#------------------------------------------------------------------------------
#$Date: 2025-10-06 10:35:37 +0200 (Mon 06 de Oct de 2025) $
#$Revision: 302595 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/54/1575417.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_1575417
loop_
_publ_author_name
'Dhara, Barun'
'Bulgarevich, Kirill'
'Takimiya, Kazuo'
_publ_section_title
;
 Radical cation salts of
 dinaphtho[2,3-b:2′,3′-f]thieno[3,2-b]thiophene:
 characteristic crystal structures and properties
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              6333
_journal_page_last               6340
_journal_paper_doi               10.1039/D5CE00680E
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C6 H5 Br, 2.5(C22 H12 S2), 2(F6 P)'
_chemical_formula_sum            'C61 H35 Br F12 P2 S5'
_chemical_formula_weight         1298.04
_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
_audit_creation_date             2025-02-17
_audit_creation_method
;
Olex2 1.5-ac7-012
(compiled 2024.11.06 svn.r97f918c9 for Rigaku Oxford Diffraction, GUI svn.r7082)
;
_audit_update_record
;
2025-07-06 deposited with the CCDC.	2025-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                70.7150(10)
_cell_angle_beta                 85.9760(10)
_cell_angle_gamma                79.0570(10)
_cell_formula_units_Z            2
_cell_length_a                   13.57690(10)
_cell_length_b                   14.0578(2)
_cell_length_c                   14.6788(2)
_cell_measurement_reflns_used    29471
_cell_measurement_temperature    200
_cell_measurement_theta_max      77.4930
_cell_measurement_theta_min      3.8140
_cell_volume                     2596.24(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.136a 64-bit (release 23-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac7-012 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-012 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.00
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00 -37.00   0.50    0.30    --  -47.91 154.00   2.00  146
  2  ω    -89.00 -20.00   0.50    0.30    --  -47.91 120.00-155.00  138
  3  ω   -120.00 -62.00   0.50    0.30    --  -47.91-154.00 -36.00  116
  4  ω     56.00 120.00   0.50    0.30    --   47.91 154.00   2.00  128
  5  ω     15.00  89.00   0.50    0.30    --   47.91-120.00 120.00  148
  6  ω     31.00 111.00   0.50    0.30    --   47.91-154.00 -36.00  160
  7  ω   -109.00 -28.00   0.50    2.00    --  -97.00 120.00-155.00  162
  8  ω   -162.00 -62.00   0.50    2.00    --  -97.00-154.00 -36.00  200
  9  ω   -166.00 -85.00   0.50    2.00    --  -97.00-120.00 120.00  162
 10  ω   -132.00 -37.00   0.50    2.00    --  -97.00 154.00   2.00  190
 11  ω     37.00 109.00   0.50    2.00    --  106.00-120.00 120.00  144
 12  ω     80.00 175.00   0.50    2.00    --  106.00 120.00-155.00  190
 13  ω     34.00 132.00   0.50    2.00    --  106.00-154.00 -36.00  196
 14  ω     56.00 162.00   0.50    2.00    --  106.00 154.00   2.00  212
 15  ω    -31.00  26.00   0.50    0.30    --  -47.91  19.00-150.00  114
 16  ω    -31.00  26.00   0.50    0.30    --  -47.91  19.00-180.00  114
 17  ω    -31.00  26.00   0.50    0.30    --  -47.91  19.00  60.00  114
 18  ω    -45.00  25.00   0.50    0.30    --  -47.91  37.00 120.00  140
 19  ω    -24.00  27.00   0.50    0.30    --   47.91 -19.00 -30.00  102
 20  ω    -23.00  41.00   0.50    0.30    --   47.91 -37.00-150.00  128
 21  ω   -169.00 -85.00   0.50    2.00    --  -97.00 -54.00-169.66  168
 22  ω     37.00 112.00   0.50    2.00    --  106.00-125.00  90.00  150
 23  ω     34.00 100.00   0.50    2.00    --  106.00 -77.00 -30.00  132
 24  ω     34.00 100.00   0.50    2.00    --  106.00 -77.00 -90.00  132
 25  ω     34.00 106.00   0.50    2.00    --  106.00 -94.00 -30.00  144
 26  ω     37.00 112.00   0.50    2.00    --  106.00-125.00  30.00  150
 27  ω     98.00 175.00   0.50    2.00    --  106.00  15.00 -90.00  154
 28  ω     34.00 106.00   0.50    2.00    --  106.00 -94.00-120.00  144
 29  ω     37.00 112.00   0.50    2.00    --  106.00-125.00-150.00  150
 30  ω     37.00 112.00   0.50    2.00    --  106.00-125.00-150.00  150
 31  ω     97.00 175.00   0.50    2.00    --  106.00  45.00   0.00  156
 32  ω     76.00 175.00   0.50    2.00    --  106.00 125.00-180.00  198
 33  ω     34.00 106.00   0.50    2.00    --  106.00 -94.00 -60.00  144
