#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/05/4110553.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_4110553
loop_
_publ_author_name
'Miguel A. Esteruelas'
'Francisco J. Fernández-Alvarez'
'Montserrat Oliván'
'Enrique Oñate'
_publ_contact_author
;
  Dr. Enrique Oñate
  Departamento de Química Inorgánica - I.C.M.A.
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       enriqueo@unizar.es
_publ_section_title
;
 C-H Bond Activation and Subsequent C-C Bond Formation Promoted by Osmium:
 2-Vinylpyridine-Acetylene Couplings
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4596
_journal_page_last               4597
_journal_paper_doi               10.1021/ja060901t
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C52.5 H61 B Cl3 N2 Os P'
_chemical_formula_weight         1058.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.093(3)
_cell_angle_beta                 108.341(2)
_cell_angle_gamma                109.829(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4068(18)
_cell_length_b                   14.961(2)
_cell_length_c                   15.509(3)
_cell_measurement_reflns_used    979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      3
_cell_volume                     2339.7(7)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'ω rotations with narrow 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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0668
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29659
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.969
_exptl_absorpt_correction_T_max  0.6480
_exptl_absorpt_correction_T_min  0.5882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.261
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         11267
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0218P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                9764
_reflns_number_total             11267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja060901tsi20060308_121721_3.cif
_cod_data_source_block           mae184as
_cod_original_cell_volume        2339.8(6)
_cod_original_formula_sum        'C52.50 H61 B Cl3 N2 Os P'
_cod_database_code               4110553
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.526704(14) 0.783601(10) 0.679633(10) 0.01483(4) Uani 1 1 d . . .
P P 0.70134(9) 0.74132(7) 0.64982(6) 0.01718(19) Uani 1 1 d . . .
N1 N 0.4275(3) 0.6407(2) 0.6883(2) 0.0183(6) Uani 1 1 d . . .
N2 N 0.6050(3) 0.93551(19) 0.69701(18) 0.0163(6) Uani 1 1 d . . .
C1 C 0.4135(4) 0.7792(3) 0.5607(2) 0.0199(8) Uani 1 1 d . . .
H1 H 0.365(3) 0.724(2) 0.523(2) 0.014(9) Uiso 1 1 d . . .
C2 C 0.3727(4) 0.8539(3) 0.5165(3) 0.0246(9) Uani 1 1 d . . .
H2 H 0.378(3) 0.855(2) 0.462(2) 0.022(10) Uiso 1 1 d . . .
C3 C 0.3253(4) 0.9121(3) 0.5484(3) 0.0260(9) Uani 1 1 d . . .
H3 H 0.302(3) 0.952(2) 0.513(2) 0.013(9) Uiso 1 1 d . . .
C4 C 0.2928(4) 0.9121(3) 0.6348(3) 0.0277(9) Uani 1 1 d . . .
H4A H 0.217(3) 0.858(2) 0.628(2) 0.013(9) Uiso 1 1 d . . .
H4B H 0.266(4) 0.964(3) 0.641(3) 0.033(11) Uiso 1 1 d . . .
C5 C 0.4007(4) 0.9143(3) 0.7262(3) 0.0209(8) Uani 1 1 d . . .
H5 H 0.380(3) 0.939(2) 0.769(2) 0.013(9) Uiso 1 1 d . . .
C6 C 0.4056(4) 0.8170(3) 0.7436(2) 0.0183(8) Uani 1 1 d . . .
H6 H 0.329(3) 0.770(3) 0.731(2) 0.022 Uiso 1 1 d . . .
C7 C 0.5162(4) 0.8140(3) 0.8190(2) 0.0182(8) Uani 1 1 d . . .
H7 H 0.569(3) 0.865(3) 0.855(2) 0.022 Uiso 1 1 d . . .
C8 C 0.5515(4) 0.7344(3) 0.8308(2) 0.0194(8) Uani 1 1 d . . .
H8 H 0.621(3) 0.738(2) 0.878(2) 0.016(10) Uiso 1 1 d . . .
C9 C 0.4626(3) 0.6381(3) 0.7800(2) 0.0182(7) Uani 1 1 d . . .
C10 C 0.4232(4) 0.5539(3) 0.8158(3) 0.0235(8) Uani 1 1 d . . .
H10 H 0.4485 0.5532 0.8788 0.028 Uiso 1 1 calc R . .
