#------------------------------------------------------------------------------
#$Date: 2024-09-15 00:53:50 +0200 (Sun 15 de Sep de 2024) $
#$Revision: 294761 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/70/7717008.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_7717008
loop_
_publ_author_name
'Krieft, Jonas'
'Koch, Hannah'
'Neumann, Beate'
'Stammler, Georg'
'Lamm, Jan-Hendrik'
'Mix, Andreas'
'Mitzel, Norbert Werner'
_publ_section_title
;
 Adducts of Lewis acidic stibanes with phosphane chalcogenides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D4DT02268H
_journal_year                    2024
_chemical_formula_moiety         'C24 H25 Cl F12 O P Sb'
_chemical_formula_sum            'C24 H25 Cl F12 O P Sb'
_chemical_formula_weight         745.61
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-02
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-07-03 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.045(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3245(12)
_cell_length_b                   14.4630(6)
_cell_length_c                   9.6209(4)
_cell_measurement_reflns_used    11162
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5850
_cell_measurement_theta_min      2.8040
_cell_volume                     2912.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      7.00  37.00   1.00   57.50    --   12.30  57.00-120.00   30
  2  ω     25.00  76.00   1.00   57.50    --   12.30  38.00-150.00   51
  3  ω    -40.00 -12.00   1.00   57.50    --   12.30 -77.00 -60.00   28
  4  ω     -3.00  80.00   1.00   57.50    --   12.30  57.00 150.00   83
  5  ω     11.00  37.00   1.00   57.50    --   12.30 -77.00 -60.00   26
  6  ω    -40.00  29.00   1.00   57.50    --   12.30 -77.00-120.00   69
  7  ω    -42.00  42.00   1.00   57.50    --   12.30 -77.00  30.00   84
  8  ω    -27.00   3.00   1.00   57.50    --  -12.46 -77.00-180.00   30
  9  ω    -42.00  12.00   1.00   57.50    --  -12.46  77.00 -30.00   54
 10  ω    -20.00   5.00   1.00   57.50    --  -12.46 -38.00  60.00   25
 11  ω    -37.00  18.00   1.00   57.50    --  -12.46 -77.00-150.00   55
;
_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      -0.0336738000
_diffrn_orient_matrix_UB_12      0.0016805000
_diffrn_orient_matrix_UB_13      -0.0224402000
_diffrn_orient_matrix_UB_21      0.0028163000
_diffrn_orient_matrix_UB_22      -0.0223398000
_diffrn_orient_matrix_UB_23      -0.0641394000
_diffrn_orient_matrix_UB_31      -0.0027154000
_diffrn_orient_matrix_UB_32      -0.0436096000
_diffrn_orient_matrix_UB_33      0.0320164000
_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  0.0971
_diffrn_reflns_av_unetI/netI     0.1228
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40116
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.576
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.188
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       needle
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.140
_refine_diff_density_min         -2.375
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         6677
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0853
_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)+68.0581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.1924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5581
_reflns_number_total             6677
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02268h3.cif
_cod_data_source_block           8
_cod_database_code               7717008
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H25 Cl F12 O P 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   0.977
_shelx_estimated_absorpt_t_min   0.771
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.892(2)
 0.108(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
F1A \\sim F1B \\sim F2A \\sim F2B \\sim F3A \\sim F3B \\sim C7: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F7A \\sim F7B \\sim F8A \\sim F8B \\sim F9A \\sim F9B \\sim C15: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 F1A, F1B, F2A, F2B, F3A, F3B, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F7A, F7B, F8A, F8B, F9A, F9B, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
 Sof(F7B)=Sof(F8B)=Sof(F9B)=1-FVAR(2)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C10(H10), C12(H12), C14(H14)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_olex2_date_sample_data_collection 2023-07-27
_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 1.253
_oxdiff_exptl_absorpt_empirical_full_min 0.806
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 0.74100(3) 0.30743(4) 0.80618(6) 0.01565(15) Uani 1 1 d . . . . .
Cl1 Cl 0.73850(11) 0.13816(13) 0.7500(2) 0.0199(4) Uani 1 1 d . . . . .
