##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
# Software is freely available for graphical display of the structure(s) #
# in this CIF. For information consult the CIF software page #
# http://www.iucr.org/resources/cif/software. #
# #
# This file may be used for bona fide research purposes within the #
# scientific community so long as proper attribution is given to the journal #
# article from which it was obtained. #
# #
##############################################################################
data_global
_audit_creation_method 'from SHELXL-2014'
_journal_date_recd_electronic 2019-01-08
_journal_date_accepted 2019-01-09
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2019
_journal_volume 75
_journal_issue 2
_journal_page_first 202
_journal_page_last 207
_journal_paper_category GO
_journal_paper_doi 10.1107/S2056989019000458
_journal_coeditor_code ZL2747
loop_
_publ_contact_author_name
_publ_contact_author_address
_publ_contact_author_email
'Yathirajan, Hemmige S.'
; Department of Studies in Chemistry,
University of Mysore,
Manasagangotri, Mysuru-570 006,
India
;
yathirajan@hotmail.com
_publ_contact_author_fax ?
_publ_contact_author_phone ?
_publ_section_title
;
Three closely related
1-[(1,3-benzodioxol-5-yl)methyl]-4-(halobenzoyl)piperazines:
similar molecular structures but different intermolecular interactions
;
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
'Mahesha, Ninganayaka' .
;
Department of Studies in Chemistry,
University of Mysore,
Manasagangotri,
Mysuru-570 006,
India
;
'Sagar, Belakavadi K.' .
;
Department of Studies in Chemistry,
University of Mysore,
Manasagangotri,
Mysuru-570 006,
India
;
'Yathirajan, Hemmige S.' .
; Department of Studies in Chemistry,
University of Mysore,
Manasagangotri,
Mysuru-570 006,
India
;
'Furuya, Tetsundo' .
;
Department of Chemistry,
Faculty of Science,
Tokyo University of Science,
1-3 Kagurazaka,
Shinjuku-ku,
Tokyo 162-8601,
Japan
;
'Haraguchi, Tomoyuki' .
;
Department of Chemistry,
Faculty of Science,
Tokyo University of Science,
1-3 Kagurazaka,
Shinjuku-ku,
Tokyo 162-8601,
Japan
;
'Akitsu, Takashiro' .
;
Department of Chemistry,
Faculty of Science,
Tokyo University of Science,
1-3 Kagurazaka,
Shinjuku-ku,
Tokyo 162-8601,
Japan
;
'Glidewell, Christopher' .
; School of Chemistry, University of St Andrews,
St Andrews, Fife KY16 9ST, UK
;
_publ_section_synopsis
;
Three 1-[(1,3-benzodioxol-5-yl)methyl]-4-(halobenzoyl)piperazines adopt very
similar molecular conformations but, while the molecules of the
3-fluorobenzoyl are linked by hydrogen bonds into a three-dimensional
structure, there are no hydrogen bonds in either of the 2,6-difluorobenzoyl
and 2,4-dichlorobenzoyl analogues.
;
data_I
_database_code_depnum_ccdc_archive 'CCDC 1889708'
_audit_creation_method SHELXL-2014
_chemical_name_systematic
;
1-[(1,3-Benzodioxol-5-yl)methyl]-4-(3-fluorobenzoyl)piperazine
;
_chemical_name_common ?
_chemical_formula_moiety 'C19 H19 F N2 O3'
_chemical_formula_sum 'C19 H19 F N2 O3'
_chemical_formula_iupac 'C19 H19 F N2 O3'
_chemical_formula_weight 342.36
_chemical_melting_point ?
_space_group_crystal_system monoclinic
_space_group_name_H-M_alt 'P 21/n'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.2358(16)
_cell_length_b 10.3185(14)
_cell_length_c 14.2310(19)
_cell_angle_alpha 90
_cell_angle_beta 111.199(2)
_cell_angle_gamma 90
_cell_volume 1675.2(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 3689
_cell_measurement_theta_min 1.887
_cell_measurement_theta_max 27.574
_cell_measurement_temperature 173(2)
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.479
_exptl_crystal_size_mid 0.293
_exptl_crystal_size_min 0.282
_exptl_crystal_density_diffrn 1.357
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_F_000 720
_exptl_absorpt_coefficient_mu 0.100
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_absorpt_correction_T_min 0.813
_exptl_absorpt_correction_T_max 0.972
_exptl_special_details ?
_diffrn_ambient_temperature 173(2)
_diffrn_source 'fine focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean 0.3333
_diffrn_reflns_number 8635
_diffrn_reflns_av_R_equivalents 0.0213
_diffrn_reflns_av_unetI/netI 0.0279
_diffrn_reflns_theta_min 1.887
_diffrn_reflns_theta_max 27.573
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 9
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_refine_special_details ?
_reflns_number_total 3674
_reflns_number_gt 2975
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0502
_refine_ls_R_factor_gt 0.0397
_refine_ls_wR_factor_gt 0.1084
_refine_ls_wR_factor_ref 0.1141
_refine_ls_goodness_of_fit_ref 1.096
_refine_ls_restrained_S_all 1.096
_refine_ls_number_reflns 3674
_refine_ls_number_parameters 226
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.4713P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.238
_refine_diff_density_min -0.179
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
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'
'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'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick,2015)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2014 and PLATON (Spek, 2009)
;
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N N1 0.57212(10) 0.47476(11) 0.26954(9) 0.0303(3) Uani d 1 . .
C C2 0.51223(13) 0.44782(14) 0.33984(11) 0.0330(3) Uani d 1 . .
H H2A 0.5622 0.3918 0.3952 0.040 Uiso calc 1 . .
H H2B 0.4379 0.4014 0.3043 0.040 Uiso calc 1 . .
C C3 0.48694(13) 0.57400(15) 0.38272(11) 0.0356(3) Uani d 1 . .
H H3A 0.4438 0.5560 0.4283 0.043 Uiso calc 1 . .
H H3B 0.5616 0.6173 0.4224 0.043 Uiso calc 1 . .
N N4 0.41697(11) 0.65903(12) 0.30093(9) 0.0327(3) Uani d 1 . .
C C5 0.47088(13) 0.68273(14) 0.22552(11) 0.0327(3) Uani d 1 . .
H H5A 0.5444 0.7325 0.2564 0.039 Uiso calc 1 . .
H H5B 0.4170 0.7344 0.1691 0.039 Uiso calc 1 . .
C C6 0.49704(13) 0.55452(14) 0.18609(11) 0.0313(3) Uani d 1 . .
H H6A 0.4228 0.5081 0.1502 0.038 Uiso calc 1 . .
H H6B 0.5368 0.5704 0.1377 0.038 Uiso calc 1 . .
C C11 0.60711(14) 0.35498(14) 0.23287(12) 0.0368(3) Uani d 1 . .
H H11A 0.5367 0.3124 0.1845 0.044 Uiso calc 1 . .
H H11B 0.6424 0.2951 0.2903 0.044 Uiso calc 1 . .
O O11 0.95161(10) 0.44449(12) 0.06543(9) 0.0460(3) Uani d 1 . .
C C12 1.01387(15) 0.54464(18) 0.13322(13) 0.0450(4) Uani d 1 . .
H H12A 1.0984 0.5232 0.1624 0.054 Uiso calc 1 . .
H H12B 1.0049 0.6279 0.0967 0.054 Uiso calc 1 . .
O O13 0.96722(10) 0.55552(12) 0.21141(9) 0.0453(3) Uani d 1 . .
C C3A 0.86787(13) 0.48056(14) 0.18111(11) 0.0317(3) Uani d 1 . .
C C14 0.78769(13) 0.46591(14) 0.22718(11) 0.0323(3) Uani d 1 . .
H H14 0.7950 0.5118 0.2870 0.039 Uiso calc 1 . .
C C15 0.69410(13) 0.37999(14) 0.18201(11) 0.0327(3) Uani d 1 . .
C C16 0.68486(14) 0.31574(15) 0.09369(12) 0.0384(4) Uani d 1 . .
H H16 0.6203 0.2592 0.0636 0.046 Uiso calc 1 . .
C C17 0.76762(14) 0.33156(16) 0.04750(12) 0.0399(4) Uani d 1 . .
H H17 0.7610 0.2869 -0.0127 0.048 Uiso calc 1 . .
C C7A 0.85801(14) 0.41432(14) 0.09347(11) 0.0347(3) Uani d 1 . .
C C47 0.32103(13) 0.72461(14) 0.29797(11) 0.0328(3) Uani d 1 . .
O O47 0.27475(12) 0.80626(13) 0.23290(10) 0.0583(4) Uani d 1 . .
C C41 0.26784(12) 0.69823(13) 0.37650(11) 0.0291(3) Uani d 1 . .
C C42 0.22151(13) 0.57722(14) 0.38544(11) 0.0333(3) Uani d 1 . .
H H42 0.2306 0.5049 0.3476 0.040 Uiso calc 1 . .
C C43 0.16209(14) 0.56607(15) 0.45098(12) 0.0367(3) Uani d 1 . .
F F43 0.11374(10) 0.44972(10) 0.45775(9) 0.0590(3) Uani d 1 . .
C C44 0.14867(13) 0.66616(16) 0.50952(12) 0.0377(4) Uani d 1 . .
H H44 0.1079 0.6542 0.5544 0.045 Uiso calc 1 . .
C C45 0.19660(13) 0.78531(16) 0.50088(12) 0.0381(4) Uani d 1 . .
H H45 0.1896 0.8563 0.5409 0.046 Uiso calc 1 . .
C C46 0.25459(13) 0.80141(14) 0.43428(12) 0.0345(3) Uani d 1 . .
H H46 0.2857 0.8839 0.4280 0.041 Uiso calc 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N1 0.0328(6) 0.0277(6) 0.0323(6) 0.0018(5) 0.0140(5) 0.0033(5)
C2 0.0307(7) 0.0341(8) 0.0338(8) 0.0021(6) 0.0113(6) 0.0106(6)
C3 0.0349(8) 0.0444(9) 0.0275(7) 0.0076(6) 0.0114(6) 0.0080(6)
N4 0.0373(7) 0.0345(7) 0.0283(6) 0.0068(5) 0.0145(5) 0.0068(5)
C5 0.0388(8) 0.0300(7) 0.0317(7) 0.0015(6) 0.0157(6) 0.0061(6)
C6 0.0350(8) 0.0311(7) 0.0285(7) -0.0005(6) 0.0121(6) 0.0025(6)
C11 0.0408(8) 0.0276(7) 0.0427(9) 0.0007(6) 0.0160(7) 0.0009(6)
O11 0.0512(7) 0.0504(7) 0.0447(7) -0.0015(5) 0.0275(6) -0.0093(5)
C12 0.0400(9) 0.0524(10) 0.0469(10) 0.0013(7) 0.0209(8) -0.0054(8)
O13 0.0426(6) 0.0511(7) 0.0478(7) -0.0086(5) 0.0231(6) -0.0146(5)
C3A 0.0325(7) 0.0279(7) 0.0318(7) 0.0059(6) 0.0082(6) -0.0006(6)
C14 0.0367(8) 0.0306(7) 0.0290(7) 0.0048(6) 0.0113(6) -0.0022(6)
C15 0.0351(8) 0.0273(7) 0.0344(8) 0.0064(6) 0.0108(6) 0.0013(6)
C16 0.0358(8) 0.0344(8) 0.0391(8) 0.0030(6) 0.0066(7) -0.0068(6)
C17 0.0465(9) 0.0388(8) 0.0324(8) 0.0077(7) 0.0117(7) -0.0073(6)
C7A 0.0401(8) 0.0330(8) 0.0330(8) 0.0109(6) 0.0160(7) 0.0023(6)
C47 0.0369(8) 0.0260(7) 0.0370(8) 0.0018(6) 0.0150(6) 0.0059(6)
O47 0.0624(8) 0.0576(8) 0.0686(9) 0.0303(6) 0.0401(7) 0.0385(7)
C41 0.0263(7) 0.0280(7) 0.0303(7) 0.0019(5) 0.0071(6) 0.0036(5)
C42 0.0400(8) 0.0268(7) 0.0329(7) -0.0001(6) 0.0128(7) 0.0002(6)
C43 0.0383(8) 0.0311(8) 0.0398(8) -0.0047(6) 0.0130(7) 0.0068(6)
F43 0.0759(8) 0.0378(6) 0.0757(7) -0.0142(5) 0.0424(6) 0.0061(5)
C44 0.0342(8) 0.0466(9) 0.0337(8) 0.0027(7) 0.0141(7) 0.0058(7)
C45 0.0368(8) 0.0382(8) 0.0387(8) 0.0020(6) 0.0127(7) -0.0064(7)
C46 0.0332(8) 0.0270(7) 0.0431(8) -0.0020(6) 0.0135(7) -0.0006(6)
_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 C6 . 1.4638(18) ?
N1 C11 . 1.4645(18) ?
N1 C2 . 1.4647(18) ?
C2 C3 . 1.517(2) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 N4 . 1.4619(18) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
N4 C47 . 1.3423(19) ?
N4 C5 . 1.4692(17) ?
C5 C6 . 1.5156(19) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C11 C15 . 1.510(2) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
O11 C7A . 1.3777(19) ?
O11 C12 . 1.431(2) ?
C12 O13 . 1.4268(19) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
O13 C3A . 1.3722(18) ?
C3A C14 . 1.371(2) ?
C3A C7A . 1.389(2) ?
C14 C15 . 1.406(2) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.389(2) ?
C16 C17 . 1.402(2) ?
C16 H16 . 0.9500 ?
C17 C7A . 1.363(2) ?
C17 H17 . 0.9500 ?
C47 O47 . 1.2283(18) ?
C47 C41 . 1.507(2) ?
C41 C46 . 1.390(2) ?
C41 C42 . 1.3960(19) ?
C42 C43 . 1.379(2) ?
C42 H42 . 0.9500 ?
C43 F43 . 1.3572(17) ?
C43 C44 . 1.374(2) ?
C44 C45 . 1.387(2) ?
C44 H44 . 0.9500 ?
C45 C46 . 1.384(2) ?
C45 H45 . 0.9500 ?
C46 H46 . 0.9500 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 N1 C11 . . 111.35(11) ?
C6 N1 C2 . . 109.80(11) ?
C11 N1 C2 . . 111.48(11) ?
N1 C2 C3 . . 109.70(12) ?
N1 C2 H2A . . 109.7 ?
C3 C2 H2A . . 109.7 ?
N1 C2 H2B . . 109.7 ?
C3 C2 H2B . . 109.7 ?
H2A C2 H2B . . 108.2 ?
N4 C3 C2 . . 109.93(12) ?
N4 C3 H3A . . 109.7 ?
C2 C3 H3A . . 109.7 ?
N4 C3 H3B . . 109.7 ?
C2 C3 H3B . . 109.7 ?
H3A C3 H3B . . 108.2 ?
C47 N4 C3 . . 125.54(12) ?
C47 N4 C5 . . 120.78(12) ?
C3 N4 C5 . . 113.15(11) ?
N4 C5 C6 . . 109.62(11) ?
N4 C5 H5A . . 109.7 ?
C6 C5 H5A . . 109.7 ?
N4 C5 H5B . . 109.7 ?
C6 C5 H5B . . 109.7 ?
H5A C5 H5B . . 108.2 ?
N1 C6 C5 . . 110.19(12) ?
N1 C6 H6A . . 109.6 ?
C5 C6 H6A . . 109.6 ?
N1 C6 H6B . . 109.6 ?
C5 C6 H6B . . 109.6 ?
H6A C6 H6B . . 108.1 ?
N1 C11 C15 . . 111.97(12) ?
N1 C11 H11A . . 109.2 ?
C15 C11 H11A . . 109.2 ?
N1 C11 H11B . . 109.2 ?
C15 C11 H11B . . 109.2 ?
H11A C11 H11B . . 107.9 ?
C7A O11 C12 . . 105.29(11) ?
O13 C12 O11 . . 108.48(13) ?
O13 C12 H12A . . 110.0 ?
O11 C12 H12A . . 110.0 ?
O13 C12 H12B . . 110.0 ?
O11 C12 H12B . . 110.0 ?
H12A C12 H12B . . 108.4 ?
C3A O13 C12 . . 105.63(12) ?
C14 C3A O13 . . 128.14(13) ?
C14 C3A C7A . . 122.03(14) ?
O13 C3A C7A . . 109.82(13) ?
C3A C14 C15 . . 117.14(13) ?
C3A C14 H14 . . 121.4 ?
C15 C14 H14 . . 121.4 ?
C16 C15 C14 . . 120.05(14) ?
C16 C15 C11 . . 120.75(14) ?
C14 C15 C11 . . 119.16(13) ?
C15 C16 C17 . . 122.17(15) ?
C15 C16 H16 . . 118.9 ?
C17 C16 H16 . . 118.9 ?
C7A C17 C16 . . 116.51(14) ?
C7A C17 H17 . . 121.7 ?
C16 C17 H17 . . 121.7 ?
C17 C7A O11 . . 128.17(14) ?
C17 C7A C3A . . 122.10(14) ?
O11 C7A C3A . . 109.73(14) ?
O47 C47 N4 . . 121.94(13) ?
O47 C47 C41 . . 118.54(13) ?
N4 C47 C41 . . 119.52(12) ?
C46 C41 C42 . . 119.54(13) ?
C46 C41 C47 . . 118.31(12) ?
C42 C41 C47 . . 121.84(13) ?
C43 C42 C41 . . 117.84(13) ?
