# 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_enrique105 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H57 B O3 Os P2 S' _chemical_formula_weight 700.72 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' 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' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 9.0107(5) _cell_length_b 11.3802(6) _cell_length_c 16.2396(8) _cell_angle_alpha 96.9060(10) _cell_angle_beta 96.1840(10) _cell_angle_gamma 106.0440(10) _cell_volume 1571.36(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9606 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description 'irregular block' _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 4.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.673 _exptl_absorpt_correction_T_max 0.862 _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). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19347 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.50 _reflns_number_total 7308 _reflns_number_gt 6790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'apex2 v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.14 (Bruker, 2000)' _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. The structures of all compounds was solved by direct methods. Refinement, by full-matrix least squares on F2 with SHELXL97,2 was similar for all complexes, including isotropic and subsequently anisotropic displacement parameters. The C-H hydrogen atoms were calculated and refined using a restricted riding model. The hydrides h1, h2 and h3 were located in de last diference fourier map, but does not refined properly. By this reason, the osmium-hydride distances were refined with restrains: dfix 1.59 0.01 os h1 os h2 os h3 and free displacement parameters. ; _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^)+(0.0228P)^2^+0.9360P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7308 _refine_ls_number_parameters 326 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0540 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _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 0.342638(12) 0.214181(10) 0.209426(7) 0.01516(4) Uani 1 1 d D . . H3 H 0.410(5) 0.341(3) 0.273(3) 0.074(16) Uiso 1 1 d D . . H2 H 0.440(5) 0.282(5) 0.2982(17) 0.09(2) Uiso 1 1 d D . . H1 H 0.248(4) 0.107(3) 0.1371(18) 0.058(13) Uiso 1 1 d D . . P1 P 0.46033(8) 0.06430(7) 0.25497(4) 0.01506(14) Uani 1 1 d . . . P2 P 0.20750(8) 0.33986(7) 0.14456(5) 0.01621(14) Uani 1 1 d . . . S1 S 0.12212(8) 0.14218(7) 0.28809(4) 0.01737(14) Uani 1 1 d . . . O1 O 0.2862(2) 0.31080(18) 0.43534(12) 0.0191(4) Uani 1 1 d . . . O2 O 0.0500(2) 0.17725(19) 0.44766(12) 0.0207(4) Uani 1 1 d . . . O3 O 0.5890(3) 0.2801(2) 0.09801(15) 0.0316(5) Uani 1 1 d . . . B1 B 0.1578(4) 0.2155(3) 0.3948(2) 0.0172(6) Uani 1 1 d . . . C1 C 0.2510(3) 0.3493(3) 0.51829(18) 0.0208(6) Uani 1 1 d . . . C2 C 0.1872(4) 0.4594(3) 0.5118(2) 0.0274(7) Uani 1 1 d . . . H2A H 0.2629 0.5242 0.4907 0.041 Uiso 1 1 calc R . . H2B H 0.1693 0.4918 0.5674 0.041 Uiso 1 1 calc R . . H2C H 0.0885 0.4327 0.4732 0.041 Uiso 1 1 calc R . . C3 C 0.4000(4) 0.3883(3) 0.5808(2) 0.0274(7) Uani 1 1 d . . . H3A H 0.4531 0.3239 0.5754 0.041 Uiso 1 1 calc R . . H3B H 0.3746 0.4002 0.6378 0.041 Uiso 1 1 calc R . . H3C H 0.4687 0.4661 0.5696 0.041 Uiso 1 1 calc R . . C4 C 0.1250(3) 0.2311(3) 0.53289(18) 0.0220(6) Uani 1 1 d . . . C5 C 0.1946(4) 0.1372(3) 0.5678(2) 0.0280(7) Uani 1 1 d . . . H5A H 0.1120 0.0597 0.5659 0.042 Uiso 1 1 calc R . . H5B H 0.2438 0.1695 0.6260 0.042 Uiso 1 1 calc R . . H5C H 0.2732 0.1219 0.5341 0.042 Uiso 1 1 calc R . . C6 C 0.0029(4) 0.2560(4) 0.5840(2) 0.0334(8) Uani 1 1 d . . . H6A H -0.0540 0.3050 0.5552 0.050 Uiso 1 1 calc R . . H6B H 0.0540 0.3020 0.6395 0.050 Uiso 1 1 calc R . . H6C H -0.0703 0.1773 0.5904 0.050 Uiso 1 1 calc R . . C7 C 0.4946(3) 0.2560(3) 0.14226(19) 0.0214(6) Uani 1 1 d . . . C8 C 0.5623(3) 0.0038(3) 0.17339(18) 0.0206(6) Uani 1 1 d . . . H8 H 0.6274 0.0790 0.1542 0.025 Uiso 1 1 calc R . . C9 C 0.4520(4) -0.0710(4) 0.0949(2) 0.0351(8) Uani 1 1 d . . . H9A H 0.5113 -0.0755 0.0481 0.053 Uiso 1 1 calc R . . H9B H 0.3716 -0.0307 0.0808 0.053 Uiso 1 1 calc R . . H9C H 0.4022 -0.1548 0.1055 0.053 Uiso 1 1 calc R . . C10 C 0.6775(4) -0.0656(3) 0.2016(2) 0.0265(7) Uani 1 1 d . . . H10A H 0.6207 -0.1421 0.2201 0.040 Uiso 1 1 calc R . . H10B H 0.7549 -0.0132 0.2481 0.040 Uiso 1 1 calc R . . H10C H 0.7306 -0.0857 0.1546 0.040 Uiso 1 1 calc R . . C11 C 0.6201(3) 0.1257(3) 0.34419(18) 0.0202(6) Uani 1 1 d . . . H11 H 0.6687 0.0583 0.3530 0.024 Uiso 1 1 calc R . . C12 C 0.7468(3) 0.2345(3) 0.3243(2) 0.0262(7) Uani 1 1 d . . . H12A H 0.7031 0.3028 0.3161 0.039 Uiso 1 1 calc R . . H12B H 0.7852 0.2084 0.2730 0.039 Uiso 1 1 calc R . . H12C H 0.8332 0.2619 0.3709 0.039 Uiso 1 1 calc R . . C13 C 0.5627(4) 0.1628(3) 0.42607(19) 0.0257(7) Uani 1 1 d . . . H13A H 0.6517 0.1946 0.4712 0.039 Uiso 1 1 calc R . . H13B H 0.4882 0.0903 0.4405 0.039 Uiso 1 1 calc R . . H13C H 0.5114 0.2272 0.4189 0.039 Uiso 1 1 calc R . . C14 C 