#------------------------------------------------------------------------------
#$Date: 2024-08-05 21:55:39 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/64/7716456.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_7716456
loop_
_publ_author_name
'Krieft, Jonas'
'Neumann, Beate'
'Stammler, Hans-Georg'
'Mitzel, Norbert W.'
_publ_section_title
;
 Oxidation-dependent Lewis acidity in chalcogen adducts of Sb/P frustrated
 Lewis pairs.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11762
_journal_page_last               11768
_journal_paper_doi               10.1039/d4dt01591f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C19 H20 Cl4 F10 O2 P S Sb'
_chemical_formula_sum            'C19 H20 Cl4 F10 O2 P S Sb'
_chemical_formula_weight         796.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-16
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.4434(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   8.83394(11)
_cell_length_b                   19.19795(19)
_cell_length_c                   49.5311(5)
_cell_measurement_reflns_used    89184
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      34.6870
_cell_measurement_theta_min      2.8050
_cell_volume                     8397.49(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00   8.00   1.00   38.50    --  -22.30 -77.00-120.00   50
  2  ω    -85.00 -35.00   1.00   38.50    --  -22.30 139.00-110.03   50
  3  ω    -82.00 -32.00   1.00   38.50    --  -22.30 135.00  20.00   50
  4  ω     -3.00  91.00   1.00   38.50    --   22.30  57.00 150.00   94
  5  ω    -46.00  47.00   1.00   38.50    --   22.30 -57.00-120.00   93
  6  ω    -46.00  47.00   1.00   38.50    --   22.30 -57.00   0.00   93
  7  ω     17.00  92.00   1.00   38.50    --   22.30-149.00 -85.53   75
  8  ω     -3.00  91.00   1.00   38.50    --   22.30  57.00 -90.00   94
  9  ω    -55.00  56.00   1.00   38.50    --   22.30 -19.00  60.00  111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0144251000
_diffrn_orient_matrix_UB_12      0.0018892000
_diffrn_orient_matrix_UB_13      -0.0140038000
_diffrn_orient_matrix_UB_21      0.0771400000
_diffrn_orient_matrix_UB_22      0.0076144000
_diffrn_orient_matrix_UB_23      0.0030113000
_diffrn_orient_matrix_UB_31      0.0170489000
_diffrn_orient_matrix_UB_32      -0.0361110000
_diffrn_orient_matrix_UB_33      -0.0001005000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            162456
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         2.539
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.584
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.408
_refine_diff_density_min         -2.549
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.343
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1039
_refine_ls_number_reflns         24488
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.344
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0895
_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)+105.6168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22879
_reflns_number_total             24488
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01591f2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7716449--7716457.cif.'
_cod_original_cell_volume        8397.50(16)
_cod_database_code               7716456
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 H20 Cl4 F10 O2 P S Sb'
_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_max   0.845
_shelx_estimated_absorpt_t_min   0.764
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
S2 \\sim C24 \\sim H24A \\sim H24B: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Uanis(S2) = Uanis(C24)
3.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C5(H5A,H5B), C24(H24A,H24B)
3.b Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C7(H7A,H7B,H7C), C8(H8A,H8B,
 H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_olex2_date_sample_data_collection 2023-05-11
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.386
_oxdiff_exptl_absorpt_empirical_full_min 0.673
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Sb1 Sb 0.29546(4) 0.52405(2) 0.42257(2) 0.01317(8) Uani 1 1 d . . . . .
Sb2 Sb 0.02231(4) 0.04442(2) 0.41191(2) 0.00931(7) Uani 1 1 d . . . . .
Sb3 Sb -0.32679(4) -0.02686(2) 0.26081(2) 0.01209(8) Uani 1 1 d . . . . .
Cl9 Cl -0.81416(18) -0.11355(10) 0.21867(4) 0.0262(4) Uani 1 1 d . . . . .
Cl10 Cl -0.7690(2) -0.25882(9) 0.19072(4) 0.0264(4) Uani 1 1 d . . . . .
Cl11 Cl -0.4448(2) -0.32599(8) 0.19049(3) 0.0242(3) Uani 1 1 d . . . . .
Cl12 Cl -0.1797(2) -0.25563(8) 0.22418(3) 0.0232(3) Uani 1 1 d . . . . .
S3 S -0.26051(19) 0.00053(8) 0.21063(3) 0.0179(3) Uani 1 1 d . . . . .
P3 P -0.34685(19) 0.09511(8) 0.22029(3) 0.0150(3) Uani 1 1 d . . . . .
F21 F -0.0736(4) 0.0464(2) 0.28863(9) 0.0224(8) Uani 1 1 d . . . . .
F22 F 0.0077(5) -0.0154(3) 0.25476(9) 0.0295(10) Uani 1 1 d . . . . .
F23 F -0.0206(7) -0.1337(3) 0.28600(12) 0.0483(16) Uani 1 1 d . . . . .
F24 F -0.0848(5) -0.0696(3) 0.31946(10) 0.0324(10) Uani 1 1 d . . . . .
F25 F 0.1298(5) -0.0547(3) 0.30123(10) 0.0379(12) Uani 1 1 d . . . . .
F26 F -0.3430(5) 0.0042(2) 0.31926(8) 0.0220(8) Uani 1 1 d . . . . .
F27 F -0.5644(4) 0.0021(2) 0.29881(8) 0.0203(8) Uani 1 1 d . . . . .
F28 F -0.5729(6) -0.1353(2) 0.29946(12) 0.0414(13) Uani 1 1 d . . . . .
F29 F -0.3431(5) -0.1444(2) 0.31337(11) 0.0340(11) Uani 1 1 d . . . . .
F30 F -0.5083(7) -0.0982(3) 0.33883(11) 0.0468(15) Uani 1 1 d . . . . .
O5 O -0.2723(5) -0.1267(2) 0.25182(10) 0.0169(9) Uani 1 1 d . . . . .
O6 O -0.5345(5) -0.0617(2) 0.24687(10) 0.0163(9) Uani 1 1 d . . . . .
C39 C -0.0861(7) -0.0175(4) 0.27595(14) 0.0210(13) Uani 1 1 d . . . . .
C40 C -0.0153(8) -0.0697(4) 0.29605(16) 0.0254(15) Uani 1 1 d . . . . .
C41 C -0.4306(7) -0.0322(3) 0.30118(13) 0.0164(12) Uani 1 1 d . . . . .
C42 C -0.4644(9) -0.1033(4) 0.31392(15) 0.0233(14) Uani 1 1 d . . . . .
C43 C -0.3903(7) 0.0823(3) 0.25539(12) 0.0124(11) Uani 1 1 d . . . . .
H43A H -0.499224 0.089865 0.258654 0.015 Uiso 1 1 calc R U . . .
H43B H -0.329205 0.113291 0.267353 0.015 Uiso 1 1 calc R U . . .
C44 C -0.1962(8) 0.1620(4) 0.21677(13) 0.0211(13) Uani 1 1 d . . . . .