C11 C 0.3454(4) 0.4706(3) 0.7556(3) 0.0269(9) Uani 1 1 d . . .
H11 H 0.3203 0.4124 0.7778 0.032 Uiso 1 1 calc R . .
C12 C 0.3045(4) 0.4737(3) 0.6626(3) 0.0240(8) Uani 1 1 d . . .
H12 H 0.2490 0.4181 0.6217 0.029 Uiso 1 1 calc R . .
C13 C 0.3471(3) 0.5603(3) 0.6309(3) 0.0225(8) Uani 1 1 d . . .
H13 H 0.3190 0.5627 0.5681 0.027 Uiso 1 1 calc R . .
C14 C 0.5338(3) 0.9792(3) 0.7249(2) 0.0192(8) Uani 1 1 d . . .
C15 C 0.5811(4) 1.0773(3) 0.7497(2) 0.0228(8) Uani 1 1 d . . .
H15 H 0.5311 1.1053 0.7695 0.027 Uiso 1 1 calc R . .
C16 C 0.7026(4) 1.1340(3) 0.7453(2) 0.0231(8) Uani 1 1 d . . .
H16 H 0.7356 1.2001 0.7622 0.028 Uiso 1 1 calc R . .
C17 C 0.7735(4) 1.0899(3) 0.7152(2) 0.0223(8) Uani 1 1 d . . .
H17 H 0.8554 1.1260 0.7111 0.027 Uiso 1 1 calc R . .
C18 C 0.7224(3) 0.9922(2) 0.6915(2) 0.0184(8) Uani 1 1 d . . .
H18 H 0.7709 0.9636 0.6706 0.022 Uiso 1 1 calc R . .
C19 C 0.6932(4) 0.7433(3) 0.5281(2) 0.0224(8) Uani 1 1 d . . .
H19 H 0.7684 0.7284 0.5232 0.027 Uiso 1 1 calc R . .
C20 C 0.5662(4) 0.6660(3) 0.4624(2) 0.0271(9) Uani 1 1 d . . .
H20A H 0.4925 0.6863 0.4542 0.041 Uiso 1 1 calc R . .
H20B H 0.5503 0.6068 0.4878 0.041 Uiso 1 1 calc R . .
H20C H 0.5765 0.6567 0.4042 0.041 Uiso 1 1 calc R . .
C21 C 0.7058(4) 0.8407(3) 0.4968(3) 0.0261(9) Uani 1 1 d . . .
H21A H 0.7004 0.8372 0.4337 0.039 Uiso 1 1 calc R . .
H21B H 0.7897 0.8877 0.5338 0.039 Uiso 1 1 calc R . .
H21C H 0.6354 0.8587 0.5031 0.039 Uiso 1 1 calc R . .
C22 C 0.6883(4) 0.6158(2) 0.6671(3) 0.0222(8) Uani 1 1 d . . .
H22 H 0.5932 0.5772 0.6435 0.027 Uiso 1 1 calc R . .
C23 C 0.7353(4) 0.6044(3) 0.7687(3) 0.0296(9) Uani 1 1 d . . .
H23A H 0.7031 0.5377 0.7752 0.044 Uiso 1 1 calc R . .
H23B H 0.7019 0.6389 0.8018 0.044 Uiso 1 1 calc R . .
H23C H 0.8305 0.6296 0.7927 0.044 Uiso 1 1 calc R . .
C24 C 0.7519(4) 0.5683(3) 0.6159(3) 0.0291(9) Uani 1 1 d . . .
H24A H 0.8466 0.6001 0.6398 0.044 Uiso 1 1 calc R . .
H24B H 0.7200 0.5733 0.5517 0.044 Uiso 1 1 calc R . .
H24C H 0.7291 0.5019 0.6241 0.044 Uiso 1 1 calc R . .
C25 C 0.8744(3) 0.8207(3) 0.7139(2) 0.0207(8) Uani 1 1 d . . .
H25 H 0.8869 0.8798 0.6858 0.025 Uiso 1 1 calc R . .
C26 C 0.8958(4) 0.8514(3) 0.8141(2) 0.0256(9) Uani 1 1 d . . .
H26A H 0.8966 0.7984 0.8479 0.038 Uiso 1 1 calc R . .
H26B H 0.8252 0.8713 0.8169 0.038 Uiso 1 1 calc R . .
