#data_New_Global_Publ_Block
data_global
_audit_creation_method
;
manual editing of the CIF file
created by SHELXTL Ver. 6.10
;
# 1. SUBMISSION DETAILS
_publ_contact_author_name
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Raines, Ronald T.
;
_publ_contact_author_address
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Department of Biochemistry
University of Wisconsin-Madison
433 Babcock Drive
Madison, WI 53706
USA
;
_publ_contact_author_phone '608-262-8588'
_publ_contact_author_fax '608-262-3453'
_publ_contact_author_email rtraines@wisc.edu
_publ_contact_letter
;
Please consider this CIF submission
for publication in
;
_publ_requested_journal
;
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_publ_requested_category FA
# FA 'Full article'
# FI 'Full submission - inorganic (Acta C)'
# FO 'Full submission - organic (Acta C)'
# FM 'Full submission - metal-organic (Acta C)'
# CI 'CIF-access paper - inorganic (Acta C)'
# CO 'CIF-access paper - organic (Acta C)'
# CM 'CIF-access paper - metal-organic (Acta C)'
# 2. TITLE AND AUTHOR LIST
_publ_section_title
;
;
loop_
_publ_author_name
_publ_author_address
'Raines, Ronald T.'
;
Department of Biochemistry
University of Wisconsin-Madison
433 Babcock Drive
Madison, WI 53706
USA
;
''
;
Department of Biochemistry
University of Wisconsin-Madison
433 Babcock Drive
Madison, WI 53706
USA
;
_publ_section_synopsis
;
;
_publ_section_abstract
;
;
_publ_section_comment
;
;
_publ_section_references
;
Allen, F.H. (2002). Acta Cryst. B58, 380-388.
Bruker-AXS. (2007-2009). APEX2 (Ver. 2.1-4), SADABS,
SAINTPLUS,
SHELXTL. Bruker-AXS Inc., Madison, WI, USA.
Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M.,
Macrae, C. F., McCabe, P., Pearson, J,
& Taylor, R. (2002). Acta Cryst. B58, 389-397.
Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc.
97, 1358-1367.
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Pushmann,
H. (2009). J. Appl. Cryst. 42, 339--341.
Frisch, M. J., Trucks, G. W.,
Schlegel, H. B., Scuseria, G. E., Robb, M. A., Cheeseman,
J. R., Montgomery, Jr., J. A., Vreven, T., Kudin, K. N., Burant,
J. C., Millam, J. M., Iyengar, S. S., Tomasi, J., Barone, V.,
Mennucci, B. et al. (2004).
Gaussian 03, Revision C.02,
Gaussian, Inc., Wallingford, CT, USA.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
Westrip, S. P. (2009). publCIF. In preparation.
;
_publ_section_acknowledgements
;
We thank Lara C. Spencer and Dr. Ilia A. Guzei.
;
_publ_section_figure_captions
;
Figure 1. Molecular structure of (I). The thermal ellipsoids are
shown at 50% probability level.
;
_publ_section_exptl_prep
;
;
_publ_section_exptl_refinement
;
All H-atoms were placed in idealized locations and
refined as riding with appropriate thermal displacement
coefficients U~iso~(H) = 1.2 or 1.5 times U~eq~(bearing atom).
;
_iucr_refine_instruction_details ?
#3. data
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C10 H15 N O4 S'
_chemical_formula_weight 245.29
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'
'S' 'S' 0.1246 0.1234
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
_chemical_absolute_configuration 'ad'