C45 C -0.0713(9) 0.1467(5) 0.23842(16) 0.0335(18) Uani 1 1 d . . . . .
H45A H -0.113906 0.150639 0.256438 0.050 Uiso 1 1 calc R U . . .
H45B H 0.011284 0.180366 0.236680 0.050 Uiso 1 1 calc R U . . .
H45C H -0.032259 0.099465 0.235863 0.050 Uiso 1 1 calc R U . . .
C46 C -0.2578(11) 0.2353(4) 0.2215(2) 0.039(2) Uani 1 1 d . . . . .
H46A H -0.331338 0.247091 0.207049 0.058 Uiso 1 1 calc R U . . .
H46B H -0.174189 0.268850 0.221457 0.058 Uiso 1 1 calc R U . . .
H46C H -0.307404 0.236962 0.238942 0.058 Uiso 1 1 calc R U . . .
C47 C -0.1225(10) 0.1556(5) 0.18934(17) 0.0368(19) Uani 1 1 d . . . . .
H47A H -0.083648 0.108166 0.187124 0.055 Uiso 1 1 calc R U . . .
H47B H -0.038767 0.188889 0.188302 0.055 Uiso 1 1 calc R U . . .
H47C H -0.197736 0.165565 0.174984 0.055 Uiso 1 1 calc R U . . .
C48 C -0.5253(8) 0.1158(4) 0.20102(15) 0.0224(14) Uani 1 1 d . . . . .
C49 C -0.6154(9) 0.1733(4) 0.21549(18) 0.0317(17) Uani 1 1 d . . . . .
H49A H -0.647424 0.155995 0.233064 0.047 Uiso 1 1 calc R U . . .
H49B H -0.704825 0.185842 0.204427 0.047 Uiso 1 1 calc R U . . .
H49C H -0.551063 0.214427 0.218140 0.047 Uiso 1 1 calc R U . . .
C50 C -0.4889(10) 0.1402(4) 0.17234(15) 0.0292(16) Uani 1 1 d . . . . .
H50A H -0.441659 0.186352 0.173218 0.044 Uiso 1 1 calc R U . . .
H50B H -0.582635 0.142674 0.161381 0.044 Uiso 1 1 calc R U . . .
H50C H -0.419158 0.107091 0.164153 0.044 Uiso 1 1 calc R U . . .
C51 C -0.6203(9) 0.0498(4) 0.19910(18) 0.0306(17) Uani 1 1 d . . . . .
H51A H -0.566472 0.014554 0.188703 0.046 Uiso 1 1 calc R U . . .
H51B H -0.717603 0.060244 0.190077 0.046 Uiso 1 1 calc R U . . .
H51C H -0.637887 0.031961 0.217300 0.046 Uiso 1 1 calc R U . . .
C52 C -0.3811(7) -0.1572(3) 0.23636(13) 0.0155(12) Uani 1 1 d . . . . .
C53 C -0.5226(7) -0.1232(3) 0.23418(13) 0.0144(11) Uani 1 1 d . . . . .
C54 C -0.6406(7) -0.1542(3) 0.21985(13) 0.0166(12) Uani 1 1 d . . . . .
C55 C -0.6180(8) -0.2182(3) 0.20717(13) 0.0177(12) Uani 1 1 d . . . . .
C56 C -0.4774(8) -0.2495(3) 0.20790(12) 0.0166(12) Uani 1 1 d . . . . .
C57 C -0.3573(8) -0.2187(3) 0.22257(13) 0.0178(12) Uani 1 1 d . . . . .
Cl1 Cl -0.19044(19) 0.60499(11) 0.37873(4) 0.0323(4) Uani 1 1 d . . . . .
Cl2 Cl -0.1556(2) 0.75471(9) 0.35285(4) 0.0252(3) Uani 1 1 d . . . . .
Cl3 Cl 0.1605(2) 0.82810(8) 0.35529(4) 0.0226(3) Uani 1 1 d . . . . .
Cl4 Cl 0.43109(19) 0.75783(8) 0.38762(4) 0.0217(3) Uani 1 1 d . . . . .
Cl5 Cl 0.51262(17) 0.07587(9) 0.46335(3) 0.0204(3) Uani 1 1 d . . . . .
Cl6 Cl 0.54415(19) 0.22881(9) 0.48628(4) 0.0235(3) Uani 1 1 d . . . . .
Cl7 Cl 0.2652(2) 0.32863(8) 0.48315(3) 0.0240(3) Uani 1 1 d . . . . .
Cl8 Cl -0.02791(18) 0.28347(8) 0.44991(3) 0.0181(3) Uani 1 1 d . . . . .
S1 S 0.3886(2) 0.48966(8) 0.37428(3) 0.0207(3) Uani 1 1 d . . . . .
S2 S -0.10592(17) 0.00706(8) 0.45677(3) 0.0150(2) Uani 1 1 d . . . . .
P1 P 0.2933(2) 0.39694(9) 0.38427(4) 0.0186(3) Uani 1 1 d . . . . .
P2 P -0.04857(18) -0.08952(8) 0.44349(3) 0.0121(3) Uani 1 1 d . . . . .
F1 F 0.2636(5) 0.5026(2) 0.48175(8) 0.0247(9) Uani 1 1 d . . . . .
F2 F 0.0491(5) 0.4955(2) 0.45924(9) 0.0243(9) Uani 1 1 d . . . . .
F3 F 0.0353(5) 0.6359(2) 0.45519(10) 0.0288(10) Uani 1 1 d . . . . .
F4 F 0.2516(5) 0.6470(2) 0.47567(11) 0.0327(11) Uani 1 1 d . . . . .
F5 F 0.0633(6) 0.5999(3) 0.49579(11) 0.0401(12) Uani 1 1 d . . . . .
F6 F 0.5398(5) 0.4570(2) 0.45461(9) 0.0231(8) Uani 1 1 d . . . . .
F7 F 0.6332(5) 0.5102(2) 0.41968(9) 0.0297(10) Uani 1 1 d . . . . .
F8 F 0.6037(7) 0.6343(3) 0.44544(14) 0.062(2) Uani 1 1 d . . . . .
F9 F 0.5189(6) 0.5797(3) 0.48029(12) 0.0443(14) Uani 1 1 d . . . . .
F10 F 0.7414(5) 0.5585(2) 0.46579(10) 0.0306(10) Uani 1 1 d . . . . .
F11 F 0.1453(5) 0.1268(2) 0.36550(9) 0.0226(8) Uani 1 1 d . . . . .
F12 F 0.0914(4) 0.0175(2) 0.35536(8) 0.0222(8) Uani 1 1 d . . . . .
F13 F 0.3472(5) -0.0211(2) 0.38588(9) 0.0242(9) Uani 1 1 d . . . . .
F14 F 0.4001(4) 0.0879(2) 0.39122(9) 0.0229(9) Uani 1 1 d . . . . .
F15 F 0.3815(5) 0.0444(2) 0.35125(9) 0.0262(9) Uani 1 1 d . . . . .
