#------------------------------------------------------------------------------
#$Date: 2019-11-23 05:53:44 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232276 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/73/4347340.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_4347340
loop_
_publ_author_name
'Bera, Sachinath'
'Mondal, Sandip'
'Maity, Suvendu'
'Weyhermüller, Thomas'
'Ghosh, Prasanta'
_publ_section_title
;
 Radical and Non-Radical States of the [Os(PIQ)] Core (PIQ =
 9,10-Phenanthreneiminoquinone): Iminosemiquinone to Iminoquinone
 Conversion Promoted o-Metalation Reaction.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4746
_journal_page_last               4756
_journal_paper_doi               10.1021/acs.inorgchem.6b00040
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C52 H41 Br3 Cl4 N O Os P2'
_chemical_formula_weight         1329.53
_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
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 118.1180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.3136(11)
_cell_length_b                   9.5495(4)
_cell_length_c                   23.6568(10)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    114(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      2.89
_cell_volume                     4844.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      114(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35971
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.569
_diffrn_reflns_theta_min         2.586
_diffrn_source                   Mo
_exptl_absorpt_coefficient_mu    5.434
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.190
_exptl_transmission_factor_max   0.348
_exptl_transmission_factor_min   0.225
_refine_diff_density_max         2.679
_refine_diff_density_min         -2.062
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         12263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0402
_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)+(0.0079P)²+57.1861P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11073
_reflns_number_total             12263
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            4.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347340
_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_min   0.115
_shelx_estimated_absorpt_t_max   0.425
_shelxl_version_number           2014/6
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
Os1 Os 0.17537(2) 0.65812(2) 0.66321(2) 0.00896(5) Uani 1 1 d . .
Br2 Br 0.07317(2) 0.53515(5) 0.61943(2) 0.01392(9) Uani 1 1 d . .
Br1 Br 0.14264(2) 0.91458(4) 0.64083(2) 0.01500(9) Uani 1 1 d . .
Br3 Br 0.35012(2) 0.07436(5) 0.72835(3) 0.02283(11) Uani 1 1 d . .
P20 P 0.16405(5) 0.63695(11) 0.55653(5) 0.0102(2) Uani 1 1 d . .
P50 P 0.18129(5) 0.69193(12) 0.76677(5) 0.0131(2) Uani 1 1 d . .
N1 N 0.26446(16) 0.7224(4) 0.69735(17) 0.0115(7) Uani 1 1 d . .
H1 H 0.2730 0.8120 0.6977 0.014 Uiso 1 1 calc R U
C4 C 0.22493(19) 0.4756(5) 0.6913(2) 0.0126(8) Uani 1 1 d . .
C3 C 0.2904(2) 0.4893(4) 0.7181(2) 0.0114(8) Uani 1 1 d . .
O16 O 0.38911(17) 0.7882(4) 0.7315(2) 0.0298(9) Uani 1 1 d . .
C2 C 0.3090(2) 0.6306(4) 0.7188(2) 0.0118(8) Uani 1 1 d . .
C6 C 0.2440(2) 0.2251(5) 0.7018(2) 0.0168(9) Uani 1 1 d . .
H6 H 0.2280 0.1325 0.6961 0.020 Uiso 1 1 calc R U
C5 C 0.2032(2) 0.3369(5) 0.6865(2) 0.0154(8) Uani 1 1 d . .
H5 H 0.1602 0.3201 0.6727 0.018 Uiso 1 1 calc R U
C8 C 0.3345(2) 0.3779(5) 0.7379(2) 0.0136(8) Uani 1 1 d . .
C7 C 0.3072(2) 0.2448(4) 0.7250(2) 0.0147(8) Uani 1 1 d . .
C61 C 0.1210(2) 0.8003(5) 0.7716(2) 0.0167(9) Uani 1 1 d . .
C62 C 0.0599(2) 0.7937(5) 0.7220(3) 0.0201(9) Uani 1 1 d . .
H62 H 0.0507 0.7403 0.6847 0.024 Uiso 1 1 calc R U
C15 C 0.3745(2) 0.6694(5) 0.7383(2) 0.0170(9) Uani 1 1 d . .
