#------------------------------------------------------------------------------
#$Date: 2025-07-06 19:08:53 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300836 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/84/7718459.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_7718459
loop_
_publ_author_name
'Møller, Mads Sondrup'
'McKee, Vickie'
'McKenzie, Christine J.'
_publ_section_title
;
 Stereochemically (In)active lone pairs in Sb(III) complexes of a soft
 scorpionate ligand.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6665
_journal_page_last               6673
_journal_paper_doi               10.1039/d5dt00261c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C24 H32 B2 N12 S6 Sb, F6 P, C3 H6 O'
_chemical_formula_sum            'C27 H38 B2 F6 N12 O P S6 Sb'
_chemical_formula_weight         1027.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-03 deposited with the CCDC.	2025-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.992(5)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   45.083(3)
_cell_length_b                   9.2529(5)
_cell_length_c                   30.1304(17)
_cell_measurement_reflns_used    6253
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      62.1810
_cell_measurement_theta_min      3.7570
_cell_volume                     12475.4(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.115a 64-bit (release 15-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (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 5.2923
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -13.00  25.00   1.00   12.50    --   -0.78 -77.00 -90.00   38
  2  ω    -66.00  14.00   1.00   12.50    --   -0.78 -38.00   0.00   80
  3  ω    -19.00  72.00   1.00   12.50    --   -0.78  19.00-180.00   91
  4  ω     56.00 110.00   1.00   37.50    --   73.78-125.00 120.00   54
  5  ω     53.00 110.00   1.00   37.50    --   73.78-125.00-120.00   57
  6  ω     45.00  84.00   1.00   37.50    --   73.78-125.00 -60.00   39
  7  ω     52.00 110.00   1.00   37.50    --   73.78-125.00   0.00   58
  8  ω    -45.00  -9.00   1.00   37.50    --  -75.34  38.00  90.00   36
  9  ω    -48.00  -9.00   1.00   37.50    --  -75.34  57.00   0.00   39
 10  ω    -86.00 -55.00   1.00   37.50    --  -75.34 125.00 -30.00   31
 11  ω    -45.00 -20.00   1.00   37.50    --  -75.34  38.00 120.00   25
 12  ω    -45.00  -9.00   1.00   37.50    --  -75.34  38.00-120.00   36
 13  ω    -79.00 -14.00   1.00   37.50    --  -75.34 125.00  60.00   65
 14  ω    -40.00  -9.00   1.00   37.50    --  -75.34  38.00 -30.00   31
 15  ω    -69.00  -9.00   1.00   37.50    --  -75.34  57.00-180.00   60
 16  ω    -45.00 -10.00   1.00   37.50    --  -75.34  38.00  60.00   35
 17  ω    -79.00  -8.00   1.00   37.50    --  -75.34   0.00  60.00   71
 18  ω   -142.00 -67.00   1.00   37.50    --  -75.34 -38.00-120.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0081002000
_diffrn_orient_matrix_UB_12      -0.1567305000
_diffrn_orient_matrix_UB_13      -0.0138474000
_diffrn_orient_matrix_UB_21      0.0059864000
_diffrn_orient_matrix_UB_22      -0.0475302000
_diffrn_orient_matrix_UB_23      0.0492468000
_diffrn_orient_matrix_UB_31      -0.0329003000
_diffrn_orient_matrix_UB_32      0.0299071000
_diffrn_orient_matrix_UB_33      0.0058022000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            15324
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        62.497
_diffrn_reflns_theta_max         62.497
_diffrn_reflns_theta_min         2.955
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.052
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       lath
_exptl_crystal_F_000             6216
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         15324
_refine_ls_number_restraints     774
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0523P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9817
_reflns_number_total             15324
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by -179.4683° 
around [0.06 1.00 0.06] (reciprocal) or [0.00 1.00 0.01] (direct)
;
_cod_data_source_file            d5dt00261c2.cif
_cod_data_source_block           sbpf6_hklf5_(3b)
_cod_depositor_comments
'Adding full bibliography for 7718459--7718463.cif.'
_cod_original_cell_volume        12475.4(12)
_cod_database_code               7718459
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C30H30N10O1F6PS6B2Sb
_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   0.773
_shelx_estimated_absorpt_t_min   0.278
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5697(11)
 0.4303(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H) groups, All C(H,H,H) groups
3. Restrained distances
 B1-H1 \\sim B2-H2 \\sim B3-H3A
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O41, C41, C42, C43} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O51, C51, C52, C53}
6. Others
 Fixed Sof: P2(0.5) F7(0.5) F8(0.5) F9(0.5) F101(0.5) F11(0.5) F12(0.5)
 O51(0.5) C51(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53(0.5) H53A(0.5)
 H53B(0.5) H53C(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C15(H15),
 C18(H18), C19(H19), C22(H22), C23(H23), C26(H26), C27(H27), C30(H30), C31(H31),
  C34(H34), C35(H35)
7.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C),
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C32(H32A,H32B,
 H32C), C36(H36A,H36B,H36C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C52(H52A,
 H52B,H52C), C53(H53A,H53B,H53C)
;
_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 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.619
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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 0.59548(2) 0.76225(6) 0.47212(2) 0.01994(13) Uani 1 1 d . . . . .
B1 B 0.58513(18) 0.9368(9) 0.5982(3) 0.0247(18) Uani 1 1 d D . . . .
H1 H 0.5836(13) 0.982(7) 0.6350(15) 0.037 Uiso 1 1 d D U . . .
B2 B 0.60569(19) 0.6053(10) 0.3470(3) 0.0273(19) Uani 1 1 d D . . . .
H2 H 0.6088(14) 0.562(7) 0.3101(16) 0.041 Uiso 1 1 d D U . . .
S1 S 0.63327(4) 0.7086(2) 0.54680(6) 0.0281(5) Uani 1 1 d . . . . .
S2 S 0.59505(4) 1.0494(2) 0.49044(6) 0.0255(4) Uani 1 1 d . . . . .
S3 S 0.54897(4) 0.70353(19) 0.51684(6) 0.0231(4) Uani 1 1 d . . . . .
S4 S 0.55250(4) 0.7996(2) 0.39975(6) 0.0309(5) Uani 1 1 d . . . . .
S5 S 0.59624(4) 0.4733(2) 0.45342(6) 0.0253(4) Uani 1 1 d . . . . .
S6 S 0.64435(4) 0.8301(2) 0.42863(7) 0.0318(5) Uani 1 1 d . . . . .
N1 N 0.61844(11) 0.9610(6) 0.58999(18) 0.0236(13) Uani 1 1 d . . . . .
N2 N 0.66265(12) 0.9594(7) 0.56779(19) 0.0300(15) Uani 1 1 d . . . . .
