# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1.2toluene _database_code_depnum_ccdc_archive 'CCDC 917746' #TrackingRef '16520_web_deposit_cif_file_0_Dr.PrasantaGhosh_1356954009.RKM-PQ(cif-1,2,4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H54 Cl2 O2 P2 Ru' _chemical_formula_weight 1088.98 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' Cl Cl 0.1484 0.1585 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M c2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.3724(16) _cell_length_b 11.4673(4) _cell_length_c 17.5890(9) _cell_angle_alpha 90.00 _cell_angle_beta 123.500(3) _cell_angle_gamma 90.00 _cell_volume 5276.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6492 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.69 _exptl_crystal_description rectangle _exptl_crystal_colour Dark_green _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.985 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19262 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4474 _reflns_number_gt 3836 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+6.3424P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4474 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.053 _refine_ls_shift/su_mean 0.002 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 Ru1 Ru 0.0000 0.39545(2) 0.2500 0.03090(14) Uani 1 2 d S . . P1 P 0.08709(3) 0.39121(6) 0.38168(6) 0.0347(2) Uani 1 1 d . . . Cl1 Cl -0.02386(3) 0.25822(6) 0.31977(6) 0.0415(2) Uani 1 1 d . . . O1 O 0.01775(8) 0.53263(17) 0.19924(14) 0.0362(5) Uani 1 1 d . . . C1 C 0.00950(11) 0.6327(3) 0.2217(2) 0.0358(7) Uani 1 1 d . . . C2 C 0.01779(11) 0.7400(3) 0.1891(2) 0.0394(7) Uani 1 1 d . . . C3 C 0.00806(12) 0.8462(3) 0.2180(2) 0.0432(8) Uani 1 1 d . . . C4 C 0.01450(14) 0.9485(3) 0.1824(3) 0.0566(10) Uani 1 1 d . . . H4A H 0.0091 1.0200 0.2007 0.068 Uiso 1 1 calc R . . C5 C 0.02849(15) 0.9465(3) 0.1220(3) 0.0644(11) Uani 1 1 d . . . H5A H 0.0320 1.0165 0.0992 0.077 Uiso 1 1 calc R . . C6 C 0.03766(15) 0.8422(3) 0.0933(3) 0.0614(10) Uani 1 1 d . . . H6A H 0.0469 0.8418 0.0514 0.074 Uiso 1 1 calc R . . C7 C 0.03284(13) 0.7402(3) 0.1280(3) 0.0512(9) Uani 1 1 d . . . H7A H 0.0397 0.6698 0.1106 0.061 Uiso 1 1 calc R . . C8 C 0.10747(12) 0.2630(3) 0.4557(2) 0.0418(7) Uani 1 1 d . . . C9 C 0.09552(14) 0.1545(3) 0.4151(3) 0.0552(9) Uani 1 1 d . . . H9A H 0.0764 0.1483 0.3518 0.066 Uiso 1 1 calc R . . C10 C 0.11210(16) 0.0550(4) 0.4685(3) 0.0697(12) Uani 1 1 d . . . H10A H 0.1038 -0.0180 0.4408 0.084 Uiso 1 1 calc R . . C11 C 0.14020(16) 0.0627(4) 0.5607(3) 0.0713(13) Uani 1 1 d . . . H11A H 0.1514 -0.0047 0.5959 0.086 Uiso 1 1 calc R . . C12 C 0.15213(16) 0.1695(4) 0.6018(3) 0.0704(12) Uani 1 1 d . . . H12A H 0.1711 0.1748 0.6650 0.084 Uiso 1 1 calc R . . C13 C 0.13584(14) 0.2711(3) 0.5490(3) 0.0562(9) Uani 1 1 d . . . H13A H 0.1442 0.3438 0.5770 0.067 Uiso 1 1 calc R . . C14 C 0.13962(12) 0.4119(3) 0.3662(2) 0.0406(7) Uani 1 1 d . . . C15 C 0.18979(15) 0.3877(3) 0.4375(3) 0.0617(11) Uani 1 1 d . . . H15A H 0.1963 0.3556 0.4915 0.074 Uiso 1 1 calc R . . C16 C 0.22984(16) 0.4114(4) 0.4278(4) 0.0741(13) Uani 1 1 d . . . H16A H 0.2632 0.3954 0.4756 0.089 Uiso 1 1 calc R . . C17 C 0.22097(16) 0.4576(4) 0.3496(3) 0.0732(12) Uani 1 1 d . . . H17A H 0.2482 0.4743 0.3441 0.088 Uiso 1 1 calc R . . C18 C 0.17160(16) 0.4798(4) 0.2781(3) 0.0758(13) Uani 1 1 d . . . H18A H 0.1654 0.5109 0.2241 0.091 Uiso 1 1 calc R . . C19 C 0.13099(14) 0.4556(4) 0.2867(3) 0.0580(10) Uani 1 1 d . . . H19A H 0.0977 0.4694 0.2378 0.070 Uiso 1 1 calc R . . C20 C 0.09467(13) 0.5133(3) 0.4545(2) 0.0440(8) Uani 1 1 d . . . C21 C 0.12107(17) 0.6122(3) 0.4611(3) 0.0636(11) Uani 1 1 d . . . H21A H 0.1385 0.6165 0.4322 0.076 Uiso 1 1 calc R . . C22 C 0.1214(2) 0.7073(4) 0.5121(4) 0.0944(18) Uani 1 1 d . . . H22A H 0.1396 0.7744 0.5177 0.113 Uiso 1 1 calc R . . C23 C 0.0952(2) 0.7016(5) 0.5537(4) 0.0956(19) Uani 1 1 d . . . H23A H 0.0954 0.7650 0.5869 0.115 Uiso 1 1 calc R . . C24 C 0.0691(2) 0.6036(4) 0.5466(3) 0.0784(15) Uani 1 1 d . . . H24A H 0.0516 0.5999 0.5754 0.094 Uiso 1 1 calc R . . C25 C 0.06821(15) 0.5101(4) 0.4973(3) 0.0580(10) Uani 1 1 d . . . H25A H 0.0497 0.4438 0.4922 0.070 Uiso 1 1 calc R . . C26 C 0.1883(4) 1.1461(7) 0.2786(6) 0.137(7) Uani 0.593(7) 1 d PG A 1 H26A H 0.1785 1.2218 0.2567 0.165 Uiso 0.593(7) 1 calc PR A 1 C27 C 0.1569(3) 1.0771(13) 0.2927(8) 0.202(11) Uani 0.593(7) 1 d PG A 1 H27A H 0.1261 1.1066 0.2804 0.243 Uiso 0.593(7) 1 calc PR A 1 C28 C 0.1716(5) 0.9639(12) 0.3253(8) 0.231(10) Uani 0.593(7) 1 d PG A 1 H28A H 0.1505 0.9177 0.3348 0.277 Uiso 0.593(7) 1 calc PR A 1 C29 C 0.2176(5) 0.9198(7) 0.3438(7) 0.171(8) Uani 0.593(7) 1 d PG A 1 C30 C 0.2490(3) 0.9889(11) 0.3296(6) 0.126(6) Uani 0.593(7) 1 d PG A 1 H30A H 0.2799 0.9594 0.3419 0.151 Uiso 0.593(7) 1 calc PR A 1 C31 C 0.2344(4) 1.1020(10) 0.2970(6) 0.082(3) Uani 0.593(7) 1 d PG A 1 H31A H 0.2554 1.1482 0.2875 0.099 Uiso 0.593(7) 1 calc PR A 1 C32 C 0.2141(5) 0.7873(12) 0.3817(8) 0.096(4) Uani 0.593(7) 1 d P A 1 H32A H 0.1914 0.7908 0.4020 0.143 Uiso 0.593(7) 1 calc PR A 1 H32B H 0.2475 0.7642 0.4315 0.143 Uiso 0.593(7) 1 calc PR A 1 H32C H 0.2015 0.7315 0.3332 