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#$Date: 2025-10-04 21:44:59 +0300 (Sat, 04 Oct 2025) $
#$Revision: 302373 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/95/7719552.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_7719552
loop_
_publ_author_name
'Wang, Lei'
'Wang, Li-Xin'
'Liu, Zhao-Long'
'Xu, Fang'
'Qi, Rui-Yue'
'Man, Wai-Lun'
'Xiang, Jing'
'Liu, Ji-Yan'
'Lau, Tai-Chu'
_publ_section_title
;
 Reaction of an osmium(VI) nitrido complex with enamines generated in
 situ from ketones and anilines.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14052
_journal_page_last               14058
_journal_paper_doi               10.1039/d5dt01334h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C65 H63 Cl4 N8 O4.5 Os P'
_chemical_formula_weight         1391.20
_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   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-11-16 deposited with the CCDC.	2025-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                99.594(3)
_cell_angle_beta                 106.007(2)
_cell_angle_gamma                106.386(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8010(8)
_cell_length_b                   16.1249(10)
_cell_length_c                   17.2027(12)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.36
_cell_volume                     3157.4(4)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Apex3'
_computing_data_reduction        'Bruker Saint'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48301
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.375
_diffrn_reflns_theta_min         2.357
_diffrn_source                   'micro focus'
_exptl_absorpt_coefficient_mu    2.268
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.258
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         12890
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0482P)²+2.6795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11266
_reflns_number_total             12890
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt01334h2.cif
_cod_data_source_block           1_a
_cod_original_formula_sum        'C65 H63 Cl4 N8 O4.50 Os P'
_cod_database_code               7719552
_shelx_shelxl_version_number     2016/6
_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.
;
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
O5_1 O -0.010(2) 0.9995(15) 0.5050(12) 0.108(3) Uiso 0.5 1 d D U P A -1
C64_1 C 0.0659(16) 1.0842(13) 0.5729(13) 0.138(7) Uiso 0.5 1 d D U P A -1
H64A_1 H 0.092095 1.134581 0.549724 0.165 Uiso 0.5 1 calc R U P A -1
H64B_1 H 0.133100 1.076162 0.610576 0.165 Uiso 0.5 1 calc R U P A -1
C65_1 C -0.023(2) 1.0968(16) 0.6182(14) 0.152(9) Uiso 0.5 1 d D U P A -1
H65A_1 H -0.009141 1.160191 0.637550 0.229 Uiso 0.5 1 calc R U P A -1
H65B_1 H -0.011881 1.071221 0.665802 0.229 Uiso 0.5 1 calc R U P A -1
H65C_1 H -0.101126 1.066705 0.579177 0.229 Uiso 0.5 1 calc R U P A -1
C66_1 C 0.0456(16) 0.9769(13) 0.4408(12) 0.142(7) Uiso 0.5 1 d D U P A -1
H66A_1 H 0.117575 0.967072 0.467735 0.170 Uiso 0.5 1 calc R U P A -1
H66B_1 H 0.063767 1.026149 0.414520 0.170 Uiso 0.5 1 calc R U P A -1
C67_1 C -0.0422(15) 0.8911(11) 0.3746(10) 0.099(5) Uiso 0.5 1 d D U P A -1
H67A_1 H -0.006259 0.870013 0.336412 0.149 Uiso 0.5 1 calc R U P A -1
H67B_1 H -0.108848 0.903892 0.343519 0.149 Uiso 0.5 1 calc R U P A -1
H67C_1 H -0.066935 0.845292 0.402315 0.149 Uiso 0.5 1 calc R U P A -1
Os1 Os 0.38788(2) 0.63947(2) 0.59024(2) 0.02893(6) Uani 1 1 d . . . . .
O1 O 0.3253(2) 0.71879(18) 0.52227(18) 0.0397(6) Uani 1 1 d . . . . .
O2 O 0.0614(2) 0.46964(18) 0.41045(17) 0.0387(6) Uani 1 1 d . . . . .
O3 O 0.0018(5) 0.5528(3) 0.1482(3) 0.116(2) Uani 1 1 d . . . . .
O4 O 0.0619(4) 0.6929(3) 0.1530(3) 0.0858(13) Uani 1 1 d . . . . .
N1 N 0.2722(3) 0.6793(3) 0.7288(2) 0.0498(9) Uani 1 1 d . . . . .
N2 N 0.6007(3) 0.8113(3) 0.7039(3) 0.0536(10) Uani 1 1 d . . . . .
N3 N 0.5164(4) 0.5971(3) 0.4608(2) 0.0484(9) Uani 1 1 d . . . . .
