# Electronic Supplementary Material (ESI) for Chemical Communications # 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_ea428 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H59 Cl O Os P2' _chemical_formula_weight 927.53 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8261(3) _cell_length_b 13.8895(3) _cell_length_c 14.4115(3) _cell_angle_alpha 83.893(2) _cell_angle_beta 78.095(2) _cell_angle_gamma 86.848(2) _cell_volume 2107.18(9) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 8422 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.288 _exptl_crystal_size_mid 0.176 _exptl_crystal_size_min 0.147 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 3.199 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.55591 _exptl_absorpt_correction_T_max 0.71718 _exptl_absorpt_process_details 'Alcock(1970) crystallographic computing,p271' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(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 'CCD Saphire 3 Xcalibur' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 19.64 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21911 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0885 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8436 _reflns_number_gt 6381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.35.11' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.35.11' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.35.11' _computing_structure_solution 'SIR-97_(Altomare & al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'MERCURY 2.4.5(CCDC, 2011)' _computing_publication_material 'WINGX (Farrugia, 1999)' _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^)+(0.0281P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8436 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.004 _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 Os1 Os -0.26365(2) 0.479520(13) 0.245581(13) 0.02507(7) Uani 1 1 d . . . Cl1 Cl -0.25696(13) 0.56184(8) 0.08785(8) 0.0358(3) Uani 1 1 d . . . P1 P -0.11559(14) 0.59181(8) 0.26936(9) 0.0292(3) Uani 1 1 d . . . P2 P -0.44575(14) 0.39875(9) 0.22760(9) 0.0375(4) Uani 1 1 d . . . O1 O -0.2870(4) 0.4012(2) 0.4456(2) 0.0421(10) Uani 1 1 d . . . C1 C -0.1371(5) 0.3769(3) 0.2003(3) 0.0262(11) Uani 1 1 d . . . H1 H -0.1017 0.3886 0.1342 0.031 Uiso 1 1 calc R . . C2 C -0.0891(5) 0.2951(3) 0.2398(3) 0.0255(11) Uani 1 1 d . . . H2 H -0.1240 0.2770 0.3050 0.031 Uiso 1 1 calc R . . C3 C 0.0102(5) 0.2311(3) 0.1938(3) 0.0229(11) Uani 1 1 d . . . C4 C 0.0879(5) 0.2572(3) 0.1037(3) 0.0275(12) Uani 1 1 d . . . H4 H 0.0697 0.3158 0.0679 0.033 Uiso 1 1 calc R . . C5 C 0.1876(5) 0.1999(3) 0.0681(3) 0.0276(12) Uani 1 1 d . . . H5 H 0.2390 0.2197 0.0080 0.033 Uiso 1 1 calc R . . C6 C 0.2175(5) 0.1113(3) 0.1179(3) 0.0244(11) Uani 