0.143 Uiso 0.593(7) 1 calc PR A 1 C26' C 0.1867(5) 0.7921(13) 0.3606(9) 0.137(7) Uani 0.407(7) 1 d PG A 2 H26B H 0.1781 0.7215 0.3746 0.165 Uiso 0.407(7) 1 calc PR A 2 C27' C 0.1517(4) 0.8834(18) 0.3254(11) 0.202(11) Uani 0.407(7) 1 d PG A 2 H27B H 0.1197 0.8738 0.3160 0.243 Uiso 0.407(7) 1 calc PR A 2 C28' C 0.1646(7) 0.9890(14) 0.3044(11) 0.231(10) Uani 0.407(7) 1 d PG A 2 H28B H 0.1413 1.0501 0.2809 0.277 Uiso 0.407(7) 1 calc PR A 2 C29' C 0.2125(8) 1.0034(10) 0.3186(11) 0.171(8) Uani 0.407(7) 1 d PG A 2 C30' C 0.2475(5) 0.9121(14) 0.3537(10) 0.126(6) Uani 0.407(7) 1 d PG A 2 H30B H 0.2795 0.9217 0.3632 0.151 Uiso 0.407(7) 1 calc PR A 2 C31' C 0.2346(4) 0.8065(11) 0.3747(8) 0.082(3) Uani 0.407(7) 1 d PG A 2 H31B H 0.2580 0.7454 0.3982 0.099 Uiso 0.407(7) 1 calc PR A 2 C32' C 0.2193(6) 1.1469(11) 0.2809(12) 0.082(6) Uani 0.407(7) 1 d P A 2 H32D H 0.1861 1.1802 0.2401 0.123 Uiso 0.407(7) 1 calc PR A 2 H32E H 0.2365 1.1388 0.2499 0.123 Uiso 0.407(7) 1 calc PR A 2 H32F H 0.2389 1.1969 0.3329 0.123 Uiso 0.407(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0400(2) 0.0235(2) 0.0342(2) 0.000 0.02361(17) 0.000 P1 0.0400(4) 0.0323(4) 0.0335(5) 0.0008(3) 0.0214(4) 0.0000(3) Cl1 0.0539(5) 0.0317(4) 0.0497(5) 0.0050(3) 0.0353(4) -0.0008(3) O1 0.0437(12) 0.0275(10) 0.0424(12) 0.0024(8) 0.0270(10) 0.0036(8) C1 0.0354(15) 0.0298(14) 0.0399(17) 0.0032(12) 0.0194(14) 0.0006(12) C2 0.0374(16) 0.0327(16) 0.0478(19) 0.0049(13) 0.0233(15) -0.0007(12) C3 0.0365(16) 0.0304(15) 0.054(2) 0.0004(14) 0.0199(15) -0.0003(13) C4 0.062(2) 0.0320(17) 0.071(3) 0.0079(16) 0.034(2) -0.0015(15) C5 0.068(3) 0.043(2) 0.083(3) 0.018(2) 0.042(2) -0.0036(18) C6 0.065(2) 0.059(2) 0.073(3) 0.019(2) 0.046(2) 0.0012(19) C7 0.055(2) 0.0434(18) 0.062(2) 0.0086(16) 0.0362(19) 0.0003(15) C8 0.0396(17) 0.0444(17) 0.0422(19) 0.0102(14) 0.0231(15) 0.0036(13) C9 0.057(2) 0.0419(19) 0.056(2) 0.0075(16) 0.0240(19) 0.0083(16) C10 0.068(3) 0.045(2) 0.083(3) 0.017(2) 0.033(2) 0.0111(19) C11 0.058(2) 0.064(3) 0.086(3) 0.039(2) 0.036(2) 0.017(2) C12 0.063(2) 0.087(3) 0.052(2) 0.031(2) 0.026(2) 0.015(2) C13 0.056(2) 0.061(2) 0.043(2) 0.0123(17) 0.0218(18) 0.0048(17) C14 0.0412(17) 0.0428(17) 0.0414(19) -0.0028(14) 0.0251(15) -0.0003(13) C15 0.049(2) 0.085(3) 0.051(2) 0.0080(19) 0.0282(19) 0.0060(18) C16 0.040(2) 0.106(4) 0.070(3) 0.009(3) 0.027(2) 0.002(2) C17 0.050(2) 0.102(3) 0.080(3) 0.006(3) 0.044(2) -0.003(2) C18 0.059(2) 0.112(4) 0.070(3) 0.025(3) 0.044(2) 0.006(2) C19 0.0422(19) 0.079(3) 0.055(2) 0.016(2) 0.0278(18) 0.0049(18) C20 0.0446(18) 0.0447(18) 0.0355(18) -0.0040(14) 0.0177(15) 0.0021(14) C21 0.067(3) 0.045(2) 0.077(3) -0.0128(18) 0.038(2) -0.0069(17) C22 0.088(4) 0.052(3) 0.116(5) -0.028(3) 0.039(3) -0.005(2) C23 0.088(4) 0.092(4) 0.078(3) -0.040(3) 0.028(3) 0.024(3) C24 0.080(3) 0.101(4) 0.049(3) -0.017(2) 0.032(2) 0.022(3) C25 0.061(2) 0.073(3) 0.041(2) -0.0032(17) 0.0293(18) 0.0072(19) C26 0.191(15) 0.075(6) 0.056(5) -0.015(4) 0.012(9) -0.016(8) C27 0.072(6) 0.37(3) 0.131(11) -0.154(16) 0.033(7) -0.003(10) C28 0.151(10) 0.46(3) 0.111(11) -0.156(15) 0.088(9) -0.118(13) C29 0.178(12) 0.187(17) 0.061(7) -0.059(10) 0.012(9) 0.066(13) C30 0.070(5) 0.223(18) 0.070(7) -0.040(10) 0.029(5) -0.009(9) C31 0.057(5) 0.089(7) 0.060(5) 0.000(4) 0.007(4) 0.001(4) C32 0.101(9) 0.092(7) 0.079(8) 0.034(6) 0.041(6) -0.012(6) C26' 0.191(15) 0.075(6) 0.056(5) -0.015(4) 0.012(9) -0.016(8) C27' 0.072(6) 0.37(3) 0.131(11) -0.154(16) 0.033(7) -0.003(10) C28' 0.151(10) 0.46(3) 0.111(11) -0.156(15) 0.088(9) -0.118(13) C29' 0.178(12) 0.187(17) 0.061(7) -0.059(10) 0.012(9) 0.066(13) C30' 0.070(5) 0.223(18) 0.070(7) -0.040(10) 0.029(5) -0.009(9) C31' 0.057(5) 0.089(7) 0.060(5) 0.000(4) 0.007(4) 0.001(4) C32' 0.064(10) 0.029(6) 0.072(9) -0.012(5) -0.014(7) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ru1 O1 2.032(2) . ? Ru1 O1 2.032(2) 2 ? Ru1 Cl1 2.3572(8) . ? Ru1 Cl1 2.3573(8) 2 ? Ru1 P1 2.4179(8) . ? Ru1 P1 2.4179(8) 2 ? P1 C20 1.823(3) . ? P1 C14 1.828(3) . ? P1 C8 1.829(3) . ? O1 C1 1.286(4) . ? C1 C1 1.415(7) 2 ? C1 C2 1.441(4) . ? C2 C7 1.391(5) . ? C2 C3 1.417(4) . ? C3 C4 1.396(5) . ? C3 C3 1.466(7) 2 ? C4 C5 1.356(6) . ? C4 H4A 0.9300 . ? C5 C6 1.389(6) . ? C5 H5A 0.9300 . ? C6 C7 1.366(5) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C13 1.371(5) . ? C8 C9 1.380(5) . ? C9 C10 1.385(5) . ? C9 H9A 0.9300 . ? C10 C11 1.355(7) . ? C10 H10A 0.9300 . ? C11 C12 1.366(7) . ? C11 H11A 0.9300 . ? C12 C13 1.399(5) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C19 1.364(5) . ? C14 C15 1.396(5) . ? C15 C16 1.385(6) . ? C15 H15A 0.9300 . ? C16 C17 1.352(7) . ? C16 H16A 0.9300 . ? C17 C18 1.376(6) . ? C17 H17A 0.9300 . ? C18 C19 1.391(5) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.372(5) . ? C20 C25 1.395(5) . ? C21 C22 1.409(7) . ? C21 H21A 0.9300 . ? C22 C23 1.372(9) . ? C22 H22A 0.9300 . ? C23 C24 1.355(8) . ? C23 H23A 0.9300 . ? C24 C25 1.370(6) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C26 H26A 0.9300 . ? C27 C28 1.3900 . ? C27 H27A 0.9300 . ? C28 C29 1.3900 . ? C28 H28A 0.9300 . ? C29 C30 1.3900 . ? C29 C32 1.688(14) . ? C30 C31 1.3900 . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C26' C27' 1.3900 . ? C26' C31' 1.3900 . ? C26' H26B 0.9300 . ? C27' C28' 1.3900 . ? C27' H27B 0.9300 . ? C28' C29' 1.3900 . ? C28' H28B 0.9300 . ? C29' C30' 1.3900 . ? C29' C32' 1.83(2) . ? C30' C31' 1.3900 . ? C30' H30B 0.9300 . ? C31' H31B 0.9300 . ? C32' H32D 0.9600 . ? C32' H32E 0.9600 . ? C32' H32F 0.9600 . ? 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 O1 Ru1 O1 78.57(11) . 2 ? O1 Ru1 Cl1 171.16(6) . . ? O1 Ru1 Cl1 92.60(6) 2 . ? O1 Ru1 Cl1 92.60(6) . 2 ? O1 Ru1 Cl1 171.16(6) 2 2 ? Cl1 Ru1 Cl1 96.23(4) . 2 ? O1 Ru1 P1 89.87(6) . . ? O1 Ru1 P1 91.92(6) 2 . ? Cl1 Ru1 P1 90.20(3) . . ? Cl1 Ru1 P1 88.26(3) 2 . ? O1 Ru1 P1 91.92(6) . 2 ? O1 Ru1 P1 89.87(6) 2 2 ? Cl1 Ru1 P1 88.26(3) . 2 ? Cl1 Ru1 P1 90.20(3) 2 2 ? P1 Ru1 P1 177.69(4) . 2 ? C20 P1 C14 103.10(15) . . ? C20 P1 C8 104.93(17) . . ? C14 P1 C8 102.76(15) . . ? C20 P1 Ru1 107.34(11) . . ? C14 P1 Ru1 119.31(11) . . ? C8 P1 Ru1 117.67(11) . . ? C1 O1 Ru1 113.9(2) . . ? O1 C1 C1 116.78(17) . 2 ? O1 C1 C2 121.9(3) . . ? C1 C1 C2 121.28(19) 2 . ? C7 C2 C3 120.6(3) . . ? C7 C2 C1 121.4(3) . . ? C3 C2 C1 117.9(3) . . ? C4 C3 C2 116.6(3) . . ? C4 C3 C3 122.8(2) . 2 ? C2 C3 C3 120.68(19) . 2 ? C5 C4 C3 121.9(4) . . ? C5 C4 H4A 119.1 . . ? C3 C4 H4A 119.1 . . ? C4 C5 C6 121.3(3) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C7 C6 C5 118.6(4) . . ? C7 C6 H6A 120.7 . . ? C5 C6 H6A 120.7 . . ? C6 C7 C2 121.0(4) . . ? C6 C7 H7A 119.5 . . ? C2 C7 H7A 119.5 . . ? C13 C8 C9 119.5(3) . . ? C13 C8 P1 122.6(3) . . ? C9 C8 P1 117.8(3) . . ? C8 C9 C10 119.9(4) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C11 C12 C13 120.2(4) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C8 C13 C12 119.7(4) . . ? C8 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C19 C14 C15 118.8(3) . . ? C19 C14 P1 121.0(3) . . ? C15 C14 P1 120.2(3) . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C17 C16 C15 120.7(4) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 119.8(4) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C17 C18 C19 120.0(4) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C14 C19 C18 120.6(4) . . ? C14 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C21 C20 C25 119.2(4) . . ? C21 C20 P1 122.2(3) . . ? C25 C20 P1 118.3(3) . . ? C20 C21 C22 119.0(5) . . ? C20 C21 H21A 120.5 . . ? C22 C21 H21A 120.5 . . ? C23 C22 C21 120.5(5) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C24 C23 C22 120.1(4) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 120.4(5) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C24 C25 C20 120.8(4) . . ? C24 C25 H25A 119.6 . . ? C20 C25 H25A 119.6 . . ? C27 C26 C31 120.0 . . ? C27 C26 H26A 120.0 . . ? C31 C26 H26A 120.0 . . ? C28 C27 C26 120.0 . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 C32 142.3(11) . . ? C28 C29 C32 97.7(11) . . ? C29 C30 C31 120.0 . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C30 C31 C26 120.0 . . ? C30 C31 H31A 120.0 . . ? C26 C31 H31A 120.0 . . ? C27' C26' C31' 120.0 . . ? C27' C26' H26B 120.0 . . ? C31' C26' H26B 120.0 . . ? C28' C27' C26' 120.0 . . ? C28' C27' H27B 120.0 . . ? C26' C27' H27B 120.0 . . ? C27' C28' C29' 120.0 . . ? C27' C28' H28B 120.0 . . ? C29' C28' H28B 120.0 . . ? C30' C29' C28' 120.0 . . ? C30' C29' C32' 128.1(14) . . ? C28' C29' C32' 111.8(13) . . ? C29' C30' C31' 120.0 . . ? C29' C30' H30B 120.0 . . ? C31' C30' H30B 120.0 . . ? C30' C31' C26' 120.0 . . ? C30' C31' H31B 120.0 . . ? C26' C31' H31B 120.0 . . ? C29' C32' H32D 109.5 . . ? C29' C32' H32E 109.4 . . ? H32D C32' H32E 109.5 . . ? C29' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.716 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.069 data_2.CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 917747' #TrackingRef '16520_web_deposit_cif_file_0_Dr.PrasantaGhosh_1356954009.RKM-PQ(cif-1,2,4).cif' _audit_creation_method SHELXL-97 _audit_creation_date 2012-09-14 _audit_block_code FNG-PG-506-83 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_compound_source 'dichloromethane, hexane' _chemical_formula_moiety 'C50 H38 Br2 O2 Os P2, C H2 Cl2' _chemical_formula_sum 'C51 H40 Br2 Cl2 O2 Os P2' _chemical_formula_weight 1167.69 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' 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.5613(9) _cell_length_b 11.6716(14) _cell_length_c 17.879(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.797(7) _cell_angle_gamma 90.00 _cell_volume 4388.