N4 N 0.4591(3) 0.5580(2) 0.64857(19) 0.0313(7) Uani 1 1 d . . . . .
H4 H 0.455667 0.510475 0.614009 0.038 Uiso 1 1 calc R U . . .
N5 N 0.5111(3) 0.6257(2) 0.7893(2) 0.0375(8) Uani 1 1 d . . . . .
H5 H 0.474719 0.661975 0.775013 0.045 Uiso 1 1 calc R U . . .
N6 N 0.5110(3) 0.4379(2) 0.7801(2) 0.0386(8) Uani 1 1 d . . . . .
N7 N 0.2301(3) 0.5351(2) 0.51557(19) 0.0308(7) Uani 1 1 d . . . . .
N8 N 0.0608(5) 0.6315(4) 0.1859(3) 0.0723(14) Uani 1 1 d . . . . .
C1 C 0.3108(3) 0.6655(3) 0.6779(2) 0.0345(9) Uani 1 1 d . . . . .
C2 C 0.5248(4) 0.7483(3) 0.6614(3) 0.0373(9) Uani 1 1 d . . . . .
C3 C 0.4672(3) 0.6125(3) 0.5042(2) 0.0342(8) Uani 1 1 d . . . . .
C4 C 0.5089(3) 0.5629(2) 0.7274(2) 0.0297(8) Uani 1 1 d . . . . .
C5 C 0.5628(3) 0.4940(3) 0.7480(2) 0.0328(8) Uani 1 1 d . . . . .
C6 C 0.6672(4) 0.4959(3) 0.7235(3) 0.0456(10) Uani 1 1 d . . . . .
H6A H 0.655034 0.505996 0.668174 0.068 Uiso 1 1 calc R U . . .
H6B H 0.679277 0.439100 0.722807 0.068 Uiso 1 1 calc R U . . .
H6C H 0.734846 0.543950 0.763798 0.068 Uiso 1 1 calc R U . . .
C7 C 0.1638(3) 0.4602(2) 0.5351(2) 0.0320(8) Uani 1 1 d . . . . .
C8 C 0.1848(4) 0.4269(3) 0.6044(3) 0.0443(10) Uani 1 1 d . . . . .
H8 H 0.254399 0.453649 0.650161 0.053 Uiso 1 1 calc R U . . .
C9 C 0.0984(4) 0.3522(3) 0.6029(3) 0.0497(11) Uani 1 1 d . . . . .
H9 H 0.109313 0.327499 0.649016 0.060 Uiso 1 1 calc R U . . .
C10 C -0.0040(4) 0.3124(3) 0.5353(3) 0.0517(12) Uani 1 1 d . . . . .
H10 H -0.060047 0.261039 0.536873 0.062 Uiso 1 1 calc R U . . .
C11 C -0.0268(4) 0.3451(3) 0.4659(3) 0.0464(11) Uani 1 1 d . . . . .
H11 H -0.096212 0.318346 0.419899 0.056 Uiso 1 1 calc R U . . .
C12 C 0.0611(3) 0.4209(3) 0.4692(3) 0.0372(9) Uani 1 1 d . . . . .
C13 C 0.1647(3) 0.5373(2) 0.4433(2) 0.0334(8) Uani 1 1 d . . . . .
C14 C 0.1869(4) 0.6053(3) 0.3985(3) 0.0369(9) Uani 1 1 d . . . . .
C15 C 0.1199(4) 0.5859(3) 0.3145(3) 0.0430(10) Uani 1 1 d . . . . .
H15 H 0.066410 0.527965 0.286127 0.052 Uiso 1 1 calc R U . . .
C16 C 0.1327(5) 0.6522(4) 0.2733(3) 0.0533(12) Uani 1 1 d . . . . .
C17 C 0.2102(5) 0.7385(4) 0.3143(3) 0.0572(13) Uani 1 1 d . . . . .
H17 H 0.218145 0.783043 0.285143 0.069 Uiso 1 1 calc R U . . .
C18 C 0.2745(4) 0.7584(3) 0.3967(3) 0.0523(12) Uani 1 1 d . . . . .
H18 H 0.326046 0.817183 0.424089 0.063 Uiso 1 1 calc R U . . .
C19 C 0.2662(4) 0.6933(3) 0.4424(3) 0.0391(9) Uani 1 1 d . . . . .
C20 C 0.5676(4) 0.6395(3) 0.8775(2) 0.0360(9) Uani 1 1 d . . . . .
C21 C 0.6853(4) 0.6875(3) 0.9140(3) 0.0400(9) Uani 1 1 d . . . . .