C43 C42 H42 . . 121.1 ?
C41 C42 H42 . . 121.1 ?
F43 C43 C44 . . 118.11(14) ?
F43 C43 C42 . . 118.15(14) ?
C44 C43 C42 . . 123.73(14) ?
C43 C44 C45 . . 117.76(14) ?
C43 C44 H44 . . 121.1 ?
C45 C44 H44 . . 121.1 ?
C46 C45 C44 . . 120.34(14) ?
C46 C45 H45 . . 119.8 ?
C44 C45 H45 . . 119.8 ?
C45 C46 C41 . . 120.77(14) ?
C45 C46 H46 . . 119.6 ?
C41 C46 H46 . . 119.6 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 N1 C2 C3 . . . . -60.96(15) ?
C11 N1 C2 C3 . . . . 175.17(12) ?
N1 C2 C3 N4 . . . . 57.23(15) ?
C2 C3 N4 C47 . . . . 133.38(15) ?
C2 C3 N4 C5 . . . . -55.00(16) ?
C47 N4 C5 C6 . . . . -133.39(14) ?
C3 N4 C5 C6 . . . . 54.54(16) ?
C11 N1 C6 C5 . . . . -175.10(11) ?
C2 N1 C6 C5 . . . . 60.95(15) ?
N4 C5 C6 N1 . . . . -56.63(15) ?
C6 N1 C11 C15 . . . . 71.31(15) ?
C2 N1 C11 C15 . . . . -165.70(12) ?
C7A O11 C12 O13 . . . . 10.19(17) ?
O11 C12 O13 C3A . . . . -9.99(17) ?
C12 O13 C3A C14 . . . . -175.37(15) ?
C12 O13 C3A C7A . . . . 5.95(17) ?
O13 C3A C14 C15 . . . . -178.36(14) ?
C7A C3A C14 C15 . . . . 0.2(2) ?
C3A C14 C15 C16 . . . . -0.9(2) ?
C3A C14 C15 C11 . . . . 176.73(13) ?
N1 C11 C15 C16 . . . . -138.33(14) ?
N1 C11 C15 C14 . . . . 44.02(18) ?
C14 C15 C16 C17 . . . . 1.1(2) ?
C11 C15 C16 C17 . . . . -176.55(14) ?
C15 C16 C17 C7A . . . . -0.4(2) ?
C16 C17 C7A O11 . . . . 178.28(14) ?
C16 C17 C7A C3A . . . . -0.4(2) ?
C12 O11 C7A C17 . . . . 174.64(16) ?
C12 O11 C7A C3A . . . . -6.53(16) ?
C14 C3A C7A C17 . . . . 0.5(2) ?
O13 C3A C7A C17 . . . . 179.30(14) ?
C14 C3A C7A O11 . . . . -178.38(13) ?
O13 C3A C7A O11 . . . . 0.39(17) ?
C3 N4 C47 O47 . . . . 171.03(16) ?
C5 N4 C47 O47 . . . . 0.0(2) ?
C3 N4 C47 C41 . . . . -8.9(2) ?
C5 N4 C47 C41 . . . . -179.92(13) ?
O47 C47 C41 C46 . . . . -56.5(2) ?
N4 C47 C41 C46 . . . . 123.39(16) ?
O47 C47 C41 C42 . . . . 116.97(17) ?
N4 C47 C41 C42 . . . . -63.11(19) ?
C46 C41 C42 C43 . . . . 1.1(2) ?
C47 C41 C42 C43 . . . . -172.33(13) ?
C41 C42 C43 F43 . . . . 178.02(14) ?
C41 C42 C43 C44 . . . . -1.7(2) ?
F43 C43 C44 C45 . . . . -178.92(14) ?
C42 C43 C44 C45 . . . . 0.8(2) ?
C43 C44 C45 C46 . . . . 0.7(2) ?
C44 C45 C46 C41 . . . . -1.3(2) ?
C42 C41 C46 C45 . . . . 0.4(2) ?
C47 C41 C46 C45 . . . . 174.01(13) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C42 H42 O47 2_545 0.95 2.34 3.273(2) 168 y
C5 H5A Cg1 2_655 0.99 2.76 3.7310(18) 168 y
C45 H45 Cg1 4_576 0.95 2.90 3.7470(18) 149 y
_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.
;
_shelx_estimated_absorpt_T_min 0.954
_shelx_estimated_absorpt_T_max 0.972
_shelx_hkl_file
;
1 0 0 0.00 0.10
1 0 0 0.00 0.10
-2 0 0 29.80 0.90
2 0 0 30.70 1.00
2 0 0 29.80 1.20
-3 0 0 -0.10 0.10
3 0 0 0.20 0.20
3 0 0 0.00 0.30
4 0 0 1675.83 44.80
4 0 0 1688.13 43.80
-4 0 0 1677.83 43.50
5 0 0 0.00 0.40
5 0 0 0.20 0.20
-5 0 0 0.10 0.20
6 0 0 22.20 1.40
-6 0 0 21.50 0.90
6 0 0 22.60 1.00
-7 0 0 0.00 0.30
7 0 0 -0.20 0.30
7 0 0 -0.20 0.50
8 0 0 60.29 2.70
8 0 0 60.39 2.10
9 0 0 0.00 0.40
9 0 0 -0.50 0.70
10 0 0 12.90 1.00
10 0 0 11.90 1.50
11 0 0 0.00 0.90
11 0 0 0.70 0.50
12 0 0 3.70 1.20
13 0 0 0.90 1.10
14 0 0 5.10 1.40
0 -1 0 -2.60 0.10
1 -1 0 54.79 1.80
-1 -1 0 51.89 1.70
-1 1 0 54.69 1.80
-2 -1 0 738.03 19.70
2 -1 0 760.12 20.00
2 -1 0 760.22 19.80
2 1 0 761.52 19.60
-2 1 0 760.52 19.80
3 -1 0 1990.40 65.79
3 -1 0 1942.31 50.69
-3 -1 0 1940.11 54.59
-3 1 0 1983.50 50.59
3 1 0 1919.01 51.79
3 1 0 1944.91 50.39
4 -1 0 98.49 3.00
4 -1 0 98.09 2.80
-4 -1 0 100.19 2.80
4 1 0 100.19 2.80
-4 1 0 100.19 2.80
4 1 0 91.89 3.20
5 -1 0 0.70 0.30
5 -1 0 0.00 0.30
-5 -1 0 0.10 0.20
-5 1 0 0.20 0.20
5 1 0 0.20 0.40
5 1 0 -0.10 0.20
6 -1 0 170.98 4.80
6 -1 0 169.08 5.20
-6 -1 0 167.98 4.70
-6 1 0 172.88 4.70
6 1 0 171.88 4.70
6 1 0 167.08 5.40
7 -1 0 28.60 1.60
-7 -1 0 28.50 1.20
7 -1 0 30.70 1.30
-7 1 0 28.10 1.20
7 1 0 27.40 1.80
7 1 0 28.30 1.20
8 -1 0 56.79 2.50
8 -1 0 53.89 2.00
-8 1 0 52.79 1.90
8 1 0 57.29 2.70
8 1 0 55.89 2.00
9 -1 0 2.60 0.60
9 -1 0 3.20 0.90
9 1 0 2.30 0.90
9 1 0 2.50 0.50
10 -1 0 -0.30 0.40
10 -1 0 0.50 0.80
10 1 0 -0.20 0.80
10 1 0 0.10 0.40
11 -1 0 313.17 9.70
11 -1 0 319.47 9.10
11 1 0 326.67 10.10
12 -1 0 55.69 3.00
12 1 0 54.09 3.20
13 -1 0 1.10 1.60
13 1 0 1.10 1.10
14 1 0 7.40 1.70
0 -2 0 1731.73 45.10
-1 -2 0 4312.57 121.99
1 -2 0 4110.69 122.69
2 -2 0 6236.88 180.28
-2 -2 0 6302.67 176.58
-2 2 0 6383.16 177.68
2 2 0 6546.85 177.38
-3 -2 0 404.16 10.40
3 -2 0 399.76 10.50
3 -2 0 394.26 10.50
3 2 0 394.86 10.40
-3 2 0 400.06 10.40
4 -2 0 25.70 1.10
4 -2 0 27.50 1.10
-4 -2 0 26.70 1.00
4 2 0 26.60 1.00
4 2 0 24.20 1.40
-4 2 0 26.40 1.00
5 -2 0 0.00 0.30
-5 -2 0 0.10 0.20
5 -2 0 0.10 0.40
5 2 0 -0.20 0.30
-5 2 0 0.10 0.20
5 2 0 -0.20 0.50
6 -2 0 152.88 4.60
6 -2 0 151.18 4.40
-6 -2 0 151.88 4.30
-6 2 0 150.08 4.30
6 2 0 149.59 5.00
6 2 0 155.68 4.30
7 -2 0 87.39 2.90
-7 -2 0 88.49 2.70
7 -2 0 88.69 3.10
7 2 0 89.99 2.70
7 2 0 85.89 3.50
-7 2 0 89.79 2.70
8 -2 0 52.39 2.00
8 -2 0 47.80 2.20
-8 2 0 49.20 1.80
8 2 0 50.39 1.80
8 2 0 48.60 2.60
9 -2 0 2.40 0.60
9 -2 0 2.20 0.80
9 2 0 2.00 0.50
9 2 0 2.90 1.10
10 -2 0 10.80 1.30
10 -2 0 11.30 1.10
10 2 0 12.30 1.70
11 -2 0 0.20 0.70
11 -2 0 0.50 0.60
11 2 0 0.80 1.00
12 -2 0 11.00 1.20
12 2 0 6.80 1.60
13 2 0 1.60 1.30
14 2 0 47.30 3.50
0 -3 0 -0.20 0.20
1 -3 0 1948.31 50.89
-1 -3 0 1925.61 50.69
-2 -3 0 112.79 3.30
-3 -3 0 369.16 9.60
3 -3 0 351.56 9.70
3 3 0 384.06 9.60
-3 3 0 349.87 9.70
4 -3 0 538.45 14.20
-4 -3 0 537.65 14.00
4 3 0 534.65 14.00
-4 3 0 534.35 14.10
-5 -3 0 2.90 0.40
5 -3 0 3.10 0.50
-5 3 0 2.90 0.40
5 3 0 3.50 0.40
5 3 0 3.10 0.80
-6 -3 0 14.60 0.80
6 -3 0 16.90 1.00
6 -3 0 16.80 1.10
6 3 0 17.10 1.50
6 3 0 15.80 0.90
-6 3 0 15.70 0.90
7 -3 0 24.40 1.40
7 -3 0 22.20 1.20
-7 3 0 22.70 1.10
7 3 0 22.80 1.80
7 3 0 25.30 1.20
8 -3 0 2.00 0.70
8 -3 0 4.20 0.70
8 3 0 3.30 1.00
-8 3 0 3.20 0.50
8 3 0 3.50 0.60
9 -3 0 0.60 0.60
9 -3 0 1.90 0.60
9 3 0 1.30 0.90
-9 3 0 0.50 0.40
10 -3 0 0.20 0.50
10 3 0 0.20 1.00
11 -3 0 11.00 1.20
11 3 0 11.30 1.80
12 -3 0 95.39 3.60
12 3 0 96.59 4.60
13 -3 0 80.49 3.40
13 3 0 92.79 4.60
14 3 0 3.10 1.60
0 -4 0 188.08 5.40
1 -4 0 66.19 2.20
-1 -4 0 65.19 2.20
-2 -4 0 1.20 0.40
2 -4 0 1.70 0.40
-3 -4 0 347.57 9.30
3 -4 0 343.27 9.40
-3 4 0 348.57 9.40
4 -4 0 70.79 2.50
-4 -4 0 77.69 2.40
-4 4 0 69.09 2.40
4 4 0 79.99 2.40
5 -4 0 85.49 2.80
-5 -4 0 80.69 2.60
5 4 0 85.49 3.30
5 4 0 81.59 2.60
-5 4 0 85.49 2.70
-6 -4 0 2.90 0.50
6 -4 0 1.60 0.50
-6 4 0 1.30 0.40
6 4 0 1.50 0.80
6 4 0 2.00 0.50
7 -4 0 27.50 1.40
-7 4 0 26.60 1.30
7 4 0 27.20 2.00
7 4 0 28.30 1.30
8 -4 0 0.00 0.50
8 4 0 0.10 0.90
-8 4 0 0.30 0.40
8 4 0 0.50 0.70
9 -4 0 8.30 1.00
9 4 0 7.30 1.40
-9 4 0 7.40 0.80
10 4 0 1.60 1.10
11 -4 0 0.00 0.60
11 4 0 -0.80 1.00
12 -4 0 0.00 0.60
12 4 0 -0.40 1.20
13 -4 0 9.00 1.30
13 4 0 12.80 2.10
0 -5 0 0.50 0.40
1 -5 0 128.39 4.00
-1 -5 0 131.39 4.00
-2 -5 0 77.59 2.70
2 -5 0 82.49 2.80
-3 -5 0 31.20 1.40
-3 5 0 28.70 1.40
4 -5 0 98.09 3.30
-4 -5 0 102.29 3.20
4 5 0 97.79 3.10
-4 5 0 95.99 3.20
-5 -5 0 2.30 0.50
5 -5 0 1.40 0.50
5 5 0 1.30 0.40
-5 5 0 1.70 0.40
5 5 0 1.50 0.80
6 -5 0 54.59 2.20
-6 -5 0 48.40 1.90
-6 5 0 49.70 2.00
6 5 0 54.69 1.90
6 5 0 51.79 2.70
7 -5 0 14.80 1.20
7 5 0 17.00 1.80
-7 5 0 15.40 1.00
7 5 0 14.40 1.00
8 -5 0 40.20 2.00
-8 5 0 39.50 1.70
8 5 0 37.90 2.60
9 -5 0 76.29 3.00
9 5 0 77.29 3.80
-9 5 0 76.89 2.80
10 -5 0 1.40 0.70
10 5 0 1.00 1.10
11 -5 0 0.50 0.70
11 5 0 0.50 1.10
12 -5 0 0.90 0.80
12 5 0 -0.20 1.20
13 -5 0 0.20 0.80
13 5 0 1.00 1.40
0 -6 0 22.60 1.30
1 -6 0 1.00 0.50
-1 -6 0 0.50 0.40
-2 -6 0 123.79 4.00
-3 -6 0 21.90 1.30
-3 6 0 20.10 1.20
-4 -6 0 29.00 1.50
-4 6 0 29.50 1.50
-5 -6 0 17.70 1.20
5 -6 0 20.00 1.30
5 6 0 19.80 1.10
-5 6 0 19.50 1.20
5 6 0 19.00 1.70
6 -6 0 245.38 7.10
-6 -6 0 225.78 7.20
-6 6 0 235.58 6.80
6 6 0 229.58 6.70
6 6 0 238.98 7.60
7 -6 0 154.98 5.00
-7 6 0 149.88 4.80
7 6 0 155.98 5.60
8 -6 0 3.70 0.80
-8 6 0 2.90 0.60
8 6 0 2.80 1.10
9 -6 0 12.40 1.30
9 6 0 10.90 1.70
-9 6 0 12.50 1.10
10 -6 0 -0.90 0.60
-10 6 0 -0.10 0.50
10 6 0 -1.10 1.00
11 -6 0 3.70 1.00
11 6 0 3.50 1.40
12 -6 0 -0.50 0.70
12 6 0 -0.20 1.20
13 -6 0 0.10 0.80
0 -7 0 1.10 0.50
-1 -7 0 59.19 2.40
1 -7 0 58.49 2.40
-2 -7 0 49.50 2.20
-3 -7 0 26.20 1.50
-3 7 0 22.80 1.40
-4 -7 0 150.28 4.70
-4 7 0 144.19 4.60
-5 -7 0 206.38 6.10
-5 7 0 196.08 6.00
5 7 0 198.78 5.90
5 7 0 200.08 6.70
6 7 0 11.20 1.50
-6 7 0 13.30 1.10
7 7 0 43.70 2.70
-7 7 0 41.50 2.00
8 -7 0 4.30 1.00
8 7 0 5.00 1.30
-8 7 0 4.20 0.80
9 -7 0 4.60 1.00
-9 7 0 6.50 0.90
9 7 0 6.20 1.50
10 -7 0 1.10 0.80
-10 7 0 0.80 0.60
10 7 0 0.30 1.10
11 -7 0 16.00 1.70
11 7 0 15.20 2.10
12 -7 0 1.50 1.00
12 7 0 2.40 1.50
0 -8 0 1321.77 34.70
-1 -8 0 78.09 3.10
1 -8 0 83.99 3.20
-2 -8 0 12.00 1.20
-3 -8 0 25.70 1.70
-3 8 0 28.80 1.60
-4 -8 0 331.87 9.70
-4 8 0 343.87 9.70
-5 -8 0 73.49 2.90
5 8 0 69.29 3.30
-5 8 0 69.69 2.80
6 8 0 15.60 1.90
-6 8 0 17.50 1.30
-7 8 0 9.00 1.00
7 8 0 8.50 1.50
8 8 0 69.99 3.70
-8 8 0 73.59 2.90
-9 8 0 0.60 0.60
9 8 0 0.20 1.00
10 8 0 8.60 1.80
-10 8 0 7.60 1.10
11 8 0 -0.30 1.10
0 -9 0 0.20 0.70
-1 -9 0 24.90 1.80
-2 -9 0 27.70 1.80
-2 9 0 31.20 1.80
-3 -9 0 180.78 5.90
-3 9 0 178.68 5.70
-4 -9 0 18.50 1.50
4 9 0 17.20 1.90
-4 9 0 19.30 1.50
-5 -9 0 15.60 1.80
-5 9 0 21.90 1.50
5 9 0 25.40 2.10
6 9 0 36.30 2.60
-6 9 0 35.40 2.00
7 9 0 29.80 2.50
-7 9 0 27.50 1.80
8 9 0 3.20 1.30
-8 9 0 2.80 0.80
-9 9 0 8.50 1.10
9 9 0 8.60 1.70
10 9 0 36.00 3.10
-10 9 0 37.60 2.20
-1 -10 0 3.40 0.90
-1 10 0 2.40 0.80
-2 -10 0 256.87 8.40
-2 10 0 292.97 8.40
-3 -10 0 5.20 1.00
-3 10 0 2.70 0.80
-4 -10 0 17.80 1.60
-4 10 0 14.90 1.50
5 10 0 3.30 1.30
-5 10 0 3.90 0.90
6 10 0 12.70 1.80
-6 10 0 13.80 1.50
7 10 0 -0.30 1.00
-7 10 0 -0.50 0.60
-8 10 0 2.40 0.80
8 10 0 1.60 1.30
-9 10 0 24.00 1.80
9 10 0 22.70 2.60
0 11 0 -0.10 0.60
-1 11 0 0.50 0.70
-2 -11 0 2.20 0.90
-2 11 0 2.60 0.80
-3 -11 0 34.30 2.30
