# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_coden_Cambridge 440 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Lionel P. Clarke' 'Jacqueline M. Cole' 'John E. Davies' 'Alexandra French' 'Olivia F. Koentjoro' 'Gregory P. Shields' _publ_contact_author_name 'Paul Raithby' _publ_contact_author_address ; Department of Chemistry University of Bath Bath Avon BA2 7AY UNITED KINGDOM ; _publ_contact_author_email P.R.RAITHBY@BATH.AC.UK _publ_section_title ; Molecular rearrangements of diynes coordinated to triosmium carbonyl clusters: reactions of [Os3(Ý-H)2(CO)10] and [Os3(CO)10(MeCN)2] with 1,4-dipyridylbuta-1,3-diyne ; data_pr9610 _database_code_depnum_ccdc_archive 'CCDC 248097' _audit_creation_method SHELXL _chemical_name_systematic ; 'Compound 1' ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H10 N2 O10 Os3' _chemical_formula_weight 1056.94 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 16.374(5) _cell_length_b 17.289(5) _cell_length_c 9.688(2) _cell_angle_alpha 98.63(2) _cell_angle_beta 106.33(2) _cell_angle_gamma 74.81(2) _cell_volume 2531.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.773 _exptl_crystal_density_method ? _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 15.082 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.120 _exptl_absorpt_correction_T_max 0.221 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R four-circle diffractometer' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -3 _diffrn_reflns_number 6865 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6595 _reflns_number_observed 5503 _reflns_observed_criterion I>2\s(I) _computing_data_collection 'Rigaku AFC7R diffractometer control software' _computing_cell_refinement 'Rigaku AFC7R diffractometer control software' _computing_data_reduction 'Rigaku AFC7R diffractometer control software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. Bridging hydride ligand located with program HYDEX, A. G. Orpen, (J. Chem. Soc. Dalton Trans., 1980, 2509) and included in final cycles of refinement with fixed coordinates and isotropic thermal parameter. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0595P)^2^+1.8924P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6594 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_obs 0.0399 _refine_ls_wR_factor_all 0.1052 _refine_ls_wR_factor_obs 0.0977 _refine_ls_goodness_of_fit_all 1.024 _refine_ls_goodness_of_fit_obs 1.047 _refine_ls_restrained_S_all 1.025 _refine_ls_restrained_S_obs 1.047 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Os1 Os 0.84372(4) 1.43410(3) 0.05813(5) 0.0138(2) Uani 1 d . . Os1' Os 1.34903(4) 1.10376(3) 0.21127(6) 0.0151(2) Uani 1 d . . Os2 Os 0.70035(4) 1.56714(3) 0.10035(5) 0.0146(2) Uani 1 d . . Os2' Os 1.18841(4) 1.20098(3) 0.27739(6) 0.0160(2) Uani 1 d . . Os3 Os 0.79470(3) 1.46435(3) 0.33522(5) 0.0127(2) Uani 1 d . . Os3' Os 1.28096(3) 1.05881(3) 0.43173(5) 0.0140(2) Uani 1 d . . C11 C 0.9297(10) 1.3432(9) 0.0213(14) 0.022(3) Uiso 1 d . . O11 O 0.9760(7) 1.2867(6) -0.0146(11) 0.034(3) Uani 1 d . . C11' C 1.4542(9) 1.0369(8) 0.1793(14) 0.017(3) Uiso 1 d . . O11' O 1.5191(7) 0.9969(7) 0.1573(11) 0.035(3) Uani 1 d . . C12 C 0.8059(11) 1.4639(10) -0.1349(17) 0.033(4) Uiso 1 d . . O12 O 0.7832(8) 1.4794(7) -0.2514(11) 0.044(3) Uani 1 d . . C12' C 1.3205(10) 1.1641(9) 0.0491(15) 0.022(3) Uiso 1 d . . O12' O 1.3051(7) 1.1978(6) -0.0526(11) 0.035(3) Uani 1 d . . C13 C 0.9261(11) 1.5047(10) 0.1207(16) 0.029(4) Uiso 1 d . . O13 O 0.9799(8) 1.5384(7) 0.1581(12) 0.043(3) Uani 1 d . . C13' C 1.4088(9) 1.1781(9) 0.3481(14) 0.018(3) Uiso 1 d . . O13' O 1.4490(8) 1.2176(7) 0.4298(11) 0.042(3) Uani 1 d . . C21 C 0.6271(9) 1.4940(8) 0.0022(14) 0.014(3) Uiso 1 d . . O21 O 0.5765(6) 1.4580(6) -0.0639(11) 0.025(2) Uani 1 d . . C21' C 1.1305(10) 1.1411(9) 0.1153(15) 0.022(3) Uiso 1 d . . O21' O 1.0861(7) 1.1108(6) 0.0149(11) 0.037(3) Uani 1 d . . C22 C 0.7839(10) 1.6337(9) 0.1928(15) 0.023(3) Uiso 1 d . . O22 O 0.8297(7) 1.6753(7) 0.2422(11) 0.037(3) Uani 1 d . . C22' C 1.2523(10) 1.2586(9) 0.4402(16) 0.025(4) Uiso 1 d . . O22' O 1.2868(7) 1.2966(6) 0.5335(11) 0.034(3) Uani 1 d . . C23 C 0.6109(11) 1.6296(10) 0.1857(16) 0.028(4) Uiso 1 d . . O23 O 0.5568(7) 1.6662(6) 0.2391(10) 0.029(3) Uani 1 d . . C23' C 1.0902(10) 1.2323(9) 0.3540(15) 0.023(3) Uiso 1 d . . O23' O 1.0263(7) 1.2514(7) 0.3944(12) 0.040(3) Uani 1 d . . C24 C 0.6687(9) 1.6191(8) -0.0713(14) 0.017(3) Uiso 1 d . . O24 O 0.6475(8) 1.6541(6) -0.1734(10) 0.037(3) Uani 1 d . . C24' C 1.1661(11) 1.2878(10) 0.1639(17) 0.033(4) Uiso 1 d . . O24' O 1.1517(7) 1.3412(7) 0.0971(13) 0.042(3) Uani 1 d . . C31 C 0.7105(9) 1.5237(8) 0.4347(14) 0.017(3) Uiso 1 d . . O31 O 0.6628(7) 1.5601(6) 0.4984(10) 0.026(2) Uani 1 d . . C31' C 1.1881(10) 1.0841(9) 0.5225(15) 0.022(3) Uiso 1 d . . O31' O 1.1337(8) 1.1004(7) 0.5824(11) 0.043(3) Uani 1 d . . C32 C 0.8727(10) 1.5357(9) 0.4267(14) 0.018(3) Uiso 1 d . . O32 O 0.9209(7) 1.5731(7) 0.4864(11) 0.035(3) Uani 1 d . . C32' C 1.3457(9) 1.1196(8) 0.5827(14) 0.018(3) Uiso 1 d . . O32' O 1.3893(7) 1.1520(6) 0.6803(10) 0.034(3) Uani 1 d . . C33 C 0.8556(9) 1.3904(8) 0.4764(13) 0.013(3) Uiso 1 d . . O33 O 0.8919(7) 1.3473(6) 0.5651(10) 0.031(3) Uani 1 d . . C33' C 1.3402(10) 0.9618(9) 0.5227(15) 0.023(3) Uiso 1 d . . O33' O 1.3744(7) 0.9043(7) 0.5788(11) 0.037(3) Uani 1 d . . N41 N 0.6903(8) 1.3152(7) 0.4183(11) 0.019(3) Uiso 1 d . . N41' N 1.1943(7) 0.8725(6) 0.3429(11) 0.015(3) Uiso 1 d . . C42 C 0.6407(11) 1.3054(10) 0.5003(16) 0.033(4) Uiso 1 d . . H42 H 0.6652 1.2660 0.5684 0.039 Uiso 1 calc R . C42' C 1.1416(9) 0.8330(9) 0.3701(14) 0.020(3) Uiso 1 d . . H42' H 1.1665 0.7810 0.4039 0.024 Uiso 1 calc R . C43 C 0.5569(10) 1.3489(9) 0.4918(16) 0.029(4) Uiso 1 d . . H43 H 0.5235 1.3387 0.5499 0.035 Uiso 1 calc R . C43' C 1.0545(10) 0.8628(9) 0.3522(14) 0.025(3) Uiso 1 d . . H43' H 1.0201 0.8314 0.3723 0.030 Uiso 1 calc R . C44 C 0.5217(11) 1.4090(10) 0.3951(16) 0.032(4) Uiso 1 d . . H44 H 0.4642 1.4414 0.3869 0.039 Uiso 1 calc R . C44' C 1.0154(10) 0.9380(9) 0.3051(14) 0.024(3) Uiso 1 d . . H44' H 0.9546 0.9601 0.2941 0.029 Uiso 1 calc R . C45 C 0.5734(9) 1.4195(8) 0.3122(14) 0.020(3) Uiso 1 d . . H45 H 0.5517 1.4591 0.2444 0.024 Uiso 1 calc R . C45' C 1.0684(9) 0.9804(9) 0.2743(14) 0.020(3) Uiso 1 d . . H45' H 1.0444 1.0329 0.2425 0.024 Uiso 1 calc R . C46 C 0.6573(9) 1.3717(8) 0.3288(13) 0.014(3) Uiso 1 d . . C46' C 1.1571(8) 0.9455(8) 0.2904(13) 0.011(3) Uiso 1 d . . C47 C 0.7159(9) 1.3805(8) 0.2391(13) 0.015(3) Uiso 1 d . . C47' C 1.2165(9) 0.9881(8) 0.2571(13) 0.013(3) Uiso 1 d . . C48 C 0.7156(9) 1.3413(8) 0.1095(13) 0.013(3) Uiso 1 d . . C48' C 1.2309(9) 0.9787(8) 0.1264(14) 0.017(3) Uiso 1 d . . C49 C 0.7611(9) 1.3533(8) 0.0107(13) 0.014(3) Uiso 1 d . . C49' C 1.2822(9) 1.0209(8) 0.0760(13) 0.015(3) Uiso 1 d . . C50 C 0.7371(9) 1.3049(8) -0.1121(14) 0.018(3) Uiso 1 d . . H50 H 0.7572 1.3011 -0.1963 0.021 Uiso 1 calc R . C50' C 1.2766(9) 0.9957(9) -0.0661(14) 0.021(3) Uiso 1 d . . H50' H 1.3036 1.0144 -0.1255 0.026 Uiso 1 calc R . C51 C 0.6797(9) 1.2620(8) -0.0972(14) 0.020(3) Uiso 1 d . . C51' C 1.2254(9) 0.9383(8) -0.1123(14) 0.019(3) Uiso 1 d . . C52 C 0.6383(9) 1.2040(8) -0.1887(14) 0.018(3) Uiso 1 d . . H52 H 0.6465 1.1893 -0.2832 0.022 Uiso 1 calc R . C52' C 1.2023(9) 0.8920(8) -0.2443(14) 0.019(3) Uiso 1 d . . H52' H 1.2225 0.8981 -0.3238 0.023 Uiso 1 calc R . C53 C 0.5855(10) 1.1686(9) -0.1400(15) 0.023(3) Uiso 1 d . . H53 H 0.5589 1.1283 -0.1993 0.028 Uiso 1 calc R . C53' C 1.1510(9) 0.8385(8) -0.2594(14) 0.020(3) Uiso 1 d . . H53' H 1.1368 0.8067 -0.3478 0.024 Uiso 1 calc R . C54 C 0.5723(10) 1.1934(9) -0.0015(15) 0.028(4) Uiso 1 d . . H54 H 0.5341 1.1715 0.0310 0.033 Uiso 1 calc R . C54' C 1.1199(10) 0.8313(9) -0.1422(14) 0.021(3) Uiso 1 d . . H54' H 1.0827 0.7959 -0.1516 0.026 Uiso 1 calc R . C55 C 0.6125(10) 1.2470(9) 0.0852(15) 0.024(3) Uiso 1 d . . H55 H 0.6054 1.2613 0.1804 0.029 Uiso 1 calc R . C55' C 1.1430(9) 0.8753(8) -0.0151(14) 0.019(3) Uiso 1 d . . H55' H 1.1222 0.8699 0.0643 0.023 Uiso 1 calc R . N56 N 0.6641(7) 1.2814(7) 0.0359(11) 0.017(3) Uiso 1 d . . N56' N 1.1956(7) 0.9271(7) 0.0008(11) 0.015(3) Uiso 1 d . . H1 H 0.8804 1.4052 0.2459 0.030 Uiso 1 calc . . H1' H 1.3766 1.0341 0.3450 0.030 Uiso 1 calc . . 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 0.0112(3) 0.0162(3) 0.0165(3) 0.0004(2) 0.0068(2) -0.0041(2) Os1' 0.0115(3) 0.0169(3) 0.0200(3) -0.0017(2) 0.0067(2) -0.0070(2) Os2 0.0122(3) 0.0139(3) 0.0170(3) 0.0019(2) 0.0035(2) -0.0018(2) Os2' 0.0116(3) 0.0154(3) 0.0204(3) -0.0019(2) 0.0042(2) -0.0037(2) Os3 0.0104(3) 0.0153(3) 0.0129(3) 0.0000(2) 0.0038(2) -0.0035(2) Os3' 0.0104(3) 0.0178(3) 0.0149(3) -0.0005(2) 0.0034(2) -0.0058(2) O11 0.023(6) 0.030(7) 0.048(7) -0.002(5) 0.013(5) -0.003(5) O11' 0.019(6) 0.047(8) 0.034(6) 0.012(5) 0.006(5) 0.006(5) O12 0.060(9) 0.046(8) 0.018(6) 0.012(5) 0.011(6) 0.008(6) O12' 0.042(7) 0.034(7) 0.033(6) 0.013(5) 0.011(5) -0.008(6) O13 0.044(8) 0.042(8) 0.053(7) -0.016(6) 0.018(6) -0.033(6) O13' 0.039(8) 0.051(8) 0.034(6) -0.025(6) 0.009(6) -0.024(6) O21 0.014(6) 0.016(6) 0.042(6) 0.006(5) -0.001(5) -0.003(5) O21' 0.024(7) 0.023(6) 0.046(7) -0.002(5) -0.007(5) 0.006(5) O22 0.033(7) 0.032(7) 0.045(7) 0.009(5) -0.004(5) -0.019(6) O22' 0.027(7) 0.026(6) 0.039(6) -0.015(5) -0.002(5) -0.009(5) O23 0.021(6) 0.037(7) 0.023(5) -0.001(5) -0.001(5) -0.003(5) O23' 0.026(7) 0.042(8) 0.047(7) -0.005(6) 0.012(6) -0.004(6) O24 0.052(8) 0.029(7) 0.025(6) 0.014(5) -0.008(5) -0.015(6) O24' 0.028(7) 0.041(8) 0.061(8) 0.018(6) 0.006(6) -0.013(6) O31 0.026(6) 0.020(6) 0.029(5) -0.003(4) 0.008(5) -0.004(5) O31' 0.043(8) 0.061(9) 0.038(6) -0.011(6) 0.032(6) -0.021(6) O32 0.028(7) 0.038(7) 0.032(6) -0.002(5) -0.008(5) -0.018(6) O32' 0.035(7) 0.036(7) 0.025(6) -0.005(5) 0.002(5) -0.012(5) O33 0.036(7) 0.029(6) 0.030(6) 0.008(5) 0.007(5) -0.008(5) O33' 0.030(7) 0.035(7) 0.035(6) 0.009(5) -0.011(5) -0.009(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 C11 1.880(15) . ? Os1 C12 1.90(2) . ? Os1 C13 1.96(2) . ? Os1 C49 2.108(14) . ? Os1 Os2 2.8977(11) . ? Os1 Os3 2.9486(9) . ? Os1' C11' 1.884(14) . ? Os1' C12' 1.897(14) . ? Os1' C13' 1.94(2) . ? Os1' C49' 2.103(14) . ? Os1' Os2' 2.9086(11) . ? Os1' Os3' 2.9493(9) . ? Os2 C24 1.887(13) . ? Os2 C23 1.89(2) . ? Os2 C21 1.933(15) . ? Os2 C22 1.96(2) . ? Os2 Os3 2.9189(11) . ? Os2' C23' 1.877(15) . ? Os2' C24' 1.89(2) . ? Os2' C21' 1.90(2) . ? Os2' C22' 1.93(2) . ? Os2' Os3' 2.9071(12) . ? Os3 C33 1.895(13) . ? Os3 C31 1.895(14) . ? Os3 C32 1.95(2) . ? Os3 C47 2.130(14) . ? Os3' C31' 1.888(14) . ? Os3' C32' 1.902(15) . ? Os3' C33' 1.91(2) . ? Os3' C47' 2.126(13) . ? C11 O11 1.14(2) . ? C11' O11' 1.16(2) . ? C12 O12 1.13(2) . ? C12' O12' 1.15(2) . ? C13 O13 1.13(2) . ? C13' O13' 1.14(2) . ? C21 O21 1.16(2) . ? C21' O21' 1.18(2) . ? C22 O22 1.13(2) . ? C22' O22' 1.14(2) . ? C23 O23 1.15(2) . ? C23' O23' 1.17(2) . ? C24 O24 1.16(2) . ? C24' O24' 1.14(2) . ? C31 O31 1.13(2) . ? C31' O31' 1.15(2) . ? C32 O32 1.13(2) . ? C32' O32' 1.18(2) . ? C33 O33 1.15(2) . ? C33' O33' 1.14(2) . ? N41 C46 1.31(2) . ? N41 C42 1.34(2) . ? N41' C42' 1.33(2) . ? N41' C46' 1.36(2) . ? C42 C43 1.37(2) . ? C42' C43' 1.35(2) . ? C43 C44 1.40(2) . ? C43' C44' 1.37(2) . ? C44 C45 1.38(2) . ? C44' C45' 1.39(2) . ? C45 C46 1.38(2) . ? C45' C46' 1.39(2) . ? C46 C47 1.51(2) . ? C46' C47' 1.49(2) . ? C47 C48 1.33(2) . ? C47' C48' 1.33(2) . ? C48 C49 1.43(2) . ? C48 N56 1.48(2) . ? C48' C49' 1.46(2) . ? C48' N56' 1.47(2) . ? C49 C50 1.37(2) . ? C49' C50' 1.37(2) . ? C50 C51 1.39(2) . ? C50' C51' 1.41(2) . ? C51 N56 1.36(2) . ? C51 C52 1.41(2) . ? C51' N56' 1.37(2) . ? C51' C52' 1.41(2) . ? C52 C53 1.39(2) . ? C52' C53' 1.37(2) . ? C53 C54 1.40(2) . ? C53' C54' 1.40(2) . ? C54 C55 1.33(2) . ? C54' C55' 1.36(2) . ? C55 N56 1.37(2) . ? C55' N56' 1.36(2) . ? 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 C11 Os1 C12 94.9(6) . . ? C11 Os1 C13 93.7(6) . . ? C12 Os1 C13 93.8(7) . . ? C11 Os1 C49 84.8(6) . . ? C12 Os1 C49 91.8(6) . . ? C13 Os1 C49 174.3(5) . . ? C11 Os1 Os2 175.2(5) . . ? C12 Os1 Os2 83.4(5) . . ? C13 Os1 Os2 90.9(4) . . ? C49 Os1 Os2 90.8(3) . . ? C11 Os1 Os3 121.1(4) . . ? C12 Os1 Os3 142.7(5) . . ? C13 Os1 Os3 93.1(4) . . ? C49 Os1 Os3 83.1(3) . . ? Os2 Os1 Os3 59.90(3) . . ? C11' Os1' C12' 96.7(6) . . ? C11' Os1' C13' 93.0(6) . . ? C12' Os1' C13' 96.0(6) . . ? C11' Os1' C49' 88.5(6) . . ? C12' Os1' C49' 87.7(6) . . ? C13' Os1' C49' 175.8(5) . . ? C11' Os1' Os2' 176.1(4) . . ? C12' Os1' Os2' 87.2(4) . . ? C13' Os1' Os2' 86.7(4) . . ? C49' Os1' Os2' 91.6(4) . . ? C11' Os1' Os3' 116.7(4) . . ? C12' Os1' Os3' 145.0(4) . . ? C13' Os1' Os3' 92.6(4) . . ? C49' Os1' Os3' 83.2(3) . . ? Os2' Os1' Os3' 59.50(3) . . ? C24 Os2 C23 98.8(6) . . ? C24 Os2 C21 88.9(6) . . ? C23 Os2 C21 90.8(6) . . ? C24 Os2 C22 91.0(6) . . ? C23 Os2 C22 94.8(6) . . ? C21 Os2 C22 174.3(6) . . ? C24 Os2 Os1 102.9(4) . . ? C23 Os2 Os1 157.8(4) . . ? C21 Os2 Os1 84.8(4) . . ? C22 Os2 Os1 89.7(4) . . ? C24 Os2 Os3 163.2(4) . . ? C23 Os2 Os3 97.8(4) . . ? C21 Os2 Os3 93.7(4) . . ? C22 Os2 Os3 84.8(4) . . ? Os1 Os2 Os3 60.92(3) . . ? C23' Os2' C24' 99.7(6) . . ? C23' Os2' C21' 92.7(6) . . ? C24' Os2' C21' 90.4(7) . . ? C23' Os2' C22' 89.8(6) . . ? C24' Os2' C22' 90.2(7) . . ? C21' Os2' C22' 177.3(6) . . ? C23' Os2' Os3' 99.4(4) . . ? C24' Os2' Os3' 160.3(5) . . ? C21' Os2' Os3' 93.3(4) . . ? C22' Os2' Os3' 85.3(4) . . ? C23' Os2' Os1' 160.1(4) . . ? C24' Os2' Os1' 100.2(5) . . ? C21' Os2' Os1' 85.3(4) . . ? C22' Os2' Os1' 92.0(4) . . ? Os3' Os2' Os1' 60.95(2) . . ? C33 Os3 C31 96.5(5) . . ? C33 Os3 C32 90.3(6) . . ? C31 Os3 C32 90.9(6) . . ? C33 Os3 C47 86.8(5) . . ? C31 Os3 C47 91.2(5) . . ? C32 Os3 C47 176.6(5) . . ? C33 Os3 Os2 175.4(4) . . ? C31 Os3 Os2 86.5(4) . . ? C32 Os3 Os2 93.2(4) . . ? C47 Os3 Os2 89.6(3) . . ? C33 Os3 Os1 117.4(4) . . ? C31 Os3 Os1 145.3(4) . . ? C32 Os3 Os1 95.9(4) . . ? C47 Os3 Os1 83.9(3) . . ? Os2 Os3 Os1 59.19(2) . . ? C31' Os3' C32' 90.6(6) . . ? C31' Os3' C33' 95.6(6) . . ? C32' Os3' C33' 91.2(6) . . ? C31' Os3' C47' 93.4(6) . . ? C32' Os3' C47' 176.0(5) . . ? C33' Os3' C47' 87.9(6) . . ? C31' Os3' Os2' 85.6(4) . . ? C32' Os3' Os2' 91.9(4) . . ? C33' Os3' Os2' 176.7(4) . . ? C47' Os3' Os2' 88.9(3) . . ? C31' Os3' Os1' 145.1(4) . . ? C32' Os3' Os1' 92.6(4) . . ? C33' Os3' Os1' 119.0(4) . . ? C47' Os3' Os1' 84.4(3) . . ? Os2' Os3' Os1' 59.55(3) . . ? O11 C11 Os1 172.8(13) . . ? O11' C11' Os1' 178.4(12) . . ? O12 C12 Os1 178.0(15) . . ? O12' C12' Os1' 176.9(13) . . ? O13 C13 Os1 173.0(14) . . ? O13' C13' Os1' 175.3(13) . . ? O21 C21 Os2 172.0(12) . . ? O21' C21' Os2' 172.4(13) . . ? O22 C22 Os2 176.6(13) . . ? O22' C22' Os2' 176.1(14) . . ? O23 C23 Os2 178.5(13) . . ? O23' C23' Os2' 176.4(13) . . ? O24 C24 Os2 176.9(12) . . ? O24' C24' Os2' 178.7(14) . . ? O31 C31 Os3 177.3(12) . . ? O31' C31' Os3' 177.4(13) . . ? O32 C32 Os3 175.1(12) . . ? O32' C32' Os3' 175.1(12) . . ? O33 C33 Os3 178.0(11) . . ? O33' C33' Os3' 178.6(13) . . ? C46 N41 C42 117.7(12) . . ? C42' N41' C46' 117.3(12) . . ? N41 C42 C43 123.8(15) . . ? N41' C42' C43' 123.6(14) . . ? C42 C43 C44 118.2(14) . . ? C42' C43' C44' 120.5(15) . . ? C45 C44 C43 117.7(15) . . ? C43' C44' C45' 117.2(14) . . ? C44 C45 C46 119.3(13) . . ? C44' C45' C46' 119.6(13) . . ? N41 C46 C45 123.2(12) . . ? N41 C46 C47 115.6(12) . . ? C45 C46 C47 121.2(11) . . ? N41' C46' C45' 121.6(12) . . ? N41' C46' C47' 116.7(11) . . ? C45' C46' C47' 121.6(12) . . ? C48 C47 C46 122.8(13) . . ? C48 C47 Os3 123.4(10) . . ? C46 C47 Os3 113.8(9) . . ? C48' C47' C46' 121.1(12) . . ? C48' C47' Os3' 122.5(10) . . ? C46' C47' Os3' 116.3(8) . . ? C47 C48 C49 126.2(13) . . ? C47 C48 N56 126.9(12) . . ? C49 C48 N56 106.8(10) . . ? C47' C48' C49' 126.9(13) . . ? C47' C48' N56' 127.6(13) . . ? C49' C48' N56' 105.4(10) . . ? C50 C49 C48 106.2(12) . . ? C50 C49 Os1 130.5(9) . . ? C48 C49 Os1 123.3(9) . . ? C50' C49' C48' 107.5(13) . . ? C50' C49' Os1' 130.0(11) . . ? C48' C49' Os1' 122.5(9) . . ? C49 C50 C51 111.2(12) . . ? C49' C50' C51' 110.5(12) . . ? N56 C51 C50 109.5(12) . . ? N56 C51 C52 117.2(12) . . ? C50 