C22 C 0.7367(4) 0.7001(3) 0.9993(3) 0.0460(11) Uani 1 1 d . . . . .
H22 H 0.816991 0.730678 1.024525 0.055 Uiso 1 1 calc R U . . .
C23 C 0.6733(4) 0.6690(3) 1.0487(3) 0.0466(11) Uani 1 1 d . . . . .
C24 C 0.5558(4) 0.6235(3) 1.0102(3) 0.0506(11) Uani 1 1 d . . . . .
H24 H 0.511613 0.602548 1.042954 0.061 Uiso 1 1 calc R U . . .
C25 C 0.5004(4) 0.6076(3) 0.9245(3) 0.0425(10) Uani 1 1 d . . . . .
C26 C 0.7566(5) 0.7300(4) 0.8651(3) 0.0623(14) Uani 1 1 d . . . . .
H26A H 0.815421 0.786149 0.900933 0.093 Uiso 1 1 calc R U . . .
H26B H 0.706723 0.741186 0.817351 0.093 Uiso 1 1 calc R U . . .
H26C H 0.793464 0.689861 0.845611 0.093 Uiso 1 1 calc R U . . .
C27 C 0.7313(5) 0.6866(4) 1.1422(3) 0.0744(18) Uani 1 1 d . . . . .
H27A H 0.684758 0.642938 1.162889 0.112 Uiso 1 1 calc R U . . .
H27B H 0.738935 0.746426 1.170315 0.112 Uiso 1 1 calc R U . . .
H27C H 0.807491 0.681528 1.153270 0.112 Uiso 1 1 calc R U . . .
C28 C 0.3723(4) 0.5593(4) 0.8845(4) 0.0626(14) Uani 1 1 d . . . . .
H28A H 0.341344 0.537332 0.925622 0.094 Uiso 1 1 calc R U . . .
H28B H 0.357192 0.509178 0.838054 0.094 Uiso 1 1 calc R U . . .
H28C H 0.335396 0.600115 0.864049 0.094 Uiso 1 1 calc R U . . .
C29 C 0.5492(4) 0.3649(3) 0.7956(3) 0.0410(9) Uani 1 1 d . . . . .
C30 C 0.6476(4) 0.3769(3) 0.8632(3) 0.0456(10) Uani 1 1 d . . . . .
C31 C 0.6716(4) 0.3009(4) 0.8772(3) 0.0547(12) Uani 1 1 d . . . . .
H31 H 0.736954 0.307789 0.922784 0.066 Uiso 1 1 calc R U . . .
C32 C 0.6036(5) 0.2154(3) 0.8270(4) 0.0553(12) Uani 1 1 d . . . . .
C33 C 0.5070(5) 0.2057(3) 0.7606(3) 0.0550(12) Uani 1 1 d . . . . .
H33 H 0.459991 0.147865 0.726369 0.066 Uiso 1 1 calc R U . . .
C34 C 0.4768(4) 0.2792(3) 0.7426(3) 0.0475(11) Uani 1 1 d . . . . .
C35 C 0.7242(4) 0.4676(3) 0.9205(3) 0.0596(13) Uani 1 1 d . . . . .
H35A H 0.770397 0.460814 0.972577 0.089 Uiso 1 1 calc R U . . .
H35B H 0.676844 0.502205 0.932185 0.089 Uiso 1 1 calc R U . . .
H35C H 0.775058 0.498464 0.893760 0.089 Uiso 1 1 calc R U . . .
C36 C 0.6348(5) 0.1348(4) 0.8455(4) 0.0757(17) Uani 1 1 d . . . . .
H36A H 0.603802 0.086820 0.794232 0.114 Uiso 1 1 calc R U . . .
H36B H 0.602194 0.114698 0.886534 0.114 Uiso 1 1 calc R U . . .
H36C H 0.718423 0.151600 0.867500 0.114 Uiso 1 1 calc R U . . .
C37 C 0.3741(4) 0.2678(3) 0.6700(3) 0.0608(14) Uani 1 1 d . . . . .
H37A H 0.326997 0.204770 0.647652 0.091 Uiso 1 1 calc R U . . .
H37B H 0.399441 0.290122 0.626858 0.091 Uiso 1 1 calc R U . . .
H37C H 0.328790 0.301148 0.688004 0.091 Uiso 1 1 calc R U . . .
P1 P 0.18849(9) 0.94794(7) 0.86974(6) 0.0336(2) Uani 1 1 d . . . . .
C38 C 0.1458(4) 0.8423(3) 0.8951(3) 0.0391(9) Uani 1 1 d . . . . .