# Options are 'rm', 'ad', 'rmad', 'syn', 'unk' or '.'
#
# rm : absolute configuration established by the structure determination
# of a compound containing a chiral reference molecule of known
# absolute configuration.
# ad : absolute configuration established by anomalous dispersion effects
# in diffraction measurements on the crystal.
# rmad : absolute configuration established by the structure determination
# of a compound containing a chiral reference molecule of known
# absolute configuration and confirmed by anomalous dispersion
# effects in diffraction measurements on the crystal.
# syn : absolute configuration has not been established by anomalous
# dispersion effects in diffraction measurements on the crystal.
# The enantiomer has been assigned by reference to an unchanging
# chiral centre in the synthetic procedure.
# unk : absolute configuration is unknown, there being no firm chemical
# evidence for its assignment to hand and it having not been
# established by anomalous dispersion effects in diffraction
# measurements on the crystal. An arbitrary choice of enantiomer
# has been made.
# . : inapplicable.
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 6.5056(6)
_cell_length_b 8.2425(8)
_cell_length_c 21.780(2)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 1167.9(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 273(2)
_cell_measurement_reflns_used 5760
_cell_measurement_theta_min 2.6421
_cell_measurement_theta_max 28.1861
_exptl_crystal_description block
_exptl_crystal_colour colorless
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.395
_exptl_crystal_F_000 520
_exptl_crystal_size_max 0.500
_exptl_crystal_size_mid 0.460
_exptl_crystal_size_min 0.280
_exptl_absorpt_coefficient_mu 0.276
_shelx_estimated_absorpt_T_min 0.874
_shelx_estimated_absorpt_T_max 0.927
_exptl_absorpt_correction_type 'multi-scan'
_exptl_absorpt_correction_T_min 0.8743
_exptl_absorpt_correction_T_max 0.9267
_exptl_absorpt_process_details
;
SADABS (Bruker-AXS, 2003)
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 273(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source 'fine-focus sealed tube'
_diffrn_measurement_device_type 'Bruker CCD-1000 area detector'
_diffrn_measurement_method '0.30\% \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 16028
_diffrn_reflns_av_unetI/netI 0.0200
_diffrn_reflns_av_R_equivalents 0.0386
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 1.870
_diffrn_reflns_theta_max 28.278
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total 2887
_reflns_number_gt 2785
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.708
_reflns_Friedel_fraction_max 0.999
_reflns_Friedel_fraction_full 1.000
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection 'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_cell_refinement 'SAINT Ver. 6.22 (Bruker-AXS, 2003)'
_computing_data_reduction 'SAINT Ver. 6.22'
_computing_structure_solution 'SHELXTL Ver. 6.10 (Bruker-AXS, 2003)'
_computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics 'SHELXTL Ver. 6.10'
_computing_publication_material 'SHELXTL Ver. 6.10'
_refine_special_details
;
Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.1815P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack -0.01(7)
_refine_ls_number_reflns 2887
_refine_ls_number_parameters 149
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0259
_refine_ls_R_factor_gt 0.0248
_refine_ls_wR_factor_ref 0.0658
_refine_ls_wR_factor_gt 0.0650
_refine_ls_goodness_of_fit_ref 1.065
_refine_ls_restrained_S_all 1.065
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C7 C -0.1890(2) 1.00902(19) 0.92409(7) 0.0152(3) Uani 1 1 d . . . . .
S1 S -0.26349(6) 1.03404(5) 0.78720(2) 0.01991(11) Uani 1 1 d . . . . .
O1 O -0.35647(18) 0.99995(15) 0.94800(6) 0.0199(3) Uani 1 1 d . . . . .
O3 O 0.21550(17) 0.57265(14) 0.88771(5) 0.0172(2) Uani 1 1 d . . . . .
O4 O 0.55459(18) 0.54292(15) 0.87093(6) 0.0251(3) Uani 1 1 d . . . . .
C2 C -0.0176(2) 0.97598(19) 0.79320(7) 0.0149(3) Uani 1 1 d . . . . .
O2 O -0.06884(17) 1.14014(14) 0.92540(5) 0.0177(2) Uani 1 1 d . . . . .
N1 N 0.05297(19) 0.90412(17) 0.84370(6) 0.0140(3) Uani 1 1 d . . . . .
C4 C 0.2581(3) 0.73717(18) 0.90733(7) 0.0167(3) Uani 1 1 d . . . . .
H4 H 0.3843 0.7425 0.9318 0.020 Uiso 1 1 calc R U . . .
C9 C 0.3831(2) 0.4867(2) 0.87052(7) 0.0183(3) Uani 1 1 d . . . . .
C1 C 0.1328(2) 1.0021(2) 0.74174(7) 0.0187(3) Uani 1 1 d . . . . .
H1A H 0.2515 1.0583 0.7571 0.028 Uiso 1 1 calc R U . . .
H1B H 0.0692 1.0656 0.7101 0.028 Uiso 1 1 calc R U . . .
H1C H 0.1739 0.8991 0.7252 0.028 Uiso 1 1 calc R U . . .
C3 C 0.2678(2) 0.85162(19) 0.85279(7) 0.0162(3) Uani 1 1 d . . . . .
H3A H 0.3559 0.9437 0.8616 0.019 Uiso 1 1 calc R U . . .
H3B H 0.3193 0.7962 0.8166 0.019 Uiso 1 1 calc R U . . .
C6 C -0.0790(2) 0.86394(19) 0.89638(7) 0.0151(3) Uani 1 1 d . . . . .