P1 P 0.76020(12) 0.53412(15) 0.9471(2) 0.0183(5) Uani 1 1 d . . . . .
H1 H 0.781(5) 0.491(7) 1.084(11) 0.02(3) Uiso 1 1 d . . . . .
F1A F 0.4654(5) 0.2319(8) 0.3559(17) 0.053(3) Uani 0.745(19) 1 d . U P A 1
F1B F 0.4824(17) 0.237(2) 0.287(4) 0.047(6) Uani 0.255(19) 1 d . U P A 2
F2A F 0.5175(6) 0.1411(9) 0.5160(11) 0.050(3) Uani 0.745(19) 1 d . U P A 1
F2B F 0.4893(16) 0.186(3) 0.503(4) 0.048(5) Uani 0.255(19) 1 d . U P A 2
F3A F 0.5449(6) 0.1514(8) 0.3151(13) 0.040(3) Uani 0.745(19) 1 d . U P A 1
F3B F 0.5472(19) 0.135(3) 0.375(4) 0.044(5) Uani 0.255(19) 1 d . U P A 2
F4 F 0.6464(4) 0.5828(5) 0.4198(9) 0.054(2) Uani 1 1 d . . . . .
F5 F 0.5498(4) 0.5803(5) 0.4476(9) 0.063(2) Uani 1 1 d . . . . .
F6 F 0.5744(4) 0.5307(5) 0.2538(7) 0.0473(18) Uani 1 1 d . . . . .
F7A F 0.9679(5) 0.1435(7) 0.7212(13) 0.052(3) Uani 0.792(18) 1 d . U P B 1
F7B F 0.995(2) 0.193(3) 0.786(5) 0.054(6) Uani 0.208(18) 1 d . U P B 2
F8A F 0.9758(6) 0.1789(9) 0.5119(13) 0.058(3) Uani 0.792(18) 1 d . U P B 1
F8B F 0.963(2) 0.154(3) 0.554(6) 0.052(6) Uani 0.208(18) 1 d . U P B 2
F9A F 1.0277(6) 0.2566(10) 0.6847(17) 0.063(4) Uani 0.792(18) 1 d . U P B 1
F9B F 1.027(2) 0.255(4) 0.619(5) 0.046(6) Uani 0.208(18) 1 d . U P B 2
F10 F 0.8886(4) 0.4948(5) 0.3292(8) 0.052(2) Uani 1 1 d . . . . .
F11 F 0.9181(3) 0.5702(4) 0.5240(8) 0.0466(18) Uani 1 1 d . . . . .
F12 F 0.8189(3) 0.5596(4) 0.4312(7) 0.0356(15) Uani 1 1 d . . . . .
O1 O 0.7461(3) 0.4694(4) 0.8198(7) 0.0203(13) Uani 1 1 d . . . . .
C1 C 0.6631(4) 0.3327(6) 0.6297(9) 0.0172(17) Uani 1 1 d . . . . .
C2 C 0.6201(4) 0.2633(6) 0.5777(10) 0.0195(18) Uani 1 1 d . . . . .
H2 H 0.625227 0.203325 0.618507 0.023 Uiso 1 1 calc R U . . .
C3 C 0.5690(5) 0.2811(7) 0.4651(11) 0.025(2) Uani 1 1 d . . . . .
C4 C 0.5600(5) 0.3676(7) 0.4036(10) 0.026(2) Uani 1 1 d . . . . .
H4 H 0.525572 0.379233 0.327090 0.032 Uiso 1 1 calc R U . . .
C5 C 0.6030(4) 0.4373(6) 0.4571(10) 0.0217(19) Uani 1 1 d . . . . .
C6 C 0.6524(4) 0.4209(6) 0.5699(9) 0.0202(18) Uani 1 1 d . . . . .
H6 H 0.679620 0.470449 0.607668 0.024 Uiso 1 1 calc R U . . .
C7 C 0.5229(5) 0.2042(7) 0.4112(13) 0.035(2) Uani 1 1 d . U . . .