C39 C 0.0934(4) 0.8335(3) 0.9562(3) 0.0498(11) Uani 1 1 d . . . . .
H39 H 0.081895 0.882966 0.985268 0.060 Uiso 1 1 calc R U . . .
C40 C 0.0590(4) 0.7514(4) 0.9733(3) 0.0585(13) Uani 1 1 d . . . . .
H40 H 0.024794 0.745295 1.014869 0.070 Uiso 1 1 calc R U . . .
C41 C 0.0742(4) 0.6787(4) 0.9301(4) 0.0618(14) Uani 1 1 d . . . . .
H41 H 0.049966 0.623036 0.942151 0.074 Uiso 1 1 calc R U . . .
C42 C 0.1243(4) 0.6864(3) 0.8696(4) 0.0580(13) Uani 1 1 d . . . . .
H42 H 0.133847 0.636211 0.839917 0.070 Uiso 1 1 calc R U . . .
C43 C 0.1609(4) 0.7686(3) 0.8524(3) 0.0464(10) Uani 1 1 d . . . . .
H43 H 0.196161 0.774128 0.811364 0.056 Uiso 1 1 calc R U . . .
C44 C 0.2256(4) 0.9318(3) 0.7766(3) 0.0374(9) Uani 1 1 d . . . . .
C45 C 0.3281(4) 0.9194(3) 0.7798(3) 0.0516(11) Uani 1 1 d . . . . .
H45 H 0.381643 0.923384 0.831430 0.062 Uiso 1 1 calc R U . . .
C46 C 0.3527(5) 0.9008(3) 0.7063(4) 0.0587(13) Uani 1 1 d . . . . .
H46 H 0.422935 0.892179 0.708236 0.070 Uiso 1 1 calc R U . . .
C47 C 0.2756(6) 0.8952(4) 0.6320(4) 0.0733(17) Uani 1 1 d . . . . .
H47 H 0.293108 0.884167 0.582508 0.088 Uiso 1 1 calc R U . . .
C48 C 0.1730(6) 0.9054(6) 0.6290(4) 0.096(2) Uani 1 1 d . . . . .
H48 H 0.118964 0.899285 0.576768 0.115 Uiso 1 1 calc R U . . .
C49 C 0.1462(5) 0.9248(4) 0.7010(3) 0.0662(15) Uani 1 1 d . . . . .
H49 H 0.075555 0.932891 0.698262 0.079 Uiso 1 1 calc R U . . .
C50 C 0.0679(3) 0.9875(3) 0.8521(2) 0.0357(9) Uani 1 1 d . . . . .
C51 C 0.0897(4) 1.0791(3) 0.8653(3) 0.0510(12) Uani 1 1 d . . . . .
H51 H 0.166114 1.120019 0.887909 0.061 Uiso 1 1 calc R U . . .
C52 C -0.0031(4) 1.1089(3) 0.8444(4) 0.0639(15) Uani 1 1 d . . . . .
H52 H 0.010433 1.170631 0.852072 0.077 Uiso 1 1 calc R U . . .
C53 C -0.1133(4) 1.0501(4) 0.8129(3) 0.0627(14) Uani 1 1 d . . . . .
H53 H -0.175368 1.071460 0.799825 0.075 Uiso 1 1 calc R U . . .
C54 C -0.1352(4) 0.9597(4) 0.8000(4) 0.0614(14) Uani 1 1 d . . . . .
H54 H -0.211976 0.919355 0.778285 0.074 Uiso 1 1 calc R U . . .
C55 C -0.0441(4) 0.9282(3) 0.8192(3) 0.0494(11) Uani 1 1 d . . . . .
H55 H -0.058587 0.866231 0.809656 0.059 Uiso 1 1 calc R U . . .
C56 C 0.3100(3) 1.0315(3) 0.9527(3) 0.0388(9) Uani 1 1 d . . . . .
C57 C 0.3202(4) 1.0372(3) 1.0364(3) 0.0521(11) Uani 1 1 d . . . . .
H57 H 0.266496 0.993970 1.049898 0.063 Uiso 1 1 calc R U . . .
C58 C 0.4081(5) 1.1055(4) 1.0990(3) 0.0621(14) Uani 1 1 d . . . . .
H58 H 0.413587 1.109546 1.155255 0.075 Uiso 1 1 calc R U . . .
C59 C 0.4882(5) 1.1679(3) 1.0801(3) 0.0621(15) Uani 1 1 d . . . . .
H59 H 0.550236 1.213071 1.123550 0.075 Uiso 1 1 calc R U . . .