1 1 d . . . C7 C 0.3317(5) 0.0587(3) 0.0876(3) 0.0318(12) Uani 1 1 d . . . H7 H 0.3851 0.0791 0.0285 0.038 Uiso 1 1 calc R . . C8 C 0.3661(5) -0.0200(3) 0.1413(3) 0.0347(13) Uani 1 1 d . . . H8 H 0.4458 -0.0517 0.1214 0.042 Uiso 1 1 calc R . . C9 C 0.2848(5) -0.0560(3) 0.2270(3) 0.0296(12) Uani 1 1 d . . . C10 C 0.3286(6) -0.1320(3) 0.2884(4) 0.0399(14) Uani 1 1 d . . . H10 H 0.4083 -0.1637 0.2686 0.048 Uiso 1 1 calc R . . C11 C 0.2565(6) -0.1587(3) 0.3744(4) 0.0360(14) Uani 1 1 d . . . H11 H 0.2920 -0.2009 0.4191 0.043 Uiso 1 1 calc R . . C12 C 0.1293(5) -0.1254(3) 0.3996(3) 0.0281(12) Uani 1 1 d . . . C13 C 0.0543(6) -0.1528(3) 0.4907(3) 0.0319(13) Uani 1 1 d . . . H13 H 0.0907 -0.1934 0.5361 0.038 Uiso 1 1 calc R . . C14 C -0.0664(5) -0.1227(3) 0.5139(3) 0.0313(13) Uani 1 1 d . . . H14 H -0.1106 -0.1331 0.5781 0.038 Uiso 1 1 calc R . . C15 C -0.1298(5) -0.0750(3) 0.4434(3) 0.0257(11) Uani 1 1 d . . . C16 C -0.2610(5) -0.0542(3) 0.4668(3) 0.0324(13) Uani 1 1 d . . . H16 H -0.3036 -0.0641 0.5315 0.039 Uiso 1 1 calc R . . C17 C -0.3276(5) -0.0206(3) 0.3999(3) 0.0334(13) Uani 1 1 d . . . H17 H -0.4148 -0.0036 0.4179 0.040 Uiso 1 1 calc R . . C18 C -0.2663(5) -0.0109(3) 0.3020(3) 0.0271(12) Uani 1 1 d . . . C19 C -0.3382(5) 0.0116(3) 0.2307(4) 0.0336(13) Uani 1 1 d . . . H19 H -0.4262 0.0259 0.2486 0.040 Uiso 1 1 calc R . . C20 C -0.2828(6) 0.0131(3) 0.1364(4) 0.0351(13) Uani 1 1 d . . . H20 H -0.3316 0.0303 0.0890 0.042 Uiso 1 1 calc R . . C21 C -0.1551(5) -0.0106(3) 0.1100(3) 0.0319(12) Uani 1 1 d . . . H21 H -0.1176 -0.0121 0.0444 0.038 Uiso 1 1 calc R . . C22 C -0.0827(5) -0.0317(3) 0.1769(3) 0.0257(11) Uani 1 1 d . . . H22 H 0.0045 -0.0479 0.1569 0.031 Uiso 1 1 calc R . . C23 C -0.1342(5) -0.0301(3) 0.2756(3) 0.0216(11) Uani 1 1 d . . . C24 C -0.0609(5) -0.0525(3) 0.3491(3) 0.0221(11) Uani 1 1 d . . . C25 C 0.0749(5) -0.0627(3) 0.3325(3) 0.0244(11) Uani 1 1 d . . . C26 C 0.1621(5) -0.0150(3) 0.2534(3) 0.0239(11) Uani 1 1 d . . . C27 C 0.1358(5) 0.0790(3) 0.2033(3) 0.0230(11) Uani 1 1 d . . . C28 C 0.0349(4) 0.1413(3) 0.2401(3) 0.0217(10) Uani 1 1 d . . . H28 H -0.0187 0.1211 0.2992 0.026 Uiso 1 1 calc R . . C29 C -0.2786(5) 0.4286(3) 0.3696(4) 0.0358(13) Uani 1 1 d . . . C30 C -0.2082(5) 0.6994(3) 0.3159(4) 0.0364(13) Uani 1 1 d . . . H30 H -0.1467 0.7485 0.3216 0.044 Uiso 1 1 calc R . . C31 C -0.2913(6) 0.7461(3) 0.2481(4) 0.0480(16) Uani 1 1 d . . . H31A H -0.2389 0.7616 0.1848 0.072 Uiso 1 1 calc R . . H31B H -0.3323 0.8057 0.2724 0.072 Uiso 1 1 calc R . . H31C H -0.3559 0.7009 0.2439 0.072 Uiso 1 1 calc R . . C32 C -0.2893(6) 0.6751(4) 0.4151(4) 0.0586(18) Uani 1 1 d . . . H32A H -0.2353 0.6469 0.4585 0.088 Uiso 1 1 calc R . . H32B H -0.3524 0.6284 0.4114 0.088 Uiso 1 1 calc R . . H32C H -0.3320 0.7343 0.4388 