H6 H -0.1792 0.7808 0.8846 0.018 Uiso 1 1 calc R U . . .
C8 C -0.1569(3) 1.2840(2) 0.95305(9) 0.0230(4) Uani 1 1 d . . . . .
H8A H -0.2670 1.3233 0.9278 0.035 Uiso 1 1 calc R U . . .
H8B H -0.0531 1.3662 0.9566 0.035 Uiso 1 1 calc R U . . .
H8C H -0.2090 1.2578 0.9931 0.035 Uiso 1 1 calc R U . . .
C10 C 0.3296(3) 0.3160(2) 0.85371(9) 0.0233(4) Uani 1 1 d . . . . .
H10A H 0.4182 0.2797 0.8212 0.035 Uiso 1 1 calc R U . . .
H10B H 0.1892 0.3114 0.8402 0.035 Uiso 1 1 calc R U . . .
H10C H 0.3471 0.2471 0.8889 0.035 Uiso 1 1 calc R U . . .
C5 C 0.0731(3) 0.7942(2) 0.94413(7) 0.0206(3) Uani 1 1 d . . . . .
H5A H 0.1130 0.8770 0.9734 0.025 Uiso 1 1 calc R U . . .
H5B H 0.0114 0.7043 0.9662 0.025 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C7 0.0178(7) 0.0158(7) 0.0121(6) 0.0003(5) -0.0006(5) 0.0011(6)
S1 0.01493(16) 0.0257(2) 0.01913(18) 0.00414(16) 0.00012(14) 0.00461(15)
O1 0.0177(5) 0.0219(6) 0.0201(6) -0.0026(4) 0.0059(4) -0.0006(5)
O3 0.0184(5) 0.0148(5) 0.0184(5) -0.0011(4) 0.0015(4) 0.0015(4)
O4 0.0182(5) 0.0213(6) 0.0360(7) -0.0011(6) 0.0023(5) 0.0018(5)
C2 0.0156(6) 0.0137(7) 0.0153(7) -0.0012(6) 0.0010(5) 0.0010(5)
O2 0.0174(5) 0.0141(5) 0.0217(6) -0.0036(4) 0.0017(5) 0.0002(4)
N1 0.0127(6) 0.0159(6) 0.0133(6) 0.0006(5) 0.0013(5) 0.0013(5)
C4 0.0200(7) 0.0150(7) 0.0151(7) -0.0018(5) -0.0027(6) 0.0027(6)
C9 0.0203(7) 0.0182(8) 0.0163(7) 0.0029(6) 0.0012(6) 0.0032(6)
C1 0.0191(7) 0.0219(8) 0.0150(7) 0.0025(6) 0.0037(5) 0.0007(6)
C3 0.0141(7) 0.0155(7) 0.0189(7) 0.0004(5) -0.0018(6) 0.0011(6)
C6 0.0178(7) 0.0145(7) 0.0130(7) -0.0006(5) 0.0037(6) 0.0004(6)
C8 0.0238(8) 0.0154(8) 0.0299(9) -0.0072(7) -0.0019(7) 0.0019(6)
C10 0.0262(8) 0.0178(8) 0.0259(9) -0.0021(6) 0.0036(7) 0.0019(7)
C5 0.0293(9) 0.0191(8) 0.0134(7) 0.0006(6) 0.0022(7) 0.0083(7)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C7 O1 1.2099(19) . ?
C7 O2 1.3342(19) . ?
C7 C6 1.519(2) . ?
S1 C2 1.6748(15) . ?
O3 C9 1.3535(19) . ?
O3 C4 1.4484(18) . ?
O4 C9 1.208(2) . ?
C2 N1 1.3310(19) . ?
C2 C1 1.503(2) . ?
O2 C8 1.448(2) . ?
N1 C6 1.4709(19) . ?
N1 C3 1.476(2) . ?
C4 C3 1.518(2) . ?
C4 C5 1.520(2) . ?
C4 H4 0.9800 . ?
C9 C10 1.495(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C6 C5 1.547(2) . ?
C6 H6 0.9800 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C7 O2 124.64(14) . . ?
O1 C7 C6 123.13(14) . . ?
O2 C7 C6 111.74(13) . . ?
C9 O3 C4 114.69(13) . . ?
N1 C2 C1 117.08(13) . . ?
N1 C2 S1 121.40(11) . . ?
C1 C2 S1 121.51(11) . . ?
C7 O2 C8 116.13(13) . . ?