-3 11 0 43.30 2.40
-4 -11 0 23.30 1.90
-4 11 0 27.00 1.90
-5 11 0 1.10 0.80
-6 11 0 19.60 1.70
-7 11 0 0.90 0.80
-8 11 0 1.50 0.80
8 11 0 0.90 1.30
0 12 0 27.40 2.00
1 12 0 0.50 0.70
-1 12 0 0.30 0.70
-2 12 0 -0.30 0.70
-3 12 0 0.50 0.80
-4 12 0 29.30 2.20
-5 12 0 -0.40 0.70
0 13 0 0.60 0.80
-1 13 0 -0.20 0.80
1 13 0 -0.30 0.70
-2 13 0 8.70 1.70
2 13 0 7.50 1.30
3 13 0 4.10 1.00
14 0 -1 1.40 1.10
13 0 -1 119.49 5.00
12 0 -1 -1.10 0.90
12 0 -1 0.00 0.50
11 0 -1 129.29 5.00
11 0 -1 128.59 4.20
10 0 -1 0.10 0.40
10 0 -1 -0.50 0.80
9 0 -1 12.90 1.50
9 0 -1 11.20 0.90
8 0 -1 0.20 0.60
8 0 -1 -0.10 0.30
7 0 -1 192.68 5.90
7 0 -1 189.88 5.40
-7 0 1 186.78 5.10
6 0 -1 -0.10 0.50
-6 0 1 -0.10 0.20
6 0 -1 -0.10 0.30
5 0 -1 289.07 7.70
-5 0 1 288.67 7.50
5 0 -1 283.07 8.10
-4 0 1 0.00 0.10
4 0 -1 0.10 0.30
4 0 -1 -0.10 0.20
-3 0 1 649.14 16.70
3 0 -1 647.84 17.10
2 0 -1 -2.50 0.10
1 0 -1 260.67 7.00
0 0 -1 -2.40 0.10
-1 0 -1 346.57 9.30
1 0 1 354.76 9.20
1 0 1 352.36 9.20
2 0 1 0.10 0.10
2 0 1 0.10 0.30
-2 0 -1 0.10 0.20
-3 0 -1 7481.85 205.38
3 0 1 7355.46 210.08
3 0 1 7691.63 204.68
4 0 1 -0.30 0.30
4 0 1 -0.10 0.20
-4 0 -1 -0.10 0.20
5 0 1 68.49 2.10
-5 0 -1 65.19 2.10
5 0 1 66.99 2.50
6 0 1 0.00 0.20
6 0 1 0.40 0.50
-6 0 -1 -0.10 0.30
-7 0 -1 49.90 1.80
7 0 1 51.79 1.80
7 0 1 49.60 2.30
8 0 1 -0.40 0.30
-8 0 -1 -0.20 0.30
8 0 1 -0.10 0.60
9 0 1 2.70 0.50
9 0 1 2.20 0.90
10 0 1 -0.20 0.80
10 0 1 0.00 0.40
11 0 1 6.10 1.30
12 0 1 0.80 1.10
13 0 1 3.90 1.30
14 0 1 -0.10 1.10
15 1 -1 12.10 2.00
14 1 -1 0.20 1.10
13 -1 -1 13.30 2.10
13 1 -1 12.60 1.90
12 -1 -1 4.90 0.90
12 -1 -1 4.70 1.20
12 1 -1 4.40 1.30
11 -1 -1 0.70 0.90
11 -1 -1 0.40 0.50
11 1 -1 0.60 1.00
11 1 -1 1.60 0.60
10 -1 -1 92.89 3.20
10 -1 -1 96.09 3.80
10 1 -1 91.39 4.00
10 1 -1 97.39 3.20
9 -1 -1 4.20 0.70
9 -1 -1 2.40 0.90
9 1 -1 4.00 0.60
9 1 -1 2.80 0.90
8 -1 -1 231.68 7.00
8 -1 -1 232.98 6.60
8 1 -1 238.58 6.50
8 1 -1 235.28 7.30
-8 1 1 228.08 6.40
7 -1 -1 51.49 2.20
7 -1 -1 48.80 1.80
-7 -1 1 50.39 1.60
7 1 -1 47.50 2.30
-7 1 1 51.29 1.60
7 1 -1 51.99 1.80
6 -1 -1 -0.10 0.40
6 -1 -1 -0.10 0.30
-6 -1 1 0.00 0.20
6 1 -1 0.20 0.30
6 1 -1 -0.10 0.50
-6 1 1 0.00 0.20
5 -1 -1 65.39 2.30
-5 -1 1 62.19 1.80
5 -1 -1 64.49 2.00
5 1 -1 62.49 2.00
-5 1 1 63.39 1.90
-4 -1 1 114.79 3.20
4 -1 -1 124.69 3.50
4 -1 -1 115.59 3.40
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4 0 -18 6.80 1.40
3 0 -18 -0.10 1.00
5 -1 -18 -0.10 0.90
5 1 -18 0.40 1.40
4 -1 -18 0.40 1.00
4 1 -18 1.20 1.10
3 -1 -18 2.10 1.20
3 1 -18 0.90 1.10
6 -2 -18 0.40 1.30
5 -2 -18 0.40 0.90
4 -2 -18 2.50 1.10
4 2 -18 1.30 1.20
3 2 -18 4.40 1.40
6 -3 -18 5.90 1.30
5 -3 -18 14.90 1.90
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 90666
_shelx_res_file
;
TITL m1cg
CELL 0.71073 12.2358 10.3185 14.2310 90.000 111.199 90.000
ZERR 4.000 0.0016 0.0014 0.0019 0.000 0.002 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H N O F
UNIT 76 76 8 12 4
OMIT -2 180.0
L.S. 20
ACTA
BOND $H
CONF
HTAB
OMIT 12 1 6
OMIT 12 0 6
OMIT 11 1 6
OMIT 10 1 7
OMIT 10 1 8
OMIT 10 0 8
OMIT 10 1 6
OMIT 10 2 8
OMIT 9 1 7
OMIT 9 0 7
OMIT 10 2 7
OMIT 11 1 7
OMIT 11 1 5
OMIT 11 0 5
OMIT 10 0 6
FMAP 2
PLAN 20
SIZE 0.479 0.293 0.282
TEMP -100
WGHT 0.047600 0.471300
FVAR 0.56895
N1 3 0.572121 0.474757 0.269542 11.00000 0.03280 0.02768 =
0.03228 0.00332 0.01405 0.00185
C2 1 0.512231 0.447816 0.339845 11.00000 0.03066 0.03414 =
0.03382 0.01059 0.01127 0.00214
AFIX 23
H2A 2 0.562161 0.391831 0.395240 11.00000 -1.20000
H2B 2 0.437890 0.401360 0.304338 11.00000 -1.20000
AFIX 0
C3 1 0.486939 0.574002 0.382722 11.00000 0.03485 0.04444 =
0.02745 0.00798 0.01137 0.00755
AFIX 23
H3A 2 0.443830 0.555984 0.428265 11.00000 -1.20000
H3B 2 0.561595 0.617346 0.422374 11.00000 -1.20000
AFIX 0
N4 3 0.416967 0.659032 0.300927 11.00000 0.03733 0.03455 =
0.02833 0.00676 0.01448 0.00675
C5 1 0.470877 0.682728 0.225515 11.00000 0.03885 0.02997 =
0.03165 0.00606 0.01572 0.00147
AFIX 23
H5A 2 0.544371 0.732534 0.256395 11.00000 -1.20000
H5B 2 0.416951 0.734362 0.169136 11.00000 -1.20000
AFIX 0
C6 1 0.497044 0.554524 0.186093 11.00000 0.03499 0.03105 =
0.02846 0.00254 0.01213 -0.00049
AFIX 23
H6A 2 0.422788 0.508095 0.150241 11.00000 -1.20000
H6B 2 0.536760 0.570402 0.137668 11.00000 -1.20000
AFIX 0
C11 1 0.607112 0.354977 0.232875 11.00000 0.04083 0.02762 =
0.04269 0.00085 0.01603 0.00067
AFIX 23
H11A 2 0.536708 0.312427 0.184481 11.00000 -1.20000
H11B 2 0.642415 0.295113 0.290268 11.00000 -1.20000
AFIX 0
O11 4 0.951611 0.444489 0.065434 11.00000 0.05124 0.05036 =
0.04469 -0.00925 0.02748 -0.00155
C12 1 1.013873 0.544638 0.133221 11.00000 0.03998 0.05241 =
0.04694 -0.00539 0.02087 0.00131
AFIX 23
H12A 2 1.098377 0.523170 0.162415 11.00000 -1.20000
H12B 2 1.004920 0.627934 0.096668 11.00000 -1.20000
AFIX 0
O13 4 0.967225 0.555518 0.211406 11.00000 0.04256 0.05110 =
0.04778 -0.01464 0.02314 -0.00857
C3A 1 0.867869 0.480564 0.181106 11.00000 0.03251 0.02793 =
0.03175 -0.00060 0.00824 0.00593
C14 1 0.787692 0.465906 0.227177 11.00000 0.03670 0.03060 =
0.02901 -0.00220 0.01134 0.00476
AFIX 43
H14 2 0.795046 0.511809 0.287029 11.00000 -1.20000
AFIX 0
C15 1 0.694102 0.379991 0.182013 11.00000 0.03506 0.02725 =
0.03445 0.00130 0.01082 0.00637
C16 1 0.684860 0.315738 0.093690 11.00000 0.03582 0.03435 =
0.03911 -0.00677 0.00657 0.00298
AFIX 43
H16 2 0.620332 0.259210 0.063589 11.00000 -1.20000
AFIX 0
C17 1 0.767618 0.331557 0.047502 11.00000 0.04648 0.03877 =
0.03243 -0.00727 0.01175 0.00766
AFIX 43
H17 2 0.761030 0.286915 -0.012690 11.00000 -1.20000
AFIX 0
C7A 1 0.858012 0.414323 0.093465 11.00000 0.04014 0.03305 =
0.03305 0.00227 0.01596 0.01093
C47 1 0.321035 0.724612 0.297971 11.00000 0.03686 0.02604 =
0.03698 0.00594 0.01502 0.00179
O47 4 0.274752 0.806262 0.232905 11.00000 0.06241 0.05764 =
0.06863 0.03854 0.04011 0.03030
C41 1 0.267845 0.698234 0.376498 11.00000 0.02633 0.02796 =
0.03034 0.00364 0.00707 0.00192
C42 1 0.221514 0.577225 0.385443 11.00000 0.04003 0.02684 =
0.03289 0.00017 0.01284 -0.00012
AFIX 43
H42 2 0.230621 0.504904 0.347614 11.00000 -1.20000
AFIX 0
C43 1 0.162093 0.566070 0.450976 11.00000 0.03827 0.03107 =
0.03977 0.00683 0.01295 -0.00474
F43 5 0.113738 0.449716 0.457752 11.00000 0.07592 0.03784 =
0.07565 0.00611 0.04244 -0.01424
C44 1 0.148668 0.666158 0.509515 11.00000 0.03424 0.04661 =
0.03365 0.00582 0.01413 0.00275
AFIX 43
H44 2 0.107919 0.654158 0.554410 11.00000 -1.20000
AFIX 0
C45 1 0.196600 0.785313 0.500876 11.00000 0.03677 0.03820 =
0.03870 -0.00642 0.01275 0.00205
AFIX 43
H45 2 0.189600 0.856258 0.540875 11.00000 -1.20000
AFIX 0
C46 1 0.254587 0.801409 0.434279 11.00000 0.03319 0.02704 =
0.04310 -0.00062 0.01350 -0.00198
AFIX 43
H46 2 0.285689 0.883927 0.427981 11.00000 -1.20000
AFIX 0
HKLF 4
REM m1cg
REM R1 = 0.0397 for 2975 Fo > 4sig(Fo) and 0.0502 for all 3674 data
REM 226 parameters refined using 0 restraints
END
WGHT 0.0476 0.4712
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1/2, y-1/2, -z+1/2
HTAB C2 O47_$1
HTAB C42 O47_$1
REM Highest difference peak 0.238, deepest hole -0.179, 1-sigma level 0.038
Q1 1 0.8627 0.4553 0.1329 11.00000 0.05 0.20
Q2 1 0.3000 0.7087 0.3453 11.00000 0.05 0.20
Q3 1 0.2392 0.5622 0.4534 11.00000 0.05 0.20
Q4 1 0.1977 0.5960 0.5110 11.00000 0.05 0.19
Q5 1 0.6611 0.3645 0.2116 11.00000 0.05 0.18
Q6 1 0.4682 0.6161 0.1970 11.00000 0.05 0.18
Q7 1 0.4418 0.6729 0.2613 11.00000 0.05 0.18
Q8 1 0.7082 0.3217 0.1578 11.00000 0.05 0.18
Q9 1 0.8130 0.5010 0.1874 11.00000 0.05 0.18
Q10 1 0.5329 0.4635 0.2961 11.00000 0.05 0.17
Q11 1 0.1559 0.5828 0.3940 11.00000 0.05 0.17
Q12 1 0.6677 0.3816 0.1248 11.00000 0.05 0.17
Q13 1 0.7222 0.4602 0.1844 11.00000 0.05 0.17
Q14 1 0.8978 0.5954 0.1598 11.00000 0.05 0.16
Q15 1 0.1534 0.7353 0.4873 11.00000 0.05 0.16
Q16 1 0.2625 0.7765 0.5001 11.00000 0.05 0.16
Q17 1 0.3796 0.6971 0.3059 11.00000 0.05 0.16
Q18 1 0.6216 0.5137 0.3035 11.00000 0.05 0.15
Q19 1 0.2994 0.7386 0.4290 11.00000 0.05 0.15
Q20 1 0.5451 0.5210 0.2375 11.00000 0.05 0.15
;
_shelx_res_checksum 24443
_shelxl_version_number 2.014
data_II
_database_code_depnum_ccdc_archive 'CCDC 1889709'
_audit_creation_method SHELXL-2014
_chemical_name_systematic
;
1-[(1,3-Benzodioxol-5-yl)methyl]-4-(2,6-difluorobenzoyl)piperazine
;
_chemical_name_common ?
_chemical_formula_moiety 'C19 H18 F2 N2 O3'
_chemical_formula_sum 'C19 H18 F2 N2 O3'
_chemical_formula_iupac 'C19 H18 F2 N2 O3'
_chemical_formula_weight 360.35
_chemical_melting_point ?
_chemical_absolute_configuration unk
_space_group_crystal_system orthorhombic
_space_group_name_H-M_alt 'P c a 21'
_space_group_name_Hall 'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
_cell_length_a 14.2762(9)
_cell_length_b 15.9821(10)
_cell_length_c 7.3753(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1682.78(19)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 3743
_cell_measurement_theta_min 1.913
_cell_measurement_theta_max 27.503
_cell_measurement_temperature 173(2)
_exptl_crystal_description needle
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.910
_exptl_crystal_size_mid 0.352
_exptl_crystal_size_min 0.168
_exptl_crystal_density_diffrn 1.422
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_F_000 752
_exptl_absorpt_coefficient_mu 0.112
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_absorpt_correction_T_min 0.587
_exptl_absorpt_correction_T_max 0.981
_exptl_special_details ?
_diffrn_ambient_temperature 173(2)
_diffrn_source 'fine focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean 0.3333
_diffrn_reflns_number 9016
_diffrn_reflns_av_R_equivalents 0.0569
_diffrn_reflns_av_unetI/netI 0.0522
_diffrn_reflns_theta_min 1.913
_diffrn_reflns_theta_max 27.503
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_limit_l_max 9
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_refine_special_details ?
