# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Sreebrata Goswami' 'Radka Bakova' 'Sudipta Chatterjee' 'Jan Fiedler' 'W Kaim' 'Priti Singh' 'Stanislav Zalis' _publ_contact_author_name 'Sreebrata Goswami' _publ_contact_author_email ICSG@IACS.RES.IN _publ_section_title ; Effect of metal exchange (Os vs Ru) and co-ligand variation (Cl- vs acac-) on the oxidation state distribution in complexes of an o-phenylenediamido(2-)/ ; # Attachment 'Os_1.cif' data_Os_1 _database_code_depnum_ccdc_archive 'CCDC 726829' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2 (C24 H20 Cl2 N4 Os), C H2 Cl2' _chemical_formula_sum 'C24.5 H21 Cl3 N4 Os' _chemical_formula_weight 668.04 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' Cl Cl 0.1484 0.1585 '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' 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 12.7015(15) _cell_length_b 13.7738(16) _cell_length_c 14.8971(18) _cell_angle_alpha 95.768(7) _cell_angle_beta 92.310(2) _cell_angle_gamma 111.019(5) _cell_volume 2412.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16149 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 28.4 _exptl_crystal_description Square _exptl_crystal_colour Brown _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 5.639 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.352 _exptl_absorpt_correction_T_max 0.449 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16149 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.35 _reflns_number_total 11301 _reflns_number_gt 9254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX V1.70.01' _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^)+(0.0406P)^2^+20.3809P] 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 11301 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C19 C 0.2572(6) 0.5403(5) 0.4925(5) 0.0162(14) Uani 1 1 d . . . C20 C 0.3368(6) 0.6203(6) 0.4558(5) 0.0201(15) Uani 1 1 d . . . H20 H 0.3563 0.6092 0.3972 0.024 Uiso 1 1 calc R . . C40 C -0.0701(7) 0.3855(6) -0.1194(5) 0.0229(17) Uani 1 1 d . . . H40 H -0.0692 0.4505 -0.1321 0.027 Uiso 1 1 calc R . . C23 C 0.2760(7) 0.6538(6) 0.6287(5) 0.0262(18) Uani 1 1 d . . . H23 H 0.2547 0.6649 0.6867 0.031 Uiso 1 1 calc R . . C38 C 0.0126(6) 0.2863(5) -0.0343(5) 0.0171(15) Uani 1 1 d . . . H38 H 0.0662 0.2831 0.0085 0.021 Uiso 1 1 calc R . . C39 C 0.0135(7) 0.3816(6) -0.0543(5) 0.0228(16) Uani 1 1 d . . . H39 H 0.0682 0.4433 -0.0258 0.027 Uiso 1 1 calc