H26C H 0.9790 0.9039 0.8403 0.038 Uiso 1 1 calc R . .
C27 C 0.9851(3) 0.7876(3) 0.7071(3) 0.0272(9) Uani 1 1 d . . .
H27A H 1.0692 0.8389 0.7343 0.041 Uiso 1 1 calc R . .
H27B H 0.9711 0.7702 0.6437 0.041 Uiso 1 1 calc R . .
H27C H 0.9841 0.7331 0.7389 0.041 Uiso 1 1 calc R . .
C28 C 0.2256(3) 0.2744(2) 0.9227(2) 0.0174(7) Uani 1 1 d . . .
C29 C 0.0953(4) 0.2513(3) 0.9224(2) 0.0223(8) Uani 1 1 d . . .
H29 H 0.0330 0.1911 0.8939 0.027 Uiso 1 1 calc R . .
C30 C 0.0555(4) 0.3141(3) 0.9624(3) 0.0304(9) Uani 1 1 d . . .
H30 H -0.0313 0.2950 0.9619 0.036 Uiso 1 1 calc R . .
C31 C 0.1450(4) 0.4052(3) 1.0031(3) 0.0325(10) Uani 1 1 d . . .
H31 H 0.1191 0.4477 1.0304 0.039 Uiso 1 1 calc R . .
C32 C 0.2721(4) 0.4321(3) 1.0026(3) 0.0279(9) Uani 1 1 d . . .
H32 H 0.3324 0.4936 1.0286 0.033 Uiso 1 1 calc R . .
C33 C 0.3116(4) 0.3676(2) 0.9634(2) 0.0204(8) Uani 1 1 d . . .
H33 H 0.3987 0.3875 0.9644 0.024 Uiso 1 1 calc R . .
C34 C 0.1661(3) 0.1614(3) 0.7694(2) 0.0190(8) Uani 1 1 d . . .
C35 C 0.1145(3) 0.2239(3) 0.7170(2) 0.0241(8) Uani 1 1 d . . .
H35 H 0.1334 0.2849 0.7454 0.029 Uiso 1 1 calc R . .
C36 C 0.0370(4) 0.1986(3) 0.6255(3) 0.0332(10) Uani 1 1 d . . .
H36 H 0.0071 0.2429 0.5932 0.040 Uiso 1 1 calc R . .
C37 C 0.0042(4) 0.1088(3) 0.5821(3) 0.0369(11) Uani 1 1 d . . .
H37 H -0.0485 0.0914 0.5206 0.044 Uiso 1 1 calc R . .
C38 C 0.0501(4) 0.0444(3) 0.6307(3) 0.0322(10) Uani 1 1 d . . .
H38 H 0.0277 -0.0171 0.6018 0.039 Uiso 1 1 calc R . .
C39 C 0.1291(4) 0.0704(3) 0.7217(3) 0.0252(9) Uani 1 1 d . . .
H39 H 0.1590 0.0255 0.7528 0.030 Uiso 1 1 calc R . .
C40 C 0.2607(3) 0.1031(2) 0.9311(2) 0.0176(7) Uani 1 1 d . . .
C41 C 0.3294(4) 0.0436(3) 0.9211(3) 0.0265(9) Uani 1 1 d . . .
H41 H 0.3836 0.0608 0.8855 0.032 Uiso 1 1 calc R . .
C42 C 0.3210(4) -0.0392(3) 0.9614(3) 0.0269(9) Uani 1 1 d . . .
H42 H 0.3673 -0.0766 0.9514 0.032 Uiso 1 1 calc R . .
C43 C 0.2443(4) -0.0662(3) 1.0161(2) 0.0247(9) Uani 1 1 d . . .
H43 H 0.2376 -0.1218 1.0431 0.030 Uiso 1 1 calc R . .
C44 C 0.1773(3) -0.0092(2) 1.0302(2) 0.0208(8) Uani 1 1 d . . .
H44 H 0.1266 -0.0258 1.0681 0.025 Uiso 1 1 calc R . .
C45 C 0.1848(3) 0.0730(2) 0.9883(2) 0.0188(8) Uani 1 1 d . . .
H45 H 0.1376 0.1095 0.9985 0.023 Uiso 1 1 calc R . .