N3 N 0.56296(11) 1.0150(6) 0.56324(19) 0.0205(13) Uani 1 1 d . . . . .
N4 N 0.53887(12) 1.1173(6) 0.50443(19) 0.0218(13) Uani 1 1 d . . . . .
N5 N 0.57881(11) 0.7726(6) 0.60037(17) 0.0197(12) Uani 1 1 d . . . . .
N6 N 0.57233(12) 0.5411(6) 0.5880(2) 0.0226(13) Uani 1 1 d . . . . .
N7 N 0.57328(12) 0.5663(6) 0.35392(18) 0.0231(14) Uani 1 1 d . . . . .
N8 N 0.52898(12) 0.5381(7) 0.3750(2) 0.0331(16) Uani 1 1 d . . . . .
N9 N 0.62856(11) 0.5264(6) 0.38221(19) 0.0209(13) Uani 1 1 d . . . . .
N10 N 0.65326(12) 0.4236(6) 0.4402(2) 0.0274(14) Uani 1 1 d . . . . .
N11 N 0.60996(12) 0.7719(6) 0.34771(18) 0.0244(13) Uani 1 1 d . . . . .
N12 N 0.61610(14) 1.0019(7) 0.3637(2) 0.0340(15) Uani 1 1 d . . . . .
C1 C 0.63739(15) 0.8799(8) 0.5687(2) 0.0245(16) Uani 1 1 d . . . . .
C2 C 0.63228(15) 1.0906(8) 0.6015(2) 0.0323(19) Uani 1 1 d . . . . .
H2A H 0.624027 1.167906 0.616761 0.039 Uiso 1 1 calc R U . . .
C3 C 0.65892(16) 1.0889(9) 0.5878(2) 0.0341(19) Uani 1 1 d . . . . .
H3 H 0.673128 1.165163 0.591305 0.041 Uiso 1 1 calc R U . . .
C4 C 0.68949(16) 0.9091(10) 0.5494(3) 0.048(2) Uani 1 1 d . . . . .
H4A H 0.684817 0.894167 0.517062 0.072 Uiso 1 1 calc R U . . .
H4B H 0.696253 0.817860 0.563681 0.072 Uiso 1 1 calc R U . . .
H4C H 0.705316 0.981760 0.555011 0.072 Uiso 1 1 calc R U . . .
C5 C 0.56481(14) 1.0599(7) 0.5202(2) 0.0224(16) Uani 1 1 d . . . . .
C6 C 0.53472(14) 1.0469(7) 0.5728(2) 0.0255(17) Uani 1 1 d . . . . .
H6 H 0.527173 1.027656 0.600323 0.031 Uiso 1 1 calc R U . . .
C7 C 0.51920(15) 1.1112(8) 0.5361(3) 0.0264(17) Uani 1 1 d . . . . .
H7 H 0.499124 1.144578 0.533011 0.032 Uiso 1 1 calc R U . . .
C8 C 0.53179(15) 1.1813(8) 0.4598(2) 0.0311(18) Uani 1 1 d . . . . .
H8A H 0.534694 1.108848 0.437032 0.047 Uiso 1 1 calc R U . . .
H8B H 0.544993 1.263891 0.456799 0.047 Uiso 1 1 calc R U . . .
H8C H 0.510947 1.213828 0.455901 0.047 Uiso 1 1 calc R U . . .
C9 C 0.56779(14) 0.6731(8) 0.5700(2) 0.0190(15) Uani 1 1 d . . . . .
C10 C 0.59055(15) 0.6971(8) 0.6378(2) 0.0276(17) Uani 1 1 d . . . . .
H10 H 0.599730 0.739107 0.664770 0.033 Uiso 1 1 calc R U . . .
C11 C 0.58702(15) 0.5551(9) 0.6301(2) 0.0301(17) Uani 1 1 d . . . . .
H11 H 0.593487 0.478962 0.650140 0.036 Uiso 1 1 calc R U . . .
C12 C 0.56544(16) 0.4035(7) 0.5645(3) 0.0303(19) Uani 1 1 d . . . . .
H12A H 0.547094 0.414063 0.543745 0.045 Uiso 1 1 calc R U . . .
H12B H 0.562653 0.327787 0.586392 0.045 Uiso 1 1 calc R U . . .
H12C H 0.581994 0.376999 0.547872 0.045 Uiso 1 1 calc R U . . .
C13 C 0.55219(15) 0.6311(8) 0.3757(2) 0.0264(17) Uani 1 1 d . . . . .
C14 C 0.56211(16) 0.4337(8) 0.3389(3) 0.0339(19) Uani 1 1 d . . . . .
H14 H 0.572016 0.366892 0.321842 0.041 Uiso 1 1 calc R U . . .
C15 C 0.53507(17) 0.4139(9) 0.3523(3) 0.041(2) Uani 1 1 d . . . . .
H15 H 0.522629 0.331197 0.347247 0.049 Uiso 1 1 calc R U . . .
C16 C 0.50181(15) 0.5640(10) 0.3954(3) 0.045(2) Uani 1 1 d . . . . .
H16A H 0.494538 0.662035 0.388143 0.067 Uiso 1 1 calc R U . . .
H16B H 0.506077 0.553828 0.427970 0.067 Uiso 1 1 calc R U . . .
H16C H 0.486516 0.493723 0.383955 0.067 Uiso 1 1 calc R U . . .
C17 C 0.62635(14) 0.4764(7) 0.4238(2) 0.0210(16) Uani 1 1 d . . . . .
C18 C 0.65770(14) 0.5047(8) 0.3736(3) 0.0289(18) Uani 1 1 d . . . . .
H18 H 0.665554 0.530449 0.346776 0.035 Uiso 1 1 calc R U . . .
C19 C 0.67282(15) 0.4420(8) 0.4089(3) 0.0308(18) Uani 1 1 d . . . . .
H19 H 0.693283 0.414777 0.412064 0.037 Uiso 1 1 calc R U . . .
C20 C 0.66032(17) 0.3595(9) 0.4847(3) 0.043(2) Uani 1 1 d . . . . .
H20A H 0.645835 0.283152 0.488766 0.065 Uiso 1 1 calc R U . . .
H20B H 0.659381 0.434185 0.507513 0.065 Uiso 1 1 calc R U . . .
H20C H 0.680481 0.318185 0.487480 0.065 Uiso 1 1 calc R U . . .
C21 C 0.62288(15) 0.8659(8) 0.3791(2) 0.0244(16) Uani 1 1 d . . . . .
C22 C 0.59522(17) 0.8510(9) 0.3128(3) 0.0361(19) Uani 1 1 d . . . . .
H22 H 0.584514 0.812567 0.286267 0.043 Uiso 1 1 calc R U . . .
C23 C 0.59879(18) 0.9934(9) 0.3231(3) 0.042(2) Uani 1 1 d . . . . .