F16 F -0.2461(5) 0.0078(2) 0.37758(9) 0.0308(11) Uani 1 1 d . . . . .
F17 F -0.3016(4) 0.0808(3) 0.40964(9) 0.0325(11) Uani 1 1 d . . . . .
F18 F -0.1648(6) 0.1852(2) 0.37887(11) 0.0382(13) Uani 1 1 d . . . . .
F19 F -0.1416(5) 0.1097(3) 0.34740(10) 0.0330(11) Uani 1 1 d . . . . .
F20 F -0.3603(4) 0.1338(2) 0.36191(9) 0.0270(10) Uani 1 1 d . . . . .
O1 O 0.0915(5) 0.5552(2) 0.40589(10) 0.0182(9) Uani 1 1 d . . . . .
O2 O 0.3487(5) 0.6234(2) 0.41278(10) 0.0168(9) Uani 1 1 d . . . . .
O3 O 0.0020(5) 0.1440(2) 0.42453(9) 0.0136(8) Uani 1 1 d . . . . .
O4 O 0.2214(5) 0.0529(2) 0.43322(9) 0.0129(8) Uani 1 1 d . . . . .
C1 C 0.1798(8) 0.5339(3) 0.46190(14) 0.0186(12) Uani 1 1 d . . . . .
C2 C 0.1311(8) 0.6049(3) 0.47229(14) 0.0201(13) Uani 1 1 d . . . . .
C3 C 0.6004(8) 0.5741(4) 0.45815(16) 0.0248(15) Uani 1 1 d . . . . .
C4 C 0.5335(7) 0.5170(4) 0.44016(14) 0.0199(13) Uani 1 1 d . . . . .
C5 C 0.2294(7) 0.4153(3) 0.41799(12) 0.0141(11) Uani 1 1 d . . . . .
H5A H 0.281210 0.385386 0.431629 0.017 Uiso 1 1 calc R U . . .
H5B H 0.118506 0.409350 0.419238 0.017 Uiso 1 1 calc R U . . .
C6 C 0.4434(9) 0.3275(4) 0.38539(16) 0.0263(15) Uani 1 1 d . . . . .
C7 C 0.5498(10) 0.3419(4) 0.40943(18) 0.0317(17) Uani 1 1 d . . . . .
H7A H 0.590865 0.389135 0.407973 0.047 Uiso 1 1 calc R U . . .
H7B H 0.632959 0.308139 0.409584 0.047 Uiso 1 1 calc R U . . .
H7C H 0.493864 0.337753 0.426197 0.047 Uiso 1 1 calc R U . . .
C8 C 0.3714(11) 0.2548(4) 0.38905(18) 0.0344(19) Uani 1 1 d . . . . .
H8A H 0.303548 0.255902 0.404394 0.052 Uiso 1 1 calc R U . . .
H8B H 0.451382 0.220315 0.392452 0.052 Uiso 1 1 calc R U . . .
H8C H 0.313648 0.242173 0.372622 0.052 Uiso 1 1 calc R U . . .
C9 C 0.5340(11) 0.3306(4) 0.35924(18) 0.0354(19) Uani 1 1 d . . . . .
H9A H 0.465804 0.322533 0.343649 0.053 Uiso 1 1 calc R U . . .
H9B H 0.612978 0.294762 0.359786 0.053 Uiso 1 1 calc R U . . .
H9C H 0.581030 0.376655 0.357650 0.053 Uiso 1 1 calc R U . . .
C10 C 0.1268(9) 0.3756(4) 0.36185(14) 0.0247(15) Uani 1 1 d . . . . .
C11 C 0.0256(10) 0.3212(4) 0.37533(17) 0.036(2) Uani 1 1 d . . . . .
H11A H 0.083604 0.278327 0.378570 0.054 Uiso 1 1 calc R U . . .
H11B H -0.062050 0.310996 0.363453 0.054 Uiso 1 1 calc R U . . .
H11C H -0.009341 0.339465 0.392567 0.054 Uiso 1 1 calc R U . . .
C12 C 0.1764(12) 0.3497(4) 0.33459(15) 0.038(2) Uani 1 1 d . . . . .
H12A H 0.250326 0.382196 0.327226 0.056 Uiso 1 1 calc R U . . .
H12B H 0.088198 0.346612 0.322244 0.056 Uiso 1 1 calc R U . . .
H12C H 0.222716 0.303579 0.336650 0.056 Uiso 1 1 calc R U . . .
C13 C 0.0342(9) 0.4428(4) 0.35770(17) 0.0318(17) Uani 1 1 d . . . . .
H13A H 0.006032 0.461413 0.375293 0.048 Uiso 1 1 calc R U . . .
H13B H -0.057551 0.432468 0.346908 0.048 Uiso 1 1 calc R U . . .
H13C H 0.095211 0.477278 0.348247 0.048 Uiso 1 1 calc R U . . .
C14 C 0.0998(7) 0.6179(3) 0.39469(13) 0.0158(12) Uani 1 1 d . . . . .
C15 C -0.0205(7) 0.6485(4) 0.38081(13) 0.0179(12) Uani 1 1 d . . . . .
C16 C -0.0042(7) 0.7153(3) 0.36941(13) 0.0177(12) Uani 1 1 d . . . . .
C17 C 0.1356(8) 0.7494(3) 0.37117(14) 0.0192(13) Uani 1 1 d . . . . .
C18 C 0.2558(7) 0.7181(3) 0.38534(13) 0.0156(11) Uani 1 1 d . . . . .
C19 C 0.2385(7) 0.6538(3) 0.39740(13) 0.0148(11) Uani 1 1 d . . . . .
C20 C 0.1554(7) 0.0599(3) 0.37460(12) 0.0135(11) Uani 1 1 d . . . . .
C21 C 0.3240(7) 0.0427(3) 0.37602(14) 0.0183(12) Uani 1 1 d . . . . .
C22 C -0.2004(7) 0.0671(3) 0.39052(13) 0.0151(11) Uani 1 1 d . . . . .
C23 C -0.2161(8) 0.1258(4) 0.36975(15) 0.0209(13) Uani 1 1 d . . . . .
C24 C 0.0320(7) -0.0672(3) 0.41095(13) 0.0150(2) Uani 1 1 d . U . . .
H24A H -0.029584 -0.086376 0.395715 0.018 Uiso 1 1 calc R U . . .
H24B H 0.137486 -0.084096 0.409704 0.018 Uiso 1 1 calc R U . . .
C25 C -0.2242(8) -0.1425(3) 0.43914(14) 0.0191(13) Uani 1 1 d . . . . .
C26 C -0.3225(8) -0.1088(4) 0.41668(15) 0.0227(14) Uani 1 1 d . . . . .
H26A H -0.276437 -0.117034 0.399171 0.034 Uiso 1 1 calc R U . . .
H26B H -0.329692 -0.058597 0.419926 0.034 Uiso 1 1 calc R U . . .
H26C H -0.424056 -0.129376 0.416627 0.034 Uiso 1 1 calc R U . . .
