR_factor_gt 0.0913
_refine_ls_abs_structure_Flack 0.030(18)
_refine_ls_abs_structure_details 'Flack (1983), 2051 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration 'ad'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.44P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Agilent (2011). CrysAlisPro.
Oxford Diffraction, (2010). Supernova User Manual.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
S1 S 0.48622(9) 0.15743(6) 0.416803(12) 0.0304 1.0000 Uani . . . . . .
C2 C 0.3603(4) 0.1099(2) 0.38127(5) 0.0281 1.0000 Uani . . . . . .
C3 C 0.2838(4) -0.0364(3) 0.37682(6) 0.0346 1.0000 Uani . . . . . .
C4 C 0.1900(4) -0.0764(3) 0.34889(6) 0.0393 1.0000 Uani . . . . . .
C5 C 0.1767(4) 0.0277(3) 0.32499(6) 0.0396 1.0000 Uani . . . . . .
C6 C 0.2524(4) 0.1741(3) 0.32892(5) 0.0341 1.0000 Uani . . . . . .
C7 C 0.3456(4) 0.2158(2) 0.35687(5) 0.0276 1.0000 Uani . . . . . .
N8 N 0.4237(3) 0.3662(2) 0.36097(4) 0.0253 1.0000 Uani . . . . . .
C9 C 0.5657(3) 0.4309(3) 0.33734(5) 0.0276 1.0000 Uani . . . . . .
C10 C 0.4450(4) 0.5452(3) 0.31781(5) 0.0332 1.0000 Uani . . . . . .
N11 N 0.5822(3) 0.6363(2) 0.29678(4) 0.0337 1.0000 Uani . . . . . .
C12 C 0.7080(5) 0.7493(3) 0.31383(6) 0.0481 1.0000 Uani . . . . . .
C13 C 0.4533(5) 0.7108(4) 0.27208(6) 0.0563 1.0000 Uani . . . . . .
C14 C 0.3762(3) 0.4539(2) 0.38598(5) 0.0234 1.0000 Uani . . . . . .
O15 O 0.4559(2) 0.57880(16) 0.39037(3) 0.0283 1.0000 Uani . . . . . .
C16 C 0.2076(3) 0.3910(2) 0.40798(4) 0.0235 1.0000 Uani . . . . . .
O17 O 0.0944(2) 0.51510(16) 0.42200(3) 0.0262 1.0000 Uani . . . . . .
C18 C -0.0094(3) 0.6025(2) 0.40093(5) 0.0260 1.0000 Uani . . . . . .
O19 O -0.0057(3) 0.57586(17) 0.37345(3) 0.0304 1.0000 Uani . . . . . .
C20 C -0.1245(4) 0.7306(2) 0.41584(6) 0.0319 1.0000 Uani . . . . . .
C21 C 0.2958(3) 0.2901(2) 0.43394(5) 0.0261 1.0000 Uani . . . . . .
C22 C 0.4057(3) 0.3708(2) 0.46073(5) 0.0245 1.0000 Uani . . . . . .
C23 C 0.3056(3) 0.3782(2) 0.48979(5) 0.0244 1.0000 Uani . . . . . .
C24 C 0.4019(3) 0.4500(2) 0.51469(5) 0.0240 1.0000 Uani . . . . . .
C25 C 0.5970(4) 0.5166(2) 0.51106(5) 0.0245 1.0000 Uani . . . . . .
C26 C 0.7005(3) 0.5077(2) 0.48265(5) 0.0248 1.0000 Uani . . . . . .
C27 C 0.6027(3) 0.4344(2) 0.45783(5) 0.0264 1.0000 Uani . . . . . .
O28 O 0.6775(2) 0.58701(18) 0.53679(3) 0.0293 1.0000 Uani . . . . . .
C29 C 0.8593(4) 0.6789(3) 0.53296(5) 0.0331 1.0000 Uani . . . . . .
N30 N -0.0230(3) 0.4375(3) 0.26675(5) 0.0438 1.0000 Uani . . . . . .
O31 O -0.1894(4) 0.4705(4) 0.25294(6) 0.0814 1.0000 Uani . . . . . .
O32 O -0.0229(4) 0.4637(3) 0.29506(5) 0.0755 1.0000 Uani . . . . . .
O33 O 0.1335(5) 0.3915(4) 0.25447(7) 0.0942 1.0000 Uani . . . . . .
H211 H 0.1761 0.2310 0.4422 0.0326 1.0000 Uiso R . . . . .
H161 H 0.1071 0.3314 0.3957 0.0278 1.0000 Uiso R . . . . .
H202 H -0.1128 0.8201 0.4036 0.0489 1.0000 Uiso R . . . . .
H201 H -0.0676 0.7515 0.4360 0.0485 1.0000 Uiso R . . . . .
H203 H -0.2688 0.7064 0.4177 0.0481 1.0000 Uiso R . . . . .
H91 H 0.6828 0.4780 0.3484 0.0340 1.0000 Uiso R . . . . .
H92 H 0.6181 0.3499 0.3242 0.0343 1.0000 Uiso R . . . . .
H101 H 0.3718 0.6155 0.3315 0.0419 1.0000 Uiso R . . . . .
H102 H 0.3431 0.4928 0.3051 0.0424 1.0000 Uiso R . . . . .
H121 H 0.7961 0.8043 0.2994 0.0734 1.0000 Uiso R . . . . .
H123 H 0.7946 0.7004 0.3298 0.0728 1.0000 Uiso R . . . . .
H122 H 0.6113 0.8188 0.3239 0.0741 1.0000 Uiso R . . . . .
H131 H 0.5404 0.7701 0.2587 0.0849 1.0000 Uiso R . . . . .
H132 H 0.3504 0.7762 0.2822 0.0856 1.0000 Uiso R . . . . .
H133 H 0.3810 0.6337 0.2599 0.0847 1.0000 Uiso R . . . . .
H31 H 0.2961 -0.1064 0.3930 0.0425 1.0000 Uiso R . . . . .
H41 H 0.1338 -0.1744 0.3463 0.0483 1.0000 Uiso R . . . . .
H51 H 0.1160 0.0009 0.3056 0.0471 1.0000 Uiso R . . . . .
H61 H 0.2407 0.2435 0.3128 0.0418 1.0000 Uiso R . . . . .
H231 H 0.1699 0.3325 0.4920 0.0285 1.0000 Uiso R . . . . .
H241 H 0.3322 0.4535 0.5343 0.0290 1.0000 Uiso R . . . . .
H291 H 0.8826 0.7315 0.5524 0.0489 1.0000 Uiso R . . . . .
H293 H 0.9787 0.6182 0.5275 0.0491 1.0000 Uiso R . . . . .
H292 H 0.8342 0.7517 0.5168 0.0492 1.0000 Uiso R . . . . .
H261 H 0.8357 0.5481 0.4800 0.0293 1.0000 Uiso R . . . . .
H271 H 0.6714 0.4278 0.4386 0.0325 1.0000 Uiso R . . . . .
H111 H 0.6739 0.5738 0.2873 0.0518 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0338(3) 0.0269(2) 0.0306(2) 0.0043(2) -0.0047(2) 0.0001(2)
C2 0.0292(11) 0.0244(10) 0.0308(10) 0.0016(8) -0.0003(9) -0.0051(9)
C3 0.0408(14) 0.0255(11) 0.0374(12) 0.0032(9) 0.0028(10) -0.0042(10)
C4 0.0438(14) 0.0283(12) 0.0459(13) -0.0042(10) -0.0007(11) -0.0102(11)
C5 0.0426(15) 0.0385(13) 0.0377(12) -0.0090(10) -0.0054(11) -0.0097(11)
C6 0.0406(14) 0.0326(12) 0.0291(11) 0.0017(9) -0.0027(9) -0.0072(10)
C7 0.0300(12) 0.0248(10) 0.0280(10) 0.0013(8) 0.0013(9) -0.0047(9)
N8 0.0274(9) 0.0244(8) 0.0243(8) 0.0033(7) 0.0021(7) -0.0059(7)
C9 0.0250(11) 0.0318(11) 0.0261(10) 0.0047(8) 0.0031(8) -0.0048(9)
C10 0.0289(12) 0.0392(12) 0.0317(11) 0.0115(9) 0.0011(9) -0.0059(10)
N11 0.0324(10) 0.0390(10) 0.0296(9) 0.0107(8) 0.0006(8) -0.0081(9)
C12 0.0537(17) 0.0428(15) 0.0479(15) 0.0117(12) -0.0097(13) -0.0214(13)
C13 0.060(2) 0.0667(18) 0.0421(14) 0.0302(14) -0.0138(13) -0.0164(16)
C14 0.0208(10) 0.0258(10) 0.0235(9) 0.0068(8) -0.0033(8) -0.0024(8)
O15 0.0288(8) 0.0264(7) 0.0298(7) 0.0015(6) -0.0015(6) -0.0088(6)
C16 0.0212(10) 0.0254(10) 0.0239(9) 0.0026(8) 0.0003(8) -0.0050(8)
O17 0.0261(7) 0.0288(7) 0.0237(7) 0.0027(6) -0.0011(6) -0.0028(6)
C18 0.0178(9) 0.0294(10) 0.0307(10) 0.0051(8) -0.0012(8) -0.0080(9)
O19 0.0285(8) 0.0363(8) 0.0263(7) 0.0026(6) -0.0046(6) -0.0016(7)
C20 0.0283(11) 0.0303(11) 0.0370(11) 0.0001(10) -0.0003(10) -0.0036(9)
C21 0.0249(10) 0.0274(10) 0.0260(10) 0.0056(8) -0.0018(8) -0.0074(9)
C22 0.0252(10) 0.0231(10) 0.0252(9) 0.0069(8) -0.0011(8) -0.0013(8)
C23 0.0194(10) 0.0242(10) 0.0297(10) 0.0059(8) 0.0008(8) -0.0014(8)
C24 0.0217(10) 0.0253(10) 0.0250(9) 0.0037(8) 0.0029(8) 0.0014(8)
C25 0.0278(11) 0.0201(9) 0.0257(10) 0.0034(8) -0.0023(8) 0.0041(8)
C26 0.0191(10) 0.0272(10) 0.0282(10) 0.0047(8) 0.0024(8) -0.0037(8)
C27 0.0244(10) 0.0311(11) 0.0238(9) 0.0048(8) 0.0018(8) -0.0049(9)
O28 0.0277(8) 0.0322(8) 0.0280(7) -0.0019(6) -0.0014(6) -0.0050(6)
C29 0.0328(12) 0.0318(12) 0.0346(11) -0.0007(9) -0.0039(9) -0.0069(10)
N30 0.0283(11) 0.0607(14) 0.0424(11) -0.0088(10) -0.0009(9) -0.0010(11)
O31 0.0785(18) 0.100(2) 0.0661(15) -0.0233(15) -0.0266(14) 0.0124(17)
O32 0.0463(13) 0.129(2) 0.0510(12) -0.0063(13) 0.0041(10) 0.0218(15)
O33 0.0730(18) 0.115(2) 0.095(2) -0.0492(18) 0.0305(16) 0.0024(18)
_refine_ls_extinction_method
'None'
_oxford_refine_ls_scale 4.14(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 . C2 . 1.774(2) yes
S1 . C21 . 1.840(2) yes
C2 . C3 . 1.393(3) yes
C2 . C7 . 1.406(3) yes
C3 . C4 . 1.386(4) yes
C3 . H31 . 0.934 no
C4 . C5 . 1.379(4) yes
C4 . H41 . 0.943 no
C5 . C6 . 1.388(3) yes
C5 . H51 . 0.950 no
C6 . C7 . 1.388(3) yes
C6 . H61 . 0.927 no
C7 . N8 . 1.428(3) yes
N8 . C9 . 1.475(3) yes
N8 . C14 . 1.358(3) yes
C9 . C10 . 1.521(3) yes
C9 . H91 . 0.979 no
C9 . H92 . 0.969 no
C10 . N11 . 1.492(3) yes
C10 . H101 . 0.972 no
C10 . H102 . 0.966 no
N11 . C12 . 1.474(3) yes
N11 . C13 . 1.495(3) yes
N11 . H111 . 0.900 no
C12 . H121 . 0.966 no
C12 . H123 . 0.981 no
C12 . H122 . 0.971 no
C13 . H131 . 0.955 no
C13 . H132 . 0.975 no
C13 . H133 . 0.972 no
C14 . O15 . 1.228(2) yes
C14 . C16 . 1.534(3) yes
C16 . O17 . 1.442(2) yes
C16 . C21 . 1.533(3) yes
C16 . H161 . 0.981 no
O17 . C18 . 1.361(2) yes
C18 . O19 . 1.203(2) yes
C18 . C20 . 1.491(3) yes
C20 . H202 . 0.951 no
C20 . H201 . 0.958 no
C20 . H203 . 0.948 no
C21 . C22 . 1.523(3) yes
C21 . H211 . 0.989 no
C22 . C23 . 1.403(3) yes
C22 . C27 . 1.382(3) yes
C23 . C24 . 1.386(3) yes
C23 . H231 . 0.959 no
C24 . C25 . 1.385(3) yes
C24 . H241 . 0.954 no
C25 . C26 . 1.389(3) yes
C25 . O28 . 1.367(2) yes
C26 . C27 . 1.394(3) yes
C26 . H261 . 0.940 no
C27 . H271 . 0.937 no
O28 . C29 . 1.424(3) yes
C29 . H291 . 0.968 no
C29 . H293 . 0.959 no
C29 . H292 . 0.958 no
N30 . O31 . 1.250(3) yes
N30 . O32 . 1.238(3) yes
N30 . O33 . 1.200(3) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . S1 . C21 . 101.27(10) yes
S1 . C2 . C3 . 119.67(17) yes
S1 . C2 . C7 . 120.97(16) yes
C3 . C2 . C7 . 119.3(2) yes
C2 . C3 . C4 . 120.3(2) yes
C2 . C3 . H31 . 118.7 no
C4 . C3 . H31 . 120.9 no
C3 . C4 . C5 . 120.1(2) yes
C3 . C4 . H41 . 119.9 no
C5 . C4 . H41 . 120.0 no
C4 . C5 . C6 . 120.4(2) yes
C4 . C5 . H51 . 120.9 no
C6 . C5 . H51 . 118.7 no
C5 . C6 . C7 . 120.0(2) yes
C5 . C6 . H61 . 119.7 no
C7 . C6 . H61 . 120.3 no
C2 . C7 . C6 . 119.8(2) yes
C2 . C7 . N8 . 120.07(19) yes
C6 . C7 . N8 . 120.13(19) yes
C7 . N8 . C9 . 119.24(17) yes
C7 . N8 . C14 . 123.26(17) yes
C9 . N8 . C14 . 117.49(17) yes
N8 . C9 . C10 . 108.98(17) yes
N8 . C9 . H91 . 107.3 no
C10 . C9 . H91 . 111.9 no
N8 . C9 . H92 . 109.1 no
C10 . C9 . H92 . 110.0 no
H91 . C9 . H92 . 109.5 no
C9 . C10 . N11 . 113.19(18) yes
C9 . C10 . H101 . 109.5 no
N11 . C10 . H101 . 107.7 no
C9 . C10 . H102 . 109.5 no
N11 . C10 . H102 . 108.1 no
H101 . C10 . H102 . 108.8 no
C10 . N11 . C12 . 112.47(19) yes
C10 . N11 . C13 . 110.10(18) yes
C12 . N11 . C13 . 110.8(2) yes
C10 . N11 . H111 . 109.0 no
C12 . N11 . H111 . 106.5 no
C13 . N11 . H111 . 107.9 no
N11 . C12 . H121 . 109.7 no
N11 . C12 . H123 . 110.9 no
H121 . C12 . H123 . 110.0 no
N11 . C12 . H122 . 107.6 no
H121 . C12 . H122 . 109.7 no
H123 . C12 . H122 . 108.8 no
N11 . C13 . H131 . 110.3 no
N11 . C13 . H132 . 108.3 no
H131 . C13 . H132 . 109.6 no
N11 . C13 . H133 . 109.5 no
H131 . C13 . H133 . 109.7 no
H132 . C13 . H133 . 109.5 no
N8 . C14 . O15 . 122.67(18) yes
N8 . C14 . C16 . 115.97(17) yes
O15 . C14 . C16 . 121.30(19) yes
C14 . C16 . O17 . 109.48(16) yes
C14 . C16 . C21 . 113.60(17) yes
O17 . C16 . C21 . 108.68(16) yes
C14 . C16 . H161 . 108.7 no
O17 . C16 . H161 . 107.6 no
C21 . C16 . H161 . 108.6 no
C16 . O17 . C18 . 113.32(15) yes
O17 . C18 . O19 . 122.1(2) yes
O17 . C18 . C20 . 112.52(17) yes
O19 . C18 . C20 . 125.4(2) yes
C18 . C20 . H202 . 110.6 no
C18 . C20 . H201 . 110.4 no
H202 . C20 . H201 . 108.1 no
C18 . C20 . H203 . 110.1 no
H202 . C20 . H203 . 108.0 no
H201 . C20 . H203 . 109.5 no
C16 . C21 . S1 . 108.67(14) yes
C16 . C21 . C22 . 116.55(17) yes
S1 . C21 . C22 . 107.18(15) yes
C16 . C21 . H211 . 106.4 no
S1 . C21 . H211 . 108.5 no
C22 . C21 . H211 . 109.3 no
C21 . C22 . C23 . 118.97(18) yes
C21 . C22 . C27 . 122.67(19) yes
C23 . C22 . C27 . 118.34(19) yes
C22 . C23 . C24 . 120.41(19) yes
C22 . C23 . H231 . 118.6 no
C24 . C23 . H231 . 121.0 no
C23 . C24 . C25 . 120.32(19) yes
C23 . C24 . H241 . 119.4 no
C25 . C24 . H241 . 120.3 no
C24 . C25 . C26 . 120.12(19) yes
C24 . C25 . O28 . 116.06(18) yes
C26 . C25 . O28 . 123.8(2) yes
C25 . C26 . C27 . 119.0(2) yes
C25 . C26 . H261 . 121.3 no
C27 . C26 . H261 . 119.7 no
C26 . C27 . C22 . 121.75(19) yes
C26 . C27 . H271 . 119.6 no
C22 . C27 . H271 . 118.6 no
C25 . O28 . C29 . 118.11(17) yes
O28 . C29 . H291 . 107.3 no
O28 . C29 . H293 . 110.9 no
H291 . C29 . H293 . 110.8 no
O28 . C29 . H292 . 109.2 no
H291 . C29 . H292 . 109.3 no
H293 . C29 . H292 . 109.4 no
O31 . N30 . O32 . 115.0(2) yes
O31 . N30 . O33 . 125.2(3) yes
O32 . N30 . O33 . 119.6(3) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C20 . H201 . O28 3_466 143 0.96 2.42 3.230(3) yes
C20 . H203 . O15 1_455 141 0.95 2.39 3.186(3) yes
C9 . H91 . O19 1_655 174 0.98 2.42 3.392(3) yes
C10 . H102 . O32 . 144 0.97 2.39 3.221(3) yes
C12 . H121 . O33 4_655 149 0.97 2.48 3.346(3) yes
C12 . H123 . O19 1_655 176 0.98 2.52 3.496(3) yes
C13 . H131 . O33 4_655 153 0.95 2.41 3.283(3) yes
C5 . H51 . O31 4_545 144 0.95 2.57 3.386(3) yes
N11 . H111 . N30 1_655 168 0.90 2.44 3.327(3) yes
N11 . H111 . O31 1_655 157 0.90 1.94 2.793(3) yes
N11 . H111 . O32 1_655 141 0.90 2.19 2.943(3) yes
_iucr_refine_instructions_details
;
#
# Punched on 15/06/18 at 12:43:21
#
#LIST 12
BLOCK SCALE X'S U'S
CONT ENANTIO
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S)
RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S)
RIDE N ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S) H ( 123,X'S) H ( 122,X'S)
RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S) H ( 133,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 20,X'S) H ( 202,X'S) H ( 201,X'S) H ( 203,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 26,X'S) H ( 261,X'S)
RIDE C ( 27,X'S) H ( 271,X'S)
RIDE C ( 29,X'S) H ( 291,X'S) H ( 293,X'S) H ( 292,X'S)
END
#
# Punched on 15/06/18 at 12:43:21
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
data_Diltiazemphosphatesesquihydrate
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 8.79290(10)
_cell_length_b 12.66450(10)
_cell_length_c 23.7867(2)
_cell_angle_alpha 82.3345(7)
_cell_angle_beta 81.4117(7)
_cell_angle_gamma 89.9824(7)
_cell_volume 2595.21(4)
_symmetry_cell_setting 'triclinic'
_symmetry_space_group_name_H-M 'P 1 '
_symmetry_space_group_name_Hall ?
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687
0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424
0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975
1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536
1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260
1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C22 H26 N2 O7 P1 S1
# Dc = 1.26 Fooo = 1036.00 Mu = 20.53 M = 493.50
# Found Formula = C22 H32 N2 O9.50 P1 S1
# Dc = 1.38 FOOO = 1140.00 Mu = 21.71 M = 539.55
_chemical_formula_sum 'C44 H64 N4 O19 P2 S2'
_chemical_formula_moiety '2(C22 H27 N2 O4 S), 2(H2O4 P), 3(H2 O)'
_chemical_compound_source ?
_chemical_formula_weight 1079.05
_cell_measurement_reflns_used 109761
_cell_measurement_theta_min 4
_cell_measurement_theta_max 79
_cell_measurement_temperature 160
_exptl_crystal_description 'lath'
_exptl_crystal_colour 'colorless'
_exptl_crystal_size_min 0.019
_exptl_crystal_size_mid 0.070
_exptl_crystal_size_max 0.167
_exptl_crystal_density_diffrn 1.381
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1140
_exptl_absorpt_coefficient_mu 2.171
# Sheldrick geometric approximatio 0.86 0.96
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'CrysAlisPro, (Agilent, 2011)'
_exptl_absorpt_correction_T_min 0.62
_exptl_absorpt_correction_T_max 0.96
_diffrn_measurement_device_type 'Oxford Diffraction SuperNova'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'graphite'
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54180
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement 'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction 'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 160
_diffrn_reflns_number 264132
_reflns_number_total 19821
_diffrn_reflns_av_R_equivalents 0.066
# Number of reflections without Friedels Law is 19821
# Number of reflections with Friedels Law is 10169
# Theoretical number of reflections is about 10225
_diffrn_reflns_theta_min 3.522
_diffrn_reflns_theta_max 72.109
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 72.109
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 29
_reflns_limit_h_min -10
_reflns_limit_h_max 10
_reflns_limit_k_min -15
_reflns_limit_k_max 15
_reflns_limit_l_min -29
_reflns_limit_l_max 29
_oxford_diffrn_Wilson_B_factor 2.51
_oxford_diffrn_Wilson_scale 0.38
_atom_sites_solution_primary Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.46
_refine_diff_density_max 1.49
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns 19783
_refine_ls_number_restraints 66
_refine_ls_number_parameters 1376
_oxford_refine_ls_R_factor_ref 0.0519
_refine_ls_wR_factor_ref 0.1283
_refine_ls_goodness_of_fit_ref 0.9968
_refine_ls_shift/su_max 0.0009634
_refine_ls_shift/su_mean 0.0000379
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 19783
_refine_ls_R_factor_all 0.0519
_refine_ls_wR_factor_all 0.1283
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 18568
_refine_ls_R_factor_gt 0.0488
_refine_ls_wR_factor_gt 0.1259
_refine_ls_abs_structure_Flack 0.020(11)
_refine_ls_abs_structure_details 'Flack (1983), 9652 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration 'ad'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 1.40P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Agilent (2011). CrysAlisPro.
Oxford Diffraction, (2010). Supernova User Manual.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
S1 S 0.49980(10) 0.49990(8) 0.49983(4) 0.0335 1.0000 Uani . . . . . .
C2 C 0.4695(4) 0.5780(3) 0.43488(13) 0.0298 1.0000 Uani . . . . . .
C3 C 0.3219(4) 0.6122(3) 0.42825(16) 0.0366 1.0000 Uani . . . . . .
C4 C 0.2944(4) 0.6692(3) 0.37685(16) 0.0405 1.0000 Uani . . . . . .
C5 C 0.4141(5) 0.6922(3) 0.33212(16) 0.0430 1.0000 Uani . . . . . .
C6 C 0.5620(4) 0.6596(3) 0.33822(14) 0.0389 1.0000 Uani . . . . . .
C7 C 0.5901(4) 0.6012(3) 0.38948(13) 0.0299 1.0000 Uani . . . . . .
N8 N 0.7419(3) 0.5642(2) 0.39478(10) 0.0284 1.0000 Uani . . . . . .
C9 C 0.8195(4) 0.5022(3) 0.35076(13) 0.0282 1.0000 Uani . . . . . .
C10 C 0.9399(4) 0.5719(3) 0.31008(14) 0.0327 1.0000 Uani D . . . . .
N11 N 1.0375(3) 0.5082(2) 0.27060(11) 0.0288 1.0000 Uani D . . . . .
C12 C 1.1492(4) 0.4417(3) 0.29985(15) 0.0385 1.0000 Uani D . . . . .
C13 C 1.1160(5) 0.5789(3) 0.21937(15) 0.0452 1.0000 Uani D . . . . .
C14 C 0.8136(4) 0.5761(2) 0.44022(12) 0.0270 1.0000 Uani . . . . . .
O15 O 0.9372(3) 0.53625(19) 0.44662(9) 0.0312 1.0000 Uani . . . . . .
C16 C 0.7350(4) 0.6492(3) 0.48176(13) 0.0264 1.0000 Uani . . . . . .
O17 O 0.8502(3) 0.69849(18) 0.50760(9) 0.0297 1.0000 Uani . . . . . .
C18 C 0.9524(4) 0.7624(3) 0.46931(14) 0.0312 1.0000 Uani . . . . . .
O19 O 0.9422(3) 0.7761(2) 0.41857(10) 0.0370 1.0000 Uani . . . . . .
C20 C 1.0742(4) 0.8102(3) 0.49525(16) 0.0370 1.0000 Uani . . . . . .
C21 C 0.6172(4) 0.5912(3) 0.53066(13) 0.0299 1.0000 Uani . . . . . .
C22 C 0.6825(4) 0.5279(3) 0.57968(12) 0.0270 1.0000 Uani . . . . . .
C23 C 0.7528(4) 0.4317(3) 0.57471(13) 0.0299 1.0000 Uani . . . . . .
C24 C 0.8115(4) 0.3732(3) 0.62055(13) 0.0268 1.0000 Uani . . . . . .
C25 C 0.7985(3) 0.4129(3) 0.67268(12) 0.0238 1.0000 Uani . . . . . .
C26 C 0.7256(3) 0.5095(3) 0.67884(13) 0.0258 1.0000 Uani . . . . . .
C27 C 0.6682(4) 0.5660(3) 0.63299(13) 0.0279 1.0000 Uani . . . . . .
O28 O 0.8527(3) 0.36327(19) 0.72006(9) 0.0311 1.0000 Uani . . . . . .
C29 C 0.9507(4) 0.2737(3) 0.71292(15) 0.0349 1.0000 Uani . . . . . .
S31 S 0.51570(10) 0.01691(8) 0.49890(4) 0.0333 1.0000 Uani . . . . . .
H31 H 0.2428 0.5974 0.4585 0.0448 1.0000 Uiso R . . . . .
C32 C 0.4951(4) 0.0977(3) 0.43376(13) 0.0297 1.0000 Uani . . . . . .
C33 C 0.3519(4) 0.1387(3) 0.42525(15) 0.0357 1.0000 Uani . . . . . .
C34 C 0.3330(4) 0.1986(3) 0.37349(16) 0.0381 1.0000 Uani . . . . . .
C35 C 0.4569(4) 0.2191(3) 0.32994(15) 0.0404 1.0000 Uani . . . . . .
C36 C 0.5996(4) 0.1783(3) 0.33793(14) 0.0347 1.0000 Uani . . . . . .
C37 C 0.6192(4) 0.1181(3) 0.38908(13) 0.0282 1.0000 Uani . . . . . .
N38 N 0.7674(3) 0.0758(2) 0.39640(10) 0.0261 1.0000 Uani . . . . . .
C39 C 0.8448(4) 0.0119(3) 0.35335(12) 0.0265 1.0000 Uani . . . . . .
C40 C 0.9846(4) 0.0743(3) 0.31856(13) 0.0272 1.0000 Uani D . . . . .
N41 N 1.0839(3) 0.0063(2) 0.28162(10) 0.0238 1.0000 Uani D . . . . .
H41 H 0.1958 0.6923 0.3717 0.0481 1.0000 Uiso R . . . . .
C42 C 1.1884(4) 0.0737(3) 0.23586(14) 0.0313 1.0000 Uani D . . . . .
C43 C 1.1757(4) -0.0696(3) 0.31507(16) 0.0370 1.0000 Uani D . . . . .
C44 C 0.8358(4) 0.0855(2) 0.44275(12) 0.0252 1.0000 Uani . . . . . .
O45 O 0.9556(3) 0.04144(18) 0.45129(9) 0.0273 1.0000 Uani . . . . . .
C46 C 0.7571(3) 0.1601(3) 0.48327(12) 0.0254 1.0000 Uani . . . . . .
O47 O 0.8721(3) 0.20964(18) 0.50916(9) 0.0284 1.0000 Uani . . . . . .
C48 C 0.9762(4) 0.2725(3) 0.47017(14) 0.0286 1.0000 Uani . . . . . .
O49 O 0.9688(3) 0.28204(19) 0.41945(10) 0.0330 1.0000 Uani . . . . . .
C50 C 1.0920(4) 0.3242(3) 0.49663(16) 0.0370 1.0000 Uani . . . . . .
C51 C 0.6356(4) 0.1040(3) 0.53149(13) 0.0288 1.0000 Uani . . . . . .
H51 H 0.3977 0.7305 0.2966 0.0512 1.0000 Uiso R . . . . .
C52 C 0.6953(4) 0.0364(3) 0.58077(13) 0.0259 1.0000 Uani . . . . . .
C53 C 0.7597(4) -0.0619(3) 0.57533(13) 0.0289 1.0000 Uani . . . . . .
C54 C 0.8120(4) -0.1244(3) 0.62147(13) 0.0289 1.0000 Uani . . . . . .
C55 C 0.7982(3) -0.0861(2) 0.67425(12) 0.0231 1.0000 Uani . . . . . .
C56 C 0.7290(3) 0.0112(3) 0.68077(12) 0.0243 1.0000 Uani . . . . . .
C57 C 0.6785(3) 0.0717(3) 0.63430(13) 0.0259 1.0000 Uani . . . . . .
O58 O 0.8458(3) -0.13943(19) 0.72219(9) 0.0300 1.0000 Uani . . . . . .
C59 C 0.9404(4) -0.2308(3) 0.71554(14) 0.0346 1.0000 Uani . . . . . .
S61 S 0.56384(10) 0.68940(8) 0.80859(4) 0.0335 1.0000 Uani . . . . . .
H61 H 0.6435 0.6774 0.3076 0.0467 1.0000 Uiso R . . . . .
C62 C 0.5851(4) 0.7379(3) 0.87385(13) 0.0303 1.0000 Uani . . . . . .
C63 C 0.7268(4) 0.7751(3) 0.88228(15) 0.0355 1.0000 Uani . . . . . .
C64 C 0.7458(4) 0.8094(3) 0.93379(16) 0.0388 1.0000 Uani . . . . . .
C65 C 0.6221(5) 0.8078(3) 0.97703(15) 0.0416 1.0000 Uani . . . . . .
C66 C 0.4790(4) 0.7714(3) 0.96931(14) 0.0352 1.0000 Uani . . . . . .
C67 C 0.4587(4) 0.7362(3) 0.91831(13) 0.0274 1.0000 Uani . . . . . .
N68 N 0.3120(3) 0.6979(2) 0.91108(10) 0.0257 1.0000 Uani . . . . . .
C69 C 0.2343(4) 0.6124(3) 0.95382(13) 0.0263 1.0000 Uani . . . . . .
C70 C 0.0933(4) 0.6574(3) 0.98865(13) 0.0278 1.0000 Uani D . . . . .
N71 N -0.0052(3) 0.5704(2) 1.02538(10) 0.0246 1.0000 Uani D . . . . .
C72 C -0.1095(4) 0.6149(3) 1.07134(14) 0.0317 1.0000 Uani D . . . . .
C73 C -0.0968(4) 0.5117(3) 0.99206(16) 0.0380 1.0000 Uani D . . . . .
C74 C 0.2436(4) 0.7303(2) 0.86420(12) 0.0243 1.0000 Uani . . . . . .
O75 O 0.1245(3) 0.69089(18) 0.85576(9) 0.0269 1.0000 Uani . . . . . .
C76 C 0.3226(4) 0.8252(3) 0.82381(12) 0.0265 1.0000 Uani . . . . . .
O77 O 0.2081(3) 0.88790(19) 0.79774(9) 0.0298 1.0000 Uani . . . . . .
C78 C 0.1035(4) 0.9306(3) 0.83677(14) 0.0292 1.0000 Uani . . . . . .
O79 O 0.1100(3) 0.9154(2) 0.88740(10) 0.0334 1.0000 Uani . . . . . .
C80 C -0.0125(4) 0.9965(3) 0.80975(16) 0.0381 1.0000 Uani . . . . . .
C81 C 0.4446(4) 0.7931(3) 0.77574(12) 0.0279 1.0000 Uani . . . . . .
C82 C 0.3852(4) 0.7494(3) 0.72657(13) 0.0263 1.0000 Uani . . . . . .
C83 C 0.3196(4) 0.6494(3) 0.73214(13) 0.0310 1.0000 Uani . . . . . .
C84 C 0.2658(4) 0.6107(3) 0.68638(13) 0.0277 1.0000 Uani . . . . . .
C85 C 0.2801(3) 0.6747(3) 0.63348(12) 0.0241 1.0000 Uani . . . . . .
C86 C 0.3498(3) 0.7748(3) 0.62667(12) 0.0240 1.0000 Uani . . . . . .
C87 C 0.4025(4) 0.8118(3) 0.67277(13) 0.0261 1.0000 Uani . . . . . .
O88 O 0.2302(3) 0.64499(19) 0.58598(9) 0.0311 1.0000 Uani . . . . . .
C89 C 0.1310(4) 0.5522(3) 0.59371(15) 0.0360 1.0000 Uani . . . . . .
S91 S 0.57882(10) 0.17322(8) 0.80724(4) 0.0335 1.0000 Uani . . . . . .
H92 H 0.8663 0.4408 0.3698 0.0338 1.0000 Uiso R . . . . .
C92 C 0.6101(4) 0.2185(3) 0.87220(13) 0.0307 1.0000 Uani . . . . . .
H91 H 0.7427 0.4783 0.3300 0.0339 1.0000 Uiso R . . . . .
C93 C 0.7570(4) 0.2496(3) 0.87864(15) 0.0364 1.0000 Uani . . . . . .
C94 C 0.7837(4) 0.2807(3) 0.93031(16) 0.0397 1.0000 Uani . . . . . .
C95 C 0.6649(5) 0.2812(3) 0.97501(16) 0.0425 1.0000 Uani . . . . . .
C96 C 0.5173(4) 0.2515(3) 0.96875(15) 0.0392 1.0000 Uani . . . . . .
C97 C 0.4883(4) 0.2194(3) 0.91787(13) 0.0292 1.0000 Uani . . . . . .
N98 N 0.3373(3) 0.1847(2) 0.91256(10) 0.0277 1.0000 Uani . . . . . .
C99 C 0.2601(4) 0.1010(3) 0.95650(13) 0.0289 1.0000 Uani . . . . . .
C100 C 0.1378(4) 0.1499(3) 0.99720(14) 0.0319 1.0000 Uani D . . . . .
N101 N 0.0413(3) 0.0664(2) 1.03647(11) 0.0284 1.0000 Uani D . . . . .
H102 H 0.8917 0.6280 0.2873 0.0387 1.0000 Uiso R . . . . .
C102 C -0.0696(4) 0.0147(3) 1.00745(16) 0.0392 1.0000 Uani D . . . . .
H101 H 1.0050 0.6062 0.3313 0.0389 1.0000 Uiso R . . . . .
C103 C -0.0379(5) 0.1117(3) 1.08771(15) 0.0438 1.0000 Uani D . . . . .
C104 C 0.2655(4) 0.2190(3) 0.86705(13) 0.0267 1.0000 Uani . . . . . .
O105 O 0.1414(3) 0.18280(19) 0.86051(10) 0.0307 1.0000 Uani . . . . . .
C106 C 0.3430(4) 0.3133(3) 0.82545(13) 0.0269 1.0000 Uani . . . . . .
O107 O 0.2274(3) 0.37559(18) 0.79966(9) 0.0298 1.0000 Uani . . . . . .
C108 C 0.1266(4) 0.4204(3) 0.83847(14) 0.0301 1.0000 Uani . . . . . .
O109 O 0.1370(3) 0.4084(2) 0.88870(10) 0.0356 1.0000 Uani . . . . . .
C110 C 0.0041(4) 0.4813(3) 0.81227(15) 0.0360 1.0000 Uani . . . . . .
C111 C 0.4607(4) 0.2797(3) 0.77640(13) 0.0286 1.0000 Uani . . . . . .
H111 H 0.974(2) 0.4636(17) 0.2588(9) 0.043(2) 1.0000 Uiso D . . . . .
C112 C 0.3959(4) 0.2409(3) 0.72739(13) 0.0274 1.0000 Uani . . . . . .
C113 C 0.3269(4) 0.1415(3) 0.73213(13) 0.0294 1.0000 Uani . . . . . .
C114 C 0.2700(4) 0.1063(3) 0.68610(13) 0.0267 1.0000 Uani . . . . . .
C115 C 0.2827(3) 0.1726(2) 0.63374(12) 0.0228 1.0000 Uani . . . . . .
C116 C 0.3526(4) 0.2717(3) 0.62799(13) 0.0254 1.0000 Uani . . . . . .
C117 C 0.4091(3) 0.3059(3) 0.67411(13) 0.0263 1.0000 Uani . . . . . .
O118 O 0.2302(3) 0.14595(19) 0.58626(9) 0.0306 1.0000 Uani . . . . . .
C119 C 0.1360(4) 0.0515(3) 0.59215(14) 0.0336 1.0000 Uani . . . . . .
P121 P 0.57908(10) 0.74840(7) 0.15508(4) 0.0255 1.0000 Uani . . . . . .
H122 H 1.0980 0.4026 0.3343 0.0573 1.0000 Uiso R . . . . .
O122 O 0.7028(3) 0.8273(2) 0.11679(11) 0.0404 1.0000 Uani D . . . . .
H123 H 1.1980 0.3942 0.2748 0.0576 1.0000 Uiso R . . . . .
O123 O 0.6775(3) 0.6687(2) 0.18990(11) 0.0371 1.0000 Uani D . . . . .
H121 H 1.2250 0.4876 0.3086 0.0584 1.0000 Uiso R . . . . .
O124 O 0.4776(3) 0.8105(2) 0.19493(11) 0.0379 1.0000 Uani . . . . . .
O125 O 0.4924(3) 0.6933(2) 0.11721(10) 0.0324 1.0000 Uani . . . . . .
P126 P 0.49998(10) 1.24910(7) 0.15205(4) 0.0250 1.0000 Uani . . . . . .
O127 O 0.6010(3) 1.3315(2) 0.11205(11) 0.0385 1.0000 Uani . . . . . .
O128 O 0.5864(3) 1.17454(19) 0.19009(10) 0.0316 1.0000 Uani . . . . . .
O129 O 0.3768(3) 1.3090(2) 0.19039(11) 0.0391 1.0000 Uani D . . . . .
O130 O 0.4013(3) 1.1870(2) 0.11736(11) 0.0347 1.0000 Uani D . . . . .
P131 P 1.15434(9) 0.83729(7) 0.12313(4) 0.0249 1.0000 Uani . . . . . .
H133 H 1.0429 0.6233 0.2019 0.0678 1.0000 Uiso R . . . . .
O132 O 1.2107(3) 0.72581(19) 0.10658(10) 0.0292 1.0000 Uani D . . . . .
H131 H 1.1714 0.5375 0.1919 0.0677 1.0000 Uiso R . . . . .
O133 O 1.2047(3) 0.8473(2) 0.18246(10) 0.0353 1.0000 Uani D . . . . .
H132 H 1.1899 0.6233 0.2316 0.0674 1.0000 Uiso R . . . . .
O134 O 1.2289(3) 0.9241(2) 0.07731(11) 0.0362 1.0000 Uani . . . . . .
O135 O 0.9819(3) 0.8368(2) 0.13180(10) 0.0335 1.0000 Uani . . . . . .
P136 P 0.92475(9) 0.32205(7) 0.18405(4) 0.0249 1.0000 Uani . . . . . .
O137 O 1.0973(3) 0.3262(2) 0.17521(10) 0.0336 1.0000 Uani . . . . . .
O138 O 0.8682(3) 0.20264(19) 0.20065(10) 0.0296 1.0000 Uani D . . . . .
O139 O 0.8495(3) 0.3856(2) 0.23003(11) 0.0357 1.0000 Uani . . . . . .
O140 O 0.8738(3) 0.3621(2) 0.12440(10) 0.0351 1.0000 Uani D . . . . .
O141 O 0.8803(3) 0.8830(2) 0.24438(11) 0.0408 1.0000 Uani D . . . . .
O142 O 1.1990(3) 1.4289(2) 0.06287(11) 0.0412 1.0000 Uani D . . . . .
O143 O 0.5719(3) 0.4767(2) 0.22903(13) 0.0382 1.0000 Uani D . . . . .
O144 O 0.5911(3) -0.0327(2) 0.24859(12) 0.0356 1.0000 Uani D . . . . .
O145 O 0.5065(3) 1.0144(2) 0.07821(13) 0.0372 1.0000 Uani D . . . . .
O146 O 0.4879(3) 0.5150(2) 0.05834(12) 0.0365 1.0000 Uani D . . . . .
H161 H 0.6834 0.7045 0.4592 0.0318 1.0000 Uiso R . . . . .
H203 H 1.0582 0.8839 0.4965 0.0570 1.0000 Uiso R . . . . .
H201 H 1.0744 0.7775 0.5336 0.0567 1.0000 Uiso R . . . . .
H202 H 1.1727 0.8046 0.4737 0.0558 1.0000 Uiso R . . . . .
H211 H 0.5532 0.6462 0.5456 0.0364 1.0000 Uiso R . . . . .
H231 H 0.7607 0.4044 0.5394 0.0353 1.0000 Uiso R . . . . .
H241 H 0.8557 0.3075 0.6167 0.0315 1.0000 Uiso R . . . . .
H261 H 0.7154 0.5355 0.7140 0.0310 1.0000 Uiso R . . . . .
H271 H 0.6194 0.6301 0.6375 0.0340 1.0000 Uiso R . . . . .
H293 H 0.9890 0.2539 0.7478 0.0518 1.0000 Uiso R . . . . .
H291 H 1.0342 0.2939 0.6821 0.0514 1.0000 Uiso R . . . . .
H292 H 0.8935 0.2168 0.7037 0.0525 1.0000 Uiso R . . . . .
H331 H 0.2690 0.1243 0.4553 0.0436 1.0000 Uiso R . . . . .
H341 H 0.2361 0.2263 0.3685 0.0459 1.0000 Uiso R . . . . .
H351 H 0.4456 0.2598 0.2947 0.0486 1.0000 Uiso R . . . . .
H361 H 0.6823 0.1911 0.3087 0.0414 1.0000 Uiso R . . . . .
H391 H 0.8751 -0.0545 0.3717 0.0313 1.0000 Uiso R . . . . .
H392 H 0.7711 -0.0035 0.3290 0.0319 1.0000 Uiso R . . . . .
H401 H 0.9498 0.1323 0.2937 0.0325 1.0000 Uiso R . . . . .
H402 H 1.0464 0.1010 0.3448 0.0330 1.0000 Uiso R . . . . .
H411 H 1.021(2) -0.0294(17) 0.2648(9) 0.035(2) 1.0000 Uiso D . . . . .
H423 H 1.1239 0.1158 0.2119 0.0459 1.0000 Uiso R . . . . .
H421 H 1.2519 0.0256 0.2140 0.0463 1.0000 Uiso R . . . . .
H422 H 1.2547 0.1192 0.2523 0.0476 1.0000 Uiso R . . . . .
H431 H 1.1092 -0.1130 0.3456 0.0557 1.0000 Uiso R . . . . .
H433 H 1.2280 -0.1148 0.2895 0.0559 1.0000 Uiso R . . . . .
H432 H 1.2505 -0.0298 0.3302 0.0567 1.0000 Uiso R . . . . .
H461 H 0.7079 0.2156 0.4614 0.0306 1.0000 Uiso R . . . . .
H501 H 1.0581 0.3916 0.5062 0.0566 1.0000 Uiso R . . . . .
H503 H 1.1851 0.3338 0.4709 0.0563 1.0000 Uiso R . . . . .
H502 H 1.1082 0.2805 0.5306 0.0567 1.0000 Uiso R . . . . .
H511 H 0.5715 0.1617 0.5458 0.0341 1.0000 Uiso R . . . . .
H531 H 0.7687 -0.0884 0.5402 0.0342 1.0000 Uiso R . . . . .
H541 H 0.8526 -0.1911 0.6174 0.0348 1.0000 Uiso R . . . . .
H561 H 0.7188 0.0363 0.7164 0.0288 1.0000 Uiso R . . . . .
H571 H 0.6328 0.1366 0.6392 0.0310 1.0000 Uiso R . . . . .
H591 H 0.8829 -0.2863 0.7036 0.0517 1.0000 Uiso R . . . . .
H593 H 0.9699 -0.2553 0.7516 0.0513 1.0000 Uiso R . . . . .
H592 H 1.0294 -0.2118 0.6876 0.0517 1.0000 Uiso R . . . . .
H631 H 0.8095 0.7765 0.8532 0.0436 1.0000 Uiso R . . . . .
H641 H 0.8432 0.8324 0.9383 0.0470 1.0000 Uiso R . . . . .
H651 H 0.6336 0.8314 1.0120 0.0494 1.0000 Uiso R . . . . .
H661 H 0.3966 0.7697 0.9984 0.0423 1.0000 Uiso R . . . . .
H692 H 0.3078 0.5856 0.9783 0.0319 1.0000 Uiso R . . . . .
H691 H 0.2054 0.5556 0.9349 0.0309 1.0000 Uiso R . . . . .
H702 H 0.0330 0.6974 0.9614 0.0337 1.0000 Uiso R . . . . .
H701 H 0.1288 0.7035 1.0135 0.0329 1.0000 Uiso R . . . . .
H711 H 0.058(2) 0.5266(16) 1.0421(9) 0.036(2) 1.0000 Uiso D . . . . .
H721 H -0.0446 0.6492 1.0934 0.0473 1.0000 Uiso R . . . . .
H723 H -0.1816 0.6648 1.0554 0.0482 1.0000 Uiso R . . . . .
H722 H -0.1667 0.5561 1.0961 0.0477 1.0000 Uiso R . . . . .
H732 H -0.1486 0.4520 1.0176 0.0566 1.0000 Uiso R . . . . .
H731 H -0.0292 0.4849 0.9611 0.0566 1.0000 Uiso R . . . . .
H733 H -0.1727 0.5583 0.9776 0.0576 1.0000 Uiso R . . . . .
H761 H 0.3727 0.8707 0.8455 0.0329 1.0000 Uiso R . . . . .
H802 H -0.1016 0.9969 0.8371 0.0570 1.0000 Uiso R . . . . .
H801 H -0.0368 0.9677 0.7773 0.0577 1.0000 Uiso R . . . . .
H803 H 0.0260 1.0679 0.7980 0.0574 1.0000 Uiso R . . . . .
H811 H 0.5076 0.8565 0.7612 0.0340 1.0000 Uiso R . . . . .
H831 H 0.3122 0.6051 0.7672 0.0364 1.0000 Uiso R . . . . .
H841 H 0.2223 0.5429 0.6912 0.0328 1.0000 Uiso R . . . . .
H861 H 0.3626 0.8168 0.5910 0.0298 1.0000 Uiso R . . . . .
H871 H 0.4492 0.8793 0.6675 0.0309 1.0000 Uiso R . . . . .
H892 H 0.0968 0.5467 0.5582 0.0536 1.0000 Uiso R . . . . .
H891 H 0.0440 0.5593 0.6226 0.0538 1.0000 Uiso R . . . . .
H893 H 0.1869 0.4898 0.6051 0.0544 1.0000 Uiso R . . . . .
H931 H 0.8378 0.2505 0.8479 0.0446 1.0000 Uiso R . . . . .
H941 H 0.8819 0.3022 0.9358 0.0475 1.0000 Uiso R . . . . .
H951 H 0.6824 0.3027 1.0104 0.0503 1.0000 Uiso R . . . . .
H961 H 0.4367 0.2528 0.9999 0.0465 1.0000 Uiso R . . . . .
H991 H 0.3385 0.0668 0.9772 0.0348 1.0000 Uiso R . . . . .
H992 H 0.2120 0.0485 0.9382 0.0348 1.0000 Uiso R . . . . .
H1001 H 0.0702 0.1933 0.9759 0.0382 1.0000 Uiso R . . . . .
H1002 H 0.1859 0.1959 1.0198 0.0375 1.0000 Uiso R . . . . .
H1011 H 0.105(2) 0.0168(16) 1.0485(9) 0.043(2) 1.0000 Uiso D . . . . .
H1022 H -0.1200 -0.0443 1.0325 0.0584 1.0000 Uiso R . . . . .
H1021 H -0.1451 0.0656 0.9985 0.0594 1.0000 Uiso R . . . . .
H1023 H -0.0180 -0.0090 0.9732 0.0587 1.0000 Uiso R . . . . .
H1032 H -0.1002 0.0588 1.1131 0.0659 1.0000 Uiso R . . . . .
H1033 H -0.1030 0.1678 1.0753 0.0653 1.0000 Uiso R . . . . .
H1031 H 0.0363 0.1401 1.1073 0.0659 1.0000 Uiso R . . . . .
H1061 H 0.3954 0.3580 0.8475 0.0318 1.0000 Uiso R . . . . .
H1102 H -0.0044 0.4593 0.7767 0.0544 1.0000 Uiso R . . . . .
H1103 H -0.0935 0.4738 0.8355 0.0538 1.0000 Uiso R . . . . .
H1101 H 0.0310 0.5545 0.8050 0.0552 1.0000 Uiso R . . . . .
H1111 H 0.5244 0.3430 0.7613 0.0337 1.0000 Uiso R . . . . .
H1131 H 0.3194 0.0963 0.7671 0.0349 1.0000 Uiso R . . . . .
H1141 H 0.2268 0.0394 0.6892 0.0318 1.0000 Uiso R . . . . .
H1161 H 0.3619 0.3159 0.5928 0.0307 1.0000 Uiso R . . . . .
H1171 H 0.4569 0.3725 0.6695 0.0322 1.0000 Uiso R . . . . .
H1192 H 0.1956 -0.0090 0.6011 0.0509 1.0000 Uiso R . . . . .
H1193 H 0.0998 0.0472 0.5574 0.0506 1.0000 Uiso R . . . . .
H1191 H 0.0523 0.0532 0.6227 0.0505 1.0000 Uiso R . . . . .
H1221 H 0.796(3) 0.828(4) 0.122(2) 0.060(2) 1.0000 Uiso D . . . . .
H1231 H 0.627(5) 0.613(2) 0.201(2) 0.056(2) 1.0000 Uiso D . . . . .
H1291 H 0.287(3) 1.312(4) 0.183(2) 0.059(2) 1.0000 Uiso D . . . . .
H1301 H 0.452(5) 1.139(3) 0.1040(19) 0.053(2) 1.0000 Uiso D . . . . .
H1321 H 1.305(2) 0.714(4) 0.1081(18) 0.044(2) 1.0000 Uiso D . . . . .
H1331 H 1.293(3) 0.820(4) 0.187(2) 0.053(2) 1.0000 Uiso D . . . . .
H1381 H 0.776(2) 0.192(4) 0.1981(18) 0.044(2) 1.0000 Uiso D . . . . .
H1401 H 0.780(3) 0.342(4) 0.121(2) 0.053(2) 1.0000 Uiso D . . . . .
H1412 H 0.790(3) 0.900(4) 0.2454(17) 0.062(2) 1.0000 Uiso D . . . . .
H1411 H 0.904(5) 0.856(4) 0.2112(13) 0.061(2) 1.0000 Uiso D . . . . .
H1422 H 1.172(5) 1.391(4) 0.0971(12) 0.062(2) 1.0000 Uiso D . . . . .
H1421 H 1.290(3) 1.445(4) 0.0616(17) 0.062(2) 1.0000 Uiso D . . . . .
H1432 H 0.645(4) 0.445(4) 0.238(2) 0.057(2) 1.0000 Uiso D . . . . .
H1431 H 0.519(5) 0.446(4) 0.211(2) 0.057(2) 1.0000 Uiso D . . . . .
H1442 H 0.589(6) 0.020(3) 0.2244(17) 0.054(2) 1.0000 Uiso D . . . . .
H1441 H 0.559(6) -0.070(3) 0.2285(18) 0.054(2) 1.0000 Uiso D . . . . .
H1452 H 0.441(4) 0.993(4) 0.062(2) 0.056(2) 1.0000 Uiso D . . . . .
H1451 H 0.565(5) 0.973(3) 0.0928(19) 0.056(2) 1.0000 Uiso D . . . . .
H1462 H 0.492(6) 0.560(3) 0.0800(18) 0.055(2) 1.0000 Uiso D . . . . .
