Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_os3chira _database_code_CSD 183148 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'A. J. Deeming' 'C. S. Forth' 'G. Hogarth' 'D. Markham' 'J. O. Prince' 'J. W. Steed' _publ_contact_author_name 'Prof A Deeming' _publ_contact_author_address ; Department of Chemistry University College London 20 Gordon Street LONDON WC1H OAJ U.K. ; _publ_contact_author_email 'A.J.DEEMING@UCL.AC.UK' _publ_section_title ; Slow Epimerisation of stereochemically rigid diastereomers of the equatorially substitute cluster [Os3H2(u3-S)(CO)8{(S)-PhCHMeNH2}] ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H13 N O8 Os3 S' _chemical_formula_weight 949.93 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.4018(4) _cell_length_b 20.5782(11) _cell_length_c 11.5621(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.605(3) _cell_angle_gamma 90.00 _cell_volume 2226.25(18) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 17.213 _exptl_absorpt_correction_type scaleapck _exptl_absorpt_correction_T_min 0.0788 _exptl_absorpt_correction_T_max 0.0990 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 KAPPACCD _diffrn_measurement_method '1.5o phi & omega frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11460 _diffrn_reflns_av_R_equivalents 0.1607 _diffrn_reflns_av_sigmaI/netI 0.1769 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 24.99 _reflns_number_total 7126 _reflns_number_gt 6544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _computing_publication_material ? _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^)+(0.0868P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00171(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 7126 _refine_ls_number_parameters 526 _refine_ls_number_restraints 457 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1781 _refine_ls_wR_factor_gt 0.1731 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.009 _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 1.19018(9) 0.64521(5) 0.15888(8) 0.0051(3) Uani 1 1 d U . . S1 S 1.2616(6) 0.5754(3) 0.3209(5) 0.0047(12) Uani 1 1 d . . . O1 O 0.8679(18) 0.6386(11) 0.165(2) 0.027(5) Uani 1 1 d U . . N1 N 1.206(3) 0.5593(14) 0.052(2) 0.027(6) Uani 1 1 d U . . H1N H 1.2945 0.5416 0.0736 0.033 Uiso 1 1 calc R . . H12 H 1.1399 0.5302 0.0751 0.033 Uiso 1 1 calc R . . C1 C 1.188(3) 0.5601(17) -0.077(2) 0.021(7) Uani 1 1 d U . . H1 H 1.2553 0.5934 -0.1043 0.025 Uiso 1 1 calc R . . Os2 Os 1.47676(8) 0.62730(5) 0.27538(8) 0.0043(3) Uani 1 1 d U . . S2 S 0.6031(6) 0.9213(3) 0.8458(5) 0.0090(14) Uani 1 1 d . . . O2 O 1.172(2) 0.7493(11) -0.0260(18) 