# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1982 data_os _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_formula_sum 'C22 H8 O9 Os3' _chemical_formula_weight 986.88 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 monoclinic _symmetry_space_group_name_H-M ' P 2(1) / n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3325(13) _cell_length_b 13.960(2) _cell_length_c 17.864(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.771(13) _cell_angle_gamma 90.00 _cell_volume 2260.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 12.5 _exptl_crystal_description needle _exptl_crystal_colour deep_orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 16.872 _exptl_absorpt_correction_type '\y_scan; SHELXTL/PC(Sheldrick,1991)' _exptl_absorpt_correction_T_min 0.08 _exptl_absorpt_correction_T_max 0.28 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Siemens_R3_diffractometer _diffrn_measurement_method \q/2\q _diffrn_standards_number 2 _diffrn_standards_interval_count 98 _diffrn_standards_decay_% <1 _diffrn_reflns_number 4237 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3975 _reflns_number_gt 2892 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3/P4-PC version V4.27 (1991)' _computing_cell_refinement 'Siemens P3/P4-PC version V4.27 (1991)' _computing_data_reduction 'XDISK in SHELXTL/PC(Sheldrick,1991)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL/PC(Sheldrick,1991)' _computing_publication_material ; PARST (Nardelli,1983)' ; _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^)+(0.035P)^2^] 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_number_reflns 3975 _refine_ls_number_parameters 312 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 1.802 _refine_ls_shift/su_mean 0.006 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 0.64687(7) 0.80258(4) 0.05241(3) 0.03419(16) Uani 1 d D . . Os2 Os 0.69731(6) 0.62515(4) 0.14761(3) 0.02981(15) Uani 1 d D . . H H 0.628(9) 0.6719(15) 0.0505(15) 0.022(2) Uiso 1 d D . . Os3 Os 0.91348(6) 0.77008(4) 0.16136(3) 0.03143(15) Uani 1 d . . . C1 C 0.490(2) 0.8404(12) 0.1037(9) 0.055(5) Uani 1 d . . . C2 C 0.6808(18) 0.9341(12) 0.0393(8) 0.051(4) Uani 1 d . . . C3 C 0.5174(17) 0.7917(10) -0.0467(8) 0.044(4) Uani 1 d . . . C4 C 0.5298(19) 0.6576(12) 0.1902(10) 0.053(4) Uani 1 d . . . C5 C 0.7889(17) 0.5709(12) 0.2447(10) 0.050(4) Uani 1 d . . . C6 C 0.6160(16) 0.5086(10) 0.1036(8) 0.036(3) Uani 1 d . . . C7 C 1.005(3) 