C60 C 0.4784(4) 1.1649(3) 0.9984(4) 0.0634(14) Uani 1 1 d . . . . .
H60 H 0.532041 1.209013 0.985794 0.076 Uiso 1 1 calc R U . . .
C61 C 0.3898(4) 1.0970(3) 0.9344(3) 0.0549(12) Uani 1 1 d . . . . .
H61 H 0.383212 1.095063 0.878266 0.066 Uiso 1 1 calc R U . . .
Cl1 Cl 0.6346(7) 0.9408(5) 0.4813(4) 0.359(4) Uani 1 1 d . . . . .
Cl2 Cl 0.6052(4) 1.0061(2) 0.6309(3) 0.2156(18) Uani 1 1 d . . . . .
C62 C 0.6093(12) 0.9177(7) 0.5607(7) 0.160(4) Uani 1 1 d . . . . .
H62A H 0.669042 0.895896 0.589993 0.192 Uiso 1 1 calc R U . . .
H62B H 0.534711 0.868642 0.542171 0.192 Uiso 1 1 calc R U . . .
Cl3 Cl 0.8252(2) 0.7963(2) 0.56965(16) 0.1425(10) Uani 1 1 d . . . . .
Cl4 Cl 0.87873(17) 0.69488(12) 0.68977(13) 0.0934(5) Uani 1 1 d . . . . .
C63 C 0.7734(6) 0.7045(5) 0.6187(6) 0.113(3) Uani 1 1 d . . . . .
H63A H 0.717714 0.716941 0.643946 0.136 Uiso 1 1 calc R U . . .
H63B H 0.733429 0.647567 0.575100 0.136 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'
Os Os -1.2165 7.6030 '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'
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
C64_1 O5_1 C66_1 112.5(17) . . ?
O5_1 C64_1 C65_1 99.8(14) . . ?
O5_1 C64_1 H64A_1 111.8 . . ?
C65_1 C64_1 H64A_1 111.8 . . ?
O5_1 C64_1 H64B_1 111.8 . . ?
C65_1 C64_1 H64B_1 111.8 . . ?
H64A_1 C64_1 H64B_1 109.5 . . ?
C64_1 C65_1 H65A_1 109.5 . . ?
C64_1 C65_1 H65B_1 109.5 . . ?
H65A_1 C65_1 H65B_1 109.5 . . ?
C64_1 C65_1 H65C_1 109.5 . . ?
H65A_1 C65_1 H65C_1 109.5 . . ?
H65B_1 C65_1 H65C_1 109.5 . . ?
O5_1 C66_1 C67_1 106.8(15) . . ?
O5_1 C66_1 H66A_1 110.4 . . ?
C67_1 C66_1 H66A_1 110.4 . . ?
O5_1 C66_1 H66B_1 110.4 . . ?
C67_1 C66_1 H66B_1 110.4 . . ?
H66A_1 C66_1 H66B_1 108.6 . . ?
C66_1 C67_1 H67A_1 109.5 . . ?
C66_1 C67_1 H67B_1 109.5 . . ?
H67A_1 C67_1 H67B_1 109.5 . . ?
C66_1 C67_1 H67C_1 109.5 . . ?
H67A_1 C67_1 H67C_1 109.5 . . ?
H67B_1 C67_1 H67C_1 109.5 . . ?
C2 Os1 N4 91.38(15) . . ?
C2 Os1 O1 88.75(14) . . ?
N4 Os1 O1 173.64(11) . . ?
C2 Os1 C1 87.06(15) . . ?
N4 Os1 C1 93.51(14) . . ?
O1 Os1 C1 92.85(14) . . ?
C2 Os1 C3 92.61(16) . . ?
N4 Os1 C3 85.38(14) . . ?
O1 Os1 C3 88.26(14) . . ?
C1 Os1 C3 178.84(15) . . ?
C2 Os1 N7 172.63(14) . . ?
N4 Os1 N7 94.69(12) . . ?
O1 Os1 N7 85.69(12) . . ?
C1 Os1 N7 88.39(14) . . ?
C3 Os1 N7 92.05(14) . . ?
C19 O1 Os1 125.1(2) . . ?
C13 O2 C12 104.7(3) . . ?
C4 N4 Os1 132.9(3) . . ?
C4 N4 H4 113.5 . . ?
Os1 N4 H4 113.5 . . ?
C4 N5 C20 126.3(3) . . ?
C4 N5 H5 116.8 . . ?
C20 N5 H5 116.8 . . ?
C5 N6 C29 120.4(3) . . ?
