#------------------------------------------------------------------------------
#$Date: 2020-07-06 06:47:11 +0300 (Mon, 06 Jul 2020) $
#$Revision: 253981 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/15/75/7157534.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7157534
loop_
_publ_author_name
'Sheppard, Daniel J.'
'Cameron, Scott A.'
'Tyler, Peter C.'
'Schwörer, Ralf'
_publ_section_title
;
 Comparison of disaccharide donors for heparan sulfate synthesis: uronic
 acids vs. their pyranose equivalents.
;
_journal_issue                   25
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              4728
_journal_page_last               4733
_journal_paper_doi               10.1039/d0ob00671h
_journal_volume                  18
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C59 H56 Cl N3 O14 S'
_chemical_formula_sum            'C59 H56 Cl N3 O14 S'
_chemical_formula_weight         1098.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-03-03 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.23660(10)
_cell_length_b                   35.3229(3)
_cell_length_c                   14.56840(10)
_cell_measurement_reflns_used    26240
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.2940
_cell_measurement_theta_min      3.9400
_cell_volume                     2682.24(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48369
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.534
_diffrn_reflns_theta_min         3.944
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       rod
_exptl_crystal_F_000             1152
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.484
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 4408 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     914
_refine_ls_number_reflns         10328
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0400P)²+1.3455P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.922
_reflns_number_gt                9914
_reflns_number_total             10328
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ob00671h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7157534--7157536.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7157534
_shelx_shelxl_version_number     2016/6
_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   0.513
_shelx_estimated_absorpt_t_max   0.918
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
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
C1 C 0.7201(7) 0.70875(10) 0.6644(2) 0.0272(7) Uani 1 1 d . . . . .
H1 H 0.895743 0.711931 0.697000 0.033 Uiso 1 1 calc R U . . .
C2 C 0.5505(7) 0.68621(10) 0.7242(2) 0.0276(7) Uani 1 1 d . . . . .
H2 H 0.365920 0.690915 0.702888 0.033 Uiso 1 1 calc R U . . .
C3 C 0.6026(7) 0.64384(10) 0.7256(2) 0.0282(7) Uani 1 1 d . . . . .
H3 H 0.771462 0.639120 0.761981 0.034 Uiso 1 1 calc R U . . .
C4 C 0.6167(7) 0.62929(9) 0.6276(2) 0.0270(7) Uani 1 1 d . . . . .
H4 H 0.448308 0.631175 0.589182 0.032 Uiso 1 1 calc R U . A 1
C5 C 0.8271(7) 0.65231(10) 0.5877(2) 0.0273(7) Uani 1 1 d . . . . .
H5 H 0.984489 0.652017 0.632439 0.033 Uiso 1 1 calc R U . . .
C6 C 0.8975(7) 0.63975(11) 0.4946(2) 0.0305(7) Uani 1 1 d . . . . .
H6A H 0.952924 0.612948 0.496980 0.037 Uiso 1 1 calc R U . . .
H6B H 0.747938 0.642217 0.447968 0.037 Uiso 1 1 calc R U . . .
C7 C 0.8232(8) 0.78210(10) 0.6081(3) 0.0321(8) Uani 1 1 d . . . . .
C8 C 0.8666(10) 0.78481(13) 0.5167(3) 0.0499(11) Uani 1 1 d . . . . .
H8 H 0.769893 0.769679 0.472041 0.060 Uiso 1 1 calc R U . . .
C9 C 1.0498(12) 0.80935(13) 0.4896(4) 0.0605(14) Uani 1 1 d . . . . .
H9 H 1.074700 0.811233 0.426034 0.073 Uiso 1 1 calc R U . . .
C10 C 1.1979(9) 0.83125(11) 0.5526(4) 0.0556(13) Uani 1 1 d . . . . .
C11 C 1.4009(11) 0.85769(15) 0.5219(6) 0.085(2) Uani 1 1 d . . . . .
H11A H 1.334970 0.883677 0.519592 0.102 Uiso 1 1 calc R U . . .
H11B H 1.444342 0.850187 0.460587 0.102 Uiso 1 1 calc R U . . .
H11C H 1.554658 0.856331 0.565829 0.102 Uiso 1 1 calc R U . . .
C12 C 1.1556(11) 0.82765(12) 0.6442(4) 0.0598(14) Uani 1 1 d . . . . .
H12 H 1.257072 0.842027 0.689122 0.072 Uiso 1 1 calc R U . . .
