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#$Date: 2023-08-25 02:00:33 +0300 (Fri, 25 Aug 2023) $
#$Revision: 285867 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/37/7713782.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_7713782
loop_
_publ_author_name
'Lamata, Pilar'
'Beard, Sophie'
'Grasa, Alejandro'
'Viguri, Fernando'
'Ricardo, Rodriguez Martinez'
'López, José A.'
'Lahoz, Fernando J.'
'García-Orduña, Pilar'
'Carmona, Daniel'
_publ_section_title
;
 Molecular hydrogen and water activation by transition metal frustrated
 Lewis pairs containing ruthenium or osmium components: catalytic
 hydrogenation assays
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02339G
_journal_year                    2023
_chemical_formula_moiety         'C32 H37 Cl N2 Os P S, F6 Sb'
_chemical_formula_sum            'C32 H37 Cl F6 N2 Os P S Sb'
_chemical_formula_weight         974.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2023-02-06 deposited with the CCDC.	2023-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                97.1740(10)
_cell_angle_beta                 103.529(2)
_cell_angle_gamma                99.2620(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3781(9)
_cell_length_b                   10.4833(9)
_cell_length_c                   16.9677(15)
_cell_measurement_reflns_used    2936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.345
_cell_measurement_theta_min      2.170
_cell_volume                     1745.8(3)
_computing_cell_refinement       'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.795
_diffrn_measurement_device_type  'Bruker APEX DUO CCD system'
_diffrn_measurement_method       'narrow ω frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0910
_diffrn_reflns_Laue_measured_fraction_full 0.908
_diffrn_reflns_Laue_measured_fraction_max 0.795
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17326
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.247
_diffrn_reflns_theta_min         1.997
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.649
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Absorption correction was carried out with SORTAV program.
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/n-hexane'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.918
_refine_diff_density_min         -1.775
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         8271
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0371
_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)+(0.0186P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6087
_reflns_number_total             8271
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02339g4.cif
_cod_data_source_block           cmpnd_2
_cod_database_code               7713782
_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.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.60496(2) 0.86807(2) 0.36616(2) 0.01574(6) Uani 1 1 d . . . . .
Cl Cl 0.76411(12) 0.98105(13) 0.49255(7) 0.0204(3) Uani 1 1 d . . . . .
S S 0.55157(13) 1.07651(14) 0.33474(8) 0.0201(3) Uani 1 1 d . . . . .
P P 0.78731(13) 0.89351(14) 0.30707(7) 0.0161(3) Uani 1 1 d . . . . .
N1 N 0.7749(4) 1.1902(4) 0.2933(2) 0.0168(10) Uani 1 1 d D . . . .
H1N1 H 0.807(4) 1.227(5) 0.257(2) 0.020 Uiso 1 1 d D U . . .
N2 N 0.5680(4) 1.1955(4) 0.2093(2) 0.0180(10) Uani 1 1 d D . . . .
H1N2 H 0.482(2) 1.183(5) 0.204(3) 0.022 Uiso 1 1 d D U . . .
C1 C 0.3759(5) 0.7980(5) 0.3300(3) 0.0219(12) Uani 1 1 d . . . . .
C2 C 0.4335(5) 0.7289(5) 0.2761(3) 0.0224(13) Uani 1 1 d . . . . .
H2 H 0.4002 0.7242 0.2185 0.027 Uiso 1 1 calc R U . . .
C3 C 0.5409(5) 0.6660(5) 0.3066(3) 0.0206(12) Uani 1 1 d . . . . .
H3 H 0.5829 0.6249 0.2691 0.025 Uiso 1 1 calc R U . . .
C4 C 0.5879(5) 0.6624(5) 0.3916(3) 0.0197(12) Uani 1 1 d . . . . .
C5 C 0.5323(5) 0.7399(5) 0.4462(3) 0.0211(12) Uani 1 1 d . . . . .
H5 H 0.5679 0.7476 0.5039 0.025 Uiso 1 1 calc R U . . .
C6 C 0.4269(5) 0.8044(6) 0.4167(3) 0.0232(13) Uani 1 1 d . . . . .
H6 H 0.3895 0.8521 0.4542 0.028 Uiso 1 1 calc R U . . .