0.8914(13) 0.1554(10) 0.077(6) Uani 1 d . . . C8 C 1.0761(18) 0.7180(10) 0.2351(9) 0.043(4) Uani 1 d . . . C9 C 0.8102(18) 0.8139(11) 0.2327(9) 0.047(4) Uani 1 d . . . C10 C 0.8444(15) 0.7665(10) 0.0227(8) 0.034(3) Uani 1 d . . . C11 C 0.918(2) 0.8210(12) -0.0266(8) 0.054(4) Uani 1 d . . . H11 H 0.8774 0.8794 -0.0461 0.065 Uiso 1 calc R . . C12 C 1.039(2) 0.7908(11) -0.0447(9) 0.059(5) Uani 1 d . . . H12 H 1.0763 0.8281 -0.0789 0.070 Uiso 1 calc R . . C13 C 1.1171(19) 0.7081(11) -0.0169(9) 0.049(4) Uani 1 d . . . H13 H 1.2016 0.6904 -0.0324 0.059 Uiso 1 calc R . . C14 C 1.0641(14) 0.6541(10) 0.0342(7) 0.032(3) Uani 1 d . . . C22 C 0.9272(13) 0.6833(9) 0.0527(7) 0.025(3) Uani 1 d . . . C15 C 1.1109(15) 0.5669(9) 0.0780(8) 0.035(3) Uani 1 d . . . C16 C 1.2278(17) 0.5049(11) 0.0782(9) 0.045(4) Uani 1 d . . . H16 H 1.2915 0.5175 0.0466 0.054 Uiso 1 calc R . . C17 C 1.2501(16) 0.4251(11) 0.1250(9) 0.045(4) Uani 1 d . . . H17 H 1.3306 0.3851 0.1268 0.054 Uiso 1 calc R . . C18 C 1.1503(17) 0.4055(11) 0.1690(10) 0.054(4) Uani 1 d . . . H18 H 1.1638 0.3512 0.2000 0.064 Uiso 1 calc R . . C19 C 1.0294(17) 0.4653(10) 0.1683(8) 0.044(4) Uani 1 d . . . H19 H 0.9636 0.4504 0.1984 0.053 Uiso 1 calc R . . C20 C 1.0087(15) 0.5455(9) 0.1233(8) 0.032(3) Uani 1 d . . . C21 C 0.8905(14) 0.6179(8) 0.1109(7) 0.028(3) Uani 1 d . . . O1 O 0.4043(18) 0.8641(11) 0.1331(8) 0.097(5) Uani 1 d . . . O2 O 0.7039(15) 1.0136(8) 0.0302(8) 0.081(4) Uani 1 d . . . O3 O 0.4421(15) 0.7833(8) -0.1061(6) 0.071(4) Uani 1 d . . . O4 O 0.4358(17) 0.6753(11) 0.2167(10) 0.106(6) Uani 1 d . . . O5 O 0.8383(15) 0.5395(8) 0.3045(6) 0.066(4) Uani 1 d . . . O6 O 0.5766(12) 0.4364(7) 0.0750(6) 0.048(3) Uani 1 d . . . O7 O 1.0633(18) 0.9624(9) 0.1491(9) 0.108(6) Uani 1 d . . . O8 O 1.1673(12) 0.6854(9) 0.2821(7) 0.063(3) Uani 1 d . . . O9 O 0.7455(12) 0.8417(8) 0.2751(6) 0.060(3) Uani 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 0.0419(3) 0.0272(3) 0.0301(3) 0.0003(2) 0.0017(3) 0.0055(3) Os2 0.0345(3) 0.0258(3) 0.0306(3) -0.0005(2) 0.0105(2) -0.0006(2) Os3 0.0391(3) 0.0244(3) 0.0281(3) -0.0023(2) 0.0026(2) -0.0027(2) C1 0.071(12) 0.044(10) 0.039(10) 0.001(8) -0.006(9) 0.009(9) C2 0.056(11) 0.054(11) 0.029(8) -0.004(8) -0.019(8) 0.016(9) C3 0.060(10) 0.026(8) 0.037(9) 0.003(7) -0.005(8) 0.018(7) C4 0.050(10) 0.050(10) 0.067(12) 0.002(9) 0.028(9) 0.005(8) C5 0.042(10) 0.057(11) 0.051(10) -0.010(9) 0.013(8) -0.027(8) C6 0.043(9) 0.034(8) 