Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jason Clyburne' _publ_contact_author_address ; Dept. of Chemistry Saint Mary's University Halifax NS, B3H 3C3 CANADA ; _publ_contact_author_email CLYBURNE@SFU.CA _publ_section_title ; Non-classical NHC transfers from the reaction of (IMes)AgCl with osmium carbonyl clusters ; loop_ _publ_author_name 'Jason Clyburne' 'Craig E. Cooke' 'Michael C. Jennings' 'R. Pomeroy' 'Taramatee Ramnial' data_05119 _database_code_depnum_ccdc_archive 'CCDC 629182' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C30 H25 Cl N2 O9 Os3), C7 H8' _chemical_formula_sum 'C33.50 H29 Cl N2 O9 Os3' _chemical_formula_weight 1209.64 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' Cl Cl 0.1484 0.1585 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3651(2) _cell_length_b 10.8743(3) _cell_length_c 20.4975(7) _cell_angle_alpha 80.968(2) _cell_angle_beta 81.369(2) _cell_angle_gamma 71.935(2) _cell_volume 1740.42(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6205 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 30.03 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1122 _exptl_absorpt_coefficient_mu 11.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1899 _exptl_absorpt_correction_T_max 0.3275 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21096 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7106 _reflns_number_gt 6040 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0442P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7106 _refine_ls_number_parameters 432 _refine_ls_number_restraints 405 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.009 _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 0.21668(3) 0.72297(2) 0.248025(12) 0.01139(7) Uani 1 1 d DU . . Os2 Os -0.01816(3) 0.65229(2) 0.351792(12) 0.01251(7) Uani 1 1 d DU . . Os3 Os 0.30506(3) 0.47198(2) 0.324304(13) 0.01371(8) Uani 1 1 d U . . Cl Cl -0.05280(19) 0.68790(16) 0.23272(8) 0.0166(3) Uani 1 1 d U . . H H 0.083(7) 0.793(6) 0.327(2) 0.026(19) Uiso 1 1 d D . . C1 C 0.1331(7) 0.9180(6) 0.2029(3) 0.0129(12) Uani 1 1 d U . . N2 N 0.0432(6) 1.0290(5) 0.2307(3) 0.0143(11) Uani 1 1 d U . . C3 C 0.0276(8) 1.1370(6) 0.1848(3) 0.0179(14) Uani 1 1 d U . . H3A H -0.0290 1.2247 0.1924 0.022 Uiso 1 1 calc R . . C4 C 0.1071(8) 1.0957(6) 0.1273(3) 0.0189(14) Uani 1 1 d U . . H4A H 0.1175 1.1483 0.0862 0.023 Uiso 1 1 calc R . . N5 N 0.1714(6) 0.9621(5) 0.1388(3) 0.0148(11) Uani 1 1 d U . . C13 C 0.4145(8) 0.7434(6) 0.2668(3) 0.0171(13) Uani 1 1 d U . . O13 O 0.5403(6) 0.7549(5) 0.2781(2) 0.0256(12) Uani 1 1 d U . . C14 C 0.3363(7) 0.6441(6) 0.1733(3) 0.0155(13) Uani 1 1 d U . . O14 O 0.4096(6) 0.5848(5) 0.1311(2) 0.0271(12) Uani 1 1 d U . . O21 O -0.3632(6) 0.8361(5) 0.3971(2) 0.0246(11) Uani 1 1 d U . . C21 C -0.2323(8) 0.7760(6) 0.3754(3) 0.0151(13) Uani 1 1 d U . . C23 C 0.0409(8) 0.6287(6) 0.4383(3) 0.0170(13) Uani 1 1 d U . . O23 O 0.0782(6) 0.6164(5) 0.4913(2) 0.0255(12) Uani 1 1 d U . . O24 O -0.1703(6) 0.4262(5) 0.3723(2) 0.0265(12) Uani 1 1 d U . . C24 C -0.1140(8) 0.5094(6) 0.3676(3) 0.0154(13) Uani 1 1 d U . . C31 C 0.2875(8) 0.3354(7) 0.3945(3) 0.0173(13) Uani 1 1 d U . . O31 O 0.2803(6) 0.2548(5) 0.4370(3) 0.0265(11) Uani 1 1 d U . . O32 O 0.6555(6) 0.3709(5) 0.2479(3) 0.0297(12) Uani 1 1 d U . . C32 C 0.5265(9) 0.4069(6) 0.2778(4) 0.0205(15) Uani 1 1 d U . . O33 O 0.4448(6) 0.6066(5) 0.4149(2) 0.0267(12) Uani 1 1 d U . . C33 C 0.3916(8) 0.5586(7) 0.3819(4) 0.0216(15) Uani 1 1 d U . . O34 O 0.1346(7) 0.3796(5) 0.2261(3) 0.0372(15) Uani 1 1 d U . . C34 C 0.1948(9) 0.4174(7) 0.2617(4) 0.0221(15) Uani 1 1 d U . . C51 C 0.2643(4) 0.8877(4) 0.08666(17) 0.0179(14) Uani 1 1 d GU . . C52 C 0.1769(4) 0.8465(5) 0.0461(2) 0.0181(14) Uani 1 1 d GU . . C53 C 0.2613(5) 0.7903(4) -0.0107(2) 0.0200(14) Uani 1 1 d GU . . H53A H 0.2016 0.7621 -0.0384 0.024 Uiso 1 1 calc R . . C54 C 0.4332(5) 0.7755(4) -0.02678(18) 0.0246(16) Uani 1 1 d GU . . C55 C 0.5206(4) 0.8168(4) 0.0138(2) 0.0203(14) Uani 1 1 d GU . . H55A H 0.6380 0.8066 0.0028 0.024 Uiso 1 1 calc R . . C56 C 0.4361(4) 0.8729(4) 0.07055(19) 0.0137(13) Uani 1 1 d GU . . C57 C -0.0098(8) 0.8590(7) 0.0638(3) 0.0215(15) Uani 1 1 d U . . H57A H -0.0747 0.9514 0.0612 0.032 Uiso 1 1 calc R . . H57B H -0.0280 0.8171 0.1091 0.032 Uiso 1 1 calc R . . H57C H -0.0473 0.8168 0.0326 0.032 Uiso 1 1 calc R . . C58 C 0.5202(9) 0.7217(7) -0.0911(4) 0.0284(18) Uani 1 1 d U . . H58A H 0.6388 0.7215 -0.0966 0.043 Uiso 1 1 calc R . . H58B H 0.4633 0.7764 -0.1285 0.043 Uiso 1 1 calc R . . H58C H 0.5150 0.6326 -0.0897 0.043 Uiso 1 1 calc R . . C59 C 0.5354(8) 0.9148(7) 0.1149(4) 0.0239(16) Uani 1 1 d U . . H59A H 0.6072 0.8376 0.1393 0.036 Uiso 1 1 calc R . . H59B H 0.4565 0.9696 0.1466 0.036 Uiso 1 1 calc R . . H59C H 0.6063 0.9643 0.0875 0.036 Uiso 1 1 calc R . . C61 C -0.0320(5) 1.0435(4) 0.29717(16) 0.0138(13) Uani 1 1 d GU . . C62 C -0.2052(4) 1.0618(4) 0.31037(18) 0.0179(14) Uani 1 1 d GU . . C63 C -0.2881(4) 1.0944(5) 0.3721(2) 0.0183(14) Uani 1 1 d GU . . H63A H -0.4064 1.1069 0.3811 0.022 Uiso 1 1 calc R . . C64 C -0.1977(5) 1.1088(5) 0.42061(16) 0.0202(15) Uani 1 1 d GU . . C65 C -0.0246(5) 1.0905(5) 0.40742(18) 0.0226(15) Uani 1 1 d GU . . H65A H 0.0372 1.1003 0.4406 0.027 Uiso 1 1 calc R . . C66 C 0.0583(3) 1.0579(5) 0.3457(2) 0.0168(14) Uani 1 1 d GU . . C67 C -0.3065(8) 1.0460(7) 0.2578(4) 0.0229(16) Uani 1 1 d U . . H67A H -0.3024 1.1117 0.2195 0.034 Uiso 1 1 calc R . . H67B H -0.4243 1.0572 0.2766 0.034 Uiso 1 1 calc R . . H67C H -0.2579 0.9588 0.2436 0.034 Uiso 1 1 calc R . . C68 C -0.2899(9) 1.1493(9) 0.4863(4) 0.035(2) Uani 1 1 d U . . H68A H -0.3387 1.2442 0.4821 0.053 Uiso 1 1 calc R . . H68B H -0.2106 1.1220 0.5201 0.053 Uiso 1 1 calc R . . H68C H -0.3805 1.1079 0.4994 0.053 Uiso 1 1 calc R . . C69 C 0.2472(8) 1.0436(7) 0.3307(4) 0.0265(17) Uani 1 1 d U . . H69A H 0.2651 1.1096 0.2943 0.040 Uiso 1 1 calc R . . H69B H 0.3071 0.9566 0.3178 0.040 Uiso 1 1 calc R . . H69C H 0.2906 1.0553 0.3704 0.040 Uiso 1 1 calc R . . C71 C 0.830(2) 0.516(2) 0.1076(9) 0.038(3) Uani 0.50 1 d PU A -1 H71A H 0.9051 0.5080 0.1414 0.058 Uiso 0.50 1 calc PR A -1 H71B H 0.7793 0.4440 0.1172 0.058 Uiso 0.50 1 calc PR A -1 H71C H 0.7408 0.5990 0.1081 0.058 Uiso 0.50 1 calc PR A -1 C72 C 0.9318(12) 0.5094(14) 0.0396(4) 0.026(3) Uani 0.50 1 d PGU A -1 C73 C 1.0992(13) 0.5101(11) 0.0338(5) 0.030(3) Uani 0.50 1 d PGU A -1 H73A H 1.1464 0.5191 0.0716 0.036 Uiso 0.50 1 calc PR A -1 C74 C 1.1975(10) 0.4978(12) -0.0271(6) 0.038(4) Uani 0.50 1 d PGU A -1 H74A H 1.3119 0.4983 -0.0311 0.046 Uiso 0.50 1 calc PR A -1 C75 C 1.1284(14) 0.4847(14) -0.0823(5) 0.038(3) Uani 0.50 1 d PGU A -1 H75A H 1.1957 0.4763 -0.1240 0.046 Uiso 0.50 1 calc PR A -1 C76 C 0.9610(15) 0.4840(12) -0.0766(5) 0.037(4) Uani 0.50 1 d PGU A -1 H76A H 0.9138 0.4751 -0.1143 0.044 Uiso 0.50 1 calc PR A -1 C77 C 0.8627(10) 0.4964(12) -0.0156(6) 0.030(3) Uani 0.50 1 d PGU A -1 H77A H 0.7483 0.4959 -0.0117 0.036 Uiso 0.50 1 calc PR A -1 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 0.01015(13) 0.01141(14) 0.01133(14) -0.00101(10) 0.00037(9) -0.00220(10) Os2 0.01109(13) 0.01330(14) 0.01216(14) -0.00034(10) 0.00040(9) -0.00349(10) Os3 0.01380(13) 0.01118(14) 0.01443(14) -0.00118(10) -0.00108(10) -0.00157(10) Cl 0.0150(7) 0.0212(9) 0.0147(8) -0.0010(7) -0.0030(6) -0.0070(7) C1 0.013(3) 0.009(3) 0.015(3) 0.001(2) 0.001(2) -0.003(2) N2 0.014(3) 0.010(3) 0.018(3) -0.005(2) 0.004(2) -0.003(2) C3 0.018(3) 0.012(3) 0.021(3) -0.002(3) 0.005(3) -0.003(3) C4 0.017(3) 0.015(3) 0.019(3) 0.006(3) -0.004(3) 0.000(3) N5 0.014(3) 0.016(3) 0.011(3) -0.004(2) 0.004(2) -0.001(2) C13 0.015(3) 0.017(3) 0.015(3) 0.004(3) -0.002(2) -0.003(3) O13 0.017(2) 0.035(3) 0.028(3) -0.002(2) -0.002(2) -0.014(2) C14 