0.3235(3) -0.0667(3) 0.29124(18) 0.0183(6) Uani 1 1 d . . . H14 H 0.2759 -0.0275 0.3357 0.022 Uiso 1 1 calc R . . C15 C 0.1863(4) -0.1397(3) 0.2237(2) 0.0273(7) Uani 1 1 d . . . H15A H 0.2215 -0.1940 0.1837 0.041 Uiso 1 1 calc R . . H15B H 0.1463 -0.0820 0.1941 0.041 Uiso 1 1 calc R . . H15C H 0.1032 -0.1898 0.2501 0.041 Uiso 1 1 calc R . . C16 C 0.3976(4) -0.1538(3) 0.3337(2) 0.0267(7) Uani 1 1 d . . . H16A H 0.3186 -0.2112 0.3583 0.040 Uiso 1 1 calc R . . H16B H 0.4826 -0.1052 0.3780 0.040 Uiso 1 1 calc R . . H16C H 0.4393 -0.2007 0.2922 0.040 Uiso 1 1 calc R . . C17 C 0.0661(4) 0.2551(3) 0.05042(19) 0.0249(7) Uani 1 1 d . . . H17 H 0.0143 0.3145 0.0284 0.030 Uiso 1 1 calc R . . C18 C 0.1461(4) 0.2073(3) -0.0196(2) 0.0341(8) Uani 1 1 d . . . H18A H 0.2068 0.1552 0.0019 0.051 Uiso 1 1 calc R . . H18B H 0.2159 0.2777 -0.0389 0.051 Uiso 1 1 calc R . . H18C H 0.0668 0.1586 -0.0665 0.051 Uiso 1 1 calc R . . C19 C -0.0613(4) 0.1490(3) 0.0730(2) 0.0324(8) Uani 1 1 d . . . H19A H -0.1354 0.1065 0.0225 0.049 Uiso 1 1 calc R . . H19B H -0.1165 0.1822 0.1146 0.049 Uiso 1 1 calc R . . H19C H -0.0136 0.0902 0.0965 0.049 Uiso 1 1 calc R . . C20 C 0.3411(4) 0.4649(3) 0.1009(2) 0.0242(7) Uani 1 1 d . . . H20 H 0.3876 0.4210 0.0583 0.029 Uiso 1 1 calc R . . C21 C 0.2639(5) 0.5453(3) 0.0528(2) 0.0405(9) Uani 1 1 d . . . H21A H 0.2280 0.5997 0.0924 0.061 Uiso 1 1 calc R . . H21B H 0.1746 0.4922 0.0128 0.061 Uiso 1 1 calc R . . H21C H 0.3397 0.5957 0.0225 0.061 Uiso 1 1 calc R . . C22 C 0.4808(4) 0.5472(3) 0.1642(2) 0.0336(8) Uani 1 1 d . . . H22A H 0.5566 0.5984 0.1343 0.050 Uiso 1 1 calc R . . H22B H 0.5302 0.4949 0.1943 0.050 Uiso 1 1 calc R . . H22C H 0.4447 0.6007 0.2042 0.050 Uiso 1 1 calc R . . C23 C 0.0850(3) 0.4052(3) 0.21076(19) 0.0214(6) Uani 1 1 d . . . H23 H 0.0226 0.3338 0.2348 0.026 Uiso 1 1 calc R . . C24 C -0.0356(4) 0.4588(3) 0.1679(2) 0.0326(8) Uani 1 1 d . . . H24A H -0.1043 0.4756 0.2077 0.049 Uiso 1 1 calc R . . H24B H -0.0978 0.3991 0.1195 0.049 Uiso 1 1 calc R . . H24C H 0.0182 0.5359 0.1491 0.049 Uiso 1 1 calc R . . C25 C 0.1816(4) 0.4975(3) 0.2864(2) 0.0315(8) Uani 1 1 d . . . H25A H 0.2367 0.5745 0.2678 0.047 Uiso 1 1 calc R . . H25B H 0.2577 0.4625 0.3142 0.047 Uiso 1 1 calc R . . H25C H 0.1125 0.5149 0.3258 0.047 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 0.01460(6) 0.01682(6) 0.01537(6) 0.00513(4) 0.00345(4) 0.00520(4) P1 0.0151(3) 0.0163(3) 0.0145(3) 0.0028(3) 0.0029(3) 0.0052(3) P2 0.0177(3) 0.0157(4) 0.0151(3) 0.0036(3) 0.0012(3) 0.0047(3) S1 0.0158(3) 0.0186(3) 0.0177(3) 0.0030(3) 0.0035(3) 0.0045(3) O1 0.0177(10) 0.0226(11) 0.0174(10) 0.0038(8) 0.0045(8) 0.0057(8) O2 0.0177(10) 0.0272(11) 0.0173(10) 0.0053(9) 0.0047(8) 0.0051(9) O3 0.0311(12) 0.0384(14) 0.0338(13) 0.0184(11) 0.0174(10) 0.0141(11) B1 0.0158(14) 0.0196(16) 0.0181(16) 0.0052(13) 0.0016(12) 0.0080(13) C1 0.0201(14) 0.0251(16) 0.0177(14) 0.0010(12) 0.0039(11) 0.0080(12) C2 0.0340(18) 0.0256(17) 0.0243(16) -0.0008(13) 0.0046(14) 0.0135(14) C3 0.0224(15) 0.0344(18) 0.0219(16) 0.0018(14) -0.0005(13) 0.0051(14) C4 0.0197(14) 0.0299(17) 0.0153(14) 0.0039(12) 0.0032(11) 0.0054(13) C5 0.0266(16) 0.0329(18) 0.0256(17) 0.0129(14) 0.0033(13) 0.0068(14) C6 0.0266(17) 0.050(2) 0.0232(17) 0.0022(16) 0.0092(14) 0.0100(16) C7 0.0244(15) 0.0215(15) 0.0212(15) 0.0065(12) 0.0015(12) 0.0105(12) C8 0.0232(15) 0.0207(15) 0.0206(15) 0.0034(12) 0.0086(12) 0.0084(12) C9 0.0372(19) 0.047(2) 0.0227(17) -0.0045(15) 0.0047(14) 0.0194(17) C10 0.0317(17) 0.0279(17) 0.0256(17) 0.0033(13) 0.0098(13) 0.0164(14) C11 0.0190(14) 0.0241(15) 0.0191(14) 0.0016(12) -0.0006(11) 0.0111(12) C12 0.0178(14) 0.0277(17) 0.0296(17) -0.0014(14) -0.0006(12) 0.0051(13) C13 0.0231(15) 0.0340(18) 0.0188(15) -0.0004(13) -0.0015(12) 0.0100(14) C14 0.0204(14) 0.0159(14) 0.0202(15) 0.0043(11) 0.0071(11) 0.0056(11) C15 0.0289(16) 0.0218(16) 0.0271(17) 0.0034(13) 0.0052(13) 0.0004(13) C16 0.0302(16) 0.0230(16) 0.0329(18) 0.0137(14) 0.0121(14) 0.0110(14) C17 0.0259(16) 0.0254(16) 0.0194(15) -0.0014(13) -0.0068(12) 0.0069(13) C18 0.041(2) 0.038(2) 0.0197(16) -0.0020(14) -0.0030(14) 0.0109(16) C19 0.0228(16) 0.0277(18) 0.038(2) -0.0009(15) -0.0064(14) -0.0006(14) C20 0.0292(16) 0.0201(15) 0.0257(16) 0.0105(13) 0.0088(13) 0.0063(13) C21 0.047(2) 0.034(2) 0.048(2) 0.0255(18) 0.0127(18) 0.0147(18) C22 0.0348(18) 0.0223(17) 0.038(2) 0.0056(15) 0.0107(15) -0.0030(14) C23 0.0233(15) 0.0213(15) 0.0233(16) 0.0065(12) 0.0068(12) 0.0102(12) C24 0.0336(18) 0.037(2) 0.0359(19) 0.0090(16) 0.0070(15) 0.0224(16) C25 0.0403(19) 0.0322(19) 0.0243(17) -0.0026(14) 0.0035(14) 0.0179(16) _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 C7 1.837(3) . ? Os P2 2.3846(7) . ? Os P1 2.3907(7) . ? Os S1 2.4800(7) . ? Os H3 1.595(10) . ? Os H2 1.591(10) . ? Os H1 1.569(10) . ? P1 C11 1.847(3) . ? P1 C14 1.855(3) . ? P1 C8 1.861(3) . ? P2 C17 1.854(3) . ? P2 C23 1.856(3) . ? P2 C20 1.859(3) . ? S1 B1 1.784(3) . ? O1 B1 1.386(4) . ? O1 C1 1.461(3) . ? O2 B1 1.381(4) . ? O2 C4 1.454(3) . ? O3 C7 1.169(4) . ? C1 C3 1.517(4) . ? C1 C2 