0.088 Uiso 1 1 calc R . . C33 C -0.0094(5) 0.6442(3) 0.1604(3) 0.0324(12) Uani 1 1 d . . . H33 H -0.0670 0.6731 0.1179 0.039 Uiso 1 1 calc R . . C34 C 0.0720(6) 0.7279(3) 0.1713(4) 0.0511(16) Uani 1 1 d . . . H34A H 0.0180 0.7781 0.2038 0.077 Uiso 1 1 calc R . . H34B H 0.1150 0.7553 0.1082 0.077 Uiso 1 1 calc R . . H34C H 0.1349 0.7035 0.2089 0.077 Uiso 1 1 calc R . . C35 C 0.0715(6) 0.5697(3) 0.1047(4) 0.0546(17) Uani 1 1 d . . . H35A H 0.0200 0.5150 0.1007 0.082 Uiso 1 1 calc R . . H35B H 0.1405 0.5467 0.1369 0.082 Uiso 1 1 calc R . . H35C H 0.1066 0.5989 0.0404 0.082 Uiso 1 1 calc R . . C36 C -0.0251(5) 0.5517(3) 0.3633(3) 0.0321(12) Uani 1 1 d . . . H36 H -0.0891 0.5255 0.4194 0.039 Uiso 1 1 calc R . . C37 C 0.0413(7) 0.6297(4) 0.3998(5) 0.071(2) Uani 1 1 d . . . H37A H -0.0178 0.6846 0.4146 0.107 Uiso 1 1 calc R . . H37B H 0.1139 0.6517 0.3508 0.107 Uiso 1 1 calc R . . H37C H 0.0705 0.6029 0.4576 0.107 Uiso 1 1 calc R . . C38 C 0.0660(6) 0.4677(4) 0.3378(4) 0.0517(17) Uani 1 1 d . . . H38A H 0.0216 0.4168 0.3170 0.077 Uiso 1 1 calc R . . H38B H 0.1000 0.4418 0.3937 0.077 Uiso 1 1 calc R . . H38C H 0.1354 0.4900 0.2861 0.077 Uiso 1 1 calc R . . C39 C -0.5018(7) 0.2970(6) 0.3169(6) 0.116(4) Uani 1 1 d . . . H39 H -0.5240 0.3348 0.3737 0.140 Uiso 1 1 calc R . . C40 C -0.4167(6) 0.2320(4) 0.3506(5) 0.068(2) Uani 1 1 d . . . H40A H -0.3321 0.2585 0.3333 0.103 Uiso 1 1 calc R . . H40B H -0.4163 0.1707 0.3225 0.103 Uiso 1 1 calc R . . H40C H -0.4413 0.2206 0.4202 0.103 Uiso 1 1 calc R . . C41 C -0.6317(6) 0.2600(5) 0.3213(5) 0.078(2) Uani 1 1 d . . . H41A H -0.6715 0.2984 0.2736 0.117 Uiso 1 1 calc R . . H41B H -0.6835 0.2656 0.3849 0.117 Uiso 1 1 calc R . . H41C H -0.6244 0.1919 0.3081 0.117 Uiso 1 1 calc R . . C42 C -0.4432(5) 0.3620(3) 0.1080(4) 0.0410(15) Uani 1 1 d . . . H42 H -0.4143 0.4194 0.0622 0.049 Uiso 1 1 calc R . . C43 C -0.3468(6) 0.2816(4) 0.0827(5) 0.072(2) Uani 1 1 d . . . H43A H -0.2646 0.2997 0.0926 0.109 Uiso 1 1 calc R . . H43B H -0.3401 0.2707 0.0157 0.109 Uiso 1 1 calc R . . H43C H -0.3731 0.2221 0.1233 0.109 Uiso 1 1 calc R . . C44 C -0.5689(6) 0.3358(4) 0.0875(4) 0.0630(19) Uani 1 1 d . . . H44A H -0.6340 0.3845 0.1101 0.095 Uiso 1 1 calc R . . H44B H -0.5928 0.2721 0.1204 0.095 Uiso 1 1 calc R . . H44C H -0.5608 0.3338 0.0187 0.095 Uiso 1 1 calc R . . C45 C -0.5802(6) 0.4866(5) 0.2479(4) 0.0589(17) Uani 1 1 d . . . H45 H -0.6590 0.4506 0.2520 0.071 Uiso 1 1 calc R . . C46 C -0.5779(6) 0.5696(4) 0.1710(5) 0.068(2) Uani 1 1 d . . . H46A H -0.5755 0.5440 0.1098 0.103 Uiso 1 1 calc R . . H46B H -0.5029 0.6075 0.1666 0.103 Uiso 1 1 calc R . . H46C H -0.6540 0.6111 0.1866 0.103 Uiso 1 1 calc R . . C47 C -0.5898(7) 0.5296(6) 0.3445(5) 0.100(3) Uani 1 1 d . . . H47A H -0.5914 0.4768 0.3955 0.149 Uiso 1 1 calc