C7 C 0.2643(5) 0.8666(6) 0.2975(3) 0.0302(15) Uani 1 1 d . . . . .
H7A H 0.2773 0.8988 0.2476 0.045 Uiso 1 1 calc R U . . .
H7B H 0.2648 0.9407 0.3391 0.045 Uiso 1 1 calc R U . . .
H7C H 0.1774 0.8052 0.2845 0.045 Uiso 1 1 calc R U . . .
C8 C 0.6921(5) 0.5800(5) 0.4216(3) 0.0236(13) Uani 1 1 d . . . . .
H8 H 0.7554 0.5829 0.3853 0.028 Uiso 1 1 calc R U . . .
C9 C 0.6153(6) 0.4366(6) 0.4090(4) 0.0338(15) Uani 1 1 d . . . . .
H9A H 0.6801 0.3797 0.4243 0.051 Uiso 1 1 calc R U . . .
H9B H 0.5654 0.4081 0.3512 0.051 Uiso 1 1 calc R U . . .
H9C H 0.5519 0.4310 0.4437 0.051 Uiso 1 1 calc R U . . .
C10 C 0.7749(5) 0.6272(6) 0.5086(3) 0.0317(15) Uani 1 1 d . . . . .
H10A H 0.8157 0.7202 0.5153 0.047 Uiso 1 1 calc R U . . .
H10B H 0.8464 0.5764 0.5212 0.047 Uiso 1 1 calc R U . . .
H10C H 0.7167 0.6158 0.5462 0.047 Uiso 1 1 calc R U . . .
C11 C 0.7438(5) 0.8948(5) 0.1965(3) 0.0185(12) Uani 1 1 d . . . . .
C12 C 0.6108(5) 0.8856(5) 0.1520(3) 0.0207(12) Uani 1 1 d . . . . .
H12 H 0.5414 0.8821 0.1800 0.025 Uiso 1 1 calc R U . . .
C13 C 0.5781(6) 0.8814(6) 0.0683(3) 0.0276(14) Uani 1 1 d . . . . .
H13 H 0.4865 0.8737 0.0389 0.033 Uiso 1 1 calc R U . . .
C14 C 0.6784(6) 0.8882(6) 0.0268(3) 0.0320(15) Uani 1 1 d . . . . .
H14 H 0.6555 0.8853 -0.0310 0.038 Uiso 1 1 calc R U . . .
C15 C 0.8123(6) 0.8991(6) 0.0694(3) 0.0295(14) Uani 1 1 d . . . . .
H15 H 0.8810 0.9046 0.0409 0.035 Uiso 1 1 calc R U . . .
C16 C 0.8454(5) 0.9021(5) 0.1537(3) 0.0208(12) Uani 1 1 d . . . . .
H16 H 0.9370 0.9091 0.1829 0.025 Uiso 1 1 calc R U . . .
C17 C 0.8867(5) 0.7652(5) 0.3177(3) 0.0154(11) Uani 1 1 d . . . . .
C18 C 0.8706(5) 0.6628(5) 0.2532(3) 0.0214(12) Uani 1 1 d . . . . .
H18 H 0.8085 0.6602 0.2017 0.026 Uiso 1 1 calc R U . . .
C19 C 0.9452(5) 0.5644(6) 0.2640(3) 0.0262(13) Uani 1 1 d . . . . .
H19 H 0.9337 0.4950 0.2196 0.031 Uiso 1 1 calc R U . . .
C20 C 1.0353(5) 0.5664(6) 0.3380(3) 0.0269(13) Uani 1 1 d . . . . .
H20 H 1.0866 0.4993 0.3447 0.032 Uiso 1 1 calc R U . . .
C21 C 1.0504(5) 0.6664(5) 0.4022(3) 0.0230(13) Uani 1 1 d . . . . .
H21 H 1.1125 0.6682 0.4535 0.028 Uiso 1 1 calc R U . . .
C22 C 0.9757(5) 0.7650(5) 0.3929(3) 0.0193(12) Uani 1 1 d . . . . .
H22 H 0.9855 0.8324 0.4381 0.023 Uiso 1 1 calc R U . . .