1.526(4) . ? C1 C4 1.563(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.515(4) . ? C4 C5 1.515(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C8 C9 1.528(4) . ? C8 C10 1.533(4) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.528(4) . ? C11 C13 1.532(4) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.529(4) . ? C14 C15 1.531(4) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.531(4) . ? C17 C18 1.534(5) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.528(4) . ? C20 C22 1.534(5) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.524(4) . ? C23 C24 1.530(4) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 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 C7 Os P2 89.46(9) . . ? C7 Os P1 88.84(9) . . ? P2 Os P1 170.90(2) . . ? C7 Os S1 174.29(10) . . ? P2 Os S1 89.71(2) . . ? P1 Os S1 91.10(2) . . ? C7 Os H3 93.6(18) . . ? P2 Os H3 79.6(19) . . ? P1 Os H3 109.5(19) . . ? S1 Os H3 91.8(17) . . ? C7 Os H2 100(2) . . ? P2 Os H2 112(2) . . ? P1 Os H2 77(2) . . ? S1 Os H2 86(2) . . ? H3 Os H2 33(2) . . ? C7 Os H1 88.2(15) . . ? P2 Os H1 86.3(15) . . ? P1 Os H1 84.7(15) . . ? S1 Os H1 86.1(15) . . ? H3 Os H1 166(2) . . ? H2 Os H1 160(3) . . ? C11 P1 C14 103.86(13) . . ? C11 P1 C8 101.56(13) . . ? C14 P1 C8 109.74(13) . . ? C11 P1 Os 114.55(10) . . ? C14 P1 Os 114.09(9) . . ? C8 P1 Os 112.05(10) . . ? C17 P2 C23 102.76(14) . . ? C17 P2 C20 102.06(14) . . ? C23 P2 C20 110.16(14) . . ? C17 P2 Os 113.41(11) . . ? C23 P2 Os 115.24(10) . . ? C20 P2 Os 112.08(10) . . ? B1 S1 Os 113.86(11) . . ? B1 O1 C1 107.1(2) . . ? B1 O2 C4 107.5(2) . . ? O2 B1 O1 111.9(3) . . ? O2 B1 S1 120.0(2) . . ? O1 B1 S1 128.1(2) . . ? O1 C1 C3 109.1(2) . . ? O1 C1 C2 107.0(2) . . ? C3 C1 C2 109.8(3) . . ? O1 C1 C4 102.4(2) . . ? C3 C1 C4 115.0(3) . . ? C2 C1 C4 113.0(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 C6 108.7(2) . . ? O2 C4 C5 107.2(2) . . ? C6 C4 C5 110.4(3) . . ? O2 C4 C1 101.7(2) . . ? C6 C4 C1 114.9(3) . . ? C5 C4 C1 113.2(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 Os 178.3(3) . . ? C9 C8 C10 109.9(3) . . ? C9 C8 P1 113.4(2) . . ? C10 C8 P1 117.2(2) . . ? C9 C8 H8 105.0 . . ? C10 C8 H8 105.0 . . ? P1 C8 H8 105.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 110.5(3) . . ? C12 C11 P1 111.0(2) . . ? C13 C11 P1 112.8(2) . . ? C12 C11 H11 107.4 . . ? C13 C11 H11 107.4 . . ? P1 C11 H11 107.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C15 110.9(2) . . ? C16 C14 P1 116.0(2) . . ? C15 C14 P1 113.2(2) . . ? C16 C14 H14 105.2 . . ? C15 C14 H14 105.2 . . ? P1 C14 H14 105.2 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 110.7(3) . . ? C19 C17 P2 111.0(2) . . ? C18 C17 P2 112.2(2) . . ? C19 C17 H17 107.6 . . ? C18 C17 H17 107.6 . . ? P2 C17 H17 107.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 110.0(3) . . ? C21 C20 P2 116.1(2) . . ? C22 C20 P2 114.4(2) . . ? C21 C20 H20 105.1 . . ? C22 C20 H20 105.1 . . ? P2 C20 H20 105.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C24 109.6(3) . . ? C25 C23 P2 112.5(2) . . ? C24 C23 P2 118.2(2) . . ? C25 C23 H23 105.1 . . ? C24 C23 H23 105.1 . . ? P2 C23 H23 105.1 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.407 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.107 _database_code_depnum_ccdc_archive 'CCDC 936598' ####################################################################### # # 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_enrique123 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H59 B O Os P2 S' _chemical_formula_weight 694.75 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' 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' S S 0.1246 0.1234 '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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.5073(5) _cell_length_b 20.3829(9) _cell_length_c 27.0237(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6338.5(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9793 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description 'irregular block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 4.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.862 _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). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_decay_% 0 _diffrn_reflns_number 74109 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.74 _reflns_number_total 7829 _reflns_number_gt 6448 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'apex2 v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.14 (Bruker, 2000)' _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. The structures of all compounds was solved by direct methods. Refinement, by full-matrix least squares on F2 with SHELXL97,2 was similar for all complexes, including isotropic and subsequently anisotropic displacement parameters. The C-H hydrogen atoms were calculated and refined using a restricted riding model. The hydrides h1, h2 and h3 were located in de last diference fourier map, and refined properly with the displacement parameters related to osmium