C46 C 0.4199(3) 0.2463(2) 0.8743(2) 0.0166(7) Uani 1 1 d . . .
C47 C 0.4521(3) 0.2757(2) 0.7969(2) 0.0186(8) Uani 1 1 d . . .
H47 H 0.3835 0.2663 0.7417 0.022 Uiso 1 1 calc R . .
C48 C 0.5819(4) 0.3184(2) 0.7989(2) 0.0209(8) Uani 1 1 d . . .
H48 H 0.5982 0.3366 0.7456 0.025 Uiso 1 1 calc R . .
C49 C 0.6861(4) 0.3339(2) 0.8789(3) 0.0226(8) Uani 1 1 d . . .
H49 H 0.7730 0.3632 0.8804 0.027 Uiso 1 1 calc R . .
C50 C 0.6603(4) 0.3054(3) 0.9573(3) 0.0245(8) Uani 1 1 d . . .
H50 H 0.7300 0.3147 1.0119 0.029 Uiso 1 1 calc R . .
C51 C 0.5304(4) 0.2631(3) 0.9546(2) 0.0225(8) Uani 1 1 d . . .
H51 H 0.5154 0.2449 1.0083 0.027 Uiso 1 1 calc R . .
B B 0.2683(4) 0.1964(3) 0.8754(3) 0.0162(8) Uani 1 1 d . . .
C52 C 0.0449(5) 0.4547(3) 0.7804(5) 0.125(3) Uani 1 1 d D . .
Cl1A Cl -0.1219(5) 0.3701(3) 0.7017(3) 0.0461(11) Uiso 0.40 1 d PD A 1
Cl2A Cl 0.0399(6) 0.5495(4) 0.8203(4) 0.0419(15) Uiso 0.20 1 d PD A 1
Cl1B Cl -0.0833(4) 0.3851(3) 0.7231(3) 0.0466(11) Uiso 0.40 1 d PD A 2
Cl2B Cl 0.1106(3) 0.58355(19) 0.7715(2) 0.0316(7) Uiso 0.40 1 d PD A 2
Cl1C Cl -0.1205(7) 0.3883(5) 0.7292(5) 0.0328(16) Uiso 0.20 1 d PD A 3
Cl2C Cl 0.0830(4) 0.5694(3) 0.7977(3) 0.0478(9) Uiso 0.40 1 d PD A 3
C53A C -0.0170(9) 0.4929(7) 0.5384(6) 0.043(2) Uiso 0.50 1 d P . .
Cl3A Cl 0.0438(7) 0.5945(6) 0.4984(5) 0.057(2) Uiso 0.25 1 d P . .
Cl3B Cl 0.0675(7) 0.6151(6) 0.5572(5) 0.0510(19) Uiso 0.25 1 d P . .
Cl4A Cl 0.0332(6) 0.5809(5) 0.5507(5) 0.0464(16) Uiso 0.25 1 d P . .
Cl4B Cl 0.0511(7) 0.6188(6) 0.5217(6) 0.0412(16) Uiso 0.25 1 d P . .
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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 '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'
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
C1 Os N1 94.20(14) . .
C1 Os C6 93.93(15) . .
N1 Os C6 86.47(12) . .
C1 Os N2 91.11(14) . .
N1 Os N2 164.57(10) . .
C6 Os N2 78.72(12) . .
C1 Os C7 132.34(14) . .
N1 Os C7 85.05(12) . .
C6 Os C7 38.42(13) . .
N2 Os C7 80.68(12) . .
C1 Os C8 147.99(14) . .
N1 Os C8 61.53(12) . .
C6 Os C8 65.85(13) . .
N2 Os C8 107.68(11) . .
C7 Os C8 33.97(12) . .
C1 Os P 102.12(11) . .
N1 Os P 90.32(8) . .
C6 Os P 163.82(10) . .
N2 Os P 102.72(8) . .
C7 Os P 125.51(10) . .
C8 Os P 98.75(9) . .
C25 P C19 102.79(16) . .
C25 P C22 107.38(16) . .
C19 P C22 102.53(16) . .
C25 P Os 116.58(11) . .
C19 P Os 112.94(12) . .
C22 P Os 113.21(12) . .
C13 N1 C9 119.2(3) . .
C13 N1 Os 137.6(3) . .
C9 N1 Os 103.2(2) . .
C18 N2 C14 117.3(3) . .
