# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1551 # This CIF-file is for the paper titled "Preparation and # Crystal Structures of Oxoosmium(VI) Diolato Complexes" # by Lehtonen et al. The reference number is 9/03042E. data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 O5 Os' _chemical_formula_weight 438.51 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' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42 nm' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, x, z' '-x, -y, z' '-y, -x, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' _cell_length_a 10.251(3) _cell_length_b 10.251 _cell_length_c 7.283(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 765.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.4 _cell_measurement_theta_max 19.3 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 8.340 _exptl_absorpt_correction_type ; empirical via \y scans (North, Phillips & Mathews, 1968) ; _exptl_absorpt_correction_T_min 0.286 _exptl_absorpt_correction_T_max 0.368 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method '\w--2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 446 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 24.94 _reflns_number_total 399 _reflns_number_gt 265 _reflns_threshold_expression I>2\s(I) __computing_data_collection ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_cell_refinement ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_data_reduction ; TEXSAN for WINDOWS (Molecular Structure Corporation, 1997) ; _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for WINDOWS (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+1.9400P] 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 SHELXL _refine_ls_extinction_coef 0.0081(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(5) _refine_ls_number_reflns 399 _refine_ls_number_parameters 68 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0610 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os Os 0.5000 0.5000 0.0000 0.0463(3) Uani 1 d SDU . . O1 O 0.5278(16) 0.5278(16) -0.2257(15) 0.056(8) Uiso 0.50 d SPD . . O2A O 0.509(3) 0.3202(10) 0.056(2) 0.043(8) Uani 0.50 d PDU . . O2B O 0.507(3) 0.3391(12) 0.127(3) 0.046(6) Uani 0.50 d PDU . . C1A C 0.642(3) 0.2723(17) 0.081(3) 0.056(9) Uani 0.50 d PDU . . C1B C 0.629(2) 0.2912(16) 0.206(3) 0.046(6) Uani 0.50 d PDU . . C2A C 0.697(2) 0.257(2) -0.114(4) 0.048(9) Uani 0.50 d PD . . C2B C 0.6443(18) 0.3557(18) 0.395(3) 0.097(9) Uani 1 d SD . . C3 C 0.6248(14) 0.1433(12) 0.182(2) 0.067(4) Uani 1 d 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 0.0514(4) 0.0514(4) 0.0360(4) 0.000 0.000 0.0111(7) O2A 0.034(8) 0.032(6) 0.06(2) -0.030(7) 0.012(15) -0.013(9) O2B 0.038(10) 0.040(9) 0.060(16) -0.014(9) 0.004(14) 0.009(11) C1A 0.033(13) 0.053(14) 0.08(3) -0.007(15) -0.014(16) 0.000(10) C1B 0.037(14) 0.063(15) 0.039(14) 0.000(12) -0.011(13) 0.005(11) C2A 0.047(17) 0.054(19) 0.043(13) -0.007(14) 0.006(15) -0.014(15) C2B 0.124(15) 0.124(15) 0.044(12) 0.005(10) -0.005(10) 0.048(19) C3 0.057(9) 0.053(9) 0.092(11) 0.016(10) 0.007(9) 0.009(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os O1 1.692(10) 3_665 ? Os O1 1.692(10) . y Os O2A 1.891(10) 4_665 ? Os O2A 1.891(10) 3_665 ? Os O2A 1.891(10) . y Os O2A 1.891(10) 2 ? Os O2B 1.891(10) 4_665 ? Os O2B 1.891(10) . y Os O2B 1.891(10) 3_665 ? Os O2B 1.891(10) 2 ? O1 O1 0.81(5) 3_665 ? O2A C1A 1.462(10) . y O2B C1B 1.460(10) . y C1A C1B 1.524(11) 4_665 y C1A C3 1.523(15) . ? C1A C2A 1.535(15) . ? C1B C1A 1.524(11) 4_665 ? C1B C3 1.527(14) . ? C1B C2B 1.534(14) . ? C2B C1B 1.534(14) 4_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Os O1 27.6(16) 3_665 . ? O1 Os O2A 111.6(7) 3_665 4_665 ? O1 Os O2A 93.2(8) . 4_665 ? O1 Os O2A 111.6(7) 3_665 3_665 ? O1 Os O2A 93.2(8) . 3_665 ? O2A Os O2A 92.7(17) 4_665 3_665 ? O1 Os O2A 93.2(8) 3_665 . ? O1 Os O2A 111.6(7) . . y O2A Os O2A 81.8(18) 4_665 . ? O2A Os O2A 154.9(11) 3_665 . ? O1 Os O2A 93.2(8) 3_665 2 ? O1 Os O2A 111.6(7) . 2 ? O2A Os O2A 154.9(11) 4_665 2 ? O2A Os O2A 81.8(18) 3_665 2 ? O2A Os O2A 92.7(17) . 2 y O1 Os O2B 127.8(8) 3_665 4_665 ? O1 Os O2B 109.5(9) . 4_665 y O2A Os O2B 88.6(6) 3_665 4_665 ? O2A Os O2B 79.2(6) . 4_665 y O2A Os O2B 138.3(8) 2 4_665 ? O1 Os O2B 109.5(9) 3_665 . ? O1 Os O2B 127.8(8) . . ? O2A Os O2B 138.3(8) 3_665 . y O2A Os O2B 88.6(6) 2 . ? O2B Os O2B 72.1(1>) 4_665 . ? O1 Os O2B 127.8(8) 3_665 3_665 ? O1 Os O2B 109.5(9) . 3_665 ? O2A Os O2B 88.6(6) 4_665 3_665 ? O2A Os O2B 16.6(9) 3_665 3_665 ? O2A Os O2B 138.3(8) . 3_665 ? O2A Os O2B 79.2(6) 2 3_665 ? O2B Os O2B 80.4(16) 4_665 3_665 y O2B Os O2B 121.7(13) . 3_665 ? O1 Os O2B 109.5(9) 3_665 2 ? O1 Os O2B 127.8(8) . 2 ? O2A Os O2B 138.3(8) 4_665 2 ? O2A Os O2B 79.2(6) 3_665 2 ? O2A Os O2B 88.6(6) . 2 ? O2A Os O2B 16.6(9) 2 2 ? O2B Os O2B 121.7(13) 4_665 2 ? O2B Os O2B 80.4(16) . 2 ? O2B Os O2B 72.1(16) 3_665 2 ? O1 O1 Os 76.2(8) 3_665 . ? C1A O2A Os 113.6(14) . . ? C1B O2B Os 121.4(15) . . ? O2A C1A C1B 106(2) . 4_665 ? O2A C1A C3 104.1(15) . . ? C1B C1A C3 109.9(18) 4_665 . ? O2A C1A C2A 105.2(18) . . ? C1B C1A C2A 117.2(19) 4_665 . ? C3 C1A C2A 113.6(19) . . ? O2B C1B C1A 100.3(19) . 4_665 ? O2B C1B C3 105.3(12) . . ? C1A C1B C3 113(2) 4_665 . ? O2B C1B C2B 107.4(17) . . ? C1A C1B C2B 105.9(15) 4_665 . ? C3 C1B C2B 122.3(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2A C1A C1B O2B -42.6(18) . . 4_665 4_665 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.94 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.476 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.095 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H77 O8 Os P' _chemical_formula_weight 1075.33 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' 'Os' 'Os' -1.2165 7.6030 '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' _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 15.055(5) _cell_length_b 15.899(8) _cell_length_c 12.677(5) _cell_angle_alpha 107.08(4) _cell_angle_beta 96.18(3) _cell_angle_gamma 112.90(3) _cell_volume 2585.4(19) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 5.9 _cell_measurement_theta_max 6.9 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 2.548 _exptl_absorpt_correction_type ; empirical via \y scans (North, Phillips & Mathews, 1968) ; _exptl_absorpt_correction_T_min 0.5683 _exptl_absorpt_correction_T_max 0.7011 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method '\w--2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9491 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9113 _reflns_number_gt 7148 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; MSC/AFC Control Program (Molecular Structure Corporation, 1995) ; _computing_cell_refinement ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_data_reduction ; TEXSAN for WINDOWS(Molecular Structure Corporation, 1997) ; _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for WINDOWS (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.2500P] 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 9113 _refine_ls_number_parameters 585 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os Os 0.761757(15) 0.603246(14) 0.786013(18) 0.03769(7) Uani 1 d . . . P P 0.53653(10) 0.79586(9) 0.23360(11) 0.0448(3) Uani 1 d . . . O1 O 0.6379(3) 0.5428(2) 0.7595(3) 0.0562(10) Uani 1 d . . . O2 O 0.7973(2) 0.7325(2) 0.7930(3) 0.0392(8) Uani 1 d . . . O3 O 0.8197(2) 0.6684(2) 0.9455(3) 0.0459(8) Uani 1 d . . . O4 O 0.8250(2) 0.5233(2) 0.8022(3) 0.0417(8) Uani 1 d . . . O5 O 0.7977(2) 0.5826(2) 0.6455(3) 0.0415(8) Uani 1 d . . . O6 O 0.7065(3) 1.0135(3) 0.1091(3) 0.0589(11) Uani 1 d . . . O7 O 0.7702(4) 1.0524(3) 0.3507(4) 0.0738(14) Uani 1 d . . . O8 O 0.6084(3) 0.8696(2) 0.1964(3) 0.0602(10) Uani 1 d . . . C1 C 0.7992(4) 0.7978(3) 0.9040(4) 0.0433(12) Uani 1 d . . . C2 C 0.6910(4) 0.7737(4) 0.9083(5) 0.0534(14) Uani 1 d . . . H2A H 0.6580 0.7073 0.9069 0.080 Uiso 1 calc R . . H2B H 0.6907 0.8177 0.9798 0.080 Uiso 1 calc R . . C3 C 0.6326(4) 0.7825(4) 0.8110(5) 0.0682(17) Uani 1 d . . . H3A H 0.5652 0.7672 0.8187 0.102 Uiso 1 calc R . . H3B H 0.6290 0.7359 0.7393 0.102 Uiso 1 calc R . . C4 C 0.6825(5) 0.8868(5) 0.8107(6) 0.0770(19) Uani 1 d . . . H4A H 0.6477 0.8901 0.7442 0.115 Uiso 1 calc R . . H4B H 0.6787 0.9325 0.8781 0.115 Uiso 1 calc R . . C5 C 0.7917(5) 0.9154(4) 0.8089(5) 0.0637(16) Uani 1 d . . . H5A H 0.7942 0.8760 0.7357 0.096 Uiso 1 calc R . . H5B H 0.8233 0.9836 0.8160 0.096 Uiso 1 calc R . . C6 C 0.8511(4) 0.9023(3) 0.9033(5) 0.0535(14) Uani 1 d . . . H6A H 0.8585 0.9495 0.9765 0.080 