H23 H 0.590781 1.072527 0.305434 0.050 Uiso 1 1 calc R U . . .
C24 C 0.6240(2) 1.1362(8) 0.3875(3) 0.051(2) Uani 1 1 d . . . . .
H24A H 0.624531 1.215022 0.365851 0.076 Uiso 1 1 calc R U . . .
H24B H 0.643665 1.126112 0.404945 0.076 Uiso 1 1 calc R U . . .
H24C H 0.609028 1.157901 0.407560 0.076 Uiso 1 1 calc R U . . .
Sb2 Sb 0.750000 -0.250000 0.250000 0.01986(16) Uani 1 2 d S . P . .
B3 B 0.66327(19) -0.0949(9) 0.2179(3) 0.0251(19) Uani 1 1 d D . . . .
H3A H 0.6384(10) -0.053(7) 0.207(2) 0.038 Uiso 1 1 d D U . . .
S7 S 0.70647(4) -0.2768(2) 0.30505(6) 0.0296(5) Uani 1 1 d . . . . .
S8 S 0.73686(4) 0.0369(2) 0.23819(7) 0.0303(5) Uani 1 1 d . . . . .
S9 S 0.71370(4) -0.3295(2) 0.17479(6) 0.0273(5) Uani 1 1 d . . . . .
N13 N 0.67323(12) -0.0461(6) 0.2665(2) 0.0252(13) Uani 1 1 d . . . . .
N14 N 0.69546(13) -0.0078(7) 0.3345(2) 0.0347(15) Uani 1 1 d . . . . .
N15 N 0.68348(11) -0.0234(6) 0.18487(19) 0.0242(13) Uani 1 1 d . . . . .
N16 N 0.71879(13) 0.0619(7) 0.1497(2) 0.0375(17) Uani 1 1 d . . . . .
N17 N 0.66312(10) -0.2605(7) 0.21429(17) 0.0206(12) Uani 1 1 d . . . . .
N18 N 0.67188(11) -0.4924(6) 0.20922(19) 0.0248(14) Uani 1 1 d . . . . .
C25 C 0.69113(15) -0.1061(8) 0.3006(2) 0.0250(16) Uani 1 1 d . . . . .
C26 C 0.66539(16) 0.0916(8) 0.2793(3) 0.0351(19) Uani 1 1 d . . . . .
H26 H 0.652412 0.156909 0.262127 0.042 Uiso 1 1 calc R U . . .
C27 C 0.67965(16) 0.1153(9) 0.3207(3) 0.041(2) Uani 1 1 d . . . . .
H27 H 0.678928 0.201879 0.337521 0.049 Uiso 1 1 calc R U . . .
C28 C 0.71350(17) -0.0293(10) 0.3773(3) 0.050(2) Uani 1 1 d . . . . .
H28A H 0.733847 -0.056630 0.372399 0.075 Uiso 1 1 calc R U . . .
H28B H 0.704709 -0.106395 0.393827 0.075 Uiso 1 1 calc R U . . .
H28C H 0.714110 0.060453 0.394670 0.075 Uiso 1 1 calc R U . . .
C29 C 0.71157(14) 0.0234(8) 0.1900(2) 0.0246(16) Uani 1 1 d . . . . .
C30 C 0.67269(16) -0.0142(9) 0.1397(3) 0.0357(19) Uani 1 1 d . . . . .
H30 H 0.653181 -0.040114 0.126633 0.043 Uiso 1 1 calc R U . . .
C31 C 0.69447(17) 0.0373(9) 0.1181(3) 0.045(2) Uani 1 1 d . . . . .
H31 H 0.693472 0.053961 0.086791 0.053 Uiso 1 1 calc R U . . .
C32 C 0.74826(17) 0.1179(11) 0.1411(3) 0.062(3) Uani 1 1 d . . . . .
H32A H 0.763305 0.041580 0.146947 0.093 Uiso 1 1 calc R U . . .
H32B H 0.753761 0.200359 0.160783 0.093 Uiso 1 1 calc R U . . .
H32C H 0.747256 0.148780 0.109831 0.093 Uiso 1 1 calc R U . . .
C33 C 0.68202(14) -0.3600(7) 0.1999(2) 0.0221(16) Uani 1 1 d . . . . .
C34 C 0.64103(15) -0.3375(8) 0.2324(2) 0.0279(17) Uani 1 1 d . . . . .
H34 H 0.624729 -0.295654 0.245063 0.033 Uiso 1 1 calc R U . . .
C35 C 0.64613(15) -0.4785(8) 0.2295(2) 0.0310(18) Uani 1 1 d . . . . .
H35 H 0.634402 -0.554627 0.239353 0.037 Uiso 1 1 calc R U . . .
C36 C 0.68639(17) -0.6288(8) 0.2011(3) 0.037(2) Uani 1 1 d . . . . .
H36A H 0.671164 -0.702189 0.192156 0.055 Uiso 1 1 calc R U . . .
H36B H 0.698670 -0.659958 0.228537 0.055 Uiso 1 1 calc R U . . .
H36C H 0.699098 -0.616035 0.177246 0.055 Uiso 1 1 calc R U . . .
P1 P 0.57584(4) 0.2512(2) 0.71803(6) 0.0264(4) Uani 1 1 d . . . . .
F1 F 0.57932(9) 0.4229(4) 0.72367(13) 0.0361(11) Uani 1 1 d . . . . .
F2 F 0.57325(9) 0.0800(5) 0.71337(14) 0.0392(11) Uani 1 1 d . . . . .
F3 F 0.55256(9) 0.2730(5) 0.67447(14) 0.0482(12) Uani 1 1 d . . . . .
F4 F 0.60010(8) 0.2291(4) 0.76190(12) 0.0279(9) Uani 1 1 d . . . . .
F5 F 0.60285(8) 0.2508(5) 0.68758(12) 0.0358(10) Uani 1 1 d . . . . .
F6 F 0.54949(8) 0.2529(5) 0.74918(13) 0.0397(10) Uani 1 1 d . . . . .
P2 P 0.75467(18) 0.2123(4) 0.4939(3) 0.033(2) Uani 0.5 1 d . . P A -1
F7 F 0.7318(3) 0.2220(16) 0.5316(5) 0.050(4) Uani 0.5 1 d . . P A -1
F8 F 0.7775(3) 0.2059(15) 0.4572(5) 0.047(4) Uani 0.5 1 d . . P A -1
F9 F 0.72948(18) 0.2773(12) 0.4572(3) 0.048(2) Uani 0.5 1 d . . P A -1
F101 F 0.77953(19) 0.1467(12) 0.5294(3) 0.049(2) Uani 0.5 1 d . . P A -1
F11 F 0.7439(2) 0.0513(10) 0.4805(3) 0.051(3) Uani 0.5 1 d . . P A -1
F12 F 0.76619(18) 0.3697(10) 0.5073(4) 0.056(3) Uani 0.5 1 d . . P A -1
O41 O 0.48454(14) 0.1613(8) 0.3461(2) 0.069(2) Uani 1 1 d D . . . .