R . . C22 C 0.3557(6) 0.7351(6) 0.5937(6) 0.0243(17) Uani 1 1 d . . . H22 H 0.3880 0.8008 0.6274 0.029 Uiso 1 1 calc R . . C2 C 0.3896(7) 0.3790(6) 0.7325(6) 0.0246(17) Uani 1 1 d . . . H2 H 0.4634 0.4275 0.7386 0.029 Uiso 1 1 calc R . . C24 C 0.2270(7) 0.5558(6) 0.5788(6) 0.0256(18) Uani 1 1 d . . . H24 H 0.1742 0.5011 0.6035 0.031 Uiso 1 1 calc R . . Cl5 Cl 0.6985(2) 0.46010(19) 0.80840(15) 0.0371(5) Uani 1 1 d . . . Cl6 Cl 0.6658(3) 0.5852(2) 0.96405(17) 0.0499(7) Uani 1 1 d . . . C21 C 0.3871(6) 0.7171(6) 0.5068(5) 0.0179(15) Uani 1 1 d . . . H21 H 0.4424 0.7706 0.4830 0.022 Uiso 1 1 calc R . . C49 C 0.6960(8) 0.5825(6) 0.8513(6) 0.032(2) Uani 1 1 d . . . H49A H 0.7689 0.6366 0.8459 0.038 Uiso 1 1 calc R . . H49B H 0.6391 0.5974 0.8157 0.038 Uiso 1 1 calc R . . C43 C -0.3304(6) 0.0977(5) -0.2315(5) 0.0143(13) Uiso 1 1 d . . . Os1 Os 0.26234(2) 0.32101(2) 0.457238(18) 0.01207(7) Uani 1 1 d . . . Os2 Os -0.20086(2) -0.02074(2) -0.141479(18) 0.01141(7) Uani 1 1 d . . . Cl4 Cl -0.12317(15) -0.14458(13) -0.09842(12) 0.0167(3) Uani 1 1 d . . . Cl1 Cl 0.41338(14) 0.40108(13) 0.36788(11) 0.0163(3) Uani 1 1 d . . . Cl2 Cl 0.31598(15) 0.17223(13) 0.44471(12) 0.0174(3) Uani 1 1 d . . . Cl3 Cl -0.08607(14) -0.00412(13) -0.26559(12) 0.0155(3) Uani 1 1 d . . . N6 N -0.3060(5) -0.0642(5) -0.0458(4) 0.0143(12) Uani 1 1 d . . . N4 N 0.2084(5) 0.4380(4) 0.4399(4) 0.0123(11) Uani 1 1 d . . . N2 N 0.1621(5) 0.2604(4) 0.5532(4) 0.0109(11) Uani 1 1 d . . . C11 C -0.1172(6) 0.0679(6) 0.4580(6) 0.0233(17) Uani 1 1 d . . . H11 H -0.1466 0.0063 0.4181 0.028 Uiso 1 1 calc R . . N8 N -0.2328(5) 0.1040(4) -0.1746(4) 0.0118(11) Uani 1 1 d . . . N1 N 0.3627(5) 0.3851(5) 0.5686(4) 0.0165(12) Uani 1 1 d . . . H1N H 0.4266 0.4355 0.5673 0.020 Uiso 1 1 calc R . . N7 N -0.0831(5) 0.0971(5) -0.0634(4) 0.0136(12) Uani 1 1 d . . . H7N H -0.0427 0.0853 -0.0212 0.016 Uiso 1 1 calc R . . N3 N 0.1481(5) 0.2614(5) 0.3526(4) 0.0155(12) Uani 1 1 d . . . H3N H 0.1333 0.1985 0.3276 0.019 Uiso 1 1 calc R . . C9 C -0.1460(7) 0.2010(7) 0.5582(6) 0.0287(18) Uani 1 1 d . . . H9 H -0.1950 0.2293 0.5854 0.034 Uiso 1 1 calc R . . C47 C -0.4941(6) 0.1422(6) -0.2555(6) 0.0227(17) Uani 1 1 d . . . H47 H -0.5403 0.1779 -0.2357 0.027 Uiso 1 1 calc R . . C31 C -0.2869(6) -0.0108(5) 0.0458(4) 0.0140(14) Uani 1 1 d . . . C42 C -0.1557(6) 0.1979(5) -0.1416(5) 0.0130(13) Uani 1 1 d . . . C32 C -0.3468(7) 0.0517(6) 0.0699(6) 0.0225(16) Uani 1 1 d . . . H32 