_reflns_number_total 3743
_reflns_number_gt 3449
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0560
_refine_ls_R_factor_gt 0.0535
_refine_ls_wR_factor_gt 0.1526
_refine_ls_wR_factor_ref 0.1550
_refine_ls_goodness_of_fit_ref 1.161
_refine_ls_restrained_S_all 1.161
_refine_ls_number_reflns 3743
_refine_ls_number_parameters 235
_refine_ls_number_restraints 1
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0960P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.171
_refine_diff_density_min -0.215
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_abs_structure_details
;
Flack x determined using 1369 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
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'
'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'
'F' 'F' 0.0171 0.0103
'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'
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2014 and PLATON (Spek, 2009)
;
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N N1 0.36051(17) 0.62727(15) 0.3017(3) 0.0249(5) Uani d 1 . .
C C2 0.3856(2) 0.71107(18) 0.2369(5) 0.0302(6) Uani d 1 . .
H H2A 0.3597 0.7197 0.1138 0.036 Uiso calc 1 . .
H H2B 0.4546 0.7163 0.2299 0.036 Uiso calc 1 . .
C C3 0.3470(2) 0.77682(17) 0.3641(4) 0.0302(6) Uani d 1 . .
H H3A 0.3686 0.8328 0.3249 0.036 Uiso calc 1 . .
H H3B 0.2777 0.7762 0.3590 0.036 Uiso calc 1 . .
N N4 0.37766(17) 0.76146(14) 0.5509(4) 0.0265(5) Uani d 1 . .
C C5 0.3658(2) 0.67513(15) 0.6138(4) 0.0247(5) Uani d 1 . .
H H5A 0.2984 0.6633 0.6317 0.030 Uiso calc 1 . .
H H5B 0.3979 0.6679 0.7317 0.030 Uiso calc 1 . .
C C6 0.40582(18) 0.61456(18) 0.4776(4) 0.0243(6) Uani d 1 . .
H H6A 0.4742 0.6236 0.4659 0.029 Uiso calc 1 . .
H H6B 0.3953 0.5564 0.5193 0.029 Uiso calc 1 . .
C C11 0.3880(2) 0.5620(2) 0.1720(4) 0.0320(7) Uani d 1 . .
H H11A 0.4569 0.5628 0.1566 0.038 Uiso calc 1 . .
H H11B 0.3592 0.5740 0.0526 0.038 Uiso calc 1 . .
O O11 0.26117(18) 0.25056(13) 0.4272(4) 0.0445(6) Uani d 1 . .
C C12 0.1638(3) 0.2617(2) 0.3896(6) 0.0426(8) Uani d 1 . .
H H12A 0.1431 0.2208 0.2971 0.051 Uiso calc 1 . .
H H12B 0.1266 0.2526 0.5011 0.051 Uiso calc 1 . .
O O13 0.15012(16) 0.34454(15) 0.3247(4) 0.0436(6) Uani d 1 . .
C C3A 0.2382(2) 0.37818(18) 0.3049(5) 0.0295(6) Uani d 1 . .
C C14 0.2621(2) 0.45542(17) 0.2400(4) 0.0299(6) Uani d 1 . .
H H14 0.2157 0.4937 0.1993 0.036 Uiso calc 1 . .
C C15 0.35761(19) 0.47614(18) 0.2356(4) 0.0276(6) Uani d 1 . .
C C16 0.4231(2) 0.4189(2) 0.2983(4) 0.0309(6) Uani d 1 . .
H H16 0.4875 0.4339 0.2961 0.037 Uiso calc 1 . .
C C17 0.3983(2) 0.34019(19) 0.3646(5) 0.0336(7) Uani d 1 . .
H H17 0.4438 0.3015 0.4067 0.040 Uiso calc 1 . .
C C7A 0.3045(2) 0.32183(18) 0.3656(4) 0.0317(6) Uani d 1 . .
C C47 0.4015(2) 0.82057(17) 0.6718(4) 0.0262(6) Uani d 1 . .
O O47 0.41835(17) 0.80559(13) 0.8317(3) 0.0366(5) Uani d 1 . .
C C41 0.4064(2) 0.91022(16) 0.6064(5) 0.0277(6) Uani d 1 . .
C C42 0.3281(2) 0.96071(19) 0.5945(6) 0.0384(8) Uani d 1 . .
F F42 0.24359(14) 0.92331(12) 0.6222(4) 0.0620(8) Uani d 1 . .
C C43 0.3316(3) 1.0447(2) 0.5555(7) 0.0476(9) Uani d 1 . .
H H43 0.2760 1.0772 0.5492 0.057 Uiso calc 1 . .
C C44 0.4181(3) 1.0804(2) 0.5258(5) 0.0432(9) Uani d 1 . .
H H44 0.4221 1.1383 0.4980 0.052 Uiso calc 1 . .
C C45 0.4992(2) 1.03346(19) 0.5357(5) 0.0375(8) Uani d 1 . .
H H45 0.5587 1.0584 0.5158 0.045 Uiso calc 1 . .
C C46 0.4913(2) 0.94955(18) 0.5754(5) 0.0303(6) Uani d 1 . .
F F46 0.56966(12) 0.90206(13) 0.5843(4) 0.0464(6) Uani d 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N1 0.0308(11) 0.0227(11) 0.0214(11) -0.0015(9) -0.0005(9) 0.0023(9)
C2 0.0356(14) 0.0296(15) 0.0254(14) -0.0041(12) -0.0029(12) 0.0090(13)
C3 0.0399(14) 0.0214(12) 0.0293(16) -0.0025(11) -0.0088(12) 0.0068(12)
N4 0.0347(11) 0.0173(10) 0.0274(13) -0.0015(9) -0.0039(10) 0.0052(9)
C5 0.0328(12) 0.0169(11) 0.0243(13) -0.0024(10) -0.0002(11) 0.0029(11)
C6 0.0267(12) 0.0220(13) 0.0241(14) 0.0012(10) 0.0000(11) 0.0044(11)
C11 0.0400(15) 0.0328(15) 0.0232(14) 0.0002(13) 0.0051(12) -0.0003(12)
O11 0.0469(14) 0.0305(11) 0.0563(17) 0.0005(10) -0.0008(12) 0.0081(11)
C12 0.0465(19) 0.0387(17) 0.043(2) -0.0081(14) -0.0024(15) -0.0013(15)
O13 0.0332(11) 0.0427(13) 0.0547(16) -0.0046(10) -0.0009(11) 0.0050(12)
C3A 0.0282(13) 0.0343(14) 0.0260(14) 0.0040(12) -0.0012(11) -0.0043(12)
C14 0.0338(13) 0.0308(13) 0.0252(14) 0.0072(12) -0.0048(12) -0.0008(13)
C15 0.0371(14) 0.0266(13) 0.0191(12) 0.0031(11) 0.0018(11) -0.0044(11)
C16 0.0283(12) 0.0336(16) 0.0307(15) 0.0059(11) 0.0018(12) -0.0063(13)
C17 0.0374(14) 0.0270(14) 0.0365(17) 0.0093(12) -0.0025(13) -0.0011(13)
C7A 0.0420(15) 0.0242(13) 0.0289(16) 0.0036(12) 0.0004(13) -0.0027(12)
C47 0.0293(11) 0.0188(12) 0.0304(15) -0.0014(10) -0.0014(11) 0.0043(11)
O47 0.0560(13) 0.0233(10) 0.0305(13) -0.0055(9) -0.0064(10) 0.0021(9)
C41 0.0365(14) 0.0183(12) 0.0284(15) -0.0031(11) -0.0002(12) 0.0023(11)
C42 0.0344(14) 0.0295(16) 0.051(2) -0.0016(12) 0.0038(14) 0.0095(15)
F42 0.0323(9) 0.0451(11) 0.109(2) -0.0006(10) 0.0056(12) 0.0293(14)
C43 0.0502(19) 0.0283(16) 0.064(3) 0.0091(14) 0.0094(18) 0.0128(16)
C44 0.068(2) 0.0187(14) 0.043(2) -0.0038(14) 0.0079(17) 0.0061(13)
C45 0.0461(17) 0.0282(14) 0.038(2) -0.0127(14) 0.0074(13) 0.0019(14)
C46 0.0331(14) 0.0265(13) 0.0313(17) -0.0021(11) 0.0026(12) 0.0003(13)
F46 0.0330(9) 0.0404(11) 0.0658(16) 0.0006(8) 0.0054(10) 0.0060(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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 C6 . 1.464(4) ?
N1 C2 . 1.466(3) ?
N1 C11 . 1.469(4) ?
C2 C3 . 1.513(4) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 N4 . 1.466(4) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
N4 C47 . 1.343(4) ?
N4 C5 . 1.465(3) ?
C5 C6 . 1.507(4) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C11 C15 . 1.514(4) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
O11 C7A . 1.374(4) ?
O11 C12 . 1.429(4) ?
C12 O13 . 1.422(4) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
O13 C3A . 1.375(4) ?
C3A C14 . 1.367(4) ?
C3A C7A . 1.381(4) ?
C14 C15 . 1.404(4) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.388(4) ?
C16 C17 . 1.395(5) ?
C16 H16 . 0.9500 ?
C17 C7A . 1.370(4) ?
C17 H17 . 0.9500 ?
C47 O47 . 1.227(4) ?
C47 C41 . 1.513(4) ?
C41 C42 . 1.382(4) ?
C41 C46 . 1.384(4) ?
C42 F42 . 1.362(3) ?
C42 C43 . 1.373(4) ?
C43 C44 . 1.379(5) ?
C43 H43 . 0.9500 ?
C44 C45 . 1.381(5) ?
C44 H44 . 0.9500 ?
C45 C46 . 1.377(4) ?
C45 H45 . 0.9500 ?
C46 F46 . 1.354(3) ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 N1 C2 . . 107.9(2) ?
C6 N1 C11 . . 111.2(2) ?
C2 N1 C11 . . 111.8(2) ?
N1 C2 C3 . . 110.1(3) ?
N1 C2 H2A . . 109.6 ?
C3 C2 H2A . . 109.6 ?
N1 C2 H2B . . 109.6 ?
C3 C2 H2B . . 109.6 ?
H2A C2 H2B . . 108.2 ?
N4 C3 C2 . . 111.0(2) ?
N4 C3 H3A . . 109.4 ?
C2 C3 H3A . . 109.4 ?
N4 C3 H3B . . 109.4 ?
C2 C3 H3B . . 109.4 ?
H3A C3 H3B . . 108.0 ?
C47 N4 C5 . . 118.8(3) ?
C47 N4 C3 . . 125.6(2) ?
C5 N4 C3 . . 114.9(2) ?
N4 C5 C6 . . 110.5(2) ?
N4 C5 H5A . . 109.6 ?
C6 C5 H5A . . 109.6 ?
N4 C5 H5B . . 109.6 ?
C6 C5 H5B . . 109.6 ?
H5A C5 H5B . . 108.1 ?
N1 C6 C5 . . 109.5(2) ?
N1 C6 H6A . . 109.8 ?
C5 C6 H6A . . 109.8 ?
N1 C6 H6B . . 109.8 ?
C5 C6 H6B . . 109.8 ?
H6A C6 H6B . . 108.2 ?
N1 C11 C15 . . 111.4(2) ?
N1 C11 H11A . . 109.3 ?
C15 C11 H11A . . 109.3 ?
N1 C11 H11B . . 109.3 ?
C15 C11 H11B . . 109.3 ?
H11A C11 H11B . . 108.0 ?
C7A O11 C12 . . 105.7(2) ?
O13 C12 O11 . . 108.4(3) ?
O13 C12 H12A . . 110.0 ?
O11 C12 H12A . . 110.0 ?
O13 C12 H12B . . 110.0 ?
O11 C12 H12B . . 110.0 ?
H12A C12 H12B . . 108.4 ?
C3A O13 C12 . . 105.9(2) ?
C14 C3A O13 . . 128.2(3) ?
C14 C3A C7A . . 122.1(3) ?
O13 C3A C7A . . 109.7(3) ?
C3A C14 C15 . . 117.6(3) ?
C3A C14 H14 . . 121.2 ?
C15 C14 H14 . . 121.2 ?
C16 C15 C14 . . 119.4(3) ?
C16 C15 C11 . . 120.5(3) ?
C14 C15 C11 . . 120.0(3) ?
C15 C16 C17 . . 122.6(3) ?
C15 C16 H16 . . 118.7 ?
C17 C16 H16 . . 118.7 ?
C7A C17 C16 . . 116.3(3) ?
C7A C17 H17 . . 121.8 ?
C16 C17 H17 . . 121.8 ?
C17 C7A O11 . . 128.3(3) ?
C17 C7A C3A . . 121.9(3) ?
O11 C7A C3A . . 109.8(3) ?
O47 C47 N4 . . 123.4(3) ?
O47 C47 C41 . . 118.8(3) ?
N4 C47 C41 . . 117.8(3) ?
C42 C41 C46 . . 115.6(2) ?
C42 C41 C47 . . 122.4(2) ?
C46 C41 C47 . . 121.6(3) ?
F42 C42 C43 . . 119.5(3) ?
F42 C42 C41 . . 116.8(2) ?
C43 C42 C41 . . 123.7(3) ?
C42 C43 C44 . . 118.0(3) ?
C42 C43 H43 . . 121.0 ?
C44 C43 H43 . . 121.0 ?
C43 C44 C45 . . 121.2(3) ?
C43 C44 H44 . . 119.4 ?
C45 C44 H44 . . 119.4 ?
C46 C45 C44 . . 118.1(3) ?
C46 C45 H45 . . 120.9 ?
C44 C45 H45 . . 120.9 ?
F46 C46 C45 . . 119.2(3) ?
F46 C46 C41 . . 117.4(2) ?
C45 C46 C41 . . 123.3(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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 N1 C2 C3 . . . . -63.5(3) ?
C11 N1 C2 C3 . . . . 173.9(2) ?
N1 C2 C3 N4 . . . . 54.5(3) ?
C2 C3 N4 C47 . . . . 142.2(3) ?
C2 C3 N4 C5 . . . . -48.1(3) ?
C47 N4 C5 C6 . . . . -140.1(3) ?
C3 N4 C5 C6 . . . . 49.5(3) ?
C2 N1 C6 C5 . . . . 65.0(3) ?
C11 N1 C6 C5 . . . . -172.1(2) ?
N4 C5 C6 N1 . . . . -57.3(3) ?
C6 N1 C11 C15 . . . . 62.1(3) ?
C2 N1 C11 C15 . . . . -177.2(2) ?
C7A O11 C12 O13 . . . . -6.7(4) ?
O11 C12 O13 C3A . . . . 6.5(4) ?
C12 O13 C3A C14 . . . . 177.4(3) ?
C12 O13 C3A C7A . . . . -3.9(4) ?
O13 C3A C14 C15 . . . . 179.0(3) ?
C7A C3A C14 C15 . . . . 0.4(5) ?
C3A C14 C15 C16 . . . . -0.8(4) ?
C3A C14 C15 C11 . . . . -177.6(3) ?
N1 C11 C15 C16 . . . . -107.8(3) ?
N1 C11 C15 C14 . . . . 69.0(4) ?
C14 C15 C16 C17 . . . . 0.8(5) ?
C11 C15 C16 C17 . . . . 177.6(3) ?
C15 C16 C17 C7A . . . . -0.3(5) ?
C16 C17 C7A O11 . . . . -178.2(3) ?
C16 C17 C7A C3A . . . . -0.2(5) ?
C12 O11 C7A C17 . . . . -177.4(4) ?
C12 O11 C7A C3A . . . . 4.4(4) ?
C14 C3A C7A C17 . . . . 0.1(5) ?
O13 C3A C7A C17 . . . . -178.7(3) ?
C14 C3A C7A O11 . . . . 178.5(3) ?
O13 C3A C7A O11 . . . . -0.4(4) ?
C5 N4 C47 O47 . . . . 3.6(4) ?
C3 N4 C47 O47 . . . . 173.0(3) ?
C5 N4 C47 C41 . . . . -175.7(2) ?
C3 N4 C47 C41 . . . . -6.3(4) ?
O47 C47 C41 C42 . . . . -95.9(4) ?
N4 C47 C41 C42 . . . . 83.4(4) ?
O47 C47 C41 C46 . . . . 76.3(4) ?
N4 C47 C41 C46 . . . . -104.4(4) ?
C46 C41 C42 F42 . . . . 179.2(3) ?
C47 C41 C42 F42 . . . . -8.2(5) ?
C46 C41 C42 C43 . . . . -0.2(6) ?
C47 C41 C42 C43 . . . . 172.4(4) ?
F42 C42 C43 C44 . . . . -179.1(4) ?
C41 C42 C43 C44 . . . . 0.3(7) ?
C42 C43 C44 C45 . . . . -0.3(7) ?
C43 C44 C45 C46 . . . . 0.3(6) ?
C44 C45 C46 F46 . . . . 179.4(3) ?
C44 C45 C46 C41 . . . . -0.3(5) ?
C42 C41 C46 F46 . . . . -179.5(3) ?
C47 C41 C46 F46 . . . . 7.8(5) ?
C42 C41 C46 C45 . . . . 0.3(5) ?
C47 C41 C46 C45 . . . . -172.4(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C45 H45 O47 2_674 0.95 2.58 3.204(4) 123 no
_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.