C18 N2 Os 127.0(2) . .
C14 N2 Os 115.3(2) . .
C2 C1 Os 130.2(3) . .
C2 C1 H1 108(2) . .
Os C1 H1 122(2) . .
C3 C2 C1 127.8(4) . .
C3 C2 H2 121(2) . .
C1 C2 H2 111(2) . .
C2 C3 C4 128.4(4) . .
C2 C3 H3 117(2) . .
C4 C3 H3 114(2) . .
C3 C4 C5 118.1(3) . .
C3 C4 H4A 109(2) . .
C5 C4 H4A 108(2) . .
C3 C4 H4B 109(2) . .
C5 C4 H4B 108(2) . .
H4A C4 H4B 104(3) . .
C6 C5 C14 109.0(3) . .
C6 C5 C4 113.3(3) . .
C14 C5 C4 108.9(3) . .
C6 C5 H5 110(2) . .
C14 C5 H5 110(2) . .
C4 C5 H5 105(2) . .
C7 C6 C5 116.9(3) . .
C7 C6 Os 76.0(2) . .
C5 C6 Os 110.4(2) . .
C7 C6 H6 118(2) . .
C5 C6 H6 116(2) . .
Os C6 H6 112(2) . .
C8 C7 C6 123.5(3) . .
C8 C7 Os 80.3(2) . .
C6 C7 Os 65.55(19) . .
C8 C7 H7 116(2) . .
C6 C7 H7 120(2) . .
Os C7 H7 121(2) . .
C7 C8 C9 122.5(3) . .
C7 C8 Os 65.7(2) . .
C9 C8 Os 84.9(2) . .
C7 C8 H8 119(2) . .
C9 C8 H8 117(2) . .
Os C8 H8 133(2) . .
N1 C9 C10 122.0(3) . .
N1 C9 C8 110.4(3) . .
C10 C9 C8 127.6(3) . .
C11 C10 C9 118.2(3) . .
C11 C10 H10 120.9 . .
C9 C10 H10 120.9 . .
C12 C11 C10 120.0(3) . .
C12 C11 H11 120.0 . .
C10 C11 H11 120.0 . .
C11 C12 C13 119.1(3) . .
C11 C12 H12 120.4 . .
C13 C12 H12 120.4 . .
N1 C13 C12 121.4(3) . .
N1 C13 H13 119.3 . .
C12 C13 H13 119.3 . .
N2 C14 C15 121.5(3) . .
N2 C14 C5 116.0(3) . .
C15 C14 C5 122.5(3) . .
C14 C15 C16 120.2(3) . .
C14 C15 H15 119.9 . .
C16 C15 H15 119.9 . .
C17 C16 C15 118.2(3) . .
C17 C16 H16 120.9 . .
C15 C16 H16 120.9 . .
C18 C17 C16 119.4(3) . .
C18 C17 H17 120.3 . .
C16 C17 H17 120.3 . .
N2 C18 C17 123.3(3) . .
N2 C18 H18 118.4 . .
C17 C18 H18 118.4 . .
C21 C19 C20 109.6(3) . .
C21 C19 P 113.2(3) . .
C20 C19 P 112.0(2) . .
C21 C19 H19 107.3 . .
C20 C19 H19 107.3 . .
P C19 H19 107.3 . .
C19 C20 H20A 109.5 . .
C19 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C19 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C19 C21 H21A 109.5 . .
C19 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C19 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C23 C22 C24 109.3(3) . .
C23 C22 P 112.3(3) . .
C24 C22 P 117.4(3) . .
C23 C22 H22 105.6 . .
C24 C22 H22 105.6 . .
P C22 H22 105.6 . .
C22 C23 H23A 109.5 . .
C22 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C22 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C22 C24 H24A 109.5 . .
C22 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C22 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C26 C25 C27 110.8(3) . .
C26 C25 P 112.4(2) . .
C27 C25 P 117.4(3) . .
C26 C25 H25 105.0 . .
C27 C25 H25 105.0 . .
P C25 H25 105.0 . .
C25 C26 H26A 109.5 . .
C25 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C25 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
C25 C27 H27A 109.5 . .
C25 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C25 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C33 C28 C29 114.8(3) . .
C33 C28 B 124.1(3) . .
C29 C28 B 121.1(3) . .
C30 C29 C28 123.1(4) . .