C41 C 0.4850(2) 0.1215(11) 0.3081(4) 0.054(2) Uani 1 1 d D . . . .
C42 C 0.4661(2) 0.1978(11) 0.2700(4) 0.079(3) Uani 1 1 d D . . . .
H42A H 0.478027 0.212745 0.245267 0.119 Uiso 1 1 calc R U . . .
H42B H 0.459577 0.291531 0.280440 0.119 Uiso 1 1 calc R U . . .
H42C H 0.448641 0.138449 0.259813 0.119 Uiso 1 1 calc R U . . .
C43 C 0.5030(2) -0.0035(11) 0.2962(4) 0.072(3) Uani 1 1 d D . . . .
H43A H 0.490013 -0.072537 0.278488 0.107 Uiso 1 1 calc R U . . .
H43B H 0.512248 -0.050672 0.323593 0.107 Uiso 1 1 calc R U . . .
H43C H 0.518621 0.029986 0.278733 0.107 Uiso 1 1 calc R U . . .
O51 O 0.7183(4) 0.5937(17) 0.5234(7) 0.121(6) Uani 0.5 1 d D . P B -2
C51 C 0.7390(5) 0.658(2) 0.5104(8) 0.075(6) Uani 0.5 1 d D . P B -2
C52 C 0.7408(6) 0.686(4) 0.4594(9) 0.077(9) Uani 0.5 1 d D . P B -2
H52A H 0.756636 0.625369 0.449402 0.116 Uiso 0.5 1 calc R U P B -2
H52B H 0.745416 0.787782 0.454825 0.116 Uiso 0.5 1 calc R U P B -2
H52C H 0.721664 0.661423 0.442076 0.116 Uiso 0.5 1 calc R U P B -2
C53 C 0.7693(6) 0.701(5) 0.5331(10) 0.095(11) Uani 0.5 1 d D . P B -2
H53A H 0.784699 0.672446 0.514573 0.143 Uiso 0.5 1 calc R U P B -2
H53B H 0.773051 0.653815 0.562342 0.143 Uiso 0.5 1 calc R U P B -2
H53C H 0.769909 0.806494 0.537256 0.143 Uiso 0.5 1 calc R U P B -2
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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Sb Sb -0.0562 5.8946 '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 0.0090
-1 0 0 0.0180
-2 0 -1 0.0282
2 0 1 0.0040
0 2 -1 0.0820
1 -2 1 0.0944
0 0 -1 0.0325
0 0 1 0.0067
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
S1 Sb1 S2 91.71(6) . . ?
S1 Sb1 S4 173.95(6) . . ?
S1 Sb1 S5 88.26(6) . . ?
S1 Sb1 S6 88.76(6) . . ?
S2 Sb1 S4 90.94(6) . . ?
S2 Sb1 S5 179.64(5) . . ?
S2 Sb1 S6 84.27(5) . . ?
S3 Sb1 S1 89.81(5) . . ?
S3 Sb1 S2 94.06(5) . . ?
S3 Sb1 S4 84.58(5) . . ?
S3 Sb1 S5 86.30(5) . . ?
S3 Sb1 S6 177.77(6) . . ?
S4 Sb1 S6 96.91(6) . . ?
S5 Sb1 S4 89.12(6) . . ?
S5 Sb1 S6 95.37(5) . . ?
N1 B1 H1 105(3) . . ?
N3 B1 H1 111(3) . . ?
N3 B1 N1 112.3(6) . . ?
N3 B1 N5 112.5(6) . . ?
N5 B1 H1 106(3) . . ?
N5 B1 N1 109.3(6) . . ?
N7 B2 H2 105(3) . . ?
N7 B2 N9 110.8(6) . . ?
N7 B2 N11 110.3(6) . . ?
N9 B2 H2 109(3) . . ?
N11 B2 H2 108(3) . . ?
N11 B2 N9 112.5(6) . . ?
C1 S1 Sb1 100.3(2) . . ?
C5 S2 Sb1 100.7(2) . . ?
C9 S3 Sb1 99.9(2) . . ?
C13 S4 Sb1 100.9(3) . . ?
C17 S5 Sb1 97.0(2) . . ?
C21 S6 Sb1 93.4(2) . . ?
C1 N1 B1 131.8(6) . . ?
C1 N1 C2 108.0(6) . . ?
C2 N1 B1 119.8(6) . . ?
C1 N2 C3 108.5(6) . . ?
C1 N2 C4 124.6(6) . . ?
C3 N2 C4 126.8(6) . . ?
C5 N3 B1 132.7(5) . . ?
C6 N3 B1 119.9(6) . . ?
C6 N3 C5 107.4(6) . . ?
C5 N4 C7 110.6(6) . . ?
C5 N4 C8 125.2(5) . . ?
C7 N4 C8 124.2(6) . . ?
C9 N5 B1 134.1(6) . . ?
C9 N5 C10 106.4(6) . . ?
C10 N5 B1 118.6(6) . . ?
C9 N6 C11 108.7(6) . . ?
C9 N6 C12 125.6(6) . . ?
C11 N6 C12 125.4(6) . . ?
C13 N7 B2 133.8(6) . . ?
C13 N7 C14 107.5(6) . . ?
C14 N7 B2 118.5(6) . . ?
C13 N8 C15 109.6(6) . . ?
C13 N8 C16 125.3(6) . . ?
C15 N8 C16 125.0(6) . . ?
C17 N9 B2 132.2(5) . . ?
C17 N9 C18 107.7(6) . . ?
C18 N9 B2 120.1(6) . . ?
C17 N10 C19 109.0(6) . . ?
C17 N10 C20 124.8(6) . . ?
C19 N10 C20 126.2(6) . . ?
C21 N11 B2 133.3(6) . . ?
C21 N11 C22 108.3(6) . . ?
C22 N11 B2 117.8(6) . . ?
C21 N12 C23 109.3(7) . . ?
C21 N12 C24 126.2(7) . . ?
C23 N12 C24 124.4(7) . . ?
N1 C1 S1 130.4(5) . . ?
N1 C1 N2 106.8(6) . . ?
N2 C1 S1 122.9(5) . . ?
N1 C2 H2A 125.9 . . ?
C3 C2 N1 108.2(7) . . ?
C3 C2 H2A 125.9 . . ?
N2 C3 H3 125.8 . . ?
C2 C3 N2 108.4(7) . . ?
C2 C3 H3 125.8 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 S2 128.1(5) . . ?