H -0.3985 0.0598 0.0282 0.027 Uiso 1 1 calc R . . C13 C 0.0944(6) 0.3201(5) 0.3215(5) 0.0152(14) Uani 1 1 d . . . N5 N -0.3335(5) -0.1375(4) -0.2093(4) 0.0157(12) Uani 1 1 d . . . H5N H -0.3395 -0.1497 -0.2675 0.019 Uiso 1 1 calc R . . C28 C -0.5600(6) -0.2972(6) -0.0365(6) 0.0229(17) Uani 1 1 d . . . H28 H -0.6099 -0.3327 0.0036 0.028 Uiso 1 1 calc R . . C6 C 0.2135(6) 0.2777(5) 0.6380(5) 0.0146(14) Uani 1 1 d . . . C44 C -0.3533(6) 0.0386(5) -0.3155(5) 0.0172(15) Uani 1 1 d . . . H44 H -0.3058 0.0045 -0.3358 0.021 Uiso 1 1 calc R . . C48 C -0.4004(6) 0.1478(6) -0.1995(5) 0.0208(16) Uani 1 1 d . . . H48 H -0.3856 0.1847 -0.1417 0.025 Uiso 1 1 calc R . . C25 C -0.4116(6) -0.1951(6) -0.1597(5) 0.0154(14) Uani 1 1 d . . . C35 C -0.1934(7) 0.0257(6) 0.1950(5) 0.0230(16) Uani 1 1 d . . . H35 H -0.1424 0.0165 0.2367 0.028 Uiso 1 1 calc R . . C18 C 0.1290(6) 0.4220(5) 0.3723(5) 0.0175(15) Uani 1 1 d . . . C12 C -0.0001(6) 0.1166(5) 0.4768(4) 0.0143(14) Uani 1 1 d . . . H12 H 0.0485 0.0883 0.4490 0.017 Uiso 1 1 calc R . . C30 C -0.3953(6) -0.1541(6) -0.0654(5) 0.0159(14) Uani 1 1 d . . . C3 C 0.3411(7) 0.3381(7) 0.8063(6) 0.0283(18) Uani 1 1 d . . . H3A H 0.3823 0.3568 0.8624 0.034 Uiso 1 1 calc R . . C37 C -0.0686(6) 0.1941(5) -0.0781(5) 0.0132(13) Uani 1 1 d . . . C41 C -0.1502(7) 0.2984(6) -0.1628(5) 0.0214(16) Uani 1 1 d . . . H41 H -0.2018 0.3035 -0.2065 0.026 Uiso 1 1 calc R . . C46 C -0.5184(6) 0.0844(6) -0.3392(5) 0.0227(17) Uani 1 1 d . . . H46 H -0.5810 0.0804 -0.3760 0.027 Uiso 1 1 calc R . . C10 C -0.1898(6) 0.1106(6) 0.4981(6) 0.0232(17) Uani 1 1 d . . . H10 H -0.2676 0.0785 0.4846 0.028 Uiso 1 1 calc R . . C8 C -0.0306(7) 0.2504(6) 0.5788(6) 0.0262(18) Uani 1 1 d . . . H8 H -0.0018 0.3114 0.6194 0.031 Uiso 1 1 calc R . . C4 C 0.2262(7) 0.2661(6) 0.7977(6) 0.0258(17) Uani 1 1 d . . . H4 H 0.1938 0.2388 0.8489 0.031 Uiso 1 1 calc R . . C16 C -0.0060(6) 0.4615(6) 0.2820(5) 0.0201(15) Uani 1 1 d . . . H16 H -0.0423 0.5068 0.2686 0.024 Uiso 1 1 calc R . . C1 C 0.3288(6) 0.3483(6) 0.6461(5) 0.0186(15) Uani 1 1 d . . . C45 C -0.4479(7) 0.0313(6) -0.3688(5) 0.0223(16) Uani 1 1 d . . . H45 H -0.4652 -0.0093 -0.4250 0.027 Uiso 1 1 calc R . . C29 C -0.4699(6) -0.2074(6) -0.0043(5) 0.0153(14) Uani 1 1 d . . . H29 H -0.4585 -0.1824 0.0571 0.018 Uiso 1 1 calc R . . C5 C 0.1625(7) 0.2363(6) 0.7160(5) 0.0225(16) Uani 1 1 d . . . H5 H 0.0877 0.1902 0.7117 0.027 Uiso 1 1 calc R . . C33 C -0.3288(8) 0.1031(7) 