# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1556 data_global #================================================================= # SUBMISSION DETAILS _publ_contact_author ; Dr. Michael Ward School of Chemistry University of Bristol Cantock's Close BS8 1TS Bristol UK ; _publ_contact_author_phone '0117 9287655' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the two crystal structures in the paper 'Structural, electrochemical and UV/VIS/NIR spectroelectrochemical properties of diastereomerically pure dinuclear ruthenium complexes...' by N. C. Fletcher, et al, submitted to Dalton Transactions for publication. ; #================================================================= data_nick _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H45 Cl4 N12 O18.50 Ru2' _chemical_formula_weight 1477.94 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 29.300(8) _cell_length_b 17.762(8) _cell_length_c 22.139(8) _cell_angle_alpha 90 _cell_angle_beta 97.19(2) _cell_angle_gamma 90 _cell_volume 11430.9(74) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method ? _exptl_crystal_F_000 5960 _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 0.871 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29255 _diffrn_reflns_av_R_equivalents 0.0791 _diffrn_reflns_av_sigmaI/netI 0.0993 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10041 _reflns_number_observed 5647 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 17 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1087P)^2^+17.7352P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10024 _refine_ls_number_parameters 926 _refine_ls_number_restraints 698 _refine_ls_R_factor_all 0.1412 _refine_ls_R_factor_obs 0.0712 _refine_ls_wR_factor_all 0.2130 _refine_ls_wR_factor_obs 0.1729 _refine_ls_goodness_of_fit_all 1.017 _refine_ls_goodness_of_fit_obs 1.138 _refine_ls_restrained_S_all 1.064 _refine_ls_restrained_S_obs 1.196 _refine_ls_shift/esd_max -0.144 _refine_ls_shift/esd_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.07974(2) 0.20044(4) 1.44574(3) 0.0417(2) Uani 1 d U . Ru2 Ru 0.21574(2) 0.38752(4) 1.19138(3) 0.0420(2) Uani 1 d U . N11 N 0.0345(2) 0.2858(4) 1.4566(4) 0.051(2) Uani 1 d U . C12 C 0.0258(3) 0.2969(6) 1.5162(5) 0.062(3) Uani 1 d U . C13 C -0.0057(4) 0.3532(8) 1.5281(6) 0.087(4) Uani 1 d U . H13A H -0.0121(4) 0.3611(8) 1.5686(6) 0.104 Uiso 1 calc R . C14 C -0.0271(5) 0.3966(7) 1.4823(8) 0.097(4) Uani 1 d U . H14A H -0.0475(5) 0.4354(7) 1.4910(8) 0.117 Uiso 1 calc R . C15 C -0.0189(4) 0.3838(7) 1.4231(7) 0.086(4) Uani 1 d U . H15A H -0.0341(4) 0.4128(7) 1.3907(7) 0.103 Uiso 1 calc R . C16 C 0.0116(3) 0.3284(6) 1.4121(6) 0.070(3) Uani 1 d U . H16A H 0.0168(3) 0.3195(6) 1.3712(6) 0.084 Uiso 1 calc R . N21 N 0.0822(2) 0.2038(4) 1.5395(3) 0.047(2) Uani 1 d U . C22 C 0.0518(3) 0.2500(6) 1.5609(4) 0.052(2) Uani 1 d U . C23 C 0.0470(4) 0.2507(7) 1.6241(5) 0.070(3) Uani 1 d U . H23A H 0.0248(4) 0.2823(7) 1.6390(5) 0.084 Uiso 1 calc R . C24 C 0.0741(4) 0.2063(8) 1.6624(5) 0.077(4) Uani 1 d U . H24A H 0.0701(4) 0.2053(8) 1.7044(5) 0.092 Uiso 1 calc R . C25 C 0.1068(4) 0.1634(7) 1.6421(5) 0.071(3) Uani 1 d U . H25A H 0.1272(4) 0.1346(7) 1.6698(5) 0.085 Uiso 1 calc R . C26 C 0.1104(3) 0.1616(6) 1.5790(4) 0.054(3) Uani 1 d U . H26A H 0.1329(3) 0.1305(6) 1.5642(4) 0.065 Uiso 1 calc R . N31 N 0.0307(2) 0.1164(5) 1.4414(3) 0.047(2) Uani 1 d U . C32 C 0.0456(3) 0.0468(6) 1.4342(4) 0.050(2) Uani 1 d U . C33 C 0.0162(4) -0.0134(6) 1.4227(4) 0.067(3) Uani 1 d U . H33A H 0.0279(4) -0.0625(6) 1.4173(4) 0.081 Uiso 1 calc R . C34 C -0.0301(5) -0.0013(8) 1.4193(5) 0.080(4) Uani 1 d U . H34A H -0.0509(5) -0.0421(8) 1.4107(5) 0.096 Uiso 1 calc R . C35 C -0.0469(4) 0.0699(9) 1.4282(5) 0.080(4) Uani 1 d U . H35A H -0.0790(4) 0.0788(9) 1.4263(5) 0.096 Uiso 1 calc R . C36 C -0.0153(3) 0.1288(6) 1.4403(5) 0.063(3) Uani 1 d U . H36A H -0.0261(3) 0.1780(6) 1.4477(5) 0.076 Uiso 1 calc R . N41 N 0.1199(2) 0.1059(4) 1.4451(3) 0.048(2) Uani 1 d U . C42 C 0.0958(3) 0.0389(6) 1.4401(4) 0.050(2) Uani 1 d U . C43 C 0.1192(4) -0.0285(7) 1.4404(4) 0.070(3) Uani 1 d U . H43A H 0.1024(4) -0.0744(7) 1.4366(4) 0.084 Uiso 1 calc R . C44 C 0.1658(5) -0.0302(8) 1.4462(5) 0.082(4) Uani 1 d U . H44A H 0.1815(5) -0.0770(8) 1.4470(5) 0.098 Uiso 1 calc R . C45 C 0.1904(4) 0.0366(9) 1.4509(5) 0.077(4) Uani 1 d U . H45A H 0.2231(4) 0.0366(9) 1.4540(5) 0.093 Uiso 1 calc R . C46 C 0.1660(3) 0.1034(6) 1.4509(4) 