N4 C5 S2 124.0(5) . . ?
N4 C5 N3 107.9(5) . . ?
N3 C6 H6 125.7 . . ?
N3 C6 C7 108.6(6) . . ?
C7 C6 H6 125.7 . . ?
N4 C7 H7 127.2 . . ?
C6 C7 N4 105.5(6) . . ?
C6 C7 H7 127.2 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N5 C9 S3 127.6(5) . . ?
N6 C9 S3 123.4(6) . . ?
N6 C9 N5 108.9(6) . . ?
N5 C10 H10 125.3 . . ?
C11 C10 N5 109.3(7) . . ?
C11 C10 H10 125.3 . . ?
N6 C11 H11 126.7 . . ?
C10 C11 N6 106.7(7) . . ?
C10 C11 H11 126.7 . . ?
N6 C12 H12A 109.5 . . ?
N6 C12 H12B 109.5 . . ?
N6 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N7 C13 S4 129.3(5) . . ?
N8 C13 S4 123.3(5) . . ?
N8 C13 N7 107.3(6) . . ?
N7 C14 H14 125.3 . . ?
C15 C14 N7 109.3(6) . . ?
C15 C14 H14 125.3 . . ?
N8 C15 H15 126.9 . . ?
C14 C15 N8 106.1(7) . . ?
C14 C15 H15 126.9 . . ?
N8 C16 H16A 109.5 . . ?
N8 C16 H16B 109.5 . . ?
N8 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N9 C17 S5 129.9(5) . . ?
N10 C17 S5 122.5(5) . . ?
N10 C17 N9 107.6(5) . . ?
N9 C18 H18 125.7 . . ?
C19 C18 N9 108.6(6) . . ?
C19 C18 H18 125.7 . . ?
N10 C19 H19 126.4 . . ?
C18 C19 N10 107.2(6) . . ?
C18 C19 H19 126.4 . . ?
N10 C20 H20A 109.5 . . ?
N10 C20 H20B 109.5 . . ?
N10 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N11 C21 S6 129.1(6) . . ?
N12 C21 S6 123.7(6) . . ?
N12 C21 N11 107.2(7) . . ?
N11 C22 H22 126.1 . . ?
C23 C22 N11 107.8(7) . . ?
C23 C22 H22 126.1 . . ?
N12 C23 H23 126.3 . . ?
C22 C23 N12 107.4(7) . . ?
C22 C23 H23 126.3 . . ?
N12 C24 H24A 109.5 . . ?
N12 C24 H24B 109.5 . . ?
N12 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
S7 Sb2 S7 180.00(4) . 7_645 ?
S7 Sb2 S8 90.41(5) . . ?
S7 Sb2 S8 89.59(5) . 7_645 ?
S7 Sb2 S8 89.59(5) 7_645 . ?
S7 Sb2 S8 90.41(5) 7_645 7_645 ?
S8 Sb2 S8 180.0 7_645 . ?
S9 Sb2 S7 94.43(5) . . ?
S9 Sb2 S7 85.57(5) . 7_645 ?
S9 Sb2 S7 94.43(5) 7_645 7_645 ?
S9 Sb2 S7 85.57(5) 7_645 . ?
S9 Sb2 S8 86.84(6) 7_645 . ?
S9 Sb2 S8 93.16(6) 7_645 7_645 ?
S9 Sb2 S8 93.16(6) . . ?
S9 Sb2 S8 86.84(6) . 7_645 ?
S9 Sb2 S9 180.0 . 7_645 ?
N13 B3 H3A 109(3) . . ?
N13 B3 N15 110.6(6) . . ?
N15 B3 H3A 106(3) . . ?
N17 B3 H3A 108(3) . . ?
N17 B3 N13 110.9(6) . . ?
N17 B3 N15 111.8(6) . . ?
C25 S7 Sb2 100.4(2) . . ?
C29 S8 Sb2 98.5(2) . . ?
C33 S9 Sb2 97.2(2) . . ?
C25 N13 B3 132.9(6) . . ?
C25 N13 C26 108.4(7) . . ?
C26 N13 B3 118.4(7) . . ?
C25 N14 C27 107.7(7) . . ?
C25 N14 C28 125.9(7) . . ?
C27 N14 C28 126.3(7) . . ?
C29 N15 B3 132.9(6) . . ?
C29 N15 C30 107.9(6) . . ?
C30 N15 B3 118.9(6) . . ?
C29 N16 C31 108.7(6) . . ?
C29 N16 C32 125.0(7) . . ?
C31 N16 C32 126.3(7) . . ?
C33 N17 B3 134.4(5) . . ?
C33 N17 C34 106.6(6) . . ?
C34 N17 B3 118.7(5) . . ?
C33 N18 C35 109.4(6) . . ?
C33 N18 C36 125.6(6) . . ?
C35 N18 C36 125.0(6) . . ?
N13 C25 S7 129.4(6) . . ?
N13 C25 N14 108.3(6) . . ?
N14 C25 S7 122.3(6) . . ?
N13 C26 H26 126.4 . . ?
C27 C26 N13 107.3(8) . . ?
C27 C26 H26 126.4 . . ?
N14 C27 H27 125.9 . . ?
C26 C27 N14 108.3(7) . . ?
C26 C27 H27 125.9 . . ?
N14 C28 H28A 109.5 . . ?
N14 C28 H28B 109.5 . . ?
N14 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N15 C29 S8 129.7(5) . . ?
N15 C29 N16 108.3(6) . . ?
N16 C29 S8 122.0(5) . . ?
N15 C30 H30 125.9 . . ?
C31 C30 N15 108.1(7) . . ?
C31 C30 H30 125.9 . . ?
N16 C31 H31 126.5 . . ?
C30 C31 N16 106.9(7) . . ?
C30 C31 H31 126.5 . . ?
N16 C32 H32A 109.5 . . ?
N16 C32 H32B 109.5 . . ?
N16 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N17 C33 S9 128.0(5) . . ?
N18 C33 S9 124.2(5) . . ?
N18 C33 N17 107.8(6) . . ?
N17 C34 H34 125.1 . . ?
C35 C34 N17 109.8(6) . . ?
C35 C34 H34 125.1 . . ?
N18 C35 H35 126.8 . . ?
C34 C35 N18 106.4(6) . . ?
C34 C35 H35 126.8 . . ?
N18 C36 H36A 109.5 . . ?
N18 C36 H36B 109.5 . . ?
N18 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
F1 P1 F4 89.5(2) . . ?
F1 P1 F5 89.5(2) . . ?
F2 P1 F1 178.3(3) . . ?
F2 P1 F4 88.9(2) . . ?
F2 P1 F5 90.0(2) . . ?
F2 P1 F6 90.6(2) . . ?
F3 P1 F1 90.4(3) . . ?