Uiso 1 calc R . . H6B H 0.9172 0.9151 0.8920 0.080 Uiso 1 calc R . . C7 C 0.8551(4) 0.7745(3) 0.9927(4) 0.0418(12) Uani 1 d . . . C8 C 0.9679(4) 0.8201(4) 1.0069(4) 0.0537(14) Uani 1 d . . . H8A H 0.9816 0.7986 0.9332 0.081 Uiso 1 calc R . . H8B H 0.9939 0.8910 1.0340 0.081 Uiso 1 calc R . . C9 C 1.0216(4) 0.7927(4) 1.0898(5) 0.0639(16) Uani 1 d . . . H9A H 1.0928 0.8256 1.0983 0.096 Uiso 1 calc R . . H9B H 1.0006 0.7225 1.0597 0.096 Uiso 1 calc R . . C10 C 0.9990(5) 0.8224(5) 1.2075(5) 0.0772(19) Uani 1 d . . . H10A H 1.0317 0.8021 1.2583 0.116 Uiso 1 calc R . . H10B H 1.0246 0.8932 1.2405 0.116 Uiso 1 calc R . . C11 C 0.8874(5) 0.7743(5) 1.1945(5) 0.0719(18) Uani 1 d . . . H11A H 0.8739 0.7961 1.2683 0.108 Uiso 1 calc R . . H11B H 0.8636 0.7038 1.1689 0.108 Uiso 1 calc R . . C12 C 0.8305(5) 0.7987(4) 1.1096(4) 0.0593(15) Uani 1 d . . . H12A H 0.8470 0.8679 1.1407 0.089 Uiso 1 calc R . . H12B H 0.7595 0.7618 1.0994 0.089 Uiso 1 calc R . . C13 C 0.8633(4) 0.4854(3) 0.7061(4) 0.0413(12) Uani 1 d . . . C14 C 0.9761(4) 0.5522(4) 0.7397(4) 0.0494(13) Uani 1 d . . . H14A H 1.0041 0.5310 0.6774 0.074 Uiso 1 calc R . . H14B H 0.9869 0.6188 0.7510 0.074 Uiso 1 calc R . . C15 C 1.0309(4) 0.5518(4) 0.8478(5) 0.0616(15) Uani 1 d . . . H15A H 1.0080 0.5793 0.9120 0.092 Uiso 1 calc R . . H15B H 1.1017 0.5927 0.8625 0.092 Uiso 1 calc R . . C16 C 1.0129(4) 0.4475(4) 0.8362(5) 0.0666(17) Uani 1 d . . . H16A H 1.0414 0.4220 0.7767 0.100 Uiso 1 calc R . . H16B H 1.0452 0.4484 0.9072 0.100 Uiso 1 calc R . . C17 C 0.9014(4) 0.3816(4) 0.8067(5) 0.0574(15) Uani 1 d . . . H17A H 0.8750 0.4035 0.8702 0.086 Uiso 1 calc R . . H17B H 0.8907 0.3150 0.7956 0.086 Uiso 1 calc R . . C18 C 0.8449(4) 0.3817(3) 0.6994(4) 0.0478(13) Uani 1 d . . . H18A H 0.7741 0.3424 0.6876 0.072 Uiso 1 calc R . . H18B H 0.8650 0.3516 0.6341 0.072 Uiso 1 calc R . . C19 C 0.8067(4) 0.4898(3) 0.6018(4) 0.0429(12) Uani 1 d . . . C20 C 0.7004(4) 0.4052(4) 0.5506(4) 0.0545(14) Uani 1 d . . . H20A H 0.7046 0.3438 0.5197 0.082 Uiso 1 calc R . . H20B H 0.6660 0.4018 0.6108 0.082 Uiso 1 calc R . . C21 C 0.6924(6) 0.4234(5) 0.3615(5) 0.093(2) Uani 1 d . . . H21A H 0.6554 0.4356 0.3050 0.140 Uiso 1 calc R . . H21B H 0.6938 0.3613 0.3247 0.140 Uiso 1 calc R . . C22 C 0.6401(5) 0.4172(4) 0.4573(5) 0.0741(19) Uani 1 d . . . H22A H 0.6318 0.4763 0.4885 0.111 Uiso 1 calc R . . H22B H 0.5745 0.3617 0.4273 0.111 Uiso 1 calc R . . C23 C 0.7990(5) 0.5055(5) 0.4072(5) 0.0748(19) Uani 1 d . . . H23A H 0.8325 0.5031 0.3459 0.112 Uiso 1 calc R . . H23B H 0.7968 0.5683 0.4325 0.112 Uiso 1 calc R . . C24 C 0.8590(5) 0.4981(4) 0.5059(4) 0.0600(15) Uani 1 d . . . H24A H 0.9229 0.5558 0.5366 0.090 Uiso 1 calc R . . H24B H 0.8714 0.4412 0.4773 0.090 Uiso 1 calc R . . C25 C 0.7429(4) 1.1095(3) 0.1965(4) 0.0448(12) Uani 1 d . . . C26 C 0.6552(4) 1.1233(4) 0.2368(4) 0.0647(16) Uani 1 d . . . H26A H 0.6236 1.0747 0.2695 0.097 Uiso 1 calc R . . H26B H 0.6803 1.1877 0.2961 0.097 Uiso 1 calc R . . C27 C 0.5786(5) 1.1140(6) 0.1417(6) 0.098(3) Uani 1 d . . . H27A H 0.5275 1.1279 0.1726 0.147 Uiso 1 calc R . . H27B H 0.5471 1.0470 0.0870 0.147 Uiso 1 calc R . . C28 C 0.6245(7) 1.1835(6) 0.0814(6) 0.104(3) Uani 1 d . . . H28A H 0.6477 1.2505 0.1334 0.155 Uiso 1 calc R . . H28B H 0.5739 1.1714 0.0171 0.155 Uiso 1 calc R . . C29 C 0.7112(6) 1.1713(5) 0.0391(5) 0.080(2) Uani 1 d . . . H29A H 0.7423 1.2211 0.0077 0.121 Uiso 1 calc R . . H29B H 0.6864 1.1075 -0.0213 0.121 Uiso 1 calc R . . C30 C 0.7887(5) 1.1802(4) 0.1355(5) 0.0641(16) Uani 1 d . . . H30A H 0.8201 1.2470 0.1905 0.096 Uiso 1 calc R . . H30B H 0.8399 1.1667 0.1045 0.096 Uiso 1 calc R . . C31 C 0.8203(4) 1.1186(3) 0.2961(4) 0.0442(12) Uani 1 d . . . C32 C 0.9032(5) 1.0954(5) 0.2540(5) 0.0710(18) Uani 1 d . . . H32A H 0.8736 1.0307 0.1945 0.107 Uiso 1 calc R . . H32B H 0.9394 1.1427 0.2216 0.107 Uiso 1 calc R . . C33 C 0.9757(6) 1.0986(6) 0.3504(6) 0.095(2) Uani 1 d . . . H33A H 0.9405 1.0490 0.3804 0.143 Uiso 1 calc R . . H33B H 1.0271 1.0840 0.3212 0.143 Uiso 1 calc R . . C34 C 1.0232(5) 1.1989(5) 0.4451(6) 0.088(2) Uani 1 d . . . H34A H 1.0672 1.1989 0.5070 0.132 Uiso 1 calc R . . H34B H 1.0629 1.2478 0.4166 0.132 Uiso 1 calc R . . C35 C 0.9442(5) 1.2251(5) 0.4893(5) 0.0732(18) Uani 1 d . . . H35A H 0.9758 1.2911 0.5462 0.110 Uiso 1 calc R . . H35B H 0.9096 1.1805 0.5255 0.110 Uiso 1 calc R . . C36 C 0.8688(4) 1.2191(4) 0.3926(4) 0.0538(14) Uani 1 d . . . H36A H 0.8174 1.2328 0.4231 0.081 Uiso 1 calc R . . H36B H 0.9024 1.2690 0.3623 0.081 Uiso 1 calc R . . C37 C 0.5992(4) 0.7616(4) 0.3296(4) 0.0484(13) Uani 1 d . . . C38 C 0.6900(4) 0.8313(4) 0.4062(5) 0.0638(16) Uani 1 d . . . H38 H 0.7188 0.8938 0.4035 0.096 Uiso 1 calc R . . C39 C 0.7376(5) 0.8099(5) 0.4853(5) 0.0744(18) Uani 1 d . . . H39 H 0.7982 0.8576 0.5355 0.112 Uiso 1 calc R . . C40 C 0.6954(5) 0.7170(5) 0.4904(6) 0.0774(19) Uani 1 d . . . H40 H 0.7272 0.7018 0.5440 0.116 Uiso 1 calc R . . C41 C 0.6061(5) 0.6477(5) 0.4152(6) 0.084(2) Uani 1 d . . . H41 H 0.5775 0.5855 0.4187 0.126 Uiso 1 calc R . . C42 C 0.5582(5) 0.6683(4) 0.3352(5) 0.0678(17) Uani 1 d . . . H42 H 0.4981 0.6199 0.2845 0.102 Uiso 1 calc R . . C43 C 0.4560(4) 0.6845(3) 0.1139(4) 0.0432(12) Uani 1 d . . . C44 C 0.4978(5) 0.6512(5) 0.0300(5) 0.082(2) Uani 1 d . . . H44 H 0.5653 0.6868 0.0366 0.122 Uiso 1 calc R . . C45 C 0.4425(6) 0.5661(6) -0.0639(6) 0.100(3) Uani 1 d . . . H45 H 0.4719 0.5454 -0.1206 0.150 Uiso 1 calc R . . C46 C 0.3442(5) 0.5127(4) -0.0723(5) 0.0748(19) Uani 1 d . . . H46 H 0.3064 0.4548 -0.1348 0.112 Uiso 1 calc R . . C47 C 0.3010(4) 0.5434(4) 0.0096(5) 0.0681(17) Uani 1 d . . . H47 H 0.2338 0.5066 0.0029 0.102 Uiso 1 calc R . . C48 C 0.3564(4) 0.6291(4) 0.1033(5) 0.0593(15) Uani 1 d . . . H48 H 0.3264 0.6494 0.1595 0.089 Uiso 1 calc R . . C49 C 0.4570(4) 0.8395(4) 0.3061(4) 0.0480(13) Uani 1 d . . . C50 C 0.4467(5) 0.8385(4) 0.4129(5) 0.0671(17) Uani 1 d . . . H50 H 0.4813 0.8144 0.4511 0.101 Uiso 1 calc R . . C51 C 0.3836(6) 0.8742(5) 0.4631(6) 0.083(2) Uani 1 d . . . H51 H 0.3758 0.8729 0.5344 0.125 Uiso 1 calc R . . C52 C 0.3346(6) 0.9102(5) 0.4090(7) 0.089(2) Uani 1 d . . . H52 H 0.2931 0.9337 0.4433 0.134 Uiso 1 calc R . . C53 C 0.3447(6) 0.9126(6) 0.3047(8) 0.106(3) Uani 1 d . . . H53 H 0.3099 0.9373 0.2676 0.160 Uiso 1 calc R . . C54 C 0.4066(6) 0.8785(5) 0.2540(5) 0.084(2) Uani 1 d . . . H54 H 0.4145 0.8818 0.1833 0.126 Uiso 1 calc R . . H1 H 0.669(4) 0.973(4) 0.131(5) 0.07(2) Uiso 1 d . . . H2 H 0.722(4) 1.005(4) 0.300(5) 0.08(2) Uiso 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 0.03930(11) 0.02553(10) 0.04247(11) 0.00716(8) 0.01519(8) 0.01132(8) P 0.0422(8) 0.0395(7) 0.0435(8) 0.0182(6) 0.0080(6) 0.0075(6) O1 0.046(2) 0.039(2) 0.074(3) 0.0120(18) 0.0224(19) 0.0132(17) O2 0.0436(19) 0.0275(16) 0.0439(19) 0.0080(14) 0.0154(16) 0.0157(15) O3 0.060(2) 0.0259(17) 0.045(2) 0.0081(15) 0.0178(17) 0.0147(16) O4 0.054(2) 0.0335(17) 0.0429(19) 0.0150(15) 0.0210(16) 0.0218(16) O5 0.054(2) 0.0318(17) 0.0395(18) 0.0099(15) 0.0165(16) 0.0215(16) O6 0.079(3) 0.036(2) 0.037(2) 0.0023(17) 0.014(2) 0.009(2) O7 0.087(3) 0.054(3) 0.049(3) 0.024(2) 0.000(2) 0.001(3) O8 0.056(2) 0.044(2) 0.067(3) 0.0281(19) 0.013(2) 0.0028(18) C1 0.052(3) 0.029(2) 0.041(3) 0.005(2) 0.018(2) 0.014(2) C2 0.054(3) 0.044(3) 0.063(4) 0.012(3) 0.027(3) 0.025(3) C3 0.061(4) 0.066(4) 0.080(4) 0.016(3) 0.019(3) 0.038(3) C4 0.095(5) 0.070(4) 0.079(5) 0.025(4) 0.015(4) 0.053(4) C5 0.089(5) 0.038(3) 0.064(4) 0.020(3) 0.018(3) 0.027(3) C6 0.066(4) 0.026(3) 0.062(4) 0.013(2) 0.021(3) 0.016(3) C7 0.054(3) 0.026(2) 0.038(3) 0.005(2) 0.014(2) 0.015(2) C8 0.055(4) 0.039(3) 0.058(3) 0.014(3) 0.014(3) 0.015(3) C9 0.068(4) 0.052(3) 0.061(4) 0.014(3) 0.003(3) 0.024(3) C10 0.104(6) 0.072(4) 0.051(4) 0.014(3) 0.002(4) 0.044(4) C11 0.109(6) 0.065(4) 0.044(3) 0.019(3) 0.028(4) 0.039(4) C12 0.081(4) 0.048(3) 0.049(3) 0.011(3) 0.026(3) 0.031(3) C13 0.047(3) 0.035(3) 0.039(3) 0.008(2) 0.014(2) 0.019(2) C14 0.047(3) 0.044(3) 0.055(3) 0.017(3) 0.019(3) 0.017(3) C15 0.053(4) 0.059(4) 0.069(4) 0.025(3) 0.015(3) 0.020(3) C16 0.060(4) 0.076(4) 0.072(4) 0.029(3) 0.010(3) 0.038(4) C17 0.069(4) 0.047(3) 0.065(4) 0.021(3) 0.012(3) 0.033(3) C18 0.049(3) 0.037(3) 0.056(3) 0.012(2) 0.012(3) 0.022(3) C19 0.051(3) 0.032(3) 0.043(3) 0.007(2) 0.016(2) 0.020(2) C20 0.070(4) 0.038(3) 0.046(3) 0.004(2) 0.001(3) 0.025(3) C21 0.138(7) 0.086(5) 0.047(4) 0.009(4) -0.004(4) 0.058(5) C22 0.084(5) 0.051(4) 0.065(4) 0.009(3) -0.010(4) 0.024(3) C23 0.118(6) 0.085(5) 0.043(3) 0.028(3) 0.030(4) 0.061(5) C24 