0.042(9) -0.001(7) 0.031(7) -0.001(7) C7 0.117(18) 0.040(11) 0.054(12) -0.010(9) -0.019(11) -0.002(11) C8 0.049(10) 0.033(9) 0.042(9) -0.003(7) 0.000(8) -0.008(7) C9 0.061(11) 0.042(9) 0.037(9) 0.008(8) 0.009(8) 0.017(8) C10 0.043(9) 0.032(7) 0.029(7) 0.006(6) 0.014(7) 0.008(7) C11 0.076(13) 0.053(11) 0.036(9) 0.009(8) 0.020(9) -0.002(9) C12 0.096(15) 0.043(10) 0.045(10) 0.007(8) 0.034(10) -0.023(10) C13 0.067(11) 0.040(9) 0.046(9) 0.000(8) 0.026(9) -0.001(8) C14 0.028(7) 0.040(8) 0.028(7) -0.014(6) 0.007(6) -0.006(6) C22 0.026(7) 0.027(7) 0.024(7) -0.011(6) 0.014(6) -0.003(6) C15 0.044(9) 0.028(8) 0.035(8) -0.007(6) 0.011(7) 0.007(7) C16 0.048(10) 0.047(9) 0.048(9) 0.002(8) 0.026(8) -0.003(8) C17 0.034(9) 0.042(9) 0.059(10) -0.009(8) 0.011(8) 0.006(7) C18 0.042(10) 0.040(9) 0.072(12) -0.001(9) 0.000(9) 0.002(8) C19 0.046(9) 0.044(9) 0.046(9) 0.005(7) 0.018(8) 0.013(8) C20 0.038(8) 0.024(7) 0.033(8) -0.013(6) 0.005(6) -0.004(6) C21 0.035(8) 0.015(6) 0.034(7) -0.001(5) 0.005(6) -0.001(6) O1 0.122(13) 0.102(12) 0.081(10) -0.003(8) 0.054(10) 0.053(10) O2 0.103(11) 0.020(6) 0.109(11) 0.011(6) 0.005(9) 0.007(7) O3 0.101(10) 0.068(8) 0.031(6) 0.004(6) -0.013(7) -0.011(8) O4 0.105(12) 0.087(11) 0.155(15) -0.014(10) 0.085(12) 0.012(9) O5 0.114(11) 0.043(7) 0.032(6) 0.008(5) -0.002(7) -0.011(7) O6 0.059(7) 0.036(6) 0.048(6) 0.001(5) 0.012(6) -0.011(5) O7 0.129(14) 0.050(8) 0.125(13) 0.012(8) -0.007(10) -0.056(9) O8 0.050(7) 0.076(9) 0.056(7) -0.004(7) -0.004(6) 0.013(7) O9 0.059(7) 0.080(8) 0.038(6) -0.016(6) 0.007(6) 0.032(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 Os1 C2 1.888(18) . N Os1 C3 1.898(15) . N Os1 C1 1.98(2) . N Os1 C10 2.098(13) . N Os1 Os3 2.8070(9) . N Os1 Os2 2.9780(8) . N Os2 C6 1.886(15) . N Os2 C5 1.899(18) . N Os2 C4 1.948(17) . N Os2 C21 2.062(13) . N Os2 Os3 2.8264(8) . N Os3 C9 1.874(16) . N Os3 C8 1.901(16) . N Os3 C7 1.91(2) . N Os3 C21 2.298(12) . N Os3 C22 2.318(11) . N Os3 C10 2.407(13) . N C1 O1 1.11(2) . N C2 O2 1.149(18) . N C3 O3 1.130(16) . N C4 O4 1.118(18) . N C5 O5 1.146(18) . N C6 O6 1.149(15) . N C7 O7 1.15(2) . N C8 O8 1.139(16) . N C9 O9 1.145(16) . N C10 C22 1.427(17) . N C10 C11 1.452(19) . N C11 C12 1.32(2) . N C12 C13 1.39(2) . N C13 C14 1.364(19) . N C14 C22 1.452(17) . N C14 C15 1.456(19) . N C22 C21 1.484(17) . N C15 C16 1.391(19) . N C15 C20 1.422(19) . N C16 C17 1.38(2) . N C17 C18 1.38(2) . N C18 C19 1.40(2) . N C19 C20 1.366(19) . N C20 C21 1.474(18) . N 