H1461 H 0.525(6) 0.478(4) 0.0817(17) 0.055(2) 1.0000 Uiso D . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0310(4) 0.0384(5) 0.0281(4) 0.0033(3) -0.0019(3) 0.0009(4)
C2 0.0313(17) 0.0310(17) 0.0262(15) -0.0022(12) -0.0036(12) 0.0049(14)
C3 0.0273(17) 0.042(2) 0.0406(18) -0.0078(15) -0.0030(14) 0.0082(15)
C4 0.0356(18) 0.045(2) 0.0441(19) -0.0118(16) -0.0112(15) 0.0173(17)
C5 0.048(2) 0.049(2) 0.0339(18) -0.0046(16) -0.0132(15) 0.0208(19)
C6 0.0408(19) 0.047(2) 0.0269(16) -0.0020(14) -0.0023(14) 0.0140(17)
C7 0.0312(16) 0.0354(18) 0.0227(14) -0.0054(12) -0.0014(12) 0.0131(14)
N8 0.0294(14) 0.0317(15) 0.0218(12) -0.0024(10) 0.0020(10) 0.0115(12)
C9 0.0299(16) 0.0269(16) 0.0267(14) -0.0064(12) 0.0016(12) 0.0063(13)
C10 0.0387(18) 0.0271(17) 0.0289(16) -0.0040(13) 0.0061(13) 0.0070(15)
N11 0.0352(14) 0.0225(13) 0.0256(13) -0.0030(10) 0.0048(11) -0.0001(12)
C12 0.0330(18) 0.043(2) 0.0380(18) -0.0083(15) 0.0001(14) 0.0087(16)
C13 0.058(2) 0.038(2) 0.0319(18) 0.0009(15) 0.0141(17) -0.0097(18)
C14 0.0331(16) 0.0226(15) 0.0218(14) 0.0020(11) 0.0024(12) 0.0038(13)
O15 0.0303(12) 0.0294(12) 0.0313(11) 0.0000(9) 0.0003(9) 0.0108(10)
C16 0.0282(15) 0.0264(16) 0.0238(14) -0.0030(12) -0.0012(11) 0.0085(13)
O17 0.0340(12) 0.0264(12) 0.0261(10) 0.0007(9) 0.0000(9) 0.0031(10)
C18 0.0339(17) 0.0249(16) 0.0322(17) -0.0005(13) 0.0002(13) 0.0099(14)
O19 0.0444(14) 0.0339(13) 0.0285(12) 0.0035(10) 0.0006(10) 0.0032(11)
C20 0.0378(19) 0.0311(18) 0.0405(18) -0.0005(14) -0.0040(15) 0.0051(15)
C21 0.0313(16) 0.0290(17) 0.0260(15) 0.0003(12) 0.0032(12) 0.0070(14)
C22 0.0255(15) 0.0304(17) 0.0215(14) 0.0017(12) 0.0034(11) 0.0022(13)
C23 0.0322(17) 0.0321(18) 0.0229(14) -0.0032(12) 0.0029(12) 0.0039(14)
C24 0.0274(15) 0.0256(16) 0.0260(14) -0.0026(12) 0.0000(12) 0.0036(13)
C25 0.0184(13) 0.0280(16) 0.0231(14) 0.0015(11) -0.0007(11) -0.0034(12)
C26 0.0224(15) 0.0283(16) 0.0260(14) -0.0061(12) 0.0013(11) -0.0027(13)
C27 0.0232(15) 0.0271(16) 0.0319(15) -0.0049(12) 0.0018(12) 0.0052(13)
O28 0.0347(12) 0.0327(13) 0.0269(11) -0.0050(9) -0.0075(9) 0.0085(10)
C29 0.0376(18) 0.0312(18) 0.0358(17) -0.0011(14) -0.0082(14) 0.0100(15)
S31 0.0281(4) 0.0412(5) 0.0275(4) 0.0023(3) -0.0004(3) 0.0013(4)
C32 0.0247(15) 0.0351(18) 0.0282(15) -0.0021(13) -0.0025(12) 0.0060(14)
C33 0.0268(16) 0.046(2) 0.0344(17) -0.0093(15) -0.0031(13) 0.0096(15)
C34 0.0268(17) 0.047(2) 0.0422(19) -0.0095(16) -0.0088(14) 0.0137(16)
C35 0.0404(19) 0.051(2) 0.0307(17) -0.0028(15) -0.0094(14) 0.0159(18)
C36 0.0324(17) 0.043(2) 0.0270(15) -0.0035(14) -0.0009(13) 0.0094(15)
C37 0.0268(16) 0.0337(17) 0.0234(14) -0.0046(12) -0.0012(11) 0.0103(14)
N38 0.0237(12) 0.0345(15) 0.0189(12) -0.0046(10) 0.0016(9) 0.0121(11)
C39 0.0248(15) 0.0307(17) 0.0224(14) -0.0061(12) 0.0039(11) 0.0063(13)
C40 0.0294(16) 0.0257(16) 0.0240(14) -0.0042(12) 0.0044(12) 0.0057(13)
N41 0.0224(12) 0.0229(13) 0.0242(12) -0.0033(10) 0.0029(9) 0.0036(10)
C42 0.0287(16) 0.0297(17) 0.0313(16) -0.0016(13) 0.0072(12) 0.0036(14)
C43 0.0299(16) 0.0345(19) 0.0414(18) 0.0064(14) 0.0014(14) 0.0086(15)
C44 0.0293(16) 0.0236(15) 0.0197(13) -0.0001(11) 0.0032(11) 0.0036(13)
O45 0.0270(11) 0.0275(11) 0.0260(10) -0.0021(8) -0.0013(8) 0.0095(9)
C46 0.0262(15) 0.0275(16) 0.0215(13) -0.0031(11) -0.0009(11) 0.0084(13)
O47 0.0329(12) 0.0286(12) 0.0230(10) -0.0024(9) -0.0029(8) 0.0060(10)
C48 0.0301(16) 0.0218(15) 0.0324(16) 0.0000(12) -0.0030(12) 0.0113(13)
O49 0.0403(13) 0.0300(12) 0.0260(11) 0.0017(9) -0.0009(9) 0.0041(10)
C50 0.0363(18) 0.0329(19) 0.0419(19) -0.0028(14) -0.0082(15) 0.0055(15)
C51 0.0303(16) 0.0311(17) 0.0233(14) -0.0042(12) 0.0019(12) 0.0082(14)
C52 0.0228(15) 0.0289(16) 0.0230(14) -0.0011(12) 0.0041(11) 0.0025(12)
C53 0.0334(17) 0.0311(17) 0.0205(14) -0.0048(12) 0.0024(12) 0.0045(14)
C54 0.0308(16) 0.0287(17) 0.0258(15) -0.0036(12) 0.0004(12) 0.0085(14)
C55 0.0200(14) 0.0253(15) 0.0221(13) 0.0004(11) -0.0001(11) -0.0035(12)
C56 0.0228(15) 0.0263(16) 0.0231(14) -0.0065(11) 0.0015(11) -0.0005(12)
C57 0.0220(14) 0.0242(16) 0.0297(15) -0.0046(12) 0.0026(11) 0.0025(12)
O58 0.0353(12) 0.0313(12) 0.0241(10) -0.0038(9) -0.0069(9) 0.0078(10)
C59 0.0379(18) 0.0318(18) 0.0326(17) -0.0006(13) -0.0039(14) 0.0094(15)
S61 0.0295(4) 0.0440(5) 0.0273(4) -0.0093(3) -0.0008(3) -0.0006(4)
C62 0.0278(16) 0.0350(18) 0.0269(15) -0.0029(13) -0.0014(12) -0.0065(14)
C63 0.0273(16) 0.040(2) 0.0376(18) -0.0009(14) -0.0019(13) -0.0055(15)
C64 0.0278(17) 0.048(2) 0.0406(19) -0.0030(16) -0.0080(14) -0.0120(16)
C65 0.044(2) 0.055(2) 0.0276(16) -0.0070(15) -0.0101(14) -0.0156(18)
C66 0.0308(17) 0.044(2) 0.0290(16) -0.0028(14) 0.0002(13) -0.0090(15)
C67 0.0282(16) 0.0300(17) 0.0224(14) -0.0001(12) -0.0020(11) -0.0089(13)
N68 0.0232(12) 0.0324(15) 0.0197(12) -0.0007(10) -0.0002(9) -0.0095(11)
C69 0.0239(15) 0.0276(16) 0.0250(14) -0.0015(12) 0.0022(11) -0.0054(13)
C70 0.0266(15) 0.0285(17) 0.0261(14) -0.0039(12) 0.0035(12) -0.0063(13)
N71 0.0237(12) 0.0241(13) 0.0244(12) -0.0043(10) 0.0029(10) -0.0035(11)
C72 0.0295(16) 0.0342(18) 0.0294(16) -0.0087(13) 0.0060(12) -0.0024(14)
C73 0.0325(17) 0.043(2) 0.0390(18) -0.0163(15) 0.0014(14) -0.0069(16)
C74 0.0288(16) 0.0241(15) 0.0192(13) -0.0069(11) 0.0022(11) -0.0055(13)
O75 0.0275(11) 0.0269(12) 0.0262(10) -0.0053(8) -0.0016(8) -0.0078(9)
C76 0.0293(16) 0.0278(16) 0.0215(14) -0.0028(12) -0.0015(11) -0.0068(13)
O77 0.0347(12) 0.0286(12) 0.0254(10) -0.0042(9) -0.0018(9) -0.0044(10)
C78 0.0310(16) 0.0250(16) 0.0318(17) -0.0082(13) -0.0015(13) -0.0084(13)
O79 0.0406(14) 0.0345(13) 0.0249(11) -0.0079(9) -0.0005(9) -0.0025(11)
C80 0.0358(19) 0.039(2) 0.0411(19) -0.0067(15) -0.0101(15) -0.0015(16)
C81 0.0322(16) 0.0294(16) 0.0201(13) -0.0017(12) 0.0010(12) -0.0056(13)
C82 0.0223(15) 0.0335(17) 0.0224(14) -0.0057(12) 0.0010(11) -0.0033(13)
C83 0.0333(17) 0.0365(19) 0.0205(14) -0.0016(12) 0.0032(12) -0.0048(14)
C84 0.0327(16) 0.0237(16) 0.0259(14) -0.0046(12) -0.0003(12) -0.0044(13)
C85 0.0218(14) 0.0312(17) 0.0201(13) -0.0075(11) -0.0021(11) 0.0043(12)
C86 0.0232(14) 0.0260(16) 0.0209(13) -0.0005(11) 0.0005(11) 0.0004(12)
C87 0.0238(14) 0.0246(16) 0.0278(15) -0.0029(12) 0.0025(11) -0.0036(12)
O88 0.0347(12) 0.0345(13) 0.0245(10) -0.0034(9) -0.0058(9) -0.0060(10)
C89 0.0384(19) 0.039(2) 0.0322(17) -0.0109(14) -0.0043(14) -0.0078(16)
S91 0.0315(4) 0.0417(5) 0.0279(4) -0.0096(3) -0.0019(3) 0.0014(4)
C92 0.0306(16) 0.0356(18) 0.0254(15) -0.0038(13) -0.0029(12) -0.0038(14)
C93 0.0321(17) 0.040(2) 0.0349(17) -0.0014(15) -0.0021(14) -0.0060(15)
C94 0.0363(19) 0.042(2) 0.0417(19) 0.0000(16) -0.0124(15) -0.0148(16)
C95 0.046(2) 0.047(2) 0.0364(18) -0.0049(16) -0.0133(15) -0.0137(18)
C96 0.041(2) 0.047(2) 0.0282(16) -0.0072(15) -0.0016(14) -0.0151(17)
C97 0.0302(16) 0.0314(17) 0.0252(15) -0.0016(12) -0.0041(12) -0.0098(13)
N98 0.0305(14) 0.0293(15) 0.0212(12) -0.0024(10) 0.0020(10) -0.0110(11)
C99 0.0317(16) 0.0257(16) 0.0267(15) -0.0013(12) 0.0017(12) -0.0069(13)
C100 0.0384(18) 0.0258(17) 0.0286(15) -0.0047(13) 0.0056(13) -0.0060(14)
N101 0.0330(14) 0.0241(13) 0.0249(12) -0.0023(10) 0.0049(10) -0.0006(11)
C102 0.0314(18) 0.043(2) 0.0401(19) -0.0017(16) 0.0022(14) -0.0038(16)
C103 0.056(2) 0.037(2) 0.0329(18) -0.0100(15) 0.0154(16) 0.0028(18)
C104 0.0302(17) 0.0274(16) 0.0227(14) -0.0085(12) 0.0003(12) -0.0049(13)
O105 0.0311(12) 0.0303(12) 0.0304(11) -0.0062(9) -0.0017(9) -0.0085(10)
C106 0.0285(15) 0.0266(16) 0.0248(14) -0.0053(12) -0.0002(12) -0.0060(13)
O107 0.0333(12) 0.0295(12) 0.0258(11) -0.0054(9) -0.0007(9) -0.0018(10)
C108 0.0309(17) 0.0254(17) 0.0333(17) -0.0091(13) 0.0016(13) -0.0101(14)
O109 0.0424(14) 0.0355(13) 0.0293(12) -0.0109(10) -0.0008(10) -0.0001(11)
C110 0.0356(18) 0.0332(19) 0.0401(18) -0.0093(15) -0.0044(14) -0.0025(15)
C111 0.0284(16) 0.0307(17) 0.0247(14) -0.0040(12) 0.0031(12) -0.0054(13)
C112 0.0259(15) 0.0327(17) 0.0224(14) -0.0069(12) 0.0029(11) -0.0015(13)
C113 0.0319(17) 0.0326(18) 0.0208(14) -0.0012(12) 0.0036(12) -0.0044(14)
C114 0.0280(15) 0.0239(15) 0.0267(14) -0.0036(12) 0.0009(12) -0.0042(13)
C115 0.0181(13) 0.0268(16) 0.0233(13) -0.0058(11) -0.0004(10) 0.0031(12)
C116 0.0235(15) 0.0257(16) 0.0241(14) 0.0021(11) 0.0008(11) 0.0012(12)
C117 0.0234(14) 0.0228(15) 0.0296(15) -0.0013(12) 0.0036(11) -0.0042(12)
O118 0.0350(12) 0.0320(13) 0.0248(10) -0.0013(9) -0.0065(9) -0.0053(10)
C119 0.0377(18) 0.0340(18) 0.0305(16) -0.0088(13) -0.0053(13) -0.0048(15)
P121 0.0226(4) 0.0249(4) 0.0299(4) -0.0047(3) -0.0059(3) 0.0009(3)
O122 0.0252(12) 0.0476(16) 0.0461(14) 0.0091(12) -0.0116(11) -0.0067(11)
O123 0.0331(13) 0.0343(14) 0.0436(13) 0.0028(11) -0.0120(10) -0.0002(11)
O124 0.0296(12) 0.0452(15) 0.0452(14) -0.0218(11) -0.0118(10) 0.0080(11)
O125 0.0263(11) 0.0355(13) 0.0387(12) -0.0136(10) -0.0078(9) 0.0034(10)
P126 0.0215(4) 0.0241(4) 0.0300(4) -0.0039(3) -0.0056(3) 0.0011(3)
O127 0.0326(12) 0.0374(14) 0.0443(14) 0.0079(11) -0.0133(10) -0.0021(11)
O128 0.0247(11) 0.0293(12) 0.0398(12) 0.0019(10) -0.0076(9) -0.0008(9)
O129 0.0252(12) 0.0513(16) 0.0464(14) -0.0214(12) -0.0106(10) 0.0106(12)
O130 0.0307(12) 0.0368(14) 0.0412(13) -0.0136(10) -0.0134(10) 0.0057(11)
P131 0.0168(3) 0.0268(4) 0.0312(4) -0.0053(3) -0.0027(3) -0.0004(3)
O132 0.0221(10) 0.0306(12) 0.0372(12) -0.0111(9) -0.0061(9) -0.0005(9)
O133 0.0268(12) 0.0453(15) 0.0373(12) -0.0171(11) -0.0055(9) 0.0074(11)
O134 0.0247(11) 0.0309(13) 0.0499(14) 0.0019(10) -0.0026(10) -0.0036(10)
O135 0.0200(11) 0.0376(14) 0.0435(13) -0.0090(10) -0.0029(9) -0.0010(10)
P136 0.0167(3) 0.0267(4) 0.0313(4) -0.0034(3) -0.0034(3) 0.0027(3)
O137 0.0183(11) 0.0380(14) 0.0422(13) -0.0016(10) -0.0013(9) 0.0020(10)
O138 0.0222(10) 0.0309(12) 0.0342(11) 0.0017(9) -0.0051(9) 0.0035(10)
O139 0.0237(11) 0.0346(13) 0.0503(14) -0.0146(11) -0.0025(10) 0.0052(10)
O140 0.0265(11) 0.0387(14) 0.0366(12) 0.0089(10) -0.0060(9) -0.0037(10)
O141 0.0256(12) 0.0546(17) 0.0449(14) -0.0227(12) -0.0001(10) 0.0021(12)
O142 0.0256(12) 0.0474(16) 0.0443(14) 0.0107(12) 0.0007(10) -0.0009(11)
O143 0.0293(13) 0.0278(13) 0.0592(16) -0.0119(11) -0.0071(11) 0.0069(11)
O144 0.0352(13) 0.0260(13) 0.0479(14) -0.0078(10) -0.0107(11) -0.0015(11)
O145 0.0288(12) 0.0239(12) 0.0595(16) -0.0062(11) -0.0084(11) -0.0019(10)
O146 0.0356(13) 0.0285(13) 0.0477(14) -0.0069(10) -0.0114(11) 0.0054(11)
_refine_ls_extinction_method
'None'
_oxford_refine_ls_scale 1.392(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 . C2 . 1.776(3) yes
S1 . C21 . 1.842(4) yes
C2 . C3 . 1.392(4) yes
C2 . C7 . 1.397(4) yes
C3 . C4 . 1.389(5) yes
C3 . H31 . 0.922 no
C4 . C5 . 1.381(6) yes
C4 . H41 . 0.935 no
C5 . C6 . 1.387(5) yes
C5 . H51 . 0.947 no
C6 . C7 . 1.395(5) yes
C6 . H61 . 0.946 no
C7 . N8 . 1.432(4) yes
N8 . C9 . 1.478(4) yes
N8 . C14 . 1.355(4) yes
C9 . C10 . 1.518(5) yes
C9 . H92 . 0.970 no
C9 . H91 . 0.964 no
C10 . N11 . 1.494(4) yes
C10 . H102 . 0.972 no
C10 . H101 . 0.958 no
N11 . C12 . 1.485(4) yes
N11 . C13 . 1.490(4) yes
N11 . H111 . 0.892(18) no
C12 . H122 . 0.950 no
C12 . H123 . 0.959 no
C12 . H121 . 0.948 no
C13 . H133 . 0.960 no
C13 . H131 . 0.968 no
C13 . H132 . 0.962 no
C14 . O15 . 1.220(4) yes
C14 . C16 . 1.533(4) yes
C16 . O17 . 1.444(4) yes
C16 . C21 . 1.542(4) yes
C16 . H161 . 0.978 no
O17 . C18 . 1.361(4) yes
C18 . O19 . 1.213(4) yes
C18 . C20 . 1.480(5) yes
C20 . H203 . 0.947 no
C20 . H201 . 0.949 no
C20 . H202 . 0.947 no
C21 . C22 . 1.511(4) yes
C21 . H211 . 0.966 no
C22 . C23 . 1.377(4) yes
C22 . C27 . 1.405(4) yes
C23 . C24 . 1.399(4) yes
C23 . H231 . 0.944 no
C24 . C25 . 1.389(4) yes
C24 . H241 . 0.928 no
C25 . C26 . 1.395(4) yes
C25 . O28 . 1.365(4) yes
C26 . C27 . 1.383(4) yes
C26 . H261 . 0.930 no
C27 . H271 . 0.929 no
O28 . C29 . 1.438(4) yes
C29 . H293 . 0.945 no
C29 . H291 . 0.964 no
C29 . H292 . 0.946 no
S31 . C32 . 1.772(3) yes
S31 . C51 . 1.844(4) yes
C32 . C33 . 1.395(4) yes
C32 . C37 . 1.402(4) yes
C33 . C34 . 1.390(5) yes
C33 . H331 . 0.941 no
C34 . C35 . 1.385(5) yes
C34 . H341 . 0.939 no
C35 . C36 . 1.387(5) yes
C35 . H351 . 0.943 no
C36 . C37 . 1.381(4) yes
C36 . H361 . 0.925 no
C37 . N38 . 1.435(4) yes
N38 . C39 . 1.477(3) yes
N38 . C44 . 1.351(4) yes
C39 . C40 . 1.531(4) yes
C39 . H391 . 0.951 no
C39 . H392 . 0.968 no
C40 . N41 . 1.500(3) yes
C40 . H401 . 0.961 no
C40 . H402 . 0.978 no
N41 . C42 . 1.487(4) yes
N41 . C43 . 1.482(4) yes
N41 . H411 . 0.885(18) no
C42 . H423 . 0.972 no
C42 . H421 . 0.976 no
C42 . H422 . 0.976 no
C43 . H431 . 0.968 no
C43 . H433 . 0.959 no
C43 . H432 . 0.968 no
C44 . O45 . 1.223(4) yes
C44 . C46 . 1.530(4) yes
C46 . O47 . 1.444(4) yes
C46 . C51 . 1.542(4) yes
C46 . H461 . 0.959 no
O47 . C48 . 1.372(4) yes
C48 . O49 . 1.208(4) yes
C48 . C50 . 1.470(5) yes
C50 . H501 . 0.949 no
C50 . H503 . 0.943 no
C50 . H502 . 0.947 no
C51 . C52 . 1.516(4) yes
C51 . H511 . 0.988 no
C52 . C53 . 1.381(4) yes
C52 . C57 . 1.392(4) yes
C53 . C54 . 1.400(4) yes
C53 . H531 . 0.934 no
C54 . C55 . 1.394(4) yes
C54 . H541 . 0.928 no
C55 . C56 . 1.392(4) yes
C55 . O58 . 1.367(4) yes
C56 . C57 . 1.388(4) yes
C56 . H561 . 0.935 no
C57 . H571 . 0.928 no
O58 . C59 . 1.437(4) yes
C59 . H591 . 0.963 no
C59 . H593 . 0.945 no
C59 . H592 . 0.956 no
S61 . C62 . 1.779(3) yes
S61 . C81 . 1.845(3) yes
C62 . C63 . 1.384(5) yes
C62 . C67 . 1.413(4) yes
C63 . C64 . 1.386(5) yes
C63 . H631 . 0.924 no
C64 . C65 . 1.379(5) yes
C64 . H641 . 0.930 no
C65 . C66 . 1.386(5) yes
C65 . H651 . 0.940 no
C66 . C67 . 1.382(5) yes
C66 . H661 . 0.923 no
C67 . N68 . 1.420(4) yes
N68 . C69 . 1.474(4) yes
N68 . C74 . 1.361(4) yes
C69 . C70 . 1.538(4) yes
C69 . H692 . 0.966 no
C69 . H691 . 0.952 no
C70 . N71 . 1.498(4) yes
C70 . H702 . 0.986 no
C70 . H701 . 0.967 no
N71 . C72 . 1.490(4) yes
N71 . C73 . 1.476(5) yes
N71 . H711 . 0.887(18) no
C72 . H721 . 0.969 no
C72 . H723 . 0.976 no
C72 . H722 . 0.975 no
C73 . H732 . 0.971 no
C73 . H731 . 0.973 no
C73 . H733 . 0.962 no
C74 . O75 . 1.215(4) yes
C74 . C76 . 1.530(4) yes
C76 . O77 . 1.443(4) yes
C76 . C81 . 1.543(4) yes
C76 . H761 . 0.970 no
O77 . C78 . 1.371(4) yes
C78 . O79 . 1.204(4) yes
C78 . C80 . 1.483(5) yes
C80 . H802 . 0.940 no
C80 . H801 . 0.948 no
C80 . H803 . 0.957 no
C81 . C82 . 1.517(4) yes
C81 . H811 . 0.969 no
C82 . C83 . 1.374(5) yes
C82 . C87 . 1.399(4) yes
C83 . C84 . 1.395(5) yes
C83 . H831 . 0.935 no
C84 . C85 . 1.392(4) yes
C84 . H841 . 0.925 no
C85 . C86 . 1.387(5) yes
C85 . O88 . 1.368(4) yes
C86 . C87 . 1.388(4) yes
C86 . H861 . 0.930 no
C87 . H871 . 0.933 no
O88 . C89 . 1.439(5) yes
C89 . H892 . 0.948 no
C89 . H891 . 0.961 no
C89 . H893 . 0.961 no
S91 . C92 . 1.776(3) yes
S91 . C111 . 1.844(3) yes
C92 . C93 . 1.387(5) yes
C92 . C97 . 1.408(4) yes
C93 . C94 . 1.392(5) yes
C93 . H931 . 0.939 no
C94 . C95 . 1.375(6) yes
C94 . H941 . 0.939 no
C95 . C96 . 1.386(6) yes
C95 . H951 . 0.953 no
C96 . C97 . 1.385(5) yes
C96 . H961 . 0.947 no
C97 . N98 . 1.428(4) yes
N98 . C99 . 1.473(4) yes
N98 . C104 . 1.356(4) yes
C99 . C100 . 1.525(4) yes
C99 . H991 . 0.973 no
C99 . H992 . 0.971 no
C100 . N101 . 1.487(4) yes
C100 . H1001 . 0.963 no
C100 . H1002 . 0.980 no
N101 . C102 . 1.476(5) yes
N101 . C103 . 1.494(4) yes
N101 . H1011 . 0.889(18) no
C102 . H1022 . 0.955 no
C102 . H1021 . 0.952 no
C102 . H1023 . 0.956 no
C103 . H1032 . 0.952 no
C103 . H1033 . 0.956 no
C103 . H1031 . 0.953 no
C104 . O105 . 1.223(4) yes
C104 . C106 . 1.533(4) yes
C106 . O107 . 1.445(4) yes
C106 . C111 . 1.544(4) yes
C106 . H1061 . 0.981 no
O107 . C108 . 1.362(4) yes
C108 . O109 . 1.201(4) yes
C108 . C110 . 1.488(5) yes
C110 . H1102 . 0.939 no
C110 . H1103 . 0.946 no
C110 . H1101 . 0.944 no
C111 . C112 . 1.509(4) yes
C111 . H1111 . 0.975 no
C112 . C113 . 1.380(5) yes
C112 . C117 . 1.406(4) yes
C113 . C114 . 1.394(5) yes
C113 . H1131 . 0.939 no
C114 . C115 . 1.396(4) yes
C114 . H1141 . 0.917 no
C115 . C116 . 1.379(5) yes
C115 . O118 . 1.364(4) yes
C116 . C117 . 1.388(5) yes
C116 . H1161 . 0.936 no
C117 . H1171 . 0.928 no
O118 . C119 . 1.434(4) yes
C119 . H1192 . 0.947 no
C119 . H1193 . 0.938 no
C119 . H1191 . 0.956 no
P121 . O122 . 1.573(3) yes
P121 . O123 . 1.563(2) yes
P121 . O124 . 1.503(2) yes
P121 . O125 . 1.501(2) yes
O122 . H1221 . 0.849(19) no
O123 . H1231 . 0.824(19) no
P126 . O127 . 1.505(3) yes
P126 . O128 . 1.505(2) yes
P126 . O129 . 1.571(2) yes
P126 . O130 . 1.562(3) yes
O129 . H1291 . 0.837(19) no
O130 . H1301 . 0.822(19) no
P131 . O132 . 1.576(2) yes
P131 . O133 . 1.561(2) yes
P131 . O134 . 1.515(3) yes
P131 . O135 . 1.499(2) yes
O132 . H1321 . 0.845(18) no
O133 . H1331 . 0.864(19) no
P136 . O137 . 1.500(2) yes
P136 . O138 . 1.572(3) yes
P136 . O139 . 1.516(2) yes
P136 . O140 . 1.571(2) yes
O138 . H1381 . 0.830(18) no
O140 . H1401 . 0.883(19) no
O141 . H1412 . 0.822(18) no
O141 . H1411 . 0.896(19) no
O142 . H1422 . 0.889(19) no
O142 . H1421 . 0.816(19) no
O143 . H1432 . 0.796(19) no
O143 . H1431 . 0.812(19) no
O144 . H1442 . 0.821(19) no
O144 . H1441 . 0.794(19) no
O145 . H1452 . 0.806(19) no
O145 . H1451 . 0.814(19) no
O146 . H1462 . 0.818(19) no
O146 . H1461 . 0.789(19) no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . S1 . C21 . 101.87(16) yes
S1 . C2 . C3 . 119.4(3) yes
S1 . C2 . C7 . 120.8(2) yes
C3 . C2 . C7 . 119.7(3) yes
C2 . C3 . C4 . 120.3(3) yes
C2 . C3 . H31 . 119.4 no
C4 . C3 . H31 . 120.3 no
C3 . C4 . C5 . 119.8(3) yes
C3 . C4 . H41 . 121.3 no
C5 . C4 . H41 . 118.9 no
C4 . C5 . C6 . 120.6(3) yes
C4 . C5 . H51 . 121.2 no
C6 . C5 . H51 . 118.2 no
C5 . C6 . C7 . 119.9(3) yes
C5 . C6 . H61 . 119.8 no
C7 . C6 . H61 . 120.3 no
C2 . C7 . C6 . 119.7(3) yes
C2 . C7 . N8 . 120.6(3) yes
C6 . C7 . N8 . 119.7(3) yes
C7 . N8 . C9 . 118.3(3) yes
C7 . N8 . C14 . 123.5(2) yes
C9 . N8 . C14 . 118.1(2) yes
N8 . C9 . C10 . 109.7(3) yes
N8 . C9 . H92 . 108.7 no
C10 . C9 . H92 . 110.8 no
N8 . C9 . H91 . 108.1 no
C10 . C9 . H91 . 110.2 no
H92 . C9 . H91 . 109.2 no
C9 . C10 . N11 . 111.4(3) yes
C9 . C10 . H102 . 110.7 no
N11 . C10 . H102 . 108.9 no
C9 . C10 . H101 . 110.1 no
N11 . C10 . H101 . 108.7 no
H102 . C10 . H101 . 106.9 no
C10 . N11 . C12 . 112.5(3) yes
C10 . N11 . C13 . 110.5(3) yes
C12 . N11 . C13 . 111.5(3) yes
C10 . N11 . H111 . 106.8(14) no
C12 . N11 . H111 . 107.0(14) no
C13 . N11 . H111 . 108.3(14) no
N11 . C12 . H122 . 109.9 no
N11 . C12 . H123 . 109.8 no
H122 . C12 . H123 . 110.4 no
N11 . C12 . H121 . 108.2 no
H122 . C12 . H121 . 109.5 no
H123 . C12 . H121 . 109.0 no
N11 . C13 . H133 . 110.4 no
N11 . C13 . H131 . 110.9 no
H133 . C13 . H131 . 110.4 no
N11 . C13 . H132 . 108.4 no
H133 . C13 . H132 . 108.9 no
H131 . C13 . H132 . 107.6 no
N8 . C14 . O15 . 122.7(3) yes
N8 . C14 . C16 . 115.8(3) yes
O15 . C14 . C16 . 121.3(3) yes
C14 . C16 . O17 . 109.2(2) yes
C14 . C16 . C21 . 114.0(3) yes
O17 . C16 . C21 . 107.7(2) yes
C14 . C16 . H161 . 107.4 no
O17 . C16 . H161 . 109.0 no
C21 . C16 . H161 . 109.5 no
C16 . O17 . C18 . 113.8(2) yes
O17 . C18 . O19 . 121.3(3) yes
O17 . C18 . C20 . 114.0(3) yes
O19 . C18 . C20 . 124.6(3) yes
C18 . C20 . H203 . 111.1 no
C18 . C20 . H201 . 110.8 no
H203 . C20 . H201 . 107.3 no
C18 . C20 . H202 . 111.7 no
H203 . C20 . H202 . 106.4 no
H201 . C20 . H202 . 109.5 no
C16 . C21 . S1 . 108.3(2) yes
C16 . C21 . C22 . 116.3(3) yes
S1 . C21 . C22 . 108.1(2) yes
C16 . C21 . H211 . 105.8 no
S1 . C21 . H211 . 109.7 no
C22 . C21 . H211 . 108.5 no
C21 . C22 . C23 . 122.4(3) yes
C21 . C22 . C27 . 119.5(3) yes
C23 . C22 . C27 . 118.1(3) yes
C22 . C23 . C24 . 121.9(3) yes
C22 . C23 . H231 . 118.8 no
C24 . C23 . H231 . 119.2 no
C23 . C24 . C25 . 119.2(3) yes
C23 . C24 . H241 . 120.6 no
C25 . C24 . H241 . 120.2 no
C24 . C25 . C26 . 119.8(3) yes
C24 . C25 . O28 . 124.2(3) yes
C26 . C25 . O28 . 116.0(3) yes
C25 . C26 . C27 . 120.1(3) yes
C25 . C26 . H261 . 119.7 no
C27 . C26 . H261 . 120.2 no
C22 . C27 . C26 . 120.9(3) yes
C22 . C27 . H271 . 119.5 no
C26 . C27 . H271 . 119.6 no
C25 . O28 . C29 . 117.6(2) yes
O28 . C29 . H293 . 107.6 no
O28 . C29 . H291 . 109.3 no
H293 . C29 . H291 . 110.4 no
O28 . C29 . H292 . 109.5 no
H293 . C29 . H292 . 110.7 no
H291 . C29 . H292 . 109.2 no
C32 . S31 . C51 . 101.47(16) yes
S31 . C32 . C33 . 120.0(3) yes
S31 . C32 . C37 . 121.3(2) yes
C33 . C32 . C37 . 118.7(3) yes
C32 . C33 . C34 . 120.5(3) yes
C32 . C33 . H331 . 118.2 no
C34 . C33 . H331 . 121.3 no
C33 . C34 . C35 . 120.2(3) yes
C33 . C34 . H341 . 119.6 no
C35 . C34 . H341 . 120.2 no
C34 . C35 . C36 . 119.7(3) yes
C34 . C35 . H351 . 121.0 no
C36 . C35 . H351 . 119.3 no
C35 . C36 . C37 . 120.4(3) yes
C35 . C36 . H361 . 119.9 no
C37 . C36 . H361 . 119.7 no
C32 . C37 . C36 . 120.5(3) yes
C32 . C37 . N38 . 119.9(3) yes
C36 . C37 . N38 . 119.7(3) yes
C37 . N38 . C39 . 118.6(3) yes
C37 . N38 . C44 . 123.3(2) yes
C39 . N38 . C44 . 118.0(2) yes
N38 . C39 . C40 . 109.4(3) yes
N38 . C39 . H391 . 110.2 no
C40 . C39 . H391 . 110.6 no
N38 . C39 . H392 . 108.0 no
C40 . C39 . H392 . 111.2 no
H391 . C39 . H392 . 107.3 no
C39 . C40 . N41 . 111.8(3) yes
C39 . C40 . H401 . 109.1 no
N41 . C40 . H401 . 107.5 no
C39 . C40 . H402 . 109.3 no
N41 . C40 . H402 . 108.5 no
H401 . C40 . H402 . 110.6 no
C40 . N41 . C42 . 110.6(2) yes
C40 . N41 . C43 . 112.5(2) yes
C42 . N41 . C43 . 109.5(2) yes
C40 . N41 . H411 . 106.6(14) no
C42 . N41 . H411 . 107.8(14) no
C43 . N41 . H411 . 109.6(14) no
N41 . C42 . H423 . 107.1 no
N41 . C42 . H421 . 107.1 no
H423 . C42 . H421 . 111.0 no
N41 . C42 . H422 . 111.0 no
H423 . C42 . H422 . 111.4 no
H421 . C42 . H422 . 109.2 no
N41 . C43 . H431 . 110.4 no
N41 . C43 . H433 . 107.9 no
H431 . C43 . H433 . 109.1 no
N41 . C43 . H432 . 108.8 no
H431 . C43 . H432 . 111.1 no
H433 . C43 . H432 . 109.5 no
N38 . C44 . O45 . 123.1(3) yes
N38 . C44 . C46 . 115.5(2) yes
O45 . C44 . C46 . 121.4(3) yes
C44 . C46 . O47 . 109.2(2) yes
C44 . C46 . C51 . 113.9(3) yes
O47 . C46 . C51 . 108.5(2) yes
C44 . C46 . H461 . 109.0 no
O47 . C46 . H461 . 107.6 no
C51 . C46 . H461 . 108.4 no
C46 . O47 . C48 . 113.4(2) yes
O47 . C48 . O49 . 121.1(3) yes
O47 . C48 . C50 . 113.4(3) yes
O49 . C48 . C50 . 125.5(3) yes
C48 . C50 . H501 . 110.8 no
C48 . C50 . H503 . 109.8 no
H501 . C50 . H503 . 108.9 no
C48 . C50 . H502 . 109.0 no
H501 . C50 . H502 . 108.6 no
H503 . C50 . H502 . 109.7 no
C46 . C51 . S31 . 107.8(2) yes
C46 . C51 . C52 . 116.8(3) yes
S31 . C51 . C52 . 107.6(2) yes
C46 . C51 . H511 . 105.3 no
S31 . C51 . H511 . 108.8 no
C52 . C51 . H511 . 110.3 no
C51 . C52 . C53 . 122.3(3) yes
C51 . C52 . C57 . 119.2(3) yes
C53 . C52 . C57 . 118.3(3) yes
C52 . C53 . C54 . 121.8(3) yes
C52 . C53 . H531 . 119.9 no
C54 . C53 . H531 . 118.3 no
C53 . C54 . C55 . 118.9(3) yes
C53 . C54 . H541 . 120.7 no
C55 . C54 . H541 . 120.4 no
C54 . C55 . C56 . 119.9(3) yes
C54 . C55 . O58 . 124.2(3) yes
C56 . C55 . O58 . 115.9(3) yes
C55 . C56 . C57 . 120.0(3) yes
C55 . C56 . H561 . 119.7 no
C57 . C56 . H561 . 120.3 no
C52 . C57 . C56 . 121.0(3) yes
C52 . C57 . H571 . 119.8 no
C56 . C57 . H571 . 119.2 no
C55 . O58 . C59 . 117.9(2) yes
O58 . C59 . H591 . 110.0 no
O58 . C59 . H593 . 107.7 no
H591 . C59 . H593 . 109.4 no
O58 . C59 . H592 . 110.2 no
H591 . C59 . H592 . 109.4 no
H593 . C59 . H592 . 110.1 no
C62 . S61 . C81 . 101.58(15) yes
S61 . C62 . C63 . 120.3(3) yes
S61 . C62 . C67 . 120.5(3) yes
C63 . C62 . C67 . 119.2(3) yes
C62 . C63 . C64 . 120.7(3) yes
C62 . C63 . H631 . 119.3 no
C64 . C63 . H631 . 120.0 no
C63 . C64 . C65 . 119.9(3) yes
C63 . C64 . H641 . 118.4 no
C65 . C64 . H641 . 121.7 no
C64 . C65 . C66 . 120.3(3) yes
C64 . C65 . H651 . 120.5 no
C66 . C65 . H651 . 119.2 no
C65 . C66 . C67 . 120.5(3) yes
C65 . C66 . H661 . 120.2 no
C67 . C66 . H661 . 119.4 no
C62 . C67 . C66 . 119.4(3) yes
C62 . C67 . N68 . 120.5(3) yes
C66 . C67 . N68 . 120.0(3) yes
C67 . N68 . C69 . 119.0(2) yes
C67 . N68 . C74 . 123.3(3) yes
C69 . N68 . C74 . 117.6(3) yes
N68 . C69 . C70 . 109.6(3) yes
N68 . C69 . H692 . 107.4 no
C70 . C69 . H692 . 111.0 no
N68 . C69 . H691 . 109.5 no
C70 . C69 . H691 . 111.3 no
H692 . C69 . H691 . 108.0 no
C69 . C70 . N71 . 111.6(3) yes
C69 . C70 . H702 . 108.0 no
N71 . C70 . H702 . 109.6 no
C69 . C70 . H701 . 108.6 no
N71 . C70 . H701 . 108.2 no
H702 . C70 . H701 . 110.8 no
C70 . N71 . C72 . 110.3(2) yes
C70 . N71 . C73 . 112.7(3) yes
C72 . N71 . C73 . 109.6(3) yes
C70 . N71 . H711 . 106.3(14) no
C72 . N71 . H711 . 107.8(14) no
C73 . N71 . H711 . 110.0(14) no
N71 . C72 . H721 . 106.8 no
N71 . C72 . H723 . 111.5 no
H721 . C72 . H723 . 111.5 no
N71 . C72 . H722 . 108.5 no
H721 . C72 . H722 . 109.0 no
H723 . C72 . H722 . 109.4 no
N71 . C73 . H732 . 108.3 no
N71 . C73 . H731 . 109.7 no
H732 . C73 . H731 . 109.2 no
N71 . C73 . H733 . 109.1 no
H732 . C73 . H733 . 109.0 no
H731 . C73 . H733 . 111.5 no
N68 . C74 . O75 . 123.1(3) yes
N68 . C74 . C76 . 115.2(3) yes
O75 . C74 . C76 . 121.6(3) yes
C74 . C76 . O77 . 109.3(2) yes
C74 . C76 . C81 . 113.8(3) yes
O77 . C76 . C81 . 108.5(2) yes
C74 . C76 . H761 . 109.7 no
O77 . C76 . H761 . 107.3 no
C81 . C76 . H761 . 108.0 no
C76 . O77 . C78 . 113.2(2) yes
O77 . C78 . O79 . 121.6(3) yes
O77 . C78 . C80 . 113.1(3) yes
O79 . C78 . C80 . 125.3(3) yes
C78 . C80 . H802 . 108.1 no
C78 . C80 . H801 . 110.5 no
H802 . C80 . H801 . 109.5 no
C78 . C80 . H803 . 110.2 no
H802 . C80 . H803 . 109.4 no
H801 . C80 . H803 . 109.1 no
C76 . C81 . S61 . 107.8(2) yes
C76 . C81 . C82 . 116.7(3) yes
S61 . C81 . C82 . 107.3(2) yes
C76 . C81 . H811 . 106.0 no
S61 . C81 . H811 . 109.2 no
C82 . C81 . H811 . 109.8 no
C81 . C82 . C83 . 122.7(3) yes
C81 . C82 . C87 . 118.8(3) yes
C83 . C82 . C87 . 118.4(3) yes
C82 . C83 . C84 . 121.8(3) yes
C82 . C83 . H831 . 119.7 no
C84 . C83 . H831 . 118.5 no
C83 . C84 . C85 . 119.1(3) yes
C83 . C84 . H841 . 120.2 no
C85 . C84 . H841 . 120.7 no
C84 . C85 . C86 . 119.9(3) yes
C84 . C85 . O88 . 123.9(3) yes
C86 . C85 . O88 . 116.2(3) yes
C85 . C86 . C87 . 120.1(3) yes
C85 . C86 . H861 . 120.0 no
C87 . C86 . H861 . 119.9 no
C82 . C87 . C86 . 120.6(3) yes
C82 . C87 . H871 . 120.3 no
C86 . C87 . H871 . 119.1 no
C85 . O88 . C89 . 117.9(2) yes
O88 . C89 . H892 . 107.9 no
O88 . C89 . H891 . 109.9 no
H892 . C89 . H891 . 109.7 no
O88 . C89 . H893 . 109.7 no
H892 . C89 . H893 . 109.9 no
H891 . C89 . H893 . 109.7 no
C92 . S91 . C111 . 102.24(15) yes
S91 . C92 . C93 . 119.6(3) yes
S91 . C92 . C97 . 120.6(3) yes
C93 . C92 . C97 . 119.8(3) yes
C92 . C93 . C94 . 119.9(3) yes
C92 . C93 . H931 . 119.9 no
C94 . C93 . H931 . 120.2 no
C93 . C94 . C95 . 120.3(3) yes
C93 . C94 . H941 . 121.7 no
C95 . C94 . H941 . 118.0 no
C94 . C95 . C96 . 120.2(3) yes
C94 . C95 . H951 . 120.7 no
C96 . C95 . H951 . 119.1 no
C95 . C96 . C97 . 120.5(3) yes
C95 . C96 . H961 . 119.1 no
C97 . C96 . H961 . 120.4 no
C92 . C97 . C96 . 119.3(3) yes
C92 . C97 . N98 . 120.5(3) yes
C96 . C97 . N98 . 120.2(3) yes
C97 . N98 . C99 . 118.3(3) yes
C97 . N98 . C104 . 123.4(3) yes
C99 . N98 . C104 . 118.1(3) yes
N98 . C99 . C100 . 110.0(3) yes
N98 . C99 . H991 . 107.6 no
C100 . C99 . H991 . 110.8 no
N98 . C99 . H992 . 109.8 no
C100 . C99 . H992 . 109.3 no
H991 . C99 . H992 . 109.3 no
C99 . C100 . N101 . 111.5(3) yes
C99 . C100 . H1001 . 110.5 no
N101 . C100 . H1001 . 107.5 no
C99 . C100 . H1002 . 110.4 no
N101 . C100 . H1002 . 109.5 no
H1001 . C100 . H1002 . 107.4 no
C100 . N101 . C102 . 112.6(3) yes
C100 . N101 . C103 . 110.3(3) yes
C102 . N101 . C103 . 111.3(3) yes
C100 . N101 . H1011 . 106.7(14) no
C102 . N101 . H1011 . 107.7(14) no
C103 . N101 . H1011 . 108.0(14) no
N101 . C102 . H1022 . 110.2 no
N101 . C102 . H1021 . 107.9 no
H1022 . C102 . H1021 . 108.5 no
N101 . C102 . H1023 . 110.2 no
H1022 . C102 . H1023 . 109.7 no
H1021 . C102 . H1023 . 110.4 no
N101 . C103 . H1032 . 110.9 no
N101 . C103 . H1033 . 109.1 no
H1032 . C103 . H1033 . 108.2 no
N101 . C103 . H1031 . 109.9 no
H1032 . C103 . H1031 . 110.0 no
H1033 . C103 . H1031 . 108.7 no
N98 . C104 . O105 . 123.1(3) yes
N98 . C104 . C106 . 116.1(3) yes
O105 . C104 . C106 . 120.7(3) yes
C104 . C106 . O107 . 109.6(3) yes
C104 . C106 . C111 . 113.7(3) yes
O107 . C106 . C111 . 107.7(2) yes
C104 . C106 . H1061 . 108.0 no
O107 . C106 . H1061 . 108.8 no
C111 . C106 . H1061 . 109.1 no
C106 . O107 . C108 . 113.2(2) yes
O107 . C108 . O109 . 121.8(3) yes
O107 . C108 . C110 . 113.2(3) yes
O109 . C108 . C110 . 125.0(3) yes
C108 . C110 . H1102 . 109.7 no
C108 . C110 . H1103 . 113.5 no
H1102 . C110 . H1103 . 108.7 no
C108 . C110 . H1101 . 110.0 no
H1102 . C110 . H1101 . 106.8 no
H1103 . C110 . H1101 . 108.0 no
C106 . C111 . S91 . 108.3(2) yes
C106 . C111 . C112 . 116.6(3) yes
S91 . C111 . C112 . 108.1(2) yes
C106 . C111 . H1111 . 105.4 no
S91 . C111 . H1111 . 110.0 no
C112 . C111 . H1111 . 108.4 no
C111 . C112 . C113 . 122.4(3) yes
C111 . C112 . C117 . 119.6(3) yes
C113 . C112 . C117 . 117.9(3) yes
C112 . C113 . C114 . 121.7(3) yes
C112 . C113 . H1131 . 119.1 no
C114 . C113 . H1131 . 119.2 no
C113 . C114 . C115 . 119.5(3) yes
C113 . C114 . H1141 . 121.2 no
C115 . C114 . H1141 . 119.3 no
C114 . C115 . C116 . 119.7(3) yes
C114 . C115 . O118 . 124.1(3) yes
C116 . C115 . O118 . 116.2(3) yes
C115 . C116 . C117 . 120.3(3) yes
C115 . C116 . H1161 . 119.6 no
C117 . C116 . H1161 . 120.1 no
C112 . C117 . C116 . 120.9(3) yes
C112 . C117 . H1171 . 119.7 no
C116 . C117 . H1171 . 119.4 no
C115 . O118 . C119 . 118.5(2) yes
O118 . C119 . H1192 . 109.3 no
O118 . C119 . H1193 . 109.1 no
H1192 . C119 . H1193 . 109.2 no
O118 . C119 . H1191 . 109.8 no
H1192 . C119 . H1191 . 108.5 no
H1193 . C119 . H1191 . 110.8 no
O122 . P121 . O123 . 103.48(14) yes
O122 . P121 . O124 . 108.27(16) yes
O123 . P121 . O124 . 110.15(14) yes
O122 . P121 . O125 . 109.41(15) yes
O123 . P121 . O125 . 111.67(14) yes
O124 . P121 . O125 . 113.34(13) yes
P121 . O122 . H1221 . 122(4) no
P121 . O123 . H1231 . 109(4) no
O127 . P126 . O128 . 113.77(13) yes
O127 . P126 . O129 . 108.07(16) yes
O128 . P126 . O129 . 109.25(14) yes
O127 . P126 . O130 . 110.09(15) yes
O128 . P126 . O130 . 111.59(14) yes
O129 . P126 . O130 . 103.50(13) yes
P126 . O129 . H1291 . 119(4) no
P126 . O130 . H1301 . 110(3) no
O132 . P131 . O133 . 106.74(13) yes
O132 . P131 . O134 . 108.84(13) yes
O133 . P131 . O134 . 111.17(15) yes
O132 . P131 . O135 . 108.69(14) yes
O133 . P131 . O135 . 107.00(13) yes
O134 . P131 . O135 . 114.12(14) yes
P131 . O132 . H1321 . 115(3) no
P131 . O133 . H1331 . 114(3) no
O137 . P136 . O138 . 108.98(13) yes
O137 . P136 . O139 . 114.35(15) yes
O138 . P136 . O139 . 108.43(14) yes
O137 . P136 . O140 . 106.93(13) yes
O138 . P136 . O140 . 106.76(14) yes
O139 . P136 . O140 . 111.12(14) yes
P136 . O138 . H1381 . 115(3) no
P136 . O140 . H1401 . 114(3) no
H1412 . O141 . H1411 . 104.8(10) no
H1422 . O142 . H1421 . 105.1(10) no
H1432 . O143 . H1431 . 115(5) no
H1442 . O144 . H1441 . 91(5) no
H1452 . O145 . H1451 . 120(5) no
H1462 . O146 . H1461 . 84(5) no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C5 . H51 . O124 . 154 0.95 2.49 3.370(5) yes
C9 . H92 . O49 . 177 0.97 2.44 3.405(5) yes
N11 . H111 . O139 . 175(2) 0.892 1.747 2.637(5) yes
C12 . H122 . O49 . 174 0.95 2.49 3.438(5) yes
C20 . H203 . O45 1_565 145 0.95 2.38 3.204(5) yes
C20 . H201 . O88 1_655 138 0.95 2.49 3.255(5) yes
C39 . H391 . O19 1_545 178 0.95 2.40 3.349(5) yes
C40 . H401 . O138 . 150 0.96 2.48 3.346(5) yes
N41 . H411 . O141 1_545 169(2) 0.885 1.823 2.696(5) yes
C42 . H423 . O138 . 149 0.97 2.54 3.410(5) yes
C42 . H421 . O133 1_545 134 0.98 2.53 3.283(5) yes
C43 . H431 . O19 1_545 178 0.97 2.39 3.362(5) yes
C50 . H501 . O15 . 129 0.95 2.50 3.179(5) yes
C50 . H502 . O118 1_655 155 0.95 2.37 3.257(5) yes
C69 . H691 . O109 . 178 0.95 2.41 3.357(5) yes
C70 . H701 . O132 1_456 149 0.97 2.48 3.346(5) yes
N71 . H711 . O142 1_446 169(2) 0.887 1.822 2.698(5) yes
C72 . H721 . O132 1_456 152 0.97 2.52 3.409(5) yes
C72 . H722 . O140 1_456 137 0.97 2.50 3.276(5) yes
C73 . H731 . O109 . 176 0.97 2.39 3.366(5) yes
C80 . H801 . O58 1_465 160 0.95 2.35 3.254(5) yes
C80 . H803 . O105 1_565 126 0.96 2.53 3.179(5) yes
C95 . H951 . O127 1_546 153 0.95 2.49 3.370(5) yes
C99 . H992 . O79 1_545 176 0.97 2.44 3.413(5) yes
N101 . H1011 . O134 1_446 175(2) 0.889 1.744 2.630(5) yes
C102 . H1023 . O79 1_545 176 0.96 2.49 3.441(5) yes
C110 . H1102 . O28 1_455 149 0.94 2.41 3.251(5) yes
C110 . H1101 . O75 . 138 0.94 2.44 3.209(5) yes
O122 . H1221 . O135 . 177(6) 0.849 1.689 2.538(5) yes
O123 . H1231 . O143 . 163(5) 0.824 1.804 2.603(5) yes
O129 . H1291 . O137 1_465 173(5) 0.837 1.710 2.542(5) yes
O130 . H1301 . O145 . 163(5) 0.822 1.809 2.605(5) yes
O132 . H1321 . O125 1_655 175(4) 0.845 1.713 2.555(5) yes
O133 . H1331 . O124 1_655 160(5) 0.864 1.667 2.498(5) yes
O138 . H1381 . O128 1_545 177(5) 0.830 1.728 2.557(5) yes
O140 . H1401 . O127 1_545 167(5) 0.883 1.627 2.496(5) yes
O141 . H1412 . O144 1_565 169(5) 0.822 1.939 2.750(5) yes
O141 . H1411 . O135 . 164(5) 0.896 1.958 2.831(5) yes
O142 . H1422 . O137 1_565 171(5) 0.889 1.945 2.827(5) yes
O142 . H1421 . O146 1_665 167(5) 0.816 1.945 2.747(5) yes
O143 . H1432 . O139 . 159(5) 0.796 1.941 2.702(5) yes
O143 . H1431 . O129 1_545 156(5) 0.812 2.287 3.049(5) yes
O144 . H1442 . O128 1_545 160(5) 0.821 2.021 2.805(5) yes
O144 . H1441 . O124 1_545 166(5) 0.794 1.985 2.762(5) yes
O145 . H1452 . O134 1_455 141(5) 0.806 2.025 2.700(5) yes
O145 . H1451 . O122 . 164(5) 0.814 2.263 3.054(5) yes
O146 . H1462 . O125 . 167(5) 0.818 2.011 2.814(5) yes
O146 . H1461 . O127 1_545 150(5) 0.789 2.044 2.759(5) yes
_iucr_refine_instructions_details
;
#
# Punched on 15/06/18 at 13:08:37
#
#LIST 12
BLOCK
CONT SCALE
CONT S ( 1 ,X'S,U'S) UNTIL S ( 31 )
CONT C ( 32 ,X'S,U'S) UNTIL N ( 41 )
CONT C ( 42 ,X'S,U'S) UNTIL C ( 51 )
CONT C ( 52 ,X'S,U'S) UNTIL S ( 61 )
CONT C ( 62 ,X'S,U'S) UNTIL S ( 91 )
CONT C ( 92 ,X'S,U'S)
CONT C ( 93 ,X'S,U'S) UNTIL N ( 101 )
CONT C ( 102 ,X'S,U'S)
CONT C ( 103 ,X'S,U'S) UNTIL C ( 111 )
CONT H ( 111 ,X'S,U[ISO])
CONT C ( 112 ,X'S,U'S) UNTIL P ( 121 )
CONT O ( 122 ,X'S,U'S)
CONT O ( 123 ,X'S,U'S)
CONT O ( 124 ,X'S,U'S) UNTIL P ( 131 )
CONT O ( 132 ,X'S,U'S)
CONT O ( 133 ,X'S,U'S)
CONT O ( 134 ,X'S,U'S) UNTIL O ( 146 )
CONT H ( 411 ,X'S,U[ISO])
CONT H ( 711 ,X'S,U[ISO])
CONT H ( 1011 ,X'S,U[ISO])
CONT H ( 1221 ,X'S,U[ISO]) UNTIL H ( 1461 )
CONT ENANTIO
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 9,X'S) H ( 92,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 102,X'S) H ( 101,X'S)
RIDE C ( 12,X'S) H ( 122,X'S) H ( 123,X'S) H ( 121,X'S)
RIDE C ( 13,X'S) H ( 133,X'S) H ( 131,X'S) H ( 132,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 20,X'S) H ( 203,X'S) H ( 201,X'S) H ( 202,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 26,X'S) H ( 261,X'S)
RIDE C ( 27,X'S) H ( 271,X'S)
RIDE C ( 29,X'S) H ( 293,X'S) H ( 291,X'S) H ( 292,X'S)
RIDE C ( 33,X'S) H ( 331,X'S)
RIDE C ( 34,X'S) H ( 341,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 39,X'S) H ( 391,X'S) H ( 392,X'S)
RIDE C ( 40,X'S) H ( 401,X'S) H ( 402,X'S)
RIDE C ( 42,X'S) H ( 423,X'S) H ( 421,X'S) H ( 422,X'S)
RIDE C ( 43,X'S) H ( 431,X'S) H ( 433,X'S) H ( 432,X'S)
RIDE C ( 46,X'S) H ( 461,X'S)
RIDE C ( 50,X'S) H ( 501,X'S) H ( 503,X'S) H ( 502,X'S)
RIDE C ( 51,X'S) H ( 511,X'S)
RIDE C ( 53,X'S) H ( 531,X'S)
RIDE C ( 54,X'S) H ( 541,X'S)
RIDE C ( 56,X'S) H ( 561,X'S)
RIDE C ( 57,X'S) H ( 571,X'S)
RIDE C ( 59,X'S) H ( 591,X'S) H ( 593,X'S) H ( 592,X'S)
RIDE C ( 63,X'S) H ( 631,X'S)
RIDE C ( 64,X'S) H ( 641,X'S)
RIDE C ( 65,X'S) H ( 651,X'S)
RIDE C ( 66,X'S) H ( 661,X'S)
RIDE C ( 69,X'S) H ( 692,X'S) H ( 691,X'S)
RIDE C ( 70,X'S) H ( 702,X'S) H ( 701,X'S)
RIDE C ( 72,X'S) H ( 721,X'S) H ( 723,X'S) H ( 722,X'S)
RIDE C ( 73,X'S) H ( 732,X'S) H ( 731,X'S) H ( 733,X'S)
RIDE C ( 76,X'S) H ( 761,X'S)
RIDE C ( 80,X'S) H ( 802,X'S) H ( 801,X'S) H ( 803,X'S)
RIDE C ( 81,X'S) H ( 811,X'S)
RIDE C ( 83,X'S) H ( 831,X'S)
RIDE C ( 84,X'S) H ( 841,X'S)
RIDE C ( 86,X'S) H ( 861,X'S)
RIDE C ( 87,X'S) H ( 871,X'S)
RIDE C ( 89,X'S) H ( 892,X'S) H ( 891,X'S) H ( 893,X'S)
RIDE C ( 93,X'S) H ( 931,X'S)
RIDE C ( 94,X'S) H ( 941,X'S)
RIDE C ( 95,X'S) H ( 951,X'S)
RIDE C ( 96,X'S) H ( 961,X'S)
RIDE C ( 99,X'S) H ( 991,X'S) H ( 992,X'S)
RIDE C ( 100,X'S) H (1001,X'S) H (1002,X'S)
RIDE C ( 102,X'S) H (1022,X'S) H (1021,X'S) H (1023,X'S)
RIDE C ( 103,X'S) H (1032,X'S) H (1033,X'S) H (1031,X'S)
RIDE C ( 106,X'S) H (1061,X'S)
RIDE C ( 110,X'S) H (1102,X'S) H (1103,X'S) H (1101,X'S)
RIDE C ( 111,X'S) H (1111,X'S)
RIDE C ( 113,X'S) H (1131,X'S)
RIDE C ( 114,X'S) H (1141,X'S)
RIDE C ( 116,X'S) H (1161,X'S)
RIDE C ( 117,X'S) H (1171,X'S)
RIDE C ( 119,X'S) H (1192,X'S) H (1193,X'S) H (1191,X'S)
END
#
# Punched on 15/06/18 at 13:08:37
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM NO H NO #H U MULT DIST
REM C-H
REM >4 1.5 .96 DISORDER
REM 1 1 1.2 .93 C C-H (ACETYLENE)
REM 1 2 1.2 .93 C-C(H)-C
REM 1 3 1.2 .98 (C)3-C-H
REM 2 1 1.2 .93 C=C-H(2)
REM 2 2 1.2 .97 (C)2-C-(H)2
REM 3 1 1.5 .96 C-C-(H)3
REM N-H
REM >4 1.5 .89 DISORDER
REM 1 1 1.2 .86 N-N/H
REM 1 2 1.2 .86 (C)2-N-H
REM 1 3 1.2 .89 (C)3-N-H
REM 2 1 1.2 .86 C-N-(H)2
REM 2 2 1.2 .89 (C)2-N-(H)2
REM 3 1 1.2 .89 C-H-(H)3
REM O-H
REM 1 1 1.5 .82 O-H
REM
REM DIST ESD = 0.02
REM VIB ESD = 0.002
REM ANGLE ESD = 2.0
REM
REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM
REM POSSIBLY DISORDERED, NO OF H ATOMS= 1
DIST 0.89, 0.02 =
CONT N ( 11) TO H(111)
REST 0.043, 0.002 = H(111,U[ISO])
ANGLE 109.54, 2.0 =
CONT C(10) TO N ( 11) TO H(111)
CONT C(12) TO N ( 11) TO H(111)
CONT C(13) TO N ( 11) TO H(111)
REM POSSIBLY DISORDERED, NO OF H ATOMS= 1
DIST 0.89, 0.02 =
CONT N ( 41) TO H(411)
REST 0.036, 0.002 = H(411,U[ISO])
ANGLE 109.54, 2.0 =
CONT C(40) TO N ( 41) TO H(411)
CONT C(42) TO N ( 41) TO H(411)
CONT C(43) TO N ( 41) TO H(411)
REM POSSIBLY DISORDERED, NO OF H ATOMS= 1
DIST 0.89, 0.02 =
CONT N ( 71) TO H(711)
REST 0.037, 0.002 = H(711,U[ISO])
ANGLE 109.54, 2.0 =
CONT C(70) TO N ( 71) TO H(711)
CONT C(72) TO N ( 71) TO H(711)
CONT C(73) TO N ( 71) TO H(711)
REM POSSIBLY DISORDERED, NO OF H ATOMS= 1
DIST 0.89, 0.02 =
CONT N ( 101) TO H(1011)
REST 0.043, 0.002 = H(1011,U[ISO])
ANGLE 109.54, 2.0 =
CONT C(100) TO N ( 101) TO H(1011)
CONT C(102) TO N ( 101) TO H(1011)
CONT C(103) TO N ( 101) TO H(1011)
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 122) TO H(1221)
REST 0.060, 0.002 = H(1221,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 123) TO H(1231)
REST 0.056, 0.002 = H(1231,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 129) TO H(1291)
REST 0.059, 0.002 = H(1291,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 130) TO H(1301)
REST 0.052, 0.002 = H(1301,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 132) TO H(1321)
REST 0.044, 0.002 = H(1321,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 133) TO H(1331)
REST 0.053, 0.002 = H(1331,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 138) TO H(1381)
REST 0.044, 0.002 = H(1381,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 140) TO H(1401)
REST 0.053, 0.002 = H(1401,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 141) TO H(1412)
CONT O ( 141) TO H(1411)
REST 0.061, 0.002 = H(1412,U[ISO])
REST 0.061, 0.002 = H(1411,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 142) TO H(1422)
CONT O ( 142) TO H(1421)
REST 0.062, 0.002 = H(1422,U[ISO])
REST 0.062, 0.002 = H(1421,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 143) TO H(1432)
CONT O ( 143) TO H(1431)
REST 0.057, 0.002 = H(1432,U[ISO])
REST 0.057, 0.002 = H(1431,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 144) TO H(1442)
CONT O ( 144) TO H(1441)
REST 0.054, 0.002 = H(1442,U[ISO])
REST 0.054, 0.002 = H(1441,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 145) TO H(1452)
CONT O ( 145) TO H(1451)
REST 0.056, 0.002 = H(1452,U[ISO])
REST 0.056, 0.002 = H(1451,U[ISO])
REM H ON O-HETRO ATOM
DIST 0.82, 0.02 =
CONT O ( 146) TO H(1462)
CONT O ( 146) TO H(1461)
REST 0.055, 0.002 = H(1462,U[ISO])
REST 0.055, 0.002 = H(1461,U[ISO])
REM HREST END (DO NOT REMOVE THIS LINE)
ANGLE 104.500000 , 1.000000 = H(1412) TO O(141) TO H(1411)
ANGLE 104.500000 , 1.000000 = H(1421) TO O(142) TO H(1422)
ANGLE 104.500000 , 1.000000 = H(1381) TO O(138) TO H(1382)
ANGLE 104.500000 , 1.000000 = H(1371) TO O(137) TO H(1372)
DISTANCE 0.820000 , 0.050000 = O(141) TO H(1412)
END
;
# Manually omitted reflections
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-3 -11 -8 x .
-6 -12 -4 x .
-9 -8 -8 x .
-8 -10 -8 x .
-9 -5 -10 x .
-7 -6 -13 x .
-9 -8 -7 x .
-8 -10 -7 x .
-5 -13 -4 x .
-6 -12 -3 x .
-3 -10 -9 x .
-9 -6 -9 x .
-2 -14 -4 x .
-6 -12 -2 x .
-7 -11 -6 x .
-8 -10 -6 x .
-6 -12 -2 x .
-9 -5 -9 x .
-9 -7 -8 x .
-8 -10 -4 x .
-5 -13 -5 x .
-6 -12 -5 x .
-5 -12 -2 x .
-10 -5 -3 x .
-1 -14 -5 x .
-6 -12 -1 x .
-2 -13 -1 x .
-8 -10 -5 x .
-9 -8 -6 x .
-2 -12 -6 x .
-2 -12 -11 x .
-9 -6 -8 x .
-3 -10 -8 x .
-7 -11 -5 x .
-2 -14 -5 x .
-2 -12 -10 x .
0 0 -2 x .
5 9 -3 x .
4 7 6 x .
data_pn180815_uo_eph_1_180814_pyrolidcarbox
_audit_creation_date 2018-08-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number '2014/7'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C10 H16 N O, C5 H6 N O3, H2 O'
_chemical_formula_sum 'C15 H24 N2 O5'
_chemical_formula_weight 312.36
_chemical_absolute_configuration rmad
_chemical_melting_point ?
_chemical_oxdiff_formula 'C15 H25 N2 O5'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system 'monoclinic'
_space_group_IT_number 4
_space_group_name_H-M_alt 'P 1 21 1'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 11.47377(11)
_cell_length_b 6.14747(5)
_cell_length_c 11.71348(12)
_cell_angle_alpha 90
_cell_angle_beta 111.9780(11)
_cell_angle_gamma 90
_cell_volume 766.163(14)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 12100
_cell_measurement_temperature 159.99(10)
_cell_measurement_theta_max 78.6290
_cell_measurement_theta_min 4.0570
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.843
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.708
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.354
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 336
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 0 -5 0.0222
0 -4 0 0.1919
-1 4 -1 0.1804
-2 0 8 0.0153
2 0 -8 0.0226
3 3 -6 0.1244
6 0 -6 0.0133
-6 0 6 0.0181
-5 -3 1 0.1463
1 -3 -5 0.1483
7 0 -4 0.0067
3 0 5 0.0166
_exptl_crystal_size_max 0.381
_exptl_crystal_size_mid 0.042
_exptl_crystal_size_min 0.031
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2.9944 0.0012 -4.9994 -0.2200 -0.7906 0.4972
-0.0103 -3.9997 0.0117 0.1525 0.4968 0.8574
-0.9883 4.0002 -1.0119 -0.2443 -0.6788 -0.7357
-2.0046 0.0021 7.9942 -0.4602 0.8594 -0.4158
2.0046 -0.0021 -7.9942 0.4602 -0.8594 0.4158
3.0102 2.9973 -6.0034 0.4099 -0.9277 -0.4150
6.0006 -0.0043 -5.9925 0.8826 -0.3762 0.0605
-6.0006 0.0043 5.9925 -0.8826 0.3762 -0.0605
-5.0053 -2.9967 1.0047 -0.5104 0.1968 0.8564
0.9953 -3.0009 -4.9877 0.3722 -0.1794 0.9169
6.9985 -0.0046 -3.9929 0.9467 -0.0719 -0.1272
2.9944 -0.0012 4.9994 0.2200 0.7906 -0.4972
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0235
_diffrn_reflns_av_unetI/netI 0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 13893
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 78.863
_diffrn_reflns_theta_min 4.070
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 159.99(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
--------------------------------------------------------------------------
1 \w 143.00 178.00 0.50 2.00 -- 107.75 45.00 120.00 70
2 \w 148.00 177.00 0.50 2.00 -- 107.75 57.00 69.33 58
3 \w 146.00 175.00 0.50 2.00 -- 107.75 15.00 30.00 58
4 \w 143.00 178.00 0.50 2.00 -- 107.75 45.00 -30.00 70
5 \w 144.00 171.00 0.50 2.00 -- 107.75 15.00 -90.00 54
6 \w 142.00 168.00 0.50 2.00 -- 107.75 15.00-120.00 52
7 \w 134.00 170.00 0.50 2.00 -- 107.75 45.00-120.00 72
8 \w 129.00 163.00 0.50 2.00 -- 107.75 45.00 0.00 68
9 \w 128.00 154.00 0.50 2.00 -- 107.75 45.00 60.00 52
10 \w 128.00 167.00 0.50 2.00 -- 107.75 40.00 55.22 78
11 \w 111.00 137.00 0.50 2.00 -- 107.75 15.00 30.00 52
12 \w 108.00 134.00 0.50 2.00 -- 107.75 45.00 -30.00 52
13 \w 100.00 139.00 0.50 2.00 -- 107.75 45.00 30.00 78
14 \w 103.00 131.00 0.50 2.00 -- 107.75 45.00 90.00 56
15 \w 103.00 129.00 0.50 2.00 -- 107.75 45.00 120.00 52
16 \w 103.00 140.00 0.50 2.00 -- 107.75 30.00 150.00 74
17 \w 96.00 132.00 0.50 2.00 -- 107.75 30.00 120.00 72
18 \w 94.00 129.00 0.50 2.00 -- 107.75 57.00 69.33 70
19 \w 94.00 139.00 0.50 2.00 -- 107.75 45.00 150.00 90
20 \w 95.00 121.00 0.50 2.00 -- 107.75 45.00 60.00 52
21 \w 96.00 121.00 0.50 2.00 -- 107.75 40.00 55.22 50
22 \w 62.00 88.00 0.50 2.00 -- 107.75 -15.00 150.00 52
23 \w 36.00 124.00 0.50 0.50 -- 50.71 57.00 120.00 176
24 \w 49.00 75.00 0.50 2.00 -- 107.75 -15.00 -30.00 52
25 \w 74.00 100.00 0.50 2.00 -- 107.75 -59.00 -19.47 52
26 \w 80.00 106.00 0.50 2.00 -- 107.75 -8.00-100.61 52
27 \w 85.00 115.00 0.50 2.00 -- 107.75 -15.00-180.00 60
28 \w 59.00 85.00 0.50 2.00 -- 107.75 -54.00-171.92 52
29 \w 56.00 88.00 0.50 2.00 -- 107.75 -54.00-144.42 64
30 \w 55.00 80.00 0.50 2.00 -- 107.75 -54.00 -97.01 50
31 \w 49.00 85.00 0.50 2.00 -- 107.75 -57.00-105.58 72
32 \w 38.00 76.00 0.50 2.00 -- 107.75 -45.00 -60.00 76
33 \w 43.00 71.00 0.50 2.00 -- 107.75 -49.00 18.32 56
34 \w 36.00 88.00 0.50 2.00 -- 107.75 -53.00 44.59 104
35 \w 37.00 65.00 0.50 2.00 -- 107.75 -30.00 -60.00 56
36 \w 34.00 80.00 0.50 2.00 -- 107.75 -50.00 -0.20 92
37 \w 30.00 64.00 0.50 2.00 -- 107.75 -30.00 60.00 68
38 \w 35.00 90.00 0.50 2.00 -- 107.75 -57.00 95.29 110
39 \w 34.00 78.00 0.50 2.00 -- 107.75 -53.00 178.23 88
40 \w 39.00 88.00 0.50 2.00 -- 107.75 -60.00 161.56 98
41 \w 39.00 68.00 0.50 2.00 -- 107.75 -30.00 120.00 58
42 \w 35.00 61.00 0.50 2.00 -- 107.75 -53.00 60.74 52
43 \w 32.00 67.00 0.50 2.00 -- 107.75 -30.00 0.00 70
44 \w 39.00 65.00 0.50 2.00 -- 107.75 -30.00-150.00 52
45 \w 31.00 65.00 0.50 2.00 -- 107.75 -30.00-180.00 68
46 \w -22.00 66.00 0.50 0.50 -- 50.71 -57.00 -30.00 176
47 \w -69.00 -8.00 0.50 2.00 -- -86.25 30.00 120.00 122
48 \w -97.00 -70.00 0.50 2.00 -- -86.25 -60.00 73.44 54
49 \w -95.00 -70.00 0.50 2.00 -- -86.25 -60.00 61.00 50
50 \w -124.00 -36.00 0.50 0.50 -- -50.71 -56.00 80.71 176
51 \w -128.00 -39.00 0.50 0.50 -- -50.71 -38.00-120.00 178
52 \w -128.00 -39.00 0.50 0.50 -- -50.71 -38.00 120.00 178
53 \w -128.00 -39.00 0.50 0.50 -- -50.71 -41.00 176.00 178
54 \w -158.00 -70.00 0.50 2.00 -- -86.25 -60.00 25.37 176
55 \w -149.00 -72.00 0.50 2.00 -- -86.25 -60.00 35.81 154
56 \w -161.00 -73.00 0.50 2.00 -- -86.25 -49.00 88.37 176
57 \w -160.00 -72.00 0.50 2.00 -- -86.25 -54.00 38.74 176
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.1195062000
_diffrn_orient_matrix_UB_12 -0.0385301000
_diffrn_orient_matrix_UB_13 -0.0275917000
_diffrn_orient_matrix_UB_21 0.0595102000
_diffrn_orient_matrix_UB_22 -0.1240044000
_diffrn_orient_matrix_UB_23 0.1224599000
_diffrn_orient_matrix_UB_31 -0.0559583000
_diffrn_orient_matrix_UB_32 -0.2144269000
_diffrn_orient_matrix_UB_33 -0.0659819000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage 0.802
_reflns_Friedel_fraction_full 0.997
_reflns_Friedel_fraction_max 0.970
_reflns_number_gt 3223
_reflns_number_total 3268
_reflns_odcompleteness_completeness 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 79.66
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.204
_refine_diff_density_min -0.136
_refine_diff_density_rms 0.033
_refine_ls_abs_structure_details
;
Flack x determined using 1425 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.03(5)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 205
_refine_ls_number_reflns 3268
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0249
_refine_ls_R_factor_gt 0.0246
_refine_ls_restrained_S_all 1.044
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.1159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0655
_refine_ls_wR_factor_ref 0.0656
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
O5(H5A,H5B)
2.b Ternary CH refined with riding coordinates:
C1(H1C), C2(H2), C12(H12)
2.c Secondary CH2 refined with riding coordinates:
N1(H1A,H1B), C13(H13A,H13B), C14(H14A,H14B)
2.d Aromatic/amide H refined with riding coordinates:
N2(H2A), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
2.e Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
2.f Idealised tetrahedral OH refined as rotating group:
O1(H1)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.36233(10) 0.63183(19) 0.82268(10) 0.0217(2) Uani 1 1 d . . . . .
H1 H 0.3939 0.5443 0.7872 0.033 Uiso 1 1 calc GR . . . .
O2 O 0.45666(11) 0.3683(2) 0.70244(10) 0.0306(3) Uani 1 1 d . . . . .
O3 O 0.57405(10) 0.21348(19) 0.88122(9) 0.0196(2) Uani 1 1 d . . . . .
O4 O 0.86010(11) -0.2218(2) 0.83263(11) 0.0256(3) Uani 1 1 d . . . . .
O5 O 1.02189(12) -0.1350(2) 1.07667(11) 0.0293(3) Uani 1 1 d . . . . .
H5A H 1.0501 -0.0085 1.1011 0.044 Uiso 1 1 d G . . . .
H5B H 0.9727 -0.1295 1.0016 0.044 Uiso 1 1 d G . . . .
N1 N 0.36998(11) 1.0452(2) 0.93810(11) 0.0156(2) Uani 1 1 d . . . . .
H1A H 0.3950 0.9283 0.9891 0.019 Uiso 1 1 calc R . . . .
H1B H 0.4371 1.0910 0.9210 0.019 Uiso 1 1 calc R . . . .
N2 N 0.76034(11) 0.1063(2) 0.79509(12) 0.0187(3) Uani 1 1 d . . . . .
H2A H 0.8178 0.1761 0.8558 0.022 Uiso 1 1 calc R . . . .
C1 C 0.32586(13) 0.8239(2) 0.75197(13) 0.0164(3) Uani 1 1 d . . . . .
H1C H 0.4032 0.8957 0.7498 0.020 Uiso 1 1 calc R . . . .
C2 C 0.26721(13) 0.9748(2) 0.81993(13) 0.0158(3) Uani 1 1 d . . . . .
H2 H 0.2334 1.1065 0.7679 0.019 Uiso 1 1 calc R . . . .
C3 C 0.16114(13) 0.8683(3) 0.84745(14) 0.0214(3) Uani 1 1 d . . . . .
H3A H 0.1955 0.7539 0.9092 0.032 Uiso 1 1 calc GR . . . .
H3B H 0.1006 0.8045 0.7718 0.032 Uiso 1 1 calc GR . . . .
H3C H 0.1188 0.9779 0.8790 0.032 Uiso 1 1 calc GR . . . .
C4 C 0.33182(15) 1.2229(3) 1.00359(15) 0.0235(3) Uani 1 1 d . . . . .
H4A H 0.3077 1.3517 0.9506 0.035 Uiso 1 1 calc GR . . . .
H4B H 0.4024 1.2593 1.0797 0.035 Uiso 1 1 calc GR . . . .
H4C H 0.2603 1.1744 1.0235 0.035 Uiso 1 1 calc GR . . . .
C5 C 0.23581(13) 0.7874(2) 0.62021(13) 0.0164(3) Uani 1 1 d . . . . .
C6 C 0.21765(14) 0.9537(2) 0.53407(14) 0.0190(3) Uani 1 1 d . . . . .
H6 H 0.2617 1.0872 0.5584 0.023 Uiso 1 1 calc R . . . .
C7 C 0.13549(15) 0.9251(3) 0.41288(14) 0.0216(3) Uani 1 1 d . . . . .
H7 H 0.1230 1.0393 0.3549 0.026 Uiso 1 1 calc R . . . .
C8 C 0.07161(14) 0.7291(3) 0.37662(14) 0.0229(3) Uani 1 1 d . . . . .
H8 H 0.0164 0.7087 0.2936 0.027 Uiso 1 1 calc R . . . .
C9 C 0.08861(14) 0.5641(3) 0.46157(14) 0.0235(3) Uani 1 1 d . . . . .
H9 H 0.0444 0.4308 0.4370 0.028 Uiso 1 1 calc R . . . .
C10 C 0.17063(14) 0.5929(3) 0.58338(14) 0.0203(3) Uani 1 1 d . . . . .
H10 H 0.1820 0.4791 0.6414 0.024 Uiso 1 1 calc R . . . .
C11 C 0.55185(13) 0.2692(2) 0.77137(13) 0.0168(3) Uani 1 1 d . . . . .
C12 C 0.64694(13) 0.2113(3) 0.71199(13) 0.0176(3) Uani 1 1 d . . . . .
H12 H 0.6706 0.3467 0.6785 0.021 Uiso 1 1 calc R . . . .
C13 C 0.59343(14) 0.0436(3) 0.60660(14) 0.0222(3) Uani 1 1 d . . . . .
H13A H 0.5008 0.0339 0.5791 0.027 Uiso 1 1 calc R . . . .
H13B H 0.6157 0.0835 0.5354 0.027 Uiso 1 1 calc R . . . .