0.1582(6) 0.030(2) Uani 1 1 d . . . H33 H -0.3673 0.1472 0.1751 0.036 Uiso 1 1 calc R . . C7 C 0.0426(6) 0.2069(5) 0.5372(5) 0.0150(14) Uani 1 1 d . . . C27 C -0.5780(7) -0.3364(6) -0.1295(6) 0.0271(18) Uani 1 1 d . . . H27 H -0.6392 -0.3977 -0.1493 0.033 Uiso 1 1 calc R . . C14 C 0.0102(6) 0.2924(6) 0.2481(5) 0.0211(16) Uani 1 1 d . . . H14 H -0.0115 0.2274 0.2134 0.025 Uiso 1 1 calc R . . C15 C -0.0380(7) 0.3614(6) 0.2295(5) 0.0227(16) Uani 1 1 d . . . H15 H -0.0932 0.3435 0.1814 0.027 Uiso 1 1 calc R . . C17 C 0.0764(6) 0.4921(5) 0.3511(5) 0.0162(14) Uani 1 1 d . . . H17 H 0.0978 0.5583 0.3839 0.019 Uiso 1 1 calc R . . C34 C -0.2539(7) 0.0885(6) 0.2201(5) 0.0226(16) Uani 1 1 d . . . H34 H -0.2440 0.1210 0.2793 0.027 Uiso 1 1 calc R . . C26 C -0.5079(6) -0.2862(6) -0.1903(5) 0.0186(15) Uani 1 1 d . . . H26 H -0.5227 -0.3113 -0.2516 0.022 Uiso 1 1 calc R . . C36 C -0.2098(7) -0.0236(7) 0.1061(5) 0.0235(17) Uani 1 1 d . . . H36 H -0.1687 -0.0649 0.0880 0.028 Uiso 1 1 calc 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 C19 0.010(3) 0.013(3) 0.027(4) 0.001(3) -0.002(3) 0.007(3) C20 0.016(4) 0.017(4) 0.024(4) 0.006(3) 0.001(3) 0.003(3) C40 0.032(4) 0.014(3) 0.025(4) 0.008(3) 0.005(3) 0.009(3) C23 0.028(4) 0.024(4) 0.018(4) -0.008(3) 0.004(3) 0.003(3) C38 0.010(3) 0.015(3) 0.027(4) 0.004(3) -0.008(3) 0.006(3) C39 0.022(4) 0.016(4) 0.028(4) -0.002(3) -0.008(3) 0.006(3) C22 0.015(4) 0.016(4) 0.037(5) -0.010(3) -0.010(3) 0.005(3) C2 0.023(4) 0.021(4) 0.027(4) -0.005(3) -0.003(3) 0.007(3) C24 0.028(4) 0.014(4) 0.030(4) -0.002(3) 0.014(4) 0.003(3) Cl5 0.0477(14) 0.0446(13) 0.0332(11) 0.0027(10) 0.0024(10) 0.0345(12) Cl6 0.073(2) 0.0467(14) 0.0317(12) 0.0038(11) 0.0172(13) 0.0231(14) C21 0.010(3) 0.016(3) 0.027(4) 0.006(3) 0.002(3) 0.003(3) C49 0.047(6) 0.019(4) 0.026(4) 0.012(3) -0.003(4) 0.005(4) Os1 0.00973(13) 0.01074(13) 0.01433(14) 0.00121(10) -0.00072(10) 0.00230(10) Os2 0.00995(13) 0.01054(13) 0.01375(13) 0.00193(10) -0.00171(10) 0.00391(10) Cl4 0.0162(8) 0.0141(8) 0.0205(8) 0.0020(6) -0.0042(7) 0.0070(7) Cl1 0.0144(8) 0.0161(8) 0.0158(8) 0.0027(6) 0.0020(6) 0.0023(6) Cl2 0.0168(8) 0.0136(7) 0.0211(8) 0.0012(6) -0.0008(7) 0.0053(7) Cl3 0.0127(8) 0.0130(7) 0.0200(8) 0.0023(6) 0.0020(6) 0.0036(6) N6 0.013(3) 0.016(3) 0.015(3) 0.006(2) 0.001(2) 0.006(2) N4 0.012(3) 0.010(3) 0.012(3) 0.003(2) -0.002(2) 0.001(2) N2 0.008(3) 0.005(2) 0.016(3) 0.001(2) 0.001(2) -0.002(2) C11 0.017(4) 0.013(3) 