;
_shelx_estimated_absorpt_T_min 0.905
_shelx_estimated_absorpt_T_max 0.981
_shelx_hkl_file
;
0 0 -1 -0.10 0.20
0 0 -2 194.58 8.40
0 0 -3 -0.10 0.40
0 0 -4 2556.64 103.39
0 0 -5 0.00 0.60
0 0 -6 13.90 2.10
0 0 -7 -0.30 0.90
0 0 -8 29.50 3.60
1 0 -8 -0.20 1.10
1 0 -7 -0.50 0.90
1 0 -6 -0.30 0.80
1 0 -5 -0.10 0.70
1 0 -4 -0.20 0.60
1 0 -3 -0.20 0.40
1 0 -2 -0.40 0.40
1 0 -1 -1.50 0.10
1 0 -1 -1.40 0.20
1 0 0 -0.30 0.10
-1 0 -1 -1.50 0.10
-1 0 -2 -0.30 0.30
-1 0 -3 0.00 0.40
-1 0 -4 0.40 0.60
-1 0 -5 0.10 0.60
-1 0 -6 0.00 0.70
-1 0 -7 -0.40 0.80
-1 0 -8 0.30 1.00
2 0 -8 13.60 2.90
2 0 -7 21.30 3.00
2 0 -6 30.90 3.20
2 0 -5 34.60 3.10
2 0 -4 248.18 11.40
2 0 -3 925.21 36.80
2 0 -2 1023.20 41.70
2 0 -1 3236.08 120.69
2 0 -1 2903.61 124.59
2 0 0 368.76 15.50
2 0 0 377.46 14.80
2 0 1 3348.47 133.79
-2 0 -2 1049.30 41.80
2 0 2 1058.69 40.80
-2 0 -3 1008.10 40.50
-2 0 -4 248.68 10.90
-2 0 -5 34.70 2.80
-2 0 -6 31.80 3.00
-2 0 -7 22.90 2.70
3 0 -8 -0.20 1.00
3 0 -7 -0.40 0.90
3 0 -6 0.20 0.90
3 0 -5 0.20 0.60
3 0 -4 0.10 0.60
3 0 -3 -0.20 0.50
3 0 -2 -0.10 0.10
3 0 -2 -0.10 0.30
3 0 -1 -0.10 0.10
3 0 -1 -0.30 0.20
3 0 0 -0.60 0.30
3 0 1 -0.20 0.10
-3 0 -2 -0.10 0.20
3 0 2 -0.10 0.10
-3 0 -3 -0.10 0.30
3 0 3 -0.10 0.10
-3 0 -4 0.20 0.40
3 0 4 0.00 0.10
-3 0 -5 0.10 0.50
3 0 5 -0.10 0.20
-3 0 -6 -0.40 0.60
3 0 6 0.00 0.20
3 0 7 0.10 0.30
3 0 8 -0.10 1.00
4 0 -8 20.00 3.20
4 0 -7 -0.10 1.00
4 0 -6 69.39 5.20
4 0 -5 159.08 8.50
4 0 -3 135.39 5.50
4 0 -3 140.49 6.80
4 0 -2 326.67 12.90
4 0 -2 337.67 13.90
4 0 -1 82.99 3.50
4 0 -1 82.19 3.90
4 0 -1 78.89 3.30
4 0 0 4063.69 166.38
4 0 1 83.89 3.40
-4 0 -2 357.56 14.00
4 0 2 356.86 13.80
-4 0 -3 146.89 6.40
4 0 3 148.29 5.80
-4 0 -4 154.18 7.10
4 0 4 155.38 6.20
-4 0 -5 164.18 7.90
4 0 5 169.58 6.70
4 0 6 75.69 3.30
4 0 7 0.30 0.30
4 0 8 15.50 3.00
-5 0 9 0.40 0.90
5 0 -8 -0.50 0.90
5 0 -7 -0.30 1.00
5 0 -6 -0.20 0.90
5 0 -5 0.20 0.80
5 0 -4 -0.20 0.50
5 0 -3 -0.30 0.50
5 0 -3 0.00 0.20
5 0 -2 0.10 0.10
5 0 -2 -0.10 0.40
5 0 -1 -0.20 0.10
5 0 -1 0.00 0.30
-5 0 0 0.20 0.20
5 0 0 0.30 0.10
5 0 1 -0.30 0.10
5 0 2 0.10 0.10
-5 0 -3 -0.10 0.20
5 0 3 -0.10 0.10
-5 0 -4 0.10 0.40
5 0 4 -0.10 0.20
5 0 5 0.20 0.20
5 0 6 -0.20 0.20
5 0 8 -0.20 1.00
6 0 -7 4.00 1.80
6 0 -6 126.49 7.80
6 0 -5 4.80 1.50
6 0 -4 75.89 3.30
6 0 -4 72.29 4.70
6 0 -3 463.95 18.20
6 0 -3 470.95 19.70
6 0 -2 96.59 4.10
6 0 -2 100.09 5.10
6 0 -1 124.99 5.20
6 0 -1 123.89 5.80
6 0 -1 134.59 5.80
-6 0 0 1267.27 66.49
6 0 0 1308.37 50.19
6 0 1 129.99 5.20
6 0 2 98.99 4.00
-6 0 -3 489.25 19.20
6 0 3 494.85 19.00
6 0 4 76.89 3.20
6 0 5 5.40 0.50
6 0 6 121.79 5.10
6 0 8 2.30 1.60
6 0 9 1.10 1.40
7 0 -7 0.90 1.30
7 0 -6 0.70 1.10
7 0 -5 -0.40 0.70
7 0 -4 0.20 0.30
7 0 -4 0.90 0.90
7 0 -3 0.30 0.30
7 0 -3 0.20 0.60
7 0 -2 -0.30 0.20
7 0 -2 -0.20 0.10
7 0 -2 -0.10 0.50
7 0 -1 -0.20 0.30
7 0 -1 0.00 0.20
7 0 -1 -0.20 0.30
-7 0 0 0.50 0.30
7 0 0 0.50 0.20
7 0 1 -0.10 0.20
7 0 2 -0.10 0.20
7 0 3 0.20 0.20
7 0 4 0.10 0.20
7 0 5 0.20 0.20
7 0 6 0.00 0.30
7 0 8 0.00 1.10
-8 0 8 3.80 1.50
8 0 -7 20.50 3.20
8 0 -6 9.00 2.20
8 0 -5 21.50 2.70
8 0 -4 42.30 2.10
8 0 -4 40.40 3.40
8 0 -3 145.99 5.90
8 0 -3 140.59 7.30
8 0 -2 157.08 7.30
8 0 -2 144.89 6.10
-8 0 1 103.39 5.00
8 0 -1 103.19 4.30
8 0 -1 104.19 5.20
-8 0 0 1102.39 44.00
8 0 0 1106.79 42.70
-8 0 -1 108.99 4.30
8 0 1 107.79 4.50
8 0 2 147.89 6.00
8 0 3 131.59 5.30
8 0 4 37.60 1.80
8 0 5 21.10 1.20
8 0 6 11.00 0.80
8 0 8 2.00 1.70
-9 0 8 -0.30 0.90
9 0 -6 -0.10 0.90
9 0 -5 -0.60 0.30
9 0 -5 0.20 0.90
9 0 -4 -0.20 0.30
9 0 -4 0.20 0.80
9 0 -3 0.50 0.70
9 0 -3 -0.10 0.30
9 0 -2 -0.10 0.20
-9 0 1 -0.20 0.40
9 0 -1 0.30 0.50
9 0 -1 0.10 0.20
9 0 0 0.70 0.60
9 0 0 0.60 0.30
9 0 1 0.00 0.20
9 0 2 -0.20 0.20
9 0 3 0.00 0.20
9 0 4 0.00 0.20
9 0 5 0.00 0.20
9 0 6 0.20 0.30
9 0 8 -0.50 1.20
-10 0 7 1.80 1.20
10 0 -5 47.80 2.50
10 0 -4 26.50 2.80
10 0 -4 24.80 1.50
10 0 -3 23.30 1.40
-10 0 2 126.39 6.50
10 0 -2 131.99 5.50
-10 0 1 121.79 5.90
10 0 -1 122.29 5.10
10 0 0 66.49 4.40
10 0 0 67.49 3.00
10 0 1 117.19 4.90
10 0 2 127.49 5.30
10 0 3 19.80 1.10
10 0 4 21.30 1.20
10 0 5 39.20 1.90
10 0 6 61.59 3.40
10 0 7 2.40 2.00
-11 0 7 0.20 1.00
-11 0 6 0.20 0.90
-11 0 5 0.20 0.80
11 0 -5 -0.10 0.40
-11 0 4 -0.20 0.70
11 0 -4 -0.10 0.30
-11 0 3 0.00 0.70
11 0 -3 0.30 0.40
-11 0 2 0.00 0.60
11 0 -2 -0.10 0.30
11 0 -1 -0.10 0.30
11 0 1 -0.20 0.30
11 0 1 -0.20 0.60
11 0 2 0.10 0.30
11 0 3 -0.10 0.20
11 0 4 0.00 0.30
11 0 5 0.10 0.30
11 0 6 -0.60 1.00
11 0 7 -0.10 1.30
-12 0 7 5.50 1.80
-12 0 6 3.10 1.40
-12 0 5 30.50 3.20
12 0 -5 39.60 2.20
-12 0 4 58.99 4.40
12 0 -4 69.99 3.20
-12 0 3 15.30 2.10
12 0 -3 20.60 1.40
12 0 -2 25.20 1.50
12 0 -1 162.28 6.80
12 0 0 527.65 20.70
12 0 1 151.78 6.30
12 0 1 151.08 8.70
12 0 2 23.90 1.40
12 0 2 23.70 3.20
12 0 3 17.40 1.10
12 0 4 53.59 2.50
12 0 5 29.90 1.60
12 0 5 30.90 4.20
12 0 6 3.20 2.10
12 0 7 5.60 3.80
-13 0 6 0.30 0.90
-13 0 5 -0.30 0.80
13 0 -5 0.10 0.50
-13 0 4 -0.40 0.70
13 0 -4 0.50 0.50
13 0 -3 0.50 0.40
13 0 -2 -0.50 0.30
13 0 -1 0.20 0.30
13 0 1 0.10 0.30
13 0 1 0.20 0.80
13 0 2 0.00 0.40
13 0 2 -0.40 0.90
13 0 3 0.00 0.90
13 0 3 0.20 0.30
13 0 4 -0.60 1.00
13 0 4 -0.20 0.30
13 0 5 0.40 1.40
13 0 5 -0.10 0.30
13 0 6 0.20 1.40
-14 0 6 2.90 1.50
-14 0 5 14.70 2.40
14 0 -5 18.80 1.50
14 0 -4 122.99 5.60
14 0 -3 30.00 1.90
14 0 -2 14.90 1.20
14 0 -1 38.40 2.10
14 0 0 3.20 0.60
14 0 1 37.00 2.00
14 0 2 14.30 1.10
14 0 2 13.10 2.50
14 0 3 21.00 3.30
14 0 3 22.80 1.40
14 0 4 91.49 4.10
14 0 4 94.59 7.60
14 0 5 13.60 3.20
14 0 5 14.40 1.10
14 0 6 4.00 3.60
15 0 -5 -0.30 0.40
15 0 -4 -0.10 0.50
15 0 -3 0.00 0.40
15 0 -2 0.10 0.40
15 0 -1 0.10 0.40
15 0 0 1.30 0.50
15 0 1 0.00 0.40
15 0 2 0.20 1.00
15 0 2 0.10 0.40
15 0 3 0.20 1.10
15 0 3 0.10 0.40
15 0 4 0.20 0.40
15 0 4 -0.40 0.90
15 0 5 0.60 1.40
16 0 -4 19.40 1.60
16 0 -3 21.90 1.70
16 0 -2 43.80 2.50
16 0 -1 1.50 0.60
16 0 0 5.10 0.80
16 0 1 1.10 0.50
16 0 2 43.40 2.30
16 0 3 16.70 1.30
16 0 3 17.40 3.20
16 0 4 15.80 1.20
16 0 4 14.70 3.20
17 0 -3 0.20 0.60
17 0 -2 -0.40 0.40
17 0 -1 0.50 0.50
17 0 0 0.80 0.50
17 0 1 0.30 0.40
17 0 2 0.10 0.40
17 0 3 0.20 0.40
18 0 -1 9.00 1.30
18 0 0 13.40 1.20
18 0 1 10.40 1.10
18 0 2 15.80 1.30
18 -1 2 0.60 0.50
18 -1 1 1.00 0.50
18 -1 0 17.30 1.40
18 -1 -1 1.10 0.60
17 -1 3 8.10 1.00
17 -1 2 0.10 0.40
17 -1 1 3.30 0.70
17 -1 0 -0.20 0.40
17 -1 -1 2.90 0.70
17 -1 -2 0.50 0.50
17 -1 -3 9.60 1.30
16 -1 4 2.50 1.70
16 -1 4 1.80 0.60
16 -1 3 24.60 3.70
16 -1 3 25.30 1.60
16 -1 2 15.40 1.20
16 -1 1 7.10 0.90
16 -1 0 8.60 1.00
16 -1 -1 6.40 0.90
16 -1 -2 17.20 1.50
16 -1 -3 30.60 2.10
16 -1 -4 2.60 0.80
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7 18 -1 4.10 1.30
7 18 0 0.20 0.60
8 18 -2 6.70 1.70
8 18 -1 11.10 2.10
-7 19 -1 11.20 2.10
-7 19 0 11.90 3.00
-6 19 -2 5.50 1.50
-6 19 -1 7.40 1.60
-6 19 0 114.49 6.40
-6 19 1 7.80 1.80
-5 19 -2 6.10 1.50
-5 19 -1 2.70 1.10
-5 19 0 4.00 1.30
-5 19 1 3.60 1.20
-5 19 2 11.10 2.90
-4 19 -3 3.40 2.00
-4 19 -2 4.00 1.30
-4 19 -1 20.80 2.30
-4 19 0 10.90 1.80
-4 19 1 24.90 2.50
-4 19 2 5.20 1.40
-3 19 -3 0.80 1.00
-3 19 -2 3.60 1.30
-3 19 -1 1.90 1.00
-3 19 0 2.20 1.00
-3 19 1 2.30 1.00
-3 19 2 4.20 1.30
-3 19 3 1.10 1.70
-2 19 -3 16.40 2.30
-2 19 -2 8.60 1.70
-2 19 -1 25.90 2.60
-2 19 0 3.80 1.20
-2 19 1 31.90 2.80
-2 19 2 12.80 1.80
-2 19 3 35.40 3.10
-1 19 -3 1.20 1.00
-1 19 -2 1.00 0.90
-1 19 -1 15.60 2.10
-1 19 0 30.60 2.70
-1 19 1 18.90 2.10
-1 19 2 0.80 0.80
-1 19 3 2.40 1.10
0 19 -3 -0.20 0.60
0 19 -2 13.30 1.90
0 19 -1 0.00 0.60
0 19 0 14.80 2.00
0 19 1 0.60 0.80
0 19 2 18.90 2.20
0 19 3 0.00 0.80
1 19 -3 0.90 0.90
1 19 -2 0.40 0.80
1 19 -1 14.20 2.00
1 19 0 29.40 2.70
1 19 1 15.50 2.00
1 19 2 1.10 0.90
1 19 3 2.40 1.10
2 19 -3 17.40 2.60
2 19 -2 7.70 1.50
2 19 -1 22.80 2.50
2 19 0 3.00 1.10
2 19 1 30.20 2.70
2 19 2 12.80 1.80
2 19 3 28.30 2.60
3 19 -2 2.80 1.10
3 19 -1 1.50 0.90
3 19 0 1.60 0.90
3 19 1 2.00 1.00
3 19 2 4.90 1.40
3 19 3 1.20 0.90
4 19 -2 2.00 1.10
4 19 -1 16.50 2.10
4 19 0 10.40 1.70
4 19 1 22.20 2.30
4 19 2 4.80 1.40
5 19 -2 5.20 1.50
5 19 -1 1.90 1.00
5 19 0 2.90 1.20
5 19 1 2.50 1.00
6 19 -2 4.20 1.40
6 19 -1 5.70 1.50
6 19 0 79.39 5.10
7 19 -1 9.30 1.80
-3 20 0 29.70 4.20
-2 20 -1 40.00 4.30
-2 20 0 4.50 1.30
-2 20 1 48.70 4.10
-1 20 -1 1.20 0.90
-1 20 0 39.60 3.30
-1 20 1 2.10 1.10
0 20 -1 -0.20 0.70
0 20 0 24.50 2.60
0 20 1 0.40 0.80
0 20 2 30.10 3.20
1 20 -1 1.50 1.00
1 20 0 35.00 3.10
1 20 1 1.50 1.00
1 20 2 12.40 1.90
2 20 -1 34.90 3.20
2 20 0 3.60 1.30
2 20 1 43.60 3.50
2 20 2 3.60 1.20
3 20 -1 4.50 1.40
3 20 0 27.10 2.70
3 20 1 5.80 1.50
3 20 2 7.30 1.70
4 20 -1 8.40 2.00
4 20 0 25.70 2.70
4 20 1 9.80 1.70
5 20 0 -0.20 0.70
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 9447
_shelx_res_file
;
TITL m3cg
CELL 0.71073 14.2762 15.9821 7.3753 90.000 90.000 90.000
ZERR 4.000 0.0009 0.0010 0.0005 0.000 0.000 0.000
LATT -1
SYMM -X, -Y, 1/2+Z
SYMM 1/2+X, -Y, Z
SYMM 1/2-X, Y, 1/2+Z
SFAC C N O F H
UNIT 76 8 12 8 72
OMIT -2 180.0
L.S. 20
ACTA
BOND $H
CONF
HTAB
FMAP 2
PLAN 20
SIZE 0.910 0.352 0.168
TEMP -100
WGHT 0.096000
FVAR 0.51353
N1 2 0.360510 0.627271 0.301714 11.00000 0.03077 0.02270 =
0.02135 0.00229 -0.00050 -0.00153
C2 1 0.385551 0.711071 0.236882 11.00000 0.03561 0.02963 =
0.02540 0.00898 -0.00293 -0.00410
AFIX 23
H2A 5 0.359698 0.719747 0.113754 11.00000 -1.20000
H2B 5 0.454559 0.716266 0.229906 11.00000 -1.20000
AFIX 0
C3 1 0.346990 0.776821 0.364138 11.00000 0.03986 0.02141 =
0.02933 0.00684 -0.00882 -0.00248
AFIX 23
H3A 5 0.368636 0.832813 0.324883 11.00000 -1.20000
H3B 5 0.277698 0.776204 0.358977 11.00000 -1.20000
AFIX 0
N4 2 0.377658 0.761464 0.550901 11.00000 0.03474 0.01729 =
0.02738 0.00523 -0.00388 -0.00149
C5 1 0.365802 0.675129 0.613762 11.00000 0.03278 0.01693 =
0.02429 0.00291 -0.00021 -0.00237
AFIX 23
H5A 5 0.298368 0.663280 0.631674 11.00000 -1.20000
H5B 5 0.397915 0.667881 0.731693 11.00000 -1.20000
AFIX 0
C6 1 0.405824 0.614559 0.477597 11.00000 0.02674 0.02202 =
0.02406 0.00443 -0.00005 0.00120
AFIX 23
H6A 5 0.474169 0.623555 0.465915 11.00000 -1.20000
H6B 5 0.395300 0.556431 0.519268 11.00000 -1.20000
AFIX 0
C11 1 0.387985 0.562029 0.171955 11.00000 0.03995 0.03282 =
0.02323 -0.00030 0.00508 0.00017
AFIX 23
H11A 5 0.456869 0.562794 0.156572 11.00000 -1.20000
H11B 5 0.359158 0.573978 0.052648 11.00000 -1.20000
AFIX 0
O11 3 0.261170 0.250557 0.427238 11.00000 0.04685 0.03049 =
0.05627 0.00807 -0.00076 0.00049
C12 1 0.163803 0.261684 0.389567 11.00000 0.04651 0.03867 =
0.04271 -0.00128 -0.00243 -0.00813
