#------------------------------------------------------------------------------
#$Date: 2024-12-16 19:33:52 +0200 (Mon, 16 Dec 2024) $
#$Revision: 296876 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/01/7130140.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_7130140
loop_
_publ_author_name
'Volla, Chandra'
'Nair, Akshay Murali'
'Halder, Indranil'
_publ_section_title
;
 A Metal-free Four-component Sulfonylation, Giese Cyclization,
 Selenylation Cascade via Insertion of Sulfur Dioxide
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02315F
_journal_year                    2022
_chemical_formula_moiety         'C34 H27 Br O5 S Se'
_chemical_formula_sum            'C34 H27 Br O5 S Se'
_chemical_formula_weight         706.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-22
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-03-28 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                115.650(4)
_cell_angle_beta                 98.002(3)
_cell_angle_gamma                97.217(3)
_cell_formula_units_Z            4
_cell_length_a                   7.7248(2)
_cell_length_b                   20.4230(8)
_cell_length_c                   21.7248(10)
_cell_measurement_reflns_used    6985
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      22.2340
_cell_measurement_theta_min      1.8710
_cell_volume                     2992.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ   -349.73  10.27   1.00    5.00   6.61  -9.84 -31.50    --   360
  2  ω    -60.89   0.11   1.00    5.00    --  -14.77  94.56 -34.84   61
  3  ω    -65.46  -0.46   1.00    5.00    --  -19.34  94.56 145.16   65
  4  ω   -100.81  15.19   1.00    5.00    --   -9.84 -59.25 164.08  116
  5  φ    -10.27 349.73   1.00    5.00  81.02  -9.84  31.50    --   360
  6  ω    -65.46  -0.46   1.00    5.00    --  -19.34  94.56  73.16   65
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0216290000
_diffrn_orient_matrix_UB_12      0.0322558000
_diffrn_orient_matrix_UB_13      -0.0011389000
_diffrn_orient_matrix_UB_21      -0.0329985000
_diffrn_orient_matrix_UB_22      -0.0206484000
_diffrn_orient_matrix_UB_23      -0.0366715000
_diffrn_orient_matrix_UB_31      -0.0862023000
_diffrn_orient_matrix_UB_32      -0.0092099000
_diffrn_orient_matrix_UB_33      0.0054921000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1078
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.876
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.702
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         10535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0261P)²+1.8156P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7734
_reflns_number_total             10535
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc02315f2.cif
_cod_data_source_block           cmrv_ih_8_2_10_autored
_cod_depositor_comments
;

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C68 H54 Br2 O10 S2 Se2'
_cod_original_formula_weight         1412.97
_cod_original_formula_moiety         '2(C34 H27 Br O5 S Se)'
_cod_original_formula_units_Z            2
_cod_database_code               7130140
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H52N2O2S1
_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.
;
_reflns_odcompleteness_completeness 76.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.76
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C12(H12), C41(H41), C42(H42)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C48(H48A,H48B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C17(H17), C18(H18),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29),
  C30(H30), C32(H32), C33(H33), C36(H36), C37(H37), C38(H38), C39(H39),
 C40(H40), C44(H44), C45(H45), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55),
  C57(H57), C58(H58), C60(H60), C61(H61), C63(H63), C64(H64), C66(H66), C67(H67)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C68(H68A,H68B,H68C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.790
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Se1 Se 1.03370(5) 1.10870(2) 0.68388(2) 0.02563(11) Uani 1 1 d . . . . .
Br2 Br 0.74322(8) 0.59038(3) 0.38895(3) 0.06556(19) Uani 1 1 d . . . . .
Se3 Se 0.05724(5) 0.34555(2) 0.01108(2) 0.02685(11) Uani 1 1 d . . . . .
Br4 Br 0.33449(6) 0.81757(2) 0.42151(2) 0.03509(12) Uani 1 1 d . . . . .
S1 S 0.61742(12) 0.90216(6) 0.69253(5) 0.0248(2) Uani 1 1 d . . . . .
S2 S 0.51538(12) 0.41739(5) 0.22443(5) 0.0220(2) Uani 1 1 d . . . . .
O1 O 1.4778(3) 1.09346(15) 0.66948(14) 0.0330(7) Uani 1 1 d . . . . .
O2 O 0.8527(3) 0.96455(14) 0.56678(13) 0.0215(6) Uani 1 1 d . . . . .