0.009(3) 0.015(3) 0.021(3) 0.004(3) -0.007(2) -0.002(3) O14 0.034(3) 0.019(3) 0.020(3) -0.005(2) 0.005(2) 0.001(2) O21 0.018(2) 0.025(3) 0.028(3) -0.005(2) 0.004(2) -0.004(2) C21 0.019(3) 0.012(3) 0.013(3) 0.006(3) 0.000(2) -0.009(2) C23 0.013(3) 0.015(3) 0.022(3) -0.002(3) 0.008(2) -0.008(3) O23 0.029(3) 0.039(3) 0.011(2) -0.001(2) -0.002(2) -0.015(2) O24 0.036(3) 0.027(3) 0.021(3) 0.007(2) -0.009(2) -0.018(2) C24 0.017(3) 0.018(3) 0.008(3) 0.002(3) -0.004(2) -0.002(3) C31 0.016(3) 0.016(3) 0.019(3) -0.009(3) 0.002(3) 0.000(3) O31 0.025(3) 0.021(3) 0.028(3) 0.001(2) 0.006(2) -0.005(2) O32 0.019(3) 0.030(3) 0.034(3) -0.002(3) 0.009(2) -0.004(2) C32 0.023(3) 0.012(3) 0.025(4) -0.006(3) -0.003(3) 0.000(3) O33 0.027(3) 0.031(3) 0.026(3) -0.010(2) -0.009(2) -0.009(2) C33 0.013(3) 0.021(4) 0.025(4) -0.003(3) 0.000(3) 0.001(3) O34 0.046(3) 0.032(3) 0.042(4) -0.015(3) -0.020(3) -0.011(3) C34 0.023(3) 0.014(3) 0.025(4) -0.003(3) 0.003(3) -0.002(3) C51 0.020(3) 0.017(3) 0.016(3) -0.001(3) -0.001(2) -0.006(3) C52 0.022(3) 0.015(3) 0.015(3) 0.001(3) 0.001(3) -0.004(3) C53 0.021(3) 0.015(4) 0.020(4) -0.003(3) -0.005(3) 0.002(3) C54 0.031(4) 0.017(4) 0.021(4) -0.004(3) 0.002(3) -0.001(3) C55 0.027(3) 0.017(4) 0.009(3) 0.005(3) 0.003(3) -0.001(3) C56 0.013(3) 0.013(3) 0.012(3) 0.002(3) 0.002(2) -0.003(3) C57 0.016(3) 0.027(4) 0.020(4) -0.001(3) -0.003(3) -0.004(3) C58 0.036(4) 0.026(4) 0.018(4) -0.006(3) 0.005(3) -0.004(3) C59 0.021(4) 0.027(4) 0.022(4) -0.002(3) -0.004(3) -0.004(3) C61 0.019(3) 0.009(3) 0.012(3) -0.004(3) 0.004(2) -0.003(3) C62 0.018(3) 0.011(3) 0.021(3) 0.001(3) 0.000(3) -0.001(3) C63 0.017(3) 0.016(3) 0.020(3) 0.001(3) 0.005(2) -0.007(3) C64 0.023(3) 0.020(4) 0.016(3) -0.004(3) 0.004(3) -0.006(3) C65 0.021(3) 0.026(4) 0.018(4) -0.004(3) -0.002(3) -0.003(3) C66 0.012(3) 0.016(3) 0.019(3) -0.006(3) 0.001(2) 0.001(3) C67 0.016(3) 0.023(4) 0.025(4) -0.005(3) 0.004(3) -0.001(3) C68 0.024(4) 0.056(6) 0.024(4) -0.015(4) 0.008(3) -0.007(4) C69 0.022(3) 0.028(4) 0.032(4) -0.010(4) -0.001(3) -0.009(3) C71 0.036(6) 0.034(5) 0.036(8) 0.014(8) 0.001(5) -0.006(6) C72 0.019(6) 0.017(7) 0.035(7) 0.004(7) -0.004(5) 0.000(6) C73 0.024(5) 0.025(5) 0.042(7) -0.005(6) -0.002(5) -0.008(5) C74 0.022(7) 0.022(8) 0.061(9) -0.008(8) 0.006(6) 0.002(7) C75 0.036(6) 0.034(5) 0.036(8) 0.014(8) 0.001(5) -0.006(6) C76 0.041(8) 0.035(9) 0.027(7) 0.011(7) -0.006(6) -0.007(8) C77 0.024(5) 0.025(5) 0.042(7) -0.005(6) -0.002(5) -0.008(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 C13 1.839(6) . ? Os1 C14 1.872(7) . ? Os1 C1 2.122(6) . ? Os1 Cl 2.4715(15) . ? Os1 Os2 2.8536(4) . ? Os1 Os3 2.8629(4) . ? Os1 H 1.93(4) . ? Os2 C23 1.869(7) . ? Os2 C24 1.923(7) . ? Os2 C21 1.925(6) . ? Os2 Cl 2.4569(16) . ? Os2 Os3 2.8415(3) . ? Os2 H 1.93(4) . ? Os3 C31 1.923(8) . ? Os3 C32 1.926(7) . ? Os3 C34 1.945(7) . ? Os3 C33 1.959(7) . ? C1 N5 1.353(8) . ? C1 N2 1.368(7) . ? N2 C3 1.370(9) . ? N2 C61 1.423(6) . ? C3 C4 1.333(9) . ? C3 H3A 0.9500 . ? C4 N5 1.379(8) . ? C4 H4A 0.9500 . ? N5 C51 1.425(5) . ? C13 O13 1.158(7) . ? C14 O14 1.145(7) . ? O21 C21 1.150(7) . ? C23 O23 1.152(8) . ? O24 C24 1.128(8) . ? C31 O31 1.144(8) . ? O32 C32 1.144(8) . ? O33 C33 1.128(8) . ? O34 C34 1.135(8) . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C52 C57 1.517(7) . ? C53 C54 1.3900 . ? C53 H53A 0.9500 . ? C54 C55 1.3900 . ? C54 C58 1.517(7) . ? C55 C56 1.3900 . ? C55 H55A 0.9500 . ? C56 C59 1.522(7) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C62 C67 1.527(7) . ? C63 C64 1.3900 . ? C63 H63A 0.9500 . ? C64 C65 1.3900 . ? C64 C68 1.505(7) . ? C65 C66 1.3900 . ? C65 H65A 0.9500 . ? C66 C69 1.527(7) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C71 C72 1.519(18) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.3900 . ? C72 C77 1.3900 . ? C73 C74 1.3900 . ? C73 H73A 0.9500 . ? C74 C75 1.3900 . ? C74 H74A 0.9500 . ? C75 C76 1.3900 . ? C75 H75A 0.9500 . ? C76 C77 1.3900 . ? C76 H76A 0.9500 . ? C77 H77A 0.9500 . ? 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 C14 88.7(3) . . ? C13 Os1 C1 92.6(3) . . ? C14 Os1 C1 99.0(3) . . ? C13 Os1 Cl 175.2(2) . . ? C14 Os1 Cl 94.46(18) . . ? C1 Os1 Cl 90.51(17) . . ? C13 Os1 Os2 120.9(2) . . ? C14 Os1 Os2 132.5(2) . . ? C1 Os1 Os2 114.19(16) . . ? Cl Os1 Os2 54.38(4) . . ? C13 Os1 Os3 88.0(2) . . ? C14 Os1 Os3 88.4(2) . . ? C1 Os1 Os3 172.62(16) . . ? Cl Os1 Os3 88.53(4) . . ? Os2 Os1 Os3 59.611(9) . . ? C13 Os1 H 95.0(17) . . ? C14 Os1 H 174.9(14) . . ? C1 Os1 H 84.3(18) . . ? Cl Os1 H 81.6(17) . . ? Os2 Os1 H 42.4(14) . . ? Os3 Os1 H 88.3(18) . . ? C23 Os2 C24 93.7(3) . . ? C23 Os2 C21 91.8(3) . . ? C24 Os2 C21 92.5(3) . . ? C23 Os2 Cl 171.21(19) . . ? C24 Os2 Cl 92.69(18) . . ? C21 Os2 Cl 93.98(19) . . ? C23 Os2 Os3 84.81(19) . . ? C24 Os2 Os3 88.75(18) . . ? C21 Os2 Os3 176.40(18) . . ? Cl Os2 Os3 89.31(4) . . ? C23 Os2 Os1 116.39(19) . . ? C24 Os2 Os1 132.19(18) . . ? C21 Os2 Os1 120.6(2) . . ? Cl Os2 Os1 54.86(4) . . ? Os3 Os2 Os1 60.357(9) . . ? C23 Os2 H 91.3(18) . . ? C24 Os2 H 174.3(15) . . ? C21 Os2 H 90.0(17) . . ? Cl Os2 H 82.0(17) . . ? Os3 Os2 H 89.0(18) . . ? Os1 Os2 H 42.5(14) . . ? C31 Os3 C32 104.5(3) . . ? C31 Os3 C34 95.9(3) . . ? C32 Os3 C34 93.0(3) . . ? C31 Os3 C33 91.7(3) . . ? C32 Os3 C33 91.8(3) . . ? C34 Os3 C33 169.7(3) . . ? C31 Os3 Os2 98.78(18) . . ? C32 Os3 Os2 156.7(2) . . ? C34 Os3 Os2 84.40(19) . . ? C33 Os3 Os2 87.58(18) . . ? C31 Os3 Os1 158.51(18) . . ? C32 Os3 Os1 96.7(2) . . ? C34 Os3 Os1 86.1(2) . . ? C33 Os3 Os1 84.3(2) . . ? Os2 Os3 Os1 60.031(9) . . ? Os2 Cl Os1 70.76(4) . . ? N5 C1 N2 103.6(5) . . ? N5 C1 Os1 126.3(4) . . ? N2 C1 Os1 129.9(5) . . ? C1 N2 C3 111.2(5) . . ? C1 N2 C61 129.2(5) . . ? C3 N2 C61 119.5(5) . . ? C4 C3 N2 106.9(6) . . ? C4 C3 H3A 126.5 . . ? N2 C3 H3A 126.5 . . ? C3 C4 N5 107.1(6) . . ? C3 C4 H4A 126.4 . . ? N5 C4 H4A 126.4 . . ? C1 N5 C4 111.2(5) . . ? C1 N5 C51 127.8(5) . . ? C4 N5 C51 121.0(5) . . ? O13 C13 Os1 179.1(6) . . ? O14 C14 Os1 173.5(6) . . ? O21 C21 Os2 169.9(6) . . ? O23 C23 Os2 178.6(6) . . ? O24 C24 Os2 175.3(6) . . ? O31 C31 Os3 178.2(6) . . ? O32 C32 Os3 177.3(7) . . ? O33 C33 Os3 178.5(6) . . ? O34 C34 Os3 176.7(6) . . ? C52 C51 C56 120.0 . . ? C52 C51 N5 119.0(3) . . ? C56 C51 N5 120.3(3) . . ? C53 C52 C51 120.0 . . ? C53 C52 C57 119.3(3) . . ? C51 C52 C57 120.6(3) . . ? C52 C53 C54 120.0 . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 C58 120.9(4) . . ? C53 C54 C58 119.0(4) . . ? C56 C55 C54 120.0 . . ? C56 C55 H55A 120.0 . . ? C54 C55 H55A 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 C59 119.0(4) . . ? C51 C56 C59 121.0(4) . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C62 C61 C66 120.0 . . ? C62 C61 N2 118.0(3) . . ? C66 C61 N2 121.4(3) . . ? C63 C62 C61 120.0 . . ? C63 C62 C67 119.2(3) . . ? C61 C62 C67 120.8(3) . . ? C64 C63 C62 120.0 . . ? C64 C63 H63A 120.0 . . ? C62 C63 H63A 120.0 . . ? C63 C64 C65 120.0 . . ? C63 C64 C68 119.5(4) . . ? C65 C64 C68 120.5(4) . . ? C66 C65 C64 120.0 . . ? C66 C65 H65A 120.0 . . ? C64 C65 H65A 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 C69 119.6(4) . . ? C61 C66 C69 120.4(4) . . ? C62 C67 H67A 109.5 . . ? C62 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C62 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C64 C68 H68A 109.5 . . ? C64 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C64 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C66 C69 H69A 109.5 . . ? C66 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C66 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C73 C72 C77 120.0 . . ? C73 C72 C71 118.8(11) . . ? C77 C72 C71 121.1(11) . . ? C74 C73 C72 120.0 . . ? C74 C73 H73A 120.0 . . ? C72 C73 H73A 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H74A 120.0 . . ? C75 C74 H74A 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 H75A 120.0 . . ? C74 C75 H75A 120.0 . . ? C75 C76 C77 120.0 . . ? C75 C76 H76A 120.0 . . ? C77 C76 H76A 120.0 . . ? C76 C77 C72 120.0 . . ? C76 C77 H77A 120.0 . . ? C72 C77 H77A 120.0 . . ? 