# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ic13993 _database_code_depnum_ccdc_archive 'CCDC 903912' #TrackingRef 'web_deposit_cif_file_0_WaiLunMan_1349106073.total.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H72 Mn N8 O16 Ru2' _chemical_formula_weight 1322.26 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' Mn Mn 0.3368 0.7283 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8446(2) _cell_length_b 12.6986(3) _cell_length_c 27.9148(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.1090(11) _cell_angle_gamma 90.00 _cell_volume 3133.10(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5965 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description rod _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1362 _exptl_absorpt_coefficient_mu 0.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_process_details ? _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 KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15205 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5498 _reflns_number_gt 4127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1281P)^2^+16.4996P] 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 SHELXL _refine_ls_extinction_coef 0.0141(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5498 _refine_ls_number_parameters 326 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.1355 _refine_ls_R_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.3049 _refine_ls_wR_factor_gt 0.2858 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.003 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 Ru Ru 0.13950(8) 0.43603(8) 0.18440(3) 0.0629(4) Uani 1 1 d . . . Mn Mn 0.0000 0.5000 0.0000 0.0718(8) Uani 1 2 d S . . N1 N 0.0217(10) 0.4611(10) 0.0751(3) 0.087(3) Uani 1 1 d . A . N2 N 0.2705(10) 0.4240(8) 0.2930(3) 0.073(3) Uani 1 1 d . . . C1 C 0.0590(11) 0.4497(11) 0.1145(4) 0.075(3) Uani 1 1 d . A . C2 C 0.2239(10) 0.4263(8) 0.2544(4) 0.057(2) Uani 1 1 d . A . O3 O 0.1570(16) 0.3664(12) -0.0143(5) 0.090(4) Uiso 0.657(7) 1 d PD A 1 H3B H 0.2121 0.3887 -0.0365 0.108 Uiso 0.657(7) 1 d PR A 1 O4 O -0.1782(15) 0.3818(11) -0.0048(5) 0.087(4) Uiso 0.657(7) 1 d PD A 1 H4B H -0.1563 0.3219 0.0071 0.105 Uiso 0.657(7) 1 d PR A 1 C21 C 0.259(2) 0.3132(18) 0.0205(7) 0.107(7) Uiso 0.657(7) 1 d PD A 1 H21A H 0.3150 0.2580 0.0042 0.160 Uiso 0.657(7) 1 calc PR A 1 H21B H 0.1994 0.2816 0.0457 0.160 Uiso 0.657(7) 1 calc PR A 1 H21C H 0.3300 0.3645 0.0347 0.160 Uiso 0.657(7) 1 calc PR A 1 C22 C -0.331(2) 0.404(2) -0.0215(11) 0.136(10) Uiso 0.657(7) 1 d PD A 1 H22A H -0.3937 0.3409 -0.0180 0.204 Uiso 0.657(7) 1 calc PR A 1 H22B H -0.3318 0.4247 -0.0553 0.204 Uiso 0.657(7) 1 calc PR A 1 H22C H -0.3724 0.4615 -0.0025 0.204 Uiso 0.657(7) 1 calc PR A 1 O3' O 0.212(3) 0.423(2) -0.0128(10) 0.091(8) Uiso 0.343(7) 1 d PD A 2 H3'B H 0.2167 0.3734 -0.0331 0.109 Uiso 0.343(7) 1 d PR A 2 O4' O -0.113(3) 0.349(2) -0.0269(11) 0.102(8) Uiso 0.343(7) 1 d PD A 2 H4'B H -0.1070 0.3042 -0.0042 0.122 Uiso 0.343(7) 1 d PR A 2 C21' C 0.352(4) 0.443(4) 0.0148(16) 0.120 Uiso 0.343(7) 1 d PD A 2 H21D H 0.4321 0.3975 0.0029 0.180 Uiso 0.343(7) 1 calc PR A 2 H21E H 0.3370 0.4271 0.0487 0.180 Uiso 0.343(7) 1 calc PR A 2 H21F H 0.3809 0.5167 0.0114 0.180 Uiso 0.343(7) 1 calc PR A 2 C22' C -0.276(4) 0.353(4) -0.0357(19) 0.120 Uiso 0.343(7) 1 d PD A 2 H22D H -0.3195 0.2831 -0.0299 0.180 Uiso 0.343(7) 1 calc PR A 2 H22E H -0.2985 0.3735 -0.0690 0.180 Uiso 0.343(7) 1 calc PR A 2 H22F H -0.3203 0.4042 -0.0141 0.180 Uiso 0.343(7) 1 calc PR A 2 O1 O 0.0463(11) 0.5695(8) 0.1972(4) 0.066(3) Uani 0.657(7) 1 d PD A 1 N3 N -0.0668(12) 0.3787(10) 0.2084(4) 0.057(3) Uani 0.657(7) 1 d PD A 1 C3 C -0.1178(19) 0.2829(12) 0.2127(7) 0.058(5) Uiso 0.657(7) 1 d PD A 1 H3A H -0.0584 0.2259 0.2019 0.070 Uiso 0.657(7) 1 calc PR A 1 C4 C -0.2586(19) 0.2610(13) 0.2330(6) 0.072(5) Uiso 0.657(7) 1 d PD A 1 H4A H -0.2915 0.1901 0.2354 0.086 Uiso 0.657(7) 1 calc PR A 1 C5 C -0.352(2) 0.3439(15) 0.2500(9) 0.072(7) Uiso 0.657(7) 1 d PD A 1 H5A H -0.4462 0.3302 0.2644 0.086 Uiso 0.657(7) 1 calc PR A 1 C6 C -0.2969(14) 0.4482(11) 0.2440(6) 0.050(4) Uiso 0.657(7) 1 d PD A 1 C7 C -0.369(2) 0.5387(14) 0.2576(8) 0.065(6) Uiso 0.657(7) 1 d PD A 1 H7A H -0.4637 0.5326 0.2720 0.078 Uiso 0.657(7) 1 calc PR A 1 C8 C -0.3141(19) 0.6313(14) 0.2517(7) 0.076(5) Uiso 0.657(7) 1 d PD A 1 H8A H -0.3694 0.6911 0.2616 0.091 Uiso 0.657(7) 1 calc PR A 1 C9 C -0.1742(18) 0.6448(12) 0.2311(6) 0.072(4) Uiso 0.657(7) 1 d PD A 1 H9A H -0.1370 0.7142 0.2268 0.086 Uiso 0.657(7) 1 calc PR A 1 C10 C -0.0906(17) 0.5635(13) 0.2170(7) 0.056(4) Uiso 0.657(7) 1 d PD A 1 C11 C -0.1540(14) 0.4615(9) 0.2229(5) 0.052(3) Uiso 0.657(7) 1 d PD A 1 O1' O 0.0463(17) 0.3079(13) 0.1888(6) 0.056(5) Uiso 0.343(7) 1 d PD A 2 N3' N -0.0669(19) 0.4961(13) 0.2119(7) 0.042(5) Uiso 0.343(7) 1 d PD A 2 C3' C -0.114(3) 0.5899(16) 0.2235(12) 0.053(9) Uiso 0.343(7) 1 d PD A 2 H3'A H -0.0518 0.6497 0.2186 0.064 Uiso 0.343(7) 1 calc PR A 2 C4' C -0.257(3) 0.6024(19) 0.2431(11) 0.062(8) Uiso 0.343(7) 1 d PD A 2 H4'A H -0.2944 0.6715 0.2486 0.074 Uiso 0.343(7) 1 calc PR A 2 C5' C -0.349(4) 0.5137(19) 0.2550(16) 0.073(13) Uiso 