C27 C -0.1890(9) -0.2180(4) 0.43192(17) 0.0273(16) Uani 1 1 d . . . . .
H27A H -0.283529 -0.242691 0.427541 0.041 Uiso 1 1 calc R U . . .
H27B H -0.137476 -0.240703 0.447307 0.041 Uiso 1 1 calc R U . . .
H27C H -0.123280 -0.219068 0.416271 0.041 Uiso 1 1 calc R U . . .
C28 C -0.3147(8) -0.1396(4) 0.46513(16) 0.0265(15) Uani 1 1 d . . . . .
H28A H -0.334218 -0.090936 0.469846 0.040 Uiso 1 1 calc R U . . .
H28B H -0.256520 -0.162023 0.479831 0.040 Uiso 1 1 calc R U . . .
H28C H -0.411171 -0.164094 0.462314 0.040 Uiso 1 1 calc R U . . .
C29 C 0.1038(7) -0.1309(3) 0.46480(12) 0.0141(11) Uani 1 1 d . . . . .
C30 C 0.1788(8) -0.1911(3) 0.44883(14) 0.0210(13) Uani 1 1 d . . . . .
H30A H 0.258495 -0.212692 0.460115 0.032 Uiso 1 1 calc R U . . .
H30B H 0.223042 -0.172337 0.432400 0.032 Uiso 1 1 calc R U . . .
H30C H 0.102087 -0.226020 0.443935 0.032 Uiso 1 1 calc R U . . .
C31 C 0.0397(8) -0.1577(4) 0.49120(14) 0.0246(14) Uani 1 1 d . . . . .
H31A H -0.026162 -0.197794 0.487444 0.037 Uiso 1 1 calc R U . . .
H31B H -0.018999 -0.120651 0.499653 0.037 Uiso 1 1 calc R U . . .
H31C H 0.123025 -0.171785 0.503437 0.037 Uiso 1 1 calc R U . . .
C32 C 0.2248(7) -0.0760(3) 0.47119(15) 0.0200(13) Uani 1 1 d . . . . .
H32A H 0.304642 -0.096482 0.482772 0.030 Uiso 1 1 calc R U . . .
H32B H 0.178834 -0.036638 0.480548 0.030 Uiso 1 1 calc R U . . .
H32C H 0.268639 -0.059657 0.454344 0.030 Uiso 1 1 calc R U . . .
C33 C 0.2383(7) 0.1163(3) 0.44451(12) 0.0124(11) Uani 1 1 d . . . . .
C34 C 0.3681(7) 0.1358(3) 0.45913(13) 0.0140(11) Uani 1 1 d . . . . .
C35 C 0.3789(7) 0.2029(3) 0.46997(13) 0.0156(12) Uani 1 1 d . . . . .
C36 C 0.2576(7) 0.2484(3) 0.46763(12) 0.0144(11) Uani 1 1 d . . . . .
C37 C 0.1276(7) 0.2289(3) 0.45291(12) 0.0121(10) Uani 1 1 d . . . . .
C38 C 0.1203(7) 0.1643(3) 0.44029(12) 0.0121(11) 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 0.0033 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 2 0.0548
0 1 -2 0.0548
0 2 5 0.0674
0 -2 -5 0.0663
3 0 5 0.0405
-4 4 -5 0.0705
-3 -3 -5 0.0772
-1 2 5 0.0732
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 Sb1 S1 89.92(15) . . ?
O1 Sb1 C1 84.8(2) . . ?
O1 Sb1 C4 166.3(2) . . ?
O1 Sb1 C5 90.4(2) . . ?
O2 Sb1 S1 86.51(15) . . ?
O2 Sb1 O1 80.58(17) . . ?
O2 Sb1 C1 104.1(2) . . ?
O2 Sb1 C4 86.0(2) . . ?
O2 Sb1 C5 160.1(2) . . ?
C1 Sb1 S1 167.20(17) . . ?
C1 Sb1 C4 96.4(3) . . ?
C4 Sb1 S1 91.51(19) . . ?
C5 Sb1 S1 75.76(17) . . ?
C5 Sb1 C1 92.6(2) . . ?
C5 Sb1 C4 103.1(2) . . ?
O3 Sb2 S2 87.31(14) . . ?
O3 Sb2 O4 81.14(16) . . ?
O3 Sb2 C20 100.5(2) . . ?
O3 Sb2 C22 83.0(2) . . ?
O3 Sb2 C24 162.9(2) . . ?
O4 Sb2 S2 88.20(13) . . ?
O4 Sb2 C20 87.3(2) . . ?
O4 Sb2 C22 164.0(2) . . ?
O4 Sb2 C24 93.3(2) . . ?
C20 Sb2 S2 170.25(16) . . ?
C20 Sb2 C22 93.2(2) . . ?
C22 Sb2 S2 93.48(16) . . ?
C24 Sb2 S2 76.32(18) . . ?
C24 Sb2 C20 95.3(2) . . ?
C24 Sb2 C22 102.6(2) . . ?
O5 Sb3 S3 85.50(14) . . ?
O5 Sb3 O6 80.41(17) . . ?
O5 Sb3 C39 85.4(2) . . ?
O5 Sb3 C41 105.1(2) . . ?
O5 Sb3 C43 160.3(2) . . ?
O6 Sb3 S3 88.04(14) . . ?
O6 Sb3 C39 165.5(2) . . ?
O6 Sb3 C41 84.4(2) . . ?
O6 Sb3 C43 92.7(2) . . ?
C39 Sb3 S3 93.93(19) . . ?
C41 Sb3 S3 165.74(17) . . ?
C41 Sb3 C39 96.4(2) . . ?
C43 Sb3 S3 75.75(16) . . ?
C43 Sb3 C39 101.7(2) . . ?
C43 Sb3 C41 92.5(2) . . ?
P3 S3 Sb3 82.05(7) . . ?
C43 P3 S3 101.3(2) . . ?
C43 P3 C44 110.7(3) . . ?
C43 P3 C48 108.9(3) . . ?
C44 P3 S3 108.7(3) . . ?
C44 P3 C48 113.7(3) . . ?
C48 P3 S3 112.8(2) . . ?
C52 O5 Sb3 111.4(4) . . ?
C53 O6 Sb3 111.3(4) . . ?
F21 C39 Sb3 106.7(4) . . ?
F21 C39 C40 105.0(5) . . ?
F22 C39 Sb3 109.7(4) . . ?
F22 C39 F21 106.3(5) . . ?
F22 C39 C40 106.0(6) . . ?
C40 C39 Sb3 122.1(5) . . ?
F23 C40 F25 107.3(6) . . ?
F23 C40 C39 110.6(6) . . ?
F24 C40 F23 108.5(7) . . ?
F24 C40 F25 107.2(6) . . ?
F24 C40 C39 112.2(6) . . ?
F25 C40 C39 110.9(6) . . ?
F26 C41 Sb3 109.2(4) . . ?