0.022(5) Uani 1 1 d U . . N2 N 0.623(2) 0.9272(11) 0.5697(17) 0.008(4) Uani 1 1 d U . . H3N H 0.5290 0.9395 0.5727 0.010 Uiso 1 1 calc R . . H4N H 0.6782 0.9620 0.5959 0.010 Uiso 1 1 calc R . . C2 C 1.231(4) 0.495(2) -0.122(3) 0.036(8) Uani 1 1 d U . . H2A H 1.3137 0.4787 -0.0725 0.054 Uiso 1 1 calc R . . H2B H 1.2554 0.4996 -0.2018 0.054 Uiso 1 1 calc R . . H2C H 1.1510 0.4646 -0.1198 0.054 Uiso 1 1 calc R . . Os3 Os 1.26694(9) 0.68394(5) 0.39471(8) 0.0062(3) Uani 1 1 d U . . O3 O 1.634(2) 0.5413(10) 0.1095(18) 0.021(5) Uani 1 1 d U . . C3 C 1.041(3) 0.5787(15) -0.123(3) 0.017(6) Uani 1 1 d U . . Os4 Os 0.66363(9) 0.85154(5) 0.69241(8) 0.0064(3) Uani 1 1 d U . . O4 O 1.6602(19) 0.5887(10) 0.4954(16) 0.015(4) Uani 1 1 d U . . C4 C 1.010(3) 0.6293(16) -0.197(2) 0.022(7) Uani 1 1 d U . . H4 H 1.0861 0.6566 -0.2156 0.026 Uiso 1 1 calc R . . Os5 Os 0.60077(10) 0.81445(5) 0.92257(9) 0.0093(3) Uani 1 1 d U . . O5 O 1.663(2) 0.7461(10) 0.2444(18) 0.019(5) Uani 1 1 d U . . C5 C 0.873(5) 0.643(3) -0.244(4) 0.070(14) Uani 1 1 d U . . H5 H 0.8561 0.6756 -0.3022 0.084 Uiso 1 1 calc R . . Os6 Os 0.38399(9) 0.86905(5) 0.77480(8) 0.0055(3) Uani 1 1 d U . . O6 O 1.419(2) 0.6517(12) 0.6362(17) 0.028(5) Uani 1 1 d U . . C6 C 0.769(5) 0.611(3) -0.210(4) 0.059(12) Uani 1 1 d U . . H6 H 0.6748 0.6217 -0.2405 0.071 Uiso 1 1 calc R . . O7 O 0.972(2) 0.7014(13) 0.478(2) 0.037(6) Uani 1 1 d U . . C7 C 0.784(4) 0.567(2) -0.140(3) 0.035(8) Uani 1 1 d U . . H7 H 0.7018 0.5482 -0.1107 0.042 Uiso 1 1 calc R . . O8 O 1.363(2) 0.8242(12) 0.405(2) 0.034(6) Uani 1 1 d U . . C8 C 0.927(3) 0.5423(18) -0.098(3) 0.026(7) Uani 1 1 d U . . H8 H 0.9397 0.5027 -0.0560 0.031 Uiso 1 1 calc R . . O9 O 0.981(2) 0.8731(13) 0.724(2) 0.031(5) Uani 1 1 d U . . C9 C 0.987(3) 0.6434(16) 0.156(2) 0.018(6) Uani 1 1 d U . . O10 O 0.675(2) 0.7412(12) 0.5170(18) 0.024(5) Uani 1 1 d U . . C10 C 1.174(2) 0.7104(12) 0.041(2) 0.001(5) Uani 1 1 d U . . O2N O 0.490(2) 0.6742(11) 0.9235(18) 0.024(5) Uani 1 1 d U . . C11 C 1.569(3) 0.5710(14) 0.170(2) 0.013(6) Uani 1 1 d U . . O12 O 0.459(2) 0.8487(13) 1.1365(17) 0.031(5) Uani 1 1 d U . . C12 C 1.590(3) 0.6036(15) 0.412(2) 0.012(6) Uani 1 1 d U . . O13 O 0.895(2) 0.7935(12) 1.0624(17) 0.024(5) Uani 1 1 d U . . C13 C 1.590(2) 0.7043(12) 0.261(2) 0.004(5) Uani 1 1 d U . . O14 O 0.193(2) 0.7551(12) 0.7007(19) 0.028(5) Uani 1 1 d U . . C14 C 1.360(3) 0.6667(14) 0.546(2) 0.012(6) Uani 1 1 d U . . O15 O 0.208(3) 0.9085(13) 0.9700(19) 0.035(6) Uani 1 1 d U . . C15 C 1.081(3) 0.6920(17) 0.446(3) 0.025(7) Uani 1 1 d U . . O16 O 0.228(2) 0.9748(12) 0.622(2) 0.033(6) Uani 1 1 d