 34  ω     34.00 100.00   0.50    2.00    --  106.00 -77.00  90.00  132
 35  ω     34.00 106.00   0.50    2.00    --  106.00 -94.00-180.00  144
 36  ω     34.00 100.00   0.50    2.00    --  106.00 -77.00-180.00  132
 37  ω     37.00 112.00   0.50    2.00    --  106.00-125.00 -90.00  150
 38  ω     98.00 175.00   0.50    2.00    --  106.00  15.00-180.00  154
 39  ω     34.00 106.00   0.50    2.00    --  106.00 -94.00 120.00  144
 40  ω     34.00 106.00   0.50    2.00    --  106.00 -94.00 120.00  144
 41  ω     98.00 175.00   0.50    2.00    --  106.00  30.00  60.00  154
 42  ω     34.00 106.00   0.50    2.00    --  106.00 -94.00 -90.00  144
 43  ω     34.00 100.00   0.50    2.00    --  106.00 -77.00  30.00  132
 44  ω     34.00 106.00   0.50    2.00    --  106.00 -94.00 150.00  144
 45  ω     76.00 175.00   0.50    2.00    --  106.00 125.00-180.00  198
 46  ω     34.00  69.00   0.50    2.00    --  106.00 -61.00-180.00   70
 47  ω     34.00 100.00   0.50    2.00    --  106.00 -77.00 -60.00  132
 48  ω     85.00 175.00   0.50    2.00    --  106.00  77.00  60.00  180
 49  ω     37.00 112.00   0.50    2.00    --  106.00-125.00  60.00  150
 50  ω     37.00 112.00   0.50    2.00    --  106.00-125.00  60.00  150
 51  ω     98.00 175.00   0.50    2.00    --  106.00  15.00-150.00  154
 52  ω     37.00 112.00   0.50    2.00    --  106.00-125.00 150.00  150
 53  ω     37.00 112.00   0.50    2.00    --  106.00-125.00 150.00  150
 54  ω     85.00 175.00   0.50    2.00    --  106.00  77.00 -60.00  180
 55  ω     98.00 175.00   0.50    2.00    --  106.00  15.00  60.00  154
 56  ω     34.00 100.00   0.50    2.00    --  106.00 -77.00-150.00  132
 57  ω     85.00 175.00   0.50    2.00    --  106.00  77.00  60.00  180
 58  ω     92.00 175.00   0.50    2.00    --  106.00  61.00 -30.00  166
 59  ω     92.00 175.00   0.50    2.00    --  106.00  61.00 -30.00  166
 60  ω     34.00 100.00   0.50    2.00    --  106.00 -77.00   0.00  132
 61  ω     76.00 175.00   0.50    2.00    --  106.00 125.00  90.00  198
 62  ω     76.00 175.00   0.50    2.00    --  106.00 125.00-120.00  198
 63  ω     98.00 175.00   0.50    2.00    --  106.00  15.00   0.00  154
 64  ω     76.00 175.00   0.50    2.00    --  106.00 125.00  30.00  198
 65  ω     76.00 175.00   0.50    2.00    --  106.00 125.00  30.00  198
 66  ω     34.00 106.00   0.50    2.00    --  106.00 -94.00  90.00  144
 67  ω     37.00 112.00   0.50    2.00    --  106.00-125.00-120.00  150
 68  ω     98.00 175.00   0.50    2.00    --  106.00  30.00-150.00  154
 69  ω     98.00 175.00   0.50    2.00    --  106.00  30.00   0.00  154
 70  ω     97.00 175.00   0.50    2.00    --  106.00  45.00 -90.00  156
 71  ω     97.00 175.00   0.50    2.00    --  106.00  45.00 -60.00  156
 72  ω     92.00 175.00   0.50    2.00    --  106.00  61.00-120.00  166
 73  ω     85.00 154.00   0.50    2.00    --  106.00  77.00  30.00  138
 74  ω    133.00 175.00   0.50    2.00    --  106.00  77.00  30.00   84
 75  ω     86.00 130.00   0.50    2.00    --  106.00  77.00 150.00   88
 76  ω    130.00 172.00   0.50    2.00    --  106.00 125.00 -60.00   84
 77  ω     39.00  64.00   0.50    2.00    --  106.00 -61.00 120.00   50
 78  ω    116.00 149.00   0.50    2.00    --  106.00  45.00 120.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20949
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.379
_diffrn_reflns_theta_min         3.190
_exptl_absorpt_coefficient_mu    4.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.136a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       needle
_exptl_crystal_F_000             1308
_refine_diff_density_max         1.790
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.094
_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     731
_refine_ls_number_reflns         20949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1217P)²+2.3257P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1906
_refine_ls_wR_factor_ref         0.1990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17935
_reflns_number_total             20949
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by 179.9980° 
around [-0.00 -0.00 1.00] (reciprocal) or [-0.01 -0.33 0.95] (direct)
;
_cod_data_source_file            d5ce00680e2.cif
_cod_data_source_block           dntt-pf6-bb-200k
_cod_depositor_comments
'Adding full bibliography for 1575411--1575428.cif.'