C51 C 0.1831(2) 0.5377(5) 0.8137(2) 0.0169(9) Uani 1 1 d . .
C21 C 0.1506(2) 0.4569(5) 0.5276(2) 0.0124(8) Uani 1 1 d . .
C26 C 0.0915(2) 0.4121(5) 0.4824(2) 0.0158(9) Uani 1 1 d . .
H26 H 0.0586 0.4780 0.4626 0.019 Uiso 1 1 calc R U
C41 C 0.1019(2) 0.7379(5) 0.4924(2) 0.0140(8) Uani 1 1 d . .
C56 C 0.1505(2) 0.4178(6) 0.7824(2) 0.0214(10) Uani 1 1 d . .
H56 H 0.1279 0.4166 0.7369 0.026 Uiso 1 1 calc R U
C31 C 0.2319(2) 0.6946(5) 0.5487(2) 0.0147(8) Uani 1 1 d . .
C9 C 0.4016(2) 0.4150(5) 0.7686(2) 0.0170(9) Uani 1 1 d . .
C14 C 0.4203(2) 0.5539(5) 0.7665(2) 0.0180(9) Uani 1 1 d . .
C22 C 0.1987(2) 0.3576(5) 0.5559(2) 0.0164(9) Uani 1 1 d . .
H22 H 0.2394 0.3870 0.5863 0.020 Uiso 1 1 calc R U
C46 C 0.1090(2) 0.7835(5) 0.4405(2) 0.0170(9) Uani 1 1 d . .
H46 H 0.1469 0.7649 0.4395 0.020 Uiso 1 1 calc R U
C32 C 0.2554(2) 0.8282(5) 0.5711(2) 0.0189(9) Uani 1 1 d . .
H32 H 0.2375 0.8830 0.5918 0.023 Uiso 1 1 calc R U
C63 C 0.0126(3) 0.8646(6) 0.7268(3) 0.0259(11) Uani 1 1 d . .
H63 H -0.0291 0.8572 0.6934 0.031 Uiso 1 1 calc R U
C66 C 0.1336(3) 0.8792(5) 0.8254(3) 0.0230(10) Uani 1 1 d . .
H66 H 0.1749 0.8831 0.8599 0.028 Uiso 1 1 calc R U
C42 C 0.0465(2) 0.7688(5) 0.4937(2) 0.0196(10) Uani 1 1 d . .
H42 H 0.0411 0.7405 0.5293 0.024 Uiso 1 1 calc R U
C71 C 0.2540(2) 0.7826(7) 0.8174(2) 0.0269(12) Uani 1 1 d . .
C52 C 0.2137(3) 0.5398(6) 0.8804(2) 0.0237(10) Uani 1 1 d . .
H52 H 0.2346 0.6223 0.9026 0.028 Uiso 1 1 calc R U
C23 C 0.1875(2) 0.2180(5) 0.5397(2) 0.0212(10) Uani 1 1 d . .
H23 H 0.2203 0.1518 0.5591 0.025 Uiso 1 1 calc R U
C43 C -0.0007(2) 0.8409(6) 0.4433(3) 0.0232(10) Uani 1 1 d . .
H43 H -0.0385 0.8604 0.4444 0.028 Uiso 1 1 calc R U
C55 C 0.1506(3) 0.2995(6) 0.8168(3) 0.0271(11) Uani 1 1 d . .
H55 H 0.1288 0.2176 0.7951 0.032 Uiso 1 1 calc R U
C33 C 0.3042(2) 0.8818(6) 0.5635(3) 0.0259(11) Uani 1 1 d . .
H33 H 0.3199 0.9727 0.5791 0.031 Uiso 1 1 calc R U
C44 C 0.0063(2) 0.8848(5) 0.3915(2) 0.0209(10) Uani 1 1 d . .
H44 H -0.0262 0.9343 0.3572 0.025 Uiso 1 1 calc R U
C25 C 0.0807(2) 0.2707(5) 0.4663(2) 0.0193(9) Uani 1 1 d . .
H25 H 0.0404 0.2407 0.4352 0.023 Uiso 1 1 calc R U
C13 C 0.4832(2) 0.5897(6) 0.7928(3) 0.0283(12) Uani 1 1 d . .