C23 C 0.9187(5) 1.0407(5) 0.3504(3) 0.0198(12) Uani 1 1 d . . . . .
H23A H 0.9759 1.0268 0.4029 0.024 Uiso 1 1 calc R U . . .
H23B H 0.9769 1.0528 0.3122 0.024 Uiso 1 1 calc R U . . .
C24 C 0.8655(5) 1.1641(5) 0.3661(3) 0.0173(11) Uani 1 1 d . . . . .
H24A H 0.8169 1.1568 0.4096 0.021 Uiso 1 1 calc R U . . .
H24B H 0.9426 1.2392 0.3867 0.021 Uiso 1 1 calc R U . . .
C25 C 0.6408(5) 1.1581(5) 0.2750(3) 0.0176(11) Uani 1 1 d . . . . .
C26 C 0.6187(5) 1.2754(5) 0.1560(3) 0.0213(12) Uani 1 1 d . . . . .
C27 C 0.5668(5) 1.3882(6) 0.1423(3) 0.0246(13) Uani 1 1 d . . . . .
H27 H 0.5006 1.4120 0.1685 0.029 Uiso 1 1 calc R U . . .
C28 C 0.6137(5) 1.4650(6) 0.0899(3) 0.0293(14) Uani 1 1 d . . . . .
H28 H 0.5775 1.5408 0.0796 0.035 Uiso 1 1 calc R U . . .
C29 C 0.7119(6) 1.4338(6) 0.0523(3) 0.0309(15) Uani 1 1 d . . . . .
C30 C 0.7617(5) 1.3212(6) 0.0666(3) 0.0286(14) Uani 1 1 d . . . . .
H30 H 0.8296 1.2988 0.0415 0.034 Uiso 1 1 calc R U . . .
C31 C 0.7143(5) 1.2405(6) 0.1169(3) 0.0220(12) Uani 1 1 d . . . . .
H31 H 0.7471 1.1622 0.1245 0.026 Uiso 1 1 calc R U . . .
C32 C 0.7668(6) 1.5202(7) -0.0020(4) 0.0461(19) Uani 1 1 d . . . . .
H32A H 0.7119 1.5871 -0.0123 0.069 Uiso 1 1 calc R U . . .
H32B H 0.7634 1.4666 -0.0544 0.069 Uiso 1 1 calc R U . . .
H32C H 0.8606 1.5628 0.0255 0.069 Uiso 1 1 calc R U . . .
Sb Sb 0.84425(3) 0.74652(4) 0.80190(2) 0.02283(10) Uani 1 1 d . . . . .
F1 F 0.9888(3) 0.7226(3) 0.75651(19) 0.0321(8) Uani 1 1 d . . . . .
F2 F 0.7003(3) 0.7751(4) 0.8471(2) 0.0453(10) Uani 1 1 d . . . . .
F3 F 0.9637(4) 0.8119(5) 0.9042(2) 0.0665(13) Uani 1 1 d . . . . .
F4 F 0.7243(4) 0.6817(5) 0.7019(2) 0.0714(14) Uani 1 1 d . . . . .
F5 F 0.8308(4) 0.5786(4) 0.8270(3) 0.0723(14) Uani 1 1 d . . . . .
F6 F 0.8586(4) 0.9140(4) 0.7768(3) 0.0615(12) 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'
N N 0.0061 0.0033 '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'
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'
Cl Cl 0.1484 0.1585 '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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Os C5 67.70(19) . . ?
C3 Os C2 37.59(19) . . ?
C5 Os C2 78.79(19) . . ?
C3 Os C4 37.56(17) . . ?
C5 Os C4 37.78(18) . . ?
C2 Os C4 67.30(18) . . ?
C3 Os C6 79.2(2) . . ?
C5 Os C6 36.74(18) . . ?
C2 Os C6 65.88(19) . . ?
C4 Os C6 67.08(19) . . ?
C3 Os C1 66.6(2) . . ?
C5 Os C1 66.36(18) . . ?
C2 Os C1 36.02(18) . . ?
C4 Os C1 78.91(18) . . ?
C6 Os C1 36.77(17) . . ?
C3 Os P 90.87(13) . . ?
C5 Os P 136.11(14) . . ?
C2 Os P 107.66(14) . . ?