0.034(4) 0.004(3) 0.002(3) -0.001(3) N8 0.016(3) 0.014(3) 0.008(2) -0.001(2) -0.003(2) 0.010(2) N1 0.009(3) 0.013(3) 0.026(3) 0.007(2) 0.002(2) 0.001(2) N7 0.012(3) 0.018(3) 0.012(3) 0.001(2) -0.005(2) 0.007(2) N3 0.010(3) 0.012(3) 0.022(3) 0.001(2) 0.001(2) 0.002(2) C9 0.019(4) 0.031(4) 0.039(5) 0.011(4) 0.003(4) 0.010(4) C47 0.005(3) 0.030(4) 0.035(4) 0.000(3) 0.001(3) 0.011(3) C31 0.018(4) 0.013(3) 0.011(3) 0.005(3) 0.003(3) 0.005(3) C42 0.010(3) 0.015(3) 0.013(3) 0.000(3) 0.002(3) 0.004(3) C32 0.020(4) 0.022(4) 0.029(4) -0.004(3) -0.004(3) 0.015(3) C13 0.011(3) 0.017(3) 0.016(3) -0.004(3) -0.001(3) 0.004(3) N5 0.020(3) 0.015(3) 0.013(3) -0.006(2) 0.000(2) 0.009(3) C28 0.013(4) 0.022(4) 0.031(4) 0.007(3) 0.012(3) 0.002(3) C6 0.022(4) 0.009(3) 0.012(3) -0.005(3) -0.001(3) 0.006(3) C44 0.019(4) 0.012(3) 0.020(4) 0.002(3) -0.002(3) 0.005(3) C48 0.016(4) 0.029(4) 0.017(4) 0.004(3) -0.004(3) 0.009(3) C25 0.012(3) 0.017(3) 0.017(3) 0.001(3) 0.000(3) 0.007(3) C35 0.019(4) 0.025(4) 0.026(4) 0.003(3) -0.001(3) 0.010(3) C18 0.010(3) 0.012(3) 0.026(4) 0.002(3) 0.001(3) -0.002(3) C12 0.012(3) 0.013(3) 0.010(3) -0.004(3) -0.004(3) -0.002(3) C30 0.016(4) 0.017(3) 0.016(3) 0.004(3) -0.004(3) 0.009(3) C3 0.025(4) 0.034(5) 0.024(4) 0.004(4) -0.006(3) 0.010(4) C37 0.016(3) 0.015(3) 0.012(3) 0.001(3) -0.001(3) 0.011(3) C41 0.033(4) 0.017(4) 0.020(4) 0.003(3) -0.002(3) 0.016(3) C46 0.013(4) 0.024(4) 0.029(4) 0.010(3) -0.007(3) 0.003(3) C10 0.007(3) 0.022(4) 0.034(4) 0.009(3) -0.003(3) -0.003(3) C8 0.017(4) 0.021(4) 0.039(5) 0.004(4) 0.002(3) 0.006(3) C4 0.022(4) 0.024(4) 0.033(5) 0.007(3) 0.005(3) 0.008(3) C16 0.015(4) 0.028(4) 0.019(4) 0.003(3) -0.001(3) 0.011(3) C1 0.016(4) 0.019(4) 0.022(4) 0.002(3) 0.000(3) 0.009(3) C45 0.028(4) 0.021(4) 0.020(4) 0.003(3) -0.011(3) 0.011(3) C29 0.016(3) 0.019(3) 0.010(3) 0.003(3) 0.005(3) 0.005(3) C5 0.025(4) 0.018(4) 0.023(4) 0.007(3) 0.000(3) 0.004(3) C33 0.040(5) 0.032(5) 0.026(4) -0.015(4) -0.007(4) 0.028(4) C7 0.014(3) 0.014(3) 0.019(3) 0.005(3) 0.004(3) 0.007(3) C27 0.020(4) 0.023(4) 0.035(5) 0.001(4) 0.002(4) 0.005(3) C14 0.017(4) 0.027(4) 0.017(4) -0.001(3) 0.003(3) 0.006(3) C15 0.018(4) 0.030(4) 0.018(4) -0.003(3) -0.007(3) 0.009(3) C17 0.010(3) 0.013(3) 0.021(4) -0.002(3) -0.006(3) 0.001(3) C34 0.019(4) 0.024(4) 0.020(4) 0.002(3) 0.000(3) 0.003(3) C26 0.013(3) 0.019(4) 0.023(4) -0.003(3) 0.001(3) 0.005(3) C36 0.022(4) 0.037(5) 0.015(3) -0.003(3) -0.006(3) 