_cod_database_code               1575417
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H S Br P F'
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5681(11)
 0.4319(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C53(H53), C27(H27), C11(H11), C35(H35), C46(H46), C22(H22),
 C42(H42), C18(H18), C51(H51), C37(H37), C24(H24), C25(H25), C13(H13), C63(H63),
  C26(H26), C14(H14), C15(H15), C65(H65), C6(H6), C48(H48), C38(H38), C39(H39),
 C62(H62), C16(H16), C60(H60), C49(H49), C40(H40), C50(H50), C61(H61), C58(H58),
  C2(H2), C5(H5), C3(H3), C4(H4)
;
_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 1.446
_oxdiff_exptl_absorpt_empirical_full_min 0.732
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
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
Br7 Br -0.20776(6) 0.36994(6) 0.22082(4) 0.0801(2) Uani 1 1 d . . . . .
S20 S 0.08431(6) 0.23969(7) 0.46988(6) 0.0320(2) Uani 1 1 d . . . . .
S31 S 0.33313(6) 0.38054(6) 0.44844(6) 0.03197(19) Uani 1 1 d . . . . .
S44 S 0.50745(6) 0.15643(7) 0.53568(6) 0.0323(2) Uani 1 1 d . . . . .
S55 S 0.25661(6) 0.01940(6) 0.55028(7) 0.0332(2) Uani 1 1 d . . . . .
S56 S -0.12408(7) 0.42835(7) 0.50745(7) 0.0379(2) Uani 1 1 d . . . . .
P68 P 0.51368(9) 0.32532(9) 0.75700(8) 0.0438(3) Uani 1 1 d . . . . .
P77 P 0.07657(9) 0.07484(9) 0.25453(8) 0.0452(3) Uani 1 1 d . . . . .
F81 F -0.0032(3) 0.0248(3) 0.3320(2) 0.0716(9) Uani 1 1 d . . . . .
F79 F 0.1557(3) 0.1264(3) 0.1791(2) 0.0766(10) Uani 1 1 d . . . . .
F78 F 0.1433(3) 0.0713(4) 0.3400(3) 0.0904(13) Uani 1 1 d . . . . .
F83 F 0.0080(3) 0.0788(4) 0.1714(3) 0.1029(15) Uani 1 1 d . . . . .
C34 C 0.3995(3) 0.1170(3) 0.4121(3) 0.0311(7) Uani 1 1 d . . . . .
F72 F 0.4699(4) 0.2363(4) 0.8342(3) 0.1095(18) Uani 1 1 d . . . . .
C10 C 0.1943(3) 0.2814(2) 0.5899(3) 0.0296(7) Uani 1 1 d . . . . .
F73 F 0.4740(4) 0.2978(5) 0.6742(3) 0.127(2) Uani 1 1 d . . . . .
C8 C 0.1828(3) 0.3000(2) 0.4246(3) 0.0291(7) Uani 1 1 d . . . . .
C29 C 0.1922(3) 0.3336(3) 0.2430(3) 0.0321(7) Uani 1 1 d . . . . .
H29 H 0.135843 0.303226 0.241449 0.039 Uiso 1 1 calc R U . . .
C32 C 0.4071(3) 0.0972(2) 0.5780(3) 0.0297(7) Uani 1 1 d . . . . .
C12 C 0.1708(3) 0.2399(3) 0.7629(3) 0.0350(8) Uani 1 1 d . . . . .