C13 N7 C7 105.5(3) . . ?
C13 N7 Os1 123.3(3) . . ?
C7 N7 Os1 130.4(2) . . ?
O4 N8 O3 122.8(5) . . ?
O4 N8 C16 118.5(5) . . ?
O3 N8 C16 118.8(5) . . ?
N1 C1 Os1 177.0(4) . . ?
N2 C2 Os1 177.4(4) . . ?
N3 C3 Os1 175.6(4) . . ?
N4 C4 N5 121.9(3) . . ?
N4 C4 C5 118.6(3) . . ?
N5 C4 C5 119.5(3) . . ?
N6 C5 C6 127.2(4) . . ?
N6 C5 C4 115.8(3) . . ?
C6 C5 C4 116.9(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C7 C8 121.0(4) . . ?
C12 C7 N7 106.9(3) . . ?
C8 C7 N7 132.1(4) . . ?
C9 C8 C7 116.5(4) . . ?
C9 C8 H8 121.8 . . ?
C7 C8 H8 121.8 . . ?
C8 C9 C10 121.9(5) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
C11 C10 C9 122.5(4) . . ?
C11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C10 C11 C12 114.6(4) . . ?
C10 C11 H11 122.7 . . ?
C12 C11 H11 122.7 . . ?
C7 C12 O2 108.8(3) . . ?
C7 C12 C11 123.6(4) . . ?
O2 C12 C11 127.5(4) . . ?
N7 C13 O2 114.1(3) . . ?
N7 C13 C14 128.0(4) . . ?
O2 C13 C14 117.8(3) . . ?
C15 C14 C19 120.6(4) . . ?
C15 C14 C13 118.8(4) . . ?
C19 C14 C13 120.2(4) . . ?
C16 C15 C14 119.5(4) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 121.2(4) . . ?
C15 C16 N8 118.9(5) . . ?
C17 C16 N8 119.8(5) . . ?
C18 C17 C16 119.6(4) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 121.9(5) . . ?
C17 C18 H18 119.0 . . ?
C19 C18 H18 119.0 . . ?
O1 C19 C18 118.2(4) . . ?
O1 C19 C14 124.6(4) . . ?
C18 C19 C14 117.1(4) . . ?
C21 C20 C25 121.9(4) . . ?
C21 C20 N5 119.7(4) . . ?
C25 C20 N5 118.3(4) . . ?
C20 C21 C22 118.1(4) . . ?
C20 C21 C26 122.3(4) . . ?
C22 C21 C26 119.6(4) . . ?
C21 C22 C23 122.0(4) . . ?
C21 C22 H22 119.0 . . ?
C23 C22 H22 119.0 . . ?
C24 C23 C22 118.0(4) . . ?
C24 C23 C27 121.4(4) . . ?
C22 C23 C27 120.7(4) . . ?
C23 C24 C25 122.3(4) . . ?
C23 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C20 C25 C24 117.7(4) . . ?
C20 C25 C28 121.2(4) . . ?
C24 C25 C28 121.1(4) . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 121.8(4) . . ?
C30 C29 N6 121.9(4) . . ?
C34 C29 N6 116.0(4) . . ?
C31 C30 C29 117.5(4) . . ?
C31 C30 C35 120.3(4) . . ?
C29 C30 C35 122.2(4) . . ?
C32 C31 C30 122.9(5) . . ?
C32 C31 H31 118.6 . . ?
C30 C31 H31 118.6 . . ?
C33 C32 C31 118.3(4) . . ?
C33 C32 C36 121.4(5) . . ?
C31 C32 C36 120.3(5) . . ?
C32 C33 C34 122.2(5) . . ?
C32 C33 H33 118.9 . . ?
C34 C33 H33 118.9 . . ?
C33 C34 C29 117.3(4) . . ?
C33 C34 C37 121.6(4) . . ?
C29 C34 C37 121.1(4) . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C30 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C44 P1 C56 108.9(2) . . ?
C44 P1 C38 109.19(19) . . ?
C56 P1 C38 112.4(2) . . ?
C44 P1 C50 109.87(19) . . ?
C56 P1 C50 108.26(18) . . ?
C38 P1 C50 108.2(2) . . ?
C43 C38 C39 119.4(4) . . ?
C43 C38 P1 120.3(3) . . ?
C39 C38 P1 120.3(3) . . ?
C40 C39 C38 119.4(5) . . ?
C40 C39 H39 120.3 . . ?
C38 C39 H39 120.3 . . ?
C41 C40 C39 120.5(5) . . ?
C41 C40 H40 119.8 . . ?