F3 P1 F2 91.1(3) . . ?
F3 P1 F4 178.9(2) . . ?
F3 P1 F5 89.9(2) . . ?
F3 P1 F6 91.2(2) . . ?
F5 P1 F4 89.0(2) . . ?
F6 P1 F1 89.9(2) . . ?
F6 P1 F4 89.9(2) . . ?
F6 P1 F5 178.7(3) . . ?
F8 P2 F7 178.7(8) . . ?
F8 P2 F9 89.9(7) . . ?
F8 P2 F11 89.5(7) . . ?
F9 P2 F7 90.3(7) . . ?
F9 P2 F11 90.4(7) . . ?
F101 P2 F7 90.3(7) . . ?
F101 P2 F8 89.5(7) . . ?
F101 P2 F9 179.1(7) . . ?
F101 P2 F11 89.0(6) . . ?
F101 P2 F12 89.9(8) . . ?
F11 P2 F7 91.7(7) . . ?
F12 P2 F7 89.3(7) . . ?
F12 P2 F8 89.5(7) . . ?
F12 P2 F9 90.7(7) . . ?
F12 P2 F11 178.5(6) . . ?
O41 C41 C42 120.2(10) . . ?
O41 C41 C43 122.9(10) . . ?
C43 C41 C42 116.9(10) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O51 C51 C52 122(2) . . ?
O51 C51 C53 133(3) . . ?
C53 C51 C52 104.2(16) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 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 S1 2.698(2) . ?
Sb1 S2 2.714(2) . ?
Sb1 S3 2.6825(16) . ?
Sb1 S4 2.757(2) . ?
Sb1 S5 2.7338(19) . ?
Sb1 S6 2.7692(18) . ?
B1 H1 1.19(4) . ?
B1 N1 1.568(9) . ?
B1 N3 1.542(10) . ?
B1 N5 1.549(10) . ?
B2 H2 1.21(4) . ?
B2 N7 1.544(9) . ?
B2 N9 1.567(10) . ?
B2 N11 1.553(10) . ?
S1 C1 1.719(7) . ?
S2 C5 1.722(6) . ?
S3 C9 1.743(7) . ?
S4 C13 1.719(8) . ?
S5 C17 1.714(6) . ?
S6 C21 1.711(8) . ?
N1 C1 1.354(8) . ?
N1 C2 1.377(9) . ?
N2 C1 1.359(8) . ?
N2 C3 1.361(9) . ?
N2 C4 1.467(8) . ?
N3 C5 1.375(8) . ?
N3 C6 1.371(7) . ?
N4 C5 1.319(8) . ?
N4 C7 1.380(8) . ?
N4 C8 1.467(8) . ?
N5 C9 1.349(8) . ?
N5 C10 1.375(8) . ?
N6 C9 1.341(8) . ?
N6 C11 1.365(9) . ?
N6 C12 1.470(8) . ?
N7 C13 1.358(8) . ?
N7 C14 1.381(8) . ?
N8 C13 1.353(9) . ?
N8 C15 1.382(9) . ?
N8 C16 1.456(8) . ?
N9 C17 1.350(8) . ?
N9 C18 1.385(7) . ?
N10 C17 1.345(8) . ?
N10 C19 1.378(8) . ?
N10 C20 1.464(9) . ?
N11 C21 1.362(8) . ?
N11 C22 1.384(9) . ?
N12 C21 1.362(9) . ?
N12 C23 1.372(10) . ?
N12 C24 1.456(9) . ?
C2 H2A 0.9500 . ?
C2 C3 1.317(9) . ?
C3 H3 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 H6 0.9500 . ?
C6 C7 1.372(10) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 H10 0.9500 . ?
C10 C11 1.340(10) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 H14 0.9500 . ?
C14 C15 1.343(9) . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C18 H18 0.9500 . ?
C18 C19 1.327(10) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C22 H22 0.9500 . ?
C22 C23 1.359(11) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
Sb2 S7 2.7307(16) . ?
Sb2 S7 2.7308(16) 7_645 ?
Sb2 S8 2.7337(19) 7_645 ?
Sb2 S8 2.7337(19) . ?
Sb2 S9 2.730(2) 7_645 ?
Sb2 S9 2.730(2) . ?
B3 H3A 1.20(4) . ?
B3 N13 1.547(10) . ?
B3 N15 1.574(9) . ?
B3 N17 1.536(10) . ?
S7 C25 1.724(7) . ?
S8 C29 1.739(7) . ?
S9 C33 1.718(6) . ?
N13 C25 1.346(9) . ?
N13 C26 1.389(9) . ?
N14 C25 1.363(9) . ?
N14 C27 1.380(10) . ?
N14 C28 1.454(9) . ?
N15 C29 1.329(8) . ?
N15 C30 1.390(9) . ?
N16 C29 1.342(8) . ?
N16 C31 1.381(10) . ?
N16 C32 1.478(9) . ?
N17 C33 1.361(8) . ?
N17 C34 1.390(8) . ?
N18 C33 1.349(8) . ?
N18 C35 1.382(8) . ?
N18 C36 1.456(9) . ?
C26 H26 0.9500 . ?
C26 C27 1.350(11) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C30 H30 0.9500 . ?
C30 C31 1.332(9) . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C34 H34 0.9500 . ?
C34 C35 1.330(10) . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
P1 F1 1.604(4) . ?
P1 F2 1.593(4) . ?
P1 F3 1.590(4) . ?
P1 F4 1.623(4) . ?
P1 F5 1.611(4) . ?
P1 F6 1.601(4) . ?
P2 F7 1.626(14) . ?
P2 F8 1.600(11) . ?
P2 F9 1.603(13) . ?
P2 F101 1.573(13) . ?
P2 F11 1.604(10) . ?
P2 F12 1.581(11) . ?
O41 C41 1.203(10) . ?
C41 C42 1.518(12) . ?
C41 C43 1.481(13) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
O51 C51 1.209(17) . ?
C51 C52 1.57(2) . ?