C14 C 0.65528(14) -0.1711(3) 0.66342(15) 0.0231(3) Uani 1 1 d . . . . .
H14A H 0.5981 -0.2592 0.6904 0.028 Uiso 1 1 calc R . . . .
H14B H 0.6790 -0.2566 0.6038 0.028 Uiso 1 1 calc R . . . .
C15 C 0.77080(14) -0.1031(3) 0.77253(13) 0.0179(3) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0274(5) 0.0199(5) 0.0175(5) 0.0016(4) 0.0082(4) 0.0087(4)
O2 0.0307(6) 0.0397(7) 0.0218(5) 0.0037(5) 0.0101(5) 0.0189(5)
O3 0.0226(5) 0.0205(5) 0.0175(5) -0.0005(4) 0.0096(4) -0.0002(4)
O4 0.0234(5) 0.0267(6) 0.0241(5) 0.0031(5) 0.0059(4) 0.0091(4)
O5 0.0337(6) 0.0237(6) 0.0238(6) 0.0033(5) 0.0031(5) 0.0028(5)
N1 0.0167(5) 0.0161(6) 0.0147(5) -0.0001(4) 0.0067(4) 0.0007(4)
N2 0.0157(5) 0.0194(7) 0.0200(6) -0.0034(5) 0.0055(5) 0.0001(5)
C1 0.0166(6) 0.0176(7) 0.0159(6) -0.0002(5) 0.0070(5) 0.0010(5)
C2 0.0163(6) 0.0166(7) 0.0140(6) 0.0000(5) 0.0050(5) 0.0017(5)
C3 0.0166(6) 0.0279(8) 0.0210(7) -0.0006(6) 0.0086(5) 0.0002(6)
C4 0.0267(7) 0.0229(8) 0.0223(7) -0.0065(6) 0.0109(6) 0.0011(6)
C5 0.0154(6) 0.0199(7) 0.0153(6) -0.0011(5) 0.0073(5) 0.0006(5)
C6 0.0203(7) 0.0201(7) 0.0187(7) 0.0000(6) 0.0099(6) -0.0020(6)
C7 0.0215(7) 0.0266(8) 0.0179(7) 0.0039(6) 0.0088(6) 0.0018(6)
C8 0.0184(7) 0.0333(9) 0.0160(7) -0.0038(6) 0.0055(5) -0.0010(6)
C9 0.0218(7) 0.0250(8) 0.0232(7) -0.0058(6) 0.0080(6) -0.0042(6)
C10 0.0222(7) 0.0193(8) 0.0198(7) 0.0006(6) 0.0082(6) -0.0021(5)
C11 0.0196(6) 0.0152(7) 0.0167(6) -0.0020(5) 0.0081(5) 0.0007(5)
C12 0.0192(6) 0.0174(6) 0.0179(6) 0.0019(5) 0.0089(5) 0.0022(5)
C13 0.0231(7) 0.0271(8) 0.0151(7) -0.0009(6) 0.0057(5) 0.0076(6)
C14 0.0213(7) 0.0211(8) 0.0241(7) -0.0051(6) 0.0052(6) 0.0023(6)
C15 0.0188(7) 0.0201(7) 0.0169(6) 0.0012(5) 0.0091(5) 0.0020(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.8400 . ?
O1 C1 1.4127(18) . ?
O2 C11 1.2471(19) . ?
O3 C11 1.2621(18) . ?
O4 C15 1.2401(19) . ?
O5 H5A 0.8503 . ?
O5 H5B 0.8496 . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C2 1.5073(18) . ?
N1 C4 1.4914(19) . ?
N2 H2A 0.8800 . ?
N2 C12 1.4522(19) . ?
N2 C15 1.329(2) . ?
C1 H1C 1.0000 . ?
C1 C2 1.5324(19) . ?
C1 C5 1.5187(19) . ?
C2 H2 1.0000 . ?
C2 C3 1.519(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.396(2) . ?
C5 C10 1.390(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.390(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.392(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.396(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.5391(19) . ?
C12 H12 1.0000 . ?
C12 C13 1.548(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.528(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.515(2) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 H1 109.5 . . ?
H5A O5 H5B 109.5 . . ?
H1A N1 H1B 107.7 . . ?
C2 N1 H1A 108.8 . . ?
C2 N1 H1B 108.8 . . ?
C4 N1 H1A 108.8 . . ?
C4 N1 H1B 108.8 . . ?
C4 N1 C2 113.79(11) . . ?
C12 N2 H2A 122.5 . . ?
C15 N2 H2A 122.5 . . ?
C15 N2 C12 114.99(13) . . ?
O1 C1 H1C 108.2 . . ?
O1 C1 C2 107.02(11) . . ?
O1 C1 C5 114.32(12) . . ?
C2 C1 H1C 108.2 . . ?
C5 C1 H1C 108.2 . . ?
C5 C1 C2 110.69(11) . . ?
N1 C2 C1 107.83(11) . . ?
N1 C2 H2 108.6 . . ?
N1 C2 C3 110.03(11) . . ?
C1 C2 H2 108.6 . . ?
C3 C2 C1 113.07(12) . . ?
C3 C2 H2 108.6 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C1 119.14(14) . . ?
C10 C5 C1 121.65(13) . . ?
C10 C5 C6 119.20(13) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.40(14) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 119.96(14) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 119.95(14) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.13(15) . . ?
C10 C9 H9 119.9 . . ?
C5 C10 C9 120.34(14) . . ?
C5 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
O2 C11 O3 125.89(13) . . ?
O2 C11 C12 114.68(13) . . ?
O3 C11 C12 119.42(13) . . ?
N2 C12 C11 114.13(12) . . ?
N2 C12 H12 109.1 . . ?
N2 C12 C13 103.12(12) . . ?
C11 C12 H12 109.1 . . ?
C11 C12 C13 112.20(12) . . ?
C13 C12 H12 109.1 . . ?
C12 C13 H13A 110.9 . . ?
C12 C13 H13B 110.9 . . ?
H13A C13 H13B 108.9 . . ?
C14 C13 C12 104.29(12) . . ?
C14 C13 H13A 110.9 . . ?
C14 C13 H13B 110.9 . . ?
C13 C14 H14A 110.9 . . ?
C13 C14 H14B 110.9 . . ?
H14A C14 H14B 108.9 . . ?
C15 C14 C13 104.26(13) . . ?
C15 C14 H14A 110.9 . . ?
C15 C14 H14B 110.9 . . ?
O4 C15 N2 125.04(15) . . ?
O4 C15 C14 126.35(15) . . ?
N2 C15 C14 108.61(13) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 67.64(14) . . . . ?
O1 C1 C2 C3 -54.23(15) . . . . ?
O1 C1 C5 C6 -164.37(12) . . . . ?
O1 C1 C5 C10 15.91(19) . . . . ?
O2 C11 C12 N2 176.92(14) . . . . ?
O2 C11 C12 C13 -66.24(18) . . . . ?
O3 C11 C12 N2 -3.8(2) . . . . ?
O3 C11 C12 C13 113.00(15) . . . . ?
N2 C12 C13 C14 20.25(15) . . . . ?
C1 C5 C6 C7 -179.80(13) . . . . ?
C1 C5 C10 C9 -179.92(13) . . . . ?
C2 C1 C5 C6 74.69(16) . . . . ?
C2 C1 C5 C10 -105.03(15) . . . . ?
C4 N1 C2 C1 169.88(12) . . . . ?
C4 N1 C2 C3 -66.38(16) . . . . ?
C5 C1 C2 N1 -167.18(11) . . . . ?
C5 C1 C2 C3 70.95(15) . . . . ?
C5 C6 C7 C8 -0.6(2) . . . . ?
C6 C5 C10 C9 0.4(2) . . . . ?
C6 C7 C8 C9 0.9(2) . . . . ?
C7 C8 C9 C10 -0.6(2) . . . . ?
C8 C9 C10 C5 0.0(2) . . . . ?
C10 C5 C6 C7 -0.1(2) . . . . ?
C11 C12 C13 C14 -103.01(14) . . . . ?
C12 N2 C15 O4 -179.94(14) . . . . ?
C12 N2 C15 C14 -0.81(17) . . . . ?
C12 C13 C14 C15 -20.88(15) . . . . ?
C13 C14 C15 O4 -166.74(15) . . . . ?
C13 C14 C15 N2 14.15(16) . . . . ?
C15 N2 C12 C11 109.32(15) . . . . ?
C15 N2 C12 C13 -12.66(16) . . . . ?
_shelx_res_file
;
pn180815_uo_eph_1_180814_pyrolidcarbox.res created by SHELXL-2014/7
TITL pn180815_uo_eph_1_180814_pyrolidcarbox_a.res in P2(1)
REM Old TITL PN180815_UO_Eph_1_180814_PyrolidCarbox in P2(1)
REM SHELXT solution in P2(1)
REM R1 0.077, Rweak 0.028, Alpha 0.005, Orientation as input
REM Flack x = 0.157 ( 0.049 ) from Parsons' quotients
REM Formula found by SHELXT: C6 N2 O5
CELL 1.54184 11.47377 6.147468 11.71348 90 111.978 90
ZERR 2 0.00011 0.000053 0.00012 0 0.0011 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O
UNIT 30 48 4 10
L.S. 4
PLAN 5
TEMP -113
BOND $H
LIST 4
MORE -1
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.038500 0.115900
FVAR 11.06048
O1 4 0.362332 0.631833 0.822677 11.00000 0.02742 0.01986 =
0.01753 0.00159 0.00820 0.00871
AFIX 147
H1 2 0.393875 0.544308 0.787212 11.00000 -1.50000
AFIX 0
O2 4 0.456664 0.368258 0.702444 11.00000 0.03074 0.03968 =
0.02176 0.00368 0.01014 0.01889
O3 4 0.574049 0.213476 0.881223 11.00000 0.02258 0.02052 =
0.01752 -0.00054 0.00964 -0.00017
O4 4 0.860102 -0.221788 0.832632 11.00000 0.02344 0.02668 =
0.02412 0.00309 0.00591 0.00910
AFIX 6
O5 4 1.021893 -0.135049 1.076675 11.00000 0.03372 0.02367 =
0.02378 0.00327 0.00306 0.00276
H5A 2 1.050138 -0.008456 1.101096 11.00000 -1.50000
H5B 2 0.972728 -0.129518 1.001576 11.00000 -1.50000
AFIX 0
N1 3 0.369979 1.045228 0.938099 11.00000 0.01669 0.01607 =
0.01475 -0.00014 0.00665 0.00073
AFIX 23
H1A 2 0.395033 0.928259 0.989105 11.00000 -1.20000
H1B 2 0.437103 1.091025 0.920990 11.00000 -1.20000
AFIX 0
N2 3 0.760335 0.106282 0.795085 11.00000 0.01573 0.01939 =
0.02003 -0.00342 0.00551 0.00008
AFIX 43
H2A 2 0.817813 0.176126 0.855837 11.00000 -1.20000
AFIX 0
C1 1 0.325865 0.823899 0.751974 11.00000 0.01655 0.01756 =
0.01589 -0.00018 0.00703 0.00099
AFIX 13
H1C 2 0.403237 0.895666 0.749837 11.00000 -1.20000
AFIX 0
C2 1 0.267213 0.974809 0.819932 11.00000 0.01635 0.01660 =
0.01395 -0.00002 0.00503 0.00166
AFIX 13
H2 2 0.233389 1.106454 0.767898 11.00000 -1.20000
AFIX 0
C3 1 0.161141 0.868346 0.847449 11.00000 0.01663 0.02788 =
0.02097 -0.00062 0.00859 0.00016
AFIX 137
H3A 2 0.195487 0.753939 0.909246 11.00000 -1.50000
H3B 2 0.100649 0.804509 0.771813 11.00000 -1.50000
H3C 2 0.118849 0.977899 0.879043 11.00000 -1.50000
AFIX 0
C4 1 0.331823 1.222877 1.003594 11.00000 0.02666 0.02294 =
0.02228 -0.00645 0.01087 0.00110
AFIX 137
H4A 2 0.307704 1.351671 0.950584 11.00000 -1.50000
H4B 2 0.402412 1.259254 1.079710 11.00000 -1.50000
H4C 2 0.260282 1.174438 1.023524 11.00000 -1.50000
AFIX 0
C5 1 0.235810 0.787389 0.620207 11.00000 0.01542 0.01994 =
0.01528 -0.00105 0.00731 0.00064
C6 1 0.217653 0.953689 0.534065 11.00000 0.02035 0.02006 =
0.01875 0.00004 0.00988 -0.00196
AFIX 43
H6 2 0.261709 1.087192 0.558408 11.00000 -1.20000
AFIX 0
C7 1 0.135491 0.925105 0.412879 11.00000 0.02151 0.02659 =
0.01794 0.00394 0.00876 0.00182
AFIX 43
H7 2 0.122964 1.039323 0.354855 11.00000 -1.20000
AFIX 0
C8 1 0.071609 0.729084 0.376621 11.00000 0.01845 0.03332 =
0.01600 -0.00379 0.00547 -0.00101
AFIX 43
H8 2 0.016361 0.708659 0.293564 11.00000 -1.20000
AFIX 0
C9 1 0.088607 0.564059 0.461574 11.00000 0.02183 0.02498 =
0.02321 -0.00579 0.00801 -0.00415
AFIX 43
H9 2 0.044365 0.430781 0.436978 11.00000 -1.20000
AFIX 0
C10 1 0.170631 0.592924 0.583376 11.00000 0.02225 0.01932 =
0.01978 0.00065 0.00824 -0.00209
AFIX 43
H10 2 0.181988 0.479109 0.641422 11.00000 -1.20000
AFIX 0
C11 1 0.551854 0.269238 0.771368 11.00000 0.01960 0.01524 =
0.01668 -0.00197 0.00812 0.00074
C12 1 0.646940 0.211288 0.711989 11.00000 0.01916 0.01741 =
0.01792 0.00194 0.00893 0.00219
AFIX 13
H12 2 0.670569 0.346721 0.678514 11.00000 -1.20000
AFIX 0
C13 1 0.593430 0.043605 0.606597 11.00000 0.02310 0.02715 =
0.01506 -0.00091 0.00574 0.00758
AFIX 23
H13A 2 0.500825 0.033902 0.579093 11.00000 -1.20000
H13B 2 0.615668 0.083468 0.535392 11.00000 -1.20000
AFIX 0
C14 1 0.655283 -0.171058 0.663425 11.00000 0.02132 0.02111 =
0.02410 -0.00514 0.00518 0.00231
AFIX 23
H14A 2 0.598078 -0.259249 0.690422 11.00000 -1.20000
H14B 2 0.678981 -0.256581 0.603809 11.00000 -1.20000
AFIX 0
C15 1 0.770805 -0.103111 0.772526 11.00000 0.01882 0.02013 =
0.01689 0.00124 0.00908 0.00200
HKLF 4
REM pn180815_uo_eph_1_180814_pyrolidcarbox_a.res in P2(1)
REM R1 = 0.0246 for 3223 Fo > 4sig(Fo) and 0.0249 for all 3268 data
REM 205 parameters refined using 1 restraints
END
WGHT 0.0385 0.1159
REM Highest difference peak 0.204, deepest hole -0.136, 1-sigma level 0.033
Q1 1 0.6022 0.2294 0.7397 11.00000 0.05 0.20
Q2 1 0.2667 0.8063 0.6815 11.00000 0.05 0.19
Q3 1 0.2917 0.8985 0.7872 11.00000 0.05 0.16
Q4 1 0.6252 0.1296 0.6565 11.00000 0.05 0.15
Q5 1 0.4346 -0.2711 0.6237 11.00000 0.05 0.12
;
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12 3 -9 9113.19 266.039 19
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-12 3 8 10916.9 352.452 11
12 3 -8 10724.8 312.758 19
-12 3 7 7348.16 287.038 11
-12 3 7 7337.72 252.862 54
-12 3 7 7928.29 287.890 13
-12 3 6 3696.87 197.961 11
-12 3 6 3356.12 155.449 57
-12 3 6 3207.18 156.014 55
-12 3 6 3482.84 202.966 8
-12 3 6 3926.03 196.301 13
-12 3 5 330.864 93.9250 11
-12 3 5 331.406 69.5613 57
-12 3 5 327.514 67.1900 55
-12 3 5 274.133 65.8074 54
-12 3 5 388.734 104.722 8
-12 3 5 480.313 94.9063 13
-12 3 4 4870.51 209.626 21
-12 3 4 4914.75 202.718 57
-12 3 4 4918.28 199.450 54
-12 3 4 5005.53 245.528 8
-12 3 4 4825.63 229.587 13
-12 3 3 8585.83 288.910 21
-12 3 3 8682.04 288.762 55
-12 3 3 8604.35 281.304 54
-12 3 3 8646.65 334.063 8
-12 3 3 8594.09 319.278 13
-12 3 2 5561.27 207.514 21
-12 3 2 5736.67 215.518 57
-12 3 2 5611.62 208.683 55
-12 3 2 5653.76 197.928 54
-12 3 2 5600.44 250.089 8
-12 3 2 5663.28 240.207 13
-12 3 1 6356.06 253.631 3
-12 3 1 5552.74 203.645 57
-12 3 1 5709.82 240.945 8
-12 3 1 6230.61 239.588 13
-12 3 1 5736.86 219.759 45
-12 3 0 3717.38 170.403 3
-12 3 0 3051.20 130.394 45
-12 3 -1 5600.03 190.682 3
-12 4 8 1490.42 75.4860 13
-12 4 7 478.572 59.5018 13
-12 4 6 2304.10 113.993 21
-12 4 6 2297.69 120.512 13
-12 4 5 1598.62 97.6865 21
-12 4 5 1492.95 83.0424 20
-12 4 5 1671.36 107.552 13
-12 4 4 2601.69 121.984 21
-12 4 4 2571.28 105.696 20
-12 4 4 2526.54 126.947 3
-12 4 4 2702.89 134.388 13
-12 4 3 668.424 64.3956 21
-12 4 3 618.694 72.8087 3
-12 4 3 727.289 74.0083 13
-12 4 2 648.115 53.9206 21
-12 4 2 776.081 67.6026 3
-12 4 2 767.367 69.2014 13
-13 -3 8 855.122 68.2558 40
-13 -3 7 3476.61 153.972 40
13 -3 -7 3259.67 139.088 26
-13 -3 7 3319.41 135.814 41
-13 -3 6 4985.45 200.001 40
13 -3 -6 4667.86 186.390 26
-13 -3 6 5071.42 179.006 41
-13 -3 5 2318.68 137.022 40
13 -3 -5 2236.16 99.5895 36
13 -3 -5 2602.34 130.980 26
-13 -3 5 2564.74 116.387 41
-13 -3 4 5790.81 221.151 40
-13 -3 3 419.208 66.8929 40
13 -3 -3 403.851 54.6362 24
-13 -3 2 626.001 63.0205 40
13 -2 -10 2774.02 111.974 26
13 -2 -9 19438.6 498.300 26
-13 -2 9 17266.9 489.631 41
13 -2 -8 1925.35 125.854 26
-13 -2 8 1870.38 128.652 41
-13 -2 7 3445.03 172.602 4
13 -2 -7 3877.23 189.984 26
-13 -2 7 3526.51 184.233 41
-13 -2 6 4095.09 198.764 4
-13 -2 6 4074.64 205.055 41
-13 -2 5 3887.53 197.799 4
-13 -2 5 4025.22 203.424 41
-13 -2 4 6607.70 268.160 4
13 -2 -4 7002.97 272.279 26
-13 -2 4 7231.01 278.400 41
-13 -2 3 415.532 81.8340 41
-13 -2 3 354.465 86.4277 39
-13 -2 2 5664.33 235.706 39
-13 -2 1 9271.77 300.044 39
-13 -2 0 835.137 66.9600 40
13 -1 -11 1075.44 64.6916 26
-13 -1 10 2494.50 134.278 4
-13 -1 10 2542.35 122.518 41
-13 -1 9 2400.48 139.526 41
-13 -1 9 2196.40 147.214 4
-13 -1 8 626.517 100.528 41
13 -1 -8 464.599 57.1653 35
-13 -1 8 476.879 78.0446 54
-13 -1 8 622.310 106.427 4
-13 -1 7 3917.06 191.363 54
-13 -1 7 4039.16 225.431 4
13 -1 -7 4265.43 213.817 26
-13 -1 7 3604.68 206.543 41
-13 -1 6 13758.5 434.814 54
-13 -1 6 14204.7 488.643 4
13 -1 -6 14624.2 467.390 26
-13 -1 5 760.187 114.266 41
-13 -1 5 914.140 100.505 54
13 -1 -5 951.176 115.984 26
-13 -1 5 876.449 137.836 4
-13 -1 4 2157.21 171.156 40
-13 -1 4 2515.55 141.342 54
-13 -1 4 2422.10 191.292 4
13 -1 -4 2459.04 158.010 26
-13 -1 4 2411.86 175.288 41
-13 -1 3 14.1937 79.9259 41
-13 -1 3 35.6294 82.0239 40
-13 -1 3 107.126 95.6581 4
13 -1 -3 62.5669 59.9255 26
-13 -1 2 3561.69 192.145 40
-13 -1 2 3655.51 214.724 39
-13 -1 1 6133.81 240.346 40
-13 -1 1 5702.82 254.378 39
-13 -1 0 2917.84 138.060 40
-13 -1 0 3386.15 164.203 39
-13 -1 -1 2760.32 119.752 39
-13 0 11 115.582 46.0153 4
-13 0 10 14920.7 413.160 11
-13 0 10 15041.4 450.882 4
-13 0 9 3511.04 166.793 11
-13 0 9 3256.34 156.588 54
-13 0 9 3832.50 206.134 4
-13 0 9 3400.11 157.010 41
-13 0 8 3338.51 173.744 11
-13 0 8 3544.24 170.989 8
-13 0 8 3377.46 212.085 4
-13 0 8 2919.71 167.445 41
-13 0 7 3254.09 177.076 11
-13 0 7 3426.96 178.353 57
-13 0 7 3401.64 179.123 54
-13 0 7 3461.85 182.189 8
-13 0 7 3354.74 224.738 4
13 0 -7 2842.61 172.809 26
-13 0 7 3594.93 192.804 41
-13 0 6 1468.80 122.027 11
-13 0 6 1439.66 119.167 54
-13 0 6 1354.14 130.476 8
-13 0 6 1455.63 164.728 4
13 0 -6 1336.22 121.114 26
-13 0 6 1320.29 135.820 41
-13 0 5 10845.4 364.710 11
-13 0 5 10482.2 379.320 40
-13 0 5 11220.7 376.064 57
-13 0 5 10936.1 373.923 55
-13 0 5 10886.8 361.260 54
-13 0 5 11251.9 387.936 8
-13 0 5 11207.6 439.835 4
13 0 -5 10631.3 364.897 26
-13 0 5 11305.3 402.628 41
-13 0 4 5763.28 234.414 11
-13 0 4 5931.58 257.604 40
-13 0 4 6136.24 250.144 57
-13 0 4 5697.49 242.908 55
-13 0 4 5641.17 230.119 54
-13 0 4 5945.59 306.119 4
-13 0 4 6136.37 267.356 8
13 0 -4 5565.04 229.447 26
-13 0 4 6166.38 280.714 41
-13 0 3 707.309 109.828 41
-13 0 3 577.200 91.9708 40
-13 0 3 640.716 89.6515 57
-13 0 3 650.187 89.1327 55
-13 0 3 678.721 104.538 8
-13 0 3 785.469 137.480 4
-13 0 2 190.173 71.7752 40
-13 0 2 371.884 106.615 39
-13 0 2 166.024 59.4538 57
-13 0 2 192.169 80.9032 8
-13 0 1 7482.05 244.133 40
-13 0 1 7511.69 299.135 39
-13 0 0 3977.17 185.546 39
-13 0 0 4016.38 184.595 45
-13 0 -1 14.7103 38.9759 39
-13 0 -1 11.4075 39.3338 45
-13 1 11 1148.89 67.2918 11
-13 1 10 2710.89 133.837 11
-13 1 10 2699.03 144.473 4
-13 1 9 2129.64 137.952 11
-13 1 9 2745.82 162.960 4
-13 1 8 589.988 93.5178 11
-13 1 8 476.117 73.4769 54
-13 1 8 662.342 106.754 4
-13 1 7 4279.68 213.278 11
-13 1 7 4207.07 188.028 57
-13 1 7 3748.98 182.283 55
-13 1 7 4174.42 189.794 54
-13 1 7 4566.41 224.428 8
-13 1 7 4224.39 234.538 4
13 1 -7 3622.04 161.647 26
-13 1 7 4045.23 176.103 41
-13 1 6 14038.9 461.845 11
-13 1 6 13748.3 431.745 57
-13 1 6 14191.9 432.275 54
-13 1 6 15377.8 483.676 8
-13 1 6 15081.3 504.743 4
-13 1 6 14292.5 434.852 41
-13 1 5 857.873 110.534 11
-13 1 5 855.275 97.9795 55
-13 1 5 902.976 94.7030 54
-13 1 5 1067.73 131.724 8
-13 1 5 846.061 136.874 4
-13 1 5 995.716 106.406 41
-13 1 4 2331.98 161.575 11
-13 1 4 2325.79 147.382 57
-13 1 4 2485.79 147.951 55
-13 1 4 2549.15 143.019 54
-13 1 4 2329.96 187.147 4
-13 1 4 2271.58 175.083 8
-13 1 3 99.0430 62.2693 57
-13 1 3 14.9785 57.7185 55
-13 1 3 37.5456 50.4262 54
-13 1 3 7.26400 81.0717 8
-13 1 3 74.7181 103.779 4
-13 1 2 3586.14 190.413 39
-13 1 2 3564.88 163.577 57
-13 1 2 3681.70 160.947 55
-13 1 2 3408.84 198.709 8
-13 1 1 6367.28 237.520 39
-13 1 1 6596.83 227.099 3
-13 1 1 5884.37 255.173 8
-13 1 0 2912.68 154.969 45
-13 1 -1 2876.06 123.402 45
-13 2 10 2947.39 122.288 8
-13 2 8 1797.20 124.192 11
-13 2 8 1785.56 116.344 4
-13 2 8 1923.45 132.249 8
-13 2 7 3684.85 185.304 11
-13 2 7 3412.46 177.871 4
-13 2 7 3763.42 195.447 8
-13 2 6 4020.87 201.335 11
-13 2 6 4020.92 173.873 57
-13 2 6 3930.17 172.824 55
-13 2 6 3853.43 173.348 54
-13 2 6 4046.03 196.387 4
-13 2 6 4459.46 219.100 8
-13 2 6 4183.16 174.539 13
-13 2 5 3863.40 199.173 11
-13 2 5 3841.06 174.711 57
-13 2 5 3845.55 168.456 54
-13 2 5 3436.96 189.842 4
-13 2 5 4062.47 212.936 8
-13 2 5 3967.68 170.838 13
-13 2 4 7300.24 279.219 11
-13 2 4 6996.73 248.524 57
-13 2 4 6940.75 246.021 55
-13 2 4 6503.45 266.561 4
-13 2 4 6618.97 236.391 54
-13 2 4 7379.38 294.209 8
-13 2 4 7070.22 244.599 13
-13 2 3 454.893 68.6266 57
-13 2 3 486.329 67.2429 55
-13 2 3 471.161 93.4202 8
-13 2 3 436.618 65.3264 13
-13 2 2 6367.73 243.182 3
-13 2 2 5804.54 248.009 8
-13 2 1 9963.56 301.301 3
-13 2 1 9319.07 306.340 45
-13 2 0 731.238 63.1886 45
-13 3 8 861.752 65.5184 8
-13 3 7 3047.92 133.084 11
-13 3 7 3339.37 144.139 8
-13 3 7 3275.42 127.991 13
-13 3 6 5220.48 198.009 8
-13 3 6 4917.82 178.743 13
-13 3 6 4964.41 188.749 11
-13 3 5 2391.46 133.720 8
-13 3 5 2558.05 121.739 13
-13 3 4 5828.45 215.741 8
-13 3 4 5743.91 199.934 13
-13 3 3 334.155 66.3826 3
-13 3 3 402.460 62.0059 8
-13 3 3 373.804 52.2944 13
-13 3 2 781.629 68.3991 3
-14 -2 7 3668.22 133.235 41
-14 -2 6 3579.20 142.984 40
14 -2 -6 3520.49 134.949 26
-14 -2 6 3936.20 142.946 41
-14 -2 5 13808.6 373.761 40
-14 -2 4 2113.19 98.9310 40
-14 -1 8 81.2864 39.0233 41
14 -1 -8 99.3159 36.4353 26
-14 -1 8 99.3041 47.2694 4
-14 -1 7 5500.60 197.081 40
-14 -1 7 5547.79 212.514 4
14 -1 -7 5536.76 193.739 26
-14 -1 7 5956.46 208.894 41
-14 -1 6 6903.94 230.174 40
-14 -1 6 6228.38 241.207 4
14 -1 -6 6612.14 219.249 26
-14 -1 5 1633.02 102.371 40
-14 -1 5 1470.52 114.473 4
14 -1 -5 1362.15 83.9765 26
-14 -1 4 3508.97 146.393 40
-14 -1 4 3593.77 171.191 39
-14 -1 3 7647.28 259.118 39
-14 -1 2 2998.19 127.655 39
-14 0 9 722.232 68.2391 4
-14 0 8 23004.2 608.794 4
-14 0 7 277.223 54.3399 41
-14 0 7 271.808 75.0398 4
-14 0 6 4695.24 217.747 4
-14 0 6 4837.09 191.227 41
-14 0 5 1974.73 144.936 4
-14 0 4 13063.4 412.761 4
-14 0 3 20591.6 551.821 39
-14 0 2 5877.83 197.116 39
-14 0 2 5736.73 193.413 45
-14 1 8 144.416 40.0531 11
-14 1 8 142.667 42.0715 8
-14 1 8 46.8656 44.8036 4
-14 1 7 5723.51 196.995 11
-14 1 7 5835.91 220.492 4
-14 1 7 5748.62 204.150 8
-14 1 6 6795.39 224.713 11
-14 1 6 6592.87 248.719 4
-14 1 6 7042.50 240.044 8
-14 1 5 1547.90 116.850 4
-14 1 5 1756.85 113.065 8
-14 1 4 3024.88 129.957 39
-14 1 4 3463.38 154.493 8
-14 1 3 6653.00 225.794 8
-14 1 2 2866.18 124.041 45
-14 2 7 3779.11 139.340 8
-14 2 6 3873.84 151.115 8
-14 2 5 12939.6 358.775 8
-14 2 4 2045.28 103.134 8
0 0 0 0.00 0.00 0
TITL PN180815_UO_Eph_1_180814_PyrolidCarbox in P2(1)
REM P2(1) (#4 in standard setting)
CELL 1.54184 11.473774 6.147468 11.713480 90.0000 111.9780 90.0000
ZERR 2.00 0.000110 0.000053 0.000118 0.0000 0.0011 0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C H N O
UNIT 30.00 50.00 4.00 10.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 49217
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.788
data_pn180815_uo_traz_1_180814_c6_nitrate_mo
_audit_creation_date 2018-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number '2014/7'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C19 H23 Cl N5 O, N O3'
_chemical_formula_sum 'C19 H23 Cl N6 O4'
_chemical_formula_weight 434.88
_chemical_melting_point ?
_chemical_oxdiff_formula 'C20 H23 Cl N5 O4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system 'monoclinic'
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 12.6065(3)
_cell_length_b 13.0726(3)
_cell_length_c 12.6694(3)
_cell_angle_alpha 90
_cell_angle_beta 106.397(3)
_cell_angle_gamma 90
_cell_volume 2003.00(8)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 14972
_cell_measurement_temperature 160.00(10)
_cell_measurement_theta_max 32.9840
_cell_measurement_theta_min 2.5610
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.231
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.560
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.442
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-17 0 1 0.0991
17 0 -1 0.0891
-6 17 4 0.2266
-8 -1 18 0.0840
8 1 -18 0.0840
9 4 11 0.1430
2 -5 -17 0.0752
-12 -8 -6 0.1429
-8 2 17 0.0941
-12 0 16 0.0891
-16 -4 10 0.1246
3 7 15 0.1539
17 5 -8 0.1506
-8 -5 17 0.1142
5 5 -17 0.1043
13 0 8 0.1163
-14 -1 -6 0.0893
-5 10 15 0.1493
1 -13 -13 0.1569
-7 -14 -8 0.1646
-3 18 -3 0.2371
-13 13 3 0.1948
0 -18 4 0.2683
-9 -15 8 0.1943
-9 14 9 0.1882
-3 -9 15 0.1573
-10 -9 15 0.1297
_exptl_crystal_size_max 0.533
_exptl_crystal_size_mid 0.204
_exptl_crystal_size_min 0.168
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-16.9708 0.0097 0.9997 0.5067 0.0969 0.8347
16.9708 -0.0097 -0.9997 -0.5067 -0.0969 -0.8347
-5.9890 16.9709 4.0133 0.5589 -0.8096 0.1047
-7.9809 -1.0180 17.9720 -0.5383 -0.5631 0.6612
7.9809 1.0180 -17.9720 0.5383 0.5631 -0.6612
8.9880 3.9725 10.9871 -0.6326 -0.6458 -0.3319
1.9916 -4.9698 -16.9798 0.5008 0.8234 -0.2715
-11.9813 -7.9710 -5.9989 0.3910 0.6507 0.6062
-7.9813 1.9785 16.9769 -0.4014 -0.6511 0.6039
-11.9748 -0.0143 15.9764 -0.2926 -0.4991 0.8109
-15.9697 -3.9969 9.9814 -0.0342 -0.0782 0.9740
2.9993 6.9660 14.9847 -0.5143 -0.8720 -0.0272
16.9686 4.9919 -7.9834 -0.0517 -0.0456 -1.0076
-7.9811 -5.0102 16.9690 -0.6217 -0.3593 0.7038
4.9862 5.0121 -16.9688 0.7187 0.3830 -0.5591
12.9804 -0.0195 7.9869 -0.7602 -0.3993 -0.5112
-13.9780 -0.9810 -5.9910 0.6759 0.3747 0.6027
-4.9872 9.9664 14.9887 -0.1614 -0.9339 0.3159
0.9946 -12.9617 -12.9948 0.1112 1.0163 -0.0511
-6.9902 -13.9618 -8.0030 0.1256 0.9355 0.4217
-2.9962 17.9770 -2.9751 0.7911 -0.6152 -0.1558
-12.9773 12.9833 3.0109 0.7017 -0.5506 0.4850
0.0016 -17.9765 3.9738 -0.7367 0.6018 0.3151
-8.9820 -14.9810 7.9717 -0.5216 0.3993 0.7644
-8.9823 13.9708 9.0026 0.3488 -0.8465 0.3648
-2.9902 -9.0042 14.9673 -0.8242 -0.1578 0.4907
-9.9783 -8.9997 14.9678 -0.5980 -0.1026 0.8285
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0196
_diffrn_reflns_av_unetI/netI 0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 21495
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 33.232
_diffrn_reflns_theta_min 2.288
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 160.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
--------------------------------------------------------------------------
1 \w -1.00 66.00 0.50 45.00 -- 10.11 38.00 -30.00 134
2 \w -6.00 61.00 0.50 45.00 -- -11.36 38.00 60.00 134
3 \w -37.00 15.00 0.50 45.00 -- 10.11 -57.00 -60.00 104
4 \w -12.00 24.00 0.50 45.00 -- 10.11 -57.00-180.00 72
5 \w -55.00 2.00 0.50 45.00 -- 10.11 -57.00 -90.00 114
6 \w -37.00 -1.00 0.50 45.00 -- -11.36 -57.00 -90.00 72
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0323458000
_diffrn_orient_matrix_UB_12 0.0315766000
_diffrn_orient_matrix_UB_13 -0.0425298000
_diffrn_orient_matrix_UB_21 -0.0079284000
_diffrn_orient_matrix_UB_22 -0.0417034000
_diffrn_orient_matrix_UB_23 -0.0372172000
_diffrn_orient_matrix_UB_31 -0.0483361000
_diffrn_orient_matrix_UB_32 -0.0143217000
_diffrn_orient_matrix_UB_33 0.0145148000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5530
_reflns_number_total 6532
_reflns_odcompleteness_completeness 96.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 30.44
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.400
_refine_diff_density_min -0.294
_refine_diff_density_rms 0.045
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 274
_refine_ls_number_reflns 6532
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0429
_refine_ls_R_factor_gt 0.0357
_refine_ls_restrained_S_all 1.053
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+0.3895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1017
_refine_ls_wR_factor_ref 0.1059
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,
H16B), C18(H18A,H18B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C21(H21), C23(H23), C24(H24), C25(H25)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl26 Cl 0.82838(3) 1.05094(2) 0.83765(2) 0.03897(8) Uani 1 1 d . . . . .
O10 O 0.09502(7) 0.67054(7) 0.12314(7) 0.03800(18) Uani 1 1 d . . . . .
O28 O 0.43563(8) 0.51734(7) 0.27552(7) 0.0426(2) Uani 1 1 d . . . . .
O29 O 0.53436(7) 0.39815(5) 0.37420(6) 0.03386(17) Uani 1 1 d . . . . .
O30 O 0.55841(8) 0.55663(6) 0.42729(8) 0.0445(2) Uani 1 1 d . . . . .
N2 N 0.03849(7) 0.65742(6) 0.28322(7) 0.02562(16) Uani 1 1 d . . . . .
N3 N -0.04645(7) 0.69337(7) 0.32215(6) 0.02694(16) Uani 1 1 d . . . . .
N8 N -0.06210(6) 0.74893(6) 0.15201(6) 0.02094(14) Uani 1 1 d . . . . .
N14 N 0.39661(6) 0.72816(6) 0.41840(6) 0.02118(14) Uani 1 1 d . . . . .
H14 H 0.4366(10) 0.6718(10) 0.4492(10) 0.025 Uiso 1 1 d R . . . .
N17 N 0.56757(6) 0.88233(6) 0.49464(6) 0.02097(14) Uani 1 1 d . . . . .
N27 N 0.51008(7) 0.49074(6) 0.35862(7) 0.02418(15) Uani 1 1 d . . . . .
C1 C 0.03291(8) 0.68863(7) 0.17939(7) 0.02428(17) Uani 1 1 d . . . . .
C4 C -0.20601(9) 0.80342(8) 0.22989(9) 0.0313(2) Uani 1 1 d . . . . .
H4 H -0.2392 0.8051 0.2885 0.038 Uiso 1 1 calc R . . . .
C5 C -0.25250(9) 0.85343(8) 0.13448(10) 0.0338(2) Uani 1 1 d . . . . .
H5 H -0.3193 0.8902 0.1263 0.041 Uiso 1 1 calc R . . . .
C6 C -0.20331(9) 0.85218(8) 0.04575(9) 0.0312(2) Uani 1 1 d . . . . .
H6 H -0.2375 0.8882 -0.0202 0.037 Uiso 1 1 calc R . . . .
C7 C -0.10896(8) 0.80034(8) 0.05485(7) 0.02650(18) Uani 1 1 d . . . . .
H7 H -0.0757 0.7992 -0.0037 0.032 Uiso 1 1 calc R . . . .
C9 C -0.10625(8) 0.74827(7) 0.24034(7) 0.02249(16) Uani 1 1 d . . . . .
C11 C 0.11892(9) 0.58567(8) 0.34778(10) 0.0339(2) Uani 1 1 d . . . . .
H11A H 0.1424 0.5388 0.2973 0.041 Uiso 1 1 calc R . . . .
H11B H 0.0833 0.5440 0.3935 0.041 Uiso 1 1 calc R . . . .
C12 C 0.22069(8) 0.63785(8) 0.42241(9) 0.0301(2) Uani 1 1 d . . . . .
H12A H 0.1978 0.6877 0.4706 0.036 Uiso 1 1 calc R . . . .
H12B H 0.2690 0.5862 0.4697 0.036 Uiso 1 1 calc R . . . .
C13 C 0.28392(8) 0.69255(7) 0.35340(7) 0.02533(17) Uani 1 1 d . . . . .
H13A H 0.2919 0.6458 0.2946 0.030 Uiso 1 1 calc R . . . .
H13B H 0.2403 0.7524 0.3175 0.030 Uiso 1 1 calc R . . . .
C15 C 0.39353(8) 0.80252(7) 0.50691(7) 0.02247(16) Uani 1 1 d . . . . .
H15A H 0.3591 0.7695 0.5594 0.027 Uiso 1 1 calc R . . . .
H15B H 0.3473 0.8619 0.4739 0.027 Uiso 1 1 calc R . . . .
C16 C 0.50821(8) 0.83947(7) 0.56830(7) 0.02320(17) Uani 1 1 d . . . . .
H16A H 0.5021 0.8923 0.6223 0.028 Uiso 1 1 calc R . . . .
H16B H 0.5512 0.7815 0.6095 0.028 Uiso 1 1 calc R . . . .
C18 C 0.56703(8) 0.81464(7) 0.40203(7) 0.02380(17) Uani 1 1 d . . . . .
H18A H 0.6145 0.7546 0.4298 0.029 Uiso 1 1 calc R . . . .
H18B H 0.5987 0.8516 0.3498 0.029 Uiso 1 1 calc R . . . .
C19 C 0.45226(8) 0.77845(7) 0.34223(7) 0.02467(17) Uani 1 1 d . . . . .
H19A H 0.4074 0.8375 0.3062 0.030 Uiso 1 1 calc R . . . .
H19B H 0.4567 0.7293 0.2841 0.030 Uiso 1 1 calc R . . . .
C20 C 0.66838(7) 0.93099(6) 0.54464(7) 0.02075(16) Uani 1 1 d . . . . .
C21 C 0.69872(8) 0.95883(7) 0.65659(7) 0.02364(17) Uani 1 1 d . . . . .
H21 H 0.6526 0.9413 0.7015 0.028 Uiso 1 1 calc R . . . .
C22 C 0.79649(8) 1.01202(7) 0.70079(8) 0.02620(18) Uani 1 1 d . . . . .
C23 C 0.86837(9) 1.03794(8) 0.64059(9) 0.0299(2) Uani 1 1 d . . . . .
H23 H 0.9352 1.0737 0.6731 0.036 Uiso 1 1 calc R . . . .
C24 C 0.83867(9) 1.00945(8) 0.53037(9) 0.0305(2) Uani 1 1 d . . . . .
H24 H 0.8865 1.0258 0.4867 0.037 Uiso 1 1 calc R . . . .
C25 C 0.74116(8) 0.95790(7) 0.48290(8) 0.02630(18) Uani 1 1 d . . . . .
H25 H 0.7229 0.9403 0.4071 0.032 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl26 0.04455(17) 0.04064(15) 0.02811(12) -0.00800(9) 0.00436(10) -0.00862(11)
O10 0.0306(4) 0.0492(5) 0.0372(4) -0.0083(3) 0.0144(3) 0.0088(3)
O28 0.0528(5) 0.0350(4) 0.0297(4) 0.0042(3) -0.0052(3) 0.0083(4)
O29 0.0411(4) 0.0230(3) 0.0345(4) -0.0015(3) 0.0059(3) 0.0092(3)
O30 0.0398(5) 0.0305(4) 0.0524(5) -0.0118(3) -0.0043(4) -0.0073(3)
N2 0.0215(4) 0.0264(4) 0.0261(3) 0.0030(3) 0.0021(3) 0.0021(3)
N3 0.0254(4) 0.0323(4) 0.0233(3) 0.0022(3) 0.0072(3) -0.0012(3)
N8 0.0197(4) 0.0242(3) 0.0187(3) -0.0010(3) 0.0049(3) 0.0018(3)
N14 0.0211(4) 0.0176(3) 0.0228(3) 0.0009(2) 0.0029(3) 0.0021(3)
N17 0.0249(4) 0.0190(3) 0.0206(3) -0.0010(2) 0.0090(3) -0.0019(3)
N27 0.0233(4) 0.0220(3) 0.0268(3) 0.0000(3) 0.0063(3) -0.0006(3)
C1 0.0207(4) 0.0269(4) 0.0240(4) -0.0036(3) 0.0044(3) 0.0020(3)
C4 0.0259(5) 0.0313(5) 0.0408(5) -0.0051(4) 0.0158(4) 0.0014(4)
C5 0.0218(5) 0.0252(4) 0.0516(6) -0.0011(4) 0.0060(4) 0.0032(3)
C6 0.0276(5) 0.0240(4) 0.0346(5) 0.0043(4) -0.0033(4) -0.0021(3)
C7 0.0277(5) 0.0285(4) 0.0202(4) 0.0013(3) 0.0018(3) -0.0035(3)
C9 0.0219(4) 0.0240(4) 0.0228(4) -0.0021(3) 0.0083(3) -0.0014(3)
C11 0.0249(5) 0.0246(4) 0.0434(5) 0.0098(4) -0.0046(4) -0.0016(4)
C12 0.0238(5) 0.0297(4) 0.0313(4) 0.0093(4) -0.0012(4) -0.0029(3)
C13 0.0209(4) 0.0264(4) 0.0251(4) 0.0002(3) 0.0007(3) -0.0003(3)
C15 0.0247(4) 0.0208(4) 0.0230(4) -0.0004(3) 0.0085(3) -0.0007(3)
C16 0.0261(4) 0.0240(4) 0.0206(3) -0.0005(3) 0.0084(3) -0.0041(3)
C18 0.0245(4) 0.0244(4) 0.0234(4) -0.0036(3) 0.0084(3) 0.0004(3)
C19 0.0256(4) 0.0276(4) 0.0210(4) -0.0015(3) 0.0068(3) 0.0001(3)
C20 0.0239(4) 0.0157(3) 0.0234(4) 0.0015(3) 0.0080(3) 0.0013(3)
C21 0.0280(4) 0.0202(4) 0.0233(4) 0.0014(3) 0.0082(3) -0.0009(3)
C22 0.0295(5) 0.0209(4) 0.0260(4) 0.0000(3) 0.0043(3) 0.0003(3)
C23 0.0253(5) 0.0262(4) 0.0366(5) 0.0011(4) 0.0063(4) -0.0025(3)
C24 0.0288(5) 0.0298(5) 0.0363(5) 0.0019(4) 0.0144(4) -0.0029(4)
C25 0.0298(5) 0.0253(4) 0.0264(4) 0.0001(3) 0.0122(4) -0.0020(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl26 C22 1.7417(10) . ?
O10 C1 1.2215(11) . ?
O28 N27 1.2459(11) . ?
O29 N27 1.2505(10) . ?
O30 N27 1.2533(11) . ?
N2 N3 1.3818(12) . ?
N2 C1 1.3600(12) . ?
N2 C11 1.4521(12) . ?
N3 C9 1.3101(12) . ?
N8 C1 1.3934(12) . ?
N8 C7 1.3804(11) . ?
N8 C9 1.3835(11) . ?
N14 C13 1.5009(12) . ?
N14 C15 1.4928(11) . ?
N14 C19 1.4959(12) . ?
N17 C16 1.4626(11) . ?
N17 C18 1.4680(11) . ?
N17 C20 1.4023(12) . ?
C4 C5 1.3535(16) . ?
C4 C9 1.4230(13) . ?
C5 C6 1.4290(17) . ?
C6 C7 1.3453(15) . ?
C11 C12 1.5234(14) . ?
C12 C13 1.5180(14) . ?
C15 C16 1.5145(13) . ?
C18 C19 1.5074(13) . ?
C20 C21 1.4086(12) . ?
C20 C25 1.4081(12) . ?
C21 C22 1.3880(14) . ?
C22 C23 1.3812(14) . ?
C23 C24 1.3906(15) . ?
C24 C25 1.3819(15) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 N2 C11 120.46(8) . . ?
C1 N2 N3 114.18(8) . . ?
C1 N2 C11 125.16(9) . . ?
C9 N3 N2 103.57(7) . . ?
C7 N8 C1 128.23(8) . . ?
C7 N8 C9 123.76(8) . . ?
C9 N8 C1 107.99(7) . . ?
C15 N14 C13 113.13(7) . . ?
C15 N14 C19 108.36(7) . . ?
C19 N14 C13 109.02(7) . . ?
C16 N17 C18 113.04(7) . . ?
C20 N17 C16 116.56(7) . . ?
C20 N17 C18 115.70(7) . . ?
O28 N27 O29 119.74(8) . . ?
O28 N27 O30 119.83(9) . . ?
O29 N27 O30 120.41(8) . . ?
O10 C1 N2 129.76(9) . . ?
O10 C1 N8 127.72(9) . . ?
N2 C1 N8 102.51(7) . . ?
C5 C4 C9 118.44(9) . . ?
C4 C5 C6 121.49(9) . . ?
C7 C6 C5 120.52(9) . . ?
C6 C7 N8 117.85(9) . . ?
N3 C9 N8 111.74(8) . . ?
N3 C9 C4 130.33(9) . . ?
N8 C9 C4 117.93(8) . . ?
N2 C11 C12 113.09(8) . . ?
C13 C12 C11 109.91(8) . . ?
N14 C13 C12 113.56(7) . . ?
N14 C15 C16 111.71(7) . . ?
N17 C16 C15 112.38(7) . . ?
N17 C18 C19 112.22(7) . . ?
N14 C19 C18 111.84(7) . . ?
N17 C20 C21 121.73(8) . . ?
N17 C20 C25 120.79(8) . . ?
C25 C20 C21 117.42(9) . . ?
C22 C21 C20 119.57(8) . . ?
C21 C22 Cl26 118.50(7) . . ?
C23 C22 Cl26 118.36(8) . . ?
C23 C22 C21 123.12(9) . . ?
C22 C23 C24 117.14(9) . . ?
C25 C24 C23 121.46(9) . . ?
C24 C25 C20 121.27(9) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N14 H14 O29 0.916(13) 2.348(13) 3.0162(11) 129.7(10) 3_666
N14 H14 O30 0.916(13) 2.223(13) 3.0120(12) 143.9(10) .
_shelx_res_file
;
pn180815_uo_traz_1_180814_c6_nitrate_mo.res created by SHELXL-2014/7
TITL pn180815_uo_traz_1_180814_c6_nitrate_mo_a.res in P2(1)/c
REM Old TITL PN180815_UO_Traz_1_180814_C6_Nitrate_Mo in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.156, Rweak 0.009, Alpha 0.120, Orientation as input
REM Formula found by SHELXT: C22 N6 O Cl
CELL 0.71073 12.606513 13.072571 12.669429 90 106.3969 90
ZERR 4 0.000342 0.000257 0.000271 0 0.0026 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N O
UNIT 76 92 4 24 16
EQIV $1 1-X,1-Y,1-Z
L.S. 4
PLAN 20
TEMP -113
HTAB N14 O29_$1
HTAB N14 O30
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.058400 0.389500
FVAR 2.76701
CL26 3 0.828379 1.050943 0.837650 11.00000 0.04455 0.04064 =
0.02811 -0.00800 0.00436 -0.00862
O10 5 0.095018 0.670539 0.123137 11.00000 0.03059 0.04919 =
0.03719 -0.00828 0.01442 0.00882
O28 5 0.435632 0.517341 0.275518 11.00000 0.05276 0.03504 =
0.02973 0.00424 -0.00518 0.00833
O29 5 0.534360 0.398149 0.374199 11.00000 0.04108 0.02301 =
0.03455 -0.00152 0.00588 0.00920
O30 5 0.558414 0.556628 0.427286 11.00000 0.03982 0.03053 =
0.05243 -0.01181 -0.00433 -0.00732
N2 4 0.038492 0.657419 0.283216 11.00000 0.02148 0.02644 =
0.02612 0.00302 0.00213 0.00211
N3 4 -0.046452 0.693372 0.322154 11.00000 0.02543 0.03229 =
0.02329 0.00216 0.00721 -0.00123
N8 4 -0.062096 0.748932 0.152012 11.00000 0.01968 0.02418 =
0.01869 -0.00103 0.00494 0.00180
N14 4 0.396613 0.728164 0.418403 11.00000 0.02107 0.01763 =
0.02282 0.00086 0.00292 0.00206
H14 2 0.436560 0.671773 0.449180 11.00000 -1.20000
N17 4 0.567573 0.882325 0.494642 11.00000 0.02488 0.01899 =
0.02062 -0.00097 0.00901 -0.00186
N27 4 0.510076 0.490744 0.358616 11.00000 0.02330 0.02199 =
0.02678 -0.00003 0.00633 -0.00057
C1 1 0.032908 0.688631 0.179390 11.00000 0.02067 0.02693 =
0.02405 -0.00357 0.00437 0.00202
C4 1 -0.206014 0.803415 0.229887 11.00000 0.02590 0.03127 =
0.04075 -0.00507 0.01575 0.00137
AFIX 43
H4 2 -0.239212 0.805091 0.288499 11.00000 -1.20000
AFIX 0
C5 1 -0.252500 0.853429 0.134480 11.00000 0.02180 0.02520 =
0.05164 -0.00111 0.00598 0.00324
AFIX 43
H5 2 -0.319341 0.890192 0.126319 11.00000 -1.20000
AFIX 0
C6 1 -0.203314 0.852184 0.045748 11.00000 0.02761 0.02400 =
0.03457 0.00432 -0.00333 -0.00207
AFIX 43
H6 2 -0.237507 0.888246 -0.020182 11.00000 -1.20000
AFIX 0
C7 1 -0.108962 0.800341 0.054852 11.00000 0.02774 0.02851 =
0.02017 0.00129 0.00176 -0.00346
AFIX 43
H7 2 -0.075665 0.799152 -0.003698 11.00000 -1.20000
AFIX 0
C9 1 -0.106251 0.748266 0.240342 11.00000 0.02193 0.02401 =
0.02275 -0.00208 0.00830 -0.00144
C11 1 0.118920 0.585668 0.347778 11.00000 0.02487 0.02462 =
0.04344 0.00980 -0.00462 -0.00165
AFIX 23
H11A 2 0.142446 0.538770 0.297290 11.00000 -1.20000
H11B 2 0.083305 0.544002 0.393469 11.00000 -1.20000
AFIX 0
C12 1 0.220692 0.637855 0.422411 11.00000 0.02381 0.02974 =
0.03134 0.00932 -0.00117 -0.00286
AFIX 23
H12A 2 0.197823 0.687714 0.470603 11.00000 -1.20000
H12B 2 0.268999 0.586204 0.469736 11.00000 -1.20000
AFIX 0
C13 1 0.283923 0.692548 0.353404 11.00000 0.02088 0.02640 =
0.02515 0.00020 0.00069 -0.00029
AFIX 23
H13A 2 0.291867 0.645774 0.294650 11.00000 -1.20000
H13B 2 0.240346 0.752430 0.317544 11.00000 -1.20000
AFIX 0
C15 1 0.393526 0.802519 0.506913 11.00000 0.02469 0.02078 =
0.02302 -0.00042 0.00852 -0.00067
AFIX 23
H15A 2 0.359088 0.769503 0.559407 11.00000 -1.20000
H15B 2 0.347258 0.861897 0.473878 11.00000 -1.20000
AFIX 0
C16 1 0.508210 0.839470 0.568303 11.00000 0.02609 0.02397 =
0.02065 -0.00051 0.00843 -0.00407
AFIX 23
H16A 2 0.502066 0.892272 0.622285 11.00000 -1.20000
H16B 2 0.551163 0.781532 0.609542 11.00000 -1.20000
AFIX 0
C18 1 0.567027 0.814642 0.402028 11.00000 0.02454 0.02439 =
0.02343 -0.00363 0.00836 0.00043
AFIX 23
H18A 2 0.614542 0.754577 0.429787 11.00000 -1.20000
H18B 2 0.598695 0.851616 0.349795 11.00000 -1.20000
AFIX 0
C19 1 0.452258 0.778448 0.342228 11.00000 0.02560 0.02759 =
0.02097 -0.00146 0.00684 0.00010
AFIX 23
H19A 2 0.407359 0.837546 0.306150 11.00000 -1.20000
H19B 2 0.456686 0.729331 0.284144 11.00000 -1.20000
AFIX 0
C20 1 0.668382 0.930986 0.544644 11.00000 0.02385 0.01573 =
0.02345 0.00153 0.00795 0.00132
C21 1 0.698725 0.958831 0.656589 11.00000 0.02798 0.02020 =
0.02333 0.00136 0.00823 -0.00088
AFIX 43
H21 2 0.652571 0.941316 0.701547 11.00000 -1.20000
AFIX 0
C22 1 0.796490 1.012025 0.700791 11.00000 0.02953 0.02085 =
0.02603 -0.00004 0.00429 0.00032
C23 1 0.868365 1.037939 0.640594 11.00000 0.02530 0.02622 =
0.03661 0.00114 0.00629 -0.00247
AFIX 43
H23 2 0.935225 1.073694 0.673095 11.00000 -1.20000
AFIX 0
C24 1 0.838670 1.009452 0.530374 11.00000 0.02875 0.02976 =
0.03625 0.00192 0.01440 -0.00293
AFIX 43
H24 2 0.886477 1.025794 0.486744 11.00000 -1.20000
AFIX 0
C25 1 0.741159 0.957896 0.482900 11.00000 0.02979 0.02527 =
0.02643 0.00007 0.01217 -0.00201
AFIX 43
H25 2 0.722874 0.940269 0.407144 11.00000 -1.20000
AFIX 0
HKLF 4
REM pn180815_uo_traz_1_180814_c6_nitrate_mo_a.res in P2(1)/c
REM R1 = 0.0357 for 5530 Fo > 4sig(Fo) and 0.0429 for all 6532 data
REM 274 parameters refined using 0 restraints
END
WGHT 0.0584 0.3895
REM Highest difference peak 0.400, deepest hole -0.294, 1-sigma level 0.045
Q1 1 0.7063 0.9421 0.5147 11.00000 0.05 0.40
Q2 1 -0.0832 0.7498 0.1948 11.00000 0.05 0.40
Q3 1 0.8223 1.0268 0.6634 11.00000 0.05 0.36
Q4 1 0.0402 0.6716 0.2363 11.00000 0.05 0.36
Q5 1 -0.2218 0.8487 0.0938 11.00000 0.05 0.36
Q6 1 0.3945 0.7650 0.4635 11.00000 0.05 0.35
Q7 1 0.6876 0.9421 0.6013 11.00000 0.05 0.35
Q8 1 0.5832 0.5499 0.3780 11.00000 0.05 0.32
Q9 1 0.5697 0.8522 0.4546 11.00000 0.05 0.31
Q10 1 0.5350 0.8643 0.5261 11.00000 0.05 0.30
Q11 1 0.2599 0.6640 0.3960 11.00000 0.05 0.30
Q12 1 -0.2195 0.8426 0.1873 11.00000 0.05 0.29
Q13 1 0.4261 0.7542 0.3803 11.00000 0.05 0.29
Q14 1 0.1710 0.6133 0.3818 11.00000 0.05 0.28
Q15 1 0.8478 1.0364 0.5824 11.00000 0.05 0.28
Q16 1 0.4511 0.8232 0.5345 11.00000 0.05 0.27
Q17 1 -0.0895 0.7689 0.1018 11.00000 0.05 0.27
Q18 1 -0.1476 0.7803 0.2368 11.00000 0.05 0.26
Q19 1 0.8515 1.0625 0.7943 11.00000 0.05 0.26
Q20 1 -0.0697 0.7298 0.2869 11.00000 0.05 0.24
;
_shelx_res_checksum 83133
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17 -1 -4 559.919 34.3052 6
17 -1 -3 3.29393 25.0542 6
17 2 -10 271.692 26.3861 6
17 -2 -10 260.076 30.4095 6
17 2 -9 209.409 25.0448 6
17 -2 -9 177.510 28.1220 6
17 2 -8 340.813 28.2503 6
17 -2 -8 375.356 31.3931 6
17 2 -7 26.0026 22.8176 6
17 -2 -7 17.9026 25.7845 6
17 2 -6 151.152 25.3063 6
17 -2 -6 98.9612 26.5715 6
17 2 -5 164.231 25.2817 6
17 -2 -5 128.627 26.5004 6
17 2 -4 19.3690 23.2513 6
17 -2 -4 12.3898 24.8149 6
17 -2 -3 127.064 27.2169 6
17 -3 -10-1.71908 26.8763 6
17 3 -9 114.455 22.8223 6
17 -3 -9 69.3372 26.2241 6
17 3 -8 19.3101 21.1644 6
17 -3 -8 16.7810 25.1167 6
17 3 -7 542.768 30.9469 6
17 -3 -7 590.119 35.7743 6
17 3 -6 38.8037 22.6249 6
17 -3 -6 5.03112 25.5284 6
17 3 -5 231.849 27.0719 6
17 -3 -5 201.336 27.4162 6
17 -3 -4 55.4557 26.9465 6
17 -3 -3-3.50551 26.4889 6
17 -3 -2 6.98278 25.5785 6
17 -4 -10 7.03490 26.6064 6
17 -4 -9 53.6856 26.6072 6
17 -4 -8 42.1379 26.0560 6
17 4 -7 1.22241 20.4892 6
17 -4 -7 32.7275 27.1144 6
17 4 -6 8.52344 21.5196 6
17 -4 -6 17.7461 25.1503 6
17 4 -5 31.3431 22.0383 6
17 -4 -5 41.6503 26.3555 6
17 -4 -4 137.579 28.2812 6
17 -4 -3 18.6742 26.6744 6
17 -4 -2 248.959 30.8404 6
17 -4 -1 461.459 35.3068 6
17 -5 -10 12.4587 24.4916 1
17 -5 -10 22.1487 27.0017 6
17 -5 -9-8.74628 22.6917 1
17 -5 -9 22.1272 27.6963 6
17 -5 -8 86.8432 27.5721 6
17 -5 -7 81.0240 28.5752 6
17 5 -6 360.263 27.0824 6
17 -5 -6 368.441 33.7296 6
17 5 -5 22.6058 22.2013 6
17 -5 -5 14.3348 25.8561 6
17 -5 -4 253.731 30.5855 6
17 -5 -3 150.836 30.5025 6
17 -5 -2 955.607 44.4335 6
17 -6 -11 101.224 26.6663 1
17 -6 -10 134.486 27.2642 1
17 -6 -9 10.0284 24.6198 1
17 -6 -8-5.65176 27.9746 6
17 -6 -7 208.810 31.5899 6
17 -6 -6 194.005 30.8892 6
17 -6 -5 8.08854 26.7190 6
17 -6 -4 43.9802 27.6363 6
17 -6 -3 160.979 31.1118 6
17 -7 -10 113.184 28.0166 1
17 -7 -9 88.7137 26.6712 1
17 -8 -9 4.82008 26.3090 1
18 0 -10 81.3920 26.8259 6
18 0 -9-14.0860 25.1926 6
18 0 -8 1345.47 49.7510 6
18 0 -7 3.14001 24.7316 6
18 0 -6 1509.78 52.5935 6
18 0 -5 5.05938 25.8092 6
18 0 -4 133.274 27.8258 6
18 0 -3 6.03691 27.2850 6
18 -1 -11 123.586 29.6511 6
18 1 -10 110.239 26.7746 6
18 -1 -10 155.572 29.4707 6
18 1 -9-1.49412 24.7395 6
18 -1 -9 0.83305 26.0604 6
18 1 -8 26.8933 25.2769 6
18 -1 -8 22.6339 25.8776 6
18 1 -7 19.7579 24.6190 6
18 -1 -7 23.9123 26.5822 6
18 1 -6 309.394 31.1597 6
18 -1 -6 384.522 32.6388 6
18 1 -5-19.3887 25.2246 6
18 -1 -5 11.1929 26.8963 6
18 1 -4 1.65123 25.6809 6
18 -1 -4-22.1438 26.6061 6
18 1 -3 934.841 42.6350 6
18 -1 -3 924.759 44.0471 6
18 -2 -11 148.729 31.1040 6
18 -2 -10 295.686 32.7481 6
18 -2 -9 43.0709 26.8449 6
18 2 -8 81.1928 24.2750 6
18 -2 -8 20.7187 26.1126 6
18 2 -7-8.06861 24.3940 6
18 -2 -7-7.82586 27.9036 6
18 2 -6 0.75617 25.2947 6
18 -2 -6-1.73047 25.9383 6
18 2 -5 3.85329 24.0053 6
18 -2 -5-6.97108 25.7692 6
18 2 -4 33.4625 26.0405 6
18 -2 -4 20.6315 26.9240 6
18 -2 -3 5.42634 27.7360 6
18 -3 -10 92.1647 29.0875 6
18 -3 -9 40.1552 27.1734 6
18 -3 -8-15.9852 26.7892 6
18 3 -7 598.301 33.3578 6
18 -3 -7 586.965 37.6879 6
18 3 -6 298.812 29.1452 6
18 -3 -6 216.190 30.7080 6
18 3 -5 27.2258 24.1109 6
18 -3 -5 8.12515 27.3313 6
18 3 -4-0.76971 25.0772 6
18 -3 -4 33.2186 28.4393 6
18 -4 -7-9.45523 28.6084 6
18 4 -6 269.484 28.9510 6
18 4 -5 41.6158 24.8675 6
18 4 -4 68.6464 25.4762 6
18 5 -4 73.6231 25.5891 6
19 0 -9-7.56417 26.7260 6
19 0 -8 9.37211 26.8307 6
19 0 -7-2.53054 26.5127 6
19 0 -6 167.765 30.3928 6
19 1 -8 3.29208 26.4581 6
19 1 -7 47.6863 25.5086 6
19 1 -6 121.182 28.3276 6
19 1 -5 11.3385 27.4149 6
19 2 -7 11.5470 25.9644 6
19 2 -6 33.2593 26.6396 6
19 2 -5 265.374 31.5834 6
19 3 -5 671.303 38.3881 6
19 3 -4 373.971 33.7575 6
19 4 -4 408.039 33.6152 6
0 0 0 0.00 0.00 0
TITL PN180815_UO_Traz_1_180814_C6_Nitrate_Mo in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 12.606513 13.072571 12.669429 90.0000 106.3969 90.0000
ZERR 4.00 0.000342 0.000257 0.000271 0.0000 0.0026 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O Cl
UNIT 80.00 92.00 20.00 16.00 4.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 92982
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.138
_oxdiff_exptl_absorpt_empirical_full_min 0.907
data_pn180815_uo_traz_1_180814_scn
_audit_creation_date 2018-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number '2014/7'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '1(C19 H23 Cl N5 O), C N S'
_chemical_formula_sum 'C20 H23 Cl N6 O S'
_chemical_formula_weight 430.95
_chemical_melting_point ?