AFIX 23
H12A 5 0.143086 0.220765 0.297114 11.00000 -1.20000
H12B 5 0.126584 0.252620 0.501111 11.00000 -1.20000
AFIX 0
O13 3 0.150123 0.344538 0.324667 11.00000 0.03325 0.04272 =
0.05470 0.00496 -0.00089 -0.00461
C3A 1 0.238204 0.378176 0.304903 11.00000 0.02820 0.03428 =
0.02600 -0.00429 -0.00122 0.00405
C14 1 0.262068 0.455417 0.239954 11.00000 0.03381 0.03082 =
0.02520 -0.00079 -0.00481 0.00724
AFIX 43
H14 5 0.215679 0.493677 0.199274 11.00000 -1.20000
AFIX 0
C15 1 0.357610 0.476141 0.235559 11.00000 0.03715 0.02658 =
0.01913 -0.00437 0.00182 0.00308
C16 1 0.423149 0.418888 0.298316 11.00000 0.02829 0.03355 =
0.03073 -0.00629 0.00184 0.00592
AFIX 43
H16 5 0.487529 0.433889 0.296057 11.00000 -1.20000
AFIX 0
C17 1 0.398270 0.340193 0.364582 11.00000 0.03740 0.02695 =
0.03653 -0.00112 -0.00250 0.00928
AFIX 43
H17 5 0.443834 0.301468 0.406668 11.00000 -1.20000
AFIX 0
C7A 1 0.304524 0.321827 0.365630 11.00000 0.04196 0.02420 =
0.02891 -0.00269 0.00042 0.00360
C47 1 0.401462 0.820568 0.671836 11.00000 0.02927 0.01884 =
0.03038 0.00426 -0.00138 -0.00144
O47 3 0.418354 0.805591 0.831683 11.00000 0.05603 0.02330 =
0.03048 0.00206 -0.00641 -0.00554
C41 1 0.406410 0.910215 0.606413 11.00000 0.03650 0.01826 =
0.02840 0.00235 -0.00022 -0.00312
C42 1 0.328101 0.960710 0.594540 11.00000 0.03444 0.02947 =
0.05117 0.00951 0.00375 -0.00158
F42 4 0.243587 0.923307 0.622238 11.00000 0.03230 0.04514 =
0.10853 0.02933 0.00559 -0.00061
C43 1 0.331562 1.044654 0.555508 11.00000 0.05023 0.02827 =
0.06421 0.01275 0.00941 0.00908
AFIX 43
H43 5 0.275953 1.077170 0.549167 11.00000 -1.20000
AFIX 0
C44 1 0.418122 1.080361 0.525790 11.00000 0.06829 0.01875 =
0.04258 0.00610 0.00792 -0.00380
AFIX 43
H44 5 0.422070 1.138291 0.497961 11.00000 -1.20000
AFIX 0
C45 1 0.499167 1.033458 0.535740 11.00000 0.04609 0.02825 =
0.03805 0.00186 0.00740 -0.01265
AFIX 43
H45 5 0.558706 1.058363 0.515808 11.00000 -1.20000
AFIX 0
C46 1 0.491264 0.949547 0.575377 11.00000 0.03313 0.02650 =
0.03131 0.00028 0.00258 -0.00208
F46 4 0.569655 0.902060 0.584279 11.00000 0.03301 0.04044 =
0.06575 0.00595 0.00544 0.00056
HKLF 4
REM m3cg
REM R1 = 0.0535 for 3449 Fo > 4sig(Fo) and 0.0560 for all 3743 data
REM 235 parameters refined using 1 restraints
END
WGHT 0.0960 0.0000
REM Instructions for potential hydrogen bonds
EQIV $1 x, y, z-1
HTAB C2 O47_$1
EQIV $2 -x+1/2, y, z-1/2
HTAB C3 F42_$2
EQIV $3 -x+1/2, y, z+1/2
HTAB C5 N1_$3
EQIV $4 -x+1, -y+2, z-1/2
HTAB C45 O47_$4
REM Highest difference peak 0.171, deepest hole -0.215, 1-sigma level 0.040
Q1 1 0.3730 0.6333 0.5398 11.00000 0.05 0.17
Q2 1 0.4970 0.9929 0.6272 11.00000 0.05 0.17
Q3 1 0.4064 0.8638 0.6308 11.00000 0.05 0.17
Q4 1 0.3817 0.4509 0.3048 11.00000 0.05 0.16
Q5 1 0.5971 1.0388 0.3303 11.00000 0.05 0.16
Q6 1 0.4033 0.6455 0.5578 11.00000 0.05 0.16
Q7 1 0.3116 0.4733 0.2829 11.00000 0.05 0.15
Q8 1 0.4588 1.0565 0.5931 11.00000 0.05 0.15
Q9 1 0.3610 0.9257 0.5408 11.00000 0.05 0.15
Q10 1 0.4368 0.9300 0.6440 11.00000 0.05 0.15
Q11 1 0.3610 0.3204 0.2934 11.00000 0.05 0.14
Q12 1 0.3314 0.9978 0.5049 11.00000 0.05 0.14
Q13 1 0.3831 0.6757 0.2850 11.00000 0.05 0.14
Q14 1 0.3665 0.5937 0.2385 11.00000 0.05 0.14
Q15 1 0.3749 0.7142 0.6049 11.00000 0.05 0.14
Q16 1 0.4963 0.9926 0.4870 11.00000 0.05 0.13
Q17 1 0.2467 0.4230 0.3104 11.00000 0.05 0.13
Q18 1 0.2576 1.0587 0.4617 11.00000 0.05 0.13
Q19 1 0.3386 1.0030 0.6527 11.00000 0.05 0.13
Q20 1 0.3797 0.9433 0.6484 11.00000 0.05 0.13
;
_shelx_res_checksum 16120
_shelxl_version_number 2.014
data_III
_database_code_depnum_ccdc_archive 'CCDC 1889710'
_audit_creation_method SHELXL-2014
_chemical_name_systematic
;
1-[(1,3-Benzodioxol-5-yl)methyl]-4-(2,4-dichlorobenzoyl)piperazine
;
_chemical_name_common ?
_chemical_formula_moiety 'C19 H18 Cl2 N2 O3'
_chemical_formula_sum 'C19 H18 Cl2 N2 O3'
_chemical_formula_iupac 'C19 H18 Cl2 N2 O3'
_chemical_formula_weight 393.25
_chemical_melting_point ?
_space_group_crystal_system monoclinic
_space_group_name_H-M_alt 'P 21/n'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.2889(14)
_cell_length_b 12.3034(14)
_cell_length_c 13.3667(15)
_cell_angle_alpha 90
_cell_angle_beta 116.2950(10)
_cell_angle_gamma 90
_cell_volume 1811.9(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 4054
_cell_measurement_theta_min 2.372
_cell_measurement_theta_max 27.434
_cell_measurement_temperature 173(2)
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.490
_exptl_crystal_size_mid 0.480
_exptl_crystal_size_min 0.375
_exptl_crystal_density_diffrn 1.442
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_F_000 816
_exptl_absorpt_coefficient_mu 0.380
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_absorpt_correction_T_min 0.776
_exptl_absorpt_correction_T_max 0.867
_exptl_special_details ?
_diffrn_ambient_temperature 173(2)
_diffrn_source 'fine focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean 0.3333
_diffrn_reflns_number 9718
_diffrn_reflns_av_R_equivalents 0.0174
_diffrn_reflns_av_unetI/netI 0.0203
_diffrn_reflns_theta_min 2.372
_diffrn_reflns_theta_max 27.434
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_refine_special_details ?
_reflns_number_total 4054
_reflns_number_gt 3545
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0363
_refine_ls_R_factor_gt 0.0312
_refine_ls_wR_factor_gt 0.0836
_refine_ls_wR_factor_ref 0.0869
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_restrained_S_all 1.042
_refine_ls_number_reflns 4054
_refine_ls_number_parameters 235
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.6034P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.371
_refine_diff_density_min -0.375
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
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'
'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'
'Cl' 'Cl' 0.1484 0.1585
'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'
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2014 and PLATON (Spek, 2009)
;
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N N1 0.52986(10) 0.18706(10) 0.64831(10) 0.0293(3) Uani d 1 . .
C C2 0.48214(12) 0.13857(13) 0.72047(12) 0.0335(3) Uani d 1 . .
H H2A 0.5451 0.1407 0.7989 0.040 Uiso calc 1 . .
H H2B 0.4609 0.0616 0.6993 0.040 Uiso calc 1 . .
C C3 0.37079(12) 0.19934(13) 0.71033(11) 0.0321(3) Uani d 1 . .
H H3A 0.3360 0.1622 0.7553 0.038 Uiso calc 1 . .
H H3B 0.3939 0.2740 0.7398 0.038 Uiso calc 1 . .
N N4 0.27950(10) 0.20437(11) 0.59349(9) 0.0310(3) Uani d 1 . .
C C5 0.32597(13) 0.24338(15) 0.51615(12) 0.0376(3) Uani d 1 . .
H H5A 0.3457 0.3217 0.5292 0.045 Uiso calc 1 . .
H H5B 0.2629 0.2343 0.4384 0.045 Uiso calc 1 . .
C C6 0.43884(13) 0.18029(13) 0.53272(12) 0.0342(3) Uani d 1 . .
H H6A 0.4173 0.1032 0.5122 0.041 Uiso calc 1 . .
H H6B 0.4723 0.2103 0.4834 0.041 Uiso calc 1 . .
C C11 0.64509(13) 0.13691(12) 0.66549(15) 0.0371(3) Uani d 1 . .
H H11A 0.6295 0.0625 0.6341 0.045 Uiso calc 1 . .
H H11B 0.6988 0.1313 0.7465 0.045 Uiso calc 1 . .
O O11 0.87114(9) 0.40074(9) 0.46855(9) 0.0362(2) Uani d 1 . .
C C12 0.83867(16) 0.50226(13) 0.49898(14) 0.0407(4) Uani d 1 . .
H H12A 0.7743 0.5375 0.4326 0.049 Uiso calc 1 . .
H H12B 0.9100 0.5511 0.5296 0.049 Uiso calc 1 . .
O O13 0.79616(10) 0.48304(9) 0.58078(10) 0.0391(3) Uani d 1 . .
C C3A 0.77539(12) 0.37264(11) 0.57687(12) 0.0280(3) Uani d 1 . .
C C14 0.71953(12) 0.31497(12) 0.62874(12) 0.0312(3) Uani d 1 . .
H H14 0.6897 0.3498 0.6751 0.037 Uiso calc 1 . .
C C15 0.70819(12) 0.20229(12) 0.61057(12) 0.0299(3) Uani d 1 . .
C C16 0.75523(12) 0.15362(12) 0.54436(12) 0.0316(3) Uani d 1 . .
H H16 0.7471 0.0773 0.5330 0.038 Uiso calc 1 . .
C C17 0.81427(12) 0.21356(12) 0.49382(11) 0.0311(3) Uani d 1 . .
H H17 0.8479 0.1795 0.4501 0.037 Uiso calc 1 . .
C C7A 0.82108(11) 0.32314(12) 0.51047(11) 0.0269(3) Uani d 1 . .
C C47 0.15968(12) 0.18798(11) 0.55740(11) 0.0273(3) Uani d 1 . .
O O47 0.08510(9) 0.19648(11) 0.45924(8) 0.0426(3) Uani d 1 . .
C C41 0.11656(11) 0.15520(11) 0.64264(10) 0.0240(3) Uani d 1 . .
C C42 0.09914(11) 0.22960(10) 0.71238(10) 0.0236(3) Uani d 1 . .
Cl Cl42 0.13921(3) 0.36508(3) 0.71225(3) 0.03486(11) Uani d 1 . .
C C43 0.04921(11) 0.19988(11) 0.78313(11) 0.0261(3) Uani d 1 . .
H H43 0.0384 0.2518 0.8306 0.031 Uiso calc 1 . .
C C44 0.01549(11) 0.09273(12) 0.78272(11) 0.0276(3) Uani d 1 . .
Cl Cl44 -0.04771(4) 0.05479(4) 0.87079(3) 0.04291(12) Uani d 1 . .
C C45 0.02990(12) 0.01613(11) 0.71408(12) 0.0310(3) Uani d 1 . .
H H45 0.0052 -0.0570 0.7143 0.037 Uiso calc 1 . .
C C46 0.08095(12) 0.04794(11) 0.64495(12) 0.0291(3) Uani d 1 . .
H H46 0.0920 -0.0044 0.5980 0.035 Uiso calc 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N1 0.0239(5) 0.0337(6) 0.0344(6) 0.0016(5) 0.0165(5) 0.0087(5)
C2 0.0262(6) 0.0420(8) 0.0328(7) -0.0015(6) 0.0135(6) 0.0125(6)
C3 0.0253(6) 0.0480(9) 0.0241(6) -0.0042(6) 0.0119(5) 0.0031(6)
N4 0.0243(5) 0.0478(7) 0.0239(5) 0.0012(5) 0.0135(5) 0.0061(5)
C5 0.0304(7) 0.0575(10) 0.0312(7) 0.0080(7) 0.0194(6) 0.0154(7)
C6 0.0313(7) 0.0454(9) 0.0332(7) 0.0022(6) 0.0208(6) 0.0042(6)
C11 0.0294(7) 0.0333(8) 0.0526(9) 0.0061(6) 0.0217(7) 0.0129(7)
O11 0.0389(6) 0.0424(6) 0.0378(6) -0.0031(5) 0.0265(5) 0.0000(5)
C12 0.0499(9) 0.0396(8) 0.0452(9) -0.0087(7) 0.0326(8) -0.0021(7)
O13 0.0537(6) 0.0300(5) 0.0509(6) -0.0066(5) 0.0388(6) -0.0041(5)
C3A 0.0256(6) 0.0292(7) 0.0320(7) 0.0002(5) 0.0153(6) -0.0009(5)
C14 0.0307(7) 0.0328(7) 0.0389(8) 0.0036(6) 0.0235(6) 0.0016(6)
C15 0.0214(6) 0.0319(7) 0.0377(7) 0.0051(5) 0.0143(6) 0.0062(6)
C16 0.0250(6) 0.0287(7) 0.0378(8) 0.0046(5) 0.0110(6) -0.0008(6)
C17 0.0255(6) 0.0386(8) 0.0291(7) 0.0053(6) 0.0120(5) -0.0041(6)
C7A 0.0193(6) 0.0379(7) 0.0241(6) -0.0003(5) 0.0103(5) 0.0004(5)
C47 0.0259(6) 0.0336(7) 0.0251(6) 0.0026(5) 0.0137(5) -0.0010(5)
O47 0.0286(5) 0.0743(8) 0.0238(5) 0.0021(5) 0.0106(4) 0.0031(5)
C41 0.0186(5) 0.0306(7) 0.0226(6) 0.0011(5) 0.0090(5) -0.0002(5)
C42 0.0232(6) 0.0246(6) 0.0233(6) -0.0024(5) 0.0105(5) 0.0000(5)
Cl42 0.0493(2) 0.02548(18) 0.03616(19) -0.00753(14) 0.02471(17) -0.00147(13)
C43 0.0246(6) 0.0315(7) 0.0237(6) -0.0015(5) 0.0121(5) -0.0013(5)
C44 0.0211(6) 0.0351(7) 0.0261(6) -0.0021(5) 0.0101(5) 0.0063(5)
Cl44 0.0431(2) 0.0533(2) 0.0397(2) -0.01166(17) 0.02503(17) 0.00825(17)
C45 0.0276(7) 0.0253(7) 0.0361(7) -0.0013(5) 0.0105(6) 0.0046(6)
C46 0.0274(6) 0.0271(7) 0.0311(7) 0.0039(5) 0.0115(5) -0.0025(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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 C6 . 1.4540(19) ?