H13 H 0.4947 0.6833 0.7896 0.034 Uiso 1 1 calc R U
C10 C 0.4489(2) 0.3178(6) 0.8022(3) 0.0274(11) Uani 1 1 d . .
H10 H 0.4383 0.2245 0.8071 0.033 Uiso 1 1 calc R U
C76 C 0.3088(3) 0.7065(9) 0.8504(3) 0.0359(15) Uani 1 1 d . .
H76 H 0.3079 0.6070 0.8499 0.043 Uiso 1 1 calc R U
C45 C 0.0618(2) 0.8556(6) 0.3901(2) 0.0220(10) Uani 1 1 d . .
H45 H 0.0673 0.8850 0.3547 0.026 Uiso 1 1 calc R U
C24 C 0.1283(3) 0.1736(5) 0.4953(3) 0.0228(10) Uani 1 1 d . .
H24 H 0.1205 0.0771 0.4848 0.027 Uiso 1 1 calc R U
C54 C 0.1829(3) 0.3026(6) 0.8833(3) 0.0299(12) Uani 1 1 d . .
H54 H 0.1837 0.2218 0.9071 0.036 Uiso 1 1 calc R U
C36 C 0.2580(2) 0.6168(6) 0.5175(2) 0.0216(10) Uani 1 1 d . .
H36 H 0.2423 0.5261 0.5015 0.026 Uiso 1 1 calc R U
C65 C 0.0860(3) 0.9528(6) 0.8289(3) 0.0302(13) Uani 1 1 d . .
H65 H 0.0951 1.0088 0.8655 0.036 Uiso 1 1 calc R U
C64 C 0.0255(3) 0.9452(6) 0.7795(3) 0.0311(13) Uani 1 1 d . .
H64 H -0.0068 0.9957 0.7822 0.037 Uiso 1 1 calc R U
C53 C 0.2137(3) 0.4217(7) 0.9148(3) 0.0316(13) Uani 1 1 d . .
H53 H 0.2352 0.4235 0.9603 0.038 Uiso 1 1 calc R U
C34 C 0.3306(2) 0.8027(7) 0.5328(3) 0.0290(12) Uani 1 1 d . .
H34 H 0.3645 0.8391 0.5280 0.035 Uiso 1 1 calc R U
C35 C 0.3072(2) 0.6711(7) 0.5096(3) 0.0278(12) Uani 1 1 d . .
H35 H 0.3246 0.6175 0.4881 0.033 Uiso 1 1 calc R U
C72 C 0.2561(3) 0.9292(7) 0.8171(3) 0.0352(15) Uani 1 1 d . .
H72 H 0.2190 0.9819 0.7933 0.042 Uiso 1 1 calc R U
C11 C 0.5114(3) 0.3558(6) 0.8287(3) 0.0332(13) Uani 1 1 d . .
H11 H 0.5428 0.2877 0.8508 0.040 Uiso 1 1 calc R U
C12 C 0.5286(2) 0.4905(7) 0.8233(3) 0.0323(13) Uani 1 1 d . .
H12 H 0.5715 0.5146 0.8405 0.039 Uiso 1 1 calc R U
C75 C 0.3657(3) 0.7784(12) 0.8846(3) 0.055(2) Uani 1 1 d . .
H75 H 0.4034 0.7274 0.9074 0.066 Uiso 1 1 calc R U
C73 C 0.3132(4) 0.9969(9) 0.8522(3) 0.055(2) Uani 1 1 d . .
H73 H 0.3147 1.0963 0.8532 0.066 Uiso 1 1 calc R U
C74 C 0.3667(4) 0.9221(12) 0.8851(4) 0.065(3) Uani 1 1 d . .
H74 H 0.4052 0.9699 0.9086 0.078 Uiso 1 1 calc R U
Cl1 Cl 0.4663(2) 0.5017(8) 0.5789(3) 0.187(3) Uani 1 1 d . .
C16 C 0.4519(12) 0.4559(13) 0.6319(6) 0.190(12) Uani 1 1 d . .