0.056(3) Uani 1 d U . H46A H 0.1827(3) 0.1494(6) 1.4551(4) 0.067 Uiso 1 calc R . N51 N 0.2671(3) 0.3070(5) 1.1997(3) 0.054(2) Uani 1 d U . C52 C 0.3105(3) 0.3332(8) 1.2012(4) 0.065(3) Uani 1 d U . C53 C 0.3475(4) 0.2857(10) 1.2005(5) 0.090(4) Uani 1 d U . H53A H 0.3777(4) 0.3056(10) 1.2017(5) 0.108 Uiso 1 calc R . C54 C 0.3405(5) 0.2083(12) 1.1981(6) 0.111(6) Uani 1 d U . H54A H 0.3654(5) 0.1746(12) 1.1959(6) 0.133 Uiso 1 calc R . C55 C 0.2964(5) 0.1819(8) 1.1990(5) 0.083(4) Uani 1 d U . H55A H 0.2907(5) 0.1293(8) 1.1992(5) 0.100 Uiso 1 calc R . C56 C 0.2607(4) 0.2319(7) 1.1995(4) 0.063(3) Uani 1 d U . H56A H 0.2304(4) 0.2128(7) 1.1997(4) 0.075 Uiso 1 calc R . N61 N 0.2735(3) 0.4545(5) 1.1943(3) 0.057(2) Uani 1 d U . C62 C 0.3147(4) 0.4164(9) 1.2025(4) 0.076(4) Uani 1 d U . C63 C 0.3568(4) 0.4548(12) 1.2114(5) 0.108(6) Uani 1 d U . H63A H 0.3851(4) 0.4283(12) 1.2175(5) 0.130 Uiso 1 calc R . C64 C 0.3556(6) 0.5348(14) 1.2108(6) 0.129(8) Uani 1 d U . H64A H 0.3834(6) 0.5630(14) 1.2163(6) 0.155 Uiso 1 calc R . C65 C 0.3153(6) 0.5697(10) 1.2026(6) 0.106(5) Uani 1 d U . H65A H 0.3144(6) 0.6232(10) 1.2023(6) 0.127 Uiso 1 calc R . C66 C 0.2746(4) 0.5299(7) 1.1947(4) 0.069(3) Uani 1 d U . H66A H 0.2464(4) 0.5568(7) 1.1893(4) 0.082 Uiso 1 calc R . N71 N 0.1670(2) 0.4700(4) 1.1705(3) 0.049(2) Uani 1 d U . C72 C 0.1529(3) 0.4809(5) 1.1099(4) 0.050(2) Uani 1 d U . C73 C 0.1168(4) 0.5290(6) 1.0905(5) 0.065(3) Uani 1 d U . H73A H 0.1087(4) 0.5388(6) 1.0483(5) 0.078 Uiso 1 calc R . C74 C 0.0927(4) 0.5628(6) 1.1335(6) 0.079(3) Uani 1 d U . H74A H 0.0667(4) 0.5934(6) 1.1206(6) 0.095 Uiso 1 calc R . C75 C 0.1062(4) 0.5521(6) 1.1933(6) 0.077(3) Uani 1 d U . H75A H 0.0906(4) 0.5765(6) 1.2230(6) 0.092 Uiso 1 calc R . C76 C 0.1433(4) 0.5048(6) 1.2109(5) 0.067(3) Uani 1 d U . H76A H 0.1523(4) 0.4966(6) 1.2531(5) 0.080 Uiso 1 calc R . N81 N 0.2101(2) 0.3889(4) 1.0971(3) 0.043(2) Uani 1 d U . C82 C 0.1790(3) 0.4389(5) 1.0688(4) 0.051(2) Uani 1 d U . C83 C 0.1728(4) 0.4472(6) 1.0063(4) 0.066(3) Uani 1 d U . H83A H 0.1508(4) 0.4821(6) 0.9877(4) 0.080 Uiso 1 calc R . C84 C 0.1989(4) 0.4041(7) 0.9704(5) 0.081(4) Uani 1 d U . H84A H 0.1954(4) 0.4097(7) 0.9274(5) 0.098 Uiso 1 calc R . C85 C 0.2301(4) 0.3529(7) 0.9993(5) 0.071(3) Uani 1 d U . H85A H 0.2480(4) 0.3221(7) 0.9762(5) 0.085 Uiso 1 calc R . C86 C 0.2350(3) 0.3470(6) 1.0620(4) 0.057(3) Uani 1 d U . H86A H 0.2567(3) 0.3120(6) 1.0812(4) 0.069 Uiso 1 calc R . N101 N 0.2144(2) 0.3880(4) 1.2832(3) 0.041(2) Uani 1 d U . C102 C 0.2431(5) 0.4206(8) 1.3270(6) 0.044(4) Uani 0.602(6) d PU 1 H10A H 0.2681(5) 0.4485(8) 1.3150(6) 0.052 Uiso 0.602(6) calc PR 1 C103 C 0.2391(4) 0.4167(8) 1.3900(6) 0.044(4) Uani 0.602(6) d PU 1 H10B H 0.2612(4) 0.4418(8) 1.4180(6) 0.052 Uiso 0.602(6) calc PR 1 C104 C 0.2043(3) 0.3781(5) 1.4114(4) 0.044(2) Uani 1 d U . C105 C 0.1756(3) 0.3392(5) 1.3666(3) 0.037(2) Uani 1 d U . C106 C 0.1820(3) 0.3457(5) 1.3035(4) 0.039(2) Uani 1 d U . N111 N 0.1620(2) 0.3165(4) 1.1993(3) 0.041(2) Uani 1 d U . C112 C 0.1331(4) 0.2811(8) 1.1563(6) 0.038(3) Uani 0.602(6) d PU 1 H11A H 0.1391(4) 0.2866(8) 1.1153(6) 0.046 Uiso 0.602(6) calc PR 1 C113 C 0.0954(4) 0.2374(8) 1.1663(6) 0.041(4) Uani 0.602(6) d PU 1 H11B H 0.0758(4) 0.2173(8) 1.1328(6) 0.049 Uiso 0.602(6) calc PR 1 C114 C 0.0867(3) 0.2234(5) 1.2243(4) 0.043(2) Uani 1 d U . C115 C 0.1153(3) 0.2608(5) 1.2706(4) 0.038(2) Uani 1 d U . C116 C 0.1522(3) 0.3057(5) 1.2563(4) 0.039(2) Uani 1 d U . N121 N 0.0785(2) 0.2072(4) 1.3548(3) 0.043(2) Uani 1 d U . C122 C 0.1093(3) 0.2509(5) 1.3344(3) 0.039(2) Uani 1 d U . C123 C 0.1394(3) 0.2897(5) 1.3809(4) 0.042(2) Uani 1 d U . N124 N 0.1307(2) 0.2750(4) 1.4377(3) 0.048(2) Uani 1 d U . C202 C 0.1561(8) 0.3171(14) 1.4798(10) 0.054(7) Uani 0.398(6) d PU 2 H20A H 0.1499(8) 0.3124(14) 1.5208(10) 0.064 Uiso 0.398(6) calc PR 2 C203 C 0.1922(7) 0.3694(11) 1.4679(9) 0.044(6) Uani 0.398(6) d PU 2 H20B H 0.2077(7) 0.3979(11) 1.5006(9) 0.053 Uiso 0.398(6) calc PR 2 C212 C 0.0537(7) 0.1702(14) 1.3087(11) 0.057(7) Uani 0.398(6) d PU 2 H21A H 0.0313(7) 0.1360(14) 1.3198(11) 0.069 Uiso 0.398(6) calc PR 2 C213 C 0.0575(7) 0.1766(13) 1.2425(9) 0.046(6) Uani 0.398(6) d PU 2 H21B H 0.0386(7) 0.1466(13) 1.2139(9) 0.055 Uiso 0.398(6) calc PR 2 Cl1 Cl 0.08210(11) 0.4875(2) 0.36446(14) 0.0782(9) Uani 1 d U . Cl2 Cl 0.2099(2) 0.3061(3) 0.5917(2) 0.0651(15) Uani 0.602(6) d PDU 1 Cl2' Cl 0.2299(3) 0.2895(4) 0.6301(4) 0.066(2) Uani 0.398(6) d PDU 2 