C8 C 0.5923(5) 0.5325(7) 0.3935(12) 0.031(2) Uani 1 1 d . . . . .
C9 C 0.8161(4) 0.3275(6) 0.6836(9) 0.0192(18) Uani 1 1 d . . . . .
C10 C 0.8668(4) 0.2650(6) 0.6965(10) 0.0199(18) Uani 1 1 d . . . . .
H10 H 0.866121 0.210215 0.750677 0.024 Uiso 1 1 calc R U . . .
C11 C 0.9178(5) 0.2825(7) 0.6310(10) 0.024(2) Uani 1 1 d . . . . .
C12 C 0.9207(4) 0.3634(7) 0.5535(10) 0.0230(19) Uani 1 1 d . . . . .
H12 H 0.956634 0.375850 0.511465 0.028 Uiso 1 1 calc R U . . .
C13 C 0.8704(4) 0.4251(6) 0.5389(10) 0.0208(18) Uani 1 1 d . . . . .
C14 C 0.8184(5) 0.4075(6) 0.6049(9) 0.0210(18) Uani 1 1 d . . . . .
H14 H 0.784345 0.450866 0.595726 0.025 Uiso 1 1 calc R U . . .
C15 C 0.9728(5) 0.2174(8) 0.6428(14) 0.040(2) Uani 1 1 d . U . . .
C16 C 0.8739(5) 0.5114(7) 0.4565(11) 0.029(2) Uani 1 1 d . . . . .
C17 C 0.8322(4) 0.6010(6) 0.9369(10) 0.0226(19) Uani 1 1 d . . . . .
C18 C 0.8867(5) 0.5295(7) 0.9567(11) 0.028(2) Uani 1 1 d . . . . .
H18A H 0.890525 0.500028 1.049668 0.042 Uiso 1 1 calc R U . . .
H18B H 0.926924 0.560542 0.950566 0.042 Uiso 1 1 calc R U . . .
H18C H 0.877330 0.482373 0.882385 0.042 Uiso 1 1 calc R U . . .
C19 C 0.8255(5) 0.6466(7) 0.7905(10) 0.026(2) Uani 1 1 d . . . . .
H19A H 0.810573 0.600696 0.716690 0.040 Uiso 1 1 calc R U . . .
H19B H 0.867061 0.670870 0.778615 0.040 Uiso 1 1 calc R U . . .
H19C H 0.794598 0.697400 0.782894 0.040 Uiso 1 1 calc R U . . .
C20 C 0.8468(5) 0.6739(7) 1.0558(11) 0.030(2) Uani 1 1 d . . . . .
H20A H 0.815058 0.723503 1.037551 0.045 Uiso 1 1 calc R U . . .
H20B H 0.889550 0.699627 1.058226 0.045 Uiso 1 1 calc R U . . .
H20C H 0.845248 0.644736 1.146986 0.045 Uiso 1 1 calc R U . . .
C21 C 0.6881(5) 0.5967(6) 0.9680(10) 0.0218(19) Uani 1 1 d . . . . .
C22 C 0.6352(5) 0.5238(7) 0.9513(11) 0.027(2) Uani 1 1 d . . . . .
H22A H 0.628872 0.497431 0.855781 0.040 Uiso 1 1 calc R U . . .
H22B H 0.595420 0.552590 0.966065 0.040 Uiso 1 1 calc R U . . .
H22C H 0.647503 0.474639 1.021338 0.040 Uiso 1 1 calc R U . . .
C23 C 0.6704(6) 0.6716(7) 0.8537(13) 0.038(3) Uani 1 1 d . . . . .
H23A H 0.701191 0.722437 0.872330 0.057 Uiso 1 1 calc R U . . .
H23B H 0.627412 0.695022 0.855489 0.057 Uiso 1 1 calc R U . . .
H23C H 0.671198 0.644965 0.760357 0.057 Uiso 1 1 calc R U . . .
C24 C 0.6963(5) 0.6384(8) 1.1169(12) 0.035(3) Uani 1 1 d . . . . .
H24A H 0.710114 0.590082 1.187591 0.053 Uiso 1 1 calc R U . . .