R . . H47B H -0.6674 0.5699 0.3578 0.149 Uiso 1 1 calc R . . H47C H -0.5165 0.5693 0.3410 0.149 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 Os1 0.02402(14) 0.02619(10) 0.02425(10) 0.00185(7) -0.00469(8) -0.00334(8) Cl1 0.0349(9) 0.0360(6) 0.0352(7) 0.0057(5) -0.0076(6) -0.0060(6) P1 0.0308(9) 0.0247(6) 0.0315(7) -0.0025(5) -0.0049(6) -0.0021(6) P2 0.0302(10) 0.0496(8) 0.0318(7) 0.0147(6) -0.0096(7) -0.0164(7) O1 0.045(3) 0.051(2) 0.030(2) -0.0073(17) -0.0025(19) -0.0084(19) C1 0.032(4) 0.027(2) 0.020(2) 0.0003(18) -0.003(2) -0.011(2) C2 0.030(3) 0.027(2) 0.019(2) 0.0016(18) -0.004(2) -0.005(2) C3 0.025(3) 0.024(2) 0.021(2) -0.0013(18) -0.005(2) -0.006(2) C4 0.027(4) 0.030(2) 0.025(2) 0.0053(19) -0.007(2) -0.006(2) C5 0.026(4) 0.035(3) 0.020(2) 0.000(2) -0.001(2) -0.013(2) C6 0.015(3) 0.031(2) 0.030(3) -0.012(2) -0.005(2) -0.004(2) C7 0.026(4) 0.042(3) 0.026(3) -0.008(2) 0.003(2) -0.007(3) C8 0.019(4) 0.042(3) 0.043(3) -0.017(2) -0.001(3) 0.002(2) C9 0.025(4) 0.030(2) 0.037(3) -0.012(2) -0.010(3) 0.002(2) C10 0.037(4) 0.037(3) 0.051(3) -0.013(3) -0.017(3) 0.009(3) C11 0.043(4) 0.029(3) 0.040(3) -0.003(2) -0.020(3) 0.003(3) C12 0.029(4) 0.023(2) 0.036(3) -0.010(2) -0.011(3) 0.000(2) C13 0.049(4) 0.023(2) 0.027(3) 0.0009(19) -0.018(3) -0.004(2) C14 0.048(4) 0.024(2) 0.022(2) -0.0026(19) -0.006(3) -0.008(2) C15 0.031(4) 0.019(2) 0.026(2) -0.0031(18) -0.002(2) -0.007(2) C16 0.041(4) 0.024(2) 0.028(3) -0.001(2) 0.005(3) -0.010(2) C17 0.025(4) 0.026(2) 0.046(3) -0.008(2) 0.004(3) -0.003(2) C18 0.027(4) 0.018(2) 0.037(3) -0.0043(19) -0.003(3) -0.007(2) C19 0.019(4) 0.031(3) 0.053(3) -0.006(2) -0.013(3) -0.002(2) C20 0.038(4) 0.034(3) 0.039(3) -0.003(2) -0.017(3) -0.008(3) C21 0.033(4) 0.034(3) 0.029(3) -0.002(2) -0.007(3) -0.009(2) C22 0.026(3) 0.020(2) 0.031(3) -0.0034(19) -0.004(2) -0.005(2) C23 0.022(3) 0.013(2) 0.029(2) -0.0033(18) -0.003(2) -0.007(2) C24 0.026(4) 0.013(2) 0.028(2) -0.0064(17) -0.005(2) -0.003(2) C25 0.033(4) 0.020(2) 0.024(2) -0.0074(18) -0.009(2) -0.004(2) C26 0.018(3) 0.029(2) 0.027(3) -0.011(2) -0.006(2) -0.002(2) C27 0.026(3) 0.025(2) 0.022(2) -0.0056(19) -0.010(2) -0.007(2) C28 0.018(3) 0.027(2) 0.020(2) -0.0011(18) -0.003(2) -0.009(2) C29 0.022(4) 0.024(2) 0.066(4) -0.015(3) -0.014(3) 0.000(2) C30 0.035(4) 0.025(2) 0.049(3) -0.007(2) -0.005(3) 0.000(2) C31 0.044(4) 0.037(3) 0.065(4) -0.008(3) -0.014(3) 0.004(3) C32 0.070(5) 0.042(3) 0.058(4) -0.012(3) 0.000(4) 0.012(3) C33 0.030(4) 0.030(2) 0.037(3) -0.008(2) -0.004(3) -0.002(2) C34 0.046(5) 0.033(3) 0.064(4) -0.006(3) 0.015(3) -0.005(3) C35 0.059(5) 0.047(3) 0.049(3) -0.018(3) 0.021(3) -0.025(3) C36 0.036(4) 0.033(3) 0.031(3) -0.010(2) -0.010(3) -0.002(2) C37 0.097(6) 0.052(3) 0.086(5) -0.004(3) -0.065(5) -0.018(4) C38 0.048(5) 0.057(3) 