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 C13 Os1 Os2 C23 0.0(3) . . . . ? C14 Os1 Os2 C23 120.9(3) . . . . ? C1 Os1 Os2 C23 -109.0(3) . . . . ? Cl Os1 Os2 C23 179.1(2) . . . . ? Os3 Os1 Os2 C23 66.5(2) . . . . ? C13 Os1 Os2 C24 -123.2(3) . . . . ? C14 Os1 Os2 C24 -2.3(3) . . . . ? C1 Os1 Os2 C24 127.9(3) . . . . ? Cl Os1 Os2 C24 55.9(2) . . . . ? Os3 Os1 Os2 C24 -56.7(2) . . . . ? C13 Os1 Os2 C21 109.5(3) . . . . ? C14 Os1 Os2 C21 -129.6(3) . . . . ? C1 Os1 Os2 C21 0.5(3) . . . . ? Cl Os1 Os2 C21 -71.4(2) . . . . ? Os3 Os1 Os2 C21 176.0(2) . . . . ? C13 Os1 Os2 Cl -179.1(2) . . . . ? C14 Os1 Os2 Cl -58.2(2) . . . . ? C1 Os1 Os2 Cl 71.95(18) . . . . ? Os3 Os1 Os2 Cl -112.55(5) . . . . ? C13 Os1 Os2 Os3 -66.5(2) . . . . ? C14 Os1 Os2 Os3 54.4(2) . . . . ? C1 Os1 Os2 Os3 -175.49(18) . . . . ? Cl Os1 Os2 Os3 112.55(5) . . . . ? C23 Os2 Os3 C31 51.7(3) . . . . ? C24 Os2 Os3 C31 -42.1(3) . . . . ? C21 Os2 Os3 C31 69(3) . . . . ? Cl Os2 Os3 C31 -134.79(19) . . . . ? Os1 Os2 Os3 C31 176.16(19) . . . . ? C23 Os2 Os3 C32 -128.6(5) . . . . ? C24 Os2 Os3 C32 137.6(5) . . . . ? C21 Os2 Os3 C32 -111(3) . . . . ? Cl Os2 Os3 C32 44.9(5) . . . . ? Os1 Os2 Os3 C32 -4.1(5) . . . . ? C23 Os2 Os3 C34 146.9(3) . . . . ? C24 Os2 Os3 C34 53.0(3) . . . . ? C21 Os2 Os3 C34 164(3) . . . . ? Cl Os2 Os3 C34 -39.7(2) . . . . ? Os1 Os2 Os3 C34 -88.7(2) . . . . ? C23 Os2 Os3 C33 -39.6(3) . . . . ? C24 Os2 Os3 C33 -133.5(3) . . . . ? C21 Os2 Os3 C33 -22(3) . . . . ? Cl Os2 Os3 C33 133.8(2) . . . . ? Os1 Os2 Os3 C33 84.8(2) . . . . ? C23 Os2 Os3 Os1 -124.4(2) . . . . ? C24 Os2 Os3 Os1 141.75(18) . . . . ? C21 Os2 Os3 Os1 -107(3) . . . . ? Cl Os2 Os3 Os1 49.05(4) . . . . ? C13 Os1 Os3 C31 117.6(5) . . . . ? C14 Os1 Os3 C31 -153.6(5) . . . . ? C1 Os1 Os3 C31 23.5(14) . . . . ? Cl Os1 Os3 C31 -59.1(5) . . . . ? Os2 Os1 Os3 C31 -10.4(5) . . . . ? C13 Os1 Os3 C32 -53.6(3) . . . . ? C14 Os1 Os3 C32 35.2(3) . . . . ? C1 Os1 Os3 C32 -147.7(13) . . . . ? Cl Os1 Os3 C32 129.68(19) . . . . ? Os2 Os1 Os3 C32 178.35(19) . . . . ? C13 Os1 Os3 C34 -146.2(3) . . . . ? C14 Os1 Os3 C34 -57.4(3) . . . . ? C1 Os1 Os3 C34 119.7(13) . . . . ? Cl Os1 Os3 C34 37.1(2) . . . . ? Os2 Os1 Os3 C34 85.8(2) . . . . ? C13 Os1 Os3 C33 37.5(3) . . . . ? C14 Os1 Os3 C33 126.3(3) . . . . ? C1 Os1 Os3 C33 -56.6(13) . . . . ? Cl Os1 Os3 C33 -139.2(2) . . . . ? Os2 Os1 Os3 C33 -90.51(19) . . . . ? C13 Os1 Os3 Os2 128.0(2) . . . . ? C14 Os1 Os3 Os2 -143.18(18) . . . . ? C1 Os1 Os3 Os2 33.9(13) . . . . ? Cl Os1 Os3 Os2 -48.68(4) . . . . ? C23 Os2 Cl Os1 -5.5(13) . . . . ? C24 Os2 Cl Os1 -142.11(18) . . . . ? C21 Os2 Cl Os1 125.15(19) . . . . ? Os3 Os2 Cl Os1 -53.39(3) . . . . ? C13 Os1 Cl Os2 10(2) . . . . ? C14 Os1 Cl Os2 141.1(2) . . . . ? C1 Os1 Cl Os2 -119.85(17) . . . . ? Os3 Os1 Cl Os2 52.84(3) . . . . ? C13 Os1 C1 N5 86.0(6) . . . . ? C14 Os1 C1 N5 -3.1(6) . . . . ? Cl Os1 C1 N5 -97.7(5) . . . . ? Os2 Os1 C1 N5 -148.4(5) . . . . ? Os3 Os1 C1 N5 179.8(9) . . . . ? C13 Os1 C1 N2 -87.8(6) . . . . ? C14 Os1 C1 N2 -177.0(5) . . . . ? Cl Os1 C1 N2 88.4(5) . . . . ? Os2 Os1 C1 N2 37.8(6) . . . . ? Os3 Os1 C1 N2 6.0(17) . . . . ? N5 C1 N2 C3 0.0(7) . . . . ? Os1 C1 N2 C3 174.8(5) . . . . ? N5 C1 N2 C61 179.3(5) . . . . ? Os1 C1 N2 C61 -5.8(9) . . . . ? C1 N2 C3 C4 0.2(7) . . . . ? C61 N2 C3 C4 -179.3(5) . . . . ? N2 C3 C4 N5 -0.2(7) . . . . ? N2 C1 N5 C4 -0.1(7) . . . . ? Os1 C1 N5 C4 -175.2(4) . . . . ? N2 C1 N5 C51 -179.8(5) . . . . ? Os1 C1 N5 C51 5.0(9) . . . . ? C3 C4 N5 C1 0.2(7) . . . . ? C3 C4 N5 C51 180.0(5) . . . . ? C14 Os1 C13 O13 -26(46) . . . . ? C1 Os1 C13 O13 -125(46) . . . . ? Cl Os1 C13 O13 106(45) . . . . ? Os2 Os1 C13 O13 115(46) . . . . ? Os3 Os1 C13 O13 63(46) . . . . ? C13 Os1 C14 O14 101(5) . . . . ? C1 Os1 C14 O14 -167(5) . . . . ? Cl Os1 C14 O14 -76(5) . . . . ? Os2 Os1 C14 O14 -32(5) . . . . ? Os3 Os1 C14 O14 13(5) . . . . ? C23 Os2 C21 O21 -51(3) . . . . ? C24 Os2 C21 O21 42(3) . . . . ? Cl Os2 C21 O21 135(3) . . . . ? Os3 Os2 C21 O21 -69(5) . . . . ? Os1 Os2 C21 O21 -174(3) . . . . ? C24 Os2 C23 O23 -172(25) . . . . ? C21 Os2 C23 O23 -79(25) . . . . ? Cl Os2 C23 O23 52(26) . . . . ? Os3 Os2 C23 O23 100(25) . . . . ? Os1 Os2 C23 O23 47(25) . . . . ? C23 Os2 C24 O24 -167(7) . . . . ? C21 Os2 C24 O24 101(7) . . . . ? Cl Os2 C24 O24 7(7) . . . . ? Os3 Os2 C24 O24 -83(7) . . . . ? Os1 Os2 C24 O24 -36(7) . . . . ? C32 Os3 C31 O31 68(19) . . . . ? C34 Os3 C31 O31 163(19) . . . . ? C33 Os3 C31 O31 -24(19) . . . . ? Os2 Os3 C31 O31 -112(19) . . . . ? Os1 Os3 C31 O31 -103(19) . . . . ? C31 Os3 C32 O32 148(13) . . . . ? C34 Os3 C32 O32 51(13) . . . . ? C33 Os3 C32 O32 -119(13) . . . . ? Os2 Os3 C32 O32 -31(14) . . . . ? Os1 Os3 C32 O32 -35(13) . . . . ? C31 Os3 C33 O33 78(27) . . . . ? C32 Os3 C33 O33 -27(27) . . . . ? C34 Os3 C33 O33 -144(26) . . . . ? Os2 Os3 C33 O33 176(100) . . . . ? Os1 Os3 C33 O33 -123(27) . . . . ? C31 Os3 C34 O34 -41(12) . . . . ? C32 Os3 C34 O34 64(12) . . . . ? C33 Os3 C34 O34 -178(100) . . . . ? Os2 Os3 C34 O34 -139(12) . . . . ? Os1 Os3 C34 O34 161(12) . . . . ? C1 N5 C51 C52 92.9(6) . . . . ? C4 N5 C51 C52 -86.8(6) . . . . ? C1 N5 C51 C56 -96.3(6) . . . . ? C4 N5 C51 C56 84.0(6) . . . . ? C56 C51 C52 C53 0.0 . . . . ? N5 C51 C52 C53 170.8(5) . . . . ? C56 C51 C52 C57 178.5(5) . . . . ? N5 C51 C52 C57 -10.7(6) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C57 C52 C53 C54 -178.6(5) . . . . ? C52 C53 C54 C55 0.0 . . . . ? C52 C53 C54 C58 -176.3(5) . . . . ? C53 C54 C55 C56 0.0 . . . . ? C58 C54 C55 C56 176.2(5) . . . . ? C54 C55 C56 C51 0.0 . . . . ? C54 C55 C56 C59 178.8(5) . . . . ? C52 C51 C56 C55 0.0 . . . . ? N5 C51 C56 C55 -170.7(5) . . . . ? C52 C51 C56 C59 -178.8(5) . . . . ? N5 C51 C56 C59 10.6(6) . . . . ? C1 N2 C61 C62 -100.9(6) . . . . ? C3 N2 C61 C62 78.5(6) . . . . ? C1 N2 C61 C66 88.2(6) . . . . ? C3 N2 C61 C66 -92.4(6) . . . . ? C66 C61 C62 C63 0.0 . . . . ? N2 C61 C62 C63 -171.0(4) . . . . ? C66 C61 C62 C67 -179.8(5) . . . . ? N2 C61 C62 C67 9.2(5) . . . . ? C61 C62 C63 C64 0.0 . . . . ? C67 C62 C63 C64 179.8(5) . . . . ? C62 C63 C64 C65 0.0 . . . . ? C62 C63 C64 C68 177.6(6) . . . . ? C63 C64 C65 C66 0.0 . . . . ? C68 C64 C65 C66 -177.6(6) . . . . ? C64 C65 C66 C61 0.0 . . . . ? C64 C65 C66 C69 177.5(5) . . . . ? C62 C61 C66 C65 0.0 . . . . ? N2 C61 C66 C65 170.7(5) . . . . ? C62 C61 C66 C69 -177.5(5) . . . . ? N2 C61 C66 C69 -6.7(6) . . . . ? C77 C72 C73 C74 0.0 . . . . ? C71 C72 C73 C74 176.7(18) . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C77 0.0 . . . . ? C75 C76 C77 C72 0.0 . . . . ? C73 C72 C77 C76 0.0 . . . . ? C71 C72 C77 C76 -176.6(18) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.942 _refine_diff_density_min -2.338 _refine_diff_density_rms 0.242 # Attachment 'Revised_2.cif' data_04141 _database_code_depnum_ccdc_archive 'CCDC 629183' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H24 Ag Cl N2 O10 Os3' _chemical_formula_sum 'C31 H24 Ag Cl N2 O10 Os3' _chemical_formula_weight 1298.44 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1388(6) _cell_length_b 12.5307(9) _cell_length_c 18.0480(10) _cell_angle_alpha 93.746(4) _cell_angle_beta 97.217(4) _cell_angle_gamma 97.567(3) _cell_volume 1803.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4867 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 11.