H24B H 0.655492 0.664243 1.130933 0.053 Uiso 1 1 calc R U . . .
H24C H 0.728543 0.687466 1.127375 0.053 Uiso 1 1 calc R U . . .
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'
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
1 0 0 0.0098
-1 0 0 0.0098
0 -1 0 0.0220
0 1 0 0.0220
1 0 -2 0.1151
-1 0 2 0.1151
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 Cl1 170.37(16) . . ?
C1 Sb1 Cl1 90.8(2) . . ?
C1 Sb1 O1 84.0(3) . . ?
C1 Sb1 C9 95.0(3) . . ?
C9 Sb1 Cl1 90.1(2) . . ?
C9 Sb1 O1 82.3(3) . . ?
O1 P1 H1 117(4) . . ?
O1 P1 C17 108.6(4) . . ?
O1 P1 C21 110.5(4) . . ?
C17 P1 H1 99(4) . . ?
C21 P1 H1 103(4) . . ?
C21 P1 C17 118.4(4) . . ?
P1 O1 Sb1 131.0(4) . . ?
C2 C1 Sb1 121.0(6) . . ?
C2 C1 C6 117.8(8) . . ?
C6 C1 Sb1 121.0(6) . . ?
C1 C2 H2 119.8 . . ?
C1 C2 C3 120.5(8) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 C7 119.3(9) . . ?
C4 C3 C2 121.3(9) . . ?
C4 C3 C7 119.5(9) . . ?
C3 C4 H4 121.0 . . ?
C3 C4 C5 118.0(9) . . ?
C5 C4 H4 121.0 . . ?
C4 C5 C8 118.2(9) . . ?
C6 C5 C4 121.0(9) . . ?
C6 C5 C8 120.7(9) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 C1 121.3(9) . . ?
C5 C6 H6 119.4 . . ?
F1A C7 F2A 107.3(11) . . ?
F1A C7 F3A 108.5(11) . . ?
F1A C7 C3 114.5(10) . . ?
F1B C7 C3 107.0(16) . . ?
F2A C7 C3 112.1(9) . . ?
F2B C7 F1B 109(2) . . ?
F2B C7 C3 109.4(16) . . ?
F3A C7 F2A 102.4(10) . . ?
F3A C7 C3 111.3(10) . . ?
F3B C7 F1B 105(2) . . ?
F3B C7 F2B 111(3) . . ?
F3B C7 C3 115(2) . . ?
F4 C8 C5 111.1(8) . . ?
F5 C8 F4 105.6(9) . . ?
F5 C8 F6 108.9(9) . . ?
F5 C8 C5 112.3(9) . . ?
F6 C8 F4 105.7(9) . . ?
F6 C8 C5 112.7(9) . . ?
C10 C9 Sb1 120.1(6) . . ?
C14 C9 Sb1 120.7(6) . . ?
C14 C9 C10 118.8(8) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.3(8) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C12 121.1(9) . . ?
C10 C11 C15 121.8(9) . . ?
C12 C11 C15 117.2(9) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 C11 118.9(9) . . ?
C13 C12 H12 120.5 . . ?
C12 C13 C14 120.2(9) . . ?
C12 C13 C16 118.6(8) . . ?
C14 C13 C16 121.2(8) . . ?
C9 C14 C13 120.7(9) . . ?
C9 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
F7A C15 F8A 102.4(11) . . ?
F7A C15 C11 114.0(9) . . ?
F7B C15 C11 109.8(17) . . ?
F8A C15 C11 110.9(10) . . ?
F8B C15 F7B 118(3) . . ?
F8B C15 F9B 102(3) . . ?
F8B C15 C11 113(2) . . ?
F9A C15 F7A 110.0(12) . . ?
F9A C15 F8A 105.2(11) . . ?
F9A C15 C11 113.5(11) . . ?
F9B C15 F7B 98(3) . . ?
F9B C15 C11 115(2) . . ?
F10 C16 F12 106.0(9) . . ?
F10 C16 C13 112.3(8) . . ?
F11 C16 F10 106.8(8) . . ?