H16A H 0.4430 0.5394 0.6510 0.228 Uiso 1 1 calc R U
H16B H 0.4888 0.4082 0.6659 0.228 Uiso 1 1 calc R U
Cl4 Cl 0.3813(4) 0.3308(7) 0.6001(4) 0.223(4) Uani 1 1 d . .
Cl3 Cl 0.4638(17) 0.087(3) 0.4778(17) 0.75(3) Uiso 1 1 d . .
Cl2 Cl 0.3850(15) 0.165(3) 0.4405(16) 0.661(19) Uiso 1 1 d . .
C17 C 0.403(3) 0.253(8) 0.534(4) 0.59(5) Uiso 1 1 d . .
H17A H 0.3848 0.2059 0.5587 0.711 Uiso 1 1 calc R U
H17B H 0.4133 0.3533 0.5427 0.711 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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
N1 Os1 C4 76.82(16) .
N1 Os1 P50 90.79(10) .
C4 Os1 P50 92.28(12) .
N1 Os1 P20 90.92(10) .
C4 Os1 P20 91.62(12) .
P50 Os1 P20 176.01(4) .
N1 Os1 Br2 169.24(11) .
C4 Os1 Br2 93.03(12) .
P50 Os1 Br2 93.20(3) .
P20 Os1 Br2 85.75(3) .
N1 Os1 Br1 87.84(11) .
C4 Os1 Br1 164.63(12) .
P50 Os1 Br1 86.89(3) .
P20 Os1 Br1 89.58(3) .
Br2 Os1 Br1 102.342(15) .
C21 P20 C31 104.9(2) .
C21 P20 C41 104.7(2) .
C31 P20 C41 100.9(2) .
C21 P20 Os1 112.52(14) .
C31 P20 Os1 114.62(15) .
C41 P20 Os1 117.67(15) .
C71 P50 C51 104.2(2) .
C71 P50 C61 104.3(3) .
C51 P50 C61 101.9(2) .
C71 P50 Os1 107.88(17) .
C51 P50 Os1 118.81(16) .
C61 P50 Os1 118.12(16) .
C2 N1 Os1 119.5(3) .
C2 N1 H1 120.2 .
Os1 N1 H1 120.2 .
C5 C4 C3 115.0(4) .
C5 C4 Os1 129.3(3) .
C3 C4 Os1 115.7(3) .
C4 C3 C2 112.2(4) .
C4 C3 C8 126.3(4) .
C2 C3 C8 121.3(4) .
N1 C2 C3 115.8(4) .
N1 C2 C15 122.0(4) .
C3 C2 C15 122.1(4) .
C7 C6 C5 121.8(4) .
C7 C6 H6 119.1 .
C5 C6 H6 119.1 .
C6 C5 C4 120.5(4) .
C6 C5 H5 119.8 .
C4 C5 H5 119.8 .
C7 C8 C3 113.6(4) .
C7 C8 C9 128.5(4) .
C3 C8 C9 117.8(4) .
C6 C7 C8 122.3(4) .
C6 C7 Br3 112.6(3) .
C8 C7 Br3 124.8(3) .
C66 C61 C62 119.0(5) .
C66 C61 P50 121.7(4) .
C62 C61 P50 119.1(4) .
C63 C62 C61 120.4(5) .
C63 C62 H62 119.8 .
C61 C62 H62 119.8 .
O16 C15 C2 121.9(4) .
O16 C15 C14 123.1(4) .
C2 C15 C14 115.0(4) .
C56 C51 C52 118.8(5) .
C56 C51 P50 119.6(4) .
C52 C51 P50 121.5(4) .
C26 C21 C22 118.9(4) .
C26 C21 P20 121.0(3) .
C22 C21 P20 119.8(3) .
C25 C26 C21 120.0(4) .
C25 C26 H26 120.0 .
C21 C26 H26 120.0 .
C46 C41 C42 118.6(4) .
C46 C41 P20 119.9(3) .
C42 C41 P20 121.5(4) .
C51 C56 C55 120.8(5) .
C51 C56 H56 119.6 .
C55 C56 H56 119.6 .
C36 C31 C32 118.7(4) .
C36 C31 P20 123.5(4) .
C32 C31 P20 117.7(4) .
C10 C9 C14 116.8(4) .
C10 C9 C8 122.7(4) .