C51 C53 1.51(2) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2A F5 0.95 2.56 3.394(8) 146.8 1_565 yes
C4 H4B O51 0.98 2.66 3.326(17) 125.8 . yes
C4 H4C F8 0.98 2.26 3.142(15) 149.1 2_666 yes
C6 H6 O41 0.95 2.48 3.310(10) 145.8 5_666 yes
C7 H7 S3 0.95 2.85 3.705(8) 149.9 5_676 yes
C8 H8B S5 0.98 3.03 3.989(7) 167.8 1_565 yes
C8 H8C S3 0.98 3.02 3.938(7) 157.3 5_676 yes
C11 H11 F1 0.95 2.44 3.131(8) 129.9 . yes
C11 H11 F5 0.95 2.41 3.337(9) 166.2 . yes
C14 H14 F4 0.95 2.49 3.400(8) 159.8 8_554 yes
C14 H14 F6 0.95 2.55 3.201(9) 125.7 8_554 yes
C15 H15 O41 0.95 2.33 3.253(10) 165.3 . yes
C18 H18 S7 0.95 2.95 3.779(7) 146.0 1_565 yes
C19 H19 F9 0.95 2.36 3.172(11) 142.5 . yes
C20 H20C F8 0.98 2.58 3.429(17) 144.3 2_656 yes
C20 H20C F9 0.98 2.52 3.407(10) 150.7 . yes
C20 H20C F101 0.98 2.50 3.419(12) 156.1 2_656 yes
C20 H20C F12 0.98 2.44 3.294(11) 145.7 2_656 yes
C23 H23 F1 0.95 2.46 3.115(9) 126.5 8_564 yes
C23 H23 F4 0.95 2.32 3.166(9) 147.4 8_564 yes
C24 H24C S2 0.98 2.83 3.600(8) 135.7 . yes
C26 H26 F4 0.95 2.58 3.364(9) 139.7 8_554 yes
C28 H28C F101 0.98 2.41 3.231(12) 141.3 2_656 yes
C30 H30 S1 0.95 2.91 3.609(9) 130.9 8_554 yes
C32 H32C F8 0.98 2.57 3.456(17) 151.0 7_655 yes
C32 H32C F9 0.98 2.48 3.383(12) 152.6 7_655 yes
C35 H35 F4 0.95 2.39 3.336(8) 173.5 8_544 yes
C42 H42C F2 0.98 2.43 3.198(10) 134.9 5_656 yes
C43 H43A F6 0.98 2.51 3.465(11) 165.5 5_656 yes
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 S1 C1 N1 75.0(7) . . . . ?
Sb1 S1 C1 N2 -106.3(6) . . . . ?
Sb1 S2 C5 N3 73.8(6) . . . . ?
Sb1 S2 C5 N4 -107.5(6) . . . . ?
Sb1 S3 C9 N5 79.0(5) . . . . ?
Sb1 S3 C9 N6 -104.2(5) . . . . ?
Sb1 S4 C13 N7 -70.0(7) . . . . ?
Sb1 S4 C13 N8 111.1(6) . . . . ?
Sb1 S5 C17 N9 -73.4(7) . . . . ?
Sb1 S5 C17 N10 107.2(6) . . . . ?
Sb1 S6 C21 N11 -78.7(6) . . . . ?
Sb1 S6 C21 N12 102.4(5) . . . . ?
B1 N1 C1 S1 -7.1(12) . . . . ?
B1 N1 C1 N2 174.1(7) . . . . ?
B1 N1 C2 C3 -174.5(7) . . . . ?
B1 N3 C5 S2 -3.3(11) . . . . ?
B1 N3 C5 N4 177.8(7) . . . . ?
B1 N3 C6 C7 -177.9(6) . . . . ?
B1 N5 C9 S3 -14.5(10) . . . . ?
B1 N5 C9 N6 168.4(6) . . . . ?
B1 N5 C10 C11 -169.6(6) . . . . ?
B2 N7 C13 S4 8.3(12) . . . . ?
B2 N7 C13 N8 -172.7(7) . . . . ?
B2 N7 C14 C15 173.3(7) . . . . ?
B2 N9 C17 S5 3.4(11) . . . . ?
B2 N9 C17 N10 -177.1(7) . . . . ?
B2 N9 C18 C19 177.3(6) . . . . ?
B2 N11 C21 S6 9.9(10) . . . . ?
B2 N11 C21 N12 -171.1(6) . . . . ?
B2 N11 C22 C23 172.0(6) . . . . ?
N1 B1 N3 C5 24.5(11) . . . . ?
N1 B1 N3 C6 -158.3(6) . . . . ?
N1 B1 N5 C9 -93.5(8) . . . . ?
N1 B1 N5 C10 73.4(7) . . . . ?
N1 C2 C3 N2 -0.4(9) . . . . ?
N3 B1 N1 C1 -96.5(9) . . . . ?
N3 B1 N1 C2 76.4(8) . . . . ?
N3 B1 N5 C9 31.9(9) . . . . ?
N3 B1 N5 C10 -161.2(5) . . . . ?
N3 C6 C7 N4 -0.2(8) . . . . ?
N5 B1 N1 C1 29.1(10) . . . . ?
N5 B1 N1 C2 -158.1(6) . . . . ?
N5 B1 N3 C5 -99.3(8) . . . . ?
N5 B1 N3 C6 77.9(7) . . . . ?
N5 C10 C11 N6 -1.4(7) . . . . ?
N7 B2 N9 C17 -26.2(10) . . . . ?
N7 B2 N9 C18 157.8(6) . . . . ?
N7 B2 N11 C21 102.6(8) . . . . ?
N7 B2 N11 C22 -68.0(8) . . . . ?
N7 C14 C15 N8 1.6(9) . . . . ?
N9 B2 N7 C13 96.4(9) . . . . ?
N9 B2 N7 C14 -77.5(8) . . . . ?
N9 B2 N11 C21 -21.6(9) . . . . ?
N9 B2 N11 C22 167.7(5) . . . . ?
N9 C18 C19 N10 0.0(8) . . . . ?
N11 B2 N7 C13 -28.9(11) . . . . ?
N11 B2 N7 C14 157.3(6) . . . . ?
N11 B2 N9 C17 97.8(8) . . . . ?
N11 B2 N9 C18 -78.2(7) . . . . ?
N11 C22 C23 N12 1.1(8) . . . . ?
C1 N1 C2 C3 -0.1(8) . . . . ?
C1 N2 C3 C2 0.8(9) . . . . ?
C2 N1 C1 S1 179.4(6) . . . . ?
C2 N1 C1 N2 0.6(8) . . . . ?
C3 N2 C1 S1 -179.8(6) . . . . ?
C3 N2 C1 N1 -0.8(8) . . . . ?
C4 N2 C1 S1 -1.7(10) . . . . ?
C4 N2 C1 N1 177.3(7) . . . . ?
C4 N2 C3 C2 -177.3(7) . . . . ?
C5 N3 C6 C7 -0.1(8) . . . . ?
C5 N4 C7 C6 0.4(8) . . . . ?
C6 N3 C5 S2 179.2(5) . . . . ?
C6 N3 C5 N4 0.4(7) . . . . ?
C7 N4 C5 S2 -179.4(5) . . . . ?
C7 N4 C5 N3 -0.5(8) . . . . ?
C8 N4 C5 S2 -0.4(10) . . . . ?
C8 N4 C5 N3 178.6(6) . . . . ?
C8 N4 C7 C6 -178.6(6) . . . . ?