C13 C 0.9686(9) 0.80356(11) 0.6724(3) 0.0453(10) Uani 1 1 d . . . . .
H13 H 0.941227 0.801901 0.735832 0.054 Uiso 1 1 calc R U . . .
C14 C 0.4255(7) 0.72066(11) 0.8554(2) 0.0309(7) Uani 1 1 d . . . . .
C15 C 0.5178(7) 0.73183(11) 0.9516(2) 0.0313(7) Uani 1 1 d . . . . .
C16 C 0.7410(8) 0.71745(13) 0.9971(3) 0.0418(9) Uani 1 1 d . . . . .
H16 H 0.847004 0.700857 0.966218 0.050 Uiso 1 1 calc R U . . .
C17 C 0.8091(9) 0.72752(15) 1.0887(3) 0.0483(11) Uani 1 1 d . . . . .
H17 H 0.959641 0.717152 1.120689 0.058 Uiso 1 1 calc R U . . .
C18 C 0.6612(8) 0.75220(15) 1.1330(2) 0.0470(10) Uani 1 1 d . . . . .
H18 H 0.709375 0.758947 1.195373 0.056 Uiso 1 1 calc R U . . .
C19 C 0.4410(9) 0.76735(14) 1.0867(3) 0.0473(10) Uani 1 1 d . . . . .
H19 H 0.339229 0.784744 1.117108 0.057 Uiso 1 1 calc R U . . .
C20 C 0.3699(8) 0.75710(12) 0.9965(2) 0.0388(8) Uani 1 1 d . . . . .
H20 H 0.218619 0.767442 0.964844 0.047 Uiso 1 1 calc R U . . .
C21 C 0.5042(9) 0.60984(15) 0.8583(3) 0.0496(11) Uani 1 1 d . . . . .
H21A H 0.621596 0.628266 0.891695 0.060 Uiso 1 1 calc R U . . .
H21B H 0.603661 0.586652 0.847915 0.060 Uiso 1 1 calc R U . . .
C22 C 0.2924(8) 0.60034(12) 0.9161(3) 0.0379(9) Uani 1 1 d . . . . .
C23 C 0.1964(9) 0.62765(15) 0.9717(3) 0.0475(10) Uani 1 1 d . . . . .
H23 H 0.255791 0.652974 0.968328 0.057 Uiso 1 1 calc R U . . .
C24 C 0.0184(9) 0.61918(17) 1.0314(3) 0.0567(13) Uani 1 1 d . . . . .
H24 H -0.044357 0.638492 1.068626 0.068 Uiso 1 1 calc R U . . .
C25 C -0.0699(10) 0.58257(18) 1.0374(4) 0.0642(16) Uani 1 1 d . . . . .
H25 H -0.192119 0.576479 1.079261 0.077 Uiso 1 1 calc R U . . .
C26 C 0.0197(11) 0.55518(16) 0.9828(5) 0.079(2) Uani 1 1 d . . . . .
H26 H -0.040801 0.529929 0.986677 0.095 Uiso 1 1 calc R U . . .
C27 C 0.1984(11) 0.56389(14) 0.9218(4) 0.0620(14) Uani 1 1 d . . . . .
H27 H 0.256901 0.544631 0.883420 0.074 Uiso 1 1 calc R U . . .
C28 C 1.0456(7) 0.69134(11) 0.4078(2) 0.0299(7) Uani 1 1 d . . . . .
C29 C 1.2724(7) 0.71757(11) 0.4092(2) 0.0345(8) Uani 1 1 d . . . . .
H29A H 1.431756 0.702460 0.409895 0.041 Uiso 1 1 calc R U . . .
H29B H 1.283065 0.733017 0.466161 0.041 Uiso 1 1 calc R U . . .