0.061(4) -0.022(3) -0.031(3) 0.012(3) C39 0.062(6) 0.158(7) 0.124(7) 0.117(6) -0.057(6) -0.070(6) C40 0.043(5) 0.039(3) 0.110(6) 0.027(3) -0.001(4) -0.007(3) C41 0.046(5) 0.097(5) 0.086(5) 0.058(4) -0.025(4) -0.048(4) C42 0.042(4) 0.042(3) 0.044(3) 0.005(2) -0.022(3) -0.017(3) C43 0.061(5) 0.073(4) 0.101(5) -0.047(4) -0.043(5) 0.008(4) C44 0.060(5) 0.074(4) 0.061(4) 0.016(3) -0.030(4) -0.031(4) C45 0.027(4) 0.106(5) 0.042(3) -0.003(3) -0.001(3) -0.014(4) C46 0.033(5) 0.072(4) 0.097(5) -0.007(4) -0.011(4) 0.018(3) C47 0.050(6) 0.168(8) 0.083(5) -0.053(5) -0.006(5) 0.024(6) _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 Os1 C29 1.829(6) . ? Os1 C1 1.988(5) . ? Os1 P2 2.3933(14) . ? Os1 P1 2.3947(13) . ? Os1 Cl1 2.4224(11) . ? P1 C33 1.850(5) . ? P1 C36 1.852(4) . ? P1 C30 1.860(5) . ? P2 C42 1.843(5) . ? P2 C45 1.843(6) . ? P2 C39 1.846(6) . ? O1 C29 1.108(6) . ? C1 C2 1.343(5) . ? C1 H1 0.9500 . ? C2 C3 1.453(6) . ? C2 H2 0.9500 . ? C3 C28 1.390(5) . ? C3 C4 1.417(6) . ? C4 C5 1.352(6) . ? C4 H4 0.9500 . ? C5 C6 1.413(6) . ? C5 H5 0.9500 . ? C6 C27 1.406(6) . ? C6 C7 1.413(6) . ? C7 C8 1.352(6) . ? C7 H7 0.9500 . ? C8 C9 1.421(7) . ? C8 H8 0.9500 . ? C9 C26 1.410(7) . ? C9 C10 1.428(6) . ? C10 C11 1.348(7) . ? C10 H10 0.9500 . ? C11 C12 1.415(7) . ? C11 H11 0.9500 . ? C12 C13 1.420(7) . ? C12 C25 1.428(6) . ? C13 C14 1.336(7) . ? C13 H13 0.9500 . ? C14 C15 1.427(6) . ? C14 H14 0.9500 . ? C15 C16 1.411(7) . ? C15 C24 1.420(6) . ? C16 C17 1.350(6) . ? C16 H16 0.9500 . ? C17 C18 1.425(7) . ? C17 H17 0.9500 . ? C18 C19 1.411(6) . ? C18 C23 1.419(7) . ? C19 C20 1.367(7) . ? C19 H19 0.9500 . ? C20 C21 1.387(7) . ? C20 H20 0.9500 . ? C21 C22 1.362(6) . ? C21 H21 0.9500 . ? C22 C23 1.419(6) . ? C22 H22 0.9500 . ? C23 C24 1.449(6) . ? C24 C25 1.442(7) . ? C25 C26 1.447(6) . ? C26 C27 1.466(5) . ? C27 C28 1.407(6) . ? C28 H28 0.9500 . ? C30 C32 1.529(7) . ? C30 C31 1.533(6) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.506(7) . ? C33 C34 1.537(6) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C38 1.511(6) . ? C36 C37 1.527(6) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.378(8) . ? C39 C41 1.511(8) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.507(7) . ? C42 C44 1.522(7) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.509(7) . ? C45 C47 1.555(8) . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? 