O3 O 0.6820(3) 0.91515(16) 0.76239(14) 0.0328(7) Uani 1 1 d . . . . .
O4 O 0.4652(3) 0.92972(17) 0.67605(16) 0.0381(8) Uani 1 1 d . . . . .
O5 O 0.4736(5) 0.5790(2) 0.5151(2) 0.0749(12) Uani 1 1 d . . . . .
O6 O 0.2641(3) 0.50595(14) 0.11207(13) 0.0232(6) Uani 1 1 d . . . . .
O7 O -0.3749(3) 0.38483(15) 0.02069(14) 0.0299(7) Uani 1 1 d . . . . .
O8 O 0.5000(3) 0.43362(15) 0.29419(14) 0.0317(7) Uani 1 1 d . . . . .
O9 O 0.6750(3) 0.45050(15) 0.21294(15) 0.0354(7) Uani 1 1 d . . . . .
O10 O 0.3353(5) 0.09431(16) 0.05080(16) 0.0504(9) Uani 1 1 d . . . . .
C1 C 1.1744(5) 1.1985(2) 0.7608(2) 0.0237(9) Uani 1 1 d . . . . .
C2 C 1.2709(5) 1.2018(2) 0.8211(2) 0.0310(10) Uani 1 1 d . . . . .
H2 H 1.276602 1.157331 0.824736 0.037 Uiso 1 1 calc R . . . .
C3 C 1.3596(6) 1.2699(2) 0.8763(2) 0.0360(11) Uani 1 1 d . . . . .
H3 H 1.428519 1.271830 0.917070 0.043 Uiso 1 1 calc R . . . .
C4 C 1.3479(5) 1.3340(2) 0.8721(2) 0.0350(11) Uani 1 1 d . . . . .
H4 H 1.406431 1.380585 0.910315 0.042 Uiso 1 1 calc R . . . .
C5 C 1.2512(5) 1.3312(2) 0.8123(2) 0.0343(11) Uani 1 1 d . . . . .
H5 H 1.243309 1.376002 0.809663 0.041 Uiso 1 1 calc R . . . .
C6 C 1.1655(5) 1.2637(2) 0.7562(2) 0.0264(9) Uani 1 1 d . . . . .
H6 H 1.101075 1.262023 0.714823 0.032 Uiso 1 1 calc R . . . .
C7 C 1.1966(5) 1.0401(2) 0.67977(19) 0.0214(9) Uani 1 1 d . . . . .
H7 H 1.259443 1.053733 0.728461 0.026 Uiso 1 1 calc R . . . .
C8 C 1.3326(5) 1.0510(2) 0.6400(2) 0.0234(9) Uani 1 1 d . . . . .
C9 C 1.2764(5) 1.0091(2) 0.5636(2) 0.0247(9) Uani 1 1 d . . . . .
H9 H 1.349938 1.019479 0.536034 0.030 Uiso 1 1 calc R . . . .
C10 C 1.1278(5) 0.9573(2) 0.5313(2) 0.0218(9) Uani 1 1 d . . . . .
H10 H 1.095571 0.935457 0.481716 0.026 Uiso 1 1 calc R . . . .
C11 C 1.0060(5) 0.9308(2) 0.56877(19) 0.0203(9) Uani 1 1 d . . . . .
C12 C 1.0940(4) 0.9591(2) 0.64525(18) 0.0190(8) Uani 1 1 d . . . . .
H12 H 1.184228 0.928294 0.646352 0.023 Uiso 1 1 calc R . . . .
C13 C 0.9622(4) 0.9476(2) 0.68708(19) 0.0187(8) Uani 1 1 d . . . . .
C14 C 0.7885(5) 0.9343(2) 0.65994(19) 0.0193(8) Uani 1 1 d . . . . .
C15 C 0.7163(5) 0.9390(2) 0.5938(2) 0.0241(9) Uani 1 1 d . . . . .
H15A H 0.649213 0.889206 0.557790 0.029 Uiso 1 1 calc R . . . .
H15B H 0.631664 0.972972 0.603691 0.029 Uiso 1 1 calc R . . . .
C16 C 0.9455(5) 0.8464(2) 0.5272(2) 0.0227(9) Uani 1 1 d . . . . .
C17 C 0.8379(5) 0.8170(2) 0.4603(2) 0.0305(10) Uani 1 1 d . . . . .