U . . C16 C 1.323(3) 0.7724(14) 0.404(2) 0.009(5) Uani 1 1 d U . . C17 C 0.644(3) 0.9180(15) 0.442(2) 0.012(6) Uani 1 1 d U . . H17 H 0.6084 0.8739 0.4176 0.014 Uiso 1 1 calc R . . C18 C 0.548(3) 0.9709(18) 0.371(3) 0.032(8) Uani 1 1 d U . . H18A H 0.4472 0.9577 0.3667 0.048 Uiso 1 1 calc R . . H18B H 0.5771 0.9744 0.2919 0.048 Uiso 1 1 calc R . . H18C H 0.5597 1.0131 0.4097 0.048 Uiso 1 1 calc R . . C19 C 0.799(3) 0.9245(13) 0.412(2) 0.007(5) Uani 1 1 d U . . C20 C 0.857(3) 0.8742(18) 0.371(3) 0.029(8) Uani 1 1 d U . . H20 H 0.8026 0.8353 0.3623 0.034 Uiso 1 1 calc R . . C21 C 0.997(3) 0.8736(18) 0.339(3) 0.026(7) Uani 1 1 d U . . H21 H 1.0375 0.8355 0.3097 0.031 Uiso 1 1 calc R . . C22 C 1.076(3) 0.9328(16) 0.354(2) 0.020(6) Uani 1 1 d U . . H22 H 1.1698 0.9356 0.3307 0.024 Uiso 1 1 calc R . . C23 C 1.013(3) 0.9868(14) 0.402(2) 0.009(5) Uani 1 1 d U . . H23 H 1.0637 1.0265 0.4143 0.011 Uiso 1 1 calc R . . C24 C 0.872(2) 0.9802(12) 0.4328(19) 0.002(5) Uani 1 1 d U . . H24 H 0.8275 1.0155 0.4686 0.002 Uiso 1 1 calc R . . C25 C 0.679(3) 0.7836(15) 0.579(2) 0.012(6) Uani 1 1 d U . . C26 C 0.864(3) 0.8651(17) 0.713(3) 0.023(7) Uani 1 1 d U . . C27 C 0.528(3) 0.7246(15) 0.919(2) 0.014(6) Uani 1 1 d U . . C28 C 0.510(3) 0.8357(16) 1.057(3) 0.021(7) Uani 1 1 d U . . C29 C 0.790(3) 0.8023(15) 1.006(2) 0.014(6) Uani 1 1 d U . . C30 C 0.264(2) 0.7954(12) 0.7250(19) 0.003(5) Uani 1 1 d U . . C31 C 0.277(3) 0.8946(16) 0.900(3) 0.021(7) Uani 1 1 d U . . C32 C 0.291(3) 0.9327(14) 0.674(2) 0.012(6) Uani 1 1 d U . . H1H H 1.3807 0.6568 0.1373 0.014 Uiso 1 1 d R . . H4H H 0.6897 0.7843 0.7973 0.014 Uiso 1 1 d R . . H3H H 0.4706 0.8399 0.6478 0.014 Uiso 1 1 d R . . H2H H 1.1779 0.7163 0.2558 0.014 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0014(4) 0.0069(5) 0.0066(4) 0.0000(4) -0.0014(3) 0.0019(3) S1 0.004(3) 0.003(3) 0.007(3) -0.001(3) 0.001(2) 0.001(2) O1 0.004(7) 0.020(10) 0.054(11) -0.003(10) -0.009(8) 0.003(7) N1 0.031(11) 0.022(12) 0.025(11) -0.010(10) -0.018(9) 0.013(9) C1 0.013(10) 0.031(13) 0.017(11) -0.008(11) -0.001(9) 0.017(10) Os2 0.0007(4) 0.0058(5) 0.0061(5) -0.0004(4) -0.0007(3) 0.0017(4) S2 0.005(3) 0.013(4) 0.007(3) -0.004(3) -0.004(2) 0.006(3) O2 0.019(9) 0.019(10) 0.028(9) 0.001(9) -0.007(8) 0.007(8) N2 0.009(6) 0.009(6) 0.007(6) -0.002(4) 0.004(4) 0.002(4) C2 0.044(13) 0.047(15) 0.016(11) -0.023(11) -0.009(11) 0.018(12) Os3 0.0035(4) 0.0069(6) 0.0083(5) -0.0024(4) 0.0011(4) 0.0013(4) O3 0.020(8) 0.016(10) 0.028(9) 0.002(9) 0.010(8) -0.007(8) C3 0.016(10) 0.012(12) 0.022(11) -0.008(10) -0.003(10) 0.003(9) Os4 0.0018(4) 0.0070(6) 0.0106(5) 0.0003(5) 