0.343(7) 1 d PD A 2 H5'A H -0.4445 0.5222 0.2688 0.088 Uiso 0.343(7) 1 calc PR A 2 C6' C -0.289(2) 0.4121(16) 0.2451(10) 0.044(7) Uiso 0.343(7) 1 d PD A 2 C7' C -0.361(3) 0.317(2) 0.2498(15) 0.062(12) Uiso 0.343(7) 1 d PD A 2 H7'A H -0.4606 0.3189 0.2615 0.074 Uiso 0.343(7) 1 calc PR A 2 C8' C -0.308(3) 0.226(2) 0.2400(12) 0.072(9) Uiso 0.343(7) 1 d PD A 2 H8'A H -0.3630 0.1643 0.2477 0.087 Uiso 0.343(7) 1 calc PR A 2 C9' C -0.170(2) 0.2188(17) 0.2179(9) 0.056(7) Uiso 0.343(7) 1 d PD A 2 H9'A H -0.1303 0.1517 0.2098 0.068 Uiso 0.343(7) 1 calc PR A 2 C10' C -0.092(3) 0.3071(18) 0.2080(16) 0.070(13) Uiso 0.343(7) 1 d PD A 2 C11' C -0.148(2) 0.4069(12) 0.2224(8) 0.037(5) Uiso 0.343(7) 1 d PD A 2 O2 O 0.2264(10) 0.2902(8) 0.1675(4) 0.063(3) Uani 0.657(7) 1 d PD A 1 N4 N 0.3467(13) 0.4795(10) 0.1596(4) 0.069(4) Uani 0.657(7) 1 d PD A 1 C12 C 0.397(2) 0.5754(14) 0.1560(8) 0.076(6) Uiso 0.657(7) 1 d PD A 1 H12A H 0.3349 0.6315 0.1663 0.091 Uiso 0.657(7) 1 calc PR A 1 C13 C 0.538(2) 0.5996(14) 0.1373(7) 0.090(6) Uiso 0.657(7) 1 d PD A 1 H13A H 0.5717 0.6706 0.1358 0.108 Uiso 0.657(7) 1 calc PR A 1 C14 C 0.630(2) 0.5175(15) 0.1209(8) 0.090(6) Uiso 0.657(7) 1 d PD A 1 H14A H 0.7246 0.5318 0.1074 0.108 Uiso 0.657(7) 1 calc PR A 1 C15 C 0.5765(16) 0.4128(11) 0.1252(6) 0.064(4) Uiso 0.657(7) 1 d PD A 1 C16 C 0.645(2) 0.3221(15) 0.1098(7) 0.092(6) Uiso 0.657(7) 1 d PD A 1 H16A H 0.7394 0.3292 0.0952 0.111 Uiso 0.657(7) 1 calc PR A 1 C17 C 0.591(2) 0.2292(15) 0.1135(7) 0.096(6) Uiso 0.657(7) 1 d PD A 1 H17A H 0.6479 0.1709 0.1027 0.115 Uiso 0.657(7) 1 calc PR A 1 C18 C 0.4492(19) 0.2120(14) 0.1337(7) 0.091(6) Uiso 0.657(7) 1 d PD A 1 H18A H 0.4111 0.1423 0.1362 0.109 Uiso 0.657(7) 1 calc PR A 1 C19 C 0.367(2) 0.2937(14) 0.1492(9) 0.078(7) Uiso 0.657(7) 1 d PD A 1 C20 C 0.4309(16) 0.3958(11) 0.1444(6) 0.069(4) Uiso 0.657(7) 1 d PD A 1 O2' O 0.2341(17) 0.5944(13) 0.1811(6) 0.053(5) Uiso 0.343(7) 1 d PD A 2 N4' N 0.344(2) 0.4113(13) 0.1561(11) 0.068(8) Uiso 0.343(7) 1 d PD A 2 C12' C 0.393(3) 0.3166(14) 0.1474(11) 0.037(7) Uiso 0.343(7) 1 d PD A 2 H12B H 0.3311 0.2580 0.1549 0.045 Uiso 0.343(7) 1 calc PR A 2 C13' C 0.535(3) 0.2988(19) 0.1271(13) 0.089(11) Uiso 0.343(7) 1 d PD A 2 H13B H 0.5681 0.2287 0.1218 0.107 Uiso 0.343(7) 1 calc PR A 2 C14' C 0.629(3) 0.3843(17) 0.1144(10) 0.052(6) Uiso 0.343(7) 1 d PD A 2 H14B H 0.7221 0.3742 0.0994 0.062 Uiso 0.343(7) 1 calc PR A 2 C15' C 0.573(2) 0.4864(14) 0.1258(9) 0.047(6) Uiso 0.343(7) 1 d PD A 2 C16' C 0.639(3) 0.5817(16) 0.1173(10) 0.060(7) Uiso 0.343(7) 1 d PD A 2 H16B H 0.7359 0.5799 0.1038 0.072 Uiso 