H17 H 0.805983 0.849727 0.442237 0.037 Uiso 1 1 calc R . . . .
C18 C 0.7767(5) 0.7414(3) 0.4198(2) 0.0393(12) Uani 1 1 d . . . . .
H18 H 0.702604 0.722222 0.374493 0.047 Uiso 1 1 calc R . . . .
C19 C 0.8245(6) 0.6944(2) 0.4458(2) 0.0375(12) Uani 1 1 d . . . . .
C20 C 0.9303(6) 0.7205(2) 0.5112(2) 0.0388(11) Uani 1 1 d . . . . .
H20 H 0.962089 0.687274 0.528622 0.047 Uiso 1 1 calc R . . . .
C21 C 0.9898(5) 0.7970(2) 0.5514(2) 0.0305(10) Uani 1 1 d . . . . .
H21 H 1.063086 0.815658 0.596792 0.037 Uiso 1 1 calc R . . . .
C22 C 1.0485(4) 0.9572(2) 0.75701(19) 0.0202(9) Uani 1 1 d . . . . .
C23 C 1.0363(5) 1.0176(2) 0.8173(2) 0.0286(10) Uani 1 1 d . . . . .
H23 H 0.959305 1.049468 0.814441 0.034 Uiso 1 1 calc R . . . .
C24 C 1.1349(5) 1.0324(2) 0.8819(2) 0.0342(11) Uani 1 1 d . . . . .
H24 H 1.126982 1.074517 0.922895 0.041 Uiso 1 1 calc R . . . .
C25 C 1.2450(5) 0.9855(3) 0.8864(2) 0.0338(11) Uani 1 1 d . . . . .
H25 H 1.312084 0.995279 0.930662 0.041 Uiso 1 1 calc R . . . .
C26 C 1.2577(5) 0.9250(2) 0.8273(2) 0.0334(11) Uani 1 1 d . . . . .
H26 H 1.332327 0.892513 0.830483 0.040 Uiso 1 1 calc R . . . .
C27 C 1.1607(5) 0.9115(2) 0.7628(2) 0.0257(9) Uani 1 1 d . . . . .
H27 H 1.171653 0.870149 0.721783 0.031 Uiso 1 1 calc R . . . .
C28 C 0.5727(5) 0.8056(2) 0.6381(2) 0.0271(10) Uani 1 1 d . . . . .
C29 C 0.6694(5) 0.7615(2) 0.6561(2) 0.0339(11) Uani 1 1 d . . . . .
H29 H 0.761221 0.783460 0.697342 0.041 Uiso 1 1 calc R . . . .
C30 C 0.6324(6) 0.6856(3) 0.6140(2) 0.0424(12) Uani 1 1 d . . . . .
H30 H 0.696367 0.654950 0.626817 0.051 Uiso 1 1 calc R . . . .
C31 C 0.5005(6) 0.6544(3) 0.5527(3) 0.0468(13) Uani 1 1 d . . . . .
C32 C 0.4066(6) 0.6985(3) 0.5345(3) 0.0483(13) Uani 1 1 d . . . . .
H32 H 0.316874 0.676694 0.492625 0.058 Uiso 1 1 calc R . . . .
C33 C 0.4417(5) 0.7746(3) 0.5768(2) 0.0399(12) Uani 1 1 d . . . . .
H33 H 0.377201 0.805133 0.564104 0.048 Uiso 1 1 calc R . . . .
C34 C 0.3384(8) 0.5430(3) 0.4505(3) 0.091(2) Uani 1 1 d . . . . .
H34A H 0.365536 0.564443 0.419574 0.137 Uiso 1 1 calc GR . . . .
H34B H 0.220943 0.550394 0.460967 0.137 Uiso 1 1 calc GR . . . .
H34C H 0.337578 0.489680 0.427456 0.137 Uiso 1 1 calc GR . . . .
C35 C -0.1140(5) 0.2549(2) -0.0500(2) 0.0297(10) Uani 1 1 d . . . . .
C36 C -0.1962(6) 0.2089(2) -0.0258(3) 0.0430(12) Uani 1 1 d . . . . .
H36 H -0.172560 0.222427 0.022702 0.052 Uiso 1 1 calc R . . . .
C37 C -0.3121(6) 0.1434(3) -0.0729(3) 0.0501(13) Uani 1 1 d . . . . .
H37 H -0.370927 0.112730 -0.056208 0.060 Uiso 1 1 calc R . . . .
