# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 ####################################################################### # # 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_MSC01012 _database_code_depnum_ccdc_archive 'CCDC 245545' _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C30 H54 O2 P2 Ru1' _chemical_formula_moiety ? _chemical_formula_weight 609.775 _cell_length_a 11.224(2) _cell_length_b 11.907(2) _cell_length_c 12.510(2) _cell_angle_alpha 77.529(5) _cell_angle_beta 89.453(5) _cell_angle_gamma 76.548(5) _cell_volume 1586.1(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 952 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 23.26 _cell_measurement_temperature 153(2) _exptl_crystal_colour orange _exptl_crystal_description irregular _exptl_crystal_size_max .45 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .25 _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.6186 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_ambient_temperature 153(2) _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_measurement_method '\w scans' _diffrn_measurement_details ' 0.30 degree frames measured for 5.15 seconds each' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_reflns_number 3 _diffrn_reflns_av_R_equivalents 2810 _diffrn_reflns_theta_min 2.17107 _diffrn_reflns_theta_max 23.2683 _diffrn_reflns_theta_full 23.2683 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 953 _diffrn_standards_decay_% 0.0 _diffrn_standards_interval_time 208 _reflns_number_total 3450 _reflns_number_gt 2810 _reflns_threshold_expression 'Fo^2^> 2.33\s(Fo^2^)' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source RU Ru -1.42 0.836 'International Tables Vol. IV (1974) Table 2.2B' P P 0.09 0.095 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 2810 _refine_ls_number_parameters 532 _refine_ls_hydrogen_treatment ? _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.00F)^2^ _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0346 _refine_ls_goodness_of_fit_ref 1.0330 _refine_ls_shift/su_max 0.0044 _refine_diff_density_max 0.88 _refine_diff_density_min -0.99 _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly RU1 RU 0.24675(4) 0.77137(4) 0.90589(3) 0.01342(14) Uani 1 0 . O2 O 0.1709(3) 0.6796(3) 1.0331(3) 0.0190(13) Uani 1 0 . C3 C 0.2105(4) 0.6892(4) 1.1313(4) 0.0163(18) Uani 1 0 . C4 C 0.1673(5) 0.6386(5) 1.2302(5) 0.024(2) Uani 1 0 . C5 C 0.2154(5) 0.6507(5) 1.3272(5) 0.026(2) Uani 1 0 . C6 C 0.3066(5) 0.7106(5) 1.3263(5) 0.025(2) Uani 1 0 . C7 C 0.3495(5) 0.7620(5) 1.2304(5) 0.023(2) Uani 1 0 . C8 C 0.3016(4) 0.7528(4) 1.1313(4) 0.0166(18) Uani 1 0 . O9 O 0.3353(3) 0.8043(3) 1.0325(3) 0.0175(13) Uani 1 0 . P10 P 0.40845(12) 0.80609(12) 0.80253(11) 0.0155(5) Uani 1 0 . C11 C 0.5329(5) 0.6688(5) 0.8183(4) 0.0208(19) Uani 1 0 . C12 C 0.5825(6) 0.6215(6) 0.9371(5) 0.029(2) Uani 1 0 . C13 C 0.4936(5) 0.5734(5) 0.7717(5) 0.027(2) Uani 1 0 . C14 C 0.3823(5) 0.8585(5) 0.6519(5) 0.023(2) Uani 1 0 . C15 C 0.3114(5) 0.9881(5) 0.6180(5) 0.026(2) Uani 1 0 . C16 C 0.4944(5) 0.8360(6) 0.5808(5) 0.030(2) Uani 1 0 . C17 C 0.4839(5) 0.9073(5) 0.8565(5) 0.023(2) Uani 1 0 . C18 C 0.5950(7) 0.9361(7) 0.7947(7) 0.037(3) Uani 1 0 . C19 C 0.3975(5) 1.0220(5) 0.8696(5) 0.025(2) Uani 1 0 . P20 P 0.07201(11) 0.78512(11) 0.80637(10) 0.0150(5) Uani 1 0 . C21 C 0.0765(5) 0.8077(5) 0.6551(4) 0.022(2) Uani 1 0 . C22 C 0.1432(5) 0.6964(5) 0.6177(5) 0.027(2) Uani 1 0 . C23 C -0.0456(5) 0.8637(6) 0.5889(5) 0.030(2) Uani 1 0 . C24 C 0.0066(5) 0.6559(4) 0.8605(4) 0.020(2) Uani 1 0 . C25 C 0.0956(5) 0.5363(5) 0.8679(5) 0.023(2) Uani 1 0 . C26 C -0.1144(6) 0.6563(6) 0.8065(6) 0.031(3) Uani 1 0 . C27 C -0.0507(5) 0.9125(5) 0.8265(4) 0.020(2) Uani 1 0 . C28 C -0.0855(6) 0.9016(6) 0.9455(5) 0.027(2) Uani 1 0 . C29 C -0.0171(5) 1.0310(5) 0.7820(5) 0.026(2) Uani 1 0 . C30 C 0.2875(9) 0.3255(7) 0.7362(8) 0.065(4) Uani 1 0 . C31 C 0.1786(9) 0.2949(7) 0.7219(8) 0.059(4) Uani 1 0 . C32 C 0.1280(7) 0.3170(7) 0.6193(8) 0.052(4) Uani 1 0 . C33 C 0.1876(7) 0.3660(7) 0.5342(7) 0.054(3) Uani 1 0 . C34 C 0.2960(7) 0.3937(6) 0.5504(8) 0.055(3) Uani 1 0 . C35 C 0.3455(7) 0.3732(7) 0.6512(9) 0.055(4) Uani 1 0 . H1 H 0.225(4) 0.899(4) 0.834(4) 0.027(14) Uiso 1 0 . H2 H 0.259(5) 0.687(5) 0.843(5) 0.06(2) Uiso 1 0 . H3 H 0.109(4) 0.600(4) 1.235(3) 0.003(12) Uiso 1 0 . H4 H 0.186(4) 0.625(4) 1.378(4) 0.004(14) Uiso 