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1488 _exptl_absorpt_correction_T_max 0.4873 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17458 _diffrn_reflns_av_R_equivalents 0.095 _diffrn_reflns_av_sigmaI/netI 0.1405 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6323 _reflns_number_gt 3864 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0468P)^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_number_reflns 6323 _refine_ls_number_parameters 415 _refine_ls_number_restraints 163 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.64298(7) 0.56500(5) 0.20364(3) 0.02382(18) Uani 1 1 d U . . Os2 Os 0.57308(7) 0.67904(5) 0.33315(3) 0.02478(18) Uani 1 1 d U . . Os3 Os 0.77412(8) 0.51047(5) 0.34761(3) 0.02870(19) Uani 1 1 d U . . Ag Ag 0.71103(14) 0.79136(9) 0.22145(6) 0.0248(3) Uani 1 1 d U . . Cl Cl 0.3699(4) 0.5475(3) 0.2502(2) 0.0313(9) Uani 1 1 d U . . C1 C 0.8166(16) 0.9379(11) 0.1822(7) 0.019(3) Uani 1 1 d U . . N2 N 0.8297(16) 1.0373(9) 0.2147(6) 0.034(3) Uani 1 1 d U . . C3 C 0.906(2) 1.1155(12) 0.1716(8) 0.045(5) Uani 1 1 d U . . H3A H 0.9286 1.1915 0.1834 0.054 Uiso 1 1 calc R . . C4 C 0.939(2) 1.0579(12) 0.1094(8) 0.044(5) Uani 1 1 d U . . H4A H 0.9933 1.0855 0.0696 0.053 Uiso 1 1 calc R . . N5 N 0.8763(15) 0.9501(9) 0.1163(6) 0.030(3) Uani 1 1 d U . . C41 C 0.7878(11) 1.0649(7) 0.2873(4) 0.021(3) Uani 1 1 d GU . . C42 C 0.9052(8) 1.0673(8) 0.3505(5) 0.030(3) Uani 1 1 d GU . . C43 C 0.8615(10) 1.0898(8) 0.4213(4) 0.034(4) Uani 1 1 d GU . . H43A H 0.9418 1.0914 0.4646 0.041 Uiso 1 1 calc R . . C44 C 0.7002(11) 1.1099(8) 0.4289(4) 0.029(3) Uani 1 1 d GU . . C45 C 0.5827(9) 1.1075(8) 0.3656(5) 0.031(4) Uani 1 1 d GU . . H45A H 0.4725 1.1213 0.3708 0.037 Uiso 1 1 calc R . . C46 C 0.6265(9) 1.0850(8) 0.2948(4) 0.024(3) Uani 1 1 d GU . . C47 C 0.499(2) 1.0842(14) 0.2253(8) 0.046(5) Uani 1 1 d U . . H47A H 0.4814 1.0128 0.1976 0.069 Uiso 1 1 calc R . . H47B H 0.5397 1.1390 0.1932 0.069 Uiso 1 1 calc R . . H47C H 0.3923 1.1001 0.2404 0.069 Uiso 1 1 calc R . . C48 C 0.653(2) 1.1296(14) 0.5063(8) 0.054(5) Uani 1 1 d U . . H48A H 0.7070 1.2010 0.5284 0.081 Uiso 1 1 calc R . . H48B H 0.6888 1.0740 0.5378 0.081 Uiso 1 1 calc R . . H48C H 0.5309 1.1267 0.5028 0.081 Uiso 1 1 calc R . . C49 C 1.081(2) 1.0463(15) 0.3432(9) 0.062(6) Uani 1 1 d U . . H49A H 1.0770 0.9802 0.3104 0.092 Uiso 1 1 calc R . . H49B H 1.1398 1.0376 0.3928 0.092 Uiso 1 1 calc R . . H49C H 1.1405 1.1074 0.3216 0.092 Uiso 1 1 calc R . . C51 C 0.8916(12) 0.8633(6) 0.0640(4) 0.024(3) Uani 1 1 d GU . . C52 C 0.7571(9) 0.8259(7) 0.0091(5) 0.028(3) Uani 1 1 d GU . . C53 C 0.7681(9) 0.7408(7) -0.0427(4) 0.030(3) Uani 1 1 d GU . . H53A H 0.6762 0.7152 -0.0802 0.036 Uiso 1 1 calc R . . C54 C 0.9135(11) 0.6933(6) -0.0395(4) 0.031(3) Uani 1 1 d GU . . C55 C 1.0480(9) 0.7308(7) 0.0154(5) 0.032(3) Uani 1 1 d GU . . H55A H 1.1473 0.6983 0.0176 0.038 Uiso 1 1 calc R . . C56 C 1.0370(9) 0.8158(7) 0.0672(4) 0.026(3) Uani 1 1 d GU . . C57 C 0.5992(19) 0.8783(14) 0.0038(8) 0.048(5) Uani 1 1 d U . . H57A H 0.5600 0.8823 0.0529 0.072 Uiso 1 1 calc R . . H57B H 0.5126 0.8353 -0.0328 0.072 Uiso 1 1 calc R . . H57C H 0.6228 0.9514 -0.0122 0.072 Uiso 1 1 calc R . . C58 C 0.923(2) 0.5982(12) -0.0937(9) 0.049(5) Uani 1 1 d U . . H58A H 0.8571 0.5336 -0.0794 0.073 Uiso 1 1 calc R . . H58B H 1.0403 0.5862 -0.0924 0.073 Uiso 1 1 calc R . . H58C H 0.8793 0.6130 -0.1444 0.073 Uiso 1 1 calc R . . C59 C 1.183(2) 0.8565(13) 0.1268(8) 0.045(4) Uani 1 1 d U . . H59A H 1.2725 0.8125 0.1224 0.068 Uiso 1 1 calc R . . H59B H 1.1464 0.8514 0.1764 0.068 Uiso 1 1 calc R . . H59C H 1.2236 0.9320 0.1204 0.068 Uiso 1 1 calc R . . O11 O 0.9956(13) 0.6251(8) 0.1709(6) 0.036(3) Uani 1 1 d U . . C11 C 0.8626(18) 0.6050(11) 0.1849(8) 0.025(3) Uani 1 1 d U . . O12 O 0.6487(14) 0.3301(9) 0.1531(6) 0.049(3) Uani 1 1 d U . . C12 C 0.6501(18) 0.4218(13) 0.1744(8) 0.029(3) Uani 1 1 d U . . O13 O 0.4737(14) 0.6296(9) 0.0574(5) 0.045(3) Uani 1 1 d U . . C13 C 0.539(2) 0.6113(14) 0.1143(8) 0.045(4) Uani 1 1 d U . . O21 O 0.8623(15) 0.8314(10) 0.4205(6) 0.051(3) Uani 1 1 d U . . C21 C 0.753(2) 0.7758(13) 0.3861(8) 0.034(3) Uani 1 1 d U . . O22 O 0.4607(16) 0.6207(9) 0.4817(6) 0.064(4) Uani 1 1 d U . . C22 C 0.502(2) 0.6422(13) 0.4258(8) 0.044(4) Uani 1 1 d U . . O23 O 0.3611(11) 0.8610(8) 0.3059(5) 0.028(2) Uani 1 1 d U . . C23 C 0.4420(18) 0.7913(11) 0.3124(8) 0.029(3) Uani 1 1 d U . . O31 O 1.0801(14) 0.6831(9) 0.3420(6) 0.052(3) Uani 1 1 d U . . C31 C 0.963(2) 0.6192(14) 0.3412(8) 0.037(3) Uani 1 1 d U . . O32 O 0.4498(15) 0.3456(9) 0.3409(7) 0.060(4) Uani 1 1 d U . . C32 C 0.568(2) 0.4101(12) 0.3426(8) 0.033(3) Uani 1 1 d U . . O33 O 0.8345(14) 0.5395(11) 0.5191(6) 0.069(4) Uani 1 1 d U . . C33 C 0.812(2) 0.5238(14) 0.4549(9) 0.044(4) Uani 1 1 d U . . O34 O 0.9784(15) 0.3307(9) 0.3095(6) 0.056(3) Uani 1 1 d U . . C34 C 0.896(2) 0.3966(13) 0.3246(8) 0.040(4) Uani 1 1 d U . . 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 0.0280(4) 0.0210(4) 0.0223(3) 0.0014(3) 0.0030(3) 0.0035(3) Os2 0.0300(4) 0.0238(4) 0.0222(3) 0.0039(3) 0.0071(3) 0.0056(3) Os3 0.0331(4) 0.0285(4) 0.0253(3) 0.0047(3) 0.0020(3) 0.0083(3) Ag 0.0302(7) 0.0212(7) 0.0240(6) 0.0034(5) 0.0072(5) 0.0036(6) Cl 0.023(2) 0.025(2) 0.044(2) 0.0031(18) 0.0022(17) -0.0012(17) C1 0.015(8) 0.013(5) 0.027(7) -0.001(5) 0.006(6) -0.002(6) N2 0.066(10) 0.013(5) 0.028(6) -0.001(5) 0.024(6) 0.007(6) C3 0.089(14) 0.011(6) 0.039(9) 0.001(6) 0.038(10) -0.004(9) C4 0.084(14) 0.025(7) 0.031(9) 0.005(7) 0.036(9) 0.005(9) N5 0.050(9) 0.021(6) 0.019(6) -0.001(4) 0.016(6) 0.002(6) C41 0.031(7) 0.012(8) 0.022(6) 0.001(6) 0.011(5) 0.003(7) C42 0.032(8) 0.026(9) 0.033(6) 0.009(7) 0.002(5) 0.001(8) C43 0.039(8) 0.037(10) 0.025(6) 0.001(8) -0.003(6) 0.004(8) C44 0.042(9) 0.022(9) 0.020(6) -0.002(7) 0.001(5) -0.010(8) C45 0.026(8) 0.043(11) 0.030(6) 0.003(8) 0.015(5) 0.020(8) C46 0.030(7) 0.022(9) 0.022(6) 0.004(7) 0.011(5) 0.004(7) C47 0.043(9) 0.059(13) 0.039(7) 0.017(9) -0.001(7) 0.015(10) C48 0.075(14) 0.058(13) 0.032(7) -0.005(9) 0.017(8) 0.018(11) C49 0.033(9) 0.090(17) 0.066(13) 0.022(12) 0.015(8) 0.012(11) C51 0.036(7) 0.015(7) 0.023(7) 0.001(5) 0.014(5) -0.001(6) C52 0.033(8) 0.022(9) 0.028(8) -0.007(5) 0.007(5) 0.007(7) C53 0.024(8) 0.028(9) 0.032(8) -0.005(6) 0.000(6) -0.008(7) C54 0.040(9) 0.024(9) 0.028(8) -0.008(6) 0.009(6) 0.005(7) C55 0.031(8) 0.043(10) 0.020(8) -0.012(6) 0.011(5) 0.001(7) C56 0.034(8) 0.026(9) 0.019(7) 0.001(5) 0.006(5) 0.003(7) C57 0.048(10) 0.068(13) 0.037(10) 0.010(9) 0.010(8) 0.033(10) C58 0.055(13) 0.027(10) 0.054(11) -0.029(7) 0.001(9) -0.006(8) C59 0.044(9) 0.045(12) 0.040(10) -0.011(7) -0.007(7) -0.002(9) O11 0.030(6) 0.020(6) 0.061(7) 0.001(5) 0.021(6) 0.002(5) C11 0.026(6) 0.009(7) 0.037(8) -0.002(6) 0.003(6) -0.008(6) O12 0.050(8) 0.028(6) 0.059(8) -0.023(6) -0.005(6) -0.009(6) C12 0.019(8) 0.027(5) 0.035(7) -0.014(6) 0.004(6) -0.013(6) O13 0.054(8) 0.049(8) 0.026(6) 0.004(6) -0.008(5) -0.003(6) C13 0.049(9) 0.065(10) 0.021(5) -0.001(6) -0.001(5) 0.020(8) O21 0.052(8) 0.058(9) 0.034(7) -0.007(6) -0.014(5) 0.001(6) C21 0.049(8) 0.032(7) 0.019(6) -0.003(5) -0.010(6) 0.012(6) O22 0.106(11) 0.063(9) 0.041(7) 0.022(7) 0.055(7) 0.026(8) C22 0.070(12) 0.040(11) 0.032(6) 0.013(6) 0.023(7) 0.020(8) O23 0.025(6) 0.031(6) 0.029(6) -0.001(5) 0.002(5) 0.006(5) C23 0.031(8) 0.019(7) 0.039(9) 0.007(6) 0.018(6) 0.000(6) O31 0.042(8) 0.048(8) 0.057(8) -0.016(6) -0.002(6) -0.006(5) C31 0.026(7) 0.047(9) 0.037(8) 0.006(8) -0.003(6) 0.005(5) O32 0.057(8) 0.041(8) 0.085(10) 0.030(7) 0.013(7) 0.000(5) C32 0.046(7) 0.022(7) 0.031(8) 0.010(7) 0.005(7) 0.003(5) O33 0.046(8) 0.137(13) 0.025(5) 0.000(7) -0.004(6) 0.023(8) C33 0.038(10) 0.069(13) 0.028(5) 0.004(7) 0.002(6) 0.018(8) O34 0.054(9) 0.032(8) 0.078(9) -0.011(6) -0.005(7) 0.014(6) C34 0.051(10) 0.037(8) 0.037(9) 0.008(7) 0.010(8) 0.014(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 1.847(16) . ? Os1 