Cl3 Cl 0.3229(2) -0.5899(4) 0.8853(3) 0.077(2) Uani 0.602(6) d PDU 1 Cl3' Cl 0.3086(3) -0.5331(6) 0.8738(3) 0.073(3) Uani 0.398(6) d PDU 2 Cl4 Cl 0.0000 -0.0514(5) 0.7500 0.068(2) Uani 0.50 d SPDU . Cl4' Cl 0.0000 0.0487(17) 0.7500 0.207(11) Uani 0.50 d SPDU . Cl5 Cl 0.1035(2) 0.2422(3) 0.9498(3) 0.078(2) Uani 0.50 d PU . O11 O 0.0781(3) 0.4263(5) 0.3216(3) 0.088(2) Uani 1 d U . O12 O 0.1201(3) 0.5324(5) 0.3542(4) 0.103(3) Uani 1 d U . O13 O 0.0881(3) 0.4599(5) 0.4253(3) 0.096(3) Uani 1 d U . O14 O 0.0397(3) 0.5295(6) 0.3550(4) 0.115(3) Uani 1 d U . O21 O 0.2030(8) 0.3720(8) 0.5592(7) 0.186(11) Uani 0.602(6) d PDU 1 O21' O 0.2120(8) 0.2299(13) 0.6191(19) 0.255(25) Uani 0.398(6) d PDU 2 O22 O 0.1925(5) 0.3194(9) 0.6405(6) 0.215(8) Uani 1 d DU . O23 O 0.1939(6) 0.2485(10) 0.5563(7) 0.137(8) Uani 0.602(6) d PDU 1 O23' O 0.2492(10) 0.2812(20) 0.6761(10) 0.336(33) Uani 0.398(6) d PDU 2 O24 O 0.2560(4) 0.2943(8) 0.5992(9) 0.276(12) Uani 1 d DU . O31 O 0.2752(4) -0.5783(11) 0.8893(11) 0.337(14) Uani 1 d DU . O32 O 0.3374(7) -0.6363(9) 0.9344(7) 0.157(9) Uani 0.602(6) d PDU 1 O32' O 0.2890(11) -0.4916(18) 0.8211(13) 0.337(35) Uani 0.398(6) d PDU 2 O33 O 0.3315(5) -0.6068(9) 0.8348(6) 0.236(9) Uani 1 d DU . O34 O 0.3455(4) -0.5132(6) 0.8982(7) 0.172(6) Uani 1 d DU . O41 O -0.0314(6) -0.0016(8) 0.7582(8) 0.212(8) Uani 1 d DU . O42 O 0.0173(8) -0.0909(12) 0.7995(6) 0.183(11) Uani 0.602(6) d PDU 1 O42' O 0.0310(11) 0.0806(31) 0.7926(16) 0.351(47) Uani 0.398(6) d PDU 2 O51 O 0.0685(6) 0.1986(10) 0.9277(13) 0.145(10) Uani 0.50 d PU . O52 O 0.0987(6) 0.3090(8) 0.9191(9) 0.098(6) Uani 0.50 d PU . O53 O 0.0984(7) 0.2521(14) 1.0128(7) 0.128(8) Uani 0.50 d PU . O54 O 0.1467(5) 0.2088(8) 0.9445(7) 0.080(5) Uani 0.50 d PU . O1 O 0.1177(13) 0.2471(25) 1.0682(23) 0.327(28) Uani 0.50 d PU . O2 O -0.0373(4) 0.3280(8) 0.7075(7) 0.183(6) Uani 1 d U . O3 O 0.0000 0.3579(8) 0.2500 0.118(5) Uani 1 d SU . O4 O 0.0473(8) 0.1779(17) 0.8240(19) 0.216(17) Uani 0.50 d PU . 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 Ru1 0.0370(4) 0.0510(5) 0.0372(4) -0.0007(3) 0.0048(3) -0.0050(4) Ru2 0.0444(4) 0.0508(5) 0.0306(4) -0.0027(3) 0.0035(3) -0.0089(4) N11 0.044(4) 0.054(5) 0.057(5) 0.002(4) 0.010(4) -0.004(4) C12 0.052(6) 0.068(7) 0.069(7) -0.025(6) 0.021(5) -0.005(6) C13 0.070(8) 0.106(10) 0.088(9) -0.026(8) 0.024(7) 0.007(8) C14 0.084(9) 0.078(10) 0.130(13) -0.016(9) 0.011(9) 0.031(8) C15 0.065(7) 0.075(9) 0.116(11) -0.002(8) 0.005(7) 0.020(7) C16 0.050(6) 0.072(8) 0.088(9) 0.003(6) 0.011(6) 0.001(6) N21 0.033(4) 0.062(5) 0.046(5) -0.007(4) 0.006(3) -0.015(4) C22 0.041(5) 0.073(7) 0.044(6) -0.010(5) 0.006(4) -0.008(5) C23 0.068(7) 0.089(9) 0.058(7) -0.022(6) 0.025(6) -0.015(6) C24 0.078(8) 0.121(11) 0.034(6) -0.005(6) 0.019(6) -0.015(8) C25 0.068(7) 0.092(9) 0.052(7) 0.008(6) 0.005(6) -0.028(7) C26 0.044(5) 0.072(7) 0.047(6) 0.005(5) 0.005(4) -0.020(5) N31 0.045(4) 0.061(5) 0.035(4) 0.005(4) 0.004(3) -0.011(4) C32 0.063(6) 0.056(7) 0.029(5) 0.009(4) 0.003(4) -0.006(5) C33 0.088(9) 0.063(7) 0.053(7) 0.005(5) 0.020(6) -0.018(7) C34 0.100(10) 0.080(9) 0.060(7) -0.001(6) 0.013(7) -0.042(8) C35 0.056(7) 0.119(11) 0.062(7) 0.014(7) 0.003(5) -0.029(8) C36 0.052(6) 0.070(8) 0.066(7) 0.010(5) 0.004(5) -0.007(6) N41 0.045(4) 0.061(5) 0.037(4) 0.001(4) 0.006(3) 0.004(4) C42 0.065(6) 0.061(7) 0.024(5) -0.002(4) 0.009(4) 0.009(6) C43 0.092(9) 0.074(8) 0.048(6) 0.000(5) 0.021(6) 0.021(7) C44 0.095(10) 0.096(10) 0.057(7) 0.016(7) 0.018(7) 0.033(9) C45 0.060(7) 0.118(11) 0.054(7) 0.000(7) 0.009(5) 0.027(8) C46 0.047(6) 0.080(8) 0.041(5) 0.001(5) 0.009(4) 0.007(6) N51 0.051(5) 0.078(7) 0.033(4) 0.000(4) 0.008(3) 0.000(5) C52 0.049(6) 0.119(11) 0.027(5) 0.008(5) -0.001(4) 0.003(7) C53 0.046(7) 0.161(14) 0.064(8) 0.009(9) 0.007(5) 0.020(9) C54 0.077(10) 0.181(18) 0.076(9) 0.017(11) 0.017(7) 0.054(12) C55 0.089(9) 0.105(10) 0.056(7) 0.008(6) 0.011(6) 0.043(8) C56 0.065(7) 0.070(8) 0.051(6) -0.003(5) 0.004(5) 0.012(6) N61 0.057(5) 0.080(7) 0.038(5) -0.005(4) 0.015(4) -0.029(5) C62 0.063(8) 0.138(12) 0.029(5) 0.005(6) 0.008(5) -0.031(8) C63 0.057(8) 0.219(19) 0.047(7) 0.007(9) 0.005(6) -0.054(11) C64 0.116(14) 0.208(22) 0.066(10) -0.016(11) 0.021(10) -0.100(16) C65 0.133(13) 0.131(13) 0.058(8) -0.020(8) 0.033(9) -0.078(12) C66 0.091(8) 0.080(8) 0.039(6) -0.009(5) 0.023(5) -0.041(7) N71 0.052(5) 0.041(4) 0.053(5) -0.005(4) 0.000(4) -0.007(4) C72 0.052(6) 0.052(6) 0.044(6) -0.007(5) -0.002(4) -0.009(5) C73 