0.090(5) 0.062(4) 0.047(3) 0.021(3) 0.030(3) 0.048(3) C25 0.058(3) 0.031(3) 0.032(3) 0.006(2) 0.008(2) 0.011(2) C26 0.069(4) 0.070(4) 0.040(3) 0.003(3) 0.005(3) 0.031(3) C27 0.087(6) 0.132(7) 0.063(5) 0.004(5) -0.002(4) 0.066(5) C28 0.149(8) 0.111(6) 0.050(4) 0.007(4) -0.017(5) 0.085(6) C29 0.116(6) 0.067(4) 0.060(4) 0.028(3) 0.015(4) 0.041(4) C30 0.083(4) 0.046(3) 0.050(3) 0.020(3) 0.009(3) 0.015(3) C31 0.055(3) 0.032(3) 0.038(3) 0.011(2) 0.014(2) 0.013(2) C32 0.089(5) 0.078(4) 0.057(4) 0.014(3) 0.019(3) 0.055(4) C33 0.109(6) 0.123(7) 0.077(5) 0.016(5) 0.018(4) 0.089(6) C34 0.067(5) 0.109(6) 0.073(5) 0.007(4) 0.005(4) 0.047(4) C35 0.068(4) 0.076(4) 0.055(4) -0.002(3) 0.003(3) 0.034(4) C36 0.047(3) 0.047(3) 0.049(3) -0.003(3) 0.004(3) 0.020(3) C37 0.047(3) 0.045(3) 0.044(3) 0.016(2) 0.008(3) 0.014(3) C38 0.054(4) 0.060(4) 0.059(4) 0.022(3) 0.000(3) 0.011(3) C39 0.065(4) 0.078(5) 0.066(4) 0.024(4) -0.006(3) 0.025(4) C40 0.083(5) 0.100(6) 0.072(5) 0.042(4) 0.010(4) 0.057(5) C41 0.088(5) 0.071(5) 0.100(6) 0.048(4) 0.009(4) 0.034(4) C42 0.064(4) 0.052(4) 0.076(4) 0.032(3) 0.000(3) 0.013(3) C43 0.044(3) 0.041(3) 0.040(3) 0.018(2) 0.013(2) 0.012(2) C44 0.050(4) 0.080(5) 0.065(4) -0.003(4) 0.025(3) -0.001(3) C45 0.087(6) 0.104(6) 0.063(4) -0.010(4) 0.031(4) 0.023(5) C46 0.071(5) 0.054(4) 0.062(4) 0.007(3) 0.006(4) 0.003(3) C47 0.044(3) 0.068(4) 0.060(4) 0.014(3) 0.009(3) 0.001(3) C48 0.044(3) 0.061(4) 0.055(3) 0.017(3) 0.019(3) 0.007(3) C49 0.050(3) 0.043(3) 0.038(3) 0.011(2) 0.003(2) 0.013(3) C50 0.086(5) 0.065(4) 0.051(4) 0.029(3) 0.023(3) 0.026(4) C51 0.104(6) 0.076(5) 0.065(4) 0.021(4) 0.044(4) 0.033(4) C52 0.101(6) 0.062(4) 0.103(6) 0.016(4) 0.045(5) 0.040(4) C53 0.130(7) 0.113(7) 0.114(7) 0.039(6) 0.037(6) 0.092(6) C54 0.117(6) 0.104(6) 0.055(4) 0.032(4) 0.022(4) 0.071(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os O1 1.672(3) . y Os O2 1.882(3) . y Os O5 1.892(3) . y Os O3 1.899(3) . y Os O4 1.902(3) . y P O8 1.488(3) . y P C37 1.791(5) . y P C43 1.806(5) . y P C49 1.808(5) . y O2 C1 1.473(5) . y O3 C7 1.458(5) . y O4 C13 1.472(5) . y O5 C19 1.481(5) . y O6 C25 1.443(5) . y O6 H1 0.81(5) . y O7 C31 1.441(6) . y O7 H2 0.83(6) . y C1 C2 1.533(7) . ? C1 C6 1.540(6) . ? C1 C7 1.546(7) . y C2 C3 1.509(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.532(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.530(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.528(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.531(7) . ? C7 C12 1.542(6) . ? C8 C9 1.518(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.544(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.516(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.532(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C19 1.529(7) . ? C13 C18 1.535(6) . ? C13 C14 1.539(7) . ? C14 C15 1.524(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.531(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.524(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.526(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.528(7) . ? C19 C20 1.542(7) . ? C20 C22 1.514(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.523(9) . ? C21 C23 1.529(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.523(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C30 1.536(7) . ? C25 C26 1.536(7) . ? C25 C31 1.553(7) . y C26 C27 1.505(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.516(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.522(10) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.530(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C36 1.528(6) . ? C31 C32 1.539(7) . ? C32 C33 1.522(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.516(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.515(8) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.531(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.394(7) . ? C37 C42 1.396(7) . ? C38 C39 1.367(7) . ? C38 H38 0.9300 . ? C39 C40 1.388(8) . ? C39 H39 0.9300 . ? C40 C41 1.372(9) . ? C40 H40 0.9300 . ? C41 C42 1.370(8) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.371(7) . ? C43 C48 1.379(7) . ? C44 C45 1.380(8) . ? C44 H44 0.9300 . ? C45 C46 1.363(9) . ? C45 H45 0.9300 . ? C46 C47 1.353(8) . ? C46 H46 0.9300 . ? C47 C48 1.384(7) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C54 1.377(7) . ? C49 C50 1.383(7) . ? C50 C51 1.402(8) . ? C50 H50 0.9300 . ? C51 C52 1.338(9) . ? C51 H51 0.9300 . ? C52 C53 1.358(10) . ? C52 H52 0.9300 . ? C53 C54 1.376(9) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Os O2 109.39(15) . . y O1 Os O5 108.51(17) . . y O2 Os O5 85.56(13) . . y O1 Os O3 110.56(16) . . y O2 Os O3 82.14(14) . . y O5 Os O3 140.93(14) . . y O1 Os O4 111.86(15) . . y O2 Os O4 138.75(14) . . y O5 Os O4 82.32(13) . . y O3 Os O4 82.95(14) . . y O8 P C37 111.6(2) . . ? O8 P C43 111.4(2) . . ? C37 P C43 106.7(2) . . ? O8 P C49 113.0(2) . . ? C37 P C49 106.8(2) . . ? C43 P C49 107.1(2) . . ? C1 O2 Os 112.8(3) . . y C7 O3 Os 117.5(3) . . y C13 O4 Os 116.9(3) . . y C19 O5 Os 113.2(3) . . y C25 O6 H1 109(4) . . ? C31 O7 H2 106(4) . . ? O2 C1 C2 107.6(4) . . ? O2 C1 C6 105.3(4) . . ? C2 C1 C6 109.1(4) . . ? O2 C1 C7 104.4(3) . . ? C2 C1 C7 113.7(4) . . ? C6 C1 C7 116.0(4) . . ? C3 C2 C1 113.4(4) . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 110.3(5) . . ? C2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? C2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 110.3(5) . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C4 114.0(5) . . ? C6 C5 H5A 108.7 . . ? C4 C5 H5A 108.7 . . ? C6 C5 H5B 108.7 . . ? C4 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C5 C6 C1 111.4(4) . . ? C5 C6 H6A 109.3 . . ? C1 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C1 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? O3 C7 C8 106.5(4) . . ? O3 C7 C12 106.5(4) . . ? C8 C7 C12 110.6(4) . . ? O3 C7 C1 105.2(4) . . ? C8 C7 C1 113.2(4) . . ? C12 C7 C1 114.2(4) . . ? C9 C8 C7 112.7(4) . . ? C9 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? C9 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 110.8(5) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 109.9(5) . . ? C11 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? C11 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C10 C11 C12 112.4(5) . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C7 112.4(4) . . ? C11 C12 H12A 109.1 . . ? C7 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? C7 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? O4 C13 C19 106.1(4) . . ? O4 C13 C18 105.6(4) . . ? C19 C13 C18 115.0(4) . . ? O4 C13 C14 106.1(4) . . ? C19 C13 C14 113.7(4) . . ? C18 C13 C14 109.6(4) . . ? C15 C14 C13 113.3(4) . . ? C15 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? C15 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C14 C15 C16 111.0(5) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 109.7(4) . . ? C17 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? C17 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C16 C17 C18 112.5(5) . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? C17 C18 C13 112.7(4) . . ? C17 C18 H18A 109.0 . . ? C13 C18 H18A 109.0 . . ? C17 C18 H18B 109.0 . . ? C13 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O5 C19 C24 105.0(4) . . ? O5 C19 C13 104.7(4) . . ? C24 C19 C13 116.6(4) . . ? O5 C19 C20 107.7(4) . . ? C24 C19 C20 108.9(4) . . ? C13 C19 C20 113.2(4) . . ? C22 C20 C19 112.9(5) . . ? C22 C20 H20A 109.0 . . ? C19 C20 H20A 109.0 . . ? C22 C20 H20B 109.0 . . ? C19 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C23 111.0(5) . . ? C22 C21 H21A 109.4 . . ? C23 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C23 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C20 C22 C21 110.3(6) . . ? C20 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? C20 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C21 112.8(5) . . ? C24 C23 H23A 109.0 . . ? C21 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? C21 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C23 C24 C19 113.1(5) . . ? C23 C24 H24A 109.0 . . ? C19 C24 H24A 109.0 . . ? C23 C24 H24B 109.0 . . ? C19 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O6 C25 C30 103.9(4) . . ? O6 C25 C26 109.5(4) . . ? C30 C25 C26 109.9(5) . . ? O6 C25 C31 108.5(4) . . ? C30 C25 C31 113.2(4) . . ? C26 C25 C31 111.5(4) . . ? C27 C26 C25 112.7(5) . . ? C27 C26 H26A 109.1 . . ? C25 C26 H26A 109.1 . . ? C27 C26 H26B 109.1 . . ? C25 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C26 C27 C28 111.8(6) . . ? C26 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? C26 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 112.0(6) . . ? C27 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? C27 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C28 C29 C30 111.3(5) . . ? C28 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? C28 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C29 C30 C25 112.4(5) . . ? C29 C30 H30A 109.1 . . ? C25 C30 H30A 109.1 . . ? C29 C30 H30B 109.1 . . ? C25 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? O7 C31 C36 103.6(4) . . ? O7 C31 C32 109.6(4) . . ? C36 C31 C32 108.3(4) . . ? O7 C31 C25 109.3(4) . . ? C36 C31 C25 114.0(4) . . ? C32 C31 C25 111.6(4) . . ? C33 C32 C31 111.6(5) . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 110.6(6) . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C35 C34 C33 110.6(6) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 111.3(5) . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C31 C36 C35 112.4(4) . . ? C31 C36 H36A 109.1 . . ? C35 C36 H36A 109.1 . . ? C31 C36 H36B 109.1 . . ? C35 C36 H36B 109.1 . . ? H36A C36 H36B 107.9 . . ? C38 C37 C42 117.9(5) . . ? C38 C37 P 119.6(4) . . ? C42 C37 P 122.5(4) . . ? C39 C38 C37 121.6(6) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? C38 C39 C40 119.9(6) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C41 C40 C39 119.1(6) . . ? C41 C40 H40 120.5 . . ? C39 C40 H40 120.5 . . ? C42 C41 C40 121.5(6) . . ? C42 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C41 C42 C37 120.2(6) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? C44 C43 C48 118.0(5) . . ? C44 C43 P 117.6(4) . . ? C48 C43 P 124.4(4) . . ? C43 C44 C45 121.7(6) . . ? C43 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C46 C45 C44 119.1(6) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C47 C46 C45 120.5(6) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 120.4(5) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C43 C48 C47 120.3(5) . . ? C43 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C54 C49 C50 118.3(6) . . ? C54 C49 P 118.4(4) . . ? C50 C49 P 123.3(4) . . ? C49 C50 C51 119.5(6) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C52 C51 C50 120.5(6) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C51 C52 C53 120.8(7) . . ? C51 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? C52 C53 C54 119.8(7) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C53 C54 C49 121.1(6) . . ? C53 C54 H54 119.5 . . ? C49 C54 H54 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Os O2 C1 80.8(3) . . . . ? O5 Os O2 C1 -171.1(3) . . . . ? O3 Os O2 C1 -28.3(3) . . . . ? O4 Os O2 C1 -98.1(3) . . . . ? O1 Os O3 C7 -104.9(3) . . . . ? O2 Os O3 C7 2.9(3) . . . . ? O5 Os O3 C7 75.8(4) . . . . ? O4 Os O3 C7 144.4(3) . . . . ? O1 Os O4 C13 104.8(3) . . . . ? O2 Os O4 C13 -76.4(4) . . . . ? O5 Os O4 C13 -2.2(3) . . . . ? O3 Os O4 C13 -145.9(3) . . . . ? O1 Os O5 C19 -83.8(3) . . . . ? O2 Os O5 C19 167.2(3) . . . . ? O3 Os O5 C19 95.5(3) . . . . ? O4 Os O5 C19 26.7(3) . . . . ? Os O2 C1 C2 -75.8(4) . . . . ? Os O2 C1 C6 167.9(3) . . . . ? Os O2 C1 C7 45.3(4) . . . . ? O2 C1 C2 C3 -56.5(5) . . . . ? C6 C1 C2 C3 57.2(6) . . . . ? C7 C1 C2 C3 -171.6(4) . . . . ? C1 C2 C3 C4 -58.7(6) . . . . ? C2 C3 C4 C5 54.4(6) . . . . ? C3 C4 C5 C6 -53.1(7) . . . . ? C4 C5 C6 C1 53.0(6) . . . . ? O2 C1 C6 C5 62.6(5) . . . . ? C2 C1 C6 C5 -52.7(6) . . . . ? C7 C1 C6 C5 177.3(4) . . . . ? Os O3 C7 C8 -99.7(4) . . . . ? Os O3 C7 C12 142.2(3) . . . . ? Os O3 C7 C1 20.6(4) . . . . ? O2 C1 C7 O3 -39.4(4) . . . . y C2 C1 C7 O3 77.6(5) . . . . ? C6 C1 C7 O3 -154.7(4) . . . . ? O2 C1 C7 C8 76.4(4) . . . . ? C2 C1 C7 C8 -166.6(4) . . . . ? C6 C1 C7 C8 -38.9(6) . . . . ? O2 C1 C7 C12 -155.8(4) . . . . ? C2 C1 C7 C12 -38.8(6) . . . . ? C6 C1 C7 C12 88.9(5) . . . . ? O3 C7 C8 C9 -62.1(5) . . . . ? C12 C7 C8 C9 53.2(5) . . . . ? C1 C7 C8 C9 -177.2(4) . . . . ? C7 C8 C9 C10 -56.8(6) . . . . ? C8 C9 C10 C11 57.1(6) . . . . ? C9 C10 C11 C12 -56.0(6) . . . . ? C10 C11 C12 C7 53.9(6) . . . . ? O3 C7 C12 C11 64.3(6) . . . . ? C8 C7 C12 C11 -51.0(6) . . . . ? C1 C7 C12 C11 179.9(4) . . . . ? Os O4 C13 C19 -21.0(4) . . . . ? Os O4 C13 C18 -143.4(3) . . . . ? Os O4 C13 C14 100.3(4) . . . . ? O4 C13 C14 C15 60.4(5) . . . . ? C19 C13 C14 C15 176.6(4) . . . . ? C18 C13 C14 C15 -53.1(5) . . . . ? C13 C14 C15 C16 56.4(6) . . . . ? C14 C15 C16 C17 -56.1(6) . . . . ? C15 C16 C17 C18 55.8(6) . . . . ? C16 C17 C18 C13 -54.9(6) . . . . ? O4 C13 C18 C17 -62.2(5) . . . . ? C19 C13 C18 C17 -178.8(4) . . . . ? C14 C13 C18 C17 51.7(6) . . . . ? Os O5 C19 C24 -167.0(3) . . . . ? Os O5 C19 C13 -43.7(4) . . . . ? Os O5 C19 C20 77.0(4) . . . . ? O4 C13 C19 O5 38.7(4) . . . . y C18 C13 C19 O5 154.9(4) . . . . ? C14 C13 C19 O5 -77.6(5) . . . . ? O4 C13 C19 C24 154.2(4) . . . . ? C18 C13 C19 C24 -89.5(5) . . . . ? C14 C13 C19 C24 38.0(6) . . . . ? O4 C13 C19 C20 -78.3(5) . . . . ? C18 C13 C19 C20 38.0(6) . . . . ? C14 C13 C19 C20 165.4(4) . . . . ? O5 C19 C20 C22 57.3(6) . . . . ? C24 C19 C20 C22 -56.1(6) . . . . ? C13 C19 C20 C22 172.5(4) . . . . ? C19 C20 C22 C21 58.4(6) . . . . ? C23 C21 C22 C20 -55.2(7) . . . . ? C22 C21 C23 C24 52.8(7) . . . . ? C21 C23 C24 C19 -52.4(7) . . . . ? O5 C19 C24 C23 -62.8(6) . . . . ? C13 C19 C24 C23 -178.1(4) . . . . ? C20 C19 C24 C23 52.3(6) . . . . ? O6 C25 C26 C27 -59.4(7) . . . . ? C30 C25 C26 C27 54.1(7) . . . . ? C31 C25 C26 C27 -179.5(5) . . . . ? C25 C26 C27 C28 -54.9(8) . . . . ? C26 C27 C28 C29 54.3(8) . . . . ? C27 C28 C29 C30 -53.6(8) . . . . ? C28 C29 C30 C25 54.1(7) . . . . ? O6 C25 C30 C29 63.5(6) . . . . ? C26 C25 C30 C29 -53.7(6) . . . . ? C31 C25 C30 C29 -179.1(5) . . . . ? O6 C25 C31 O7 -67.4(5) . . . . y C30 C25 C31 O7 177.9(4) . . . . ? C26 C25 C31 O7 53.4(5) . . . . ? O6 C25 C31 C36 177.2(4) . . . . ? C30 C25 C31 C36 62.5(6) . . . . ? C26 C25 C31 C36 -62.0(6) . . . . ? O6 C25 C31 C32 54.0(5) . . . . ? C30 C25 C31 C32 -60.7(6) . . . . ? C26 C25 C31 C32 174.8(5) . . . . ? O7 C31 C32 C33 -55.5(7) . . . . ? C36 C31 C32 C33 57.0(7) . . . . ? C25 C31 C32 C33 -176.7(5) . . . . ? C31 C32 C33 C34 -58.9(8) . . . . ? C32 C33 C34 C35 57.0(8) . . . . ? C33 C34 C35 C36 -55.3(8) . . . . ? O7 C31 C36 C35 61.1(6) . . . . ? C32 C31 C36 C35 -55.3(6) . . . . ? C25 C31 C36 C35 179.8(4) . . . . ? C34 C35 C36 C31 55.7(7) . . . . ? O8 P C37 C38 34.5(5) . . . . ? C43 P C37 C38 156.4(5) . . . . ? C49 P C37 C38 -89.4(5) . . . . ? O8 P C37 C42 -148.9(5) . . . . ? C43 P C37 C42 -27.0(5) . . . . ? C49 P C37 C42 87.3(5) . . . . ? C42 C37 C38 C39 -0.5(9) . . . . ? P C37 C38 C39 176.3(5) . . . . ? C37 C38 C39 C40 -0.1(10) . . . . ? C38 C39 C40 C41 0.1(10) . . . . ? C39 C40 C41 C42 0.3(11) . . . . ? C40 C41 C42 C37 -0.9(11) . . . . ? C38 C37 C42 C41 0.9(9) . . . . ? P C37 C42 C41 -175.8(5) . . . . ? O8 P C43 C44 40.0(5) . . . . ? C37 P C43 C44 -82.1(5) . . . . ? C49 P C43 C44 163.9(5) . . . . ? O8 P C43 C48 -142.5(5) . . . . ? C37 P C43 C48 95.5(5) . . . . ? C49 P C43 C48 -18.5(5) . . . . ? C48 C43 C44 C45 1.4(10) . . . . ? P C43 C44 C45 179.1(6) . . . . ? C43 C44 C45 C46 -1.4(12) . . . . ? C44 C45 C46 C47 0.8(12) . . . . ? C45 C46 C47 C48 -0.4(11) . . . . ? C44 C43 C48 C47 -1.0(9) . . . . ? P C43 C48 C47 -178.5(5) . . . . ? C46 C47 C48 C43 0.4(10) . . . . ? O8 P C49 C54 51.5(5) . . . . ? C37 P C49 C54 174.5(5) . . . . ? C43 P C49 C54 -71.5(5) . . . . ? O8 P C49 C50 -126.4(5) . . . . ? C37 P C49 C50 -3.4(5) . . . . ? C43 P C49 C50 110.6(5) . . . . ? C54 C49 C50 C51 1.9(9) . . . . ? P C49 C50 C51 179.7(5) . . . . ? C49 C50 C51 C52 -0.8(10) . . . . ? C50 C51 C52 C53 0.1(12) . . . . ? C51 C52 C53 C54 -0.5(13) . . . . ? C52 C53 C54 C49 1.6(13) . . . . ? C50 C49 C54 C53 -2.3(10) . . . . ? P C49 C54 C53 179.8(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _gmom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H1 O8 0.81(5) 2.01(5) 2.802(5) 166(6) . O7 H2 O8 0.83(6) 2.07(6) 2.886(6) 167(6) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.817 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.090 #===END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H40 O5 Os' _chemical_formula_weight 598.76 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' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.421(8) _cell_length_b 17.103(5) _cell_length_c 12.299(5) _cell_angle_alpha 107.61(3) _cell_angle_beta 96.28(4) _cell_angle_gamma 67.01(3) _cell_volume 3031(2) _cell_formula_units_Z 5 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 