_chemical_oxdiff_formula 'C20 H23 Cl N6 O S'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system 'triclinic'
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.1482(2)
_cell_length_b 13.1848(2)
_cell_length_c 13.82510(17)
_cell_angle_alpha 90.2630(12)
_cell_angle_beta 90.2180(12)
_cell_angle_gamma 108.0045(15)
_cell_volume 2105.89(6)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 34827
_cell_measurement_temperature 159.99(10)
_cell_measurement_theta_max 78.6650
_cell_measurement_theta_min 3.5170
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.729
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.532
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.359
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 904
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 0 0 0.0145
-8 1 1 0.0496
0 0 -9 0.1106
-5 5 5 0.0697
-3 -6 0 0.0611
3 5 5 0.0619
2 7 1 0.0751
-3 1 -8 0.1063
-2 4 -8 0.1143
2 -3 -8 0.1075
-7 7 0 0.0867
-6 -3 0 0.0502
-5 -4 3 0.0647
4 -5 6 0.0902
3 -8 1 0.0769
0 -6 -6 0.1042
5 4 -2 0.0584
_exptl_crystal_size_max 0.234
_exptl_crystal_size_mid 0.189
_exptl_crystal_size_min 0.073
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6.9974 -0.0038 0.0023 0.5139 0.6979 -0.3452
-7.9964 1.0044 0.9970 -0.4944 -0.8719 0.2782
0.0008 -0.0048 -9.0000 0.2020 0.3053 0.9337
-4.9948 5.0033 4.9961 0.0975 -0.8698 -0.3351
-3.0035 -5.9960 0.0018 -0.9123 -0.0570 0.2234
3.0023 4.9990 4.9987 0.6848 -0.0722 -0.7296
2.0045 6.9967 0.9974 0.9318 -0.1169 -0.2904
-2.9975 0.9970 -8.0014 0.0746 -0.0681 0.9653
-1.9955 3.9952 -8.0024 0.4941 -0.0894 0.8783
1.9976 -3.0041 -7.9979 -0.0197 0.5918 0.7691
-6.9921 7.0010 -0.0055 0.2935 -0.9804 0.2571
-6.0001 -2.9956 -0.0006 -0.7865 -0.4772 0.3336
-5.0015 -3.9941 3.0002 -0.8958 -0.4389 -0.0144
3.9942 -4.9970 6.0036 -0.4177 0.3970 -0.7568
2.9927 -7.9979 1.0046 -0.7250 0.5880 -0.1511
-0.0041 -6.0008 -5.9972 -0.5574 0.4456 0.6980
5.0014 3.9946 -2.0002 0.8733 0.4050 -0.0894
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0319
_diffrn_reflns_av_unetI/netI 0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 52525
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 78.923
_diffrn_reflns_theta_min 3.197
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 159.99(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
--------------------------------------------------------------------------
1 \w -89.00 -35.00 0.50 0.25 -- -50.46 -57.00-180.00 108
2 \w -80.00 -38.00 0.50 0.25 -- -50.46 -57.00-120.00 84
3 \w -65.00 -39.00 0.50 0.25 -- -50.46 -57.00 -30.00 52
4 \w -60.00 -35.00 0.50 0.25 -- -50.46 -57.00 120.00 50
5 \w -33.00 9.00 0.50 0.25 -- -50.46 57.00 150.00 84
6 \w -72.00 -46.00 0.50 1.00 -- -86.25 60.00 166.42 52
7 \w -69.00 -43.00 0.50 1.00 -- -86.25 60.00 79.04 52
8 \w -93.00 -67.00 0.50 1.00 -- -86.25 60.00 125.16 52
9 \w -92.00 -63.00 0.50 1.00 -- -86.25 60.00 31.45 58
10 \w -77.00 -51.00 0.50 1.00 -- -86.25 60.00 -64.27 52
11 \w -121.00 -65.00 0.50 0.25 -- -50.46 -57.00 120.00 112
12 \w -121.00 -89.00 0.50 0.25 -- -50.46 -57.00 60.00 64
13 \w -21.00 5.00 0.50 0.25 -- 50.46 -60.00 -28.26 52
14 \w 21.00 66.00 0.50 0.25 -- 50.46 -60.00 -28.26 90
15 \w 64.00 89.00 0.50 1.00 -- 107.75 -58.00 -31.90 50
16 \w 80.00 106.00 0.50 1.00 -- 107.75 -60.00 -40.20 52
17 \w 90.00 116.00 0.50 1.00 -- 107.75 -60.00 17.59 52
18 \w 75.00 104.00 0.50 1.00 -- 107.75 -15.00 30.00 58
19 \w 95.00 125.00 0.50 1.00 -- 107.75 15.00 90.00 60
20 \w 125.00 178.00 0.50 1.00 -- 107.75 42.00 53.04 106
21 \w 127.00 176.00 0.50 1.00 -- 107.75 15.00 150.00 98
22 \w 112.00 138.00 0.50 1.00 -- 107.75 32.00 36.61 52
23 \w 87.00 115.00 0.50 0.25 -- 50.46 57.00 0.00 56
24 \w 145.00 176.00 0.50 1.00 -- 107.75 30.00 -90.00 62
25 \w 138.00 175.00 0.50 1.00 -- 107.75 15.00-180.00 74
26 \w 127.00 178.00 0.50 1.00 -- 107.75 45.00-148.92 102
27 \w 109.00 135.00 0.50 1.00 -- 107.75 30.00 -90.00 52
28 \w 98.00 133.00 0.50 1.00 -- 107.75 15.00-120.00 70
29 \w 98.00 126.00 0.50 1.00 -- 107.75 15.00-180.00 56
30 \w 81.00 107.00 0.50 1.00 -- 107.75 -60.00-174.15 52
31 \w 64.00 110.00 0.50 1.00 -- 107.75 -60.00-135.99 92
32 \w 58.00 94.00 0.50 1.00 -- 107.75 -60.00-101.89 72
33 \w 50.00 101.00 0.50 1.00 -- 107.75 -59.00 -83.65 102
34 \w 46.00 71.00 0.50 1.00 -- 107.75 -59.00-173.99 50
35 \w 41.00 69.00 0.50 1.00 -- 107.75 -45.00-120.00 56
36 \w 50.00 75.00 0.50 1.00 -- 107.75 -50.00-153.39 50
37 \w 51.00 77.00 0.50 1.00 -- 107.75 -45.00-150.00 52
38 \w 35.00 102.00 0.50 1.00 -- 107.75 -15.00-120.00 134
39 \w 100.00 158.00 0.50 1.00 -- 107.75 15.00 -90.00 116
40 \w 70.00 108.00 0.50 1.00 -- 107.75 -60.00 88.14 76
41 \w 81.00 124.00 0.50 1.00 -- 107.75 -60.00 136.87 86
42 \w 71.00 107.00 0.50 1.00 -- 107.75 -60.00 166.31 72
43 \w 61.00 98.00 0.50 1.00 -- 107.75 -60.00 78.55 74
44 \w 49.00 78.00 0.50 1.00 -- 107.75 -46.00 168.52 58
45 \w 40.00 98.00 0.50 1.00 -- 107.75 -60.00 120.05 116
46 \w 43.00 112.00 0.50 1.00 -- 107.75 -60.00 45.09 138
47 \w 51.00 103.00 0.50 1.00 -- 107.75 -60.00 -68.77 104
48 \w 50.00 75.00 0.50 1.00 -- 107.75 -52.00 -39.62 50
49 \w 36.00 75.00 0.50 1.00 -- 107.75 -59.00 10.56 78
50 \w 36.00 106.00 0.50 1.00 -- 107.75 -60.00 -13.71 140
51 \w 37.00 90.00 0.50 1.00 -- 107.75 -59.00 24.62 106
52 \w 39.00 64.00 0.50 1.00 -- 107.75 -60.00 136.87 50
53 \w 33.00 59.00 0.50 1.00 -- 107.75 -30.00 90.00 52
54 \w 29.00 68.00 0.50 1.00 -- 107.75 -30.00 60.00 78
55 \w 38.00 67.00 0.50 1.00 -- 107.75 -15.00 30.00 58
56 \w 34.00 74.00 0.50 1.00 -- 107.75 -45.00 60.00 80
57 \w 32.00 63.00 0.50 1.00 -- 107.75 -30.00 120.00 62
58 \w 35.00 67.00 0.50 1.00 -- 107.75 -53.00 153.80 64
59 \w 29.00 57.00 0.50 1.00 -- 107.75 -30.00 150.00 56
60 \w 31.00 64.00 0.50 0.25 -- 50.46 -57.00 150.00 66
61 \w 35.00 72.00 0.50 0.25 -- 50.46 57.00 90.00 74
62 \w 35.00 79.00 0.50 0.25 -- 50.46 59.00 41.94 88
63 \w 35.00 82.00 0.50 0.25 -- 50.46 57.00 0.00 94
64 \w 35.00 75.00 0.50 0.25 -- 50.46 57.00 -60.00 80
65 \w 35.00 65.00 0.50 0.25 -- 50.46 59.00 -23.68 60
66 \w 35.00 95.00 0.50 1.00 -- 107.75 -9.00 -75.56 120
67 \w 36.00 65.00 0.50 0.25 -- 50.46 -57.00-180.00 58
68 \w 29.00 54.00 0.50 1.00 -- 107.75 -30.00-120.00 50
69 \w 35.00 63.00 0.50 1.00 -- 107.75 -45.00-166.76 56
70 \w 36.00 67.00 0.50 1.00 -- 107.75 -55.00-163.59 62
71 \w 29.00 54.00 0.50 1.00 -- 107.75 -30.00 -90.00 50
72 \w 37.00 76.00 0.50 1.00 -- 107.75 -45.00 -75.62 78
73 \w 33.00 61.00 0.50 1.00 -- 107.75 -45.00 -60.00 56
74 \w 32.00 76.00 0.50 1.00 -- 107.75 -45.00 0.00 88
75 \w 35.00 72.00 0.50 0.25 -- 50.46 57.00 150.00 74
76 \w 36.00 74.00 0.50 0.25 -- 50.46 57.00-180.00 76
77 \w -9.00 36.00 0.50 0.25 -- 6.00 59.00 102.59 90
78 \w -57.00 -31.00 0.50 0.25 -- -46.00 -60.00 37.28 52
79 \w -61.00 -35.00 0.50 0.25 -- -50.00 -60.00 73.90 52
80 \w -61.00 -35.00 0.50 0.25 -- -50.00 -59.00 -50.03 52
81 \w -120.00 -95.00 0.50 0.25 -- -50.00 -59.00 -50.03 50
82 \w -118.00 -91.00 0.50 0.25 -- -50.00 -60.00 73.90 54
83 \w -64.00 -38.00 0.50 0.25 -- -50.46 -38.00 0.00 52
84 \w -128.00 -93.00 0.50 0.25 -- -50.46 -38.00 0.00 70
85 \w 18.00 54.00 0.50 0.25 -- 50.46 -57.00 -90.00 72
86 \w -75.00 -40.00 0.50 0.25 -- -54.00 -58.00-144.74 70
87 \w -64.00 -38.00 0.50 0.25 -- -54.00 -60.00 116.61 52
88 \w -76.00 -42.00 0.50 0.25 -- -58.00 -60.00 167.61 68
89 \w -69.00 -43.00 0.50 0.25 -- -58.00 -60.00-112.28 52
90 \w -69.00 -43.00 0.50 0.25 -- -58.00 -58.00 32.35 52
91 \w -77.00 -42.00 0.50 0.25 -- -58.00 -60.00 5.62 70
92 \w -67.00 -42.00 0.50 0.25 -- -58.00 -59.00 -82.65 50
93 \w -129.00-103.00 0.50 0.25 -- -58.00 -59.00 -82.65 52
94 \w -117.00 -90.00 0.50 0.25 -- -58.00 -60.00 167.61 54
95 \w -81.00 -52.00 0.50 0.25 -- -66.00 -60.00 -50.14 58
96 \w -123.00 -97.00 0.50 1.00 -- -70.00 -60.00 43.15 52
97 \w -81.00 -55.00 0.50 1.00 -- -70.00 -60.00 -82.12 52
98 \w 54.00 80.00 0.50 0.25 -- 70.00 60.00 130.16 52
99 \w -79.00 -54.00 0.50 1.00 -- -70.00 -60.00 117.59 50
100 \w -80.00 -54.00 0.50 1.00 -- -70.00 -60.00 43.15 52
101 \w -81.00 -55.00 0.50 1.00 -- -70.00 -60.00 -28.22 52
102 \w -86.00 -78.50 0.50 1.00 -- -74.00 -59.00 33.16 15
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0735116000
_diffrn_orient_matrix_UB_12 0.1153264000
_diffrn_orient_matrix_UB_13 -0.0224963000
_diffrn_orient_matrix_UB_21 0.0997303000
_diffrn_orient_matrix_UB_22 -0.0404534000
_diffrn_orient_matrix_UB_23 -0.0338894000
_diffrn_orient_matrix_UB_31 -0.0493045000
_diffrn_orient_matrix_UB_32 -0.0125931000
_diffrn_orient_matrix_UB_33 -0.1037459000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7824
_reflns_number_total 8412
_reflns_odcompleteness_completeness 93.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 74.33
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.514
_refine_diff_density_min -0.548
_refine_diff_density_rms 0.049
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 723
_refine_ls_number_reflns 8412
_refine_ls_number_restraints 45
_refine_ls_R_factor_all 0.0599
_refine_ls_R_factor_gt 0.0574
_refine_ls_restrained_S_all 1.055
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+2.3014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1344
_refine_ls_wR_factor_ref 0.1358
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
S59B-C58B = S59-C58
1.64 with sigma of 0.001
N32-C41 \\sim N32-C41B
with sigma of 0.02
3. Rigid body (RIGU) restrains
C50, C51, C52, C55
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
N32, C41B, C42B
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
S59B, N57B, C58B
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
S59, N57, C58
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
Sof(S29B)=Sof(N27B)=Sof(C28B)=1-FVAR(1)
Sof(S29)=Sof(N27)=Sof(C28)=FVAR(1)
Sof(Cl57)=Sof(S59B)=Sof(N44B)=Sof(H44B)=Sof(N47B)=Sof(N57B)=Sof(C41B)=
Sof(H41C)=Sof(H41D)=Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=
Sof(H43D)=Sof(C45B)=Sof(H45C)=Sof(H45D)=Sof(C46B)=Sof(H46C)=Sof(H46D)=
Sof(C48B)=Sof(H48C)=Sof(H48D)=Sof(C49B)=Sof(H49C)=Sof(H49D)=Sof(C50B)=
Sof(C51B)=Sof(H51B)=Sof(C52B)=Sof(C53B)=Sof(H53B)=Sof(C54B)=Sof(H54B)=
Sof(C55B)=Sof(H55B)=Sof(C58B)=1-FVAR(2)
Sof(Cl56)=Sof(S59)=Sof(N44)=Sof(H44)=Sof(N47)=Sof(N57)=Sof(C41)=Sof(H41A)=
Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C45)=
Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C48)=Sof(H48A)=Sof(H48B)=
Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(C53)=
Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C58)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
N14(H14), N44(H44), N44B(H44B)
5.b Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,
H16B), C18(H18A,H18B), C19(H19A,H19B), C41(H41A,H41B), C41B(H41C,H41D),
C42(H42A,H42B), C42B(H42C,H42D), C43(H43A,H43B), C43B(H43C,H43D), C45(H45A,
H45B), C45B(H45C,H45D), C46(H46A,H46B), C46B(H46C,H46D), C48(H48A,H48B),
C48B(H48C,H48D), C49(H49A,H49B), C49B(H49C,H49D)
5.c Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C21(H21), C23(H23), C24(H24), C25(H25),
C34(H34), C35(H35), C36(H36), C37(H37), C51(H51), C51B(H51B), C53(H53),
C53B(H53B), C54(H54), C54B(H54B), C55(H55), C55B(H55B)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl26 Cl 0.84874(7) 0.82750(5) -0.05159(5) 0.0598(2) Uani 1 1 d . . . . .
Cl56 Cl 0.15284(16) -0.32691(14) 0.45633(11) 0.0505(4) Uani 0.492(3) 1 d . . P A
3
Cl57 Cl 0.12284(11) -0.28589(15) 0.43681(12) 0.0468(4) Uani 0.508(3) 1 d . . P A
4
S29 S 0.54688(11) 0.31572(9) 0.58920(9) 0.0439(4) Uani 0.502(2) 1 d . . P B 1
S29B S 0.45272(17) 0.28178(13) 0.46543(12) 0.0682(6) Uani 0.498(2) 1 d . . P B 2
S59 S 0.4566(6) -0.2109(5) 1.0373(4) 0.0703(13) Uani 0.492(3) 1 d D U P A 3
S59B S 0.4379(5) -0.2233(4) 1.0463(3) 0.0476(6) Uani 0.508(3) 1 d D U P A 4
O10 O 0.07854(17) 0.1159(2) 0.3335(2) 0.0916(9) Uani 1 1 d . . . . .
O40 O 0.93035(19) 0.3870(2) 0.8324(2) 0.1078(11) Uani 1 1 d . . . . .
N2 N 0.01486(17) 0.2651(2) 0.31321(17) 0.0541(6) Uani 1 1 d . . . . .
N3 N -0.06980(17) 0.29125(18) 0.26031(16) 0.0466(5) Uani 1 1 d . . . . .
N8 N -0.07820(17) 0.12207(17) 0.23658(17) 0.0519(6) Uani 1 1 d . . . . .
N14 N 0.38422(14) 0.41764(14) 0.24813(13) 0.0335(4) Uani 1 1 d . . . . .
H14 H 0.4257 0.4440 0.3103 0.040 Uiso 1 1 calc R . . . .
N17 N 0.57940(15) 0.50147(14) 0.12163(13) 0.0327(4) Uani 1 1 d . . . . .
N27 N 0.4571(4) 0.3732(4) 0.4197(3) 0.0527(11) Uani 0.502(2) 1 d . . P B 1
N27B N 0.5511(4) 0.4393(4) 0.6014(3) 0.0497(11) Uani 0.498(2) 1 d . . P B 2
N32 N 0.99770(19) 0.2395(2) 0.81158(18) 0.0628(7) Uani 1 1 d D U . . .
N33 N 1.08098(18) 0.21322(18) 0.75689(17) 0.0504(5) Uani 1 1 d . . . . .
N38 N 1.08185(16) 0.38075(17) 0.73186(17) 0.0507(6) Uani 1 1 d . . . . .
N44 N 0.6218(10) 0.0916(10) 0.7514(6) 0.0269(19) Uani 0.492(3) 1 d . . P A 3
H44 H 0.5832 0.0586 0.8124 0.032 Uiso 0.492(3) 1 calc R . P A 3
N44B N 0.6613(3) 0.0089(3) 0.7380(3) 0.0304(8) Uani 0.508(3) 1 d . . P A 4
H44B H 0.6215 -0.0334 0.7948 0.036 Uiso 0.508(3) 1 calc R . P A 4
N47 N 0.4273(5) 0.0075(5) 0.6210(5) 0.0306(12) Uani 0.492(3) 1 d . . P A 3
N47B N 0.4527(5) -0.0205(5) 0.6257(4) 0.0272(11) Uani 0.508(3) 1 d . . P A 4
N57 N 0.5556(4) -0.0582(4) 0.8993(3) 0.0451(10) Uani 0.492(3) 1 d . U P A 3
N57B N 0.5660(4) -0.1156(4) 0.8926(3) 0.0488(11) Uani 0.508(3) 1 d . U P A 4
C1 C 0.0143(2) 0.1625(3) 0.3000(2) 0.0632(9) Uani 1 1 d . . . . .
C4 C -0.2187(2) 0.1784(2) 0.1482(2) 0.0518(6) Uani 1 1 d . . . . .
H4 H -0.2530 0.2314 0.1304 0.062 Uiso 1 1 calc R . . . .
C5 C -0.2587(3) 0.0792(2) 0.1108(2) 0.0609(7) Uani 1 1 d . . . . .
H5 H -0.3210 0.0632 0.0658 0.073 Uiso 1 1 calc R . . . .
C6 C -0.2106(3) -0.0020(3) 0.1365(3) 0.0682(9) Uani 1 1 d . . . . .
H6 H -0.2416 -0.0716 0.1098 0.082 Uiso 1 1 calc R . . . .
C7 C -0.1215(3) 0.0197(2) 0.1985(3) 0.0693(10) Uani 1 1 d . . . . .
H7 H -0.0883 -0.0341 0.2162 0.083 Uiso 1 1 calc R . . . .
C9 C -0.1242(2) 0.2027(2) 0.21484(18) 0.0423(6) Uani 1 1 d . . . . .
C11 C 0.0930(2) 0.3432(3) 0.3758(2) 0.0692(9) Uani 1 1 d . . . . .
H11A H 0.1229 0.3057 0.4264 0.083 Uiso 1 1 calc R . . . .
H11B H 0.0496 0.3859 0.4083 0.083 Uiso 1 1 calc R . . . .
C12 C 0.1945(2) 0.4178(3) 0.3217(2) 0.0569(7) Uani 1 1 d . . . . .
H12A H 0.1658 0.4586 0.2732 0.068 Uiso 1 1 calc R . . . .
H12B H 0.2456 0.4691 0.3677 0.068 Uiso 1 1 calc R . . . .
C13 C 0.2622(2) 0.3538(2) 0.27163(19) 0.0518(7) Uani 1 1 d . . . . .
H13A H 0.2637 0.2937 0.3137 0.062 Uiso 1 1 calc R . . . .
H13B H 0.2216 0.3233 0.2110 0.062 Uiso 1 1 calc R . . . .
C15 C 0.3948(2) 0.5113(2) 0.18572(18) 0.0467(6) Uani 1 1 d . . . . .
H15A H 0.3582 0.5598 0.2179 0.056 Uiso 1 1 calc R . . . .
H15B H 0.3538 0.4873 0.1237 0.056 Uiso 1 1 calc R . . . .
C16 C 0.5206(2) 0.57030(19) 0.1662(2) 0.0476(6) Uani 1 1 d . . . . .
H16A H 0.5256 0.6312 0.1230 0.057 Uiso 1 1 calc R . . . .
H16B H 0.5598 0.5991 0.2278 0.057 Uiso 1 1 calc R . . . .
C18 C 0.5688(2) 0.40778(18) 0.18042(18) 0.0401(5) Uani 1 1 d . . . . .
H18A H 0.6101 0.4300 0.2426 0.048 Uiso 1 1 calc R . . . .
H18B H 0.6053 0.3603 0.1465 0.048 Uiso 1 1 calc R . . . .
C19 C 0.4437(2) 0.34787(19) 0.1999(2) 0.0488(6) Uani 1 1 d . . . . .
H19A H 0.4039 0.3206 0.1381 0.059 Uiso 1 1 calc R . . . .
H19B H 0.4391 0.2859 0.2417 0.059 Uiso 1 1 calc R . . . .
C20 C 0.68396(17) 0.54862(17) 0.07376(15) 0.0314(4) Uani 1 1 d . . . . .
C21 C 0.71671(19) 0.65540(17) 0.04478(15) 0.0346(4) Uani 1 1 d . . . . .
H21 H 0.6717 0.6998 0.0628 0.041 Uiso 1 1 calc R . . . .
C22 C 0.8155(2) 0.69575(18) -0.01057(16) 0.0406(5) Uani 1 1 d . . . . .
C23 C 0.8853(2) 0.6363(2) -0.03819(18) 0.0462(6) Uani 1 1 d . . . . .
H23 H 0.9522 0.6661 -0.0764 0.055 Uiso 1 1 calc R . . . .
C24 C 0.85426(19) 0.5316(2) -0.00830(18) 0.0450(6) Uani 1 1 d . . . . .
H24 H 0.9010 0.4886 -0.0259 0.054 Uiso 1 1 calc R . . . .
C25 C 0.75637(19) 0.48817(19) 0.04681(17) 0.0389(5) Uani 1 1 d . . . . .
H25 H 0.7376 0.4160 0.0669 0.047 Uiso 1 1 calc R . . . .
C28 C 0.4950(4) 0.3500(3) 0.4913(4) 0.0313(10) Uani 0.502(2) 1 d . . P B 1
C28B C 0.5126(4) 0.3751(4) 0.5448(4) 0.0352(10) Uani 0.498(2) 1 d . . P B 2
C31 C 0.9939(2) 0.3411(3) 0.7979(2) 0.0676(10) Uani 1 1 d . . . . .
C34 C 1.2208(2) 0.3262(2) 0.6408(2) 0.0522(7) Uani 1 1 d . . . . .
H34 H 1.2568 0.2744 0.6232 0.063 Uiso 1 1 calc R . . . .
C35 C 1.2559(3) 0.4243(3) 0.6008(2) 0.0621(7) Uani 1 1 d . . . . .
H35 H 1.3165 0.4403 0.5546 0.075 Uiso 1 1 calc R . . . .
C36 C 1.2056(3) 0.5027(3) 0.6256(3) 0.0700(9) Uani 1 1 d . . . . .
H36 H 1.2321 0.5711 0.5965 0.084 Uiso 1 1 calc R . . . .
C37 C 1.1204(3) 0.4818(2) 0.6901(3) 0.0675(10) Uani 1 1 d . . . . .
H37 H 1.0863 0.5350 0.7075 0.081 Uiso 1 1 calc R . . . .
C39 C 1.12930(19) 0.3012(2) 0.70968(19) 0.0427(6) Uani 1 1 d . . . . .
C41 C 0.9147(8) 0.1780(8) 0.8740(7) 0.067(3) Uani 0.492(3) 1 d D . P A 3
H41A H 0.8810 0.2249 0.9121 0.080 Uiso 0.492(3) 1 calc R . P A 3
H41B H 0.9515 0.1406 0.9197 0.080 Uiso 0.492(3) 1 calc R . P A 3
C41B C 0.9333(6) 0.1492(7) 0.8816(6) 0.0546(14) Uani 0.508(3) 1 d D U P A 4
H41C H 0.9714 0.0928 0.8798 0.066 Uiso 0.508(3) 1 calc R . P A 4
H41D H 0.9412 0.1785 0.9482 0.066 Uiso 0.508(3) 1 calc R . P A 4
C42 C 0.8179(5) 0.0957(5) 0.8176(5) 0.0403(15) Uani 0.492(3) 1 d . . P A 3
H42A H 0.7722 0.0389 0.8610 0.048 Uiso 0.492(3) 1 calc R . P A 3
H42B H 0.8505 0.0627 0.7650 0.048 Uiso 0.492(3) 1 calc R . P A 3
C42B C 0.8069(6) 0.0997(7) 0.8588(5) 0.0558(19) Uani 0.508(3) 1 d . U P A 4
H42C H 0.7679 0.1554 0.8612 0.067 Uiso 0.508(3) 1 calc R . P A 4
H42D H 0.7713 0.0457 0.9084 0.067 Uiso 0.508(3) 1 calc R . P A 4
C43 C 0.7425(3) 0.1600(3) 0.7760(3) 0.0315(9) Uani 0.492(3) 1 d . . P A 3
H43A H 0.7386 0.2148 0.8239 0.038 Uiso 0.492(3) 1 calc R . P A 3
H43B H 0.7796 0.1972 0.7170 0.038 Uiso 0.492(3) 1 calc R . P A 3
C43B C 0.7889(4) 0.0476(4) 0.7603(3) 0.0366(10) Uani 0.508(3) 1 d . . P A 4
H43C H 0.8298 0.0996 0.7108 0.044 Uiso 0.508(3) 1 calc R . P A 4
H43D H 0.8206 -0.0131 0.7593 0.044 Uiso 0.508(3) 1 calc R . P A 4
C45 C 0.6173(4) 0.0041(3) 0.6805(4) 0.0305(10) Uani 0.492(3) 1 d . . P A 3
H45A H 0.6575 -0.0441 0.7082 0.037 Uiso 0.492(3) 1 calc R . P A 3
H45B H 0.6579 0.0351 0.6205 0.037 Uiso 0.492(3) 1 calc R . P A 3
C45B C 0.6346(3) -0.0631(3) 0.6516(3) 0.0296(9) Uani 0.508(3) 1 d . . P A 4
H45C H 0.6654 -0.1235 0.6619 0.035 Uiso 0.508(3) 1 calc R . P A 4
H45D H 0.6731 -0.0233 0.5941 0.035 Uiso 0.508(3) 1 calc R . P A 4
C46 C 0.4928(4) -0.0593(5) 0.6566(4) 0.0335(10) Uani 0.492(3) 1 d . . P A 3
H46A H 0.4921 -0.1141 0.6072 0.040 Uiso 0.492(3) 1 calc R . P A 3
H46B H 0.4551 -0.0966 0.7154 0.040 Uiso 0.492(3) 1 calc R . P A 3
C46B C 0.5048(4) -0.1058(4) 0.6333(4) 0.0308(10) Uani 0.508(3) 1 d . . P A 4
H46C H 0.4902 -0.1481 0.5726 0.037 Uiso 0.508(3) 1 calc R . P A 4
H46D H 0.4679 -0.1537 0.6868 0.037 Uiso 0.508(3) 1 calc R . P A 4
C48 C 0.4317(4) 0.0940(4) 0.6890(4) 0.0382(11) Uani 0.492(3) 1 d . . P A 3
H48A H 0.3931 0.0637 0.7500 0.046 Uiso 0.492(3) 1 calc R . P A 3
H48B H 0.3892 0.1403 0.6613 0.046 Uiso 0.492(3) 1 calc R . P A 3
C48B C 0.4813(4) 0.0520(3) 0.7087(3) 0.0333(10) Uani 0.508(3) 1 d . . P A 4
H48C H 0.4460 0.0133 0.7677 0.040 Uiso 0.508(3) 1 calc R . P A 4
H48D H 0.4486 0.1112 0.6986 0.040 Uiso 0.508(3) 1 calc R . P A 4
C49 C 0.5549(4) 0.1598(3) 0.7104(3) 0.0348(10) Uani 0.492(3) 1 d . . P A 3
H49A H 0.5922 0.1937 0.6501 0.042 Uiso 0.492(3) 1 calc R . P A 3
H49B H 0.5556 0.2171 0.7571 0.042 Uiso 0.492(3) 1 calc R . P A 3
C49B C 0.6102(12) 0.0966(12) 0.7226(8) 0.033(2) Uani 0.508(3) 1 d . . P A 4
H49C H 0.6453 0.1380 0.6648 0.040 Uiso 0.508(3) 1 calc R . P A 4
H49D H 0.6275 0.1454 0.7791 0.040 Uiso 0.508(3) 1 calc R . P A 4
C50 C 0.3260(15) -0.0381(12) 0.5756(14) 0.025(2) Uani 0.492(3) 1 d . U P A 3
C50B C 0.3353(18) -0.0522(14) 0.5885(15) 0.036(3) Uani 0.508(3) 1 d . . P A 4
C51 C 0.2921(14) -0.1535(14) 0.5456(14) 0.023(2) Uani 0.492(3) 1 d . U P A 3
H51 H 0.3404 -0.1965 0.5582 0.027 Uiso 0.492(3) 1 calc R . P A 3
C51B C 0.2830(16) -0.1418(16) 0.5448(17) 0.037(4) Uani 0.508(3) 1 d . . P A 4
H51B H 0.3183 -0.1968 0.5483 0.044 Uiso 0.508(3) 1 calc R . P A 4
C52 C 0.1847(15) -0.1943(8) 0.4976(13) 0.034(2) Uani 0.492(3) 1 d . U P A 3
C52B C 0.1822(14) -0.1631(8) 0.4944(12) 0.036(2) Uani 0.508(3) 1 d . . P A 4
C53 C 0.1174(6) -0.1358(7) 0.4657(5) 0.0413(15) Uani 0.492(3) 1 d . . P A 3
H53 H 0.0509 -0.1669 0.4265 0.050 Uiso 0.492(3) 1 calc R . P A 3
C53B C 0.1194(6) -0.0927(8) 0.4991(6) 0.0437(16) Uani 0.508(3) 1 d . . P A 4
H53B H 0.0447 -0.1089 0.4704 0.052 Uiso 0.508(3) 1 calc R . P A 4
C54 C 0.1492(6) -0.0291(7) 0.4922(5) 0.0429(14) Uani 0.492(3) 1 d . . P A 3
H54 H 0.1019 0.0130 0.4733 0.051 Uiso 0.492(3) 1 calc R . P A 3
C54B C 0.1689(5) 0.0025(5) 0.5469(5) 0.0442(12) Uani 0.508(3) 1 d . . P A 4
H54B H 0.1283 0.0536 0.5498 0.053 Uiso 0.508(3) 1 calc R . P A 4
C55 C 0.2485(6) 0.0171(5) 0.5458(5) 0.0383(14) Uani 0.492(3) 1 d . U P A 3
H55 H 0.2658 0.0901 0.5636 0.046 Uiso 0.492(3) 1 calc R . P A 3
C55B C 0.2766(5) 0.0255(4) 0.5911(5) 0.0381(13) Uani 0.508(3) 1 d . . P A 4
H55B H 0.3106 0.0921 0.6225 0.046 Uiso 0.508(3) 1 calc R . P A 4
C58 C 0.5140(7) -0.1210(4) 0.9552(4) 0.0325(13) Uani 0.492(3) 1 d D U P A 3
C58B C 0.5161(5) -0.1566(4) 0.9574(4) 0.0268(10) Uani 0.508(3) 1 d D U P A 4
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl26 0.0730(4) 0.0428(3) 0.0479(4) -0.0007(3) 0.0060(3) -0.0052(3)
Cl56 0.0509(8) 0.0406(8) 0.0477(8) 0.0064(6) -0.0125(6) -0.0037(6)
Cl57 0.0331(6) 0.0522(9) 0.0459(8) -0.0013(6) -0.0052(5) -0.0001(5)
S29 0.0567(7) 0.0456(7) 0.0346(7) -0.0005(5) -0.0122(5) 0.0237(5)
S29B 0.1058(13) 0.0485(9) 0.0581(10) -0.0269(7) -0.0349(9) 0.0360(9)
S59 0.082(3) 0.0468(14) 0.088(2) 0.0378(12) 0.0446(14) 0.0278(15)
S59B 0.0570(13) 0.0381(12) 0.0496(12) 0.0112(10) 0.0206(10) 0.0170(9)
O10 0.0431(11) 0.1097(19) 0.134(2) 0.0811(17) 0.0188(12) 0.0395(12)
O40 0.0476(12) 0.133(2) 0.144(2) -0.098(2) -0.0014(14) 0.0311(13)
N2 0.0322(10) 0.0763(15) 0.0563(14) 0.0293(12) 0.0113(10) 0.0201(10)
N3 0.0393(10) 0.0593(13) 0.0496(13) 0.0151(10) 0.0106(9) 0.0273(10)
N8 0.0368(10) 0.0548(12) 0.0734(15) 0.0357(11) 0.0256(10) 0.0271(9)
N14 0.0282(8) 0.0439(10) 0.0260(9) -0.0053(7) -0.0014(7) 0.0079(7)
N17 0.0327(9) 0.0399(9) 0.0307(10) 0.0034(7) 0.0042(7) 0.0185(7)
N27 0.067(3) 0.057(3) 0.039(3) 0.008(2) -0.005(2) 0.027(2)
N27B 0.051(2) 0.052(2) 0.044(3) -0.014(2) -0.012(2) 0.013(2)
N32 0.0369(11) 0.0803(16) 0.0573(15) -0.0322(12) 0.0008(10) -0.0016(10)
N33 0.0392(10) 0.0568(13) 0.0549(14) -0.0183(10) -0.0060(10) 0.0147(10)
N38 0.0323(10) 0.0548(12) 0.0694(15) -0.0339(11) -0.0163(10) 0.0204(9)
N44 0.025(2) 0.034(2) 0.021(5) 0.002(3) 0.000(3) 0.0085(18)
N44B 0.0293(17) 0.0371(18) 0.022(2) 0.0016(13) -0.0009(16) 0.0060(14)
N47 0.026(3) 0.036(3) 0.034(2) -0.003(2) -0.004(2) 0.016(2)
N47B 0.029(3) 0.031(3) 0.027(2) -0.001(2) -0.002(2) 0.0167(18)
N57 0.049(2) 0.038(2) 0.047(2) 0.0098(17) 0.0106(17) 0.0117(18)
N57B 0.052(2) 0.050(3) 0.0418(19) 0.0127(18) 0.0110(17) 0.012(2)
C1 0.0345(12) 0.080(2) 0.082(2) 0.0530(17) 0.0226(13) 0.0278(13)
C4 0.0549(15) 0.0631(16) 0.0479(16) 0.0127(12) 0.0075(12) 0.0336(13)
C5 0.0731(19) 0.0684(18) 0.0457(16) 0.0033(13) 0.0160(14) 0.0283(15)
C6 0.075(2) 0.0597(17) 0.075(2) 0.0047(15) 0.0414(18) 0.0276(16)
C7 0.0629(18) 0.0538(16) 0.104(3) 0.0368(17) 0.0516(19) 0.0359(14)
C9 0.0403(12) 0.0511(13) 0.0451(14) 0.0189(11) 0.0171(10) 0.0276(11)
C11 0.0432(14) 0.120(3) 0.0437(17) 0.0132(16) 0.0135(13) 0.0235(17)
C12 0.0341(12) 0.094(2) 0.0396(15) -0.0028(13) 0.0051(11) 0.0152(13)
C13 0.0299(11) 0.0734(17) 0.0399(15) -0.0149(12) 0.0029(10) -0.0016(11)
C15 0.0415(12) 0.0768(17) 0.0337(13) 0.0140(11) 0.0079(10) 0.0354(12)
C16 0.0526(14) 0.0439(12) 0.0566(16) 0.0165(11) 0.0262(12) 0.0292(11)
C18 0.0408(12) 0.0402(12) 0.0442(14) 0.0056(9) 0.0076(10) 0.0197(10)
C19 0.0499(14) 0.0390(12) 0.0536(16) -0.0075(10) 0.0172(12) 0.0080(10)
C20 0.0314(10) 0.0408(11) 0.0235(11) -0.0044(8) -0.0021(8) 0.0134(8)
C21 0.0371(11) 0.0382(11) 0.0275(11) -0.0079(8) -0.0006(9) 0.0103(9)
C22 0.0433(12) 0.0423(12) 0.0275(12) -0.0076(9) -0.0006(9) 0.0004(10)
C23 0.0333(11) 0.0616(15) 0.0355(13) -0.0113(11) 0.0055(10) 0.0029(10)
C24 0.0330(11) 0.0609(15) 0.0441(14) -0.0118(11) 0.0028(10) 0.0191(10)
C25 0.0355(11) 0.0436(12) 0.0417(13) -0.0011(9) 0.0020(9) 0.0183(9)
C28 0.030(2) 0.025(3) 0.035(3) -0.004(2) 0.001(2) 0.0031(17)
C28B 0.045(3) 0.033(2) 0.030(3) -0.003(2) -0.004(2) 0.015(2)
C31 0.0350(13) 0.083(2) 0.082(2) -0.0582(18) -0.0099(13) 0.0158(13)
C34 0.0447(13) 0.0664(17) 0.0542(17) -0.0177(13) -0.0108(12) 0.0303(13)
C35 0.0564(16) 0.074(2) 0.0541(19) -0.0052(14) -0.0136(14) 0.0182(15)
C36 0.0606(19) 0.0644(19) 0.085(3) -0.0043(16) -0.0322(18) 0.0195(15)
C37 0.0611(18) 0.0494(15) 0.100(3) -0.0329(16) -0.0482(18) 0.0303(14)
C39 0.0346(11) 0.0495(13) 0.0490(15) -0.0226(11) -0.0150(10) 0.0209(10)
C41 0.072(6) 0.067(5) 0.055(5) 0.008(4) -0.014(4) 0.012(4)
C41B 0.027(2) 0.080(3) 0.048(3) -0.036(2) 0.0023(18) 0.0038(19)
C42 0.033(3) 0.042(3) 0.044(5) 0.000(3) 0.007(3) 0.008(2)
C42B 0.031(2) 0.081(4) 0.045(4) -0.021(3) -0.001(2) 0.0029(19)
C43 0.0278(19) 0.034(2) 0.030(2) 0.0015(16) -0.0005(16) 0.0056(16)
C43B 0.031(2) 0.044(2) 0.029(3) 0.000(2) -0.0014(18) 0.0035(18)
C45 0.030(2) 0.035(2) 0.028(3) -0.0013(17) -0.0006(19) 0.0129(17)
C45B 0.033(2) 0.032(2) 0.027(2) -0.0013(15) -0.0041(16) 0.0150(16)
C46 0.032(2) 0.029(3) 0.041(3) -0.006(2) -0.005(2) 0.012(2)
C46B 0.031(2) 0.027(2) 0.036(3) -0.0028(19) -0.0097(18) 0.0113(18)
C48 0.036(2) 0.043(2) 0.041(3) -0.0090(19) -0.0021(19) 0.019(2)
C48B 0.036(2) 0.038(2) 0.028(2) -0.0049(16) 0.0014(17) 0.0153(19)
C49 0.038(2) 0.037(2) 0.034(3) -0.0022(17) -0.0028(18) 0.0173(18)
C49B 0.038(4) 0.034(3) 0.026(6) -0.005(4) 0.000(4) 0.010(2)
C50 0.027(3) 0.026(4) 0.021(5) 0.006(3) 0.004(3) 0.005(3)
C50B 0.048(5) 0.038(5) 0.030(6) 0.016(3) 0.015(4) 0.026(3)
C51 0.018(3) 0.026(3) 0.021(4) 0.005(3) 0.000(3) 0.003(4)
C51B 0.037(5) 0.042(6) 0.040(5) 0.007(4) 0.002(3) 0.025(4)
C52 0.029(3) 0.034(5) 0.030(3) 0.020(4) 0.002(2) -0.005(4)
C52B 0.034(3) 0.035(5) 0.030(3) 0.016(5) 0.002(2) -0.003(5)
C53 0.028(3) 0.066(5) 0.028(4) 0.005(3) -0.002(3) 0.012(3)
C53B 0.023(3) 0.070(6) 0.040(4) 0.009(4) 0.004(3) 0.017(3)
C54 0.032(3) 0.066(4) 0.037(4) 0.000(4) -0.002(3) 0.027(3)
C54B 0.034(3) 0.061(3) 0.047(4) 0.004(3) 0.005(3) 0.027(2)
C55 0.036(3) 0.049(3) 0.036(4) -0.003(3) -0.006(3) 0.022(2)
C55B 0.035(3) 0.049(3) 0.036(4) 0.000(2) 0.002(2) 0.022(2)
C58 0.041(3) 0.021(2) 0.0343(19) -0.0052(18) 0.0059(17) 0.009(2)
C58B 0.0316(19) 0.019(2) 0.0296(17) -0.0029(17) -0.0013(13) 0.008(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl26 C22 1.755(2) . ?
Cl56 C52 1.761(13) . ?
Cl57 C52B 1.743(13) . ?
S29 C28 1.615(6) . ?
S29B C28B 1.636(6) . ?
S59 C58 1.6396(10) . ?
S59B C58B 1.6388(10) . ?
O10 C1 1.223(3) . ?
O40 C31 1.216(3) . ?
N2 N3 1.388(3) . ?
N2 C1 1.362(4) . ?
N2 C11 1.445(4) . ?
N3 C9 1.307(3) . ?
N8 C1 1.391(4) . ?
N8 C7 1.389(4) . ?
N8 C9 1.379(3) . ?
N14 C13 1.498(3) . ?
N14 C15 1.482(3) . ?
N14 C19 1.491(3) . ?
N17 C16 1.454(3) . ?
N17 C18 1.454(3) . ?
N17 C20 1.400(3) . ?
N27 C28 1.171(7) . ?
N27B C28B 1.137(7) . ?
N32 N33 1.391(3) . ?
N32 C31 1.368(4) . ?
N32 C41 1.389(9) . ?
N32 C41B 1.551(8) . ?
N33 C39 1.306(4) . ?
N38 C31 1.384(4) . ?
N38 C37 1.397(4) . ?
N38 C39 1.378(3) . ?
N44 C43 1.502(12) . ?
N44 C45 1.499(13) . ?
N44 C49 1.497(11) . ?
N44B C43B 1.504(6) . ?
N44B C45B 1.493(5) . ?
N44B C49B 1.488(14) . ?
N47 C46 1.444(7) . ?
N47 C48 1.464(7) . ?
N47 C50 1.343(18) . ?
N47B C46B 1.455(6) . ?
N47B C48B 1.460(7) . ?
N47B C50B 1.45(2) . ?
N57 C58 1.134(6) . ?
N57B C58B 1.127(5) . ?
C4 C5 1.347(4) . ?
C4 C9 1.425(4) . ?
C5 C6 1.414(4) . ?
C6 C7 1.338(5) . ?
C11 C12 1.520(4) . ?
C12 C13 1.515(4) . ?
C15 C16 1.510(3) . ?
C18 C19 1.506(3) . ?
C20 C21 1.400(3) . ?
C20 C25 1.408(3) . ?
C21 C22 1.388(3) . ?
C22 C23 1.374(3) . ?
C23 C24 1.379(4) . ?
C24 C25 1.383(3) . ?
C34 C35 1.352(4) . ?
C34 C39 1.426(4) . ?
C35 C36 1.396(5) . ?
C36 C37 1.332(5) . ?
C41 C42 1.538(12) . ?
C41B C42B 1.503(10) . ?
C42 C43 1.538(8) . ?
C42B C43B 1.507(7) . ?
C45 C46 1.520(6) . ?
C45B C46B 1.521(6) . ?
C48 C49 1.508(6) . ?
C48B C49B 1.505(15) . ?
C50 C51 1.50(3) . ?
C50 C55 1.419(16) . ?
C50B C51B 1.30(3) . ?
C50B C55B 1.416(16) . ?
C51 C52 1.41(2) . ?
C51B C52B 1.36(2) . ?
C52 C53 1.360(14) . ?
C52B C53B 1.374(15) . ?
C53 C54 1.387(10) . ?
C53B C54B 1.377(10) . ?
C54 C55 1.381(9) . ?
C54B C55B 1.388(8) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 N2 C11 120.6(2) . . ?
C1 N2 N3 113.7(2) . . ?
C1 N2 C11 125.8(2) . . ?
C9 N3 N2 103.7(2) . . ?
C7 N8 C1 128.7(2) . . ?
C9 N8 C1 108.3(2) . . ?
C9 N8 C7 123.0(3) . . ?
C15 N14 C13 114.51(19) . . ?
C15 N14 C19 108.55(18) . . ?
C19 N14 C13 109.71(18) . . ?
C16 N17 C18 111.13(17) . . ?
C20 N17 C16 118.60(18) . . ?
C20 N17 C18 118.46(17) . . ?
N33 N32 C41B 112.6(4) . . ?
C31 N32 N33 114.4(2) . . ?
C31 N32 C41 115.0(5) . . ?
C31 N32 C41B 132.8(4) . . ?
C41 N32 N33 130.5(5) . . ?
C39 N33 N32 102.5(2) . . ?
C31 N38 C37 129.1(2) . . ?
C39 N38 C31 108.4(2) . . ?
C39 N38 C37 122.5(3) . . ?
C45 N44 C43 113.6(8) . . ?
C49 N44 C43 109.5(8) . . ?
C49 N44 C45 108.6(6) . . ?
C45B N44B C43B 111.9(3) . . ?
C49B N44B C43B 113.5(6) . . ?
C49B N44B C45B 108.5(6) . . ?
C46 N47 C48 111.3(6) . . ?
C50 N47 C46 119.1(8) . . ?
C50 N47 C48 116.8(9) . . ?
C46B N47B C48B 112.1(4) . . ?
C50B N47B C46B 115.4(8) . . ?
C50B N47B C48B 118.4(10) . . ?
O10 C1 N2 129.9(3) . . ?
O10 C1 N8 127.5(3) . . ?
N2 C1 N8 102.5(2) . . ?
C5 C4 C9 119.0(3) . . ?
C4 C5 C6 122.0(3) . . ?
C7 C6 C5 119.7(3) . . ?
C6 C7 N8 118.9(3) . . ?
N3 C9 N8 111.7(2) . . ?
N3 C9 C4 131.0(2) . . ?
N8 C9 C4 117.3(2) . . ?
N2 C11 C12 112.9(2) . . ?
C13 C12 C11 109.8(3) . . ?
N14 C13 C12 113.7(2) . . ?
N14 C15 C16 110.57(18) . . ?
N17 C16 C15 111.7(2) . . ?
N17 C18 C19 111.09(19) . . ?
N14 C19 C18 111.22(19) . . ?
N17 C20 C21 121.52(18) . . ?
N17 C20 C25 121.00(19) . . ?
C21 C20 C25 117.32(19) . . ?
C22 C21 C20 119.4(2) . . ?
C21 C22 Cl26 117.98(19) . . ?
C23 C22 Cl26 118.68(18) . . ?
C23 C22 C21 123.3(2) . . ?
C22 C23 C24 117.4(2) . . ?
C23 C24 C25 121.2(2) . . ?
C24 C25 C20 121.4(2) . . ?
N27 C28 S29 178.9(5) . . ?
N27B C28B S29B 177.9(5) . . ?
O40 C31 N32 130.5(4) . . ?
O40 C31 N38 127.4(4) . . ?
N32 C31 N38 102.0(2) . . ?
C35 C34 C39 119.5(2) . . ?
C34 C35 C36 121.8(3) . . ?
C37 C36 C35 120.0(3) . . ?
C36 C37 N38 119.3(3) . . ?
N33 C39 N38 112.7(2) . . ?
N33 C39 C34 130.5(2) . . ?
N38 C39 C34 116.8(2) . . ?
N32 C41 C42 110.9(7) . . ?
C42B C41B N32 114.2(6) . . ?
C41 C42 C43 104.7(5) . . ?
C41B C42B C43B 111.5(6) . . ?
N44 C43 C42 112.9(5) . . ?
N44B C43B C42B 108.9(4) . . ?
N44 C45 C46 110.7(6) . . ?
N44B C45B C46B 111.1(4) . . ?
N47 C46 C45 112.3(5) . . ?
N47B C46B C45B 112.0(4) . . ?
N47 C48 C49 111.1(4) . . ?
N47B C48B C49B 111.1(7) . . ?
N44 C49 C48 110.7(6) . . ?
N44B C49B C48B 110.4(10) . . ?
N47 C50 C51 120.3(13) . . ?
N47 C50 C55 124.5(12) . . ?
C55 C50 C51 115.0(13) . . ?
C51B C50B N47B 125.6(16) . . ?
C51B C50B C55B 117.0(17) . . ?
C55B C50B N47B 117.0(14) . . ?
C52 C51 C50 116.3(16) . . ?
C50B C51B C52B 125.2(18) . . ?
C51 C52 Cl56 114.9(11) . . ?
C53 C52 Cl56 118.3(11) . . ?
C53 C52 C51 125.6(12) . . ?
C51B C52B Cl57 120.6(12) . . ?
C51B C52B C53B 119.4(14) . . ?
C53B C52B Cl57 119.5(11) . . ?
C52 C53 C54 117.6(8) . . ?
C52B C53B C54B 117.4(8) . . ?
C55 C54 C53 121.1(6) . . ?
C53B C54B C55B 121.5(5) . . ?
C54 C55 C50 123.7(8) . . ?
C54B C55B C50B 118.9(10) . . ?
N57 C58 S59 178.7(8) . . ?
N57B C58B S59B 175.7(6) . . ?