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 44241 _cell_measurement_theta_min 2.7636 _cell_measurement_theta_max 33.0989 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.0250 0.00 0.00 -1.00 0.0250 3.00 0.00 -1.00 0.1100 -2.00 0.00 1.00 0.1100 0.00 -1.00 0.00 0.1200 -1.00 1.00 0.00 0.1000 _exptl_crystal_description prism _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 4.963 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)' _exptl_absorpt_correction_T_min 0.45601 _exptl_absorpt_correction_T_max 0.82384 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Enraf-Nonius KappaCCD' _diffrn_measurement_method 'CCD \f- and \w-scans' _diffrn_detector_area_resol_mean 18.02 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40373 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 33.04 _reflns_number_total 8269 _reflns_number_gt 7688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DATCOL (Bruker AXS, 2006)' _computing_cell_refinement 'DENZO (Bruker AXS, 2006)' _computing_data_reduction 'DENZO (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+16.2779P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8269 _refine_ls_number_parameters 285 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.226 _refine_ls_restrained_S_all 1.226 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.5000 0.627759(10) 0.2500 0.00916(3) Uani 1 2 d S . . O1 O 0.52104(8) 0.49467(16) 0.32842(12) 0.0157(3) Uani 1 1 d . . . C2 C 0.51172(11) 0.3933(2) 0.29439(15) 0.0120(4) Uani 1 1 d . . . C3 C 0.52282(11) 0.2864(2) 0.34069(16) 0.0136(4) Uani 1 1 d . . . C4 C 0.54278(13) 0.2865(2) 0.42742(17) 0.0177(5) Uani 1 1 d . . . H4 H 0.5509 0.3572 0.4568 0.021 Uiso 1 1 calc R . . C5 C 0.55076(15) 0.1847(2) 0.47048(19) 0.0226(5) Uani 1 1 d . . . H5 H 0.5632 0.1852 0.5290 0.027 Uiso 1 1 calc R . . C6 C 0.54028(15) 0.0809(2) 0.4270(2) 0.0244(6) Uani 1 1 d . . . H6 H 0.5465 0.0105 0.4564 0.029 Uiso 1 1 calc R . . C7 C 0.52089(14) 0.0799(2) 0.34123(19) 0.0221(5) Uani 1 1 d . . . H7 H 0.5140 0.0086 0.3128 0.026 Uiso 1 1 calc R . . C8 C 0.51124(12) 0.1821(2) 0.29580(17) 0.0155(4) Uani 1 1 d . . . P20 P 0.60746(3) 0.63472(5) 0.26728(4) 0.01115(10) Uani 1 1 d . . . C21 C 0.61652(12) 0.5182(2) 0.20597(17) 0.0174(4) Uani 1 1 d . . . C22 C 0.64710(16) 0.4172(3) 0.2437(2) 0.0338(8) Uani 1 1 d . . . H22 H 0.6690 0.4118 0.3031 0.041 Uiso 1 1 calc R . . C23 C 0.64562(19) 0.3232(4) 0.1943(3) 0.0487(12) Uani 1 1 d . . . H23 H 0.6663 0.2539 0.2201 0.058 Uiso 1 1 calc R . . C24 C 0.61429(16) 0.3308(4) 0.1081(3) 0.0384(9) Uani 1 1 d . . . H24 H 0.6140 0.2672 0.0749 0.046 Uiso 1 1 calc R . . C25 C 0.58315(15) 0.4311(3) 0.0698(2) 0.0288(7) Uani 1 1 d . . . H25 H 0.5615 0.4359 0.0104 0.035 Uiso 1 1 calc R . . C26 C 0.58369(14) 0.5245(3) 0.11825(18) 0.0223(5) Uani 1 1 d . . . H26 H 0.5618 0.5928 0.0920 0.027 Uiso 1 1 calc R . . C31 C 0.63092(12) 0.7635(2) 0.23050(16) 0.0164(4) Uani 1 1 d . . . C32 C 0.66887(14) 0.7594(3) 0.1890(2) 0.0267(6) Uani 1 1 d . . . H32 H 0.6816 0.6877 0.1763 0.032 Uiso 1 1 calc R . . C33 C 0.68808(18) 0.8618(4) 0.1660(2) 0.0379(9) Uani 1 1 d . . . H33 H 0.7137 0.8588 0.1375 0.045 Uiso 1 1 calc R . . C34 C 0.67053(17) 0.9660(3) 0.1842(2) 0.0371(8) Uani 1 1 d . . . H34 H 0.6839 1.0347 0.1684 0.045 Uiso 1 1 calc R . . C35 C 0.63312(16) 0.9708(3) 0.2258(2) 0.0310(7) Uani 1 1 d . . . H35 H 0.6210 1.0429 0.2387 0.037 Uiso 1 1 calc R . . C36 C 0.61327(13) 0.8701(2) 0.24863(19) 0.0212(5) Uani 1 1 d . . . H36 H 0.5875 0.8740 0.2768 0.025 Uiso 1 1 calc R . . C41 C 0.67307(11) 0.6152(2) 0.37239(15) 0.0128(4) Uani 1 1 d . . . C42 C 0.66327(12) 0.5606(2) 0.43501(17) 0.0181(5) Uani 1 1 d . . . H42 H 0.6217 0.5365 0.4240 0.022 Uiso 1 1 calc R . . C43 C 0.71392(13) 0.5414(3) 0.51346(18) 0.0228(5) Uani 1 1 d . . . H43 H 0.7070 0.5039 0.5558 0.027 Uiso 1 1 calc R . . C44 C 0.77504(13) 0.5771(3) 0.53005(18) 0.0230(5) Uani 1 1 d . . . H44 H 0.8098 0.5627 0.5833 0.028 Uiso 1 1 calc R . . C45 C 0.78496(13) 0.6335(3) 0.46909(18) 0.0224(5) Uani 1 1 d . . . H45 H 0.8264 0.6589 0.4808 0.027 Uiso 1 1 calc R . . C46 C 0.73428(12) 0.6532(2) 0.39040(17) 0.0171(5) Uani 1 1 d . . . H46 H 0.7413 0.6927 0.3488 0.021 Uiso 1 1 calc R . . Br50 Br 0.533844(11) 0.76479(2) 0.371891(15) 0.01318(5) Uani 1 1 d . . . C60 C 0.7860(4) 0.2846(9) 0.5095(4) 0.044(2) Uani 0.50 1 d PD . . H60A H 0.7924 0.3588 0.4876 0.053 Uiso 0.50 1 calc PR . . H60B H 0.8131 0.2268 0.5004 0.053 Uiso 0.50 1 calc PR . . Cl61 Cl 0.70599(11) 0.24376(19) 0.45417(17) 0.0448(5) Uani 0.50 1 d PD . . Cl62 Cl 0.80964(11) 0.2976(2) 0.61804(14) 0.0471(5) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os 0.00894(5) 0.00711(5) 0.01165(6) 0.000 0.00485(4) 0.000 O1 0.0149(7) 0.0137(8) 0.0183(9) -0.0009(7) 0.0073(7) -0.0007(6) C2 0.0110(9) 0.0093(9) 0.0152(10) 0.0006(7) 0.0053(8) 0.0015(7) C3 0.0138(9) 0.0087(9) 0.0174(11) -0.0003(8) 0.0061(8) 0.0015(7) C4 0.0209(11) 0.0136(10) 0.0172(11) 0.0018(9) 0.0074(9) 0.0004(9) C5 0.0309(14) 0.0165(12) 0.0195(13) 0.0081(10) 0.0106(11) 0.0040(10) C6 0.0328(15) 0.0128(11) 0.0236(14) 0.0060(10) 0.0093(11) 0.0001(10) C7 0.0282(13) 0.0104(10) 0.0229(13) 0.0025(9) 0.0073(11) 0.0014(9) C8 0.0167(10) 0.0096(10) 0.0183(11) 0.0016(8) 0.0060(9) 0.0004(8) P20 0.0094(2) 0.0127(3) 0.0114(2) -0.0001(2) 0.00475(19) 0.00017(19) C21 0.0134(9) 0.0223(12) 0.0168(11) -0.0047(9) 0.0071(8) 0.0011(9) C22 0.0257(14) 0.0310(16) 0.0272(16) -0.0111(13) -0.0035(12) 0.0133(12) C23 0.0350(18) 0.039(2) 0.047(2) -0.0232(18) -0.0036(16) 0.0226(16) C24 0.0226(14) 0.047(2) 0.041(2) -0.0287(17) 0.0098(14) 0.0039(14) C25 0.0247(13) 0.0434(19) 0.0241(14) -0.0154(13) 0.0162(12) -0.0068(13) C26 0.0231(12) 0.0289(14) 0.0176(12) -0.0048(10) 0.0116(10) -0.0024(11) C31 0.0128(10) 0.0216(12) 0.0127(10) 0.0041(9) 0.0039(8) -0.0031(8) C32 0.0215(13) 0.0384(17) 0.0247(14) 0.0018(12) 0.0143(11) -0.0060(11) C33 0.0335(17) 0.054(2) 0.0337(18) 0.0064(16) 0.0220(15) -0.0143(16) C34 0.0325(16) 