C2 N1 C6 122.91(13) . . ?
C2 N1 C3 124.59(13) . . ?
C6 N1 C3 112.47(12) . . ?
O3 C4 C3 111.03(12) . . ?
O3 C4 C5 107.07(14) . . ?
C3 C4 C5 104.68(13) . . ?
O3 C4 H4 111.3 . . ?
C3 C4 H4 111.3 . . ?
C5 C4 H4 111.3 . . ?
O4 C9 O3 122.75(15) . . ?
O4 C9 C10 125.32(15) . . ?
O3 C9 C10 111.89(14) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C3 C4 104.34(13) . . ?
N1 C3 H3A 110.9 . . ?
C4 C3 H3A 110.9 . . ?
N1 C3 H3B 110.9 . . ?
C4 C3 H3B 110.9 . . ?
H3A C3 H3B 108.9 . . ?
N1 C6 C7 114.06(13) . . ?
N1 C6 C5 103.56(12) . . ?
C7 C6 C5 109.08(13) . . ?
N1 C6 H6 110.0 . . ?
C7 C6 H6 110.0 . . ?
C5 C6 H6 110.0 . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C4 C5 C6 105.48(13) . . ?
C4 C5 H5A 110.6 . . ?
C6 C5 H5A 110.6 . . ?
C4 C5 H5B 110.6 . . ?
C6 C5 H5B 110.6 . . ?
H5A C5 H5B 108.8 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C7 O2 C8 -5.6(2) . . . . ?
C6 C7 O2 C8 -177.88(13) . . . . ?
C1 C2 N1 C6 -177.00(14) . . . . ?
S1 C2 N1 C6 2.8(2) . . . . ?
C1 C2 N1 C3 1.1(2) . . . . ?
S1 C2 N1 C3 -179.11(12) . . . . ?
C9 O3 C4 C3 84.95(16) . . . . ?
C9 O3 C4 C5 -161.34(13) . . . . ?
C4 O3 C9 O4 -0.6(2) . . . . ?
C4 O3 C9 C10 177.29(13) . . . . ?
C2 N1 C3 C4 -164.39(14) . . . . ?
C6 N1 C3 C4 13.89(17) . . . . ?
O3 C4 C3 N1 87.78(15) . . . . ?
C5 C4 C3 N1 -27.42(16) . . . . ?
C2 N1 C6 C7 -58.0(2) . . . . ?
C3 N1 C6 C7 123.66(14) . . . . ?
C2 N1 C6 C5 -176.45(14) . . . . ?
C3 N1 C6 C5 5.23(17) . . . . ?
O1 C7 C6 N1 148.59(15) . . . . ?
O2 C7 C6 N1 -39.03(18) . . . . ?
O1 C7 C6 C5 -96.18(18) . . . . ?
O2 C7 C6 C5 76.20(16) . . . . ?
O3 C4 C5 C6 -86.82(15) . . . . ?
C3 C4 C5 C6 31.11(17) . . . . ?
N1 C6 C5 C4 -22.36(16) . . . . ?
C7 C6 C5 C4 -144.19(13) . . . . ?
_refine_diff_density_max 0.320
_refine_diff_density_min -0.186
_refine_diff_density_rms 0.044
_shelxl_version_number 2013-4
_shelx_res_file
;
TITL raines12 in P2(1)2(1)2(1)
CELL 0.71073 6.5056 8.2425 21.7804 90.000 90.000 90.000
ZERR 4.00 0.0006 0.0008 0.0022 0.000 0.000 0.000
LATT -1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SFAC C H N O S
UNIT 40 60 4 16 4
L.S. 100
ACTA
bond $h
conf
twin
wpdb -2
BOND
FMAP 2
PLAN 10
SIZE 0.28 0.46 0.50
TEMP 0
WGHT 0.040000 0.181500
BASF -0.00965
FVAR 0.65090
MOLE 1
C7 1 -0.189004 1.009018 0.924090 11.00000 0.01778 0.01577 =
0.01213 0.00026 -0.00058 0.00114
S1 5 -0.263490 1.034042 0.787199 11.00000 0.01493 0.02567 =
0.01913 0.00414 0.00012 0.00461
O1 4 -0.356471 0.999945 0.948002 11.00000 0.01773 0.02185 =
0.02008 -0.00264 0.00586 -0.00062
O3 4 0.215502 0.572653 0.887715 11.00000 0.01840 0.01484 =
0.01843 -0.00106 0.00146 0.00153
O4 4 0.554594 0.542923 0.870929 11.00000 0.01815 0.02130 =
0.03599 -0.00108 0.00228 0.00179