0.086(8) 0.042(6) 0.062(7) 0.005(5) -0.009(6) -0.009(6) C74 0.088(9) 0.057(8) 0.089(10) 0.000(7) -0.003(7) 0.012(6) C75 0.081(8) 0.058(7) 0.090(10) -0.018(6) 0.007(7) 0.017(6) C76 0.090(8) 0.062(7) 0.049(6) -0.006(5) 0.008(6) 0.007(6) N81 0.047(4) 0.046(5) 0.034(4) 0.000(3) 0.000(3) -0.006(4) C82 0.055(6) 0.056(6) 0.037(5) 0.000(4) -0.009(4) -0.011(5) C83 0.069(7) 0.084(8) 0.042(6) 0.014(5) -0.008(5) -0.006(6) C84 0.092(9) 0.102(10) 0.050(7) 0.011(7) 0.006(6) -0.007(8) C85 0.088(8) 0.083(8) 0.046(6) -0.013(6) 0.024(6) -0.014(7) C86 0.073(7) 0.061(7) 0.039(6) 0.005(5) 0.013(5) -0.005(6) N101 0.038(4) 0.050(5) 0.036(4) -0.010(3) 0.003(3) -0.010(4) C102 0.043(8) 0.052(9) 0.037(8) -0.008(7) 0.011(7) -0.014(7) C103 0.032(7) 0.049(9) 0.047(9) -0.004(7) -0.008(6) -0.012(7) C104 0.043(5) 0.053(6) 0.034(5) 0.002(4) -0.004(4) -0.010(4) C105 0.042(5) 0.039(5) 0.028(4) -0.004(4) -0.003(4) 0.000(4) C106 0.035(5) 0.046(5) 0.038(5) 0.003(4) 0.004(4) -0.001(4) N111 0.044(4) 0.044(5) 0.035(4) -0.003(3) 0.002(3) 0.007(3) C112 0.039(8) 0.053(9) 0.024(7) -0.007(6) 0.010(6) 0.000(7) C113 0.036(8) 0.053(9) 0.029(8) -0.015(6) -0.008(6) -0.010(7) C114 0.044(5) 0.053(6) 0.032(5) -0.001(4) 0.001(4) -0.017(5) C115 0.030(4) 0.040(5) 0.042(5) -0.001(4) -0.005(4) -0.001(4) C116 0.040(5) 0.044(5) 0.032(5) -0.007(4) 0.001(4) 0.006(4) N121 0.035(4) 0.043(4) 0.050(5) -0.002(4) -0.002(3) -0.006(4) C122 0.039(5) 0.049(6) 0.027(4) -0.007(4) -0.006(4) 0.001(4) C123 0.033(4) 0.046(5) 0.046(5) -0.005(4) 0.004(4) -0.002(4) N124 0.040(4) 0.070(5) 0.033(4) -0.004(4) 0.006(3) -0.003(4) C202 0.052(14) 0.074(18) 0.036(13) 0.001(12) 0.008(11) -0.018(13) C203 0.053(14) 0.037(13) 0.035(12) -0.011(9) -0.025(10) -0.015(11) C212 0.038(13) 0.068(17) 0.068(17) 0.030(14) 0.013(12) -0.021(12) C213 0.050(13) 0.055(15) 0.029(11) -0.023(10) -0.013(10) -0.015(12) Cl1 0.070(2) 0.099(2) 0.065(2) -0.009(2) 0.0050(14) 0.002(2) Cl2 0.054(3) 0.091(4) 0.049(3) 0.003(3) 0.003(2) -0.003(3) Cl2' 0.081(6) 0.059(5) 0.060(5) 0.002(4) 0.018(4) 0.017(4) Cl3 0.066(3) 0.080(4) 0.088(4) -0.006(3) 0.017(3) 0.019(3) Cl3' 0.066(5) 0.104(7) 0.052(4) 0.013(4) 0.014(4) 0.023(5) Cl4 0.055(4) 0.090(6) 0.053(5) 0.000 -0.014(4) 0.000 Cl4' 0.210(25) 0.318(33) 0.091(12) 0.000 0.016(15) 0.000 Cl5 0.075(4) 0.049(3) 0.120(5) -0.001(3) 0.052(4) -0.004(3) O11 0.080(5) 0.108(6) 0.072(5) -0.018(5) -0.001(4) 0.019(5) O12 0.115(7) 0.109(7) 0.083(6) -0.002(5) 0.006(5) -0.036(6) O13 0.101(6) 0.133(8) 0.052(5) 0.000(5) 0.003(4) -0.036(6) O14 0.109(7) 0.119(8) 0.120(8) -0.006(6) 0.026(6) 0.038(6) O21 0.362(32) 0.125(15) 0.088(13) 0.050(11) 0.097(16) 0.126(18) O21' 0.095(22) 0.086(23) 0.557(75) -0.080(36) -0.060(35) 0.048(19) O22 0.185(14) 0.325(22) 0.127(12) -0.066(12) -0.010(10) 0.090(15) O23 0.131(16) 0.196(20) 0.078(12) -0.030(12) -0.017(10) -0.060(15) O23' 0.647(80) 0.290(47) 0.103(25) 0.111(28) 0.170(38) 0.354(52) O24 0.131(12) 0.159(13) 0.577(36) 0.099(17) 0.196(18) 0.044(10) O31 0.117(12) 0.356(27) 0.562(39) 0.076(27) 0.131(18) -0.047(16) O32 0.260(26) 0.132(16) 0.078(12) 0.017(11) 0.014(13) -0.031(17) O32' 0.417(71) 0.360(64) 0.213(45) 0.063(41) -0.036(43) 0.286(59) O33 0.267(20) 0.312(23) 0.128(13) -0.018(13) 0.022(12) -0.075(17) O34 0.105(9) 0.116(10) 0.287(18) -0.011(10) -0.013(10) -0.005(8) O41 0.148(13) 0.188(15) 0.271(22) 0.040(14) -0.092(14) 0.064(12) O42 0.247(23) 0.236(23) 0.057(10) -0.002(12) -0.020(12) 0.175(20) O42' 0.090(25) 0.847(149) 0.104(29) 0.047(54) -0.037(21) -0.047(53) O51 0.061(11) 0.064(12) 0.302(33) -0.047(15) -0.011(14) 0.029(10) O52 0.103(13) 0.046(10) 0.161(17) 0.028(10) 0.077(12) 0.017(9) O53 0.113(15) 0.241(25) 0.028(9) 0.031(12) -0.001(9) 0.036(16) O54 0.094(11) 0.046(9) 0.108(13) 0.010(8) 0.045(10) 0.004(8) O1 0.204(35) 0.355(53) 0.392(61) 0.177(46) -0.082(35) -0.188(37) O2 0.152(11) 0.184(12) 0.231(15) 0.017(11) 0.097(10) 0.043(9) O3 0.117(11) 0.119(11) 0.106(11) 0.000 -0.027(8) 0.000 O4 0.095(17) 0.194(26) 0.390(48) 0.099(27) 0.153(25) 0.047(17) _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 Ru1 N121 2.013(7) . ? Ru1 N124 2.019(7) . ? Ru1 N11 2.047(8) . ? Ru1 N41 2.051(7) . ? Ru1 N31 2.065(7) . ? Ru1 N21 2.068(7) . ? Ru2 N101 2.038(7) . ? Ru2 N111 2.043(7) . ? Ru2 N71 2.058(8) . ? Ru2 N61 2.062(8) . ? Ru2 N51 2.067(8) . ? Ru2 N81 2.073(7) . ? N11 C16 1.354(13) . ? N11 C12 1.389(12) . ? C12 C13 1.406(15) . ? C12 C22 1.437(14) . ? C13 C14 1.36(2) . ? C14 C15 1.38(2) . ? C15 