C51 C52 133.3(12) . . ? N56' C51' C50' 109.0(12) . . ? N56' C51' C52' 117.7(13) . . ? C50' C51' C52' 133.4(12) . . ? C53 C52 C51 119.9(12) . . ? C53' C52' C51' 121.2(12) . . ? C52 C53 C54 118.8(14) . . ? C52' C53' C54' 118.9(13) . . ? C55 C54 C53 121.1(15) . . ? C55' C54' C53' 119.8(14) . . ? C54 C55 N56 119.4(13) . . ? C54' C55' N56' 121.3(12) . . ? C51 N56 C55 123.6(12) . . ? C51 N56 C48 106.3(11) . . ? C55 N56 C48 130.0(11) . . ? C55' N56' C51' 121.2(11) . . ? C55' N56' C48' 131.1(11) . . ? C51' N56' C48' 107.7(11) . . ? _refine_diff_density_max 1.516 _refine_diff_density_min -2.350 _refine_diff_density_rms 0.283 data_pr9612 _database_code_depnum_ccdc_archive 'CCDC 248098' _audit_creation_method SHELXL _chemical_name_systematic ; 'Compound 2' ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H10 N2 O10 Os3' _chemical_formula_weight 1056.94 _chemical_melting_point ? _chemical_compound_source 'CH2Cl2/CDCl3 evaporation' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.296(2) _cell_length_b 13.576(2) _cell_length_c 18.931(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.150(10) _cell_angle_gamma 90.00 _cell_volume 5229.9(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description 'Irregular block' _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.685 _exptl_crystal_density_method ? _exptl_crystal_F_000 3808 _exptl_absorpt_coefficient_mu 14.600 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.059 _exptl_absorpt_correction_T_max 0.150 _exptl_special_details ; ? ; _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 'Stoe-Siemens four-circle diffractometer' _diffrn_measurement_method '\w\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 7025 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6808 _reflns_number_observed 4790 _reflns_observed_criterion I>2\s(I) _computing_data_collection DIF4 _computing_cell_refinement DIF4 _computing_data_reduction REDU4 _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0469P)^2^+16.1225P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6807 _refine_ls_number_parameters 503 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_obs 0.0448 _refine_ls_wR_factor_all 0.0955 _refine_ls_wR_factor_obs 0.0833 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_obs 1.111 _refine_ls_restrained_S_all 1.052 _refine_ls_restrained_S_obs 1.111 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Os1 Os 0.33012(3) 0.20585(5) 0.91733(3) 0.0374(2) Uani 1 d . . Os1' Os 0.17422(3) 0.78099(6) 0.36808(4) 0.0439(2) Uani 1 d . . Os2 Os 0.31116(3) 0.31728(5) 0.78699(3) 0.0387(2) Uani 1 d . . Os2' Os 0.17624(3) 0.87888(5) 0.50088(4) 0.0378(2) Uani 1 d . . Os3 Os 0.37158(3) 0.13668(5) 0.79933(4) 0.0414(2) Uani 1 d . . Os3' Os 0.13656(3) 0.68577(5) 0.48115(4) 0.0386(2) Uani 1 d . . O11 O 0.2678(7) 0.3548(11) 0.9974(8) 0.084(4) Uiso 1 d . . O11' O 0.2072(6) 0.9197(11) 0.2556(8) 0.080(4) Uiso 1 d . . C11 C 0.2927(8) 0.2986(14) 0.9694(9) 0.052(5) Uiso 1 d . . C11' C 0.1955(8) 0.8682(14) 0.2973(10) 0.053(5) Uiso 1 d . . O12 O 0.3779(6) 0.0567(10) 1.0424(7) 0.068(4) Uiso 1 d . . O12' O 0.1483(6) 0.6061(11) 0.2635(8) 0.076(4) Uiso 1 d . . C12 C 0.3591(8) 0.1134(14) 0.9947(10) 0.057(5) Uiso 1 d . . C12' C 0.1589(9) 0.6711(15) 0.3044(11) 0.061(5) Uiso 1 d . . O13 O 0.2029(6) 0.0953(9) 0.8524(7) 0.063(3) Uiso 1 d . . O13' O 0.3171(7) 0.7248(12) 0.4381(8) 0.092(5) Uiso 1 d . . C13 C 0.2520(8) 0.1367(13) 0.8781(9) 0.048(4) Uiso 1 d . . C13' C 0.2609(9) 0.7465(15) 0.4100(11) 0.063(5) Uiso 1 d . . O21 O 0.3264(6) 0.4924(11) 0.8917(8) 0.076(4) Uiso 1 d . . O21' O 0.1591(6) 1.0348(10) 0.3778(7) 0.068(4) Uiso 1 d . . C21 C 0.3212(8) 0.4218(15) 0.8540(10) 0.055(5) Uiso 1 d . . C21' C 0.1660(8) 0.9654(13) 0.4163(9) 0.048(4) Uiso 1 d . . O22 O 0.1615(7) 0.3012(11) 0.7598(7) 0.080(4) Uiso 1 d . . O22' O 0.3247(7) 0.9116(12) 0.5555(8) 0.097(5) Uiso 1 d . . C22 C 0.2180(9) 0.3096(14) 0.7687(10) 0.058(5) Uiso 1 d . . C22' C 0.2681(9) 0.8983(14) 0.5308(10) 0.058(5) Uiso 1 d . . O23 O 0.2848(7) 0.4553(12) 0.6557(9) 0.091(5) Uiso 1 d . . O23' O 0.1557(7) 1.0553(13) 0.5894(8) 0.096(5) Uiso 1 d . . C23 C 0.2986(10) 0.3990(16) 0.7049(12) 0.073(6) Uiso 1 d . . C23' C 0.1639(9) 0.9844(15) 0.5590(10) 0.062(5) Uiso 1 d . . O31 O 0.4694(8) 0.0502(13) 0.9343(9) 0.100(5) Uiso 1 d . . O31' O 0.0476(7) 0.5694(11) 0.3552(8) 0.082(4) Uiso 1 d . . C31 C 0.4268(9) 0.0838(15) 0.8845(11) 0.065(5) Uiso 1 d . . C31' C 0.0844(8) 0.6105(14) 0.4032(10) 0.054(5) Uiso 1 d . . O32 O 0.2860(9) -0.0485(16) 0.7713(11) 0.131(7) Uiso 1 d . . O32' O 0.2513(7) 0.5430(12) 0.5051(8) 0.091(5) Uiso 1 d . . C32 C 0.3175(12) 0.0218(21) 0.7812(13) 0.097(8) Uiso 1 d . . C32' C 0.2079(9) 0.5959(15) 0.4980(10) 0.061(5) Uiso 1 d . . O33 O 0.4457(7) 0.0699(11) 0.6923(8) 0.085(4) Uiso 1 d . . O33' O 0.0752(7) 0.5971(11) 0.5934(8) 0.085(4) Uiso 1 d . . C33 C 0.4192(9) 0.0996(15) 0.7341(11) 0.064(5) Uiso 1 d . . C33' C 0.0992(9) 0.6325(15) 0.5509(11) 0.066(5) Uiso 1 d . . O34 O 0.2785(9) 0.1917(15) 0.6423(11) 0.136(7) Uiso 1 d . . O34' O 0.2044(6) 0.7652(11) 0.6492(8) 0.077(4) Uiso 1 d . . C34 C 0.3044(10) 0.2003(16) 0.7079(12) 0.072(6) Uiso 1 d . . C34' C 0.1870(8) 0.7829(14) 0.5849(10) 0.054(5) Uiso 1 d . . N41 N 0.4230(5) 0.2827(9) 0.9508(6) 0.030(3) Uani 1 d . . N41' N 0.0735(6) 0.8251(9) 0.3322(6) 0.036(3) Uani 1 d . . C42 C 0.4512(7) 0.3055(12) 1.0217(8) 0.039(4) Uani 1 d . . H42 H 0.4311(7) 0.2846(12) 1.0565(8) 0.046 Uiso 1 calc R . C42' C 0.0424(9) 0.8375(13) 0.2605(8) 0.049(5) Uani 1 d . . H42' H 0.0640(9) 0.8221(13) 0.2258(8) 0.059 Uiso 1 calc R . C43 C 0.5073(8) 0.3573(13) 1.0448(8) 0.047(4) Uani 1 d . . H43 H 0.5264(8) 0.3702(13) 1.0947(8) 0.056 Uiso 1 calc R . C43' C -0.0207(9) 0.8726(13) 0.2370(11) 0.059(5) Uani 1 d . . H43' H -0.0417(9) 0.8790(13) 0.1866(11) 0.071 Uiso 1 calc R . C44 C 0.5361(8) 0.3912(14) 0.9922(9) 0.052(5) Uani 1 d . . H44 H 0.5745(8) 0.4284(14) 1.0064(9) 0.062 Uiso 1 calc R . C44' C -0.0532(9) 0.8982(13) 0.2869(11) 0.060(5) Uani 1 d . . H44' H -0.0954(9) 0.9241(13) 0.2709(11) 0.071 Uiso 1 calc R . C45 C 0.5071(7) 0.3687(13) 0.9192(8) 0.042(4) Uani 1 d . . H45 H 0.5255(7) 0.3919(13) 0.8836(8) 0.051 Uiso 1 calc R . C45' C -0.0220(7) 0.8851(11) 0.3621(10) 0.042(4) Uani 1 d . . H45' H -0.0425(7) 0.9039(11) 0.3972(10) 0.050 Uiso 1 calc R . C46 C 0.4502(7) 0.3114(12) 0.8977(8) 0.035(4) Uani 1 d . . C46' C 0.0408(7) 0.8428(11) 0.3836(8) 0.034(4) Uani 1 d . . C47 C 0.4181(6) 0.2870(11) 0.8213(8) 0.031(4) Uani 1 d . . C47' C 0.0762(7) 0.8177(10) 0.4614(8) 0.033(4) Uani 1 d . . C48 C 0.4588(7) 0.3109(12) 0.7707(8) 0.035(4) Uani 1 d . . C48' C 0.0320(7) 0.8253(11) 0.5119(8) 0.035(4) Uani 1 d . . C49 C 0.4493(8) 0.3704(13) 0.7098(9) 0.052(5) Uani 1 d . . H49 H 0.4134(8) 0.4116(13) 0.6906(9) 0.062 Uiso 1 calc R . C49' C 0.0389(7) 0.8744(13) 0.5763(9) 0.047(5) Uani 1 d . . H49' H 0.0730(7) 0.9177(13) 0.5980(9) 0.057 Uiso 1 calc R . C50 C 0.5022(10) 0.3589(15) 0.6818(10) 0.063(6) Uani 1 d . . H50 H 0.5071(10) 0.3909(15) 0.6403(10) 0.075 Uiso 1 calc R . C50' C -0.0137(8) 0.8498(13) 0.6060(10) 0.049(5) Uani 1 d . . H50' H -0.0195(8) 0.8719(13) 0.6501(10) 0.059 Uiso 1 calc R . C51 C 0.5455(9) 0.2942(15) 0.7240(10) 0.054(5) Uani 1 d . . C51' C -0.0536(8) 0.7870(13) 0.5558(9) 0.048(5) Uani 1 d . . C52 C 0.6066(10) 0.2547(19) 0.7233(13) 0.078(7) Uani 1 d . . H52 H 0.6253(10) 0.2746(19) 0.6870(13) 0.093 Uiso 1 calc R . C52' C -0.1130(9) 0.7385(15) 0.5529(11) 0.062(5) Uani 1 d . . H52' H -0.1340(9) 0.7530(15) 0.5884(11) 0.074 Uiso 1 calc R . C53 C 0.6388(9) 0.1872(18) 0.7757(13) 0.076(7) Uani 1 d . . H53 H 0.6778(9) 0.1586(18) 0.7733(13) 0.091 Uiso 1 calc R . C53' C -0.1405(10) 0.6707(16) 0.4992(11) 0.068(6) Uani 1 d . . H53' H -0.1778(10) 0.6354(16) 0.4996(11) 0.081 Uiso 1 calc R . C54 C 0.6124(9) 0.1623(16) 0.8321(12) 0.075(6) Uani 1 d . . H54 H 0.6355(9) 0.1207(16) 0.8699(12) 0.090 Uiso 1 calc R . C54' C -0.1097(8) 0.6566(14) 0.4430(10) 0.061(5) Uani 1 d . . H54' H -0.1291(8) 0.6137(14) 0.4044(10) 0.074 Uiso 1 calc R . C55 C 0.5534(8) 0.1982(14) 0.8323(10) 0.055(5) Uani 1 d . . H55 H 0.5349(8) 0.1772(14) 0.8684(10) 0.066 Uiso 1 calc R . C55' C -0.0533(8) 0.7027(14) 0.4429(10) 0.054(5) Uani 1 d . . H55' H -0.0339(8) 0.6899(14) 0.4058(10) 0.065 Uiso 1 calc R . N56 N 0.5198(6) 0.2655(11) 0.7801(7) 0.047(4) Uani 1 d . . N56' N -0.0243(6) 0.7706(10) 0.4998(7) 0.042(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 0.0372(4) 0.0486(5) 0.0287(4) -0.0003(3) 0.0133(3) -0.0058(3) Os1' 0.0419(4) 0.0551(5) 0.0405(4) -0.0035(3) 0.0211(3) 0.0031(3) Os2 0.0368(4) 0.0468(5) 0.0312(4) 0.0020(3) 0.0078(3) 0.0013(3) Os2' 0.0325(3) 0.0405(4) 0.0422(4) -0.0056(3) 0.0137(3) -0.0003(3) Os3 0.0475(4) 0.0412(4) 0.0398(4) -0.0064(3) 0.0197(3) -0.0040(3) Os3' 0.0433(4) 0.0339(4) 0.0414(4) 0.0032(3) 0.0169(3) 0.0089(3) N41 0.030(6) 0.032(8) 0.032(8) 0.001(6) 0.013(6) -0.003(6) N41' 0.043(7) 0.040(9) 0.028(8) -0.003(6) 0.013(6) -0.004(6) C42 0.045(10) 0.044(11) 0.024(9) -0.004(8) 0.007(7) -0.006(8) C42' 0.065(12) 0.057(13) 0.023(10) -0.014(8) 0.010(9) -0.004(10) C43 0.054(11) 0.057(12) 0.023(9) -0.012(8) 0.004(8) -0.010(9) C43' 0.071(13) 0.043(13) 0.057(13) 0.001(10) 0.009(11) 0.004(11) C44 0.047(10) 0.067(14) 0.042(11) -0.004(10) 0.016(9) -0.004(9) C44' 0.045(10) 0.046(13) 0.072(15) 0.004(11) -0.005(10) 0.003(9) C45 0.038(9) 0.054(12) 0.032(10) -0.009(8) 0.006(8) 0.003(9) C45' 0.036(9) 0.024(10) 0.066(12) 0.013(8) 0.014(8) 0.014(8) C46 0.027(8) 0.050(11) 0.024(8) 0.007(8) 0.005(7) 0.016(8) C46' 0.038(9) 0.027(10) 0.043(10) -0.002(8) 0.020(8) -0.006(7) C47 0.029(8) 0.034(10) 0.030(9) -0.003(7) 0.010(7) -0.004(7) C47' 0.034(8) 0.014(9) 0.053(10) -0.009(8) 0.016(8) -0.007(7) C48 0.041(9) 0.044(11) 0.026(9) -0.004(8) 0.018(7) 0.002(8) C48' 0.047(9) 0.021(9) 0.040(10) -0.010(8) 0.020(8) -0.003(8) C49 0.051(10) 0.052(13) 0.051(12) 0.005(10) 0.013(9) -0.014(9) C49' 0.030(9) 0.057(13) 0.058(12) -0.018(10) 0.018(8) -0.011(8) C50 0.106(16) 0.055(14) 0.046(12) 0.007(10) 0.053(12) -0.024(12) C50' 0.048(10) 0.053(12) 0.056(11) -0.021(10) 0.032(9) -0.012(9) C51 0.065(12) 0.058(14) 0.047(12) -0.007(10) 0.029(10) -0.011(10) C51' 0.055(11) 0.058(13) 0.043(11) -0.005(9) 0.035(9) 0.000(9) C52 0.062(14) 0.101(19) 0.090(18) -0.029(15) 0.052(13) -0.019(14) C52' 0.067(12) 0.069(15) 0.064(13) -0.002(11) 0.042(11) -0.008(11) C53 0.045(12) 0.090(19) 0.102(18) -0.026(15) 0.036(13) -0.004(12) C53' 0.065(13) 0.068(15) 0.084(16) 0.001(12) 0.042(12) -0.002(11) C54 0.061(13) 0.071(16) 0.094(17) -0.001(13) 0.023(12) 0.018(11) C54' 0.047(11) 0.065(14) 0.068(13) -0.011(11) 0.010(10) -0.021(10) C55 0.046(11) 0.059(14) 0.062(13) -0.001(11) 0.019(9) -0.005(10) C55' 0.042(10) 0.056(13) 0.068(13) 0.006(11) 0.021(9) 0.003(9) N56 0.051(8) 0.052(10) 0.047(9) 0.013(8) 0.028(7) 0.011(8) N56' 0.037(7) 0.040(9) 0.055(9) -0.002(7) 0.022(7) -0.010(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 C13 1.86(2) . ? Os1 C12 1.89(2) . ? Os1 C11 1.91(2) . ? Os1 N41 2.159(11) . ? Os1 Os3 2.7954(9) . ? Os1 Os2 2.8201(9) . ? Os1' C13' 1.84(2) . ? Os1' C12' 1.89(2) . ? Os1' C11' 1.94(2) . ? Os1' N41' 2.136(12) . ? Os1' Os3' 2.8122(9) . ? Os1' Os2' 2.8328(9) . ? Os2 C23 1.86(2) . ? Os2 C21 1.87(2) . ? Os2 C22 1.91(2) . ? Os2 C34 2.16(2) . ? Os2 C47 2.215(13) . ? Os2 Os3 2.7468(10) . ? Os2' C23' 1.87(2) . ? Os2' C22' 1.89(2) . ? Os2' C21' 1.95(2) . ? Os2' C34' 2.02(2) . ? Os2' C47' 2.203(13) . ? Os2' Os3' 2.7460(10) . ? Os3 C31 1.84(2) . ? Os3 C33 1.88(2) . ? Os3 C32 1.91(3) . ? Os3 C34 2.08(2) . ? Os3 C47 2.253(15) . ? Os3' C31' 1.87(2) . ? Os3' C33' 1.88(2) . ? Os3' C32' 1.90(2) . ? Os3' C47' 2.172(14) . ? Os3' C34' 2.35(2) . ? O11 C11 1.14(2) . ? O11' C11' 1.13(2) . ? O12 C12 1.16(2) . ? O12' C12' 1.15(2) . ? O13 C13 1.16(2) . ? O13' C13' 1.19(2) . ? O21 C21 1.18(2) . ? O21' C21' 1.17(2) . ? O22 C22 1.17(2) . ? O22' C22' 1.17(2) . ? O23 C23 1.17(2) . ? O23' C23' 1.16(2) . ? O31 C31 1.19(2) . ? O31' C31' 1.15(2) . ? O32 C32 1.15(3) . ? O32' C32' 1.15(2) . ? O33 C33 1.17(2) . ? O33' C33' 1.17(2) . ? O34 C34 1.21(2) . ? O34' C34' 1.19(2) . ? N41 C42 1.34(2) . ? N41 C46 1.36(2) . ? N41' C42' 1.33(2) . ? N41' C46' 1.37(2) . ? C42 C43 1.34(2) . ? C42' C43' 1.37(2) . ? C43 C44 1.39(2) . ? C43' C44' 1.37(2) . ? C44 C45 1.37(2) . ? C44' C45' 1.39(2) . ? C45 C46 1.40(2) . ? C45' C46' 1.40(2) . ? C46 C47 1.45(2) . ? C46' C47' 1.48(2) . ? C47 C48 1.50(2) . ? C47' C48' 1.53(2) . ? C48 C49 1.37(2) . ? C48 N56 1.40(2) . ? C48' C49' 1.36(2) . ? C48' N56' 1.37(2) . ? C49 C50 1.39(2) . ? C49' C50' 1.43(2) . ? C50 C51 1.35(3) . ? C50' C51' 1.37(2) . ? C51 N56 1.39(2) . ? C51 C52 1.41(3) . ? C51' N56' 1.40(2) . ? C51' C52' 1.41(2) . ? C52 C53 1.38(3) . ? C52' C53' 1.37(3) . ? C53 C54 1.39(3) . ? C53' C54' 1.42(2) . ? C54 C55 1.35(2) . ? C54' C55' 1.35(2) . ? C55 N56 1.38(2) . ? C55' N56' 1.41(2) . ? 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 C13 Os1 C12 91.3(8) . . ? C13 Os1 C11 94.5(7) . . ? C12 Os1 C11 97.4(8) . . ? C13 Os1 N41 173.3(6) . . ? C12 Os1 N41 91.9(6) . . ? C11 Os1 N41 90.9(6) . . ? C13 Os1 Os3 88.1(5) . . ? C12 Os1 Os3 106.8(5) . . ? C11 Os1 Os3 155.7(5) . . ? N41 Os1 Os3 85.3(3) . . ? C13 Os1 Os2 92.3(5) . . ? C12 Os1 Os2 164.7(5) . . ? C11 Os1 Os2 97.1(5) . . ? N41 Os1 Os2 83.1(3) . . ? Os3 Os1 Os2 58.57(2) . . ? C13' Os1' C12' 92.1(8) . . ? C13' Os1' C11' 92.5(8) . . ? C12' Os1' C11' 94.2(8) . . ? C13' Os1' N41' 173.3(7) . . ? C12' Os1' N41' 92.9(6) . . ? C11' Os1' N41' 91.6(6) . . ? C13' Os1' Os3' 91.7(6) . . ? C12' Os1' Os3' 95.1(6) . . ? C11' Os1' Os3' 169.7(5) . . ? N41' Os1' Os3' 83.4(3) . . ? C13' Os1' Os2' 89.2(6) . . ? C12' Os1' Os2' 153.3(6) . . ? C11' Os1' Os2' 112.4(5) . . ? N41' Os1' Os2' 84.3(3) . . ? Os3' Os1' Os2' 58.21(2) . . ? C23 Os2 C21 94.2(9) . . ? C23 Os2 C22 89.7(8) . . ? C21 Os2 C22 94.0(8) . . ? C23 Os2 C34 84.0(9) . . ? C21 Os2 C34 176.6(7) . . ? C22 Os2 C34 88.9(8) . . ? C23 Os2 C47 103.7(7) . . ? C21 Os2 C47 92.3(6) . . ? C22 Os2 C47 164.7(7) . . ? C34 Os2 C47 85.4(6) . . ? C23 Os2 Os3 123.4(6) . . ? C21 Os2 Os3 131.4(5) . . ? C22 Os2 Os3 113.7(6) . . ? C34 Os2 Os3 48.4(6) . . ? C47 Os2 Os3 52.7(4) . . ? C23 Os2 Os1 175.9(7) . . ? C21 Os2 Os1 81.7(6) . . ? C22 Os2 Os1 90.1(5) . . ? C34 Os2 Os1 100.1(6) . . ? C47 Os2 Os1 77.0(4) . . ? Os3 Os2 Os1 60.27(2) . . ? C23' Os2' C22' 91.6(8) . . ? C23' Os2' C21' 91.2(8) . . ? C22' Os2' C21' 91.0(7) . . ? C23' Os2' C34' 91.9(8) . . ? C22' Os2' C34' 89.2(7) . . ? C21' Os2' C34' 176.8(7) . . ? C23' Os2' C47' 101.5(7) . . ? C22' Os2' C47' 165.5(7) . . ? C21' Os2' C47' 94.9(6) . . ? C34' Os2' C47' 84.1(6) . . ? C23' Os2' Os3' 136.1(6) . . ? C22' Os2' Os3' 115.1(6) . . ? C21' Os2' Os3' 120.6(5) . . ? C34' Os2' Os3' 56.6(5) . . ? C47' Os2' Os3' 50.6(4) . . ? C23' Os2' Os1' 155.9(6) . . ? C22' Os2' Os1' 94.3(5) . . ? C21' Os2' Os1' 65.4(5) . . ? C34' Os2' Os1' 111.4(5) . . ? C47' Os2' Os1' 76.2(4) . . ? Os3' Os2' Os1' 60.52(2) . . ? C31 Os3 C33 98.2(8) . . ? C31 Os3 C32 92.0(10) . . ? C33 Os3 C32 94.4(9) . . ? C31 Os3 C34 175.5(8) . . ? C33 Os3 C34 86.3(8) . . ? C32 Os3 C34 87.7(9) . . ? C31 Os3 C47 93.4(7) . . ? C33 Os3 C47 94.0(7) . . ? C32 Os3 C47 169.2(8) . . ? C34 Os3 C47 86.2(7) . . ? C31 Os3 Os2 125.8(6) . . ? C33 Os3 Os2 120.8(6) . . ? C32 Os3 Os2 118.1(7) . . ? C34 Os3 Os2 50.8(6) . . ? C47 Os3 Os2 51.4(3) . . ? C31 Os3 Os1 72.6(6) . . ? C33 Os3 Os1 166.4(6) . . ? C32 Os3 Os1 95.9(7) . . ? C34 Os3 Os1 102.9(6) . . ? C47 Os3 Os1 76.9(3) . . ? Os2 Os3 Os1 61.16(2) . . ? C31' Os3' C33' 93.9(8) . . ? C31' Os3' C32' 92.4(8) . . ? C33' Os3' C32' 96.8(8) . . ? C31' Os3' C47' 97.5(7) . . ? C33' Os3' C47' 94.9(7) . . ? C32' Os3' C47' 164.1(7) . . ? C31' Os3' C34' 170.9(7) . . ? C33' Os3' C34' 79.2(7) . . ? C32' Os3' C34' 94.2(7) . . ? C47' Os3' C34' 77.5(6) . . ? C31' Os3' Os2' 135.9(6) . . ? C33' Os3' Os2' 116.7(6) . . ? C32' Os3' Os2' 113.0(6) . . ? C47' Os3' Os2' 51.6(4) . . ? C34' Os3' Os2' 45.8(5) . . ? C31' Os3' Os1' 83.5(5) . . ? C33' Os3' Os1' 171.2(6) . . ? C32' Os3' Os1' 91.7(6) . . ? C47' Os3' Os1' 77.1(4) . . ? C34' Os3' Os1' 102.5(4) . . ? Os2' Os3' Os1' 61.27(2) . . ? O11 C11 Os1 176.6(16) . . ? O11' C11' Os1' 179.1(16) . . ? O12 C12 Os1 178.9(15) . . ? O12' C12' Os1' 