C38 C -0.3444(6) 0.1216(3) -0.1435(3) 0.0488(14) Uani 1 1 d . . . . .
H38 H -0.422666 0.075796 -0.175472 0.059 Uiso 1 1 calc R . . . .
C39 C -0.2618(6) 0.1671(3) -0.1675(3) 0.0485(13) Uani 1 1 d . . . . .
H39 H -0.284338 0.152667 -0.216210 0.058 Uiso 1 1 calc R . . . .
C40 C -0.1465(5) 0.2335(2) -0.1211(2) 0.0368(11) Uani 1 1 d . . . . .
H40 H -0.089507 0.264407 -0.137957 0.044 Uiso 1 1 calc R . . . .
C41 C -0.0867(5) 0.3922(2) 0.0815(2) 0.0219(9) Uani 1 1 d . . . . .
H41 H -0.150364 0.353080 0.091173 0.026 Uiso 1 1 calc R . . . .
C42 C 0.0284(5) 0.4548(2) 0.15090(19) 0.0199(8) Uani 1 1 d . . . . .
H42 H -0.054205 0.471670 0.183571 0.024 Uiso 1 1 calc R . . . .
C43 C 0.1133(4) 0.5232(2) 0.14455(19) 0.0194(8) Uani 1 1 d . . . . .
C44 C -0.0095(5) 0.5387(2) 0.09486(19) 0.0232(9) Uani 1 1 d . . . . .
H44 H 0.023651 0.584307 0.093417 0.028 Uiso 1 1 calc R . . . .
C45 C -0.1610(5) 0.4934(2) 0.0528(2) 0.0242(9) Uani 1 1 d . . . . .
H45 H -0.232136 0.508817 0.024315 0.029 Uiso 1 1 calc R . . . .
C46 C -0.2230(5) 0.4202(2) 0.04861(19) 0.0234(9) Uani 1 1 d . . . . .
C47 C 0.1675(5) 0.4268(2) 0.18461(19) 0.0204(9) Uani 1 1 d . . . . .
C48 C 0.4052(5) 0.4938(2) 0.1529(2) 0.0242(9) Uani 1 1 d . . . . .
H48A H 0.473987 0.542353 0.190618 0.029 Uiso 1 1 calc R . . . .
H48B H 0.487075 0.469863 0.122907 0.029 Uiso 1 1 calc R . . . .
C49 C 0.3390(5) 0.4457(2) 0.1850(2) 0.0212(9) Uani 1 1 d . . . . .
C50 C 0.0913(5) 0.3787(2) 0.2142(2) 0.0250(9) Uani 1 1 d . . . . .
C51 C 0.0488(5) 0.3020(2) 0.1754(3) 0.0366(11) Uani 1 1 d . . . . .
H51 H 0.078703 0.279332 0.130967 0.044 Uiso 1 1 calc R . . . .
C52 C -0.0372(6) 0.2580(3) 0.2007(3) 0.0481(14) Uani 1 1 d . . . . .
H52 H -0.064411 0.205513 0.173873 0.058 Uiso 1 1 calc R . . . .
C53 C -0.0825(6) 0.2907(3) 0.2645(3) 0.0509(14) Uani 1 1 d . . . . .
H53 H -0.143098 0.260745 0.281457 0.061 Uiso 1 1 calc R . . . .
C54 C -0.0410(6) 0.3663(3) 0.3037(3) 0.0462(13) Uani 1 1 d . . . . .
H54 H -0.071199 0.388414 0.348128 0.055 Uiso 1 1 calc R . . . .
C55 C 0.0452(5) 0.4108(3) 0.2789(2) 0.0366(11) Uani 1 1 d . . . . .
H55 H 0.072656 0.463260 0.306207 0.044 Uiso 1 1 calc R . . . .
C56 C 0.1720(5) 0.5931(2) 0.21504(19) 0.0204(9) Uani 1 1 d . . . . .
C57 C 0.2888(5) 0.6539(2) 0.2197(2) 0.0267(9) Uani 1 1 d . . . . .
H57 H 0.333877 0.649581 0.179899 0.032 Uiso 1 1 calc R . . . .
C58 C 0.3405(5) 0.7201(2) 0.2806(2) 0.0274(10) Uani 1 1 d . . . . .
H58 H 0.420439 0.760829 0.282818 0.033 Uiso 1 1 calc R . . . .