1 0 . H5 H 0.337(4) 0.717(4) 1.384(4) 0.003(13) Uiso 1 0 . H6 H 0.408(4) 0.804(4) 1.221(4) 0.014(14) Uiso 1 0 . H7 H 0.590(5) 0.686(5) 0.774(4) 0.025(16) Uiso 1 0 . H8 H 0.527(5) 0.611(5) 0.973(4) 0.029(18) Uiso 1 0 . H9 H 0.625(5) 0.678(5) 0.964(5) 0.050(19) Uiso 1 0 . H10 H 0.644(6) 0.540(6) 0.936(5) 0.06(2) Uiso 1 0 . H11 H 0.563(6) 0.506(6) 0.762(5) 0.053(19) Uiso 1 0 . H12 H 0.466(5) 0.593(5) 0.691(5) 0.043(17) Uiso 1 0 . H13 H 0.443(5) 0.539(5) 0.818(5) 0.032(16) Uiso 1 0 . H14 H 0.342(4) 0.807(4) 0.637(4) 0.013(14) Uiso 1 0 . H15 H 0.359(4) 1.040(4) 0.627(4) 0.024(15) Uiso 1 0 . H16 H 0.238(4) 1.010(4) 0.666(4) 0.024(14) Uiso 1 0 . H17 H 0.282(4) 1.007(4) 0.549(4) 0.020(14) Uiso 1 0 . H18 H 0.475(4) 0.857(4) 0.502(5) 0.029(15) Uiso 1 0 . H19 H 0.536(5) 0.751(5) 0.595(5) 0.039(18) Uiso 1 0 . H20 H 0.550(4) 0.884(4) 0.590(4) 0.016(13) Uiso 1 0 . H21 H 0.517(4) 0.865(4) 0.928(4) 0.032(16) Uiso 1 0 . H22 H 0.579(5) 1.002(5) 0.725(5) 0.049(19) Uiso 1 0 . H23 H 0.630(5) 0.892(5) 0.788(5) 0.02(2) Uiso 1 0 . H24 H 0.643(5) 0.971(5) 0.852(4) 0.037(16) Uiso 1 0 . H25 H 0.434(5) 1.065(5) 0.902(5) 0.041(19) Uiso 1 0 . H26 H 0.331(4) 1.007(4) 0.915(4) 0.007(12) Uiso 1 0 . H27 H 0.358(5) 1.079(5) 0.807(5) 0.047(19) Uiso 1 0 . H28 H 0.118(4) 0.863(4) 0.639(4) 0.004(12) Uiso 1 0 . H29 H 0.100(4) 0.639(4) 0.614(4) 0.026(15) Uiso 1 0 . H30 H 0.220(4) 0.650(4) 0.661(4) 0.014(13) Uiso 1 0 . H31 H 0.164(4) 0.712(4) 0.537(4) 0.021(13) Uiso 1 0 . H32 H -0.029(5) 0.869(5) 0.505(5) 0.043(17) Uiso 1 0 . H33 H -0.084(5) 0.942(5) 0.606(4) 0.032(16) Uiso 1 0 . H34 H -0.102(4) 0.812(4) 0.602(3) 0.005(11) Uiso 1 0 . H35 H -0.008(4) 0.665(3) 0.929(4) -0.002(11) Uiso 1 0 . H36 H 0.066(5) 0.480(5) 0.906(5) 0.034(17) Uiso 1 0 . H37 H 0.167(5) 0.526(4) 0.907(4) 0.026(15) Uiso 1 0 . H38 H 0.125(6) 0.510(6) 0.785(6) 0.08(2) Uiso 1 0 . H39 H -0.105(5) 0.636(5) 0.729(5) 0.042(17) Uiso 1 0 . H40 H -0.160(5) 0.714(5) 0.804(5) 0.03(2) Uiso 1 0 . H41 H -0.146(5) 0.593(5) 0.849(5) 0.045(18) Uiso 1 0 . H42 H -0.113(4) 0.918(4) 0.791(4) 0.006(13) Uiso 1 0 . H43 H -0.016(5) 0.893(4) 0.998(4) 0.027(15) Uiso 1 0 . H44 H -0.127(5) 0.852(5) 0.977(4) 0.023(16) Uiso 1 0 . H45 H -0.149(4) 0.980(4) 0.956(4) 0.019(13) Uiso 1 0 . H46 H -0.091(5) 1.103(5) 0.785(4) 0.033(15) Uiso 1 0 . H47 H 0.004(5) 1.038(5) 0.714(5) 0.037(18) Uiso 1 0 . H48 H 0.042(4) 1.049(4) 0.828(4) 0.024(15) Uiso 1 0 . H49 H 0.302(5) 0.299(5) 0.794(4) 0.009(17) Uiso 1 0 . H50 H 0.137(4) 0.277(4) 0.761(4) -0.006(14) Uiso 1 0 . H51 H 0.060(6) 0.297(6) 0.608(6) 0.06(3) Uiso 1 0 . H52 H 0.158(5) 0.383(5) 0.477(5) 0.03(2) Uiso 1 0 . H53 H 0.335(5) 0.424(5) 0.494(5) 0.036(19) Uiso 1 0 . H54 H 0.414(6) 0.390(5) 0.665(5) 0.05(2) Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 RU1 0.0113(6) 0.0147(8) 0.0138(9) -0.00293(16) 0.00155(16) -0.00251(17) O2 0.020(2) 0.021(2) 0.018(2) -0.0088(16) -0.0003(16) -0.0050(16) C3 0.018(3) 0.014(3) 0.016(3) 0.000(2) 0.005(2) -0.005(2) C4 0.019(3) 0.026(4) 0.029(4) -0.007(3) 0.005(3) -0.009(3) C5 0.036(4) 0.029(4) 0.014(3) -0.008(3) 0.013(3) -0.006(3) C6 0.030(4) 0.026(3) 0.018(3) -0.003(3) -0.004(3) -0.008(3) C7 0.015(3) 0.021(3) 0.034(4) -0.002(3) 0.000(3) -0.010(3) C8 0.018(3) 0.013(3) 0.016(3) 0.001(2) 0.001(2) -0.003(2) O9 0.016(2) 0.022(2) 0.015(2) -0.0082(16) -0.0001(15) -0.0018(16) P10 0.0127(9) 0.0136(10) 0.0183(13) -0.0025(6) 0.0029(6) -0.0006(6) C11 0.018(3) 0.016(3) 0.024(3) -0.004(2) 0.010(3) 0.002(2) C12 0.019(4) 0.026(4) 0.034(4) -0.002(3) 0.001(3) 0.005(3) C13 0.027(4) 0.020(3) 0.034(4) -0.005(3) 0.011(3) -0.006(3) C14 0.022(3) 0.024(3) 0.024(4) -0.008(3) 0.005(2) -0.002(3) C15 0.023(3) 0.028(4) 0.022(4) -0.005(3) -0.001(3) 0.004(3) C16 0.030(4) 0.036(4) 0.022(4) -0.007(3) 0.014(3) -0.003(3) C17 0.022(3) 0.020(3) 0.027(4) -0.006(2) -0.008(2) -0.004(2) C18 0.025(4) 0.020(4) 0.069(7) -0.006(3) 0.009(4) -0.011(4) C19 0.024(3) 0.022(3) 0.029(4) -0.009(3) 0.001(3) -0.005(3) P20 0.0124(9) 0.0162(11) 0.0167(12) -0.0024(6) 0.0017(6) -0.0052(6) C21 0.022(3) 0.020(3) 0.024(4) -0.007(3) -0.002(3) -0.003(3) C22 0.029(4) 0.031(4) 0.022(4) -0.005(3) 0.004(3) -0.013(3) C23 0.026(4) 0.035(4) 0.028(4) -0.008(3) -0.004(3) -0.005(3) C24 0.022(3) 0.023(3) 0.018(3) -0.009(2) 0.007(2) -0.004(2) C25 0.022(3) 0.019(3) 0.027(4) -0.009(3) 0.000(3) -0.001(3) C26 0.026(4) 0.022(4) 0.048(5) -0.008(3) -0.002(3) -0.008(3) C27 0.010(3) 0.025(3) 