6.5 _exptl_crystal_description black _exptl_crystal_colour prism _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1500 _exptl_absorpt_coefficient_mu 5.290 _exptl_absorpt_correction_type ; empirical via \y scans (North, Phillips & Mathews, 1968) ; _exptl_absorpt_correction_T_min 0.3891 _exptl_absorpt_correction_T_max 0.4494 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method '\w--2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.8 _diffrn_reflns_number 11092 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0920 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10686 _reflns_number_gt 7331 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; MSC/AFC Control Program (Molecular Structure Corporation, 1995) ; _computing_cell_refinement ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_data_reduction ; TEXSAN for WINDOWS(Molecular Structure Corporation, 1997) ; _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for WINDOWS (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.3230P] 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 10686 _refine_ls_number_parameters 766 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.040 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.83357(2) 0.24561(2) 0.37930(3) 0.03100(10) Uani 1 d . . . Os2 Os 0.56743(2) 0.14494(2) 0.81595(3) 0.02877(10) Uani 1 d . . . Os3 Os 0.01550(4) 0.47110(4) 1.06084(6) 0.02966(16) Uani 0.50 d P . . O1 O 0.8620(4) 0.1700(4) 0.2528(5) 0.0441(16) Uani 1 d . . . O2 O 0.9316(4) 0.2707(4) 0.4523(5) 0.0333(14) Uani 1 d . . . O3 O 0.8005(4) 0.3594(4) 0.3568(5) 0.0354(14) Uani 1 d . . . O4 O 0.7125(4) 0.2879(4) 0.4197(5) 0.0372(14) Uani 1 d . . . O5 O 0.8457(4) 0.1830(4) 0.4861(5) 0.0382(15) Uani 1 d . . . O6 O 0.5526(4) 0.2043(4) 0.7244(5) 0.0456(16) Uani 1 d . . . O7 O 0.4561(3) 0.1516(3) 0.8551(4) 0.0303(13) Uani 1 d . . . O8 O 0.5809(4) 0.0256(4) 0.7379(5) 0.0352(14) Uani 1 d . . . O9 O 0.6889(4) 0.0922(4) 0.8494(5) 0.0373(15) Uani 1 d . . . O10 O 0.5651(4) 0.2198(4) 0.9668(5) 0.0340(14) Uani 1 d . . . O11 O 0.0345(8) 0.4221(9) 1.1642(10) 0.046(3) Uani 0.50 d P . . O12A O 0.0097(9) 0.5893(11) 1.1217(15) 0.035(4) Uani 0.50 d PD . . O12B O -0.0094(9) 0.6142(11) 1.0818(14) 0.032(4) Uani 0.50 d PD . . O13A O 0.122(2) 0.4521(16) 0.994(3) 0.049(8) Uani 0.50 d PD . . O13B O 0.1099(18) 0.4761(15) 0.973(2) 0.039(7) Uani 0.50 d PD . . C1 C 0.9508(5) 0.3361(5) 0.4139(7) 0.031(2) Uani 1 d . . . C2 C 1.0005(6) 0.2871(6) 0.2999(8) 0.047(2) Uani 1 d . . . H2A H 1.0145 0.3281 0.2729 0.056 Uiso 1 calc R . . H2B H 0.9627 0.2644 0.2440 0.056 Uiso 1 calc R . . C3 C 1.0867(7) 0.2096(7) 0.3111(10) 0.067(3) Uani 1 d . . . H3A H 1.0725 0.1653 0.3302 0.080 Uiso 1 calc R . . H3B H 1.1185 0.1821 0.2389 0.080 Uiso 1 calc R . . C4 C 1.1450(7) 0.2430(8) 0.4040(12) 0.087(5) Uani 1 d . . . H4A H 1.1978 0.1931 0.4115 0.105 Uiso 1 calc R . . H4B H 1.1633 0.2832 0.3810 0.105 Uiso 1 calc R . . C5 C 1.0982(7) 0.2901(7) 0.5184(10) 0.061(3) Uani 1 d . . . C6 C 1.0124(6) 0.3663(6) 0.5061(8) 0.050(3) Uani 1 d . . . H6A H 1.0270 0.4104 0.4871 0.060 Uiso 1 calc R . . H6B H 0.9812 0.3941 0.5788 0.060 Uiso 1 calc R . . C7 C 0.8586(6) 0.4075(6) 0.4054(7) 0.032(2) Uani 1 d . . . C8 C 0.8179(6) 0.4693(6) 0.5214(7) 0.040(2) Uani 1 d . . . H8A H 0.8558 0.5008 0.5592 0.048 Uiso 1 calc R . . H8B H 0.8148 0.4342 0.5687 0.048 Uiso 1 calc R . . C9 C 0.7247(7) 0.5365(6) 0.5097(9) 0.055(3) Uani 1 d . . . H9A H 0.6857 0.5052 0.4769 0.066 Uiso 1 calc R . . H9B H 0.7018 0.5749 0.5847 0.066 Uiso 1 calc R . . C10 C 0.7253(7) 0.5921(7) 0.4354(9) 0.059(3) Uani 1 d . . . H10A H 0.7598 0.6278 0.4713 0.071 Uiso 1 calc R . . H10B H 0.6654 0.6318 0.4265 0.071 Uiso 1 calc R . . C11 C 0.7647(7) 0.5332(6) 0.3199(9) 0.054(3) Uani 1 d . . . H11A H 0.7693 0.5694 0.2755 0.065 Uiso 1 calc R . . H11B H 0.7252 0.5042 0.2803 0.065 Uiso 1 calc R . . C12 C 0.8573(6) 0.4617(6) 0.3274(8) 0.046(2) Uani 1 d . . . H12A H 0.8763 0.4223 0.2515 0.055 Uiso 1 calc R . . H12B H 0.8992 0.4903 0.3550 0.055 Uiso 1 calc R . . C13 C 0.6902(6) 0.2551(6) 0.5043(7) 0.038(2) Uani 1 d . . . C14 C 0.6823(6) 0.3245(6) 0.6190(7) 0.041(2) Uani 1 d . . . H14A H 0.7381 0.3326 0.6356 0.049 Uiso 1 calc R . . H14B H 0.6712 0.3030 0.6780 0.049 Uiso 1 calc R . . C15 C 0.6087(6) 0.4139(6) 0.6225(9) 0.051(3) Uani 1 d . . . H15A H 0.6056 0.4549 0.6977 0.061 Uiso 1 calc R . . H15B H 0.6216 0.4382 0.5677 0.061 Uiso 1 calc R . . C16 C 0.5203(7) 0.4035(7) 0.5948(9) 0.061(3) Uani 1 d . . . H16A H 0.5051 0.3835 0.6527 0.074 Uiso 1 calc R . . H16B H 0.4744 0.4602 0.5940 0.074 Uiso 1 calc R . . C17 C 0.5263(6) 0.3373(7) 0.4802(9) 0.057(3) Uani 1 d . . . H17A H 0.5356 0.3609 0.4222 0.069 Uiso 1 calc R . . H17B H 0.4704 0.3293 0.4647 0.069 Uiso 1 calc R . . C18 C 0.5997(6) 0.2482(6) 0.4712(8) 0.046(2) Uani 1 d . . . H18A H 0.6030 0.2108 0.3934 0.055 Uiso 1 calc R . . H18B H 0.5858 0.2203 0.5206 0.055 Uiso 1 calc R . . C19 C 0.7681(6) 0.1657(6) 0.5004(7) 0.036(2) Uani 1 d . . . C20 C 0.7631(6) 0.0900(6) 0.3968(8) 0.046(2) Uani 1 d . . . H20A H 0.7566 0.1083 0.3280 0.055 Uiso 1 calc R . . H20B H 0.7113 0.0780 0.4046 0.055 Uiso 1 calc R . . C21 C 0.8464(7) 0.0047(6) 0.3858(10) 0.063(3) Uani 1 d . . . H21A H 0.8398 -0.0423 0.3220 0.076 Uiso 1 calc R . . H21B H 0.8976 0.0149 0.3708 0.076 Uiso 1 calc R . . C22 C 0.8604(9) -0.0234(7) 0.4950(11) 0.079(4) Uani 1 d . . . H22A H 0.8123 -0.0400 0.5052 0.095 Uiso 1 calc R . . H22B H 0.9151 -0.0747 0.4886 0.095 Uiso 1 calc R . . C23 C 0.8645(8) 0.0501(7) 0.5964(9) 0.065(3) Uani 1 d . . . H23A H 0.9171 0.0613 0.5904 0.078 Uiso 1 calc R . . H23B H 0.8694 0.0318 0.6649 0.078 Uiso 1 calc R . . C24 C 0.7842(7) 0.1348(6) 0.6069(8) 0.050(3) Uani 1 d . . . H24A H 0.7919 0.1809 0.6712 0.060 Uiso 1 calc R . . H24B H 0.7325 0.1255 0.6225 0.060 Uiso 1 calc R . . C25 C 0.4252(5) 0.0855(6) 0.7726(7) 0.032(2) Uani 1 d . . . C26 C 0.3903(6) 0.1197(6) 0.6676(7) 0.036(2) Uani 1 d . . . H26A H 0.3676 0.0788 0.6131 0.043 Uiso 1 calc R . . H26B H 0.4386 0.1218 0.6313 0.043 Uiso 1 calc R . . C27 C 0.3164(6) 0.2126(6) 0.7004(8) 0.044(2) Uani 1 d . . . H27A H 0.3399 0.2542 0.7514 0.053 Uiso 1 calc R . . H27B H 0.2957 0.2318 0.6324 0.053 Uiso 1 calc R . . C28 C 0.2396(6) 0.2123(7) 0.7583(9) 0.056(3) Uani 1 d . . . H28A H 0.2116 0.1761 0.7046 0.067 Uiso 1 calc R . . H28B H 0.1959 0.2722 0.7835 0.067 Uiso 1 calc R . . C29 C 0.2726(6) 0.1759(6) 0.8602(9) 0.050(3) Uani 1 d . . . H29A H 0.2912 0.2182 0.9184 0.060 Uiso 1 calc R . . H29B H 0.2237 0.1710 0.8915 0.060 Uiso 1 calc R . . C30 C 0.3486(6) 0.0865(6) 0.8349(8) 0.043(2) Uani 1 d . . . H30A H 0.3275 0.0414 0.7882 0.051 Uiso 1 calc R . . H30B H 0.3699 0.0721 0.9059 0.051 Uiso 1 calc R . . C31 C 0.5080(6) -0.0005(5) 0.7466(7) 0.034(2) Uani 1 d . . . C32 C 0.5314(6) -0.0447(6) 0.8433(8) 0.042(2) Uani 1 d . . . H32A H 0.5390 -0.0028 0.9131 0.051 Uiso 1 calc Z . . H32B H 0.4825 -0.0597 0.8553 0.051 Uiso 1 calc R . . C33 C 0.6154(7) -0.1284(6) 0.8189(8) 0.052(3) Uani 1 d . . . H33A H 0.6655 -0.1130 0.8139 0.063 Uiso 1 calc R . . H33B H 0.6257 -0.1548 0.8812 0.063 Uiso 1 calc R . . C34 C 0.6077(7) -0.1946(6) 0.7087(8) 0.054(3) Uani 1 d . . . H34A H 0.5614 -0.2145 0.7163 0.065 Uiso 1 calc R . . H34B H 0.6629 -0.2458 0.6929 0.065 Uiso 1 calc R . . C35 C 0.5865(6) -0.1536(6) 0.6101(8) 0.045(2) Uani 1 d . . . H35A H 0.5776 -0.1959 0.5416 0.054 Uiso 1 calc R . . H35B H 0.6365 -0.1408 0.5964 0.054 Uiso 1 calc R . . C36 C 0.5031(6) -0.0674(5) 0.6337(7) 0.036(2) Uani 1 d . . . H36A H 0.4959 -0.0408 0.5721 0.043 Uiso 1 calc R . . H36B H 0.4516 -0.0816 0.6349 0.043 Uiso 1 calc R . . C37 C 0.7190(6) 0.1316(6) 0.9616(8) 0.035(2) Uani 1 d . . . C38 C 0.7200(6) 0.0745(6) 1.0371(8) 0.046(2) Uani 1 d . . . H38A H 0.7340 0.1014 1.1146 0.055 Uiso 1 calc R . . H38B H 0.6614 0.0738 1.0382 0.055 Uiso 1 calc R . . C39 C 0.7864(7) -0.0206(7) 0.9976(10) 0.061(3) Uani 1 d . . . H39A H 0.7688 -0.0505 0.9241 0.073 Uiso 1 calc R . . H39B H 0.7870 -0.0520 1.0516 0.073 Uiso 1 calc R . . C40 C 0.8795(7) -0.0221(7) 0.9875(10) 0.065(3) Uani 1 d . . . H40A H 0.8992 0.0033 1.0622 0.078 Uiso 1 calc R . . H40B H 0.9206 -0.0828 0.9590 0.078 Uiso 1 calc R . . C41 C 0.8788(6) 0.0305(6) 0.9069(9) 0.052(3) Uani 1 d . . . H41A H 0.9373 0.0311 0.9039 0.063 Uiso 1 calc R . . H41B H 0.8643 0.0018 0.8307 0.063 Uiso 1 calc R . . C42 C 0.8120(6) 0.1253(6) 0.9453(8) 0.045(2) Uani 1 d . . . H42A H 0.8314 0.1562 1.0167 0.053 Uiso 1 calc R . . H42B H 0.8105 0.1552 0.8891 0.053 Uiso 1 calc R . . C43 C 0.6499(6) 0.2273(6) 1.0023(7) 0.034(2) Uani 1 d . . . C44 C 0.6632(6) 0.2895(6) 0.9457(8) 0.042(2) Uani 1 d . . . H44A H 0.6633 0.2651 0.8635 0.051 Uiso 1 calc R . . H44B H 0.7203 0.2937 0.9672 0.051 Uiso 1 calc R . . C45 C 0.5899(7) 0.3832(6) 0.9803(9) 0.051(3) Uani 1 d . . . H45A H 0.6010 0.4211 0.9438 0.061 Uiso 1 calc R . . H45B H 0.5330 0.3799 0.9547 0.061 Uiso 1 calc R . . C46 C 0.5876(8) 0.4225(7) 1.1088(10) 0.072(4) Uani 1 d . . . H46A H 0.6424 0.4312 1.1331 0.087 Uiso 1 calc R . . H46B H 0.5394 0.4800 1.1295 0.087 Uiso 1 calc R . . C47 C 0.5753(8) 0.3632(7) 1.1702(9) 0.067(3) Uani 1 d . . . H47A H 0.5163 0.3623 1.1552 0.080 Uiso 1 calc R . . H47B H 0.5799 0.3877 1.2517 0.080 Uiso 1 calc R . . C48 C 0.6443(7) 0.2668(6) 1.1328(8) 0.049(3) Uani 1 d . . . H48A H 0.7020 0.2661 1.1613 0.059 Uiso 1 calc R . . H48B H 0.6286 0.2301 1.1665 0.059 Uiso 1 calc R . . C49 C 0.0812(5) 0.6148(6) 1.0999(7) 0.032(2) Uani 1 d DU . . C50A C 0.0558(13) 0.6527(12) 0.9972(14) 0.040(5) Uani 0.50 d PDU . . C50B C 0.0921(14) 0.6697(12) 1.0259(16) 0.042(5) Uani 0.50 d PDU . . C51A C -0.0279(13) 0.7396(12) 1.0286(16) 0.053(6) Uani 0.50 d PDU . . C51B C 0.0209(15) 0.7634(13) 1.0475(19) 0.064(6) Uani 0.50 d PDU . . C52A C -0.0109(16) 0.8040(14) 1.1384(16) 0.046(6) Uani 0.50 d PDU . . C52B C 0.0245(18) 0.8176(15) 1.1692(18) 0.062(7) Uani 0.50 d PDU . . C53 C 0.0124(6) 0.7674(6) 1.2440(8) 0.051(3) Uani 1 d DU . . C54 C 0.0887(7) 0.6735(6) 1.2177(9) 0.067(3) Uani 1 d D . . C55 C 0.1547(6) 0.5191(6) 1.0683(7) 0.041(2) Uani 1 d DU . . C56A C 0.2055(12) 0.4896(11) 1.1740(14) 0.046(5) Uani 0.50 d PDU . . C56B C 0.1518(15) 0.4736(11) 1.1602(16) 0.057(6) Uani 0.50 d PDU . . C57A C 0.2805(16) 0.3960(13) 1.143(2) 0.052(7) Uani 0.50 d PDU . . C57B C 0.2131(15) 0.3761(10) 1.1281(18) 0.061(6) Uani 0.50 d PDU . . C58A C 0.3498(15) 0.3893(18) 1.061(2) 0.075(7) Uani 0.50 d PDU . . C58B C 0.3044(17) 0.3693(18) 1.101(3) 0.079(9) Uani 0.50 d PDU . . C59A C 0.3053(19) 0.4165(16) 0.954(2) 0.069(9) Uani 0.50 d PDU . . C59B C 0.3015(15) 0.4128(13) 1.005(2) 0.065(7) Uani 0.50 d PDU . . C60 C 0.2354(7) 0.5098(6) 1.0105(11) 0.075(3) Uani 1 d DU . . 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 0.0311(2) 0.0338(2) 0.0291(2) 0.00662(16) -0.00222(16) -0.01554(17) Os2 0.0261(2) 0.0329(2) 0.0300(2) 0.01074(16) -0.00199(15) -0.01298(16) Os3 0.0288(4) 0.0345(4) 0.0285(4) 0.0090(3) -0.0011(3) -0.0151(3) O1 0.047(4) 0.044(4) 0.036(4) 0.000(3) 0.007(3) -0.019(3) O2 0.027(3) 0.043(4) 0.038(3) 0.017(3) -0.007(3) -0.019(3) O3 0.029(3) 0.044(4) 0.040(4) 0.019(3) -0.007(3) -0.016(3) O4 0.029(3) 0.045(4) 0.042(4) 0.015(3) 0.001(3) -0.016(3) O5 0.035(4) 0.046(4) 0.042(4) 0.015(3) -0.006(3) -0.023(3) O6 0.044(4) 0.055(4) 0.048(4) 0.026(3) -0.007(3) -0.023(3) O7 0.028(3) 0.032(3) 0.028(3) 0.002(3) 0.004(2) -0.012(3) O8 0.032(3) 0.032(3) 0.040(4) 0.004(3) -0.002(3) -0.015(3) O9 0.030(3) 0.041(4) 0.038(4) 0.006(3) -0.004(3) -0.015(3) O10 0.030(3) 0.036(3) 0.036(3) 0.007(3) 0.001(3) -0.015(3) O11 0.051(8) 0.074(9) 0.031(7) 0.032(7) -0.015(6) -0.033(7) O12A 0.023(8) 0.033(10) 0.042(11) 0.004(7) 0.004(7) -0.007(7) O12B 0.015(7) 0.031(10) 0.040(11) 0.002(6) -0.003(6) -0.005(7) O13A 0.040(13) 0.023(13) 0.084(15) 0.003(10) 0.005(9) -0.019(12) O13B 0.018(10) 0.020(12) 0.069(13) -0.013(10) 0.033(9) -0.006(9) C1 0.020(4) 0.032(5) 0.047(6) 0.017(4) -0.001(4) -0.010(4) C2 0.036(6) 0.049(6) 0.056(7) 0.016(5) 0.004(5) -0.014(5) C3 0.049(7) 0.041(6) 0.091(9) 0.018(6) 0.019(6) 0.006(5) C4 0.017(6) 0.086(9) 0.164(14) 0.062(10) -0.012(7) -0.009(6) C5 0.030(6) 0.073(8) 0.078(8) 0.030(7) -0.006(6) -0.013(6) C6 0.046(6) 0.063(7) 0.052(6) 0.024(5) -0.014(5) -0.028(5) C7 0.037(5) 0.038(5) 0.030(5) 0.012(4) -0.001(4) -0.021(4) C8 0.042(6) 0.042(6) 0.038(5) 0.010(4) -0.002(4) -0.019(5) C9 0.052(7) 0.037(6) 0.065(7) 0.006(5) 0.019(6) -0.006(5) C10 0.053(7) 0.050(7) 0.075(8) 0.019(6) 0.009(6) -0.016(6) C11 0.055(7) 0.048(6) 0.065(7) 0.031(6) 0.002(6) -0.013(5) C12 0.053(7) 0.053(6) 0.038(6) 0.013(5) 0.011(5) -0.024(5) C13 0.048(6) 0.045(5) 0.027(5) 0.006(4) 0.003(4) -0.027(5) C14 0.032(5) 0.059(6) 0.031(5) 0.004(4) 0.006(4) -0.021(5) C15 0.051(7) 0.042(6) 0.054(7) 0.000(5) 0.007(5) -0.020(5) C16 0.046(7) 0.053(7) 0.070(8) 0.002(6) 0.013(6) -0.010(5) C17 0.038(6) 0.074(8) 0.058(7) 0.008(6) 0.005(5) -0.027(6) C18 0.047(6) 0.042(6) 0.045(6) 0.001(5) 0.011(5) -0.019(5) C19 0.035(5) 0.038(5) 0.038(5) 0.017(4) -0.009(4) -0.015(4) C20 0.047(6) 0.041(6) 0.053(6) 0.007(5) 0.008(5) -0.022(5) C21 0.066(8) 0.030(6) 0.082(9) -0.003(5) 0.012(6) -0.016(5) C22 0.087(10) 0.047(7) 0.097(10) 0.034(7) 0.010(8) -0.007(7) C23 0.080(9) 0.055(7) 0.063(8) 0.032(6) -0.003(6) -0.018(6) C24 0.056(7) 0.052(6) 0.043(6) 0.013(5) 0.001(5) -0.022(5) C25 0.024(5) 0.042(5) 0.027(5) 0.009(4) -0.004(4) -0.012(4) C26 0.030(5) 0.042(5) 0.035(5) 0.006(4) 0.000(4) -0.016(4) C27 0.039(6) 0.043(6) 0.043(6) 0.014(5) -0.008(5) -0.008(5) C28 0.040(6) 0.047(6) 0.069(8) 0.016(6) -0.010(5) -0.006(5) C29 0.029(5) 0.053(6) 0.071(7) 0.013(6) 0.008(5) -0.018(5) C30 0.044(6) 0.044(6) 0.046(6) 0.012(5) -0.002(5) -0.024(5) C31 0.042(6) 0.031(5) 0.027(5) 0.007(4) -0.001(4) -0.015(4) C32 0.049(6) 0.038(5) 0.038(6) 0.009(4) -0.002(5) -0.015(5) C33 0.059(7) 0.045(6) 0.044(6) 0.012(5) -0.006(5) -0.013(5) C34 0.068(8) 0.029(5) 0.051(7) 0.003(5) 0.003(6) -0.010(5) C35 0.049(6) 0.036(5) 0.047(6) 0.006(5) -0.005(5) -0.019(5) C36 0.046(6) 0.024(5) 0.030(5) 0.003(4) -0.002(4) -0.009(4) C37 0.028(5) 0.038(5) 0.048(6) 0.021(4) -0.003(4) -0.016(4) C38 0.051(6) 0.039(5) 0.049(6) 0.019(5) -0.006(5) -0.015(5) C39 0.060(8) 0.056(7) 0.077(8) 0.037(6) -0.004(6) -0.020(6) C40 0.048(7) 0.051(7) 0.089(9) 0.032(6) -0.017(6) -0.005(6) C41 0.024(5) 0.059(7) 0.078(8) 0.032(6) -0.010(5) -0.013(5) C42 0.039(6) 0.053(6) 0.054(6) 0.025(5) -0.012(5) -0.025(5) C43 0.029(5) 0.036(5) 0.036(5) 0.010(4) -0.008(4) -0.014(4) C44 0.034(6) 0.037(5) 0.060(7) 0.018(5) -0.010(5) -0.016(4) C45 0.052(7) 0.047(6) 0.066(7) 0.027(5) -0.016(5) -0.026(5) C46 0.077(9) 0.045(7) 0.090(10) 0.018(6) -0.010(7) -0.021(6) C47 0.076(9) 0.060(7) 0.048(7) -0.002(6) 0.003(6) -0.020(7) C48 0.050(6) 0.052(6) 0.042(6) 0.013(5) -0.001(5) -0.016(5) C49 0.031(5) 0.042(5) 0.025(5) 0.004(4) -0.002(4) -0.023(4) C50A 0.031(13) 0.041(11) 0.030(12) 0.001(9) 0.005(9) 0.001(9) C50B 0.052(15) 0.044(11) 0.028(11) 0.015(9) -0.016(10) -0.017(10) C51A 0.052(14) 0.041(12) 0.037(11) 0.010(9) 0.009(10) 0.014(10) C51B 0.070(18) 0.054(13) 0.065(13) 0.016(12) -0.009(14) -0.024(12) C52A 0.056(18) 0.024(11) 0.066(14) 0.012(10) 0.018(12) -0.019(11) C52B 0.054(18) 0.032(12) 0.101(17) 0.001(11) 0.013(14) -0.027(12) C53 0.051(7) 0.039(6) 0.046(6) -0.005(5) 0.001(5) -0.013(5) C54 0.074(8) 0.042(6) 0.050(7) -0.018(5) -0.011(6) -0.012(6) C55 0.048(6) 0.037(5) 0.028(5) 0.002(4) 0.005(4) -0.009(4) C56A 0.028(10) 0.050(12) 0.053(12) 0.008(9) -0.022(8) -0.019(9) C56B 0.060(14) 0.041(11) 0.057(14) 0.023(10) 0.003(11) 0.001(10) C57A 0.063(17) 0.026(12) 0.055(18) 0.010(13) -0.001(11) -0.008(10) C57B 0.091(17) 0.023(9) 0.065(15) 0.011(9) -0.019(12) -0.025(11) C58A 0.037(14) 0.076(18) 0.10(2) 0.013(15) 0.005(12) -0.021(12) C58B 0.053(15) 0.049(17) 0.08(2) -0.008(15) -0.036(16) 0.008(14) C59A 0.047(16) 0.066(16) 0.062(19) 0.005(14) 0.032(13) 0.012(12) C59B 0.018(12) 0.070(15) 0.08(2) -0.021(13) 0.000(13) -0.016(10) C60 0.034(6) 0.050(6) 0.120(10) -0.016(6) 0.023(6) -0.018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 O1 1.667(6) . y Os1 O5 1.882(6) . y Os1 O2 1.889(5) . y Os1 O4 1.897(6) . y Os1 O3 1.903(5) . y Os2 O6 1.672(6) . y Os2 O7 1.893(5) . y Os2 O9 1.898(6) . y Os2 O10 1.904(5) . y Os2 O8 1.909(5) . y Os3 O11 1.664(11) . y Os3 O13A 1.89(4) . y Os3 O12A 1.899(17) . y Os3 O12B 1.934(17) 2_567 y Os3 O13B 1.95(3) 2_567 y O2 C1 1.485(9) . y O3 C7 1.462(9) . y O4 C13 1.457(10) . y O5 C19 1.454(10) . y O7 C25 1.486(9) . y O8 C31 1.456(10) . y O9 C37 1.467(10) . y O10 C43 1.455(9) . y O12A C49 1.476(14) . y O12A Os3 2.237(17) 2_567 ? O12B C49 1.484(14) . y O12B Os3 1.934(17) 2_567 ? O13A C55 1.474(17) . y O13A Os3 2.27(3) 2_567 ? O13B C55 1.471(17) . y O13B Os3 1.95(3) 2_567 ? C1 C2 1.530(12) . ? C1 C6 1.542(11) . ? C1 C7 1.546(11) . y C2 C3 1.543(12) . ? C3 C4 1.530(15) . ? C4 C5 1.512(16) . ? C5 C6 1.532(13) . ? C7 C12 1.516(11) . ? C7 C8 1.531(11) . ? C8 C9 1.538(12) . ? C9 C10 1.508(13) . ? C10 C11 1.509(13) . ? C11 C12 1.550(13) . ? C13 C14 1.523(11) . ? C13 C18 1.538(12) . ? C13 C19 1.556(12) . y C14 C15 1.526(12) . ? C15 C16 1.519(13) . ? C16 C17 1.502(13) . ? C17 C18 1.510(12) . ? C19 C24 1.516(12) . ? C19 C20 1.538(12) . ? C20 