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 C2 Os1 C3 92.9(6) . . N C2 Os1 C1 87.8(7) . . N C3 Os1 C1 94.4(7) . . N C2 Os1 C10 91.1(6) . . N C3 Os1 C10 98.5(6) . . N C1 Os1 C10 167.1(6) . . N C2 Os1 Os3 95.5(4) . . N C3 Os1 Os3 153.7(5) . . N C1 Os1 Os3 110.8(4) . . N C10 Os1 Os3 56.6(4) . . N C2 Os1 Os2 150.6(4) . . N C3 Os1 Os2 116.5(4) . . N C1 Os1 Os2 89.5(5) . . N C10 Os1 Os2 85.2(4) . . N Os3 Os1 Os2 58.404(19) . . N C6 Os2 C5 94.9(6) . . N C6 Os2 C4 94.8(6) . . N C5 Os2 C4 88.0(7) . . N C6 Os2 C21 96.9(5) . . N C5 Os2 C21 91.9(6) . . N C4 Os2 C21 168.3(6) . . N C6 Os2 Os3 149.5(4) . . N C5 Os2 Os3 92.8(4) . . N C4 Os2 Os3 115.0(5) . . N C21 Os2 Os3 53.3(3) . . N C6 Os2 Os1 119.1(4) . . N C5 Os2 Os1 146.0(4) . . N C4 Os2 Os1 89.9(5) . . N C21 Os2 Os1 83.7(3) . . N Os3 Os2 Os1 57.77(2) . . N C9 Os3 C8 96.2(6) . . N C9 Os3 C7 93.3(8) . . N C8 Os3 C7 94.8(7) . . N C9 Os3 C21 123.6(6) . . N C8 Os3 C21 84.4(5) . . N C7 Os3 C21 143.0(7) . . N C9 Os3 C22 151.6(6) . . N C8 Os3 C22 100.8(5) . . N C7 Os3 C22 107.6(7) . . N C21 Os3 C22 37.5(4) . . N C9 Os3 C10 130.6(6) . . N C8 Os3 C10 132.8(6) . . N C7 Os3 C10 88.6(6) . . N C21 Os3 C10 66.4(5) . . N C22 Os3 C10 35.1(4) . . N C9 Os3 Os1 84.5(5) . . N C8 Os3 Os1 166.4(4) . . N C7 Os3 Os1 98.8(6) . . N C21 Os3 Os1 83.9(3) . . N C22 Os3 Os1 73.7(3) . . N C10 Os3 Os1 46.7(3) . . N C9 Os3 Os2 79.7(5) . . N C8 Os3 Os2 102.8(4) . . N C7 Os3 Os2 161.6(6) . . N C21 Os3 Os2 46.0(3) . . N C22 Os3 Os2 74.5(3) . . N C10 Os3 Os2 83.4(3) . . N Os1 Os3 Os2 63.83(2) . . N O1 C1 Os1 177.8(17) . . N O2 C2 Os1 178.2(16) . . N O3 C3 Os1 178.3(13) . . N O4 C4 Os2 178.0(18) . . N O5 C5 Os2 176.7(15) . . N O6 C6 Os2 174.6(12) . . N O7 C7 Os3 177(2) . . N O8 C8 Os3 175.6(14) . . N O9 C9 Os3 178.7(13) . . N C22 C10 C11 111.3(12) . . N C22 C10 Os1 122.1(9) . . N C11 C10 Os1 126.6(11) . . N C22 C10 Os3 69.1(7) . . N C11 C10 Os3 124.3(10) . . N Os1 C10 Os3 76.8(4) . . N C12 C11 C10 122.4(16) . . N C11 C12 C13 125.6(15) . . N C14 C13 C12 117.2(15) . . N C13 C14 C22 118.4(13) . . N C13 C14 C15 135.3(13) . . N C22 C14 C15 106.3(11) . . N C10 C22 C14 124.8(12) . . N C10 C22 C21 124.7(11) . . N C14 C22 C21 110.4(11) . . N C10 C22 Os3 75.9(7) . . N C14 C22 Os3 124.3(9) . . N C21 C22 Os3 70.5(6) . . N C16 C15 C20 119.9(13) . . N C16 C15 C14 131.0(13) . . N C20 C15 C14 109.0(12) . . N C17 C16 C15 120.7(14) . . N C16 C17 C18 118.6(14) . . N C17 C18 C19 121.9(15) . . N C20 C19 C18 