0.026(4) -0.002(2) -0.004(2) -0.009(3) C28 0.024(4) 0.031(4) 0.030(4) -0.007(3) 0.010(3) -0.015(3) C29 0.025(4) 0.019(3) 0.033(4) 0.001(3) -0.002(3) -0.009(3) C30 0.090(9) 0.037(5) 0.051(7) 0.027(5) -0.037(6) -0.020(5) C31 0.071(7) 0.035(5) 0.067(8) -0.002(4) 0.036(6) -0.018(4) C32 0.035(5) 0.045(5) 0.080(8) -0.004(4) 0.003(4) -0.031(4) C33 0.059(6) 0.052(5) 0.048(6) 0.003(4) -0.016(5) -0.023(4) C34 0.045(5) 0.040(5) 0.071(7) 0.003(4) 0.019(5) -0.013(4) C35 0.032(5) 0.033(5) 0.095(10) 0.007(3) -0.015(5) -0.021(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU1 P10 2.2833(15) . . no RU1 P20 2.2876(14) . . no RU1 O2 2.027(3) . . no RU1 O9 2.031(3) . . no RU1 H1 1.56(5) . . no RU1 H2 1.39(6) . . no P10 C11 1.862(5) . . no P10 C14 1.856(6) . . no P10 C17 1.861(5) . . no P20 C21 1.855(6) . . no P20 C24 1.853(5) . . no P20 C27 1.856(5) . . no O2 C3 1.348(6) . . no O9 C8 1.350(6) . . no C3 C4 1.389(7) . . no C3 C8 1.406(6) . . no C4 C5 1.382(8) . . no C4 H3 0.88(4) . . no C5 C6 1.376(8) . . no C5 H4 0.76(5) . . no C6 C7 1.362(8) . . no C6 H5 0.83(4) . . no C7 C8 1.392(7) . . no C7 H6 0.91(5) . . no C11 C12 1.531(8) . . no C11 C13 1.532(8) . . no C11 H7 0.88(5) . . no C12 H8 0.79(5) . . no C12 H9 1.03(6) . . no C12 H10 1.05(6) . . no C13 H11 1.01(6) . . no C13 H12 1.02(6) . . no C13 H13 0.91(5) . . no C14 C15 1.533(8) . . no C14 C16 1.540(7) . . no C14 H14 0.89(5) . . no C15 H15 0.93(5) . . no C15 H16 1.03(5) . . no C15 H17 0.88(5) . . no C16 H18 0.97(5) . . no C16 H19 0.99(6) . . no C16 H20 0.96(5) . . no C17 C18 1.529(9) . . no C17 C19 1.520(7) . . no C17 H21 0.95(5) . . no C18 H22 1.03(6) . . no C18 H23 0.60(5) . . no C18 H24 1.11(5) . . no C19 H25 0.89(6) . . no C19 H26 0.96(4) . . no C19 H27 0.96(6) . . no C21 C22 1.528(8) . . no C21 C23 1.539(7) . . no C21 H28 0.87(4) . . no C22 H29 0.94(5) . . no C22 H30 1.00(5) . . no C22 H31 1.02(5) . . no C23 H32 1.05(6) . . no C23 H33 0.99(5) . . no C23 H34 0.97(4) . . no C24 C25 1.522(7) . . no C24 C26 1.521(8) . . no C24 H35 0.90(4) . . no C25 H36 0.86(5) . . no C25 H37 0.91(5) . . no C25 H38 1.17(7) . . no C26 H39 1.05(6) . . no C26 H40 0.75(6) . . no C26 H41 0.96(6) . . no C27 C28 1.522(8) . . no C27 C29 1.533(8) . . no C27 H42 0.82(4) . . no C28 H43 1.00(5) . . no C28 H44 0.86(5) . . no C28 H45 1.07(5) . . no C29 H46 1.05(6) . . no C29 H47 0.88(6) . . no C29 H48 0.98(5) . . no C30 C31 1.379(12) . . no C30 C35 1.332(12) . . no C30 H49 0.73(5) . . no C31 C32 1.356(11) . . no C31 H50 0.71(4) . . no C32 C33 1.349(11) . . no C32 H51 0.87(7) . . no C33 C34 1.360(10) . . no C33 H52 0.76(6) . . no C34 C35 1.332(11) . . no C34 H53 0.88(6) . . no C35 H54 0.86(6) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P10 RU1 P20 114.39(5) . . . no P10 RU1 O2 152.75(10) . . . no P10 RU1 O9 87.22(10) . . . no P10 RU1 H1 66.0(17) . . . no P10 RU1 H2 79(2) . . . no P20 RU1 O2 86.21(10) . . . no P20 RU1 O9 151.58(10) . . . no P20 RU1 H1 78.2(16) . . . no P20 RU1 H2 66(2) . . . no O2 RU1 O9 80.51(13) . . . no O2 RU1 H1 139.1(17) . . . no O2 RU1 H2 95(2) . . . no O9 RU1 H1 95.7(17) . . . no O9 RU1 H2 139(2) . . . no H1 RU1 H2 112(3) . . . no RU1 P10 C11 110.79(18) . . . no RU1 P10 C14 118.59(18) . . . no RU1 P10 C17 110.36(18) . . . no C11 P10 C14 103.8(3) . . . no C11 P10 C17 102.7(2) . . . no C14 P10 C17 109.4(3) . . . no RU1 P20 C21 119.26(18) . . . no RU1 P20 C24 110.05(17) . . . no RU1 P20 C27 110.76(17) . . . no C21 P20 C24 109.0(3) . . . no C21 P20 C27 103.2(2) . . . no C24 P20 C27 103.3(2) . . . no RU1 O2 C3 112.9(3) . . . no RU1 O9 C8 112.9(3) . . . no O2 C3 C4 123.4(4) . . . no O2 C3 C8 116.9(4) . . . no C4 C3 C8 119.6(5) . . . no C3 C4 C5 119.4(5) . . . no C3 C4 H3 123(3) . . . no C5 C4 H3 117(3) . . . no C4 C5 C6 120.5(6) . . . no C4 C5 H4 115(4) . . . no C6 C5 H4 124(4) . . . no C5 C6 C7 121.2(5) . . . no C5 C6 H5 121(3) . . . no C7 C6 H5 117(3) . . . no C6 C7 C8 119.6(5) . . . no C6 C7 H6 128(3) . . . no C8 C7 H6 112(3) . . . no O9 C8 C3 116.6(4) . . . no O9 C8 C7 123.7(4) . . . no C3 C8 C7 119.7(5) . . . no P10 C11 C12 112.0(4) . . . no P10 C11 C13 112.1(4) . . . no P10 C11 H7 107(3) . . . no C12 C11 C13 111.7(5) . . . no C12 C11 H7 112(3) . . . no C13 C11 H7 102(4) . . . no C11 C12 H8 107(4) . . . no C11 C12 H9 112(3) . . . no C11 C12 H10 104(3) . . . no H8 C12 H9 111(5) . . . no H8 C12 H10 110(5) . . . no H9 C12 H10 112(4) . . . no