_shelx_res_file
;
pn180815_uo_traz_1_180814_scn.res created by SHELXL-2014/7
TITL pn180815_uo_traz_1_180814_scn_a.res in P-1
REM Old TITL PN180815_UO_Traz_1_180814_SCN in P-1 #2
REM SHELXT solution in P-1
REM R1 0.279, Rweak 0.044, Alpha 0.101, Orientation as input
REM Formula found by SHELXT: C45 N11 O4 Cl57
CELL 1.54184 12.14821 13.184753 13.825099 90.263 90.218 108.0045
ZERR 4 0.000219 0.00021 0.000166 0.0012 0.0012 0.0015
LATT 1
SFAC C H Cl N O S
UNIT 80 92 4 24 4 4
DFIX 1.64 0.001 S59B C58B S59 C58
SADI N32 C41 N32 C41B
RIGU C50 C51 C52 C55
RIGU 0.001 0.001 N32 C41B C42B
RIGU 0.001 0.001 S59B N57B C58B
RIGU 0.001 0.001 S59 N57 C58
L.S. 4
PLAN 20
TEMP -113
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.041100 2.301400
FVAR 4.47182 0.50234 0.49186
CL26 3 0.848738 0.827495 -0.051591 11.00000 0.07302 0.04280 =
0.04790 -0.00072 0.00601 -0.00520
PART 3
CL56 3 0.152843 -0.326911 0.456325 31.00000 0.05087 0.04063 =
0.04770 0.00640 -0.01246 -0.00371
PART 0
PART 4
CL57 3 0.122838 -0.285895 0.436805 -31.00000 0.03307 0.05224 =
0.04594 -0.00127 -0.00515 -0.00013
PART 0
PART 1
S29 6 0.546884 0.315719 0.589197 21.00000 0.05667 0.04564 =
0.03456 -0.00053 -0.01216 0.02370
PART 0
PART 2
S29B 6 0.452722 0.281784 0.465425 -21.00000 0.10577 0.04853 =
0.05807 -0.02685 -0.03493 0.03598
PART 0
PART 3
S59 6 0.456594 -0.210868 1.037314 31.00000 0.08188 0.04676 =
0.08837 0.03785 0.04458 0.02776
PART 0
PART 4
S59B 6 0.437933 -0.223312 1.046264 -31.00000 0.05700 0.03811 =
0.04961 0.01123 0.02056 0.01705
PART 0
O10 5 0.078538 0.115921 0.333451 11.00000 0.04312 0.10969 =
0.13381 0.08109 0.01883 0.03947
O40 5 0.930349 0.387011 0.832421 11.00000 0.04764 0.13316 =
0.14376 -0.09769 -0.00145 0.03111
N2 4 0.014860 0.265141 0.313208 11.00000 0.03223 0.07632 =
0.05630 0.02925 0.01130 0.02009
N3 4 -0.069804 0.291254 0.260309 11.00000 0.03928 0.05932 =
0.04963 0.01514 0.01062 0.02733
N8 4 -0.078201 0.122074 0.236581 11.00000 0.03681 0.05483 =
0.07339 0.03568 0.02559 0.02711
N14 4 0.384219 0.417645 0.248129 11.00000 0.02819 0.04387 =
0.02604 -0.00527 -0.00137 0.00792
AFIX 13
H14 2 0.425678 0.443980 0.310348 11.00000 -1.20000
AFIX 0
N17 4 0.579403 0.501470 0.121631 11.00000 0.03267 0.03991 =
0.03068 0.00338 0.00424 0.01852
PART 1
N27 4 0.457132 0.373206 0.419731 21.00000 0.06726 0.05746 =
0.03854 0.00813 -0.00515 0.02664
PART 0
PART 2
N27B 4 0.551098 0.439309 0.601379 -21.00000 0.05060 0.05233 =
0.04386 -0.01393 -0.01177 0.01305
PART 0
N32 4 0.997697 0.239523 0.811585 11.00000 0.03693 0.08025 =
0.05733 -0.03220 0.00082 -0.00156
N33 4 1.080983 0.213222 0.756891 11.00000 0.03923 0.05676 =
0.05491 -0.01832 -0.00602 0.01474
N38 4 1.081854 0.380746 0.731862 11.00000 0.03232 0.05476 =
0.06936 -0.03392 -0.01634 0.02040
PART 3
N44 4 0.621778 0.091636 0.751416 31.00000 0.02503 0.03385 =
0.02131 0.00186 0.00049 0.00851
AFIX 13
H44 2 0.583166 0.058595 0.812370 31.00000 -1.20000
AFIX 0
PART 0
PART 4
N44B 4 0.661333 0.008867 0.738022 -31.00000 0.02930 0.03713 =
0.02182 0.00158 -0.00094 0.00597
AFIX 13
H44B 2 0.621541 -0.033384 0.794772 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
N47 4 0.427326 0.007464 0.620963 31.00000 0.02634 0.03556 =
0.03442 -0.00273 -0.00368 0.01644
PART 0
PART 4
N47B 4 0.452674 -0.020515 0.625723 -31.00000 0.02920 0.03055 =
0.02680 -0.00095 -0.00232 0.01667
PART 0
PART 3
N57 4 0.555638 -0.058227 0.899312 31.00000 0.04940 0.03830 =
0.04662 0.00976 0.01057 0.01174
PART 0
PART 4
N57B 4 0.565999 -0.115554 0.892606 -31.00000 0.05179 0.05037 =
0.04177 0.01275 0.01100 0.01177
PART 0
C1 1 0.014337 0.162539 0.299957 11.00000 0.03450 0.08034 =
0.08229 0.05304 0.02256 0.02782
C4 1 -0.218689 0.178427 0.148193 11.00000 0.05492 0.06312 =
0.04793 0.01272 0.00747 0.03360
AFIX 43
H4 2 -0.252954 0.231422 0.130413 11.00000 -1.20000
AFIX 0
C5 1 -0.258661 0.079154 0.110783 11.00000 0.07310 0.06840 =
0.04568 0.00328 0.01600 0.02827
AFIX 43
H5 2 -0.321032 0.063199 0.065758 11.00000 -1.20000
AFIX 0
C6 1 -0.210650 -0.002005 0.136466 11.00000 0.07484 0.05968 =
0.07507 0.00465 0.04138 0.02756
AFIX 43
H6 2 -0.241562 -0.071632 0.109789 11.00000 -1.20000
AFIX 0
C7 1 -0.121498 0.019694 0.198500 11.00000 0.06292 0.05379 =
0.10424 0.03685 0.05162 0.03586
AFIX 43
H7 2 -0.088332 -0.034081 0.216221 11.00000 -1.20000
AFIX 0
C9 1 -0.124221 0.202696 0.214841 11.00000 0.04034 0.05114 =
0.04508 0.01889 0.01711 0.02760
C11 1 0.092966 0.343192 0.375770 11.00000 0.04320 0.11990 =
0.04372 0.01317 0.01353 0.02353
AFIX 23
H11A 2 0.122891 0.305679 0.426449 11.00000 -1.20000
H11B 2 0.049575 0.385927 0.408256 11.00000 -1.20000
AFIX 0
C12 1 0.194530 0.417765 0.321700 11.00000 0.03409 0.09393 =
0.03957 -0.00279 0.00506 0.01521
AFIX 23
H12A 2 0.165754 0.458637 0.273204 11.00000 -1.20000
H12B 2 0.245626 0.469062 0.367667 11.00000 -1.20000
AFIX 0
C13 1 0.262228 0.353820 0.271633 11.00000 0.02987 0.07336 =
0.03994 -0.01486 0.00290 -0.00160
AFIX 23
H13A 2 0.263662 0.293703 0.313738 11.00000 -1.20000
H13B 2 0.221565 0.323317 0.210968 11.00000 -1.20000
AFIX 0
C15 1 0.394831 0.511255 0.185715 11.00000 0.04151 0.07675 =
0.03369 0.01396 0.00790 0.03541
AFIX 23
H15A 2 0.358230 0.559782 0.217921 11.00000 -1.20000
H15B 2 0.353787 0.487293 0.123712 11.00000 -1.20000
AFIX 0
C16 1 0.520556 0.570300 0.166205 11.00000 0.05259 0.04390 =
0.05658 0.01654 0.02621 0.02917
AFIX 23
H16A 2 0.525645 0.631219 0.122978 11.00000 -1.20000
H16B 2 0.559844 0.599090 0.227848 11.00000 -1.20000
AFIX 0
C18 1 0.568791 0.407780 0.180417 11.00000 0.04078 0.04024 =
0.04422 0.00558 0.00763 0.01967
AFIX 23
H18A 2 0.610139 0.429961 0.242583 11.00000 -1.20000
H18B 2 0.605337 0.360258 0.146525 11.00000 -1.20000
AFIX 0
C19 1 0.443742 0.347874 0.199885 11.00000 0.04986 0.03898 =
0.05365 -0.00750 0.01722 0.00801
AFIX 23
H19A 2 0.403917 0.320610 0.138072 11.00000 -1.20000
H19B 2 0.439139 0.285947 0.241686 11.00000 -1.20000
AFIX 0
C20 1 0.683958 0.548624 0.073761 11.00000 0.03139 0.04084 =
0.02350 -0.00437 -0.00210 0.01338
C21 1 0.716707 0.655395 0.044778 11.00000 0.03705 0.03816 =
0.02747 -0.00787 -0.00063 0.01028
AFIX 43
H21 2 0.671670 0.699816 0.062840 11.00000 -1.20000
AFIX 0
C22 1 0.815550 0.695748 -0.010574 11.00000 0.04327 0.04228 =
0.02753 -0.00764 -0.00062 0.00036
C23 1 0.885285 0.636297 -0.038188 11.00000 0.03335 0.06162 =
0.03550 -0.01135 0.00552 0.00292
AFIX 43
H23 2 0.952248 0.666127 -0.076372 11.00000 -1.20000
AFIX 0
C24 1 0.854263 0.531606 -0.008300 11.00000 0.03302 0.06095 =
0.04406 -0.01181 0.00279 0.01910
AFIX 43
H24 2 0.900995 0.488561 -0.025892 11.00000 -1.20000
AFIX 0
C25 1 0.756368 0.488171 0.046810 11.00000 0.03549 0.04365 =
0.04172 -0.00112 0.00203 0.01835
AFIX 43
H25 2 0.737605 0.416035 0.066891 11.00000 -1.20000
AFIX 0
PART 1
C28 1 0.494965 0.349966 0.491304 21.00000 0.03005 0.02476 =
0.03548 -0.00364 0.00078 0.00309
PART 0
PART 2
C28B 1 0.512629 0.375077 0.544806 -21.00000 0.04454 0.03298 =
0.03003 -0.00312 -0.00436 0.01487
PART 0
C31 1 0.993857 0.341079 0.797873 11.00000 0.03495 0.08343 =
0.08201 -0.05822 -0.00993 0.01581
C34 1 1.220784 0.326235 0.640841 11.00000 0.04472 0.06637 =
0.05422 -0.01768 -0.01078 0.03034
AFIX 43
H34 2 1.256776 0.274359 0.623223 11.00000 -1.20000
AFIX 0
C35 1 1.255916 0.424334 0.600833 11.00000 0.05639 0.07438 =
0.05409 -0.00517 -0.01360 0.01825
AFIX 43
H35 2 1.316456 0.440331 0.554620 11.00000 -1.20000
AFIX 0
C36 1 1.205605 0.502727 0.625623 11.00000 0.06063 0.06441 =
0.08471 -0.00427 -0.03216 0.01952
AFIX 43
H36 2 1.232123 0.571059 0.596499 11.00000 -1.20000
AFIX 0
C37 1 1.120431 0.481769 0.690095 11.00000 0.06111 0.04938 =
0.10046 -0.03287 -0.04817 0.03028
AFIX 43
H37 2 1.086257 0.535016 0.707498 11.00000 -1.20000
AFIX 0
C39 1 1.129304 0.301202 0.709681 11.00000 0.03456 0.04948 =
0.04902 -0.02260 -0.01503 0.02092
PART 3
C41 1 0.914668 0.177987 0.874024 31.00000 0.07172 0.06726 =
0.05536 0.00807 -0.01373 0.01245
AFIX 23
H41A 2 0.881040 0.224850 0.912075 31.00000 -1.20000
H41B 2 0.951508 0.140564 0.919721 31.00000 -1.20000
AFIX 0
PART 0
PART 4
C41B 1 0.933324 0.149226 0.881584 -31.00000 0.02659 0.08044 =
0.04775 -0.03644 0.00233 0.00378
AFIX 23
H41C 2 0.971380 0.092810 0.879835 -31.00000 -1.20000
H41D 2 0.941151 0.178461 0.948234 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
C42 1 0.817903 0.095687 0.817602 31.00000 0.03310 0.04160 =
0.04361 -0.00041 0.00676 0.00761
AFIX 23
H42A 2 0.772153 0.038853 0.861029 31.00000 -1.20000
H42B 2 0.850514 0.062677 0.765050 31.00000 -1.20000
AFIX 0
PART 0
PART 4
C42B 1 0.806917 0.099689 0.858806 -31.00000 0.03144 0.08065 =
0.04535 -0.02112 -0.00111 0.00295
AFIX 23
H42C 2 0.767856 0.155353 0.861208 -31.00000 -1.20000
H42D 2 0.771346 0.045662 0.908369 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
C43 1 0.742540 0.159961 0.776045 31.00000 0.02785 0.03407 =
0.02987 0.00149 -0.00050 0.00559
AFIX 23
H43A 2 0.738589 0.214830 0.823869 31.00000 -1.20000
H43B 2 0.779646 0.197216 0.717015 31.00000 -1.20000
AFIX 0
PART 0
PART 4
C43B 1 0.788862 0.047629 0.760277 -31.00000 0.03105 0.04363 =
0.02943 -0.00048 -0.00143 0.00347
AFIX 23
H43C 2 0.829751 0.099598 0.710827 -31.00000 -1.20000
H43D 2 0.820580 -0.013086 0.759291 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
C45 1 0.617349 0.004067 0.680517 31.00000 0.03003 0.03542 =
0.02801 -0.00127 -0.00056 0.01285
AFIX 23
H45A 2 0.657536 -0.044062 0.708228 31.00000 -1.20000
H45B 2 0.657949 0.035119 0.620528 31.00000 -1.20000
AFIX 0
PART 0
PART 4
C45B 1 0.634617 -0.063073 0.651560 -31.00000 0.03347 0.03168 =
0.02693 -0.00128 -0.00410 0.01501
AFIX 23
H45C 2 0.665441 -0.123488 0.661879 -31.00000 -1.20000
H45D 2 0.673138 -0.023339 0.594077 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
C46 1 0.492772 -0.059322 0.656623 31.00000 0.03191 0.02919 =
0.04075 -0.00551 -0.00456 0.01160
AFIX 23
H46A 2 0.492134 -0.114070 0.607191 31.00000 -1.20000
H46B 2 0.455079 -0.096609 0.715448 31.00000 -1.20000
AFIX 0
PART 0
PART 4
C46B 1 0.504848 -0.105753 0.633256 -31.00000 0.03094 0.02729 =
0.03576 -0.00284 -0.00970 0.01135
AFIX 23
H46C 2 0.490240 -0.148117 0.572595 -31.00000 -1.20000
H46D 2 0.467898 -0.153716 0.686770 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
C48 1 0.431683 0.094029 0.689030 31.00000 0.03566 0.04329 =
0.04050 -0.00902 -0.00207 0.01933
AFIX 23
H48A 2 0.393122 0.063662 0.749987 31.00000 -1.20000
H48B 2 0.389249 0.140317 0.661318 31.00000 -1.20000
AFIX 0
PART 0
PART 4
C48B 1 0.481275 0.051991 0.708658 -31.00000 0.03645 0.03832 =
0.02777 -0.00493 0.00138 0.01534
AFIX 23
H48C 2 0.446039 0.013336 0.767666 -31.00000 -1.20000
H48D 2 0.448552 0.111231 0.698562 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
C49 1 0.554939 0.159828 0.710376 31.00000 0.03760 0.03651 =
0.03431 -0.00225 -0.00279 0.01731
AFIX 23
H49A 2 0.592236 0.193674 0.650103 31.00000 -1.20000
H49B 2 0.555571 0.217126 0.757110 31.00000 -1.20000
AFIX 0
PART 0
PART 4
C49B 1 0.610241 0.096599 0.722551 -31.00000 0.03800 0.03446 =
0.02569 -0.00517 -0.00010 0.00960
AFIX 23
H49C 2 0.645298 0.138006 0.664784 -31.00000 -1.20000
H49D 2 0.627460 0.145367 0.779133 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
C50 1 0.326037 -0.038116 0.575582 31.00000 0.02724 0.02620 =
0.02110 0.00617 0.00374 0.00537
PART 0
PART 4
C50B 1 0.335279 -0.052155 0.588504 -31.00000 0.04760 0.03818 =
0.03035 0.01628 0.01487 0.02563
PART 0
PART 3
C51 1 0.292121 -0.153500 0.545566 31.00000 0.01798 0.02577 =
0.02149 0.00474 0.00040 0.00295
AFIX 43
H51 2 0.340427 -0.196515 0.558220 31.00000 -1.20000
AFIX 0
PART 0
PART 4
C51B 1 0.283036 -0.141813 0.544762 -31.00000 0.03719 0.04246 =
0.03955 0.00660 0.00153 0.02543
AFIX 43
H51B 2 0.318277 -0.196762 0.548325 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
C52 1 0.184694 -0.194341 0.497612 31.00000 0.02909 0.03383 =
0.03014 0.02042 0.00195 -0.00511
PART 0
PART 4
C52B 1 0.182182 -0.163123 0.494431 -31.00000 0.03375 0.03467 =
0.03021 0.01609 0.00216 -0.00298
PART 0
PART 3
C53 1 0.117375 -0.135809 0.465666 31.00000 0.02808 0.06570 =
0.02847 0.00536 -0.00167 0.01206
AFIX 43
H53 2 0.050932 -0.166944 0.426536 31.00000 -1.20000
AFIX 0
PART 0
PART 4
C53B 1 0.119355 -0.092650 0.499064 -31.00000 0.02305 0.06981 =
0.04022 0.00854 0.00446 0.01725
AFIX 43
H53B 2 0.044677 -0.108943 0.470373 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
C54 1 0.149180 -0.029063 0.492247 31.00000 0.03248 0.06646 =
0.03741 -0.00024 -0.00160 0.02671
AFIX 43
H54 2 0.101905 0.012982 0.473335 31.00000 -1.20000
AFIX 0
PART 0
PART 4
C54B 1 0.168870 0.002539 0.546928 -31.00000 0.03403 0.06091 =
0.04651 0.00449 0.00515 0.02738
AFIX 43
H54B 2 0.128344 0.053625 0.549776 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
C55 1 0.248470 0.017149 0.545773 31.00000 0.03585 0.04945 =
0.03562 -0.00329 -0.00585 0.02203
AFIX 43
H55 2 0.265799 0.090090 0.563639 31.00000 -1.20000
AFIX 0
PART 0
PART 4
C55B 1 0.276650 0.025455 0.591079 -31.00000 0.03532 0.04942 =
0.03565 -0.00037 0.00232 0.02193
AFIX 43
H55B 2 0.310557 0.092120 0.622521 -31.00000 -1.20000
AFIX 0
PART 0
PART 3
C58 1 0.514041 -0.120966 0.955183 31.00000 0.04146 0.02138 =
0.03428 -0.00519 0.00588 0.00921
PART 0
PART 4
C58B 1 0.516069 -0.156586 0.957433 -31.00000 0.03162 0.01927 =
0.02964 -0.00290 -0.00126 0.00826
HKLF 4
REM pn180815_uo_traz_1_180814_scn_a.res in P-1
REM R1 = 0.0574 for 7824 Fo > 4sig(Fo) and 0.0599 for all 8412 data
REM 723 parameters refined using 45 restraints
END
WGHT 0.0409 2.3059
REM Highest difference peak 0.514, deepest hole -0.548, 1-sigma level 0.049
Q1 1 0.9202 0.3998 0.8107 11.00000 0.05 0.51
Q2 1 0.9095 0.3392 0.8798 11.00000 0.05 0.50
Q3 1 0.8896 0.8124 0.0022 11.00000 0.05 0.37
Q4 1 0.0706 0.0985 0.3056 11.00000 0.05 0.34
Q5 1 0.9650 0.2751 0.8256 11.00000 0.05 0.34
Q6 1 1.0795 0.4648 0.7435 11.00000 0.05 0.33
Q7 1 0.0800 0.1580 0.3567 11.00000 0.05 0.30
Q8 1 0.5107 0.3182 0.4411 11.00000 0.05 0.26
Q9 1 1.0427 0.3561 0.7754 11.00000 0.05 0.26
Q10 1 -0.0371 0.1365 0.2752 11.00000 0.05 0.25
Q11 1 0.9891 0.1987 0.8398 11.00000 0.05 0.25
Q12 1 -0.2143 0.0539 0.1289 11.00000 0.05 0.24
Q13 1 1.2181 0.4424 0.6260 11.00000 0.05 0.24
Q14 1 -0.0780 0.0020 0.2506 11.00000 0.05 0.23
Q15 1 1.0201 0.2089 0.7693 11.00000 0.05 0.23
Q16 1 -0.1755 -0.0079 0.1913 11.00000 0.05 0.21
Q17 1 1.1037 0.4972 0.6650 11.00000 0.05 0.21
Q18 1 -0.0637 -0.0209 0.2666 11.00000 0.05 0.20
Q19 1 0.8596 0.0690 0.8629 11.00000 0.05 0.20
Q20 1 0.5351 0.0688 0.9328 11.00000 0.05 0.20
;
_shelx_res_checksum 91508
_shelx_hkl_file
;
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0 0 -2 14767.2 471.432 67
0 0 -2 15864.7 491.962 14
0 0 -3 2178.74 111.478 14
0 0 -3 2129.35 88.2079 67
0 0 -4 40565.3 1260.07 60
0 0 -4 42160.0 1304.05 14
0 0 4 41244.9 1300.26 77
0 0 4 39987.2 1269.14 63
0 0 -5 5009.60 225.988 14
0 0 5 4494.16 217.723 77
0 0 5 4346.56 176.456 65
0 0 5 4604.25 185.664 4
0 0 5 4733.52 188.736 63
0 0 -5 4773.65 175.055 60
0 0 6 6992.92 259.214 65
0 0 6 7659.58 274.147 4
0 0 -6 7413.40 247.277 6
0 0 -6 7981.66 329.517 14
0 0 6 7683.47 277.456 63
0 0 6 7934.20 329.457 77
0 0 6 7314.60 281.565 87
0 0 6 6496.95 238.973 64
0 0 7 909.330 68.0586 4
0 0 7 730.064 82.0152 79
0 0 7 769.998 83.4583 62
0 0 -7 879.205 55.0567 6
0 0 7 762.284 65.4144 63
0 0 7 809.533 96.8284 77
0 0 -7 813.577 99.5302 14
0 0 7 801.163 70.9232 87
0 0 -8 7438.96 274.188 6
0 0 8 7993.80 381.638 77
0 0 8 7697.84 340.979 62
0 0 8 7858.53 347.157 79
0 0 -8 8244.55 380.867 14
0 0 9 7360.46 342.646 62
0 0 -9 7208.23 270.472 50
0 0 9 7339.70 384.782 77
0 0 -9 7749.67 382.265 14
0 0 9 8247.57 389.683 78
0 0 9 7103.05 344.578 79
0 0 -9 7060.72 267.618 6
0 0 10 12266.1 544.854 61
0 0 -10 11777.2 414.608 51
0 0 -10 11948.8 417.814 50
0 0 -10 12111.3 547.506 14
0 0 10 11761.3 504.459 79
0 0 10 12266.6 506.243 62
0 0 -10 12105.0 420.801 15
0 0 -10 11688.0 414.472 49
0 0 10 12757.7 558.932 78
0 0 10 11620.8 514.149 83
0 0 -11 3884.90 179.240 50
0 0 -11 3899.94 175.708 49
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10 2 0 40.3918 41.0015 28
10 2 0 21.3656 67.2351 88
-10 -2 0 68.4321 43.2817 41
-10 -2 0 120.468 42.6739 22
-10 -2 0 48.2815 85.6889 67
10 2 0 115.330 87.5259 1
10 2 0 39.7294 34.9871 66
-10 -2 0 46.4336 36.6711 10
-10 -2 0 132.008 53.3608 59
-10 -2 0 90.2731 52.3499 58
10 2 1 3791.05 181.676 28
-10 -2 -1 3385.89 180.526 41
-10 -2 -1 3452.00 314.652 67
10 2 1 3785.87 318.953 1
-10 -2 -1 3643.81 179.171 10
-10 -2 -1 3995.02 193.902 59
-10 -2 -1 3667.47 191.985 58
10 2 2 5.03557 36.3709 28
-10 -2 -2-6.13961 42.7886 45
-10 -2 -2 11.4665 43.1580 41
10 2 2 25.0117 78.6738 1
-10 -2 -2 78.0438 98.6888 67
-10 -2 -2-11.3756 38.8987 10
-10 -2 -2-37.1537 51.1975 59
-10 -2 -2 25.8673 44.6497 58
10 2 3 6257.01 251.111 28
-10 -2 -3 6117.43 266.428 41
10 2 3 5964.65 423.713 1
-10 -2 -3 6402.50 268.894 10
-10 -2 -3 6802.90 276.962 59
-10 -2 -4 316.739 62.3988 45
10 2 4 281.590 109.138 1
-10 -2 -4 159.721 104.681 67
-10 -2 -4 503.466 66.5587 59
-10 -2 -4 418.952 72.4493 58
-10 -2 -5 94.6815 50.8841 45
-10 -2 -5 40.6916 46.1957 44
-10 -2 -5 63.2352 48.8301 41
-10 -2 -5 93.8558 51.1106 70
-10 -2 -5 130.593 102.164 67
-10 -2 -5 109.472 48.0167 10
-10 -2 -5 102.674 54.1527 58
-10 -2 -6 16.8511 43.6117 45
-10 -2 -6 32.5665 40.2121 44
-10 -2 -6 49.6601 47.9681 41
-10 -2 -6-11.7155 48.4379 70
-10 -2 -6 10.2389 38.8500 69
-10 -2 -6 61.4918 51.5115 34
-10 -2 -6 44.2627 43.5945 10
-10 -2 -7 609.663 66.7266 45
-10 -2 -7 395.400 56.1651 44
-10 -2 -7 497.245 63.3122 41
-10 -2 -7 562.681 66.5283 70
-10 -2 -7 548.945 58.6202 69
-10 -2 -7 427.963 65.1774 34
-10 -2 -8 947.691 72.4313 44
-10 -2 -8 879.898 76.7175 41
-10 -2 -8 874.372 74.0726 70
-10 -2 -8 930.352 80.5297 34
-10 -2 -9 524.805 57.3942 42
-10 -2 -9 436.091 52.4655 41
-10 -2 -9 571.671 58.2659 34
-10 -2 -10 2.92181 25.8495 42
-10 -2 -10 25.1218 28.0189 41
10 3 -11 3750.51 130.405 51
10 3 -11 3606.12 128.960 74
-10 -3 11 3830.89 132.115 19
10 3 -10-6.17446 19.8103 51
10 3 -10 4.34465 20.1862 26
10 3 -10 5.79141 19.1148 74
-10 -3 10 6.88603 21.9858 19
10 3 -9 1402.36 82.0111 26
-10 -3 9 1442.21 82.0140 22
10 3 -9 1329.70 73.1004 74
10 3 -8 546.623 55.2378 28
10 3 -8 624.431 60.5642 26
-10 -3 8 512.269 50.6970 96
-10 -3 8 717.795 62.4585 22
10 3 -8 525.445 47.7034 74
10 3 -8 525.850 51.3050 39
10 3 -8 531.752 62.2365 66
10 3 -7 473.851 59.7640 28
10 3 -7 584.892 63.3296 26
-10 -3 7 453.172 53.3623 96
10 3 -7 590.976 51.6708 74
10 3 -7 550.738 65.5265 66
10 3 -6 1687.44 111.394 28
10 3 -6 1859.06 115.750 26
-10 -3 6 1531.95 99.5227 96
-10 -3 6 1878.70 112.764 22
10 3 -6 1804.37 93.6361 74
10 3 -5 5.62080 41.2935 28
-10 -3 5 18.1652 32.5190 96
-10 -3 5-9.59215 40.4304 22
10 3 -5 45.6639 48.7224 66
10 3 -4 11.6842 41.8322 28
-10 -3 4 23.0563 30.6148 96
10 3 -4 5.47686 39.2170 25
-10 -3 4 7.99338 29.1168 44
-10 -3 4 44.1248 42.6170 22
10 3 -4-11.5674 45.2336 66
-10 -3 4-10.5029 39.2177 59
-10 -3 3 5419.48 234.970 96
10 3 -3 6063.03 251.724 25
-10 -3 3 5828.81 242.914 22
10 3 -3 6035.46 254.277 66
-10 -3 3 6020.23 252.833 59
10 3 -2 107.062 53.1188 28
-10 -3 2 182.822 39.9965 96
10 3 -2 182.985 47.7832 25
-10 -3 2 150.120 42.8412 22
10 3 -2 131.836 46.5352 66
-10 -3 2 147.632 51.5378 59
10 3 -1 5359.32 246.895 28
10 3 -1 5836.44 238.674 25
-10 -3 1 5251.82 227.590 41
-10 -3 1 5672.54 235.871 22
10 3 -1 6084.22 243.627 66
-10 -3 1 6348.89 250.576 58
10 3 0 272.317 99.1633 1
10 3 0 372.449 60.7174 28
10 3 0 420.761 54.6775 25
10 3 0 292.319 99.5470 88
-10 -3 0 368.926 56.7309 41
-10 -3 0 363.712 54.5119 22
-10 -3 0 165.809 100.992 67
10 3 0 312.409 49.4096 66
-10 -3 0 335.765 65.5468 59
-10 -3 0 323.453 61.8633 58
10 3 1 2262.83 242.384 1
10 3 1 2291.76 131.609 28
10 3 1 2079.19 229.698 88
-10 -3 -1 2268.25 131.600 41
-10 -3 -1 2167.93 253.296 67
-10 -3 -1 2419.26 142.861 59
-10 -3 -1 2203.98 139.390 58
10 3 2 483.087 58.6593 28
-10 -3 -2 591.220 73.5331 45
10 3 2 305.097 107.814 88
-10 -3 -2 517.008 63.5513 41
-10 -3 -2 404.364 132.152 67
10 3 2 707.760 147.170 1
-10 -3 -2 478.104 71.5006 59
-10 -3 -2 534.315 73.7380 58
10 3 3 3068.79 151.772 28
-10 -3 -3 3613.42 181.144 45
10 3 3 3112.23 292.749 88
-10 -3 -3 3374.61 173.508 41
-10 -3 -3 3723.33 179.423 59
10 3 3 3648.46 313.555 1
10 3 4 631.489 145.860 88
-10 -3 -4 802.108 80.1233 59
-10 -3 -4 868.203 90.1256 58
-10 -3 -5 344.405 62.9547 45
10 3 5 190.653 91.1410 88
-10 -3 -5 437.360 62.7338 44
-10 -3 -5 339.830 60.4506 70
-10 -3 -5 575.258 76.4835 58
-10 -3 -6-10.4169 44.1819 45
-10 -3 -6 4.94063 39.7595 44
-10 -3 -6-15.2320 42.5280 41
-10 -3 -6-10.5177 39.8999 70
-10 -3 -6 4.51172 33.9630 69
-10 -3 -6-16.8254 45.7563 34
-10 -3 -6 22.5175 47.1518 58
-10 -3 -7 1226.94 88.6720 45
-10 -3 -7 1250.85 85.6524 44
-10 -3 -7 1277.14 91.8355 41
-10 -3 -7 1159.78 87.3831 70
-10 -3 -7 1211.19 92.4131 34
-10 -3 -8 496.587 49.9332 44
-10 -3 -8 453.274 54.8138 41
-10 -3 -8 442.163 49.9502 70
-10 -3 -8 530.407 60.6027 34
-10 -3 -9 1702.98 93.7275 42
-10 -3 -9 1532.40 89.3857 41
-10 -3 -9 1758.81 90.6735 34
-10 -3 -10 62.6599 24.9430 42
-10 -3 -10 88.5084 26.5435 41
10 4 -10 375.431 28.6212 51
10 4 -10 279.895 23.5692 74
-10 -4 10 340.927 30.7150 19
10 4 -9 1187.60 65.3471 26
-10 -4 9 1104.72 65.3046 22
10 4 -9 1035.03 56.1504 74
10 4 -8 456.832 47.4625 28
10 4 -8 375.289 44.2811 26
10 4 -8 375.101 36.9490 74
10 4 -8 343.822 48.5358 66
10 4 -7 1525.53 95.1829 28
10 4 -7 1571.71 95.0651 26
-10 -4 7 1564.30 93.8410 22
10 4 -7 1557.13 79.5620 74
10 4 -7 1672.34 102.034 66
10 4 -6-4.60845 35.2378 28
-10 -4 6 4.03400 28.8851 96
10 4 -6 17.6924 37.2852 26
-10 -4 6 24.5020 39.4968 22
10 4 -6 2.69937 23.6035 74
10 4 -5 187.706 50.4453 28
-10 -4 5 230.394 42.9613 96
10 4 -5 205.356 48.4296 25
-10 -4 5 303.560 50.4782 22
10 4 -5 184.942 49.1775 66
10 4 -4 1116.76 91.6619 28
-10 -4 4 888.716 74.4229 96
10 4 -4 1065.23 86.9055 25
-10 -4 4 936.898 68.4295 44
-10 -4 4 1081.20 82.2562 22
10 4 -4 1104.74 90.1991 66
-10 -4 4 1215.20 87.6772 59
-10 -4 3 53.9345 35.6817 96
10 4 -3 10.0324 38.3718 25
-10 -4 3 44.9414 38.3769 22
10 4 -3 10.4403 38.3654 66
-10 -4 3 88.9792 49.1541 59
10 4 -2 50.5471 43.3153 28
10 4 -2 77.8903 40.5587 25
-10 -4 2 35.3787 39.6138 22
10 4 -2 50.1455 42.8450 66
-10 -4 2 116.491 46.7994 59
10 4 -1 658.479 72.3495 28
10 4 -1 585.666 62.3795 25
-10 -4 1 597.941 58.7457 41
-10 -4 1 541.861 60.7361 22
10 4 -1 602.916 64.5206 66
-10 -4 1 699.564 72.8667 58
10 4 0 452.846 62.4599 28
10 4 0 416.266 53.5064 25
-10 -4 0 606.303 61.9461 41
-10 -4 0 376.340 51.3740 22
10 4 0 333.394 48.4224 66
-10 -4 0 536.858 71.7598 59
-10 -4 0 504.229 68.3902 58
10 4 1 49.8575 39.3345 28
10 4 1 42.1097 77.3662 88
-10 -4 -1 104.690 39.9146 41
-10 -4 -1 45.8533 48.0551 59
-10 -4 -1 90.3761 53.0740 58
10 4 2 1053.99 80.9972 28
-10 -4 -2 951.719 87.2125 45
10 4 2 970.088 158.429 88
-10 -4 -2 1184.31 89.3273 41
-10 -4 -2 1130.30 93.1922 59
-10 -4 -2 1145.62 98.6153 58
10 4 3 3164.03 148.292 28
-10 -4 -3 3300.08 170.230 45
10 4 3 2993.55 281.097 88
-10 -4 -3 3451.78 168.672 41
-10 -4 -3 3591.73 172.540 59
-10 -4 -3 3575.72 178.011 58
-10 -4 -4 284.226 58.8100 45
-10 -4 -4 273.269 50.9999 59
-10 -4 -5 472.654 57.6542 59
-10 -4 -5 518.634 69.7429 58
-10 -4 -6 23.1664 39.7915 45
-10 -4 -6-8.63453 33.5153 44
-10 -4 -6 4.48663 36.3561 41
-10 -4 -6-4.50684 35.5053 70
-10 -4 -6-29.9785 31.1863 69
-10 -4 -6 9.82475 40.6156 34
-10 -4 -6-4.98036 43.2907 58
-10 -4 -7 86.5253 39.7322 45
-10 -4 -7 118.394 34.2811 44
-10 -4 -7 60.3513 36.8780 41
-10 -4 -7 51.2324 33.7361 70
-10 -4 -7 89.0603 40.4945 34
-10 -4 -8 2071.26 104.801 41
-10 -4 -8 1923.24 102.481 34
-10 -4 -9 262.487 36.7470 42
-10 -4 -9 255.180 36.3881 41
-10 -4 -10 1466.87 65.7897 41
10 5 -9 1882.90 75.4071 51
10 5 -8 1811.99 81.7430 28
10 5 -8 1700.76 80.3639 26
10 5 -7 1664.66 89.8712 28
10 5 -7 1583.08 87.7876 26
-10 -5 7 1755.94 90.5982 22
10 5 -7 1500.20 71.8964 74
10 5 -7 1866.67 97.4696 66
10 5 -6 226.348 42.5826 28
10 5 -6 138.952 36.7291 26
-10 -5 6 158.542 38.4603 22
10 5 -5 17.4660 35.6245 28
-10 -5 5 3.71818 31.3434 22
10 5 -5 4.38994 36.0569 66
10 5 -4 7137.09 277.848 28
10 5 -4 7539.88 276.197 25
-10 -5 4 6304.80 247.419 44
-10 -5 4 7053.67 265.236 22
10 5 -4 7321.48 277.245 66
-10 -5 4 7052.02 268.415 59
10 5 -3 4244.76 189.091 25
-10 -5 3 4279.41 183.732 22
10 5 -3 4465.02 193.035 66
-10 -5 3 4347.48 192.676 59
10 5 -2 17.2376 35.1614 25
-10 -5 2-7.63371 33.7677 22
10 5 -2 34.6616 36.0607 66
-10 -5 2 34.9010 43.8537 59
10 5 -1 3066.49 152.092 28
10 5 -1 2898.02 139.900 25
-10 -5 1 2836.89 134.262 22
10 5 -1 2750.78 136.056 66
10 5 0 144.168 46.1702 28
10 5 0 103.535 36.4879 25
-10 -5 0 72.4664 34.5513 41
10 5 0 137.010 34.3232 66
-10 -5 0 199.309 53.6957 59
-10 -5 0 118.279 45.0142 58
10 5 1 2454.38 130.395 28
-10 -5 -1 2409.29 124.882 41
-10 -5 -1 2357.03 137.417 59
-10 -5 -1 2502.09 135.848 58
10 5 2 117.413 36.1023 28
-10 -5 -2 124.404 42.1825 41
-10 -5 -2 60.3190 43.0012 59
-10 -5 -2 61.7566 49.3778 58
10 5 3 325.094 41.7965 28
-10 -5 -3 481.253 60.0328 45
-10 -5 -3 419.177 56.1163 41
-10 -5 -3 435.518 60.6251 59
-10 -5 -3 466.069 63.1965 58
-10 -5 -4 3484.63 166.289 45
-10 -5 -4 3311.13 162.297 41
-10 -5 -4 3836.22 167.597 59
-10 -5 -5 41.2707 35.4621 44
-10 -5 -5 44.9248 37.1692 41
-10 -5 -5 51.2285 36.4567 70
-10 -5 -5 9.27960 40.3463 58
-10 -5 -6 863.601 67.3326 44
-10 -5 -6 949.017 69.5223 70
-10 -5 -6 1056.70 77.3158 34
-10 -5 -7 1303.38 74.5827 44
-10 -5 -7 1371.38 80.8762 41
-10 -5 -7 1279.15 80.3403 34
-10 -5 -8 1043.38 64.3839 41
-10 -5 -8 935.273 59.0427 34
-10 -5 -9 1346.11 64.1885 42
-10 -5 -9 1403.39 66.8802 41
-10 -6 8 1180.63 57.0346 19
10 6 -7 444.887 39.8735 28
10 6 -7 454.226 38.8482 26
-10 -6 7 442.609 40.5587 22
10 6 -6-5.88666 26.9211 28
10 6 -6 2.73155 24.9843 26
-10 -6 6 42.7514 27.9912 22
10 6 -6 3.13998 29.6315 66
10 6 -5 272.146 43.2492 28
-10 -6 5 232.178 38.7442 22
10 6 -5 301.541 42.8473 66
10 6 -4 27.2508 32.0102 28
10 6 -4 71.5821 34.8154 25
-10 -6 4 40.0683 31.9236 22
10 6 -4 69.1637 35.0703 66
10 6 -3 803.214 71.0165 28
10 6 -3 943.059 69.6329 25
-10 -6 3 810.682 61.8291 22
10 6 -3 723.166 62.9680 66
-10 -6 3 834.571 68.0005 59
10 6 -2 740.776 62.4942 25
-10 -6 2 715.117 56.1737 22
10 6 -2 525.155 53.7856 66
-10 -6 2 753.654 68.6130 59
10 6 -1 493.782 58.8803 28
10 6 -1 405.961 45.7186 25
10 6 -1 433.318 43.7846 66
10 6 0 97.6917 38.5247 28
10 6 0 103.639 29.7291 25
-10 -6 0 135.183 49.3740 59
-10 -6 0 69.2664 38.0426 58
10 6 1 1301.65 82.7636 28
-10 -6 -1 1155.68 74.3250 41
-10 -6 -1 1369.39 93.8133 59
-10 -6 -1 1375.27 90.2908 58
10 6 2 3951.02 168.402 28
-10 -6 -2 4047.76 171.587 41
-10 -6 -2 4287.54 185.214 59
10 6 3 403.443 38.9871 28
-10 -6 -3 518.671 54.4640 41
-10 -6 -3 461.201 55.2595 59
-10 -6 -4 44.1187 33.1767 41
-10 -6 -4 62.6079 32.8612 59
-10 -6 -5 637.148 56.0614 44
-10 -6 -5 742.389 58.8971 41
-10 -6 -5 852.203 62.1385 70
-10 -6 -5 735.033 53.9343 69
-10 -6 -5 645.597 60.2499 34
-10 -6 -5 820.877 67.6614 58
-10 -6 -6 79.2567 27.6137 44
-10 -6 -6 125.203 32.1881 41
-10 -6 -6 114.393 29.3547 70
-10 -6 -6 88.7613 33.1082 34
-10 -6 -7 716.248 50.6278 34
-10 -6 -8 1308.23 62.5644 42
-10 -6 -8 1361.70 63.7594 41
10 7 -6 7792.85 247.508 28
10 7 -6 6883.60 240.292 26
-10 -7 6 8015.91 246.303 22
-10 -7 6 6690.11 238.803 19
10 7 -5 158.286 29.9025 28
10 7 -5 154.627 27.2882 26
-10 -7 5 145.384 28.3300 22
10 7 -5 218.891 32.5343 66
10 7 -4 4859.71 187.231 28
-10 -7 4 4804.71 175.947 22
10 7 -4 4808.02 181.646 66
10 7 -3 207.081 38.2139 28
-10 -7 3 136.365 24.2069 44
-10 -7 3 126.527 28.1754 22
10 7 -3 131.617 28.3117 66
-10 -7 3 132.913 33.1189 59
10 7 -2 2033.03 93.4897 66
-10 -7 2 2227.86 108.036 59
10 7 -1 1367.58 82.4674 28
-10 -7 1 1329.69 84.5779 59
10 7 0 25.0837 27.4262 28
10 7 1 529.530 46.9893 28
-10 -7 -1 544.226 55.2549 59
10 7 2 2874.77 121.492 28
-10 -7 -2 2908.17 120.616 41
-10 -7 -2 3261.38 139.807 59
-10 -7 -3 27.7049 24.0273 41
-10 -7 -3 44.7249 30.6198 59
-10 -7 -3 85.5266 32.6643 58
-10 -7 -4 7152.27 260.122 44
-10 -7 -4 7429.64 254.163 41
-10 -7 -4 7319.33 260.196 70
-10 -7 -4 7366.98 252.088 69
-10 -7 -5 153.070 28.1910 44
-10 -7 -5 145.010 27.8234 41
-10 -7 -5 113.488 24.4973 70
-10 -7 -5 114.376 29.5863 34
-10 -7 -6 5321.82 183.878 44
-10 -7 -6 5109.70 187.634 41
10 8 -4 502.661 36.3586 28
10 8 -4 432.832 31.5829 26
10 8 -3 2412.47 101.285 28
10 8 -2 680.985 47.2379 28
10 8 -1 286.508 33.3007 28
-10 -8 1 234.755 28.9134 44
-10 -8 1 298.805 35.4763 59
10 8 0 2362.65 99.3575 28
-10 -8 0 2354.94 100.678 44
10 8 1 1108.18 55.6485 28
-10 -8 -1 1228.74 66.8978 59
-10 -8 -2 167.975 28.4948 59
-10 -8 -3 977.739 55.0840 44
-10 -8 -3 1117.88 55.9632 70
-10 -8 -3 1005.58 57.3048 34
-10 -8 -4 160.125 22.6981 44
-10 -8 -4 177.766 26.5113 34
11 -14 -3 94.8283 23.9304 24
-11 14 3 100.637 22.3961 38
11 -14 -2 198.454 28.1306 24
-11 14 2 168.200 28.2157 38
11 -14 -1 1439.55 69.7230 24
11 -14 0 50.8127 16.5330 24
-11 14 0 57.7382 26.2714 38
-11 14 -1 12.6516 21.7482 71
-11 14 -1 53.0258 26.2477 38
-11 14 -2 1402.22 70.0666 71
-11 14 -2 1259.30 67.6915 38
-11 14 -2 1210.21 60.5901 33
-11 14 -3 261.756 29.3286 71
-11 14 -3 202.364 25.9897 38
-11 14 -3 203.554 24.8589 33
-11 14 -4 165.532 23.4880 72
-11 14 -4 98.7744 18.2137 71
-11 14 -4 136.071 20.2930 33
11 -13 -6 419.636 36.0388 24
11 -13 -5 35.0166 17.4747 54
11 -13 -5 41.8359 26.7319 24
-11 13 5 24.0054 18.5588 38
11 -13 -4 450.412 32.5510 54
-11 13 4 562.345 46.7413 38
11 -13 -3 119.126 35.6389 24
-11 13 3 106.215 33.6088 38
11 -13 -2 186.387 40.0500 24
-11 13 2 58.7451 28.5892 68
11 -13 -1 406.595 47.7023 24
-11 13 1 431.469 45.3200 68
-11 13 1 392.646 51.5496 38
11 -13 -1 426.739 37.3965 18
11 -13 0 141.688 31.6005 24
-11 13 0 152.579 36.6576 68
-11 13 0 175.119 39.7743 38
-11 13 0 118.801 26.0662 35
11 -13 1 695.098 49.3369 24
-11 13 -1 692.447 61.6110 38
-11 13 -1 722.622 60.0756 68
-11 13 -1 721.102 52.4101 35
-11 13 -2 142.431 27.0412 32
-11 13 -2 161.289 34.1684 38
-11 13 -2 146.283 30.2902 35
-11 13 -3 1009.86 59.9949 32
-11 13 -3 1150.84 70.5980 71
-11 13 -3 1101.29 67.3946 38
-11 13 -3 983.307 63.8958 35
-11 13 -4 70.7612 25.1274 32
-11 13 -4 48.3294 24.5331 71
-11 13 -4 41.0613 21.7474 38
-11 13 -5 118.348 24.7063 32
-11 13 -5 185.590 30.0655 72
-11 13 -5 171.005 24.8988 71
-11 13 -5 172.212 31.8550 33
-11 13 -6 26.3620 16.2983 32
-11 13 -6 63.8865 17.1886 72
11 -12 -8 356.939 28.7948 54
11 -12 -7 125.612 30.6984 55
11 -12 -7 149.542 27.2829 54
11 -12 -7 147.377 28.9205 24
11 -12 -6 27.7603 25.2259 54
11 -12 -6 6.56613 28.7148 24
-11 12 6 28.4554 21.1817 38
11 -12 -5 1638.49 89.0579 55
11 -12 -5 1429.28 81.5177 54
11 -12 -5 1758.92 98.8695 24
11 -12 -4 115.065 34.9366 55
11 -12 -4 56.1577 27.8914 54
11 -12 -4 48.3436 36.6425 24
-11 12 4 80.2521 26.5367 68
11 -12 -3 248.751 35.8622 54
-11 12 3 331.010 43.4652 68
11 -12 -2 258.437 41.1076 55
11 -12 -2 366.138 56.2130 24
-11 12 2 243.915 42.6781 68
11 -12 -1 51.3494 40.4138 24
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-14 2 0 47.0746 32.0844 69
-14 2 -1 373.764 36.3667 42
-14 2 -1 419.093 45.9365 41
14 -2 1 309.574 34.2100 39
-14 2 -1 438.539 47.3443 70
-14 2 -1 423.402 49.3570 69
-14 2 -2 241.041 36.6211 42
-14 2 -2 280.715 41.7797 41
-14 2 -2 347.992 44.0106 70
-14 2 -3 48.6495 27.1728 42
-14 2 -3 70.5752 33.3453 41
-14 2 -3 98.5961 33.6260 70
-14 2 -3 74.2815 31.4256 69
-14 2 -3-12.6382 29.5541 36
-14 2 -4 36.6897 26.8168 42
-14 2 -4 57.7518 27.8805 37
-14 2 -4 67.4556 28.9999 36
-14 2 -5 641.801 47.2229 30
-14 2 -5 612.113 46.7192 42
-14 2 -5 512.258 45.5808 41
-14 2 -5 500.833 40.3659 37
-14 2 -5 617.946 45.7627 36
-14 2 -6 1056.50 58.6981 41
-14 2 -6 1206.36 54.9833 36
14 -1 -6 108.606 17.5944 39
-14 1 6 122.545 18.2244 20
14 -1 -5 42.3781 17.2370 27
14 -1 -5 53.9432 19.3343 26
14 -1 -5 58.0037 23.1488 39
-14 1 5 91.4680 20.4763 20
14 -1 -4 243.282 30.6279 27
14 -1 -4 254.442 29.2676 26
14 -1 -4 258.712 33.9282 39
-14 1 4 231.724 28.4404 20
14 -1 -3 15.2615 19.4882 26
-14 1 3 3.64667 18.6266 20
14 -1 -2 177.761 25.7417 26
14 -1 -2 175.136 32.5937 39
-14 1 2 183.481 30.6537 69
14 -1 -1 164.706 29.4929 39
-14 1 1 165.186 27.5828 70
-14 1 1 140.400 32.4184 69
14 -1 0 766.436 52.1318 39
-14 1 0 740.495 54.4867 70
-14 1 0 782.749 59.3803 69
-14 1 -1 503.644 44.8618 41
14 -1 1 467.879 38.0660 39
-14 1 -1 577.109 50.2523 70
-14 1 -1 628.609 53.9868 69
-14 1 -2 356.311 35.9018 42
-14 1 -2 345.671 41.3252 41
-14 1 -2 458.903 46.9977 70
-14 1 -2 448.839 46.4009 69
-14 1 -3 459.217 40.3853 42
-14 1 -3 476.076 45.1956 41
-14 1 -3 529.626 47.4885 70
-14 1 -3 479.617 46.1936 69
-14 1 -3 499.136 46.5987 36
-14 1 -4 1669.59 80.3351 42
-14 1 -4 1795.48 84.7011 41
-14 1 -4 1621.50 78.6135 37
-14 1 -4 1667.97 82.9123 36
-14 1 -5 98.1424 24.8753 30
-14 1 -5 97.1571 24.5623 42
-14 1 -5 103.126 22.3095 36
-14 1 -6 371.943 29.5313 42
-14 1 -6 374.244 29.5504 41
14 0 -5 642.134 38.9637 39
14 0 -4 1.73960 16.5093 27
14 0 -4 31.6940 15.8858 26
14 0 -4 30.2726 18.7632 39
14 0 -3-1.57643 16.3779 26
14 0 -2 509.276 34.6185 26
14 0 -2 646.921 47.2936 39
-14 0 2 646.496 42.7410 69
14 0 -1 1420.92 72.3725 39
-14 0 1 1377.28 64.7494 70
-14 0 1 1347.20 72.9507 69
14 0 0 1823.12 84.1971 39
-14 0 0 2025.88 88.8322 70
-14 0 0 1894.47 92.5151 69
14 0 1 226.798 23.1669 39
-14 0 -1 332.268 36.9599 70
-14 0 -2 72.9119 18.2925 42
-14 0 -2 124.293 24.9379 41
-14 0 -2 125.235 29.1588 70
-14 0 -2 133.103 31.4598 69
-14 0 -3 28.3485 16.5887 42
-14 0 -3-16.3032 22.0378 41
-14 0 -3 4.71550 23.5598 69
-14 0 -3 9.16033 22.3624 36
-14 0 -4 442.186 33.3752 42
-14 0 -4 461.266 37.3101 41
-14 0 -4 572.037 41.5371 70
-14 0 -4 463.362 32.5362 37
-14 0 -4 453.509 35.8966 36
-14 0 -5 272.627 26.0545 30
14 1 -4 390.630 27.8731 39
14 1 -2 62.3337 18.9769 39
14 1 -1 720.107 43.8367 39
-14 -1 1 774.005 46.3254 69
14 1 0 13.4104 13.5879 39
-14 -1 0 19.7595 18.0162 70
-14 -1 0 16.6507 21.8081 69
-14 -1 -1 708.034 45.7515 70
-14 -1 -2 312.685 31.4516 70
-14 -1 -2 315.082 31.6514 69
-14 -1 -3 874.935 47.6286 69
-14 -1 -3 796.011 45.8190 36
-15 8 2 1637.39 69.5280 20
-15 8 2 1693.62 70.8165 68
-15 8 1 35.0707 16.1094 68
-15 8 1 33.7966 16.9326 20
-15 8 1 41.6420 16.7255 35
-15 8 0 769.753 42.8837 68
-15 8 0 732.579 43.6845 35
-15 8 -1 43.5977 14.6353 68
-15 8 -1 74.1840 19.1552 35
-15 8 -2 73.4088 17.4196 35
15 -7 -3 853.676 44.2626 39
-15 7 3 897.237 46.4558 20
15 -7 -2 207.949 24.8149 27
15 -7 -2 152.467 20.4634 39
-15 7 2 160.018 23.8343 20
15 -7 -1 62.3796 19.7790 27
-15 7 1 46.1661 19.2837 20
15 -7 0 362.819 29.7360 27
-15 7 0 438.862 31.0887 20
-15 7 0 418.828 33.1309 68
-15 7 0 340.771 27.9834 37
-15 7 -1 119.498 19.9949 68
-15 7 -1 112.601 20.8185 37
-15 7 -1 153.082 25.1160 35
-15 7 -2 38.5502 17.4549 37
-15 7 -2 41.9105 18.5556 35
-15 7 -3 1483.39 63.0331 35
15 -6 -4 733.304 40.0537 27
-15 6 4 765.627 40.0201 20
15 -6 -3 1094.06 56.3900 27
15 -6 -3 992.892 52.7343 39
-15 6 3 1164.97 54.9604 20
15 -6 -2 850.362 46.8742 39
-15 6 2 817.043 47.7529 20
15 -6 -1 1279.91 62.6154 27
15 -6 -1 1114.08 52.8160 39
-15 6 1 1197.14 58.1603 20
15 -6 0-1.83817 17.4333 27
-15 6 0-7.14773 17.2830 37
-15 6 0 2.93296 16.6318 20
15 -6 1 35.9838 14.3328 27
-15 6 -1 46.4055 17.3331 68
-15 6 -1 62.3997 21.3779 37
-15 6 -1 62.2964 18.4470 36
-15 6 -2 2011.81 84.9525 37
-15 6 -2 1897.82 80.3863 36
-15 6 -2 2117.95 84.9627 35
-15 6 -3 1791.42 77.6619 31
-15 6 -3 1906.34 81.8819 37
-15 6 -3 2028.28 77.7717 35
-15 6 -4 79.4273 16.4468 37
15 -5 -4 1802.39 73.1014 27
-15 5 4 1724.89 70.9408 20
15 -5 -3 167.571 25.6144 27
15 -5 -3 193.401 24.9100 39
-15 5 3 233.186 25.0373 20
15 -5 -2 28.0060 19.3889 39
-15 5 2 43.0562 19.1602 20
15 -5 -1 171.018 26.4216 27
15 -5 -1 124.685 20.2876 39
-15 5 1 145.255 22.3241 37
-15 5 1 176.576 23.4755 20
15 -5 0 33.3700 20.0803 27
-15 5 0 27.5942 20.1626 37
-15 5 0 44.7436 17.2426 36
15 -5 1 81.8850 18.2647 27
-15 5 -1 87.6101 24.4275 37
-15 5 -1 71.0135 20.8959 36
-15 5 -2-3.67542 18.6906 36
-15 5 -3 339.798 31.5860 37
-15 5 -3 315.512 29.7853 36
-15 5 -4 479.148 33.1719 31
-15 5 -4 541.108 32.8096 37
15 -4 -4 299.218 24.5111 27
15 -4 -3 743.671 43.8631 27
15 -4 -3 638.742 40.2197 39
-15 4 3 679.219 37.8704 20
15 -4 -2 329.574 29.8062 39
-15 4 2 317.758 26.5899 20
15 -4 -1 141.128 25.4266 27
15 -4 -1 151.212 20.6917 39
-15 4 1 138.994 23.4165 37
15 -4 0 68.2134 21.4988 27
-15 4 0 62.1036 21.5974 37
-15 4 0 77.1559 19.6938 36
15 -4 1 2502.09 97.9287 27
-15 4 -1 2545.81 104.842 37
-15 4 -1 2470.49 100.981 36
-15 4 -2 29.8337 21.8498 37
-15 4 -2 24.0948 18.9489 36
-15 4 -3 477.030 35.2943 37
-15 4 -4 2028.99 79.9060 36
15 -3 -3 33.1854 16.2499 27
15 -3 -3 40.8690 14.9514 39
15 -3 -2 324.120 31.2583 27
15 -3 -2 380.346 28.7549 39
15 -3 -1 42.1416 19.9457 27
-15 3 1 46.6678 18.6173 37
15 -3 0 61.3807 19.1192 27
-15 3 0 56.8226 20.9205 37
-15 3 0 31.1156 16.8193 36
15 -3 1-8.81204 14.4089 27
-15 3 -1 1.73865 17.6063 36
-15 3 -2 537.035 38.6596 37
-15 3 -2 529.451 37.6852 36
-15 3 -3 355.891 27.8648 37
15 -2 -2 18.3127 14.6989 27
-15 2 1 47.3905 16.1778 37
15 -2 0 582.325 36.1398 27
-15 2 0 514.550 36.0942 37
-15 2 -1 290.969 26.3669 36
-15 2 -2 114.596 19.0592 37
0 0 0 0.00 0.00 0
TITL PN180815_UO_Traz_1_180814_SCN in P-1
REM P-1 (#2 in standard setting)
CELL 1.54184 12.148210 13.184753 13.825099 90.2630 90.2180 108.0045
ZERR 4.00 0.000219 0.000210 0.000166 0.0012 0.0012 0.0015
LATT 1
SFAC C H N O S Cl
UNIT 80.00 92.00 24.00 4.00 4.00 4.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 92417
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.360
_oxdiff_exptl_absorpt_empirical_full_min 0.813
data_pn180817_uo_trh_1_180814_b1_bf4
_audit_creation_date 2018-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number '2014/7'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C19 H23 Cl N5 O, B F4'
_chemical_formula_sum 'C19 H23 B Cl F4 N5 O'
_chemical_formula_weight 459.68
_chemical_melting_point ?
_chemical_oxdiff_formula 'C19 H23 B Cl F4 N5 O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system 'monoclinic'
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 12.46473(13)
_cell_length_b 12.98315(16)
_cell_length_c 13.42014(13)
_cell_angle_alpha 90
_cell_angle_beta 106.7648(11)
_cell_angle_gamma 90
_cell_volume 2079.49(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 36021
_cell_measurement_temperature 159.99(10)
_cell_measurement_theta_max 78.6160
_cell_measurement_theta_min 3.6800
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.148
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.531
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.468
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 952
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 5 -7 0.0914
-1 6 6 0.0727
2 -3 -8 0.0929
-2 -6 6 0.0733
-3 -1 9 0.0808
-8 0 0 0.0143
8 0 0 0.0026
-1 -8 0 0.1031
2 7 -5 0.0990
-5 -3 -4 0.0601
6 0 4 0.0306
_exptl_crystal_size_max 0.185
_exptl_crystal_size_mid 0.171
_exptl_crystal_size_min 0.017
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.0001 5.0000 -7.0000 -0.8807 -0.0211 -0.4920
-1.0000 6.0000 6.0000 0.5856 -0.0378 -0.8015
2.0000 -3.0000 -8.0000 -0.8621 0.0357 0.4754
-2.0001 -6.0000 6.0000 0.7746 -0.0793 0.6137
-3.0001 -1.0000 9.0000 1.0427 -0.0060 -0.0134
-8.0000 -0.0000 -0.0000 0.0824 1.0240 0.1132
8.0000 0.0000 0.0000 -0.0824 -1.0240 -0.1132
-1.0000 -8.0000 0.0000 0.1294 0.0150 0.9482
2.0001 7.0000 -5.0000 -0.6787 0.0516 -0.7497
-5.0000 -3.0000 -4.0000 -0.3469 0.7646 0.4977
5.9999 -0.0000 4.0000 0.3813 -0.9350 -0.1616
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0288
_diffrn_reflns_av_unetI/netI 0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 48534
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 78.777
_diffrn_reflns_theta_min 3.704
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 159.99(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
--------------------------------------------------------------------------
1 \w 52.00 83.00 0.50 2.40 -- 107.75 -54.00 95.67 62
2 \w 50.00 86.00 0.50 2.40 -- 107.75 -20.00 155.62 72
3 \w 79.00 106.00 0.50 2.40 -- 107.75 -60.00 168.37 54
4 \w 38.00 66.00 0.50 2.40 -- 107.75 -30.00 150.00 56
5 \w 42.00 77.00 0.50 2.40 -- 107.75 -50.00 108.48 70
6 \w 33.00 85.00 0.50 2.40 -- 107.75 -52.00 58.78 104
7 \w 85.00 111.00 0.50 2.40 -- 107.75 -60.00 20.58 52
8 \w 72.00 98.00 0.50 2.40 -- 107.75 -60.00 -42.33 52
9 \w 58.00 85.00 0.50 2.40 -- 107.75 -60.00 -64.42 54
10 \w 68.00 121.00 0.50 2.40 -- 107.75 -60.00-123.70 106
11 \w 129.00 174.00 0.50 2.40 -- 107.75 15.00 -90.00 90
12 \w 134.00 172.00 0.50 2.40 -- 107.75 15.00 30.00 76
13 \w 146.00 178.00 0.50 2.40 -- 107.75 45.00 30.00 64
14 \w 97.00 122.00 0.50 2.40 -- 107.75 15.00 30.00 50
15 \w 105.00 139.00 0.50 2.40 -- 107.75 45.00 30.00 68
16 \w 64.00 120.00 0.50 2.40 -- 107.75 -60.00 -80.02 112
17 \w 96.00 128.00 0.50 2.40 -- 107.75 15.00-150.00 64
18 \w 53.00 103.00 0.50 2.40 -- 107.75 -60.00-162.37 100
19 \w 47.00 87.00 0.50 2.40 -- 107.75 -53.00-114.66 80
20 \w 44.00 69.00 0.50 2.40 -- 107.75 -45.00 -60.00 50
21 \w 47.00 72.00 0.50 2.40 -- 107.75 -48.00 -19.73 50
22 \w 54.00 79.00 0.50 2.40 -- 107.75 -49.00 11.90 50
23 \w 37.00 63.00 0.50 2.40 -- 107.75 -52.00 -23.37 52
24 \w 37.00 71.00 0.50 2.40 -- 107.75 -53.00 -28.90 68
25 \w 40.00 65.00 0.50 2.40 -- 107.75 -60.00 20.58 50
26 \w 37.00 63.00 0.50 2.40 -- 107.75 -30.00 60.00 52
27 \w 44.00 78.00 0.50 2.40 -- 107.75 -46.00 55.58 68
28 \w 34.00 68.00 0.50 2.40 -- 107.75 -30.00 90.00 68
29 \w 43.00 92.00 0.50 2.40 -- 107.75 -4.00 59.26 98
30 \w 35.00 61.00 0.50 0.60 -- 50.46 57.00 -30.00 52
31 \w 36.00 64.00 0.50 0.60 -- 50.46 57.00 0.00 56
32 \w 37.00 63.00 0.50 2.40 -- 107.75 -60.00 168.37 52
33 \w -79.00 -43.00 0.50 0.60 -- -50.46 -19.00 -60.00 72
34 \w -23.00 19.00 0.50 0.60 -- -50.46 57.00 60.00 84
35 \w -58.00 -27.00 0.50 0.60 -- -50.46 57.00 60.00 62
36 \w -65.00 -39.00 0.50 2.40 -- -86.25 60.00 21.93 52
37 \w -116.00 -35.00 0.50 0.60 -- -50.46 -57.00-120.00 162
38 \w -125.00 -81.00 0.50 0.60 -- -50.46 -19.00 -60.00 88
39 \w -62.00 -24.00 0.50 0.60 -- -50.46 38.00 -60.00 76
40 \w -45.00 -9.00 0.50 0.60 -- -50.46 38.00-180.00 72
41 \w -5.00 21.00 0.50 0.60 -- -50.46 38.00-180.00 52
42 \w 37.00 64.00 0.50 0.60 -- 50.46 60.00 47.85 54
43 \w 36.00 71.00 0.50 0.60 -- 50.46 57.00 0.00 70
44 \w 38.00 64.00 0.50 0.60 -- 50.46 57.00 30.00 52
45 \w 36.00 63.00 0.50 0.60 -- 50.46 57.00-120.00 54
46 \w 40.00 83.00 0.50 0.60 -- 50.46 19.00 -30.00 86
47 \w 23.00 62.00 0.50 0.60 -- 50.46 -57.00-120.00 78
48 \w 44.00 73.00 0.50 0.60 -- 50.46 38.00 -90.00 58
49 \w 37.00 64.00 0.50 0.60 -- 50.46 60.00 -83.29 54
50 \w -96.00 -71.00 0.50 2.40 -- -86.25 -59.00 -65.41 50
51 \w -101.00 -75.00 0.50 2.40 -- -86.25 -58.00 4.64 52
52 \w -98.00 -72.00 0.50 2.40 -- -86.25 -60.00 17.66 52
53 \w -98.00 -71.00 0.50 2.40 -- -86.25 -59.00 -13.45 54
54 \w -96.00 -70.00 0.50 2.40 -- -86.25 -60.00-105.68 52
55 \w -101.00 -75.00 0.50 2.40 -- -86.25 -57.00-118.61 52
56 \w -97.00 -71.00 0.50 2.40 -- -86.25 -59.00-122.77 52
57 \w -97.00 -71.00 0.50 2.40 -- -86.25 -60.00 -97.25 52
58 \w -97.00 -71.00 0.50 2.40 -- -86.25 -60.00 -75.32 52
59 \w -96.00 -71.00 0.50 2.40 -- -86.25 -59.00 -32.53 50
60 \w -98.00 -72.00 0.50 2.40 -- -86.25 -56.00 -53.38 52
61 \w -95.00 -70.00 0.50 2.40 -- -86.25 -60.00 -82.23 50
62 \w -107.00 -70.00 0.50 2.40 -- -86.25 -60.00-137.53 74
63 \w -97.00 -71.00 0.50 2.40 -- -86.25 -58.00 7.93 52
64 \w -96.00 -71.00 0.50 2.40 -- -86.25 -57.00 -94.82 50
65 \w -98.00 -72.00 0.50 2.40 -- -86.25 -53.00 -74.48 52
66 \w -96.00 -70.00 0.50 2.40 -- -86.25 -60.00 -27.53 52
67 \w -97.00 -71.00 0.50 2.40 -- -86.25 -59.00 -20.69 52
68 \w -98.00 -71.00 0.50 2.40 -- -86.25 -58.00-114.40 54
69 \w -99.00 -72.00 0.50 2.40 -- -86.25 -59.00 -56.20 54
70 \w -96.00 -70.00 0.50 2.40 -- -86.25 -60.00 -9.62 52
71 \w -98.00 -72.00 0.50 2.40 -- -86.25 -56.00 -6.79 52
72 \w -97.00 -71.00 0.50 2.40 -- -86.25 -60.00 -38.53 52
73 \w 95.00 120.00 0.50 2.40 -- 107.75 45.00 30.00 50
74 \w 94.00 120.00 0.50 2.40 -- 107.75 45.00 0.00 52
75 \w 120.00 146.00 0.50 2.40 -- 107.75 4.00-123.74 52
76 \w 63.00 101.00 0.50 2.40 -- 107.75 4.00-123.74 76
77 \w 95.00 121.00 0.50 2.40 -- 107.75 47.00 70.26 52
78 \w 110.00 157.00 0.50 2.40 -- 107.75 30.00 90.00 94
79 \w 96.00 131.00 0.50 2.40 -- 107.75 45.00 60.00 70
80 \w 145.00 177.00 0.50 2.40 -- 107.75 60.00 144.46 64
81 \w 50.00 76.00 0.50 2.40 -- 107.75 -45.00-150.00 52
82 \w 111.00 137.00 0.50 2.40 -- 107.75 30.00 -60.00 52
83 \w 102.00 153.00 0.50 2.40 -- 107.75 45.00 90.00 102
84 \w 105.00 131.00 0.50 2.40 -- 107.75 30.00 30.00 52
85 \w 101.00 126.00 0.50 2.40 -- 107.75 60.00 144.46 50
86 \w 104.00 131.00 0.50 2.40 -- 107.75 30.00 -30.00 54
87 \w 153.00 178.00 0.50 2.40 -- 107.75 45.00 120.00 50
88 \w 97.00 128.00 0.50 2.40 -- 107.75 45.00 -90.00 62
89 \w 95.00 121.00 0.50 2.40 -- 107.75 15.00 60.00 52
90 \w 115.00 141.00 0.50 2.40 -- 107.75 30.00 0.00 52
91 \w 146.00 172.00 0.50 2.40 -- 107.75 49.00-132.85 52
92 \w 100.00 125.00 0.50 2.40 -- 107.75 45.00 120.00 50
93 \w 94.00 138.00 0.50 2.40 -- 107.75 45.00 -30.00 88
94 \w 98.00 124.00 0.50 2.40 -- 107.75 49.00-132.85 52
95 \w 138.00 164.00 0.50 2.40 -- 107.75 45.00-180.00 52
96 \w 98.00 136.00 0.50 2.40 -- 107.75 45.00-180.00 76
97 \w 32.00 69.00 0.50 2.40 -- 107.75 -30.00 0.00 74
98 \w 94.00 147.00 0.50 2.40 -- 107.75 45.00 -60.00 106
99 \w 99.00 127.00 0.50 2.40 -- 107.75 40.00 0.78 56
100 \w 86.00 112.00 0.50 2.40 -- 107.75 -60.00 -54.81 52
101 \w 40.00 66.00 0.50 2.40 -- 107.75 -60.00 -54.81 52
102 \w 92.00 117.00 0.50 2.40 -- 107.75 -15.00 90.00 50
103 \w 143.00 173.00 0.50 2.40 -- 107.75 47.00 70.26 60
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0103051000
_diffrn_orient_matrix_UB_12 -0.0148874000
_diffrn_orient_matrix_UB_13 0.1107700000
_diffrn_orient_matrix_UB_21 -0.1279942000
_diffrn_orient_matrix_UB_22 0.0141188000
_diffrn_orient_matrix_UB_23 -0.0417587000
_diffrn_orient_matrix_UB_31 -0.0141502000
_diffrn_orient_matrix_UB_32 -0.1167544000
_diffrn_orient_matrix_UB_33 -0.0191807000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4165
_reflns_number_total 4315
_reflns_odcompleteness_completeness 95.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 79.66
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.328
_refine_diff_density_min -0.311
_refine_diff_density_rms 0.051
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.164
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 293
_refine_ls_number_reflns 4315
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0423
_refine_ls_R_factor_gt 0.0415
_refine_ls_restrained_S_all 1.164
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+2.2045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1039
_refine_ls_wR_factor_ref 0.1042
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
2. Others
Sof(F1)=Sof(F2)=Sof(F3)=1-FVAR(1)
Sof(F29)=Sof(F27)=Sof(F30)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
N16(H16)
3.b Secondary CH2 refined with riding coordinates:
C12(H12A,H12B), C14(H14A,H14B), C18(H18A,H18B), C17(H17A,H17B), C15(H15A,
H15B), C10(H10A,H10B), C11(H11A,H11B)
3.c Aromatic/amide H refined with riding coordinates:
C20(H20), C4(H4), C24(H24), C23(H23), C22(H22), C7(H7), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl25 Cl 0.85574(4) 1.05286(4) 0.81194(4) 0.03444(14) Uani 1 1 d . . . . .
F31 F 0.56726(12) 0.46652(11) 0.61432(13) 0.0505(4) Uani 1 1 d . . . . .
O26 O 0.09252(12) 0.63897(13) 0.16171(11) 0.0375(4) Uani 1 1 d . . . . .
N3 N -0.06166(12) 0.74773(12) 0.14934(11) 0.0225(3) Uani 1 1 d . . . . .
N9 N -0.06722(13) 0.74091(13) 0.31384(12) 0.0250(3) Uani 1 1 d . . . . .
N13 N 0.57458(12) 0.87012(12) 0.50597(11) 0.0234(3) Uani 1 1 d . . . . .
N16 N 0.38170(12) 0.73589(12) 0.43954(11) 0.0212(3) Uani 1 1 d . . . . .
H16 H 0.4180 0.6712 0.4736 0.025 Uiso 1 1 calc R . . . .
F29 F 0.4050(2) 0.44050(16) 0.6531(3) 0.0541(6) Uani 0.910(8) 1 d . . P A 1
N1 N 0.01837(12) 0.68007(13) 0.29821(12) 0.0248(3) Uani 1 1 d . . . . .
F27 F 0.4500(3) 0.6010(2) 0.6109(2) 0.0604(8) Uani 0.910(8) 1 d . . P A 1
F30 F 0.54252(18) 0.5304(2) 0.76267(15) 0.0631(8) Uani 0.910(8) 1 d . . P A 1
C8 C -0.11390(15) 0.78077(15) 0.22159(13) 0.0231(4) Uani 1 1 d . . . . .
C20 C 0.71654(15) 0.95133(14) 0.65045(14) 0.0235(4) Uani 1 1 d . . . . .
H20 H 0.6755 0.9344 0.6978 0.028 Uiso 1 1 calc R . . . .
C2 C 0.02605(15) 0.68205(15) 0.19910(14) 0.0253(4) Uani 1 1 d . . . . .
C19 C 0.67851(14) 0.91925(14) 0.54624(14) 0.0222(4) Uani 1 1 d . . . . .
C12 C 0.26288(15) 0.71104(15) 0.37971(14) 0.0257(4) Uani 1 1 d . . . . .
H12A H 0.2634 0.6571 0.3277 0.031 Uiso 1 1 calc R . . . .
H12B H 0.2277 0.7733 0.3414 0.031 Uiso 1 1 calc R . . . .
C14 C 0.56598(15) 0.79118(15) 0.42613(14) 0.0248(4) Uani 1 1 d . . . . .
H14A H 0.6000 0.7263 0.4594 0.030 Uiso 1 1 calc R . . . .
H14B H 0.6077 0.8137 0.3774 0.030 Uiso 1 1 calc R . . . .
C18 C 0.51288(15) 0.83978(16) 0.57890(14) 0.0268(4) Uani 1 1 d . . . . .
H18A H 0.5159 0.8963 0.6291 0.032 Uiso 1 1 calc R . . . .
H18B H 0.5488 0.7784 0.6185 0.032 Uiso 1 1 calc R . . . .
C4 C -0.09293(16) 0.77886(16) 0.04663(14) 0.0277(4) Uani 1 1 d . . . . .
H4 H -0.0552 0.7536 -0.0006 0.033 Uiso 1 1 calc R . . . .
C17 C 0.39154(15) 0.81541(15) 0.52239(14) 0.0247(4) Uani 1 1 d . . . . .
H17A H 0.3537 0.7902 0.5732 0.030 Uiso 1 1 calc R . . . .
H17B H 0.3531 0.8792 0.4905 0.030 Uiso 1 1 calc R . . . .
C24 C 0.74436(16) 0.94448(15) 0.48051(15) 0.0272(4) Uani 1 1 d . . . . .
H24 H 0.7207 0.9233 0.4098 0.033 Uiso 1 1 calc R . . . .
C15 C 0.44479(15) 0.77242(15) 0.36659(14) 0.0249(4) Uani 1 1 d . . . . .
H15A H 0.4109 0.8369 0.3323 0.030 Uiso 1 1 calc R . . . .
H15B H 0.4402 0.7200 0.3120 0.030 Uiso 1 1 calc R . . . .
C23 C 0.84282(16) 0.99947(16) 0.51686(16) 0.0296(4) Uani 1 1 d . . . . .
H23 H 0.8860 1.0147 0.4708 0.035 Uiso 1 1 calc R . . . .
C22 C 0.88003(16) 1.03293(15) 0.61944(16) 0.0288(4) Uani 1 1 d . . . . .
H22 H 0.9474 1.0712 0.6444 0.035 Uiso 1 1 calc R . . . .
C7 C -0.20488(16) 0.85090(16) 0.18771(15) 0.0286(4) Uani 1 1 d . . . . .
H7 H -0.2436 0.8752 0.2345 0.034 Uiso 1 1 calc R . . . .
C5 C -0.17808(17) 0.84582(17) 0.01533(15) 0.0313(4) Uani 1 1 d . . . . .
H5 H -0.2006 0.8692 -0.0547 0.038 Uiso 1 1 calc R . . . .
C21 C 0.81480(15) 1.00811(15) 0.68340(14) 0.0252(4) Uani 1 1 d . . . . .
B28 B 0.49146(18) 0.51001(17) 0.65970(16) 0.0249(4) Uani 1 1 d . . . . .
C6 C -0.23499(16) 0.88219(16) 0.08699(16) 0.0311(4) Uani 1 1 d . . . . .
H6 H -0.2953 0.9294 0.0635 0.037 Uiso 1 1 calc R . . . .
C10 C 0.08810(16) 0.61766(16) 0.38200(15) 0.0297(4) Uani 1 1 d . . . . .
H10A H 0.1121 0.5552 0.3518 0.036 Uiso 1 1 calc R . . . .
H10B H 0.0428 0.5951 0.4277 0.036 Uiso 1 1 calc R . . . .
C11 C 0.19198(16) 0.67406(16) 0.44786(15) 0.0281(4) Uani 1 1 d . . . . .
H11A H 0.1689 0.7338 0.4828 0.034 Uiso 1 1 calc R . . . .
H11B H 0.2368 0.6272 0.5023 0.034 Uiso 1 1 calc R . . . .
F1 F 0.5521(17) 0.579(2) 0.733(2) 0.058(7) Uiso 0.090(8) 1 d . . P A 2
F2 F 0.4382(16) 0.4421(14) 0.6877(13) 0.022(4) Uiso 0.090(8) 1 d . . P A 2
F3 F 0.4257(19) 0.568(2) 0.579(2) 0.051(6) Uiso 0.090(8) 1 d . . P A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl25 0.0346(3) 0.0345(3) 0.0281(2) -0.00437(19) -0.00078(18) -0.00614(19)
F31 0.0529(8) 0.0334(8) 0.0773(10) 0.0002(7) 0.0379(8) 0.0060(6)
O26 0.0270(7) 0.0496(10) 0.0363(8) -0.0129(7) 0.0094(6) 0.0050(6)
N3 0.0193(7) 0.0281(9) 0.0195(7) -0.0039(6) 0.0045(5) -0.0040(6)
N9 0.0225(7) 0.0295(9) 0.0230(7) -0.0019(6) 0.0063(6) -0.0004(6)
N13 0.0233(7) 0.0243(8) 0.0229(7) -0.0040(6) 0.0072(6) -0.0023(6)
N16 0.0201(7) 0.0181(8) 0.0221(7) 0.0010(6) 0.0012(6) 0.0014(6)
F29 0.0432(12) 0.0540(11) 0.0698(16) -0.0255(10) 0.0237(12) -0.0224(9)
N1 0.0212(7) 0.0275(9) 0.0235(7) -0.0007(6) 0.0031(6) 0.0008(6)
F27 0.0923(16) 0.0408(14) 0.0503(13) 0.0217(10) 0.0242(12) 0.0342(12)
F30 0.0824(14) 0.0664(17) 0.0260(9) -0.0087(9) -0.0072(8) -0.0103(11)
C8 0.0231(8) 0.0254(10) 0.0210(8) -0.0054(7) 0.0070(7) -0.0051(7)
C20 0.0235(8) 0.0218(10) 0.0245(9) 0.0019(7) 0.0056(7) 0.0005(7)
C2 0.0204(8) 0.0283(10) 0.0257(9) -0.0064(7) 0.0043(7) -0.0031(7)
C19 0.0217(8) 0.0178(9) 0.0258(9) 0.0016(7) 0.0048(7) 0.0031(7)
C12 0.0208(8) 0.0274(10) 0.0239(9) 0.0012(7) -0.0017(7) 0.0011(7)
C14 0.0241(9) 0.0243(10) 0.0253(9) -0.0045(7) 0.0057(7) 0.0007(7)
C18 0.0255(9) 0.0312(11) 0.0232(9) -0.0041(7) 0.0064(7) -0.0059(7)
C4 0.0269(9) 0.0364(11) 0.0193(8) -0.0038(7) 0.0058(7) -0.0104(8)
C17 0.0242(9) 0.0233(10) 0.0263(9) -0.0035(7) 0.0070(7) -0.0005(7)
C24 0.0284(9) 0.0263(10) 0.0269(9) -0.0005(7) 0.0081(7) -0.0002(7)
C15 0.0266(9) 0.0260(10) 0.0208(8) -0.0003(7) 0.0045(7) -0.0003(7)
C23 0.0285(9) 0.0275(11) 0.0354(10) 0.0033(8) 0.0136(8) 0.0016(8)
C22 0.0227(9) 0.0239(10) 0.0377(10) 0.0020(8) 0.0053(8) -0.0014(7)
C7 0.0273(9) 0.0285(11) 0.0297(9) -0.0052(8) 0.0077(7) 0.0006(8)
C5 0.0321(10) 0.0342(12) 0.0229(9) 0.0040(8) 0.0003(7) -0.0108(8)
C21 0.0252(9) 0.0194(10) 0.0271(9) 0.0009(7) 0.0013(7) 0.0022(7)
B28 0.0296(10) 0.0216(11) 0.0208(9) 0.0010(8) 0.0033(8) 0.0013(8)
C6 0.0271(9) 0.0250(11) 0.0355(10) -0.0011(8) 0.0000(8) -0.0020(8)
C10 0.0255(9) 0.0275(11) 0.0316(10) 0.0044(8) 0.0011(7) -0.0010(8)
C11 0.0253(9) 0.0290(11) 0.0263(9) 0.0038(7) 0.0015(7) -0.0013(7)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl25 C21 1.7510(19) . ?
F31 B28 1.384(3) . ?
O26 C2 1.221(2) . ?
N3 C8 1.383(2) . ?
N3 C2 1.395(2) . ?
N3 C4 1.380(2) . ?
N9 N1 1.391(2) . ?
N9 C8 1.313(2) . ?
N13 C19 1.405(2) . ?