0.0023(4) -0.0006(4) O4 0.014(5) 0.015(5) 0.015(5) 0.000(3) 0.000(3) 0.001(3) C4 0.035(12) 0.012(12) 0.017(11) 0.008(11) -0.010(10) 0.005(10) Os5 0.0087(5) 0.0101(6) 0.0091(5) 0.0025(5) 0.0013(4) 0.0059(4) O5 0.021(9) 0.009(9) 0.026(9) 0.008(8) -0.005(8) -0.005(7) C5 0.077(18) 0.067(19) 0.064(18) 0.001(14) -0.006(13) 0.015(13) Os6 0.0017(4) 0.0052(6) 0.0095(5) 0.0027(4) 0.0003(4) 0.0005(4) O6 0.039(10) 0.026(11) 0.015(8) -0.017(9) -0.018(8) 0.011(9) C6 0.052(15) 0.073(18) 0.051(16) -0.014(13) -0.005(12) 0.016(13) O7 0.009(8) 0.053(12) 0.050(11) 0.012(10) 0.012(9) 0.013(8) C7 0.030(12) 0.052(15) 0.026(12) -0.013(12) 0.017(11) 0.001(11) O8 0.028(9) 0.023(11) 0.050(11) -0.008(10) -0.002(9) -0.006(9) C8 0.015(11) 0.035(14) 0.027(12) 0.000(11) 0.003(10) -0.009(10) O9 0.005(8) 0.043(12) 0.045(11) 0.007(10) 0.005(8) -0.009(8) C9 0.018(7) 0.018(7) 0.019(7) -0.002(5) 0.000(4) -0.002(4) O10 0.024(9) 0.031(11) 0.019(9) -0.009(9) 0.006(8) 0.003(8) C10 0.001(5) 0.001(5) 0.001(5) 0.000(2) 0.000(2) 0.000(2) O2N 0.025(9) 0.024(11) 0.027(9) -0.001(9) 0.020(8) 0.005(8) C11 0.010(7) 0.014(7) 0.015(7) 0.003(5) -0.002(4) 0.000(4) O12 0.033(10) 0.045(12) 0.016(8) -0.011(9) 0.009(8) 0.018(9) C12 0.012(7) 0.013(7) 0.011(7) -0.003(4) 0.000(4) 0.000(4) O13 0.020(9) 0.029(11) 0.021(9) 0.004(9) -0.001(8) 0.008(8) C13 0.003(5) 0.004(6) 0.004(5) 0.001(3) -0.002(3) -0.001(3) O14 0.027(6) 0.028(6) 0.029(6) 0.000(3) 0.004(3) -0.002(3) C14 0.010(7) 0.011(7) 0.014(7) -0.002(4) 0.001(4) 0.003(4) O15 0.036(10) 0.046(12) 0.027(10) -0.012(10) 0.015(9) -0.006(9) C15 0.026(12) 0.025(13) 0.023(11) 0.012(11) -0.003(10) -0.008(10) O16 0.033(10) 0.020(11) 0.044(11) 0.013(10) -0.012(9) 0.004(8) C16 0.007(6) 0.010(7) 0.012(6) -0.003(4) 0.000(4) 0.001(4) C17 0.012(7) 0.013(7) 0.011(7) 0.000(4) 0.001(4) -0.005(4) C18 0.027(12) 0.035(14) 0.033(13) -0.002(12) -0.003(11) 0.001(11) C19 0.008(6) 0.006(7) 0.006(6) 0.001(4) 0.000(4) 0.000(4) C20 0.021(11) 0.036(14) 0.030(12) 0.006(11) 0.008(10) -0.004(11) C21 0.017(11) 0.031(13) 0.029(12) -0.009(11) -0.005(10) -0.004(10) C22 0.021(11) 0.025(13) 0.013(10) 0.006(11) 0.004(9) -0.001(10) C23 0.010(6) 0.010(7) 0.007(6) 0.002(4) 0.002(4) -0.002(4) C24 0.002(5) 0.002(5) 0.001(5) 0.000(3) 0.000(3) 0.000(3) C25 0.005(9) 0.012(12) 0.017(11) 0.003(10) -0.007(9) -0.002(9) C26 0.019(11) 0.028(13) 0.022(11) -0.001(11) -0.004(9) -0.002(10) C27 0.023(11) 0.006(11) 0.014(10) -0.008(10) 0.012(9) -0.010(9) C28 0.021(7) 0.020(8) 0.022(8) 0.000(5) -0.002(5) 0.004(4) C29 0.013(10) 0.020(12) 0.009(10) -0.002(10) 0.002(9) 0.001(9) C30 0.003(5) 0.002(5) 0.003(5) 0.000(3) 0.000(3) -0.001(3) C31 