177.6(18) . . ? O13 C13 Os1 178.5(16) . . ? O13' C13' Os1' 179.1(16) . . ? O21 C21 Os2 175.0(17) . . ? O21' C21' Os2' 163.5(15) . . ? O22 C22 Os2 176.8(17) . . ? O22' C22' Os2' 174.1(16) . . ? O23 C23 Os2 172.2(18) . . ? O23' C23' Os2' 173.7(18) . . ? O31 C31 Os3 170.2(17) . . ? O31' C31' Os3' 173.9(16) . . ? O32 C32 Os3 178.5(22) . . ? O32' C32' Os3' 176.8(17) . . ? O33 C33 Os3 174.6(18) . . ? O33' C33' Os3' 178.2(19) . . ? O34 C34 Os3 144.0(19) . . ? O34 C34 Os2 134.6(19) . . ? Os3 C34 Os2 80.8(8) . . ? O34' C34' Os2' 150.2(16) . . ? O34' C34' Os3' 132.2(15) . . ? Os2' C34' Os3' 77.6(6) . . ? C42 N41 C46 121.0(12) . . ? C42 N41 Os1 120.5(9) . . ? C46 N41 Os1 118.4(9) . . ? C42' N41' C46' 119.7(13) . . ? C42' N41' Os1' 120.6(10) . . ? C46' N41' Os1' 119.7(10) . . ? N41 C42 C43 122.7(14) . . ? N41' C42' C43' 121.3(15) . . ? C42 C43 C44 118.5(15) . . ? C42' C43' C44' 120.6(17) . . ? C45 C44 C43 118.9(16) . . ? C43' C44' C45' 119.2(16) . . ? C44 C45 C46 120.9(15) . . ? C44' C45' C46' 118.4(15) . . ? N41 C46 C45 117.9(13) . . ? N41 C46 C47 119.8(13) . . ? C45 C46 C47 122.2(13) . . ? N41' C46' C45' 120.4(14) . . ? N41' C46' C47' 116.6(13) . . ? C45' C46' C47' 123.0(13) . . ? C46 C47 C48 113.4(12) . . ? C46 C47 Os2 113.1(9) . . ? C48 C47 Os2 120.7(10) . . ? C46 C47 Os3 116.4(10) . . ? C48 C47 Os3 112.5(10) . . ? Os2 C47 Os3 75.9(4) . . ? C46' C47' C48' 112.3(12) . . ? C46' C47' Os3' 117.5(10) . . ? C48' C47' Os3' 113.0(10) . . ? C46' C47' Os2' 114.1(9) . . ? C48' C47' Os2' 118.3(10) . . ? Os3' C47' Os2' 77.8(5) . . ? C49 C48 N56 105.5(13) . . ? C49 C48 C47 133.7(14) . . ? N56 C48 C47 120.8(13) . . ? C49' C48' N56' 105.9(12) . . ? C49' C48' C47' 132.1(14) . . ? N56' C48' C47' 121.8(12) . . ? C48 C49 C50 108.6(17) . . ? C48' C49' C50' 110.3(14) . . ? C51 C50 C49 109.7(16) . . ? C51' C50' C49' 105.7(14) . . ? C50 C51 N56 106.3(15) . . ? C50 C51 C52 135.4(19) . . ? N56 C51 C52 118.3(19) . . ? C50' C51' N56' 107.5(13) . . ? C50' C51' C52' 133.0(15) . . ? N56' C51' C52' 119.4(15) . . ? C53 C52 C51 120.8(19) . . ? C53' C52' C51' 121.6(16) . . ? C52 C53 C54 119.3(18) . . ? C52' C53' C54' 117.3(17) . . ? C55 C54 C53 120.1(20) . . ? C55' C54' C53' 123.0(18) . . ? C54 C55 N56 121.7(17) . . ? C54' C55' N56' 119.2(16) . . ? C55 N56 C51 119.7(14) . . ? C55 N56 C48 130.4(13) . . ? C51 N56 C48 109.9(14) . . ? C48' N56' C51' 110.5(13) . . ? C48' N56' C55' 130.1(13) . . ? C51' N56' C55' 119.3(13) . . ? _refine_diff_density_max 1.315 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.216 data_pr9615 _database_code_depnum_ccdc_archive 'CCDC 248099' _audit_creation_method SHELXL _chemical_name_systematic ; 'Compound 3' ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H10 N2 O9 Os3' _chemical_formula_weight 1028.93 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.250(5) _cell_length_b 14.515(4) _cell_length_c 8.843(2) _cell_angle_alpha 107.27(2) _cell_angle_beta 102.64(4) _cell_angle_gamma 85.36(3) _cell_volume 1225.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.788 _exptl_crystal_density_method ? _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 15.567 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.171 _exptl_absorpt_correction_T_max 0.288 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5R four-circle diffractometer' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 7473 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0986 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5621 _reflns_number_observed 3738 _reflns_observed_criterion I>2\s(I) _computing_data_collection 'Rigaku AFC5R diffractometer control software' _computing_cell_refinement 'Rigaku AFC5R diffractometer control software' _computing_data_reduction 'Rigaku AFC5R diffractometer control software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. Bridging hydride atom located with program HYDEX (A. G. Orpen, J. Chem. Soc., Dalton Trans., 1980, 2509. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w==1/[\s^2^(Fo^2^)+(0.0408P)^2^+1.3110P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5617 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_obs 0.0406 _refine_ls_wR_factor_all 0.1068 _refine_ls_wR_factor_obs 0.0891 _refine_ls_goodness_of_fit_all 1.012 _refine_ls_goodness_of_fit_obs 1.056 _refine_ls_restrained_S_all 1.017 _refine_ls_restrained_S_obs 1.056 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Os1 Os 0.17751(5) 0.28167(3) 0.29713(5) 0.02926(12) Uani 1 d . . Os2 Os 0.30736(5) 0.18066(3) 0.52047(5) 0.02820(12) Uani 1 d . . Os3 Os 0.30935(5) 0.38409(3) 0.63464(5) 0.02841(12) Uani 1 d . . O11 O 0.1418(11) 0.3991(7) 0.0554(11) 0.059(3) Uani 1 d . . C11 C 0.1567(12) 0.3555(8) 0.1494(14) 0.033(3) Uani 1 d . . O12 O 0.0528(12) 0.1095(7) 0.0293(13) 0.076(4) Uani 1 d . . C12 C 0.1006(14) 0.1738(9) 0.1319(15) 0.043(3) Uani 1 d . . C13 C 0.0008(14) 0.3130(8) 0.3589(15) 0.039(3) Uani 1 d . . O13 O -0.0991(11) 0.3268(8) 0.3897(13) 0.067(3) Uani 1 d . . O21 O 0.2006(14) -0.0057(7) 0.2672(13) 0.086(4) Uani 1 d . . C21 C 0.2383(16) 0.0646(10) 0.3625(16) 0.050(4) Uani 1 d . . O22 O 0.0818(13) 0.2077(9) 0.7023(16) 0.091(4) Uani 1 d . . C22 C 0.1648(15) 0.1982(9) 0.6336(19) 0.052(4) Uani 1 d . . O23 O 0.4815(12) 0.0576(7) 0.7166(13) 0.073(3) Uani 1 d . . C23 C 0.4224(13) 0.1089(9) 0.6506(14) 0.040(3) Uani 1 d . . C31 C 0.3711(12) 0.4000(8) 0.8647(15) 0.035(3) Uani 1 d . . O31 O 0.4062(11) 0.4148(8) 0.9989(10) 0.067(3) Uani 1 d . . C32 C 0.1370(14) 0.4395(9) 0.6782(14) 0.043(3) Uani 1 d . . O32 O 0.0354(10) 0.4724(7) 0.7023(13) 0.063(3) Uani 1 d . . C33 C 0.3801(14) 0.5047(9) 0.6536(14) 0.040(3) Uani 1 d . . O33 O 0.4276(12) 0.5747(7) 0.6603(12) 0.067(3) Uani 1 d . . N41 N 0.5946(12) 0.2624(8) 0.8325(13) 0.048(3) Uiso 1 d . . C42 C 0.7003(16) 0.2802(11) 0.9525(16) 0.059(4) Uani 1 d . . H42 H 0.7012(16) 0.2574(11) 1.0406(16) 0.071 Uiso 1 calc R . C43 C 0.8089(16) 0.3304(11) 0.9544(18) 0.062(4) Uani 1 d . . H43 H 0.8827(16) 0.3376(11) 1.0394(18) 0.075 Uiso 1 calc R . C44 C 0.8092(15) 0.3693(11) 0.8331(17) 0.057(4) Uani 1 d . . H44 H 0.8815(15) 0.4043(11) 0.8335(17) 0.068 Uiso 1 calc R . C45 C 0.6971(14) 0.3552(10) 0.7077(16) 0.047(3) Uani 1 d . . H45 H 0.6918(14) 0.3822(10) 0.6234(16) 0.056 Uiso 1 calc R . C46 C 0.5924(11) 0.2997(7) 0.7100(12) 0.028(2) Uani 1 d . . C47 C 0.4689(10) 0.2874(7) 0.5795(12) 0.024(2) Uani 1 d . . C48 C 0.4706(10) 0.2281(8) 0.4171(12) 0.027(2) Uani 1 d . . C49 C 0.3684(12) 0.2267(7) 0.2738(13) 0.033(3) Uani 1 d . . C50 C 0.4223(13) 0.1738(9) 0.1446(13) 0.041(3) Uani 1 d . . H50 H 0.3785(13) 0.1619(9) 0.0370(13) 0.050 Uiso 1 calc R . C51 C 0.5519(13) 0.1402(8) 0.1956(13) 0.036(3) Uani 1 d . . C52 C 0.6518(14) 0.0851(10) 0.1183(16) 0.050(4) Uani 1 d . . H52 H 0.6368(14) 0.0641(10) 0.0059(16) 0.060 Uiso 1 calc R . C53 C 0.7687(16) 0.0628(11) 0.2062(18) 0.060(4) Uani 1 d . . H53 H 0.8348(16) 0.0287(11) 0.1540(18) 0.072 Uiso 1 calc R . C54 C 0.7912(14) 0.0908(9) 0.3762(16) 0.049(4) Uani 1 d . . H54 H 0.8705(14) 0.0730(9) 0.4358(16) 0.059 Uiso 1 calc R . C55 C 0.6983(13) 0.1429(8) 0.4522(14) 0.040(3) Uani 1 d . . H55 H 0.7129(13) 0.1606(8) 0.5645(14) 0.048 Uiso 1 calc R . N56 N 0.5821(10) 0.1704(6) 0.3658(10) 0.031(2) Uiso 1 d . . H1 H 0.2519 0.3971 0.4286 0.080 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 Os1 0.0254(3) 0.0314(2) 0.0278(2) 0.0080(2) 0.0000(2) 0.0016(2) Os2 0.0270(3) 0.0281(2) 0.0285(2) 0.0089(2) 0.0016(2) -0.0027(2) Os3 0.0275(3) 0.0284(2) 0.0267(2) 0.0045(2) 0.0052(2) 0.0004(2) O11 0.058(7) 0.078(7) 0.055(6) 0.038(5) 0.017(5) 0.009(6) C11 0.023(6) 0.041(7) 0.038(6) 0.015(5) 0.006(5) -0.001(5) O12 0.078(9) 0.048(6) 0.072(7) -0.010(5) -0.008(6) 0.002(6) C12 0.041(8) 0.046(8) 0.039(7) 0.014(6) 0.001(6) 0.007(6) C13 0.039(8) 0.027(6) 0.049(7) 0.009(5) 0.005(6) -0.003(6) O13 0.033(6) 0.085(8) 0.083(8) 0.019(6) 0.019(6) 0.003(6) O21 0.124(12) 0.038(6) 0.074(7) 0.007(5) -0.020(7) -0.018(7) C21 0.062(10) 0.041(8) 0.047(8) 0.023(6) -0.004(7) -0.001(7) O22 0.085(10) 0.090(9) 0.117(10) 0.021(8) 0.074(9) 0.004(7) C22 0.043(9) 0.037(7) 0.084(11) 0.016(7) 0.031(8) -0.001(6) O23 0.071(8) 0.067(7) 0.079(7) 0.044(6) -0.019(6) -0.004(6) C23 0.024(7) 0.053(8) 0.043(7) 0.020(6) -0.004(5) -0.013(6) C31 0.022(6) 0.036(6) 0.051(8) 0.013(5) 0.014(5) 0.003(5) O31 0.074(8) 0.109(9) 0.018(4) 0.017(5) 0.006(5) -0.008(7) C32 0.042(9) 0.048(8) 0.033(6) 0.005(5) 0.009(6) 0.003(6) O32 0.040(6) 0.065(7) 0.082(7) 0.010(5) 0.029(5) 0.020(5) C33 0.046(9) 0.039(7) 0.033(6) 0.007(5) 0.005(6) -0.011(6) O33 0.085(9) 0.052(6) 0.059(6) 0.012(5) -0.002(6) -0.030(6) C42 0.058(11) 0.076(10) 0.043(8) 0.033(7) -0.016(7) -0.011(8) C43 0.040(9) 0.075(11) 0.064(9) 0.023(8) -0.015(7) -0.020(8) C44 0.033(8) 0.069(10) 0.069(10) 0.027(8) -0.005(7) -0.009(7) C45 0.039(8) 0.054(8) 0.049(8) 0.020(6) 0.004(6) -0.009(7) C46 0.012(5) 0.030(6) 0.036(6) 0.010(5) -0.007(4) 0.000(4) C47 0.013(5) 0.028(5) 0.032(5) 0.008(4) 0.005(4) -0.002(4) C48 0.015(6) 0.041(6) 0.024(5) 0.009(5) 0.008(4) 0.011(5) C49 0.034(7) 0.023(5) 0.032(6) 0.001(4) -0.002(5) -0.001(5) C50 0.034(8) 0.057(8) 0.027(6) 0.011(5) -0.003(5) 0.008(6) C51 0.042(8) 0.039(7) 0.032(6) 0.009(5) 0.018(5) -0.003(6) C52 0.041(9) 0.060(9) 0.047(7) 0.008(7) 0.018(7) 0.015(7) C53 0.053(10) 0.063(10) 0.067(10) 0.014(8) 0.031(8) 0.013(8) C54 0.043(9) 0.038(7) 0.060(8) 0.009(6) 0.007(7) 0.015(6) C55 0.036(8) 0.040(7) 0.036(6) 0.006(5) -0.001(5) 0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C12 1.883(13) . ? Os1 C11 1.890(12) . ? Os1 C13 1.984(14) . ? Os1 C49 2.082(12) . ? Os1 Os2 2.8417(11) . ? Os1 Os3 2.9782(14) . ? Os2 C22 1.905(14) . ? Os2 C21 1.911(14) . ? Os2 C23 1.929(13) . ? Os2 C47 2.229(10) . ? Os2 C48 2.311(11) . ? Os2 Os3 2.8229(10) . ? Os3 C33 1.897(13) . ? Os3 C31 1.943(12) . ? Os3 C32 1.949(14) . ? Os3 C47 2.110(10) . ? O11 C11 1.164(13) . ? O12 C12 1.145(15) . ? C13 O13 1.10(2) . ? O21 C21 1.15(2) . ? O22 C22 1.13(2) . ? O23 C23 1.136(14) . ? C31 O31 1.122(13) . ? C32 O32 1.146(15) . ? C33 O33 1.142(15) . ? N41 C42 1.32(2) . ? N41 C46 1.342(15) . ? C42 C43 1.37(2) . ? C43 C44 1.35(2) . ? C44 C45 1.39(2) . ? C45 C46 1.40(2) . ? C46 C47 1.497(14) . ? C47 C48 1.442(14) . ? C48 N56 1.435(13) . ? C48 C49 1.453(14) . ? C49 C50 1.37(2) . ? C50 C51 1.40(2) . ? C51 N56 1.407(13) . ? C51 C52 1.42(2) . ? C52 C53 1.35(2) . ? C53 C54 1.41(2) . ? C54 C55 1.34(2) . ? C55 N56 1.366(14) . ? 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 C12 Os1 C11 91.2(5) . . ? C12 Os1 C13 88.7(5) . . ? C11 Os1 C13 97.6(5) . . ? C12 Os1 C49 90.6(5) . . ? C11 Os1 C49 97.5(5) . . ? C13 Os1 C49 164.9(5) . . ? C12 Os1 Os2 97.1(4) . . ? C11 Os1 Os2 159.1(4) . . ? C13 Os1 Os2 101.6(4) . . ? C49 Os1 Os2 63.5(3) . . ? C12 Os1 Os3 154.0(4) . . ? C11 Os1 Os3 114.7(4) . . ? C13 Os1 Os3 89.3(4) . . ? C49 Os1 Os3 84.7(3) . . ? Os2 Os1 Os3 57.97(3) . . ? C22 Os2 C21 94.6(6) . . ? C22 Os2 C23 95.6(6) . . ? C21 Os2 C23 91.7(5) . . ? C22 Os2 C47 123.5(5) . . ? C21 Os2 C47 141.5(5) . . ? C23 Os2 C47 89.6(5) . . ? C22 Os2 C48 156.1(5) . . ? C21 Os2 C48 104.9(5) . . ? C23 Os2 C48 97.4(5) . . ? C47 Os2 C48 37.0(4) . . ? C22 Os2 Os3 82.0(4) . . ? C21 Os2 Os3 150.1(4) . . ? C23 Os2 Os3 118.2(4) . . ? C47 Os2 Os3 47.6(3) . . ? C48 Os2 Os3 74.2(3) . . ? C22 Os2 Os1 95.1(5) . . ? C21 Os2 Os1 87.5(4) . . ? C23 Os2 Os1 169.3(4) . . ? C47 Os2 Os1 84.4(3) . . ? C48 Os2 Os1 72.5(2) . . ? Os3 Os2 Os1 63.44(3) . . ? C33 Os3 C31 91.7(5) . . ? C33 Os3 C32 93.8(6) . . ? C31 Os3 C32 88.8(5) . . ? C33 Os3 C47 102.4(5) . . ? C31 Os3 C47 91.4(4) . . ? C32 Os3 C47 163.7(5) . . ? C33 Os3 Os2 151.3(4) . . ? C31 Os3 Os2 99.4(3) . . ? C32 Os3 Os2 112.6(4) . . ? C47 Os3 Os2 51.3(3) . . ? C33 Os3 Os1 113.1(3) . . ? C31 Os3 Os1 155.3(4) . . ? C32 Os3 Os1 89.9(4) . . ? C47 Os3 Os1 83.1(3) . . ? Os2 Os3 Os1 58.59(3) . . ? O11 C11 Os1 178.3(11) . . ? O12 C12 Os1 178.5(12) . . ? O13 C13 Os1 177.2(12) . . ? O21 C21 Os2 178.0(15) . . ? O22 C22 Os2 178.7(15) . . ? O23 C23 Os2 172.1(11) . . ? O31 C31 Os3 176.0(11) . . ? O32 C32 Os3 179.3(11) . . ? O33 C33 Os3 176.3(13) . . ? C42 N41 C46 117.3(12) . . ? N41 C42 C43 123.6(14) . . ? C44 C43 C42 120.3(14) . . ? C43 C44 C45 117.5(15) . . ? C44 C45 C46 119.1(13) . . ? N41 C46 C45 122.0(11) . . ? N41 C46 C47 118.2(11) . . ? C45 C46 C47 119.6(10) . . ? C48 C47 C46 121.0(9) . . ? C48 C47 Os3 122.1(7) . . ? C46 C47 Os3 115.6(7) . . ? C48 C47 Os2 74.6(6) . . ? C46 C47 Os2 127.6(8) . . ? Os3 C47 Os2 81.1(4) . . ? N56 C48 C47 125.4(9) . . ? N56 C48 C49 107.9(8) . . ? C47 C48 C49 126.1(9) . . ? N56 C48 Os2 126.2(7) . . ? C47 C48 Os2 68.4(6) . . ? C49 C48 Os2 87.2(7) . . ? C50 C49 C48 105.8(10) . . ? C50 C49 Os1 133.5(9) . . ? C48 C49 Os1 120.0(8) . . ? C49 C50 C51 111.4(10) . . ? C50 C51 N56 107.7(10) . . ? C50 C51 C52 135.7(11) . . ? N56 C51 C52 116.6(11) . . ? C53 C52 C51 120.6(13) . . ? C52 C53 C54 120.5(13) . . ? C55 C54 C53 120.0(13) . . ? C54 C55 N56 120.5(11) . . ? C55 N56 C51 121.7(10) . . ? C55 N56 C48 131.3(9) . . ? C51 N56 C48 107.0(9) . . ? _refine_diff_density_max 1.214 _refine_diff_density_min -1.867 _refine_diff_density_rms 0.295 data_pr9707 _database_code_depnum_ccdc_archive 'CCDC 248100' _audit_creation_method SHELXL _chemical_name_systematic ; 'Compound 6 . 2 dichloromethane' ; _chemical_name_common ? _chemical_formula_moiety 'C34 H8 N2 O20 Os6, 2(C H2 Cl2)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H12 Cl4 N2 O20 Os6' _chemical_formula_weight 2075.48 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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 11.258(2) _cell_length_b 12.994(3) _cell_length_c 8.381(2) _cell_angle_alpha 104.69(3) _cell_angle_beta 103.26(3) _cell_angle_gamma 85.71(3) _cell_volume 1154.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.986 _exptl_crystal_density_method ? _exptl_crystal_F_000 926 _exptl_absorpt_coefficient_mu 16.759 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.026 _exptl_absorpt_correction_T_max 0.040 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5R four-circle diffractometer' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.3 _diffrn_reflns_number 7402 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5297 _reflns_number_observed 3942 _reflns_observed_criterion I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXTL-PLUS (Siemens, 1991)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS (Siemens, 1991)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0407P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5291 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_obs 0.0379 _refine_ls_wR_factor_all 0.1484 _refine_ls_wR_factor_obs 0.0882 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.077 _refine_ls_restrained_S_all 1.549 _refine_ls_restrained_S_obs 1.077 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Os1 Os 0.28836(4) 0.17766(3) -0.15713(5) 0.01483(10) Uani 1 d . . Os2 Os 0.28744(4) 0.36622(3) 0.09769(5) 0.01413(10) Uani 1 d . . Os3 Os 0.21900(4) 0.37492(3) -0.23597(5) 0.01479(10) Uani 1 d . . N1 N 0.0987(8) 0.1704(7) -0.1491(11) 0.017(2) Uani 1 d . . C1 C 0.2694(10) 0.0909(10) -0.3823(14) 0.022(2) Uani 1 d . . O1 O 0.2621(8) 0.0397(7) -0.5156(11) 0.034(2) Uani 1 d . . O2 O 0.3567(8) -0.0067(7) 0.0141(11) 0.032(2) Uani 1 d . . C2 C 0.3313(10) 0.0620(9) -0.0508(14) 0.020(2) Uani 1 d . . O3 O 0.5536(7) 0.2138(7) -0.1495(11) 0.031(2) Uani 1 d . . C3 C 0.4540(11) 0.2015(8) -0.1493(14) 0.022(2) Uani 1 d . . O4 O 0.2359(8) 0.1880(7) 0.2514(10) 0.029(2) Uani 1 d . . C4 C 0.2583(9) 0.2511(9) 0.1891(14) 0.018(2) Uani 1 d . . O5 O 0.5604(7) 0.3673(8) 0.2681(12) 0.037(2) Uani 1 d . . C5 C 0.4600(11) 0.3643(9) 0.2006(14) 0.023(2) Uani 1 d . . C6 C 0.2457(11) 0.4767(9) 0.2726(13) 0.024(2) Uani 1 d . . O6 O 0.2170(9) 0.5446(8) 0.3774(12) 0.045(3) Uani 1 d . . C7 C 0.3219(10) 0.4849(9) -0.0156(13) 0.022(2) Uani 1 d . . O7 O 0.3711(9) 0.5653(7) 0.0160(11) 0.037(2) Uani 1 d . . O8 O 0.4304(7) 0.3764(7) -0.4114(11) 0.033(2) Uani 1 d . . C8 C 0.3519(10) 0.3767(9) -0.3490(14) 0.023(2) Uani 1 d . . C9 C 0.1366(10) 0.5007(10) -0.2904(15) 0.026(3) Uani 1 d . . O9 O 0.0820(9) 0.5728(8) -0.3253(12) 0.042(2) Uani 1 d . . O10 O 0.0581(7) 0.2278(7) -0.5358(11) 