C11 C13 H11 115(3) . . . no C11 C13 H12 118(3) . . . no C11 C13 H13 110(3) . . . no H11 C13 H12 92(4) . . . no H11 C13 H13 105(5) . . . no H12 C13 H13 114(5) . . . no P10 C14 C15 112.9(4) . . . no P10 C14 C16 117.3(4) . . . no P10 C14 H14 101(3) . . . no C15 C14 C16 110.0(5) . . . no C15 C14 H14 114(3) . . . no C16 C14 H14 101(3) . . . no C14 C15 H15 112(3) . . . no C14 C15 H16 114(3) . . . no C14 C15 H17 113(3) . . . no H15 C15 H16 102(4) . . . no H15 C15 H17 109(4) . . . no H16 C15 H17 107(4) . . . no C14 C16 H18 115(3) . . . no C14 C16 H19 112(3) . . . no C14 C16 H20 111(3) . . . no H18 C16 H19 104(4) . . . no H18 C16 H20 104(4) . . . no H19 C16 H20 112(4) . . . no P10 C17 C18 115.3(4) . . . no P10 C17 C19 114.4(4) . . . no P10 C17 H21 105(3) . . . no C18 C17 C19 109.0(5) . . . no C18 C17 H21 105(3) . . . no C19 C17 H21 107(3) . . . no C17 C18 H22 118(3) . . . no C17 C18 H23 112(6) . . . no C17 C18 H24 104(3) . . . no H22 C18 H23 112(7) . . . no H22 C18 H24 104(4) . . . no H23 C18 H24 106(7) . . . no C17 C19 H25 112(4) . . . no C17 C19 H26 111(3) . . . no C17 C19 H27 120(4) . . . no H25 C19 H26 105(5) . . . no H25 C19 H27 102(5) . . . no H26 C19 H27 104(4) . . . no P20 C21 C22 112.8(4) . . . no P20 C21 C23 117.2(4) . . . no P20 C21 H28 102(3) . . . no C22 C21 C23 110.2(5) . . . no C22 C21 H28 110(3) . . . no C23 C21 H28 103(3) . . . no C21 C22 H29 118(3) . . . no C21 C22 H30 116(3) . . . no C21 C22 H31 114(3) . . . no H29 C22 H30 103(4) . . . no H29 C22 H31 96(4) . . . no H30 C22 H31 107(4) . . . no C21 C23 H32 108(3) . . . no C21 C23 H33 110(3) . . . no C21 C23 H34 112(3) . . . no H32 C23 H33 113(4) . . . no H32 C23 H34 102(4) . . . no H33 C23 H34 110(4) . . . no P20 C24 C25 114.6(4) . . . no P20 C24 C26 116.1(4) . . . no P20 C24 H35 100(3) . . . no C25 C24 C26 109.6(5) . . . no C25 C24 H35 108(3) . . . no C26 C24 H35 108(3) . . . no C24 C25 H36 111(4) . . . no C24 C25 H37 115(3) . . . no C24 C25 H38 117(3) . . . no H36 C25 H37 101(5) . . . no H36 C25 H38 107(5) . . . no H37 C25 H38 105(4) . . . no C24 C26 H39 113(3) . . . no C24 C26 H40 110(5) . . . no C24 C26 H41 109(4) . . . no H39 C26 H40 111(6) . . . no H39 C26 H41 103(4) . . . no H40 C26 H41 109(6) . . . no P20 C27 C28 112.5(4) . . . no P20 C27 C29 112.0(4) . . . no P20 C27 H42 111(3) . . . no C28 C27 C29 110.6(5) . . . no C28 C27 H42 107(3) . . . no C29 C27 H42 103(3) . . . no C27 C28 H43 115(3) . . . no C27 C28 H44 123(4) . . . no C27 C28 H45 111(3) . . . no H43 C28 H44 106(4) . . . no H43 C28 H45 103(4) . . . no H44 C28 H45 97(4) . . . no C27 C29 H46 112(3) . . . no C27 C29 H47 112(4) . . . no C27 C29 H48 114(3) . . . no H46 C29 H47 108(5) . . . no H46 C29 H48 98(4) . . . no H47 C29 H48 112(5) . . . no C31 C30 C35 121.4(8) . . . no C31 C30 H49 101(5) . . . no C35 C30 H49 137(5) . . . no C30 C31 C32 119.0(8) . . . no C30 C31 H50 130(4) . . . no C32 C31 H50 110(4) . . . no C31 C32 C33 118.7(8) . . . no C31 C32 H51 121(5) . . . no C33 C32 H51 121(5) . . . no C32 C33 C34 121.1(8) . . . no C32 C33 H52 120(5) . . . no C34 C33 H52 119(5) . . . no C33 C34 C35 120.4(8) . . . no C33 C34 H53 120(4) . . . no C35 C34 H53 119(4) . . . no C30 C35 C34 119.3(8) . . . no C30 C35 H54 117(4) . . . no C34 C35 H54 123(5) . . . no data_01088 _database_code_depnum_ccdc_archive 'CCDC 245546' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H52 N2 Os P2' _chemical_formula_weight 632.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.9882(3) _cell_length_b 21.8475(9) _cell_length_c 14.1438(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.4220(10) _cell_angle_gamma 90.00 _cell_volume 2754.14(19) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7153 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.53 _exptl_crystal_description 'thin plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 4.761 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.3293 _exptl_absorpt_correction_T_max 0.7019 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 30.16 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_number 7154 _diffrn_standards_decay_% 0.0 _diffrn_standards_interval_time 640 _diffrn_reflns_number 22120 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.52 _reflns_number_total 12431 _reflns_number_gt 11366 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XMView; WMView; (local