F11 C16 F12 105.4(8) . . ?
F11 C16 C13 112.1(9) . . ?
F12 C16 C13 113.6(8) . . ?
C18 C17 P1 105.0(6) . . ?
C18 C17 C20 109.1(8) . . ?
C19 C17 P1 110.1(7) . . ?
C19 C17 C18 109.7(8) . . ?
C19 C17 C20 110.8(8) . . ?
C20 C17 P1 111.9(7) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 P1 105.4(6) . . ?
C22 C21 C23 109.6(9) . . ?
C22 C21 C24 108.6(8) . . ?
C23 C21 P1 111.5(7) . . ?
C24 C21 P1 110.4(7) . . ?
C24 C21 C23 111.1(8) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
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 Cl1 2.505(2) . ?
Sb1 O1 2.348(5) . ?
Sb1 C1 2.168(9) . ?
Sb1 C9 2.183(9) . ?
P1 H1 1.45(10) . ?
P1 O1 1.525(6) . ?
P1 C17 1.833(9) . ?
P1 C21 1.828(9) . ?
F1A C7 1.303(15) . ?
F1B C7 1.42(4) . ?
F2A C7 1.381(16) . ?
F2B C7 1.27(3) . ?
F3A C7 1.350(16) . ?
F3B C7 1.21(4) . ?
F4 C8 1.348(13) . ?
F5 C8 1.323(13) . ?
F6 C8 1.325(12) . ?
F7A C15 1.324(14) . ?
F7B C15 1.41(4) . ?
F8A C15 1.389(17) . ?
F8B C15 1.25(5) . ?
F9A C15 1.293(17) . ?
F9B C15 1.34(5) . ?
F10 C16 1.344(12) . ?
F11 C16 1.341(12) . ?
F12 C16 1.345(12) . ?
C1 C2 1.386(12) . ?
C1 C6 1.401(12) . ?
C2 H2 0.9500 . ?
C2 C3 1.405(13) . ?
C3 C4 1.383(14) . ?
C3 C7 1.509(13) . ?
C4 H4 0.9500 . ?
C4 C5 1.393(14) . ?
C5 C6 1.380(13) . ?
C5 C8 1.506(13) . ?
C6 H6 0.9500 . ?
C9 C10 1.395(12) . ?
C9 C14 1.389(12) . ?
C10 H10 0.9500 . ?
C10 C11 1.383(13) . ?
C11 C12 1.394(13) . ?
C11 C15 1.491(13) . ?
C12 H12 0.9500 . ?
C12 C13 1.382(13) . ?
C13 C14 1.402(13) . ?
C13 C16 1.488(13) . ?
C14 H14 0.9500 . ?
C17 C18 1.540(13) . ?
C17 C19 1.537(13) . ?
C17 C20 1.542(13) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.529(13) . ?
C21 C23 1.538(14) . ?
C21 C24 1.533(13) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
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 C1 C2 C3 178.7(7) . . . . ?
Sb1 C1 C6 C5 179.7(7) . . . . ?
Sb1 C9 C10 C11 -173.2(7) . . . . ?
Sb1 C9 C14 C13 173.0(7) . . . . ?
O1 P1 C17 C18 -66.3(7) . . . . ?
O1 P1 C17 C19 51.7(7) . . . . ?
O1 P1 C17 C20 175.4(7) . . . . ?
O1 P1 C21 C22 45.9(7) . . . . ?
O1 P1 C21 C23 -73.0(8) . . . . ?
O1 P1 C21 C24 163.0(7) . . . . ?
C1 C2 C3 C4 -0.2(14) . . . . ?
C1 C2 C3 C7 -179.8(9) . . . . ?
C2 C1 C6 C5 -3.9(13) . . . . ?
C2 C3 C4 C5 -0.4(14) . . . . ?
C2 C3 C7 F1A 151.6(12) . . . . ?
C2 C3 C7 F1B -172(2) . . . . ?
C2 C3 C7 F2A 29.1(14) . . . . ?
C2 C3 C7 F2B 70(2) . . . . ?