0.033(2) Uani 1 d . . C10 C 0.1210(10) 0.2805(9) -0.4222(13) 0.020(2) Uani 1 d . . C11 C 0.0431(10) 0.0785(9) -0.1818(15) 0.024(2) Uani 1 d . . H11 H 0.0849(10) 0.0146(9) -0.2235(15) 0.029 Uiso 1 calc R . C12 C -0.0724(10) 0.0722(9) -0.1578(14) 0.024(2) Uani 1 d . . H12 H -0.1071(10) 0.0045(9) -0.1764(14) 0.028 Uiso 1 calc R . C13 C -0.1394(11) 0.1646(11) -0.1061(16) 0.033(3) Uani 1 d . . H13 H -0.2205(11) 0.1616(11) -0.0926(16) 0.040 Uiso 1 calc R . C14 C -0.0834(10) 0.2597(9) -0.0758(15) 0.025(2) Uani 1 d . . H14 H -0.1264(10) 0.3238(9) -0.0388(15) 0.030 Uiso 1 calc R . C15 C 0.0366(9) 0.2655(8) -0.0978(13) 0.016(2) Uani 1 d . . C16 C 0.1013(9) 0.3652(8) -0.0646(12) 0.014(2) Uani 1 d . . C17 C 0.0274(9) 0.4597(8) -0.0195(13) 0.017(2) Uani 1 d . . C18 C -0.3423(12) 0.2002(11) -0.4995(18) 0.038(3) Uani 1 d . . H18A H -0.3123(12) 0.1736(11) -0.3964(18) 0.045 Uiso 1 calc R . H18B H -0.3642(12) 0.2765(11) -0.4639(18) 0.045 Uiso 1 calc R . Cl1 Cl -0.4722(3) 0.1304(3) -0.6212(5) 0.0430(8) Uani 1 d . . Cl2 Cl -0.2246(4) 0.1863(3) -0.6126(7) 0.0631(13) 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 0.0139(2) 0.0112(2) 0.0192(2) 0.00334(15) 0.00455(15) 0.00232(14) Os2 0.0161(2) 0.0133(2) 0.0139(2) 0.00392(14) 0.00460(14) 0.00087(15) Os3 0.0167(2) 0.0152(2) 0.0150(2) 0.00658(15) 0.00695(15) 0.00430(15) N1 0.014(4) 0.013(4) 0.023(5) 0.008(3) 0.003(3) 0.004(3) C1 0.021(6) 0.030(6) 0.018(5) 0.015(5) 0.000(4) 0.004(5) O1 0.049(6) 0.027(5) 0.026(5) 0.007(4) 0.008(4) -0.001(4) O2 0.043(5) 0.027(5) 0.029(5) 0.018(4) 0.005(4) 0.006(4) C2 0.018(5) 0.017(5) 0.023(5) -0.001(4) 0.007(4) 0.004(4) O3 0.018(4) 0.033(5) 0.043(5) 0.011(4) 0.010(4) 0.005(4) C3 0.031(6) 0.012(5) 0.020(5) -0.001(4) 0.006(5) -0.001(5) O4 0.045(5) 0.024(4) 0.029(4) 0.017(4) 0.015(4) -0.002(4) C4 0.007(5) 0.021(5) 0.030(6) 0.012(5) 0.003(4) 0.003(4) O5 0.017(4) 0.046(6) 0.047(6) 0.021(5) -0.003(4) -0.007(4) C5 0.038(7) 0.014(5) 0.025(6) 0.010(4) 0.019(5) -0.001(5) C6 0.035(6) 0.022(6) 0.016(5) 0.002(4) 0.009(5) -0.011(5) O6 0.055(6) 0.033(6) 0.037(5) -0.012(4) 0.018(5) 0.007(5) C7 0.030(6) 0.017(6) 0.017(5) 0.004(4) 0.003(4) -0.005(5) O7 0.056(6) 0.024(5) 0.035(5) 0.012(4) 0.007(4) -0.014(4) O8 0.023(4) 0.042(5) 0.044(5) 0.012(4) 0.025(4) 0.004(4) C8 0.027(6) 0.021(6) 0.024(6) 0.008(5) 0.009(5) 0.009(5) C9 0.026(6) 0.029(7) 0.032(6) 0.018(5) 0.017(5) 0.008(5) O9 0.046(6) 0.038(6) 0.050(6) 0.028(5) 0.016(5) 0.021(5) O10 0.025(4) 0.039(5) 0.029(5) 0.000(4) 0.001(4) -0.003(4) C10 0.031(6) 0.020(6) 0.015(5) 0.008(4) 0.010(4) 0.003(5) C11 0.017(5) 0.017(6) 0.034(6) 0.005(5) -0.001(5) 0.000(4) C12 0.024(6) 0.024(6) 0.021(6) 0.008(5) -0.006(4) -0.008(5) C13 0.019(6) 0.044(8) 0.041(7) 0.024(6) 0.001(5) -0.005(5) C14 0.024(6) 0.023(6) 0.032(6) 0.008(5) 0.011(5) -0.004(5) C15 0.016(5) 0.018(5) 0.015(5) 0.007(4) 0.004(4) 0.009(4) C16 0.014(5) 0.021(5) 0.012(5) 0.007(4) 0.012(4) 0.009(4) C17 0.016(5) 0.019(5) 0.014(5) 0.002(4) 0.006(4) 0.003(4) C18 0.029(7) 0.027(7) 0.047(8) -0.001(6) -0.002(6) -0.002(6) Cl1 0.029(2) 0.033(2) 0.059(2) 0.008(2) -0.0020(15) -0.0021(14) Cl2 0.043(2) 0.039(2) 0.113(4) 0.005(2) 0.042(2) 0.000(2) _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 C3 1.896(12) . ? Os1 C1 1.911(11) . ? Os1 C2 1.912(11) . ? Os1 N1 2.161(8) . ? Os1 Os2 2.8137(12) . ? Os1 Os3 2.8176(9) . ? Os2 C6 1.892(11) . ? Os2 C4 1.924(11) . ? Os2 C5 1.937(13) . ? Os2 C7 2.105(11) . ? Os2 C16 2.220(10) . ? Os2 Os3 2.7541(9) . ? Os3 C10 1.897(11) . ? Os3 C9 1.923(11) . ? Os3 C8 1.951(11) . ? Os3 C7 2.173(11) . ? Os3 C16 2.197(9) . ? N1 C11 1.328(14) . ? N1 C15 1.392(12) . ? C1 O1 1.134(13) . ? O2 C2 1.145(13) . ? O3 C3 1.145(13) . ? O4 C4 1.147(13) . ? O5 C5 1.141(14) . ? C6 O6 1.161(13) . ? C7 O7 1.160(13) . ? O8 C8 1.124(13) . ? C9 O9 1.145(14) . ? O10 C10 1.144(13) . ? C11 C12 1.37(2) . ? C12 C13 1.40(2) . ? C13 C14 1.37(2) . ? C14 C15 1.414(14) . ? C15 C16 1.467(14) . ? C16 C17 1.448(13) . ? C17 C17 1.19(2) 2_565 ? C18 Cl1 1.745(13) . ? C18 Cl2 1.772(14) . ? 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 C3 Os1 C1 90.9(5) . . ? C3 Os1 C2 92.2(5) . . ? C1 Os1 C2 95.0(5) . . ? C3 Os1 N1 173.0(4) . . ? C1 Os1 N1 94.6(4) . . ? C2 Os1 N1 91.6(4) . . ? C3 Os1 Os2 88.9(3) . . ? C1 Os1 Os2 156.9(3) . . ? C2 Os1 Os2 108.1(3) . . ? N1 Os1 Os2 84.3(2) . . ? C3 Os1 Os3 90.7(3) . . ? C1 Os1 Os3 98.4(3) . . ? C2 Os1 Os3 166.3(3) . . ? N1 Os1 Os3 84.3(2) . . ? Os2 Os1 Os3 58.56(2) . . ? C6 Os2 C4 96.0(5) . . ? C6 Os2 C5 95.3(5) . . ? C4 Os2 C5 91.5(4) . . ? C6 Os2 C7 87.6(4) . . ? C4 Os2 C7 176.4(4) . . ? C5 Os2 C7 88.3(4) . . ? C6 Os2 C16 92.7(4) . . ? C4 Os2 C16 94.6(4) . . ? C5 Os2 C16 169.3(4) . . ? C7 Os2 C16 85.0(4) . . ? C6 Os2 Os3 121.6(4) . . ? C4 Os2 Os3 126.2(3) . . ? C5 Os2 Os3 118.4(3) . . ? C7 Os2 Os3 51.0(3) . . ? C16 Os2 Os3 51.1(2) . . ? C6 Os2 Os1 163.8(3) . . ? C4 Os2 Os1 72.9(3) . . ? C5 Os2 Os1 96.8(3) . . ? C7 Os2 Os1 103.5(3) . . ? C16 Os2 Os1 76.8(2) . . ? Os3 Os2 Os1 60.79(3) . . ? C10 Os3 C9 94.1(5) . . ? C10 Os3 C8 95.1(5) . . ? C9 Os3 C8 95.9(4) . . ? C10 Os3 C7 176.6(4) . . ? C9 Os3 C7 84.9(5) . . ? C8 Os3 C7 88.2(4) . . ? C10 Os3 C16 92.9(4) . . ? C9 Os3 C16 93.1(4) . . ? C8 Os3 C16 167.5(4) . . ? C7 Os3 C16 84.0(4) . . ? C10 Os3 Os2 129.6(3) . . ? C9 Os3 Os2 119.0(3) . . ? C8 Os3 Os2 115.9(3) . . ? C7 Os3 Os2 48.9(3) . . ? C16 Os3 Os2 51.8(3) . . ? C10 Os3 Os1 78.9(3) . . ? C9 Os3 Os1 167.5(3) . . ? C8 Os3 Os1 95.0(3) . . ? C7 Os3 Os1 101.5(3) . . ? C16 Os3 Os1 77.1(3) . . ? Os2 Os3 Os1 60.65(3) . . ? C11 N1 C15 119.7(9) . . ? C11 N1 Os1 121.9(7) . . ? C15 N1 Os1 118.3(7) . . ? O1 C1 Os1 177.8(10) . . ? O2 C2 Os1 179.4(9) . . ? O3 C3 Os1 177.9(10) . . ? O4 C4 Os2 174.7(10) . . ? O5 C5 Os2 176.4(10) . . ? O6 C6 Os2 178.2(11) . . ? O7 C7 Os2 141.6(9) . . ? O7 C7 Os3 138.3(9) . . ? Os2 C7 Os3 80.1(4) . . ? O8 C8 Os3 178.2(10) . . ? O9 C9 Os3 176.5(11) . . ? O10 C10 Os3 176.5(10) . . ? N1 C11 C12 122.5(11) . . ? C11 C12 C13 120.4(11) . . ? C14 C13 C12 117.2(11) . . ? C13 C14 C15 122.0(11) . . ? N1 C15 C14 118.0(10) . . ? N1 C15 C16 117.9(8) . . ? C14 C15 C16 124.1(9) . . ? C17 C16 C15 113.8(8) . . ? C17 C16 Os3 114.7(7) . . ? C15 C16 Os3 117.4(7) . . ? C17 C16 Os2 115.2(7) . . ? C15 C16 Os2 113.9(7) . . ? Os3 C16 Os2 77.1(3) . . ? C17 C17 C16 176.4(15) 2_565 . ? Cl1 C18 Cl2 111.8(7) . . ? _refine_diff_density_max 1.918 _refine_diff_density_min -2.198 _refine_diff_density_rms 0.358 data_pr0016 _database_code_depnum_ccdc_archive 'CCDC 248101' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Compound 6' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H8 N2 O20 Os6' _chemical_formula_weight 1905.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7840(6) _cell_length_b 28.201(3) _cell_length_c 16.7970(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.085(5) _cell_angle_gamma 90.00 _cell_volume 4129.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 20039 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.065 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3368 _exptl_absorpt_coefficient_mu 18.472 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.565 _exptl_absorpt_correction_T_max 0.691 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24123 _diffrn_reflns_av_R_equivalents 0.0855 _diffrn_reflns_av_sigmaI/netI 0.1112 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12818 _reflns_number_gt 10371 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; "Collect" data collection software, Nonius' B.V., 1998. ; _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0433P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(16) _refine_ls_number_reflns 12818 _refine_ls_number_parameters 1117 _refine_ls_number_restraints 631 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os -0.46494(10) -0.02703(3) 0.44753(5) 0.0248(2) Uani 1 1 d . . . Os2 Os -0.26521(10) 0.02402(3) 0.36036(5) 0.0222(2) Uani 1 1 d . . . Os3 Os -0.56169(10) 0.05535(3) 0.36265(5) 0.0237(2) Uani 1 1 d . . . Os4 Os -0.12848(10) 0.32011(3) 0.37225(5) 0.0269(2) Uani 1 1 d . . . Os5 Os -0.31547(10) 0.26650(3) 0.46209(5) 0.0229(2) Uani 1 1 d . . . Os6 Os -0.01619(10) 0.23898(3) 0.45679(5) 0.0235(2) Uani 1 1 d . . . Os7 Os 0.63566(10) 0.82034(3) 0.12699(5) 0.0253(2) Uani 1 1 d . . . Os8 Os 0.56971(10) 0.72949(3) 0.18058(5) 0.0233(2) Uani 1 1 d . . . Os9 Os 0.87268(10) 0.75643(3) 0.17959(5) 0.0250(2) Uani 1 1 d . . . Os10 Os 0.91329(10) 0.46856(3) 0.05338(5) 0.0267(2) Uani 1 1 d . . . Os11 Os 0.98449(10) 0.55817(3) -0.00453(5) 0.0227(2) Uani 1 1 d . . . Os12 Os 0.68133(10) 0.53353(3) -0.00265(5) 0.0249(2) Uani 1 1 d . . . C1 C -0.635(3) -0.0463(10) 0.4990(15) 0.042(7) Uani 1 1 d U . . O1 O -0.7364(19) -0.0556(6) 0.5326(11) 0.047(5) Uani 1 1 d U . . C2 C -0.351(3) -0.0781(9) 0.4945(15) 0.041(7) Uani 1 1 d U . . O2 O -0.287(2) -0.1105(7) 0.5233(12) 0.062(6) Uani 1 1 d U . . C3 C -0.542(2) -0.0599(8) 0.3513(13) 0.027(5) Uani 1 1 d U . . O3 O -0.582(2) -0.0815(5) 0.2945(10) 0.042(4) Uani 1 1 d U . . C4 C -0.138(2) -0.0038(8) 0.4491(13) 0.026(5) Uani 1 1 d U . . O4 O -0.0507(19) -0.0189(7) 0.4985(11) 0.056(5) Uani 1 1 d U . . C5 C -0.116(3) 0.0653(8) 0.3282(14) 0.034(6) Uani 1 1 d U . . O5 O -0.0173(19) 0.0905(6) 0.3099(10) 0.043(4) Uani 1 1 d U . . C6 C -0.230(3) -0.0275(9) 0.2908(13) 0.032(5) Uani 1 1 d U . . O6 O -0.204(2) -0.0592(6) 0.2506(10) 0.042(4) Uani 1 1 d U . . C7 C -0.624(3) 0.1193(9) 0.3313(14) 0.035(5) Uani 1 1 d U . . O7 O -0.650(3) 0.1575(6) 0.3123(13) 0.071(6) Uani 1 1 d U . . C8 C -0.679(3) 0.0534(8) 0.4505(13) 0.030(6) Uani 1 1 d U . . O8 O -0.756(2) 0.0550(7) 0.5009(11) 0.061(6) Uani 1 1 d U . . C9 C -0.719(3) 0.0255(8) 0.2918(13) 0.030(5) Uani 1 1 d U . . O9 O -0.816(2) 0.0072(6) 0.2510(11) 0.051(5) Uani 1 1 d U . . C10 C -0.415(2) 0.0569(8) 0.2691(13) 0.025(5) Uani 1 1 d U . . O10 O -0.4230(17) 0.0706(6) 0.2030(10) 0.036(4) Uani 1 1 d U . . C11 C 0.036(3) 0.3437(8) 0.3192(13) 0.031(5) Uani 1 1 d U . . O11 O 0.133(2) 0.3595(7) 0.2868(11) 0.057(5) Uani 1 1 d U . . C12 C -0.271(3) 0.3674(9) 0.3271(15) 0.040(6) Uani 1 1 d U . . O12 O -0.351(2) 0.3968(8) 0.3019(12) 0.076(7) Uani 1 1 d U . . C13 C -0.065(2) 0.3540(7) 0.4666(13) 0.024(5) Uani 1 1 d U . . O13 O -0.0236(18) 0.3738(6) 0.5274(9) 0.036(4) Uani 1 1 d U . . C14 C -0.452(3) 0.2909(9) 0.3836(13) 0.034(5) Uani 1 1 d U . . O14 O -0.555(2) 0.3056(8) 0.3326(12) 0.065(6) Uani 1 1 d U . . C15 C -0.461(2) 0.2223(9) 0.5030(15) 0.034(6) Uani 1 1 d U . . O15 O -0.549(2) 0.1978(7) 0.5206(12) 0.058(5) Uani 1 1 d U . . C16 C -0.347(2) 0.3186(8) 0.5352(13) 0.027(5) Uani 1 1 d U . . O16 O -0.363(2) 0.3490(6) 0.5775(10) 0.047(5) Uani 1 1 d U . . C17 C 0.096(3) 0.2428(8) 0.3670(16) 0.039(6) Uani 1 1 d U . . O17 O 0.158(2) 0.2414(7) 0.3098(12) 0.063(6) Uani 1 1 d U . . C18 C 0.049(3) 0.1739(10) 0.4888(17) 0.045(7) Uani 1 1 d U . . O18 O 0.088(2) 0.1380(6) 0.5050(12) 0.063(6) Uani 1 1 d U . . C19 C 0.146(3) 0.2712(9) 0.5221(16) 0.043(7) Uani 1 1 d U . . O19 O 0.2476(19) 0.2898(6) 0.5629(11) 0.045(5) Uani 1 1 d U . . C20 C -0.151(2) 0.2345(7) 0.5517(12) 0.023(5) Uani 1 1 d U . . O20 O -0.1435(17) 0.2203(6) 0.6196(9) 0.038(4) Uani 1 1 d U . . N1 N -0.3828(18) 0.0207(7) 0.5431(10) 0.026(4) Uani 1 1 d DU . . C21 C -0.385(2) 0.0091(9) 0.6210(13) 0.037(5) Uani 1 1 d DU . . H21 H -0.4172 -0.0219 0.6332 0.044 Uiso 1 1 calc R . . C22 C -0.343(2) 0.0392(10) 0.6824(14) 0.044(5) Uani 1 1 d DU . . H22 H -0.3499 0.0303 0.7364 0.052 Uiso 1 1 calc R . . C23 C -0.289(3) 0.0838(10) 0.6634(13) 0.038(5) Uani 1 1 d DU . . H23 H -0.2465 0.1041 0.7056 0.046 Uiso 1 1 calc R . . C24 C -0.295(2) 0.0998(10) 0.5823(13) 0.036(5) Uani 1 1 d DU . . H24 H -0.2706 0.1316 0.5699 0.043 Uiso 1 1 calc R . . C25 C -0.337(2) 0.0671(8) 0.5235(13) 0.026(4) Uani 1 1 d DU . . C26 C -0.350(2) 0.0794(7) 0.4371(11) 0.019(4) Uani 1 1 d U . . C27 C -0.301(2) 0.1268(8) 0.4205(12) 0.022(4) Uani 1 1 d U . . C28 C -0.274(2) 0.1655(8) 0.4009(13) 0.027(5) Uani 1 1 d U . . C29 C -0.223(3) 0.2130(8) 0.3862(13) 0.028(4) Uani 1 1 d U . . C30 C -0.235(2) 0.2256(8) 0.2986(13) 0.024(4) Uani 1 1 d DU . . C31 C -0.279(2) 0.1930(9) 0.2364(14) 0.040(5) Uani 1 1 d DU . . H31 H -0.3074 0.1619 0.2508 0.049 Uiso 1 1 calc R . . C32 C -0.283(3) 0.2029(10) 0.1584(15) 0.051(6) Uani 1 1 d DU . . H32 H -0.3162 0.1802 0.1180 0.061 Uiso 1 1 calc R . . C33 C -0.236(3) 0.2486(10) 0.1396(14) 0.046(6) Uani 1 1 d DU . . H33 H -0.2301 0.2573 0.0854 0.055 Uiso 1 1 calc R . . C34 C -0.199(3) 0.2813(10) 0.2015(14) 0.046(6) Uani 1 1 d DU . . H34 H -0.1720 0.3126 0.1877 0.055 Uiso 1 1 calc R . . N2 N -0.199(2) 0.2708(7) 0.2786(11) 0.033(4) Uani 1 1 d DU . . C41 C 0.436(3) 0.8435(10) 0.1025(15) 0.046(7) Uani 1 1 d U . . O41 O 0.314(2) 0.8576(6) 0.0917(11) 0.052(5) Uani 1 1 d U . . C42 C 0.721(3) 0.8768(9) 0.0894(14) 0.037(6) Uani 1 1 d U . . O42 O 0.764(2) 0.9141(6) 0.0707(10) 0.050(5) Uani 1 1 d U . . C43 C 0.652(2) 0.8410(7) 0.2351(13) 0.023(5) Uani 1 1 d U . . O43 O 0.662(2) 0.8518(6) 0.3022(10) 0.046(5) Uani 1 1 d U . . C44 C 0.393(3) 0.7395(10) 0.1067(16) 0.043(7) Uani 1 1 d U . . O44 O 0.2872(19) 0.7430(7) 0.0609(9) 0.047(5) Uani 1 1 d U . . C45 C 0.519(3) 0.6625(9) 0.1949(15) 0.037(6) Uani 1 1 d U . . O45 O 0.488(2) 0.6243(7) 0.1989(12) 0.059(5) Uani 1 1 d U . . C46 C 0.468(3) 0.7525(8) 0.2683(15) 0.031(5) Uani 1 1 d U . . O46 O 0.406(2) 0.7671(7) 0.3181(11) 0.063(6) Uani 1 1 d U . . C47 C 0.945(3) 0.7956(9) 0.0974(16) 0.039(6) Uani 1 1 d U . . O47 O 0.996(2) 0.8160(7) 0.0488(11) 0.055(5) Uani 1 1 d U . . C48 C 1.033(3) 0.7085(9) 0.1864(14) 0.037(6) Uani 1 1 d U . . O48 O 1.1266(19) 0.6814(6) 0.1912(11) 0.050(5) Uani 1 1 d U . . C49 C 0.972(2) 0.7955(9) 0.2640(13) 0.033(6) Uani 1 1 d U . . O49 O 1.031(2) 0.8212(7) 0.3142(10) 0.048(5) Uani 1 1 d U . . C50 C 0.775(3) 0.7156(9) 0.2645(13) 0.030(6) Uani 1 1 d U . . O50 O 0.8030(18) 0.6961(6) 0.3272(9) 0.040(4) Uani 1 1 d U . . C51 C 0.792(2) 0.4166(9) 0.0824(11) 0.029(5) Uani 1 1 d U . . O51 O 0.729(2) 0.3839(7) 0.0985(11) 0.061(6) Uani 1 1 d U . . C52 C 1.105(3) 0.4401(10) 0.0886(15) 0.045(7) Uani 1 1 d U . . O52 O 1.219(2) 0.4194(8) 0.1119(12) 0.063(6) Uani 1 1 d U . . C53 C 0.909(3) 0.4467(8) -0.0548(13) 0.029(5) Uani 1 1 d U . . O53 O 0.9067(19) 0.4346(6) -0.1175(10) 0.045(5) Uani 1 1 d U . . C54 C 1.155(3) 0.5432(9) 0.0720(14) 0.038(6) Uani 1 1 d U . . O54 O 1.262(2) 0.5394(7) 0.1164(11) 0.054(5) Uani 1 1 d U . . C55 C 1.045(2) 0.6229(8) -0.0161(13) 0.026(5) Uani 1 1 d U . . O55 O 1.074(2) 0.6616(6) -0.0191(11) 0.052(5) Uani 1 1 d U . . C56 C 1.087(3) 0.5358(7) -0.0934(13) 0.028(5) Uani 1 1 d U . . O56 O 1.154(2) 0.5218(7) -0.1413(11) 0.052(5) Uani 1 1 d U . . C57 C 0.599(2) 0.5000(8) 0.0786(17) 0.037(6) Uani 1 1 d U . . O57 O 0.5375(19) 0.4812(7) 0.1280(12) 0.063(6) Uani 1 1 d U . . C58 C 0.520(3) 0.5816(9) -0.0127(14) 0.035(6) Uani 1 1 d U . . O58 O 0.4301(19) 0.6094(7) -0.0169(10) 0.052(5) Uani 1 1 d U . . C59 C 0.589(3) 0.4931(8) -0.0880(14) 0.032(5) Uani 1 1 d U . . O59 O 0.532(2) 0.4684(7) -0.1352(10) 0.055(5) Uani 1 1 d U . . C60 C 0.789(2) 0.5756(8) -0.0894(12) 0.022(5) Uani 1 1 d U . . O60 O 0.7539(19) 0.5952(7) -0.1473(9) 0.046(5) Uani 1 1 d U . . N3 N 0.6399(19) 0.7861(7) 0.0126(10) 0.029(4) Uani 1 1 d DU . . C61 C 0.613(2) 0.8113(9) -0.0575(13) 0.040(5) Uani 1 1 d DU . . H61 H 0.5822 0.8436 -0.0566 0.048 Uiso 1 1 calc R . . C62 C 0.631(3) 0.7891(10) -0.1310(14) 0.051(6) Uani 1 1 d DU . . H62 H 0.6152 0.8066 -0.1797 0.061 Uiso 1 1 calc R . . C63 C 0.673(3) 0.7411(10) -0.1320(15) 0.049(6) Uani 1 1 d DU . . H63 H 0.6827 0.7251 -0.1809 0.059 Uiso 1 1 calc R . . C64 C 0.699(3) 0.7189(9) -0.0622(14) 0.036(5) Uani 1 1 d DU . . H64 H 0.7302 0.6867 -0.0626 0.043 Uiso 1 1 calc R . . C65 C 0.682(2) 0.7396(8) 0.0125(13) 0.024(4) Uani 1 1 d DU . . C66 C 0.719(2) 0.7160(7) 0.0919(13) 0.025(4) Uani 1 1 d U . . C67 C 0.764(2) 0.6662(8) 0.0860(13) 0.026(5) Uani 1 1 d U . . C68 C 0.793(2) 0.6242(8) 0.0892(12) 0.024(4) Uani 1 1 d U . . C69 C 0.830(2) 0.5747(8) 0.0833(13) 0.026(4) Uani 1 1 d U . . C70 C 0.867(2) 0.5514(8) 0.1645(12) 0.025(4) Uani 1 1 d DU . . C71 C 0.859(2) 0.5744(9) 0.2374(13) 0.038(5) Uani 1 1 d DU . . H71 H 0.8331 0.6072 0.2365 0.046 Uiso 1 1 calc R . . C72 C 0.886(3) 0.5518(9) 