N1 N 0.774(3) 0.5340(2) 0.7559(5) 0.058(3) Uani 0.507(5) 1 d D . P B 1
N2 N 0.8168(19) 0.5053(2) 0.8013(6) 0.059(2) Uani 0.507(5) 1 d D . P B 1
N3 N 0.883(2) 0.4815(3) 0.8505(7) 0.077(3) Uani 0.507(5) 1 d D . P B 1
O4 O 0.711(3) 0.5914(5) 0.6343(14) 0.034(3) Uani 0.507(5) 1 d D U P B 1
O8 O 0.375(3) 0.5613(4) 0.5410(10) 0.034(3) Uani 0.507(5) 1 d D . P B 1
O11 O 0.322(5) 0.5853(7) 0.3456(13) 0.047(4) Uani 0.507(5) 1 d D . P B 1
O14 O 0.644(3) 0.5815(6) 0.2559(15) 0.080(5) Uani 0.507(5) 1 d D . P B 1
C30 C 0.506(3) 0.5654(4) 0.6311(13) 0.033(4) Uani 0.507(5) 1 d D . P B 1
H30 H 0.380910 0.574278 0.674063 0.040 Uiso 0.507(5) 1 calc R U P B 1
C31 C 0.618(2) 0.5273(3) 0.6658(8) 0.042(2) Uani 0.507(5) 1 d D . P B 1
H31 H 0.478112 0.508616 0.673157 0.050 Uiso 0.507(5) 1 calc R U P B 1
C32 C 0.794(3) 0.5132(3) 0.5966(10) 0.046(4) Uani 0.507(5) 1 d D . P B 1
H32 H 0.925790 0.533439 0.591682 0.056 Uiso 0.507(5) 1 calc R U P B 1
C33 C 0.648(3) 0.5097(5) 0.5012(12) 0.041(5) Uani 0.507(5) 1 d D . P B 1
H33 H 0.510762 0.490053 0.501832 0.049 Uiso 0.507(5) 1 calc R U P B 1
C34 C 0.532(5) 0.5476(6) 0.4723(12) 0.034(4) Uani 0.507(5) 1 d D . P B 1
H34 H 0.675340 0.566007 0.468372 0.041 Uiso 0.507(5) 1 calc R U P B 1
C35 C 0.375(4) 0.5476(6) 0.3818(13) 0.047(5) Uani 0.507(5) 1 d D . P B 1
H35A H 0.465757 0.532952 0.337041 0.056 Uiso 0.507(5) 1 calc R U P B 1
H35B H 0.209819 0.534620 0.388638 0.056 Uiso 0.507(5) 1 calc R U P B 1
O9 O 0.9308(14) 0.47994(18) 0.6256(5) 0.0520(17) Uani 0.507(5) 1 d D . P B 1
C36 C 0.784(2) 0.4466(3) 0.6367(8) 0.058(3) Uani 0.507(5) 1 d D . P B 1
H36A H 0.700397 0.438152 0.576419 0.070 Uiso 0.507(5) 1 calc R U P B 1
H36B H 0.649990 0.451546 0.678565 0.070 Uiso 0.507(5) 1 calc R U P B 1
C37 C 0.969(3) 0.4164(4) 0.6775(9) 0.052(3) Uani 0.507(5) 1 d D . P B 1
C38 C 1.217(2) 0.4132(3) 0.6540(9) 0.063(3) Uani 0.507(5) 1 d D . P B 1
H38 H 1.276419 0.430060 0.609697 0.075 Uiso 0.507(5) 1 calc R U P B 1
C39 C 1.381(2) 0.3860(3) 0.6938(10) 0.074(3) Uani 0.507(5) 1 d D . P B 1
H39 H 1.554405 0.384960 0.679714 0.089 Uiso 0.507(5) 1 calc R U P B 1
C40 C 1.291(3) 0.3604(4) 0.7541(11) 0.077(4) Uani 0.507(5) 1 d D . P B 1
H40 H 1.403974 0.341812 0.782624 0.093 Uiso 0.507(5) 1 calc R U P B 1
C41 C 1.036(4) 0.3615(5) 0.7735(13) 0.091(6) Uani 0.507(5) 1 d D . P B 1
H41 H 0.971436 0.342499 0.811238 0.109 Uiso 0.507(5) 1 calc R U P B 1
C42 C 0.876(3) 0.3904(3) 0.7373(9) 0.076(4) Uani 0.507(5) 1 d D . P B 1
H42 H 0.705308 0.392348 0.753494 0.091 Uiso 0.507(5) 1 calc R U P B 1
C58 C 0.453(5) 0.5978(5) 0.276(2) 0.051(6) Uani 0.507(5) 1 d D . P B 1
C59 C 0.387(6) 0.6368(5) 0.2427(18) 0.063(7) Uani 0.507(5) 1 d D . P B 1
H59A H 0.526679 0.654131 0.263888 0.076 Uiso 0.507(5) 1 calc R U P B 1
H59B H 0.228320 0.644975 0.266955 0.076 Uiso 0.507(5) 1 calc R U P B 1
H59C H 0.364018 0.636779 0.175135 0.076 Uiso 0.507(5) 1 calc R U P B 1
N101 N 0.624(2) 0.5237(2) 0.7344(7) 0.0448(19) Uani 0.493(5) 1 d D . P B 2