N13 C14 1.464(2) . ?
N13 C18 1.462(2) . ?
N16 H16 1.0000 . ?
N16 C12 1.502(2) . ?
N16 C17 1.496(2) . ?
N16 C15 1.499(2) . ?
F29 B28 1.389(3) . ?
N1 C2 1.361(2) . ?
N1 C10 1.453(2) . ?
F27 B28 1.377(3) . ?
F30 B28 1.370(3) . ?
C8 C7 1.423(3) . ?
C20 H20 0.9500 . ?
C20 C19 1.404(3) . ?
C20 C21 1.388(3) . ?
C19 C24 1.406(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.521(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.511(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C17 1.517(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.342(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C24 H24 0.9500 . ?
C24 C23 1.382(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C23 H23 0.9500 . ?
C23 C22 1.389(3) . ?
C22 H22 0.9500 . ?
C22 C21 1.380(3) . ?
C7 H7 0.9500 . ?
C7 C6 1.356(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.430(3) . ?
B28 F1 1.38(2) . ?
B28 F2 1.226(19) . ?
B28 F3 1.38(2) . ?
C6 H6 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.528(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 N3 C2 108.44(15) . . ?
C4 N3 C8 123.70(16) . . ?
C4 N3 C2 127.84(16) . . ?
C8 N9 N1 103.43(14) . . ?
C19 N13 C14 117.66(14) . . ?
C19 N13 C18 118.00(14) . . ?
C18 N13 C14 111.07(15) . . ?
C12 N16 H16 108.1 . . ?
C17 N16 H16 108.1 . . ?
C17 N16 C12 113.72(14) . . ?
C17 N16 C15 108.73(14) . . ?
C15 N16 H16 108.1 . . ?
C15 N16 C12 109.94(13) . . ?
N9 N1 C10 120.88(15) . . ?
C2 N1 N9 114.19(15) . . ?
C2 N1 C10 124.87(16) . . ?
N3 C8 C7 117.87(16) . . ?
N9 C8 N3 111.63(16) . . ?
N9 C8 C7 130.48(17) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C21 C20 C19 119.22(17) . . ?
O26 C2 N3 127.89(18) . . ?
O26 C2 N1 129.81(19) . . ?
N1 C2 N3 102.30(15) . . ?
N13 C19 C24 120.33(16) . . ?
C20 C19 N13 121.79(16) . . ?
C20 C19 C24 117.73(17) . . ?
N16 C12 H12A 108.8 . . ?
N16 C12 H12B 108.8 . . ?
N16 C12 C11 113.62(14) . . ?
H12A C12 H12B 107.7 . . ?
C11 C12 H12A 108.8 . . ?
C11 C12 H12B 108.8 . . ?
N13 C14 H14A 109.5 . . ?
N13 C14 H14B 109.5 . . ?
N13 C14 C15 110.54(15) . . ?
H14A C14 H14B 108.1 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
N13 C18 H18A 109.4 . . ?
N13 C18 H18B 109.4 . . ?
N13 C18 C17 111.26(15) . . ?
H18A C18 H18B 108.0 . . ?
C17 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
N3 C4 H4 120.9 . . ?
C5 C4 N3 118.17(18) . . ?
C5 C4 H4 120.9 . . ?
N16 C17 C18 111.81(15) . . ?
N16 C17 H17A 109.3 . . ?
N16 C17 H17B 109.3 . . ?
C18 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
H17A C17 H17B 107.9 . . ?
C19 C24 H24 119.4 . . ?
C23 C24 C19 121.26(18) . . ?
C23 C24 H24 119.4 . . ?
N16 C15 C14 109.78(14) . . ?
N16 C15 H15A 109.7 . . ?
N16 C15 H15B 109.7 . . ?
C14 C15 H15A 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C24 C23 H23 119.3 . . ?
C24 C23 C22 121.33(18) . . ?
C22 C23 H23 119.3 . . ?
C23 C22 H22 121.5 . . ?
C21 C22 C23 117.07(18) . . ?
C21 C22 H22 121.5 . . ?
C8 C7 H7 120.8 . . ?
C6 C7 C8 118.43(18) . . ?
C6 C7 H7 120.8 . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.29(18) . . ?
C6 C5 H5 119.9 . . ?
C20 C21 Cl25 118.01(15) . . ?
C22 C21 Cl25 118.60(15) . . ?
C22 C21 C20 123.37(18) . . ?
F31 B28 F29 108.84(18) . . ?
F27 B28 F31 110.54(18) . . ?
F27 B28 F29 110.5(2) . . ?
F30 B28 F31 110.19(19) . . ?
F30 B28 F29 108.4(2) . . ?
F30 B28 F27 108.4(2) . . ?
F1 B28 F31 105.9(9) . . ?
F2 B28 F31 109.9(8) . . ?
F2 B28 F1 118.8(12) . . ?
F2 B28 F3 112.4(12) . . ?
F3 B28 F31 101.6(11) . . ?
F3 B28 F1 106.7(13) . . ?
C7 C6 C5 121.53(19) . . ?
C7 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
N1 C10 H10A 108.9 . . ?
N1 C10 H10B 108.9 . . ?
N1 C10 C11 113.47(16) . . ?
H10A C10 H10B 107.7 . . ?
C11 C10 H10A 108.9 . . ?
C11 C10 H10B 108.9 . . ?
C12 C11 C10 110.24(16) . . ?
C12 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
C10 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C8 C7 C6 -0.5(3) . . . . ?
N3 C4 C5 C6 -0.8(3) . . . . ?
N9 N1 C2 O26 178.61(19) . . . . ?
N9 N1 C2 N3 -0.7(2) . . . . ?
N9 N1 C10 C11 -89.6(2) . . . . ?
N9 C8 C7 C6 178.4(2) . . . . ?
N13 C19 C24 C23 175.19(18) . . . . ?
N13 C14 C15 N16 -60.5(2) . . . . ?
N13 C18 C17 N16 54.7(2) . . . . ?
N16 C12 C11 C10 -161.26(16) . . . . ?
N1 N9 C8 N3 0.0(2) . . . . ?
N1 N9 C8 C7 -178.86(19) . . . . ?
N1 C10 C11 C12 -57.9(2) . . . . ?
C8 N3 C2 O26 -178.66(19) . . . . ?
C8 N3 C2 N1 0.67(19) . . . . ?
C8 N3 C4 C5 0.7(3) . . . . ?
C8 N9 N1 C2 0.4(2) . . . . ?
C8 N9 N1 C10 -177.00(16) . . . . ?
C8 C7 C6 C5 0.4(3) . . . . ?
C20 C19 C24 C23 -0.4(3) . . . . ?
C2 N3 C8 N9 -0.5(2) . . . . ?
C2 N3 C8 C7 178.58(16) . . . . ?
C2 N3 C4 C5 -177.66(18) . . . . ?
C2 N1 C10 C11 93.2(2) . . . . ?
C19 N13 C14 C15 -160.97(16) . . . . ?
C19 N13 C18 C17 164.44(16) . . . . ?
C19 C20 C21 Cl25 176.58(14) . . . . ?
C19 C20 C21 C22 -1.8(3) . . . . ?
C19 C24 C23 C22 -0.7(3) . . . . ?
C12 N16 C17 C18 -178.65(15) . . . . ?
C12 N16 C15 C14 -176.59(15) . . . . ?
C14 N13 C19 C20 -146.04(17) . . . . ?
C14 N13 C19 C24 38.6(2) . . . . ?
C14 N13 C18 C17 -55.4(2) . . . . ?
C18 N13 C19 C20 -8.4(3) . . . . ?
C18 N13 C19 C24 176.19(17) . . . . ?
C18 N13 C14 C15 58.7(2) . . . . ?
C4 N3 C8 N9 -179.13(16) . . . . ?
C4 N3 C8 C7 -0.1(3) . . . . ?
C4 N3 C2 O26 -0.1(3) . . . . ?
C4 N3 C2 N1 179.26(17) . . . . ?
C4 C5 C6 C7 0.3(3) . . . . ?
C17 N16 C12 C11 -57.3(2) . . . . ?
C17 N16 C15 C14 58.32(19) . . . . ?
C24 C23 C22 C21 0.5(3) . . . . ?
C15 N16 C12 C11 -179.50(16) . . . . ?
C15 N16 C17 C18 -55.81(19) . . . . ?
C23 C22 C21 Cl25 -177.63(15) . . . . ?
C23 C22 C21 C20 0.8(3) . . . . ?
C21 C20 C19 N13 -173.91(17) . . . . ?
C21 C20 C19 C24 1.6(3) . . . . ?
C10 N1 C2 O26 -4.1(3) . . . . ?
C10 N1 C2 N3 176.63(16) . . . . ?
_shelx_res_file
;
pn180817_uo_trh_1_180814_b1_bf4.res created by SHELXL-2014/7
TITL pn180817_uo_trh_1_180814_b1_bf4_a.res in P2(1)/c
REM Old TITL PN180817_UO_TrH_1_180814_B1_BF4 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.157, Rweak 0.014, Alpha 0.046, Orientation as input
REM Formula found by SHELXT: C24 N5 O Cl
CELL 1.54184 12.464727 12.983151 13.420138 90 106.7648 90
ZERR 4 0.000127 0.000165 0.000132 0 0.0011 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H B Cl F N O
UNIT 76 92 4 4 16 20 4
L.S. 4
PLAN 5
TEMP -113
BOND $H
LIST 4
CONF
fmap 2
acta
OMIT -6 1 2
OMIT -5 6 2
OMIT 4 5 2
OMIT -7 1 2
OMIT -10 7 2
REM
REM
REM
WGHT 0.024700 2.204500
FVAR 4.46312 0.90988
CL25 4 0.855739 1.052860 0.811943 11.00000 0.03460 0.03446 =
0.02809 -0.00437 -0.00078 -0.00614
F31 5 0.567261 0.466521 0.614322 11.00000 0.05292 0.03336 =
0.07731 0.00020 0.03789 0.00602
O26 7 0.092523 0.638969 0.161714 11.00000 0.02701 0.04956 =
0.03625 -0.01289 0.00941 0.00504
N3 6 -0.061661 0.747728 0.149342 11.00000 0.01929 0.02813 =
0.01951 -0.00387 0.00454 -0.00400
N9 6 -0.067225 0.740912 0.313836 11.00000 0.02247 0.02950 =
0.02299 -0.00189 0.00631 -0.00039
N13 6 0.574582 0.870119 0.505971 11.00000 0.02328 0.02426 =
0.02292 -0.00397 0.00722 -0.00228
N16 6 0.381705 0.735888 0.439543 11.00000 0.02015 0.01813 =
0.02212 0.00103 0.00122 0.00143
AFIX 13
H16 2 0.418036 0.671199 0.473605 11.00000 -1.20000
AFIX 0
PART 1
F29 5 0.404978 0.440504 0.653149 21.00000 0.04319 0.05403 =
0.06978 -0.02555 0.02369 -0.02236
PART 0
N1 6 0.018374 0.680072 0.298209 11.00000 0.02121 0.02749 =
0.02346 -0.00067 0.00305 0.00079
PART 1
F27 5 0.450035 0.601032 0.610911 21.00000 0.09229 0.04078 =
0.05035 0.02175 0.02420 0.03424
F30 5 0.542522 0.530351 0.762672 21.00000 0.08240 0.06645 =
0.02595 -0.00871 -0.00720 -0.01029
PART 0
C8 1 -0.113902 0.780768 0.221589 11.00000 0.02309 0.02545 =
0.02103 -0.00541 0.00701 -0.00514
C20 1 0.716535 0.951332 0.650450 11.00000 0.02352 0.02177 =
0.02449 0.00193 0.00561 0.00053
AFIX 43
H20 2 0.675493 0.934380 0.697849 11.00000 -1.20000
AFIX 0
C2 1 0.026046 0.682046 0.199104 11.00000 0.02042 0.02828 =
0.02571 -0.00641 0.00432 -0.00312
C19 1 0.678508 0.919245 0.546240 11.00000 0.02171 0.01785 =
0.02585 0.00160 0.00480 0.00313
C12 1 0.262876 0.711039 0.379712 11.00000 0.02079 0.02737 =
0.02390 0.00123 -0.00166 0.00108
AFIX 23
H12A 2 0.263380 0.657060 0.327744 11.00000 -1.20000
H12B 2 0.227701 0.773305 0.341395 11.00000 -1.20000
AFIX 0
C14 1 0.565980 0.791176 0.426130 11.00000 0.02406 0.02428 =
0.02528 -0.00450 0.00570 0.00071
AFIX 23
H14A 2 0.600037 0.726277 0.459389 11.00000 -1.20000
H14B 2 0.607750 0.813734 0.377439 11.00000 -1.20000
AFIX 0
C18 1 0.512881 0.839782 0.578901 11.00000 0.02550 0.03123 =
0.02318 -0.00412 0.00636 -0.00590
AFIX 23
H18A 2 0.515915 0.896325 0.629134 11.00000 -1.20000
H18B 2 0.548808 0.778414 0.618465 11.00000 -1.20000
AFIX 0
C4 1 -0.092928 0.778859 0.046629 11.00000 0.02690 0.03641 =
0.01934 -0.00376 0.00582 -0.01041
AFIX 43
H4 2 -0.055216 0.753584 -0.000612 11.00000 -1.20000
AFIX 0
C17 1 0.391539 0.815414 0.522389 11.00000 0.02422 0.02331 =
0.02634 -0.00347 0.00695 -0.00051
AFIX 23
H17A 2 0.353652 0.790169 0.573151 11.00000 -1.20000
H17B 2 0.353146 0.879195 0.490453 11.00000 -1.20000
AFIX 0
C24 1 0.744356 0.944483 0.480512 11.00000 0.02844 0.02629 =
0.02687 -0.00046 0.00809 -0.00016
AFIX 43
H24 2 0.720689 0.923320 0.409759 11.00000 -1.20000
AFIX 0
C15 1 0.444788 0.772418 0.366587 11.00000 0.02657 0.02595 =
0.02076 -0.00035 0.00450 -0.00034
AFIX 23
H15A 2 0.410862 0.836938 0.332289 11.00000 -1.20000
H15B 2 0.440249 0.719971 0.311974 11.00000 -1.20000
AFIX 0
C23 1 0.842824 0.999474 0.516861 11.00000 0.02850 0.02752 =
0.03542 0.00335 0.01357 0.00164
AFIX 43
H23 2 0.885967 1.014720 0.470788 11.00000 -1.20000
AFIX 0
C22 1 0.880029 1.032931 0.619437 11.00000 0.02268 0.02389 =
0.03769 0.00197 0.00530 -0.00141
AFIX 43
H22 2 0.947413 1.071212 0.644443 11.00000 -1.20000
AFIX 0
C7 1 -0.204876 0.850898 0.187708 11.00000 0.02733 0.02853 =
0.02970 -0.00525 0.00770 0.00057
AFIX 43
H7 2 -0.243616 0.875237 0.234510 11.00000 -1.20000
AFIX 0
C5 1 -0.178079 0.845822 0.015334 11.00000 0.03205 0.03419 =
0.02285 0.00397 0.00030 -0.01084
AFIX 43
H5 2 -0.200633 0.869158 -0.054733 11.00000 -1.20000
AFIX 0
C21 1 0.814797 1.008110 0.683397 11.00000 0.02525 0.01937 =
0.02706 0.00091 0.00128 0.00219
B28 3 0.491462 0.510013 0.659702 11.00000 0.02962 0.02163 =
0.02084 0.00096 0.00334 0.00131
C6 1 -0.234988 0.882186 0.086993 11.00000 0.02712 0.02495 =
0.03547 -0.00109 0.00001 -0.00198
AFIX 43
H6 2 -0.295285 0.929351 0.063526 11.00000 -1.20000
AFIX 0
C10 1 0.088096 0.617660 0.382003 11.00000 0.02551 0.02747 =
0.03157 0.00438 0.00110 -0.00103
AFIX 23
H10A 2 0.112077 0.555238 0.351818 11.00000 -1.20000
H10B 2 0.042790 0.595075 0.427668 11.00000 -1.20000
AFIX 0
C11 1 0.191981 0.674062 0.447860 11.00000 0.02534 0.02896 =
0.02627 0.00375 0.00154 -0.00126
AFIX 23
H11A 2 0.168925 0.733750 0.482756 11.00000 -1.20000
H11B 2 0.236774 0.627184 0.502267 11.00000 -1.20000
AFIX 0
PART 2
F1 5 0.552109 0.578977 0.732878 -21.00000 0.05810
F2 5 0.438241 0.442113 0.687705 -21.00000 0.02245
F3 5 0.425670 0.567666 0.578687 -21.00000 0.05115
HKLF 4
REM pn180817_uo_trh_1_180814_b1_bf4_a.res in P2(1)/c
REM R1 = 0.0415 for 4165 Fo > 4sig(Fo) and 0.0423 for all 4315 data
REM 293 parameters refined using 0 restraints
END
WGHT 0.0247 2.2046
REM Highest difference peak 0.328, deepest hole -0.311, 1-sigma level 0.051
Q1 1 0.1472 0.5525 0.1537 11.00000 0.05 0.33
Q2 1 0.5954 0.4620 0.6852 11.00000 0.05 0.30
Q3 1 0.5002 0.5854 0.5802 11.00000 0.05 0.30
Q4 1 0.1534 0.5552 0.2337 11.00000 0.05 0.30
Q5 1 0.8604 1.0492 0.4255 11.00000 0.05 0.26
;
_shelx_res_checksum 85548
_shelx_hkl_file
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-15 4 6 173.112 24.2165 88
15 4 -6 199.368 28.0504 83
15 4 -6 224.974 30.9952 77
15 -4 -5 733.715 46.7625 13
-15 4 5 632.860 42.5860 11
-15 4 5 668.837 37.7868 91
-15 4 5 655.595 41.3576 88
15 4 -5 629.158 43.0559 83
15 4 -5 676.302 44.4686 78
-15 4 4 2308.14 88.4044 11
-15 -4 4 1917.11 80.7329 91
-15 4 4 2189.27 84.3748 88
15 4 -4 2080.19 86.3880 83
15 4 -4 2148.26 86.3584 78
-15 4 3 9536.62 301.693 11
-15 -4 3 9615.24 298.697 91
-15 4 3 9695.14 299.779 88
15 4 -3 9676.32 302.658 83
15 4 -3 9148.91 299.082 78
-15 4 2 1253.75 58.2825 11
-15 -4 2 1370.84 60.3787 6
15 5 -6 51.9070 18.2721 83
-15 -5 6 133.025 20.8086 6
-15 5 5 69.8053 20.0211 88
15 5 -5 70.4267 21.6483 83
-15 -5 5 106.684 22.0928 6
-15 -5 4 1589.52 67.1245 6
-15 5 4 1626.37 64.4361 88
15 5 -4 1488.60 64.6416 83
-15 -5 3 367.257 29.3676 6
0 0 0 0.00 0.00 0
TITL PN180817_UO_TrH_1_180814_B1_BF4 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 12.464727 12.983151 13.420138 90.0000 106.7648 90.0000
ZERR 4.00 0.000127 0.000165 0.000132 0.0000 0.0011 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H B N O F Cl
UNIT 76.00 92.00 4.00 20.00 4.00 16.00 4.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 74908
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.227
_oxdiff_exptl_absorpt_empirical_full_min 0.783
data_pn180830_uo_eph_1_180814_b12_benzsulf
_audit_creation_date 2018-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number '2014/7'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C6 H5 O3 S, C10 H16 N O'
_chemical_formula_sum 'C16 H21 N O4 S'
_chemical_formula_weight 323.40
_chemical_absolute_configuration rmad
_chemical_melting_point ?
_chemical_oxdiff_formula 'C16 H21 N O4 S'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system 'monoclinic'
_space_group_IT_number 4
_space_group_name_H-M_alt 'P 1 21 1'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 5.72587(4)
_cell_length_b 20.83882(10)
_cell_length_c 6.92054(4)
_cell_angle_alpha 90
_cell_angle_beta 98.3547(5)
_cell_angle_gamma 90
_cell_volume 816.998(8)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 12545
_cell_measurement_temperature 159.99(10)
_cell_measurement_theta_max 78.6210
_cell_measurement_theta_min 6.3580
_shelx_estimated_absorpt_T_max 0.737
_shelx_estimated_absorpt_T_min 0.347
_exptl_absorpt_coefficient_mu 1.912
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.488
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.315
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 344
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 9 3 0.1017
0 -9 -3 0.1017
-3 -4 0 0.3034
3 4 0 0.3166
0 -12 2 0.0935
0 12 -2 0.0935
-2 11 -1 0.2094
-2 -9 3 0.2248
3 -6 -1 0.3076
1 -12 2 0.1173
0 -3 4 0.1000
0 3 -4 0.1139
4 -2 1 0.2799
-3 3 -2 0.2470
2 -4 3 0.1845
0 -5 -4 0.0972
3 3 2 0.2358
-3 -3 -1 0.2799
0 -9 3 0.0936
1 -10 3 0.1176
0 14 0 0.0685
0 -14 0 0.1018
_exptl_crystal_size_max 0.702
_exptl_crystal_size_mid 0.224
_exptl_crystal_size_min 0.17
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0004 9.0075 2.9950 0.1048 0.9208 0.1957
0.0004 -9.0075 -2.9950 -0.1048 -0.9208 -0.1957
-3.0004 -4.0030 0.0031 -0.0449 -0.4524 0.7392
3.0004 4.0030 -0.0031 0.0449 0.4524 -0.7392
0.0011 -11.9862 2.0048 0.8945 -0.4283 0.0746
-0.0011 11.9862 -2.0048 -0.8945 0.4283 -0.0746
-2.0014 10.9873 -1.0038 -0.8284 0.3564 0.4793
-1.9995 -8.9870 3.0040 0.7773 -0.2686 0.6410
3.0011 -5.9961 -0.9983 0.3306 -0.2598 -0.8262
1.0013 -11.9845 2.0044 0.9705 -0.3547 -0.1759
0.0006 -2.9827 4.0001 0.8270 0.3593 0.2144
-0.0006 2.9827 -4.0001 -0.8270 -0.3593 -0.2144
4.0012 -1.9885 0.9989 0.5682 0.3119 -0.9524
-3.0011 2.9856 -1.9995 -0.7103 -0.3136 0.6491
2.0011 -3.9828 3.0001 0.8525 0.3154 -0.3457
0.0000 -5.0134 -3.9965 -0.4605 -0.8225 -0.2392
3.0007 3.0114 1.9968 0.4355 0.6610 -0.6305
-3.0006 -3.0074 -0.9971 -0.2631 -0.5278 0.6864
0.0010 -8.9837 3.0032 0.9294 -0.1214 0.1399
1.0013 -9.9815 3.0032 1.0513 -0.1056 -0.1138
-0.0011 13.9931 -0.0063 -0.6414 0.8106 0.0434
0.0011 -13.9931 0.0063 0.6414 -0.8106 -0.0434
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0141
_diffrn_reflns_av_unetI/netI 0.0081
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 13481
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 78.844
_diffrn_reflns_theta_min 6.465
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 159.99(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
--------------------------------------------------------------------------
1 \w 35.00 123.00 0.50 1.00 -- 50.46 57.00 60.00 176
2 \w 94.00 173.00 0.50 1.00 -- 107.75 30.00 150.00 158
3 \w 137.00 176.00 0.50 1.00 -- 107.75 30.00 60.00 78
4 \w 144.00 178.00 0.50 1.00 -- 107.75 15.00 30.00 68
5 \w 143.00 169.00 0.50 1.00 -- 107.75 45.00 -30.00 52
6 \w 126.00 156.00 0.50 1.00 -- 107.75 30.00 -60.00 60
7 \w 104.00 130.00 0.50 1.00 -- 107.75 45.00-150.00 52
8 \w 146.00 177.00 0.50 1.00 -- 107.75 45.00-150.00 62
9 \w 87.00 113.00 0.50 1.00 -- 107.75 -15.00 -30.00 52
10 \w 81.00 108.00 0.50 1.00 -- 107.75 -60.00 -6.14 54
11 \w 98.00 124.00 0.50 1.00 -- 107.75 -60.00 47.66 52
12 \w 83.00 114.00 0.50 1.00 -- 107.75 -60.00 17.62 62
13 \w 74.00 101.00 0.50 1.00 -- 107.75 -60.00 12.20 54
14 \w 66.00 103.00 0.50 1.00 -- 107.75 -60.00 -38.95 74
15 \w 60.00 97.00 0.50 1.00 -- 107.75 -58.00 -67.09 74
16 \w 70.00 103.00 0.50 1.00 -- 107.75 -60.00-125.43 66
17 \w 53.00 97.00 0.50 1.00 -- 107.75 -59.00-163.36 88
18 \w 42.00 68.00 0.50 1.00 -- 107.75 -45.00 -60.00 52
19 \w 37.00 63.00 0.50 1.00 -- 107.75 -46.00-103.25 52
20 \w 35.00 61.00 0.50 1.00 -- 107.75 -45.00 -90.00 52
21 \w 31.00 57.00 0.50 1.00 -- 107.75 -30.00 -30.00 52
22 \w 49.00 75.00 0.50 1.00 -- 107.75 -59.00 28.74 52
23 \w 46.00 79.00 0.50 1.00 -- 107.75 -60.00 47.66 66
24 \w 40.00 101.00 0.50 1.00 -- 107.75 -59.00 90.67 122
25 \w 74.00 100.00 0.50 1.00 -- 107.75 -59.00 151.13 52
26 \w 50.00 76.00 0.50 1.00 -- 107.75 -47.00 163.55 52
27 \w 34.00 61.00 0.50 1.00 -- 107.75 -30.00 150.00 54
28 \w 37.00 82.00 0.50 1.00 -- 107.75 -54.00 138.66 90
29 \w 41.00 67.00 0.50 1.00 -- 107.75 -55.00 152.04 52
30 \w 37.00 90.00 0.50 1.00 -- 107.75 -57.00 117.87 106
31 \w 41.00 66.00 0.50 1.00 -- 107.75 -30.00 90.00 50
32 \w 31.00 65.00 0.50 1.00 -- 107.75 -30.00 60.00 68
33 \w 38.00 64.00 0.50 1.00 -- 107.75 -60.00 -6.14 52
34 \w 32.00 58.00 0.50 1.00 -- 107.75 -45.00 60.00 52
35 \w 95.00 120.00 0.50 1.00 -- 107.75 30.00 60.00 50
36 \w 126.00 152.00 0.50 1.00 -- 107.75 30.00 90.00 52
37 \w 98.00 170.00 0.50 1.00 -- 107.75 45.00 90.00 144
38 \w 36.00 103.00 0.50 1.00 -- 50.46 59.00 74.74 134
39 \w 35.00 123.00 0.50 1.00 -- 50.46 57.00 40.29 176
40 \w 35.00 123.00 0.50 1.00 -- 50.46 57.00 -90.00 176
41 \w 35.00 123.00 0.50 1.00 -- 50.46 57.00 0.00 176
42 \w 35.00 61.00 0.50 1.00 -- 107.75 -56.00-106.50 52
43 \w 39.00 76.00 0.50 1.00 -- 107.75 -45.00-150.00 74
44 \w 36.00 89.00 0.50 1.00 -- 107.75 -59.00 -95.48 106
45 \w -22.00 66.00 0.50 1.00 -- 50.46 -57.00 -60.00 176
46 \w -22.00 66.00 0.50 1.00 -- 50.46 -57.00-120.00 176
47 \w -74.00 -49.00 0.50 1.00 -- -86.25 60.00 -38.01 50
48 \w -128.00 -38.00 0.50 1.00 -- -50.46 -38.00 -30.00 180
49 \w 29.00 55.00 0.50 1.00 -- 107.75 -15.00 150.00 52
50 \w -123.00 -35.00 0.50 1.00 -- -50.46 -57.00 120.00 176
51 \w -123.00 -35.00 0.50 1.00 -- -50.46 -57.00 -60.00 176
52 \w -123.00 -35.00 0.50 1.00 -- -50.46 -57.00-150.00 176
53 \w -123.00 -35.00 0.50 1.00 -- -50.46 -57.00-120.00 176
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0761803000
_diffrn_orient_matrix_UB_12 -0.0457499000
_diffrn_orient_matrix_UB_13 0.1726057000
_diffrn_orient_matrix_UB_21 0.0735571000
_diffrn_orient_matrix_UB_22 0.0579945000
_diffrn_orient_matrix_UB_23 0.1330496000
_diffrn_orient_matrix_UB_31 -0.2504642000
_diffrn_orient_matrix_UB_32 0.0031092000
_diffrn_orient_matrix_UB_33 0.0559553000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage 0.936
_reflns_Friedel_fraction_full 0.952
_reflns_Friedel_fraction_max 0.928
_reflns_number_gt 3290
_reflns_number_total 3292
_reflns_odcompleteness_completeness 92.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 79.66
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.176
_refine_diff_density_min -0.320
_refine_diff_density_rms 0.051
_refine_ls_abs_structure_details
;
Flack x determined using 1579 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.006(5)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.068
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 202
_refine_ls_number_reflns 3292
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0230
_refine_ls_R_factor_gt 0.0230
_refine_ls_restrained_S_all 1.068
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.1072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0611
_refine_ls_wR_factor_ref 0.0611
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H,H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
C1(H1C), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
N1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
C16(H16), C10(H10), C9(H9), C12(H12), C6(H6), C8(H8), C15(H15), C13(H13),
C7(H7), C14(H14)
2.d Idealised Me refined as rotating group:
C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
2.e Idealised tetrahedral OH refined as rotating group:
O1(H1)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.98062(7) 0.55478(2) 0.02897(5) 0.02115(11) Uani 1 1 d . . . . .
O13 O 1.2326(2) 0.54075(6) 0.04684(18) 0.0282(3) Uani 1 1 d . . . . .
O1 O 0.7315(2) 0.46320(7) 0.46627(19) 0.0284(3) Uani 1 1 d . . . . .
H1 H 0.7767 0.4785 0.3657 0.043 Uiso 1 1 calc GR . . . .
O12 O 0.8782(2) 0.57115(7) -0.16981(18) 0.0295(3) Uani 1 1 d . . . . .
O11 O 0.8462(3) 0.50525(6) 0.1117(2) 0.0322(3) Uani 1 1 d . . . . .
N1 N 0.4367(3) 0.51588(7) 0.7098(2) 0.0219(3) Uani 1 1 d . . . . .
H1A H 0.3899 0.5159 0.8299 0.026 Uiso 1 1 calc R . . . .
H1B H 0.5950 0.5232 0.7271 0.026 Uiso 1 1 calc R . . . .
C5 C 0.4383(3) 0.38366(8) 0.3261(2) 0.0228(4) Uani 1 1 d . . . . .
C16 C 0.7700(4) 0.63162(9) 0.2733(3) 0.0297(4) Uani 1 1 d . . . . .
H16 H 0.6530 0.5991 0.2675 0.036 Uiso 1 1 calc R . . . .
C11 C 0.9585(3) 0.62489(8) 0.1710(2) 0.0219(3) Uani 1 1 d . . . . .
C10 C 0.6113(4) 0.33659(9) 0.3316(3) 0.0281(4) Uani 1 1 d . . . . .
H10 H 0.7648 0.3445 0.4000 0.034 Uiso 1 1 calc R . . . .
C9 C 0.5615(4) 0.27811(10) 0.2379(3) 0.0333(4) Uani 1 1 d . . . . .
H9 H 0.6807 0.2462 0.2430 0.040 Uiso 1 1 calc R . . . .
C12 C 1.1285(3) 0.67263(9) 0.1762(3) 0.0284(4) Uani 1 1 d . . . . .
H12 H 1.2566 0.6680 0.1042 0.034 Uiso 1 1 calc R . . . .
C6 C 0.2151(4) 0.37151(10) 0.2228(3) 0.0286(4) Uani 1 1 d . . . . .
H6 H 0.0959 0.4035 0.2161 0.034 Uiso 1 1 calc R . . . .
C1 C 0.4880(3) 0.44825(8) 0.4260(2) 0.0222(3) Uani 1 1 d . . . . .
H1C H 0.4074 0.4824 0.3391 0.027 Uiso 1 1 calc R . . . .
C4 C 0.3172(4) 0.56994(9) 0.5946(3) 0.0302(4) Uani 1 1 d . . . . .
H4A H 0.3817 0.5743 0.4716 0.045 Uiso 1 1 calc GR . . . .
H4B H 0.3439 0.6098 0.6698 0.045 Uiso 1 1 calc GR . . . .
H4C H 0.1474 0.5613 0.5666 0.045 Uiso 1 1 calc GR . . . .
C8 C 0.3384(4) 0.26632(10) 0.1370(3) 0.0344(4) Uani 1 1 d . . . . .
H8 H 0.3040 0.2263 0.0731 0.041 Uiso 1 1 calc R . . . .
C2 C 0.3919(3) 0.45042(8) 0.6221(2) 0.0235(4) Uani 1 1 d . . . . .
H2 H 0.2178 0.4425 0.5981 0.028 Uiso 1 1 calc R . . . .
C15 C 0.7531(4) 0.68627(11) 0.3844(3) 0.0377(5) Uani 1 1 d . . . . .
H15 H 0.6247 0.6910 0.4562 0.045 Uiso 1 1 calc R . . . .
C13 C 1.1093(4) 0.72702(10) 0.2872(3) 0.0348(4) Uani 1 1 d . . . . .
H13 H 1.2253 0.7598 0.2918 0.042 Uiso 1 1 calc R . . . .
C7 C 0.1659(4) 0.31316(10) 0.1298(3) 0.0339(4) Uani 1 1 d . . . . .
H7 H 0.0127 0.3052 0.0608 0.041 Uiso 1 1 calc R . . . .
C3 C 0.5071(5) 0.40138(9) 0.7698(3) 0.0352(5) Uani 1 1 d . . . . .
H3A H 0.6789 0.4068 0.7870 0.053 Uiso 1 1 calc GR . . . .
H3B H 0.4662 0.3580 0.7220 0.053 Uiso 1 1 calc GR . . . .
H3C H 0.4503 0.4079 0.8952 0.053 Uiso 1 1 calc GR . . . .
C14 C 0.9221(4) 0.73407(10) 0.3916(3) 0.0368(5) Uani 1 1 d . . . . .
H14 H 0.9097 0.7715 0.4677 0.044 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0202(2) 0.02540(18) 0.01909(18) -0.00015(15) 0.00718(13) -0.00053(15)
O13 0.0232(7) 0.0386(8) 0.0239(6) -0.0025(5) 0.0071(5) 0.0071(5)
O1 0.0279(7) 0.0344(7) 0.0248(6) -0.0041(5) 0.0103(5) -0.0089(5)
O12 0.0267(7) 0.0402(8) 0.0211(6) -0.0005(5) 0.0019(5) -0.0055(5)
O11 0.0403(9) 0.0258(6) 0.0351(7) -0.0003(5) 0.0204(6) -0.0036(6)
N1 0.0201(8) 0.0280(7) 0.0187(6) -0.0015(5) 0.0057(5) -0.0006(5)
C5 0.0266(10) 0.0271(8) 0.0158(7) 0.0010(6) 0.0064(6) -0.0028(7)
C16 0.0255(10) 0.0313(9) 0.0340(9) -0.0032(8) 0.0106(8) -0.0005(7)
C11 0.0198(9) 0.0252(8) 0.0200(7) 0.0024(6) 0.0012(6) 0.0018(6)
C10 0.0264(10) 0.0298(9) 0.0275(8) 0.0002(7) 0.0017(7) -0.0008(7)
C9 0.0363(12) 0.0296(9) 0.0346(10) -0.0027(8) 0.0070(8) 0.0035(8)
C12 0.0243(10) 0.0323(9) 0.0284(9) 0.0023(7) 0.0030(7) -0.0025(7)
C6 0.0247(10) 0.0350(9) 0.0267(8) -0.0047(7) 0.0058(7) 0.0005(7)
C1 0.0230(9) 0.0269(8) 0.0174(7) 0.0006(6) 0.0057(6) -0.0011(6)
C4 0.0335(11) 0.0321(10) 0.0268(9) 0.0027(6) 0.0106(8) 0.0083(7)
C8 0.0405(13) 0.0324(9) 0.0316(9) -0.0089(8) 0.0097(8) -0.0075(8)
C2 0.0229(9) 0.0283(8) 0.0205(8) -0.0015(6) 0.0074(6) -0.0046(6)
C15 0.0331(12) 0.0424(11) 0.0402(11) -0.0106(9) 0.0142(9) 0.0029(9)
C13 0.0337(12) 0.0296(9) 0.0382(10) -0.0018(8) -0.0049(8) -0.0065(8)
C7 0.0284(11) 0.0415(11) 0.0319(10) -0.0096(8) 0.0050(8) -0.0077(8)
C3 0.0574(14) 0.0300(10) 0.0202(9) 0.0032(7) 0.0120(8) -0.0010(9)
C14 0.0389(12) 0.0325(10) 0.0372(10) -0.0108(8) -0.0005(9) 0.0031(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 O13 1.4596(14) . ?
S1 O12 1.4555(13) . ?
S1 O11 1.4536(14) . ?
S1 C11 1.7757(18) . ?
O1 H1 0.8400 . ?
O1 C1 1.416(2) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C4 1.488(2) . ?
N1 C2 1.500(2) . ?
C5 C10 1.391(3) . ?
C5 C6 1.394(3) . ?
C5 C1 1.521(2) . ?
C16 H16 0.9500 . ?
C16 C11 1.381(3) . ?
C16 C15 1.385(3) . ?
C11 C12 1.389(3) . ?
C10 H10 0.9500 . ?
C10 C9 1.390(3) . ?
C9 H9 0.9500 . ?
C9 C8 1.386(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.383(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.385(3) . ?
C1 H1C 1.0000 . ?
C1 C2 1.538(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C8 H8 0.9500 . ?
C8 C7 1.385(3) . ?
C2 H2 1.0000 . ?
C2 C3 1.526(3) . ?
C15 H15 0.9500 . ?
C15 C14 1.385(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(4) . ?
C7 H7 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C14 H14 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 S1 C11 105.49(8) . . ?
O12 S1 O13 112.63(8) . . ?
O12 S1 C11 106.20(8) . . ?
O11 S1 O13 113.43(9) . . ?
O11 S1 O12 112.02(8) . . ?
O11 S1 C11 106.37(8) . . ?
C1 O1 H1 109.5 . . ?
H1A N1 H1B 107.4 . . ?
C4 N1 H1A 108.4 . . ?
C4 N1 H1B 108.4 . . ?
C4 N1 C2 115.71(14) . . ?
C2 N1 H1A 108.4 . . ?
C2 N1 H1B 108.4 . . ?
C10 C5 C6 118.84(17) . . ?
C10 C5 C1 121.76(17) . . ?
C6 C5 C1 119.39(17) . . ?
C11 C16 H16 120.3 . . ?
C11 C16 C15 119.41(19) . . ?
C15 C16 H16 120.3 . . ?
C16 C11 S1 119.42(14) . . ?
C16 C11 C12 120.73(17) . . ?
C12 C11 S1 119.84(15) . . ?
C5 C10 H10 119.7 . . ?
C9 C10 C5 120.57(18) . . ?
C9 C10 H10 119.7 . . ?
C10 C9 H9 119.9 . . ?
C8 C9 C10 120.11(19) . . ?
C8 C9 H9 119.9 . . ?
C11 C12 H12 120.3 . . ?
C13 C12 C11 119.32(19) . . ?
C13 C12 H12 120.3 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.47(19) . . ?
C7 C6 H6 119.8 . . ?
O1 C1 C5 113.45(15) . . ?
O1 C1 H1C 108.5 . . ?
O1 C1 C2 106.74(14) . . ?
C5 C1 H1C 108.5 . . ?
C5 C1 C2 111.10(14) . . ?
C2 C1 H1C 108.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C9 C8 H8 120.2 . . ?
C7 C8 C9 119.58(18) . . ?
C7 C8 H8 120.2 . . ?
N1 C2 C1 108.76(13) . . ?
N1 C2 H2 108.9 . . ?
N1 C2 C3 107.84(14) . . ?
C1 C2 H2 108.9 . . ?
C3 C2 C1 113.34(16) . . ?
C3 C2 H2 108.9 . . ?
C16 C15 H15 119.8 . . ?
C14 C15 C16 120.4(2) . . ?
C14 C15 H15 119.8 . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.45(19) . . ?
C14 C13 H13 119.8 . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.42(19) . . ?
C8 C7 H7 119.8 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C15 C14 C13 119.67(19) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O11 0.84 1.94 2.7730(19) 171.3 .
N1 H1A O13 0.91 1.93 2.8052(19) 160.7 1_456
N1 H1B O12 0.91 1.95 2.792(2) 153.4 1_556
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C11 C12 C13 179.95(14) . . . . ?
O13 S1 C11 C16 -144.36(15) . . . . ?
O13 S1 C11 C12 36.48(16) . . . . ?
O1 C1 C2 N1 58.18(17) . . . . ?
O1 C1 C2 C3 -61.74(19) . . . . ?
O12 S1 C11 C16 95.89(15) . . . . ?
O12 S1 C11 C12 -83.27(15) . . . . ?
O11 S1 C11 C16 -23.60(17) . . . . ?
O11 S1 C11 C12 157.24(14) . . . . ?
C5 C10 C9 C8 0.3(3) . . . . ?
C5 C6 C7 C8 -0.5(3) . . . . ?
C5 C1 C2 N1 -177.66(15) . . . . ?
C5 C1 C2 C3 62.4(2) . . . . ?
C16 C11 C12 C13 0.8(3) . . . . ?
C16 C15 C14 C13 -0.1(3) . . . . ?
C11 C16 C15 C14 0.7(3) . . . . ?
C11 C12 C13 C14 -0.3(3) . . . . ?
C10 C5 C6 C7 1.0(3) . . . . ?
C10 C5 C1 O1 19.2(2) . . . . ?
C10 C5 C1 C2 -101.0(2) . . . . ?
C10 C9 C8 C7 0.1(3) . . . . ?
C9 C8 C7 C6 0.0(3) . . . . ?
C12 C13 C14 C15 0.0(3) . . . . ?
C6 C5 C10 C9 -0.8(3) . . . . ?
C6 C5 C1 O1 -159.50(16) . . . . ?
C6 C5 C1 C2 80.2(2) . . . . ?
C1 C5 C10 C9 -179.56(18) . . . . ?
C1 C5 C6 C7 179.72(17) . . . . ?
C4 N1 C2 C1 62.5(2) . . . . ?
C4 N1 C2 C3 -174.24(16) . . . . ?
C15 C16 C11 S1 179.86(16) . . . . ?
C15 C16 C11 C12 -1.0(3) . . . . ?
_shelx_res_file
;
pn180830_uo_eph_1_180814_b12_benzsulf.res created by SHELXL-2014/7
TITL pn180830_uo_eph_1_180814_b12_benzsulf_a.res in P2(1)
REM Old TITL PN180830_UO_Eph_1_180814_B12_benzsulf in P2(1)
REM SHELXT solution in P2(1)
REM R1 0.075, Rweak 0.044, Alpha 0.006, Orientation as input
REM Flack x = 0.125 ( 0.004 ) from Parsons' quotients
REM Formula found by SHELXT: C6 O5 Cl
CELL 1.54184 5.725873 20.838824 6.920538 90 98.3547 90
ZERR 2 0.000039 0.000104 0.000037 0 0.0005 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O S
UNIT 32 42 2 8 2
EQIV $1 -1+X,+Y,1+Z
EQIV $2 +X,+Y,1+Z
L.S. 4
PLAN 5
SIZE 0.17 0.224 0.702
TEMP -113
HTAB O1 O11
HTAB N1 O13_$1
HTAB N1 O12_$2
BOND $H
LIST 4
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.041400 0.107200
FVAR 12.05114
S1 5 0.980616 0.554781 0.028969 11.00000 0.02025 0.02540 =
0.01909 -0.00015 0.00718 -0.00053
O13 4 1.232591 0.540752 0.046837 11.00000 0.02323 0.03864 =
0.02390 -0.00251 0.00712 0.00705
O1 4 0.731523 0.463198 0.466271 11.00000 0.02791 0.03444 =
0.02477 -0.00405 0.01033 -0.00892
AFIX 147
H1 2 0.776688 0.478538 0.365719 11.00000 -1.50000
AFIX 0
O12 4 0.878151 0.571150 -0.169806 11.00000 0.02672 0.04015 =
0.02106 -0.00051 0.00186 -0.00554
O11 4 0.846245 0.505248 0.111683 11.00000 0.04030 0.02576 =
0.03511 -0.00029 0.02044 -0.00363
N1 3 0.436715 0.515881 0.709750 11.00000 0.02006 0.02795 =
0.01868 -0.00149 0.00570 -0.00065
AFIX 23
H1A 2 0.389907 0.515936 0.829909 11.00000 -1.20000
H1B 2 0.595045 0.523225 0.727056 11.00000 -1.20000
AFIX 0
C5 1 0.438305 0.383656 0.326059 11.00000 0.02656 0.02709 =
0.01583 0.00101 0.00640 -0.00278
C16 1 0.770023 0.631621 0.273268 11.00000 0.02554 0.03133 =
0.03398 -0.00324 0.01059 -0.00054
AFIX 43
H16 2 0.653038 0.599074 0.267453 11.00000 -1.20000
AFIX 0
C11 1 0.958474 0.624888 0.171010 11.00000 0.01984 0.02525 =
0.01999 0.00236 0.00124 0.00183
C10 1 0.611283 0.336589 0.331569 11.00000 0.02645 0.02984 =
0.02746 0.00015 0.00175 -0.00078
AFIX 43
H10 2 0.764782 0.344458 0.399959 11.00000 -1.20000
AFIX 0
C9 1 0.561542 0.278110 0.237856 11.00000 0.03634 0.02963 =
0.03456 -0.00265 0.00697 0.00345
AFIX 43
H9 2 0.680707 0.246181 0.242973 11.00000 -1.20000
AFIX 0
C12 1 1.128465 0.672627 0.176184 11.00000 0.02431 0.03230 =
0.02840 0.00227 0.00300 -0.00255
AFIX 43
H12 2 1.256632 0.667958 0.104194 11.00000 -1.20000
AFIX 0
C6 1 0.215085 0.371508 0.222776 11.00000 0.02468 0.03501 =
0.02669 -0.00474 0.00585 0.00055
AFIX 43
H6 2 0.095876 0.403470 0.216076 11.00000 -1.20000
AFIX 0
C1 1 0.487988 0.448249 0.425964 11.00000 0.02300 0.02687 =
0.01745 0.00059 0.00568 -0.00107
AFIX 13
H1C 2 0.407421 0.482393 0.339081 11.00000 -1.20000
AFIX 0
C4 1 0.317243 0.569943 0.594614 11.00000 0.03353 0.03211 =
0.02683 0.00268 0.01059 0.00826
AFIX 137
H4A 2 0.381739 0.574301 0.471628 11.00000 -1.50000
H4B 2 0.343873 0.609791 0.669788 11.00000 -1.50000
H4C 2 0.147424 0.561346 0.566589 11.00000 -1.50000
AFIX 0
C8 1 0.338363 0.266315 0.136969 11.00000 0.04052 0.03244 =
0.03157 -0.00893 0.00974 -0.00752
AFIX 43
H8 2 0.304003 0.226343 0.073125 11.00000 -1.20000
AFIX 0
C2 1 0.391887 0.450420 0.622109 11.00000 0.02295 0.02830 =
0.02045 -0.00147 0.00742 -0.00463
AFIX 13
H2 2 0.217812 0.442527 0.598135 11.00000 -1.20000
AFIX 0
C15 1 0.753065 0.686265 0.384425 11.00000 0.03313 0.04236 =
0.04024 -0.01056 0.01421 0.00286
AFIX 43
H15 2 0.624693 0.690966 0.456174 11.00000 -1.20000
AFIX 0
C13 1 1.109288 0.727021 0.287169 11.00000 0.03372 0.02961 =
0.03820 -0.00185 -0.00493 -0.00651
AFIX 43
H13 2 1.225327 0.759787 0.291838 11.00000 -1.20000
AFIX 0
C7 1 0.165854 0.313159 0.129840 11.00000 0.02840 0.04151 =
0.03192 -0.00962 0.00498 -0.00773
AFIX 43
H7 2 0.012748 0.305235 0.060774 11.00000 -1.20000
AFIX 0
C3 1 0.507126 0.401384 0.769767 11.00000 0.05737 0.02996 =
0.02018 0.00320 0.01202 -0.00103
AFIX 137
H3A 2 0.678922 0.406776 0.786962 11.00000 -1.50000
H3B 2 0.466212 0.357967 0.721964 11.00000 -1.50000
H3C 2 0.450264 0.407913 0.895217 11.00000 -1.50000
AFIX 0
C14 1 0.922082 0.734069 0.391582 11.00000 0.03891 0.03251 =
0.03721 -0.01076 -0.00051 0.00309
AFIX 43
H14 2 0.909678 0.771512 0.467737 11.00000 -1.20000
AFIX 0
HKLF 4
REM pn180830_uo_eph_1_180814_b12_benzsulf_a.res in P2(1)
REM R1 = 0.0230 for 3290 Fo > 4sig(Fo) and 0.0230 for all 3292 data
REM 202 parameters refined using 1 restraints
END
WGHT 0.0414 0.1073
REM Highest difference peak 0.176, deepest hole -0.320, 1-sigma level 0.051
Q1 1 0.8826 0.4837 0.2133 11.00000 0.05 0.18
Q2 1 0.0786 0.4607 0.2175 11.00000 0.05 0.14
Q3 1 0.8521 0.3693 0.6187 11.00000 0.05 0.13
Q4 1 0.5536 0.6118 -0.0031 11.00000 0.05 0.13
Q5 1 0.1581 0.5161 0.3096 11.00000 0.05 0.13
;
_shelx_res_checksum 5623
_shelx_hkl_file
;
0 -26 0 783.329 36.7352 2
0 -26 1 11356.0 131.355 2
0 -25 0 5.24537 17.3867 37
0 -25 0 7.42556 19.1225 2
0 -25 1 6831.30 132.747 2
0 -25 -1 6869.11 127.836 37
0 -25 -1 6835.33 129.531 2
0 -25 -2 8653.00 131.697 37
0 -25 -2 8636.79 126.704 2
0 -24 0 6075.60 143.592 37
0 -24 0 5906.82 146.830 2
0 -24 1 10610.3 194.866 2
0 -24 -1 10770.9 191.964 2
0 -24 -1 11040.3 194.176 37
0 -24 -2 2896.15 91.3192 2
0 -24 -2 2953.16 94.6643 37
0 -24 2 2987.15 95.7996 2
0 -24 -3 7234.37 125.191 37
0 -24 3 7168.33 127.235 2
0 -23 0 34.0483 29.8653 2
0 -23 0 3.57180 24.6860 37
0 -23 1 16455.7 268.343 2
0 -23 -1 16688.8 266.951 2
0 -23 1 16739.5 260.122 37
0 -23 -1 16299.3 265.682 37
0 -23 2 5900.46 153.609 2
0 -23 -2 5912.76 151.855 37
0 -23 -2 5932.26 148.873 2
0 -23 -3 3723.22 103.819 2
0 -23 3 3915.32 111.989 2
0 -23 -3 3731.41 109.362 37
0 -23 -4 3624.25 83.1508 37
0 -23 -4 3175.49 67.5574 2
0 -22 0 26168.7 373.403 2
0 -22 0 27759.7 377.284 37
0 -22 1 4258.55 146.158 2
0 -22 1 4327.13 142.932 37
0 -22 -1 4315.71 147.306 37
0 -22 -1 4335.70 147.488 2
0 -22 2 10390.2 221.725 2
0 -22 -2 10190.1 219.065 37
0 -22 -2 9927.36 214.434 36
0 -22 -3 17208.6 264.504 37
0 -22 3 17449.7 266.057 2
0 -22 -3 16998.6 259.244 36
0 -22 -4 8216.87 149.247 36
0 -22 4 8370.26 156.085 2
0 -21 0 20.0181 34.8843 2
0 -21 0 21.5290 31.7608 37
0 -21 1 1957.37 104.313 37
0 -21 1 1980.86 107.858 2
0 -21 -1 1880.86 106.289 2
0 -21 -1 1931.83 106.486 37
0 -21 -2 11222.2 245.976 37
0 -21 -2 11159.4 245.345 36
0 -21 2 11727.1 252.082 2
0 -21 -3 23270.2 334.394 36
0 -21 3 23129.2 333.490 2
0 -21 -3 22759.5 332.472 37
0 -21 4 301.567 39.6021 2
0 -21 -4 299.245 39.0119 36
0 -21 5 6337.12 115.477 2
0 -21 -5 5986.46 108.354 36
0 -20 0 6259.33 193.641 45
0 -20 0 6449.80 196.632 2
0 -20 0 6120.58 166.353 50
0 -20 0 6693.54 199.875 37
0 -20 -1 17573.1 297.110 50
0 -20 1 18320.3 330.965 2
0 -20 1 18507.8 327.329 37
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-5 12 -2 20133.1 332.888 28
-5 12 -3 6463.36 143.688 30
-5 12 -3 6356.88 156.866 29
-5 12 -3 6520.25 154.406 28
-5 12 -4 1056.21 39.1488 28
-5 13 5 372.466 27.9243 12
-5 13 4 9001.31 160.007 12
-5 13 3 21449.9 277.634 12
-5 13 3 21997.7 319.888 24
-5 13 2 2363.20 94.1214 12
-5 13 2 2483.69 116.993 24
-5 13 1 23893.9 392.475 30
-5 13 1 24184.5 370.096 24
-5 13 0 12087.6 274.866 30
-5 13 0 12110.0 278.058 28
-5 13 0 12159.7 255.755 24
-5 13 0 12516.6 233.277 11
-5 13 -1 933.651 76.7427 30
-5 13 -1 846.385 75.0007 29
-5 13 -1 994.025 82.7903 28
-5 13 -1 974.985 71.9149 24
-5 13 -1 948.734 64.4412 11
-5 13 -2 1515.37 84.2962 30
-5 13 -2 1723.50 94.8962 29
-5 13 -2 1724.02 94.2463 28
-5 13 -2 1589.94 79.7106 24
-5 13 -3 1531.39 64.7681 30
-5 13 -3 1635.78 73.8341 29
-5 13 -3 1561.69 70.2193 28
-5 14 5 1382.35 41.5123 12
-5 14 4 3053.87 85.8613 12
-5 14 3 5993.96 135.208 12
-5 14 3 6215.84 157.362 24
-5 14 2 2840.29 98.0804 12
-5 14 2 2815.02 118.743 24
-5 14 1 210.839 45.0577 30
-5 14 1 262.647 45.5581 24
-5 14 0 7755.13 209.350 30
-5 14 0 8062.63 209.372 28
-5 14 0 7978.28 194.843 24
-5 14 0 7749.88 175.768 11
-5 14 -1 8921.62 208.552 30
-5 14 -1 8705.26 207.849 29
-5 14 -1 8851.41 215.319 28
-5 14 -1 9115.42 195.689 24
-5 14 -1 8600.48 176.413 11
-5 14 -2 10210.4 195.506 30
-5 14 -2 10873.4 213.033 29
-5 14 -2 10736.1 210.478 28
-5 14 -3 14294.1 171.760 30
-5 14 -3 14259.0 186.559 28
-5 15 4 4868.79 97.3040 12
-5 15 3 23026.9 255.093 12
-5 15 3 24338.0 290.169 24
-5 15 2 6773.62 170.237 24
-5 15 1 13619.7 259.594 30
-5 15 1 13129.8 242.645 24
-5 15 1 13097.9 221.947 11
-5 15 0 13624.4 258.751 30
-5 15 0 13644.1 248.995 28
-5 15 0 13822.6 241.876 24
-5 15 0 13518.9 220.653 11
-5 15 -1 1397.51 79.6689 30
-5 15 -1 1336.93 74.2461 29
-5 15 -1 1357.30 79.7077 28
-5 15 -1 1418.24 73.6836 24
-5 15 -1 1338.86 67.3459 11
-5 15 -2 49.6237 23.4986 29
-5 15 -2 49.0719 24.0827 28
-5 15 -3 2350.39 61.4682 29
-5 15 -3 2364.07 62.3034 28
-5 16 3 3637.26 89.3348 12
-5 16 3 3893.28 101.090 24
-5 16 2 13839.5 224.344 24
-5 16 1 7173.70 170.365 30
-5 16 1 7011.38 165.677 24
-5 16 1 7037.48 151.780 11
-5 16 0 6536.09 164.198 30
-5 16 0 6427.70 149.745 28
-5 16 0 6625.09 154.623 24
-5 16 0 6177.83 138.915 11
-5 16 -1 9712.02 183.733 30
-5 16 -1 9346.15 163.474 29
-5 16 -1 9341.97 180.877 28
-5 16 -1 9389.21 159.702 11
-5 16 -2 5519.36 110.429 29
-5 16 -2 5457.60 116.707 28
-5 16 -2 5407.35 103.086 24
-5 17 3 4056.85 87.4770 24
-5 17 2 3753.12 103.638 24
-5 17 2 3463.33 93.8914 11
-5 17 1 4817.49 122.801 30
-5 17 1 4687.99 122.170 24
-5 17 1 4538.27 111.329 11
-5 17 0 4860.59 127.288 30
-5 17 0 4897.26 120.460 24
-5 17 0 4750.06 111.614 11
-5 17 -1 8791.10 155.758 30
-5 17 -1 8472.56 144.713 28
-5 17 -1 8481.15 135.821 11
-5 17 -2 317.611 24.0049 28
-5 18 3 9496.37 113.249 11
-5 18 2 1419.92 55.0849 24
-5 18 2 1322.40 51.3967 11
-5 18 1 7395.45 127.493 30
-5 18 1 7392.48 134.955 24
-5 18 1 7378.82 124.756 11
-5 18 0 6114.65 120.625 30
-5 18 0 5996.20 116.120 24
-5 18 0 5749.80 107.161 11
-5 18 -1 4128.46 87.5429 30
-5 18 -1 4090.79 79.6559 24
-5 19 1 1843.91 54.2472 24
-5 19 1 1793.93 50.9480 11
-5 19 0 4556.93 76.4661 11
-6 -14 2 1851.44 46.1573 16
-6 -14 1 106.640 15.9916 16
-6 -14 0 4717.61 79.1220 16
-6 -13 2 9152.29 118.336 16
-6 -13 1 2038.86 61.0175 16
-6 -13 0 6041.69 103.703 16
-6 -13 -1 6527.54 95.5875 16
-6 -12 2 2485.56 67.3895 16
-6 -12 1 234.970 26.4702 16
-6 -12 0 4833.48 97.5766 17
-6 -12 0 4912.23 103.751 16
-6 -12 -1 10257.1 132.891 17
-6 -11 2 16244.2 187.036 16
-6 -11 1 892.298 48.0641 16
-6 -11 0 943.047 47.9653 17
-6 -11 0 963.351 51.3072 16
-6 -11 -1 8986.88 135.960 17
-6 -11 -2 2834.40 61.9341 17
-6 -10 2 3530.50 89.0980 16
-6 -10 1 1926.78 67.6816 17
-6 -10 1 1956.64 73.0686 16
-6 -10 1 1936.23 78.8211 47
-6 -10 0 1532.27 63.5023 17
-6 -10 -1 5221.16 112.001 17
-6 -10 -2 2313.92 63.8111 17
-6 -9 2 7029.08 129.782 16
-6 -9 1 12648.5 180.637 17
-6 -9 1 13005.1 193.550 16
-6 -9 0 7210.02 143.080 17
-6 -9 -1 859.972 51.1364 17
-6 -9 -2 5383.29 106.741 17
-6 -8 1 2906.18 88.5226 17
-6 -8 1 2866.52 92.7643 16
-6 -8 0 10131.6 176.464 17
-6 -8 -1 5966.59 134.634 17
-6 -8 -2 6137.15 122.607 17
-6 -8 -3 5176.72 82.2822 17
-6 -7 1 805.478 49.8700 17
-6 -7 1 817.319 51.9657 16
-6 -7 0 1238.78 66.1217 17
-6 -7 -1 1114.01 63.4912 17
-6 -7 -2 5579.02 124.373 17
-6 -7 -3 1805.42 54.7388 17
-6 -6 1 4374.91 111.241 17
-6 -6 0 3009.80 102.169 17
-6 -6 -1 521.612 47.7919 17
-6 -6 -2 4428.80 116.914 17
-6 -6 -3 2972.93 75.8025 17
-6 -5 0 3636.16 114.255 17
-6 -5 -1 2341.70 94.8175 17
-6 -5 -1 2244.62 85.5564 25
-6 -5 -2 6080.11 142.449 17
-6 -5 -2 5883.52 127.896 25
-6 -5 -3 19065.8 210.794 17
-6 -4 0 12182.4 211.707 17
-6 -4 0 12034.3 195.751 25
-6 -4 -1 404.850 45.7876 17
-6 -4 -1 397.643 42.5162 25
-6 -4 -2 14683.1 227.912 17
-6 -4 -2 14078.9 208.083 25
-6 -4 -3 3071.35 87.5741 17
-6 -3 0 5093.39 137.042 17
-6 -3 0 4914.54 128.358 25
-6 -3 -1 2515.32 102.455 17
-6 -3 -1 2423.76 94.8320 25
-6 -3 -2 7798.14 171.048 17
-6 -3 -2 7247.19 153.153 25
-6 -3 -3 2437.85 81.0175 17
-6 -3 -3 2377.12 72.5794 25
-6 -2 0 3983.44 120.482 17
-6 -2 0 3784.79 115.786 25
-6 -2 -1 4689.44 139.423 17
-6 -2 -1 4475.23 132.132 25
-6 -2 -2 24154.7 315.156 17
-6 -2 -2 23724.8 289.957 25
-6 -2 -3 6778.35 138.243 17
-6 -2 -3 6540.03 123.885 25
-6 -1 0 12580.2 215.568 25
-6 -1 -1 3968.09 128.888 17
-6 -1 -1 3702.05 123.334 25
-6 -1 -2 2508.62 101.559 17
-6 -1 -2 2547.23 92.8670 26
-6 -1 -2 2385.91 94.4785 25
-6 -1 -3 2323.34 83.5421 17
-6 -1 -3 2066.96 72.3657 25
-6 0 0 91.0037 31.4944 25
-6 0 -1 52039.5 484.302 17
-6 0 -1 51672.2 489.014 25
-6 0 -2 12275.9 222.874 17
-6 0 -2 12160.5 204.774 26
-6 0 -2 11905.4 211.069 25
-6 0 -3 148.151 28.0832 17
-6 0 -3 106.282 25.0385 25
-6 1 0 14054.6 234.195 25
-6 1 -1 4722.81 136.800 17
-6 1 -1 4641.06 141.891 25
-6 1 -2 2273.45 97.2946 17
-6 1 -2 2075.52 86.1937 26
-6 1 -2 2119.89 92.9341 25
-6 1 -3 2355.84 83.0870 17
-6 1 -3 2256.73 76.6557 26
-6 2 0 3679.50 121.467 25
-6 2 -1 6230.86 166.499 25
-6 2 -2 26785.5 328.205 17
-6 2 -2 25920.0 304.773 26
-6 2 -2 25944.4 323.551 25
-6 2 -3 5773.06 126.380 17
-6 2 -3 5902.40 121.874 26
-6 2 -3 5776.58 124.148 25
-6 3 0 6752.22 165.142 25
-6 3 -1 2940.51 111.898 28
-6 3 -1 2901.67 116.207 25
-6 3 -2 6958.12 158.885 17
-6 3 -2 6941.48 152.982 26
-6 3 -2 6981.78 166.681 25
-6 3 -3 2320.83 76.0349 17
-6 3 -3 2234.36 74.1329 26
-6 3 -3 2257.47 77.8338 25
-6 4 0 12491.2 223.294 30
-6 4 0 13200.8 231.862 25
-6 4 -1 1012.22 68.1657 28
-6 4 -2 14862.3 238.396 28
-6 4 -2 14839.7 245.095 25
-6 4 -3 3360.37 86.1371 26
-6 4 -3 3348.95 91.6939 25
-6 5 0 3631.86 122.511 30
-6 5 -1 3007.85 113.016 30
-6 5 -1 3167.06 117.054 28
-6 5 -2 7124.67 162.426 28
-6 5 -3 17911.8 191.096 26
-6 5 -3 19029.7 217.842 25
-6 6 0 3796.44 126.820 30
-6 6 0 3762.11 118.441 24
-6 6 -1 762.958 59.4457 30
-6 6 -1 785.438 60.7061 28
-6 6 -2 4468.14 127.505 28
-6 6 -3 3505.71 88.2906 25
-6 7 0 731.482 58.9921 30
-6 7 0 760.900 56.5200 24
-6 7 -1 1427.27 78.8280 30
-6 7 -1 1448.80 78.3533 28
-6 7 -2 5753.70 140.160 28
-6 7 -3 1641.33 56.7372 25
-6 8 0 10455.0 208.724 30
-6 8 0 10375.4 199.184 24
-6 8 -1 7532.22 172.907 30
-6 8 -1 7303.75 168.746 28
-6 8 -2 5529.23 130.970 28
-6 8 -3 5828.96 95.7601 25
-6 9 0 6239.76 158.419 30
-6 9 0 6196.53 150.195 24
-6 9 -1 1047.06 66.1192 30
-6 9 -1 1172.32 66.4916 28
-6 9 -2 5648.55 123.931 28
-6 10 1 2823.27 99.9250 24
-6 10 0 2189.47 92.5619 30
-6 10 0 2198.23 88.3462 24
-6 10 -1 4638.50 127.040 30
-6 10 -1 4653.76 117.969 28
-6 10 -2 2708.20 76.7750 28
-6 11 1 765.092 52.4303 24
-6 11 0 510.348 45.2732 30
-6 11 0 577.279 45.8976 24
-6 11 -1 9562.05 166.692 30
-6 11 -2 2545.29 62.6182 28
-6 12 1 70.6039 23.0674 24
-6 12 0 6323.90 131.797 30
-6 12 0 6486.79 132.397 24
-6 12 -1 11555.4 164.680 30
-6 13 1 1446.61 56.6302 24
-6 13 0 6114.45 111.079 30
-6 13 0 6491.12 119.845 24
-6 13 -1 6491.76 103.498 30
-6 14 1 154.104 18.3996 24
-6 14 0 5203.91 90.7669 24
0 0 0 0.00 0.00 0
TITL PN180830_UO_Eph_1_180814_B12_benzsulf in P2(1)
REM P2(1) (#4 in standard setting)
CELL 1.54184 5.725870 20.838830 6.920534 90.0000 98.3547 90.0000
ZERR 2.00 0.000039 0.000104 0.000037 0.0000 0.0005 0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C H N O S
UNIT 32.00 42.00 2.00 8.00 2.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 98366
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.214
_oxdiff_exptl_absorpt_empirical_full_min 0.805
data_pn180914_uo_eph_1_180814_g4_2
_audit_creation_date 2018-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number '2014/7'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '2(C10 H16 N O), C4 H4 O5, H2 O'
_chemical_formula_sum 'C24 H38 N2 O8'
_chemical_formula_weight 482.56
_chemical_absolute_configuration rmad
_chemical_melting_point ?