C59 C 0.2744(5) 0.7262(2) 0.3378(2) 0.0248(9) Uani 1 1 d . . . . .
C60 C 0.1566(5) 0.6673(2) 0.3346(2) 0.0274(9) Uani 1 1 d . . . . .
H60 H 0.111321 0.672333 0.374584 0.033 Uiso 1 1 calc R . . . .
C61 C 0.1048(5) 0.6016(2) 0.2738(2) 0.0272(10) Uani 1 1 d . . . . .
H61 H 0.022485 0.561682 0.271809 0.033 Uiso 1 1 calc R . . . .
C62 C 0.4743(5) 0.3202(2) 0.1738(2) 0.0226(9) Uani 1 1 d . . . . .
C63 C 0.4667(5) 0.2896(2) 0.1024(2) 0.0313(10) Uani 1 1 d . . . . .
H63 H 0.492032 0.320623 0.081063 0.038 Uiso 1 1 calc R . . . .
C64 C 0.4219(6) 0.2139(2) 0.0632(2) 0.0362(11) Uani 1 1 d . . . . .
H64 H 0.416469 0.192142 0.014312 0.043 Uiso 1 1 calc R . . . .
C65 C 0.3842(5) 0.1686(2) 0.0947(2) 0.0306(10) Uani 1 1 d . . . . .
C66 C 0.3977(5) 0.1991(2) 0.1659(2) 0.0290(10) Uani 1 1 d . . . . .
H66 H 0.376637 0.168154 0.187546 0.035 Uiso 1 1 calc R . . . .
C67 C 0.4422(5) 0.2754(2) 0.2053(2) 0.0289(10) Uani 1 1 d . . . . .
H67 H 0.450677 0.297039 0.254426 0.035 Uiso 1 1 calc R . . . .
C68 C 0.2522(7) 0.0474(3) 0.0768(3) 0.0505(13) Uani 1 1 d . . . . .
H68A H 0.207291 -0.002967 0.038383 0.076 Uiso 1 1 calc GR . . . .
H68B H 0.152593 0.067109 0.096634 0.076 Uiso 1 1 calc GR . . . .
H68C H 0.340086 0.045905 0.113127 0.076 Uiso 1 1 calc GR . . . .
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'
Br Br -0.2901 2.4595 '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'
Se Se -0.0929 2.2259 '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
C1 Se1 C7 99.80(16) . . ?
C35 Se3 C41 98.63(15) . . ?
O3 S1 O4 120.39(18) . . ?
O3 S1 C14 111.10(17) . . ?
O3 S1 C28 107.82(18) . . ?
O4 S1 C14 106.11(17) . . ?
O4 S1 C28 107.91(19) . . ?
C28 S1 C14 101.93(18) . . ?
O8 S2 O9 119.57(17) . . ?
O8 S2 C49 109.60(17) . . ?
O8 S2 C62 108.38(18) . . ?
O9 S2 C49 104.30(17) . . ?
O9 S2 C62 109.36(17) . . ?
C62 S2 C49 104.60(17) . . ?
C15 O2 C11 112.3(3) . . ?
C31 O5 C34 117.7(5) . . ?
C48 O6 C43 114.0(3) . . ?
C65 O10 C68 117.7(3) . . ?
C2 C1 Se1 123.9(3) . . ?
C2 C1 C6 119.5(4) . . ?
C6 C1 Se1 116.4(3) . . ?
C1 C2 C3 120.1(4) . . ?
C4 C3 C2 120.2(4) . . ?
C3 C4 C5 120.0(4) . . ?
C4 C5 C6 120.5(4) . . ?
C5 C6 C1 119.6(4) . . ?
C8 C7 Se1 107.3(3) . . ?
C8 C7 C12 111.5(3) . . ?
C12 C7 Se1 111.5(2) . . ?
O1 C8 C7 122.1(4) . . ?
O1 C8 C9 122.6(3) . . ?
C9 C8 C7 115.2(3) . . ?
C10 C9 C8 123.1(3) . . ?
C9 C10 C11 123.9(3) . . ?
O2 C11 C10 105.3(3) . . ?
O2 C11 C12 107.4(3) . . ?
O2 C11 C16 109.1(3) . . ?
C10 C11 C12 111.4(3) . . ?
C10 C11 C16 108.4(3) . . ?
C12 C11 C16 114.8(3) . . ?