C4 Os P 103.23(13) . . ?
C6 Os P 169.64(15) . . ?
C1 Os P 140.50(14) . . ?
C3 Os Cl 134.51(14) . . ?
C5 Os Cl 83.60(14) . . ?
C2 Os Cl 162.33(12) . . ?
C4 Os Cl 99.37(13) . . ?
C6 Os Cl 98.74(14) . . ?
C1 Os Cl 132.91(14) . . ?
P Os Cl 86.18(4) . . ?
C3 Os S 135.80(14) . . ?
C5 Os S 130.60(14) . . ?
C2 Os S 100.54(14) . . ?
C4 Os S 162.89(13) . . ?
C6 Os S 97.34(14) . . ?
C1 Os S 84.28(14) . . ?
P Os S 91.77(4) . . ?
Cl Os S 89.69(5) . . ?
C25 S Os 117.74(18) . . ?
C17 P C11 103.3(2) . . ?
C17 P C23 101.1(2) . . ?
C11 P C23 104.4(2) . . ?
C17 P Os 114.50(15) . . ?
C11 P Os 115.49(16) . . ?
C23 P Os 116.22(16) . . ?
C25 N1 C24 124.7(4) . . ?
C25 N1 H1N1 115(3) . . ?
C24 N1 H1N1 120(3) . . ?
C25 N2 C26 126.8(4) . . ?
C25 N2 H1N2 116(3) . . ?
C26 N2 H1N2 116(3) . . ?
C2 C1 C6 119.2(5) . . ?
C2 C1 C7 120.3(5) . . ?
C6 C1 C7 120.5(5) . . ?
C2 C1 Os 69.9(3) . . ?
C6 C1 Os 70.6(3) . . ?
C7 C1 Os 131.0(4) . . ?
C1 C2 C3 120.5(5) . . ?
C1 C2 Os 74.1(3) . . ?
C3 C2 Os 68.4(3) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
Os C2 H2 130.3 . . ?
C2 C3 C4 121.9(5) . . ?
C2 C3 Os 74.0(3) . . ?
C4 C3 Os 74.4(3) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
Os C3 H3 124.2 . . ?
C3 C4 C5 116.4(5) . . ?
C3 C4 C8 120.7(5) . . ?
C5 C4 C8 122.9(4) . . ?
C3 C4 Os 68.1(3) . . ?
C5 C4 Os 69.6(3) . . ?
C8 C4 Os 133.2(3) . . ?
C6 C5 C4 121.8(5) . . ?
C6 C5 Os 73.8(3) . . ?
C4 C5 Os 72.6(3) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
Os C5 H5 126.4 . . ?
C5 C6 C1 119.8(5) . . ?
C5 C6 Os 69.4(3) . . ?
C1 C6 Os 72.7(3) . . ?
C5 C6 H6 120.1 . . ?
C1 C6 H6 120.1 . . ?
Os C6 H6 130.4 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C4 114.2(5) . . ?
C10 C8 C9 111.8(4) . . ?
C4 C8 C9 107.3(4) . . ?
C10 C8 H8 107.8 . . ?
C4 C8 H8 107.8 . . ?
C9 C8 H8 107.8 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 118.3(4) . . ?
C12 C11 P 121.5(4) . . ?
C16 C11 P 120.2(4) . . ?
C13 C12 C11 121.2(5) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 120.1(5) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C15 120.3(5) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 119.8(5) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C11 120.4(5) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
C22 C17 C18 118.8(5) . . ?
C22 C17 P 119.7(4) . . ?
C18 C17 P 121.5(4) . . ?
C19 C18 C17 120.1(5) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C20 C19 C18 120.8(5) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 119.3(5) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C20 C21 C22 120.7(5) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C17 C22 C21 120.3(5) . . ?
C17 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 P 114.3(3) . . ?
C24 C23 H23A 108.7 . . ?
P C23 H23A 108.7 . . ?
C24 C23 H23B 108.7 . . ?
P C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
N1 C24 C23 113.0(4) . . ?
N1 C24 H24A 109.0 . . ?
C23 C24 H24A 109.0 . . ?
N1 C24 H24B 109.0 . . ?
C23 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
N1 C25 N2 119.2(4) . . ?