package)' _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^)+(0.0324P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.265(7) _refine_ls_number_reflns 12431 _refine_ls_number_parameters 576 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0698 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 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 0.59435(2) 0.817288(10) 0.043948(14) 0.01623(5) Uani 1 1 d . . . N2 N 0.7947(6) 0.8534(3) 0.0286(4) 0.0226(11) Uani 1 1 d . . . C3 C 0.8144(8) 0.9162(3) 0.0354(5) 0.0252(15) Uani 1 1 d . . . C4 C 0.9473(8) 0.9480(4) 0.0298(5) 0.0306(17) Uani 1 1 d . . . H4 H 1.0360 0.9269 0.0190 0.037 Uiso 1 1 calc R . . C5 C 0.9477(9) 1.0108(4) 0.0402(6) 0.0368(19) Uani 1 1 d . . . H5 H 1.0382 1.0328 0.0374 0.044 Uiso 1 1 calc R . . C6 C 0.8170(9) 1.0429(4) 0.0549(6) 0.0389(19) Uani 1 1 d . . . H6 H 0.8191 1.0862 0.0614 0.047 Uiso 1 1 calc R . . C7 C 0.6857(9) 1.0109(3) 0.0597(6) 0.0349(18) Uani 1 1 d . . . H7 H 0.5975 1.0325 0.0700 0.042 Uiso 1 1 calc R . . C8 C 0.6806(8) 0.9470(3) 0.0496(5) 0.0238(14) Uani 1 1 d . . . N9 N 0.5592(6) 0.9092(3) 0.0539(4) 0.0217(11) Uani 1 1 d . . . C10 C 0.4187(8) 0.9400(4) 0.0658(6) 0.0332(17) Uani 1 1 d . . . H10A H 0.4296 0.9615 0.1272 0.050 Uiso 1 1 calc R . . H10B H 0.3381 0.9097 0.0642 0.050 Uiso 1 1 calc R . . H10C H 0.3940 0.9696 0.0141 0.050 Uiso 1 1 calc R . . P11 P 0.49357(16) 0.78272(8) 0.17582(11) 0.0186(3) Uani 1 1 d . . . C12 C 0.6146(7) 0.8098(4) 0.2851(4) 0.0284(15) Uani 1 1 d . . . H12 H 0.5765 0.7903 0.3413 0.034 Uiso 1 1 calc R . . C13 C 0.6060(8) 0.8787(3) 0.2976(5) 0.0347(17) Uani 1 1 d . . . H13A H 0.6735 0.8911 0.3545 0.052 Uiso 1 1 calc R . . H13B H 0.5029 0.8904 0.3051 0.052 Uiso 1 1 calc R . . H13C H 0.6362 0.8991 0.2414 0.052 Uiso 1 1 calc R . . C14 C 0.7773(8) 0.7890(4) 0.2848(6) 0.0375(19) Uani 1 1 d . . . H14A H 0.8204 0.8099 0.2334 0.056 Uiso 1 1 calc R . . H14B H 0.7798 0.7446 0.2747 0.056 Uiso 1 1 calc R . . H14C H 0.8357 0.7992 0.3462 0.056 Uiso 1 1 calc R . . C15 C 0.3058(6) 0.8121(4) 0.1988(4) 0.0235(12) Uani 1 1 d . . . H15 H 0.3177 0.8576 0.2031 0.028 Uiso 1 1 calc R . . C16 C 0.1789(7) 0.8017(4) 0.1196(5) 0.038(2) Uani 1 1 d . . . H16A H 0.1572 0.7578 0.1137 0.057 Uiso 1 1 calc R . . H16B H 0.2077 0.8171 0.0594 0.057 Uiso 1 1 calc R . . H16C H 0.0893 0.8235 0.1342 0.057 Uiso 1 1 calc R . . C17 C 0.2539(7) 0.7932(3) 0.2929(5) 0.0308(15) Uani 1 1 d . . . H17A H 0.1619 0.8153 0.3015 0.046 Uiso 1 1 calc R . . H17B H 0.3323 0.8029 0.3455 0.046 Uiso 1 1 calc R . . H17C H 0.2342 0.7490 0.2921 0.046 Uiso 1 1 calc R . . C18 C 0.4956(8) 0.6983(3) 0.1954(5) 0.0304(15) Uani 1 1 d . . . H18 H 0.5884 0.6835 0.1706 0.036 Uiso 1 1 calc R . . C19 C 0.5093(8) 0.6753(3) 0.2997(5) 0.0354(17) Uani 1 1 d . . . H19A H 0.4225 0.6893 0.3291 0.053 Uiso 1 1 calc R . . H19B H 0.6015 0.6915 0.3355 0.053 Uiso 1 1 calc R . . H19C H 0.5127 0.6304 0.3004 0.053 Uiso 1 1 calc R . . C20 C 0.3680(9) 0.6659(4) 0.1360(6) 0.043(2) Uani 1 1 d . . . H20A H 0.3937 0.6226 0.1298 0.064 Uiso 1 1 calc R . . H20B H 0.3504 0.6847 0.0727 0.064 Uiso 1 1 calc R . . H20C H 0.2770 0.6692 0.1671 0.064 Uiso 1 1 calc R . . P21 P 0.58042(17) 0.75334(8) -0.08467(11) 0.0193(3) Uani 1 1 d . . . C22 C 0.6074(9) 0.7973(3) -0.1947(5) 0.0303(16) Uani 1 1 d . . . H22 H 0.5544 0.7739 -0.2498 0.036 Uiso 1 1 calc R . . C23 C 0.5330(9) 0.8599(4) -0.1958(6) 0.046(2) Uani 1 1 d . . . H23A H 0.5927 0.8870 -0.1505 0.069 Uiso 1 1 calc R . . H23B H 0.4319 0.8556 -0.1775 0.069 Uiso 1 1 calc R . . H23C H 0.5263 0.8774 -0.2600 0.069 Uiso 1 1 calc R . . C24 C 0.7673(8) 0.8062(4) -0.2148(6) 0.0419(18) Uani 1 1 d . . . H24A H 0.7672 0.8281 -0.2752 0.063 Uiso 1 1 calc R . . H24B H 0.8153 0.7662 -0.2189 0.063 Uiso 1 1 calc R . . H24C H 0.8228 0.8300 -0.1631 0.063 Uiso 1 1 calc R . . C25 C 0.4017(7) 0.7131(3) -0.1242(5) 0.0293(15) Uani 1 1 d . . . H25 H 0.3805 0.6873 -0.0691 0.035 Uiso 1 1 calc R . . C26 C 0.2669(7) 0.7534(5) -0.1482(6) 0.051(2) Uani 1 1 d . . . H26A H 0.2756 0.7757 -0.2074 0.076 Uiso 1 1 calc R . . H26B H 0.2611 0.7827 -0.0963 0.076 Uiso 1 1 calc R . . H26C H 0.1759 0.7282 -0.1565 0.076 Uiso 1 1 calc R . . C27 C 0.4068(9) 0.6682(3) -0.2094(5) 0.0359(17) Uani 1 1 d . . . H27A H 0.3190 0.6413 -0.2147 0.054 Uiso 1 1 calc R . . H27B H 0.4984 0.6435 -0.1986 0.054 Uiso 1 1 calc R . . H27C H 0.4061 0.6917 -0.2685 0.054 Uiso 1 1 calc R . . C28 C 0.7177(8) 0.6895(3) -0.0821(5) 