119.6(14) . . N C19 C20 C15 119.2(13) . . N C19 C20 C21 130.3(13) . . N C15 C20 C21 110.5(12) . . N C20 C21 C22 103.7(11) . . N C20 C21 Os2 131.8(9) . . N C22 C21 Os2 123.9(9) . . N C20 C21 Os3 125.3(9) . . N C22 C21 Os3 72.0(6) . . N Os2 C21 Os3 80.6(4) . . N 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 C2 Os1 Os2 C6 -174.9(11) . . . . N C3 Os1 Os2 C6 5.8(7) . . . . N C1 Os1 Os2 C6 100.5(7) . . . . N C10 Os1 Os2 C6 -91.2(6) . . . . N Os3 Os1 Os2 C6 -144.6(5) . . . . N C2 Os1 Os2 C5 3.6(13) . . . . N C3 Os1 Os2 C5 -175.7(10) . . . . N C1 Os1 Os2 C5 -81.0(10) . . . . N C10 Os1 Os2 C5 87.3(9) . . . . N Os3 Os1 Os2 C5 33.9(8) . . . . N C2 Os1 Os2 C4 89.8(12) . . . . N C3 Os1 Os2 C4 -89.5(7) . . . . N C1 Os1 Os2 C4 5.1(7) . . . . N C10 Os1 Os2 C4 173.4(6) . . . . N Os3 Os1 Os2 C4 120.0(5) . . . . N C2 Os1 Os2 C21 -80.4(11) . . . . N C3 Os1 Os2 C21 100.3(6) . . . . N C1 Os1 Os2 C21 -165.1(6) . . . . N C10 Os1 Os2 C21 3.2(5) . . . . N Os3 Os1 Os2 C21 -50.1(3) . . . . N C2 Os1 Os2 Os3 -30.3(10) . . . . N C3 Os1 Os2 Os3 150.4(5) . . . . N C1 Os1 Os2 Os3 -114.9(5) . . . . N C10 Os1 Os2 Os3 53.4(4) . . . . N C2 Os1 Os3 C9 84.5(7) . . . . N C3 Os1 Os3 C9 -167.5(11) . . . . N C1 Os1 Os3 C9 -5.3(7) . . . . N C10 Os1 Os3 C9 172.1(7) . . . . N Os2 Os1 Os3 C9 -81.2(5) . . . . N C2 Os1 Os3 C8 178(2) . . . . N C3 Os1 Os3 C8 -74(2) . . . . N C1 Os1 Os3 C8 88(2) . . . . N C10 Os1 Os3 C8 -94(2) . . . . N Os2 Os1 Os3 C8 13(2) . . . . N C2 Os1 Os3 C7 -8.1(8) . . . . N C3 Os1 Os3 C7 100.0(12) . . . . N C1 Os1 Os3 C7 -97.8(8) . . . . N C10 Os1 Os3 C7 79.6(8) . . . . N Os2 Os1 Os3 C7 -173.7(6) . . . . N C2 Os1 Os3 C21 -150.8(6) . . . . N C3 Os1 Os3 C21 -42.8(11) . . . . N C1 Os1 Os3 C21 119.4(6) . . . . N C10 Os1 Os3 C21 -63.2(6) . . . . N Os2 Os1 Os3 C21 43.5(3) . . . . N C2 Os1 Os3 C22 -113.9(6) . . . . N C3 Os1 Os3 C22 -5.9(11) . . . . N C1 Os1 Os3 C22 156.3(6) . . . . N C10 Os1 Os3 C22 -26.3(5) . . . . N Os2 Os1 Os3 C22 80.4(3) . . . . N C2 Os1 Os3 C10 -87.7(7) . . . . N C3 Os1 Os3 C10 20.4(11) . . . . N C1 Os1 Os3 C10 -177.4(7) . . . . N Os2 Os1 Os3 C10 106.7(4) . . . . N C2 Os1 Os3 Os2 165.6(5) . . . . N C3 Os1 Os3 Os2 -86.3(10) . . . . N C1 Os1 Os3 Os2 75.9(5) . . . . N C10 Os1 Os3 Os2 -106.7(4) . . . . N C6 Os2 Os3 C9 -177.6(10) . . . . N C5 Os2 Os3 C9 -72.9(7) . . . . N C4 Os2 Os3 C9 16.2(7) . . . . N C21 Os2 Os3 C9 -163.1(6) . . . . N Os1 Os2 Os3 C9 88.9(4) . . . . N C6 Os2 Os3 C8 -83.4(10) . . . . N C5 Os2 