_chemical_oxdiff_formula 'C24 H38 N2 O8'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system 'triclinic'
_space_group_IT_number 1
_space_group_name_H-M_alt 'P 1'
_space_group_name_Hall 'P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
_cell_length_a 5.82130(7)
_cell_length_b 7.27088(8)
_cell_length_c 15.90214(13)
_cell_angle_alpha 94.7215(8)
_cell_angle_beta 96.6693(8)
_cell_angle_gamma 109.5246(11)
_cell_volume 624.781(12)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 16192
_cell_measurement_temperature 159.99(10)
_cell_measurement_theta_max 78.6150
_cell_measurement_theta_min 5.6250
_shelx_estimated_absorpt_T_max 0.989
_shelx_estimated_absorpt_T_min 0.797
_exptl_absorpt_coefficient_mu 0.794
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.463
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.16c (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.283
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 260
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 0 0 0.0829
0 -4 2 0.0912
0 5 -2 0.1587
-3 3 -1 0.1419
-3 -1 1 0.1036
0 0 -10 0.0098
0 0 10 0.0038
3 -4 1 0.1382
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.014
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.0017 0.0004 0.0035 -0.1066 0.3219 -1.0853
-0.0028 -3.9970 1.9999 -0.1531 0.7165 0.5266
0.0033 4.9962 -2.0002 0.1425 -0.8979 -0.6620
-2.9994 2.9974 -1.0028 0.1458 -0.7811 0.4153
-3.0021 -0.9996 0.9971 -0.0073 -0.0646 0.9420
0.0032 0.0015 -9.9949 0.9791 0.0452 0.0740
-0.0032 -0.0015 9.9949 -0.9791 -0.0452 -0.0740
2.9988 -3.9965 1.0031 -0.1352 0.9625 -0.2800
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0318
_diffrn_reflns_av_unetI/netI 0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 19924
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full 69.500
_diffrn_reflns_theta_max 78.859
_diffrn_reflns_theta_min 2.821
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 159.99(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
--------------------------------------------------------------------------
1 \w 35.00 123.00 0.50 0.60 -- 50.46 57.00 30.00 176
2 \w 92.00 125.00 0.50 2.40 -- 102.00 48.00 42.46 66
3 \w 134.00 160.00 0.50 2.40 -- 107.75 45.00 60.00 52
4 \w 141.00 175.00 0.50 2.40 -- 107.75 45.00 90.00 68
5 \w 146.00 172.00 0.50 2.40 -- 107.75 45.00 150.00 52
6 \w 146.00 178.00 0.50 2.40 -- 107.75 45.00 120.00 64
7 \w 123.00 159.00 0.50 2.40 -- 107.75 15.00 120.00 72
8 \w 116.00 151.00 0.50 2.40 -- 107.75 30.00 90.00 70
9 \w 114.00 178.00 0.50 2.40 -- 107.75 30.00 30.00 128
10 \w 152.00 178.00 0.50 2.40 -- 107.75 58.00 -28.47 52
11 \w 153.00 178.00 0.50 2.40 -- 107.75 15.00 -60.00 50
12 \w 153.00 178.00 0.50 2.40 -- 107.75 45.00-120.00 50
13 \w 138.00 164.00 0.50 2.40 -- 107.75 45.00-150.00 52
14 \w 110.00 162.00 0.50 2.40 -- 107.75 30.00-120.00 104
15 \w 108.00 150.00 0.50 2.40 -- 107.75 15.00 -30.00 84
16 \w 97.00 124.00 0.50 2.40 -- 107.75 45.00 60.00 54
17 \w 94.00 120.00 0.50 2.40 -- 107.75 45.00 30.00 52
18 \w 92.00 135.00 0.50 2.40 -- 107.75 58.00 -28.47 86
19 \w 100.00 125.00 0.50 2.40 -- 107.75 15.00 -60.00 50
20 \w 95.00 158.00 0.50 2.40 -- 107.75 45.00 0.00 126
21 \w 94.00 129.00 0.50 2.40 -- 107.75 45.00 90.00 70
22 \w 102.00 144.00 0.50 2.40 -- 107.75 30.00 150.00 84
23 \w 95.00 141.00 0.50 2.40 -- 107.75 45.00 150.00 92
24 \w 99.00 124.00 0.50 2.40 -- 107.75 45.00 120.00 50
25 \w 79.00 120.00 0.50 2.40 -- 107.75 -6.00 54.81 82
26 \w 84.00 111.00 0.50 2.40 -- 107.75 -60.00 51.39 54
27 \w 76.00 102.00 0.50 2.40 -- 107.75 -59.00 129.58 52
28 \w 41.00 94.00 0.50 2.40 -- 107.75 -58.00 76.83 106
29 \w 43.00 69.00 0.50 2.40 -- 107.75 -57.00 89.40 52
30 \w 39.00 86.00 0.50 2.40 -- 107.75 -52.00 139.96 94
31 \w 30.00 55.00 0.50 2.40 -- 107.75 -30.00 60.00 50
32 \w 38.00 104.00 0.50 2.40 -- 107.75 -60.00 20.05 132
33 \w 87.00 114.00 0.50 2.40 -- 107.75 -15.00 -60.00 54
34 \w 80.00 109.00 0.50 2.40 -- 107.75 -60.00 -45.07 58
35 \w 53.00 85.00 0.50 2.40 -- 90.00 -60.00-151.75 64
36 \w 73.00 123.00 0.50 2.40 -- 107.75 -60.00-150.94 100
37 \w 67.00 98.00 0.50 2.40 -- 107.75 -58.00-179.05 62
38 \w 51.00 102.00 0.50 2.40 -- 107.75 -59.00 -78.83 102
39 \w 37.00 63.00 0.50 2.40 -- 107.75 -58.00-179.05 52
40 \w 37.00 62.00 0.50 2.40 -- 107.75 -60.00-150.94 50
41 \w 32.00 65.00 0.50 2.40 -- 107.75 -30.00-150.00 66
42 \w 31.00 68.00 0.50 2.40 -- 107.75 -30.00-120.00 74
43 \w 33.00 68.00 0.50 2.40 -- 107.75 -30.00-180.00 70
44 \w 97.00 124.00 0.50 2.40 -- 107.75 45.00-150.00 54
45 \w 97.00 123.00 0.50 2.40 -- 107.75 45.00 -90.00 52
46 \w 94.00 122.00 0.50 2.40 -- 107.75 45.00 -60.00 56
47 \w 98.00 139.00 0.50 2.40 -- 107.75 45.00-120.00 82
48 \w 95.00 176.00 0.50 2.40 -- 107.75 45.00-180.00 162
49 \w 96.00 145.00 0.50 2.40 -- 107.75 45.00 -30.00 98
50 \w 66.00 97.00 0.50 2.40 -- 82.00 60.00-104.77 62
51 \w 35.00 123.00 0.50 0.60 -- 50.46 57.00-120.00 176
52 \w 35.00 123.00 0.50 0.60 -- 50.46 57.00-180.00 176
53 \w 35.00 122.00 0.50 0.60 -- 50.46 60.00-109.26 174
54 \w 33.00 70.00 0.50 2.40 -- 107.75 -45.00 -30.00 74
55 \w 37.00 63.00 0.50 2.40 -- 107.75 -60.00 51.39 52
56 \w 35.00 93.00 0.50 2.40 -- 107.75 -57.00 104.89 116
57 \w 36.00 73.00 0.50 2.40 -- 107.75 -59.00 129.58 74
58 \w 30.00 73.00 0.50 2.40 -- 107.75 -6.00 54.81 86
59 \w 38.00 84.00 0.50 2.40 -- 107.75 -57.00 -33.73 92
60 \w 36.00 66.00 0.50 2.40 -- 107.75 -60.00 -45.07 60
61 \w -6.00 82.00 0.50 0.60 -- 66.00 -60.00-120.29 176
62 \w -22.00 66.00 0.50 0.60 -- 50.46 -57.00 120.00 176
63 \w 35.00 123.00 0.50 0.60 -- 50.46 57.00 150.00 176
64 \w 10.00 98.00 0.50 0.60 -- 26.00 59.00 164.77 176
65 \w -65.00 -20.00 0.50 2.40 -- -86.25 59.00 97.75 90
66 \w -103.00 -76.00 0.50 2.40 -- -86.25 -56.00 106.55 54
67 \w -98.00 -71.00 0.50 2.40 -- -86.25 -60.00 123.27 54
68 \w -97.00 -71.00 0.50 2.40 -- -86.25 -58.00 75.39 52
69 \w -96.00 -71.00 0.50 2.40 -- -86.25 -59.00 38.58 50
70 \w -98.00 -70.00 0.50 2.40 -- -82.00 -59.00 -12.71 56
71 \w -98.00 -73.00 0.50 2.40 -- -86.25 -60.00 -68.11 50
72 \w -95.00 -68.00 0.50 2.40 -- -82.00 -58.00 -85.23 54
73 \w -95.00 -67.00 0.50 2.40 -- -82.00 -57.00 -97.74 56
74 \w -89.00 -63.00 0.50 2.40 -- -78.00 -60.00-178.80 52
75 \w -99.00 -71.00 0.50 2.40 -- -86.25 -56.00-113.80 56
76 \w -102.00 -74.00 0.50 2.40 -- -86.25 -54.00-158.17 56
77 \w -114.00 -26.00 0.50 0.60 -- -42.00 -59.00 -88.70 176
78 \w -102.00 -70.00 0.50 2.40 -- -82.00 -59.00 -45.36 64
79 \w -98.00 -71.00 0.50 2.40 -- -86.25 -60.00 18.04 54
80 \w -105.00 -71.00 0.50 2.40 -- -86.25 -59.00 65.56 68
81 \w -99.00 -73.00 0.50 2.40 -- -86.25 -60.00 153.02 52
82 \w -102.00 -72.00 0.50 2.40 -- -86.25 -60.00 174.82 60
83 \w -128.00 -38.00 0.50 0.60 -- -50.46 -38.00 60.00 180
84 \w -118.00 -30.00 0.50 0.60 -- -46.00 -60.00 13.51 176
85 \w -122.00 -34.00 0.50 0.60 -- -50.00 -59.00-114.16 176
86 \w -126.00 -39.00 0.50 0.60 -- -54.00 -58.00 40.19 174
87 \w -131.00 -38.00 0.50 0.60 -- -50.46 -19.00 -60.00 186
88 \w -82.00 -57.00 0.50 2.40 -- -86.25 60.00-170.23 50
89 \w -126.00 -39.00 0.50 0.60 -- -54.00 -58.00-158.34 174
90 \w -142.00 -54.00 0.50 2.40 -- -70.00 -60.00 -16.61 176
91 \w -131.00 -38.00 0.50 0.60 -- -50.46 -19.00 90.00 186
92 \w -126.00-100.00 0.50 2.40 -- -86.25 -59.00 38.58 52
93 \w -126.00-100.00 0.50 2.40 -- -86.25 -58.00 75.39 52
94 \w -134.00 -46.00 0.50 0.60 -- -62.00 -60.00 72.08 176
95 \w -146.00 -58.00 0.50 2.40 -- -74.00 -59.00 23.87 176
96 \w -146.00 -58.00 0.50 2.40 -- -74.00 -60.00 -51.46 176
97 \w -152.00-125.00 0.50 2.40 -- -82.00 -57.00 -97.74 54
98 \w -150.00 -62.00 0.50 2.40 -- -78.00 -60.00 147.36 176
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0265503000
_diffrn_orient_matrix_UB_12 -0.0106884000
_diffrn_orient_matrix_UB_13 -0.0979728000
_diffrn_orient_matrix_UB_21 0.0804748000
_diffrn_orient_matrix_UB_22 -0.1815815000
_diffrn_orient_matrix_UB_23 -0.0045260000
_diffrn_orient_matrix_UB_31 -0.2711991000
_diffrn_orient_matrix_UB_32 -0.1353257000
_diffrn_orient_matrix_UB_33 -0.0075118000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage 0.907
_reflns_Friedel_fraction_full 0.901
_reflns_Friedel_fraction_max 0.845
_reflns_number_gt 4709
_reflns_number_total 4803
_reflns_odcompleteness_completeness 92.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 79.66
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.40.16c (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.40.16c (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.40.16c (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.155
_refine_diff_density_min -0.182
_refine_diff_density_rms 0.031
_refine_ls_abs_structure_details
;
Flack x determined using 2188 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.00(6)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.063
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 322
_refine_ls_number_reflns 4803
_refine_ls_number_restraints 3
_refine_ls_R_factor_all 0.0275
_refine_ls_R_factor_gt 0.0270
_refine_ls_restrained_S_all 1.063
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.0580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0733
_refine_ls_wR_factor_ref 0.0735
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H,H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
C1(H1C), C2(H2), C11(H11C), C12(H12), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
N1(H1A,H1B), N11(H11A,H11B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16), C17(H17), C18(H18),
C19(H19), C20(H20)
2.d Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
2.e Idealised tetrahedral OH refined as rotating group:
O1(H1), O11(H11), O23(H23)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.3528(3) 0.7437(2) 0.71174(9) 0.0280(3) Uani 1 1 d . . . . .
H1 H 0.3828 0.6429 0.6946 0.042 Uiso 1 1 calc GR . . . .
O11 O 0.0273(3) 0.2787(2) 0.31283(9) 0.0279(3) Uani 1 1 d . . . . .
H11 H 0.0322 0.1910 0.3435 0.042 Uiso 1 1 calc GR . . . .
O21 O 0.4190(3) 0.4004(2) 0.66616(8) 0.0297(3) Uani 1 1 d . . . . .
O22 O 0.3495(3) 0.13593(19) 0.57188(8) 0.0266(3) Uani 1 1 d . . . . .
O23 O 0.5910(3) 0.65204(18) 0.55313(8) 0.0219(3) Uani 1 1 d . . . . .
H23 H 0.4607 0.6786 0.5477 0.033 Uiso 1 1 calc GR . . . .
O24 O 1.1434(3) 0.6384(2) 0.47409(9) 0.0298(3) Uani 1 1 d . . . . .
O25 O 0.8005(3) 0.6055(2) 0.38907(8) 0.0253(3) Uani 1 1 d . . . . .
O26 O 0.0579(4) 0.0217(3) 0.41762(12) 0.0467(5) Uani 1 1 d . . . . .
H26A H 0.163(7) 0.053(5) 0.467(2) 0.050(8) Uiso 1 1 d . . . . .
H26B H -0.008(7) -0.090(6) 0.408(2) 0.052(9) Uiso 1 1 d . . . . .
N1 N -0.0068(3) 0.9289(2) 0.66287(9) 0.0219(3) Uani 1 1 d . . . . .
H1A H 0.1386 0.9812 0.6429 0.026 Uiso 1 1 calc R . . . .
H1B H -0.1003 0.8193 0.6264 0.026 Uiso 1 1 calc R . . . .
N11 N 0.3851(3) 0.6649(2) 0.33349(10) 0.0232(3) Uani 1 1 d . . . . .
H11A H 0.2625 0.6384 0.3662 0.028 Uiso 1 1 calc R . . . .
H11B H 0.5093 0.6315 0.3604 0.028 Uiso 1 1 calc R . . . .
C1 C 0.1194(4) 0.6869(3) 0.73851(11) 0.0211(4) Uani 1 1 d . . . . .
H1C H -0.0018 0.5907 0.6919 0.025 Uiso 1 1 calc R . . . .
C2 C 0.0450(4) 0.8697(3) 0.74950(11) 0.0222(4) Uani 1 1 d . . . . .
H2 H -0.1105 0.8339 0.7751 0.027 Uiso 1 1 calc R . . . .
C3 C 0.2385(5) 1.0414(3) 0.80709(13) 0.0301(4) Uani 1 1 d . . . . .
H3A H 0.3864 1.0885 0.7798 0.045 Uiso 1 1 calc GR . . . .
H3B H 0.2810 0.9987 0.8618 0.045 Uiso 1 1 calc GR . . . .
H3C H 0.1733 1.1481 0.8169 0.045 Uiso 1 1 calc GR . . . .
C4 C -0.1364(4) 1.0741(3) 0.66229(15) 0.0332(5) Uani 1 1 d . . . . .
H4A H -0.1833 1.0927 0.6032 0.050 Uiso 1 1 calc GR . . . .
H4B H -0.0265 1.2001 0.6941 0.050 Uiso 1 1 calc GR . . . .
H4C H -0.2847 1.0252 0.6892 0.050 Uiso 1 1 calc GR . . . .
C5 C 0.1096(4) 0.5891(2) 0.81996(11) 0.0194(4) Uani 1 1 d . . . . .
C6 C -0.1179(4) 0.4745(3) 0.83863(12) 0.0252(4) Uani 1 1 d . . . . .
H6 H -0.2643 0.4600 0.8013 0.030 Uiso 1 1 calc R . . . .
C7 C -0.1322(4) 0.3808(3) 0.91181(13) 0.0300(5) Uani 1 1 d . . . . .
H7 H -0.2883 0.3031 0.9244 0.036 Uiso 1 1 calc R . . . .
C8 C 0.0811(5) 0.4008(3) 0.96636(12) 0.0299(5) Uani 1 1 d . . . . .
H8 H 0.0715 0.3371 1.0163 0.036 Uiso 1 1 calc R . . . .
C9 C 0.3070(4) 0.5135(3) 0.94768(12) 0.0298(5) Uani 1 1 d . . . . .
H9 H 0.4532 0.5264 0.9848 0.036 Uiso 1 1 calc R . . . .
C10 C 0.3228(4) 0.6089(3) 0.87479(12) 0.0250(4) Uani 1 1 d . . . . .
H10 H 0.4792 0.6873 0.8627 0.030 Uiso 1 1 calc R . . . .
C11 C 0.2283(4) 0.3227(3) 0.26709(11) 0.0226(4) Uani 1 1 d . . . . .
H11C H 0.3737 0.3129 0.3041 0.027 Uiso 1 1 calc R . . . .
C12 C 0.2881(4) 0.5375(3) 0.24936(11) 0.0234(4) Uani 1 1 d . . . . .
H12 H 0.4210 0.5691 0.2127 0.028 Uiso 1 1 calc R . . . .
C13 C 0.0666(4) 0.5759(3) 0.20437(13) 0.0291(4) Uani 1 1 d . . . . .
H13A H -0.0573 0.5609 0.2425 0.044 Uiso 1 1 calc GR . . . .
H13B H -0.0045 0.4816 0.1525 0.044 Uiso 1 1 calc GR . . . .
H13C H 0.1190 0.7101 0.1891 0.044 Uiso 1 1 calc GR . . . .
C14 C 0.4785(5) 0.8794(3) 0.32894(16) 0.0371(5) Uani 1 1 d . . . . .
H14A H 0.6054 0.9097 0.2917 0.056 Uiso 1 1 calc GR . . . .
H14B H 0.5497 0.9502 0.3863 0.056 Uiso 1 1 calc GR . . . .
H14C H 0.3422 0.9204 0.3059 0.056 Uiso 1 1 calc GR . . . .
C15 C 0.1768(4) 0.1836(3) 0.18465(12) 0.0232(4) Uani 1 1 d . . . . .
C16 C 0.3703(4) 0.1792(3) 0.14115(13) 0.0306(4) Uani 1 1 d . . . . .
H16 H 0.5338 0.2641 0.1629 0.037 Uiso 1 1 calc R . . . .
C17 C 0.3256(5) 0.0516(4) 0.06610(14) 0.0361(5) Uani 1 1 d . . . . .
H17 H 0.4586 0.0510 0.0368 0.043 Uiso 1 1 calc R . . . .
C18 C 0.0899(5) -0.0741(3) 0.03400(13) 0.0349(5) Uani 1 1 d . . . . .
H18 H 0.0601 -0.1622 -0.0168 0.042 Uiso 1 1 calc R . . . .
C19 C -0.1021(5) -0.0702(3) 0.07664(13) 0.0330(5) Uani 1 1 d . . . . .
H19 H -0.2652 -0.1558 0.0548 0.040 Uiso 1 1 calc R . . . .
C20 C -0.0590(4) 0.0581(3) 0.15145(13) 0.0275(4) Uani 1 1 d . . . . .
H20 H -0.1932 0.0594 0.1800 0.033 Uiso 1 1 calc R . . . .
C21 C 0.4244(4) 0.3198(3) 0.59479(11) 0.0200(4) Uani 1 1 d . . . . .
C22 C 0.5342(4) 0.4477(2) 0.52644(11) 0.0194(4) Uani 1 1 d . . . . .
H22 H 0.4122 0.4077 0.4727 0.023 Uiso 1 1 calc R . . . .
C23 C 0.7722(4) 0.4180(3) 0.50804(11) 0.0213(4) Uani 1 1 d . . . . .
H23A H 0.8790 0.4299 0.5629 0.026 Uiso 1 1 calc R . . . .
H23B H 0.7312 0.2831 0.4786 0.026 Uiso 1 1 calc R . . . .
C24 C 0.9147(4) 0.5647(3) 0.45332(11) 0.0201(4) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0328(9) 0.0230(6) 0.0352(7) 0.0089(5) 0.0184(6) 0.0131(7)
O11 0.0340(10) 0.0255(7) 0.0297(6) 0.0110(5) 0.0135(6) 0.0129(7)
O21 0.0395(10) 0.0278(7) 0.0247(6) 0.0060(5) 0.0100(6) 0.0131(7)
O22 0.0314(9) 0.0185(6) 0.0293(6) 0.0064(5) 0.0081(6) 0.0059(6)
O23 0.0188(7) 0.0163(6) 0.0316(6) 0.0024(5) 0.0042(5) 0.0074(5)
O24 0.0200(9) 0.0329(7) 0.0364(7) 0.0100(6) 0.0030(6) 0.0081(7)
O25 0.0251(8) 0.0292(7) 0.0245(6) 0.0087(5) 0.0050(5) 0.0114(6)
O26 0.0580(13) 0.0214(8) 0.0461(9) 0.0114(7) -0.0162(9) 0.0009(8)
N1 0.0210(9) 0.0184(7) 0.0260(7) 0.0057(5) 0.0028(6) 0.0058(7)
N11 0.0208(9) 0.0210(7) 0.0284(7) 0.0076(6) 0.0054(6) 0.0065(7)
C1 0.0236(11) 0.0169(8) 0.0220(8) 0.0035(6) 0.0048(7) 0.0055(8)
C2 0.0280(12) 0.0186(8) 0.0223(8) 0.0050(6) 0.0073(7) 0.0093(8)
C3 0.0418(14) 0.0197(9) 0.0257(8) -0.0004(7) 0.0020(8) 0.0083(9)
C4 0.0288(14) 0.0253(10) 0.0506(12) 0.0151(8) 0.0085(9) 0.0129(10)
C5 0.0211(11) 0.0157(8) 0.0217(8) 0.0019(6) 0.0052(7) 0.0062(8)
C6 0.0236(12) 0.0244(9) 0.0281(9) 0.0057(7) 0.0052(7) 0.0082(9)
C7 0.0318(14) 0.0270(10) 0.0321(10) 0.0099(8) 0.0127(8) 0.0072(10)
C8 0.0468(15) 0.0239(9) 0.0230(8) 0.0066(7) 0.0082(8) 0.0158(10)
C9 0.0366(14) 0.0268(9) 0.0274(9) 0.0012(7) -0.0024(8) 0.0159(10)
C10 0.0229(11) 0.0211(8) 0.0294(9) 0.0022(7) 0.0026(7) 0.0063(8)
C11 0.0233(11) 0.0242(9) 0.0230(8) 0.0072(6) 0.0034(7) 0.0108(8)
C12 0.0262(12) 0.0230(9) 0.0235(8) 0.0076(7) 0.0064(7) 0.0099(9)
C13 0.0354(13) 0.0278(10) 0.0269(8) 0.0085(7) 0.0006(8) 0.0148(10)
C14 0.0386(15) 0.0201(9) 0.0481(12) 0.0086(8) 0.0023(10) 0.0050(10)
C15 0.0249(11) 0.0233(9) 0.0247(8) 0.0070(7) 0.0032(7) 0.0119(9)
C16 0.0250(12) 0.0344(10) 0.0338(10) 0.0019(8) 0.0040(8) 0.0128(10)
C17 0.0409(15) 0.0432(13) 0.0343(10) 0.0055(9) 0.0117(9) 0.0256(12)
C18 0.0511(16) 0.0286(10) 0.0289(10) 0.0024(8) 0.0015(9) 0.0209(11)
C19 0.0363(14) 0.0233(9) 0.0344(10) 0.0018(8) -0.0030(9) 0.0072(10)
C20 0.0265(13) 0.0249(9) 0.0320(9) 0.0068(7) 0.0046(8) 0.0096(10)
C21 0.0189(10) 0.0202(8) 0.0227(8) 0.0051(6) 0.0045(7) 0.0079(8)
C22 0.0200(10) 0.0152(8) 0.0220(7) 0.0032(6) 0.0025(6) 0.0050(7)
C23 0.0239(11) 0.0201(8) 0.0229(8) 0.0055(6) 0.0065(7) 0.0099(8)
C24 0.0202(12) 0.0191(8) 0.0231(8) 0.0025(6) 0.0051(7) 0.0090(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.409(2) . ?
O11 C11 1.410(2) . ?
O21 C21 1.242(2) . ?
O22 C21 1.266(2) . ?
O23 C22 1.426(2) . ?
O24 C24 1.249(3) . ?
O25 C24 1.264(2) . ?
N1 C2 1.504(2) . ?
N1 C4 1.489(2) . ?
N11 C12 1.496(2) . ?
N11 C14 1.481(3) . ?
C1 C2 1.533(2) . ?
C1 C5 1.526(2) . ?
C2 C3 1.516(3) . ?
C5 C6 1.389(3) . ?
C5 C10 1.389(3) . ?
C6 C7 1.393(3) . ?
C7 C8 1.387(3) . ?
C8 C9 1.378(3) . ?
C9 C10 1.396(3) . ?
C11 C12 1.540(2) . ?
C11 C15 1.523(2) . ?
C12 C13 1.520(3) . ?
C15 C16 1.396(3) . ?
C15 C20 1.382(3) . ?
C16 C17 1.392(3) . ?
C17 C18 1.378(4) . ?
C18 C19 1.380(4) . ?
C19 C20 1.393(3) . ?
C21 C22 1.544(2) . ?
C22 C23 1.528(3) . ?
C23 C24 1.520(3) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 N1 C2 113.94(15) . . ?
C14 N11 C12 115.28(15) . . ?
O1 C1 C2 107.95(15) . . ?
O1 C1 C5 113.82(15) . . ?
C5 C1 C2 110.96(13) . . ?
N1 C2 C1 108.71(13) . . ?
N1 C2 C3 109.97(15) . . ?
C3 C2 C1 113.25(17) . . ?
C6 C5 C1 119.05(17) . . ?
C6 C5 C10 119.42(17) . . ?
C10 C5 C1 121.52(18) . . ?
C5 C6 C7 120.33(19) . . ?
C8 C7 C6 120.1(2) . . ?
C9 C8 C7 119.65(17) . . ?
C8 C9 C10 120.6(2) . . ?
C5 C10 C9 119.9(2) . . ?
O11 C11 C12 106.96(14) . . ?
O11 C11 C15 112.85(17) . . ?
C15 C11 C12 111.30(14) . . ?
N11 C12 C11 107.10(13) . . ?
N11 C12 C13 110.83(15) . . ?
C13 C12 C11 112.99(17) . . ?
C16 C15 C11 120.06(19) . . ?
C20 C15 C11 121.55(18) . . ?
C20 C15 C16 118.39(18) . . ?
C17 C16 C15 120.5(2) . . ?
C18 C17 C16 120.5(2) . . ?
C17 C18 C19 119.19(19) . . ?
C18 C19 C20 120.6(2) . . ?
C15 C20 C19 120.8(2) . . ?
O21 C21 O22 125.48(17) . . ?
O21 C21 C22 119.58(16) . . ?
O22 C21 C22 114.93(14) . . ?
O23 C22 C21 111.93(13) . . ?
O23 C22 C23 107.75(15) . . ?
C23 C22 C21 110.30(13) . . ?
C24 C23 C22 113.30(14) . . ?
O24 C24 O25 122.83(18) . . ?
O24 C24 C23 117.53(16) . . ?
O25 C24 C23 119.64(18) . . ?
_shelx_res_file
;
pn180914_uo_eph_1_180814_g4_2.res created by SHELXL-2014/7
TITL pn180914_uo_eph_1_180814_g4_2_a.res in P1
REM Old TITL PN180914_UO_Eph_1_180814_G4_2 in P1
REM SHELXT solution in P1
REM R1 0.086, Rweak 0.041, Alpha 0.000, Orientation as input
REM Flack x = 0.015 ( 0.134 ) from Parsons' quotients
REM Formula found by SHELXT: C24 N3 O7
CELL 1.54184 5.821302 7.270884 15.902143 94.7215 96.6693 109.5246
ZERR 1 0.000072 0.000083 0.00013 0.0008 0.0008 0.0011
LATT -1
SFAC C H N O
UNIT 24 38 2 8
L.S. 4
PLAN 20
SIZE 0.014 0.21 0.3
TEMP -113
list 4
fmap 2
acta 139
REM
REM
REM
WGHT 0.047000 0.058000
FVAR 16.55142
O1 4 0.352796 0.743675 0.711740 11.00000 0.03280 0.02298 =
0.03523 0.00892 0.01836 0.01313
AFIX 147
H1 2 0.382821 0.642890 0.694603 11.00000 -1.50000
AFIX 0
O11 4 0.027258 0.278673 0.312831 11.00000 0.03401 0.02554 =
0.02974 0.01100 0.01345 0.01293
AFIX 147
H11 2 0.032161 0.191030 0.343545 11.00000 -1.50000
AFIX 0
O21 4 0.418969 0.400409 0.666155 11.00000 0.03950 0.02785 =
0.02467 0.00601 0.01005 0.01312
O22 4 0.349498 0.135934 0.571877 11.00000 0.03141 0.01847 =
0.02932 0.00641 0.00811 0.00590
O23 4 0.591015 0.652037 0.553130 11.00000 0.01883 0.01627 =
0.03157 0.00240 0.00422 0.00744
AFIX 147
H23 2 0.460689 0.678572 0.547744 11.00000 -1.50000
AFIX 0
O24 4 1.143353 0.638425 0.474093 11.00000 0.01996 0.03285 =
0.03645 0.01005 0.00302 0.00810
O25 4 0.800459 0.605489 0.389072 11.00000 0.02509 0.02915 =
0.02448 0.00871 0.00497 0.01144
O26 4 0.057949 0.021746 0.417624 11.00000 0.05796 0.02142 =
0.04606 0.01141 -0.01620 0.00087
H26A 2 0.162858 0.052677 0.467469 11.00000 0.05026
H26B 2 -0.007875 -0.089684 0.408019 11.00000 0.05196
N1 3 -0.006761 0.928899 0.662869 11.00000 0.02098 0.01835 =
0.02601 0.00573 0.00281 0.00579
AFIX 23
H1A 2 0.138601 0.981198 0.642941 11.00000 -1.20000
H1B 2 -0.100269 0.819286 0.626422 11.00000 -1.20000
AFIX 0
N11 3 0.385051 0.664918 0.333494 11.00000 0.02081 0.02095 =
0.02841 0.00760 0.00543 0.00647
AFIX 23
H11A 2 0.262514 0.638372 0.366242 11.00000 -1.20000
H11B 2 0.509325 0.631489 0.360385 11.00000 -1.20000
AFIX 0
C1 1 0.119443 0.686865 0.738507 11.00000 0.02364 0.01695 =
0.02197 0.00350 0.00479 0.00554
AFIX 13
H1C 2 -0.001839 0.590658 0.691904 11.00000 -1.20000
AFIX 0
C2 1 0.045038 0.869703 0.749499 11.00000 0.02795 0.01859 =
0.02232 0.00502 0.00727 0.00931
AFIX 13
H2 2 -0.110542 0.833909 0.775144 11.00000 -1.20000
AFIX 0
C3 1 0.238537 1.041410 0.807090 11.00000 0.04179 0.01968 =
0.02572 -0.00045 0.00205 0.00828
AFIX 137
H3A 2 0.386376 1.088459 0.779802 11.00000 -1.50000
H3B 2 0.280996 0.998702 0.861806 11.00000 -1.50000
H3C 2 0.173320 1.148063 0.816892 11.00000 -1.50000
AFIX 0
C4 1 -0.136415 1.074133 0.662289 11.00000 0.02876 0.02529 =
0.05065 0.01514 0.00849 0.01294
AFIX 137
H4A 2 -0.183316 1.092664 0.603237 11.00000 -1.50000
H4B 2 -0.026514 1.200081 0.694069 11.00000 -1.50000
H4C 2 -0.284738 1.025233 0.689181 11.00000 -1.50000
AFIX 0
C5 1 0.109599 0.589089 0.819963 11.00000 0.02106 0.01573 =
0.02165 0.00193 0.00519 0.00625
C6 1 -0.117860 0.474541 0.838630 11.00000 0.02359 0.02439 =
0.02813 0.00573 0.00518 0.00819
AFIX 43
H6 2 -0.264328 0.460039 0.801302 11.00000 -1.20000
AFIX 0
C7 1 -0.132239 0.380835 0.911812 11.00000 0.03178 0.02695 =
0.03211 0.00990 0.01267 0.00721
AFIX 43
H7 2 -0.288350 0.303150 0.924379 11.00000 -1.20000
AFIX 0
C8 1 0.081083 0.400811 0.966357 11.00000 0.04681 0.02394 =
0.02302 0.00656 0.00823 0.01584
AFIX 43
H8 2 0.071524 0.337141 1.016329 11.00000 -1.20000
AFIX 0
C9 1 0.306960 0.513501 0.947679 11.00000 0.03658 0.02676 =
0.02742 0.00119 -0.00238 0.01588
AFIX 43
H9 2 0.453220 0.526358 0.984762 11.00000 -1.20000
AFIX 0
C10 1 0.322818 0.608904 0.874791 11.00000 0.02290 0.02111 =
0.02936 0.00225 0.00261 0.00631
AFIX 43
H10 2 0.479192 0.687285 0.862684 11.00000 -1.20000
AFIX 0
C11 1 0.228284 0.322695 0.267089 11.00000 0.02325 0.02422 =
0.02301 0.00720 0.00338 0.01076
AFIX 13
H11C 2 0.373689 0.312890 0.304133 11.00000 -1.20000
AFIX 0
C12 1 0.288105 0.537528 0.249358 11.00000 0.02616 0.02301 =
0.02352 0.00763 0.00638 0.00993
AFIX 13
H12 2 0.420982 0.569109 0.212651 11.00000 -1.20000
AFIX 0
C13 1 0.066635 0.575920 0.204372 11.00000 0.03543 0.02778 =
0.02688 0.00845 0.00063 0.01479
AFIX 137
H13A 2 -0.057336 0.560859 0.242510 11.00000 -1.50000
H13B 2 -0.004526 0.481587 0.152484 11.00000 -1.50000
H13C 2 0.118997 0.710063 0.189122 11.00000 -1.50000
AFIX 0
C14 1 0.478492 0.879427 0.328944 11.00000 0.03864 0.02012 =
0.04807 0.00861 0.00226 0.00497
AFIX 137
H14A 2 0.605397 0.909684 0.291654 11.00000 -1.50000
H14B 2 0.549664 0.950158 0.386292 11.00000 -1.50000
H14C 2 0.342234 0.920350 0.305878 11.00000 -1.50000
AFIX 0
C15 1 0.176791 0.183611 0.184652 11.00000 0.02487 0.02329 =
0.02465 0.00698 0.00320 0.01185
C16 1 0.370313 0.179248 0.141146 11.00000 0.02499 0.03445 =
0.03377 0.00186 0.00404 0.01282
AFIX 43
H16 2 0.533830 0.264103 0.162947 11.00000 -1.20000
AFIX 0
C17 1 0.325581 0.051581 0.066096 11.00000 0.04093 0.04316 =
0.03432 0.00548 0.01170 0.02560
AFIX 43
H17 2 0.458559 0.051041 0.036760 11.00000 -1.20000
AFIX 0
C18 1 0.089939 -0.074052 0.034000 11.00000 0.05107 0.02864 =
0.02892 0.00242 0.00152 0.02088
AFIX 43
H18 2 0.060107 -0.162209 -0.016848 11.00000 -1.20000
AFIX 0
C19 1 -0.102144 -0.070210 0.076637 11.00000 0.03633 0.02329 =
0.03439 0.00180 -0.00300 0.00718
AFIX 43
H19 2 -0.265230 -0.155849 0.054768 11.00000 -1.20000
AFIX 0
C20 1 -0.059028 0.058107 0.151446 11.00000 0.02655 0.02495 =
0.03201 0.00675 0.00455 0.00963
AFIX 43
H20 2 -0.193207 0.059392 0.179974 11.00000 -1.20000
AFIX 0
C21 1 0.424365 0.319828 0.594788 11.00000 0.01887 0.02019 =
0.02271 0.00513 0.00452 0.00793
C22 1 0.534181 0.447673 0.526445 11.00000 0.02002 0.01522 =
0.02204 0.00320 0.00253 0.00496
AFIX 13
H22 2 0.412213 0.407665 0.472668 11.00000 -1.20000
AFIX 0
C23 1 0.772179 0.418027 0.508043 11.00000 0.02389 0.02014 =
0.02290 0.00550 0.00648 0.00987
AFIX 23
H23A 2 0.878957 0.429930 0.562884 11.00000 -1.20000
H23B 2 0.731238 0.283114 0.478631 11.00000 -1.20000
AFIX 0
C24 1 0.914709 0.564672 0.453320 11.00000 0.02015 0.01914 =
0.02306 0.00254 0.00511 0.00901
HKLF 4
REM pn180914_uo_eph_1_180814_g4_2_a.res in P1
REM R1 = 0.0270 for 4709 Fo > 4sig(Fo) and 0.0275 for all 4803 data
REM 322 parameters refined using 3 restraints
END
WGHT 0.0470 0.0580
REM Highest difference peak 0.155, deepest hole -0.182, 1-sigma level 0.031
Q1 1 0.1166 0.6357 0.7817 11.00000 0.05 0.16
Q2 1 0.1884 0.2451 0.2269 11.00000 0.05 0.14
Q3 1 0.3044 0.5413 0.9031 11.00000 0.05 0.13
Q4 1 0.4813 0.3878 0.5604 11.00000 0.05 0.12
Q5 1 0.8409 0.4930 0.4855 11.00000 0.05 0.12
Q6 1 0.6586 0.4350 0.5168 11.00000 0.05 0.11
Q7 1 0.2259 0.6330 0.8573 11.00000 0.05 0.11
Q8 1 0.0824 0.7735 0.7464 11.00000 0.05 0.11
Q9 1 0.1047 0.3448 0.3820 11.00000 0.05 0.11
Q10 1 0.1267 0.9544 0.7814 11.00000 0.05 0.10
Q11 1 1.1294 0.6909 0.5252 11.00000 0.05 0.10
Q12 1 -0.1603 0.0425 0.4453 11.00000 0.05 0.10
Q13 1 -0.0713 -0.0018 0.1124 11.00000 0.05 0.10
Q14 1 0.3560 0.1298 0.5223 11.00000 0.05 0.09
Q15 1 0.5155 0.6587 0.6215 11.00000 0.05 0.09
Q16 1 0.0874 0.4298 0.3774 11.00000 0.05 0.09
Q17 1 0.7193 0.4764 0.3584 11.00000 0.05 0.09
Q18 1 0.7850 0.5504 0.3373 11.00000 0.05 0.09
Q19 1 0.7268 0.6557 0.3152 11.00000 0.05 0.09
Q20 1 0.3570 0.0819 0.1147 11.00000 0.05 0.09
;
_shelx_res_checksum 2821
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6 -4 2 263.582 196.627 71
6 -4 3 12801.7 553.791 46
6 -4 3 15126.6 690.112 73
6 -4 3 14261.9 669.781 72
6 -4 3 13832.9 638.773 71
6 -4 4 24173.2 878.999 46
6 -4 4 27903.5 1037.44 72
6 -4 4 26333.8 1004.21 71
6 -4 5 13775.5 654.853 72
6 -4 5 13493.2 634.061 71
6 -4 6 4655.12 347.966 71
6 -4 7 1907.37 237.638 73
6 -4 7 1856.45 222.595 71
6 -4 8 486.197 123.534 49
6 -4 9 5616.46 249.580 18
6 -3 -11 7016.41 329.206 47
6 -3 -11 7527.21 335.987 76
6 -3 -10 268.832 164.820 47
6 -3 -10 395.868 165.244 76
6 -3 -10 298.394 179.658 50
6 -3 -9 567.670 202.805 50
6 -3 -8 9222.61 496.947 50
6 -3 -7 6348.04 340.759 75
6 -3 -7 8750.22 457.390 50
6 -3 -6 6567.09 368.862 75
6 -3 -6 8277.99 445.019 50
6 -3 -5 34412.2 1262.98 75
6 -3 -5 38034.4 1306.75 50
6 -3 -4 4744.91 345.107 75
6 -3 -4 4591.24 329.082 50
6 -3 -3 9804.08 480.961 73
6 -3 -3 9108.09 464.204 50
6 -3 -2 10478.4 522.271 73
6 -3 -1 8697.30 475.268 73
6 -3 -1 8151.73 442.988 72
6 -3 0 1567.83 269.610 73
6 -3 0 1457.20 239.998 72
6 -3 1 8103.99 484.754 73
6 -3 1 7581.50 459.417 72
6 -3 2 39422.4 1365.98 72
6 -3 2 34201.5 1300.77 71
6 -3 3 37303.6 1316.60 72
6 -3 3 32547.9 1260.35 71
6 -3 4 6925.67 452.778 72
6 -3 4 6682.20 422.807 71
6 -3 5 6814.44 442.048 72
6 -3 5 6014.19 406.605 71
6 -3 6 16094.2 720.115 72
6 -3 6 15440.2 696.407 71
6 -3 7 11016.7 509.119 72
6 -3 7 10413.1 492.212 71
6 -3 9 4957.35 215.653 18
6 -2 -11 13850.4 534.432 76
6 -2 -11 15883.3 605.272 50
6 -2 -10 5288.70 293.603 76
6 -2 -10 6541.51 361.303 50
6 -2 -9 9032.31 472.945 50
6 -2 -8 3626.04 310.908 50
6 -2 -7 3252.36 298.439 50
6 -2 -6 2897.81 282.537 50
6 -2 -5 3102.55 274.641 50
6 -2 -4 2482.56 231.961 75
6 -2 -3 14426.4 620.307 75
6 -2 -1 9705.95 479.807 73
6 -2 0 19120.3 785.223 73
6 -2 1 1990.91 244.388 72
6 -2 2 8182.22 456.402 72
6 -2 3 15888.5 677.647 71
6 -2 4 6675.56 400.836 71
6 -2 5 21.7656 181.637 71
6 -2 6 50.8993 177.083 71
6 -1 -10 23204.2 859.831 50
6 -1 -9 15682.5 651.616 50
6 -1 -8 14764.8 622.641 50
6 -1 -7 5079.24 321.375 50
7 -5 -2 468.553 114.950 46
0 0 0 0.00 0.00 0
TITL PN180914_UO_Eph_1_180814_G4_2 in P1
REM P1 (#1 in standard setting)
CELL 1.54184 5.821302 7.270884 15.902143 94.7215 96.6693 109.5246
ZERR 1.00 0.000072 0.000083 0.000130 0.0008 0.0008 0.0011
LATT -1
SFAC C H N O
UNIT 24.00 38.00 2.00 8.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 13594
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.673
_oxdiff_exptl_absorpt_empirical_full_min 0.681
data_pn180914_uo_eph_1_180814_g5_tart
_audit_creation_date 2018-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number '2014/7'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '2(C10 H16 N O), C4 H4 O6, H2 O'
_chemical_formula_sum 'C24 H38 N2 O9'
_chemical_formula_weight 498.56
_chemical_absolute_configuration rmad
_chemical_melting_point ?
_chemical_oxdiff_formula 'C24 H20 O9 N2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system 'monoclinic'
_space_group_IT_number 4
_space_group_name_H-M_alt 'P 1 21 1'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 6.07189(12)
_cell_length_b 32.9414(4)
_cell_length_c 7.13830(10)
_cell_angle_alpha 90
_cell_angle_beta 114.168(2)
_cell_angle_gamma 90
_cell_volume 1302.63(4)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 17545
_cell_measurement_temperature 159.99(10)
_cell_measurement_theta_max 78.6170
_cell_measurement_theta_min 5.3390
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.808
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.370
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.271
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 536
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 21 0 0.0092
0 -21 0 0.0022
-3 0 -1 0.1436
0 -5 -4 0.1649
4 -3 -1 0.2031
0 4 4 0.1697
-4 2 1 0.1926
-3 5 4 0.2774
1 4 3 0.1727
4 -3 -2 0.2042
_exptl_crystal_size_max 0.476
_exptl_crystal_size_mid 0.346
_exptl_crystal_size_min 0.011
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0005 20.9808 -0.0073 0.6025 0.7625 0.1375
-0.0005 -20.9808 0.0073 -0.6025 -0.7625 -0.1375
-3.0002 0.0060 -0.9972 -0.4677 0.2261 0.8019
0.0038 -5.0420 -3.9978 -0.8903 0.3927 0.0503
4.0024 -3.0324 -1.0024 0.1019 -0.0754 -1.0404
-0.0038 4.0429 3.9981 0.8616 -0.4290 -0.0569
-4.0020 2.0274 0.5028 -0.2239 0.1109 1.0443
-3.0044 5.0537 3.5005 0.5159 -0.2384 0.7412
0.9971 4.0312 3.4973 0.8619 -0.3847 -0.3069
4.0029 -3.0382 -1.5023 0.0085 -0.0036 -1.0301
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0473
_diffrn_reflns_av_unetI/netI 0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 41
_diffrn_reflns_limit_k_min -41
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 31569
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 78.748
_diffrn_reflns_theta_min 5.371
_diffrn_ambient_environment N~2~
_diffrn_ambient_temperature 159.99(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
--------------------------------------------------------------------------
1 \w -66.00 22.00 0.50 1.25 -- -50.46 57.00-180.00 176
2 \w -69.00 -8.00 0.50 5.00 -- -86.25 30.00 -60.00 122
3 \w -102.00 -15.00 0.50 5.00 -- -86.25 60.00 -97.86 174
4 \w -102.00 -15.00 0.50 5.00 -- -86.25 60.00 -15.03 174
5 \w -123.00 -35.00 0.50 1.25 -- -50.46 -57.00-120.00 176
6 \w -123.00 -35.00 0.50 1.25 -- -50.46 -57.00 30.00 176
7 \w -123.00 -35.00 0.50 1.25 -- -50.46 -57.00 -30.00 176
8 \w -123.00 -35.00 0.50 1.25 -- -50.46 -57.00-150.00 176
9 \w 35.00 123.00 0.50 1.25 -- 50.46 57.00 -90.00 176
10 \w 94.00 178.00 0.50 5.00 -- 107.75 30.00 0.00 168
11 \w 96.00 121.00 0.50 5.00 -- 107.75 15.00 30.00 50
12 \w 95.00 165.00 0.50 5.00 -- 107.75 15.00 60.00 140
13 \w 98.00 175.00 0.50 5.00 -- 107.75 15.00 -30.00 154
14 \w 93.00 178.00 0.50 5.00 -- 107.75 57.00-110.49 170
15 \w 72.00 98.00 0.50 5.00 -- 107.75 -59.00 -80.05 52
16 \w 65.00 91.00 0.50 5.00 -- 107.75 -15.00-150.00 52
17 \w 64.00 93.00 0.50 5.00 -- 107.75 -57.00-155.80 58
18 \w 54.00 95.00 0.50 5.00 -- 107.75 -59.00-102.83 82
19 \w 53.00 78.00 0.50 5.00 -- 107.75 -46.00 -32.90 50
20 \w 70.00 95.00 0.50 5.00 -- 107.75 -59.00 23.23 50
21 \w 71.00 99.00 0.50 5.00 -- 107.75 -58.00 47.30 56
22 \w 84.00 118.00 0.50 5.00 -- 107.75 -15.00 90.00 68
23 \w 36.00 124.00 0.50 5.00 -- 107.75 -60.00 -51.42 176
24 \w 47.00 72.00 0.50 5.00 -- 107.75 -46.00-134.53 50
25 \w 34.00 87.00 0.50 5.00 -- 107.75 -53.00-174.09 106
26 \w 36.00 124.00 0.50 5.00 -- 107.75 -60.00-142.49 176
27 \w 35.00 123.00 0.50 1.25 -- 50.46 57.00-120.00 176
28 \w 28.00 123.00 0.50 5.00 -- 107.75 -9.00 39.84 190
29 \w 42.00 68.00 0.50 5.00 -- 107.75 -58.00 47.30 52
30 \w 35.00 96.00 0.50 5.00 -- 107.75 -57.00 92.06 122
31 \w 42.00 83.00 0.50 5.00 -- 107.75 -60.00 178.46 82
32 \w 29.00 69.00 0.50 5.00 -- 107.75 -30.00 150.00 80
33 \w 33.00 82.00 0.50 5.00 -- 107.75 -49.00 60.59 98
34 \w 35.00 99.00 0.50 5.00 -- 107.75 -58.00 138.61 128
35 \w 36.00 124.00 0.50 5.00 -- 107.75 -60.00 77.95 176
36 \w 34.00 91.00 0.50 5.00 -- 107.75 -55.00 26.55 114
37 \w 36.00 124.00 0.50 5.00 -- 107.75 -60.00 110.35 176
38 \w 35.00 98.00 0.50 5.00 -- 107.75 -15.00 30.00 126
39 \w 28.00 124.00 0.50 5.00 -- 107.75 -8.00 159.64 192
40 \w 37.00 81.00 0.50 5.00 -- 107.75 -60.00 160.60 88
41 \w 29.00 54.00 0.50 5.00 -- 107.75 -30.00 120.00 50
42 \w 30.00 68.00 0.50 5.00 -- 107.75 -30.00 30.00 76
43 \w 32.00 69.00 0.50 5.00 -- 107.75 -30.00 0.00 74
44 \w 34.00 71.00 0.50 5.00 -- 107.75 -45.00 -60.00 74
45 \w 29.00 69.00 0.50 5.00 -- 107.75 -30.00-120.00 80
46 \w 38.00 63.00 0.50 5.00 -- 107.75 -57.00-155.80 50
47 \w 35.00 74.00 0.50 5.00 -- 107.75 -45.00-150.00 78
48 \w 35.00 68.00 0.50 5.00 -- 107.75 -30.00-150.00 66
49 \w -158.00 -71.00 0.50 5.00 -- -86.25 -59.00-150.89 174
50 \w -158.00 -71.00 0.50 5.00 -- -86.25 -59.00-132.12 174
51 \w -159.00 -71.00 0.50 5.00 -- -86.25 -58.00-118.94 176
52 \w -158.00 -70.00 0.50 5.00 -- -86.25 -60.00-110.71 176
53 \w -158.00 -71.00 0.50 5.00 -- -86.25 -59.00-139.45 174
54 \w -159.00 -71.00 0.50 5.00 -- -86.25 -58.00-171.53 176
55 \w -158.00 -70.00 0.50 5.00 -- -86.25 -60.00-147.70 176
56 \w -158.00 -70.00 0.50 5.00 -- -86.25 -60.00 171.31 176
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 0.0939548000
_diffrn_orient_matrix_UB_12 0.0287795000
_diffrn_orient_matrix_UB_13 0.1864811000
_diffrn_orient_matrix_UB_21 -0.0274115000
_diffrn_orient_matrix_UB_22 0.0362923000
_diffrn_orient_matrix_UB_23 -0.1440192000
_diffrn_orient_matrix_UB_31 -0.2602706000
_diffrn_orient_matrix_UB_32 0.0065544000
_diffrn_orient_matrix_UB_33 -0.0210994000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage 0.929
_reflns_Friedel_fraction_full 0.950
_reflns_Friedel_fraction_max 0.913
_reflns_number_gt 5091
_reflns_number_total 5216
_reflns_odcompleteness_completeness 93.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 79.66
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.338
_refine_diff_density_min -0.292
_refine_diff_density_rms 0.051
_refine_ls_abs_structure_details
;
Flack x determined using 2347 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.00(7)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.104
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 329
_refine_ls_number_reflns 5216
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0429
_refine_ls_R_factor_gt 0.0422
_refine_ls_restrained_S_all 1.103
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+0.7643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1110
_refine_ls_wR_factor_ref 0.1114
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All N(H,H) groups, H23A of C23, H22 of C22, H20 of C20, H17 of C17, H16 of
C16, H19 of C19, H18 of C18, H11C of C11, H8 of C8, H1C of C1, H2 of C2, H9
of C9, H6 of C6, H12 of C12, H7 of C7, H10 of C10
At 1.5 times of:
All C(H,H,H) groups, H23 of C17, All O(H) groups, All O(H,H) groups
2. Restrained distances
O23-H23
0.86 with sigma of 0.02
3.a Free rotating group:
O27(H27A,H27B)
3.b Ternary CH refined with riding coordinates:
C1(H1C), C2(H2), C11(H11C), C12(H12), C22(H22), C23(H23A)
3.c Secondary CH2 refined with riding coordinates:
N1(H1A,H1B), N11(H11A,H11B)
3.d Aromatic/amide H refined with riding coordinates:
C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16), C17(H17), C18(H18),
C19(H19), C20(H20)
3.e Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
3.f Idealised tetrahedral OH refined as rotating group:
O1(H1), O11(H11), O24(H24)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.7143(4) 0.26054(8) 0.5007(3) 0.0275(5) Uani 1 1 d . . . . .
H1 H 0.6533 0.2708 0.5764 0.041 Uiso 1 1 calc GR . . . .
O11 O 0.6304(5) 0.48531(7) 0.7625(4) 0.0318(6) Uani 1 1 d . . . . .
H11 H 0.6269 0.4651 0.6897 0.048 Uiso 1 1 calc GR . . . .
O21 O 0.5965(5) 0.29635(7) 0.7859(4) 0.0302(5) Uani 1 1 d . . . . .
O22 O 0.7161(4) 0.34984(7) 0.6605(3) 0.0264(5) Uani 1 1 d . . . . .
O23 O 0.5695(5) 0.33470(7) 1.0911(3) 0.0284(5) Uani 1 1 d D . . . .
O24 O 0.1861(4) 0.36478(7) 0.7098(3) 0.0267(5) Uani 1 1 d . . . . .
H24 H 0.0697 0.3696 0.7413 0.040 Uiso 1 1 calc GR . . . .
O25 O 0.4980(4) 0.43635(7) 1.1083(3) 0.0265(5) Uani 1 1 d . . . . .
O26 O 0.1307(4) 0.40866(7) 0.9929(3) 0.0258(5) Uani 1 1 d . . . . .
O27 O 0.6413(6) 0.42735(8) 0.5191(4) 0.0424(7) Uani 1 1 d . . . . .
H27A H 0.5946 0.4304 0.3903 0.064 Uiso 1 1 d G . . . .
H27B H 0.6621 0.4023 0.5487 0.064 Uiso 1 1 d G . . . .
N1 N 1.0461(5) 0.30687(8) 0.3902(4) 0.0226(5) Uani 1 1 d . . . . .
H1A H 0.8853 0.3115 0.3199 0.027 Uiso 1 1 calc R . . . .
H1B H 1.0990 0.3229 0.5040 0.027 Uiso 1 1 calc R . . . .
N11 N 0.9458(5) 0.46709(8) 1.1555(4) 0.0211(5) Uani 1 1 d . . . . .
H11A H 0.7900 0.4587 1.1133 0.025 Uiso 1 1 calc R . . . .
H11B H 1.0210 0.4496 1.1022 0.025 Uiso 1 1 calc R . . . .
C1 C 0.9679(6) 0.25797(9) 0.6105(4) 0.0213(6) Uani 1 1 d . . . . .
H1C H 1.0200 0.2815 0.7074 0.026 Uiso 1 1 calc R . . . .
C2 C 1.0815(6) 0.26317(9) 0.4576(4) 0.0230(6) Uani 1 1 d . . . . .
H2 H 1.2587 0.2579 0.5304 0.028 Uiso 1 1 calc R . . . .
C3 C 0.9789(8) 0.23456(11) 0.2750(5) 0.0333(8) Uani 1 1 d . . . . .
H3A H 0.8087 0.2412 0.1936 0.050 Uiso 1 1 calc GR . . . .
H3B H 0.9921 0.2065 0.3240 0.050 Uiso 1 1 calc GR . . . .
H3C H 1.0696 0.2376 0.1895 0.050 Uiso 1 1 calc GR . . . .
C4 C 1.1722(7) 0.31931(11) 0.2586(5) 0.0315(7) Uani 1 1 d . . . . .
H4A H 1.0964 0.3059 0.1246 0.047 Uiso 1 1 calc GR . . . .
H4B H 1.3425 0.3114 0.3250 0.047 Uiso 1 1 calc GR . . . .
H4C H 1.1608 0.3488 0.2397 0.047 Uiso 1 1 calc GR . . . .
C5 C 1.0473(6) 0.21934(9) 0.7380(5) 0.0238(6) Uani 1 1 d . . . . .
C6 C 0.8791(7) 0.19152(10) 0.7459(5) 0.0313(7) Uani 1 1 d . . . . .
H6 H 0.7124 0.1952 0.6616 0.038 Uiso 1 1 calc R . . . .
C7 C 0.9543(8) 0.15818(11) 0.8773(6) 0.0364(8) Uani 1 1 d . . . . .
H7 H 0.8382 0.1395 0.8829 0.044 Uiso 1 1 calc R . . . .
C8 C 1.1954(8) 0.15214(11) 0.9988(5) 0.0358(8) Uani 1 1 d . . . . .
H8 H 1.2453 0.1294 1.0884 0.043 Uiso 1 1 calc R . . . .
C9 C 1.3644(7) 0.17927(12) 0.9899(6) 0.0374(8) Uani 1 1 d . . . . .
H9 H 1.5312 0.1751 1.0722 0.045 Uiso 1 1 calc R . . . .
C10 C 1.2897(7) 0.21284(11) 0.8599(5) 0.0330(8) Uani 1 1 d . . . . .
H10 H 1.4065 0.2315 0.8549 0.040 Uiso 1 1 calc R . . . .
C11 C 0.8614(6) 0.50329(10) 0.8363(4) 0.0234(6) Uani 1 1 d . . . . .
H11C H 0.9738 0.4841 0.8109 0.028 Uiso 1 1 calc R . . . .
C12 C 0.9472(7) 0.50860(9) 1.0698(5) 0.0263(7) Uani 1 1 d . . . . .
H12 H 1.1160 0.5193 1.1285 0.032 Uiso 1 1 calc R . . . .
C13 C 0.7881(9) 0.53674(11) 1.1285(6) 0.0417(10) Uani 1 1 d . . . . .
H13A H 0.6235 0.5259 1.0753 0.062 Uiso 1 1 calc GR . . . .
H13B H 0.7861 0.5637 1.0697 0.062 Uiso 1 1 calc GR . . . .
H13C H 0.8519 0.5388 1.2784 0.062 Uiso 1 1 calc GR . . . .
C14 C 1.0652(7) 0.46457(11) 1.3838(5) 0.0324(8) Uani 1 1 d . . . . .
H14A H 1.0671 0.4363 1.4268 0.049 Uiso 1 1 calc GR . . . .
H14B H 0.9757 0.4812 1.4430 0.049 Uiso 1 1 calc GR . . . .
H14C H 1.2312 0.4746 1.4318 0.049 Uiso 1 1 calc GR . . . .
C15 C 0.8609(7) 0.54322(10) 0.7289(5) 0.0260(7) Uani 1 1 d . . . . .
C16 C 1.0744(8) 0.56193(12) 0.7525(6) 0.0364(8) Uani 1 1 d . . . . .
H16 H 1.2237 0.5498 0.8386 0.044 Uiso 1 1 calc R . . . .
C17 C 1.0747(9) 0.59814(12) 0.6524(7) 0.0439(10) Uani 1 1 d . . . . .
H17 H 1.2232 0.6106 0.6705 0.053 Uiso 1 1 calc R . . . .
H23 H 0.537(11) 0.3092(9) 1.054(9) 0.066 Uiso 1 1 d DR . . . .
C18 C 0.8589(9) 0.61598(11) 0.5268(6) 0.0439(10) Uani 1 1 d . . . . .
H18 H 0.8580 0.6408 0.4584 0.053 Uiso 1 1 calc R . . . .
C19 C 0.6459(9) 0.59768(12) 0.5015(6) 0.0427(10) Uani 1 1 d . . . . .
H19 H 0.4971 0.6098 0.4147 0.051 Uiso 1 1 calc R . . . .
C20 C 0.6454(8) 0.56152(11) 0.6015(5) 0.0333(8) Uani 1 1 d . . . . .
H20 H 0.4963 0.5492 0.5825 0.040 Uiso 1 1 calc R . . . .
C21 C 0.6422(5) 0.33331(10) 0.7830(4) 0.0204(6) Uani 1 1 d . . . . .
C22 C 0.6050(6) 0.35999(9) 0.9434(4) 0.0220(6) Uani 1 1 d . . . . .
H22 H 0.7526 0.3769 1.0147 0.026 Uiso 1 1 calc R . . . .
C23 C 0.3888(5) 0.38800(9) 0.8364(4) 0.0197(6) Uani 1 1 d . . . . .
H23A H 0.4299 0.4072 0.7470 0.024 Uiso 1 1 calc R . . . .
C24 C 0.3341(5) 0.41289(9) 0.9931(4) 0.0188(6) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0196(12) 0.0377(12) 0.0258(11) -0.0013(9) 0.0099(9) 0.0030(9)
O11 0.0359(15) 0.0346(13) 0.0242(12) -0.0035(9) 0.0114(10) -0.0093(10)
O21 0.0334(14) 0.0268(12) 0.0369(12) -0.0016(9) 0.0208(11) 0.0003(9)
O22 0.0267(13) 0.0320(11) 0.0251(11) -0.0004(8) 0.0154(9) -0.0004(9)
O23 0.0318(14) 0.0350(13) 0.0215(11) 0.0076(9) 0.0139(9) 0.0025(10)
O24 0.0139(11) 0.0417(13) 0.0233(10) -0.0119(9) 0.0065(8) -0.0008(9)
O25 0.0273(13) 0.0335(12) 0.0198(10) -0.0053(8) 0.0105(9) -0.0077(9)
O26 0.0227(13) 0.0320(11) 0.0252(10) -0.0047(9) 0.0122(9) -0.0012(9)
O27 0.068(2) 0.0351(13) 0.0234(11) -0.0004(10) 0.0184(12) -0.0025(13)
N1 0.0207(14) 0.0256(13) 0.0189(11) -0.0001(9) 0.0056(10) 0.0000(10)
N11 0.0204(14) 0.0272(13) 0.0157(11) -0.0013(9) 0.0072(10) 0.0015(10)
C1 0.0199(16) 0.0256(14) 0.0183(13) -0.0019(11) 0.0077(11) 0.0011(11)
C2 0.0235(16) 0.0262(15) 0.0188(13) -0.0001(11) 0.0083(11) 0.0017(12)
C3 0.048(2) 0.0313(17) 0.0243(16) -0.0047(13) 0.0187(15) 0.0000(14)
C4 0.030(2) 0.0414(19) 0.0245(15) 0.0082(13) 0.0124(14) 0.0008(14)
C5 0.0283(18) 0.0245(15) 0.0200(14) -0.0016(11) 0.0113(12) 0.0004(12)
C6 0.036(2) 0.0316(17) 0.0290(16) -0.0009(13) 0.0160(15) -0.0041(14)
C7 0.049(2) 0.0306(18) 0.0343(19) -0.0003(14) 0.0218(17) -0.0120(15)
C8 0.054(2) 0.0277(17) 0.0269(17) 0.0042(13) 0.0174(16) 0.0009(15)
C9 0.032(2) 0.039(2) 0.0327(18) 0.0117(15) 0.0045(15) 0.0029(15)
C10 0.033(2) 0.0317(17) 0.0319(17) 0.0065(14) 0.0108(15) -0.0022(14)
C11 0.0226(17) 0.0294(15) 0.0184(14) -0.0027(11) 0.0087(12) -0.0020(12)
C12 0.0323(19) 0.0250(15) 0.0200(14) -0.0029(11) 0.0092(13) -0.0038(12)
C13 0.070(3) 0.0296(18) 0.0279(17) 0.0001(14) 0.0229(18) 0.0131(17)
C14 0.033(2) 0.043(2) 0.0163(14) 0.0018(13) 0.0055(13) 0.0020(14)
C15 0.031(2) 0.0284(16) 0.0203(14) -0.0020(11) 0.0123(13) -0.0006(12)
C16 0.036(2) 0.042(2) 0.0340(18) 0.0006(15) 0.0168(16) -0.0058(15)
C17 0.058(3) 0.042(2) 0.043(2) -0.0046(17) 0.032(2) -0.0143(19)
C18 0.082(3) 0.0283(18) 0.0337(19) 0.0013(14) 0.036(2) -0.0006(18)
C19 0.063(3) 0.0350(19) 0.0312(18) 0.0059(15) 0.0204(19) 0.0132(18)
C20 0.042(2) 0.0340(18) 0.0258(16) -0.0005(13) 0.0154(15) 0.0035(15)
C21 0.0101(15) 0.0292(15) 0.0204(13) -0.0004(11) 0.0046(11) 0.0018(11)
C22 0.0231(16) 0.0255(14) 0.0199(13) 0.0015(11) 0.0112(12) -0.0020(11)
C23 0.0156(15) 0.0261(14) 0.0169(12) -0.0018(11) 0.0061(10) -0.0002(11)
C24 0.0194(16) 0.0216(13) 0.0171(12) 0.0018(10) 0.0094(11) 0.0002(11)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.8400 . ?
O1 C1 1.416(4) . ?
O11 H11 0.8400 . ?
O11 C11 1.411(4) . ?
O21 C21 1.251(4) . ?
O22 C21 1.258(4) . ?
O23 H23 0.88(3) . ?
O23 C22 1.428(4) . ?
O24 H24 0.8400 . ?
O24 C23 1.416(4) . ?
O25 C24 1.263(4) . ?
O26 C24 1.242(4) . ?
O27 H27A 0.8498 . ?
O27 H27B 0.8497 . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C2 1.505(4) . ?
N1 C4 1.492(4) . ?
N11 H11A 0.9100 . ?
N11 H11B 0.9100 . ?
N11 C12 1.499(4) . ?
N11 C14 1.491(4) . ?
C1 H1C 1.0000 . ?
C1 C2 1.522(4) . ?
C1 C5 1.523(4) . ?
C2 H2 1.0000 . ?
C2 C3 1.520(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.391(5) . ?
C5 C10 1.386(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.394(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.382(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.395(5) . ?
C10 H10 0.9500 . ?
C11 H11C 1.0000 . ?
C11 C12 1.539(4) . ?
C11 C15 1.522(4) . ?
C12 H12 1.0000 . ?