F26 C41 C42 107.4(5) . . ?
F27 C41 Sb3 106.2(4) . . ?
F27 C41 F26 106.8(5) . . ?
F27 C41 C42 106.8(5) . . ?
C42 C41 Sb3 119.9(4) . . ?
F28 C42 C41 109.5(6) . . ?
F29 C42 F28 106.5(6) . . ?
F29 C42 C41 110.7(6) . . ?
F30 C42 F28 108.4(7) . . ?
F30 C42 F29 108.8(6) . . ?
F30 C42 C41 112.8(6) . . ?
Sb3 C43 H43A 111.6 . . ?
Sb3 C43 H43B 111.6 . . ?
P3 C43 Sb3 100.9(3) . . ?
P3 C43 H43A 111.6 . . ?
P3 C43 H43B 111.6 . . ?
H43A C43 H43B 109.4 . . ?
C45 C44 P3 107.6(5) . . ?
C46 C44 P3 111.3(6) . . ?
C46 C44 C45 108.6(6) . . ?
C47 C44 P3 110.5(5) . . ?
C47 C44 C45 106.8(7) . . ?
C47 C44 C46 111.8(7) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C49 C48 P3 110.7(5) . . ?
C50 C48 P3 110.1(5) . . ?
C50 C48 C49 109.4(6) . . ?
C51 C48 P3 108.2(5) . . ?
C51 C48 C49 109.5(7) . . ?
C51 C48 C50 108.9(6) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O5 C52 C53 117.3(5) . . ?
O5 C52 C57 122.4(6) . . ?
C57 C52 C53 120.2(6) . . ?
O6 C53 C52 116.8(5) . . ?
O6 C53 C54 123.6(6) . . ?
C54 C53 C52 119.6(6) . . ?
C53 C54 Cl9 118.8(5) . . ?
C53 C54 C55 119.8(6) . . ?
C55 C54 Cl9 121.4(5) . . ?
C54 C55 Cl10 119.4(5) . . ?
C56 C55 Cl10 120.0(5) . . ?
C56 C55 C54 120.7(6) . . ?
C55 C56 Cl11 121.2(5) . . ?
C55 C56 C57 120.0(6) . . ?
C57 C56 Cl11 118.8(5) . . ?
C52 C57 Cl12 118.6(5) . . ?
C52 C57 C56 119.5(6) . . ?
C56 C57 Cl12 121.8(5) . . ?
P1 S1 Sb1 81.83(7) . . ?
P2 S2 Sb2 81.89(7) . . ?
C5 P1 S1 101.2(2) . . ?
C5 P1 C6 110.3(3) . . ?
C5 P1 C10 109.4(3) . . ?
C6 P1 S1 109.4(2) . . ?
C10 P1 S1 111.8(2) . . ?
C10 P1 C6 114.0(4) . . ?
C24 P2 S2 100.2(2) . . ?
C24 P2 C25 111.5(3) . . ?
C24 P2 C29 107.9(3) . . ?
C25 P2 S2 108.8(2) . . ?
C25 P2 C29 114.8(3) . . ?
C29 P2 S2 112.8(2) . . ?
C14 O1 Sb1 112.0(4) . . ?
C19 O2 Sb1 111.9(4) . . ?
C38 O3 Sb2 112.3(3) . . ?
C33 O4 Sb2 111.9(3) . . ?
F1 C1 Sb1 109.9(4) . . ?
F1 C1 F2 105.9(5) . . ?
F1 C1 C2 107.8(5) . . ?
F2 C1 Sb1 105.8(4) . . ?
F2 C1 C2 105.7(5) . . ?
C2 C1 Sb1 120.7(5) . . ?
F3 C2 F4 107.5(5) . . ?
F3 C2 F5 107.4(6) . . ?
F3 C2 C1 111.6(6) . . ?
F4 C2 C1 110.5(6) . . ?
F5 C2 F4 107.9(6) . . ?
F5 C2 C1 111.7(6) . . ?
F8 C3 F9 110.0(7) . . ?
F8 C3 F10 107.6(6) . . ?
F8 C3 C4 111.4(6) . . ?
F9 C3 C4 109.3(6) . . ?
F10 C3 F9 107.8(6) . . ?
F10 C3 C4 110.7(6) . . ?
F6 C4 Sb1 106.3(4) . . ?
F6 C4 F7 106.9(6) . . ?
F6 C4 C3 107.0(5) . . ?
F7 C4 Sb1 109.3(4) . . ?
F7 C4 C3 104.8(6) . . ?
C3 C4 Sb1 121.8(5) . . ?
Sb1 C5 H5A 111.5 . . ?
Sb1 C5 H5B 111.5 . . ?
P1 C5 Sb1 101.2(3) . . ?
P1 C5 H5A 111.5 . . ?
P1 C5 H5B 111.5 . . ?
H5A C5 H5B 109.4 . . ?
C7 C6 P1 108.3(5) . . ?
C7 C6 C8 108.7(7) . . ?
C7 C6 C9 109.0(7) . . ?
C8 C6 P1 110.6(6) . . ?
C9 C6 P1 109.2(6) . . ?
C9 C6 C8 111.0(6) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 P1 110.4(5) . . ?
C12 C10 P1 111.2(6) . . ?
C12 C10 C11 110.4(6) . . ?
C12 C10 C13 108.7(7) . . ?
C13 C10 P1 107.7(5) . . ?
C13 C10 C11 108.3(7) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C14 C15 122.9(6) . . ?
O1 C14 C19 117.4(5) . . ?
C15 C14 C19 119.7(6) . . ?
C14 C15 Cl1 118.8(5) . . ?
C14 C15 C16 120.0(6) . . ?
C16 C15 Cl1 121.1(5) . . ?
C15 C16 Cl2 120.2(5) . . ?
C17 C16 Cl2 119.8(5) . . ?
C17 C16 C15 120.0(6) . . ?
C16 C17 Cl3 120.4(5) . . ?
C18 C17 Cl3 120.3(5) . . ?
C18 C17 C16 119.3(6) . . ?
C17 C18 Cl4 120.9(5) . . ?
C19 C18 Cl4 118.3(5) . . ?
C19 C18 C17 120.8(6) . . ?
O2 C19 C14 117.0(5) . . ?
O2 C19 C18 122.9(5) . . ?
C18 C19 C14 120.1(6) . . ?
F11 C20 Sb2 111.6(4) . . ?
F11 C20 F12 108.0(5) . . ?
F11 C20 C21 106.0(5) . . ?
F12 C20 Sb2 106.3(4) . . ?
F12 C20 C21 106.8(5) . . ?
C21 C20 Sb2 117.8(4) . . ?
F13 C21 F15 107.5(5) . . ?
F13 C21 C20 110.9(5) . . ?
F14 C21 F13 108.8(6) . . ?
F14 C21 F15 107.8(5) . . ?
F14 C21 C20 111.5(5) . . ?
F15 C21 C20 110.2(5) . . ?
F16 C22 Sb2 107.7(4) . . ?