C43 C 0.4857(3) 0.1598(3) 0.4177(3) 0.0325(7) Uani 1 1 d . . . . .
F80 F 0.1306(4) -0.0358(3) 0.2603(4) 0.0981(13) Uani 1 1 d . . . . .
C19 C 0.1075(3) 0.2374(3) 0.5870(3) 0.0318(7) Uani 1 1 d . . . . .
C28 C 0.2445(3) 0.3758(3) 0.1571(3) 0.0326(7) Uani 1 1 d . . . . .
C53 C 0.3948(3) 0.0603(3) 0.7597(3) 0.0332(7) Uani 1 1 d . . . . .
H53 H 0.450164 0.091738 0.762105 0.040 Uiso 1 1 calc R U . . .
C30 C 0.2233(3) 0.3367(2) 0.3294(3) 0.0300(7) Uani 1 1 d . . . . .
C52 C 0.3442(3) 0.0158(3) 0.8455(3) 0.0349(8) Uani 1 1 d . . . . .
C54 C 0.3657(3) 0.0592(2) 0.6727(3) 0.0302(7) Uani 1 1 d . . . . .
C9 C 0.2362(3) 0.3167(2) 0.4954(3) 0.0290(7) Uani 1 1 d . . . . .
C27 C 0.2150(3) 0.3723(3) 0.0672(3) 0.0377(8) Uani 1 1 d . . . . .
H27 H 0.159240 0.341581 0.064304 0.045 Uiso 1 1 calc R U . . .
C11 C 0.2251(3) 0.2825(3) 0.6776(3) 0.0328(7) Uani 1 1 d . . . . .
H11 H 0.282083 0.311557 0.680563 0.039 Uiso 1 1 calc R U . . .
C35 C 0.3716(3) 0.1157(3) 0.3233(3) 0.0342(7) Uani 1 1 d . . . . .
H35 H 0.314494 0.087683 0.318734 0.041 Uiso 1 1 calc R U . . .
C23 C 0.3284(3) 0.4218(3) 0.1599(3) 0.0338(7) Uani 1 1 d . . . . .
C47 C 0.2607(3) -0.0300(3) 0.8405(3) 0.0355(8) Uani 1 1 d . . . . .
C66 C 0.0185(3) 0.5300(3) 0.3702(3) 0.0359(8) Uani 1 1 d . . . . .
C46 C 0.2286(3) -0.0297(3) 0.7502(3) 0.0372(8) Uani 1 1 d . . . . .
H46 H 0.171952 -0.058826 0.746545 0.045 Uiso 1 1 calc R U . . .
C67 C -0.0250(3) 0.4919(3) 0.4648(3) 0.0363(8) Uani 1 1 d . . . . .
C21 C 0.3072(3) 0.3835(3) 0.3313(3) 0.0307(7) Uani 1 1 d . . . . .
C22 C 0.3592(3) 0.4252(3) 0.2491(3) 0.0336(7) Uani 1 1 d . . . . .
H22 H 0.415087 0.455991 0.251518 0.040 Uiso 1 1 calc R U . . .
C42 C 0.5419(3) 0.1990(3) 0.3383(3) 0.0355(8) Uani 1 1 d . . . . .
H42 H 0.599434 0.225859 0.344137 0.043 Uiso 1 1 calc R U . . .
F82 F 0.0219(4) 0.1846(3) 0.2544(4) 0.1118(17) Uani 1 1 d . . . . .
C33 C 0.3553(3) 0.0820(3) 0.5058(3) 0.0302(7) Uani 1 1 d . . . . .
C17 C 0.0851(3) 0.1974(3) 0.7575(3) 0.0364(8) Uani 1 1 d . . . . .
F75 F 0.5492(5) 0.3559(6) 0.8406(3) 0.146(3) Uani 1 1 d . . . . .
C18 C 0.0536(3) 0.1971(3) 0.6680(3) 0.0354(8) Uani 1 1 d . . . . .
H18 H -0.004019 0.169435 0.664249 0.043 Uiso 1 1 calc R U . . .
C45 C 0.2812(3) 0.0134(3) 0.6687(3) 0.0325(7) Uani 1 1 d . . . . .
C51 C 0.3760(3) 0.0139(3) 0.9361(3) 0.0419(9) Uani 1 1 d . . . . .
H51 H 0.431510 0.044670 0.939792 0.050 Uiso 1 1 calc R U . . .
C37 C 0.4005(3) 0.1583(3) 0.1478(3) 0.0437(9) Uani 1 1 d . . . . .