0.343(7) 1 calc PR A 2 C17' C 0.585(2) 0.6726(17) 0.1254(9) 0.058(7) Uiso 0.343(7) 1 d PD A 2 H17B H 0.6394 0.7332 0.1159 0.070 Uiso 0.343(7) 1 calc PR A 2 C18' C 0.447(2) 0.6855(15) 0.1482(9) 0.051(6) Uiso 0.343(7) 1 d PD A 2 H18B H 0.4089 0.7539 0.1546 0.061 Uiso 0.343(7) 1 calc PR A 2 C19' C 0.370(2) 0.5994(15) 0.1607(9) 0.035(6) Uiso 0.343(7) 1 d PD A 2 C20' C 0.431(2) 0.5000(12) 0.1475(9) 0.049(6) Uiso 0.343(7) 1 d PD A 2 O5 O 0.0486(13) 0.1603(8) 0.1154(4) 0.115(3) Uani 1 1 d . . . H5 H 0.1338 0.1796 0.1063 0.173 Uiso 1 1 d R . . C23 C 0.057(3) 0.0589(13) 0.1326(7) 0.148(8) Uani 1 1 d . . . H23A H 0.1280 0.0562 0.1603 0.222 Uiso 1 1 calc R . . H23B H 0.0918 0.0119 0.1075 0.222 Uiso 1 1 calc R . . H23C H -0.0435 0.0364 0.1423 0.222 Uiso 1 1 calc R . . O6 O 0.870(2) 0.1961(15) 0.0382(6) 0.198(6) Uiso 1 1 d D . . H6 H 0.7848 0.2088 0.0491 0.297 Uiso 1 1 d R . . C24 C 0.843(5) 0.099(3) 0.0119(14) 0.34(2) Uiso 1 1 d D . . H24A H 0.7542 0.0638 0.0240 0.510 Uiso 1 1 calc R . . H24B H 0.9318 0.0532 0.0161 0.510 Uiso 1 1 calc R . . H24C H 0.8263 0.1152 -0.0222 0.510 Uiso 1 1 calc R . . O7 O 0.1079(19) 0.2200(14) -0.0773(6) 0.200 Uiso 1 1 d . . . H7 H 0.1775 0.2640 -0.0810 0.300 Uiso 1 1 d R . . C25 C -0.024(2) 0.2361(17) -0.1209(7) 0.156(7) Uiso 1 1 d . . . H25A H -0.1029 0.1823 -0.1180 0.234 Uiso 1 1 calc R . . H25B H 0.0219 0.2292 -0.1521 0.234 Uiso 1 1 calc R . . H25C H -0.0697 0.3062 -0.1183 0.234 Uiso 1 1 calc R . . O8 O 0.339(2) 0.3991(17) 0.3877(5) 0.233(10) Uani 1 1 d . . . H8 H 0.2979 0.4499 0.3729 0.349 Uiso 1 1 d R . . C26 C 0.493(4) 0.422(2) 0.3973(13) 0.241(15) Uiso 1 1 d . . . H26A H 0.5024 0.4956 0.4052 0.362 Uiso 1 1 d R . . H26B H 0.5369 0.4139 0.3665 0.362 Uiso 1 1 d R . . H26C H 0.5378 0.3769 0.4214 0.362 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0410(5) 0.1014(8) 0.0463(5) 0.0080(4) 0.0014(3) -0.0047(4) Mn 0.0500(12) 0.121(2) 0.0438(11) 0.0074(12) -0.0016(9) -0.0109(13) N1 0.056(5) 0.153(10) 0.052(5) 0.019(6) 0.003(4) 0.000(6) N2 0.061(5) 0.105(8) 0.054(5) 0.011(5) 0.003(4) -0.008(5) C1 0.044(5) 0.136(11) 0.046(6) 0.010(6) 0.001(4) -0.003(6) C2 0.043(5) 0.078(7) 0.051(6) 0.009(5) 0.007(4) -0.003(5) O1 0.051(6) 0.074(7) 0.072(7) 0.018(5) 0.004(5) 0.004(5) N3 0.051(7) 0.080(10) 0.039(6) -0.003(6) 0.001(5) 0.007(7) O2 0.055(6) 0.069(7) 0.065(6) -0.004(5) 0.010(5) 0.002(5) N4 0.055(8) 0.107(13) 0.044(7) 0.006(8) -0.013(6) -0.021(8) O5 0.136(9) 0.091(7) 0.119(8) -0.012(6) 0.012(6) -0.009(6) C23 0.20(2) 0.098(13) 0.145(17) -0.001(11) -0.020(15) -0.048(13) O8 0.25(2) 0.32(2) 0.123(11) 