F16 C22 C23 106.2(5) . . ?
F17 C22 Sb2 107.1(4) . . ?
F17 C22 F16 107.4(5) . . ?
F17 C22 C23 106.2(5) . . ?
C23 C22 Sb2 121.5(4) . . ?
F18 C23 F19 108.3(6) . . ?
F18 C23 F20 108.8(6) . . ?
F18 C23 C22 112.7(6) . . ?
F19 C23 C22 110.4(6) . . ?
F20 C23 F19 105.8(6) . . ?
F20 C23 C22 110.5(5) . . ?
Sb2 C24 H24A 111.5 . . ?
Sb2 C24 H24B 111.5 . . ?
P2 C24 Sb2 101.4(3) . . ?
P2 C24 H24A 111.5 . . ?
P2 C24 H24B 111.5 . . ?
H24A C24 H24B 109.3 . . ?
C26 C25 P2 107.9(4) . . ?
C27 C25 P2 111.8(5) . . ?
C27 C25 C26 110.2(6) . . ?
C27 C25 C28 110.2(6) . . ?
C28 C25 P2 109.5(5) . . ?
C28 C25 C26 107.2(6) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 P2 109.8(4) . . ?
C31 C29 P2 110.4(4) . . ?
C31 C29 C30 110.9(5) . . ?
C31 C29 C32 109.1(5) . . ?
C32 C29 P2 108.3(4) . . ?
C32 C29 C30 108.2(5) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C33 C34 122.8(5) . . ?
O4 C33 C38 117.3(5) . . ?
C34 C33 C38 119.9(5) . . ?
C33 C34 Cl5 118.7(5) . . ?
C33 C34 C35 119.7(6) . . ?
C35 C34 Cl5 121.6(5) . . ?
C34 C35 Cl6 119.6(5) . . ?
C36 C35 Cl6 120.1(5) . . ?
C36 C35 C34 120.3(5) . . ?
C35 C36 Cl7 120.4(5) . . ?
C35 C36 C37 119.9(5) . . ?
C37 C36 Cl7 119.7(5) . . ?
C36 C37 Cl8 121.5(5) . . ?
C38 C37 Cl8 118.3(5) . . ?
C38 C37 C36 120.2(5) . . ?
O3 C38 C33 117.3(5) . . ?
O3 C38 C37 123.1(5) . . ?
C37 C38 C33 119.6(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
Sb1 S1 2.6329(18) . ?
Sb1 O1 2.052(4) . ?
Sb1 O2 2.027(4) . ?
Sb1 C1 2.231(7) . ?
Sb1 C4 2.259(6) . ?
Sb1 C5 2.178(6) . ?
Sb2 S2 2.6194(16) . ?
Sb2 O3 2.022(4) . ?
Sb2 O4 2.035(4) . ?
Sb2 C20 2.235(6) . ?
Sb2 C22 2.254(6) . ?
Sb2 C24 2.146(6) . ?
Sb3 S3 2.6212(17) . ?
Sb3 O5 2.029(4) . ?
Sb3 O6 2.057(4) . ?
Sb3 C39 2.244(6) . ?
Sb3 C41 2.223(6) . ?
Sb3 C43 2.185(6) . ?
Cl9 C54 1.720(7) . ?
Cl10 C55 1.731(7) . ?
Cl11 C56 1.731(6) . ?
Cl12 C57 1.721(7) . ?
S3 P3 2.031(2) . ?
P3 C43 1.807(6) . ?
P3 C44 1.861(7) . ?
P3 C48 1.865(7) . ?
F21 C39 1.383(8) . ?
F22 C39 1.354(8) . ?
F23 C40 1.325(9) . ?
F24 C40 1.325(9) . ?
F25 C40 1.333(8) . ?
F26 C41 1.361(7) . ?
F27 C41 1.356(7) . ?
F28 C42 1.333(9) . ?
F29 C42 1.331(8) . ?
F30 C42 1.307(8) . ?
O5 C52 1.348(7) . ?
O6 C53 1.342(7) . ?
C39 C40 1.534(10) . ?
C41 C42 1.536(9) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.547(10) . ?
C44 C46 1.529(11) . ?
C44 C47 1.526(11) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C49 1.547(10) . ?
C48 C50 1.537(10) . ?
C48 C51 1.522(10) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.412(9) . ?
C52 C57 1.382(8) . ?
C53 C54 1.382(8) . ?
C54 C55 1.396(9) . ?
C55 C56 1.379(9) . ?
C56 C57 1.402(9) . ?
Cl1 C15 1.719(7) . ?
Cl2 C16 1.726(6) . ?
Cl3 C17 1.720(7) . ?
Cl4 C18 1.728(7) . ?
Cl5 C34 1.727(6) . ?
Cl6 C35 1.724(6) . ?
Cl7 C36 1.721(6) . ?
Cl8 C37 1.731(6) . ?
S1 P1 2.036(2) . ?
S2 P2 2.036(2) . ?
P1 C5 1.811(6) . ?
P1 C6 1.880(8) . ?
P1 C10 1.866(7) . ?
P2 C24 1.829(7) . ?
P2 C25 1.863(7) . ?
P2 C29 1.867(6) . ?
F1 C1 1.357(8) . ?
F2 C1 1.373(7) . ?
F3 C2 1.324(8) . ?
F4 C2 1.343(8) . ?
F5 C2 1.326(8) . ?
F6 C4 1.357(7) . ?
F7 C4 1.367(8) . ?
F8 C3 1.317(9) . ?
F9 C3 1.331(10) . ?
F10 C3 1.327(8) . ?
F11 C20 1.363(7) . ?
F12 C20 1.365(7) . ?
F13 C21 1.332(8) . ?
F14 C21 1.322(7) . ?
F15 C21 1.340(7) . ?
F16 C22 1.364(7) . ?
F17 C22 1.345(8) . ?
F18 C23 1.304(8) . ?
F19 C23 1.338(9) . ?
F20 C23 1.331(7) . ?
O1 C14 1.329(7) . ?
O2 C19 1.353(7) . ?
O3 C38 1.346(7) . ?
O4 C33 1.345(7) . ?
C1 C2 1.522(9) . ?
C3 C4 1.523(10) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.524(12) . ?
C6 C8 1.545(10) . ?
C6 C9 1.541(10) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.540(10) . ?
C10 C12 1.514(10) . ?
C10 C13 1.538(11) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.382(8) . ?
C14 C19 1.409(8) . ?
C15 C16 1.410(9) . ?
C16 C17 1.398(9) . ?
C17 C18 1.394(9) . ?
C18 C19 1.382(9) . ?
C20 C21 1.526(9) . ?
C22 C23 1.529(9) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.536(9) . ?
C25 C27 1.527(10) . ?
C25 C28 1.533(10) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.557(9) . ?
C29 C31 1.527(9) . ?
C29 C32 1.529(9) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.392(8) . ?
C33 C38 1.404(8) . ?
C34 C35 1.398(9) . ?