0.3108(14) 0.043(6) Uani 1 1 d DU . . H72 H 0.8788 0.5687 0.3592 0.051 Uiso 1 1 calc R . . C73 C 0.926(3) 0.5011(10) 0.3126(15) 0.052(6) Uani 1 1 d DU . . H73 H 0.9441 0.4824 0.3599 0.063 Uiso 1 1 calc R . . C74 C 0.935(3) 0.4851(9) 0.2386(13) 0.039(5) Uani 1 1 d DU . . H74 H 0.9681 0.4531 0.2375 0.046 Uiso 1 1 calc R . . N4 N 0.906(2) 0.5043(7) 0.1656(11) 0.035(4) Uani 1 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 0.0317(5) 0.0156(5) 0.0274(5) 0.0017(4) 0.0046(4) -0.0007(4) Os2 0.0256(5) 0.0168(5) 0.0240(5) -0.0025(4) 0.0021(4) -0.0007(4) Os3 0.0259(5) 0.0149(5) 0.0300(5) 0.0000(4) 0.0026(4) 0.0017(4) Os4 0.0352(5) 0.0161(5) 0.0296(5) 0.0017(4) 0.0049(4) 0.0000(4) Os5 0.0261(5) 0.0172(5) 0.0255(5) -0.0030(4) 0.0042(4) 0.0007(4) Os6 0.0251(5) 0.0148(5) 0.0308(5) -0.0006(4) 0.0040(4) 0.0018(4) Os7 0.0307(5) 0.0180(5) 0.0272(5) 0.0001(4) 0.0041(4) 0.0015(4) Os8 0.0278(5) 0.0197(5) 0.0233(5) -0.0025(4) 0.0064(4) -0.0011(4) Os9 0.0248(5) 0.0214(5) 0.0286(5) -0.0019(4) 0.0022(4) -0.0003(4) Os10 0.0331(5) 0.0182(5) 0.0286(5) 0.0024(4) 0.0028(4) 0.0029(4) Os11 0.0263(5) 0.0200(5) 0.0223(5) -0.0016(4) 0.0049(4) -0.0016(4) Os12 0.0259(5) 0.0193(5) 0.0289(5) 0.0004(4) 0.0012(4) 0.0000(4) C1 0.038(14) 0.047(17) 0.041(15) -0.006(13) 0.004(10) -0.012(13) O1 0.032(10) 0.034(10) 0.079(13) 0.016(9) 0.017(8) -0.001(8) C2 0.029(13) 0.031(13) 0.057(16) -0.007(12) -0.022(12) 0.010(11) O2 0.065(13) 0.035(11) 0.081(14) 0.011(10) -0.004(10) 0.026(9) C3 0.026(8) 0.025(9) 0.030(8) 0.018(7) 0.006(7) 0.000(7) O3 0.071(12) 0.011(9) 0.046(10) 0.006(7) 0.016(9) 0.010(8) C4 0.030(8) 0.022(8) 0.027(8) -0.012(7) 0.005(6) -0.007(7) O4 0.040(10) 0.066(14) 0.062(12) 0.006(10) -0.003(8) 0.024(10) C5 0.040(13) 0.017(13) 0.044(14) 0.011(11) 0.005(11) 0.012(9) O5 0.040(10) 0.030(10) 0.059(11) 0.002(9) 0.011(8) -0.005(8) C6 0.046(14) 0.027(13) 0.025(12) 0.008(9) 0.011(10) 0.002(12) O6 0.059(11) 0.028(10) 0.039(10) -0.005(8) 0.013(8) -0.005(9) C7 0.046(9) 0.021(8) 0.037(9) -0.011(7) 0.001(7) 0.003(8) O7 0.110(17) 0.011(9) 0.094(16) -0.004(10) 0.017(13) 0.022(11) C8 0.051(15) 0.016(12) 0.027(12) -0.001(11) 0.021(9) 0.016(12) O8 0.083(14) 0.051(12) 0.058(12) 0.014(10) 0.048(10) 0.033(11) C9 0.033(8) 0.021(9) 0.033(8) -0.001(7) -0.003(7) 0.015(7) O9 0.046(11) 0.030(11) 0.072(13) -0.013(9) -0.011(9) -0.004(8) C10 0.019(11) 0.011(11) 0.040(11) -0.008(10) -0.012(10) 0.007(10) O10 0.035(9) 0.028(10) 0.043(9) 0.005(8) -0.004(8) 0.008(8) C11 0.043(14) 0.017(13) 0.034(14) 0.004(10) 0.007(10) 0.006(11) O11 0.061(13) 0.045(12) 0.070(13) 0.014(10) 0.031(10) -0.002(10) C12 0.041(15) 0.025(14) 0.049(16) -0.003(12) -0.012(12) 0.012(11) O12 0.066(14) 0.080(16) 0.072(14) 0.020(12) -0.034(11) 0.037(11) C13 0.035(13) 0.006(11) 0.031(11) 0.003(8) -0.002(10) 0.011(9) O13 0.050(10) 0.020(9) 0.040(9) -0.002(7) 0.011(8) 0.008(8) C14 0.030(8) 0.043(9) 0.029(8) -0.021(7) 0.006(6) -0.001(7) O14 0.040(11) 0.086(17) 0.064(12) 0.013(11) -0.011(8) -0.004(10) C15 0.013(11) 0.028(14) 0.065(16) -0.025(12) 0.023(10) 0.000(9) O15 0.042(11) 0.042(12) 0.098(15) 0.004(11) 0.039(10) -0.006(9) C16 0.034(13) 0.014(12) 0.032(13) -0.010(9) -0.005(10) -0.009(11) O16 0.076(13) 0.025(10) 0.046(11) -0.005(8) 0.029(9) 0.010(9) C17 0.047(16) 0.016(13) 0.057(15) -0.005(12) 0.014(11) 0.016(12) O17 0.078(14) 0.048(13) 0.071(13) 0.025(11) 0.033(11) 0.011(11) C18 0.044(15) 0.027(12) 0.058(17) -0.020(13) -0.019(13) 0.018(12) O18 0.088(15) 0.020(10) 0.078(14) 0.010(10) -0.002(12) 0.011(10) C19 0.025(12) 0.037(16) 0.068(18) -0.019(13) 0.013(11) 0.011(11) O19 0.044(10) 0.025(10) 0.066(12) -0.008(9) 0.003(8) 0.000(8) C20 0.032(12) 0.011(11) 0.029(10) -0.003(9) 0.016(10) 0.000(10) O20 0.042(10) 0.050(12) 0.020(7) 0.000(8) 0.003(7) 0.002(9) N1 0.029(9) 0.026(8) 0.021(7) 0.004(7) -0.001(7) 0.006(8) C21 0.052(14) 0.034(11) 0.025(9) -0.002(7) 0.010(10) -0.004(11) C22 0.051(14) 0.058(13) 0.019(8) -0.004(8) -0.006(10) 0.004(12) C23 0.043(9) 0.045(8) 0.027(6) -0.020(7) 0.007(7) 0.006(7) C24 0.033(12) 0.044(11) 0.029(8) -0.011(7) 0.000(10) -0.009(11) C25 0.033(11) 0.016(9) 0.027(7) -0.003(6) 0.003(9) 0.010(9) C26 0.033(11) 0.007(8) 0.019(7) -0.003(7) 0.013(8) 0.006(8) C27 0.009(9) 0.026(8) 0.033(11) 0.002(8) 0.011(9) -0.007(9) C28 0.031(12) 0.015(8) 0.038(11) -0.004(8) 0.011(10) 0.001(9) C29 0.038(12) 0.013(8) 0.035(8) 0.002(8) 0.017(10) 0.007(9) C30 0.015(10) 0.028(9) 0.030(7) 0.000(6) 0.008(8) 0.001(9) C31 0.053(14) 0.032(11) 0.038(8) -0.005(8) 0.012(11) -0.009(11) C32 0.075(16) 0.045(12) 0.035(8) -0.016(10) 0.011(12) -0.011(13) C33 0.055(14) 0.059(14) 0.026(9) 0.002(8) 0.009(11) -0.017(13) C34 0.071(16) 0.036(12) 0.031(9) 0.007(8) 0.009(12) -0.007(12) N2 0.042(11) 0.029(9) 0.030(7) -0.002(7) 0.010(8) -0.005(9) C41 0.036(12) 0.058(19) 0.041(15) -0.018(14) -0.005(12) 0.000(12) O41 0.034(9) 0.041(11) 0.079(14) 0.004(10) -0.007(10) 0.001(9) C42 0.031(14) 0.040(13) 0.042(14) -0.018(12) 0.017(11) -0.018(12) O42 0.056(12) 0.042(11) 0.052(11) -0.009(9) 0.007(9) -0.018(9) C43 0.030(8) 0.009(8) 0.030(7) -0.003(7) 0.003(7) 0.004(7) O43 0.074(13) 0.025(10) 0.037(8) -0.007(8) 0.002(9) -0.002(9) C44 0.026(13) 0.045(17) 0.059(17) 0.006(14) 0.005(9) 0.012(13) O44 0.054(11) 0.060(13) 0.025(9) 0.015(9) -0.004(7) -0.025(10) C45 0.029(13) 0.034(11) 0.057(16) -0.002(13) 0.039(12) -0.006(12) O45 0.063(13) 0.033(10) 0.084(14) 0.008(11) 0.023(11) -0.018(10) C46 0.028(13) 0.017(13) 0.051(14) -0.002(11) 0.010(10) 0.008(10) O46 0.085(15) 0.045(13) 0.067(13) -0.015(10) 0.043(11) 0.001(11) C47 0.019(12) 0.041(17) 0.061(17) 0.003(12) 0.021(11) 0.013(11) O47 0.063(13) 0.050(13) 0.053(12) 0.023(10) 0.008(9) 0.013(10) C48 0.042(9) 0.029(9) 0.041(9) -0.001(8) 0.008(8) 0.014(7) O48 0.037(10) 0.035(11) 0.079(13) 0.004(10) 0.011(9) 0.022(8) C49 0.020(12) 0.047(16) 0.030(12) 0.010(10) 0.001(9) -0.010(11) O49 0.065(12) 0.035(11) 0.043(10) -0.006(8) -0.001(9) -0.001(10) C50 0.045(14) 0.034(15) 0.017(10) -0.001(9) 0.022(10) 0.014(12) O50 0.049(10) 0.036(11) 0.035(9) 0.009(8) 0.002(8) 0.003(9) C51 0.030(13) 0.047(15) 0.011(10) -0.005(10) 0.010(9) -0.015(11) O51 0.078(14) 0.050(12) 0.056(12) 0.011(10) 0.016(10) -0.025(10) C52 0.048(15) 0.040(16) 0.042(15) -0.002(13) -0.010(12) -0.001(12) O52 0.038(11) 0.081(16) 0.069(13) -0.007(12) 0.003(9) 0.017(10) C53 0.040(9) 0.025(9) 0.021(7) 0.007(7) 0.002(7) 0.008(7) O53 0.056(11) 0.040(11) 0.038(9) -0.025(9) 0.007(8) -0.009(9) C54 0.033(13) 0.048(17) 0.034(13) -0.019(13) 0.007(8) 0.003(12) O54 0.042(11) 0.058(13) 0.058(12) -0.004(10) -0.012(8) 0.000(10) C55 0.029(12) 0.018(10) 0.033(13) -0.010(10) 0.019(10) -0.011(10) O55 0.062(12) 0.026(9) 0.072(13) 0.000(9) 0.021(10) -0.029(9) C56 0.050(15) 0.005(11) 0.031(12) 0.000(9) 0.015(10) -0.001(10) O56 0.061(12) 0.045(12) 0.057(12) -0.018(9) 0.040(9) -0.006(10) C57 0.006(11) 0.020(13) 0.087(19) 0.029(12) 0.006(10) 0.004(10) O57 0.029(10) 0.066(15) 0.097(15) 0.042(12) 0.020(9) -0.005(9) C58 0.022(12) 0.046(16) 0.035(13) -0.015(12) -0.001(10) 0.000(9) O58 0.039(11) 0.057(13) 0.058(11) -0.001(10) -0.005(9) 0.025(9) C59 0.038(9) 0.023(9) 0.032(8) 0.010(7) -0.004(7) -0.012(7) O59 0.068(12) 0.051(12) 0.041(10) -0.016(9) -0.016(9) -0.007(11) C60 0.024(11) 0.025(13) 0.017(10) -0.007(9) 0.001(9) 0.010(10) O60 0.046(10) 0.058(13) 0.033(9) 0.019(9) 0.003(8) -0.005(9) N3 0.041(10) 0.025(8) 0.018(7) 0.005(6) -0.006(8) -0.002(8) C61 0.062(14) 0.031(11) 0.025(9) 0.006(7) -0.007(10) -0.016(11) C62 0.084(17) 0.045(11) 0.021(8) 0.010(9) -0.001(12) -0.001(14) C63 0.075(16) 0.039(11) 0.029(8) -0.003(9) -0.015(12) -0.011(13) C64 0.046(13) 0.026(11) 0.038(8) -0.001(8) 0.011(11) 0.003(11) C65 0.019(10) 0.019(8) 0.037(8) 0.001(7) 0.018(8) -0.012(8) C66 0.024(11) 0.018(8) 0.038(9) 0.009(8) 0.018(9) -0.001(9) C67 0.027(11) 0.023(7) 0.031(11) -0.013(8) 0.011(9) -0.005(9) C68 0.026(11) 0.028(7) 0.022(11) -0.006(8) 0.019(9) 0.006(9) C69 0.021(10) 0.026(8) 0.031(8) 0.003(8) 0.002(9) 0.012(9) C70 0.023(10) 0.031(9) 0.024(7) 0.005(7) 0.012(8) -0.004(9) C71 0.061(14) 0.027(10) 0.029(8) 0.004(7) 0.010(11) 0.000(11) C72 0.073(16) 0.035(11) 0.022(8) 0.006(9) 0.012(11) -0.014(12) C73 0.086(17) 0.043(11) 0.027(8) 0.010(10) 0.004(12) -0.002(14) C74 0.050(13) 0.036(11) 0.029(9) 0.013(7) 0.002(11) 0.008(11) N4 0.045(11) 0.037(9) 0.023(8) 0.012(7) 0.004(8) 0.014(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C2 1.87(2) . ? Os1 C1 1.90(3) . ? Os1 C3 1.91(2) . ? Os1 N1 2.151(18) . ? Os1 Os3 2.8024(13) . ? Os1 Os2 2.8158(13) . ? Os2 C5 1.88(3) . ? Os2 C6 1.91(3) . ? Os2 C4 1.92(2) . ? Os2 C10 2.11(2) . ? Os2 C26 2.212(19) . ? Os2 Os3 2.7548(12) . ? Os3 C8 1.90(2) . ? Os3 C9 1.91(2) . ? Os3 C7 1.94(2) . ? Os3 C10 2.15(2) . ? Os3 C26 2.21(2) . ? Os4 C13 1.87(2) . ? Os4 C11 1.91(2) . ? Os4 C12 1.92(2) . ? Os4 N2 2.132(19) . ? Os4 Os5 2.8057(13) . ? Os4 Os6 2.8068(13) . ? Os5 C14 1.80(2) . ? Os5 C16 1.96(2) . ? Os5 C15 1.97(2) . ? Os5 C20 2.15(2) . ? Os5 C29 2.19(2) . ? Os5 Os6 2.7529(12) . ? Os6 C17 1.90(3) . ? Os6 C19 1.92(3) . ? Os6 C18 1.98(3) . ? Os6 C20 2.10(2) . ? Os6 C29 2.17(2) . ? Os7 C41 1.87(3) . ? Os7 C43 1.89(2) . ? Os7 C42 1.90(3) . ? Os7 N3 2.156(18) . ? Os7 Os8 2.7999(14) . ? Os7 Os9 2.8125(13) . ? Os8 C44 1.89(2) . ? Os8 C46 1.93(2) . ? Os8 C45 1.96(3) . ? Os8 C66 2.14(2) . ? Os8 C50 2.18(2) . ? Os8 Os9 2.7697(13) . ? Os9 C49 1.92(2) . ? Os9 C47 1.94(3) . ? Os9 C48 1.94(2) . ? Os9 C50 2.10(2) . ? Os9 C66 2.19(2) . ? Os10 C52 1.90(3) . ? Os10 C51 1.91(2) . ? Os10 C53 1.91(2) . ? Os10 N4 2.146(19) . ? Os10 Os11 2.8058(13) . ? Os10 Os12 2.8144(13) . ? Os11 C54 1.90(2) . ? Os11 C55 1.92(2) . ? Os11 C56 1.94(2) . ? Os11 C60 2.15(2) . ? Os11 C69 2.17(2) . ? Os11 Os12 2.7560(12) . ? Os12 C57 1.88(2) . ? Os12 C59 1.93(2) . ? Os12 C58 1.95(3) . ? Os12 C69 2.16(2) . ? Os12 C60 2.18(2) . ? C1 O1 1.14(3) . ? C2 O2 1.15(3) . ? C3 O3 1.15(3) . ? C4 O4 1.14(3) . ? C5 O5 1.19(3) . ? C6 O6 1.16(3) . ? C7 O7 1.14(3) . ? C8 O8 1.15(2) . ? C9 O9 1.15(3) . ? C10 O10 1.17(2) . ? C11 O11 1.16(3) . ? C12 O12 1.14(3) . ? C13 O13 1.18(2) . ? C14 O14 1.24(3) . ? C15 O15 1.11(3) . ? C16 O16 1.13(3) . ? C17 O17 1.16(3) . ? C18 O18 1.09(3) . ? C19 O19 1.18(3) . ? C20 O20 1.20(2) . ? N1 C21 1.35(3) . ? N1 C25 1.42(3) . ? C21 C22 1.35(3) . ? C22 C23 1.40(4) . ? C23 C24 1.43(3) . ? C24 C25 1.37(3) . ? C25 C26 1.48(3) . ? C26 C27 1.44(3) . ? C27 C28 1.17(2) . ? C28 C29 1.44(3) . ? C29 C30 1.50(3) . ? C30 N2 1.37(3) . ? C30 C31 1.41(3) . ? C31 C32 1.33(3) . ? C32 C33 1.40(4) . ? C33 C34 1.40(3) . ? C34 N2 1.33(3) . ? C41 O41 1.14(3) . ? C42 O42 1.17(3) . ? C43 O43 1.16(2) . ? C44 O44 1.13(3) . ? C45 O45 1.11(3) . ? C46 O46 1.13(3) . ? C47 O47 1.14(3) . ? C48 O48 1.12(3) . ? C49 O49 1.18(3) . ? C50 O50 1.19(2) . ? C51 O51 1.12(3) . ? C52 O52 1.18(3) . ? C53 O53 1.11(2) . ? C54 O54 1.13(3) . ? C55 O55 1.12(2) . ? C56 O56 1.12(2) . ? C57 O57 1.17(3) . ? C58 O58 1.11(3) . ? C59 O59 1.13(3) . ? C60 O60 1.13(2) . ? N3 C65 1.36(3) . ? N3 C61 1.37(3) . ? C61 C62 1.41(3) . ? C62 C63 1.40(4) . ? C63 C64 1.32(3) . ? C64 C65 1.41(3) . ? C65 C66 1.49(3) . ? C66 C67 1.47(3) . ? C67 C68 1.21(3) . ? C68 C69 1.44(3) . ? C69 C70 1.51(3) . ? C70 N4 1.37(3) . ? C70 C71 1.39(3) . ? C71 C72 1.38(3) . ? C72 C73 1.47(4) . ? C73 C74 1.33(3) . ? C74 N4 1.34(3) . ? 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 C1 89.8(12) . . ? C2 Os1 C3 95.5(10) . . ? C1 Os1 C3 91.7(10) . . ? C2 Os1 N1 93.2(8) . . ? C1 Os1 N1 92.9(9) . . ? C3 Os1 N1 170.2(8) . . ? C2 Os1 Os3 164.9(8) . . ? C1 Os1 Os3 105.2(8) . . ? C3 Os1 Os3 85.4(6) . . ? N1 Os1 Os3 85.0(5) . . ? C2 Os1 Os2 106.2(8) . . ? C1 Os1 Os2 163.8(8) . . ? C3 Os1 Os2 89.2(6) . . ? N1 Os1 Os2 84.0(5) . . ? Os3 Os1 Os2 58.73(3) . . ? C5 Os2 C6 97.2(10) . . ? C5 Os2 C4 96.8(9) . . ? C6 Os2 C4 92.4(9) . . ? C5 Os2 C10 85.0(9) . . ? C6 Os2 C10 91.3(9) . . ? C4 Os2 C10 175.6(9) . . ? C5 Os2 C26 91.6(9) . . ? C6 Os2 C26 169.4(9) . . ? C4 Os2 C26 92.4(8) . . ? C10 Os2 C26 83.6(8) . . ? C5 Os2 Os3 119.9(7) . . ? C6 Os2 Os3 118.3(7) . . ? C4 Os2 Os3 125.5(6) . . ? C10 Os2 Os3 50.4(6) . . ? C26 Os2 Os3 51.6(5) . . ? C5 Os2 Os1 165.1(7) . . ? C6 Os2 Os1 94.9(7) . . ? C4 Os2 Os1 74.1(6) . . ? C10 Os2 Os1 103.3(6) . . ? C26 Os2 Os1 77.4(5) . . ? Os3 Os2 Os1 60.39(3) . . ? C8 Os3 C9 93.0(10) . . ? C8 Os3 C7 94.4(10) . . ? C9 Os3 C7 94.7(9) . . ? C8 Os3 C10 175.9(9) . . ? C9 Os3 C10 90.5(9) . . ? C7 Os3 C10 87.6(9) . . ? C8 Os3 C26 93.8(9) . . ? C9 Os3 C26 169.1(8) . . ? C7 Os3 C26 93.3(8) . . ? C10 Os3 C26 82.5(7) . . ? C8 Os3 Os2 127.1(7) . . ? C9 Os3 Os2 117.7(7) . . ? C7 Os3 Os2 122.0(7) . . ? C10 Os3 Os2 49.0(5) . . ? C26 Os3 Os2 51.5(5) . . ? C8 Os3 Os1 74.9(7) . . ? C9 Os3 Os1 95.9(7) . . ? C7 Os3 Os1 165.2(7) . . ? C10 Os3 Os1 102.5(6) . . ? C26 Os3 Os1 77.6(5) . . ? Os2 Os3 Os1 60.88(3) . . ? C13 Os4 C11 93.1(10) . . ? C13 Os4 C12 95.3(9) . . ? C11 Os4 C12 93.9(10) . . ? C13 Os4 N2 169.8(8) . . ? C11 Os4 N2 92.9(8) . . ? C12 Os4 N2 92.5(9) . . ? C13 Os4 Os5 87.3(7) . . ? C11 Os4 Os5 165.1(7) . . ? C12 Os4 Os5 100.9(8) . . ? N2 Os4 Os5 84.8(5) . . ? C13 Os4 Os6 86.5(6) . . ? C11 Os4 Os6 106.4(7) . . ? C12 Os4 Os6 159.5(8) . . ? N2 Os4 Os6 83.9(5) . . ? Os5 Os4 Os6 58.75(3) . . ? C14 Os5 C16 92.3(10) . . ? C14 Os5 C15 95.6(10) . . ? C16 Os5 C15 96.3(9) . . ? C14 Os5 C20 177.1(9) . . ? C16 Os5 C20 90.6(8) . . ? C15 Os5 C20 84.1(9) . . ? C14 Os5 C29 95.5(9) . . ? C16 Os5 C29 166.4(9) . . ? C15 Os5 C29 94.0(8) . . ? C20 Os5 C29 81.6(8) . . ? C14 Os5 Os6 129.3(7) . . ? C16 Os5 Os6 116.2(6) . . ? C15 Os5 Os6 119.7(7) . . ? C20 Os5 Os6 49.0(5) . . ? C29 Os5 Os6 50.5(6) . . ? C14 Os5 Os4 77.3(8) . . ? C16 Os5 Os4 94.0(7) . . ? C15 Os5 Os4 167.8(7) . . ? C20 Os5 Os4 102.5(5) . . ? C29 Os5 Os4 77.0(6) . . ? Os6 Os5 Os4 60.65(3) . . ? C17 Os6 C19 90.3(11) . . ? C17 Os6 C18 96.1(11) . . ? C19 Os6 C18 96.7(10) . . ? C17 Os6 C20 176.9(10) . . ? C19 Os6 C20 92.5(9) . . ? C18 Os6 C20 84.8(10) . . ? C17 Os6 C29 93.8(10) . . ? C19 Os6 C29 170.2(9) . . ? C18 Os6 C29 91.7(9) . . ? C20 Os6 C29 83.2(8) . . ? C17 Os6 Os5 126.9(7) . . ? C19 Os6 Os5 119.5(7) . . ? C18 Os6 Os5 119.9(8) . . ? C20 Os6 Os5 50.4(6) . . ? C29 Os6 Os5 51.3(6) . . ? C17 Os6 Os4 74.8(7) . . ? C19 Os6 Os4 95.3(8) . . ? C18 Os6 Os4 165.0(7) . . ? C20 Os6 Os4 103.7(6) . . ? C29 Os6 Os4 77.3(6) . . ? Os5 Os6 Os4 60.61(3) . . ? C41 Os7 C43 93.5(10) . . ? C41 Os7 C42 91.7(12) . . ? C43 Os7 C42 94.3(9) . . ? C41 Os7 N3 94.6(9) . . ? C43 Os7 N3 169.9(8) . . ? C42 Os7 N3 91.7(8) . . ? C41 Os7 Os8 99.5(9) . . ? C43 Os7 Os8 88.1(6) . . ? C42 Os7 Os8 168.4(8) . . ? N3 Os7 Os8 84.4(5) . . ? C41 Os7 Os9 158.6(9) . . ? C43 Os7 Os9 86.1(6) . . ? C42 Os7 Os9 109.6(8) . . ? N3 Os7 Os9 84.2(5) . . ? Os8 Os7 Os9 59.14(3) . . ? C44 Os8 C46 91.7(11) . . ? C44 Os8 C45 92.6(11) . . ? C46 Os8 C45 95.6(9) . . ? C44 Os8 C66 95.4(10) . . ? C46 Os8 C66 167.2(9) . . ? C45 Os8 C66 94.7(8) . . ? C44 Os8 C50 178.2(10) . . ? C46 Os8 C50 89.4(9) . . ? C45 Os8 C50 85.8(10) . . ? C66 Os8 C50 83.7(8) . . ? C44 Os8 Os9 132.0(8) . . ? C46 Os8 Os9 116.7(7) . . ? C45 Os8 Os9 119.7(7) . . ? C66 Os8 Os9 51.1(6) . . ? C50 Os8 Os9 48.4(6) . . ? C44 Os8 Os7 80.7(8) . . ? C46 Os8 Os7 94.1(7) . . ? C45 Os8 Os7 168.3(7) . . ? C66 Os8 Os7 76.6(6) . . ? C50 Os8 Os7 100.7(6) . . ? Os9 Os8 Os7 60.66(3) . . ? C49 Os9 C47 92.2(10) . . ? C49 Os9 C48 95.6(10) . . ? C47 Os9 C48 98.0(10) . . ? C49 Os9 C50 90.0(9) . . ? C47 Os9 C50 175.1(9) . . ? C48 Os9 C50 86.1(10) . . ? C49 Os9 C66 169.0(9) . . ? C47 Os9 C66 92.7(9) . . ? C48 Os9 C66 93.4(9) . . ? C50 Os9 C66 84.3(8) . . ? C49 Os9 Os8 120.2(7) . . ? C47 Os9 Os8 124.2(7) . . ? C48 Os9 Os8 119.8(8) . . ? C50 Os9 Os8 51.0(7) . . ? C66 Os9 Os8 49.3(5) . . ? C49 Os9 Os7 96.6(7) . . ? C47 Os9 Os7 72.9(7) . . ? C48 Os9 Os7 165.1(7) . . ? C50 Os9 Os7 102.4(6) . . ? C66 Os9 Os7 75.6(6) . . ? Os8 Os9 Os7 60.20(3) . . ? C52 Os10 C51 95.7(11) . . ? C52 Os10 C53 94.2(10) . . ? C51 Os10 C53 92.7(9) . . ? C52 Os10 N4 92.6(9) . . ? C51 Os10 N4 93.4(8) . . ? C53 Os10 N4 170.4(8) . . ? C52 Os10 Os11 105.1(8) . . ? C51 Os10 Os11 159.1(7) . . ? C53 Os10 Os11 86.6(7) . . ? N4 Os10 Os11 85.0(5) . . ? C52 Os10 Os12 163.6(8) . . ? C51 Os10 Os12 100.4(7) . . ? C53 Os10 Os12 87.9(6) . . ? N4 Os10 Os12 83.7(5) . . ? Os11 Os10 Os12 