C14 C9 C8 120.4(4) .
C13 C14 C9 121.3(4) .
C13 C14 C15 116.8(4) .
C9 C14 C15 121.9(4) .
C23 C22 C21 120.6(4) .
C23 C22 H22 119.7 .
C21 C22 H22 119.7 .
C45 C46 C41 121.2(4) .
C45 C46 H46 119.4 .
C41 C46 H46 119.4 .
C33 C32 C31 120.9(5) .
C33 C32 H32 119.6 .
C31 C32 H32 119.6 .
C64 C63 C62 120.4(5) .
C64 C63 H63 119.8 .
C62 C63 H63 119.8 .
C61 C66 C65 120.0(5) .
C61 C66 H66 120.0 .
C65 C66 H66 120.0 .
C43 C42 C41 120.2(4) .
C43 C42 H42 119.9 .
C41 C42 H42 119.9 .
C76 C71 C72 119.9(6) .
C76 C71 P50 119.8(5) .
C72 C71 P50 119.9(5) .
C53 C52 C51 120.3(5) .
C53 C52 H52 119.9 .
C51 C52 H52 119.9 .
C22 C23 C24 120.3(5) .
C22 C23 H23 119.8 .
C24 C23 H23 119.8 .
C44 C43 C42 121.0(5) .
C44 C43 H43 119.5 .
C42 C43 H43 119.5 .
C54 C55 C56 119.4(5) .
C54 C55 H55 120.3 .
C56 C55 H55 120.3 .
C32 C33 C34 120.1(5) .
C32 C33 H33 120.0 .
C34 C33 H33 120.0 .
C43 C44 C45 119.2(4) .
C43 C44 H44 120.4 .
C45 C44 H44 120.4 .
C24 C25 C26 120.4(5) .
C24 C25 H25 119.8 .
C26 C25 H25 119.8 .
C12 C13 C14 120.4(5) .
C12 C13 H13 119.8 .
C14 C13 H13 119.8 .
C11 C10 C9 120.9(5) .
C11 C10 H10 119.5 .
C9 C10 H10 119.5 .
C71 C76 C75 119.3(8) .
C71 C76 H76 120.4 .
C75 C76 H76 120.4 .
C46 C45 C44 119.8(4) .
C46 C45 H45 120.1 .
C44 C45 H45 120.1 .
C25 C24 C23 119.7(5) .
C25 C24 H24 120.1 .
C23 C24 H24 120.1 .
C53 C54 C55 120.3(5) .
C53 C54 H54 119.8 .
C55 C54 H54 119.8 .
C35 C36 C31 120.4(5) .
C35 C36 H36 119.8 .
C31 C36 H36 119.8 .
C64 C65 C66 120.5(5) .
C64 C65 H65 119.8 .
C66 C65 H65 119.8 .
C63 C64 C65 119.7(5) .
C63 C64 H64 120.2 .
C65 C64 H64 120.2 .
C54 C53 C52 120.3(5) .
C54 C53 H53 119.8 .
C52 C53 H53 119.8 .
C35 C34 C33 119.7(5) .
C35 C34 H34 120.1 .
C33 C34 H34 120.1 .
C34 C35 C36 120.2(5) .
C34 C35 H35 119.9 .
C36 C35 H35 119.9 .
C73 C72 C71 119.2(7) .
C73 C72 H72 120.4 .
C71 C72 H72 120.4 .
C12 C11 C10 121.2(5) .
C12 C11 H11 119.4 .
C10 C11 H11 119.4 .
C13 C12 C11 119.2(5) .
C13 C12 H12 120.4 .
C11 C12 H12 120.4 .
C74 C75 C76 120.1(8) .
C74 C75 H75 119.9 .
C76 C75 H75 119.9 .
C74 C73 C72 120.8(8) .
C74 C73 H73 119.6 .
C72 C73 H73 119.6 .
C73 C74 C75 120.7(7) .
C73 C74 H74 119.6 .
C75 C74 H74 119.6 .
Cl1 C16 Cl4 111.4(9) .
Cl1 C16 H16A 109.3 .
Cl4 C16 H16A 109.3 .
Cl1 C16 H16B 109.3 .