C21 1.543(12) . ? C21 C22 1.524(15) . ? C22 C23 1.496(15) . ? C23 C24 1.511(13) . ? C25 C30 1.536(12) . ? C25 C31 1.537(11) . ? C25 C26 1.540(11) . ? C26 C27 1.540(11) . ? C27 C28 1.518(13) . ? C28 C29 1.521(13) . ? C29 C30 1.516(12) . ? C31 C36 1.526(11) . ? C31 C32 1.533(11) . ? C32 C33 1.526(12) . ? C33 C34 1.511(12) . ? C34 C35 1.523(12) . ? C35 C36 1.543(11) . ? C37 C42 1.519(11) . ? C37 C38 1.532(11) . ? C37 C43 1.548(12) . y C38 C39 1.524(12) . ? C39 C40 1.537(14) . ? C40 C41 1.524(13) . ? C41 C42 1.523(12) . ? C43 C44 1.526(11) . ? C43 C48 1.539(12) . ? C44 C45 1.546(12) . ? C45 C46 1.518(14) . ? C46 C47 1.515(14) . ? C47 C48 1.553(13) . ? C49 C54 1.517(12) . ? C49 C50A 1.535(15) . ? C49 C50B 1.558(15) . ? C49 C55 1.569(12) . y C50A C51A 1.556(16) . ? C50B C51B 1.534(17) . ? C51A C52A 1.541(17) . ? C51B C52B 1.512(18) . ? C52A C53 1.556(16) . ? C52B C53 1.509(17) . ? C53 C54 1.567(11) . ? C55 C60 1.503(13) . ? C55 C56B 1.567(15) . ? C55 C56A 1.572(14) . ? C56A C57A 1.554(17) . ? C56B C57B 1.526(16) . ? C57A C58A 1.554(18) . ? C57B C58B 1.526(19) . ? C58A C59A 1.538(18) . ? C58B C59B 1.557(19) . ? C59A C60 1.556(17) . ? C59B C60 1.575(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Os1 O5 106.4(3) . . y O1 Os1 O2 111.5(3) . . y O5 Os1 O2 85.6(2) . . y O1 Os1 O4 114.8(3) . . y O5 Os1 O4 81.6(2) . . y O2 Os1 O4 133.7(2) . . y O1 Os1 O3 108.0(3) . . y O5 Os1 O3 145.6(3) . . y O2 Os1 O3 82.8(2) . . y O4 Os1 O3 83.3(2) . . y O6 Os2 O7 109.2(3) . . y O6 Os2 O9 111.5(3) . . y O7 Os2 O9 139.3(2) . . y O6 Os2 O10 108.4(3) . . y O7 Os2 O10 85.0(2) . . y O9 Os2 O10 82.2(2) . . y O6 Os2 O8 111.4(3) . . y O7 Os2 O8 82.2(2) . . y O9 Os2 O8 83.5(2) . . y O10 Os2 O8 140.2(2) . . y O11 Os3 O13A 111.4(9) . . y O11 Os3 O12A 110.3(6) . . y O13A Os3 O12A 83.9(8) . . y O11 Os3 O12B 108.0(6) . 2_567 y O13A Os3 O12B 81.3(7) . 2_567 y O12A Os3 O12B 141.7(5) . 2_567 y O11 Os3 O13B 113.6(9) . 2_567 y O13A Os3 O13B 134.6(14) . 2_567 y O12A Os3 O13B 85.9(7) . 2_567 y O12B Os3 O13B 80.0(7) 2_567 2_567 y C1 O2 Os1 113.7(4) . . y C7 O3 Os1 116.7(5) . . y C13 O4 Os1 117.4(5) . . y C19 O5 Os1 115.0(5) . . y C25 O7 Os2 113.4(4) . . y C31 O8 Os2 117.1(5) . . y C37 O9 Os2 117.1(5) . . y C43 O10 Os2 113.3(5) . . y C49 O12A Os3 121.1(11) . . y C49 O12A Os3 96.8(9) . 2_567 ? Os3 O12A Os3 55.6(5) . 2_567 ? C49 O12B Os3 110.6(10) . 2_567 ? C55 O13A Os3 106(2) . . y C55 O13A Os3 106.0(15) . 2_567 ? Os3 O13A Os3 55.0(9) . 2_567 ? C55 O13B Os3 123.9(16) . 2_567 ? O2 C1 C2 107.4(7) . . ? O2 C1 C6 104.4(6) . . ? C2 C1 C6 110.0(7) . . ? O2 C1 C7 104.1(6) . . ? C2 C1 C7 113.9(7) . . ? C6 C1 C7 116.0(7) . . ? C1 C2 C3 111.5(8) . . ? C4 C3 C2 110.3(9) . . ? C5 C4 C3 112.6(9) . . ? C4 C5 C6 109.5(9) . . ? C5 C6 C1 113.1(8) . . ? O3 C7 C12 107.9(7) . . ? O3 C7 C8 105.9(7) . . ? C12 C7 C8 109.8(7) . . ? O3 C7 C1 105.9(6) . . ? C12 C7 C1 113.4(7) . . ? C8 C7 C1 113.5(7) . . ? C7 C8 C9 112.0(7) . . ? C10 C9 C8 111.6(9) . . ? C9 C10 C11 109.9(8) . . ? C10 C11 C12 112.9(8) . . ? C7 C12 C11 112.9(8) . . ? O4 C13 C14 106.9(7) . . ? O4 C13 C18 106.8(7) . . ? C14 C13 C18 109.6(7) . . ? O4 C13 C19 105.5(7) . . ? C14 C13 C19 112.5(7) . . ? C18 C13 C19 115.0(7) . . ? C13 C14 C15 113.1(8) . . ? C16 C15 C14 110.4(8) . . ? C17 C16 C15 109.5(8) . . ? C16 C17 C18 113.6(9) . . ? C17 C18 C13 112.6(8) . . ? O5 C19 C24 105.9(7) . . ? O5 C19 C20 108.2(7) . . ? C24 C19 C20 109.2(7) . . ? O5 C19 C13 103.4(7) . . ? C24 C19 C13 117.2(8) . . ? C20 C19 C13 112.3(7) . . ? C19 C20 C21 111.7(8) . . ? C22 C21 C20 110.4(9) . . ? C23 C22 C21 111.0(9) . . ? C22 C23 C24 112.5(9) . . ? C23 C24 C19 112.8(8) . . ? O7 C25 C30 104.3(6) . . ? O7 C25 C31 104.2(6) . . ? C30 C25 C31 116.8(7) . . ? O7 C25 C26 107.3(6) . . ? C30 C25 C26 110.0(7) . . ? C31 C25 C26 113.2(7) . . ? C25 C26 C27 111.6(7) . . ? C28 C27 C26 111.0(8) . . ? C27 C28 C29 109.8(8) . . ? C30 C29 C28 115.2(9) . . ? C29 C30 C25 111.8(7) . . ? O8 C31 C36 107.7(7) . . ? O8 C31 C32 106.3(7) . . ? C36 C31 C32 110.0(7) . . ? O8 C31 C25 105.8(6) . . ? C36 C31 C25 113.4(7) . . ? C32 C31 C25 113.1(7) . . ? C33 C32 C31 113.0(8) . . ? C34 C33 C32 111.0(8) . . ? C33 C34 C35 110.8(8) . . ? C34 C35 C36 112.3(8) . . ? C31 C36 C35 112.5(7) . . ? O9 C37 C42 107.0(7) . . ? O9 C37 C38 105.9(7) . . ? C42 C37 C38 110.7(7) . . ? O9 C37 C43 105.5(6) . . ? C42 C37 C43 114.5(7) . . ? C38 C37 C43 112.5(7) . . ? C39 C38 C37 113.5(8) . . ? C38 C39 C40 110.4(9) . . ? C41 C40 C39 110.3(8) . . ? C42 C41 C40 111.5(9) . . ? C37 C42 C41 113.4(7) . . ? O10 C43 C44 108.6(7) . . ? O10 C43 C48 106.4(7) . . ? C44 C43 C48 110.4(7) . . ? O10 C43 C37 104.9(6) . . ? C44 C43 C37 112.4(7) . . ? C48 C43 C37 113.8(7) . . ? C43 C44 C45 111.9(8) . . ? C46 C45 C44 110.2(8) . . ? C47 C46 C45 111.7(9) . . ? C46 C47 C48 112.7(9) . . ? C43 C48 C47 112.3(8) . . ? O12A C49 O12B 27.9(6) . . ? O12A C49 C54 99.9(10) . . ? O12B C49 C54 110.6(10) . . ? O12A C49 C50A 108.7(11) . . ? O12B C49 C50A 81.3(11) . . ? C54 C49 C50A 120.4(10) . . ? O12A C49 C50B 135.6(11) . . ? O12B C49 C50B 107.7(11) . . ? C54 C49 C50B 99.5(10) . . ? C50A C49 C50B 28.8(9) . . ? O12A C49 C55 96.6(9) . . ? O12B C49 C55 112.5(9) . . ? C54 C49 C55 115.2(7) . . ? C50A C49 C55 112.0(9) . . ? C50B C49 C55 110.4(10) . . ? C49 C50A C51A 109.0(14) . . ? C51B C50B C49 114.2(16) . . ? C52A C51A C50A 109.5(17) . . ? C52B C51B C50B 110.7(19) . . ? C51A C52A C53 114.5(14) . . ? C53 C52B C51B 106.2(16) . . ? C52B C53 C52A 27.6(10) . . ? C52B C53 C54 108.9(13) . . ? C52A C53 C54 112.3(11) . . ? C49 C54 C53 112.3(8) . . ? O13B C55 O13A 19.8(18) . . ? O13B C55 C60 102.1(14) . . ? O13A C55 C60 106.5(17) . . ? O13B C55 C56B 100.4(15) . . ? O13A C55 C56B 82.6(16) . . ? C60 C55 C56B 127.2(11) . . ? O13B C55 C49 98.8(12) . . ? O13A C55 C49 112.9(14) . . ? C60 C55 C49 114.9(7) . . ? C56B C55 C49 107.9(9) . . ? O13B C55 C56A 131.5(14) . . ? O13A C55 C56A 111.7(14) . . ? C60 C55 C56A 95.4(11) . . ? C56B C55 C56A 37.3(10) . . ? C49 C55 C56A 114.0(9) . . ? C57A C56A C55 114.3(16) . . ? C57B C56B C55 111.6(14) . . ? C58A C57A C56A 111.6(18) . . ? C58B C57B C56B 108.3(18) . . ? C59A C58A C57A 111(2) . . ? C57B C58B C59B 112(2) . . ? C58A C59A C60 100.4(17) . . ? C58B C59B C60 122(2) . . ? C55 C60 C59A 120.5(15) . . ? C55 C60 C59B 103.6(12) . . ? C59A C60 C59B 24.5(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Os1 O2 C1 82.8(5) . . . . ? O5 Os1 O2 C1 -171.3(5) . . . . ? O4 Os1 O2 C1 -97.3(5) . . . . ? O3 Os1 O2 C1 -23.8(5) . . . . ? O1 Os1 O3 C7 -112.4(5) . . . . ? O5 Os1 O3 C7 69.2(7) . . . . ? O2 Os1 O3 C7 -2.1(5) . . . . ? O4 Os1 O3 C7 133.6(5) . . . . ? O1 Os1 O4 C13 104.3(6) . . . . ? O5 Os1 O4 C13 0.1(5) . . . . ? O2 Os1 O4 C13 -75.6(6) . . . . ? O3 Os1 O4 C13 -148.9(6) . . . . ? O1 Os1 O5 C19 -87.3(6) . . . . ? O2 Os1 O5 C19 161.5(6) . . . . ? O4 Os1 O5 C19 26.2(5) . . . . ? O3 Os1 O5 C19 91.1(6) . . . . ? O6 Os2 O7 C25 85.1(5) . . . . ? O9 Os2 O7 C25 -95.3(5) . . . . ? O10 Os2 O7 C25 -167.2(5) . . . . ? O8 Os2 O7 C25 -24.9(5) . . . . ? O6 Os2 O8 C31 -108.5(5) . . . . ? O7 Os2 O8 C31 -0.9(5) . . . . ? O9 Os2 O8 C31 141.0(5) . . . . ? O10 Os2 O8 C31 71.4(6) . . . . ? O6 Os2 O9 C37 105.6(5) . . . . ? O7 Os2 O9 C37 -74.1(6) . . . . ? O10 Os2 O9 C37 -1.2(5) . . . . ? O8 Os2 O9 C37 -143.9(5) . . . . ? O6 Os2 O10 C43 -83.6(5) . . . . ? O7 Os2 O10 C43 167.8(5) . . . . ? O9 Os2 O10 C43 26.5(5) . . . . ? O8 Os2 O10 C43 96.5(6) . . . . ? O11 Os3 O12A C49 108.3(11) . . . . ? O13A Os3 O12A C49 -2.2(12) . . . . ? O12B Os3 O12A C49 -69.8(15) 2_567 . . . ? O13B Os3 O12A C49 -138.0(13) 2_567 . . . ? O11 Os3 O12A Os3 -175.8(5) . . . 2_567 ? O13A Os3 O12A Os3 73.6(8) . . . 2_567 ? O12B Os3 O12A Os3 6.0(12) 2_567 . . 2_567 ? O13B Os3 O12A Os3 -62.2(9) 2_567 . . 2_567 ? O11 Os3 O13A C55 -82.8(15) . . . . ? O12A Os3 O13A C55 26.6(14) . . . . ? O12B Os3 O13A C55 171.2(15) 2_567 . . . ? O13B Os3 O13A C55 104.6(16) 2_567 . . . ? O11 Os3 O13A Os3 178.6(5) . . . 2_567 ? O12A Os3 O13A Os3 -72.0(5) . . . 2_567 ? O12B Os3 O13A Os3 72.6(4) 2_567 . . 2_567 ? O13B Os3 O13A Os3 6.1(14) 2_567 . . 