C16 1.371(15) . ? N21 C22 1.341(11) . ? N21 C26 1.353(11) . ? C22 C23 1.423(13) . ? C23 C24 1.34(2) . ? C24 C25 1.35(2) . ? C25 C26 1.415(13) . ? N31 C32 1.327(11) . ? N31 C36 1.364(12) . ? C32 C33 1.376(13) . ? C32 C42 1.469(13) . ? C33 C34 1.37(2) . ? C34 C35 1.38(2) . ? C35 C36 1.398(15) . ? N41 C46 1.342(11) . ? N41 C42 1.380(12) . ? C42 C43 1.379(13) . ? C43 C44 1.36(2) . ? C44 C45 1.39(2) . ? C45 C46 1.385(14) . ? N51 C56 1.347(12) . ? N51 C52 1.351(12) . ? C52 C53 1.38(2) . ? C52 C62 1.48(2) . ? C53 C54 1.39(2) . ? C54 C55 1.38(2) . ? C55 C56 1.373(14) . ? N61 C66 1.339(13) . ? N61 C62 1.376(14) . ? C62 C63 1.40(2) . ? C63 C64 1.42(2) . ? C64 C65 1.33(2) . ? C65 C66 1.38(2) . ? N71 C76 1.349(12) . ? N71 C72 1.366(11) . ? C72 C73 1.386(13) . ? C72 C82 1.465(13) . ? C73 C74 1.391(15) . ? C74 C75 1.348(15) . ? C75 C76 1.392(14) . ? N81 C86 1.355(11) . ? N81 C82 1.367(11) . ? C82 C83 1.380(12) . ? C83 C84 1.40(2) . ? C84 C85 1.39(2) . ? C85 C86 1.380(13) . ? N101 C106 1.332(10) . ? N101 C102 1.333(14) . ? C102 C103 1.41(2) . ? C103 C104 1.36(2) . ? C104 C203 1.35(2) . ? C104 C105 1.399(11) . ? C105 C106 1.437(11) . ? C105 C123 1.443(11) . ? C106 C116 1.459(11) . ? N111 C116 1.341(10) . ? N111 C112 1.348(14) . ? C112 C113 1.39(2) . ? C113 C114 1.363(15) . ? C114 C213 1.29(2) . ? C114 C115 1.406(11) . ? C115 C116 1.412(11) . ? C115 C122 1.454(11) . ? N121 C122 1.312(10) . ? N121 C212 1.35(3) . ? C122 C123 1.445(11) . ? C123 N124 1.340(10) . ? N124 C202 1.34(2) . ? C202 C203 1.46(3) . ? C212 C213 1.49(3) . ? Cl1 O12 1.411(9) . ? Cl1 O13 1.422(8) . ? Cl1 O11 1.438(8) . ? Cl1 O14 1.442(9) . ? Cl2 O22 1.272(12) . ? Cl2 O23 1.337(13) . ? Cl2 O24 1.356(12) . ? Cl2 O21 1.375(13) . ? Cl2' O24 1.093(12) . ? Cl2' O23' 1.11(2) . ? Cl2' O21' 1.19(2) . ? Cl2' O22 1.262(12) . ? Cl3 O33 1.213(12) . ? Cl3 O32 1.388(14) . ? Cl3 O31 1.424(13) . ? Cl3 O34 1.526(11) . ? Cl3' O34 1.200(11) . ? Cl3' O31 1.343(14) . ? Cl3' O32' 1.44(2) . ? Cl3' O33 1.746(15) . ? Cl4 O41 1.305(15) 2_556 ? Cl4 O41 1.305(15) . ? Cl4 O42 1.345(14) 2_556 ? Cl4 O42 1.345(14) . ? Cl4 Cl4' 1.78(3) . ? Cl4' O41 1.31(2) 2_556 ? Cl4' O41 1.31(2) . ? Cl4' O42' 1.35(2) . ? Cl4' O42' 1.35(2) 2_556 ? Cl5 O51 1.33(2) . ? Cl5 O52 1.37(2) . ? Cl5 O54 1.42(2) . ? Cl5 O53 1.43(2) . ? O21' O22 1.77(2) . ? O23' O24 1.76(2) . ? O53 O1 1.29(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N121 Ru1 N124 78.1(3) . . ? N121 Ru1 N11 98.2(3) . . ? N124 Ru1 N11 91.2(3) . . ? N121 Ru1 N41 88.8(3) . . ? N124 Ru1 N41 96.0(3) . . ? N11 Ru1 N41 170.8(3) . . ? N121 Ru1 N31 94.1(3) . . ? N124 Ru1 N31 170.8(3) . . ? N11 Ru1 N31 94.8(3) . . ? N41 Ru1 N31 78.7(3) . . ? N121 Ru1 N21 174.8(3) . . ? N124 Ru1 N21 97.8(3) . . ? N11 Ru1 N21 78.6(3) . . ? N41 Ru1 N21 94.8(3) . . ? N31 Ru1 N21 90.2(3) . . ? N101 Ru2 N111 78.8(3) . . ? N101 Ru2 N71 97.0(3) . . ? N111 Ru2 N71 86.4(3) . . ? N101 Ru2 N61 94.9(3) . . ? N111 Ru2 N61 172.7(3) . . ? N71 Ru2 N61 98.1(3) . . ? N101 Ru2 N51 91.1(3) . . ? N111 Ru2 N51 97.2(3) . . ? N71 Ru2 N51 171.7(3) . . ? N61 Ru2 N51 79.2(4) . . ? N101 Ru2 N81 174.3(3) . . ? N111 Ru2 N81 97.4(3) . . ? N71 Ru2 N81 78.4(3) . . ? N61 Ru2 N81 89.2(3) . . ? N51 Ru2 N81 93.6(3) . . ? C16 N11 C12 118.5(9) . . ? C16 N11 Ru1 126.7(7) . . ? C12 N11 Ru1 114.6(7) . . ? N11 C12 C13 118.8(11) . . ? N11 C12 C22 115.2(8) . . ? C13 C12 C22 125.9(10) . . ? C14 C13 C12 120.9(12) . . ? C13 C14 C15 119.7(12) . . ? C16 C15 C14 118.8(12) . . ? N11 C16 C15 123.1(12) . . ? C22 N21 C26 119.3(8) . . ? C22 N21 Ru1 115.6(6) . . ? C26 N21 Ru1 125.1(6) . . ? N21 C22 C23 120.2(10) . . ? N21 C22 C12 115.5(8) . . ? C23 C22 C12 124.3(10) . . ? C24 C23 C22 119.6(10) . . ? C23 C24 C25 120.7(10) . . ? C24 C25 C26 119.2(11) . . ? N21 C26 C25 120.8(10) . . ? C32 N31 C36 119.1(9) . . ? C32 N31 Ru1 116.2(6) . . ? C36 N31 Ru1 124.4(7) . . ? N31 C32 C33 122.6(10) . . ? N31 C32 C42 114.7(9) . . ? C33 C32 C42 122.6(10) . . ? C34 C33 C32 118.8(11) . . ? C33 C34 C35 120.3(11) . . ? C34 C35 C36 118.4(11) . . ? N31 C36 C35 120.7(11) . . ? C46 N41 C42 118.5(8) . . ? C46 N41 Ru1 126.8(7) . . ? C42 N41 Ru1 114.7(6) . . ? C43 C42 N41 120.0(9) . . ? C43 C42 C32 125.1(10) . . ? N41 C42 C32 114.9(8) . . ? C44 C43 C42 120.8(12) . . ? C43 C44 C45 119.9(12) . . ? C44 C45 C46 117.9(11) . . ? N41 C46 C45 122.9(10) . . ? C56 N51 C52 118.1(10) . . ? C56 N51 Ru2 125.9(7) . . ? C52 N51 Ru2 115.8(8) . . ? N51 C52 C53 122.0(13) . . ? N51 C52 C62 114.8(10) . . ? C53 