N102 N 0.545(2) 0.4951(3) 0.7715(6) 0.067(3) Uani 0.493(5) 1 d D . P B 2
N103 N 0.487(3) 0.4704(3) 0.8175(8) 0.093(4) Uani 0.493(5) 1 d D . P B 2
O104 O 0.662(3) 0.5887(5) 0.6226(12) 0.022(2) Uani 0.493(5) 1 d D U P B 2
O108 O 0.328(3) 0.5667(5) 0.5164(10) 0.031(3) Uani 0.493(5) 1 d D . P B 2
O111 O 0.310(4) 0.5922(6) 0.3232(12) 0.039(3) Uani 0.493(5) 1 d D . P B 2
O114 O 0.605(5) 0.5774(7) 0.2279(16) 0.113(10) Uani 0.493(5) 1 d D . P B 2
C130 C 0.439(3) 0.5660(4) 0.6096(12) 0.025(3) Uani 0.493(5) 1 d D . P B 2
H130 H 0.310163 0.575408 0.650617 0.030 Uiso 0.493(5) 1 calc R U P B 2
C131 C 0.511(2) 0.5253(3) 0.6364(8) 0.034(2) Uani 0.493(5) 1 d D . P B 2
H131 H 0.352773 0.509346 0.629730 0.041 Uiso 0.493(5) 1 calc R U P B 2
C132 C 0.704(3) 0.5092(3) 0.5732(10) 0.035(3) Uani 0.493(5) 1 d D . P B 2
H132 H 0.867793 0.523897 0.580773 0.042 Uiso 0.493(5) 1 calc R U P B 2
C133 C 0.580(4) 0.5126(5) 0.4747(13) 0.036(3) Uani 0.493(5) 1 d D . P B 2
H133 H 0.438737 0.493752 0.461876 0.043 Uiso 0.493(5) 1 calc R U P B 2
C134 C 0.490(4) 0.5526(6) 0.4499(11) 0.027(4) Uani 0.493(5) 1 d D . P B 2
H134 H 0.641876 0.569591 0.447803 0.033 Uiso 0.493(5) 1 calc R U P B 2
C135 C 0.329(4) 0.5536(6) 0.3577(12) 0.036(3) Uani 0.493(5) 1 d D . P B 2
H13A H 0.409142 0.537340 0.312979 0.043 Uiso 0.493(5) 1 calc R U P B 2
H13B H 0.155709 0.543609 0.364726 0.043 Uiso 0.493(5) 1 calc R U P B 2
O109 O 0.7497(11) 0.47064(15) 0.5994(5) 0.0402(15) Uani 0.493(5) 1 d D . P B 2
C136 C 1.006(2) 0.4567(3) 0.5947(7) 0.052(2) Uani 0.493(5) 1 d D . P B 2
H13C H 1.130058 0.477773 0.605100 0.063 Uiso 0.493(5) 1 calc R U P B 2
H13D H 1.022465 0.446041 0.532699 0.063 Uiso 0.493(5) 1 calc R U P B 2
C137 C 1.066(3) 0.4262(3) 0.6675(9) 0.043(3) Uani 0.493(5) 1 d D . P B 2
C138 C 1.121(2) 0.3900(3) 0.6405(7) 0.051(2) Uani 0.493(5) 1 d D . P B 2
H138 H 1.126920 0.384433 0.577006 0.061 Uiso 0.493(5) 1 calc R U P B 2
C139 C 1.167(3) 0.3617(3) 0.7062(9) 0.062(3) Uani 0.493(5) 1 d D . P B 2
H139 H 1.206671 0.336714 0.687928 0.075 Uiso 0.493(5) 1 calc R U P B 2
C140 C 1.155(3) 0.3704(4) 0.8002(10) 0.059(4) Uani 0.493(5) 1 d D . P B 2
H140 H 1.189286 0.351347 0.845893 0.070 Uiso 0.493(5) 1 calc R U P B 2
C141 C 1.095(2) 0.4065(3) 0.8253(7) 0.055(3) Uani 0.493(5) 1 d D . P B 2
H141 H 1.083830 0.412421 0.888401 0.066 Uiso 0.493(5) 1 calc R U P B 2
C142 C 1.0491(19) 0.4342(3) 0.7588(6) 0.049(2) Uani 0.493(5) 1 d D . P B 2
H142 H 1.005783 0.459114 0.776551 0.059 Uiso 0.493(5) 1 calc R U P B 2
C158 C 0.477(7) 0.6011(8) 0.262(3) 0.070(9) Uani 0.493(5) 1 d D . P B 2
C159 C 0.431(7) 0.6412(7) 0.232(2) 0.065(7) Uani 0.493(5) 1 d D . P B 2
H15A H 0.509265 0.658295 0.279253 0.078 Uiso 0.493(5) 1 calc R U P B 2
H15B H 0.245986 0.645923 0.222249 0.078 Uiso 0.493(5) 1 calc R U P B 2
H15C H 0.507514 0.645589 0.173753 0.078 Uiso 0.493(5) 1 calc R U P B 2
C43 C 0.7984(8) 0.46809(12) 0.3861(3) 0.0447(10) Uani 1 1 d . . . . .