C11 C12 C7 112.9(3) . . ?
C13 C12 C7 111.4(3) . . ?
C13 C12 C11 112.1(3) . . ?
C14 C13 C12 118.2(3) . . ?
C14 C13 C22 128.0(3) . . ?
C22 C13 C12 113.7(3) . . ?
C13 C14 S1 124.0(3) . . ?
C13 C14 C15 123.4(3) . . ?
C15 C14 S1 112.4(2) . . ?
O2 C15 C14 113.1(3) . . ?
C17 C16 C11 118.0(4) . . ?
C21 C16 C11 124.5(4) . . ?
C21 C16 C17 117.5(4) . . ?
C18 C17 C16 121.4(4) . . ?
C19 C18 C17 119.1(4) . . ?
C18 C19 Br2 118.7(4) . . ?
C18 C19 C20 121.7(4) . . ?
C20 C19 Br2 119.5(4) . . ?
C19 C20 C21 118.3(4) . . ?
C16 C21 C20 121.9(4) . . ?
C23 C22 C13 120.5(3) . . ?
C27 C22 C13 120.7(3) . . ?
C27 C22 C23 118.3(4) . . ?
C22 C23 C24 120.9(4) . . ?
C25 C24 C23 119.7(4) . . ?
C26 C25 C24 120.3(4) . . ?
C25 C26 C27 119.5(4) . . ?
C22 C27 C26 121.3(4) . . ?
C29 C28 S1 119.9(3) . . ?
C29 C28 C33 120.6(4) . . ?
C33 C28 S1 119.4(3) . . ?
C30 C29 C28 120.0(4) . . ?
C29 C30 C31 119.4(4) . . ?
O5 C31 C30 114.8(5) . . ?
O5 C31 C32 124.7(5) . . ?
C32 C31 C30 120.4(5) . . ?
C31 C32 C33 120.5(4) . . ?
C32 C33 C28 119.1(4) . . ?
C36 C35 Se3 122.5(3) . . ?
C40 C35 Se3 117.8(3) . . ?
C40 C35 C36 119.6(4) . . ?
C37 C36 C35 119.3(5) . . ?
C38 C37 C36 121.3(5) . . ?
C37 C38 C39 119.3(4) . . ?
C38 C39 C40 120.4(5) . . ?
C39 C40 C35 120.1(4) . . ?
C42 C41 Se3 112.7(2) . . ?
C46 C41 Se3 106.7(3) . . ?
C46 C41 C42 111.6(3) . . ?
C43 C42 C41 113.5(3) . . ?
C47 C42 C41 111.9(3) . . ?
C47 C42 C43 111.6(3) . . ?
O6 C43 C42 107.9(3) . . ?
O6 C43 C44 104.1(3) . . ?
O6 C43 C56 110.6(3) . . ?
C44 C43 C42 111.9(3) . . ?
C44 C43 C56 109.1(3) . . ?
C56 C43 C42 112.8(3) . . ?
C45 C44 C43 124.8(4) . . ?
C44 C45 C46 122.5(4) . . ?
O7 C46 C41 122.1(4) . . ?
O7 C46 C45 122.4(4) . . ?
C45 C46 C41 115.6(3) . . ?
C49 C47 C42 119.5(3) . . ?
C49 C47 C50 126.4(3) . . ?
C50 C47 C42 114.0(3) . . ?
O6 C48 C49 112.8(3) . . ?
C47 C49 S2 123.6(3) . . ?
C47 C49 C48 123.2(3) . . ?
C48 C49 S2 113.2(2) . . ?
C51 C50 C47 121.2(4) . . ?
C51 C50 C55 118.7(4) . . ?
C55 C50 C47 119.9(4) . . ?
C50 C51 C52 120.8(5) . . ?
C53 C52 C51 119.7(5) . . ?
C54 C53 C52 120.3(4) . . ?
C53 C54 C55 120.4(5) . . ?
C54 C55 C50 120.1(4) . . ?
C57 C56 C43 118.5(3) . . ?
C61 C56 C43 123.5(3) . . ?
C61 C56 C57 117.8(4) . . ?
C58 C57 C56 121.8(4) . . ?
C59 C58 C57 118.9(4) . . ?
C58 C59 Br4 120.3(3) . . ?
C58 C59 C60 120.7(4) . . ?
C60 C59 Br4 118.9(3) . . ?
C61 C60 C59 120.2(4) . . ?