atom. ; _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^)+(0.0246P)^2^+7.1112P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7829 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0533 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.005 _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 0.622037(8) 0.876247(4) 0.098061(3) 0.01371(3) Uani 1 1 d . . . H1 H 0.700(2) 0.8312(12) 0.1272(9) 0.016 Uiso 1 1 d . . . H2 H 0.569(2) 0.9405(13) 0.0667(10) 0.016 Uiso 1 1 d . . . H3 H 0.506(2) 0.9163(13) 0.0803(10) 0.016 Uiso 1 1 d . . . P1 P 0.47163(5) 0.80741(3) 0.12977(2) 0.01594(12) Uani 1 1 d . . . P2 P 0.81012(5) 0.91679(3) 0.07699(2) 0.01551(12) Uani 1 1 d . . . S1 S 0.61868(5) 0.94222(3) 0.17527(2) 0.01636(12) Uani 1 1 d . . . O1 O 0.62441(17) 0.79067(10) 0.00734(8) 0.0328(5) Uani 1 1 d . . . B1 B 0.5441(2) 1.01880(14) 0.17507(11) 0.0194(6) Uani 1 1 d . . . C1 C 0.5300(2) 1.05654(13) 0.22573(10) 0.0242(6) Uani 1 1 d . . . H1A H 0.5697 1.0314 0.2526 0.029 Uiso 1 1 calc R . . C2 C 0.3973(3) 1.05889(16) 0.23622(12) 0.0373(8) Uani 1 1 d . . . H2A H 0.3840 1.0843 0.2669 0.045 Uiso 1 1 calc R . . H2B H 0.3693 1.0136 0.2421 0.045 Uiso 1 1 calc R . . C3 C 0.3236(3) 1.09015(18) 0.19363(12) 0.0418(8) Uani 1 1 d . . . H3A H 0.2406 1.0797 0.1994 0.050 Uiso 1 1 calc R . . H3B H 0.3321 1.1384 0.1952 0.050 Uiso 1 1 calc R . . C4 C 0.3561(3) 1.06759(16) 0.14268(13) 0.0402(8) Uani 1 1 d . . . H4A H 0.3236 1.0992 0.1185 0.048 Uiso 1 1 calc R . . H4B H 0.3180 1.0248 0.1366 0.048 Uiso 1 1 calc R . . C5 C 0.4856(3) 1.05989(13) 0.13196(11) 0.0293(6) Uani 1 1 d . . . H5 H 0.4958 1.0360 0.0999 0.035 Uiso 1 1 calc R . . C6 C 0.5468(3) 1.12727(14) 0.12857(12) 0.0380(8) Uani 1 1 d . . . H6A H 0.6277 1.1203 0.1174 0.046 Uiso 1 1 calc R . . H6B H 0.5070 1.1540 0.1031 0.046 Uiso 1 1 calc R . . C7 C 0.5491(3) 1.16559(15) 0.17639(11) 0.0376(7) Uani 1 1 d . . . H7A H 0.4705 1.1834 0.1828 0.045 Uiso 1 1 calc R . . H7B H 0.6028 1.2032 0.1726 0.045 Uiso 1 1 calc R . . C8 C 0.5870(3) 1.12500(13) 0.22071(11) 0.0300(6) Uani 1 1 d . . . H8A H 0.5701 1.1503 0.2511 0.036 Uiso 1 1 calc R . . H8B H 0.6723 1.1190 0.2190 0.036 Uiso 1 1 calc R . . C9 C 0.5283(2) 0.73434(12) 0.16232(9) 0.0227(5) Uani 1 1 d . . . H9 H 0.4600 0.7095 0.1754 0.027 Uiso 1 1 calc R . . C10 C 0.6036(3) 0.75418(15) 0.20687(11) 0.0311(6) Uani 1 1 d . . . H10A H 0.6216 0.7152 0.2267 0.047 Uiso 1 1 calc R . . H10B H 0.5613 0.7860 0.2273 0.047 Uiso 1 1 calc R . . H10C H 0.6761 0.7740 0.1951 0.047 Uiso 1 1 calc R . . C11 C 0.5965(3) 0.68773(14) 0.12877(12) 0.0315(6) Uani 1 1 d . . . H11A H 0.6594 0.7119 0.1125 0.047 Uiso 1 1 calc R . . H11B H 0.5443 0.6694 0.1037 0.047 Uiso 1 1 calc R . . H11C H 0.6294 0.6521 0.1487 0.047 Uiso 1 1 calc R . . C12 C 0.3828(2) 0.76934(13) 0.07992(10) 0.0212(5) Uani 1 1 d . . . H12 H 0.4380 0.7408 0.0611 0.025 Uiso 1 1 calc R . . C13 C 0.2867(3) 0.72305(15) 0.09793(10) 0.0320(7) Uani 1 1 d . . . H13A H 0.2246 0.7487 0.1135 0.048 Uiso 1 1 calc R . . H13B H 0.3189 0.6922 0.1221 0.048 Uiso 1 1 calc R . . H13C H 0.2550 0.6987 0.0697 0.048 Uiso 1 1 calc R . . C14 C 0.3343(3) 0.81775(15) 0.04162(11) 0.0306(6) Uani 1 1 d . . . H14A H 0.3015 0.7933 0.0137 0.046 Uiso 1 1 calc R . . H14B H 0.3970 0.8463 0.0298 0.046 Uiso 1 1 calc R . . H14C H 0.2734 0.8445 0.0570 0.046 Uiso 1 1 calc R . . C15 C 0.3733(2) 0.84514(14) 0.17608(11) 0.0280(6) Uani 1 1 d . . . H15 H 0.4238 0.8742 0.1967 0.034 Uiso 1 1 calc R . . C16 C 0.3108(3) 0.79976(16) 0.21285(11) 0.0377(8) Uani 1 1 d . . . H16A H 0.2655 0.8263 0.2362 0.057 Uiso 1 1 calc R . . H16B H 0.3683 0.7738 0.2311 0.057 Uiso 1 1 calc R . . H16C H 0.2586 0.7703 0.1948 0.057 Uiso 1 1 calc R . . C17 C 0.2849(3) 0.89093(16) 0.15150(15) 0.0475(9) Uani 1 1 d . . . H17A H 0.2228 0.8648 0.1364 0.071 Uiso 1 1 calc R . . H17B H 0.3237 0.9170 0.1259 0.071 Uiso 1 1 calc R . . H17C H 0.2515 0.9203 0.1765 0.071 Uiso 1 1 calc R . . C18 C 0.8930(2) 0.95143(13) 0.13004(10) 0.0214(5) Uani 1 1 d . . . H18 H 0.8391 0.9837 0.1458 0.026 Uiso 1 1 calc R . . C19 C 0.9200(3) 0.90150(15) 0.17048(11) 0.0290(6) Uani 1 1 d . . . H19A H 0.9824 0.8723 0.1593 0.043 Uiso 1 1 calc R . . H19B H 0.8502 0.8756 0.1776 0.043 Uiso 1 1 calc R . . H19C H 0.9446 0.9245 0.2005 0.043 Uiso 1 1 calc R . . C20 C 1.0032(3) 0.99099(15) 0.11759(11) 0.0316(6) Uani 1 1 d . . . H20A H 1.0295 1.0146 0.1471 0.047 Uiso 1 1 calc R . . H20B H 0.9857 1.0225 0.0913 0.047 Uiso 1 1 calc R . . H20C H 1.0644 0.9610 0.1064 0.047 Uiso 1 1 calc R . . C21 C 0.8124(2) 0.98396(12) 0.03064(9) 0.0209(5) Uani 1 1 d . . . H21 H 0.8956 0.9945 0.0234 0.025 Uiso 1 1 calc R . . C22 C 0.7555(3) 1.04605(13) 0.05117(11) 0.0280(6) Uani 1 1 d . . . H22A H 0.7621 1.0815 0.0268 0.042 Uiso 1 1 calc R . . H22B H 0.7946 1.0590 0.0819 0.042 Uiso 1 1 calc R . . H22C H 0.6732 1.0374 0.0580 0.042 Uiso 1 1 calc R . . C23 C 0.7548(3) 0.96388(15) -0.01802(10) 0.0299(6) Uani 1 1 d . . . H23A H 0.6748 0.9498 -0.0116 0.045 Uiso 1 1 calc R . . H23B H 0.7985 0.9276 -0.0329 0.045 Uiso 1 1 calc R . . H23C H 0.7542 1.0013 -0.0407 0.045 Uiso 1 1 calc R . . C24 C 0.8976(2) 0.85230(12) 0.04484(10) 0.0203(5) Uani 1 1 d . . . H24 H 0.8480 0.8372 0.0167 0.024 Uiso 1 1 calc R . . C25 C 0.9208(3) 0.79083(14) 0.07577(12) 0.0352(7) Uani 1 1 d . . . H25A H 0.9518 0.7561 0.0544 0.053 Uiso 1 1 calc R . . H25B H 0.8481 0.7759 0.0910 0.053 Uiso 1 1 calc R . . H25C H 0.9774 0.8010 0.1017 0.053 Uiso 1 1 calc R . . C26 C 1.0112(3) 0.87523(14) 0.02116(13) 0.0354(7) Uani 1 1 d . . . H26A H 1.0651 0.8895 0.0471 0.053 Uiso 1 1 calc R . . H26B H 0.9953 0.9119 -0.0013 0.053 Uiso 1 1 calc R . . H26C H 1.0459 0.8390 0.0025 0.053 Uiso 1 1 calc R . . C27 C 0.6246(2) 0.82391(13) 0.04238(10) 0.0209(5) Uani 1 1 d . . . 