0.017(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 C19 C24 1.374(10) . ? C19 C20 1.379(10) . ? C19 N4 1.448(9) . ? C20 C21 1.382(10) . ? C40 C41 1.345(11) . ? C40 C39 1.427(11) . ? C23 C22 1.378(11) . ? C23 C24 1.386(10) . ? C38 C39 1.372(10) . ? C38 C37 1.393(10) . ? C22 C21 1.395(11) . ? C2 C3 1.354(12) . ? C2 C1 1.418(11) . ? Cl5 C49 1.754(9) . ? Cl6 C49 1.738(9) . ? C43 C48 1.379(10) . ? C43 C44 1.382(10) . ? C43 N8 1.444(9) . ? Os1 N1 1.971(6) . ? Os1 N3 1.978(6) . ? Os1 N2 1.996(5) . ? Os1 N4 1.998(6) . ? Os1 Cl2 2.3736(17) . ? Os1 Cl1 2.3773(17) . ? Os2 N6 1.981(6) . ? Os2 N7 1.991(6) . ? Os2 N8 2.004(5) . ? Os2 N5 2.010(6) . ? Os2 Cl3 2.3790(17) . ? Os2 Cl4 2.3814(17) . ? N6 C30 1.341(9) . ? N6 C31 1.451(9) . ? N4 C18 1.339(9) . ? N2 C6 1.357(9) . ? N2 C7 1.427(9) . ? C11 C10 1.384(11) . ? C11 C12 1.397(10) . ? N8 C42 1.341(9) . ? N1 C1 1.332(9) . ? N7 C37 1.325(9) . ? N3 C13 1.334(9) . ? C9 C10 1.379(12) . ? C9 C8 1.383(11) . ? C47 C46 1.370(11) . ? C47 C48 1.400(10) . ? C31 C32 1.370(10) . ? C31 C36 1.371(10) . ? C42 C41 1.429(9) . ? C42 C37 1.445(9) . ? C32 C33 1.398(11) . ? C13 C14 1.418(10) . ? C13 C18 1.434(10) . ? N5 C25 1.331(9) . ? C28 C29 1.375(10) . ? C28 C27 1.414(12) . ? C6 C5 1.423(10) . ? C6 C1 1.429(10) . ? C44 C45 1.380(10) . ? C25 C26 1.421(10) . ? C25 C30 1.438(10) . ? C35 C34 1.382(11) . ? C35 C36 1.397(11) . ? C18 C17 1.409(10) . ? C12 C7 1.380(9) . ? C30 C29 1.403(9) . ? C3 C4 1.432(11) . ? C46 C45 1.402(11) . ? C8 C7 1.406(11) . ? C4 C5 1.373(11) . ? C16 C17 1.357(10) . ? C16 C15 1.426(11) . ? C33 C34 1.379(11) . ? C27 C26 1.357(11) . ? C14 C15 1.345(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 C19 C20 120.9(7) . . ? C24 C19 N4 120.1(6) . . ? C20 C19 N4 118.9(7) . . ? C19 C20 C21 119.4(7) . . ? C41 C40 C39 122.3(7) . . ? C22 C23 C24 121.0(7) . . ? C39 C38 C37 120.1(7) . . ? C38 C39 C40 119.4(7) . . ? C23 C22 C21 118.8(7) . . ? C3 C2 C1 120.5(8) . . ? C19 C24 C23 119.3(7) . . ? C20 C21 C22 120.6(7) . . ? Cl6 C49 Cl5 111.2(4) . . ? C48 C43 C44 121.7(7) . . ? C48 C43 N8 119.3(6) . . ? C44 C43 N8 119.0(6) . . ? N1 Os1 N3 173.3(2) . . ? N1 Os1 N2 78.0(2) . . ? N3 Os1 N2 97.5(2) . . ? N1 Os1 N4 98.6(2) . . ? N3 Os1 N4 77.1(2) . . ? N2 Os1 N4 97.8(2) . . ? N1 Os1 Cl2 92.54(18) . . ? N3 Os1 Cl2 92.27(18) . . ? N2 Os1 Cl2 89.08(16) . . ? N4 Os1 Cl2 167.94(17) . . ? N1 Os1 Cl1 90.33(17) . . ? N3 Os1 Cl1 94.51(17) . . ? N2 Os1 Cl1 167.68(17) . . ? N4 Os1 Cl1 