C11 1.871(14) . ? Os1 C13 1.886(14) . ? Os1 Cl 2.462(3) . ? Os1 Ag 2.8068(13) . ? Os1 Os2 2.8179(8) . ? Os1 Os3 2.8435(8) . ? Os2 C21 1.885(19) . ? Os2 C22 1.902(14) . ? Os2 C23 1.902(13) . ? Os2 Cl 2.455(4) . ? Os2 Ag 2.7980(11) . ? Os2 Os3 2.8429(8) . ? Os3 C34 1.898(15) . ? Os3 C33 1.914(15) . ? Os3 C31 1.935(18) . ? Os3 C32 1.945(17) . ? Ag C1 2.125(12) . ? C1 N2 1.328(16) . ? C1 N5 1.350(14) . ? N2 C3 1.417(16) . ? N2 C41 1.427(12) . ? C3 C4 1.371(19) . ? C3 H3A 0.9500 . ? C4 N5 1.399(18) . ? C4 H4A 0.9500 . ? N5 C51 1.421(12) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C42 C49 1.509(15) . ? C43 C44 1.3900 . ? C43 H43A 0.9500 . ? C44 C45 1.3900 . ? C44 C48 1.510(14) . ? C45 C46 1.3900 . ? C45 H45A 0.9500 . ? C46 C47 1.525(16) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C52 C57 1.515(14) . ? C53 C54 1.3900 . ? C53 H53A 0.9500 . ? C54 C55 1.3900 . ? C54 C58 1.508(15) . ? C55 C56 1.3900 . ? C55 H55A 0.9500 . ? C56 C59 1.507(17) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? O11 C11 1.142(15) . ? O12 C12 1.186(16) . ? O13 C13 1.148(15) . ? O21 C21 1.142(18) . ? O22 C22 1.141(14) . ? O23 C23 1.164(14) . ? O31 C31 1.160(18) . ? O32 C32 1.171(18) . ? O33 C33 1.151(16) . ? O34 C34 1.167(15) . ? 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 91.7(6) . . ? C12 Os1 C13 100.8(7) . . ? C11 Os1 C13 95.9(6) . . ? C12 Os1 Cl 99.7(4) . . ? C11 Os1 Cl 166.9(5) . . ? C13 Os1 Cl 88.5(5) . . ? C12 Os1 Ag 162.6(4) . . ? C11 Os1 Ag 72.2(4) . . ? C13 Os1 Ag 75.1(5) . . ? Cl Os1 Ag 97.11(9) . . ? C12 Os1 Os2 135.4(4) . . ? C11 Os1 Os2 112.1(4) . . ? C13 Os1 Os2 112.9(4) . . ? Cl Os1 Os2 54.92(10) . . ? Ag Os1 Os2 59.66(3) . . ? C12 Os1 Os3 84.5(4) . . ? C11 Os1 Os3 88.5(4) . . ? C13 Os1 Os3 173.0(4) . . ? Cl Os1 Os3 86.06(8) . . ? Ag Os1 Os3 101.21(3) . . ? Os2 Os1 Os3 60.28(2) . . ? C21 Os2 C22 89.4(7) . . ? C21 Os2 C23 92.8(6) . . ? C22 Os2 C23 99.3(6) . . ? C21 Os2 Cl 171.0(5) . . ? C22 Os2 Cl 97.9(6) . . ? C23 Os2 Cl 91.2(5) . . ? C21 Os2 Ag 76.0(4) . . ? C22 Os2 Ag 163.1(5) . . ? C23 Os2 Ag 73.3(4) . . ? Cl Os2 Ag 97.50(8) . . ? C21 Os2 Os1 115.8(4) . . ? C22 Os2 Os1 136.0(5) . . ? C23 Os2 Os1 113.7(4) . . ? Cl Os2 Os1 55.14(8) . . ? Ag Os2 Os1 59.97(3) . . ? C21 Os2 Os3 89.0(4) . . ? C22 Os2 Os3 86.6(4) . . ? C23 Os2 Os3 173.8(4) . . ? Cl Os2 Os3 86.20(8) . . ? Ag Os2 Os3 101.44(3) . . ? Os1 Os2 Os3 60.304(19) . . ? C34 Os3 C33 101.8(6) . . ? C34 Os3 C31 92.1(7) . . ? C33 Os3 C31 92.3(7) . . ? C34 Os3 C32 91.6(7) . . ? C33 Os3 C32 93.8(7) . . ? C31 Os3 C32 172.1(6) . . ? C34 Os3 Os2 162.3(4) . . ? C33 Os3 Os2 95.9(4) . . ? C31 Os3 Os2 86.6(4) . . ? C32 Os3 Os2 87.7(4) . . ? C34 Os3 Os1 102.9(4) . . ? C33 Os3 Os1 155.3(4) . . ? C31 Os3 Os1 86.2(4) . . ? C32 Os3 Os1 86.2(4) . . ? Os2 Os3 Os1 59.414(19) . . ? C1 Ag Os2 150.4(4) . . ? C1 Ag Os1 148.9(3) . . ? Os2 Ag Os1 60.37(3) . . ? Os2 Cl Os1 69.94(10) . . ? N2 C1 N5 105.1(11) . . ? N2 C1 Ag 127.8(9) . . ? N5 C1 Ag 127.0(10) . . ? C1 N2 C3 112.0(11) . . ? C1 N2 C41 125.6(10) . . ? C3 N2 C41 122.2(12) . . ? C4 C3 N2 105.1(13) . . ? C4 C3 H3A 127.4 . . ? N2 C3 H3A 127.4 . . ? C3 C4 N5 105.9(12) . . ? C3 C4 H4A 127.0 . . ? N5 C4 H4A 127.0 . . ? C1 N5 C4 111.7(11) . . ? C1 N5 C51 124.4(11) . . ? C4 N5 C51 123.5(10) . . ? C42 C41 C46 120.0 . . ? C42 C41 N2 120.3(8) . . ? C46 C41 N2 119.7(8) . . ? C43 C42 C41 120.0 . . ? C43 C42 C49 119.4(9) . . ? C41 C42 C49 120.6(9) . . ? C42 C43 C44 120.0 . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 C48 120.6(9) . . ? C43 C44 C48 119.4(9) . . ? C44 C45 C46 120.0 . . ? C44 C45 H45A 120.0 . . ? C46 C45 H45A 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 C47 120.1(8) . . ? C41 C46 C47 119.9(8) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C42 C49 H49A 109.5 . . ? C42 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C42 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 C51 C56 120.0 . . ? C52 C51 N5 118.6(8) . . ? C56 C51 N5 121.4(8) . . ? C53 C52 C51 120.0 . . ? C53 C52 C57 119.3(9) . . ? C51 C52 C57 120.7(9) . . ? C52 C53 C54 120.0 . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 C58 120.2(9) . . ? C55 C54 C58 119.8(9) . . ? C56 C55 C54 120.0 . . ? C56 C55 H55A 120.0 . . ? C54 C55 H55A 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 C59 120.1(8) . . ? C51 C56 C59 119.9(8) . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O11 C11 Os1 176.6(13) . . ? O12 C12 Os1 177.0(14) . . ? O13 C13 Os1 173.7(15) . . ? O21 C21 Os2 177.2(13) . . ? O22 C22 Os2 179.4(18) . . ? O23 C23 Os2 174.5(12) . . ? O31 C31 Os3 175.6(14) . . ? O32 C32 Os3 176.4(12) . . ? O33 C33 Os3 175.2(16) . . ? O34 C34 Os3 176.3(15) . . ? 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 C12 Os1 Os2 C21 115.1(8) . . . . ? C11 Os1 Os2 C21 -2.1(6) . . . . ? C13 Os1 Os2 C21 -109.0(8) . . . . ? Cl Os1 Os2 C21 -179.7(5) . . . . ? Ag Os1 Os2 C21 -53.8(5) . . . . ? Os3 Os1 Os2 C21 72.6(5) . . . . ? C12 Os1 Os2 C22 -3.9(10) . . . . ? C11 Os1 Os2 C22 -121.1(9) . . . . ? C13 Os1 Os2 C22 132.0(10) . . . . ? Cl Os1 Os2 C22 61.3(8) . . . . ? Ag Os1 Os2 C22 -172.8(8) . . . . ? Os3 Os1 Os2 C22 -46.4(8) . . . . ? C12 Os1 Os2 C23 -139.1(8) . . . . ? C11 Os1 Os2 C23 103.7(6) . . . . ? C13 Os1 Os2 C23 -3.2(8) . . . . ? Cl Os1 Os2 C23 -73.9(5) . . . . ? Ag Os1 Os2 C23 52.0(5) . . . . ? Os3 Os1 Os2 C23 178.4(5) . . . . ? C12 Os1 Os2 Cl -65.2(7) . . . . ? C11 Os1 Os2 Cl 177.6(4) . . . . ? C13 Os1 Os2 Cl 70.7(6) . . . . ? Ag Os1 Os2 Cl 125.89(10) . . . . ? Os3 Os1 Os2 Cl -107.71(9) . . . . ? C12 Os1 Os2 Ag 168.9(7) . . . . ? C11 Os1 Os2 Ag 51.7(4) . . . . ? C13 Os1 Os2 Ag -55.2(6) . . . . ? Cl Os1 Os2 Ag -125.89(10) . . . . ? Os3 Os1 Os2 Ag 126.40(4) . . . . ? C12 Os1 Os2 Os3 42.5(7) . . . . ? C11 Os1 Os2 Os3 -74.7(4) . . . . ? C13 Os1 Os2 Os3 178.4(6) . . . . ? Cl Os1 Os2 Os3 107.71(9) . . . . ? Ag Os1 Os2 Os3 -126.40(4) . . . . ? C21 Os2 Os3 C34 -119.6(18) . . . . ? C22 Os2 Os3 C34 150.9(18) . . . . ? C23 Os2 Os3 C34 -13(5) . . . . ? Cl Os2 Os3 C34 52.8(17) . . . . ? Ag Os2 Os3 C34 -44.1(17) . . . . ? Os1 Os2 Os3 C34 1.2(17) . . . . ? C21 Os2 Os3 C33 58.8(7) . . . . ? C22 Os2 Os3 C33 -30.7(8) . . . . ? C23 Os2 Os3 C33 166(4) . . . . ? Cl Os2 Os3 C33 -128.9(6) . . . . ? Ag Os2 Os3 C33 134.2(5) . . . . ? Os1 Os2 Os3 C33 179.6(5) . . . . ? C21 Os2 Os3 C31 -33.2(6) . . . . ? C22 Os2 Os3 C31 -122.7(7) . . . . ? C23 Os2 Os3 C31 74(4) . . . . ? Cl Os2 Os3 C31 139.1(5) . . . . ? Ag Os2 Os3 C31 42.3(5) . . . . ? Os1 Os2 Os3 C31 87.6(5) . . . . ? C21 Os2 Os3 C32 152.3(6) . . . . ? C22 Os2 Os3 C32 62.8(7) . . . . ? C23 Os2 Os3 C32 -101(4) . . . . ? Cl Os2 Os3 C32 -35.3(4) . . . . ? Ag Os2 Os3 C32 -132.2(4) . . . . ? Os1 Os2 Os3 C32 -86.9(4) . . . . ? C21 Os2 Os3 Os1 -120.8(4) . . . . ? C22 Os2 Os3 Os1 149.7(6) . . . . ? C23 Os2 Os3 Os1 -14(4) . . . . ? Cl Os2 Os3 Os1 51.58(8) . . . . ? Ag Os2 Os3 Os1 -45.31(3) . . . . ? C12 Os1 Os3 C34 28.8(7) . . . . ? C11 Os1 Os3 C34 -63.0(7) . . . . ? C13 Os1 Os3 C34 168(5) . . . . ? Cl Os1 Os3 C34 129.0(5) . . . . ? Ag Os1 Os3 C34 -134.5(5) . . . . ? Os2 Os1 Os3 C34 -179.6(5) . . . . ? C12 Os1 Os3 C33 -152.6(14) . . . . ? C11 Os1 Os3 C33 115.6(14) . . . . ? C13 Os1 Os3 C33 -13(5) . . . . ? Cl Os1 Os3 C33 -52.4(13) . . . . ? Ag Os1 Os3 C33 44.0(13) . . . . ? Os2 Os1 Os3 C33 -1.0(13) . . . . ? C12 Os1 Os3 C31 120.1(6) . . . . ? C11 Os1 Os3 C31 28.3(6) . . . . ? C13 Os1 Os3 C31 -100(5) . . . . ? Cl Os1 Os3 C31 -139.7(5) . . . . ? Ag Os1 Os3 C31 -43.2(5) . . . . ? Os2 Os1 Os3 C31 -88.3(5) . . . . ? C12 Os1 Os3 C32 -61.9(6) . . . . ? C11 Os1 Os3 C32 -153.7(6) . . . . ? C13 Os1 Os3 C32 77(5) . . . . ? Cl Os1 Os3 C32 38.2(4) . . . . ? Ag Os1 Os3 C32 134.7(4) . . . . ? Os2 Os1 Os3 C32 89.6(4) . . . . ? C12 Os1 Os3 Os2 -151.5(4) . . . . ? C11 Os1 Os3 Os2 116.6(4) . . . . ? C13 