C30 C29 H29 118.5 . .
C28 C29 H29 118.5 . .
C29 C30 C31 119.9(4) . .
C29 C30 H30 120.0 . .
C31 C30 H30 120.0 . .
C32 C31 C30 119.1(4) . .
C32 C31 H31 120.4 . .
C30 C31 H31 120.4 . .
C31 C32 C33 120.4(4) . .
C31 C32 H32 119.8 . .
C33 C32 H32 119.8 . .
C32 C33 C28 122.7(4) . .
C32 C33 H33 118.7 . .
C28 C33 H33 118.7 . .
C39 C34 C35 114.5(3) . .
C39 C34 B 123.6(3) . .
C35 C34 B 121.8(3) . .
C36 C35 C34 122.9(4) . .
C36 C35 H35 118.6 . .
C34 C35 H35 118.6 . .
C37 C36 C35 120.2(4) . .
C37 C36 H36 119.9 . .
C35 C36 H36 119.9 . .
C36 C37 C38 119.2(4) . .
C36 C37 H37 120.4 . .
C38 C37 H37 120.4 . .
C37 C38 C39 120.4(4) . .
C37 C38 H38 119.8 . .
C39 C38 H38 119.8 . .
C38 C39 C34 122.8(4) . .
C38 C39 H39 118.6 . .
C34 C39 H39 118.6 . .
C45 C40 C41 114.1(3) . .
C45 C40 B 125.3(3) . .
C41 C40 B 120.6(3) . .
C42 C41 C40 123.7(3) . .
C42 C41 H41 118.2 . .
C40 C41 H41 118.2 . .
C43 C42 C41 120.0(3) . .
C43 C42 H42 120.0 . .
C41 C42 H42 120.0 . .
C42 C43 C44 118.8(3) . .
C42 C43 H43 120.6 . .
C44 C43 H43 120.6 . .
C43 C44 C45 120.6(3) . .
C43 C44 H44 119.7 . .
C45 C44 H44 119.7 . .
C44 C45 C40 122.8(3) . .
C44 C45 H45 118.6 . .
C40 C45 H45 118.6 . .
C47 C46 C51 114.4(3) . .
C47 C46 B 124.7(3) . .
C51 C46 B 121.0(3) . .
C48 C47 C46 122.9(3) . .
C48 C47 H47 118.5 . .
C46 C47 H47 118.5 . .
C49 C48 C47 120.5(3) . .
C49 C48 H48 119.7 . .
C47 C48 H48 119.7 . .
C48 C49 C50 119.0(3) . .
C48 C49 H49 120.5 . .
C50 C49 H49 120.5 . .
C49 C50 C51 120.0(4) . .
C49 C50 H50 120.0 . .
C51 C50 H50 120.0 . .
C50 C51 C46 123.1(3) . .
C50 C51 H51 118.4 . .
C46 C51 H51 118.4 . .
C34 B C46 108.8(3) . .
C34 B C40 109.9(3) . .
C46 B C40 108.3(3) . .
C34 B C28 107.5(3) . .
C46 B C28 110.7(3) . .
C40 B C28 111.5(3) . .
Cl1B C52 Cl2A 114.8(5) . .
Cl1B C52 Cl2C 125.8(4) . .
Cl2A C52 Cl2C 24.7(2) . .
Cl1B C52 Cl1C 14.8(3) . .
Cl2A C52 Cl1C 101.2(5) . .
Cl2C C52 Cl1C 115.6(4) . .
Cl1B C52 Cl2B 126.1(4) . .
Cl2A C52 Cl2B 42.7(3) . .
Cl2C C52 Cl2B 18.16(17) . .
Cl1C C52 Cl2B 120.5(4) . .
Cl1B C52 Cl1A 3.4(3) . .
Cl2A C52 Cl1A 113.0(4) . .
Cl2C C52 Cl1A 122.9(3) . .
Cl1C C52 Cl1A 14.8(3) . .
Cl2B C52 Cl1A 122.8(3) . .
Cl4A C53A Cl3A 156.3(9) . 2_566
Cl4A C53A C53A 80.4(9) . 2_566
Cl3A C53A C53A 76.8(9) 2_566 2_566
Cl4A C53A Cl3A 30.8(5) . .
Cl3A C53A Cl3A 127.0(7) 2_566 .
C53A C53A Cl3A 50.1(7) 2_566 .