Os3 C8 21.2(7) . . . . N C4 Os2 Os3 C8 110.3(7) . . . . N C21 Os2 Os3 C8 -69.0(6) . . . . N Os1 Os2 Os3 C8 -177.0(5) . . . . N C6 Os2 Os3 C7 114(2) . . . . N C5 Os2 Os3 C7 -141.7(19) . . . . N C4 Os2 Os3 C7 -53(2) . . . . N C21 Os2 Os3 C7 128.0(19) . . . . N Os1 Os2 Os3 C7 20.1(19) . . . . N C6 Os2 Os3 C21 -14.4(10) . . . . N C5 Os2 Os3 C21 90.3(7) . . . . N C4 Os2 Os3 C21 179.3(7) . . . . N Os1 Os2 Os3 C21 -107.9(4) . . . . N C6 Os2 Os3 C22 14.3(9) . . . . N C5 Os2 Os3 C22 119.0(6) . . . . N C4 Os2 Os3 C22 -151.9(7) . . . . N C21 Os2 Os3 C22 28.8(5) . . . . N Os1 Os2 Os3 C22 -79.2(3) . . . . N C6 Os2 Os3 C10 49.0(9) . . . . N C5 Os2 Os3 C10 153.7(6) . . . . N C4 Os2 Os3 C10 -117.3(6) . . . . N C21 Os2 Os3 C10 63.4(5) . . . . N Os1 Os2 Os3 C10 -44.5(3) . . . . N C6 Os2 Os3 Os1 93.5(9) . . . . N C5 Os2 Os3 Os1 -161.8(5) . . . . N C4 Os2 Os3 Os1 -72.7(6) . . . . N C21 Os2 Os3 Os1 107.9(4) . . . . N C2 Os1 C1 O1 -30(42) . . . . N C3 Os1 C1 O1 -123(42) . . . . N C10 Os1 C1 O1 55(43) . . . . N Os3 Os1 C1 O1 65(42) . . . . N Os2 Os1 C1 O1 121(42) . . . . N C3 Os1 C2 O2 -77(42) . . . . N C1 Os1 C2 O2 -171(42) . . . . N C10 Os1 C2 O2 21(42) . . . . N Os3 Os1 C2 O2 78(42) . . . . N Os2 Os1 C2 O2 103(42) . . . . N C2 Os1 C3 O3 133(50) . . . . N C1 Os1 C3 O3 -139(50) . . . . N C10 Os1 C3 O3 41(50) . . . . N Os3 Os1 C3 O3 24(51) . . . . N Os2 Os1 C3 O3 -48(50) . . . . N C6 Os2 C4 O4 99(46) . . . . N C5 Os2 C4 O4 4(46) . . . . N C21 Os2 C4 O4 -85(46) . . . . N Os3 Os2 C4 O4 -88(46) . . . . N Os1 Os2 C4 O4 -142(46) . . . . N C6 Os2 C5 O5 -96(23) . . . . N C4 Os2 C5 O5 -2(23) . . . . N C21 Os2 C5 O5 167(23) . . . . N Os3 Os2 C5 O5 113(23) . . . . N Os1 Os2 C5 O5 85(23) . . . . N C5 Os2 C6 O6 -88(13) . . . . N C4 Os2 C6 O6 -177(13) . . . . N C21 Os2 C6 O6 4(13) . . . . N Os3 Os2 C6 O6 16(14) . . . . N Os1 Os2 C6 O6 91(13) . . . . N C9 Os3 C7 O7 -176(30) . . . . N C8 Os3 C7 O7 87(30) . . . . N C21 Os3 C7 O7 0(31) . . . . N C22 Os3 C7 O7 -16(31) . . . . N C10 Os3 C7 O7 -46(30) . . . . N Os1 Os3 C7 O7 -92(30) . . . . N Os2 Os3 C7 O7 -110(30) . . . . N C9 Os3 C8 O8 34(17) . . . . N C7 Os3 C8 O8 128(17) . . . . N C21 Os3 C8 O8 -89(17) . . . . N C22 Os3 C8 O8 -123(17) . . . . N C10 Os3 C8 O8 -140(17) . . . . N Os1 Os3 C8 O8 -59(18) . . . . N Os2 Os3 C8 O8 -47(17) . . . . N C8 Os3 C9 O9 163(68) . . . . N C7 Os3 C9 O9 68(68) . . . . N C21 Os3 C9 O9 -109(68) . . . . N C22 Os3 C9 O9 -70(68) . . . . N C10 Os3 C9 O9 -23(69) . . . . N