Cl4 C16 H16B 109.3 .
H16A C16 H16B 108.0 .
Cl3 Cl3 C17 130(3) 3_656
Cl2 C17 Cl3 39.8(17) .
Cl2 C17 H17A 119.4 .
Cl3 C17 H17A 119.4 .
Cl2 C17 H17B 119.4 .
Cl3 C17 H17B 119.4 .
H17A C17 H17B 117.0 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os1 N1 2.018(4) .
Os1 C4 2.044(5) .
Os1 P50 2.4072(11) .
Os1 P20 2.4147(11) .
Os1 Br2 2.4900(4) .
Os1 Br1 2.5523(5) .
Br3 C7 1.914(4) .
P20 C21 1.822(5) .
P20 C31 1.829(5) .
P20 C41 1.831(5) .
P50 C71 1.820(5) .
P50 C51 1.833(5) .
P50 C61 1.841(5) .
N1 C2 1.296(5) .
N1 H1 0.8800 .
C4 C5 1.411(6) .
C4 C3 1.415(6) .
C3 C2 1.421(6) .
C3 C8 1.424(6) .
O16 C15 1.221(6) .
C2 C15 1.481(6) .
C6 C7 1.380(6) .
C6 C5 1.384(6) .
C6 H6 0.9500 .
C5 H5 0.9500 .
C8 C7 1.399(6) .
C8 C9 1.483(6) .
C61 C66 1.383(7) .
C61 C62 1.394(7) .
C62 C63 1.386(7) .
C62 H62 0.9500 .
C15 C14 1.484(6) .
C51 C56 1.390(7) .
C51 C52 1.392(7) .
C21 C26 1.394(6) .
C21 C22 1.406(6) .
C26 C25 1.394(7) .
C26 H26 0.9500 .
C41 C46 1.389(6) .
C41 C42 1.393(6) .
C56 C55 1.392(7) .
C56 H56 0.9500 .
C31 C36 1.395(7) .
C31 C32 1.396(7) .
C9 C10 1.399(7) .
C9 C14 1.411(7) .
C14 C13 1.394(7) .
C22 C23 1.378(7) .
C22 H22 0.9500 .
C46 C45 1.387(6) .
C46 H46 0.9500 .
C32 C33 1.380(7) .
C32 H32 0.9500 .
C63 C64 1.370(8) .
C63 H63 0.9500 .
C66 C65 1.390(8) .
C66 H66 0.9500 .
C42 C43 1.387(6) .
C42 H42 0.9500 .
C71 C76 1.390(9) .
C71 C72 1.401(9) .
C52 C53 1.390(8) .
C52 H52 0.9500 .
C23 C24 1.389(8) .
C23 H23 0.9500 .
C43 C44 1.380(7) .
C43 H43 0.9500 .
C55 C54 1.388(8) .
C55 H55 0.9500 .
C33 C34 1.394(9) .
C33 H33 0.9500 .
C44 C45 1.393(7) .
C44 H44 0.9500 .
C25 C24 1.386(7) .
C25 H25 0.9500 .
C13 C12 1.374(8) .
C13 H13 0.9500 .
C10 C11 1.392(8) .
C10 H10 0.9500 .
C76 C75 1.409(9) .
C76 H76 0.9500 .
C45 H45 0.9500 .
C24 H24 0.9500 .
C54 C53 1.373(9) .
C54 H54 0.9500 .
C36 C35 1.394(7) .
C36 H36 0.9500 .
C65 C64 1.383(9) .
C65 H65 0.9500 .
C64 H64 0.9500 .
C53 H53 0.9500 .
C34 C35 1.382(9) .
C34 H34 0.9500 .
C35 H35 0.9500 .
C72 C73 1.396(8) .
C72 H72 0.9500 .
C11 C12 1.376(9) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C75 C74 1.372(15) .
C75 H75 0.9500 .
C73 C74 1.362(14) .
C73 H73 0.9500 .
C74 H74 0.9500 .
Cl1 C16 1.518(16) .
C16 Cl4 1.93(2) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
Cl3 Cl3 2.29(6) 3_656
Cl3 C17 2.88(8) .
Cl2 C17 2.20(7) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