N1 C25 S 124.0(3) . . ?
N2 C25 S 116.8(4) . . ?
C31 C26 C27 120.2(5) . . ?
C31 C26 N2 121.1(5) . . ?
C27 C26 N2 118.6(5) . . ?
C28 C27 C26 119.0(5) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C29 C28 C27 121.6(5) . . ?
C29 C28 H28 119.2 . . ?
C27 C28 H28 119.2 . . ?
C28 C29 C30 118.4(5) . . ?
C28 C29 C32 121.5(6) . . ?
C30 C29 C32 120.1(6) . . ?
C31 C30 C29 121.4(5) . . ?
C31 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
C26 C31 C30 119.3(5) . . ?
C26 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
F4 Sb F6 90.3(2) . . ?
F4 Sb F5 89.8(2) . . ?
F6 Sb F5 179.70(16) . . ?
F4 Sb F3 179.05(16) . . ?
F6 Sb F3 90.0(2) . . ?
F5 Sb F3 89.9(2) . . ?
F4 Sb F1 90.41(15) . . ?
F6 Sb F1 89.60(14) . . ?
F5 Sb F1 90.11(15) . . ?
F3 Sb F1 90.50(15) . . ?
F4 Sb F2 89.83(16) . . ?
F6 Sb F2 88.93(16) . . ?
F5 Sb F2 91.35(16) . . ?
F3 Sb F2 89.27(15) . . ?
F1 Sb F2 178.52(15) . . ?
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
Os C3 2.156(5) . ?
Os C5 2.197(4) . ?
Os C2 2.228(5) . ?
Os C4 2.238(5) . ?
Os C6 2.255(4) . ?
Os C1 2.282(5) . ?
Os P 2.3345(12) . ?
Os Cl 2.4101(13) . ?
Os S 2.4308(13) . ?
S C25 1.737(5) . ?
P C17 1.823(5) . ?
P C11 1.826(5) . ?
P C23 1.831(5) . ?
N1 C25 1.329(6) . ?
N1 C24 1.452(6) . ?
N1 H1N1 0.867(19) . ?
N2 C25 1.333(6) . ?
N2 C26 1.438(6) . ?
N2 H1N2 0.863(19) . ?
C1 C2 1.395(7) . ?
C1 C6 1.431(7) . ?
C1 C7 1.494(7) . ?
C2 C3 1.414(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.417(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.436(7) . ?
C4 C8 1.526(7) . ?
C5 C6 1.404(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.500(7) . ?
C8 C9 1.548(7) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.391(7) . ?
C11 C16 1.410(6) . ?
C12 C13 1.375(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.389(6) . ?
C17 C18 1.394(7) . ?
C18 C19 1.391(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.375(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.376(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.392(7) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.504(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 C31 1.387(7) . ?
C26 C27 1.399(7) . ?
C27 C28 1.390(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.383(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.389(8) . ?
C29 C32 1.510(7) . ?
C30 C31 1.389(7) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
Sb F4 1.828(4) . ?
Sb F6 1.849(4) . ?
Sb F5 1.853(4) . ?
Sb F3 1.856(4) . ?
Sb F1 1.876(3) . ?
Sb F2 1.879(3) . ?
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
C6 C1 C2 C3 -0.1(7) . . . . ?
C7 C1 C2 C3 178.8(5) . . . . ?
Os C1 C2 C3 52.3(4) . . . . ?
C6 C1 C2 Os -52.4(4) . . . . ?
C7 C1 C2 Os 126.5(5) . . . . ?
C1 C2 C3 C4 4.5(8) . . . . ?
Os C2 C3 C4 59.4(4) . . . . ?
C1 C2 C3 Os -54.9(5) . . . . ?
C2 C3 C4 C5 -7.5(7) . . . . ?
Os C3 C4 C5 51.7(4) . . . . ?
C2 C3 C4 C8 172.5(5) . . . . ?
Os C3 C4 C8 -128.2(5) . . . . ?
C2 C3 C4 Os -59.2(4) . . . . ?
C3 C4 C5 C6 6.6(7) . . . . ?
C8 C4 C5 C6 -173.5(5) . . . . ?