0.086(13) -0.044(12) -0.112(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 Ru O1' 1.830(17) . ? Ru O1 1.924(10) . ? Ru N4' 2.03(2) . ? Ru N4 2.058(12) . ? Ru C1 2.060(10) . ? Ru O2 2.066(10) . ? Ru C2 2.069(10) . ? Ru N3 2.097(11) . ? Ru N3' 2.146(16) . ? Ru O2' 2.181(16) . ? Mn O3' 2.15(3) 3_565 ? Mn O3' 2.15(3) . ? Mn N1 2.156(9) . ? Mn N1 2.156(9) 3_565 ? Mn O4 2.177(13) . ? Mn O4 2.177(13) 3_565 ? Mn O3 2.238(13) . ? Mn O3 2.238(13) 3_565 ? Mn O4' 2.28(3) 3_565 ? Mn O4' 2.28(3) . ? N1 C1 1.145(13) . ? N2 C2 1.140(12) . ? O3 C21 1.465(16) . ? O4 C22 1.443(17) . ? O3' C21' 1.459(19) . ? O4' C22' 1.454(19) . ? O1 C10 1.351(16) . ? N3 C3 1.305(18) . ? N3 C11 1.374(14) . ? C3 C4 1.41(2) . ? C4 C5 1.43(2) . ? C5 C6 1.42(2) . ? C6 C7 1.37(2) . ? C6 C11 1.424(14) . ? C7 C8 1.283(19) . ? C8 C9 1.395(19) . ? C9 C10 1.34(2) . ? C10 C11 1.424(17) . ? O1' C10' 1.35(2) . ? N3' C3' 1.31(2) . ? N3' C11' 1.377(16) . ? C3' C4' 1.41(2) . ? C4' C5' 1.43(2) . ? C5' C6' 1.42(2) . ? C6' C7' 1.37(2) . ? C6' C11' 1.425(17) . ? C7' C8' 1.28(2) . ? C8' C9' 1.40(2) . ? C9' C10' 1.35(2) . ? C10' C11' 1.42(2) . ? O2 C19 1.364(17) . ? N4 C12 1.301(18) . ? N4 C20 1.373(15) . ? C12 C13 1.41(2) . ? C13 C14 1.41(2) . ? C14 C15 1.42(2) . ? C15 C16 1.376(19) . ? C15 C20 1.431(16) . ? C16 C17 1.28(2) . ? C17 C18 1.412(19) . ? C18 C19 1.35(2) . ? C19 C20 1.422(19) . ? O2' C19' 1.351(19) . ? N4' C12' 1.302(19) . ? N4' C20' 1.390(16) . ? C12' C13' 1.42(2) . ? C13' C14' 1.42(2) . ? C14' C15' 1.43(2) . ? C15' C16' 1.37(2) . ? C15' C20' 1.425(17) . ? C16' C17' 1.27(2) . ? C17' C18' 1.41(2) . ? C18' C19' 1.34(2) . ? C19' C20' 1.43(2) . ? O5 C23 1.375(18) . ? O6 C24 1.447(18) . ? O7 C25 1.67(2) . ? O8 C26 1.41(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1' Ru O1 125.0(6) . . ? O1' Ru N4' 107.4(7) . . ? O1 Ru N4' 127.2(6) . . ? O1' Ru N4 132.0(6) . . ? O1 Ru N4 102.7(5) . . ? N4' Ru N4 24.6(6) . . ? O1' Ru C1 89.8(7) . . ? O1 Ru C1 88.1(5) . . ? N4' Ru C1 85.8(9) . . ? N4 Ru C1 86.6(4) . . ? O1' Ru O2 52.5(5) . . ? O1 Ru O2 175.9(4) . . ? N4' Ru O2 55.0(5) . . ? N4 Ru O2 79.6(4) . . ? C1 Ru O2 88.7(5) . . ? O1' Ru C2 91.8(6) . . ? O1 Ru C2 91.1(4) . . ? N4' Ru C2 93.5(9) . . ? N4 Ru C2 92.2(4) . . ? C1 Ru C2 178.3(5) . . ? O2 Ru C2 92.2(4) . . ? O1' Ru N3 43.2(6) . . ? O1 Ru N3 82.1(4) . . ? N4' Ru N3 150.6(6) . . ? N4 Ru N3 175.2(4) . . ? C1 Ru N3 93.3(4) . . ? O2 Ru N3 95.6(4) . . ? C2 Ru N3 88.1(4) . . ? O1' Ru N3' 84.3(6) . . ? O1 Ru N3' 40.9(5) . . ? N4' Ru N3' 168.1(6) . . ? N4 Ru N3' 143.6(6) . . ? C1 Ru N3' 92.3(6) . . ? O2 Ru N3' 136.8(5) . . ? C2 Ru N3' 88.0(6) . . ? N3 Ru N3' 41.2(6) . . ? O1' Ru O2' 175.5(5) . . ? O1 Ru O2' 50.5(5) . . ? N4' Ru O2' 77.1(6) . . ? N4 Ru O2' 52.5(5) . . ? C1 Ru O2' 90.1(6) . . ? O2 Ru O2' 132.1(5) . . ? C2 Ru O2' 88.3(5) . . ? N3 Ru O2' 132.3(5) . . ? N3' Ru O2' 91.2(6) . . ? O3' Mn O3' 180.0(14) 3_565 . ? O3' Mn N1 89.4(8) 3_565 . ? O3' Mn N1 90.6(8) . . ? O3' Mn N1 90.6(8) 3_565 3_565 ? O3' Mn N1 89.4(8) . 