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 0.01464(5) 0.01216(5) 0.01433(5) -0.00068(3) 0.00227(3) -0.00157(3) P1 0.0168(3) 0.0154(3) 0.0156(3) 0.0006(2) 0.0011(2) -0.0034(2) P2 0.0156(3) 0.0140(3) 0.0169(3) 0.0007(2) 0.0020(2) -0.0011(2) S1 0.0183(3) 0.0152(3) 0.0156(3) -0.0012(2) 0.0007(2) 0.0010(2) O1 0.0296(11) 0.0398(12) 0.0289(11) -0.0177(9) 0.0073(9) -0.0097(9) B1 0.0179(13) 0.0190(14) 0.0212(14) -0.0018(11) 0.0023(11) 0.0004(11) C1 0.0332(15) 0.0197(13) 0.0198(13) -0.0042(10) -0.0003(11) 0.0066(11) C2 0.0422(19) 0.0315(16) 0.0381(18) 0.0006(14) 0.0194(14) 0.0111(13) C3 0.0328(17) 0.049(2) 0.044(2) -0.0050(16) 0.0035(15) 0.0058(15) C4 0.0397(18) 0.0334(17) 0.047(2) -0.0112(15) -0.0180(15) 0.0136(14) C5 0.0396(17) 0.0225(13) 0.0258(14) -0.0077(11) -0.0059(13) 0.0112(12) C6 0.061(2) 0.0236(15) 0.0289(16) 0.0011(12) 0.0021(15) 0.0081(14) C7 0.051(2) 0.0267(15) 0.0349(17) -0.0038(13) 0.0013(15) 0.0030(14) C8 0.0347(15) 0.0233(14) 0.0319(15) -0.0080(12) -0.0071(12) 0.0041(12) C9 0.0292(14) 0.0183(12) 0.0206(13) 0.0059(10) -0.0060(11) -0.0068(10) C10 0.0375(16) 0.0330(15) 0.0227(14) 0.0098(12) -0.0101(12) -0.0103(13) C11 0.0392(17) 0.0195(13) 0.0357(16) 0.0047(12) -0.0076(13) 0.0031(12) C12 0.0189(12) 0.0249(13) 0.0199(12) 0.0036(10) -0.0028(10) -0.0048(10) C13 0.0306(16) 0.0372(17) 0.0281(15) 0.0059(12) -0.0073(12) -0.0189(13) C14 0.0260(14) 0.0345(16) 0.0312(16) 0.0078(13) -0.0096(12) -0.0033(12) C15 0.0290(15) 0.0270(14) 0.0280(15) -0.0051(12) 0.0120(12) -0.0070(12) C16 0.0390(17) 0.0431(18) 0.0312(17) -0.0051(14) 0.0174(14) -0.0151(14) C17 0.0379(19) 0.0370(18) 0.068(2) 0.0024(17) 0.0280(18) 0.0093(15) C18 0.0188(13) 0.0233(13) 0.0221(13) -0.0026(10) -0.0012(10) -0.0041(10) C19 0.0266(14) 0.0364(16) 0.0239(14) 0.0025(12) -0.0058(12) -0.0013(12) C20 0.0262(15) 0.0376(16) 0.0311(15) -0.0019(13) -0.0021(12) -0.0118(13) C21 0.0207(12) 0.0186(12) 0.0234(13) 0.0037(10) 0.0053(10) -0.0034(10) C22 0.0309(15) 0.0171(13) 0.0361(16) 0.0063(12) 0.0053(12) 0.0005(11) C23 0.0338(16) 0.0344(16) 0.0214(14) 0.0097(12) 0.0007(12) -0.0031(12) C24 0.0197(12) 0.0165(12) 0.0247(13) -0.0018(10) 0.0051(10) 0.0006(9) C25 0.0424(18) 0.0255(15) 0.0376(17) 0.0086(13) 0.0147(14) 0.0161(13) C26 0.0257(14) 0.0256(15) 0.055(2) -0.0060(14) 0.0191(14) -0.0001(12) C27 0.0181(12) 0.0224(13) 0.0221(13) -0.0035(10) 0.0048(10) -0.0057(10) _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 C27 1.845(3) . ? Os P2 2.3857(6) . ? Os P1 2.3872(6) . ? Os S1 2.4826(6) . ? Os H1 1.51(3) . ? Os H2 1.68(3) . ? Os H3 1.63(3) . ? P1 C9 1.848(3) . ? P1 C15 1.854(3) . ? P1 C12 1.860(3) . ? P2 C21 1.856(3) . ? P2 C18 1.861(3) . ? P2 C24 1.870(3) . ? S1 B1 1.781(3) . ? O1 C27 1.164(3) . ? B1 C1 1.579(4) . ? B1 C5 1.585(4) . ? C1 C8 1.548(4) . ? C1 C2 1.554(4) . ? C1 H1A 1.0000 . ? C2 C3 1.566(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.499(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.526(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.546(4) . ? C5 H5 1.0000 . ? C6 C7 1.510(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.520(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.530(4) . ? C9 C10 1.538(4) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.534(4) . ? C12 C14 1.535(4) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.532(5) . ? C15 C16 1.536(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.525(4) . ? C18 C20 1.540(4) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.528(4) . ? C21 C22 1.530(4) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.529(4) . ? C24 C25 1.530(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 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 C27 Os P2 89.49(8) . . ? C27 Os P1 87.97(8) . . ? P2 Os P1 161.27(2) . . ? C27 Os S1 177.47(8) . . ? P2 Os S1 91.55(2) . . ? P1 Os S1 90.31(2) . . ? C27 Os H1 93.7(10) . . ? P2 Os H1 78.2(10) . . ? P1 Os H1 83.4(10) . . ? S1 Os H1 84.2(10) . . ? C27 Os H2 92.6(9) . . ? P2 Os H2 86.7(10) . . ? P1 Os H2 112.0(10) . . ? S1 Os H2 89.8(9) . . ? H1 Os H2 163.6(13) . . ? C27 Os H3 93.6(9) . . ? P2 Os H3 119.8(10) . . ? P1 Os H3 78.9(10) . . ? S1 Os H3 87.9(9) . . ? H1 Os H3 160.6(14) . . ? H2 Os H3 33.1(11) . . ? C9 P1 C15 103.20(13) . . ? C9 P1 C12 101.67(12) . . ? C15 P1 C12 109.06(13) . . ? C9 P1 Os 112.87(9) . . ? C15 P1 Os 116.17(9) . . ? C12 P1 Os 112.54(8) . . ? C21 P2 C18 103.45(12) . . ? C21 P2 C24 101.38(12) . . ? C18 P2 C24 110.40(12) . . ? C21 P2 Os 115.45(9) . . ? C18 P2 Os 114.36(8) . . ? C24 P2 Os 110.85(8) . . ? B1 S1 Os 118.66(10) . . ? C1 B1 C5 109.6(2) . . ? C1 B1 S1 118.3(2) . . ? C5 B1 S1 132.1(2) . . ? C8 C1 C2 113.9(2) . . ? C8 C1 B1 108.7(2) . . ? C2 C1 B1 105.9(2) . . ? C8 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? B1 C1 H1A 109.4 . . ? C1 C2 C3 114.3(3) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 114.5(3) . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? C2 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C3 C4 C5 116.7(3) . . ? C3 C4 H4A 108.1 . . ? C5 C4 H4A 108.1 . . ? C3 C4 H4B 108.1 . . ? C5 C4 H4B 108.1 . . ? H4A C4 H4B 107.3 . . ? C4 C5 C6 111.4(2) . . ? C4 C5 B1 109.2(3) . . ? C6 C5 B1 108.6(2) . . ? C4 C5 H5 109.2 . . ? C6 C5 H5 109.2 . . ? B1 C5 H5 109.2 . . ? C7 C6 C5 114.6(3) . . ? C7 C6 H6A 108.6 . . ? C5 C6 H6A 108.6 . . ? C7 C6 H6B 108.6 . . ? C5 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C6 C7 C8 113.5(2) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C1 116.0(2) . . ? C7 C8 H8A 108.3 . . ? C1 C8 H8A 108.3 . . ? C7 C8 H8B 108.3 . . ? C1 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? C11 C9 C10 109.8(2) . . ? C11 C9 P1 113.54(18) . . ? C10 C9 P1 111.07(18) . . ? C11 C9 H9 107.4 . . ? C10 C9 H9 107.4 . . ? P1 C9 H9 107.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 110.3(2) . . ? C13 C12 P1 115.03(19) . . ? C14 C12 P1 114.83(19) . . ? C13 C12 H12 105.2 . . ? C14 C12 H12 105.2 . . ? P1 C12 H12 105.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 109.6(2) . . ? C17 C15 P1 111.4(2) . . ? C16 C15 P1 118.2(2) . . ? C17 C15 H15 105.5 . . ? C16 C15 H15 105.5 . . ? P1 C15 H15 105.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 109.8(2) . . ? C19 C18 P2 113.77(18) . . ? C20 C18 P2 116.89(19) . . ? C19 C18 H18 105.1 . . ? C20 C18 H18 105.1 . . ? P2 C18 H18 105.1 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C22 110.4(2) . . ? C23 C21 P2 112.14(18) . . ? C22 C21 P2 111.06(18) . . ? C23 C21 H21 107.7 . . ? C22 C21 H21 107.7 . . ? P2 C21 H21 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C25 109.3(2) . . ? C26 C24 P2 116.11(18) . . ? C25 C24 P2 114.58(19) . . ? C26 C24 H24 105.3 . . ? C25 C24 H24 105.3 . . ? P2 C24 H24 105.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 C27 Os 179.0(2) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.258 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 936599' ####################################################################### # # 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_enrique124 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H47 B O3 Os P2 S' _chemical_formula_weight 690.64 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' S S 0.1246 0.1234 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.2977(7) _cell_length_b 10.9590(5) _cell_length_c 16.8715(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.1190(10) _cell_angle_gamma 90.00 _cell_volume 2894.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9914 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description 'irregular block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 4.611 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.673 _exptl_absorpt_correction_T_max 0.862 _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). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34451 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.68 _reflns_number_total 7005 _reflns_number_gt 6132 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'apex2 v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ v. 7.56a (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.14 (Bruker, 2000)' _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. The structures of all compounds was solved by direct methods. Refinement, by full-matrix least squares on F2 with SHELXL97,2 was similar for all complexes, including isotropic and subsequently anisotropic displacement parameters. The C-H hydrogen atoms were calculated and refined using a restricted riding model. The hydrogen bonded to sulfur atom was located in the difference fourier map and refined freely with restrained displacement parameter. ; _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^)+(0.0257P)^2^+5.2112P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7005 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0562 _refine_ls_wR_factor_gt 0.0531 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.013 _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 0.236500(7) 0.288517(10) -0.001913(6) 0.01639(4) Uani 1 1 d . . . P1 P 0.28703(5) 0.48134(7) 0.05843(5) 0.01877(15) Uani 1 1 d . . . P2 P 0.16665(5) 0.12517(7) -0.08709(4) 0.01745(15) Uani 1 1 d . . . S S 0.12055(6) 0.28775(9) 0.05870(6) 0.0359(2) Uani 1 1 d . . . H H 0.131(2) 0.374(4) 0.103(2) 0.043 Uiso 1 1 d . . . O1 O 0.40495(14) 0.1355(2) 0.04984(14) 0.0270(5) Uani 1 1 d . . . O2 O 0.32336(14) 0.1216(2) 0.14102(13) 0.0260(5) Uani 1 1 d . . . O3 O 0.34471(16) 0.3190(2) -0.11344(15) 