H37 H 0.343722 0.130374 0.141718 0.052 Uiso 1 1 calc R U . . .
C24 C 0.3789(3) 0.4650(3) 0.0726(3) 0.0400(8) Uani 1 1 d . . . . .
H24 H 0.433723 0.497984 0.073029 0.048 Uiso 1 1 calc R U . . .
C25 C 0.3490(3) 0.4597(3) -0.0124(3) 0.0433(9) Uani 1 1 d . . . . .
H25 H 0.384435 0.487835 -0.070305 0.052 Uiso 1 1 calc R U . . .
C13 C 0.2018(3) 0.2369(3) 0.8541(3) 0.0410(9) Uani 1 1 d . . . . .
H13 H 0.258861 0.265132 0.858534 0.049 Uiso 1 1 calc R U . . .
C63 C 0.0140(3) 0.5731(3) 0.1040(3) 0.0436(9) Uani 1 1 d . . . . .
H63 H -0.041562 0.543544 0.098083 0.052 Uiso 1 1 calc R U . . .
C64 C 0.0416(3) 0.5707(3) 0.1967(3) 0.0375(8) Uani 1 1 d . . . . .
F70 F 0.5590(6) 0.4114(4) 0.6801(3) 0.147(3) Uani 1 1 d . . . . .
C36 C 0.4281(3) 0.1561(3) 0.2402(3) 0.0361(8) Uani 1 1 d . . . . .
C26 C 0.2677(3) 0.4137(3) -0.0156(3) 0.0427(9) Uani 1 1 d . . . . .
H26 H 0.248416 0.410860 -0.075434 0.051 Uiso 1 1 calc R U . . .
C57 C 0.1015(3) 0.5757(3) 0.3741(3) 0.0386(8) Uani 1 1 d . . . . .
C59 C 0.1257(3) 0.6156(3) 0.2038(3) 0.0386(8) Uani 1 1 d . . . . .
C14 C 0.1497(4) 0.1934(3) 0.9360(3) 0.0480(10) Uani 1 1 d . . . . .
H14 H 0.171490 0.190964 0.996947 0.058 Uiso 1 1 calc R U . . .
C15 C 0.0655(4) 0.1528(3) 0.9308(3) 0.0498(11) Uani 1 1 d . . . . .
H15 H 0.030132 0.123574 0.988363 0.060 Uiso 1 1 calc R U . . .
C65 C -0.0120(3) 0.5273(3) 0.2821(3) 0.0403(9) Uani 1 1 d . . . . .
H65 H -0.067958 0.496758 0.279590 0.048 Uiso 1 1 calc R U . . .
C6 C -0.1729(4) 0.2284(3) 0.4085(3) 0.0465(9) Uani 1 1 d . . . . .
H6 H -0.119633 0.194455 0.378812 0.056 Uiso 1 1 calc R U . . .
C41 C 0.5141(3) 0.1994(3) 0.2477(3) 0.0369(8) Uani 1 1 d . . . . .
C48 C 0.2101(3) -0.0754(3) 0.9271(3) 0.0450(9) Uani 1 1 d . . . . .
H48 H 0.152852 -0.104430 0.925013 0.054 Uiso 1 1 calc R U . . .
C38 C 0.4550(4) 0.2003(4) 0.0676(3) 0.0516(11) Uani 1 1 d . . . . .
H38 H 0.435478 0.201711 0.006219 0.062 Uiso 1 1 calc R U . . .
C39 C 0.5390(4) 0.2412(4) 0.0748(3) 0.0503(11) Uani 1 1 d . . . . .
H39 H 0.575987 0.269823 0.018099 0.060 Uiso 1 1 calc R U . . .
C62 C 0.0667(4) 0.6174(4) 0.0239(3) 0.0503(10) Uani 1 1 d . . . . .
H62 H 0.046668 0.619562 -0.037619 0.060 Uiso 1 1 calc R U . . .
C16 C 0.0324(3) 0.1542(3) 0.8437(3) 0.0431(9) Uani 1 1 d . . . . .
H16 H -0.025552 0.126273 0.841434 0.052 Uiso 1 1 calc R U . . .
C60 C 0.1801(3) 0.6593(3) 0.1180(4) 0.0483(10) Uani 1 1 d . . . . .
H60 H 0.237136 0.687971 0.121641 0.058 Uiso 1 1 calc R U . . .
C49 C 0.2436(4) -0.0776(3) 1.0145(3) 0.0522(11) Uani 1 1 d . . . . .
H49 H 0.210177 -0.109899 1.072340 0.063 Uiso 1 1 calc R U . . .