3_565 ? N1 Mn N1 180.00(12) . 3_565 ? O3' Mn O4 72.0(9) 3_565 . ? O3' Mn O4 108.0(9) . . ? N1 Mn O4 86.6(4) . . ? N1 Mn O4 93.4(4) 3_565 . ? O3' Mn O4 108.0(9) 3_565 3_565 ? O3' Mn O4 72.0(9) . 3_565 ? N1 Mn O4 93.4(4) . 3_565 ? N1 Mn O4 86.6(4) 3_565 3_565 ? O4 Mn O4 180.0(5) . 3_565 ? O3' Mn O3 157.4(7) 3_565 . ? O3' Mn O3 22.6(7) . . ? N1 Mn O3 88.1(4) . . ? N1 Mn O3 91.9(4) 3_565 . ? O4 Mn O3 85.4(5) . . ? O4 Mn O3 94.6(5) 3_565 . ? O3' Mn O3 22.6(7) 3_565 3_565 ? O3' Mn O3 157.4(7) . 3_565 ? N1 Mn O3 91.9(4) . 3_565 ? N1 Mn O3 88.1(4) 3_565 3_565 ? O4 Mn O3 94.6(5) . 3_565 ? O4 Mn O3 85.4(5) 3_565 3_565 ? O3 Mn O3 180.0(7) . 3_565 ? O3' Mn O4' 86.4(10) 3_565 3_565 ? O3' Mn O4' 93.6(10) . 3_565 ? N1 Mn O4' 81.4(8) . 3_565 ? N1 Mn O4' 98.6(8) 3_565 3_565 ? O4 Mn O4' 155.4(7) . 3_565 ? O4 Mn O4' 24.6(7) 3_565 3_565 ? O3 Mn O4' 115.4(8) . 3_565 ? O3 Mn O4' 64.6(8) 3_565 3_565 ? O3' Mn O4' 93.6(10) 3_565 . ? O3' Mn O4' 86.4(10) . . ? N1 Mn O4' 98.6(8) . . ? N1 Mn O4' 81.4(8) 3_565 . ? O4 Mn O4' 24.6(7) . . ? O4 Mn O4' 155.4(7) 3_565 . ? O3 Mn O4' 64.6(8) . . ? O3 Mn O4' 115.4(8) 3_565 . ? O4' Mn O4' 180.0(14) 3_565 . ? C1 N1 Mn 167.1(9) . . ? N1 C1 Ru 175.8(10) . . ? N2 C2 Ru 178.1(10) . . ? C21 O3 Mn 127.0(12) . . ? C22 O4 Mn 123.6(15) . . ? C21' O3' Mn 124(3) . . ? C22' O4' Mn 117(3) . . ? C10 O1 Ru 115.0(9) . . ? C3 N3 C11 119.1(11) . . ? C3 N3 Ru 131.4(10) . . ? C11 N3 Ru 109.4(8) . . ? N3 C3 C4 122.2(13) . . ? C3 C4 C5 121.2(15) . . ? C6 C5 C4 115.9(15) . . ? C7 C6 C5 125.6(11) . . ? C7 C6 C11 116.1(12) . . ? C5 C6 C11 118.3(12) . . ? C8 C7 C6 123.6(16) . . ? C7 C8 C9 120.5(17) . . ? C10 C9 C8 122.4(15) . . ? C9 C10 O1 126.2(14) . . ? C9 C10 C11 116.3(13) . . ? O1 C10 C11 117.5(14) . . ? N3 C11 C10 115.7(12) . . ? N3 C11 C6 123.2(10) . . ? C10 C11 C6 121.0(11) . . ? C10' O1' Ru 116.7(13) . . ? C3' N3' C11' 121.6(15) . . ? C3' N3' Ru 134.1(14) . . ? C11' N3' Ru 103.9(10) . . ? N3' C3' C4' 120.0(18) . . ? C3' C4' C5' 122(2) . . ? C6' C5' C4' 116.9(19) . . ? C7' C6' C5' 127.1(16) . . ? C7' C6' C11' 114.8(15) . . ? C5' C6' C11' 117.6(15) . . ? C8' C7' C6' 127(2) . . ? C7' C8' C9' 119(2) . . ? C10' C9' C8' 119.8(19) . . ? C9' C10' O1' 124.2(18) . . ? C9' C10' C11' 