Os1 Os3 Os2 -12(5) . . . . ? Cl Os1 Os3 Os2 -51.39(9) . . . . ? Ag Os1 Os3 Os2 45.09(3) . . . . ? C21 Os2 Ag C1 -41.5(8) . . . . ? C22 Os2 Ag C1 -10.4(18) . . . . ? C23 Os2 Ag C1 55.8(9) . . . . ? Cl Os2 Ag C1 144.8(7) . . . . ? Os1 Os2 Ag C1 -173.1(7) . . . . ? Os3 Os2 Ag C1 -127.6(7) . . . . ? C21 Os2 Ag Os1 131.5(5) . . . . ? C22 Os2 Ag Os1 162.7(16) . . . . ? C23 Os2 Ag Os1 -131.1(5) . . . . ? Cl Os2 Ag Os1 -42.11(8) . . . . ? Os3 Os2 Ag Os1 45.51(3) . . . . ? C12 Os1 Ag C1 20.2(17) . . . . ? C11 Os1 Ag C1 43.1(8) . . . . ? C13 Os1 Ag C1 -58.2(8) . . . . ? Cl Os1 Ag C1 -144.7(7) . . . . ? Os2 Os1 Ag C1 173.4(7) . . . . ? Os3 Os1 Ag C1 127.9(7) . . . . ? C12 Os1 Ag Os2 -153.1(16) . . . . ? C11 Os1 Ag Os2 -130.2(4) . . . . ? C13 Os1 Ag Os2 128.5(5) . . . . ? Cl Os1 Ag Os2 41.92(9) . . . . ? Os3 Os1 Ag Os2 -45.45(3) . . . . ? C21 Os2 Cl Os1 2(3) . . . . ? C22 Os2 Cl Os1 -142.1(4) . . . . ? C23 Os2 Cl Os1 118.3(4) . . . . ? Ag Os2 Cl Os1 45.03(6) . . . . ? Os3 Os2 Cl Os1 -56.03(5) . . . . ? C12 Os1 Cl Os2 139.7(5) . . . . ? C11 Os1 Cl Os2 -9.8(17) . . . . ? C13 Os1 Cl Os2 -119.5(5) . . . . ? Ag Os1 Cl Os2 -44.80(7) . . . . ? Os3 Os1 Cl Os2 56.03(5) . . . . ? Os2 Ag C1 N2 -6.9(17) . . . . ? Os1 Ag C1 N2 -175.2(8) . . . . ? Os2 Ag C1 N5 177.2(7) . . . . ? Os1 Ag C1 N5 8.9(16) . . . . ? N5 C1 N2 C3 -2.7(17) . . . . ? Ag C1 N2 C3 -179.3(11) . . . . ? N5 C1 N2 C41 -177.4(12) . . . . ? Ag C1 N2 C41 6(2) . . . . ? C1 N2 C3 C4 0.2(19) . . . . ? C41 N2 C3 C4 175.1(13) . . . . ? N2 C3 C4 N5 2.3(19) . . . . ? N2 C1 N5 C4 4.2(17) . . . . ? Ag C1 N5 C4 -179.1(11) . . . . ? N2 C1 N5 C51 177.6(11) . . . . ? Ag C1 N5 C51 -5.8(19) . . . . ? C3 C4 N5 C1 -4.2(19) . . . . ? C3 C4 N5 C51 -177.6(12) . . . . ? C1 N2 C41 C42 87.0(15) . . . . ? C3 N2 C41 C42 -87.3(14) . . . . ? C1 N2 C41 C46 -90.3(14) . . . . ? C3 N2 C41 C46 95.4(14) . . . . ? C46 C41 C42 C43 0.0 . . . . ? N2 C41 C42 C43 -177.3(9) . . . . ? C46 C41 C42 C49 -179.7(11) . . . . ? N2 C41 C42 C49 3.1(12) . . . . ? C41 C42 C43 C44 0.0 . . . . ? C49 C42 C43 C44 179.7(11) . . . . ? C42 C43 C44 C45 0.0 . . . . ? C42 C43 C44 C48 177.5(11) . . . . ? C43 C44 C45 C46 0.0 . . . . ? C48 C44 C45 C46 -177.5(11) . . . . ? C44 C45 C46 C41 0.0 . . . . ? C44 C45 C46 C47 -179.0(11) . . . . ? C42 C41 C46 C45 0.0 . . . . ? N2 C41 C46 C45 177.3(9) . . . . ? C42 C41 C46 C47 179.0(11) . . . . ? N2 C41 C46 C47 -3.7(12) . . . . ? C1 N5 C51 C52 89.5(13) . . . . ? C4 N5 C51 C52 -97.9(14) . . . . ? C1 N5 C51 C56 -90.2(13) . . . . ? C4 N5 C51 C56 82.3(14) . . . . ? C56 C51 C52 C53 0.0 . . . . ? N5 C51 C52 C53 -179.7(8) . . . . ? C56 C51 C52 C57 -178.6(10) . . . . ? N5 C51 C52 C57 1.6(11) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C57 C52 C53 C54 178.7(10) . . . . ? C52 C53 C54 C55 0.0 . . . . ? C52 C53 C54 C58 177.6(10) . . . . ? C53 C54 C55 C56 0.0 . . . . ? C58 C54 C55 C56 -177.6(10) . . . . ? C54 C55 C56 C51 0.0 . . . . ? C54 C55 C56 C59 180.0(10) . . . . ? C52 C51 C56 C55 0.0 . . . . ? N5 C51 C56 C55 179.7(9) . . . . ? C52 C51 C56 C59 -180.0(10) . . . . ? N5 C51 C56 C59 -0.2(11) . . . . ? C12 Os1 C11 O11 25(21) . . . . ? C13 Os1 C11 O11 -76(21) . . . . ? Cl Os1 C11 O11 175(19) . . . . ? Ag Os1 C11 O11 -148(21) . . . . ? Os2 Os1 C11 O11 167(21) . . . . ? Os3 Os1 C11 O11 110(21) . . . . ? C11 Os1 C12 O12 -119(24) . . . . ? C13 Os1 C12 O12 -22(24) . . . . ? Cl Os1 C12 O12 68(24) . . . . ? Ag Os1 C12 O12 -97(24) . . . . ? Os2 Os1 C12 O12 117(24) . . . . ? Os3 Os1 C12 O12 153(24) . . . . ? C12 Os1 C13 O13 9(13) . . . . ? C11 Os1 C13 O13 101(13) . . . . ? Cl Os1 C13 O13 -91(13) . . . . ? Ag Os1 C13 O13 171(13) . . . . ? Os2 Os1 C13 O13 -142(12) . . . . ? Os3 Os1 C13 O13 -130(10) . . . . ? C22 Os2 C21 O21 36(30) . . . . ? C23 Os2 C21 O21 135(30) . . . . ? Cl Os2 C21 O21 -108(29) . . . . ? Ag Os2 C21 O21 -153(30) . . . . ? Os1 Os2 C21 O21 -107(30) . . . . ? Os3 Os2 C21 O21 -51(30) . . . . ? C21 Os2 C22 O22 8(100) . . . . ? C23 Os2 C22 O22 -85(100) . . . . ? Cl Os2 C22 O22 -177(100) . . . . ? Ag Os2 C22 O22 -22(100) . . . . ? Os1 Os2 C22 O22 136(100) . . . . ? Os3 Os2 C22 O22 97(100) . . . . ? C21 Os2 C23 O23 -67(14) . . . . ? C22 Os2 C23 O23 23(14) . . . . ? Cl Os2 C23 O23 121(14) . . . . ? Ag Os2 C23 O23 -142(14) . . . . ? Os1 Os2 C23 O23 173(14) . . . . ? Os3 Os2 C23 O23 -174(10) . . . . ? C34 Os3 C31 O31 -81(19) . . . . ? C33 Os3 C31 O31 21(19) . . . . ? C32 Os3 C31 O31 162(16) . . . . ? Os2 Os3 C31 O31 117(19) . . . . ? Os1 Os3 C31 O31 177(19) . . . . ? C34 Os3 C32 O32 32(23) . . . . ? C33 Os3 C32 O32 -70(23) . . . . ? C31 Os3 C32 O32 150(21) . . . . ? Os2 Os3 C32 O32 -166(23) . . . . ? Os1 Os3 C32 O32 135(23) . . . . ? C34 Os3 C33 O33 146(17) . . . . ? C31 Os3 C33 O33 54(17) . . . . ? C32 Os3 C33 O33 -121(17) . . . . ? Os2 Os3 C33 O33 -33(17) . . . . ? Os1 Os3 C33 O33 -32(18) . . . . ? C33 Os3 C34 O34 -104(22) . . . . ? C31 Os3 C34 O34 -11(22) . . . . ? C32 Os3 C34 O34 162(22) . . . . ? Os2 Os3 C34 O34 74(23) . . . . ? Os1 Os3 C34 O34 75(22) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.739 _refine_diff_density_min -2.498 _refine_diff_density_rms 0.323 # Attachment 'Revised_3.cif' data_04092c2 _database_code_depnum_ccdc_archive 'CCDC 629184' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H25 Ag Cl2 N2 O20 Os6' _chemical_formula_sum 'C41 H25 Ag Cl2 N2 O20 Os6' _chemical_formula_weight 2185.60 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.5755(8) _cell_length_b 21.6908(16) _cell_length_c 17.6188(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.714(3) _cell_angle_gamma 90.00 _cell_volume 5334.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4227 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3928 _exptl_absorpt_coefficient_mu 14.763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0955 _exptl_absorpt_correction_T_max 0.3199 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14906 _diffrn_reflns_av_R_equivalents 0.106 _diffrn_reflns_av_sigmaI/netI 0.1210 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4392 _reflns_number_gt 2622 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.1154P)^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_number_reflns 4392 _refine_ls_number_parameters 329 _refine_ls_number_restraints 263 _refine_ls_R_factor_all 0.1404 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2044 _refine_ls_wR_factor_gt 0.1721 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.002 _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 0.85576(6) 0.04148(4) 0.10520(6) 0.0404(3) Uani 1 1 d U . . Os2 Os 0.79767(6) -0.00396(5) 0.23160(6) 0.0419(3) Uani 1 1 d U . . Os3 Os 0.71195(6) -0.05223(5) 0.07642(6) 0.0445(3) Uani 1 1 d U . . Ag Ag 1.0000 0.01491(12) 0.2500 0.0415(7) Uani 1 2 d SU . . Cl Cl 0.7529(5) 0.0978(3) 0.1700(4) 0.0580(17) Uani 1 1 d U . . O12 O 0.9903(12) -0.0460(8) 0.0604(11) 0.063(5) Uani 1 1 d U . . C12 C 0.9386(18) -0.0136(12) 0.0786(15) 0.048(5) Uani 1 1 d U . . O13 O 0.9894(15) 0.1539(9) 0.1424(16) 0.103(8) Uani 1 1 d U . . C13 C 0.9439(18) 0.1090(11) 0.1309(16) 0.052(5) Uani 1 1 d U . . O14 O 0.7660(18) 0.0772(11) -0.0670(13) 0.096(7) Uani 1 1 d U . . C14 C 0.801(2) 0.0655(13) -0.0004(18) 0.059(5) Uani 1 1 d U . . O22 O 0.8945(15) -0.1224(9) 0.2897(14) 0.083(6) Uani 1 1 d U . . C22 C 0.8579(18) -0.0757(13) 0.2696(16) 0.052(5) Uani 1 1 d U . . O23 O 0.8665(13) 0.0600(10) 0.3896(12) 0.071(6) Uani 1 1 d U . . C23 C 0.8458(17) 0.0377(13) 0.3294(16) 0.053(5) Uani 1 1 d U . . O24 O 0.6105(15) -0.0420(13) 0.2630(13) 0.108(9) Uani 1 1 d U . . C24 C 0.6796(19) -0.0266(14) 0.2485(16) 0.060(5) Uani 1 1 d U . . O31 O 0.5637(16) 0.0528(11) 0.0559(15) 0.105(8) Uani 1 1 d U . . C31 C 0.6163(16) 0.0118(12) 0.0638(16) 0.054(6) Uani 1 1 d U . . O32 O 0.8781(14) -0.1471(9) 0.1140(13) 0.079(6) Uani 