0.0382(19) 0.0377(19) 0.0130(15) 0.0132(14) -0.0144(14) C35 0.0272(14) 0.0228(14) 0.0381(18) 0.0087(13) 0.0105(13) -0.0072(11) C36 0.0185(11) 0.0177(11) 0.0252(13) 0.0052(10) 0.0079(10) -0.0039(9) C41 0.0114(9) 0.0126(10) 0.0127(10) -0.0015(8) 0.0039(8) 0.0004(7) C42 0.0138(10) 0.0235(12) 0.0143(11) 0.0040(9) 0.0039(8) 0.0001(9) C43 0.0190(11) 0.0308(15) 0.0141(11) 0.0060(10) 0.0036(9) 0.0002(10) C44 0.0158(11) 0.0301(14) 0.0166(12) 0.0033(10) 0.0016(9) 0.0006(10) C45 0.0128(10) 0.0298(14) 0.0199(12) 0.0008(11) 0.0033(9) -0.0008(10) C46 0.0118(9) 0.0231(12) 0.0153(11) 0.0000(9) 0.0050(8) -0.0010(8) Br50 0.01401(10) 0.01202(10) 0.01205(10) -0.00278(7) 0.00459(8) -0.00057(7) C60 0.048(5) 0.046(5) 0.044(5) 0.006(4) 0.025(5) 0.005(4) Cl61 0.0409(10) 0.0328(10) 0.0476(13) 0.0086(9) 0.0082(10) 0.0037(8) Cl62 0.0518(11) 0.0475(11) 0.0362(10) 0.0166(9) 0.0147(9) 0.0001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O1 1.9994(19) 2_655 ? Os O1 1.9995(19) . ? Os P20 2.4096(6) 2_655 ? Os P20 2.4097(6) . ? Os Br50 2.5251(3) . ? Os Br50 2.5252(3) 2_655 ? O1 C2 1.303(3) . ? C2 C2 1.426(5) 2_655 ? C2 C3 1.454(3) . ? C3 C4 1.403(4) . ? C3 C8 1.415(3) . ? C4 C5 1.382(4) . ? C5 C6 1.401(4) . ? C6 C7 1.389(4) . ? C7 C8 1.403(4) . ? C8 C8 1.477(5) 2_655 ? P20 C21 1.819(3) . ? P20 C31 1.824(3) . ? P20 C41 1.831(2) . ? C21 C22 1.388(4) . ? C21 C26 1.404(4) . ? C22 C23 1.400(5) . ? C23 C24 1.378(6) . ? C24 C25 1.387(6) . ? C25 C26 1.389(4) . ? C31 C36 1.395(4) . ? C31 C32 1.397(4) . ? C32 C33 1.402(5) . ? C33 C34 1.370(6) . ? C34 C35 1.387(5) . ? C35 C36 1.392(4) . ? C41 C42 1.395(4) . ? C41 C46 1.401(3) . ? C42 C43 1.390(4) . ? C43 C44 1.397(4) . ? C44 C45 1.380(4) . ? C45 C46 1.394(4) . ? C60 Cl61 1.754(7) . ? C60 Cl62 1.768(7) . ? 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 O1 Os O1 78.05(11) 2_655 . ? O1 Os P20 91.28(5) 2_655 2_655 ? O1 Os P20 91.72(5) . 2_655 ? O1 Os P20 91.73(5) 2_655 . ? O1 Os P20 91.28(5) . . ? P20 Os P20 176.14(3) 2_655 . ? O1 Os Br50 168.31(5) 2_655 . ? O1 Os Br50 90.28(5) . . ? P20 Os Br50 89.658(17) 2_655 . ? P20 Os Br50 87.894(17) . . ? O1 Os Br50 90.28(6) 2_655 2_655 ? O1 Os Br50 168.31(5) . 2_655 ? P20 Os Br50 87.895(17) 2_655 2_655 ? P20 Os Br50 89.659(17) . 2_655 ? Br50 Os Br50 101.400(15) . 2_655 ? C2 O1 Os 116.22(16) . . ? O1 C2 C2 114.76(14) . 2_655 ? O1 C2 C3 124.3(2) . . ? C2 C2 C3 120.90(14) 2_655 . ? C4 C3 C8 120.7(2) . . ? C4 C3 C2 120.8(2) . . ? C8 C3 C2 118.4(2) . . ? C5 C4 C3 120.5(3) . . ? C4 C5 C6 119.3(3) . . ? C7 C6 C5 120.5(3) . . ? C6 C7 C8 121.3(3) . . ? C7 C8 C3 117.6(3) . . ? C7 C8 C8 121.70(17) . 2_655 ? C3 C8 C8 120.68(15) . 2_655 ? C21 P20 C31 105.19(13) . . ? C21 P20 C41 104.54(11) . . ? C31 P20 C41 102.70(11) . . ? C21 P20 Os 107.43(8) . . ? C31 P20 Os 116.96(9) . . ? C41 P20 Os 118.65(8) . . ? C22 C21 C26 119.5(3) . . ? C22 C21 P20 121.2(2) . . ? C26 C21 P20 118.6(2) . . ? C21 C22 C23 119.9(3) . . ? C24 C23 C22 120.2(4) . . ? C23 C24 C25 120.3(3) . . ? C24 C25 C26 120.0(3) . . ? C25 C26 C21 120.1(3) . . ? C36 C31 C32 118.9(3) . . ? C36 C31 P20 118.7(2) . . ? C32 C31 P20 122.3(2) . . ? C31 C32 C33 119.6(3) . . ? C34 C33 C32 121.0(3) . . ? C33 C34 C35 119.7(3) . . ? C34 C35 C36 120.1(3) . . ? C35 C36 C31 120.6(3) . . ? C42 C41 C46 119.1(2) . . ? C42 C41 P20 120.79(18) . . ? C46 C41 P20 120.11(19) . . ? C43 C42 C41 120.4(2) . . ? C42 C43 C44 120.0(3) . . ? C45 C44 C43 120.0(3) . . ? C44 C45 C46 120.2(3) . . ? C45 C46 C41 120.3(3) . . ? Cl61 C60 Cl62 111.6(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 33.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.999 _refine_diff_density_min -1.760 _refine_diff_density_rms 0.145 data_4(+)I3(-) _database_code_depnum_ccdc_archive 'CCDC 917748' #TrackingRef '16520_web_deposit_cif_file_0_Dr.PrasantaGhosh_1356954009.RKM-PQ(cif-1,2,4).cif' _audit_creation_method SHELXL-97 _audit_creation_date 2012-02-24 _audit_block_code WGT_PG-504-62 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H38 Br O3 Os P2, I3' _chemical_formula_sum 'C51 H38 Br I3 O3 Os P2' _chemical_formula_weight 1411.56 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' 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.243(2) _cell_length_b 14.0856(12) _cell_length_c 25.252(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.390(11) _cell_angle_gamma 90.00 _cell_volume 4710.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 93684 _cell_measurement_theta_min 2.6529 _cell_measurement_theta_max 33.0992 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 0.00 0.00 0.0600 1.00 0.00 0.00 0.0600 0.00 1.00 0.00 0.1600 0.00 -1.00 0.00 0.1600 0.00 0.00 -1.00 0.0550 0.00 0.00 1.00 0.0550 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 5.632 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)' _exptl_absorpt_correction_T_min 0.40661 _exptl_absorpt_correction_T_max 0.63432 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Enraf-Nonius KappaCCD' _diffrn_measurement_method 'CCD \f- and \w-scans' _diffrn_detector_area_resol_mean 18.02 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79466 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 31.50 _reflns_number_total 15661 _reflns_number_gt 