87.63(17) . . ? Cl2 Os1 Cl1 87.63(6) . . ? N6 Os2 N7 95.8(2) . . ? N6 Os2 N8 100.6(2) . . ? N7 Os2 N8 77.7(2) . . ? N6 Os2 N5 77.6(2) . . ? N7 Os2 N5 172.8(2) . . ? N8 Os2 N5 100.5(2) . . ? N6 Os2 Cl3 168.84(18) . . ? N7 Os2 Cl3 93.07(17) . . ? N8 Os2 Cl3 87.85(16) . . ? N5 Os2 Cl3 93.81(17) . . ? N6 Os2 Cl4 86.69(17) . . ? N7 Os2 Cl4 92.37(17) . . ? N8 Os2 Cl4 168.12(17) . . ? N5 Os2 Cl4 90.17(17) . . ? Cl3 Os2 Cl4 86.18(6) . . ? C30 N6 C31 118.2(6) . . ? C30 N6 Os2 117.2(5) . . ? C31 N6 Os2 124.3(4) . . ? C18 N4 C19 119.3(6) . . ? C18 N4 Os1 117.7(5) . . ? C19 N4 Os1 122.8(4) . . ? C6 N2 C7 120.5(6) . . ? C6 N2 Os1 115.8(5) . . ? C7 N2 Os1 123.6(4) . . ? C10 C11 C12 120.5(7) . . ? C42 N8 C43 119.9(6) . . ? C42 N8 Os2 115.8(4) . . ? C43 N8 Os2 124.2(4) . . ? C1 N1 Os1 118.1(5) . . ? C37 N7 Os2 118.3(5) . . ? C13 N3 Os1 119.2(5) . . ? C10 C9 C8 121.2(8) . . ? C46 C47 C48 120.5(7) . . ? C32 C31 C36 121.5(7) . . ? C32 C31 N6 118.8(7) . . ? C36 C31 N6 119.7(6) . . ? N8 C42 C41 127.5(7) . . ? N8 C42 C37 114.7(6) . . ? C41 C42 C37 117.8(6) . . ? C31 C32 C33 119.0(7) . . ? N3 C13 C14 128.1(7) . . ? N3 C13 C18 112.5(6) . . ? C14 C13 C18 119.4(7) . . ? C25 N5 Os2 116.5(5) . . ? C29 C28 C27 121.1(7) . . ? N2 C6 C5 126.3(7) . . ? N2 C6 C1 113.8(6) . . ? C5 C6 C1 119.8(7) . . ? C45 C44 C43 118.7(7) . . ? C43 C48 C47 118.9(7) . . ? N5 C25 C26 127.5(7) . . ? N5 C25 C30 113.6(6) . . ? C26 C25 C30 118.8(6) . . ? C34 C35 C36 119.1(7) . . ? N4 C18 C17 126.7(7) . . ? N4 C18 C13 113.5(6) . . ? C17 C18 C13 119.8(7) . . ? C7 C12 C11 119.3(7) . . ? N6 C30 C29 126.6(7) . . ? N6 C30 C25 113.3(6) . . ? C29 C30 C25 120.1(6) . . ? C2 C3 C4 119.9(8) . . ? N7 C37 C38 127.0(6) . . ? N7 C37 C42 112.2(6) . . ? C38 C37 C42 120.5(6) . . ? C40 C41 C42 119.6(7) . . ? C47 C46 C45 119.4(7) . . ? C9 C10 C11 119.6(7) . . ? C9 C8 C7 118.9(8) . . ? C5 C4 C3 121.9(8) . . ? C17 C16 C15 121.3(7) . . ? N1 C1 C2 127.3(7) . . ? N1 C1 C6 112.9(7) . . ? C2 C1 C6 119.4(7) . . ? C44 C45 C46 120.8(7) . . ? C28 C29 C30 119.0(7) . . ? C4 C5 C6 118.5(7) . . ? C34 C33 C32 120.0(7) . . ? C12 C7 C8 120.5(7) . . ? C12 C7 N2 119.7(6) . . ? C8 C7 N2 119.6(6) . . ? C26 C27 C28 121.2(7) . . ? C15 C14 C13 119.2(7) . . ? C14 C15 C16 121.3(7) . . ? C16 C17 C18 118.9(7) . . ? C33 C34 C35 120.5(7) . . ? C27 C26 C25 119.6(7) . . ? C31 C36 C35 119.8(7) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 2.335 _refine_diff_density_min -1.923 _refine_diff_density_rms 0.233