0.0303(15) Uani 1 1 d . . . H28 H 0.7204 0.6758 -0.1493 0.036 Uiso 1 1 calc R . . C29 C 0.8787(7) 0.7069(4) -0.0402(6) 0.0377(17) Uani 1 1 d . . . H29A H 0.8802 0.7191 0.0266 0.057 Uiso 1 1 calc R . . H29B H 0.9133 0.7411 -0.0766 0.057 Uiso 1 1 calc R . . H29C H 0.9451 0.6717 -0.0440 0.057 Uiso 1 1 calc R . . C30 C 0.6716(8) 0.6344(3) -0.0256(5) 0.0316(16) Uani 1 1 d . . . H30A H 0.7481 0.6023 -0.0246 0.047 Uiso 1 1 calc R . . H30B H 0.5751 0.6186 -0.0559 0.047 Uiso 1 1 calc R . . H30C H 0.6623 0.6470 0.0398 0.047 Uiso 1 1 calc R . . Os31 Os 0.85878(2) 0.476691(10) 0.455076(15) 0.01868(5) Uani 1 1 d . . . N32 N 0.6615(7) 0.4375(3) 0.4677(4) 0.0278(12) Uani 1 1 d . . . C33 C 0.6472(8) 0.3751(4) 0.4628(5) 0.0277(17) Uani 1 1 d . . . C34 C 0.5187(9) 0.3406(4) 0.4691(5) 0.0361(18) Uani 1 1 d . . . H34 H 0.4270 0.3603 0.4773 0.043 Uiso 1 1 calc R . . C35 C 0.5256(10) 0.2772(4) 0.4634(6) 0.043(2) Uani 1 1 d . . . H35 H 0.4382 0.2536 0.4682 0.051 Uiso 1 1 calc R . . C36 C 0.6565(11) 0.2483(4) 0.4509(6) 0.043(2) Uani 1 1 d . . . H36 H 0.6588 0.2049 0.4472 0.052 Uiso 1 1 calc R . . C37 C 0.7855(10) 0.2813(4) 0.4434(6) 0.040(2) Uani 1 1 d . . . H37 H 0.8755 0.2607 0.4341 0.048 Uiso 1 1 calc R . . C38 C 0.7837(8) 0.3462(4) 0.4497(5) 0.0284(15) Uani 1 1 d . . . N39 N 0.9014(6) 0.3853(3) 0.4432(4) 0.0266(13) Uani 1 1 d . . . C40 C 1.0443(9) 0.3561(4) 0.4338(6) 0.0374(19) Uani 1 1 d . . . H40A H 1.0712 0.3282 0.4877 0.056 Uiso 1 1 calc R . . H40B H 1.1221 0.3874 0.4334 0.056 Uiso 1 1 calc R . . H40C H 1.0358 0.3329 0.3741 0.056 Uiso 1 1 calc R . . P41 P 0.96484(17) 0.51495(8) 0.32716(11) 0.0194(3) Uani 1 1 d . . . C42 C 1.1511(6) 0.4850(4) 0.3040(4) 0.0251(14) Uani 1 1 d . . . H42 H 1.1362 0.4398 0.2956 0.030 Uiso 1 1 calc R . . C43 C 1.2075(7) 0.5066(4) 0.2118(5) 0.0308(15) Uani 1 1 d . . . H43A H 1.2272 0.5507 0.2157 0.046 Uiso 1 1 calc R . . H43B H 1.1312 0.4981 0.1575 0.046 Uiso 1 1 calc R . . H43C H 1.3003 0.4848 0.2034 0.046 Uiso 1 1 calc R . . C44 C 1.2799(7) 0.4916(5) 0.3879(5) 0.044(2) Uani 1 1 d . . . H60A H 1.3616 0.4635 0.3782 0.066 Uiso 1 1 calc R . . H60B H 1.2420 0.4817 0.4480 0.066 Uiso 1 1 calc R . . H60C H 1.3174 0.5338 0.3903 0.066 Uiso 1 1 calc R . . C45 C 0.8468(7) 0.4912(3) 0.2144(4) 0.0235(16) Uani 1 1 d . . . H44 H 0.8852 0.5127 0.1600 0.028 Uiso 1 1 calc R . . C46 C 0.8559(8) 0.4215(4) 0.1974(5) 0.0344(17) Uani 1 1 d . . . H46A H 0.8281 0.3995 0.2530 0.052 Uiso 1 1 calc R . . H46B H 0.9586 0.4105 0.1878 0.052 Uiso 1 1 calc R . . H46C H 0.7869 0.4102 0.1407 0.052 Uiso 1 1 calc R . . C47 C 0.6830(7) 0.5108(4) 0.2166(5) 0.040(2) Uani 1 1 d . . . H45A H 0.6237 0.5008 0.1554 0.061 Uiso 1 1 calc R . . H45B H 0.6789 0.5550 0.2277 0.061 Uiso 1 1 calc R . . H45C H 0.6419 0.4890 0.2680 0.061 Uiso 1 1 calc R . . C48 C 0.9720(9) 0.5997(3) 0.3138(6) 0.0347(18) Uani 1 1 d . . . H47 H 0.8825 0.6155 0.3414 0.042 Uiso 1 1 calc R . . C49 C 1.1082(10) 0.6271(5) 0.3761(7) 0.052(3) Uani 1 1 d . . . H48A H 1.1964 0.6247 0.3422 0.077 Uiso 1 1 calc R . . H48B H 1.1272 0.6040 0.4359 0.077 Uiso 1 1 calc R . . H48C H 1.0879 0.6700 0.3901 0.077 Uiso 1 1 calc R . . C50 C 0.9584(9) 0.6258(4) 0.2133(6) 0.047(2) Uani 1 1 d . . . H49A H 0.9717 0.6703 0.2165 0.070 Uiso 1 1 calc R . . H49B H 0.8590 0.6162 0.1795 0.070 Uiso 1 1 calc R . . H49C H 1.0358 0.6078 0.1791 0.070 Uiso 1 1 calc R . . P51 P 0.86806(17) 0.53743(8) 0.58759(11) 0.0199(3) Uani 1 1 d . . . C52 C 0.9207(8) 0.6196(3) 0.5859(5) 0.0268(14) Uani 1 1 d . . . H51 H 1.0153 0.6206 0.5557 0.032 Uiso 1 1 calc R . . C53 C 0.8099(10) 0.6593(4) 0.5218(6) 0.048(2) Uani 1 1 d . . . H52A H 0.7302 0.6733 0.5578 0.072 Uiso 1 1 calc R . . H52B H 0.7657 0.6352 0.4667 0.072 Uiso 1 1 calc R . . H52C H 0.8625 0.6947 0.4996 0.072 Uiso 1 1 calc R . . C54 C 0.9613(9) 0.6509(3) 0.6842(5) 0.0396(17) Uani 1 1 d . . . H53A H 1.0097 0.6903 0.6756 0.059 Uiso 1 1 calc R . . H53B H 1.0300 0.6245 0.7255 0.059 Uiso 1 1 calc R . . H53C H 0.8697 0.6575 0.7136 0.059 Uiso 1 1 calc R . . C55 C 0.6895(8) 0.5304(4) 0.6413(5) 0.0359(16) Uani 1 1 d . . . H54 H 0.6648 0.4857 0.6374 0.043 Uiso 1 1 calc R . . C56 C 0.5575(8) 0.5616(4) 0.5814(6) 0.051(2) Uani 1 1 d . . . H55A H 0.4636 0.5421 0.5937 0.076 Uiso 1 1 calc R . . H55B H 0.5686 0.5577 0.5137 0.076 Uiso 1 1 calc R . . H55C H 0.5554 0.6050 0.5986 0.076 Uiso 1 1 calc R . . C57 C 0.6955(10) 0.5464(4) 0.7475(6) 0.051(2) Uani 1 1 d . . . H56A H 0.7209 0.5898 0.7570 0.076 Uiso 1 1 calc R . . H56B H 0.7720 0.5212 0.7848 0.076 Uiso 1 1 calc R . . H56C H 0.5975 0.5384 0.7683 0.076 Uiso 1 1 calc R . . C58 C 1.0056(9) 0.5083(4) 0.6875(5) 0.0328(17) Uani 1 1 d . . . H57 H 0.9883 0.5310 0.7465 0.039 Uiso 1 1 calc R . . C59 C 0.9817(11) 0.4405(4) 0.7057(6) 0.044(2) Uani 1 1 d . . . H58A H 0.9973 0.4170 0.6488 0.066 Uiso 1 1 calc R . . H58B H 0.8792 0.4340 0.7201 0.066 Uiso 1 1 calc R . . H58C H 1.0533 0.4269 0.7598 0.066 Uiso 1 1 calc R . . C60 C 1.1703(8) 0.5202(4) 0.6702(6) 0.0396(18) Uani 1 1 d . . . H59A H 1.2385 0.5076 0.7265 0.059 Uiso 1 1 calc R . . H59B H 1.1839 0.5639 0.6584 0.059 Uiso 1 1 calc R . . H59C H 1.1922 0.4967 0.6146 0.059 Uiso 1 1 calc R . . H2 H 0.875(7) 0.841(3) 0.016(5) 0.018(19) Uiso 1 1 d . . . H32 H 0.584(7) 0.461(3) 0.478(5) 0.023(19) Uiso 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 Os1 0.01583(11) 0.01914(11) 0.01351(10) -0.00079(9) 0.00107(7) -0.00038(9) N2 0.020(3) 0.024(3) 0.022(3) 0.004(2) -0.005(2) -0.001(2) C3 0.035(4) 0.026(4) 0.013(3) 0.003(3) -0.001(2) -0.006(3) C4 0.030(4) 0.041(5) 0.018(4) 0.005(3) -0.006(3) -0.011(3) C5 0.048(5) 0.032(4) 0.027(4) 0.003(3) -0.010(3) -0.023(3) C6 0.061(5) 0.020(4) 0.033(5) -0.005(3) 0.001(3) -0.012(3) C7 0.061(5) 0.018(4) 0.026(4) -0.003(3) 0.007(3) 0.003(3) C8 0.038(4) 0.020(3) 0.012(3) 0.000(3) 0.002(2) -0.002(3) N9 0.029(3) 0.022(3) 0.014(3) 0.002(2) 0.004(2) 0.002(2) C10 0.037(4) 0.031(4) 0.032(4) 0.008(3) 0.004(3) 0.008(3) P11 0.0173(8) 0.0239(9) 0.0144(8) -0.0009(6) 0.0016(5) -0.0011(6) C12 0.024(3) 0.037(4) 0.022(3) 0.001(3) -0.003(2) -0.004(3) C13 0.043(4) 0.037(4) 0.024(4) -0.011(3) 0.006(3) -0.017(3) C14 0.022(4) 0.062(5) 0.027(4) 0.002(4) -0.002(3) -0.005(3) C15 0.018(3) 0.034(4) 0.019(3) 0.000(3) 0.003(2) 0.000(3) C16 0.023(3) 0.068(7) 0.023(3) 0.003(3) 0.002(2) 0.003(3) C17 0.029(4) 0.042(4) 0.024(4) 0.006(3) 0.010(3) 0.003(3) C18 0.036(4) 0.026(4) 0.031(4) 0.001(3) 0.014(3) 0.002(3) C19 0.049(4) 0.026(4) 0.032(4) 0.013(3) 0.007(3) 0.007(3) C20 0.071(6) 0.031(4) 0.028(4) -0.006(3) 0.017(4) -0.025(4) P21 0.0192(8) 0.0229(8) 0.0161(8) -0.0028(6) 0.0032(6) -0.0031(6) C22 0.040(4) 0.029(4) 0.023(4) -0.001(3) 0.009(3) -0.007(3) C23 0.050(5) 0.057(6) 0.031(5) 0.026(4) 0.010(3) 0.013(4) C24 0.048(4) 0.038(5) 0.043(4) 0.004(3) 0.020(3) -0.002(3) C25 0.031(4) 0.037(4) 0.020(3) -0.002(3) 0.001(3) -0.015(3) C26 0.013(3) 0.094(7) 0.045(5) -0.030(5) 0.000(3) 0.008(4) C27 0.045(4) 0.033(4) 0.028(4) -0.003(3) -0.003(3) -0.013(3) C28 0.036(4) 0.026(4) 0.031(4) -0.010(3) 0.012(3) -0.004(3) C29 0.028(4) 0.034(4) 0.053(5) -0.008(4) 0.012(3) 0.006(3) C30 0.037(4) 0.018(4) 0.039(4) 0.000(3) 0.002(3) 0.003(3) Os31 0.01765(11) 0.02472(12) 0.01329(11) -0.00111(10) 0.00057(7) 0.00047(9) N32 0.035(3) 0.029(3) 0.019(3) -0.001(2) 0.000(2) -0.002(2) C33 0.026(4) 0.045(5) 0.011(3) 0.003(3) -0.001(2) -0.007(3) C34 0.042(4) 0.046(5) 0.020(4) 0.001(3) 0.003(3) -0.018(3) C35 0.066(6) 0.042(5) 0.018(4) 0.006(3) -0.003(3) -0.031(4) C36 0.079(6) 0.036(5) 0.014(4) 0.004(3) 0.003(3) -0.011(4) C37 0.070(6) 0.033(5) 0.016(4) 0.000(4) 0.006(3) 0.000(4) C38 0.042(4) 0.031(4) 0.012(3) 0.002(3) 0.003(3) 0.000(3) N39 0.034(3) 0.033(4) 0.014(3) 0.006(2) 0.007(2) 0.006(2) C40 0.050(5) 0.032(5) 0.033(5) 0.009(4) 0.017(3) 0.014(3) P41 0.0186(8) 0.0230(9) 0.0162(8) -0.0012(6) 0.0005(5) -0.0009(6) C42 0.020(3) 0.040(4) 0.015(3) 0.001(3) 0.001(2) 0.000(3) C43 0.023(3) 0.046(4) 0.024(4) 0.003(3) 0.006(2) -0.001(3) C44 0.018(3) 0.084(8) 0.029(4) 0.003(4) -0.001(3) 0.001(4) C45 0.018(3) 0.042(5) 0.010(3) -0.001(3) -0.003(2) 0.002(3) C46 0.030(4) 0.050(5) 0.023(4) -0.004(3) -0.001(3) -0.006(3) C47 0.021(4) 0.076(6) 0.022(4) -0.005(4) -0.008(3) 0.007(3) C48 0.048(5) 0.024(4) 0.037(5) 0.003(3) 0.022(3) -0.006(3) C49 0.062(6) 0.051(6) 0.049(6) -0.012(5) 0.033(4) -0.026(4) C50 0.050(5) 0.038(5) 0.057(6) 0.015(4) 0.023(4) 0.009(4) P51 0.0203(8) 0.0243(9) 0.0148(8) -0.0019(6) 0.0016(6) 0.0000(6) C52 0.037(4) 0.021(3) 0.024(3) 0.000(3) 0.011(3) 0.003(3) C53 0.067(6) 0.036(5) 0.041(5) 0.005(4) 0.006(4) 0.018(4) C54 0.053(5) 0.032(4) 0.036(4) -0.012(3) 0.014(3) -0.013(3) C55 0.033(4) 0.045(4) 0.031(4) -0.011(3) 0.008(3) -0.006(3) C56 0.025(4) 0.073(6) 0.056(6) -0.019(5) 0.011(3) 0.010(4) C57 0.058(5) 0.061(6) 0.039(5) -0.013(4) 0.028(4) -0.010(4) C58 0.048(5) 0.037(4) 0.011(3) -0.005(3) -0.007(3) 