N1 C2 . 1.4600(17) ?
N1 C11 . 1.4665(17) ?
C2 C3 . 1.512(2) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 N4 . 1.4660(17) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
N4 C47 . 1.3462(17) ?
N4 C5 . 1.4658(17) ?
C5 C6 . 1.518(2) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C11 C15 . 1.5138(19) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
O11 C7A . 1.3817(17) ?
O11 C12 . 1.4242(19) ?
C12 O13 . 1.4249(17) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
O13 C3A . 1.3787(17) ?
C3A C14 . 1.3701(19) ?
C3A C7A . 1.3839(19) ?
C14 C15 . 1.404(2) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.389(2) ?
C16 C17 . 1.400(2) ?
C16 H16 . 0.9500 ?
C17 C7A . 1.363(2) ?
C17 H17 . 0.9500 ?
C47 O47 . 1.2276(17) ?
C47 C41 . 1.5088(17) ?
C41 C42 . 1.3890(18) ?
C41 C46 . 1.3950(19) ?
C42 C43 . 1.3852(17) ?
C42 Cl42 . 1.7383(13) ?
C43 C44 . 1.381(2) ?
C43 H43 . 0.9500 ?
C44 C45 . 1.380(2) ?
C44 Cl44 . 1.7370(13) ?
C45 C46 . 1.384(2) ?
C45 H45 . 0.9500 ?
C46 H46 . 0.9500 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 N1 C2 . . 109.49(11) ?
C6 N1 C11 . . 112.16(12) ?
C2 N1 C11 . . 111.54(11) ?
N1 C2 C3 . . 110.56(11) ?
N1 C2 H2A . . 109.5 ?
C3 C2 H2A . . 109.5 ?
N1 C2 H2B . . 109.5 ?
C3 C2 H2B . . 109.5 ?
H2A C2 H2B . . 108.1 ?
N4 C3 C2 . . 110.58(12) ?
N4 C3 H3A . . 109.5 ?
C2 C3 H3A . . 109.5 ?
N4 C3 H3B . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 108.1 ?
C47 N4 C5 . . 120.16(11) ?
C47 N4 C3 . . 125.09(11) ?
C5 N4 C3 . . 114.32(11) ?
N4 C5 C6 . . 110.25(12) ?
N4 C5 H5A . . 109.6 ?
C6 C5 H5A . . 109.6 ?
N4 C5 H5B . . 109.6 ?
C6 C5 H5B . . 109.6 ?
H5A C5 H5B . . 108.1 ?
N1 C6 C5 . . 110.42(12) ?
N1 C6 H6A . . 109.6 ?
C5 C6 H6A . . 109.6 ?
N1 C6 H6B . . 109.6 ?
C5 C6 H6B . . 109.6 ?
H6A C6 H6B . . 108.1 ?
N1 C11 C15 . . 111.53(11) ?
N1 C11 H11A . . 109.3 ?
C15 C11 H11A . . 109.3 ?
N1 C11 H11B . . 109.3 ?
C15 C11 H11B . . 109.3 ?
H11A C11 H11B . . 108.0 ?
C7A O11 C12 . . 105.00(10) ?
O11 C12 O13 . . 108.54(12) ?
O11 C12 H12A . . 110.0 ?
O13 C12 H12A . . 110.0 ?
O11 C12 H12B . . 110.0 ?
O13 C12 H12B . . 110.0 ?
H12A C12 H12B . . 108.4 ?
C3A O13 C12 . . 105.01(11) ?
C14 C3A O13 . . 128.09(13) ?
C14 C3A C7A . . 122.22(13) ?
O13 C3A C7A . . 109.69(12) ?
C3A C14 C15 . . 117.23(13) ?
C3A C14 H14 . . 121.4 ?
C15 C14 H14 . . 121.4 ?
C16 C15 C14 . . 119.91(13) ?
C16 C15 C11 . . 121.81(13) ?
C14 C15 C11 . . 118.28(13) ?
C15 C16 C17 . . 122.09(14) ?
C15 C16 H16 . . 119.0 ?
C17 C16 H16 . . 119.0 ?
C7A C17 C16 . . 116.72(13) ?
C7A C17 H17 . . 121.6 ?
C16 C17 H17 . . 121.6 ?
C17 C7A O11 . . 128.57(12) ?
C17 C7A C3A . . 121.80(13) ?
O11 C7A C3A . . 109.63(12) ?
O47 C47 N4 . . 123.39(13) ?
O47 C47 C41 . . 118.97(12) ?
N4 C47 C41 . . 117.62(11) ?
C42 C41 C46 . . 117.74(12) ?
C42 C41 C47 . . 122.74(12) ?
C46 C41 C47 . . 119.22(12) ?
C43 C42 C41 . . 122.06(12) ?
C43 C42 Cl42 . . 117.72(10) ?
C41 C42 Cl42 . . 120.22(10) ?
C44 C43 C42 . . 118.17(12) ?
C44 C43 H43 . . 120.9 ?
C42 C43 H43 . . 120.9 ?
C45 C44 C43 . . 121.85(12) ?
C45 C44 Cl44 . . 119.64(11) ?
C43 C44 Cl44 . . 118.50(11) ?
C44 C45 C46 . . 118.71(13) ?
C44 C45 H45 . . 120.6 ?
C46 C45 H45 . . 120.6 ?
C45 C46 C41 . . 121.47(13) ?
C45 C46 H46 . . 119.3 ?
C41 C46 H46 . . 119.3 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 N1 C2 C3 . . . . -61.31(16) ?
C11 N1 C2 C3 . . . . 173.95(13) ?
N1 C2 C3 N4 . . . . 55.00(16) ?
C2 C3 N4 C47 . . . . 136.85(14) ?
C2 C3 N4 C5 . . . . -50.77(17) ?
C47 N4 C5 C6 . . . . -136.22(14) ?
C3 N4 C5 C6 . . . . 50.99(18) ?
C2 N1 C6 C5 . . . . 61.64(16) ?
C11 N1 C6 C5 . . . . -173.97(12) ?
N4 C5 C6 N1 . . . . -55.75(17) ?
C6 N1 C11 C15 . . . . 69.26(16) ?
C2 N1 C11 C15 . . . . -167.51(13) ?
C7A O11 C12 O13 . . . . 14.03(16) ?
O11 C12 O13 C3A . . . . -14.51(16) ?
C12 O13 C3A C14 . . . . -170.92(15) ?
C12 O13 C3A C7A . . . . 9.41(16) ?
O13 C3A C14 C15 . . . . 179.33(14) ?
C7A C3A C14 C15 . . . . -1.0(2) ?
C3A C14 C15 C16 . . . . 1.5(2) ?
C3A C14 C15 C11 . . . . -179.07(12) ?
N1 C11 C15 C16 . . . . -132.47(14) ?
N1 C11 C15 C14 . . . . 48.08(19) ?
C14 C15 C16 C17 . . . . -0.2(2) ?
C11 C15 C16 C17 . . . . -179.64(13) ?
C15 C16 C17 C7A . . . . -1.5(2) ?
C16 C17 C7A O11 . . . . -178.31(12) ?
C16 C17 C7A C3A . . . . 2.0(2) ?
C12 O11 C7A C17 . . . . 172.09(14) ?
C12 O11 C7A C3A . . . . -8.17(15) ?
C14 C3A C7A C17 . . . . -0.7(2) ?
O13 C3A C7A C17 . . . . 178.96(13) ?
C14 C3A C7A O11 . . . . 179.50(12) ?
O13 C3A C7A O11 . . . . -0.81(15) ?
C5 N4 C47 O47 . . . . 5.4(2) ?
C3 N4 C47 O47 . . . . 177.41(14) ?
C5 N4 C47 C41 . . . . -175.89(13) ?
C3 N4 C47 C41 . . . . -3.9(2) ?
O47 C47 C41 C42 . . . . -100.59(16) ?
N4 C47 C41 C42 . . . . 80.68(17) ?
O47 C47 C41 C46 . . . . 72.85(18) ?
N4 C47 C41 C46 . . . . -105.88(15) ?
C46 C41 C42 C43 . . . . 0.52(19) ?
C47 C41 C42 C43 . . . . 174.06(12) ?
C46 C41 C42 Cl42 . . . . -178.99(10) ?
C47 C41 C42 Cl42 . . . . -5.46(17) ?
C41 C42 C43 C44 . . . . -0.42(19) ?
Cl42 C42 C43 C44 . . . . 179.11(10) ?
C42 C43 C44 C45 . . . . -0.3(2) ?
C42 C43 C44 Cl44 . . . . -179.77(10) ?
C43 C44 C45 C46 . . . . 0.8(2) ?
Cl44 C44 C45 C46 . . . . -179.70(10) ?
C44 C45 C46 C41 . . . . -0.7(2) ?
C42 C41 C46 C45 . . . . 0.03(19) ?
C47 C41 C46 C45 . . . . -173.74(12) ?
_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.
;
_shelx_estimated_absorpt_T_min 0.836
_shelx_estimated_absorpt_T_max 0.871
_shelx_hkl_file
;
-1 0 0 0.00 0.10
-2 0 0 0.00 0.10
-2 0 0 -0.10 0.10
-3 0 0 -0.20 0.10
-3 0 0 0.00 0.10
-4 0 0 82.99 1.70
-4 0 0 82.99 1.50
-5 0 0 0.40 0.10
-5 0 0 -0.20 0.10
-6 0 0 72.59 1.50
-6 0 0 71.39 1.70
-7 0 0 0.00 0.20
-7 0 0 -0.10 0.10
-8 0 0 0.70 0.20
-8 0 0 0.70 0.30
-9 0 0 0.20 0.30
-10 0 0 87.69 2.40
-11 0 0 -0.20 0.30
-12 0 0 70.39 2.40
-13 0 0 -0.30 0.50
-14 0 0 0.30 0.60
-14 1 0 10.10 1.40
-13 1 0 9.50 1.10
-12 1 0 0.60 0.50
-11 1 0 6.70 0.90
-10 1 0 21.50 1.20
-9 1 0 54.19 1.70
-8 1 0 0.00 0.20
-8 1 0 0.10 0.20
-7 1 0 205.38 3.90
-7 1 0 201.88 3.50
-6 1 0 207.38 3.40
-6 1 0 206.88 3.80
-5 1 0 71.49 1.60
-5 1 0 73.99 1.40
-4 1 0 421.26 6.70
-4 1 0 417.96 6.90
-3 1 0 3625.94 76.09
-3 1 0 3669.23 64.29
-2 1 0 529.35 8.30
-1 1 0 116.19 1.90
0 1 0 -3.30 0.10
-2 -1 0 486.85 13.50
-3 -1 0 3516.65 72.29
-3 -1 0 3643.44 72.09
-4 -1 0 407.26 6.60
-4 -1 0 402.76 6.70
-5 -1 0 75.19 1.50
-5 -1 0 74.09 1.60
-6 -1 0 210.28 3.60
-6 -1 0 200.98 3.70
-7 -1 0 199.38 3.50
-7 -1 0 197.28 3.70
-8 -1 0 0.00 0.20
-8 -1 0 0.20 0.20
-9 -1 0 54.49 1.50
-9 -1 0 52.69 1.70
-10 -1 0 23.80 1.20
-11 -1 0 6.70 0.80
-12 -1 0 0.00 0.40
-13 -1 0 8.70 1.10
-14 -1 0 10.00 1.20
-13 2 0 18.70 1.40
-12 2 0 3.80 0.70
-11 2 0 40.80 1.70
-10 2 0 28.20 1.40
-9 2 0 107.99 2.70
-8 2 0 0.40 0.30
-7 2 0 36.20 1.20
-7 2 0 35.40 0.90
-6 2 0 0.80 0.30
-6 2 0 1.50 0.20
-5 2 0 73.89 1.70
-5 2 0 75.09 1.30
-4 2 0 148.59 2.70
-4 2 0 149.88 2.40
-3 2 0 51.49 0.90
-2 2 0 1112.19 21.20
1 -2 0 219.88 3.60
-1 2 0 227.18 3.80
0 -2 0 2211.38 43.20
1 2 0 233.38 4.00
-2 -2 0 1045.10 16.80
-3 -2 0 48.70 1.10
-4 -2 0 143.89 2.60
-4 -2 0 144.99 2.60
-5 -2 0 71.49 1.60
-5 -2 0 73.19 1.60
-6 -2 0 0.70 0.20
-6 -2 0 0.70 0.20
-7 -2 0 32.70 1.10
-7 -2 0 34.10 1.00
-8 -2 0 0.60 0.30
-8 -2 0 0.20 0.20
-9 -2 0 106.99 2.60
-9 -2 0 107.99 2.40
-10 -2 0 26.70 1.20
-10 -2 0 25.70 1.00
-11 -2 0 39.60 1.60
-12 -2 0 4.20 0.70
-13 -2 0 18.00 1.30
-14 -2 0 -0.10 0.50
-13 3 0 1.60 0.70
-12 3 0 1.90 0.60
-11 3 0 128.29 3.40
-10 3 0 5.90 0.70
-9 3 0 10.30 0.90
-8 3 0 15.00 0.90
-7 3 0 100.39 2.40
-6 3 0 249.38 3.90
-6 3 0 248.28 4.50
-5 3 0 57.89 1.00
-5 3 0 58.69 1.50
-4 3 0 734.83 12.80
-3 3 0 199.28 3.40
2 -3 0 -0.10 0.10
-2 3 0 0.20 0.10
1 -3 0 1641.44 32.50
-1 3 0 1628.24 27.40
-1 3 0 1706.43 25.90
0 -3 0 -1.70 0.10
-1 -3 0 1555.84 38.50
1 3 0 1629.64 27.00
-3 -3 0 194.98 3.40
-4 -3 0 683.73 11.70
-4 -3 0 708.63 11.60
-5 -3 0 57.69 1.40
-5 -3 0 56.69 1.30
-6 -3 0 249.88 4.40
-6 -3 0 245.68 4.30
-7 -3 0 99.29 2.10
-7 -3 0 93.09 2.10
-8 -3 0 15.10 0.80
-8 -3 0 15.60 0.80
-9 -3 0 10.50 0.70
-9 -3 0 11.40 0.80
-10 -3 0 5.30 0.60
-10 -3 0 6.10 0.70
-11 -3 0 118.39 3.00
-11 -3 0 122.79 3.80
-12 -3 0 2.00 0.60
-13 -3 0 1.30 0.60
-14 -3 0 2.50 0.70
-13 4 0 21.50 1.60
-12 4 0 1.40 0.60
-11 4 0 19.40 1.30
-10 4 0 53.79 1.90
-9 4 0 6.80 0.80
-8 4 0 484.45 8.40
-7 4 0 6.70 0.60
-6 4 0 25.80 1.00
-5 4 0 213.08 3.90
-4 4 0 202.98 3.60
3 -4 0 427.26 6.70
-3 4 0 433.26 6.90
2 -4 0 3.30 0.20
-2 4 0 3.20 0.30
1 -4 0 367.56 6.10
-1 4 0 364.86 5.90
0 -4 0 82.99 1.60
0 4 0 83.89 1.50
0 4 0 82.49 2.00
-1 -4 0 335.57 5.50
1 4 0 347.87 6.00
-2 -4 0 3.30 0.30
2 4 0 3.90 0.50
-3 -4 0 421.06 6.80
-4 -4 0 202.78 3.60
-5 -4 0 200.48 3.50
-5 -4 0 203.08 3.70
-6 -4 0 25.20 0.80
-6 -4 0 24.20 0.90
-7 -4 0 6.60 0.50
-7 -4 0 7.00 0.60
-8 -4 0 474.65 8.00
-8 -4 0 468.45 7.90
-9 -4 0 6.00 0.60
-9 -4 0 5.90 0.60
-10 -4 0 53.09 1.70
-10 -4 0 57.79 1.70
-11 -4 0 18.70 1.00
-11 -4 0 18.30 1.10
-12 -4 0 1.90 0.50
-13 -4 0 22.10 1.40
-13 5 0 1.20 0.70
-12 5 0 31.10 1.70
-11 5 0 3.40 0.70
-10 5 0 16.90 1.20
-9 5 0 0.70 0.40
-8 5 0 200.18 4.10
-7 5 0 41.80 1.40
-6 5 0 9.70 0.70
-5 5 0 423.16 7.10
-4 5 0 71.99 1.70
3 -5 0 84.79 1.50
-3 5 0 83.39 1.80
2 -5 0 834.02 13.20
-2 5 0 808.72 14.10
-2 5 0 828.92 13.60
1 -5 0 159.78 2.80
-1 5 0 167.48 2.80
-1 5 0 158.58 3.40
0 -5 0 0.30 0.10
0 5 0 0.50 0.10
-1 -5 0 153.98 2.80
1 5 0 160.98 3.40
-2 -5 0 800.12 13.60
2 5 0 778.82 12.90
-3 -5 0 79.89 1.80
-4 -5 0 70.99 1.70
-5 -5 0 424.26 6.80
-5 -5 0 426.56 7.10
-6 -5 0 10.70 0.50
-6 -5 0 10.70 0.70
-7 -5 0 43.90 1.40
-7 -5 0 42.90 1.20
-8 -5 0 197.08 3.70
-8 -5 0 191.68 3.90
-9 -5 0 0.50 0.30
-9 -5 0 0.40 0.30
-10 -5 0 16.10 1.00
-10 -5 0 15.90 1.00
-11 -5 0 3.10 0.60
-11 -5 0 2.70 0.60
-12 -5 0 29.20 1.40
-13 6 0 5.60 1.50
-12 6 0 0.40 0.60