C12 C13 1.516(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.382(5) . ?
C15 C20 1.388(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.391(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.380(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.370(7) . ?
C19 H19 0.9500 . ?
C19 C20 1.389(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.532(4) . ?
C22 H22 1.0000 . ?
C22 C23 1.529(4) . ?
C23 H23A 1.0000 . ?
C23 C24 1.529(4) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 H1 109.5 . . ?
C11 O11 H11 109.5 . . ?
C22 O23 H23 115(4) . . ?
C23 O24 H24 109.5 . . ?
H27A O27 H27B 109.5 . . ?
H1A N1 H1B 107.5 . . ?
C2 N1 H1A 108.5 . . ?
C2 N1 H1B 108.5 . . ?
C4 N1 H1A 108.5 . . ?
C4 N1 H1B 108.5 . . ?
C4 N1 C2 114.9(3) . . ?
H11A N11 H11B 107.6 . . ?
C12 N11 H11A 108.6 . . ?
C12 N11 H11B 108.6 . . ?
C14 N11 H11A 108.6 . . ?
C14 N11 H11B 108.6 . . ?
C14 N11 C12 114.5(2) . . ?
O1 C1 H1C 107.5 . . ?
O1 C1 C2 107.8(2) . . ?
O1 C1 C5 112.8(3) . . ?
C2 C1 H1C 107.5 . . ?
C2 C1 C5 113.4(3) . . ?
C5 C1 H1C 107.5 . . ?
N1 C2 C1 106.8(2) . . ?
N1 C2 H2 108.3 . . ?
N1 C2 C3 111.4(2) . . ?
C1 C2 H2 108.3 . . ?
C3 C2 C1 113.5(3) . . ?
C3 C2 H2 108.3 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C1 121.1(3) . . ?
C10 C5 C1 120.0(3) . . ?
C10 C5 C6 118.8(3) . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.2(3) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.6(3) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.7(3) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 120.1 . . ?
C8 C9 C10 119.9(4) . . ?
C10 C9 H9 120.1 . . ?
C5 C10 C9 120.9(3) . . ?
C5 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
O11 C11 H11C 108.4 . . ?
O11 C11 C12 107.2(3) . . ?
O11 C11 C15 112.2(3) . . ?
C12 C11 H11C 108.4 . . ?
C15 C11 H11C 108.4 . . ?
C15 C11 C12 112.2(2) . . ?
N11 C12 C11 106.4(2) . . ?
N11 C12 H12 109.2 . . ?
N11 C12 C13 109.5(3) . . ?
C11 C12 H12 109.2 . . ?
C13 C12 C11 113.4(3) . . ?
C13 C12 H12 109.2 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N11 C14 H14A 109.5 . . ?
N11 C14 H14B 109.5 . . ?
N11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C11 121.1(3) . . ?
C16 C15 C20 118.1(3) . . ?
C20 C15 C11 120.8(3) . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121.2(4) . . ?
C17 C16 H16 119.4 . . ?
C16 C17 H17 120.1 . . ?
C18 C17 C16 119.9(4) . . ?
C18 C17 H17 120.1 . . ?
C17 C18 H18 120.3 . . ?
C19 C18 C17 119.5(4) . . ?
C19 C18 H18 120.3 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.7(4) . . ?
C20 C19 H19 119.7 . . ?
C15 C20 C19 120.6(4) . . ?
C15 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
O21 C21 O22 125.3(3) . . ?
O21 C21 C22 116.4(3) . . ?
O22 C21 C22 118.4(3) . . ?
O23 C22 C21 109.3(2) . . ?
O23 C22 H22 108.9 . . ?
O23 C22 C23 111.3(3) . . ?
C21 C22 H22 108.9 . . ?
C23 C22 C21 109.4(2) . . ?
C23 C22 H22 108.9 . . ?
O24 C23 C22 109.7(2) . . ?
O24 C23 H23A 108.3 . . ?
O24 C23 C24 111.3(2) . . ?
C22 C23 H23A 108.3 . . ?
C22 C23 C24 111.0(2) . . ?
C24 C23 H23A 108.3 . . ?
O25 C24 C23 117.1(3) . . ?
O26 C24 O25 126.0(3) . . ?
O26 C24 C23 116.9(3) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 70.6(3) . . . . ?
O1 C1 C2 C3 -52.6(3) . . . . ?
O1 C1 C5 C6 -2.5(4) . . . . ?
O1 C1 C5 C10 -177.9(3) . . . . ?
O11 C11 C12 N11 58.1(3) . . . . ?
O11 C11 C12 C13 -62.4(4) . . . . ?
O11 C11 C15 C16 -168.5(3) . . . . ?
O11 C11 C15 C20 10.4(4) . . . . ?
O21 C21 C22 O23 11.4(4) . . . . ?
O21 C21 C22 C23 -110.6(3) . . . . ?
O22 C21 C22 O23 -168.3(3) . . . . ?
O22 C21 C22 C23 69.7(4) . . . . ?
O23 C22 C23 O24 -68.6(3) . . . . ?
O23 C22 C23 C24 54.9(3) . . . . ?
O24 C23 C24 O25 -176.7(2) . . . . ?
O24 C23 C24 O26 2.1(4) . . . . ?
C1 C5 C6 C7 -174.4(3) . . . . ?
C1 C5 C10 C9 175.0(3) . . . . ?
C2 C1 C5 C6 -125.4(3) . . . . ?
C2 C1 C5 C10 59.2(4) . . . . ?
C4 N1 C2 C1 172.8(3) . . . . ?
C4 N1 C2 C3 -62.7(4) . . . . ?
C5 C1 C2 N1 -163.8(2) . . . . ?
C5 C1 C2 C3 73.0(3) . . . . ?
C5 C6 C7 C8 -0.7(5) . . . . ?
C6 C5 C10 C9 -0.6(5) . . . . ?
C6 C7 C8 C9 -0.3(6) . . . . ?
C7 C8 C9 C10 0.8(6) . . . . ?
C8 C9 C10 C5 -0.4(6) . . . . ?
C10 C5 C6 C7 1.1(5) . . . . ?
C11 C15 C16 C17 179.1(3) . . . . ?
C11 C15 C20 C19 -179.1(3) . . . . ?
C12 C11 C15 C16 70.7(4) . . . . ?
C12 C11 C15 C20 -110.4(3) . . . . ?
C14 N11 C12 C11 169.5(3) . . . . ?
C14 N11 C12 C13 -67.6(4) . . . . ?
C15 C11 C12 N11 -178.3(3) . . . . ?
C15 C11 C12 C13 61.2(4) . . . . ?
C15 C16 C17 C18 0.0(6) . . . . ?
C16 C15 C20 C19 -0.2(5) . . . . ?
C16 C17 C18 C19 -0.2(6) . . . . ?
C17 C18 C19 C20 0.2(6) . . . . ?
C18 C19 C20 C15 -0.1(6) . . . . ?
C20 C15 C16 C17 0.2(5) . . . . ?
C21 C22 C23 O24 52.3(3) . . . . ?
C21 C22 C23 C24 175.7(2) . . . . ?
C22 C23 C24 O25 60.8(3) . . . . ?
C22 C23 C24 O26 -120.4(3) . . . . ?
_shelx_res_file
;
pn180914_uo_eph_1_180814_g5_tart.res created by SHELXL-2014/7
TITL PN180914_UO_Eph_1_180814_G5_tart in P21 #4
REM reset to P21 #4
CELL 1.54184 6.071889 32.941441 7.138305 90 114.1682 90
ZERR 2 0.000121 0.000373 0.000104 0 0.002 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O
UNIT 48 76 4 18
DFIX 0.86 O23 H23
L.S. 4
PLAN 8
TEMP -113
BOND $H
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.048100 0.764300
FVAR 9.60023
O1 4 0.714273 0.260544 0.500678 11.00000 0.01962 0.03767 =
0.02579 -0.00130 0.00995 0.00301
AFIX 147
H1 2 0.653324 0.270756 0.576350 11.00000 -1.50000
AFIX 0
O11 4 0.630400 0.485312 0.762483 11.00000 0.03586 0.03458 =
0.02420 -0.00353 0.01143 -0.00934
AFIX 147
H11 2 0.626945 0.465084 0.689680 11.00000 -1.50000
AFIX 0
O21 4 0.596532 0.296353 0.785870 11.00000 0.03338 0.02678 =
0.03685 -0.00164 0.02079 0.00032
O22 4 0.716066 0.349837 0.660455 11.00000 0.02667 0.03199 =
0.02513 -0.00040 0.01540 -0.00039
O23 4 0.569450 0.334698 1.091144 11.00000 0.03179 0.03503 =
0.02147 0.00758 0.01392 0.00251
O24 4 0.186072 0.364780 0.709844 11.00000 0.01394 0.04167 =
0.02329 -0.01188 0.00648 -0.00076
AFIX 147
H24 2 0.069674 0.369628 0.741332 11.00000 -1.50000
AFIX 0
O25 4 0.498007 0.436349 1.108343 11.00000 0.02728 0.03349 =
0.01975 -0.00525 0.01053 -0.00770
O26 4 0.130735 0.408663 0.992854 11.00000 0.02266 0.03196 =
0.02519 -0.00468 0.01218 -0.00124
AFIX 6
O27 4 0.641316 0.427346 0.519080 11.00000 0.06826 0.03507 =
0.02344 -0.00045 0.01838 -0.00250
H27A 2 0.594584 0.430398 0.390301 11.00000 -1.50000
H27B 2 0.662090 0.402256 0.548724 11.00000 -1.50000
AFIX 0
N1 3 1.046145 0.306869 0.390200 11.00000 0.02072 0.02560 =
0.01890 -0.00013 0.00558 -0.00003
AFIX 23
H1A 2 0.885278 0.311524 0.319872 11.00000 -1.20000
H1B 2 1.099010 0.322904 0.503966 11.00000 -1.20000
AFIX 0
N11 3 0.945775 0.467090 1.155484 11.00000 0.02036 0.02724 =
0.01569 -0.00134 0.00722 0.00147
AFIX 23
H11A 2 0.789961 0.458741 1.113281 11.00000 -1.20000
H11B 2 1.021016 0.449594 1.102171 11.00000 -1.20000
AFIX 0
C1 1 0.967864 0.257972 0.610544 11.00000 0.01993 0.02561 =
0.01832 -0.00190 0.00773 0.00108
AFIX 13
H1C 2 1.019972 0.281501 0.707437 11.00000 -1.20000
AFIX 0
C2 1 1.081518 0.263171 0.457564 11.00000 0.02348 0.02621 =
0.01883 -0.00011 0.00829 0.00166
AFIX 13
H2 2 1.258712 0.257903 0.530442 11.00000 -1.20000
AFIX 0
C3 1 0.978866 0.234560 0.274961 11.00000 0.04813 0.03128 =
0.02426 -0.00469 0.01868 -0.00004
AFIX 137
H3A 2 0.808737 0.241159 0.193598 11.00000 -1.50000
H3B 2 0.992102 0.206503 0.324049 11.00000 -1.50000
H3C 2 1.069577 0.237572 0.189509 11.00000 -1.50000
AFIX 0
C4 1 1.172246 0.319312 0.258600 11.00000 0.02980 0.04138 =
0.02445 0.00818 0.01241 0.00076
AFIX 137
H4A 2 1.096355 0.305928 0.124634 11.00000 -1.50000
H4B 2 1.342465 0.311360 0.325034 11.00000 -1.50000
H4C 2 1.160752 0.348823 0.239686 11.00000 -1.50000
AFIX 0
C5 1 1.047317 0.219340 0.738026 11.00000 0.02830 0.02449 =
0.02001 -0.00158 0.01134 0.00035
C6 1 0.879092 0.191518 0.745935 11.00000 0.03595 0.03161 =
0.02895 -0.00088 0.01604 -0.00412
AFIX 43
H6 2 0.712447 0.195242 0.661608 11.00000 -1.20000
AFIX 0
C7 1 0.954324 0.158180 0.877256 11.00000 0.04902 0.03056 =
0.03427 -0.00033 0.02177 -0.01195
AFIX 43
H7 2 0.838192 0.139461 0.882925 11.00000 -1.20000
AFIX 0
C8 1 1.195396 0.152136 0.998817 11.00000 0.05377 0.02766 =
0.02694 0.00419 0.01736 0.00090
AFIX 43
H8 2 1.245325 0.129414 1.088420 11.00000 -1.20000
AFIX 0
C9 1 1.364439 0.179268 0.989925 11.00000 0.03189 0.03901 =
0.03272 0.01168 0.00449 0.00289
AFIX 43
H9 2 1.531210 0.175059 1.072173 11.00000 -1.20000
AFIX 0
C10 1 1.289689 0.212844 0.859939 11.00000 0.03294 0.03166 =
0.03186 0.00649 0.01077 -0.00215
AFIX 43
H10 2 1.406455 0.231502 0.854920 11.00000 -1.20000
AFIX 0
C11 1 0.861359 0.503286 0.836320 11.00000 0.02257 0.02936 =
0.01844 -0.00269 0.00872 -0.00197
AFIX 13
H11C 2 0.973786 0.484102 0.810856 11.00000 -1.20000
AFIX 0
C12 1 0.947195 0.508601 1.069836 11.00000 0.03230 0.02500 =
0.01996 -0.00288 0.00917 -0.00377
AFIX 13
H12 2 1.116037 0.519341 1.128470 11.00000 -1.20000
AFIX 0
C13 1 0.788093 0.536738 1.128512 11.00000 0.07021 0.02964 =
0.02791 0.00008 0.02293 0.01307
AFIX 137
H13A 2 0.623528 0.525859 1.075334 11.00000 -1.50000
H13B 2 0.786051 0.563692 1.069719 11.00000 -1.50000
H13C 2 0.851871 0.538850 1.278407 11.00000 -1.50000
AFIX 0
C14 1 1.065160 0.464571 1.383830 11.00000 0.03328 0.04307 =
0.01634 0.00184 0.00554 0.00202
AFIX 137
H14A 2 1.067055 0.436271 1.426797 11.00000 -1.50000
H14B 2 0.975731 0.481169 1.443043 11.00000 -1.50000
H14C 2 1.231188 0.474618 1.431783 11.00000 -1.50000
AFIX 0
C15 1 0.860911 0.543224 0.728857 11.00000 0.03116 0.02842 =
0.02027 -0.00201 0.01227 -0.00062
C16 1 1.074403 0.561928 0.752468 11.00000 0.03620 0.04153 =
0.03397 0.00059 0.01681 -0.00575
AFIX 43
H16 2 1.223714 0.549828 0.838634 11.00000 -1.20000
AFIX 0
C17 1 1.074705 0.598140 0.652404 11.00000 0.05754 0.04223 =
0.04310 -0.00461 0.03209 -0.01431
AFIX 43
H17 2 1.223243 0.610576 0.670510 11.00000 -1.20000
AFIX 0
H23 2 0.536780 0.309201 1.053543 11.00000 -1.50000
C18 1 0.858917 0.615978 0.526788 11.00000 0.08170 0.02825 =
0.03371 0.00133 0.03582 -0.00056
AFIX 43
H18 2 0.858038 0.640753 0.458369 11.00000 -1.20000
AFIX 0
C19 1 0.645911 0.597678 0.501500 11.00000 0.06295 0.03504 =
0.03121 0.00594 0.02040 0.01321
AFIX 43
H19 2 0.497074 0.609839 0.414725 11.00000 -1.20000
AFIX 0
C20 1 0.645431 0.561525 0.601474 11.00000 0.04164 0.03397 =
0.02576 -0.00046 0.01537 0.00355
AFIX 43
H20 2 0.496309 0.549206 0.582522 11.00000 -1.20000
AFIX 0
C21 1 0.642180 0.333309 0.782951 11.00000 0.01009 0.02918 =
0.02039 -0.00037 0.00461 0.00178
C22 1 0.604971 0.359988 0.943408 11.00000 0.02313 0.02547 =
0.01988 0.00149 0.01121 -0.00201
AFIX 13
H22 2 0.752568 0.376926 1.014681 11.00000 -1.20000
AFIX 0
C23 1 0.388808 0.388000 0.836430 11.00000 0.01560 0.02606 =
0.01690 -0.00176 0.00615 -0.00025
AFIX 13
H23A 2 0.429887 0.407203 0.747026 11.00000 -1.20000
AFIX 0
C24 1 0.334107 0.412888 0.993065 11.00000 0.01944 0.02162 =
0.01714 0.00184 0.00938 0.00021
HKLF 4
REM PN180914_UO_Eph_1_180814_G5_tart in P21 #4
REM R1 = 0.0422 for 5091 Fo > 4sig(Fo) and 0.0429 for all 5216 data
REM 329 parameters refined using 2 restraints
END
WGHT 0.0481 0.7644
REM Highest difference peak 0.338, deepest hole -0.292, 1-sigma level 0.051
Q1 1 0.1930 0.3349 0.7198 11.00000 0.05 0.34
Q2 1 0.7109 0.2896 0.5041 11.00000 0.05 0.25
Q3 1 0.1429 0.3794 0.9908 11.00000 0.05 0.25
Q4 1 0.7341 0.3799 0.6781 11.00000 0.05 0.24
Q5 1 0.4948 0.4649 1.1017 11.00000 0.05 0.23
Q6 1 0.7056 0.2318 0.5018 11.00000 0.05 0.22
Q7 1 0.1418 0.4376 1.0038 11.00000 0.05 0.22
Q8 1 0.5246 0.3844 0.8942 11.00000 0.05 0.21
;
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-6 -1 6 7250.13 392.554 26
-6 -1 6 4837.10 278.077 4
-6 -1 5 11569.1 429.946 18
-6 -1 5 8993.07 331.050 4
-6 -1 -1 8217.43 315.082 35
-6 -1 -2 4366.17 171.170 35
-6 0 8 450.407 77.0980 26
-6 0 8 509.987 77.3376 18
-6 0 7 875.970 181.722 26
-6 0 7 672.941 128.007 4
-6 0 6 17970.9 668.170 26
-6 0 6 19456.1 588.747 4
-6 0 5 2487.01 294.365 26
-6 0 5 2949.62 207.624 4
-6 0 -1 7264.35 290.868 35
-6 0 -2 1409.46 105.767 35
-6 1 8 1045.64 82.4933 18
-6 1 8 871.828 117.600 15
-6 1 7 1560.81 187.354 26
-6 1 7 1900.97 182.922 18
-6 1 6 2272.74 284.686 26
-6 1 6 5624.62 255.775 4
-6 1 5 8855.06 490.699 26
-6 1 5 17464.3 518.598 18
-6 1 -1 8052.43 310.631 35
-6 1 -2 3754.64 154.504 35
-6 2 8 2056.48 98.7462 18
-6 2 8 2265.09 126.955 15
-6 2 7 805.478 169.931 26
-6 2 7 602.470 127.063 4
-6 2 7 1005.60 174.564 18
-6 2 6 3783.35 288.834 26
-6 2 6 3464.33 209.524 4
-6 2 5 15484.1 639.632 26
-6 2 5 22555.2 639.056 18
-6 2 -1 3392.58 207.887 35
-6 2 -2 7902.17 248.674 35
-6 3 8 2017.86 104.325 26
-6 3 8 2616.87 107.031 18
-6 3 7 1210.49 167.233 26
-6 3 7 1041.66 130.680 4
-6 3 7 1263.97 168.896 18
-6 3 6 2803.80 259.540 26
-6 3 6 3002.89 192.757 4
-6 3 5 6568.01 399.783 26
-6 3 5 14858.7 442.872 18
-6 4 7 623.443 146.721 26
-6 4 7 715.538 154.520 18
-6 4 6 2392.80 236.534 26
-6 4 6 3798.77 253.334 18
-6 4 5 5926.76 346.009 26
-6 4 5 9145.67 348.119 18
-6 5 7 1517.48 165.857 26
-6 5 7 4404.46 203.798 18
-6 5 6 1617.29 205.265 26
-6 5 6 1858.39 206.295 18
-6 5 5 4766.49 274.888 18
-6 6 7 9035.37 309.177 18
-6 6 7 9931.34 340.343 15
-6 6 6 962.528 182.929 26
-6 6 6 1252.02 194.639 18
-6 6 5 6838.14 310.606 18
-6 7 7 1617.77 144.292 18
-6 7 7 1827.60 214.935 15
-6 7 6 1950.33 184.642 26
-6 7 6 2312.94 194.463 18
-6 7 5 3550.04 227.877 18
-6 7 5 3880.24 284.548 15
-6 8 7 4342.11 180.238 18
-6 8 7 4019.16 223.976 15
-6 8 6 465.824 148.096 26
-6 8 6 500.280 164.472 23
-6 8 5 5293.59 256.524 18
-6 8 5 5199.41 295.231 15
-6 9 7 3512.57 163.529 23
-6 9 7 3661.23 207.652 15
-6 9 6 7256.43 281.894 23
-6 9 6 6834.02 286.372 18
-6 9 6 7605.68 328.292 15
-6 9 5 5435.96 250.708 18
-6 9 5 5631.02 293.355 15
-6 10 7 2907.05 156.843 23
-6 10 7 3166.37 198.802 15
-6 10 6 442.621 155.181 23
-6 10 6 768.118 138.631 18
-6 10 6 778.704 220.427 15
-6 10 5 1446.31 154.794 18
-6 10 5 1583.67 228.504 15
6 10 0 3261.40 310.899 56
-6 11 7 689.873 116.299 23
-6 11 7 739.466 174.115 15
-6 11 6 7052.32 275.591 23
-6 11 6 7075.83 311.712 15
-6 11 5 3677.34 266.857 15
6 11 -4 14834.6 492.559 52
-6 12 7 2050.96 132.174 23
-6 12 7 1993.91 163.610 15
-6 12 6 792.310 153.345 23
-6 12 6 683.966 214.346 15
-6 12 5 20546.2 618.066 23
-6 12 5 21851.2 633.545 15
6 12 -4 4213.33 242.910 52
-6 13 7 3373.48 154.040 23
-6 13 7 3741.99 177.414 15
-6 13 6 6014.45 250.414 23
-6 13 6 6287.93 286.100 15
-6 13 5 7685.65 314.778 23
-6 13 5 8625.69 335.079 15
6 13 -4 3818.87 215.323 52
6 13 -4 3148.60 209.533 51
6 13 -2 9260.30 383.693 55
-6 14 7 5835.51 203.563 23
-6 14 7 6365.54 219.219 15
6 14 -6 1754.57 181.811 52
-6 14 6 1992.35 169.596 23
-6 14 6 2201.19 200.477 15
6 14 -5 19050.4 603.024 52
-6 14 5 19620.1 585.492 23
-6 14 5 19950.9 581.011 15
6 14 -4 13625.7 445.421 51
6 14 -3 696.863 166.840 50
6 14 -2 10905.5 422.261 55
-6 15 7 14181.0 397.837 15
-6 15 6 5551.92 231.516 23
-6 15 6 5498.45 245.045 15
6 15 -5 1720.95 177.834 52
-6 15 5 1680.07 190.837 23
-6 15 5 1824.61 212.024 15
6 15 -4 425.929 150.987 51
6 15 -3 1922.19 192.753 50
6 15 -2 7294.55 344.382 55
6 15 -2 6975.78 340.608 49
6 15 0 1095.80 248.009 56
-6 16 6 4371.54 209.673 23
-6 16 6 4527.59 227.660 15
6 16 -5 6040.75 259.907 52
-6 16 5 6677.85 281.144 23
6 16 -4 9805.24 349.334 51
6 16 -3 519.849 172.207 50
6 16 -2 16619.2 544.397 55
6 16 -2 14902.0 540.987 49
6 16 -1 711.111 225.403 54
6 16 0 1083.46 239.090 56
-6 17 6 9929.72 326.897 23
6 17 -5 339.157 138.533 52
6 17 -5 511.638 144.113 51
-6 17 5 60.1196 168.068 23
6 17 -4 3207.18 204.543 51
6 17 -3 3361.93 229.335 53
6 17 -3 3237.99 223.654 50
6 17 -2 2254.60 232.887 55
6 17 -2 2414.23 238.793 49
6 17 -1 1633.10 237.420 54
-6 18 6 4660.10 205.661 23
6 18 -5 1091.71 142.237 52
6 18 -5 806.545 146.205 51
-6 18 5 716.486 178.624 23
6 18 -4 1014.94 158.984 51
6 18 -4 1174.89 173.866 50
6 18 -3 5562.27 282.668 53
6 18 -3 5808.79 279.604 50
6 18 -2 1982.83 223.842 55
6 18 -2 1606.99 224.717 49
6 18 -1 2886.07 258.438 54
-6 19 6 4255.00 185.509 23
-6 19 5 6207.92 267.415 23
6 19 -4 3374.87 195.280 51
6 19 -4 3144.40 210.093 50
6 19 -3 953.787 187.408 53
6 19 -3 875.347 173.279 50
6 19 -2 2015.26 224.175 55
6 19 -2 1785.54 223.215 49
6 19 -1 2776.12 248.758 54
-6 20 6 2499.48 139.841 23
-6 20 5 379.938 160.107 23
6 20 -4 1853.18 181.356 50
6 20 -3 8439.48 367.699 55
6 20 -3 9260.17 362.254 53
6 20 -2 1170.78 202.675 55
6 20 -2 1176.74 204.233 49
-6 21 5 1922.55 173.651 23
6 21 -4 562.876 153.151 53
6 21 -4 246.438 148.615 50
6 21 -3 1923.95 202.833 55
6 21 -3 1671.31 193.735 53
6 21 -3 1827.18 198.848 49
-6 22 5 217.966 138.865 23
6 22 -3 1895.66 191.985 55
6 22 -3 1434.18 185.395 49
0 0 0 0.00 0.00 0
TITL PN180914_UO_Eph_1_180814_G5_tart in P2(1)
REM P2(1) (#4 in standard setting)
CELL 1.54184 6.071889 32.941441 7.138305 90.0000 114.1682 90.0000
ZERR 2.00 0.000121 0.000373 0.000104 0.0000 0.0020 0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C H N O
UNIT 48.00 40.00 4.00 18.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 18398
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.743
_oxdiff_exptl_absorpt_empirical_full_min 0.713
data_pn180914_uo_eph_2_180814_c6_scr2
_audit_creation_date 2018-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number '2014/7'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C10 H16 N O, N O3'
_chemical_formula_sum 'C10 H16 N2 O4'
_chemical_formula_weight 228.25
_chemical_absolute_configuration rm
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system 'monoclinic'
_space_group_IT_number 4
_space_group_name_H-M_alt 'P 1 21 1'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 6.0401(3)
_cell_length_b 29.3553(8)
_cell_length_c 7.3828(3)
_cell_angle_alpha 90
_cell_angle_beta 112.806(5)
_cell_angle_gamma 90
_cell_volume 1206.70(9)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 5146
_cell_measurement_temperature 159.99(10)
_cell_measurement_theta_max 76.7640
_cell_measurement_theta_min 6.0240
_shelx_estimated_absorpt_T_max 0.992
_shelx_estimated_absorpt_T_min 0.737
_exptl_absorpt_coefficient_mu 0.819
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.811
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.256
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 488
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -9 -4 0.0184
0 9 4 0.0354
4 1 -1 0.1305
-4 1 2 0.2575
0 19 0 0.0010
0 -19 0 0.0092
_exptl_crystal_size_max 0.396
_exptl_crystal_size_mid 0.066
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0460
_diffrn_reflns_av_unetI/netI 0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -4
_diffrn_reflns_limit_k_max 36
_diffrn_reflns_limit_k_min -36
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 12312
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 77.052
_diffrn_reflns_theta_min 6.030
_diffrn_ambient_temperature 160.15
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
--------------------------------------------------------------------------
1 \w 140.00 169.00 0.50 32.00 -- 104.56 30.00 -60.00 58
2 \w 147.00 176.00 0.50 32.00 -- 104.56 15.00 60.00 58
3 \w 96.00 129.00 0.50 32.00 -- 104.56 15.00 60.00 66
4 \w 92.00 154.00 0.50 32.00 -- 104.56 15.00 90.00 124
5 \w 98.00 137.00 0.50 32.00 -- 104.56 30.00 -60.00 78
6 \w 92.00 178.00 0.50 32.00 -- 104.56 15.00-150.00 172
7 \w 83.00 112.00 0.50 32.00 -- 104.56 -60.00-106.07 58
8 \w 82.00 109.00 0.50 32.00 -- 104.56 -60.00-125.32 54
9 \w 71.00 111.00 0.50 32.00 -- 104.56 -60.00 -29.27 80
10 \w 65.00 90.00 0.50 32.00 -- 104.56 -59.00 25.05 50
11 \w 63.00 90.00 0.50 32.00 -- 104.56 -60.00 64.66 54
12 \w 74.00 100.00 0.50 32.00 -- 104.56 -59.00 120.71 52
13 \w 76.00 104.00 0.50 32.00 -- 104.56 -60.00 157.05 56
14 \w 51.00 96.00 0.50 32.00 -- 104.56 -60.00 177.08 90
15 \w 46.00 71.00 0.50 32.00 -- 104.56 -59.00 74.38 50
16 \w 46.00 83.00 0.50 32.00 -- 104.56 -60.00 49.91 74
17 \w 33.00 68.00 0.50 32.00 -- 104.56 -60.00 -29.27 70
18 \w 26.00 69.00 0.50 32.00 -- 104.56 -30.00 30.00 86
19 \w 33.00 92.00 0.50 32.00 -- 104.56 -59.00 102.56 118
20 \w 33.00 83.00 0.50 32.00 -- 104.56 -59.00 2.26 100
21 \w 28.00 63.00 0.50 32.00 -- 104.56 -30.00 120.00 70
22 \w 7.00 34.00 0.50 8.00 -- 2.14 57.00 60.00 54
23 \w 36.00 67.00 0.50 8.00 -- 2.14 57.00 60.00 62
24 \w 34.00 117.00 0.50 32.00 -- 104.56 -60.00-153.60 166
25 \w -66.00 17.00 0.50 8.00 -- 2.14 -57.00 60.00 166
26 \w -66.00 -9.00 0.50 32.00 -- -86.25 30.00 -90.00 114
27 \w -73.00 -43.00 0.50 32.00 -- -86.25 60.00 7.06 60
28 \w -68.00 -31.00 0.50 32.00 -- -86.25 30.00 0.00 74
29 \w -73.00 -16.00 0.50 32.00 -- -86.25 60.00 -76.86 114
30 \w -73.00 -47.00 0.50 32.00 -- -86.25 59.00-133.04 52
31 \w -75.00 13.00 0.50 8.00 -- 2.14 -19.00-180.00 176
32 \w -96.00 -21.00 0.50 32.00 -- -86.25 60.00 67.78 150
33 \w -101.00 -57.00 0.50 32.00 -- -86.25 60.00 175.53 88
34 \w -118.00 -85.00 0.50 32.00 -- -86.25 -58.00-123.65 66
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source ?
_reflns_Friedel_coverage 0.901
_reflns_Friedel_fraction_full 0.943
_reflns_Friedel_fraction_max 0.877
_reflns_number_gt 3727
_reflns_number_total 4637
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.633
_refine_diff_density_min -0.300
_refine_diff_density_rms 0.139
_refine_ls_abs_structure_details
;
Flack x determined using 1465 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.1(2)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.092
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 295
_refine_ls_number_reflns 4637
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0787
_refine_ls_R_factor_gt 0.0676
_refine_ls_restrained_S_all 1.092
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1253P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1823
_refine_ls_wR_factor_ref 0.1902
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H,H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
O15 \\sim O16 \\sim O17: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
3.a Ternary CH refined with riding coordinates:
C1(H1C), C2(H2), C11(H11C), C12(H12)
3.b Secondary CH2 refined with riding coordinates:
N1(H1A,H1B), N11(H11A,H11B)
3.c Aromatic/amide H refined with riding coordinates:
C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16), C17(H17), C18(H18),
C19(H19), C20(H20)
3.d Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
3.e Idealised tetrahedral OH refined as rotating group:
O1(H1), O11(H11)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.4645(8) 0.40974(12) 0.6330(6) 0.0511(9) Uani 1 1 d . . . . .
H1 H 0.4437 0.4375 0.6035 0.077 Uiso 1 1 calc GR . . . .
O11 O 1.0541(7) 0.58742(12) 0.8206(6) 0.0512(9) Uani 1 1 d . . . . .
H11 H 1.0570 0.5591 0.8384 0.077 Uiso 1 1 calc GR . . . .
O12 O 0.4335(7) 0.49914(13) 0.5078(6) 0.0562(9) Uani 1 1 d . . . . .
O13 O 0.2075(8) 0.55884(13) 0.4450(7) 0.0603(11) Uani 1 1 d . . . . .
O14 O 0.0677(8) 0.49420(15) 0.4881(7) 0.0653(11) Uani 1 1 d . . . . .
O15 O 0.9936(8) 0.43770(13) 1.0100(7) 0.0601(10) Uani 1 1 d . U . . .
O16 O 1.1647(7) 0.49810(13) 0.9579(6) 0.0568(9) Uani 1 1 d . U . . .
O17 O 0.8092(8) 0.50216(15) 0.9638(7) 0.0652(11) Uani 1 1 d . U . . .
N1 N 0.5062(9) 0.42691(14) 1.0175(6) 0.0449(10) Uani 1 1 d . . . . .
H1A H 0.6238 0.4358 0.9769 0.054 Uiso 1 1 calc R . . . .
H1B H 0.3904 0.4488 0.9795 0.054 Uiso 1 1 calc R . . . .
N11 N 0.7159(8) 0.56996(14) 0.4439(6) 0.0443(9) Uani 1 1 d . . . . .
H11A H 0.8717 0.5612 0.4799 0.053 Uiso 1 1 calc R . . . .
H11B H 0.6410 0.5482 0.4876 0.053 Uiso 1 1 calc R . . . .
N12 N 0.2327(8) 0.51762(14) 0.4790(6) 0.0453(10) Uani 1 1 d . . . . .
N13 N 0.9878(8) 0.47920(16) 0.9788(6) 0.0477(10) Uani 1 1 d . . . . .
C1 C 0.2821(9) 0.39444(16) 0.6945(7) 0.0436(10) Uani 1 1 d . . . . .
H1C H 0.1626 0.4195 0.6741 0.052 Uiso 1 1 calc R . . . .
C2 C 0.3988(10) 0.38326(15) 0.9147(7) 0.0422(10) Uani 1 1 d . . . . .
H2 H 0.2714 0.3730 0.9605 0.051 Uiso 1 1 calc R . . . .
C3 C 0.5913(12) 0.34674(19) 0.9634(8) 0.0558(13) Uani 1 1 d . . . . .
H3A H 0.7235 0.3577 0.9293 0.084 Uiso 1 1 calc GR . . . .
H3B H 0.5226 0.3191 0.8881 0.084 Uiso 1 1 calc GR . . . .
H3C H 0.6519 0.3399 1.1042 0.084 Uiso 1 1 calc GR . . . .
C4 C 0.6098(12) 0.4246(2) 1.2361(8) 0.0574(14) Uani 1 1 d . . . . .
H4A H 0.6655 0.4549 1.2902 0.086 Uiso 1 1 calc GR . . . .
H4B H 0.7453 0.4033 1.2800 0.086 Uiso 1 1 calc GR . . . .
H4C H 0.4866 0.4140 1.2821 0.086 Uiso 1 1 calc GR . . . .
C5 C 0.1536(10) 0.35281(17) 0.5795(7) 0.0460(11) Uani 1 1 d . . . . .
C6 C -0.0518(11) 0.33614(19) 0.5996(9) 0.0543(13) Uani 1 1 d . . . . .
H6 H -0.1190 0.3523 0.6774 0.065 Uiso 1 1 calc R . . . .
C7 C -0.1583(12) 0.2963(2) 0.5073(11) 0.0687(19) Uani 1 1 d . . . . .
H7 H -0.2980 0.2851 0.5221 0.082 Uiso 1 1 calc R . . . .
C8 C -0.0633(14) 0.2730(2) 0.3954(12) 0.079(2) Uani 1 1 d . . . . .
H8 H -0.1347 0.2452 0.3351 0.095 Uiso 1 1 calc R . . . .
C9 C 0.1337(16) 0.2892(2) 0.3686(11) 0.078(2) Uani 1 1 d . . . . .
H9 H 0.1964 0.2731 0.2874 0.094 Uiso 1 1 calc R . . . .
C10 C 0.2426(12) 0.3295(2) 0.4605(9) 0.0620(15) Uani 1 1 d . . . . .
H10 H 0.3788 0.3409 0.4409 0.074 Uiso 1 1 calc R . . . .
C11 C 0.8185(9) 0.60368(16) 0.7704(7) 0.0428(10) Uani 1 1 d . . . . .
H11C H 0.7201 0.5795 0.7995 0.051 Uiso 1 1 calc R . . . .
C12 C 0.7115(9) 0.61383(15) 0.5468(7) 0.0435(10) Uani 1 1 d . . . . .
H12 H 0.5413 0.6241 0.5069 0.052 Uiso 1 1 calc R . . . .
C13 C 0.8514(12) 0.64980(19) 0.4892(8) 0.0560(14) Uani 1 1 d . . . . .
H13A H 1.0159 0.6391 0.5212 0.084 Uiso 1 1 calc GR . . . .
H13B H 0.8549 0.6780 0.5614 0.084 Uiso 1 1 calc GR . . . .
H13C H 0.7739 0.6556 0.3477 0.084 Uiso 1 1 calc GR . . . .
C14 C 0.6027(11) 0.5710(2) 0.2270(8) 0.0548(13) Uani 1 1 d . . . . .
H14A H 0.5976 0.5401 0.1755 0.082 Uiso 1 1 calc GR . . . .
H14B H 0.6967 0.5907 0.1763 0.082 Uiso 1 1 calc GR . . . .
H14C H 0.4389 0.5829 0.1854 0.082 Uiso 1 1 calc GR . . . .
C15 C 0.8124(9) 0.64633(17) 0.8827(7) 0.0428(10) Uani 1 1 d . . . . .
C16 C 1.0234(10) 0.66778(19) 1.0012(8) 0.0497(12) Uani 1 1 d . . . . .
H16 H 1.1736 0.6549 1.0158 0.060 Uiso 1 1 calc R . . . .
C17 C 1.0174(11) 0.7081(2) 1.0993(9) 0.0560(13) Uani 1 1 d . . . . .
H17 H 1.1636 0.7226 1.1784 0.067 Uiso 1 1 calc R . . . .
C18 C 0.8039(12) 0.7269(2) 1.0831(8) 0.0550(14) Uani 1 1 d . . . . .
H18 H 0.8013 0.7544 1.1504 0.066 Uiso 1 1 calc R . . . .
C19 C 0.5898(11) 0.7055(2) 0.9671(8) 0.0537(13) Uani 1 1 d . . . . .
H19 H 0.4404 0.7183 0.9553 0.064 Uiso 1 1 calc R . . . .
C20 C 0.5953(9) 0.6654(2) 0.8686(7) 0.0509(12) Uani 1 1 d . . . . .
H20 H 0.4489 0.6508 0.7906 0.061 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.062(2) 0.0494(19) 0.049(2) 0.0092(15) 0.0298(17) 0.0034(16)
O11 0.045(2) 0.0510(19) 0.0492(19) 0.0040(15) 0.0092(15) 0.0044(14)
O12 0.055(2) 0.051(2) 0.068(2) 0.0066(18) 0.0293(19) 0.0043(18)
O13 0.053(2) 0.044(2) 0.086(3) 0.0010(18) 0.030(2) 0.0021(16)
O14 0.055(3) 0.062(2) 0.079(3) 0.010(2) 0.027(2) -0.0058(19)
O15 0.061(3) 0.043(2) 0.084(3) -0.0001(17) 0.036(2) -0.0021(16)
O16 0.049(2) 0.050(2) 0.074(3) 0.0049(18) 0.0259(18) -0.0041(17)
O17 0.059(3) 0.062(2) 0.077(3) 0.011(2) 0.030(2) 0.013(2)
N1 0.049(3) 0.046(2) 0.044(2) -0.0004(17) 0.0216(18) -0.0018(17)
N11 0.040(2) 0.045(2) 0.045(2) 0.0004(17) 0.0137(17) -0.0024(17)
N12 0.042(3) 0.051(2) 0.041(2) -0.0026(17) 0.0147(17) -0.0036(18)
N13 0.046(3) 0.056(3) 0.040(2) -0.0043(17) 0.0149(18) -0.0014(19)
C1 0.045(3) 0.044(2) 0.044(2) 0.0024(19) 0.021(2) 0.0048(19)
C2 0.051(3) 0.038(2) 0.042(2) 0.0018(18) 0.022(2) -0.0017(19)
C3 0.068(4) 0.048(3) 0.044(3) 0.003(2) 0.015(2) 0.006(2)
C4 0.067(4) 0.064(3) 0.039(3) -0.005(2) 0.019(3) -0.001(3)
C5 0.047(3) 0.046(2) 0.038(2) 0.0027(19) 0.008(2) 0.009(2)
C6 0.050(3) 0.053(3) 0.055(3) 0.010(2) 0.015(2) 0.007(2)
C7 0.053(4) 0.056(3) 0.077(4) 0.017(3) 0.003(3) 0.002(3)
C8 0.066(5) 0.054(3) 0.075(5) -0.009(3) -0.020(4) 0.010(3)
C9 0.080(5) 0.074(4) 0.064(4) -0.022(3) 0.010(4) 0.018(4)
C10 0.061(4) 0.068(4) 0.053(3) -0.010(3) 0.018(3) 0.007(3)
C11 0.038(3) 0.044(2) 0.043(2) 0.0048(19) 0.0115(19) -0.0037(18)
C12 0.045(3) 0.037(2) 0.044(2) 0.0021(18) 0.012(2) 0.0003(18)
C13 0.069(4) 0.049(3) 0.047(3) 0.002(2) 0.019(2) -0.013(3)
C14 0.066(4) 0.053(3) 0.040(3) -0.004(2) 0.015(2) -0.004(2)
C15 0.042(3) 0.051(3) 0.034(2) 0.0067(18) 0.0135(18) -0.0027(19)
C16 0.041(3) 0.057(3) 0.049(3) -0.004(2) 0.015(2) -0.002(2)
C17 0.049(3) 0.065(3) 0.053(3) -0.010(2) 0.019(2) -0.011(2)
C18 0.069(4) 0.053(3) 0.042(3) -0.002(2) 0.020(2) 0.002(2)
C19 0.053(3) 0.062(3) 0.045(3) 0.004(2) 0.017(2) 0.008(2)
C20 0.037(3) 0.071(3) 0.039(2) 0.000(2) 0.0079(19) -0.001(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.8400 . ?
O1 C1 1.417(6) . ?
O11 H11 0.8400 . ?
O11 C11 1.408(7) . ?
O12 N12 1.269(6) . ?
O13 N12 1.233(6) . ?
O14 N12 1.234(6) . ?
O15 N13 1.238(6) . ?
O16 N13 1.265(6) . ?
O17 N13 1.240(6) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C2 1.502(6) . ?
N1 C4 1.489(7) . ?
N11 H11A 0.9100 . ?
N11 H11B 0.9100 . ?
N11 C12 1.500(7) . ?
N11 C14 1.478(7) . ?
C1 H1C 1.0000 . ?
C1 C2 1.536(7) . ?
C1 C5 1.518(7) . ?
C2 H2 1.0000 . ?
C2 C3 1.518(8) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.393(8) . ?
C5 C10 1.377(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.381(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.358(12) . ?
C8 H8 0.9500 . ?
C8 C9 1.365(13) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(10) . ?
C10 H10 0.9500 . ?
C11 H11C 1.0000 . ?
C11 C12 1.551(7) . ?
C11 C15 1.510(7) . ?
C12 H12 1.0000 . ?
C12 C13 1.513(8) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.386(7) . ?
C15 C20 1.392(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.394(8) . ?
C17 H17 0.9500 . ?
C17 C18 1.365(9) . ?
C18 H18 0.9500 . ?
C18 C19 1.393(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.392(8) . ?
C20 H20 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 H1 109.5 . . ?
C11 O11 H11 109.5 . . ?
H1A N1 H1B 107.5 . . ?
C2 N1 H1A 108.5 . . ?
C2 N1 H1B 108.5 . . ?
C4 N1 H1A 108.5 . . ?
C4 N1 H1B 108.5 . . ?
C4 N1 C2 115.2(4) . . ?
H11A N11 H11B 107.4 . . ?
C12 N11 H11A 108.3 . . ?
C12 N11 H11B 108.3 . . ?
C14 N11 H11A 108.3 . . ?
C14 N11 H11B 108.3 . . ?
C14 N11 C12 116.1(4) . . ?
O13 N12 O12 119.2(4) . . ?
O13 N12 O14 121.3(4) . . ?
O14 N12 O12 119.5(4) . . ?
O15 N13 O16 119.4(4) . . ?
O15 N13 O17 120.8(4) . . ?
O17 N13 O16 119.8(5) . . ?
O1 C1 H1C 108.9 . . ?
O1 C1 C2 108.2(4) . . ?
O1 C1 C5 111.6(4) . . ?
C2 C1 H1C 108.9 . . ?
C5 C1 H1C 108.9 . . ?
C5 C1 C2 110.2(4) . . ?
N1 C2 C1 106.5(4) . . ?
N1 C2 H2 109.0 . . ?
N1 C2 C3 110.0(5) . . ?
C1 C2 H2 109.0 . . ?
C3 C2 C1 113.4(4) . . ?
C3 C2 H2 109.0 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C1 120.4(5) . . ?
C10 C5 C1 121.0(5) . . ?
C10 C5 C6 118.5(5) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.6(6) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0(7) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.7(6) . . ?
C9 C8 H8 119.6 . . ?
C8 C9 H9 120.1 . . ?
C8 C9 C10 119.9(7) . . ?
C10 C9 H9 120.1 . . ?
C5 C10 C9 120.3(7) . . ?
C5 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
O11 C11 H11C 109.1 . . ?
O11 C11 C12 107.9(4) . . ?
O11 C11 C15 112.0(4) . . ?
C12 C11 H11C 109.1 . . ?
C15 C11 H11C 109.1 . . ?
C15 C11 C12 109.7(4) . . ?
N11 C12 C11 107.0(4) . . ?
N11 C12 H12 109.2 . . ?
N11 C12 C13 109.6(5) . . ?
C11 C12 H12 109.2 . . ?
C13 C12 C11 112.7(4) . . ?
C13 C12 H12 109.2 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N11 C14 H14A 109.5 . . ?
N11 C14 H14B 109.5 . . ?
N11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C11 120.8(5) . . ?
C16 C15 C20 118.3(5) . . ?
C20 C15 C11 121.0(4) . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.7(5) . . ?
C17 C16 H16 119.7 . . ?
C16 C17 H17 119.6 . . ?
C18 C17 C16 120.8(5) . . ?
C18 C17 H17 119.6 . . ?
C17 C18 H18 120.3 . . ?
C17 C18 C19 119.5(5) . . ?
C19 C18 H18 120.3 . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.9(5) . . ?
C20 C19 H19 120.1 . . ?
C15 C20 C19 120.9(5) . . ?
C15 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 61.6(5) . . . . ?
O1 C1 C2 C3 -59.5(5) . . . . ?
O1 C1 C5 C6 -171.6(4) . . . . ?
O1 C1 C5 C10 11.4(7) . . . . ?
O11 C11 C12 N11 59.5(5) . . . . ?
O11 C11 C12 C13 -61.0(5) . . . . ?
O11 C11 C15 C16 6.8(6) . . . . ?
O11 C11 C15 C20 -173.8(4) . . . . ?
C1 C5 C6 C7 -174.9(5) . . . . ?
C1 C5 C10 C9 174.7(6) . . . . ?
C2 C1 C5 C6 68.2(6) . . . . ?
C2 C1 C5 C10 -108.8(6) . . . . ?
C4 N1 C2 C1 174.6(5) . . . . ?
C4 N1 C2 C3 -62.2(6) . . . . ?
C5 C1 C2 N1 -176.2(4) . . . . ?
C5 C1 C2 C3 62.8(6) . . . . ?
C5 C6 C7 C8 -0.2(9) . . . . ?
C6 C5 C10 C9 -2.3(8) . . . . ?
C6 C7 C8 C9 -1.7(10) . . . . ?
C7 C8 C9 C10 1.5(11) . . . . ?
C8 C9 C10 C5 0.5(10) . . . . ?
C10 C5 C6 C7 2.2(8) . . . . ?
C11 C15 C16 C17 177.7(5) . . . . ?
C11 C15 C20 C19 -177.9(5) . . . . ?
C12 C11 C15 C16 -112.9(5) . . . . ?
C12 C11 C15 C20 66.5(6) . . . . ?
C14 N11 C12 C11 175.1(4) . . . . ?
C14 N11 C12 C13 -62.4(6) . . . . ?
C15 C11 C12 N11 -178.3(4) . . . . ?
C15 C11 C12 C13 61.2(6) . . . . ?
C15 C16 C17 C18 1.0(9) . . . . ?
C16 C15 C20 C19 1.5(8) . . . . ?
C16 C17 C18 C19 0.0(9) . . . . ?
C17 C18 C19 C20 -0.2(8) . . . . ?
C18 C19 C20 C15 -0.6(8) . . . . ?
C20 C15 C16 C17 -1.7(8) . . . . ?
_shelx_res_file
;
pn180914_uo_eph_2_180814_c6_scr2.res created by SHELXL-2014/7
TITL pn180914_uo_eph_2_180814_c6_scr2_a.res in P2(1)
REM SHELXT solution in P2(1)
REM R1 0.113, Rweak 0.037, Alpha 0.010, Orientation as input
REM Flack x = -1.028 ( 1.811 ) from Parsons' quotients
REM Formula found by SHELXT: C20 N4 O8
CELL 1.54184 6.040122 29.355256 7.382808 90 112.8063 90
ZERR 4 0.000263 0.000834 0.000289 0 0.0047 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H N O
UNIT 40 64 8 16
SIMU O15 O16 O17
L.S. 4 0 0
PLAN 20
SIZE 0.01 0.066 0.396
TEMP -113
list 4
BOND $H
CONF
fmap 2 53
acta
OMIT -3 2 4
OMIT 1 1 2
REM
REM
REM
WGHT 0.125300
FVAR 3.86108
O1 4 0.464498 0.409743 0.633017 11.00000 0.06189 0.04940 =
0.04949 0.00924 0.02982 0.00344
AFIX 147
H1 2 0.443659 0.437494 0.603534 11.00000 -1.50000
AFIX 0
O11 4 1.054145 0.587419 0.820570 11.00000 0.04523 0.05102 =
0.04916 0.00399 0.00925 0.00443
AFIX 147
H11 2 1.056953 0.559126 0.838362 11.00000 -1.50000
AFIX 0
O12 4 0.433514 0.499138 0.507762 11.00000 0.05452 0.05099 =
0.06809 0.00662 0.02926 0.00426
O13 4 0.207478 0.558843 0.445004 11.00000 0.05348 0.04434 =
0.08586 0.00096 0.03016 0.00211
O14 4 0.067674 0.494198 0.488068 11.00000 0.05540 0.06208 =
0.07946 0.01039 0.02719 -0.00585
O15 4 0.993566 0.437697 1.010034 11.00000 0.06053 0.04272 =
0.08388 -0.00005 0.03557 -0.00208
O16 4 1.164696 0.498102 0.957950 11.00000 0.04886 0.04962 =
0.07392 0.00489 0.02587 -0.00407
O17 4 0.809154 0.502158 0.963772 11.00000 0.05946 0.06197 =
0.07733 0.01106 0.02989 0.01254
N1 3 0.506178 0.426906 1.017531 11.00000 0.04855 0.04556 =
0.04395 -0.00036 0.02161 -0.00182
AFIX 23
H1A 2 0.623816 0.435779 0.976883 11.00000 -1.20000
H1B 2 0.390450 0.448792 0.979468 11.00000 -1.20000
AFIX 0
N11 3 0.715874 0.569964 0.443922 11.00000 0.04033 0.04509 =
0.04486 0.00038 0.01371 -0.00235
AFIX 23
H11A 2 0.871667 0.561225 0.479892 11.00000 -1.20000
H11B 2 0.640982 0.548238 0.487555 11.00000 -1.20000
AFIX 0
N12 3 0.232706 0.517625 0.479045 11.00000 0.04244 0.05073 =
0.04122 -0.00265 0.01470 -0.00363
N13 3 0.987816 0.479200 0.978813 11.00000 0.04600 0.05608 =
0.03952 -0.00430 0.01493 -0.00143
C1 1 0.282099 0.394439 0.694459 11.00000 0.04542 0.04441 =
0.04413 0.00243 0.02077 0.00484
AFIX 13
H1C 2 0.162554 0.419476 0.674104 11.00000 -1.20000
AFIX 0
C2 1 0.398832 0.383258 0.914703 11.00000 0.05098 0.03769 =
0.04163 0.00184 0.02196 -0.00167
AFIX 13
H2 2 0.271429 0.372951 0.960528 11.00000 -1.20000
AFIX 0
C3 1 0.591257 0.346737 0.963399 11.00000 0.06846 0.04848 =
0.04399 0.00324 0.01478 0.00596
AFIX 137
H3A 2 0.723488 0.357665 0.929261 11.00000 -1.50000
H3B 2 0.522570 0.319098 0.888145 11.00000 -1.50000
H3C 2 0.651906 0.339876 1.104222 11.00000 -1.50000
AFIX 0
C4 1 0.609770 0.424583 1.236149 11.00000 0.06720 0.06423 =
0.03918 -0.00548 0.01895 -0.00117
AFIX 137
H4A 2 0.665522 0.454899 1.290190 11.00000 -1.50000
H4B 2 0.745346 0.403295 1.279984 11.00000 -1.50000
H4C 2 0.486603 0.414027 1.282120 11.00000 -1.50000
AFIX 0
C5 1 0.153559 0.352809 0.579508 11.00000 0.04695 0.04577 =
0.03788 0.00273 0.00819 0.00925
C6 1 -0.051757 0.336137 0.599562 11.00000 0.04980 0.05347 =
0.05502 0.01037 0.01514 0.00671
AFIX 43
H6 2 -0.119048 0.352334 0.677394 11.00000 -1.20000
AFIX 0
C7 1 -0.158326 0.296269 0.507276 11.00000 0.05278 0.05566 =
0.07703 0.01724 0.00251 0.00164
AFIX 43
H7 2 -0.298016 0.285111 0.522064 11.00000 -1.20000
AFIX 0
C8 1 -0.063310 0.273029 0.395394 11.00000 0.06603 0.05359 =
0.07490 -0.00919 -0.02007 0.01006
AFIX 43
H8 2 -0.134709 0.245200 0.335148 11.00000 -1.20000
AFIX 0
C9 1 0.133688 0.289224 0.368565 11.00000 0.08041 0.07352 =
0.06414 -0.02182 0.01020 0.01830
AFIX 43
H9 2 0.196441 0.273098 0.287438 11.00000 -1.20000
AFIX 0
C10 1 0.242565 0.329482 0.460489 11.00000 0.06094 0.06834 =
0.05321 -0.00955 0.01815 0.00744
AFIX 43
H10 2 0.378839 0.340879 0.440920 11.00000 -1.20000
AFIX 0
C11 1 0.818468 0.603677 0.770416 11.00000 0.03759 0.04412 =
0.04290 0.00481 0.01148 -0.00369
AFIX 13
H11C 2 0.720124 0.579529 0.799452 11.00000 -1.20000
AFIX 0
C12 1 0.711461 0.613829 0.546793 11.00000 0.04518 0.03708 =
0.04389 0.00209 0.01240 0.00033
AFIX 13
H12 2 0.541295 0.624135 0.506890 11.00000 -1.20000
AFIX 0
C13 1 0.851384 0.649800 0.489183 11.00000 0.06924 0.04857 =
0.04714 0.00162 0.01917 -0.01324
AFIX 137
H13A 2 1.015933 0.639095 0.521168 11.00000 -1.50000
H13B 2 0.854940 0.677990 0.561372 11.00000 -1.50000
H13C 2 0.773915 0.655617 0.347689 11.00000 -1.50000
AFIX 0
C14 1 0.602746 0.570996 0.227007 11.00000 0.06596 0.05317 =
0.04012 -0.00398 0.01476 -0.00356
AFIX 137
H14A 2 0.597603 0.540075 0.175492 11.00000 -1.50000
H14B 2 0.696671 0.590666 0.176259 11.00000 -1.50000
H14C 2 0.438949 0.582933 0.185431 11.00000 -1.50000
AFIX 0
C15 1 0.812413 0.646332 0.882698 11.00000 0.04197 0.05076 =
0.03448 0.00671 0.01355 -0.00270
C16 1 1.023361 0.667776 1.001246 11.00000 0.04082 0.05678 =
0.04907 -0.00406 0.01461 -0.00177
AFIX 43
H16 2 1.173613 0.654893 1.015825 11.00000 -1.20000
AFIX 0
C17 1 1.017364 0.708061 1.099339 11.00000 0.04943 0.06483 =
0.05310 -0.00974 0.01933 -0.01062
AFIX 43
H17 2 1.163600 0.722565 1.178403 11.00000 -1.20000
AFIX 0
C18 1 0.803859 0.726903 1.083107 11.00000 0.06877 0.05310 =
0.04157 -0.00220 0.01980 0.00209
AFIX 43
H18 2 0.801298 0.754364 1.150356 11.00000 -1.20000
AFIX 0
C19 1 0.589831 0.705537 0.967149 11.00000 0.05286 0.06172 =
0.04464 0.00449 0.01693 0.00822
AFIX 43
H19 2 0.440380 0.718331 0.955334 11.00000 -1.20000
AFIX 0
C20 1 0.595327 0.665397 0.868594 11.00000 0.03683 0.07096 =
0.03882 0.00017 0.00793 -0.00080
AFIX 43
H20 2 0.448871 0.650810 0.790618 11.00000 -1.20000
AFIX 0
HKLF 4
REM pn180914_uo_eph_2_180814_c6_scr2_a.res in P2(1)
REM R1 = 0.0676 for 3727 Fo > 4sig(Fo) and 0.0787 for all 4637 data
REM 295 parameters refined using 1 restraints
END
WGHT 0.1253 0.0000
REM Highest difference peak 0.633, deepest hole -0.300, 1-sigma level 0.139
Q1 1 1.1683 0.4599 0.9712 11.00000 0.05 0.63
Q2 1 0.9946 0.5119 0.9761 11.00000 0.05 0.55
Q3 1 0.2456 0.4857 0.4792 11.00000 0.05 0.53
Q4 1 0.4020 0.5411 0.4879 11.00000 0.05 0.52
Q5 1 0.0635 0.5252 0.4803 11.00000 0.05 0.49
Q6 1 1.0367 0.5585 0.4694 11.00000 0.05 0.45
Q7 1 0.8506 0.4729 0.9751 11.00000 0.05 0.45
Q8 1 0.8186 0.6163 0.5019 11.00000 0.05 0.43
Q9 1 0.7471 0.5400 0.4668 11.00000 0.05 0.41
Q10 1 0.5033 0.3949 0.9857 11.00000 0.05 0.40
Q11 1 0.9966 0.4068 0.9927 11.00000 0.05 0.40
Q12 1 0.7346 0.6361 0.4937 11.00000 0.05 0.40
Q13 1 0.5277 0.4619 0.9900 11.00000 0.05 0.39
Q14 1 1.3310 0.4948 0.9671 11.00000 0.05 0.39
Q15 1 0.2257 0.5856 0.4732 11.00000 0.05 0.38
Q16 1 0.1442 0.3246 0.5587 11.00000 0.05 0.37
Q17 1 0.2735 0.3001 0.4783 11.00000 0.05 0.37
Q18 1 -0.1230 0.5037 0.4942 11.00000 0.05 0.36
Q19 1 1.0435 0.7001 1.0055 11.00000 0.05 0.36
Q20 1 0.5928 0.5073 0.4985 11.00000 0.05 0.35
;
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6 8 -7 64.8431 34.3704 9
6 8 -6 99.3864 41.6551 20
6 8 -6 37.4612 40.0832 9
6 8 -5 92.1318 48.1717 20
6 8 -5 125.893 43.3069 9
6 8 -1 404.404 54.8596 11
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6 9 -4 440.437 54.0578 20
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6 9 -1 42.2882 50.7043 11
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6 9 1 52.7393 44.5038 19
6 10 -7 15.7157 29.2992 20
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6 10 -6 102.161 43.3426 20
6 10 -6 117.144 40.5805 9
6 10 -5 300.786 52.9525 20
6 10 -5 388.668 49.0834 9
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6 10 -3-1.36465 48.9369 10
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6 11 -7 175.861 31.0012 20
6 11 -7 174.551 31.6594 9
6 11 -6 133.610 42.1269 20
6 11 -6 178.302 41.5713 9
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6 11 -5 760.562 67.9112 20
6 11 -5 846.093 64.2961 9
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6 11 -3-1.93779 66.6192 33
6 11 -3 71.7563 45.7591 16
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6 11 -2 236.922 51.2138 16
6 11 -2 221.188 50.5921 15
6 11 -1 160.232 52.3442 11
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6 11 0 104.602 45.2023 11
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6 12 -7 18.9285 26.5271 20
6 12 -7 31.9035 27.9800 9
6 12 -6 82.9354 40.2132 20
6 12 -6 61.6104 37.6577 9
6 12 -5 410.201 49.3336 10
6 12 -5 414.170 54.3419 20
6 12 -5 491.976 50.7402 9
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6 12 -4 301.907 65.8297 33
6 12 -3 3428.17 166.501 10
6 12 -3 3163.99 164.393 16
6 12 -2 131.680 50.4176 11
6 12 -2 41.3966 66.5489 33
6 12 -2 49.8729 49.0922 16
6 12 -2 137.687 48.7856 15
6 12 -1 917.571 68.4681 11
6 12 -1 511.415 77.2543 33
6 12 0 33.7988 44.4545 11
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6 12 0 19.4663 54.0689 33
6 12 1 300.004 41.3272 19
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6 13 -6 235.969 40.3290 9
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6 13 -4 257.865 49.8364 10
6 13 -4 198.512 42.4858 9
6 13 -4 230.203 63.9256 33
6 13 -4 237.299 45.2602 16
6 13 -3 35.5569 43.7615 11
6 13 -3 23.1704 51.1450 10
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6 13 -3 103.118 49.4469 16
6 13 -2 226.771 52.1205 11
6 13 -2 146.828 64.5484 33
6 13 -2 207.915 51.0536 16
6 13 -2 237.388 50.0243 15
6 13 -1 77.3794 49.2455 11
6 13 -1 39.4408 62.7850 33
6 13 0 226.457 46.1116 11
6 13 0 222.143 47.2269 19
6 13 0 102.025 54.8069 33
6 13 1 8.70153 33.1190 19
6 14 -7 211.925 24.1729 9
6 14 -6 164.948 32.9347 10
6 14 -6 187.699 40.3353 20
6 14 -6 185.786 36.9363 9
6 14 -5 187.379 41.4577 10
6 14 -5 77.0579 46.4000 20
6 14 -5 130.108 40.9263 9
6 14 -4 490.852 56.7267 10
6 14 -4 390.198 47.5342 9
6 14 -4 465.234 68.1755 33
6 14 -4 464.299 50.4336 16
6 14 -3 1445.45 90.5779 11
6 14 -3 1536.07 93.3292 10
6 14 -3 1615.20 92.8259 16
6 14 -2 454.601 55.9035 11
6 14 -2 286.318 68.3686 33
6 14 -2 461.368 55.2744 16
6 14 -2 501.776 55.6023 15
6 14 -1 341.931 52.3075 11
6 14 -1 252.488 64.6702 33
6 14 0 210.130 42.5971 11
6 14 0 147.462 43.0511 19
6 14 0 97.4439 50.8806 33
6 14 1 73.8735 28.4678 19
6 15 -6 124.227 30.3702 10
6 15 -6 137.935 37.0200 20
6 15 -6 107.243 33.3356 9
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6 15 -3 22.8657 47.3992 10
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6 15 -2-33.0629 60.7528 33
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6 15 -1 252.399 48.9396 11
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6 16 -6 273.548 34.4317 9
6 16 -5 584.880 50.2841 10
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6 16 -4 304.402 46.7435 10
6 16 -4 228.418 40.8200 9
6 16 -4 262.251 42.3743 16
6 16 -3 535.937 52.0410 11
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6 17 -3-21.3785 40.3295 11
6 17 -3 31.6377 44.0226 10
6 17 -3-1.67866 58.6088 33
6 17 -3 27.8109 41.6222 16
6 17 -2 157.840 44.1044 11
6 17 -2 55.7526 58.8752 33
6 17 -2 128.945 44.2285 16
6 17 -2 150.822 42.5901 15
6 17 -1 129.653 40.6533 11
6 17 -1 68.0443 49.6958 33
6 17 0 11.9615 31.3695 11
6 17 0 55.6205 26.6143 19
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6 18 -5 270.551 35.7585 9
6 18 -4 379.660 45.6378 10
6 18 -4 246.716 37.6375 16
6 18 -3-4.99185 37.6737 11
6 18 -3 50.7206 42.2499 10
6 18 -3 71.0073 55.4941 33
6 18 -3 15.4564 38.6811 16
6 18 -2 264.344 43.5746 11
6 18 -2 198.161 56.7051 33
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6 19 -5 136.140 32.2139 10
6 19 -4 39.1786 36.0578 10
6 19 -4 13.8625 31.6663 16
6 19 -3 133.233 36.7230 11
6 19 -3 84.7487 39.9835 10
6 19 -3 98.0579 53.2714 33
6 19 -3 113.196 37.3693 16
6 19 -2 51.7119 37.1384 11
6 19 -2 68.3897 49.7056 33
6 19 -2 32.9035 36.7667 16
6 19 -2 113.836 35.9536 15
6 19 -1 71.0996 33.8574 11
6 20 -5-3.67901 24.2457 10
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6 20 -4 64.9429 28.8024 16
6 20 -3 38.9817 31.4188 11
6 20 -3 151.017 35.3506 10
6 20 -3 106.861 34.2411 16
6 20 -2-13.9196 33.5071 11
6 20 -2-18.0753 33.1627 16
6 20 -2 43.3100 31.1026 15
6 20 -1 19.2762 29.1312 11
6 21 -4 119.369 29.8773 10
6 21 -4 69.9269 24.8451 16
6 21 -3 180.076 28.6556 11
6 21 -3 128.077 31.0844 16
6 21 -2 153.804 29.8601 11
6 21 -1 52.5518 23.2969 11
6 22 -4 84.2313 24.2099 10
6 22 -3-19.9490 24.1187 16
6 22 -2 32.2620 23.1235 11
0 0 0 0.00 0.00 0
TITL PN180914_UO_Eph_2_180814_C6_scr2 in P2(1)
REM P2(1) (#4 in standard setting)
CELL 1.54184 6.040122 29.355256 7.382808 90.0000 112.8063 90.0000
ZERR 4.00 0.000263 0.000834 0.000289 0.0000 0.0047 0.0000
LATT -1
SYMM -x, y+1/2,-z
SFAC C H N O
UNIT 40.00 80.00 8.00 20.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 65547
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;