C35 C36 1.385(9) . ?
C36 C37 1.396(8) . ?
C37 C38 1.389(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
Sb1 O1 C14 C15 176.2(5) . . . . ?
Sb1 O1 C14 C19 -3.9(7) . . . . ?
Sb1 O2 C19 C14 10.4(7) . . . . ?
Sb1 O2 C19 C18 -171.7(5) . . . . ?
Sb1 C1 C2 F3 59.3(7) . . . . ?
Sb1 C1 C2 F4 -60.4(7) . . . . ?
Sb1 C1 C2 F5 179.4(5) . . . . ?
Sb2 O3 C38 C33 2.5(7) . . . . ?
Sb2 O3 C38 C37 -175.5(5) . . . . ?
Sb2 O4 C33 C34 -177.2(5) . . . . ?
Sb2 O4 C33 C38 0.7(7) . . . . ?
Sb2 C20 C21 F13 51.6(6) . . . . ?
Sb2 C20 C21 F14 -69.9(6) . . . . ?
Sb2 C20 C21 F15 170.5(4) . . . . ?
Sb2 C22 C23 F18 -51.8(8) . . . . ?
Sb2 C22 C23 F19 69.5(7) . . . . ?
Sb2 C22 C23 F20 -173.8(4) . . . . ?
Sb3 O5 C52 C53 -13.7(7) . . . . ?
Sb3 O5 C52 C57 165.1(5) . . . . ?
Sb3 O6 C53 C52 9.8(7) . . . . ?
Sb3 O6 C53 C54 -171.4(5) . . . . ?
Sb3 C39 C40 F23 58.9(8) . . . . ?
Sb3 C39 C40 F24 -62.4(7) . . . . ?
Sb3 C39 C40 F25 177.8(5) . . . . ?
Sb3 C41 C42 F28 -66.8(7) . . . . ?
Sb3 C41 C42 F29 50.3(7) . . . . ?
Sb3 C41 C42 F30 172.4(5) . . . . ?
Cl9 C54 C55 Cl10 -1.9(8) . . . . ?
Cl9 C54 C55 C56 178.8(5) . . . . ?
Cl10 C55 C56 Cl11 4.8(8) . . . . ?
Cl10 C55 C56 C57 -176.2(5) . . . . ?
Cl11 C56 C57 Cl12 -1.1(8) . . . . ?
Cl11 C56 C57 C52 179.4(5) . . . . ?
S3 P3 C43 Sb3 -2.4(2) . . . . ?
S3 P3 C44 C45 -65.9(5) . . . . ?
S3 P3 C44 C46 175.2(5) . . . . ?
S3 P3 C44 C47 50.4(6) . . . . ?
S3 P3 C48 C49 160.0(5) . . . . ?
S3 P3 C48 C50 -78.9(5) . . . . ?
S3 P3 C48 C51 40.1(6) . . . . ?
F21 C39 C40 F23 -179.9(6) . . . . ?
F21 C39 C40 F24 58.9(7) . . . . ?
F21 C39 C40 F25 -61.0(7) . . . . ?
F22 C39 C40 F23 -67.6(8) . . . . ?
F22 C39 C40 F24 171.2(6) . . . . ?
F22 C39 C40 F25 51.4(7) . . . . ?
F26 C41 C42 F28 168.0(6) . . . . ?
F26 C41 C42 F29 -74.9(7) . . . . ?
F26 C41 C42 F30 47.2(8) . . . . ?
F27 C41 C42 F28 53.8(7) . . . . ?
F27 C41 C42 F29 170.9(5) . . . . ?
F27 C41 C42 F30 -67.0(7) . . . . ?
O5 C52 C53 O6 2.6(9) . . . . ?
O5 C52 C53 C54 -176.3(6) . . . . ?
O5 C52 C57 Cl12 -2.7(9) . . . . ?
O5 C52 C57 C56 176.9(6) . . . . ?
O6 C53 C54 Cl9 -1.5(9) . . . . ?
O6 C53 C54 C55 179.8(6) . . . . ?
C43 P3 C44 C45 44.6(6) . . . . ?
C43 P3 C44 C46 -74.3(6) . . . . ?
C43 P3 C44 C47 160.8(5) . . . . ?
C43 P3 C48 C49 48.4(6) . . . . ?
C43 P3 C48 C50 169.5(5) . . . . ?
C43 P3 C48 C51 -71.5(6) . . . . ?
C44 P3 C43 Sb3 -117.6(3) . . . . ?
C44 P3 C48 C49 -75.6(6) . . . . ?
C44 P3 C48 C50 45.6(6) . . . . ?
C44 P3 C48 C51 164.5(5) . . . . ?
C48 P3 C43 Sb3 116.7(3) . . . . ?
C48 P3 C44 C45 167.6(5) . . . . ?
C48 P3 C44 C46 48.7(6) . . . . ?
C48 P3 C44 C47 -76.2(6) . . . . ?
C52 C53 C54 Cl9 177.3(5) . . . . ?
C52 C53 C54 C55 -1.4(10) . . . . ?
C53 C52 C57 Cl12 176.1(5) . . . . ?
C53 C52 C57 C56 -4.3(10) . . . . ?
C53 C54 C55 Cl10 176.7(5) . . . . ?
C53 C54 C55 C56 -2.6(10) . . . . ?
C54 C55 C56 Cl11 -175.9(5) . . . . ?
C54 C55 C56 C57 3.2(10) . . . . ?
C55 C56 C57 Cl12 179.9(5) . . . . ?
C55 C56 C57 C52 0.3(10) . . . . ?
C57 C52 C53 O6 -176.3(6) . . . . ?
C57 C52 C53 C54 4.9(10) . . . . ?
Cl1 C15 C16 Cl2 -0.4(8) . . . . ?
Cl1 C15 C16 C17 -179.4(5) . . . . ?
Cl2 C16 C17 Cl3 -3.7(8) . . . . ?
Cl2 C16 C17 C18 177.9(5) . . . . ?
Cl3 C17 C18 Cl4 0.7(8) . . . . ?
Cl3 C17 C18 C19 -177.8(5) . . . . ?
Cl4 C18 C19 O2 5.8(9) . . . . ?
Cl4 C18 C19 C14 -176.4(5) . . . . ?
Cl5 C34 C35 Cl6 3.9(8) . . . . ?
Cl5 C34 C35 C36 -176.2(5) . . . . ?
Cl6 C35 C36 Cl7 -5.0(8) . . . . ?
Cl6 C35 C36 C37 175.9(5) . . . . ?
Cl7 C36 C37 Cl8 -0.3(8) . . . . ?
Cl7 C36 C37 C38 179.9(5) . . . . ?
Cl8 C37 C38 O3 4.2(8) . . . . ?
Cl8 C37 C38 C33 -173.8(5) . . . . ?
S1 P1 C5 Sb1 1.6(3) . . . . ?
S1 P1 C6 C7 68.8(5) . . . . ?
S1 P1 C6 C8 -172.2(5) . . . . ?