0.0319(5) Uani 1 1 d . . . B1 B 0.3293(2) 0.1781(3) 0.0666(2) 0.0212(7) Uani 1 1 d . . . C1 C 0.4415(2) 0.0508(3) 0.11079(19) 0.0241(6) Uani 1 1 d . . . C2 C 0.39232(19) 0.0430(3) 0.16527(19) 0.0226(6) Uani 1 1 d . . . C3 C 0.4126(2) -0.0352(3) 0.2317(2) 0.0287(7) Uani 1 1 d . . . H3 H 0.3781 -0.0408 0.2686 0.034 Uiso 1 1 calc R . . C4 C 0.4859(2) -0.1057(3) 0.2425(2) 0.0316(7) Uani 1 1 d . . . H4 H 0.5027 -0.1592 0.2884 0.038 Uiso 1 1 calc R . . C5 C 0.5344(2) -0.0989(3) 0.1872(2) 0.0343(8) Uani 1 1 d . . . H5 H 0.5838 -0.1487 0.1956 0.041 Uiso 1 1 calc R . . C6 C 0.5128(2) -0.0207(3) 0.1194(2) 0.0329(8) Uani 1 1 d . . . H6 H 0.5457 -0.0170 0.0809 0.039 Uiso 1 1 calc R . . C7 C 0.3963(2) 0.5211(3) 0.0532(2) 0.0253(7) Uani 1 1 d . . . H7 H 0.4000 0.4886 -0.0011 0.030 Uiso 1 1 calc R . . C8 C 0.4189(2) 0.6569(3) 0.0523(3) 0.0396(9) Uani 1 1 d . . . H8A H 0.4167 0.6947 0.1043 0.059 Uiso 1 1 calc R . . H8B H 0.3778 0.6972 0.0062 0.059 Uiso 1 1 calc R . . H8C H 0.4765 0.6654 0.0458 0.059 Uiso 1 1 calc R . . C9 C 0.4650(2) 0.4529(4) 0.1176(2) 0.0368(8) Uani 1 1 d . . . H9A H 0.5203 0.4639 0.1062 0.055 Uiso 1 1 calc R . . H9B H 0.4508 0.3658 0.1156 0.055 Uiso 1 1 calc R . . H9C H 0.4681 0.4851 0.1726 0.055 Uiso 1 1 calc R . . C10 C 0.2787(2) 0.5123(3) 0.16406(19) 0.0268(7) Uani 1 1 d . . . H10 H 0.2160 0.5118 0.1589 0.032 Uiso 1 1 calc R . . C11 C 0.3104(3) 0.6379(3) 0.2007(2) 0.0421(9) Uani 1 1 d . . . H11A H 0.2941 0.6501 0.2519 0.063 Uiso 1 1 calc R . . H11B H 0.2846 0.7019 0.1611 0.063 Uiso 1 1 calc R . . H11C H 0.3728 0.6416 0.2126 0.063 Uiso 1 1 calc R . . C12 C 0.3161(2) 0.4104(3) 0.2253(2) 0.0333(8) Uani 1 1 d . . . H12A H 0.3786 0.4121 0.2384 0.050 Uiso 1 1 calc R . . H12B H 0.2950 0.3314 0.2009 0.050 Uiso 1 1 calc R . . H12C H 0.2988 0.4225 0.2760 0.050 Uiso 1 1 calc R . . C13 C 0.2204(2) 0.6049(3) -0.0031(2) 0.0273(7) Uani 1 1 d . . . H13 H 0.2480 0.6843 0.0182 0.033 Uiso 1 1 calc R . . C14 C 0.1292(2) 0.6091(4) 0.0041(3) 0.0443(10) Uani 1 1 d . . . H14A H 0.0975 0.6741 -0.0314 0.066 Uiso 1 1 calc R . . H14B H 0.1302 0.6253 0.0615 0.066 Uiso 1 1 calc R . . H14C H 0.1011 0.5306 -0.0133 0.066 Uiso 1 1 calc R . . C15 C 0.2192(3) 0.5954(3) -0.0941(2) 0.0372(8) Uani 1 1 d . . . H15A H 0.1901 0.5201 -0.1177 0.056 Uiso 1 1 calc R . . H15B H 0.2780 0.5943 -0.0984 0.056 Uiso 1 1 calc R . . H15C H 0.1889 0.6658 -0.1244 0.056 Uiso 1 1 calc R . . C16 C 0.0881(2) 0.1884(3) -0.17960(19) 0.0253(7) Uani 1 1 d . . . H16 H 0.0628 0.1180 -0.2158 0.030 Uiso 1 1 calc R . . C17 C 0.1311(2) 0.2716(3) -0.2295(2) 0.0346(8) Uani 1 1 d . . . H17A H 0.0907 0.2895 -0.2831 0.052 Uiso 1 1 calc R . . H17B H 0.1815 0.2305 -0.2378 0.052 Uiso 1 1 calc R . . H17C H 0.1486 0.3480 -0.1993 0.052 Uiso 1 1 calc R . . C18 C 0.0147(2) 0.2564(3) -0.1592(2) 0.0371(8) Uani 1 1 d . . . H18A H 0.0377 0.3236 -0.1212 0.056 Uiso 1 1 calc R . . H18B H -0.0168 0.2001 -0.1334 0.056 Uiso 1 1 calc R . . H18C H -0.0238 0.2892 -0.2101 0.056 Uiso 1 1 calc R . . C19 C 0.09877(19) 0.0228(3) -0.04474(18) 0.0207(6) Uani 1 1 d . . . H19 H 0.0538 0.0768 -0.0336 0.025 Uiso 1 1 calc R . . C20 C 0.1447(2) -0.0335(3) 0.03908(19) 0.0263(7) Uani 1 1 d . . . H20A H 0.1027 -0.0717 0.0630 0.040 Uiso 1 1 calc R . . H20B H 0.1754 0.0306 0.0762 0.040 Uiso 1 1 calc R . . H20C H 0.1855 -0.0952 0.0316 0.040 Uiso 1 1 calc R . . C21 C 0.0498(2) -0.0745(3) -0.1047(2) 0.0277(7) Uani 1 1 d . . . H21A H 0.0901 -0.1346 -0.1151 0.042 Uiso 1 1 calc R . . H21B H 0.0190 -0.0357 -0.1568 0.042 Uiso 1 1 calc R . . H21C H 0.0090 -0.1154 -0.0806 0.042 Uiso 1 1 calc R . . C22 C 0.2371(2) 0.0292(3) -0.1315(2) 0.0259(7) Uani 1 1 d . . . H22 H 0.2832 0.0848 -0.1388 0.031 Uiso 1 1 calc R . . C23 C 0.2826(2) -0.0706(3) -0.0722(2) 0.0321(8) Uani 1 1 d . . . H23A H 0.2416 -0.1347 -0.0693 0.048 Uiso 1 1 calc R . . H23B H 0.3067 -0.0355 -0.0172 0.048 Uiso 1 1 calc R . . H23C H 0.3286 -0.1055 -0.0921 0.048 Uiso 1 1 calc R . . C24 C 0.1967(3) -0.0275(3) -0.2168(2) 0.0367(8) Uani 1 1 d . . . H24A H 0.2408 -0.0701 -0.2356 0.055 Uiso 1 1 calc R . . H24B H 0.1714 0.0370 -0.2562 0.055 Uiso 1 1 calc R . . H24C H 0.1523 -0.0856 -0.2130 0.055 Uiso 1 1 calc R . . C25 C 0.3066(2) 0.3059(3) -0.0714(2) 0.0300(7) Uani 1 1 d . . . 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 0.01796(6) 0.01429(6) 0.01649(6) 0.00009(4) 0.00406(4) -0.00140(4) P1 0.0200(4) 0.0164(3) 0.0193(4) -0.0009(3) 0.0044(3) -0.0018(3) P2 0.0202(4) 0.0143(3) 0.0177(3) 0.0003(3) 0.0050(3) -0.0013(3) S 0.0342(5) 0.0341(5) 0.0434(5) -0.0046(4) 0.0174(4) -0.0016(4) O1 0.0234(11) 0.0298(12) 0.0284(12) 0.0033(10) 0.0083(9) 0.0038(9) O2 0.0273(11) 0.0272(12) 0.0236(11) 0.0039(9) 0.0075(9) 0.0069(9) O3 0.0402(14) 0.0265(12) 0.0261(12) 0.0011(10) 0.0047(11) -0.0031(10) B1 0.0220(17) 0.0185(16) 0.0222(16) -0.0014(13) 0.0048(13) -0.0031(12) C1 0.0242(16) 0.0219(15) 0.0224(15) -0.0014(12) 0.0000(12) -0.0040(12) C2 0.0215(15) 0.0206(15) 0.0227(15) -0.0014(12) 0.0009(12) 0.0026(12) C3 0.0311(17) 0.0306(18) 0.0245(16) 0.0037(13) 0.0078(13) 0.0046(14) C4 0.0312(18) 0.0277(17) 0.0294(18) 