0.008(3) C59 0.072(6) 0.032(5) 0.028(4) -0.003(4) 0.005(4) 0.017(4) C60 0.036(4) 0.047(5) 0.033(4) -0.008(3) -0.007(3) 0.010(3) _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 N2 2.004(5) . ? Os1 N9 2.041(6) . ? Os1 P21 2.2843(16) . ? Os1 P11 2.3035(15) . ? N2 C3 1.385(9) . ? C3 C4 1.394(10) . ? C3 C8 1.415(10) . ? C4 C5 1.379(10) . ? C5 C6 1.407(12) . ? C6 C7 1.381(11) . ? C7 C8 1.403(9) . ? C8 N9 1.376(9) . ? N9 C10 1.460(9) . ? P11 C18 1.864(7) . ? P11 C12 1.867(6) . ? P11 C15 1.873(6) . ? C12 C13 1.520(11) . ? C12 C14 1.532(9) . ? C15 C16 1.510(9) . ? C15 C17 1.523(8) . ? C18 C20 1.508(10) . ? C18 C19 1.548(10) . ? P21 C25 1.854(6) . ? P21 C28 1.860(7) . ? P21 C22 1.871(7) . ? C22 C24 1.513(9) . ? C22 C23 1.522(11) . ? C25 C26 1.501(10) . ? C25 C27 1.558(9) . ? C28 C30 1.530(10) . ? C28 C29 1.539(10) . ? Os31 N32 1.998(6) . ? Os31 N39 2.045(6) . ? Os31 P51 2.2892(16) . ? Os31 P41 2.3079(16) . ? N32 C33 1.370(10) . ? C33 C34 1.391(10) . ? C33 C38 1.412(11) . ? C34 C35 1.390(11) . ? C35 C36 1.366(13) . ? C36 C37 1.382(12) . ? C37 C38 1.421(10) . ? C38 N39 1.371(10) . ? N39 C40 1.455(9) . ? P41 C48 1.863(8) . ? P41 C42 1.866(6) . ? P41 C45 1.871(6) . ? C42 C43 1.533(8) . ? C42 C44 1.554(9) . ? C45 C47 1.537(9) . ? C45 C46 1.546(11) . ? C48 C50 1.523(11) . ? C48 C49 1.534(12) . ? P51 C52 1.858(7) . ? P51 C58 1.866(7) . ? P51 C55 1.869(7) . ? C52 C53 1.527(10) . ? C52 C54 1.550(9) . ? C55 C56 1.526(11) . ? C55 C57 1.536(10) . ? C58 C59 1.523(11) . ? C58 C60 1.553(11) . ? 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 N2 Os1 N9 76.7(2) . . ? N2 Os1 P21 96.45(17) . . ? N9 Os1 P21 131.58(15) . . ? N2 Os1 P11 132.04(16) . . ? N9 Os1 P11 100.74(16) . . ? P21 Os1 P11 117.22(6) . . ? C3 N2 Os1 119.4(5) . . ? N2 C3 C4 126.3(7) . . ? N2 C3 C8 112.2(6) . . ? C4 C3 C8 121.4(7) . . ? C5 C4 C3 118.7(8) . . ? C4 C5 C6 121.4(8) . . ? C7 C6 C5 119.3(8) . . ? C6 C7 C8 121.1(8) . . ? N9 C8 C7 127.5(7) . . ? N9 C8 C3 114.5(7) . . ? C7 C8 C3 118.1(7) . . ? C8 N9 C10 115.6(6) . . ? C8 N9 Os1 117.2(5) . . ? C10 N9 Os1 127.3(5) . . ? C18 P11 C12 101.3(4) . . ? C18 P11 C15 107.8(3) . . ? C12 P11 C15 100.9(3) . . ? C18 P11 Os1 116.6(2) . . ? C12 P11 Os1 108.6(2) . . ? C15 P11 Os1 119.0(2) . . ? C13 C12 C14 110.9(6) . . ? C13 C12 P11 112.2(5) . . ? C14 C12 P11 111.0(5) . . ? C16 C15 C17 108.7(5) . . ? C16 C15 P11 115.5(5) . . ? C17 C15 P11 116.3(5) . . ? C20 C18 C19 109.8(6) . . ? C20 C18 P11 113.0(6) . . ? C19 C18 P11 117.5(5) . . ? C25 P21 C28 101.3(3) . . ? C25 P21 C22 101.1(3) . . ? C28 P21 C22 104.2(3) . . ? C25 P21 Os1 119.1(2) . . ? C28 P21 Os1 118.4(2) . . ? C22 P21 Os1 110.4(2) . . ? C24 C22 C23 108.0(6) . . ? C24 C22 P21 116.8(6) . . ? C23 C22 P21 111.5(5) . . ? C26 C25 C27 107.3(6) . . ? C26 C25 P21 115.6(5) . . ? C27 C25 P21 114.9(5) . . ? C30 C28 C29 107.4(6) . . ? C30 C28 P21 112.1(5) . . ? C29 C28 P21 114.2(5) . . ? N32 Os31 N39 76.5(2) . . ? N32 Os31 P51 96.58(17) . . ? N39 Os31 P51 130.26(16) . . ? N32 Os31 P41 133.35(16) . . ? N39 Os31 P41 100.87(16) . . ? P51 Os31 P41 117.18(6) . . ? C33 N32 Os31 120.1(5) . . ? N32 C33 C34 127.5(7) . . ? N32 C33 C38 111.9(6) . . ? C34 C33 C38 120.6(8) . . ? C35 C34 C33 119.5(9) . . ? C36 C35 C34 120.9(8) . . ? C35 C36 C37 120.9(9) . . ? C36 C37 C38 120.0(9) . . ? N39 C38 C33 115.0(7) . . ? N39 C38 C37 126.9(8) . . ? C33 C38 C37 118.1(8) . . ? C38 N39 C40 115.6(7) . . ? C38 N39 Os31 116.6(5) . . ? C40 N39 Os31 127.7(5) . . ? C48 P41 C42 106.7(3) . . ? C48 P41 C45 102.3(4) . . ? C42 P41 C45 100.1(3) . . ? C48 P41 Os31 117.5(2) . . ? C42 P41 Os31 118.8(2) . . ? C45 P41 Os31 108.8(2) . . ? C43 C42 C44 108.9(5) . . ? C43 C42 P41 116.3(5) . . ? C44 C42 P41 115.5(5) . . ? C47 C45 C46 110.3(6) . . ? C47 C45 P41 110.2(5) . . ? C46 C45 P41 111.7(5) . . ? C50 C48 C49 110.6(7) . . ? C50 C48 P41 117.9(6) . . ? C49 C48 P41 111.4(6) . . ? C52 P51 C58 101.2(3) . . ? C52 P51 C55 108.6(3) . . ? C58 P51 C55 100.6(4) . . ? C52 P51 Os31 122.1(2) . . ? C58 P51 Os31 111.9(2) . . ? C55 P51 Os31 110.0(2) . . ? C53 C52 C54 110.0(6) . . ? C53 C52 P51 114.1(6) . . ? C54 C52 P51 116.4(5) . . ? C56 C55 C57 111.5(7) . . ? C56 C55 P51 112.6(5) . . ? C57 C55 P51 117.0(5) . . ? C59 C58 C60 110.4(7) . . ? C59 C58 P51 111.4(6) . . ? C60 C58 P51 112.0(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.797 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.120