12787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DATCOL (Bruker AXS, 2006)' _computing_cell_refinement 'DENZO (Bruker AXS, 2006)' _computing_data_reduction 'DENZO (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+12.6985P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15661 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1056 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 0.721349(11) 0.797500(10) 0.773471(5) 0.01235(4) Uani 1 1 d . . . C101 C 0.8376(4) 0.7458(3) 0.74518(18) 0.01793(11) Uani 0.8887(16) 1 d P A 1 O102 O 0.9127(4) 0.7199(4) 0.72981(17) 0.0280(9) Uani 0.8887(16) 1 d P A 1 Br1 Br 0.61069(3) 0.66272(3) 0.741910(17) 0.01793(11) Uani 0.8887(16) 1 d P A 1 Br1' Br 0.8853(4) 0.7422(3) 0.73846(18) 0.01793(11) Uani 0.1113(16) 1 d P A 2 I81 I 0.18220(3) 0.94145(3) 0.842496(15) 0.03772(8) Uani 1 1 d . . . I82 I 0.18460(2) 0.78403(2) 0.917727(14) 0.03106(8) Uani 1 1 d . . . I83 I 0.17994(3) 0.62179(2) 0.989749(14) 0.03473(8) Uani 1 1 d . . . O1 O 0.7971(2) 0.91284(19) 0.80060(10) 0.0146(5) Uani 1 1 d . A . C2 C 0.7490(3) 0.9747(3) 0.82680(14) 0.0155(7) Uani 1 1 d . . . C3 C 0.7954(3) 1.0564(3) 0.84960(16) 0.0171(7) Uani 1 1 d . A . C4 C 0.8984(3) 1.0740(3) 0.84152(16) 0.0202(8) Uani 1 1 d . . . H4 H 0.9365 1.0335 0.8192 0.024 Uiso 1 1 calc R A . C5 C 0.9441(3) 1.1505(3) 0.86610(17) 0.0233(8) Uani 1 1 d . A . H5 H 1.0137 1.1632 0.8607 0.028 Uiso 1 1 calc R . . C6 C 0.8874(4) 1.2089(3) 0.89883(19) 0.0268(9) Uani 1 1 d . . . H6 H 0.9190 1.2610 0.9161 0.032 Uiso 1 1 calc R A . C7 C 0.7856(4) 1.1923(3) 0.90670(19) 0.0250(9) Uani 1 1 d . A . H7 H 0.7484 1.2334 0.9291 0.030 Uiso 1 1 calc R . . C8 C 0.7364(3) 1.1157(3) 0.88213(16) 0.0198(8) Uani 1 1 d . . . C9 C 0.6287(3) 1.0956(3) 0.89115(17) 0.0193(7) Uani 1 1 d . A . C10 C 0.5696(4) 1.1511(3) 0.9250(2) 0.0292(10) Uani 1 1 d . . . H10 H 0.5994 1.2035 0.9429 0.035 Uiso 1 1 calc R A . C11 C 0.4682(4) 1.1309(4) 0.9327(2) 0.0331(11) Uani 1 1 d . A . H11 H 0.4296 1.1699 0.9557 0.040 Uiso 1 1 calc R . . C12 C 0.4225(4) 1.0546(4) 0.9075(2) 0.0293(10) Uani 1 1 d . . . H12 H 0.3528 1.0422 0.9128 0.035 Uiso 1 1 calc R A . C13 C 0.4785(3) 0.9966(3) 0.87455(17) 0.0214(8) Uani 1 1 d . A . H13 H 0.4479 0.9438 0.8575 0.026 Uiso 1 1 calc R . . C14 C 0.5816(3) 1.0170(3) 0.86665(15) 0.0181(7) Uani 1 1 d . . . C15 C 0.6415(3) 0.9546(3) 0.83461(15) 0.0156(7) Uani 1 1 d . A . O16 O 0.6088(2) 0.87925(18) 0.81327(10) 0.0145(5) Uani 1 1 d . A . P20 P 0.74848(8) 0.71687(7) 0.85603(4) 0.01464(18) Uani 1 1 d . A . C21 C 0.8365(3) 0.6178(3) 0.85566(16) 0.0175(7) Uani 1 1 d . . . C22 C 0.8334(3) 0.5557(3) 0.81280(17) 0.0216(8) Uani 1 1 d . A . H22 H 0.7904 0.5686 0.7834 0.026 Uiso 1 1 calc R . . C23 C 0.8934(3) 0.4746(3) 0.81321(18) 0.0234(8) Uani 1 1 d . . . H23 H 0.8916 0.4325 0.7838 0.028 Uiso 1 1 calc R A . C24 C 0.9559(3) 0.4546(3) 0.85622(19) 0.0241(8) Uani 1 1 d . A . H24 H 0.9952 0.3982 0.8568 0.029 Uiso 1 1 calc R . . C25 C 0.9603(3) 0.5177(3) 0.89823(18) 0.0249(9) Uani 1 1 d . . . H25 H 1.0044 0.5052 0.9272 0.030 Uiso 1 1 calc R A . C26 C 0.9009(3) 0.5994(3) 0.89846(17) 0.0221(8) Uani 1 1 d . A . H26 H 0.9042 0.6421 0.9275 0.026 Uiso 1 1 calc R . . C31 C 0.6371(3) 0.6726(3) 0.89019(15) 0.0169(7) Uani 1 1 d . . . C32 C 0.5399(3) 0.6925(3) 0.87223(18) 0.0224(8) Uani 1 1 d . A . H32 H 0.5299 0.7241 0.8394 0.027 Uiso 1 1 calc R . . C33 C 0.4574(3) 0.6660(3) 0.90273(19) 0.0258(9) Uani 1 1 d . . . H33 H 0.3909 0.6790 0.8905 0.031 Uiso 1 1 calc R A . C34 C 0.4722(4) 0.6205(4) 0.95126(19) 0.0297(10) Uani 1 1 d . A . H34 H 0.4158 0.6031 0.9723 0.036 Uiso 1 1 calc R . . C35 C 0.5691(4) 0.6008(3) 0.96864(18) 0.0278(9) Uani 1 1 d . . . H35 H 0.5790 0.5699 1.0017 0.033 Uiso 1 1 calc R A . C36 C 0.6517(3) 0.6254(3) 0.93859(17) 0.0222(8) Uani 1 1 d . A . H36 H 0.7180 0.6105 0.9506 0.027 Uiso 1 1 calc R . . C41 C 0.7963(3) 0.8045(3) 0.90304(15) 0.0171(7) Uani 1 1 d . . . C42 C 0.8965(3) 0.8340(3) 0.90186(16) 0.0198(8) Uani 1 1 d . A . H42 H 0.9432 0.8033 0.8791 0.024 Uiso 1 1 calc R . . C43 C 0.9283(3) 0.9088(3) 0.93424(17) 0.0226(8) Uani 1 1 d . . . H43 H 0.9972 0.9275 0.9342 0.027 Uiso 1 1 calc R A . C44 C 0.8605(4) 0.9560(3) 0.96644(17) 0.0231(8) Uani 1 1 d . A . H44 H 0.8828 1.0072 0.9881 0.028 Uiso 1 1 calc R . . C45 C 0.7604(3) 0.9285(3) 0.96699(16) 0.0218(8) Uani 1 1 d . . . H45 H 0.7136 0.9610 0.9888 0.026 Uiso 1 1 calc R A . C46 C 0.7283(3) 0.8532(3) 0.93554(15) 0.0184(7) Uani 1 1 d . A . H46 H 0.6594 0.8345 0.9361 0.022 Uiso 1 1 calc R . . P50 P 0.68024(7) 0.87683(7) 0.69212(4) 0.01350(17) Uani 1 1 d . A . C51 C 0.7137(3) 1.0009(3) 0.70142(15) 0.0152(7) Uani 1 1 d . . . C52 C 0.6423(3) 1.0668(3) 0.71776(18) 0.0217(8) Uani 1 1 d . A . H52 H 0.5730 1.0495 0.7196 0.026 Uiso 1 1 calc R . . C53 C 0.6726(4) 1.1586(3) 0.73149(19) 0.0257(9) Uani 1 1 d . . . H53 H 0.6239 1.2036 0.7428 0.031 Uiso 1 1 calc R A . C54 C 0.7727(4) 1.1844(3) 0.72869(18) 0.0255(9) Uani 1 1 d . A . H54 H 0.7926 1.2473 0.7375 0.031 Uiso 1 1 calc R . . C55 C 0.8440(3) 1.1189(3) 0.71311(17) 0.0222(8) Uani 1 1 d . . . H55 H 0.9132 1.1364 0.7115 0.027 Uiso 1 1 calc R A . C56 C 0.8148(3) 1.0275(3) 0.69983(16) 0.0201(8) Uani 1 1 d . A . H56 H 