C39 C40 H40 119.8 . . ?
C42 C41 C40 120.6(5) . . ?
C42 C41 H41 119.7 . . ?
C40 C41 H41 119.7 . . ?
C41 C42 C43 119.7(5) . . ?
C41 C42 H42 120.1 . . ?
C43 C42 H42 120.1 . . ?
C38 C43 C42 120.4(5) . . ?
C38 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C45 C44 C49 120.3(4) . . ?
C45 C44 P1 120.2(3) . . ?
C49 C44 P1 119.3(4) . . ?
C44 C45 C46 119.8(5) . . ?
C44 C45 H45 120.1 . . ?
C46 C45 H45 120.1 . . ?
C47 C46 C45 120.0(5) . . ?
C47 C46 H46 120.0 . . ?
C45 C46 H46 120.0 . . ?
C46 C47 C48 120.0(5) . . ?
C46 C47 H47 120.0 . . ?
C48 C47 H47 120.0 . . ?
C47 C48 C49 121.5(6) . . ?
C47 C48 H48 119.3 . . ?
C49 C48 H48 119.3 . . ?
C44 C49 C48 118.4(5) . . ?
C44 C49 H49 120.8 . . ?
C48 C49 H49 120.8 . . ?
C55 C50 C51 120.2(4) . . ?
C55 C50 P1 120.8(3) . . ?
C51 C50 P1 118.8(3) . . ?
C52 C51 C50 118.8(4) . . ?
C52 C51 H51 120.6 . . ?
C50 C51 H51 120.6 . . ?
C53 C52 C51 120.6(5) . . ?
C53 C52 H52 119.7 . . ?
C51 C52 H52 119.7 . . ?
C52 C53 C54 120.8(5) . . ?
C52 C53 H53 119.6 . . ?
C54 C53 H53 119.6 . . ?
C53 C54 C55 119.7(4) . . ?
C53 C54 H54 120.2 . . ?
C55 C54 H54 120.2 . . ?
C50 C55 C54 119.9(4) . . ?
C50 C55 H55 120.0 . . ?
C54 C55 H55 120.0 . . ?
C61 C56 C57 118.7(4) . . ?
C61 C56 P1 120.3(3) . . ?
C57 C56 P1 120.7(4) . . ?
C58 C57 C56 120.3(5) . . ?
C58 C57 H57 119.9 . . ?
C56 C57 H57 119.9 . . ?
C57 C58 C59 120.3(5) . . ?
C57 C58 H58 119.8 . . ?
C59 C58 H58 119.8 . . ?
C60 C59 C58 120.3(5) . . ?
C60 C59 H59 119.8 . . ?
C58 C59 H59 119.8 . . ?
C59 C60 C61 120.1(5) . . ?
C59 C60 H60 119.9 . . ?
C61 C60 H60 119.9 . . ?
C60 C61 C56 120.1(5) . . ?
C60 C61 H61 119.9 . . ?
C56 C61 H61 119.9 . . ?
Cl1 C62 Cl2 114.8(7) . . ?
Cl1 C62 H62A 108.6 . . ?
Cl2 C62 H62A 108.6 . . ?
Cl1 C62 H62B 108.6 . . ?
Cl2 C62 H62B 108.6 . . ?
H62A C62 H62B 107.5 . . ?
Cl4 C63 Cl3 112.0(4) . . ?
Cl4 C63 H63A 109.2 . . ?
Cl3 C63 H63A 109.2 . . ?
Cl4 C63 H63B 109.2 . . ?
Cl3 C63 H63B 109.2 . . ?
H63A C63 H63B 107.9 . . ?
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
O5_1 C64_1 1.51(2) . ?
O5_1 C66_1 1.52(2) . ?
C64_1 C65_1 1.579(19) . ?
C64_1 H64A_1 0.9800 . ?
C64_1 H64B_1 0.9800 . ?
C65_1 H65A_1 0.9700 . ?
C65_1 H65B_1 0.9700 . ?
C65_1 H65C_1 0.9700 . ?
C66_1 C67_1 1.538(18) . ?
C66_1 H66A_1 0.9800 . ?
C66_1 H66B_1 0.9800 . ?
C67_1 H67A_1 0.9700 . ?
C67_1 H67B_1 0.9700 . ?
C67_1 H67C_1 0.9700 . ?
Os1 C2 2.004(4) . ?
Os1 N4 2.044(3) . ?
Os1 O1 2.050(3) . ?
Os1 C1 2.065(4) . ?
Os1 C3 2.066(4) . ?
Os1 N7 2.120(3) . ?
O1 C19 1.302(5) . ?