58.73(3) . . ? C54 Os11 C55 94.4(11) . . ? C54 Os11 C56 92.6(10) . . ? C55 Os11 C56 94.1(9) . . ? C54 Os11 C60 178.8(9) . . ? C55 Os11 C60 85.6(9) . . ? C56 Os11 C60 88.6(9) . . ? C54 Os11 C69 95.3(9) . . ? C55 Os11 C69 93.8(9) . . ? C56 Os11 C69 168.3(9) . . ? C60 Os11 C69 83.5(8) . . ? C54 Os11 Os12 128.2(8) . . ? C55 Os11 Os12 121.3(7) . . ? C56 Os11 Os12 117.9(7) . . ? C60 Os11 Os12 51.0(6) . . ? C69 Os11 Os12 50.4(6) . . ? C54 Os11 Os10 75.8(8) . . ? C55 Os11 Os10 165.6(6) . . ? C56 Os11 Os10 96.8(6) . . ? C60 Os11 Os10 103.9(6) . . ? C69 Os11 Os10 76.9(6) . . ? Os12 Os11 Os10 60.79(3) . . ? C57 Os12 C59 94.5(11) . . ? C57 Os12 C58 94.0(10) . . ? C59 Os12 C58 96.5(9) . . ? C57 Os12 C69 92.4(10) . . ? C59 Os12 C69 167.6(9) . . ? C58 Os12 C69 93.3(8) . . ? C57 Os12 C60 175.4(10) . . ? C59 Os12 C60 90.0(8) . . ? C58 Os12 C60 86.2(9) . . ? C69 Os12 C60 83.0(8) . . ? C57 Os12 Os11 126.6(6) . . ? C59 Os12 Os11 117.2(7) . . ? C58 Os12 Os11 121.0(7) . . ? C69 Os12 Os11 50.7(6) . . ? C60 Os12 Os11 50.0(5) . . ? C57 Os12 Os10 76.0(6) . . ? C59 Os12 Os10 94.8(7) . . ? C58 Os12 Os10 165.5(7) . . ? C69 Os12 Os10 76.9(5) . . ? C60 Os12 Os10 102.9(5) . . ? Os11 Os12 Os10 60.48(3) . . ? O1 C1 Os1 176(2) . . ? O2 C2 Os1 177(2) . . ? O3 C3 Os1 176(2) . . ? O4 C4 Os2 173(2) . . ? O5 C5 Os2 177(2) . . ? O6 C6 Os2 177(2) . . ? O7 C7 Os3 175(2) . . ? O8 C8 Os3 175(2) . . ? O9 C9 Os3 178(2) . . ? O10 C10 Os2 142.7(17) . . ? O10 C10 Os3 136.7(16) . . ? Os2 C10 Os3 80.6(8) . . ? O11 C11 Os4 178(2) . . ? O12 C12 Os4 177(2) . . ? O13 C13 Os4 177.7(18) . . ? O14 C14 Os5 175(2) . . ? O15 C15 Os5 175(2) . . ? O16 C16 Os5 179(2) . . ? O17 C17 Os6 174(2) . . ? O18 C18 Os6 178(3) . . ? O19 C19 Os6 178(2) . . ? O20 C20 Os6 140.1(16) . . ? O20 C20 Os5 139.2(16) . . ? Os6 C20 Os5 80.6(7) . . ? C21 N1 C25 119.0(19) . . ? C21 N1 Os1 121.9(16) . . ? C25 N1 Os1 118.9(13) . . ? N1 C21 C22 124(2) . . ? C21 C22 C23 117(2) . . ? C22 C23 C24 122(2) . . ? C25 C24 C23 117(2) . . ? C24 C25 N1 121(2) . . ? C24 C25 C26 122(2) . . ? N1 C25 C26 116.8(18) . . ? C27 C26 C25 114.6(18) . . ? C27 C26 Os2 114.2(14) . . ? C25 C26 Os2 114.5(13) . . ? C27 C26 Os3 115.2(14) . . ? C25 C26 Os3 116.1(14) . . ? Os2 C26 Os3 77.0(6) . . ? C28 C27 C26 173(2) . . ? C27 C28 C29 172(2) . . ? C28 C29 C30 114(2) . . ? C28 C29 Os6 118.3(16) . . ? C30 C29 Os6 114.2(14) . . ? C28 C29 Os5 113.3(15) . . ? C30 C29 Os5 114.8(14) . . ? Os6 C29 Os5 78.2(7) . . ? N2 C30 C31 118(2) . . ? N2 C30 C29 118.0(19) . . ? C31 C30 C29 124(2) . . ? C32 C31 C30 124(3) . . ? C31 C32 C33 116(3) . . ? C34 C33 C32 119(2) . . ? N2 C34 C33 123(2) . . ? C34 N2 C30 118(2) . . ? C34 N2 Os4 122.7(17) . . ? C30 N2 Os4 118.9(15) . . ? O41 C41 Os7 176(2) . . ? O42 C42 Os7 173(2) . . ? O43 C43 Os7 177.3(18) . . ? O44 C44 Os8 176(2) . . ? O45 C45 Os8 176(2) . . ? O46 C46 Os8 178(2) . . ? O47 C47 Os9 175(2) . . ? O48 C48 Os9 179(2) . . ? O49 C49 Os9 177(2) . . ? O50 C50 Os9 143.0(19) . . ? O50 C50 Os8 136.3(18) . . ? Os9 C50 Os8 80.6(8) . . ? O51 C51 Os10 175(2) . . ? O52 C52 Os10 175(2) . . ? O53 C53 Os10 179(2) . . ? O54 C54 Os11 172(2) . . ? O55 C55 Os11 176(2) . . ? O56 C56 Os11 176(2) . . ? O57 C57 Os12 175.0(19) . . ? O58 C58 Os12 178(2) . . ? O59 C59 Os12 177(2) . . ? O60 C60 Os11 142.4(18) . . ? O60 C60 Os12 138.6(17) . . ? Os11 C60 Os12 79.0(7) . . ? C65 N3 C61 121(2) . . ? C65 N3 Os7 117.8(14) . . ? C61 N3 Os7 120.8(16) . . ? N3 C61 C62 120(2) . . ? C63 C62 C61 120(2) . . ? C64 C63 C62 118(3) . . ? C63 C64 C65 125(2) . . ? N3 C65 C64 117(2) . . ? N3 C65 C66 117.2(19) . . ? C64 C65 C66 125(2) . . ? C67 C66 C65 113.4(19) . . ? C67 C66 Os8 114.3(14) . . ? C65 C66 Os8 117.6(14) . . ? C67 C66 Os9 113.2(15) . . ? C65 C66 Os9 114.7(14) . . ? Os8 C66 Os9 79.6(7) . . ? C68 C67 C66 172(2) . . ? C67 C68 C69 173(2) . . ? C68 C69 C70 112.6(19) . . ? C68 C69 Os12 116.3(14) . . ? C70 C69 Os12 114.4(15) . . ? C68 C69 Os11 114.8(15) . . ? C70 C69 Os11 116.0(13) . . ? Os12 C69 Os11 78.9(7) . . ? N4 C70 C71 119(2) . . ? N4 C70 C69 117.3(19) . . ? C71 C70 C69 124(2) . . ? C72 C71 C70 123(2) . . ? C71 C72 C73 119(2) . . ? C74 C73 C72 111(2) . . ? C73 C74 N4 134(3) . . ? C74 N4 C70 115(2) . . ? C74 N4 Os10 126.4(17) . . ? C70 N4 Os10 118.5(14) . . ? 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 C5 -84(3) . . . . ? C1 Os1 Os2 C5 87(4) . . . . ? C3 Os1 Os2 C5 -179(3) . . . . ? N1 Os1 Os2 C5 8(3) . . . . ? Os3 Os1 Os2 C5 95(3) . . . . ? C2 Os1 Os2 C6 60.7(10) . . . . ? C1 Os1 Os2 C6 -128(3) . . . . ? C3 Os1 Os2 C6 -34.9(9) . . . . ? N1 Os1 Os2 C6 152.2(8) . . . . ? Os3 Os1 Os2 C6 -119.9(7) . . . . ? C2 Os1 Os2 C4 -30.5(10) . . . . ? C1 Os1 Os2 C4 141(3) . . . . ? C3 Os1 Os2 C4 -126.0(9) . . . . ? N1 Os1 Os2 C4 61.1(8) . . . . ? Os3 Os1 Os2 C4 148.9(6) . . . . ? C2 Os1 Os2 C10 153.2(9) . . . . ? C1 Os1 Os2 C10 -36(3) . . . . ? C3 Os1 Os2 C10 57.7(9) . . . . ? N1 Os1 Os2 C10 -115.3(7) . . . . ? Os3 Os1 Os2 C10 -27.4(6) . . . . ? C2 Os1 Os2 C26 -126.7(9) . . . . ? C1 Os1 Os2 C26 44(3) . . . . ? C3 Os1 Os2 C26 137.8(8) . . . . ? N1 Os1 Os2 C26 -35.1(7) . . . . ? Os3 Os1 Os2 C26 52.7(5) . . . . ? C2 Os1 Os2 Os3 -179.4(8) . . . . ? C1 Os1 Os2 Os3 -8(3) . . . . ? C3 Os1 Os2 Os3 85.1(6) . . . . ? N1 Os1 Os2 Os3 -87.9(4) . . . . ? C5 Os2 Os3 C8 -125.6(12) . . . . ? C6 Os2 Os3 C8 116.0(12) . . . . ? C4 Os2 Os3 C8 -0.3(12) . . . . ? C10 Os2 Os3 C8 -178.3(12) . . . . ? C26 Os2 Os3 C8 -60.2(11) . . . . ? Os1 Os2 Os3 C8 37.3(9) . . . . ? C5 Os2 Os3 C9 116.3(11) . . . . ? C6 Os2 Os3 C9 -2.0(11) . . . . ? C4 Os2 Os3 C9 -118.4(11) . . . . ? C10 Os2 Os3 C9 63.6(11) . . . . ? C26 Os2 Os3 C9 -178.3(10) . . . . ? Os1 Os2 Os3 C9 -80.8(8) . . . . ? C5 Os2 Os3 C7 0.3(11) . . . . ? C6 Os2 Os3 C7 -118.0(11) . . . . ? C4 Os2 Os3 C7 125.6(11) . . . . ? C10 Os2 Os3 C7 -52.4(11) . . . . ? C26 Os2 Os3 C7 65.7(10) . . . . ? Os1 Os2 Os3 C7 163.2(8) . . . . ? C5 Os2 Os3 C10 52.7(11) . . . . ? C6 Os2 Os3 C10 -65.7(11) . . . . ? C4 Os2 Os3 C10 178.0(11) . . . . ? C26 Os2 Os3 C10 118.1(10) . . . . ? Os1 Os2 Os3 C10 -144.5(7) . . . . ? C5 Os2 Os3 C26 -65.4(10) . . . . ? C6 Os2 Os3 C26 176.3(10) . . . . ? C4 Os2 Os3 C26 59.9(10) . . . . ? C10 Os2 Os3 C26 -118.1(10) . . . . ? Os1 Os2 Os3 C26 97.5(7) . . . . ? C5 Os2 Os3 Os1 -162.9(8) . . . . ? C6 Os2 Os3 Os1 78.8(7) . . . . ? C4 Os2 Os3 Os1 -37.6(8) . . . . ? C10 Os2 Os3 Os1 144.5(7) . . . . ? C26 Os2 Os3 Os1 -97.5(7) . . . . ? C2 Os1 Os3 C8 -148(3) . . . . ? C1 Os1 Os3 C8 27.6(11) . . . . ? C3 Os1 Os3 C8 118.2(10) . . . . ? N1 Os1 Os3 C8 -64.1(9) . . . . ? Os2 Os1 Os3 C8 -150.0(8) . . . . ? C2 Os1 Os3 C9 121(3) . . . . ? C1 Os1 Os3 C9 -63.9(10) . . . . ? C3 Os1 Os3 C9 26.7(9) . . . . ? N1 Os1 Os3 C9 -155.5(8) . . . . ? Os2 Os1 Os3 C9 118.5(7) . . . . ? C2 Os1 Os3 C7 -103(4) . . . . ? C1 Os1 Os3 C7 72(3) . . . . ? C3 Os1 Os3 C7 162(3) . . . . ? N1 Os1 Os3 C7 -20(3) . . . . ? Os2 Os1 Os3 C7 -106(3) . . . . ? C2 Os1 Os3 C10 29(3) . . . . ? C1 Os1 Os3 C10 -155.7(9) . . . . ? C3 Os1 Os3 C10 -65.1(8) . . . . ? N1 Os1 Os3 C10 112.6(7) . . . . ? Os2 Os1 Os3 C10 26.7(5) . . . . ? C2 Os1 Os3 C26 -50(3) . . . . ? C1 Os1 Os3 C26 125.0(9) . . . . ? C3 Os1 Os3 C26 -144.4(8) . . . . ? N1 Os1 Os3 C26 33.4(7) . . . . ? Os2 Os1 Os3 C26 -52.6(5) . . . . ? C2 Os1 Os3 Os2 2(3) . . . . ? C1 Os1 Os3 Os2 177.6(8) . . . . ? C3 Os1 Os3 Os2 -91.8(6) . . . . ? N1 Os1 Os3 Os2 85.9(4) . . . . ? C13 Os4 Os5 C14 121.9(10) . . . . ? C11 Os4 Os5 C14 -146(3) . . . . ? C12 Os4 Os5 C14 27.0(10) . . . . ? N2 Os4 Os5 C14 -64.6(9) . . . . ? Os6 Os4 Os5 C14 -150.6(7) . . . . ? C13 Os4 Os5 C16 30.4(9) . . . . ? C11 Os4 Os5 C16 122(3) . . . . ? C12 Os4 Os5 C16 -64.5(10) . . . . ? N2 Os4 Os5 C16 -156.0(8) . . . . ? Os6 Os4 Os5 C16 117.9(6) . . . . ? C13 Os4 Os5 C15 177(3) . . . . ? C11 Os4 Os5 C15 -91(4) . . . . ? C12 Os4 Os5 C15 83(3) . . . . ? N2 Os4 Os5 C15 -9(3) . . . . ? Os6 Os4 Os5 C15 -95(3) . . . . ? C13 Os4 Os5 C20 -61.1(8) . . . . ? C11 Os4 Os5 C20 31(3) . . . . ? C12 Os4 Os5 C20 -156.0(9) . . . . ? N2 Os4 Os5 C20 112.4(7) . . . . ? Os6 Os4 Os5 C20 26.4(6) . . . . ? C13 Os4 Os5 C29 -139.3(9) . . . . ? C11 Os4 Os5 C29 -47(3) . . . . ? C12 Os4 Os5 C29 125.8(10) . . . . ? N2 Os4 Os5 C29 34.3(8) . . . . ? Os6 Os4 Os5 C29 -51.8(6) . . . . ? C13 Os4 Os5 Os6 -87.5(6) . . . . ? C11 Os4 Os5 Os6 4(3) . . . . ? C12 Os4 Os5 Os6 177.6(7) . . . . ? N2 Os4 Os5 Os6 86.0(5) . . . . ? C14 Os5 Os6 C17 1.2(14) . . . . ? C16 Os5 Os6 C17 -116.2(12) . . . . ? C15 Os5 Os6 C17 128.9(12) . . . . ? C20 Os5 Os6 C17 178.1(12) . . . . ? C29 Os5 Os6 C17 60.4(12) . . . . ? Os4 Os5 Os6 C17 -37.0(9) . . . . ? C14 Os5 Os6 C19 116.8(14) . . . . ? C16 Os5 Os6 C19 -0.6(12) . . . . ? C15 Os5 Os6 C19 -115.5(13) . . . . ? C20 Os5 Os6 C19 -66.2(12) . . . . ? C29 Os5 Os6 C19 176.0(12) . . . . ? Os4 Os5 Os6 C19 78.6(10) . . . . ? C14 Os5 Os6 C18 -124.5(13) . . . . ? C16 Os5 Os6 C18 118.1(11) . . . . ? C15 Os5 Os6 C18 3.2(12) . . . . ? C20 Os5 Os6 C18 52.4(11) . . . . ? C29 Os5 Os6 C18 -65.4(11) . . . . ? Os4 Os5 Os6 C18 -162.7(9) . . . . ? C14 Os5 Os6 C20 -176.9(13) . . . . ? C16 Os5 Os6 C20 65.7(10) . . . . ? C15 Os5 Os6 C20 -49.2(11) . . . . ? C29 Os5 Os6 C20 -117.8(10) . . . . ? Os4 Os5 Os6 C20 144.9(7) . . . . ? C14 Os5 Os6 C29 -59.2(12) . . . . ? C16 Os5 Os6 C29 -176.6(10) . . . . ? C15 Os5 Os6 C29 68.6(11) . . . . ? C20 Os5 Os6 C29 117.8(10) . . . . ? Os4 Os5 Os6 C29 -97.4(7) . . . . ? C14 Os5 Os6 Os4 38.2(10) . . . . ? C16 Os5 Os6 Os4 -79.2(7) . . . . ? C15 Os5 Os6 Os4 165.9(8) . . . . ? C20 Os5 Os6 Os4 -144.9(7) . . . . ? C29 Os5 Os6 Os4 97.4(7) . . . . ? C13 Os4 Os6 C17 -120.9(10) . . . . ? C11 Os4 Os6 C17 -28.8(11) . . . . ? C12 Os4 Os6 C17 143(2) . . . . ? N2 Os4 Os6 C17 62.5(9) . . . . ? Os5 Os4 Os6 C17 150.1(8) . . . . ? C13 Os4 Os6 C19 -32.1(10) . . . . ? C11 Os4 Os6 C19 60.1(10) . . . . ? C12 Os4 Os6 C19 -128(2) . . . . ? N2 Os4 Os6 C19 151.4(9) . . . . ? Os5 Os4 Os6 C19 -121.1(7) . . . . ? C13 Os4 Os6 C18 -175(3) . . . . ? C11 Os4 Os6 C18 -83(3) . . . . ? C12 Os4 Os6 C18 89(4) . . . . ? N2 Os4 Os6 C18 9(3) . . . . ? Os5 Os4 Os6 C18 96(3) . . . . ? C13 Os4 Os6 C20 61.8(9) . . . . ? C11 Os4 Os6 C20 154.0(9) . . . . ? C12 Os4 Os6 C20 -34(2) . . . . ? N2 Os4 Os6 C20 -114.7(8) . . . . ? Os5 Os4 Os6 C20 -27.2(6) . . . . ? C13 Os4 Os6 C29 141.5(9) . . . . ? C11 Os4 Os6 C29 -126.4(9) . . . . ? C12 Os4 Os6 C29 46(2) . . . . ? N2 Os4 Os6 C29 -35.1(8) . . . . ? Os5 Os4 Os6 C29 52.5(6) . . . . ? C13 Os4 Os6 Os5 89.0(7) . . . . ? C11 Os4 Os6 Os5 -178.8(7) . . . . ? C12 Os4 Os6 Os5 -7(2) . . . . ? N2 Os4 Os6 Os5 -87.6(5) . . . . ? C41 Os7 Os8 C44 29.7(12) . . . . ? C43 Os7 Os8 C44 122.9(10) . . . . ? C42 Os7 Os8 C44 -135(4) . . . . ? N3 Os7 Os8 C44 -64.0(9) . . . . ? Os9 Os7 Os8 C44 -150.5(8) . . . . ? C41 Os7 Os8 C46 -61.3(10) . . . . ? C43 Os7 Os8 C46 31.9(9) . . . . ? C42 Os7 Os8 C46 134(4) . . . . ? N3 Os7 Os8 C46 -155.0(8) . . . . ? Os9 Os7 Os8 C46 118.4(7) . . . . ? C41 Os7 Os8 C45 85(3) . . . . ? C43 Os7 Os8 C45 178(3) . . . . ? C42 Os7 Os8 C45 -79(5) . . . . ? N3 Os7 Os8 C45 -9(3) . . . . ? Os9 Os7 Os8 C45 -95(3) . . . . ? C41 Os7 Os8 C66 127.6(10) . . . . ? C43 Os7 Os8 C66 -139.2(9) . . . . ? C42 Os7 Os8 C66 -37(4) . . . . ? N3 Os7 Os8 C66 33.9(8) . . . . ? Os9 Os7 Os8 C66 -52.6(6) . . . . ? C41 Os7 Os8 C50 -151.5(9) . . . . ? C43 Os7 Os8 C50 -58.3(8) . . . . ? C42 Os7 Os8 C50 44(4) . . . . ? N3 Os7 Os8 C50 114.8(7) . . . . ? Os9 Os7 Os8 C50 28.2(5) . . . . ? C41 Os7 Os8 Os9 -179.7(8) . . . . ? C43 Os7 Os8 Os9 -86.5(6) . . . . ? C42 Os7 Os8 Os9 16(3) . . . . ? N3 Os7 Os8 Os9 86.6(5) . . . . ? C44 Os8 Os9 C49 120.5(14) . . . . ? C46 Os8 Os9 C49 0.6(11) . . . . ? C45 Os8 Os9 C49 -113.7(12) . . . . ? C66 Os8 Os9 C49 176.2(11) . . . . ? C50 Os8 Os9 C49 -61.9(11) . . . . ? Os7 Os8 Os9 C49 79.7(8) . . . . ? C44 Os8 Os9 C47 3.7(14) . . . . ? C46 Os8 Os9 C47 -116.1(12) . . . . ? C45 Os8 Os9 C47 129.5(12) . . . . ? C66 Os8 Os9 C47 59.4(11) . . . . ? C50 Os8 Os9 C47 -178.7(12) . . . . ? Os7 Os8 Os9 C47 -37.1(9) . . . . ? C44 Os8 Os9 C48 -122.0(14) . . . . ? C46 Os8 Os9 C48 118.2(11) . . . . ? C45 Os8 Os9 C48 3.8(12) . . . . ? C66 Os8 Os9 C48 -66.3(11) . . . . ? C50 Os8 Os9 C48 55.6(11) . . . . ? Os7 Os8 Os9 C48 -162.8(8) . . . . ? C44 Os8 Os9 C50 -177.6(13) . . . . ? C46 Os8 Os9 C50 62.6(11) . . . . ? C45 Os8 Os9 C50 -51.8(11) . . . . ? C66 Os8 Os9 C50 -121.9(11) . . . . ? Os7 Os8 Os9 C50 141.6(8) . . . . ? C44 Os8 Os9 C66 -55.7(13) . . . . ? C46 Os8 Os9 C66 -175.5(10) . . . . ? C45 Os8 Os9 C66 70.1(11) . . . . ? C50 Os8 Os9 C66 121.9(11) . . . . ? Os7 Os8 Os9 C66 -96.5(7) . . . . ? C44 Os8 Os9 Os7 40.8(11) . . . . ? C46 Os8 Os9 Os7 -79.0(8) . . . . ? C45 Os8 Os9 Os7 166.6(8) . . . . ? C66 Os8 Os9 Os7 96.5(7) . . . . ? C50 Os8 Os9 Os7 -141.6(8) . . . . ? C41 Os7 Os9 C49 -120(2) . . . . ? C43 Os7 Os9 C49 -30.9(9) . . . . ? C42 Os7 Os9 C49 62.2(10) . . . . ? N3 Os7 Os9 C49 151.9(8) . . . . ? Os8 Os7 Os9 C49 -121.1(7) . . . . ? C41 Os7 Os9 C47 149(2) . . . . ? C43 Os7 Os9 C47 -121.3(10) . . . . ? C42 Os7 Os9 C47 -28.1(11) . . . . ? N3 Os7 Os9 C47 61.6(9) . . . . ? Os8 Os7 Os9 C47 148.6(8) . . . . ? C41 Os7 Os9 C48 95(4) . . . . ? C43 Os7 Os9 C48 -176(3) . . . . ? C42 Os7 Os9 C48 -82(3) . . . . ? N3 Os7 Os9 C48 7(3) . . . . ? Os8 Os7 Os9 C48 94(3) . . . . ? C41 Os7 Os9 C50 -29(2) . . . . ? C43 Os7 Os9 C50 60.5(9) . . . . ? C42 Os7 Os9 C50 153.7(10) . . . . ? N3 Os7 Os9 C50 -116.6(8) . . . . ? Os8 Os7 Os9 C50 -29.6(6) . . . . ? C41 Os7 Os9 C66 52(2) . . . . ? C43 Os7 Os9 C66 141.3(9) . . . . ? C42 Os7 Os9 C66 -125.6(9) . . . . ? N3 Os7 Os9 C66 -35.9(7) . . . . ? Os8 Os7 Os9 C66 51.1(5) . . . . ? C41 Os7 Os9 Os8 1(2) . . . . ? C43 Os7 Os9 Os8 90.2(6) . . . . ? C42 Os7 Os9 Os8 -176.7(7) . . . . ? N3 Os7 Os9 Os8 -87.0(5) . . . . ? C52 Os10 Os11 C54 -26.2(11) . . . . ? C51 Os10 Os11 C54 151.5(18) . . . . ? C53 Os10 Os11 C54 -119.7(10) . . . . ? N4 Os10 Os11 C54 65.1(9) . . . . ? Os12 Os10 Os11 C54 150.7(7) . . . . ? C52 Os10 Os11 C55 -74(3) . . . . ? C51 Os10 Os11 C55 103(3) . . . . ? C53 Os10 Os11 C55 -168(3) . . . . ? N4 Os10 Os11 C55 17(3) . . . . ? Os12 Os10 Os11 C55 103(3) . . . . ? C52 Os10 Os11 C56 64.7(11) . . . . ? C51 Os10 Os11 C56 -117.5(18) . . . . ? C53 Os10 Os11 C56 -28.7(10) . . . . ? N4 Os10 Os11 C56 156.0(8) . . . . ? Os12 Os10 Os11 C56 -118.3(7) . . . . ? C52 Os10 Os11 C60 154.9(10) . . . . ? C51 Os10 Os11 C60 -27.3(17) . . . . ? C53 Os10 Os11 C60 61.5(9) . . . . ? N4 Os10 Os11 C60 -113.8(7) . . . . ? Os12 Os10 Os11 C60 -28.1(5) . . . . ? C52 Os10 Os11 C69 -125.3(10) . . . . ? C51 Os10 Os11 C69 52.5(17) . . . . ? C53 Os10 Os11 C69 141.3(9) . . . . ? N4 Os10 Os11 C69 -34.0(7) . . . . ? Os12 Os10 Os11 C69 51.7(6) . . . . ? C52 Os10 Os11 Os12 -177.0(8) . . . . ? C51 Os10 Os11 Os12 0.8(16) . . . . ? C53 Os10 Os11 Os12 89.6(7) . . . . ? N4 Os10 Os11 Os12 -85.7(5) . . . . ? C54 Os11 Os12 C57 2.9(14) . . . . ? C55 Os11 Os12 C57 -123.5(12) . . . . ? C56 Os11 Os12 C57 121.8(12) . . . . ? C60 Os11 Os12 C57 -176.0(12) . . . . ? C69 Os11 Os12 C57 -57.2(12) . . . . ? Os10 Os11 Os12 C57 40.0(10) . . . . ? C54 Os11 Os12 C59 -116.6(12) . . . . ? C55 Os11 Os12 C59 117.0(11) . . . . ? C56 Os11 Os12 C59 2.3(10) . . . . ? C60 Os11 Os12 C59 64.5(10) . . . . ? C69 Os11 Os12 C59 -176.7(10) . . . . ? Os10 Os11 Os12 C59 -79.4(7) . . . . ? C54 Os11 Os12 C58 126.2(12) . . . . ? C55 Os11 Os12 C58 -0.2(11) . . . . ? C56 Os11 Os12 C58 -114.9(10) . . . . ? C60 Os11 Os12 C58 -52.7(10) . . . . ? C69 Os11 Os12 C58 66.1(10) . . . . ? Os10 Os11 Os12 C58 163.3(8) . . . . ? C54 Os11 Os12 C69 60.1(12) . . . . ? C55 Os11 Os12 C69 -66.3(10) . . . . ? C56 Os11 Os12 C69 179.0(10) . . . . ? C60 Os11 Os12 C69 -118.8(10) . . . . ? Os10 Os11 Os12 C69 97.2(7) . . . . ? C54 Os11 Os12 C60 178.9(12) . . . . ? C55 Os11 Os12 C60 52.5(10) . . . . ? C56 Os11 Os12 C60 -62.2(10) . . . . ? C69 Os11 Os12 C60 118.8(10) . . . . ? Os10 Os11 Os12 C60 -144.0(7) . . . . ? C54 Os11 Os12 Os10 -37.1(9) . . . . ? C55 Os11 Os12 Os10 -163.5(7) . . . . ? C56 Os11 Os12 Os10 81.8(7) . . . . ? C60 Os11 Os12 Os10 144.0(7) . . . . ? C69 Os11 Os12 Os10 -97.2(7) . . . . ? C52 Os10 Os12 C57 -137(3) . . . . ? C51 Os10 Os12 C57 32.4(10) . . . . ? C53 Os10 Os12 C57 124.8(11) . . . . ? N4 Os10 Os12 C57 -59.9(10) . . . . ? Os11 Os10 Os12 C57 -147.9(8) . . . . ? C52 Os10 Os12 C59 129(3) . . . . ? C51 Os10 Os12 C59 -61.0(9) . . . . ? C53 Os10 Os12 C59 31.3(10) . . . . ? N4 Os10 Os12 C59 -153.4(9) . . . . ? Os11 Os10 Os12 C59 118.7(7) . . . . ? C52 Os10 Os12 C58 -90(4) . . . . ? C51 Os10 Os12 C58 80(3) . . . . ? C53 Os10 Os12 C58 172(3) . . . . ? N4 Os10 Os12 C58 -12(3) . . . . ? Os11 Os10 Os12 C58 -100(3) . . . . ? C52 Os10 Os12 C69 -42(3) . . . . ? C51 Os10 Os12 C69 128.3(8) . . . . ? C53 Os10 Os12 C69 -139.4(9) . . . . ? N4 Os10 Os12 C69 35.9(8) . . . . ? Os11 Os10 Os12 C69 -52.0(6) . . . . ? C52 Os10 Os12 C60 38(3) . . . . ? C51 Os10 Os12 C60 -152.2(8) . . . . ? C53 Os10 Os12 C60 -59.8(9) . . . . ? N4 Os10 Os12 C60 115.5(8) . . . . ? Os11 Os10 Os12 C60 27.6(5) . . . . ? C52 Os10 Os12 Os11 10(3) . . . . ? C51 Os10 Os12 Os11 -179.7(6) . . . . ? C53 Os10 Os12 Os11 -87.3(7) . . . . ? N4 Os10 Os12 Os11 88.0(5) . . . . ? C2 Os1 C1 O1 111(34) . . . . ? C3 Os1 C1 O1 -154(34) . . . . ? N1 Os1 C1 O1 18(34) . . . . ? Os3 Os1 C1 O1 -68(34) . . . . ? Os2 Os1 C1 O1 -61(35) . . . . ? C1 Os1 C2 O2 29(52) . . . . ? C3 Os1 C2 O2 -63(52) . . . . ? N1 Os1 C2 O2 122(52) . . . . ? Os3 Os1 C2 O2 -156(50) . . . . ? Os2 Os1 C2 O2 -154(52) . . . . ? C2 Os1 C3 O3 -13(32) . . . . ? C1 Os1 C3 O3 -103(32) . . . . ? N1 Os1 C3 O3 139(30) . . . . ? Os3 Os1 C3 O3 152(32) . . . . ? Os2 Os1 C3 O3 94(32) . . . . ? C5 Os2 C4 O4 -21(18) . . . . ? C6 Os2 C4 O4 77(18) . . . . ? C10 Os2 C4 O4 -134(16) . . . . ? C26 Os2 C4 O4 -112(18) . . . . ? Os3 Os2 C4 O4 -155(17) . . . . ? Os1 Os2 C4 O4 171(18) . . . . ? C6 Os2 C5 O5 -83(48) . . . . ? C4 Os2 C5 O5 11(48) . . . . ? C10 Os2 C5 O5 -173(100) . . . . ? C26 Os2 C5 O5 103(47) . . . . ? Os3 Os2 C5 O5 149(47) . . . . ? Os1 Os2 C5 O5 62(49) . . . . ? C5 Os2 C6 O6 73(42) . . . . ? C4 Os2 C6 O6 -25(42) . . . . ? C10 Os2 C6 O6 158(42) . . . . ? C26 Os2 C6 O6 -142(40) . . . . ? Os3 Os2 C6 O6 -158(41) . . . . ? Os1 Os2 C6 O6 -99(42) . . . . ? C8 Os3 C7 O7 137(26) . . . . ? C9 Os3 C7 O7 -130(26) . . . . ? C10 Os3 C7 O7 -40(26) . . . . ? C26 Os3 C7 O7 42(26) . . . . ? Os2 Os3 C7 O7 -3(26) . . . . ? Os1 Os3 C7 O7 94(26) . . . . ? C9 Os3 C8 O8 -74(26) . . . . ? C7 Os3 C8 O8 21(26) . . . . ? C10 Os3 C8 O8 139(22) . . . . ? C26 Os3 C8 O8 115(25) . . . . ? Os2 Os3 C8 O8 157(25) . . . . ? Os1 Os3 C8 O8 -169(26) . . . . ? C8 Os3 C9 O9 -17(63) . . . . ? C7 Os3 C9 O9 -112(63) . . . . ? C10 Os3 C9 O9 161(63) . . . . ? C26 Os3 C9 O9 111(62) . . . . ? Os2 Os3 C9 O9 118(63) . . . . ? Os1 Os3 C9 O9 58(63) . . . . ? C5 Os2 C10 O10 43(3) . . . . ? C6 Os2 C10 O10 -55(3) . . . . ? C4 Os2 C10 O10 157(10) . . . . ? C26 Os2 C10 O10 135(3) . . . . ? Os3 Os2 C10 O10 179(3) . . . . ? Os1 Os2 C10 O10 -150(3) . . . . ? C5 Os2 C10 Os3 -136.2(9) . . . . ? C6 Os2 C10 Os3 126.7(8) . . . . ? C4 Os2 C10 Os3 -22(12) . . . . ? C26 Os2 C10 Os3 -44.1(7) . . . . ? Os1 Os2 C10 Os3 31.3(6) . . . . ? C8 Os3 C10 O10 -159(12) . . . . ? C9 Os3 C10 O10 54(3) . . . . ? C7 Os3 C10 O10 -41(3) . . . . ? C26 Os3 C10 O10 -135(3) . . . . ? Os2 Os3 C10 O10 -179(3) . . . . ? Os1 Os3 C10 O10 150(2) . . . . ? C8 Os3 C10 Os2 20(13) . . . . ? C9 Os3 C10 Os2 -127.5(8) . . . . ? C7 Os3 C10 Os2 137.8(8) . . . . ? C26 Os3 C10 Os2 44.1(7) . . . . ? Os1 Os3 C10 Os2 -31.4(6) . . . . ? C13 Os4 C11 O11 -73(53) . . . . ? C12 Os4 C11 O11 23(53) . . . . ? N2 Os4 C11 O11 115(53) . . . . ? Os5 Os4 C11 O11 -164(51) . . . . ? Os6 Os4 C11 O11 -160(53) . . . . ? C13 Os4 C12 O12 35(49) . . . . ? C11 Os4 C12 O12 -59(49) . . . . ? N2 Os4 C12 O12 -152(48) . . . . ? Os5 Os4 C12 O12 123(48) . . . . ? Os6 Os4 C12 O12 129(47) . . . . ? C11 Os4 C13 O13 -113(48) . . . . ? C12 Os4 C13 O13 153(48) . . . . ? N2 Os4 C13 O13 13(52) . . . . ? Os5 Os4 C13 O13 52(48) . . . . ? Os6 Os4 C13 O13 -6(48) . . . . ? C16 Os5 C14 O14 -87(23) . . . . ? C15 Os5 C14 O14 9(24) . . . . ? C20 Os5 C14 O14 93(28) . . . . ? C29 Os5 C14 O14 104(23) . . . . ? Os6 Os5 C14 O14 146(23) . . . . ? Os4 Os5 C14 O14 179(100) . . . . ? C14 Os5 C15 O15 19(21) . . . . ? C16 Os5 C15 O15 112(21) . . . . ? C20 Os5 C15 O15 -158(21) . . . . ? C29 Os5 C15 O15 -77(21) . . . . ? Os6 Os5 C15 O15 -123(21) . . . . ? Os4 Os5 C15 O15 -35(24) . . . . ? C14 Os5 C16 O16 -119(100) . . . . ? C15 Os5 C16 O16 146(100) . . . . ? C20 Os5 C16 O16 61(100) . . . . ? C29 Os5 C16 O16 7(100) . . . . ? Os6 Os5 C16 O16 18(100) . . . . ? Os4 Os5 C16 O16 -41(100) . . . . ? C19 Os6 C17 O17 153(21) . . . . ? C18 Os6 C17 O17 56(21) . . . . ? C20 Os6 C17 O17 -51(32) . . . . ? C29 Os6 C17 O17 -36(21) . . . . ? Os5 Os6 C17 O17 -79(21) . . . . ? Os4 Os6 C17 O17 -112(21) . . . . ? C17 Os6 C18 O18 15(67) . . . . ? C19 Os6 C18 O18 -76(67) . . . . ? C20 Os6 C18 O18 -168(67) . . . . ? C29 Os6 C18 O18 109(67) . . . . ? Os5 Os6 C18 O18 154(67) . . . . ? Os4 Os6 C18 O18 67(68) . . . . ? C17 Os6 C19 O19 -92(65) . . . . ? C18 Os6 C19 O19 4(65) . . . . ? C20 Os6 C19 O19 89(65) . . . . ? C29 Os6 C19 O19 153(61) . . . . ? Os5 Os6 C19 O19 134(65) . . . . ? Os4 Os6 C19 O19 -167(65) . . . . ? C17 Os6 C20 O20 149(16) . . . . ? C19 Os6 C20 O20 -55(3) . . . . ? C18 Os6 C20 O20 42(3) . . . . ? C29 Os6 C20 O20 134(3) . . . . ? Os5 Os6 C20 O20 178(3) . . . . ? Os4 Os6 C20 O20 -151(2) . . . . ? C17 Os6 C20 Os5 -29(18) . . . . ? C19 Os6 C20 Os5 127.1(9) . . . . ? C18 Os6 C20 Os5 -136.4(9) . . . . ? C29 Os6 C20 Os5 -44.0(7) . . . . ? Os4 Os6 C20 Os5 31.1(6) . . . . ? C14 Os5 C20 O20 -123(18) . . . . ? C16 Os5 C20 O20 57(3) . . . . ? C15 Os5 C20 O20 -39(3) . . . . ? C29 Os5 C20 O20 -134(3) . . . . ? Os6 Os5 C20 O20 -178(3) . . . . ? Os4 Os5 C20 O20 151(2) . . . . ? C14 Os5 C20 Os6 55(19) . . . . ? C16 Os5 C20 Os6 -125.1(8) . . . . ? C15 Os5 C20 Os6 138.6(8) . . . . ? C29 Os5 C20 Os6 43.7(7) . . . . ? Os4 Os5 C20 Os6 -30.9(6) . . . . ? C2 Os1 N1 C21 -49.2(14) . . . . ? C1 Os1 N1 C21 40.8(14) . . . . ? C3 Os1 N1 C21 159(4) . . . . ? Os3 Os1 N1 C21 145.9(11) . . . . ? Os2 Os1 N1 C21 -155.1(11) . . . . ? C2 Os1 N1 C25 136.1(16) . . . . ? C1 Os1 N1 C25 -133.9(15) . . . . ? C3 Os1 N1 C25 -16(5) . . . . ? Os3 Os1 N1 C25 -28.9(13) . . . . ? Os2 Os1 N1 C25 30.1(13) . . . . ? C25 N1 C21 C22 -1.1(17) . . . . ? Os1 N1 C21 C22 -175.8(13) . . . . ? N1 C21 C22 C23 -2.9(18) . . . . ? C21 C22 C23 C24 8(3) . . . . ? C22 C23 C24 C25 -9(3) . . . . ? C23 C24 C25 N1 4(3) . . . . ? C23 C24 C25 C26 179.1(19) . . . . ? C21 N1 C25 C24 0(3) . . . . ? Os1 N1 C25 C24 175.2(16) . . . . ? C21 N1 C25 C26 -174.8(16) . . . . ? Os1 N1 C25 C26 0(2) . . . . ? C24 C25 C26 C27 6(3) . . . . ? N1 C25 C26 C27 -179.4(17) . . . . ? C24 C25 C26 Os2 140.5(18) . . . . ? N1 C25 C26 Os2 -45(2) . . . . ? C24 C25 C26 Os3 -132.5(19) . . . . ? N1 C25 C26 Os3 42(2) . . . . ? C5 Os2 C26 C27 15.9(16) . . . . ? C6 Os2 C26 C27 -130(4) . . . . ? C4 Os2 C26 C27 112.8(16) . . . . ? C10 Os2 C26 C27 -68.8(16) . . . . ? Os3 Os2 C26 C27 -112.0(16) . . . . ? Os1 Os2 C26 C27 -174.1(16) . . . . ? C5 Os2 C26 C25 -119.1(16) . . . . ? C6 Os2 C26 C25 95(5) . . . . ? C4 Os2 C26 C25 -22.2(16) . . . . ? C10 Os2 C26 C25 156.2(16) . . . . ? Os3 Os2 C26 C25 113.0(17) . . . . ? Os1 Os2 C26 C25 50.9(14) . . . . ? C5 Os2 C26 Os3 128.0(8) . . . . ? C6 Os2 C26 Os3 -18(5) . . . . ? C4 Os2 C26 Os3 -135.2(7) . . . . ? C10 Os2 C26 Os3 43.2(7) . . . . ? Os1 Os2 C26 Os3 -62.1(4) . . . . ? C8 Os3 C26 C27 -113.0(16) . . . . ? C9 Os3 C26 C27 119(5) . . . . ? C7 Os3 C26 C27 -18.4(16) . . . . ? C10 Os3 C26 C27 68.7(15) . . . . ? Os2 Os3 C26 C27 110.9(16) . . . . ? Os1 Os3 C26 C27 173.4(15) . . . . ? C8 Os3 C26 C25 24.9(16) . . . . ? C9 Os3 C26 C25 -103(5) . . . . ? C7 Os3 C26 C25 119.5(16) . . . . ? C10 Os3 C26 C25 -153.4(16) . . . . ? Os2 Os3 C26 C25 -111.2(16) . . . . ? Os1 Os3 C26 C25 -48.7(14) . . . . ? C8 Os3 C26 Os2 136.1(8) . . . . ? C9 Os3 C26 Os2 8(5) . . . . ? C7 Os3 C26 Os2 -129.3(8) . . . . ? C10 Os3 C26 Os2 -42.2(7) . . . . ? Os1 Os3 C26 Os2 62.5(4) . . . . ? C25 C26 C27 C28 -139(17) . . . . ? Os2 C26 C27 C28 86(17) . . . . ? Os3 C26 C27 C28 -1(18) . . . . ? C26 C27 C28 C29 175(14) . . . . ? C27 C28 C29 C30 144(15) . . . . ? C27 C28 C29 Os6 6(17) . . . . ? C27 C28 C29 Os5 -82(16) . . . . ? C17 Os6 C29 C28 113.9(18) . . . . ? C19 Os6 C29 C28 -131(6) . . . . ? C18 Os6 C29 C28 17.7(19) . . . . ? C20 Os6 C29 C28 -66.9(17) . . . . ? Os5 Os6 C29 C28 -110.2(18) . . . . ? Os4 Os6 C29 C28 -172.6(18) . . . . ? C17 Os6 C29 C30 -23.7(16) . . . . ? C19 Os6 C29 C30 91(6) . . . . ? C18 Os6 C29 C30 -120.0(17) . . . . ? C20 Os6 C29 C30 155.5(16) . . . . ? Os5 Os6 C29 C30 112.1(16) . . . . ? Os4 Os6 C29 C30 49.7(14) . . . . ? C17 Os6 C29 Os5 -135.8(8) . . . . ? C19 Os6 C29 Os5 -21(6) . . . . ? C18 Os6 C29 Os5 127.9(10) . . . . ? C20 Os6 C29 Os5 43.4(7) . . . . ? Os4 Os6 C29 Os5 -62.3(4) . . . . ? C14 Os5 C29 C28 -105.9(18) . . . . ? C16 Os5 C29 C28 129(3) . . . . ? C15 Os5 C29 C28 -9.9(18) . . . . ? C20 Os5 C29 C28 73.5(17) . . . . ? Os6 Os5 C29 C28 115.9(18) . . . . ? Os4 Os5 C29 C28 178.5(17) . . . . ? C14 Os5 C29 C30 26.8(18) . . . . ? C16 Os5 C29 C30 -98(4) . . . . ? C15 Os5 C29 C30 122.8(16) . . . . ? C20 Os5 C29 C30 -153.8(17) . . . . ? Os6 Os5 C29 C30 -111.4(17) . . . . ? Os4 Os5 C29 C30 -48.8(14) . . . . ? C14 Os5 C29 Os6 138.1(9) . . . . ? C16 Os5 C29 Os6 13(4) . . . . ? C15 Os5 C29 Os6 -125.8(8) . . . . ? C20 Os5 C29 Os6 -42.4(7) . . . . ? Os4 Os5 C29 Os6 62.5(4) . . . . ? C28 C29 C30 N2 176.0(18) . . . . ? Os6 C29 C30 N2 -44(2) . . . . ? Os5 C29 C30 N2 43(2) . . . . ? C28 C29 C30 C31 -5(3) . . . . ? Os6 C29 C30 C31 134.4(14) . . . . ? Os5 C29 C30 C31 -137.9(14) . . . . ? N2 C30 C31 C32 2.1(18) . . . . ? C29 C30 C31 C32 -176.5(19) . . . . ? C30 C31 C32 C33 1.8(19) . . . . ? C31 C32 C33 C34 -4(3) . . . . ? C32 C33 C34 N2 3(4) . . . . ? C33 C34 N2 C30 1(3) . . . . ? C33 C34 N2 Os4 176.2(18) . . . . ? C31 C30 N2 C34 -4(3) . . . . ? C29 C30 N2 C34 175(2) . . . . ? C31 C30 N2 Os4 -178.8(12) . . . . ? C29 C30 N2 Os4 0(2) . . . . ? C13 Os4 N2 C34 -165(4) . . . . ? C11 Os4 N2 C34 -39.1(19) . . . . ? C12 Os4 N2 C34 55(2) . . . . ? Os5 Os4 N2 C34 155.6(18) . . . . ? Os6 Os4 N2 C34 -145.3(18) . . . . ? C13 Os4 N2 C30 10(6) . . . . ? C11 Os4 N2 C30 135.9(16) . . . . ? C12 Os4 N2 C30 -130.0(16) . . . . ? Os5 Os4 N2 C30 -29.3(14) . . . . ? Os6 Os4 N2 C30 29.7(14) . . . . ? C43 Os7 C41 O41 -20(40) . . . . ? C42 Os7 C41 O41 -114(40) . . . . ? N3 Os7 C41 O41 154(40) . . . . ? Os8 Os7 C41 O41 69(40) . . . . ? Os9 Os7 C41 O41 68(40) . . . . ? C41 Os7 C42 O42 49(20) . . . . ? C43 Os7 C42 O42 -45(20) . . . . ? N3 Os7 C42 O42 143(20) . . . . ? Os8 Os7 C42 O42 -146(17) . . . . ? Os9 Os7 C42 O42 -132(19) . . . . ? C41 Os7 C43 O43 115(41) . . . . ? C42 Os7 C43 O43 -153(41) . . . . ? N3 Os7 C43 O43 -28(44) . . . . ? Os8 Os7 C43 O43 15(41) . . . . ? Os9 Os7 C43 O43 -44(41) . . . . ? C46 Os8 C44 O44 -129(36) . . . . ? C45 Os8 C44 O44 -33(36) . . . . ? C66 Os8 C44 O44 62(36) . . . . ? C50 Os8 C44 O44 -1(63) . . . . ? Os9 Os8 C44 O44 102(36) . . . . ? Os7 Os8 C44 O44 137(36) . . . . ? C44 Os8 C45 O45 39(34) . . . . ? C46 Os8 C45 O45 131(34) . . . . ? C66 Os8 C45 O45 -57(34) . . . . ? C50 Os8 C45 O45 -140(34) . . . . ? Os9 Os8 C45 O45 -104(34) . . . . ? Os7 Os8 C45 O45 -15(36) . . . . ? C44 Os8 C46 O46 -36(59) . . . . ? C45 Os8 C46 O46 -129(59) . . . . ? C66 Os8 C46 O46 88(59) . . . . ? C50 Os8 C46 O46 146(59) . . . . ? Os9 Os8 C46 O46 104(59) . . . . ? Os7 Os8 C46 O46 45(59) . . . . ? C49 Os9 C47 O47 101(27) . . . . ? C48 Os9 C47 O47 5(27) . . . . ? C50 Os9 C47 O47 -142(22) . . . . ? C66 Os9 C47 O47 -89(27) . . . . ? Os8 Os9 C47 O47 -130(26) . . . . ? Os7 Os9 C47 O47 -163(27) . . . . ? C49 Os9 C48 O48 -17(100) . . . . ? C47 Os9 C48 O48 76(100) . . . . ? C50 Os9 C48 O48 -107(100) . . . . ? C66 Os9 C48 O48 169(100) . . . . ? Os8 Os9 C48 O48 -147(100) . . . . ? Os7 Os9 C48 O48 128(99) . . . . ? C47 Os9 C49 O49 46(43) . . . . ? C48 Os9 C49 O49 145(43) . . . . ? C50 Os9 C49 O49 -129(43) . . . . ? C66 Os9 C49 O49 -71(44) . . . . ? Os8 Os9 C49 O49 -86(43) . . . . ? Os7 Os9 C49 O49 -27(43) . . . . ? C49 Os9 C50 O50 -46(3) . . . . ? C47 Os9 C50 O50 -163(10) . . . . ? C48 Os9 C50 O50 49(3) . . . . ? C66 Os9 C50 O50 143(3) . . . . ? Os8 Os9 C50 O50 -177(3) . . . . ? Os7 Os9 C50 O50 -143(3) . . . . ? C49 Os9 C50 Os8 130.3(9) . . . . ? C47 Os9 C50 Os8 13(12) . . . . ? C48 Os9 C50 Os8 -134.1(9) . . . . ? C66 Os9 C50 Os8 -40.3(7) . . . . ? Os7 Os9 C50 Os8 33.5(6) . . . . ? C44 Os8 C50 O50 -79(32) . . . . ? C46 Os8 C50 O50 49(3) . . . . ? C45 Os8 C50 O50 -46(3) . . . . ? C66 Os8 C50 O50 -141(3) . . . . ? Os9 Os8 C50 O50 177(3) . . . . ? Os7 Os8 C50 O50 144(2) . . . . ? C44 Os8 C50 Os9 104(32) . . . . ? C46 Os8 C50 Os9 -127.5(9) . . . . ? C45 Os8 C50 Os9 136.8(8) . . . . ? C66 Os8 C50 Os9 41.6(7) . . . . ? Os7 Os8 C50 Os9 -33.5(6) . . . . ? C52 Os10 C51 O51 -29(21) . . . . ? C53 Os10 C51 O51 66(21) . . . . ? N4 Os10 C51 O51 -121(21) . . . . ? Os11 Os10 C51 O51 154(20) . . . . ? Os12 Os10 C51 O51 154(21) . . . . ? C51 Os10 C52 O52 4(26) . . . . ? C53 Os10 C52 O52 -90(26) . . . . ? N4 Os10 C52 O52 97(26) . . . . ? Os11 Os10 C52 O52 -177(100) . . . . ? Os12 Os10 C52 O52 173(24) . . . . ? C52 Os10 C53 O53 -97(100) . . . . ? C51 Os10 C53 O53 167(100) . . . . ? N4 Os10 C53 O53 38(100) . . . . ? Os11 Os10 C53 O53 8(100) . . . . ? Os12 Os10 C53 O53 67(100) . . . . ? C55 Os11 C54 O54 -2(16) . . . . ? C56 Os11 C54 O54 92(16) . . . . ? C60 Os11 C54 O54 -93(54) . . . . ? C69 Os11 C54 O54 -96(16) . . . . ? Os12 Os11 C54 O54 -139(15) . . . . ? Os10 Os11 C54 O54 -171(16) . . . . ? C54 Os11 C55 O55 -91(29) . . . . ? C56 Os11 C55 O55 176(29) . . . . ? C60 Os11 C55 O55 87(29) . . . . ? C69 Os11 C55 O55 4(29) . . . . ? Os12 Os11 C55 O55 49(30) . . . . ? Os10 Os11 C55 O55 -45(31) . . . . ? C54 Os11 C56 O56 7(27) . . . . ? C55 Os11 C56 O56 102(27) . . . . ? C60 Os11 C56 O56 -173(27) . . . . ? C69 Os11 C56 O56 -125(26) . . . . ? Os12 Os11 C56 O56 -129(27) . . . . ? Os10 Os11 C56 O56 -69(27) . . . . ? C59 Os12 C57 O57 -87(29) . . . . ? C58 Os12 C57 O57 10(29) . . . . ? C69 Os12 C57 O57 104(29) . . . . ? C60 Os12 C57 O57 103(28) . . . . ? Os11 Os12 C57 O57 144(28) . . . . ? Os10 Os12 C57 O57 179(100) . . . . ? C57 Os12 C58 O58 80(95) . . . . ? C59 Os12 C58 O58 175(100) . . . . ? C69 Os12 C58 O58 -13(95) . . . . ? C60 Os12 C58 O58 -95(95) . . . . ? Os11 Os12 C58 O58 -58(95) . . . . ? Os10 Os12 C58 O58 34(97) . . . . ? C57 Os12 C59 O59 2(40) . . . . ? C58 Os12 C59 O59 -93(40) . . . . ? C69 Os12 C59 O59 125(39) . . . . ? C60 Os12 C59 O59 -179(100) . . . . ? Os11 Os12 C59 O59 137(40) . . . . ? Os10 Os12 C59 O59 78(40) . . . . ? C54 Os11 C60 O60 134(50) . . . . ? C55 Os11 C60 O60 43(3) . . . . ? C56 Os11 C60 O60 -51(3) . . . . ? C69 Os11 C60 O60 137(3) . . . . ? Os12 Os11 C60 O60 180(3) . . . . ? Os10 Os11 C60 O60 -148(3) . . . . ? C54 Os11 C60 Os12 -46(51) . . . . ? C55 Os11 C60 Os12 -137.2(8) . . . . ? C56 Os11 C60 Os12 128.6(8) . . . . ? C69 Os11 C60 Os12 -42.8(7) . . . . ? Os10 Os11 C60 Os12 31.9(6) . . . . ? C57 Os12 C60 O60 -136(10) . . . . ? C59 Os12 C60 O60 53(3) . . . . ? C58 Os12 C60 O60 -43(3) . . . . ? C69 Os12 C60 O60 -137(3) . . . . ? Os11 Os12 C60 O60 -180(3) . . . . ? Os10 Os12 C60 O60 148(3) . . . . ? C57 Os12 C60 Os11 44(11) . . . . ? C59 Os12 C60 Os11 -126.6(8) . . . . ? C58 Os12 C60 Os11 136.9(8) . . . . ? C69 Os12 C60 Os11 43.1(7) . . . . ? Os10 Os12 C60 Os11 -31.7(6) . . . . ? C41 Os7 N3 C65 -128.4(16) . . . . ? C43 Os7 N3 C65 14(5) . . . . ? C42 Os7 N3 C65 139.7(15) . . . . ? Os8 Os7 N3 C65 -29.3(13) . . . . ? Os9 Os7 N3 C65 30.2(13) . . . . ? C41 Os7 N3 C61 56.8(15) . . . . ? C43 Os7 N3 C61 -161(4) . . . . ? C42 Os7 N3 C61 -35.1(14) . . . . ? Os8 Os7 N3 C61 155.9(12) . . . . ? Os9 Os7 N3 C61 -144.7(12) . . . . ? C65 N3 C61 C62 -0.8(17) . . . . ? Os7 N3 C61 C62 173.8(13) . . . . ? N3 C61 C62 C63 1.6(19) . . . . ? C61 C62 C63 C64 -2(3) . . . . ? C62 C63 C64 C65 2(4) . . . . ? C61 N3 C65 C64 1(3) . . . . ? Os7 N3 C65 C64 -174.1(14) . . . . ? C61 N3 C65 C66 176.1(16) . . . . ? Os7 N3 C65 C66 1(2) . . . . ? C63 C64 C65 N3 -1(3) . . . . ? C63 C64 C65 C66 -176(2) . . . . ? N3 C65 C66 C67 -179.7(17) . . . . ? C64 C65 C66 C67 -5(3) . . . . ? N3 C65 C66 Os8 43(2) . . . . ? C64 C65 C66 Os8 -141.6(18) . . . . ? N3 C65 C66 Os9 -48(2) . . . . ? C64 C65 C66 Os9 127.5(19) . . . . ? C44 Os8 C66 C67 -107.2(17) . . . . ? C46 Os8 C66 C67 129(4) . . . . ? C45 Os8 C66 C67 -14.1(18) . . . . ? C50 Os8 C66 C67 71.1(17) . . . . ? Os9 Os8 C66 C67 110.8(17) . . . . ? Os7 Os8 C66 C67 173.7(17) . . . . ? C44 Os8 C66 C65 29.4(17) . . . . ? C46 Os8 C66 C65 -94(4) . . . . ? C45 Os8 C66 C65 122.5(17) . . . . ? C50 Os8 C66 C65 -152.2(17) . . . . ? Os9 Os8 C66 C65 -112.5(17) . . . . ? Os7 Os8 C66 C65 -49.7(14) . . . . ? C44 Os8 C66 Os9 141.9(9) . . . . ? C46 Os8 C66 Os9 18(4) . . . . ? C45 Os8 C66 Os9 -125.0(9) . . . . ? C50 Os8 C66 Os9 -39.7(8) . . . . ? Os7 Os8 C66 Os9 62.9(4) . . . . ? C49 Os9 C66 C67 -130(4) . . . . ? C47 Os9 C66 C67 113.4(16) . . . . ? C48 Os9 C66 C67 15.2(16) . . . . ? C50 Os9 C66 C67 -70.6(15) . . . . ? Os8 Os9 C66 C67 -112.1(16) . . . . ? Os7 Os9 C66 C67 -175.0(15) . . . . ? C49 Os9 C66 C65 98(5) . . . . ? C47 Os9 C66 C65 -18.8(16) . . . . ? C48 Os9 C66 C65 -117.1(16) . . . . ? C50 Os9 C66 C65 157.2(16) . . . . ? Os8 Os9 C66 C65 115.7(17) . . . . ? Os7 Os9 C66 C65 52.8(14) . . . . ? C49 Os9 C66 Os8 -18(5) . . . . ? C47 Os9 C66 Os8 -134.5(8) . . . . ? C48 Os9 C66 Os8 127.2(9) . . . . ? C50 Os9 C66 Os8 41.5(7) . . . . ? Os7 Os9 C66 Os8 -62.9(4) . . . . ? C65 C66 C67 C68 -147(16) . . . . ? Os8 C66 C67 C68 -9(17) . . . . ? Os9 C66 C67 C68 80(17) . . . . ? C66 C67 C68 C69 160(16) . . . . ? C67 C68 C69 C70 166(18) . . . . ? C67 C68 C69 Os12 -60(20) . . . . ? C67 C68 C69 Os11 30(20) . . . . ? C57 Os12 C69 C68 -110.2(17) . . . . ? C59 Os12 C69 C68 126(4) . . . . ? C58 Os12 C69 C68 -16.0(17) . . . . ? C60 Os12 C69 C68 69.8(16) . . . . ? Os11 Os12 C69 C68 112.3(18) . . . . ? Os10 Os12 C69 C68 174.8(17) . . . . ? C57 Os12 C69 C70 23.8(16) . . . . ? C59 Os12 C69 C70 -100(4) . . . . ? C58 Os12 C69 C70 118.0(15) . . . . ? C60 Os12 C69 C70 -156.2(15) . . . . ? Os11 Os12 C69 C70 -113.7(16) . . . . ? Os10 Os12 C69 C70 -51.2(13) . . . . ? C57 Os12 C69 Os11 137.5(8) . . . . ? C59 Os12 C69 Os11 14(4) . . . . ? C58 Os12 C69 Os11 -128.3(8) . . . . ? C60 Os12 C69 Os11 -42.6(7) . . . . ? Os10 Os12 C69 Os11 62.4(4) . . . . ? C54 Os11 C69 C68 109.2(17) . . . . ? C55 Os11 C69 C68 14.4(17) . . . . ? C56 Os11 C69 C68 -118(4) . . . . ? C60 Os11 C69 C68 -70.8(16) . . . . ? Os12 Os11 C69 C68 -114.0(17) . . . . ? Os10 Os11 C69 C68 -176.7(16) . . . . ? C54 Os11 C69 C70 -24.9(18) . . . . ? C55 Os11 C69 C70 -119.7(17) . . . . ? C56 Os11 C69 C70 108(4) . . . . ? C60 Os11 C69 C70 155.1(17) . . . . ? Os12 Os11 C69 C70 111.9(18) . . . . ? Os10 Os11 C69 C70 49.2(15) . . . . ? C54 Os11 C69 Os12 -136.8(9) . . . . ? C55 Os11 C69 Os12 128.4(8) . . . . ? C56 Os11 C69 Os12 -4(4) . . . . ? C60 Os11 C69 Os12 43.2(7) . . . . ? Os10 Os11 C69 Os12 -62.7(4) . . . . ? C68 C69 C70 N4 -178.9(18) . . . . ? Os12 C69 C70 N4 45(2) . . . . ? Os11 C69 C70 N4 -44(2) . . . . ? C68 C69 C70 C71 3(3) . . . . ? Os12 C69 C70 C71 -132.7(14) . . . . ? Os11 C69 C70 C71 138.1(14) . . . . ? N4 C70 C71 C72 -1.1(17) . . . . ? C69 C70 C71 C72 176.9(19) . . . . ? C70 C71 C72 C73 0.3(18) . . . . ? C71 C72 C73 C74 2(3) . . . . ? C72 C73 C74 N4 -4(4) . . . . ? C73 C74 N4 C70 4(4) . . . . ? C73 C74 N4 Os10 -175(2) . . . . ? C71 C70 N4 C74 -1(3) . . . . ? C69 C70 N4 C74 -178.7(19) . . . . ? C71 C70 N4 Os10 178.4(12) . . . . ? C69 C70 N4 Os10 0(2) . . . . ? C52 Os10 N4 C74 -48(2) . . . . ? C51 Os10 N4 C74 48(2) . . . . ? C53 Os10 N4 C74 178(5) . . . . ? Os11 Os10 N4 C74 -152.5(19) . . . . ? Os12 Os10 N4 C74 148.4(19) . . . . ? C52 Os10 N4 C70 133.7(17) . . . . ? C51 Os10 N4 C70 -130.4(16) . . . . ? C53 Os10 N4 C70 -1(6) . . . . ? Os11 Os10 N4 C70 28.7(14) . . . . ? Os12 Os10 N4 C70 -30.4(14) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.961 _refine_diff_density_min -2.303 _refine_diff_density_rms 0.311 data_pr9701 _database_code_depnum_ccdc_archive 'CCDC 248102' _audit_creation_method SHELXL _chemical_name_systematic ; 'Compound 7' ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H10 N2 O20 Os6' _chemical_formula_weight 1907.64 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 21/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 11.211(4) _cell_length_b 19.277(4) _cell_length_c 19.435(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.13(2) _cell_angle_gamma 90.00 _cell_volume 4054.6(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.125 _exptl_crystal_density_method ? _exptl_crystal_F_000 3376 _exptl_absorpt_coefficient_mu 18.812 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.124 _exptl_absorpt_correction_T_max 0.152 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5R four-circle diffractometer' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -2 _diffrn_reflns_number 5609 _diffrn_reflns_av_R_equivalents 0.1145 _diffrn_reflns_av_sigmaI/netI 0.2232 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 22.54 _reflns_number_total 5294 _reflns_number_observed 2831 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXTL-PLUS (Siemens, 1991)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS (Siemens, 1991)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. Bridging hydride ligands located with HYDEX (A. G. Orpen, J. Chem. Soc., Dalton Trans., 2509, 1980). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w==1/[\s^2^(Fo^2^)+(0.0562P)^2^+44.7795P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5289 _refine_ls_number_parameters 279 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1858 _refine_ls_R_factor_obs 0.0636 _refine_ls_wR_factor_all 0.1995 _refine_ls_wR_factor_obs 0.1342 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.103 _refine_ls_restrained_S_all 1.174 _refine_ls_restrained_S_obs 1.100 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Os1 Os 0.02281(14) 0.83996(8) 0.52403(8) 0.0198(4) Uani 1 d . . Os2 Os 0.26998(15) 0.79073(9) 0.53087(8) 0.0226(4) Uani 1 d . . Os3 Os 0.07452(14) 0.68921(8) 0.52450(8) 0.0155(4) Uani 1 d . . H1 H -0.0517 0.7537 0.5089 0.040 Uiso 1 d . . Os4 Os -0.14241(14) 0.53065(8) 0.79039(8) 0.0174(4) Uani 1 d . . Os5 Os -0.27631(14) 0.50992(8) 0.64340(8) 0.0169(4) Uani 1 d . . Os6 Os -0.19100(13) 0.64704(8) 0.69243(8) 0.0135(4) Uani 1 d . . H2 H -0.1817 0.6241 0.7861 0.040 Uiso 1 d . . C11 C -0.1366(34) 0.8657(19) 0.5301(19) 0.020(5) Uiso 1 d U . O11 O -0.2296(29) 0.8829(16) 0.5428(16) 0.046(9) Uiso 1 d . . C12 C 0.0940(36) 0.9256(20) 0.5374(20) 0.023(5) Uiso 1 d U . O12 O 0.1317(30) 0.9845(17) 0.5540(16) 0.054(9) Uiso 1 d . . C13 C -0.0272(34) 0.8492(20) 0.4208(20) 0.020(5) Uiso 1 d U . O13 O -0.0610(25) 0.8587(15) 0.3593(15) 0.036(8) Uiso 1 d . . C21 C 0.3055(35) 0.7837(20) 0.6316(21) 0.023(10) Uiso 1 d . . O21 O 0.3433(28) 0.7796(16) 0.6957(16) 0.048(9) Uiso 1 d . . C22 C 0.2218(35) 0.8006(21) 0.4296(21) 0.025(10) Uiso 1 d . . O22 O 0.2017(29) 0.8063(17) 0.3702(17) 0.052(9) Uiso 1 d . . C23 C 0.4182(42) 0.7334(24) 0.5280(24) 0.039(12) Uiso 1 d . . O23 O 0.4910(29) 0.6945(17) 0.5286(16) 0.048(9) Uiso 1 d . . C24 C 0.3430(50) 0.8788(29) 0.5419(28) 0.061(16) Uiso 1 d . . O24 O 0.3942(31) 0.9316(17) 0.5491(17) 0.054(9) Uiso 1 d . . C31 C 0.2060(34) 0.6278(19) 0.5382(19) 0.019(5) Uiso 1 d U . O31 O 0.2825(29) 0.5822(17) 0.5428(16) 0.050(9) Uiso 1 d . . C32 C 0.0537(32) 0.6906(19) 0.4234(19) 0.017(5) Uiso 1 d U . O32 O 0.0309(26) 0.6866(15) 0.3602(15) 0.038(8) Uiso 1 d . . C33 C -0.0458(32) 0.6239(18) 0.5109(18) 0.014(5) Uiso 1 d U . O33 O -0.1218(22) 0.5749(12) 0.4953(12) 0.021(6) Uiso 1 d . . N41 N -0.0035(25) 0.6089(14) 0.7043(14) 0.010(7) Uiso 1 d . . C42 C 0.0163(33) 0.5549(19) 0.7490(19) 0.017(9) Uiso 1 d . . C43 C 0.1326(31) 0.5254(18) 0.7754(18) 0.013(8) Uiso 1 d . . H43 H 0.1452(31) 0.4926(18) 0.8131(18) 0.016 Uiso 1 calc R . C44 C 0.2298(35) 0.5431(19) 0.7479(19) 0.021(9) Uiso 1 d . . H44 H 0.3060(35) 0.5188(19) 0.7620(19) 0.025 Uiso 1 calc R . C45 C 0.2136(35) 0.5983(19) 0.6980(19) 0.021(10) Uiso 1 d . . H45 H 0.2785(35) 0.6114(19) 0.6775(19) 0.025 Uiso 1 calc R . C46 C 0.1010(32) 0.6329(18) 0.6797(18) 0.014(8) Uiso 1 d . . C47 C 0.0851(35) 0.6966(20) 0.6345(20) 0.023(10) Uiso 1 d . . C48 C 0.0848(34) 0.7599(20) 0.6698(19) 0.018(9) Uiso 1 d . . C49 C 0.0691(39) 0.8263(22) 0.6348(23) 0.034(11) Uiso 1 d . . C50 C 0.0823(38) 0.8732(23) 0.6891(22) 0.035(11) Uiso 1 d . . H50 H 0.0741(38) 0.9220(23) 0.6823(22) 0.042 Uiso 1 calc R . C51 C 0.1101(31) 0.8402(18) 0.7576(17) 0.011(8) Uiso 1 d . . C52 C 0.1397(36) 0.8671(22) 0.8273(21) 0.031(11) Uiso 1 d . . H52 H 0.1396(36) 0.9157(22) 0.8356(21) 0.038 Uiso 1 calc R . C53 C 0.1698(38) 0.8193(23) 0.8850(23) 0.036(12) Uiso 1 d . . H53 H 0.1908(38) 0.8351(23) 0.9329(23) 0.043 Uiso 1 calc R . C54 C 0.1678(33) 0.7545(19) 0.8704(19) 0.017(9) Uiso 1 d . . H54 H 0.1832(33) 0.7227(19) 0.9091(19) 0.021 Uiso 1 calc R . C55 C 0.1444(33) 0.7273(20) 0.8015(19) 0.020(9) Uiso 1 d . . H55 H 0.1528(33) 0.6792(20) 0.7932(19) 0.024 Uiso 1 calc R . N56 N 0.1095(26) 0.7728(14) 0.7479(15) 0.013(7) Uiso 1 d . . C60 C -0.1136(34) 0.4917(19) 0.6264(19) 0.017(9) Uiso 1 d . . O60 O -0.0231(23) 0.4786(13) 0.6132(13) 0.024(6) Uiso 1 d . . C61 C -0.3506(34) 0.5395(19) 0.5497(20) 0.020(9) Uiso 1 d . . O61 O -0.4004(27) 0.5534(15) 0.4922(15) 0.041(8) Uiso 1 d . . C62 C -0.4242(34) 0.5214(20) 0.6757(19) 0.020(9) Uiso 1 d . . O62 O -0.5133(28) 0.5313(16) 0.6938(15) 0.044(8) Uiso 1 d . . C63 C -0.3080(33) 0.4119(19) 0.6280(18) 0.015(9) Uiso 1 d . . O63 O -0.3294(29) 0.3565(16) 0.6184(16) 0.046(9) Uiso 1 d . . C70 C -0.1526(39) 0.7346(22) 0.7319(22) 0.030(11) Uiso 1 d . . O70 O -0.1438(27) 0.7902(16) 0.7514(15) 0.044(8) Uiso 1 d . . C71 C -0.2184(36) 0.6820(21) 0.5997(21) 0.025(10) Uiso 1 d . . O71 O -0.2473(23) 0.7077(14) 0.5443(14) 0.028(7) Uiso 1 d . . C72 C -0.3575(40) 0.6653(22) 0.6895(21) 0.031(11) Uiso 1 d . . O72 O -0.4525(28) 0.6803(16) 0.6928(15) 0.043(8) Uiso 1 d . . C80 C -0.0462(34) 0.5604(19) 0.8818(19) 0.018(9) Uiso 1 d . . O80 O 0.0203(32) 0.5799(18) 0.9346(18) 0.061(10) Uiso 1 d . . C81 C -0.2873(34) 0.5221(20) 0.8238(18) 0.018(9) Uiso 1 d . . O81 O -0.3644(29) 0.5170(16) 0.8529(16) 0.050(9) Uiso 1 d . . C82 C -0.1117(37) 0.4375(21) 0.7930(21) 0.027(10) Uiso 1 d . . O82 O -0.0886(29) 0.3772(16) 0.7984(16) 0.046(9) 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 Os1 0.0202(9) 0.0134(9) 0.0207(9) 0.0029(7) -0.0037(7) 0.0002(7) Os2 0.0177(9) 0.0279(10) 0.0199(9) -0.0007(8) 0.0010(7) -0.0060(8) Os3 0.0167(9) 0.0140(9) 0.0137(8) -0.0010(7) 0.0001(7) -0.0009(7) Os4 0.0184(9) 0.0175(9) 0.0157(8) 0.0031(7) 0.0036(7) 0.0034(7) Os5 0.0159(9) 0.0159(9) 0.0177(9) -0.0010(7) 0.0021(7) -0.0008(7) Os6 0.0122(8) 0.0141(9) 0.0135(8) 0.0005(7) 0.0020(7) 0.0049(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 C12 1.82(4) . ? Os1 C11 1.89(4) . ? Os1 C13 1.95(4) . ? Os1 C49 2.09(4) . ? Os1 Os2 2.899(2) . ? Os1 Os3 2.963(2) . ? Os2 C24 1.87(6) . ? Os2 C21 1.90(4) . ? Os2 C22 1.91(4) . ? Os2 C23 2.01(5) . ? Os2 Os3 2.916(2) . ? Os3 C33 1.81(4) . ? Os3 C31 1.85(4) . ? Os3 C32 1.92(4) . ? Os3 C47 2.11(4) . ? Os4 C82 1.83(4) . ? Os4 C81 1.91(4) . ? Os4 C80 1.91(4) . ? Os4 C42 2.19(4) . ? Os4 Os5 2.887(2) . ? Os4 Os6 2.901(2) . ? Os5 C61 1.88(4) . ? Os5 C63 1.93(4) . ? Os5 C62 1.93(4) . ? Os5 C60 1.97(4) . ? Os5 Os6 2.887(2) . ? Os6 C70 1.86(4) . ? Os6 C71 1.87(4) . ? Os6 C72 1.89(4) . ? Os6 N41 2.18(3) . ? C11 O11 1.18(4) . ? C12 O12 1.23(5) . ? C13 O13 1.17(4) . ? C21 O21 1.21(4) . ? C22 O22 1.12(4) . ? C23 O23 1.11(5) . ? C24 O24 1.16(6) . ? C31 O31 1.22(4) . ? C32 O32 1.19(4) . ? C33 O33 1.25(4) . ? N41 C42 1.34(4) . ? N41 C46 1.45(4) . ? C42 C43 1.39(5) . ? C43 C44 1.38(5) . ? C44 C45 1.42(5) . ? C45 C46 1.39(5) . ? C46 C47 1.49(5) . ? C47 C48 1.40(5) . ? C48 C49 1.44(5) . ? C48 N56 1.49(4) . ? C49 C50 1.37(5) . ? C50 C51 1.43(5) . ? C51 N56 1.31(4) . ? C51 C52 1.41(5) . ? C52 C53 1.42(5) . ? C53 C54 1.28(5) . ? C54 C55 1.40(5) . ? C55 N56 1.34(4) . ? C60 O60 1.14(4) . ? C61 O61 1.14(4) . ? C62 O62 1.16(4) . ? C63 O63 1.10(4) . ? C70 O70 1.13(4) . ? C71 O71 1.15(4) . ? C72 O72 1.12(5) . ? C80 O80 1.16(4) . ? C81 O81 1.15(4) . ? C82 O82 1.19(4) . ? 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 C12 Os1 C11 98.0(16) . . ? C12 Os1 C13 93.5(16) . . ? C11 Os1 C13 91.0(15) . . ? C12 Os1 C49 89.2(17) . . ? C11 Os1 C49 87.3(16) . . ? C13 Os1 C49 177.0(16) . . ? C12 Os1 Os2 85.0(12) . . ? C11 Os1 Os2 172.8(11) . . ? C13 Os1 Os2 95.3(11) . . ? C49 Os1 Os2 86.2(12) . . ? C12 Os1 Os3 144.1(12) . . ? C11 Os1 Os3 116.4(11) . . ? C13 Os1 Os3 95.5(11) . . ? C49 Os1 Os3 83.0(12) . . ? Os2 Os1 Os3 59.66(5) . . ? C24 Os2 C21 88.8(20) . . ? C24 Os2 C22 91.4(20) . . ? C21 Os2 C22 175.5(17) . . ? C24 Os2 C23 99.3(21) . . ? C21 Os2 C23 92.1(17) . . ? C22 Os2 C23 92.3(17) . . ? C24 Os2 Os1 95.3(17) . . ? C21 Os2 Os1 90.7(12) . . ? C22 Os2 Os1 84.9(12) . . ? C23 Os2 Os1 165.2(13) . . ? C24 Os2 Os3 156.1(17) . . ? C21 Os2 Os3 87.1(12) . . ? C22 Os2 Os3 90.9(12) . . ? C23 Os2 Os3 104.3(13) . . ? Os1 Os2 Os3 61.26(6) . . ? C33 Os3 C31 96.4(16) . . ? C33 Os3 C32 88.5(15) . . ? C31 Os3 C32 92.0(16) . . ? C33 Os3 C47 92.2(15) . . ? C31 Os3 C47 93.7(15) . . ? C32 Os3 C47 174.1(15) . . ? C33 Os3 Os2 173.8(11) . . ? C31 Os3 Os2 82.0(11) . . ? C32 Os3 Os2 85.6(11) . . ? C47 Os3 Os2 93.9(10) . . ? C33 Os3 Os1 122.9(11) . . ? C31 Os3 Os1 140.7(11) . . ? C32 Os3 Os1 90.7(11) . . ? C47 Os3 Os1 84.1(11) . . ? Os2 Os3 Os1 59.08(6) . . ? C82 Os4 C81 94.4(17) . . ? C82 Os4 C80 102.3(17) . . ? C81 Os4 C80 91.9(15) . . ? C82 Os4 C42 93.1(16) . . ? C81 Os4 C42 172.3(15) . . ? C80 Os4 C42 87.8(14) . . ? C82 Os4 Os5 86.4(12) . . ? C81 Os4 Os5 93.2(10) . . ? C80 Os4 Os5 169.5(11) . . ? C42 Os4 Os5 85.9(9) . . ? C82 Os4 Os6 141.3(12) . . ? C81 Os4 Os6 105.0(11) . . ? C80 Os4 Os6 110.0(11) . . ? C42 Os4 Os6 68.0(9) . . ? Os5 Os4 Os6 59.84(5) . . ? C61 Os5 C63 97.4(15) . . ? C61 Os5 C62 94.6(15) . . ? C63 Os5 C62 91.3(15) . . ? C61 Os5 C60 95.0(15) . . ? C63 Os5 C60 86.6(15) . . ? C62 Os5 C60 170.4(15) . . ? C61 Os5 Os6 93.8(11) . . ? C63 Os5 Os6 168.1(10) . . ? C62 Os5 Os6 91.5(11) . . ? C60 Os5 Os6 88.7(11) . . ? C61 Os5 Os4 154.1(11) . . ? C63 Os5 Os4 108.4(10) . . ? C62 Os5 Os4 86.1(10) . . ? C60 Os5 Os4 85.7(10) . . ? Os6 Os5 Os4 60.31(5) . . ? C70 Os6 C71 91.8(17) . . ? C70 Os6 C72 87.9(18) . . ? C71 Os6 C72 89.5(17) . . ? C70 Os6 N41 98.6(15) . . ? C71 Os6 N41 97.7(14) . . ? C72 Os6 N41 170.1(15) . . ? C70 Os6 Os5 171.7(13) . . ? C71 Os6 Os5 93.2(12) . . ? C72 Os6 Os5 85.5(13) . . ? N41 Os6 Os5 87.3(7) . . ? C70 Os6 Os4 116.6(12) . . ? C71 Os6 Os4 150.0(12) . . ? C72 Os6 Os4 100.3(13) . . ? N41 Os6 Os4 70.1(7) . . ? Os5 Os6 Os4 59.85(5) . . ? O11 C11 Os1 171.8(32) . . ? O12 C12 Os1 170.1(35) . . ? O13 C13 Os1 175.6(34) . . ? O21 C21 Os2 171.9(34) . . ? O22 C22 Os2 175.3(36) . . ? O23 C23 Os2 170.4(41) . . ? O24 C24 Os2 176.4(48) . . ? O31 C31 Os3 172.5(33) . . ? O32 C32 Os3 173.1(32) . . ? O33 C33 Os3 171.9(30) . . ? C42 N41 C46 116.8(29) . . ? C42 N41 Os6 108.8(22) . . ? C46 N41 Os6 134.1(22) . . ? N41 C42 C43 122.5(33) . . ? N41 C42 Os4 113.1(24) . . ? C43 C42 Os4 123.5(26) . . ? C44 C43 C42 121.1(34) . . ? C43 C44 C45 118.6(36) . . ? C46 C45 C44 118.7(35) . . ? C45 C46 N41 121.4(32) . . ? C45 C46 C47 120.4(33) . . ? N41 C46 C47 118.3(30) . . ? C48 C47 C46 116.3(32) . . ? C48 C47 Os3 123.2(28) . . ? C46 C47 Os3 120.4(26) . . ? C47 C48 C49 124.0(34) . . ? C47 C48 N56 128.4(33) . . ? C49 C48 N56 107.5(32) . . ? C50 C49 C48 104.3(36) . . ? C50 C49 Os1 131.1(33) . . ? C48 C49 Os1 124.4(30) . . ? C49 C50 C51 112.1(39) . . ? N56 C51 C52 119.7(33) . . ? N56 C51 C50 108.3(32) . . ? C52 C51 C50 132.0(36) . . ? C51 C52 C53 117.9(38) . . ? C54 C53 C52 118.1(41) . . ? C53 C54 C55 124.4(40) . . ? N56 C55 C54 116.3(34) . . ? C51 N56 C55 123.1(31) . . ? C51 N56 C48 107.8(29) . . ? C55 N56 C48 128.4(30) . . ? O60 C60 Os5 175.8(32) . . ? O61 C61 Os5 175.2(35) . . ? O62 C62 Os5 176.8(35) . . ? O63 C63 Os5 178.0(36) . . ? O70 C70 Os6 171.4(39) . . ? O71 C71 Os6 171.7(34) . . ? O72 C72 Os6 173.6(38) . . ? O80 C80 Os4 174.1(34) . . ? O81 C81 Os4 171.0(32) . . ? O82 C82 Os4 176.6(36) . . ? _refine_diff_density_max 2.307 _refine_diff_density_min -2.261 _refine_diff_density_rms 0.520