C52 C62 123.2(12) . . ? C52 C53 C54 119.6(13) . . ? C55 C54 C53 118.2(14) . . ? C56 C55 C54 119.8(14) . . ? N51 C56 C55 122.3(11) . . ? C66 N61 C62 118.0(10) . . ? C66 N61 Ru2 126.7(8) . . ? C62 N61 Ru2 115.0(8) . . ? N61 C62 C63 121.4(14) . . ? N61 C62 C52 114.7(9) . . ? C63 C62 C52 123.9(14) . . ? C62 C63 C64 117.7(16) . . ? C65 C64 C63 119.2(16) . . ? C64 C65 C66 121.2(18) . . ? N61 C66 C65 122.4(14) . . ? C76 N71 C72 118.0(8) . . ? C76 N71 Ru2 125.3(7) . . ? C72 N71 Ru2 115.9(6) . . ? N71 C72 C73 121.2(9) . . ? N71 C72 C82 114.9(8) . . ? C73 C72 C82 123.9(9) . . ? C72 C73 C74 119.1(10) . . ? C75 C74 C73 120.0(11) . . ? C74 C75 C76 118.9(11) . . ? N71 C76 C75 122.7(10) . . ? C86 N81 C82 118.0(8) . . ? C86 N81 Ru2 126.2(6) . . ? C82 N81 Ru2 115.7(6) . . ? N81 C82 C83 121.7(9) . . ? N81 C82 C72 114.5(8) . . ? C83 C82 C72 123.8(9) . . ? C82 C83 C84 119.9(10) . . ? C85 C84 C83 118.1(11) . . ? C86 C85 C84 119.5(11) . . ? N81 C86 C85 122.7(10) . . ? C106 N101 C102 114.2(9) . . ? C106 N101 Ru2 116.0(5) . . ? C102 N101 Ru2 129.7(7) . . ? N101 C102 C103 125.0(12) . . ? C104 C103 C102 121.6(12) . . ? C203 C104 C105 113.3(11) . . ? C103 C104 C105 114.3(9) . . ? C104 C105 C106 120.6(8) . . ? C104 C105 C123 122.5(7) . . ? C106 C105 C123 116.8(7) . . ? N101 C106 C105 123.9(7) . . ? N101 C106 C116 114.9(7) . . ? C105 C106 C116 121.2(7) . . ? C116 N111 C112 114.2(8) . . ? C116 N111 Ru2 115.3(5) . . ? C112 N111 Ru2 130.5(7) . . ? N111 C112 C113 126.1(11) . . ? C114 C113 C112 119.8(11) . . ? C213 C114 C115 115.6(11) . . ? C113 C114 C115 115.9(9) . . ? C114 C115 C116 120.3(7) . . ? C114 C115 C122 121.2(7) . . ? C116 C115 C122 118.4(7) . . ? N111 C116 C115 123.5(7) . . ? N111 C116 C106 115.1(7) . . ? C115 C116 C106 121.4(7) . . ? C122 N121 C212 110.9(11) . . ? C122 N121 Ru1 117.0(5) . . ? C212 N121 Ru1 131.9(10) . . ? N121 C122 C123 114.9(7) . . ? N121 C122 C115 125.3(7) . . ? C123 C122 C115 119.8(8) . . ? N124 C123 C105 123.9(7) . . ? N124 C123 C122 113.9(7) . . ? C105 C123 C122 122.3(8) . . ? C123 N124 C202 112.8(12) . . ? C123 N124 Ru1 116.1(6) . . ? C202 N124 Ru1 130.9(11) . . ? N124 C202 C203 125.5(18) . . ? C104 C203 C202 121.4(16) . . ? N121 C212 C213 127.5(17) . . ? C114 C213 C212 119.3(16) . . ? O12 Cl1 O13 109.9(5) . . ? O12 Cl1 O11 108.8(5) . . ? O13 Cl1 O11 110.8(6) . . ? O12 Cl1 O14 111.5(6) . . ? O13 Cl1 O14 108.5(6) . . ? O11 Cl1 O14 107.3(5) . . ? O22 Cl2 O23 119.5(11) . . ? O22 Cl2 O24 115.0(11) . . ? O23 Cl2 O24 102.9(10) . . ? O22 Cl2 O21 103.7(10) . . ? O23 Cl2 O21 109.1(10) . . ? O24 Cl2 O21 105.9(10) . . ? O24 Cl2' O23' 105.5(15) . . ? O24 Cl2' O21' 105.4(16) . . ? O23' Cl2' O21' 103.4(17) . . ? O24 Cl2' O22 140.5(14) . . ? O23' Cl2' O22 104.1(14) . . ? O21' Cl2' O22 92.4(12) . . ? O33 Cl3 O32 119.6(11) . . ? O33 Cl3 O31 114.3(12) . . ? O32 Cl3 O31 104.2(10) . . ? O33 Cl3 O34 104.9(9) . . ? O32 Cl3 O34 107.3(9) . . ? O31 Cl3 O34 105.4(10) . . ? O34 Cl3' O31 134.8(13) . . ? O34 Cl3' O32' 117.5(15) . . ? O31 Cl3' O32' 106.4(13) . . ? O34 Cl3' O33 93.7(9) . . ? O31 Cl3' O33 90.9(11) . . ? O32' Cl3' O33 97.1(13) . . ? O41 Cl4 O41 94.5(17) 2_556 . ? O41 Cl4 O42 116.2(11) 2_556 2_556 ? O41 Cl4 O42 105.4(14) . 2_556 ? O41 Cl4 O42 105.4(14) 2_556 . ? O41 Cl4 O42 116.2(11) . . ? O42 Cl4 O42 117.2(21) 2_556 . ? O41 Cl4 Cl4' 47.3(8) 2_556 . ? O41 Cl4 Cl4' 47.3(9) . . ? O42 Cl4 Cl4' 121.4(10) 2_556 . ? O42 Cl4 Cl4' 121.4(10) . . ? O41 Cl4' O41 94.0(24) 2_556 . ? O41 Cl4' O42' 87.7(23) 2_556 . ? O41 Cl4' O42' 127.7(22) . . ? O41 Cl4' O42' 127.7(22) 2_556 2_556 ? O41 Cl4' O42' 87.7(23) . 2_556 ? O42' Cl4' O42' 130.4(54) . 2_556 ? O41 Cl4' Cl4 47.0(12) 2_556 . ? O41 Cl4' Cl4 47.0(12) . . ? O42' Cl4' Cl4 114.8(27) . . ? O42' Cl4' Cl4 114.8(27) 2_556 . ? O51 Cl5 O52 107.3(14) . . ? O51 Cl5 O54 112.5(10) . . ? O52 Cl5 O54 111.0(9) . . ? O51 Cl5 O53 105.2(16) . . ? O52 Cl5 O53 111.2(13) . . ? O54 Cl5 O53 109.6(11) . . ? Cl2' O21' O22 45.4(8) . . ? Cl2' O22 O21' 42.2(7) . . ? Cl2' O23' O24 36.9(8) . . ? Cl2' O24 O23' 37.6(10) . . ? Cl4 O41 Cl4' 85.7(18) . . ? O1 O53 Cl5 146.3(30) . . ? _refine_diff_density_max 0.973 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.120 #=END data_rock _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H34 F12 N10 P2 Ru' _chemical_formula_weight 1033.77 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 13.862(2) _cell_length_b 15.622(2) _cell_length_c 19.794(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4286.