O2 C13 1.351(5) . ?
O2 C12 1.380(5) . ?
O3 N8 1.230(7) . ?
O4 N8 1.218(6) . ?
N1 C1 1.140(5) . ?
N2 C2 1.146(5) . ?
N3 C3 1.142(5) . ?
N4 C4 1.307(5) . ?
N4 H4 0.8700 . ?
N5 C4 1.330(5) . ?
N5 C20 1.438(5) . ?
N5 H5 0.8700 . ?
N6 C5 1.263(5) . ?
N6 C29 1.433(5) . ?
N7 C13 1.306(5) . ?
N7 C7 1.416(5) . ?
N8 C16 1.455(6) . ?
C4 C5 1.505(5) . ?
C5 C6 1.502(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 C12 1.372(5) . ?
C7 C8 1.378(6) . ?
C8 C9 1.377(6) . ?
C8 H8 0.9400 . ?
C9 C10 1.385(7) . ?
C9 H9 0.9400 . ?
C10 C11 1.377(7) . ?
C10 H10 0.9400 . ?
C11 C12 1.388(6) . ?
C11 H11 0.9400 . ?
C13 C14 1.451(6) . ?
C14 C15 1.391(6) . ?
C14 C19 1.421(6) . ?
C15 C16 1.373(7) . ?
C15 H15 0.9400 . ?
C16 C17 1.388(7) . ?
C17 C18 1.359(7) . ?
C17 H17 0.9400 . ?
C18 C19 1.409(6) . ?
C18 H18 0.9400 . ?
C20 C21 1.387(6) . ?
C20 C25 1.389(6) . ?
C21 C22 1.387(6) . ?
C21 C26 1.506(6) . ?
C22 C23 1.388(6) . ?
C22 H22 0.9400 . ?
C23 C24 1.380(7) . ?
C23 C27 1.513(6) . ?
C24 C25 1.392(6) . ?
C24 H24 0.9400 . ?
C25 C28 1.500(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 H28C 0.9700 . ?
C29 C30 1.399(6) . ?
C29 C34 1.411(6) . ?
C30 C31 1.386(6) . ?
C30 C35 1.500(7) . ?
C31 C32 1.384(7) . ?
C31 H31 0.9400 . ?
C32 C33 1.382(7) . ?
C32 C36 1.520(7) . ?
C33 C34 1.401(6) . ?
C33 H33 0.9400 . ?
C34 C37 1.485(7) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 H35C 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 H36C 0.9700 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 H37C 0.9700 . ?
P1 C44 1.791(4) . ?
P1 C56 1.796(4) . ?
P1 C38 1.800(4) . ?
P1 C50 1.801(4) . ?
C38 C43 1.381(6) . ?
C38 C39 1.400(6) . ?
C39 C40 1.380(7) . ?
C39 H39 0.9400 . ?
C40 C41 1.373(8) . ?
C40 H40 0.9400 . ?
C41 C42 1.370(8) . ?
C41 H41 0.9400 . ?
C42 C43 1.385(7) . ?
C42 H42 0.9400 . ?
C43 H43 0.9400 . ?
C44 C45 1.371(6) . ?
C44 C49 1.377(6) . ?
C45 C46 1.390(7) . ?
C45 H45 0.9400 . ?
C46 C47 1.353(8) . ?
C46 H46 0.9400 . ?
C47 C48 1.358(9) . ?
C47 H47 0.9400 . ?
C48 C49 1.384(8) . ?
C48 H48 0.9400 . ?
C49 H49 0.9400 . ?
C50 C55 1.375(6) . ?
C50 C51 1.389(6) . ?
C51 C52 1.385(6) . ?
C51 H51 0.9400 . ?
C52 C53 1.354(7) . ?
C52 H52 0.9400 . ?
C53 C54 1.371(7) . ?
C53 H53 0.9400 . ?
C54 C55 1.381(7) . ?
C54 H54 0.9400 . ?
C55 H55 0.9400 . ?
C56 C61 1.392(7) . ?
C56 C57 1.394(6) . ?
C57 C58 1.370(7) . ?
C57 H57 0.9400 . ?
C58 C59 1.372(8) . ?
C58 H58 0.9400 . ?
C59 C60 1.367(8) . ?
C59 H59 0.9400 . ?
C60 C61 1.380(7) . ?
C60 H60 0.9400 . ?
C61 H61 0.9400 . ?
Cl1 C62 1.567(10) . ?
Cl2 C62 1.732(10) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
Cl3 C63 1.875(9) . ?
Cl4 C63 1.614(9) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