C40 C 0.5692(3) 0.2409(3) 0.1624(3) 0.0450(9) Uani 1 1 d . . . . .
H40 H 0.626995 0.268531 0.165889 0.054 Uiso 1 1 calc R U . . .
C50 C 0.3257(4) -0.0331(3) 1.0191(3) 0.0475(10) Uani 1 1 d . . . . .
H50 H 0.347328 -0.035043 1.079935 0.057 Uiso 1 1 calc R U . . .
C61 C 0.1504(4) 0.6599(4) 0.0309(4) 0.0512(11) Uani 1 1 d . . . . .
H61 H 0.186773 0.689593 -0.025778 0.061 Uiso 1 1 calc R U . . .
C58 C 0.1561(3) 0.6177(3) 0.2940(3) 0.0414(9) Uani 1 1 d . . . . .
H58 H 0.212266 0.647196 0.298254 0.050 Uiso 1 1 calc R U . . .
C1 C -0.2328(3) 0.3170(4) 0.3549(3) 0.0463(10) Uani 1 1 d . . . . .
C2 C -0.3117(4) 0.3678(4) 0.3959(5) 0.0601(13) Uani 1 1 d . . . . .
H2 H -0.353056 0.428668 0.358191 0.072 Uiso 1 1 calc R U . . .
C5 C -0.1916(5) 0.1895(4) 0.5061(4) 0.0620(14) Uani 1 1 d . . . . .
H5 H -0.150553 0.128546 0.544051 0.074 Uiso 1 1 calc R U . . .
C3 C -0.3280(4) 0.3256(5) 0.4952(5) 0.0685(17) Uani 1 1 d . . . . .
H3 H -0.381209 0.358400 0.525827 0.082 Uiso 1 1 calc R U . . .
C4 C -0.2680(5) 0.2376(5) 0.5487(4) 0.0710(17) Uani 1 1 d . . . . .
H4 H -0.279983 0.209923 0.616056 0.085 Uiso 1 1 calc R U . . .
F76 F 0.4142(7) 0.3943(6) 0.7644(5) 0.199(4) Uani 1 1 d . . . . .
F69 F 0.6118(6) 0.2543(7) 0.7522(6) 0.205(4) 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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 S20 C19 91.38(17) . . ?
C9 S31 C21 90.94(17) . . ?
C32 S44 C43 90.77(18) . . ?
C33 S55 C45 91.05(18) . . ?
C67 S56 C57 90.27(19) . 2_566 ?
F73 P68 F72 90.9(2) . . ?
F73 P68 F75 177.6(4) . . ?
F73 P68 F70 88.7(2) . . ?
F75 P68 F72 89.0(2) . . ?
F70 P68 F72 178.6(4) . . ?
F70 P68 F75 91.5(2) . . ?
F76 P68 F72 86.9(4) . . ?
F76 P68 F73 91.7(5) . . ?
F76 P68 F75 85.9(5) . . ?
F76 P68 F70 94.4(4) . . ?
F69 P68 F72 91.5(4) . . ?
F69 P68 F73 88.6(5) . . ?
F69 P68 F75 93.8(5) . . ?
F69 P68 F70 87.2(5) . . ?
F69 P68 F76 178.4(4) . . ?
F79 P77 F81 178.6(2) . . ?
F78 P77 F81 89.13(19) . . ?
F78 P77 F79 89.90(19) . . ?
F83 P77 F81 89.6(2) . . ?
F83 P77 F79 91.3(2) . . ?
F83 P77 F78 178.5(3) . . ?
F83 P77 F82 91.4(3) . . ?
F80 P77 F81 88.5(2) . . ?
F80 P77 F79 92.6(2) . . ?
F80 P77 F78 90.1(3) . . ?
F80 P77 F83 90.7(3) . . ?
F80 P77 F82 177.2(3) . . ?
F82 P77 F81 89.6(2) . . ?
F82 P77 F79 89.3(2) . . ?
F82 P77 F78 87.8(3) . . ?
C35 C34 C43 119.4(3) . . ?
C35 C34 C33 130.8(3) . . ?
C33 C34 C43 109.8(3) . . ?
C9 C10 C19 110.1(3) . . ?
C11 C10 C19 119.4(3) . . ?
C11 C10 C9 130.4(3) . . ?
C30 C8 S20 133.1(3) . . ?
C9 C8 S20 113.5(3) . . ?
C9 C8 C30 113.3(3) . . ?
C30 C29 C28 119.8(3) . . ?