Os1 Os3 C9 O9 -30(68) . . . . N Os2 Os3 C9 O9 -95(68) . . . . N C2 Os1 C10 C22 150.4(11) . . . . N C3 Os1 C10 C22 -116.5(11) . . . . N C1 Os1 C10 C22 65(3) . . . . N Os3 Os1 C10 C22 54.5(9) . . . . N Os2 Os1 C10 C22 -0.5(10) . . . . N C2 Os1 C10 C11 -27.2(13) . . . . N C3 Os1 C10 C11 65.9(14) . . . . N C1 Os1 C10 C11 -112(3) . . . . N Os3 Os1 C10 C11 -123.1(14) . . . . N Os2 Os1 C10 C11 -178.1(13) . . . . N C2 Os1 C10 Os3 95.9(5) . . . . N C3 Os1 C10 Os3 -171.0(5) . . . . N C1 Os1 C10 Os3 11(3) . . . . N Os2 Os1 C10 Os3 -55.0(2) . . . . N C9 Os3 C10 C22 -142.7(9) . . . . N C8 Os3 C10 C22 28.9(11) . . . . N C7 Os3 C10 C22 124.1(10) . . . . N C21 Os3 C10 C22 -27.8(7) . . . . N Os1 Os3 C10 C22 -132.4(9) . . . . N Os2 Os3 C10 C22 -72.4(7) . . . . N C9 Os3 C10 C11 115.2(13) . . . . N C8 Os3 C10 C11 -73.2(14) . . . . N C7 Os3 C10 C11 22.0(14) . . . . N C21 Os3 C10 C11 -130.0(13) . . . . N C22 Os3 C10 C11 -102.1(15) . . . . N Os1 Os3 C10 C11 125.5(14) . . . . N Os2 Os3 C10 C11 -174.6(12) . . . . N C9 Os3 C10 Os1 -10.3(9) . . . . N C8 Os3 C10 Os1 161.3(6) . . . . N C7 Os3 C10 Os1 -103.5(7) . . . . N C21 Os3 C10 Os1 104.5(5) . . . . N C22 Os3 C10 Os1 132.4(9) . . . . N Os2 Os3 C10 Os1 59.9(3) . . . . N C22 C10 C11 C12 5(2) . . . . N Os1 C10 C11 C12 -177.3(13) . . . . N Os3 C10 C11 C12 83.5(19) . . . . N C10 C11 C12 C13 -4(3) . . . . N C11 C12 C13 C14 -1(3) . . . . N C12 C13 C14 C22 3(2) . . . . N C12 C13 C14 C15 -177.9(15) . . . . N C11 C10 C22 C14 -2.3(19) . . . . N Os1 C10 C22 C14 179.8(9) . . . . N Os3 C10 C22 C14 -122.2(12) . . . . N C11 C10 C22 C21 173.5(12) . . . . N Os1 C10 C22 C21 -4.4(18) . . . . N Os3 C10 C22 C21 53.6(11) . . . . N C11 C10 C22 Os3 119.9(12) . . . . N Os1 C10 C22 Os3 -58.1(8) . . . . N C13 C14 C22 C10 -2(2) . . . . N C15 C14 C22 C10 179.2(12) . . . . N C13 C14 C22 C21 -178.1(12) . . . . N C15 C14 C22 C21 2.9(14) . . . . N C13 C14 C22 Os3 -98.3(14) . . . . N C15 C14 C22 Os3 82.7(12) . . . . N C9 Os3 C22 C10 75.4(13) . . . . N C8 Os3 C22 C10 -158.8(8) . . . . N C7 Os3 C22 C10 -60.2(10) . . . . N C21 Os3 C22 C10 135.4(11) . . . . N Os1 Os3 C22 C10 34.0(7) . . . . N Os2 Os3 C22 C10 100.7(7) . . . . N C9 Os3 C22 C14 -161.9(12) . . . . N C8 Os3 C22 C14 -36.1(12) . . . . N C7 Os3 C22 C14 62.5(13) . . . . N C21 Os3 C22 C14 -101.9(13) . . . . N C10 Os3 C22 C14 122.7(14) . . . . N Os1 Os3 C22 C14 156.8(11) . . . . N Os2 Os3 C22 C14 -136.6(11) . . . . N C9 Os3 C22 C21 -59.9(14) . . . . N