1 1 d U . . C32 C 0.817(2) -0.1116(11) 0.1033(17) 0.056(6) Uani 1 1 d U . . O33 O 0.5722(15) -0.1454(11) 0.1090(15) 0.108(9) Uani 1 1 d U . . C33 C 0.619(2) -0.1108(14) 0.0969(18) 0.074(7) Uani 1 1 d U . . C34 C 0.6828(16) -0.0623(11) -0.0314(17) 0.046(5) Uani 1 1 d U . . O34 O 0.6586(14) -0.0682(12) -0.1002(13) 0.093(7) Uani 1 1 d U . . C1 C 0.5000 0.2470(15) 0.2500 0.052(8) Uani 1 2 d SU . . H1A H 0.5000 0.2899 0.2500 0.062 Uiso 1 2 calc SR . . N2 N 0.5631(14) 0.2085(8) 0.2308(13) 0.048(5) Uani 1 1 d U . . C3 C 0.5406(19) 0.1490(11) 0.2402(19) 0.068(8) Uani 1 1 d U . . H3A H 0.5756 0.1144 0.2341 0.081 Uiso 1 1 calc R . . C41 C 0.6434(18) 0.2312(11) 0.2045(19) 0.057(5) Uani 1 1 d U . . C42 C 0.733(2) 0.2341(12) 0.264(2) 0.068(6) Uani 1 1 d U . . C43 C 0.809(2) 0.2579(12) 0.238(2) 0.075(7) Uani 1 1 d U . . H43A H 0.8687 0.2624 0.2750 0.090 Uiso 1 1 calc R . . C44 C 0.801(2) 0.2741(13) 0.163(2) 0.077(7) Uani 1 1 d U . . C45 C 0.703(2) 0.2687(14) 0.103(2) 0.083(7) Uani 1 1 d U . . H45A H 0.6939 0.2811 0.0505 0.100 Uiso 1 1 calc R . . C46 C 0.6275(19) 0.2451(12) 0.1261(19) 0.064(6) Uani 1 1 d U . . C47 C 0.752(2) 0.2184(14) 0.348(2) 0.082(8) Uani 1 1 d U . . H47A H 0.8186 0.2240 0.3746 0.124 Uiso 1 1 calc R . . H47B H 0.7342 0.1763 0.3529 0.124 Uiso 1 1 calc R . . H47C H 0.7147 0.2448 0.3717 0.124 Uiso 1 1 calc R . . C48 C 0.876(2) 0.3022(16) 0.133(2) 0.114(12) Uani 1 1 d U . . H48A H 0.9087 0.3335 0.1689 0.171 Uiso 1 1 calc R . . H48B H 0.8467 0.3203 0.0817 0.171 Uiso 1 1 calc R . . H48C H 0.9205 0.2710 0.1279 0.171 Uiso 1 1 calc R . . C49 C 0.533(2) 0.2390(16) 0.068(2) 0.095(10) Uani 1 1 d U . . H49A H 0.4844 0.2527 0.0912 0.142 Uiso 1 1 calc R . . H49B H 0.5218 0.1966 0.0524 0.142 Uiso 1 1 calc R . . H49C H 0.5308 0.2637 0.0223 0.142 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 Os1 0.0278(5) 0.0463(6) 0.0441(7) 0.0044(5) 0.0055(4) 0.0001(4) Os2 0.0250(5) 0.0581(7) 0.0424(7) -0.0039(5) 0.0093(4) 0.0001(4) Os3 0.0270(5) 0.0561(7) 0.0479(8) -0.0063(5) 0.0068(5) -0.0038(4) Ag 0.0262(13) 0.0519(16) 0.0446(18) 0.000 0.0074(11) 0.000 Cl 0.049(4) 0.051(3) 0.070(5) -0.010(3) 0.010(3) 0.015(3) O12 0.038(10) 0.081(13) 0.077(15) 0.014(10) 0.027(10) 0.013(8) C12 0.040(10) 0.060(12) 0.047(9) -0.005(10) 0.019(8) -0.003(7) O13 0.062(14) 0.047(12) 0.20(3) 0.015(13) 0.030(15) -0.017(8) C13 0.045(11) 0.044(10) 0.065(15) 0.001(8) 0.010(9) -0.007(7) O14 0.12(2) 0.103(17) 0.047(10) 0.020(13) 0.004(12) 0.010(14) C14 0.066(16) 0.056(15) 0.047(7) 0.008(9) 0.005(7) -0.005(10) O22 0.070(14) 0.070(12) 0.097(18) 0.014(12) 0.004(12) 0.008(9) C22 0.038(11) 0.062(9) 0.051(11) 0.015(9) 0.004(9) -0.005(7) O23 0.044(11) 0.118(16) 0.050(12) -0.033(11) 0.011(9) 0.002(10) C23 0.025(11) 0.093(16) 0.045(7) -0.013(7) 0.014(8) 0.004(10) O24 0.046(12) 0.20(3) 0.085(18) -0.024(16) 0.031(12) -0.035(13) C24 0.035(8) 0.099(16) 0.048(13) -0.009(12) 0.012(11) -0.013(10) O31 0.069(15) 0.106(17) 0.11(2) -0.022(15) -0.022(13) 0.045(11) C31 0.018(8) 0.062(12) 0.064(14) -0.039(12) -0.019(8) -0.006(6) O32 0.056(12) 0.079(15) 0.104(18) 0.020(12) 0.026(12) 0.019(8) C32 0.072(14) 0.035(8) 0.056(14) 0.006(9) 0.009(12) 0.010(8) O33 0.062(14) 0.120(19) 0.14(2) 0.012(15) 0.023(14) -0.049(12) C33 0.073(15) 0.080(15) 0.063(16) -0.002(14) 0.013(14) -0.038(10) C34 0.025(12) 0.058(15) 0.051(7) -0.003(9) 0.003(8) 0.002(8) O34 0.054(13) 0.16(2) 0.048(8) -0.015(14) -0.004(11) -0.004(13) C1 0.049(17) 0.040(13) 0.08(2) 0.000 0.048(17) 0.000 N2 0.042(9) 0.033(9) 0.076(14) -0.004(9) 0.028(9) 0.005(7) C3 0.054(15) 0.040(10) 0.13(2) -0.023(14) 0.053(15) -0.011(10) C41 0.042(9) 0.047(12) 0.096(12) -0.014(12) 0.043(8) 0.001(9) C42 0.054(10) 0.048(14) 0.105(14) -0.028(13) 0.030(9) -0.011(11) C43 0.047(10) 0.046(15) 0.136(17) -0.005(16) 0.033(12) 0.007(11) C44 0.047(10) 0.064(16) 0.133(18) -0.023(15) 0.047(12) -0.009(11) C45 0.059(11) 0.090(19) 0.114(17) 0.004(16) 0.048(11) -0.019(13) C46 0.051(10) 0.059(15) 0.094(13) -0.021(13) 0.042(9) -0.022(11) C47 0.061(18) 0.07(2) 0.115(15) -0.006(18) 0.021(13) 0.001(15) C48 0.067(17) 0.11(3) 0.18(3) 0.00(2) 0.06(2) -0.028(19) C49 0.047(12) 0.14(3) 0.105(18) -0.02(2) 0.032(11) -0.009(18) _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 1.85(2) . ? Os1 C14 1.87(3) . ? Os1 C13 1.91(2) . ? Os1 Cl 2.455(6) . ? Os1 Os2 2.7807(13) . ? Os1 Os3 2.8584(13) . ? Os1 Ag 2.8593(11) . ? Os2 C22 1.82(3) . ? Os2 C23 1.89(3) . ? Os2 C24 1.89(2) . ? Os2 Cl 2.464(7) . ? Os2 Os3 2.8578(15) . ? Os2 Ag 2.9017(10) . ? Os3 C34 1.84(3) . ? Os3 C31 1.94(2) . ? Os3 C32 1.95(3) . ? Os3 C33 1.97(3) . ? Ag Os1 2.8593(11) 2_755 ? Ag Os2 2.9017(9) 2_755 ? O12 C12 1.14(3) . ? O13 C13 1.16(3) . ? O14 C14 1.17(3) . ? O22 C22 1.15(3) . ? O23 C23 1.13(3) . ? O24 C24 1.16(3) . ? O31 C31 1.16(3) . ? O32 C32 1.15(3) . ? O33 C33 1.08(3) . ? C34 O34 1.17(3) . ? C1 N2 1.36(3) 2_655 ? C1 N2 1.36(3) . ? C1 H1A 0.9300 . ? N2 C3 1.36(3) . ? N2 C41 1.46(3) . ? C3 C3 1.32(4) 2_655 ? C3 H3A 0.9300 . ? C41 C46 1.37(4) . ? C41 C42 1.42(4) . ? C42 C43 1.42(4) . ? C42 C47 1.46(4) . ? C43 C44 1.34(4) . ? C43 H43A 0.9300 . ? C44 C48 1.48(4) . ? C44 C45 1.52(5) . ? C45 C46 1.38(3) . ? C45 H45A 0.9300 . ? C46 C49 1.47(4) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? 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 C14 92.9(12) . . ? C12 Os1 C13 96.4(10) . . ? C14 Os1 C13 95.0(12) . . ? C12 Os1 Cl 165.5(8) . . ? C14 Os1 Cl 100.4(9) . . ? C13 Os1 Cl 88.1(8) . . ? C12 Os1 Os2 110.2(8) . . ? C14 Os1 Os2 138.8(8) . . ? C13 Os1 Os2 114.8(8) . . ? Cl Os1 Os2 55.73(17) . . ? C12 Os1 Os3 89.7(7) . . ? C14 Os1 Os3 86.6(8) . . ? C13 Os1 Os3 173.6(8) . . ? Cl Os1 Os3 85.53(16) . . ? Os2 Os1 Os3 60.88(4) . . ? C12 Os1 Ag 74.3(8) . . ? C14 Os1 Ag 159.2(8) . . ? C13 Os1 Ag 70.8(8) . . ? Cl Os1 Ag 94.36(17) . . ? Os2 Os1 Ag 61.91(3) . . ? Os3 Os1 Ag 109.18(6) . . ? C22 Os2 C23 93.5(12) . . ? C22 Os2 C24 94.8(12) . . ? C23 Os2 C24 95.5(11) . . ? C22 Os2 Cl 165.5(8) . . ? C23 Os2 Cl 87.4(9) . . ? C24 Os2 Cl 99.5(9) . . ? C22 Os2 Os1 111.9(8) . . ? C23 Os2 Os1 116.2(8) . . ? C24 Os2 Os1 135.9(9) . . ? Cl Os2 Os1 55.43(15) . . ? C22 Os2 Os3 94.1(9) . . ? C23 Os2 Os3 172.5(8) . . ? C24 Os2 Os3 83.6(8) . . ? Cl Os2 Os3 85.38(17) . . ? Os1 Os2 Os3 60.90(4) . . ? C22 Os2 Ag 73.3(7) . . ? C23 Os2 Ag 74.5(7) . . ? C24 Os2 Ag 163.6(9) . . ? Cl Os2 Ag 93.12(16) . . ? Os1 Os2 Ag 60.38(3) . . ? Os3 Os2 Ag 108.01(4) . . ? C34 Os3 C31 91.2(11) . . ? C34 Os3 C32 96.0(11) . . ? C31 Os3 C32 172.1(11) . . ? C34 Os3 C33 98.4(12) . . ? C31 Os3 C33 88.5(13) . . ? C32 Os3 C33 93.7(13) . . ? C34 Os3 Os2 160.2(7) . . ? C31 Os3 Os2 87.1(7) . . ? C32 Os3 Os2 85.0(8) . . ? C33 Os3 Os2 101.3(9) . . ? C34 Os3 Os1 102.0(7) . . ? C31 Os3 Os1 88.7(7) . . ? C32 Os3 Os1 86.7(8) . . ? C33 Os3 Os1 159.4(9) . . ? Os2 Os3 Os1 58.22(3) . . ? Os1 Ag Os1 156.75(11) 2_755 . ? Os1 Ag Os2 126.23(3) 2_755 . ? Os1 Ag Os2 57.72(3) . . ? Os1 Ag Os2 57.71(3) 2_755 2_755 ? Os1 Ag Os2 126.23(3) . 2_755 ? Os2 Ag Os2 163.78(11) . 