C44 C 1.0526(9) 0.42828(11) 0.3023(3) 0.0403(9) Uani 1 1 d . . . . .
H44A H 0.895963 0.412585 0.302192 0.048 Uiso 1 1 calc R U . . .
H44B H 1.197540 0.414029 0.334451 0.048 Uiso 1 1 calc R U . . .
C45 C 1.1075(8) 0.43663(11) 0.2040(3) 0.0385(9) Uani 1 1 d . . . . .
H45 H 1.261349 0.453330 0.202924 0.046 Uiso 1 1 calc R U . . .
C46 C 1.1477(8) 0.39946(11) 0.1551(3) 0.0371(8) Uani 1 1 d . . . . .
C47 C 1.3352(9) 0.37256(13) 0.1750(3) 0.0484(11) Uani 1 1 d . . . . .
H47 H 1.463575 0.376131 0.224930 0.058 Uiso 1 1 calc R U . . .
C48 C 1.3340(10) 0.34000(13) 0.1209(3) 0.0506(11) Uani 1 1 d . . . . .
H48 H 1.464400 0.321491 0.133139 0.061 Uiso 1 1 calc R U . . .
C49 C 1.1446(10) 0.33453(13) 0.0496(3) 0.0489(11) Uani 1 1 d . . . . .
H49 H 1.144270 0.312023 0.013868 0.059 Uiso 1 1 calc R U . . .
C50 C 0.9543(9) 0.36146(14) 0.0293(3) 0.0484(10) Uani 1 1 d . . . . .
H50 H 0.824770 0.357639 -0.020107 0.058 Uiso 1 1 calc R U . . .
C51 C 0.9569(8) 0.39429(12) 0.0829(3) 0.0379(8) Uani 1 1 d . . . . .
C52 C 0.7906(8) 0.42789(12) 0.0767(3) 0.0405(9) Uani 1 1 d . . . . .
C53 C 0.5791(10) 0.43676(15) 0.0166(3) 0.0534(11) Uani 1 1 d . . . . .
H53 H 0.518123 0.419509 -0.030567 0.064 Uiso 1 1 calc R U . . .
C54 C 0.4569(10) 0.47107(15) 0.0259(4) 0.0586(13) Uani 1 1 d . . . . .
H54 H 0.309449 0.477188 -0.014568 0.070 Uiso 1 1 calc R U . . .
C55 C 0.5477(10) 0.49671(13) 0.0937(4) 0.0528(11) Uani 1 1 d . . . . .
H55 H 0.463483 0.520337 0.098632 0.063 Uiso 1 1 calc R U . . .
C56 C 0.7605(9) 0.48802(11) 0.1544(3) 0.0446(10) Uani 1 1 d . . . . .
H56 H 0.823086 0.505552 0.200635 0.054 Uiso 1 1 calc R U . . .
C57 C 0.8803(8) 0.45327(11) 0.1463(3) 0.0389(9) Uani 1 1 d . . . . .
O1 O 0.7345(5) 0.69050(7) 0.57750(15) 0.0284(5) Uani 1 1 d . . . . .
O2 O 0.6043(5) 0.69935(7) 0.81775(15) 0.0304(5) Uani 1 1 d . . . . .
O3 O 0.4067(5) 0.62562(7) 0.77070(16) 0.0315(5) Uani 1 1 d . . . . .