Cl4A C53A Cl4A 126.6(7) . 2_566
Cl3A C53A Cl4A 31.1(4) 2_566 2_566
C53A C53A Cl4A 46.3(6) 2_566 2_566
Cl3A C53A Cl4A 96.2(5) . 2_566
Cl4A C53A Cl3B 5.4(5) . .
Cl3A C53A Cl3B 152.6(8) 2_566 .
C53A C53A Cl3B 78.4(9) 2_566 .
Cl3A C53A Cl3B 30.1(4) . .
Cl4A C53A Cl3B 124.5(6) 2_566 .
Cl4A C53A Cl4B 150.7(8) . 2_566
Cl3A C53A Cl4B 6.2(5) 2_566 2_566
C53A C53A Cl4B 70.8(8) 2_566 2_566
Cl3A C53A Cl4B 120.9(6) . 2_566
Cl4A C53A Cl4B 24.9(4) 2_566 2_566
Cl3B C53A Cl4B 147.6(6) . 2_566
Cl4A C53A Cl4B 16.5(6) . .
Cl3A C53A Cl4B 141.4(8) 2_566 .
C53A C53A Cl4B 64.6(8) 2_566 .
Cl3A C53A Cl4B 14.5(4) . .
Cl4A C53A Cl4B 110.7(6) 2_566 .
Cl3B C53A Cl4B 16.8(3) . .
Cl4B C53A Cl4B 135.4(5) 2_566 .
Cl4A C53A Cl3B 138.9(8) . 2_566
Cl3A C53A Cl3B 21.0(5) 2_566 2_566
C53A C53A Cl3B 58.9(8) 2_566 2_566
Cl3A C53A Cl3B 108.2(6) . 2_566
Cl4A C53A Cl3B 13.2(4) 2_566 2_566
Cl3B C53A Cl3B 137.3(5) . 2_566
Cl4B C53A Cl3B 15.1(3) 2_566 2_566
Cl4B C53A Cl3B 122.7(6) . 2_566
Cl4A Cl3A Cl3B 33.9(7) . .
Cl4A Cl3A C53A 98.1(10) . 2_566
Cl3B Cl3A C53A 126.8(12) . 2_566
Cl4A Cl3A C53A 45.9(7) . .
Cl3B Cl3A C53A 78.6(9) . .
C53A Cl3A C53A 53.0(7) 2_566 .
Cl4A Cl3B Cl4B 90.8(17) . .
Cl4A Cl3B Cl3A 72.3(13) . .
Cl4B Cl3B Cl3A 27.2(11) . .
Cl4A Cl3B C53A 13.0(11) . .
Cl4B Cl3B C53A 93.8(16) . .
Cl3A Cl3B C53A 71.3(8) . .
Cl4A Cl3B C53A 48.6(13) . 2_566
Cl4B Cl3B C53A 59.0(14) . 2_566
Cl3A Cl3B C53A 32.2(7) . 2_566
C53A Cl3B C53A 42.7(5) . 2_566
Cl3B Cl4A Cl4B 45.7(11) . .
Cl3B Cl4A Cl3A 73.8(15) . .
Cl4B Cl4A Cl3A 32.9(8) . .
Cl3B Cl4A C53A 161.6(16) . .
Cl4B Cl4A C53A 135.7(14) . .
Cl3A Cl4A C53A 103.3(10) . .
Cl3B Cl4A C53A 118.2(15) . 2_566
Cl4B Cl4A C53A 83.6(11) . 2_566
Cl3A Cl4A C53A 50.8(7) . 2_566
C53A Cl4A C53A 53.4(7) . 2_566
Cl3B Cl4B Cl4A 43.5(11) . .
Cl3B Cl4B C53A 105.9(15) . 2_566
Cl4A Cl4B C53A 71.5(10) . 2_566
Cl3B Cl4B C53A 69.4(15) . .
Cl4A Cl4B C53A 27.9(9) . .
C53A Cl4B C53A 44.6(5) 2_566 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os C1 1.874(4) .
Os N1 2.082(3) .
Os C6 2.110(3) .
Os N2 2.117(3) .
Os C7 2.249(3) .
Os C8 2.431(4) .
Os P 2.4506(9) .
P C25 1.850(4) .
P C19 1.862(4) .
P C22 1.864(3) .