0.8644 0.9825 0.6895 0.024 Uiso 1 1 calc R . . C61 C 0.5479(3) 0.8782(3) 0.67296(16) 0.0166(7) Uani 1 1 d . . . C62 C 0.5214(3) 0.8845(3) 0.61915(16) 0.0228(8) Uani 1 1 d . A . H62 H 0.5724 0.8833 0.5929 0.027 Uiso 1 1 calc R . . C63 C 0.4208(3) 0.8926(3) 0.60442(18) 0.0253(9) Uani 1 1 d . . . H63 H 0.4032 0.8964 0.5679 0.030 Uiso 1 1 calc R A . C64 C 0.3463(3) 0.8953(3) 0.64175(18) 0.0226(8) Uani 1 1 d . A . H64 H 0.2776 0.9012 0.6312 0.027 Uiso 1 1 calc R . . C65 C 0.3718(3) 0.8892(3) 0.69504(18) 0.0231(8) Uani 1 1 d . . . H65 H 0.3204 0.8915 0.7211 0.028 Uiso 1 1 calc R A . C66 C 0.4721(3) 0.8798(3) 0.71049(16) 0.0195(7) Uani 1 1 d . A . H66 H 0.4888 0.8745 0.7470 0.023 Uiso 1 1 calc R . . C71 C 0.7479(3) 0.8352(3) 0.63416(14) 0.0149(7) Uani 1 1 d . . . C72 C 0.7845(3) 0.8976(3) 0.59585(15) 0.0182(7) Uani 1 1 d . A . H72 H 0.7747 0.9640 0.5998 0.022 Uiso 1 1 calc R . . C73 C 0.8352(3) 0.8627(3) 0.55193(16) 0.0216(8) Uani 1 1 d . . . H73 H 0.8605 0.9054 0.5261 0.026 Uiso 1 1 calc R A . C74 C 0.8490(3) 0.7657(3) 0.54564(16) 0.0201(8) Uani 1 1 d . A . H74 H 0.8847 0.7420 0.5159 0.024 Uiso 1 1 calc R . . C75 C 0.8103(3) 0.7030(3) 0.58310(16) 0.0191(7) Uani 1 1 d . . . H75 H 0.8183 0.6365 0.5784 0.023 Uiso 1 1 calc R A . C76 C 0.7603(3) 0.7374(3) 0.62702(16) 0.0176(7) Uani 1 1 d . A . H76 H 0.7342 0.6943 0.6525 0.021 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os 0.01244(7) 0.01201(7) 0.01261(7) 0.00001(5) 0.00036(4) 0.00004(5) C101 0.0184(2) 0.0163(2) 0.0190(2) 0.00027(15) -0.00029(15) -0.00163(15) O102 0.028(2) 0.031(2) 0.024(2) 0.0021(16) 0.0007(16) 0.0042(18) Br1 0.0184(2) 0.0163(2) 0.0190(2) 0.00027(15) -0.00029(15) -0.00163(15) Br1' 0.0184(2) 0.0163(2) 0.0190(2) 0.00027(15) -0.00029(15) -0.00163(15) I81 0.03456(18) 0.03407(17) 0.0445(2) -0.01036(14) -0.00166(14) 0.00243(14) I82 0.02086(14) 0.03366(16) 0.03860(17) -0.01574(13) -0.00455(12) 0.00636(12) I83 0.03541(18) 0.02960(16) 0.03914(18) -0.01484(13) -0.00319(13) 0.00001(13) O1 0.0161(13) 0.0123(11) 0.0154(12) -0.0010(9) 0.0006(10) -0.0021(10) C2 0.0188(18) 0.0141(16) 0.0136(16) -0.0025(12) -0.0022(13) 0.0015(14) C3 0.0195(18) 0.0134(16) 0.0183(17) 0.0010(13) -0.0021(14) -0.0021(14) C4 0.0198(19) 0.0207(18) 0.0200(18) 0.0009(15) 0.0004(14) -0.0061(15) C5 0.023(2) 0.023(2) 0.024(2) -0.0006(16) 0.0007(16) -0.0091(16) C6 0.030(2) 0.022(2) 0.028(2) -0.0024(16) -0.0026(18) -0.0095(17) C7 0.029(2) 0.0177(18) 0.028(2) -0.0066(16) -0.0002(17) -0.0003(16) C8 0.026(2) 0.0149(16) 0.0187(18) -0.0009(14) -0.0015(15) 0.0019(15) C9 0.0194(19) 0.0141(16) 0.0243(19) -0.0021(14) -0.0013(15) 0.0015(14) C10 0.028(2) 0.024(2) 0.035(2) -0.0101(18) 0.0029(19) 0.0045(18) C11 0.030(2) 0.032(2) 0.037(3) -0.009(2) 0.008(2) 0.006(2) C12 0.020(2) 0.034(2) 0.034(2) -0.0087(19) 0.0051(18) 0.0030(18) C13 0.0196(19) 0.0212(19) 0.0236(19) 0.0006(15) 0.0025(15) 0.0038(15) C14 0.0191(18) 0.0184(17) 0.0169(17) -0.0008(14) 0.0022(14) 0.0032(14) C15 0.0168(17) 0.0143(16) 0.0158(16) 0.0006(13) -0.0014(13) 0.0026(13) O16 0.0170(13) 0.0123(11) 0.0142(12) -0.0026(9) 0.0005(10) 0.0009(10) P20 0.0145(4) 0.0154(4) 0.0140(4) 0.0014(3) 0.0001(3) 0.0017(3) C21 0.0155(17) 0.0165(17) 0.0205(18) 0.0040(14) 0.0004(14) 0.0025(14) C22 0.0203(19) 0.0196(18) 0.025(2) 0.0004(15) 0.0020(15) -0.0022(15) C23 0.023(2) 0.0170(18) 0.030(2) -0.0019(16) 0.0019(16) -0.0009(16) C24 0.019(2) 0.0193(18) 0.034(2) 0.0063(16) 0.0021(17) 0.0064(15) C25 0.021(2) 0.027(2) 0.027(2) 0.0079(17) -0.0006(16) 0.0034(17) C26 0.022(2) 0.0212(19) 0.0225(19) 0.0037(15) -0.0026(15) 0.0029(16) C31 0.0193(18) 0.0162(16) 0.0153(16) 0.0009(13) 0.0011(13) -0.0005(14) C32 0.0194(19) 0.024(2) 0.024(2) 0.0021(16) 0.0006(15) -0.0012(16) C33 0.0175(19) 0.029(2) 0.030(2) 0.0017(18) 0.0034(16) -0.0026(17) C34 0.029(2) 0.032(2) 0.029(2) 0.0005(18) 0.0109(18) -0.0068(19) C35 0.033(2) 0.031(2) 0.0196(19) 0.0045(17) 0.0021(17) -0.0057(19) C36 0.025(2) 0.0217(19) 0.0197(18) 0.0018(15) -0.0005(15) -0.0003(16) C41 0.0191(18) 0.0186(17) 0.0136(16) 0.0032(13) -0.0015(13) 0.0003(14) C42 0.0190(19) 0.0220(19) 0.0183(18) -0.0002(14) -0.0051(14) 0.0018(15) C43 0.022(2) 0.0222(19) 0.024(2) 0.0003(16) -0.0037(15) -0.0029(16) C44 0.031(2) 0.0184(18) 0.0194(18) -0.0009(15) -0.0056(16) 0.0015(16) C45 0.029(2) 0.0194(18) 0.0170(18) -0.0001(14) -0.0006(15) 0.0049(16) C46 0.0207(19) 0.0178(17) 0.0167(17) 0.0022(14) -0.0019(14) 0.0034(15) P50 0.0146(4) 0.0124(4) 0.0135(4) 0.0006(3) 0.0008(3) 0.0001(3) C51 0.0183(18) 0.0115(15) 0.0158(16) 0.0037(12) -0.0010(13) -0.0007(13) C52 0.022(2) 0.0150(17) 0.028(2) -0.0005(15) -0.0007(16) 0.0032(15) C53 0.027(2) 0.0138(17) 0.037(2) -0.0011(16) -0.0020(18) 0.0047(16) C54 0.032(2) 0.0143(17) 0.030(2) -0.0004(15) -0.0045(18) -0.0030(16) C55 0.023(2) 0.0202(19) 0.0233(19) -0.0007(15) -0.0007(15) -0.0051(16) C56 0.0199(19) 0.0187(18) 0.0218(19) -0.0014(15) 0.0011(15) -0.0016(15) C61 0.0181(18) 0.0116(15) 0.0200(17) 0.0020(13) -0.0030(14) 0.0008(13) C62 0.021(2) 0.030(2) 0.0168(18) 0.0002(16) -0.0030(14) 0.0035(17) C63 0.024(2) 0.030(2) 0.022(2) -0.0006(17) -0.0067(16) 0.0044(17) C64 0.0196(19) 0.0193(18) 0.029(2) -0.0014(16) -0.0052(16) 0.0030(15) C65 0.0174(19) 0.024(2) 0.028(2) 