Os C4 C5 C6 57.5(4) . . . . ?
C3 C4 C5 Os -51.0(4) . . . . ?
C8 C4 C5 Os 129.0(5) . . . . ?
C4 C5 C6 C1 -2.5(8) . . . . ?
Os C5 C6 C1 54.4(4) . . . . ?
C4 C5 C6 Os -57.0(4) . . . . ?
C2 C1 C6 C5 -0.9(7) . . . . ?
C7 C1 C6 C5 -179.7(5) . . . . ?
Os C1 C6 C5 -52.9(4) . . . . ?
C2 C1 C6 Os 52.1(4) . . . . ?
C7 C1 C6 Os -126.8(5) . . . . ?
C3 C4 C8 C10 154.9(5) . . . . ?
C5 C4 C8 C10 -25.0(7) . . . . ?
Os C4 C8 C10 67.2(6) . . . . ?
C3 C4 C8 C9 -80.5(6) . . . . ?
C5 C4 C8 C9 99.5(6) . . . . ?
Os C4 C8 C9 -168.3(4) . . . . ?
C17 P C11 C12 127.8(5) . . . . ?
C23 P C11 C12 -126.8(5) . . . . ?
Os P C11 C12 2.0(5) . . . . ?
C17 P C11 C16 -50.6(5) . . . . ?
C23 P C11 C16 54.8(5) . . . . ?
Os P C11 C16 -176.4(4) . . . . ?
C16 C11 C12 C13 1.1(8) . . . . ?
P C11 C12 C13 -177.4(4) . . . . ?
C11 C12 C13 C14 -0.9(8) . . . . ?
C12 C13 C14 C15 0.1(9) . . . . ?
C13 C14 C15 C16 0.6(9) . . . . ?
C14 C15 C16 C11 -0.4(8) . . . . ?
C12 C11 C16 C15 -0.4(8) . . . . ?
P C11 C16 C15 178.0(4) . . . . ?
C11 P C17 C22 157.7(4) . . . . ?
C23 P C17 C22 49.9(4) . . . . ?
Os P C17 C22 -75.8(4) . . . . ?
C11 P C17 C18 -25.6(5) . . . . ?
C23 P C17 C18 -133.5(4) . . . . ?
Os P C17 C18 100.8(4) . . . . ?
C22 C17 C18 C19 -1.5(7) . . . . ?
P C17 C18 C19 -178.2(4) . . . . ?
C17 C18 C19 C20 0.1(8) . . . . ?
C18 C19 C20 C21 0.7(9) . . . . ?
C19 C20 C21 C22 0.0(8) . . . . ?
C18 C17 C22 C21 2.2(7) . . . . ?
P C17 C22 C21 178.9(4) . . . . ?
C20 C21 C22 C17 -1.4(8) . . . . ?
C17 P C23 C24 -168.5(3) . . . . ?
C11 P C23 C24 84.5(4) . . . . ?
Os P C23 C24 -43.9(4) . . . . ?
C25 N1 C24 C23 96.6(6) . . . . ?
P C23 C24 N1 -55.8(5) . . . . ?
C24 N1 C25 N2 175.3(5) . . . . ?
C24 N1 C25 S -1.2(8) . . . . ?
C26 N2 C25 N1 -3.6(8) . . . . ?
C26 N2 C25 S 173.1(4) . . . . ?
Os S C25 N1 -55.3(5) . . . . ?
Os S C25 N2 128.2(4) . . . . ?
C25 N2 C26 C31 55.9(8) . . . . ?
C25 N2 C26 C27 -125.7(6) . . . . ?
C31 C26 C27 C28 -0.7(8) . . . . ?
N2 C26 C27 C28 -179.0(5) . . . . ?
C26 C27 C28 C29 -1.2(8) . . . . ?
C27 C28 C29 C30 1.4(8) . . . . ?
C27 C28 C29 C32 -177.6(6) . . . . ?
C28 C29 C30 C31 0.4(8) . . . . ?
C32 C29 C30 C31 179.3(5) . . . . ?
C27 C26 C31 C30 2.4(8) . . . . ?
N2 C26 C31 C30 -179.3(5) . . . . ?
C29 C30 C31 C26 -2.3(8) . . . . ?