2_755 ? Os1 Cl Os2 68.84(16) . . ? O12 C12 Os1 177(2) . . ? O13 C13 Os1 173(2) . . ? O14 C14 Os1 176(3) . . ? O22 C22 Os2 176(3) . . ? O23 C23 Os2 173(2) . . ? O24 C24 Os2 176(3) . . ? O31 C31 Os3 176(3) . . ? O32 C32 Os3 176(3) . . ? O33 C33 Os3 176(3) . . ? O34 C34 Os3 176(2) . . ? N2 C1 N2 104(3) 2_655 . ? N2 C1 H1A 128.0 2_655 . ? N2 C1 H1A 128.0 . . ? C3 N2 C1 111(2) . . ? C3 N2 C41 127.2(19) . . ? C1 N2 C41 122(2) . . ? C3 C3 N2 107.4(12) 2_655 . ? C3 C3 H3A 126.3 2_655 . ? N2 C3 H3A 126.3 . . ? C46 C41 C42 126(2) . . ? C46 C41 N2 118(3) . . ? C42 C41 N2 115(3) . . ? C41 C42 C43 114(3) . . ? C41 C42 C47 127(3) . . ? C43 C42 C47 118(3) . . ? C44 C43 C42 124(3) . . ? C44 C43 H43A 118.0 . . ? C42 C43 H43A 118.0 . . ? C43 C44 C48 127(3) . . ? C43 C44 C45 118(3) . . ? C48 C44 C45 115(3) . . ? C46 C45 C44 119(3) . . ? C46 C45 H45A 120.5 . . ? C44 C45 H45A 120.5 . . ? C41 C46 C45 118(3) . . ? C41 C46 C49 123(2) . . ? C45 C46 C49 120(3) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Os1 Os2 C22 4.3(12) . . . . ? C14 Os1 Os2 C22 124.5(16) . . . . ? C13 Os1 Os2 C22 -103.1(12) . . . . ? Cl Os1 Os2 C22 -172.1(9) . . . . ? Os3 Os1 Os2 C22 82.2(9) . . . . ? Ag Os1 Os2 C22 -54.2(9) . . . . ? C12 Os1 Os2 C23 110.0(12) . . . . ? C14 Os1 Os2 C23 -129.8(16) . . . . ? C13 Os1 Os2 C23 2.5(12) . . . . ? Cl Os1 Os2 C23 -66.4(9) . . . . ? Os3 Os1 Os2 C23 -172.2(8) . . . . ? Ag Os1 Os2 C23 51.5(8) . . . . ? C12 Os1 Os2 C24 -118.6(15) . . . . ? C14 Os1 Os2 C24 1.5(19) . . . . ? C13 Os1 Os2 C24 133.9(16) . . . . ? Cl Os1 Os2 C24 65.0(13) . . . . ? Os3 Os1 Os2 C24 -40.8(13) . . . . ? Ag Os1 Os2 C24 -177.1(13) . . . . ? C12 Os1 Os2 Cl 176.4(9) . . . . ? C14 Os1 Os2 Cl -63.4(14) . . . . ? C13 Os1 Os2 Cl 68.9(9) . . . . ? Os3 Os1 Os2 Cl -105.8(2) . . . . ? Ag Os1 Os2 Cl 117.9(2) . . . . ? C12 Os1 Os2 Os3 -77.8(8) . . . . ? C14 Os1 Os2 Os3 42.3(13) . . . . ? C13 Os1 Os2 Os3 174.7(8) . . . . ? Cl Os1 Os2 Os3 105.8(2) . . . . ? Ag Os1 Os2 Os3 -136.35(7) . . . . ? C12 Os1 Os2 Ag 58.5(8) . . . . ? C14 Os1 Os2 Ag 178.7(13) . . . . ? C13 Os1 Os2 Ag -49.0(8) . . . . ? Cl Os1 Os2 Ag -117.9(2) . . . . ? Os3 Os1 Os2 Ag 136.35(7) . . . . ? C22 Os2 Os3 C34 -118(2) . . . . ? C23 Os2 Os3 C34 64(6) . . . . ? C24 Os2 Os3 C34 148(2) . . . . ? Cl Os2 Os3 C34 48(2) . . . . ? Os1 Os2 Os3 C34 -5(2) . . . . ? Ag Os2 Os3 C34 -44(2) . . . . ? C22 Os2 Os3 C31 156.9(11) . . . . ? C23 Os2 Os3 C31 -21(5) . . . . ? C24 Os2 Os3 C31 62.5(12) . . . . ? Cl Os2 Os3 C31 -37.6(8) . . . . ? Os1 Os2 Os3 C31 -90.3(8) . . . . ? Ag Os2 Os3 C31 -129.4(8) . . . . ? C22 Os2 Os3 C32 -23.7(11) . . . . ? C23 Os2 Os3 C32 158(5) . . . . ? C24 Os2 Os3 C32 -118.1(12) . . . . ? Cl Os2 Os3 C32 141.8(8) . . . . ? Os1 Os2 Os3 C32 89.2(8) . . . . ? Ag Os2 Os3 C32 50.0(8) . . . . ? C22 Os2 Os3 C33 69.1(13) . . . . ? C23 Os2 Os3 C33 -109(6) . . . . ? C24 Os2 Os3 C33 -25.3(14) . . . . ? Cl Os2 Os3 C33 -125.4(10) . . . . ? Os1 Os2 Os3 C33 -178.1(10) . . . . ? Ag Os2 Os3 C33 142.8(10) . . . . ? C22 Os2 Os3 Os1 -112.8(7) . . . . ? C23 Os2 Os3 Os1 69(5) . . . . ? C24 Os2 Os3 Os1 152.8(9) . . . . ? Cl Os2 Os3 Os1 52.66(15) . . . . ? Ag Os2 Os3 Os1 -39.12(6) . . . . ? C12 Os1 Os3 C34 -68.2(11) . . . . ? C14 Os1 Os3 C34 24.7(12) . . . . ? C13 Os1 Os3 C34 129(7) . . . . ? Cl Os1 Os3 C34 125.5(8) . . . . ? Os2 Os1 Os3 C34 178.4(7) . . . . ? Ag Os1 Os3 C34 -141.5(7) . . . . ? C12 Os1 Os3 C31 -159.2(11) . . . . ? C14 Os1 Os3 C31 -66.3(12) . . . . ? C13 Os1 Os3 C31 38(8) . . . . ? Cl Os1 Os3 C31 34.5(9) . . . . ? Os2 Os1 Os3 C31 87.4(8) . . . . ? Ag Os1 Os3 C31 127.5(8) . . . . ? C12 Os1 Os3 C32 27.2(12) . . . . ? C14 Os1 Os3 C32 120.2(12) . . . . ? C13 Os1 Os3 C32 -135(8) . . . . ? Cl Os1 Os3 C32 -139.1(9) . . . . ? Os2 Os1 Os3 C32 -86.2(8) . . . . ? Ag Os1 Os3 C32 -46.1(8) . . . . ? C12 Os1 Os3 C33 119(3) . . . . ? C14 Os1 Os3 C33 -148(3) . . . . ? C13 Os1 Os3 C33 -44(8) . . . . ? Cl Os1 Os3 C33 -48(3) . . . . ? Os2 Os1 Os3 C33 5(3) . . . . ? Ag Os1 Os3 C33 45(3) . . . . ? C12 Os1 Os3 Os2 113.4(8) . . . . ? C14 Os1 Os3 Os2 -153.6(9) . . . . ? C13 Os1 Os3 Os2 -49(7) . . . . ? Cl Os1 Os3 Os2 -52.92(17) . . . . ? Ag Os1 Os3 Os2 40.14(5) . . . . ? C12 Os1 Ag Os1 128.8(8) . . . 2_755 ? C14 Os1 Ag Os1 75(2) . . . 2_755 ? C13 Os1 Ag Os1 26.1(8) . . . 2_755 ? Cl Os1 Ag Os1 -60.39(16) . . . 2_755 ? Os2 Os1 Ag Os1 -107.48(4) . . . 2_755 ? Os3 Os1 Ag Os1 -147.16(4) . . . 2_755 ? C12 Os1 Ag Os2 -123.7(8) . . . . ? C14 Os1 Ag Os2 -178(2) . . . . ? C13 Os1 Ag Os2 133.5(8) . . . . ? Cl Os1 Ag Os2 47.10(16) . . . . ? Os3 Os1 Ag Os2 -39.68(5) . . . . ? C12 Os1 Ag Os2 37.2(8) . . . 2_755 ? C14 Os1 Ag Os2 -17(2) . . . 2_755 ? C13 Os1 Ag Os2 -65.5(8) . . . 2_755 ? Cl Os1 Ag Os2 -151.98(19) . . . 2_755 ? Os2 Os1 Ag Os2 160.93(13) . . . 2_755 ? Os3 Os1 Ag Os2 121.25(10) . . . 2_755 ? C22 Os2 Ag Os1 -79.6(9) . . . 2_755 ? C23 Os2 Ag Os1 19.0(9) . . . 2_755 ? C24 Os2 Ag Os1 -35(3) . . . 2_755 ? Cl Os2 Ag Os1 105.39(19) . . . 2_755 ? Os1 Os2 Ag Os1 152.18(14) . . . 2_755 ? Os3 Os2 Ag Os1 -168.46(9) . . . 2_755 ? C22 Os2 Ag Os1 128.2(9) . . . . ? C23 Os2 Ag Os1 -133.2(9) . . . . ? C24 Os2 Ag Os1 173(3) . . . . ? Cl Os2 Ag Os1 -46.79(17) . . . . ? Os3 Os2 Ag Os1 39.36(6) . . . . ? C22 Os2 Ag Os2 18.9(9) . . . 2_755 ? C23 Os2 Ag Os2 117.5(9) . . . 2_755 ? C24 Os2 Ag Os2 64(3) . . . 2_755 ? Cl Os2 Ag Os2 -156.11(16) . . . 2_755 ? Os1 Os2 Ag Os2 -109.32(4) . . . 2_755 ? Os3 Os2 Ag Os2 -69.96(4) . . . 2_755 ? C12 Os1 Cl Os2 -14(3) . . . . ? C14 Os1 Cl Os2 143.2(9) . . . . ? C13 Os1 Cl Os2 -122.1(8) . . . . ? Os3 Os1 Cl Os2 57.50(11) . . . . ? Ag Os1 Cl Os2 -51.44(13) . . . . ? C22 Os2 Cl Os1 31(4) . . . . ? C23 Os2 Cl Os1 124.6(7) . . . . ? C24 Os2 Cl Os1 -140.2(8) . . . . ? Os3 Os2 Cl Os1 -57.53(11) . . . . ? Ag Os2 Cl Os1 50.30(12) . . . . ? C14 Os1 C12 O12 43(59) . . . . ? C13 Os1 C12 O12 -53(59) . . . . ? Cl Os1 C12 O12 -160(56) . . . . ? Os2 Os1 C12 O12 -172(59) . . . . ? Os3 Os1 C12 O12 129(59) . . . . ? Ag Os1 C12 O12 -121(59) . . . . ? C12 Os1 C13 O13 138(21) . . . . ? C14 Os1 C13 O13 44(21) . . . . ? Cl Os1 C13 O13 -56(21) . . . . ? Os2 Os1 C13 O13 -106(21) . . . . ? Os3 Os1 C13 O13 -60(26) . . . . ? Ag Os1 C13 O13 -151(21) . . . . ? C12 Os1 C14 O14 55(43) . . . . ? C13 Os1 C14 O14 152(43) . . . . ? Cl Os1 C14 O14 -119(43) . . . . ? Os2 Os1 C14 O14 -71(44) . . . . ? Os3 Os1 C14 O14 -35(43) . . . . ? Ag Os1 C14 O14 106(43) . . . . ? C23 Os2 C22 O22 -173(36) . . . . ? C24 Os2 C22 O22 92(36) . . . . ? Cl Os2 C22 O22 -80(37) . . . . ? Os1 Os2 C22 O22 -53(36) . . . . ? Os3 Os2 C22 O22 8(36) . . . . ? Ag Os2 C22 O22 -100(36) . . . . ? C22 Os2 C23 O23 -86(21) . . . . ? C24 Os2 C23 O23 10(21) . . . . ? Cl Os2 C23 O23 109(21) . . . . ? Os1 Os2 C23 O23 158(21) . . . . ? Os3 Os2 C23 O23 92(23) . . . . ? Ag Os2 C23 O23 -157(21) . . . . ? C22 Os2 C24 O24 40(41) . . . . ? C23 Os2 C24 O24 -53(41) . . . . ? Cl Os2 C24 O24 -142(40) . . . . ? Os1 Os2 C24 O24 169(40) . . . . ? Os3 Os2 C24 O24 134(41) . . . . ? Ag Os2 C24 O24 -2(43) . . . . ? C34 Os3 C31 O31 -88(33) . . . . ? C32 Os3 C31 O31 68(37) . . . . ? C33 Os3 C31 O31 174(33) . . . . ? Os2 Os3 C31 O31 72(33) . . . . ? Os1 Os3 C31 O31 14(33) . . . . ? C34 Os3 C32 O32 3(33) . . . . ? C31 Os3 C32 O32 -153(29) . . . . ? C33 Os3 C32 O32 102(33) . . . . ? Os2 Os3 C32 O32 -157(33) . . . . ? Os1 Os3 C32 O32 -99(33) . . . . ? C34 Os3 C33 O33 94(40) . . . . ? C31 Os3 C33 O33 -175(40) . . . . ? C32 Os3 C33 O33 -3(40) . . . . ? Os2 Os3 C33 O33 -88(40) . . . . ? Os1 Os3 C33 O33 -93(40) . . . . ? C31 Os3 C34 O34 -38(35) . . . . ? C32 Os3 C34 O34 145(35) . . . . ? C33 Os3 C34 O34 50(35) . . . . ? Os2 Os3 C34 O34 -123(34) . . . . ? Os1 Os3 C34 O34 -127(35) . . . . ? N2 C1 N2 C3 -1.7(16) 2_655 . . . ? N2 C1 N2 C41 179(3) 2_655 . . . ? C1 N2 C3 C3 4(4) . . . 2_655 ? C41 N2 C3 C3 -176(3) . . . 2_655 ? C3 N2 C41 C46 96(3) . . . . ? C1 N2 C41 C46 -85(3) . . . . ? C3 N2 C41 C42 -82(3) . . . . ? C1 N2 C41 C42 98(3) . . . . ? C46 C41 C42 C43 4(4) . . . . ? N2 C41 C42 C43 -178(2) . . . . ? C46 C41 C42 C47 -179(3) . . . . ? N2 C41 C42 C47 -2(4) . . . . ? C41 C42 C43 C44 -3(4) . . . . ? C47 C42 C43 C44 -180(3) . . . . ? C42 C43 C44 C48 176(3) . . . . ? C42 C43 C44 C45 2(5) . . . . ? C43 C44 C45 C46 -3(4) . . . . ? C48 C44 C45 C46 -178(3) . . . . ? C42 C41 C46 C45 -5(4) . . . . ? N2 C41 C46 C45 178(2) . . . . ? C42 C41 C46 C49 178(3) . . . . ? N2 C41 C46 C49 1(4) . . . . ? C44 C45 C46 C41 4(4) . . . . ? C44 C45 C46 C49 -179(3) . . . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 2.428 _refine_diff_density_min -2.843 _refine_diff_density_rms 0.400