0.0027(16) 0.0005(15) -0.0006(16) C66 0.0196(19) 0.0192(18) 0.0197(18) 0.0025(14) -0.0016(14) -0.0017(15) C71 0.0145(16) 0.0168(16) 0.0134(15) 0.0003(13) -0.0002(12) 0.0008(13) C72 0.0223(19) 0.0156(16) 0.0167(17) 0.0014(13) 0.0004(14) -0.0040(14) C73 0.027(2) 0.0210(18) 0.0164(17) -0.0018(14) 0.0016(15) -0.0058(16) C74 0.0210(19) 0.0249(19) 0.0143(16) -0.0039(14) 0.0030(14) 0.0009(16) C75 0.023(2) 0.0156(17) 0.0189(18) -0.0037(14) 0.0020(15) 0.0011(15) C76 0.0186(18) 0.0159(16) 0.0182(17) 0.0005(14) 0.0002(14) 0.0001(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C101 1.851(6) . ? Os O1 2.026(3) . ? Os O16 2.140(3) . ? Os P50 2.3978(10) . ? Os P20 2.3989(10) . ? Os Br1' 2.476(6) . ? Os Br1 2.5241(5) . ? C101 O102 1.131(7) . ? I81 I82 2.9198(6) . ? I82 I83 2.9216(6) . ? O1 C2 1.268(4) . ? C2 C3 1.425(5) . ? C2 C15 1.466(6) . ? C3 C4 1.403(6) . ? C3 C8 1.411(6) . ? C4 C5 1.381(6) . ? C5 C6 1.389(7) . ? C6 C7 1.385(7) . ? C7 C8 1.402(6) . ? C8 C9 1.473(6) . ? C9 C10 1.402(6) . ? C9 C14 1.412(6) . ? C10 C11 1.388(7) . ? C11 C12 1.387(7) . ? C12 C13 1.385(6) . ? C13 C14 1.411(6) . ? C14 C15 1.436(5) . ? C15 O16 1.266(5) . ? P20 C21 1.818(4) . ? P20 C41 1.823(4) . ? P20 C31 1.824(4) . ? C21 C22 1.393(6) . ? C21 C26 1.397(6) . ? C22 C23 1.391(6) . ? C23 C24 1.390(6) . ? C24 C25 1.385(7) . ? C25 C26 1.393(6) . ? C31 C32 1.390(6) . ? C31 C36 1.403(6) . ? C32 C33 1.392(6) . ? C33 C34 1.396(7) . ? C34 C35 1.382(7) . ? C35 C36 1.380(6) . ? C41 C42 1.391(6) . ? C41 C46 1.402(6) . ? C42 C43 1.397(6) . ? C43 C44 1.385(6) . ? C44 C45 1.381(7) . ? C45 C46 1.390(6) . ? P50 C61 1.815(4) . ? P50 C71 1.818(4) . ? P50 C51 1.818(4) . ? C51 C52 1.390(6) . ? C51 C56 1.391(6) . ? C52 C53 1.397(6) . ? C53 C54 1.376(7) . ? C54 C55 1.381(6) . ? C55 C56 1.384(6) . ? C61 C66 1.385(6) . ? C61 C62 1.404(6) . ? C62 C63 1.386(6) . ? C63 C64 1.369(6) . ? C64 C65 1.388(6) . ? C65 C66 1.388(6) . ? C71 C72 1.396(5) . ? C71 C76 1.400(5) . ? C72 C73 1.390(6) . ? C73 C74 1.388(6) . ? C74 C75 1.394(6) . ? C75 C76 1.383(5) . ? 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 C101 Os O1 91.99(17) . . ? C101 Os O16 167.68(17) . . ? O1 Os O16 75.80(11) . . ? C101 Os P50 92.14(14) . . ? O1 Os P50 91.43(8) . . ? O16 Os P50 89.82(8) . . ? C101 Os P20 91.67(14) . . ? O1 Os P20 90.85(8) . . ? O16 Os P20 86.98(8) . . ? P50 Os P20 175.49(3) . . ? C101 Os Br1' 5.44(18) . . ? O1 Os Br1' 86.55(13) . . ? O16 Os Br1' 162.29(13) . . ? P50 Os Br1' 92.02(11) . . ? P20 Os Br1' 91.99(11) . . ? C101 Os Br1 93.72(15) . . ? O1 Os Br1 174.19(8) . . ? O16 Os Br1 98.52(7) . . ? P50 Os Br1 87.25(3) . . ? P20 Os Br1 90.09(3) . . ? Br1' Os Br1 99.15(11) . . ? O102 C101 Os 174.5(5) . . ? I81 I82 I83 177.237(15) . . ? C2 O1 Os 118.5(3) . . ? O1 C2 C3 123.3(4) . . ? O1 C2 C15 115.5(3) . . ? C3 C2 C15 121.2(3) . . ? C4 C3 C8 121.5(4) . . ? C4 C3 C2 120.1(4) . . ? C8 C3 C2 118.3(4) . . ? C5 C4 C3 119.8(4) . . ? C4 C5 C6 119.4(4) . . ? C7 C6 C5 121.1(4) . . ? C6 C7 C8 121.1(4) . . ? C7 C8 C3 117.1(4) . . ? C7 C8 C9 121.7(4) . . ? C3 C8 C9 121.1(4) . . ? C10 C9 C14 117.2(4) . . ? C10 C9 C8 122.2(4) . . ? C14 C9 C8 120.5(4) . . ? C11 C10 C9 121.1(4) . . ? C12 C11 C10 120.9(4) . . ? C13 C12 C11 119.9(4) . . ? C12 C13 C14 119.2(4) . . ? C13 C14 C9 121.5(4) . . ? C13 C14 C15 119.6(4) . . ? C9 C14 C15 118.9(4) . . ? O16 C15 C14 124.4(4) . . ? O16 C15 C2 115.7(3) . . ? C14 C15 C2 119.9(3) . . ? C15 O16 Os 114.5(2) . . ? C21 P20 C41 107.63(19) . . ? C21 P20 C31 105.13(18) . . ? C41 P20 C31 101.65(18) . . ? C21 P20 Os 116.82(13) . . ? C41 P20 Os 107.13(13) . . ? C31 P20 Os 117.13(14) . . ? C22 C21 C26 120.0(4) . . ? C22 C21 P20 118.1(3) . . ? C26 C21 P20 121.8(3) . . ? C23 C22 C21 119.7(4) . . ? C24 C23 C22 120.6(4) . . ? C25 C24 C23 119.4(4) . . ? C24 C25 C26 120.8(4) . . ? C25 C26 C21 119.5(4) . . ? C32 C31 C36 120.1(4) . . ? C32 C31 P20 121.8(3) . . ? C36 C31 P20 117.8(3) . . ? C31 C32 C33 119.6(4) . . ? C32 C33 C34 120.2(4) . . ? C35 C34 C33 119.7(4) . . ? C36 C35 C34 120.9(4) . . ? C35 C36 C31 119.5(4) . . ? C42 C41 C46 118.9(4) . . ? C42 C41 P20 121.0(3) . . ? C46 C41 P20 119.4(3) . . ? C41 C42 C43 119.7(4) . . ? C44 C43 C42 120.8(4) . . ? C45 C44 C43 119.8(4) . . ? C44 C45 C46 119.9(4) . . ? C45 C46 C41 120.8(4) . . ? C61 P50 C71 105.59(18) . . ? C61 P50 C51 104.99(18) . . ? C71 P50 C51 107.03(18) . . ? C61 P50 Os 116.52(13) . . ? C71 P50 Os 115.41(13) . . ? C51 P50 Os 106.48(12) . . ? C52 C51 C56 119.1(4) . . ? C52 C51 P50 120.9(3) . . ? C56 C51 P50 119.3(3) . . ? C51 C52 C53 119.7(4) . . ? C54 C53 C52 120.5(4) . . ? C53 C54 C55 120.0(4) . . ? C54 C55 C56 120.0(4) . . ? C55 C56 C51 120.7(4) . . ? C66 C61 C62 118.9(4) . . ? C66 C61 P50 121.4(3) . . ? C62 C61 P50 119.6(3) . . ? C63 C62 C61 119.9(4) . . ? C64 C63 C62 120.9(4) . . ? C63 C64 C65 119.6(4) . . ? C66 C65 C64 120.3(4) . . ? C61 C66 C65 120.4(4) . . ? C72 C71 C76 119.3(3) . . ? C72 C71 P50 122.0(3) . . ? C76 C71 P50 118.7(3) . . ? C73 C72 C71 120.1(4) . . ? C74 C73 C72 120.3(4) . . ? C73 C74 C75 119.8(4) . . ? C76 C75 C74 120.2(4) . . ? C75 C76 C71 120.3(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.959 _refine_diff_density_min -3.001 _refine_diff_density_rms 0.208