0.0016(14) -0.0026(14) 0.0060(14) C5 0.0229(17) 0.0326(19) 0.042(2) -0.0057(16) -0.0002(14) 0.0075(14) C6 0.0237(17) 0.041(2) 0.0335(18) -0.0051(15) 0.0066(14) 0.0044(14) C7 0.0224(15) 0.0247(16) 0.0300(17) -0.0017(13) 0.0092(13) -0.0058(12) C8 0.034(2) 0.032(2) 0.052(2) -0.0011(17) 0.0089(17) -0.0133(16) C9 0.0212(17) 0.039(2) 0.047(2) 0.0043(17) 0.0046(15) -0.0019(15) C10 0.0329(17) 0.0267(17) 0.0223(15) -0.0035(13) 0.0105(13) -0.0017(13) C11 0.067(3) 0.0302(19) 0.0313(19) -0.0117(16) 0.0168(18) -0.0037(18) C12 0.047(2) 0.0314(18) 0.0215(16) -0.0016(14) 0.0103(15) -0.0017(15) C13 0.0312(18) 0.0176(15) 0.0294(17) 0.0017(13) 0.0024(13) 0.0019(12) C14 0.0302(19) 0.035(2) 0.064(3) 0.0126(19) 0.0071(18) 0.0106(16) C15 0.051(2) 0.0259(18) 0.0272(18) 0.0011(14) -0.0015(16) 0.0015(16) C16 0.0311(17) 0.0217(16) 0.0178(14) 0.0026(12) -0.0017(12) -0.0041(12) C17 0.046(2) 0.0302(19) 0.0231(17) 0.0091(14) 0.0027(15) -0.0071(15) C18 0.0320(19) 0.0331(19) 0.040(2) 0.0065(16) -0.0007(15) 0.0056(15) C19 0.0206(14) 0.0198(14) 0.0216(15) 0.0026(12) 0.0057(11) -0.0017(11) C20 0.0297(17) 0.0232(16) 0.0264(16) 0.0055(13) 0.0082(13) -0.0042(13) C21 0.0297(17) 0.0232(16) 0.0296(17) 0.0018(13) 0.0071(13) -0.0054(13) C22 0.0279(16) 0.0223(16) 0.0308(17) -0.0035(13) 0.0135(13) -0.0008(12) C23 0.0287(18) 0.0223(16) 0.045(2) -0.0051(15) 0.0104(15) 0.0008(13) C24 0.052(2) 0.0318(19) 0.0318(19) -0.0084(15) 0.0216(17) 0.0010(16) C25 0.0275(18) 0.0207(16) 0.0343(19) -0.0050(14) -0.0042(15) 0.0012(13) _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 C25 1.860(4) . ? Os B1 2.029(4) . ? Os P2 2.3785(7) . ? Os S 2.3854(9) . ? Os P1 2.3905(8) . ? P1 C10 1.856(3) . ? P1 C7 1.860(3) . ? P1 C13 1.861(3) . ? P2 C19 1.853(3) . ? P2 C16 1.856(3) . ? P2 C22 1.862(3) . ? S H 1.19(4) . ? O1 C1 1.391(4) . ? O1 B1 1.418(4) . ? O2 C2 1.385(4) . ? O2 B1 1.427(4) . ? O3 C25 1.074(4) . ? C1 C6 1.374(5) . ? C1 C2 1.380(4) . ? C2 C3 1.376(4) . ? C3 C4 1.390(5) . ? C3 H3 0.9500 . ? C4 C5 1.383(5) . ? C4 H4 0.9500 . ? C5 C6 1.394(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C9 1.522(5) . ? C7 C8 1.533(5) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.529(5) . ? C10 C11 1.538(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.525(5) . ? C13 C15 1.534(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.528(5) . ? C16 C17 1.535(4) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C21 1.532(4) . ? C19 C20 1.534(4) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.527(5) . ? C22 C24 1.538(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 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 C25 Os B1 85.90(14) . . ? C25 Os P2 88.35(10) . . ? B1 Os P2 92.95(10) . . ? C25 Os S 165.70(10) . . ? B1 Os S 107.92(10) . . ? P2 Os S 87.32(3) . . ? C25 Os P1 88.76(10) . . ? B1 Os P1 99.80(10) . . ? P2 Os P1 166.69(3) . . ? S Os P1 92.34(3) . . ? C10 P1 C7 109.23(15) . . ? C10 P1 C13 102.44(15) . . ? C7 P1 C13 102.81(15) . . ? C10 P1 Os 117.53(11) . . ? C7 P1 Os 114.10(11) . . ? C13 P1 Os 109.06(10) . . ? C19 P2 C16 101.79(14) . . ? C19 P2 C22 108.34(14) . . ? C16 P2 C22 103.35(15) . . ? C19 P2 Os 117.36(10) . . ? C16 P2 Os 109.24(10) . . ? C22 P2 Os 115.03(11) . . ? Os S H 105.6(18) . . ? C1 O1 B1 106.9(2) . . ? C2 O2 B1 106.4(2) . . ? O1 B1 O2 107.9(3) . . ? O1 B1 Os 129.4(2) . . ? O2 B1 Os 122.5(2) . . ? C6 C1 C2 121.6(3) . . ? C6 C1 O1 129.4(3) . . ? C2 C1 O1 108.9(3) . . ? C3 C2 C1 121.9(3) . . ? C3 C2 O2 128.3(3) . . ? C1 C2 O2 109.8(3) . . ? C2 C3 C4 117.1(3) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.4 . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 121.6(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 116.8(3) . . ? C1 C6 H6 121.6 . . ? C5 C6 H6 121.6 . . ? C9 C7 C8 110.7(3) . . ? C9 C7 P1 112.0(2) . . ? C8 C7 P1 117.6(2) . . ? C9 C7 H7 105.1 . . ? C8 C7 H7 105.1 . . ? P1 C7 H7 105.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 110.8(3) . . ? C12 C10 P1 113.2(2) . . ? C11 C10 P1 116.3(2) . . ? C12 C10 H10 105.1 . . ? C11 C10 H10 105.1 . . ? P1 C10 H10 105.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 109.9(3) . . ? C14 C13 P1 114.1(2) . . ? C15 C13 P1 110.6(2) . . ? C14 C13 H13 107.3 . . ? C15 C13 H13 107.3 . . ? P1 C13 H13 107.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 109.8(3) . . ? C18 C16 P2 113.2(2) . . ? C17 C16 P2 111.7(2) . . ? C18 C16 H16 107.3 . . ? C17 C16 H16 107.3 . . ? P2 C16 H16 107.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C20 111.1(3) . . ? C21 C19 P2 115.1(2) . . ? C20 C19 P2 114.1(2) . . ? C21 C19 H19 105.1 . . ? C20 C19 H19 105.1 . . ? P2 C19 H19 105.1 . . ? 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 109.1(3) . . ? C23 C22 P2 112.5(2) . . ? C24 C22 P2 117.0(2) . . ? C23 C22 H22 105.8 . . ? C24 C22 H22 105.8 . . ? P2 C22 H22 105.8 . . ? 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 . . ? O3 C25 Os 177.0(3) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.323 _refine_diff_density_min -0.932 _refine_diff_density_rms 0.107 #===END _database_code_depnum_ccdc_archive 'CCDC 936600'