0.017(11) 0.017(12) 0.026(12) 0.012(11) -0.009(10) 0.004(9) C32 0.011(7) 0.013(7) 0.011(7) 0.003(5) 0.000(4) 0.002(4) _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 C10 1.91(2) . ? Os1 C9 1.91(3) . ? Os1 N1 2.17(3) . ? Os1 S1 2.404(6) . ? Os1 Os3 2.8647(13) . ? Os1 Os2 2.9155(12) . ? S1 Os3 2.390(6) . ? S1 Os2 2.391(6) . ? O1 C9 1.14(3) . ? N1 C1 1.49(4) . ? C1 C3 1.48(4) . ? C1 C2 1.50(5) . ? Os2 C12 1.88(3) . ? Os2 C13 1.92(2) . ? Os2 C11 1.94(3) . ? Os2 Os3 2.7723(12) . ? S2 Os5 2.372(7) . ? S2 Os4 2.394(6) . ? S2 Os6 2.397(6) . ? O2 C10 1.11(3) . ? N2 C17 1.52(3) . ? N2 Os4 2.12(2) . ? Os3 C16 1.90(3) . ? Os3 C15 1.91(3) . ? Os3 C14 1.91(3) . ? O3 C11 1.15(3) . ? C3 C4 1.35(4) . ? C3 C8 1.36(4) . ? Os4 C26 1.90(3) . ? Os4 C25 1.93(3) . ? Os4 Os5 2.8846(14) . ? Os4 Os6 2.9050(12) . ? O4 C12 1.16(3) . ? C4 C5 1.38(6) . ? Os5 C28 1.90(3) . ? Os5 C29 1.96(3) . ? Os5 C27 1.97(3) . ? Os5 Os6 2.7669(14) . ? O5 C13 1.13(3) . ? C5 C6 1.28(7) . ? Os6 C32 1.91(3) . ? Os6 C31 1.91(3) . ? Os6 C30 1.95(2) . ? O6 C14 1.17(3) . ? C6 C7 1.21(6) . ? O7 C15 1.14(4) . ? C7 C8 1.48(5) . ? O8 C16 1.13(4) . ? O9 C26 1.11(4) . ? O10 C25 1.13(3) . ? O2N C27 1.10(4) . ? O12 C28 1.11(3) . ? O13 C29 1.14(3) . ? O14 C30 1.08(3) . ? O15 C31 1.12(4) . ? O16 C32 1.18(4) . ? C17 C19 1.54(3) . ? C17 C18 1.59(4) . ? C19 C20 1.28(4) . ? C19 C24 1.35(4) . ? C20 C21 1.40(4) . ? C21 C22 1.43(5) . ? C22 C23 1.40(4) . ? C23 C24 1.41(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 C10 Os1 C9 89.5(11) . . ? C10 Os1 N1 99.9(10) . . ? C9 Os1 N1 95.6(12) . . ? C10 Os1 S1 166.8(7) . . ? C9 Os1 S1 101.9(9) . . ? N1 Os1 S1 85.8(7) . . ? C10 Os1 Os3 118.6(7) . . ? C9 Os1 Os3 100.5(8) . . ? N1 Os1 Os3 138.0(7) . . ? S1 Os1 Os3 53.09(15) . . ? C10 Os1 Os2 115.1(7) . . ? C9 Os1 Os2 152.2(9) . . ? N1 Os1 Os2 92.7(7) . . ? S1 Os1 Os2 52.35(14) . . ? Os3 Os1 Os2 57.31(3) . . ? Os3 S1 Os2 70.88(17) . . ? Os3 S1 Os1 73.39(18) . . ? Os2 S1 Os1 74.89(18) . . ? C1 N1 Os1 124(2) . . ? C3 C1 N1 112(2) . . ? C3 C1 C2 112(3) . . ? N1 C1 C2 109(3) . . ? C12 Os2 C13 91.0(11) . . ? C12 Os2 C11 96.9(11) . . ? C13 Os2 C11 98.7(11) . . ? C12 Os2 S1 96.8(8) . . ? C13 Os2 S1 150.9(7) . . ? C11 Os2 S1 108.0(8) . . ? C12 Os2 Os3 93.5(8) . . ? C13 Os2 Os3 97.1(7) . . ? C11 Os2 Os3 160.8(8) . . ? S1 Os2 Os3 54.55(15) . . ? C12 Os2 Os1 147.3(8) . . ? C13 Os2 Os1 110.4(7) . . ? C11 Os2 Os1 103.6(8) . . ? S1 Os2 Os1 52.75(15) . . ? Os3 Os2 Os1 60.42(3) . . ? Os5 S2 Os4 74.5(2) . . ? Os5 S2 Os6 70.9(2) . . ? Os4 S2 Os6 74.66(19) . . ? C17 N2 Os4 121.8(17) . . ? C16 Os3 C15 99.0(13) . . ? C16 Os3 C14 91.4(12) . . ? C15 Os3 C14 