C54 C32 S44 132.7(3) . . ?
C33 C32 S44 113.7(3) . . ?
C33 C32 C54 113.6(3) . . ?
C11 C12 C17 119.8(3) . . ?
C13 C12 C11 120.9(4) . . ?
C13 C12 C17 119.2(4) . . ?
C34 C43 S44 112.6(3) . . ?
C42 C43 S44 125.5(3) . . ?
C42 C43 C34 121.9(4) . . ?
C10 C19 S20 112.0(3) . . ?
C18 C19 S20 125.9(3) . . ?
C18 C19 C10 122.1(3) . . ?
C29 C28 C27 121.0(4) . . ?
C29 C28 C23 119.7(3) . . ?
C23 C28 C27 119.3(3) . . ?
C54 C53 C52 121.2(3) . . ?
C29 C30 C8 130.0(3) . . ?
C29 C30 C21 120.0(3) . . ?
C21 C30 C8 110.0(3) . . ?
C53 C52 C47 118.6(4) . . ?
C53 C52 C51 121.4(4) . . ?
C51 C52 C47 120.0(4) . . ?
C32 C54 C45 109.9(3) . . ?
C53 C54 C32 130.5(3) . . ?
C53 C54 C45 119.5(3) . . ?
C10 C9 S31 133.9(3) . . ?
C8 C9 S31 113.1(3) . . ?
C8 C9 C10 112.9(3) . . ?
C26 C27 C28 119.7(4) . . ?
C10 C11 C12 119.3(3) . . ?
C34 C35 C36 119.8(3) . . ?
C22 C23 C28 120.0(3) . . ?
C24 C23 C28 118.8(4) . . ?
C24 C23 C22 121.2(4) . . ?
C46 C47 C52 120.6(3) . . ?
C48 C47 C52 118.6(4) . . ?
C48 C47 C46 120.8(4) . . ?
C57 C66 C67 110.8(4) . . ?
C65 C66 C67 128.7(4) . . ?
C65 C66 C57 120.5(4) . . ?
C45 C46 C47 118.6(3) . . ?
C66 C67 S56 133.2(3) . . ?
C67 C67 S56 114.1(4) 2_566 . ?
C67 C67 C66 112.7(4) 2_566 . ?
C30 C21 S31 112.6(3) . . ?
C22 C21 S31 125.9(3) . . ?
C22 C21 C30 121.5(3) . . ?
C21 C22 C23 119.0(3) . . ?
C43 C42 C41 119.4(4) . . ?
C34 C33 S55 133.8(3) . . ?
C32 C33 S55 113.0(3) . . ?
C32 C33 C34 113.1(3) . . ?
C18 C17 C12 120.6(3) . . ?
C18 C17 C16 120.5(4) . . ?
C16 C17 C12 118.9(4) . . ?
C19 C18 C17 118.7(4) . . ?
C54 C45 S55 112.4(3) . . ?
C46 C45 S55 126.2(3) . . ?
C46 C45 C54 121.4(4) . . ?
C50 C51 C52 119.5(4) . . ?
C38 C37 C36 120.4(4) . . ?
C25 C24 C23 120.3(4) . . ?
C24 C25 C26 121.1(4) . . ?
C14 C13 C12 120.2(4) . . ?
C62 C63 C64 120.6(4) . . ?
C63 C64 C59 118.7(4) . . ?
C65 C64 C63 122.8(4) . . ?
C65 C64 C59 118.5(4) . . ?
C35 C36 C37 121.4(4) . . ?
C35 C36 C41 119.7(3) . . ?
C37 C36 C41 118.9(4) . . ?
C27 C26 C25 120.7(4) . . ?
C66 C57 S56 112.1(3) . 2_566 ?
C58 C57 S56 125.4(3) . 2_566 ?
C58 C57 C66 122.4(4) . . ?
C60 C59 C64 118.8(4) . . ?
C58 C59 C64 121.7(4) . . ?
C58 C59 C60 119.5(4) . . ?
C13 C14 C15 120.7(4) . . ?
C16 C15 C14 121.2(4) . . ?
C66 C65 C64 119.3(4) . . ?
C1 C6 C5 118.8(5) . . ?
C42 C41 C36 119.7(4) . . ?
C42 C41 C40 121.7(4) . . ?
C40 C41 C36 118.6(4) . . ?
C49 C48 C47 120.2(4) . . ?
C37 C38 C39 120.8(4) . . ?
C40 C39 C38 121.2(4) . . ?