C9 N5 C10 C11 0.6(7) . . . . ?
C9 N6 C11 C10 1.6(7) . . . . ?
C10 N5 C9 S3 177.5(5) . . . . ?
C10 N5 C9 N6 0.4(6) . . . . ?
C11 N6 C9 S3 -178.6(4) . . . . ?
C11 N6 C9 N5 -1.2(7) . . . . ?
C12 N6 C9 S3 7.3(8) . . . . ?
C12 N6 C9 N5 -175.4(5) . . . . ?
C12 N6 C11 C10 175.8(6) . . . . ?
C13 N7 C14 C15 -2.0(9) . . . . ?
C13 N8 C15 C14 -0.5(9) . . . . ?
C14 N7 C13 S4 -177.4(6) . . . . ?
C14 N7 C13 N8 1.7(8) . . . . ?
C15 N8 C13 S4 178.4(6) . . . . ?
C15 N8 C13 N7 -0.7(8) . . . . ?
C16 N8 C13 S4 -2.1(11) . . . . ?
C16 N8 C13 N7 178.8(7) . . . . ?
C16 N8 C15 C14 179.9(7) . . . . ?
C17 N9 C18 C19 0.4(8) . . . . ?
C17 N10 C19 C18 -0.4(8) . . . . ?
C18 N9 C17 S5 179.8(6) . . . . ?
C18 N9 C17 N10 -0.7(7) . . . . ?
C19 N10 C17 S5 -179.8(5) . . . . ?
C19 N10 C17 N9 0.7(8) . . . . ?
C20 N10 C17 S5 -0.7(10) . . . . ?
C20 N10 C17 N9 179.8(6) . . . . ?
C20 N10 C19 C18 -179.5(7) . . . . ?
C21 N11 C22 C23 -0.9(7) . . . . ?
C21 N12 C23 C22 -1.0(8) . . . . ?
C22 N11 C21 S6 -178.8(5) . . . . ?
C22 N11 C21 N12 0.2(7) . . . . ?
C23 N12 C21 S6 179.6(5) . . . . ?
C23 N12 C21 N11 0.5(7) . . . . ?
C24 N12 C21 S6 -4.3(9) . . . . ?
C24 N12 C21 N11 176.6(6) . . . . ?
C24 N12 C23 C22 -177.2(6) . . . . ?
Sb2 S7 C25 N13 74.2(6) . . . . ?
Sb2 S7 C25 N14 -107.4(5) . . . . ?
Sb2 S8 C29 N15 74.1(7) . . . . ?
Sb2 S8 C29 N16 -105.5(6) . . . . ?
Sb2 S9 C33 N17 76.0(6) . . . . ?
Sb2 S9 C33 N18 -103.0(6) . . . . ?
B3 N13 C25 S7 -9.5(11) . . . . ?
B3 N13 C25 N14 171.9(6) . . . . ?
B3 N13 C26 C27 -172.3(6) . . . . ?
B3 N15 C29 S8 -5.9(11) . . . . ?
B3 N15 C29 N16 173.9(7) . . . . ?
B3 N15 C30 C31 -174.4(6) . . . . ?
B3 N17 C33 S9 -5.9(12) . . . . ?
B3 N17 C33 N18 173.2(7) . . . . ?
B3 N17 C34 C35 -174.6(6) . . . . ?
N13 B3 N15 C29 27.7(10) . . . . ?
N13 B3 N15 C30 -159.1(6) . . . . ?
N13 B3 N17 C33 -101.2(8) . . . . ?
N13 B3 N17 C34 71.9(8) . . . . ?
N13 C26 C27 N14 -2.0(8) . . . . ?
N15 B3 N13 C25 -96.3(8) . . . . ?
N15 B3 N13 C26 76.6(7) . . . . ?
N15 B3 N17 C33 22.8(11) . . . . ?
N15 B3 N17 C34 -164.1(6) . . . . ?
N15 C30 C31 N16 -0.7(9) . . . . ?
N17 B3 N13 C25 28.3(10) . . . . ?
N17 B3 N13 C26 -158.8(6) . . . . ?
N17 B3 N15 C29 -96.4(9) . . . . ?
N17 B3 N15 C30 76.8(8) . . . . ?
N17 C34 C35 N18 0.1(8) . . . . ?
C25 N13 C26 C27 2.2(8) . . . . ?
C25 N14 C27 C26 1.1(8) . . . . ?
C26 N13 C25 S7 177.0(5) . . . . ?
C26 N13 C25 N14 -1.5(7) . . . . ?
C27 N14 C25 S7 -178.4(5) . . . . ?
C27 N14 C25 N13 0.3(7) . . . . ?
C28 N14 C25 S7 1.5(9) . . . . ?
C28 N14 C25 N13 -179.8(6) . . . . ?
C28 N14 C27 C26 -178.8(6) . . . . ?
C29 N15 C30 C31 0.4(9) . . . . ?
C29 N16 C31 C30 0.8(9) . . . . ?
C30 N15 C29 S8 -179.6(6) . . . . ?
C30 N15 C29 N16 0.1(8) . . . . ?
C31 N16 C29 S8 179.2(5) . . . . ?
C31 N16 C29 N15 -0.5(8) . . . . ?
C32 N16 C29 S8 0.6(11) . . . . ?
C32 N16 C29 N15 -179.2(7) . . . . ?
C32 N16 C31 C30 179.4(7) . . . . ?
C33 N17 C34 C35 0.2(8) . . . . ?
C33 N18 C35 C34 -0.4(8) . . . . ?
C34 N17 C33 S9 -179.5(5) . . . . ?
C34 N17 C33 N18 -0.4(7) . . . . ?
C35 N18 C33 S9 179.7(5) . . . . ?
C35 N18 C33 N17 0.5(8) . . . . ?
C36 N18 C33 S9 2.1(10) . . . . ?
C36 N18 C33 N17 -177.0(6) . . . . ?
C36 N18 C35 C34 177.2(7) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5697(11) 16456 24645 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4303(11) 0 24645 nmt -1.0014 0.1326 -0.0112 0.0065 0.9985 0.0121 0.0066
0.1148 -0.9986
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
0.9998 0.0002 -0.0002 -0.0081 0.0060 -0.0329
-0.9998 -0.0002 0.0002 0.0081 -0.0060 0.0329
-1.9996 -0.0004 -0.9991 0.0301 -0.0612 0.0600
1.9996 0.0004 0.9991 -0.0301 0.0612 -0.0600
0.0035 1.9998 -1.0042 -0.2996 -0.1445 0.0539
0.9962 -1.9996 1.0039 0.2914 0.1504 -0.0868
-0.0000 0.0001 -0.9995 0.0138 -0.0492 -0.0058
0.0000 -0.0001 0.9995 -0.0138 0.0492 0.0058