O5 O 1.1050(5) 0.66387(7) 0.47092(16) 0.0299(5) Uani 1 1 d . . . . .
O6 O 0.2204(5) 0.72890(8) 0.81657(18) 0.0388(6) Uani 1 1 d . . . . .
O7 O 0.8486(5) 0.69405(9) 0.36086(18) 0.0392(6) Uani 1 1 d . . . . .
O10 O 0.8067(6) 0.50254(8) 0.4257(3) 0.0532(9) Uani 1 1 d . . . . .
O12 O 0.6246(6) 0.44643(9) 0.3848(3) 0.0705(12) Uani 1 1 d . . . . .
O13 O 1.0170(5) 0.46382(7) 0.3502(2) 0.0397(6) Uani 1 1 d . . . . .
S1 S 0.56898(17) 0.75420(2) 0.64422(6) 0.03241(19) Uani 1 1 d . . . . .
Cl1 Cl 1.2469(2) 0.74790(3) 0.31172(6) 0.0445(2) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 110.7(3) . . ?
O1 C1 S1 108.5(2) . . ?
C2 C1 S1 106.7(2) . . ?
O2 C2 C3 106.6(3) . . ?
O2 C2 C1 107.4(3) . . ?
C3 C2 C1 114.1(3) . . ?
O3 C3 C2 108.3(3) . . ?
O3 C3 C4 112.4(3) . . ?
C2 C3 C4 110.1(3) . . ?
O4 C4 C3 107.4(8) . . ?
O104 C4 C3 113.6(7) . . ?
O4 C4 C5 105.5(8) . . ?
O104 C4 C5 112.2(7) . . ?
C3 C4 C5 106.1(3) . . ?
O1 C5 C6 107.0(3) . . ?
O1 C5 C4 106.9(3) . . ?
C6 C5 C4 115.7(3) . . ?
O5 C6 C5 107.2(3) . . ?
C8 C7 C13 119.2(4) . . ?
C8 C7 S1 121.6(3) . . ?
C13 C7 S1 119.0(3) . . ?
C7 C8 C9 120.4(4) . . ?
C8 C9 C10 121.6(5) . . ?
C12 C10 C9 117.3(4) . . ?
C12 C10 C11 121.7(6) . . ?
C9 C10 C11 121.0(6) . . ?
C10 C12 C13 121.8(4) . . ?
C7 C13 C12 119.7(4) . . ?
O6 C14 O2 124.4(3) . . ?
O6 C14 C15 124.9(4) . . ?
O2 C14 C15 110.6(3) . . ?
C16 C15 C20 119.7(3) . . ?
C16 C15 C14 122.4(4) . . ?
C20 C15 C14 117.9(3) . . ?
C15 C16 C17 119.4(4) . . ?
C18 C17 C16 120.7(4) . . ?
C17 C18 C19 119.9(4) . . ?
C20 C19 C18 119.8(4) . . ?
C19 C20 C15 120.4(4) . . ?
O3 C21 C22 111.5(3) . . ?
C27 C22 C23 117.5(4) . . ?
C27 C22 C21 122.0(4) . . ?
C23 C22 C21 120.3(4) . . ?
C24 C23 C22 121.8(5) . . ?
C23 C24 C25 120.0(5) . . ?
C26 C25 C24 119.4(5) . . ?
C25 C26 C27 120.5(5) . . ?
C22 C27 C26 120.7(5) . . ?
O7 C28 O5 125.5(3) . . ?
O7 C28 C29 126.9(3) . . ?
O5 C28 C29 107.6(3) . . ?
C28 C29 Cl1 111.2(2) . . ?
N2 N1 C31 113.5(8) . . ?
N3 N2 N1 170.2(12) . . ?
C30 O4 C4 110.5(13) . . ?
C30 O8 C34 114.7(13) . . ?
C58 O11 C35 118.8(18) . . ?
O4 C30 O8 113.2(15) . . ?
O4 C30 C31 107.1(13) . . ?
O8 C30 C31 110.3(12) . . ?
N1 C31 C32 108.7(10) . . ?
N1 C31 C30 108.0(9) . . ?
C32 C31 C30 107.9(10) . . ?
O9 C32 C31 113.3(11) . . ?
O9 C32 C33 113.5(11) . . ?
C31 C32 C33 110.4(11) . . ?
O10 C33 C34 100.7(12) . . ?
O10 C33 C32 115.3(13) . . ?
C34 C33 C32 109.6(12) . . ?