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method ? _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_T_max 0.771 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13053 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4809 _reflns_number_observed 3951 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 4809 _refine_ls_number_parameters 290 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_obs 0.0295 _refine_ls_wR_factor_all 0.0802 _refine_ls_wR_factor_obs 0.0780 _refine_ls_goodness_of_fit_all 0.997 _refine_ls_goodness_of_fit_obs 1.077 _refine_ls_restrained_S_all 0.997 _refine_ls_restrained_S_obs 1.076 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.5000 0.0000 0.21559(3) 0.02946(8) Uani 1 d S . N11 N 0.6093(2) 0.08878(13) 0.20899(13) 0.0361(5) Uani 1 d . . C12 C 0.6914(2) 0.0874(2) 0.2450(2) 0.0447(7) Uani 1 d . . H12A H 0.6990(2) 0.0462(2) 0.2785(2) 0.054 Uiso 1 calc R . C13 C 0.7645(3) 0.1448(2) 0.2337(2) 0.0534(9) Uani 1 d . . H13A H 0.8207(3) 0.1423(2) 0.2593(2) 0.064 Uiso 1 calc R . C14 C 0.7540(3) 0.2059(3) 0.1844(2) 0.0669(12) Uani 1 d . . H14A H 0.8037(3) 0.2441(3) 0.1752(2) 0.080 Uiso 1 calc R . C15 C 0.6696(3) 0.2099(2) 0.1490(2) 0.0567(10) Uani 1 d . . H15A H 0.6608(3) 0.2520(2) 0.1164(2) 0.068 Uiso 1 calc R . C16 C 0.5973(3) 0.1513(2) 0.16180(15) 0.0418(7) Uani 1 d . . N21 N 0.4473(2) 0.08035(15) 0.14159(12) 0.0360(6) Uani 1 d . . C22 C 0.5047(2) 0.1486(2) 0.12560(14) 0.0401(7) Uani 1 d . . C23 C 0.4744(3) 0.2102(2) 0.0795(2) 0.0552(10) Uani 1 d . . H23A H 0.5131(3) 0.2574(2) 0.0701(2) 0.066 Uiso 1 calc R . C24 C 0.3857(3) 0.2007(3) 0.0475(2) 0.0616(11) Uani 1 d . . H24A H 0.3644(3) 0.2417(3) 0.0169(2) 0.074 Uiso 1 calc R . C25 C 0.3302(3) 0.1309(2) 0.0614(2) 0.0544(9) Uani 1 d . . H25A H 0.2715(3) 0.1231(2) 0.0395(2) 0.065 Uiso 1 calc R . C26 C 0.3623(3) 0.0713(2) 0.10872(15) 0.0433(7) Uani 1 d . . H26A H 0.3240(3) 0.0239(2) 0.11802(15) 0.052 Uiso 1 calc R . N31 N 0.4449(2) 0.0683(2) 0.29697(12) 0.0327(6) Uani 1 d . . C32 C 0.3895(3) 0.1385(2) 0.2935(2) 0.0470(8) Uani 1 d . . H32D H 0.3715(3) 0.1590(2) 0.2513(2) 0.056 Uiso 1 calc R . C33 C 0.3580(3) 0.1820(2) 0.3506(2) 0.0525(9) Uani 1 d . . H33A H 0.3186(3) 0.2299(2) 0.3466(2) 0.063 Uiso 1 calc R . C34 C 0.3863(3) 0.1525(2) 0.4141(2) 0.0471(8) Uani 1 d . . H34A H 0.3675(3) 0.1814(2) 0.4530(2) 0.057 Uiso 1 calc R . C35 C 0.4428(2) 0.0798(2) 0.41853(14) 0.0371(6) Uani 1 d . . C36 C 0.4706(2) 0.0390(2) 0.35836(14) 0.0303(6) Uani 1 d . . C41 C 0.4725(2) 0.0407(2) 0.48184(15) 0.0402(7) Uani 1 d . . N42 N 0.4559(2) 0.0662(2) 0.54258(13) 0.0504(7) Uani 1 d . . C43 C 0.5000 0.0000 0.5864(2) 0.0554(14) Uani 1 d S . C44 C 0.4219(3) -0.0401(3) 0.6300(2) 0.0730(12) Uani 1 d . . H44A H 0.4500(3) -0.0831(3) 0.6585(2) 0.109 Uiso 1 calc R . H44B H 0.3739(3) -0.0659(3) 0.6015(2) 0.109 Uiso 1 calc R . H44C H 0.3924(3) 0.0033(3) 0.6574(2) 0.109 Uiso 1 calc R . P P 0.78586(7) 0.09276(6) 0.44848(5) 0.0518(2) Uani 1 d . . F1 F 0.7641(3) 0.0049(2) 0.4138(3) 0.131(2) Uani 1 d . . F2 F 0.7301(3) 0.0640(3) 0.5134(2) 0.157(2) Uani 1 d . . F3 F 0.6910(3) 0.1278(3) 0.4183(2) 0.160(2) Uani 1 d . . F4 F 0.8441(3) 0.1200(2) 0.38450(13) 0.1031(10) Uani 1 d . . F5 F 0.8827(2) 0.0516(3) 0.4778(2) 0.1187(12) Uani 1 d . . F6 F 0.8045(3) 0.1808(2) 0.4842(2) 0.1122(12) Uani 1 d . . C51 C 0.5800(5) 0.3373(7) 0.3745(3) 0.180(5) Uani 1 d . . H51A H 0.5977(5) 0.3947(7) 0.3866(3) 0.270 Uiso 1 calc R . H51B H 0.6350(5) 0.3004(7) 0.3789(3) 0.270 Uiso 1 calc R . H51C H 0.5295(5) 0.3177(7) 0.4039(3) 0.270 Uiso 1 calc R . C52 C 0.5465(4) 0.3358(4) 0.3060(3) 0.087(2) Uani 1 d . . N53 N 0.5176(4) 0.3143(3) 0.2556(2) 0.0929(14) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.04413(14) 0.02284(12) 0.02141(11) 0.000 0.000 0.00027(13) N11 0.0491(13) 0.0298(10) 0.0294(12) -0.0058(11) 0.0080(12) -0.0032(9) C12 0.050(2) 0.049(2) 0.0351(14) -0.0096(14) 0.0044(14) -0.0057(15) C13 0.054(2) 0.066(2) 0.040(2) -0.018(2) 0.0040(13) -0.015(2) C14 0.088(3) 0.070(3) 0.043(2) -0.013(2) 0.016(2) -0.041(2) C15 0.090(3) 0.043(2) 0.037(2) 0.0001(14) 0.014(2) -0.021(2) C16 0.067(2) 0.0308(15) 0.0275(14) -0.0020(12) 0.0155(14) -0.0050(14) N21 0.057(2) 0.0265(13) 0.0248(11) -0.0008(10) 0.0007(12) 0.0049(12) C22 0.064(2) 0.0304(15) 0.0259(13) 0.0015(11) 0.0109(13) 0.0041(14) C23 0.087(3) 0.037(2) 0.041(2) 0.0116(15) 0.021(2) 0.013(2) C24 0.093(3) 0.058(2) 0.034(2) 0.012(2) 0.001(2) 0.032(2) C25 