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 C29 Os1 C1 91.83(19) . . ? C29 Os1 P2 92.30(15) . . ? C1 Os1 P2 96.68(13) . . ? C29 Os1 P1 89.69(15) . . ? C1 Os1 P1 96.50(13) . . ? P2 Os1 P1 166.61(5) . . ? C29 Os1 Cl1 173.87(15) . . ? C1 Os1 Cl1 94.20(12) . . ? P2 Os1 Cl1 88.07(4) . . ? P1 Os1 Cl1 88.56(4) . . ? C33 P1 C36 110.5(2) . . ? C33 P1 C30 103.1(2) . . ? C36 P1 C30 102.8(2) . . ? C33 P1 Os1 115.81(15) . . ? C36 P1 Os1 115.67(15) . . ? C30 P1 Os1 107.18(18) . . ? C42 P2 C45 104.4(2) . . ? C42 P2 C39 108.6(4) . . ? C45 P2 C39 101.8(4) . . ? C42 P2 Os1 116.04(19) . . ? C45 P2 Os1 106.8(2) . . ? C39 P2 Os1 117.4(2) . . ? C2 C1 Os1 135.9(4) . . ? C2 C1 H1 112.0 . . ? Os1 C1 H1 112.0 . . ? C1 C2 C3 127.2(4) . . ? C1 C2 H2 116.4 . . ? C3 C2 H2 116.4 . . ? C28 C3 C4 117.4(4) . . ? C28 C3 C2 119.8(4) . . ? C4 C3 C2 122.8(4) . . ? C5 C4 C3 120.8(4) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 121.8(4) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C27 C6 C5 118.8(4) . . ? C27 C6 C7 119.5(4) . . ? C5 C6 C7 121.5(5) . . ? C8 C7 C6 121.1(5) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 120.9(5) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C26 C9 C8 120.3(4) . . ? C26 C9 C10 119.7(5) . . ? C8 C9 C10 120.0(5) . . ? C11 C10 C9 119.9(5) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 121.5(5) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C13 121.3(4) . . ? C11 C12 C25 119.6(5) . . ? C13 C12 C25 119.1(5) . . ? C14 C13 C12 121.2(4) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 120.8(4) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C24 120.6(4) . . ? C16 C15 C14 119.9(4) . . ? C24 C15 C14 119.5(5) . . ? C17 C16 C15 121.8(4) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 119.6(5) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C23 119.8(4) . . ? C19 C18 C17 119.9(5) . . ? C23 C18 C17 120.2(4) . . ? C20 C19 C18 120.8(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.8(5) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 120.8(5) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 121.7(5) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 116.9(4) . . ? C22 C23 C24 123.5(4) . . ? C18 C23 C24 119.5(4) . . ? C15 C24 C25 118.0(4) . . ? C15 C24 C23 116.7(4) . . ? C25 C24 C23 125.1(4) . . ? C12 C25 C24 117.6(4) . . ? C12 C25 C26 116.6(4) . . ? C24 C25 C26 125.8(4) . . ? C9 C26 C25 118.9(4) . . ? C9 C26 C27 116.6(4) . . ? C25 C26 C27 124.3(4) . . ? C28 C27 C6 118.1(4) . . ? C28 C27 C26 122.4(4) . . ? C6 C27 C26 119.5(4) . . ? C3 C28 C27 122.8(4) . . ? C3 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? O1 C29 Os1 177.3(4) . . ? C32 C30 C31 109.8(5) . . ? C32 C30 P1 112.0(3) . . ? C31 C30 P1 112.2(3) . . ? C32 C30 H30 107.5 . . ? C31 C30 H30 107.5 . . ? P1 C30 H30 107.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C34 109.8(4) . . ? C35 C33 P1 113.7(3) . . ? C34 C33 P1 117.0(3) . . ? C35 C33 H33 105.0 . . ? C34 C33 H33 105.0 . . ? P1 C33 H33 105.0 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 C37 110.0(5) . . ? C38 C36 P1 112.7(3) . . ? C37 C36 P1 117.0(3) . . ? C38 C36 H36 105.4 . . ? C37 C36 H36 105.4 . . ? P1 C36 H36 105.4 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C41 116.2(5) . . ? C40 C39 P2 120.4(5) . . ? C41 C39 P2 118.4(4) . . ? C40 C39 H39 97.5 . . ? C41 C39 H39 97.5 . . ? P2 C39 H39 97.