94.6(12) . . ? C16 Os3 S1 156.1(7) . . ? C15 Os3 S1 101.8(11) . . ? C14 Os3 S1 98.4(9) . . ? C16 Os3 Os2 103.0(7) . . ? C15 Os3 Os2 155.5(10) . . ? C14 Os3 Os2 95.5(7) . . ? S1 Os3 Os2 54.58(14) . . ? C16 Os3 Os1 111.5(8) . . ? C15 Os3 Os1 99.6(9) . . ? C14 Os3 Os1 150.5(8) . . ? S1 Os3 Os1 53.53(15) . . ? Os2 Os3 Os1 62.27(3) . . ? C4 C3 C8 116(3) . . ? C4 C3 C1 124(3) . . ? C8 C3 C1 120(3) . . ? C26 Os4 C25 93.1(12) . . ? C26 Os4 N2 95.2(12) . . ? C25 Os4 N2 95.6(10) . . ? C26 Os4 S2 97.1(10) . . ? C25 Os4 S2 167.4(8) . . ? N2 Os4 S2 90.8(6) . . ? C26 Os4 Os5 102.3(9) . . ? C25 Os4 Os5 118.0(8) . . ? N2 Os4 Os5 140.6(5) . . ? S2 Os4 Os5 52.41(17) . . ? C26 Os4 Os6 149.3(10) . . ? C25 Os4 Os6 116.2(7) . . ? N2 Os4 Os6 91.0(5) . . ? S2 Os4 Os6 52.71(15) . . ? Os5 Os4 Os6 57.10(3) . . ? C3 C4 C5 123(4) . . ? C28 Os5 C29 94.9(12) . . ? C28 Os5 C27 92.8(12) . . ? C29 Os5 C27 100.9(13) . . ? C28 Os5 S2 96.6(10) . . ? C29 Os5 S2 105.2(9) . . ? C27 Os5 S2 151.4(9) . . ? C28 Os5 Os6 93.0(9) . . ? C29 Os5 Os6 159.4(9) . . ? C27 Os5 Os6 97.7(9) . . ? S2 Os5 Os6 54.95(15) . . ? C28 Os5 Os4 147.7(10) . . ? C29 Os5 Os4 103.2(8) . . ? C27 Os5 Os4 109.4(8) . . ? S2 Os5 Os4 53.10(15) . . ? Os6 Os5 Os4 61.82(3) . . ? C6 C5 C4 119(5) . . ? C32 Os6 C31 91.5(11) . . ? C32 Os6 C30 97.8(11) . . ? C31 Os6 C30 96.0(12) . . ? C32 Os6 S2 103.3(9) . . ? C31 Os6 S2 96.7(9) . . ? C30 Os6 S2 155.1(7) . . ? C32 Os6 Os5 157.3(8) . . ? C31 Os6 Os5 93.2(8) . . ? C30 Os6 Os5 103.8(7) . . ? S2 Os6 Os5 54.12(17) . . ? C32 Os6 Os4 105.2(7) . . ? C31 Os6 Os4 147.3(9) . . ? C30 Os6 Os4 109.0(6) . . ? S2 Os6 Os4 52.63(15) . . ? Os5 Os6 Os4 61.08(3) . . ? C7 C6 C5 124(5) . . ? C6 C7 C8 121(4) . . ? C3 C8 C7 117(3) . . ? O1 C9 Os1 173(3) . . ? O2 C10 Os1 176(2) . . ? O3 C11 Os2 174(2) . . ? O4 C12 Os2 179(2) . . ? O5 C13 Os2 173(2) . . ? O6 C14 Os3 175(2) . . ? O7 C15 Os3 175(3) . . ? O8 C16 Os3 175(2) . . ? N2 C17 C19 116(2) . . ? N2 C17 C18 107(2) . . ? C19 C17 C18 109(2) . . ? C20 C19 C24 122(3) . . ? C20 C19 C17 118(3) . . ? C24 C19 C17 120(2) . . ? C19 C20 C21 123(3) . . ? C20 C21 C22 117(3) . . ? C23 C22 C21 119(3) . . ? C22 C23 C24 118(3) . . ? C19 C24 C23 120(2) . . ? O10 C25 Os4 173(2) . . ? O9 C26 Os4 179(3) . . ? O2N C27 Os5 176(3) . . ? O12 C28 Os5 179(3) . . ? O13 C29 Os5 174(2) . . ? O14 C30 Os6 177(2) . . ? O15 C31 Os6 177(3) . . ? O16 C32 Os6 173(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N S2 0.92 2.78 3.50(3) 135.8 2_746 N2 H4N S1 0.92 2.57 3.44(2) 158.2 2_756 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.964 _refine_diff_density_min -3.821 _refine_diff_density_rms 0.563