-11 6 0 51.69 2.10
-10 6 0 12.60 1.10
-9 6 0 0.20 0.40
-8 6 0 1.40 0.50
-7 6 0 114.69 2.70
-6 6 0 30.60 1.20
-5 6 0 240.48 4.40
-4 6 0 2.50 0.40
3 -6 0 90.49 1.70
-3 6 0 90.29 2.50
-3 6 0 91.59 1.90
2 -6 0 270.17 4.30
-2 6 0 267.47 4.50
-2 6 0 255.97 5.20
1 -6 0 555.94 8.70
-1 6 0 541.05 9.50
-1 6 0 543.05 8.70
0 -6 0 1183.98 19.70
0 6 0 1177.38 19.90
0 6 0 1189.08 18.50
-1 -6 0 528.25 8.50
1 6 0 542.35 9.40
-2 -6 0 254.57 4.50
2 6 0 261.17 5.20
-3 -6 0 85.99 1.90
-4 -6 0 2.90 0.40
-5 -6 0 232.68 4.30
-5 -6 0 233.18 3.90
-6 -6 0 28.50 0.90
-6 -6 0 29.80 1.10
-7 -6 0 111.89 2.60
-7 -6 0 113.39 2.30
-8 -6 0 1.40 0.40
-10 -6 0 12.90 1.00
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4 0 -15 0.30 0.40
3 0 -15 4.20 0.80
3 0 -15 4.00 0.70
2 0 -15 0.00 0.50
2 0 -15 0.40 0.60
1 0 -15 81.79 2.80
0 0 -15 0.10 0.70
-1 0 -15 40.80 2.20
-12 1 15 38.10 1.80
-11 1 15 0.80 0.60
-10 1 15 40.80 1.70
-9 1 15 12.40 1.10
-8 1 15 5.00 0.70
6 -1 -15 97.39 2.60
5 -1 -15 0.70 0.50
4 -1 -15 1.80 0.50
4 -1 -15 1.70 0.60
3 -1 -15 45.60 1.70
3 -1 -15 45.70 1.80
2 -1 -15 -0.10 0.50
2 -1 -15 -0.60 0.40
1 -1 -15 5.90 0.90
1 -1 -15 7.10 0.90
0 -1 -15 25.90 1.70
-12 2 15 -0.90 0.50
-11 2 15 2.60 0.70
-10 2 15 91.59 2.60
-9 2 15 65.99 2.10
7 -2 -15 38.60 1.60
6 -2 -15 125.59 3.10
5 -2 -15 0.10 0.50
4 -2 -15 -0.10 0.50
4 -2 -15 1.30 0.50
3 -2 -15 0.90 0.50
3 -2 -15 0.60 0.60
2 -2 -15 55.19 2.00
1 -2 -15 61.09 2.20
-12 3 15 6.20 0.90
-11 3 15 0.70 0.60
-10 3 15 23.00 1.30
8 -3 -15 22.10 1.30
7 -3 -15 7.90 0.90
6 -3 -15 42.00 1.80
5 -3 -15 0.10 0.50
4 -3 -15 0.70 0.60
3 -3 -15 87.39 2.70
2 -3 -15 1.10 0.60
1 -3 -15 9.20 1.00
0 -3 -15 2.60 0.80
-12 4 15 69.99 2.40
-11 4 15 3.60 0.70
9 -4 -15 44.30 1.80
8 -4 -15 -0.70 0.50
7 -4 -15 -0.10 0.50
6 -4 -15 0.40 0.60
5 -4 -15 26.40 1.50
4 -4 -15 20.50 1.40
3 -4 -15 3.20 0.80
2 -4 -15 32.60 1.70
1 -4 -15 2.50 0.80
0 -4 -15 3.40 0.80
-11 5 15 29.40 1.50
10 -5 -15 2.60 0.70
9 -5 -15 24.60 1.40
8 -5 -15 5.00 0.80
7 -5 -15 91.19 2.70
6 -5 -15 9.20 1.10
5 -5 -15 69.59 2.50
4 -5 -15 1.00 0.60
3 -5 -15 9.10 1.10
2 -5 -15 10.70 1.20
1 -5 -15 0.70 0.70
10 -6 -15 40.80 1.80
9 -6 -15 1.10 0.60
8 -6 -15 0.60 0.60
7 -6 -15 9.40 1.10
6 -6 -15 16.90 1.40
5 -6 -15 -0.60 0.60
4 -6 -15 51.69 2.30
3 -6 -15 4.70 1.00
2 -6 -15 7.40 1.40
8 -7 -15 94.79 3.10
7 -7 -15 40.60 2.00
6 -7 -15 18.00 1.50
5 -7 -15 0.50 0.70
-7 -6 16 0.00 0.60
-9 -5 16 0.60 0.60
-8 -5 16 1.80 0.70
-7 -5 16 8.10 1.00
-10 -4 16 30.90 2.00
-9 -4 16 5.00 0.90
-8 -4 16 9.00 1.00
-7 -4 16 81.09 2.50
-6 -4 16 85.29 2.50
5 4 -16 2.00 0.60
4 4 -16 0.40 0.60
-10 -3 16 13.10 1.30
-9 -3 16 3.60 0.80
-8 -3 16 24.00 1.40
-7 -3 16 1.10 0.60
-6 -3 16 9.80 1.10
5 3 -16 0.80 0.60
-5 -3 16 0.60 0.50
4 3 -16 0.50 0.50
3 3 -16 56.09 2.30
-10 -2 16 50.39 2.10
-9 -2 16 1.00 0.60
-8 -2 16 5.40 0.80
-7 -2 16 -0.20 0.50
-6 -2 16 8.60 1.00
5 2 -16 31.20 1.60
-5 -2 16 30.80 1.40
4 2 -16 1.60 0.60
-4 -2 16 1.10 0.50
3 2 -16 41.40 2.00
2 2 -16 19.50 1.50
-11 -1 16 56.99 2.80
-10 -1 16 -0.10 0.60
-9 -1 16 29.70 1.60
-8 -1 16 43.60 1.80
-7 -1 16 0.60 0.50
-6 -1 16 0.30 0.50
5 1 -16 12.20 1.10
-5 -1 16 11.60 1.00
4 1 -16 2.50 0.60
3 1 -16 3.00 0.70
2 1 -16 13.00 1.30
-11 0 16 0.10 0.60
-10 0 16 -0.10 0.50
-9 0 16 -0.30 0.50
-8 0 16 99.69 2.70
-7 0 16 0.00 0.40
4 0 -16 141.49 3.30
4 0 -16 145.69 3.60
3 0 -16 0.20 0.50
3 0 -16 -0.40 0.50
2 0 -16 0.40 0.60
-11 1 16 56.99 2.50
-10 1 16 -0.50 0.50
-9 1 16 29.10 1.50
-8 1 16 42.00 1.70
6 -1 -16 0.00 0.50
5 -1 -16 10.80 1.10
4 -1 -16 2.50 0.60
4 -1 -16 3.00 0.60
3 -1 -16 2.10 0.60
3 -1 -16 3.20 0.70
2 -1 -16 12.30 1.20
2 -1 -16 10.50 1.10
-10 2 16 56.59 2.00
-9 2 16 0.00 0.50
7 -2 -16 0.10 0.50
6 -2 -16 8.50 1.00
5 -2 -16 32.00 1.50
4 -2 -16 0.80 0.60
3 -2 -16 40.10 1.80
2 -2 -16 19.40 1.40
-10 3 16 13.10 1.20
8 -3 -16 25.40 1.40
7 -3 -16 0.30 0.60
6 -3 -16 11.30 1.20
5 -3 -16 0.70 0.60
4 -3 -16 0.20 0.60
3 -3 -16 50.79 2.10
2 -3 -16 0.20 0.60
9 -4 -16 7.30 1.00
8 -4 -16 11.60 1.20
7 -4 -16 88.59 2.70
6 -4 -16 87.09 2.70
5 -4 -16 0.90 0.60
4 -4 -16 0.00 0.60
3 -4 -16 0.10 0.60
7 -5 -16 10.10 1.60
6 -5 -16 43.50 2.50
-7 -3 17 13.40 1.20
-8 -2 17 33.40 1.70
-7 -2 17 4.80 0.80
-6 -2 17 1.20 0.60
-5 -2 17 24.40 1.40
-8 -1 17 0.70 0.60
-7 -1 17 53.79 2.00
-6 -1 17 3.60 0.70
-5 -1 17 9.40 1.00
-8 0 17 -0.10 0.60
-7 0 17 34.60 1.60
-6 0 17 -0.40 0.50
5 -1 -17 8.00 0.90
_computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 63551
_shelx_res_file
;
TITL m5cg
CELL 0.71073 12.2889 12.3034 13.3667 90.000 116.295 90.000
ZERR 4.000 0.0014 0.0014 0.0015 0.000 0.001 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C N O Cl H
UNIT 76 8 12 8 72
OMIT -2 180.0
L.S. 20
ACTA
BOND $H
CONF
HTAB
FMAP 2
PLAN 20
SIZE 0.490 0.480 0.375
TEMP -100
WGHT 0.043000 0.603400
FVAR 0.43879
N1 2 0.529862 0.187062 0.648306 11.00000 0.02390 0.03369 =
0.03441 0.00866 0.01653 0.00156
C2 1 0.482138 0.138574 0.720470 11.00000 0.02619 0.04200 =
0.03284 0.01254 0.01346 -0.00147
AFIX 23
H2A 5 0.545148 0.140660 0.798902 11.00000 -1.20000
H2B 5 0.460937 0.061570 0.699329 11.00000 -1.20000
AFIX 0
C3 1 0.370785 0.199344 0.710330 11.00000 0.02528 0.04799 =
0.02409 0.00312 0.01194 -0.00416
AFIX 23
H3A 5 0.336045 0.162243 0.755337 11.00000 -1.20000
H3B 5 0.393904 0.273976 0.739830 11.00000 -1.20000
AFIX 0
N4 2 0.279499 0.204371 0.593494 11.00000 0.02430 0.04778 =
0.02390 0.00612 0.01351 0.00122
C5 1 0.325971 0.243378 0.516147 11.00000 0.03038 0.05748 =
0.03122 0.01539 0.01941 0.00802
AFIX 23
H5A 5 0.345694 0.321690 0.529222 11.00000 -1.20000
H5B 5 0.262899 0.234342 0.438365 11.00000 -1.20000
AFIX 0
C6 1 0.438843 0.180287 0.532716 11.00000 0.03135 0.04538 =
0.03316 0.00417 0.02080 0.00215
AFIX 23
H6A 5 0.417331 0.103219 0.512163 11.00000 -1.20000
H6B 5 0.472344 0.210271 0.483420 11.00000 -1.20000
AFIX 0
C11 1 0.645092 0.136907 0.665490 11.00000 0.02937 0.03327 =
0.05262 0.01287 0.02171 0.00615
AFIX 23
H11A 5 0.629519 0.062463 0.634138 11.00000 -1.20000
H11B 5 0.698842 0.131274 0.746508 11.00000 -1.20000
AFIX 0
O11 3 0.871138 0.400741 0.468554 11.00000 0.03893 0.04236 =
0.03781 0.00005 0.02654 -0.00308
C12 1 0.838669 0.502258 0.498981 11.00000 0.04991 0.03963 =
0.04517 -0.00212 0.03258 -0.00865
AFIX 23
H12A 5 0.774276 0.537505 0.432555 11.00000 -1.20000
H12B 5 0.910044 0.551111 0.529649 11.00000 -1.20000
AFIX 0
O13 3 0.796157 0.483037 0.580776 11.00000 0.05365 0.03001 =
0.05086 -0.00414 0.03884 -0.00658
C3A 1 0.775391 0.372639 0.576870 11.00000 0.02556 0.02920 =
0.03196 -0.00088 0.01532 0.00020
C14 1 0.719534 0.314966 0.628743 11.00000 0.03075 0.03283 =
0.03893 0.00160 0.02347 0.00361
AFIX 43
H14 5 0.689722 0.349787 0.675084 11.00000 -1.20000
AFIX 0
C15 1 0.708187 0.202289 0.610567 11.00000 0.02140 0.03189 =
0.03773 0.00622 0.01431 0.00507
C16 1 0.755226 0.153621 0.544361 11.00000 0.02500 0.02874 =
0.03783 -0.00083 0.01098 0.00462
AFIX 43
H16 5 0.747084 0.077250 0.533002 11.00000 -1.20000
AFIX 0
C17 1 0.814270 0.213557 0.493824 11.00000 0.02547 0.03859 =
0.02908 -0.00407 0.01203 0.00526
AFIX 43
H17 5 0.847924 0.179515 0.450085 11.00000 -1.20000
AFIX 0
C7A 1 0.821084 0.323142 0.510474 11.00000 0.01930 0.03793 =
0.02410 0.00040 0.01030 -0.00030
C47 1 0.159676 0.187976 0.557399 11.00000 0.02588 0.03358 =
0.02506 -0.00096 0.01367 0.00255
O47 3 0.085101 0.196477 0.459236 11.00000 0.02860 0.07429 =
0.02377 0.00312 0.01062 0.00212
C41 1 0.116561 0.155203 0.642641 11.00000 0.01859 0.03058 =
0.02260 -0.00020 0.00905 0.00110
C42 1 0.099142 0.229600 0.712380 11.00000 0.02323 0.02456 =
0.02328 0.00001 0.01049 -0.00242
CL42 4 0.139211 0.365083 0.712250 11.00000 0.04931 0.02548 =
0.03616 -0.00147 0.02471 -0.00753
C43 1 0.049209 0.199876 0.783126 11.00000 0.02456 0.03150 =
0.02370 -0.00134 0.01212 -0.00149
AFIX 43
H43 5 0.038447 0.251764 0.830623 11.00000 -1.20000
AFIX 0
C44 1 0.015494 0.092726 0.782719 11.00000 0.02115 0.03512 =
0.02610 0.00629 0.01011 -0.00215
CL44 4 -0.047707 0.054794 0.870792 11.00000 0.04308 0.05334 =
0.03968 0.00825 0.02503 -0.01166
C45 1 0.029897 0.016126 0.714078 11.00000 0.02759 0.02528 =
0.03606 0.00458 0.01052 -0.00129
AFIX 43
H45 5 0.005236 -0.057018 0.714296 11.00000 -1.20000
AFIX 0
C46 1 0.080949 0.047945 0.644952 11.00000 0.02737 0.02712 =
0.03114 -0.00247 0.01150 0.00389
AFIX 43
H46 5 0.091996 -0.004417 0.598017 11.00000 -1.20000
AFIX 0
HKLF 4
REM m5cg
REM R1 = 0.0312 for 3545 Fo > 4sig(Fo) and 0.0363 for all 4054 data
REM 235 parameters refined using 0 restraints
END
WGHT 0.0429 0.6033
REM Instructions for potential hydrogen bonds
EQIV $1 x+1, y, z
HTAB C11 Cl44_$1
EQIV $2 -x+1, -y+1, -z+1
HTAB C12 Cl42_$2
EQIV $3 -x+1/2, y+1/2, -z+3/2
HTAB C14 Cl44_$3
REM Highest difference peak 0.371, deepest hole -0.375, 1-sigma level 0.042
Q1 1 -0.0377 0.0038 0.8321 11.00000 0.05 0.37
Q2 1 0.1450 0.1720 0.6054 11.00000 0.05 0.34
Q3 1 0.7767 0.3432 0.5325 11.00000 0.05 0.29
Q4 1 0.0458 0.0561 0.7594 11.00000 0.05 0.26
Q5 1 0.3802 0.2045 0.5272 11.00000 0.05 0.25
Q6 1 0.0323 0.0410 0.6683 11.00000 0.05 0.25
Q7 1 0.1196 0.1885 0.6824 11.00000 0.05 0.24
Q8 1 0.0856 0.0235 0.7054 11.00000 0.05 0.24
Q9 1 0.6824 0.1728 0.6381 11.00000 0.05 0.23
Q10 1 0.3222 0.2083 0.6469 11.00000 0.05 0.23
Q11 1 0.4183 0.1601 0.7088 11.00000 0.05 0.23
Q12 1 0.0452 0.1387 0.7902 11.00000 0.05 0.23
Q13 1 0.5086 0.1688 0.6764 11.00000 0.05 0.23
Q14 1 0.2212 0.2136 0.5830 11.00000 0.05 0.23
Q15 1 0.1013 0.2029 0.7636 11.00000 0.05 0.22
Q16 1 0.7154 0.3468 0.5746 11.00000 0.05 0.22
Q17 1 0.7197 0.1833 0.5677 11.00000 0.05 0.22
Q18 1 0.5797 0.1619 0.6552 11.00000 0.05 0.21
Q19 1 0.1048 0.1000 0.6469 11.00000 0.05 0.21
Q20 1 0.7183 0.2515 0.6240 11.00000 0.05 0.21
;
_shelx_res_checksum 20592
_shelxl_version_number 2.014