0.076(3) 0.053(2) 0.034(2) -0.0017(15) -0.013(2) 0.023(2) C26 0.061(2) 0.036(2) 0.0327(14) -0.0045(12) -0.0077(14) 0.0090(13) N31 0.046(2) 0.0251(12) 0.0265(12) 0.0007(9) 0.0034(11) -0.0014(10) C32 0.070(2) 0.035(2) 0.036(2) 0.0028(13) 0.0074(15) 0.010(2) C33 0.083(3) 0.032(2) 0.042(2) 0.0005(14) 0.016(2) 0.013(2) C34 0.069(2) 0.035(2) 0.038(2) -0.0049(14) 0.018(2) -0.0019(15) C35 0.050(2) 0.0335(15) 0.0276(13) -0.0029(12) 0.0061(12) -0.0139(13) C36 0.0367(14) 0.0244(14) 0.0298(13) -0.0008(11) 0.0016(11) -0.0077(11) C41 0.047(2) 0.046(2) 0.0280(13) -0.0047(13) 0.0020(12) -0.0161(13) N42 0.061(2) 0.060(2) 0.0295(12) -0.0063(12) 0.0057(13) -0.018(2) C43 0.052(3) 0.088(4) 0.027(2) 0.000 0.000 -0.017(3) C44 0.069(3) 0.111(3) 0.039(2) 0.023(2) -0.001(2) -0.024(3) P 0.0563(5) 0.0526(5) 0.0464(4) 0.0049(4) 0.0007(4) -0.0115(4) F1 0.107(3) 0.079(2) 0.208(4) -0.047(2) 0.008(3) -0.028(2) F2 0.174(4) 0.160(4) 0.136(3) 0.034(3) 0.088(3) -0.031(3) F3 0.119(3) 0.197(4) 0.164(3) -0.056(3) -0.058(3) 0.096(3) F4 0.143(3) 0.101(2) 0.0656(15) 0.0313(15) 0.036(2) 0.017(2) F5 0.092(2) 0.155(3) 0.109(2) 0.045(2) -0.026(2) 0.012(2) F6 0.165(3) 0.078(2) 0.094(2) -0.023(2) 0.019(2) -0.040(2) C51 0.077(4) 0.377(15) 0.087(4) -0.019(6) 0.000(3) -0.023(7) C52 0.065(3) 0.132(5) 0.064(3) -0.012(3) 0.004(2) -0.001(3) N53 0.125(4) 0.090(3) 0.064(3) -0.008(2) -0.010(2) 0.017(3) _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 Ru N11 2.058(2) . ? Ru N11 2.058(2) 2_655 ? Ru N21 2.063(3) . ? Ru N21 2.063(3) 2_655 ? Ru N31 2.077(3) . ? Ru N31 2.077(3) 2_655 ? N11 C12 1.344(4) . ? N11 C16 1.362(4) . ? C12 C13 1.370(5) . ? C13 C14 1.374(5) . ? C14 C15 1.365(6) . ? C15 C16 1.380(5) . ? C16 C22 1.471(5) . ? N21 C26 1.354(4) . ? N21 C22 1.368(4) . ? C22 C23 1.392(5) . ? C23 C24 1.391(6) . ? C24 C25 1.362(6) . ? C25 C26 1.393(4) . ? N31 C32 1.342(4) . ? N31 C36 1.346(4) . ? C32 C33 1.389(4) . ? C33 C34 1.395(5) . ? C34 C35 1.381(5) . ? C35 C36 1.405(4) . ? C35 C41 1.454(4) . ? C36 C36 1.465(6) 2_655 ? C41 N42 1.288(4) . ? C41 C41 1.482(7) 2_655 ? N42 C43 1.483(4) . ? C43 N42 1.483(4) 2_655 ? C43 C44 1.519(5) 2_655 ? C43 C44 1.519(5) . ? P F3 1.544(3) . ? P F4 1.561(3) . ? P F1 1.565(3) . ? P F2 1.565(3) . ? P F6 1.568(3) . ? P F5 1.598(3) . ? C51 C52 1.432(8) . ? C52 N53 1.128(6) . ? 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 N11 Ru N11 172.72(15) . 2_655 ? N11 Ru N21 78.79(11) . . ? N11 Ru N21 95.98(10) 2_655 . ? N11 Ru N21 95.98(10) . 2_655 ? N11 Ru N21 78.79(11) 2_655 2_655 ? N21 Ru N21 89.52(14) . 2_655 ? N11 Ru N31 88.50(10) . . ? N11 Ru N31 97.16(10) 2_655 . ? N21 Ru N31 96.20(9) . . ? N21 Ru N31 173.34(10) 2_655 . ? N11 Ru N31 97.16(10) . 2_655 ? N11 Ru N31 88.50(10) 2_655 2_655 ? N21 Ru N31 173.34(10) . 2_655 ? N21 Ru N31 96.20(9) 2_655 2_655 ? N31 Ru N31 78.30(14) . 2_655 ? C12 N11 C16 118.6(3) . . ? C12 N11 Ru 125.4(2) . . ? C16 N11 Ru 116.0(2) . . ? N11 C12 C13 122.0(3) . . ? C12 C13 C14 119.5(4) . . ? C15 C14 C13 119.2(3) . . ? C14 C15 C16 119.9(3) . . ? N11 C16 C15 120.9(3) . . ? N11 C16 C22 114.8(3) . . ? C15 C16 C22 124.3(3) . . ? C26 N21 C22 118.5(3) . . ? C26 N21 Ru 125.9(2) . . ? C22 N21 Ru 115.6(2) . . ? N21 C22 C23 121.0(3) . . ? N21 C22 C16 114.7(3) . . ? C23 C22 C16 124.3(3) . . ? C24 C23 C22 119.4(4) . . ? C25 C24 C23 119.6(3) . . ? C24 C25 C26 119.3(4) . . ? N21 C26 C25 122.1(3) . . ? C32 N31 C36 118.4(3) . . ? C32 N31 Ru 126.2(2) . . ? C36 N31 Ru 115.4(2) . . ? N31 C32 C33 122.6(3) . . ? C32 C33 C34 118.9(3) . . ? C35 C34 C33 119.2(3) . . ? C34 C35 C36 118.4(3) . . ? C34 C35 C41 124.1(3) . . ? C36 C35 C41 117.5(3) . . ? N31 C36 C35 122.5(3) . . ? N31 C36 C36 115.4(2) . 2_655 ? C35 C36 C36 122.0(2) . 2_655 ? N42 C41 C35 128.6(3) . . ? N42 C41 C41 111.0(2) . 2_655 ? C35 C41 C41 120.4(2) . 2_655 ? C41 N42 C43 104.9(3) . . ? N42 C43 N42 108.3(4) . 2_655 ? N42 C43 C44 109.8(2) . 2_655 ? N42 C43 C44 109.0(2) 2_655 2_655 ? N42 C43 C44 109.0(2) . . ? N42 C43 C44 109.8(2) 2_655 . ? C44 C43 C44 110.9(4) 2_655 . ? F3 P F4 91.7(2) . . ? F3 P F1 88.7(3) . . ? F4 P F1 89.0(2) . . ? F3 P F2 90.0(3) . . ? F4 P F2 178.3(2) . . ? F1 P F2 90.7(2) . . ? F3 P F6 90.2(2) . . ? F4 P F6 92.4(2) . . ? F1 P F6 178.2(2) . . ? F2 P F6 87.9(2) . . ? F3 P F5 176.9(2) . . ? F4 P F5 88.2(2) . . ? F1 P F5 88.2(2) . . ? F2 P F5 90.1(2) . . ? F6 P F5 92.9(2) . . ? N53 C52 C51 163.3(8) . . ? _refine_diff_density_max 0.580 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.061