C60 C61 C56 120.5(4) . . ?
C63 C62 S2 119.9(3) . . ?
C67 C62 S2 119.3(3) . . ?
C67 C62 C63 120.8(4) . . ?
C64 C63 C62 118.8(4) . . ?
C63 C64 C65 120.4(4) . . ?
O10 C65 C64 115.8(4) . . ?
O10 C65 C66 123.8(4) . . ?
C66 C65 C64 120.4(4) . . ?
C65 C66 C67 119.2(4) . . ?
C62 C67 C66 120.3(4) . . ?
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
Se1 C1 1.918(4) . ?
Se1 C7 1.980(4) . ?
Br2 C19 1.899(4) . ?
Se3 C35 1.925(4) . ?
Se3 C41 1.990(4) . ?
Br4 C59 1.901(4) . ?
S1 O3 1.425(3) . ?
S1 O4 1.432(3) . ?
S1 C14 1.767(4) . ?
S1 C28 1.762(4) . ?
S2 O8 1.430(3) . ?
S2 O9 1.436(3) . ?
S2 C49 1.796(4) . ?
S2 C62 1.762(4) . ?
O1 C8 1.222(4) . ?
O2 C11 1.448(4) . ?
O2 C15 1.424(4) . ?
O5 C31 1.365(6) . ?
O5 C34 1.451(6) . ?
O6 C43 1.448(4) . ?
O6 C48 1.423(4) . ?
O7 C46 1.215(4) . ?
O10 C65 1.362(5) . ?
O10 C68 1.438(5) . ?
C1 C2 1.384(5) . ?
C1 C6 1.386(5) . ?
C2 C3 1.389(6) . ?
C3 C4 1.365(6) . ?
C4 C5 1.379(6) . ?
C5 C6 1.384(5) . ?
C7 C8 1.504(5) . ?
C7 C12 1.535(5) . ?
C8 C9 1.467(5) . ?
C9 C10 1.325(5) . ?
C10 C11 1.519(5) . ?
C11 C12 1.521(5) . ?
C11 C16 1.529(5) . ?
C12 C13 1.516(5) . ?
C13 C14 1.331(5) . ?
C13 C22 1.489(5) . ?
C14 C15 1.514(5) . ?
C16 C17 1.396(5) . ?
C16 C21 1.382(6) . ?
C17 C18 1.381(6) . ?
C18 C19 1.370(6) . ?
C19 C20 1.372(6) . ?
C20 C21 1.393(6) . ?
C22 C23 1.383(5) . ?
C22 C27 1.382(5) . ?
C23 C24 1.384(5) . ?
C24 C25 1.383(6) . ?
C25 C26 1.370(6) . ?
C26 C27 1.387(5) . ?
C28 C29 1.383(6) . ?
C28 C33 1.390(5) . ?
C29 C30 1.382(6) . ?
C30 C31 1.394(6) . ?
C31 C32 1.374(7) . ?
C32 C33 1.386(6) . ?
C35 C36 1.392(6) . ?
C35 C40 1.384(6) . ?
C36 C37 1.376(6) . ?
C37 C38 1.375(7) . ?
C38 C39 1.379(7) . ?
C39 C40 1.383(6) . ?
C41 C42 1.539(5) . ?
C41 C46 1.497(5) . ?
C42 C43 1.538(5) . ?
C42 C47 1.520(5) . ?
C43 C44 1.500(5) . ?
C43 C56 1.530(5) . ?
C44 C45 1.326(5) . ?
C45 C46 1.470(5) . ?
C47 C49 1.330(5) . ?
C47 C50 1.495(5) . ?
C48 C49 1.511(5) . ?
C50 C51 1.385(6) . ?
C50 C55 1.390(6) . ?
C51 C52 1.388(6) . ?
C52 C53 1.372(7) . ?
C53 C54 1.367(7) . ?
C54 C55 1.390(6) . ?
C56 C57 1.396(5) . ?
C56 C61 1.395(5) . ?
C57 C58 1.381(5) . ?
C58 C59 1.371(5) . ?
C59 C60 1.384(5) . ?
C60 C61 1.374(5) . ?
C62 C63 1.388(5) . ?
C62 C67 1.379(5) . ?
C63 C64 1.371(6) . ?
C64 C65 1.395(6) . ?
C65 C66 1.376(6) . ?
C66 C67 1.380(5) . ?