S1 P1 C6 C9 -49.8(6) . . . . ?
S1 P1 C10 C11 -160.1(5) . . . . ?
S1 P1 C10 C12 77.0(6) . . . . ?
S1 P1 C10 C13 -42.0(6) . . . . ?
S2 P2 C24 Sb2 4.0(3) . . . . ?
S2 P2 C25 C26 64.4(5) . . . . ?
S2 P2 C25 C27 -174.3(4) . . . . ?
S2 P2 C25 C28 -51.9(5) . . . . ?
S2 P2 C29 C30 -161.2(4) . . . . ?
S2 P2 C29 C31 76.2(5) . . . . ?
S2 P2 C29 C32 -43.2(5) . . . . ?
F1 C1 C2 F3 -173.3(5) . . . . ?
F1 C1 C2 F4 67.0(7) . . . . ?
F1 C1 C2 F5 -53.2(7) . . . . ?
F2 C1 C2 F3 -60.5(7) . . . . ?
F2 C1 C2 F4 179.9(5) . . . . ?
F2 C1 C2 F5 59.7(7) . . . . ?
F8 C3 C4 Sb1 -59.8(9) . . . . ?
F8 C3 C4 F6 177.9(6) . . . . ?
F8 C3 C4 F7 64.6(8) . . . . ?
F9 C3 C4 Sb1 61.9(7) . . . . ?
F9 C3 C4 F6 -60.4(7) . . . . ?
F9 C3 C4 F7 -173.6(6) . . . . ?
F10 C3 C4 Sb1 -179.5(5) . . . . ?
F10 C3 C4 F6 58.2(8) . . . . ?
F10 C3 C4 F7 -55.0(7) . . . . ?
F11 C20 C21 F13 177.3(5) . . . . ?
F11 C20 C21 F14 55.8(7) . . . . ?
F11 C20 C21 F15 -63.8(6) . . . . ?
F12 C20 C21 F13 -67.8(6) . . . . ?
F12 C20 C21 F14 170.8(5) . . . . ?
F12 C20 C21 F15 51.1(6) . . . . ?
F16 C22 C23 F18 -175.0(6) . . . . ?
F16 C22 C23 F19 -53.7(7) . . . . ?
F16 C22 C23 F20 63.0(7) . . . . ?
F17 C22 C23 F18 70.8(7) . . . . ?
F17 C22 C23 F19 -167.9(5) . . . . ?
F17 C22 C23 F20 -51.2(7) . . . . ?
O1 C14 C15 Cl1 2.0(10) . . . . ?
O1 C14 C15 C16 180.0(6) . . . . ?
O1 C14 C19 O2 -4.4(9) . . . . ?
O1 C14 C19 C18 177.6(6) . . . . ?
O4 C33 C34 Cl5 -0.9(8) . . . . ?
O4 C33 C34 C35 179.0(6) . . . . ?
O4 C33 C38 O3 -2.2(8) . . . . ?
O4 C33 C38 C37 175.9(6) . . . . ?
C5 P1 C6 C7 -41.7(6) . . . . ?
C5 P1 C6 C8 77.3(6) . . . . ?
C5 P1 C6 C9 -160.3(5) . . . . ?
C5 P1 C10 C11 -48.8(7) . . . . ?
C5 P1 C10 C12 -171.7(5) . . . . ?
C5 P1 C10 C13 69.3(6) . . . . ?
C6 P1 C5 Sb1 117.4(3) . . . . ?
C6 P1 C10 C11 75.2(7) . . . . ?
C6 P1 C10 C12 -47.7(6) . . . . ?
C6 P1 C10 C13 -166.7(5) . . . . ?
C10 P1 C5 Sb1 -116.5(3) . . . . ?
C10 P1 C6 C7 -165.2(5) . . . . ?
C10 P1 C6 C8 -46.2(6) . . . . ?
C10 P1 C6 C9 76.2(6) . . . . ?
C14 C15 C16 Cl2 -178.2(5) . . . . ?
C14 C15 C16 C17 2.7(10) . . . . ?
C15 C14 C19 O2 175.5(6) . . . . ?
C15 C14 C19 C18 -2.5(10) . . . . ?
C15 C16 C17 Cl3 175.4(5) . . . . ?
C15 C16 C17 C18 -3.0(10) . . . . ?
C16 C17 C18 Cl4 179.1(5) . . . . ?
C16 C17 C18 C19 0.6(10) . . . . ?
C17 C18 C19 O2 -175.7(6) . . . . ?
C17 C18 C19 C14 2.2(10) . . . . ?
C19 C14 C15 Cl1 -177.9(5) . . . . ?
C19 C14 C15 C16 0.0(10) . . . . ?
C24 P2 C25 C26 -45.2(6) . . . . ?
C24 P2 C25 C27 76.1(5) . . . . ?
C24 P2 C25 C28 -161.5(5) . . . . ?
C24 P2 C29 C30 -51.5(5) . . . . ?
C24 P2 C29 C31 -174.1(5) . . . . ?
C24 P2 C29 C32 66.5(5) . . . . ?
C25 P2 C24 Sb2 119.0(3) . . . . ?
C25 P2 C29 C30 73.5(5) . . . . ?
C25 P2 C29 C31 -49.1(6) . . . . ?
C25 P2 C29 C32 -168.5(4) . . . . ?
C29 P2 C24 Sb2 -114.1(3) . . . . ?
C29 P2 C25 C26 -168.2(5) . . . . ?
C29 P2 C25 C27 -46.9(6) . . . . ?
C29 P2 C25 C28 75.4(5) . . . . ?
C33 C34 C35 Cl6 -176.0(5) . . . . ?
C33 C34 C35 C36 3.9(9) . . . . ?
C34 C33 C38 O3 175.7(6) . . . . ?
C34 C33 C38 C37 -6.2(9) . . . . ?
C34 C35 C36 Cl7 175.1(5) . . . . ?
C34 C35 C36 C37 -4.1(9) . . . . ?
C35 C36 C37 Cl8 178.9(5) . . . . ?
C35 C36 C37 C38 -0.9(9) . . . . ?
C36 C37 C38 O3 -176.0(6) . . . . ?
C36 C37 C38 C33 6.0(9) . . . . ?
C38 C33 C34 Cl5 -178.7(5) . . . . ?
C38 C33 C34 C35 1.3(9) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0015 -1.0001 1.9952 -0.0298 -0.0015 0.0359
-0.0015 1.0001 -1.9952 0.0298 0.0015 -0.0359
-0.0091 1.9948 5.0130 -0.0666 0.0296 -0.0727
0.0091 -1.9948 -5.0130 0.0666 -0.0296 0.0727
2.9946 0.0311 5.0349 -0.0273 0.2464 0.0494
-4.0053 3.9531 -5.0237 0.0200 -0.2940 -0.2105
-2.9861 -3.0278 -5.0515 0.0219 -0.2686 0.0589
-1.0084 1.9834 5.0021 -0.0808 -0.0476 -0.0893