C2 1 -0.017600 0.975976 0.793197 11.00000 0.01560 0.01373 =
0.01528 -0.00119 0.00104 0.00097
O2 4 -0.068843 1.140144 0.925403 11.00000 0.01736 0.01405 =
0.02166 -0.00364 0.00172 0.00021
N1 3 0.052974 0.904125 0.843705 11.00000 0.01266 0.01586 =
0.01334 0.00055 0.00134 0.00132
C4 1 0.258088 0.737167 0.907326 11.00000 0.01996 0.01500 =
0.01505 -0.00179 -0.00274 0.00272
AFIX 13
H4 2 0.384327 0.742509 0.931793 11.00000 -1.20000
AFIX 0
C9 1 0.383145 0.486666 0.870516 11.00000 0.02034 0.01823 =
0.01629 0.00292 0.00120 0.00319
C1 1 0.132837 1.002109 0.741742 11.00000 0.01914 0.02192 =
0.01503 0.00250 0.00371 0.00065
AFIX 137
H1A 2 0.251469 1.058310 0.757065 11.00000 -1.50000
H1B 2 0.069217 1.065626 0.710059 11.00000 -1.50000
H1C 2 0.173886 0.899078 0.725246 11.00000 -1.50000
AFIX 0
C3 1 0.267789 0.851617 0.852786 11.00000 0.01410 0.01555 =
0.01893 0.00038 -0.00184 0.00110
AFIX 23
H3A 2 0.355907 0.943676 0.861558 11.00000 -1.20000
H3B 2 0.319308 0.796161 0.816645 11.00000 -1.20000
AFIX 0
C6 1 -0.079050 0.863941 0.896379 11.00000 0.01775 0.01453 =
0.01299 -0.00061 0.00367 0.00038
AFIX 13
H6 2 -0.179224 0.780778 0.884599 11.00000 -1.20000
AFIX 0
C8 1 -0.156918 1.283997 0.953045 11.00000 0.02378 0.01540 =
0.02985 -0.00721 -0.00188 0.00186
AFIX 137
H8A 2 -0.267023 1.323342 0.927758 11.00000 -1.50000
H8B 2 -0.053074 1.366202 0.956633 11.00000 -1.50000
H8C 2 -0.209050 1.257819 0.993072 11.00000 -1.50000
AFIX 0
C10 1 0.329612 0.315962 0.853711 11.00000 0.02623 0.01782 =
0.02592 -0.00207 0.00365 0.00189
AFIX 137
H10A 2 0.418161 0.279744 0.821225 11.00000 -1.50000
H10B 2 0.189232 0.311400 0.840235 11.00000 -1.50000
H10C 2 0.347068 0.247126 0.888881 11.00000 -1.50000
AFIX 0
C5 1 0.073107 0.794184 0.944130 11.00000 0.02933 0.01911 =
0.01337 0.00065 0.00215 0.00833
AFIX 23
H5A 2 0.113038 0.876971 0.973449 11.00000 -1.20000
H5B 2 0.011449 0.704305 0.966205 11.00000 -1.20000
AFIX 0
HKLF 4
REM raines12 in P2(1)2(1)2(1)
REM R1 = 0.0248 for 2785 Fo > 4sig(Fo) and 0.0259 for all 2887 data
REM 149 parameters refined using 0 restraints
END
WGHT 0.0383 0.1983
REM Highest difference peak 0.320, deepest hole -0.186, 1-sigma level 0.044
Q1 1 -0.1345 1.0137 0.7936 11.00000 0.05 0.32
Q2 1 0.1666 0.7591 0.9248 11.00000 0.05 0.30
Q3 1 -0.1298 0.9380 0.9077 11.00000 0.05 0.30
Q4 1 0.2624 0.7963 0.8826 11.00000 0.05 0.29
Q5 1 -0.0174 0.8859 0.8695 11.00000 0.05 0.25
Q6 1 -0.0007 0.8343 0.9205 11.00000 0.05 0.25
Q7 1 0.1553 0.8815 0.8485 11.00000 0.05 0.23
Q8 1 0.0607 0.9871 0.7675 11.00000 0.05 0.22
Q9 1 0.2394 0.6562 0.8947 11.00000 0.05 0.21
Q10 1 -0.1529 1.1019 0.9096 11.00000 0.05 0.20
;
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8 -4 -3 89.45 5.74
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