N1 C13 1.334(4) .
N1 C9 1.355(4) .
N2 C18 1.350(4) .
N2 C14 1.358(4) .
C1 C2 1.455(5) .
C1 H1 0.90(3) .
C2 C3 1.329(5) .
C2 H2 0.87(3) .
C3 C4 1.499(5) .
C3 H3 0.88(3) .
C4 C5 1.548(5) .
C4 H4A 0.94(3) .
C4 H4B 0.93(4) .
C5 C6 1.503(5) .
C5 C14 1.506(5) .
C5 H5 0.88(3) .
C6 C7 1.440(5) .
C6 H6 0.88(3) .
C7 C8 1.378(5) .
C7 H7 0.85(4) .
C8 C9 1.479(5) .
C8 H8 0.88(3) .
C9 C10 1.378(5) .
C10 C11 1.376(5) .
C10 H10 0.9300 .
C11 C12 1.375(5) .
C11 H11 0.9300 .
C12 C13 1.381(5) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 C15 1.380(5) .
C15 C16 1.382(5) .
C15 H15 0.9300 .
C16 C17 1.377(5) .
C16 H16 0.9300 .
C17 C18 1.369(5) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 C21 1.520(5) .
C19 C20 1.537(5) .
C19 H19 0.9800 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C22 C23 1.529(5) .
C22 C24 1.534(5) .
C22 H22 0.9800 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 C26 1.531(5) .
C25 C27 1.535(5) .
C25 H25 0.9800 .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
C27 H27A 0.9600 .
C27 H27B 0.9600 .
C27 H27C 0.9600 .
C28 C33 1.398(5) .
C28 C29 1.405(5) .
C28 B 1.649(5) .
C29 C30 1.385(5) .
C29 H29 0.9300 .
C30 C31 1.385(5) .
C30 H30 0.9300 .
C31 C32 1.369(5) .
C31 H31 0.9300 .
C32 C33 1.396(5) .
C32 H32 0.9300 .
C33 H33 0.9300 .
C34 C39 1.397(5) .
C34 C35 1.408(5) .
C34 B 1.638(5) .
C35 C36 1.379(5) .
C35 H35 0.9300 .
C36 C37 1.365(6) .
C36 H36 0.9300 .
C37 C38 1.375(6) .
C37 H37 0.9300 .
C38 C39 1.378(5) .
C38 H38 0.9300 .
C39 H39 0.9300 .
C40 C45 1.404(5) .
C40 C41 1.405(5) .
C40 B 1.648(5) .
C41 C42 1.386(5) .
C41 H41 0.9300 .
C42 C43 1.375(5) .
C42 H42 0.9300 .
C43 C44 1.378(5) .
C43 H43 0.9300 .
C44 C45 1.391(4) .
C44 H44 0.9300 .
C45 H45 0.9300 .
C46 C47 1.398(5) .
C46 C51 1.410(5) .
C46 B 1.640(5) .
C47 C48 1.390(5) .
C47 H47 0.9300 .
C48 C49 1.371(5) .
C48 H48 0.9300 .
C49 C50 1.380(5) .
C49 H49 0.9300 .
C50 C51 1.386(5) .
C50 H50 0.9300 .
C51 H51 0.9300 .
C52 Cl1B 1.458(6) .
C52 Cl2A 1.562(7) .
C52 Cl2C 1.616(6) .
C52 Cl1C 1.713(8) .
C52 Cl2B 1.842(5) .
C52 Cl1A 1.886(6) .
C53A Cl4A 1.228(10) .
C53A Cl3A 1.311(11) 2_566
C53A C53A 1.364(17) 2_566
C53A Cl3A 1.663(13) .
C53A Cl4A 1.676(12) 2_566
C53A Cl3B 1.721(12) .
C53A Cl4B 1.756(12) 2_566
C53A Cl4B 1.835(13) .
C53A Cl3B 1.970(13) 2_566
Cl3A Cl4A 0.874(9) .
Cl3A Cl3B 0.881(10) .
Cl3A C53A 1.311(11) 2_566
Cl3B Cl4A 0.512(9) .
Cl3B Cl4B 0.533(9) .
Cl3B C53A 1.970(13) 2_566
Cl4A Cl4B 0.744(9) .
Cl4A C53A 1.676(12) 2_566
Cl4B C53A 1.756(12) 2_566