C63 C62 C61 120.8(4) . . ?
C15 C16 C17 119.7(4) . . ?
C61 C60 C59 120.1(4) . . ?
C48 C49 C50 120.9(4) . . ?
C39 C40 C41 120.1(4) . . ?
C51 C50 C49 120.8(4) . . ?
C60 C61 C62 121.0(4) . . ?
C57 C58 C59 117.6(4) . . ?
C6 C1 Br7 118.9(4) . . ?
C6 C1 C2 122.0(5) . . ?
C2 C1 Br7 119.2(4) . . ?
C1 C2 C3 117.2(5) . . ?
C4 C5 C6 120.7(6) . . ?
C4 C3 C2 120.8(5) . . ?
C5 C4 C3 120.4(5) . . ?
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
Br7 C1 1.891(5) . ?
S20 C8 1.697(4) . ?
S20 C19 1.759(4) . ?
S31 C9 1.710(4) . ?
S31 C21 1.764(4) . ?
S44 C32 1.705(4) . ?
S44 C43 1.761(4) . ?
S55 C33 1.714(4) . ?
S55 C45 1.764(4) . ?
S56 C67 1.723(4) . ?
S56 C57 1.767(4) 2_566 ?
P68 F72 1.566(3) . ?
P68 F73 1.548(4) . ?
P68 F75 1.560(4) . ?
P68 F70 1.548(4) . ?
P68 F76 1.526(6) . ?
P68 F69 1.518(6) . ?
P77 F81 1.596(3) . ?
P77 F79 1.582(3) . ?
P77 F78 1.581(4) . ?
P77 F83 1.567(4) . ?
P77 F80 1.566(4) . ?
P77 F82 1.580(4) . ?
C34 C43 1.432(5) . ?
C34 C35 1.389(5) . ?
C34 C33 1.430(5) . ?
C10 C19 1.440(5) . ?
C10 C9 1.427(5) . ?
C10 C11 1.388(5) . ?
C8 C30 1.430(5) . ?
C8 C9 1.412(5) . ?
C29 C28 1.409(5) . ?
C29 C30 1.381(5) . ?
C32 C54 1.430(5) . ?
C32 C33 1.406(5) . ?
C12 C11 1.419(5) . ?
C12 C17 1.424(6) . ?
C12 C13 1.417(5) . ?
C43 C42 1.362(6) . ?
C19 C18 1.363(5) . ?
C28 C27 1.424(5) . ?
C28 C23 1.423(5) . ?
C53 C52 1.403(5) . ?
C53 C54 1.370(5) . ?
C30 C21 1.426(5) . ?
C52 C47 1.424(5) . ?
C52 C51 1.418(6) . ?
C54 C45 1.431(5) . ?
C27 C26 1.377(6) . ?
C35 C36 1.405(6) . ?
C23 C22 1.419(5) . ?
C23 C24 1.415(5) . ?
C47 C46 1.421(6) . ?
C47 C48 1.415(6) . ?
C66 C67 1.441(6) . ?
C66 C57 1.413(6) . ?
C66 C65 1.399(6) . ?
C46 C45 1.369(6) . ?
C67 C67 1.376(8) 2_566 ?
C21 C22 1.368(5) . ?
C42 C41 1.406(6) . ?
C17 C18 1.410(6) . ?
C17 C16 1.419(5) . ?
C51 C50 1.381(6) . ?
C37 C36 1.423(6) . ?
C37 C38 1.366(7) . ?
C24 C25 1.369(6) . ?
C25 C26 1.391(7) . ?
C13 C14 1.370(6) . ?
C63 C64 1.424(6) . ?
C63 C62 1.360(7) . ?
C64 C59 1.431(6) . ?
C64 C65 1.417(6) . ?
C36 C41 1.440(6) . ?
C57 C58 1.365(6) . ?
C59 C60 1.428(6) . ?
C59 C58 1.425(6) . ?
C14 C15 1.388(7) . ?
C15 C16 1.378(7) . ?
C6 C1 1.375(7) . ?
C6 C5 1.379(7) . ?
C41 C40 1.422(6) . ?
C48 C49 1.380(7) . ?
C38 C39 1.396(8) . ?
C39 C40 1.375(7) . ?
C62 C61 1.405(7) . ?
C60 C61 1.364(7) . ?
C49 C50 1.394(7) . ?
C1 C2 1.387(7) . ?
C2 C3 1.399(9) . ?
C5 C4 1.358(9) . ?
C3 C4 1.370(10) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5681(11)
2 0.4319(11)