C8 Os3 C22 C21 65.8(8) . . . . N C7 Os3 C22 C21 164.4(9) . . . . N C10 Os3 C22 C21 -135.4(11) . . . . N Os1 Os3 C22 C21 -101.3(7) . . . . N Os2 Os3 C22 C21 -34.7(6) . . . . N C13 C14 C15 C16 -4(3) . . . . N C22 C14 C15 C16 174.8(14) . . . . N C13 C14 C15 C20 179.3(15) . . . . N C22 C14 C15 C20 -1.9(14) . . . . N C20 C15 C16 C17 -3(2) . . . . N C14 C15 C16 C17 -179.5(14) . . . . N C15 C16 C17 C18 3(2) . . . . N C16 C17 C18 C19 -1(2) . . . . N C17 C18 C19 C20 0(2) . . . . N C18 C19 C20 C15 0(2) . . . . N C18 C19 C20 C21 178.4(13) . . . . N C16 C15 C20 C19 2(2) . . . . N C14 C15 C20 C19 178.9(12) . . . . N C16 C15 C20 C21 -177.0(12) . . . . N C14 C15 C20 C21 0.2(15) . . . . N C19 C20 C21 C22 -177.0(14) . . . . N C15 C20 C21 C22 1.5(14) . . . . N C19 C20 C21 Os2 -6(2) . . . . N C15 C20 C21 Os2 172.6(10) . . . . N C19 C20 C21 Os3 105.5(15) . . . . N C15 C20 C21 Os3 -75.9(13) . . . . N C10 C22 C21 C20 -179.1(12) . . . . N C14 C22 C21 C20 -2.7(13) . . . . N Os3 C22 C21 C20 -123.1(9) . . . . N C10 C22 C21 Os2 8.9(17) . . . . N C14 C22 C21 Os2 -174.7(8) . . . . N Os3 C22 C21 Os2 64.9(8) . . . . N C10 C22 C21 Os3 -55.9(12) . . . . N C14 C22 C21 Os3 120.4(9) . . . . N C6 Os2 C21 C20 -57.6(13) . . . . N C5 Os2 C21 C20 37.6(13) . . . . N C4 Os2 C21 C20 127(3) . . . . N Os3 Os2 C21 C20 129.7(13) . . . . N Os1 Os2 C21 C20 -176.3(12) . . . . N C6 Os2 C21 C22 111.9(11) . . . . N C5 Os2 C21 C22 -152.9(11) . . . . N C4 Os2 C21 C22 -64(3) . . . . N Os3 Os2 C21 C22 -60.8(9) . . . . N Os1 Os2 C21 C22 -6.7(9) . . . . N C6 Os2 C21 Os3 172.7(5) . . . . N C5 Os2 C21 Os3 -92.1(5) . . . . N C4 Os2 C21 Os3 -3(3) . . . . N Os1 Os2 C21 Os3 54.1(2) . . . . N C9 Os3 C21 C20 -115.2(12) . . . . N C8 Os3 C21 C20 -21.4(12) . . . . N C7 Os3 C21 C20 69.1(16) . . . . N C22 Os3 C21 C20 94.3(13) . . . . N C10 Os3 C21 C20 120.5(12) . . . . N Os1 Os3 C21 C20 165.6(11) . . . . N Os2 Os3 C21 C20 -135.3(13) . . . . N C9 Os3 C21 C22 150.4(8) . . . . N C8 Os3 C21 C22 -115.8(8) . . . . N C7 Os3 C21 C22 -25.2(13) . . . . N C10 Os3 C21 C22 26.1(7) . . . . N Os1 Os3 C21 C22 71.2(7) . . . . N Os2 Os3 C21 C22 130.4(8) . . . . N C9 Os3 C21 Os2 20.0(7) . . . . N C8 Os3 C21 Os2 113.8(6) . . . . N C7 Os3 C21 Os2 -155.6(10) . . . . N C22 Os3 C21 Os2 -130.4(8) . . . . N C10 Os3 C21 Os2 -104.3(5) . . . . N Os1 Os3 C21 Os2 -59.2(3) . . . . N _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.183 _refine_diff_density_min -1.258 _refine_diff_density_rms 0.267