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C44 109.2(4) . . ? C43 C42 P2 112.2(3) . . ? C44 C42 P2 116.7(4) . . ? C43 C42 H42 106.0 . . ? C44 C42 H42 106.0 . . ? P2 C42 H42 106.0 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C47 108.2(6) . . ? C46 C45 P2 115.1(4) . . ? C47 C45 P2 110.6(4) . . ? C46 C45 H45 107.6 . . ? C47 C45 H45 107.6 . . ? P2 C45 H45 107.6 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C29 Os1 P1 C33 158.6(2) . . . . ? C1 Os1 P1 C33 66.7(2) . . . . ? P2 Os1 P1 C33 -102.8(3) . . . . ? Cl1 Os1 P1 C33 -27.32(18) . . . . ? C29 Os1 P1 C36 26.9(2) . . . . ? C1 Os1 P1 C36 -64.9(2) . . . . ? P2 Os1 P1 C36 125.6(2) . . . . ? Cl1 Os1 P1 C36 -158.97(18) . . . . ? C29 Os1 P1 C30 -87.0(2) . . . . ? C1 Os1 P1 C30 -178.9(2) . . . . ? P2 Os1 P1 C30 11.6(3) . . . . ? Cl1 Os1 P1 C30 87.07(17) . . . . ? C29 Os1 P2 C42 -147.8(2) . . . . ? C1 Os1 P2 C42 -55.7(2) . . . . ? P1 Os1 P2 C42 113.9(3) . . . . ? Cl1 Os1 P2 C42 38.33(19) . . . . ? C29 Os1 P2 C45 96.3(2) . . . . ? C1 Os1 P2 C45 -171.5(2) . . . . ? P1 Os1 P2 C45 -2.0(3) . . . . ? Cl1 Os1 P2 C45 -77.54(19) . . . . ? C29 Os1 P2 C39 -17.0(4) . . . . ? C1 Os1 P2 C39 75.1(4) . . . . ? P1 Os1 P2 C39 -115.3(4) . . . . ? Cl1 Os1 P2 C39 169.1(4) . . . . ? C29 Os1 C1 C2 6.8(5) . . . . ? P2 Os1 C1 C2 -85.7(5) . . . . ? P1 Os1 C1 C2 96.7(5) . . . . ? Cl1 Os1 C1 C2 -174.2(5) . . . . ? Os1 C1 C2 C3 -176.5(3) . . . . ? C1 C2 C3 C28 -169.6(4) . . . . ? C1 C2 C3 C4 12.7(7) . . . . ? C28 C3 C4 C5 -4.8(6) . . . . ? C2 C3 C4 C5 173.0(4) . . . . ? C3 C4 C5 C6 1.1(6) . . . . ? C4 C5 C6 C27 4.7(6) . . . . ? C4 C5 C6 C7 -170.5(4) . . . . ? C27 C6 C7 C8 -2.6(6) . . . . ? C5 C6 C7 C8 172.5(4) . . . . ? C6 C7 C8 C9 4.0(7) . . . . ? C7 C8 C9 C26 5.3(7) . . . . ? C7 C8 C9 C10 -172.7(4) . . . . ? C26 C9 C10 C11 -5.3(7) . . . . ? C8 C9 C10 C11 172.7(4) . . . . ? C9 C10 C11 C12 11.0(7) . . . . ? C10 C11 C12 C13 -179.2(4) . . . . ? C10 C11 C12 C25 0.6(7) . . . . ? C11 C12 C13 C14 -178.8(4) . . . . ? C25 C12 C13 C14 1.4(6) . . . . ? C12 C13 C14 C15 10.1(6) . . . . ? C13 C14 C15 C16 172.4(4) . . . . ? C13 C14 C15 C24 -5.0(6) . . . . ? C24 C15 C16 C17 5.9(6) . . . . ? C14 C15 C16 C17 -171.4(4) . . . . ? C15 C16 C17 C18 3.7(6) . . . . ? C16 C17 C18 C19 171.5(4) . . . . ? C16 C17 C18 C23 -4.2(6) . . . . ? C23 C18 C19 C20 1.5(6) . . . . ? C17 C18 C19 C20 -174.4(4) . . . . ? C18 C19 C20 C21 2.0(7) . . . . ? C19 C20 C21 C22 -2.6(7) . . . . ? C20 C21 C22 C23 -0.2(6) . . . . ? C21 C22 C23 C18 3.5(6) . . . . ? C21 C22 C23 C24 179.7(4) . . . . ? C19 C18 C23 C22 -4.1(6) . . . . ? C17 C18 C23 C22 171.7(4) . . . . ? C19 C18 C23 C24 