2_567 ? Os1 O2 C1 C2 -79.3(7) . . . . ? Os1 O2 C1 C6 164.0(5) . . . . ? Os1 O2 C1 C7 41.9(7) . . . . ? O2 C1 C2 C3 -58.4(9) . . . . ? C6 C1 C2 C3 54.6(10) . . . . ? C7 C1 C2 C3 -173.2(8) . . . . ? C1 C2 C3 C4 -55.7(12) . . . . ? C2 C3 C4 C5 56.9(13) . . . . ? C3 C4 C5 C6 -56.1(13) . . . . ? C4 C5 C6 C1 55.5(12) . . . . ? O2 C1 C6 C5 59.7(10) . . . . ? C2 C1 C6 C5 -55.2(10) . . . . ? C7 C1 C6 C5 173.7(8) . . . . ? Os1 O3 C7 C12 146.8(6) . . . . ? Os1 O3 C7 C8 -95.7(6) . . . . ? Os1 O3 C7 C1 25.1(8) . . . . ? O2 C1 C7 O3 -40.1(8) . . . . y C2 C1 C7 O3 76.6(8) . . . . ? C6 C1 C7 O3 -154.2(7) . . . . ? O2 C1 C7 C12 -158.2(7) . . . . ? C2 C1 C7 C12 -41.5(10) . . . . ? C6 C1 C7 C12 87.7(9) . . . . ? O2 C1 C7 C8 75.6(8) . . . . ? C2 C1 C7 C8 -167.7(7) . . . . ? C6 C1 C7 C8 -38.5(10) . . . . ? O3 C7 C8 C9 -61.7(9) . . . . ? C12 C7 C8 C9 54.4(10) . . . . ? C1 C7 C8 C9 -177.5(7) . . . . ? C7 C8 C9 C10 -58.1(11) . . . . ? C8 C9 C10 C11 56.5(12) . . . . ? C9 C10 C11 C12 -53.8(12) . . . . ? O3 C7 C12 C11 63.3(10) . . . . ? C8 C7 C12 C11 -51.6(10) . . . . ? C1 C7 C12 C11 -179.8(8) . . . . ? C10 C11 C12 C7 52.8(11) . . . . ? Os1 O4 C13 C14 97.0(7) . . . . ? Os1 O4 C13 C18 -145.8(5) . . . . ? Os1 O4 C13 C19 -23.0(8) . . . . ? O4 C13 C14 C15 62.2(9) . . . . ? C18 C13 C14 C15 -53.1(10) . . . . ? C19 C13 C14 C15 177.5(8) . . . . ? C13 C14 C15 C16 57.7(11) . . . . ? C14 C15 C16 C17 -57.0(12) . . . . ? C15 C16 C17 C18 56.2(12) . . . . ? C16 C17 C18 C13 -53.7(11) . . . . ? O4 C13 C18 C17 -65.2(10) . . . . ? C14 C13 C18 C17 50.2(10) . . . . ? C19 C13 C18 C17 178.2(8) . . . . ? Os1 O5 C19 C24 -167.3(5) . . . . ? Os1 O5 C19 C20 75.8(7) . . . . ? Os1 O5 C19 C13 -43.4(7) . . . . ? O4 C13 C19 O5 39.2(8) . . . . y C14 C13 C19 O5 -77.0(8) . . . . ? C18 C13 C19 O5 156.6(7) . . . . ? O4 C13 C19 C24 155.3(7) . . . . ? C14 C13 C19 C24 39.1(11) . . . . ? C18 C13 C19 C24 -87.3(10) . . . . ? O4 C13 C19 C20 -77.2(9) . . . . ? C14 C13 C19 C20 166.7(7) . . . . ? C18 C13 C19 C20 40.2(10) . . . . ? O5 C19 C20 C21 59.5(10) . . . . ? C24 C19 C20 C21 -55.3(10) . . . . ? C13 C19 C20 C21 173.0(8) . . . . ? C19 C20 C21 C22 56.5(11) . . . . ? C20 C21 C22 C23 -55.3(13) . . . . ? C21 C22 C23 C24 54.9(14) . . . . ? C22 C23 C24 C19 -55.4(12) . . . . ? O5 C19 C24 C23 -61.9(10) . . . . ? C20 C19 C24 C23 54.4(11) . . . . ? C13 C19 C24 C23 -176.6(8) . . . . ? Os2 O7 C25 C30 166.1(5) . . . . ? Os2 O7 C25 C31 43.1(7) . . . . ? Os2 O7 C25 C26 -77.3(7) . . . . ? O7 C25 C26 C27 -57.0(9) . . . . ? C30 C25 C26 C27 56.0(9) . . . . ? C31 C25 C26 C27 -171.4(7) . . . . ? C25 C26 C27 C28 -58.6(10) . . . . ? C26 C27 C28 C29 55.0(11) . . . . ? C27 C28 C29 C30 -52.9(11) . . . . ? C28 C29 C30 C25 51.9(11) . . . . ? O7 C25 C30 C29 63.1(9) . . . . ? C31 C25 C30 C29 177.5(7) . . . . ? C26 C25 C30 C29 -51.7(10) . . . . ? Os2 O8 C31 C36 145.9(5) . . . . ? Os2 O8 C31 C32 -96.2(7) . . . . ? Os2 O8 C31 C25 24.4(7) . . . . ? O7 C25 C31 O8 -40.3(8) . . . . y C30 C25 C31 O8 -154.8(7) . . . . ? C26 C25 C31 O8 76.0(8) . . . . ? O7 C25 C31 C36 -158.1(7) . . . . ? C30 C25 C31 C36 87.4(9) . . . . ? C26 C25 C31 C36 -41.8(10) . . . . ? O7 C25 C31 C32 75.7(8) . . . . ? C30 C25 C31 C32 -38.8(10) . . . . ? C26 C25 C31 C32 -168.0(7) . . . . ? O8 C31 C32 C33 -62.3(9) . . . . ? C36 C31 C32 C33 54.0(10) . . . . ? C25 C31 C32 C33 -178.0(8) . . . . ? C31 C32 C33 C34 -56.9(11) . . . . ? C32 C33 C34 C35 56.1(12) . . . . ? C33 C34 C35 C36 -54.6(11) . . . . ? O8 C31 C36 C35 63.9(9) . . . . ? C32 C31 C36 C35 -51.5(10) . . . . ? C25 C31 C36 C35 -179.4(7) . . . . ? C34 C35 C36 C31 53.1(10) . . . . ? Os2 O9 C37 C42 -144.0(5) . . . . ? Os2 O9 C37 C38 97.8(7) . . . . ? Os2 O9 C37 C43 -21.6(8) . . . . ? O9 C37 C38 C39 64.2(10) . . . . ? C42 C37 C38 C39 -51.5(11) . . . . ? C43 C37 C38 C39 178.9(8) . . . . ? C37 C38 C39 C40 55.0(11) . . . . ? C38 C39 C40 C41 -56.7(12) . . . . ? C39 C40 C41 C42 56.6(12) . . . . ? O9 C37 C42 C41 -64.2(9) . . . . ? C38 C37 C42 C41 50.7(11) . . . . ? C43 C37 C42 C41 179.2(8) . . . . ? C40 C41 C42 C37 -54.5(11) . . . . ? Os2 O10 C43 C44 76.7(7) . . . . ? Os2 O10 C43 C48 -164.5(5) . . . . ? Os2 O10 C43 C37 -43.7(7) . . . . ? O9 C37 C43 O10 39.3(8) . . . . y C42 C37 C43 O10 156.8(7) . . . . ? C38 C37 C43 O10 -75.6(8) . . . . ? O9 C37 C43 C44 -78.4(8) . . . . ? C42 C37 C43 C44 39.0(10) . . . . ? C38 C37 C43 C44 166.6(7) . . . . ? O9 C37 C43 C48 155.2(7) . . . . ? C42 C37 C43 C48 -87.4(9) . . . . ? C38 C37 C43 C48 40.2(10) . . . . ? O10 C43 C44 C45 60.4(9) . . . . ? C48 C43 C44 C45 -55.9(10) . . . . ? C37 C43 C44 C45 175.9(7) . . . . ? C43 C44 C45 C46 58.3(10) . . . . ? C44 C45 C46 C47 -56.2(12) . . . . ? C45 C46 C47 C48 53.3(13) . . . . ? O10 C43 C48 C47 -65.8(10) . . . . ? C44 C43 C48 C47 51.8(11) . . . . ? C37 C43 C48 C47 179.2(8) . . . . ? C46 C47 C48 C43 -51.1(12) . . . . ? Os3 O12A C49 O12B 107(3) . . . . ? Os3 O12A C49 O12B 53(2) 2_567 . . . ? Os3 O12A C49 C54 -137.7(9) . . . . ? Os3 O12A C49 C54 168.6(6) 2_567 . . . ? Os3 O12A C49 C50A 95.2(12) . . . . ? Os3 O12A C49 C50A 41.6(11) 2_567 . . . ? Os3 O12A C49 C50B 107.6(16) . . . . ? Os3 O12A C49 C50B 53.9(17) 2_567 . . . ? Os3 O12A C49 C55 -20.7(11) . . . . ? Os3 O12A C49 C55 -74.3(7) 2_567 . . . ? Os3 O12B C49 O12A -102(3) 2_567 . . . ? Os3 O12B C49 C54 -173.3(7) 2_567 . . . ? Os3 O12B C49 C50A 67.3(10) 2_567 . . . ? Os3 O12B C49 C50B 78.9(12) 2_567 . . . ? Os3 O12B C49 C55 -42.9(11) 2_567 . . . ? O12A C49 C50A C51A 64.6(18) . . . . ? O12B C49 C50A C51A 59.3(16) . . . . ? C54 C49 C50A C51A -49.6(19) . . . . ? C50B C49 C50A C51A -97(3) . . . . ? C55 C49 C50A C51A 170.1(13) . . . . ? O12A C49 C50B C51B 54(2) . . . . ? O12B C49 C50B C51B 54.7(18) . . . . ? C54 C49 C50B C51B -60.7(16) . . . . ? C50A C49 C50B C51B 79(3) . . . . ? C55 C49 C50B C51B 177.8(13) . . . . ? C49 C50A C51A C52A 55(2) . . . . ? C49 C50B C51B C52B 62(2) . . . . ? C50A C51A C52A C53 -59(2) . . . . ? C50B C51B C52B C53 -58(2) . . . . ? C51B C52B C53 C52A -42(3) . . . . ? C51B C52B C53 C54 59.9(19) . . . . ? C51A C52A C53 C52B 139(4) . . . . ? C51A C52A C53 C54 51(2) . . . . ? O12A C49 C54 C53 -76.9(11) . . . . ? O12B C49 C54 C53 -50.1(12) . . . . ? C50A C49 C54 C53 41.8(15) . . . . ? C50B C49 C54 C53 63.0(12) . . . . ? C55 C49 C54 C53 -179.1(8) . . . . ? C52B C53 C54 C49 -68.8(14) . . . . ? C52A C53 C54 C49 -39.5(14) . . . . ? Os3 O13B C55 O13A 124(9) 2_567 . . . ? Os3 O13B C55 C60 -130.8(17) 2_567 . . . ? Os3 O13B C55 C56B 97.3(19) 2_567 . . . ? Os3 O13B C55 C49 -13(2) 2_567 . . . ? Os3 O13B C55 C56A 120.6(18) 2_567 . . . ? Os3 O13A C55 O13B -95(8) . . . . ? Os3 O13A C55 O13B -38(6) 2_567 . . . ? Os3 O13A C55 C60 -175.3(10) . . . . ? Os3 O13A C55 C60 -117.9(15) 2_567 . . . ? Os3 O13A C55 C56B 58.1(14) . . . . ? Os3 O13A C55 C56B 115.5(17) 2_567 . . . ? Os3 O13A C55 C49 -48.3(17) . . . . ? Os3 O13A C55 C49 9(2) 2_567 . . . ? Os3 O13A C55 C56A 81.8(16) . . . . ? Os3 O13A C55 C56A 139.2(13) 2_567 . . . ? O12A C49 C55 O13B 57.4(14) . . . . ? O12B C49 C55 O13B 33.6(15) . . . . y C54 C49 C55 O13B 161.6(14) . . . . ? C50A C49 C55 O13B -55.9(16) . . . . ? C50B C49 C55 O13B -86.8(15) . . . . ? O12A C49 C55 O13A 42.8(18) . . . . y O12B C49 C55 O13A 19.1(19) . . . . ? C54 C49 C55 O13A 147.1(17) . . . . ? C50A C49 C55 O13A -70.4(19) . . . . ? C50B C49 C55 O13A -101.3(18) . . . . ? O12A C49 C55 C60 165.2(10) . . . . ? O12B C49 C55 C60 141.4(10) . . . . ? C54 C49 C55 C60 -90.6(10) . . . . ? C50A C49 C55 C60 52.0(13) . . . . ? C50B C49 C55 C60 21.1(12) . . . . ? O12A C49 C55 C56B -46.6(13) . . . . ? O12B C49 C55 C56B -70.3(14) . . . . ? C54 C49 C55 C56B 57.7(13) . . . . ? C50A C49 C55 C56B -159.8(14) . . . . ? C50B C49 C55 C56B 169.3(13) . . . . ? O12A C49 C55 C56A -86.1(12) . . . . ? O12B C49 C55 C56A -109.9(12) . . . . ? C54 C49 C55 C56A 18.1(13) . . . . ? C50A C49 C55 C56A 160.7(13) . . . . ? C50B C49 C55 C56A 129.8(13) . . . . ? O13B C55 C56A C57A 54(3) . . . . ? O13A C55 C56A C57A 52(2) . . . . ? C60 C55 C56A C57A -57.7(17) . . . . ? C56B C55 C56A C57A 94(2) . . . . ? C49 C55 C56A C57A -178.1(14) . . . . ? O13B C55 C56B C57B 70(2) . . . . ? O13A C55 C56B C57B 61(2) . . . . ? C60 C55 C56B C57B -44(2) . . . . ? C49 C55 C56B C57B 172.7(15) . . . . ? C56A C55 C56B C57B -81(2) . . . . ? C55 C56A C57A C58A 57(3) . . . . ? C55 C56B C57B C58B 51(2) . . . . ? C56A C57A C58A C59A -54(3) . . . . ? C56B C57B C58B C59B -56(3) . . . . ? C57A C58A C59A C60 54(3) . . . . ? C57B C58B C59B C60 51(3) . . . . ? O13B C55 C60 C59A -62.7(19) . . . . ? O13A C55 C60 C59A -43(2) . . . . ? C56B C55 C60 C59A 51(2) . . . . ? C49 C55 C60 C59A -168.4(15) . . . . ? C56A C55 C60 C59A 71.9(17) . . . . ? O13B C55 C60 C59B -81.9(17) . . . . ? O13A C55 C60 C59B -62.0(18) . . . . ? C56B C55 C60 C59B 31.3(19) . . . . ? C49 C55 C60 C59B 172.3(13) . . . . ? C56A C55 C60 C59B 52.6(15) . . . . ? C58A C59A C60 C55 -73(3) . . . . ? C58A C59A C60 C59B -23(4) . . . . ? C58B C59B C60 C55 -34(3) . . . . ? C58B C59B C60 C59A -170(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.679 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.152 #===END