O8 C34 C35 108.3(16) . . ?
O8 C34 C33 110.2(14) . . ?
C35 C34 C33 114.8(16) . . ?
O11 C35 C34 113.0(15) . . ?
C32 O9 C36 117.2(9) . . ?
O9 C36 C37 107.2(9) . . ?
C38 C37 C42 119.9(11) . . ?
C38 C37 C36 122.6(11) . . ?
C42 C37 C36 117.4(11) . . ?
C39 C38 C37 121.0(11) . . ?
C40 C39 C38 119.4(12) . . ?
C39 C40 C41 120.3(13) . . ?
C40 C41 C42 119.8(14) . . ?
C37 C42 C41 119.3(12) . . ?
O14 C58 O11 121(2) . . ?
O14 C58 C59 122(2) . . ?
O11 C58 C59 115.5(15) . . ?
N102 N101 C131 109.3(10) . . ?
N103 N102 N101 170.5(13) . . ?
C130 O104 C4 115.4(13) . . ?
C130 O108 C134 115.0(12) . . ?
C158 O111 C135 114.9(18) . . ?
O104 C130 O108 111.9(14) . . ?
O104 C130 C131 108.5(12) . . ?
O108 C130 C131 109.3(10) . . ?
N101 C131 C130 110.1(9) . . ?
N101 C131 C132 109.8(9) . . ?
C130 C131 C132 110.8(10) . . ?
O109 C132 C133 111.9(11) . . ?
O109 C132 C131 107.2(9) . . ?
C133 C132 C131 107.0(12) . . ?
O10 C133 C132 98.5(11) . . ?
O10 C133 C134 110.6(15) . . ?
C132 C133 C134 113.0(12) . . ?
O108 C134 C135 106.1(14) . . ?
O108 C134 C133 110.7(15) . . ?
C135 C134 C133 111.4(14) . . ?
O111 C135 C134 110.0(14) . . ?
C132 O109 C136 116.6(8) . . ?
O109 C136 C137 109.9(9) . . ?
C142 C137 C138 120.2(10) . . ?
C142 C137 C136 120.2(10) . . ?
C138 C137 C136 119.5(11) . . ?
C137 C138 C139 120.0(10) . . ?
C138 C139 C140 119.4(10) . . ?
C141 C140 C139 119.5(12) . . ?
C140 C141 C142 120.1(10) . . ?
C137 C142 C141 120.8(9) . . ?
O114 C158 O111 122(2) . . ?
O114 C158 C159 128(2) . . ?
O111 C158 C159 109(2) . . ?
O12 C43 O13 128.0(4) . . ?
O12 C43 O10 125.6(4) . . ?
O13 C43 O10 106.3(3) . . ?
O13 C44 C45 109.2(3) . . ?
C57 C45 C44 113.0(4) . . ?
C57 C45 C46 102.3(3) . . ?
C44 C45 C46 108.8(3) . . ?
C47 C46 C51 120.9(4) . . ?
C47 C46 C45 128.8(4) . . ?
C51 C46 C45 110.3(4) . . ?
C46 C47 C48 119.1(5) . . ?
C49 C48 C47 120.4(4) . . ?
C48 C49 C50 120.9(4) . . ?
C49 C50 C51 118.8(4) . . ?
C46 C51 C50 120.0(4) . . ?
C46 C51 C52 108.6(4) . . ?
C50 C51 C52 131.4(4) . . ?
C53 C52 C57 120.5(4) . . ?
C53 C52 C51 131.1(4) . . ?
C57 C52 C51 108.5(4) . . ?
C52 C53 C54 119.2(5) . . ?
C53 C54 C55 120.7(5) . . ?
C56 C55 C54 120.5(4) . . ?
C55 C56 C57 118.9(5) . . ?
C56 C57 C52 120.3(4) . . ?
C56 C57 C45 129.5(4) . . ?
C52 C57 C45 110.2(3) . . ?
C1 O1 C5 112.2(2) . . ?
C14 O2 C2 118.7(3) . . ?
C3 O3 C21 112.0(3) . . ?
C28 O5 C6 117.1(3) . . ?
C43 O10 C33 118.8(7) . . ?
C43 O10 C133 115.3(8) . . ?
C43 O13 C44 116.5(3) . . ?
C7 S1 C1 102.29(17) . . ?
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
C1 O1 1.429(4) . ?
C1 C2 1.526(5) . ?
C1 S1 1.801(4) . ?