179.6(4) . . . . ? C17 C18 C23 C24 -4.6(6) . . . . ? C16 C15 C24 C25 171.5(4) . . . . ? C14 C15 C24 C25 -11.2(6) . . . . ? C16 C15 C24 C23 -14.3(6) . . . . ? C14 C15 C24 C23 163.0(3) . . . . ? C22 C23 C24 C15 -162.5(4) . . . . ? C18 C23 C24 C15 13.5(5) . . . . ? C22 C23 C24 C25 11.2(6) . . . . ? C18 C23 C24 C25 -172.7(4) . . . . ? C11 C12 C25 C24 162.8(4) . . . . ? C13 C12 C25 C24 -17.4(6) . . . . ? C11 C12 C25 C26 -17.2(6) . . . . ? C13 C12 C25 C26 162.6(4) . . . . ? C15 C24 C25 C12 22.0(5) . . . . ? C23 C24 C25 C12 -151.7(4) . . . . ? C15 C24 C25 C26 -158.0(4) . . . . ? C23 C24 C25 C26 28.3(6) . . . . ? C8 C9 C26 C25 170.3(4) . . . . ? C10 C9 C26 C25 -11.7(6) . . . . ? C8 C9 C26 C27 -15.1(6) . . . . ? C10 C9 C26 C27 162.9(4) . . . . ? C12 C25 C26 C9 22.5(6) . . . . ? C24 C25 C26 C9 -157.5(4) . . . . ? C12 C25 C26 C27 -151.7(4) . . . . ? C24 C25 C26 C27 28.4(6) . . . . ? C5 C6 C27 C28 -6.3(6) . . . . ? C7 C6 C27 C28 168.9(4) . . . . ? C5 C6 C27 C26 177.0(4) . . . . ? C7 C6 C27 C26 -7.7(6) . . . . ? C9 C26 C27 C28 -160.2(4) . . . . ? C25 C26 C27 C28 14.1(6) . . . . ? C9 C26 C27 C6 16.3(6) . . . . ? C25 C26 C27 C6 -169.4(4) . . . . ? C4 C3 C28 C27 3.0(6) . . . . ? C2 C3 C28 C27 -174.9(4) . . . . ? C6 C27 C28 C3 2.6(6) . . . . ? C26 C27 C28 C3 179.1(4) . . . . ? C1 Os1 C29 O1 130(11) . . . . ? P2 Os1 C29 O1 -133(11) . . . . ? P1 Os1 C29 O1 34(11) . . . . ? Cl1 Os1 C29 O1 -40(12) . . . . ? C33 P1 C30 C32 -171.4(4) . . . . ? C36 P1 C30 C32 -56.4(4) . . . . ? Os1 P1 C30 C32 66.0(4) . . . . ? C33 P1 C30 C31 64.6(4) . . . . ? C36 P1 C30 C31 179.6(4) . . . . ? Os1 P1 C30 C31 -58.1(4) . . . . ? C36 P1 C33 C35 74.4(4) . . . . ? C30 P1 C33 C35 -176.3(4) . . . . ? Os1 P1 C33 C35 -59.6(4) . . . . ? C36 P1 C33 C34 -55.3(4) . . . . ? C30 P1 C33 C34 54.0(4) . . . . ? Os1 P1 C33 C34 170.7(3) . . . . ? C33 P1 C36 C38 -66.4(4) . . . . ? C30 P1 C36 C38 -175.9(4) . . . . ? Os1 P1 C36 C38 67.7(4) . . . . ? C33 P1 C36 C37 62.6(5) . . . . ? C30 P1 C36 C37 -46.9(5) . . . . ? Os1 P1 C36 C37 -163.3(4) . . . . ? C42 P2 C39 C40 94.3(8) . . . . ? C45 P2 C39 C40 -156.0(8) . . . . ? Os1 P2 C39 C40 -39.9(9) . . . . ? C42 P2 C39 C41 -59.8(9) . . . . ? C45 P2 C39 C41 49.9(8) . . . . ? Os1 P2 C39 C41 166.0(6) . . . . ? C45 P2 C42 C43 -173.9(4) . . . . ? C39 P2 C42 C43 -66.0(5) . . . . ? Os1 P2 C42 C43 68.9(4) . . . . ? C45 P2 C42 C44 -46.9(5) . . . . ? C39 P2 C42 C44 61.0(5) . . . . ? Os1 P2 C42 C44 -164.1(3) . . . . ? C42 P2 C45 C46 -53.5(5) . . . . ? C39 P2 C45 C46 -166.4(5) . . . . ? Os1 P2 C45 C46 69.9(4) . . . . ? C42 P2 C45 C47 -176.4(5) . . . . ? C39 P2 C45 C47 70.6(6) . . . . ? Os1 P2 C45 C47 -53.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.354 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.119 _database_code_depnum_ccdc_archive 'CCDC 870662'