C2 C3 C7 F3A -84.9(13) . . . . ?
C2 C3 C7 F3B -56(3) . . . . ?
C3 C4 C5 C6 -1.2(14) . . . . ?
C3 C4 C5 C8 -178.2(9) . . . . ?
C4 C3 C7 F1A -28.0(16) . . . . ?
C4 C3 C7 F1B 8(2) . . . . ?
C4 C3 C7 F2A -150.5(11) . . . . ?
C4 C3 C7 F2B -109(2) . . . . ?
C4 C3 C7 F3A 95.5(13) . . . . ?
C4 C3 C7 F3B 125(2) . . . . ?
C4 C5 C6 C1 3.4(14) . . . . ?
C4 C5 C8 F4 -159.5(9) . . . . ?
C4 C5 C8 F5 82.5(12) . . . . ?
C4 C5 C8 F6 -41.0(13) . . . . ?
C6 C1 C2 C3 2.3(13) . . . . ?
C6 C5 C8 F4 23.5(13) . . . . ?
C6 C5 C8 F5 -94.5(12) . . . . ?
C6 C5 C8 F6 142.0(9) . . . . ?
C7 C3 C4 C5 179.2(9) . . . . ?
C8 C5 C6 C1 -179.7(9) . . . . ?
C9 C10 C11 C12 1.4(14) . . . . ?
C9 C10 C11 C15 179.9(10) . . . . ?
C10 C9 C14 C13 0.4(14) . . . . ?
C10 C11 C12 C13 -2.2(14) . . . . ?
C10 C11 C15 F7A -0.4(17) . . . . ?
C10 C11 C15 F7B -48(3) . . . . ?
C10 C11 C15 F8A 114.5(12) . . . . ?
C10 C11 C15 F8B 85(3) . . . . ?
C10 C11 C15 F9A -127.3(13) . . . . ?
C10 C11 C15 F9B -158(3) . . . . ?
C11 C12 C13 C14 2.0(14) . . . . ?
C11 C12 C13 C16 179.8(9) . . . . ?
C12 C11 C15 F7A 178.1(11) . . . . ?
C12 C11 C15 F7B 130(2) . . . . ?
C12 C11 C15 F8A -67.0(14) . . . . ?
C12 C11 C15 F8B -96(3) . . . . ?
C12 C11 C15 F9A 51.1(16) . . . . ?
C12 C11 C15 F9B 21(3) . . . . ?
C12 C13 C14 C9 -1.1(14) . . . . ?
C12 C13 C16 F10 50.4(13) . . . . ?
C12 C13 C16 F11 -69.8(11) . . . . ?
C12 C13 C16 F12 170.8(9) . . . . ?
C14 C9 C10 C11 -0.5(14) . . . . ?
C14 C13 C16 F10 -131.8(10) . . . . ?
C14 C13 C16 F11 107.9(10) . . . . ?
C14 C13 C16 F12 -11.5(14) . . . . ?
C15 C11 C12 C13 179.4(10) . . . . ?
C16 C13 C14 C9 -178.8(9) . . . . ?
C17 P1 O1 Sb1 118.8(5) . . . . ?
C17 P1 C21 C22 172.0(6) . . . . ?
C17 P1 C21 C23 53.2(9) . . . . ?
C17 P1 C21 C24 -70.8(8) . . . . ?
C21 P1 O1 Sb1 -109.8(5) . . . . ?
C21 P1 C17 C18 166.6(6) . . . . ?
C21 P1 C17 C19 -75.4(8) . . . . ?
C21 P1 C17 C20 48.4(9) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.892(2)
2 0.108(2)
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
0.9987 -0.0010 -0.0006 -0.0336 0.0029 -0.0027
-0.9987 0.0010 0.0006 0.0336 -0.0029 0.0027
-0.0039 -0.9995 0.0008 -0.0016 0.0223 0.0436
0.0039 0.9995 -0.0008 0.0016 -0.0223 -0.0436
0.9767 -0.0022 -1.9979 0.0119 0.1309 -0.0665
-0.9767 0.0022 1.9979 -0.0119 -0.1309 0.0665