C2 O2 1.442(4) . ?
C2 C3 1.521(5) . ?
C3 O3 1.424(4) . ?
C3 C4 1.526(5) . ?
C4 O4 1.43(2) . ?
C4 O104 1.458(17) . ?
C4 C5 1.528(5) . ?
C5 O1 1.437(4) . ?
C5 C6 1.506(5) . ?
C6 O5 1.448(4) . ?
C7 C8 1.375(6) . ?
C7 C13 1.377(5) . ?
C7 S1 1.776(4) . ?
C8 C9 1.379(7) . ?
C9 C10 1.380(8) . ?
C10 C12 1.379(8) . ?
C10 C11 1.514(7) . ?
C12 C13 1.389(7) . ?
C14 O6 1.200(5) . ?
C14 O2 1.357(5) . ?
C14 C15 1.492(5) . ?
C15 C16 1.384(6) . ?
C15 C20 1.386(6) . ?
C16 C17 1.393(5) . ?
C17 C18 1.368(7) . ?
C18 C19 1.385(7) . ?
C19 C20 1.381(5) . ?
C21 O3 1.441(4) . ?
C21 C22 1.494(6) . ?
C22 C27 1.384(7) . ?
C22 C23 1.385(6) . ?
C23 C24 1.367(7) . ?
C24 C25 1.379(8) . ?
C25 C26 1.364(9) . ?
C26 C27 1.386(8) . ?
C28 O7 1.185(4) . ?
C28 O5 1.352(4) . ?
C28 C29 1.505(5) . ?
C29 Cl1 1.774(4) . ?
N1 N2 1.221(10) . ?
N1 C31 1.498(14) . ?
N2 N3 1.137(11) . ?
O4 C30 1.408(15) . ?
O8 C30 1.430(14) . ?
O8 C34 1.436(15) . ?
O11 C58 1.349(18) . ?
O11 C35 1.448(16) . ?
O14 C58 1.214(18) . ?
C30 C31 1.535(15) . ?
C31 C32 1.513(15) . ?
C32 O9 1.419(13) . ?
C32 C33 1.525(16) . ?
C33 O10 1.464(18) . ?
C33 C34 1.514(16) . ?
C34 C35 1.485(16) . ?
O9 C36 1.423(11) . ?
C36 C37 1.521(14) . ?
C37 C38 1.381(14) . ?
C37 C42 1.386(15) . ?
C38 C39 1.379(15) . ?
C39 C40 1.376(17) . ?
C40 C41 1.39(2) . ?
C41 C42 1.394(17) . ?
C58 C59 1.491(18) . ?
N101 N102 1.236(12) . ?
N101 C131 1.492(13) . ?
N102 N103 1.158(12) . ?
O104 C130 1.415(15) . ?
O108 C130 1.424(13) . ?
O108 C134 1.438(15) . ?
O111 C158 1.35(2) . ?
O111 C135 1.452(15) . ?
O114 C158 1.20(2) . ?
C130 C131 1.528(14) . ?
C131 C132 1.539(13) . ?
C132 O109 1.428(11) . ?
C132 C133 1.521(15) . ?
C133 O10 1.484(19) . ?
C133 C134 1.523(17) . ?
C134 C135 1.515(16) . ?
O109 C136 1.437(11) . ?
C136 C137 1.522(13) . ?
C137 C142 1.370(15) . ?
C137 C138 1.376(14) . ?
C138 C139 1.390(14) . ?
C139 C140 1.411(17) . ?
C140 C141 1.373(18) . ?
C141 C142 1.383(13) . ?
C158 C159 1.49(2) . ?
C43 O12 1.188(5) . ?
C43 O13 1.313(5) . ?
C43 O10 1.345(5) . ?
C44 O13 1.457(4) . ?
C44 C45 1.517(6) . ?
C45 C57 1.508(6) . ?
C45 C46 1.518(5) . ?
C46 C47 1.377(6) . ?
C46 C51 1.391(6) . ?
C47 C48 1.394(6) . ?
C48 C49 1.379(7) . ?
C49 C50 1.389(7) . ?
C50 C51 1.397(6) . ?
C51 C52 1.470(6) . ?
C52 C53 1.381(6) . ?
C52 C57 1.400(6) . ?
C53 C54 1.383(7) . ?
C54 C55 1.390(8) . ?
C55 C56 1.388(7) . ?
C56 C57 1.389(6) . ?