119.8(17) . . ? O1' C10' C11' 115.6(17) . . ? N3' C11' C10' 118.9(15) . . ? N3' C11' C6' 121.9(14) . . ? C10' C11' C6' 119.1(14) . . ? C19 O2 Ru 114.1(9) . . ? C12 N4 C20 120.7(13) . . ? C12 N4 Ru 125.9(11) . . ? C20 N4 Ru 113.3(9) . . ? N4 C12 C13 122.9(16) . . ? C14 C13 C12 119.2(17) . . ? C13 C14 C15 118.2(16) . . ? C16 C15 C14 127.5(14) . . ? C16 C15 C20 113.7(12) . . ? C14 C15 C20 118.7(12) . . ? C17 C16 C15 125.5(17) . . ? C16 C17 C18 120.9(17) . . ? C19 C18 C17 120.4(16) . . ? C18 C19 O2 127.2(15) . . ? C18 C19 C20 117.0(15) . . ? O2 C19 C20 115.8(14) . . ? N4 C20 C19 117.1(12) . . ? N4 C20 C15 120.3(11) . . ? C19 C20 C15 122.5(12) . . ? C19' O2' Ru 114.2(12) . . ? C12' N4' C20' 122.0(15) . . ? C12' N4' Ru 121.3(13) . . ? C20' N4' Ru 116.7(11) . . ? N4' C12' C13' 121.6(17) . . ? C14' C13' C12' 121(2) . . ? C13' C14' C15' 115.7(18) . . ? C16' C15' C20' 110.6(14) . . ? C16' C15' C14' 128.1(16) . . ? C20' C15' C14' 121.3(14) . . ? C17' C16' C15' 128(2) . . ? C16' C17' C18' 121(2) . . ? C19' C18' C17' 118.7(17) . . ? C18' C19' O2' 128.0(17) . . ? C18' C19' C20' 116.9(16) . . ? O2' C19' C20' 114.8(15) . . ? N4' C20' C15' 118.5(13) . . ? N4' C20' C19' 117.1(14) . . ? C15' C20' C19' 124.5(14) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.226 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.212 data_051210a_xj _database_code_depnum_ccdc_archive 'CCDC 903913' #TrackingRef 'web_deposit_cif_file_0_WaiLunMan_1349106073.total.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H26 Cl Mn N6 O4 Ru' _chemical_formula_weight 677.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 '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' _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 14.5641(4) _cell_length_b 10.4098(3) _cell_length_c 18.0972(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.669(3) _cell_angle_gamma 90.00 _cell_volume 2740.72(13) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 8032 _cell_measurement_theta_min 4.8891 _cell_measurement_theta_max 71.4048 _exptl_crystal_description rectangle _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 9.479 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.52689 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Oxford Diffraction Ltd' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1270 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11644 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.89 _diffrn_reflns_theta_max 66.95 _reflns_number_total 2446 _reflns_number_gt 2382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ortep-3 _computing_publication_material wingx _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^)+(0.0633P)^2^+11.7950P] 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 2446 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Ru1 Ru 1.0000 1.0000 1.0000 0.01378(15) Uani 1 2 d S . . Mn1 Mn 1.0000 0.72397(7) 0.7500 0.01264(18) Uani 1 2 d S . . Cl1 Cl 1.0000 0.49513(11) 0.7500 0.0408(4) Uani 1 2 d S . . O1 O 0.88448(16) 1.0910(2) 0.96548(13) 0.0257(5) Uani 1 1 d . . . O2 O 1.14673(15) 0.7380(2) 0.76981(14) 0.0235(5) Uani 1 1 d . . . N1 N 0.99248(18) 0.8266(3) 0.85309(15) 0.0192(6) Uani 1 1 d . . . N2 N 0.9049(2) 0.8820(3) 1.04844(15) 0.0240(6) Uani 1 1 d . . . N3 N 1.29197(19) 0.6671(3) 0.78854(16) 0.0221(6) Uani 1 1 d . . . C1 C 0.9951(2) 0.8864(3) 0.90507(18) 0.0180(7) Uani 1 1 d . . . C2 C 1.2058(2) 0.6532(3) 0.76517(18) 0.0198(7) Uani 1 1 d . . . H2 H 1.1882 0.5751 0.7439 0.024 Uiso 1 1 calc R . . C3 C 1.3604(3) 0.5684(4) 0.7765(2) 0.0374(10) Uani 1 1 d . . . H3A H 1.3305 0.4930 0.7565 0.056 Uiso 1 1 calc R . . H3B H 1.3919 0.5475 0.8227 0.056 Uiso 1 1 calc R . . H3C H 1.4037 0.5996 0.7424 0.056 Uiso 1 1 calc R . . C4 C 1.3236(3) 0.7852(4) 0.8245(2) 0.0300(8) Uani 1 1 d . . . H4A H 1.2720 0.8404 0.8318 0.045 Uiso 1 1 calc R . . H4B H 1.3662 0.8279 0.7938 0.045 Uiso 1 1 calc R . . H4C H 1.3535 0.7652 0.8714 0.045 Uiso 1 1 calc R . . C5 C 0.8182(2) 0.9281(4) 1.03809(19) 0.0242(8) Uani 1 1 d . . . C6 C 0.8080(2) 1.0431(4) 0.99284(19) 0.0230(7) Uani 1 1 d . . . C7 C 0.7211(3) 1.0914(4) 0.9797(2) 0.0309(8) Uani 1 1 d . . . H7 H 0.7121 1.1634 0.9499 0.037 Uiso 1 1 calc R . . C8 C 0.6457(3) 1.0321(5) 1.0113(2) 0.0365(9) Uani 1 1 d . . . H8 H 0.5876 1.0675 1.0027 0.044 Uiso 1 1 calc R . . C9 C 0.6543(3) 0.9253(4) 1.0540(2) 0.0346(9) Uani 1 1 d . . . H9 H 0.6027 0.8892 1.0742 0.042 Uiso 1 1 calc R . . C10 C 0.7408(2) 0.8692(4) 1.06780(18) 0.0265(8) Uani 1 1 d . . . C11 C 0.7572(3) 0.7531(4) 1.1083(2) 0.0317(9) Uani 1 1 d . . . H11 H 0.7086 0.7087 1.1281 0.038 Uiso 1 1 calc R . . C12 C 0.8458(3) 0.7078(4) 1.1177(2) 0.0312(8) Uani 1 1 d . . . H12 H 0.8580 0.6326 1.1441 0.037 Uiso 1 1 calc R . . C13 C 0.9183(3) 0.7773(4) 1.08658(19) 0.0258(8) Uani 1 1 d . . . H13 H 0.9780 0.7467 1.0938 0.031 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 Ru1 0.0120(2) 0.0213(2) 0.0079(2) -0.00119(11) -0.00059(13) -0.00222(11) Mn1 0.0102(3) 0.0197(4) 0.0079(3) 0.000 -0.0013(2) 0.000 Cl1 0.0181(6) 0.0220(7) 0.0823(12) 0.000 0.0032(7) 0.000 O1 0.0206(12) 0.0339(14) 0.0223(13) -0.0001(10) -0.0007(10) -0.0030(10) O2 0.0136(11) 0.0297(13) 0.0268(13) -0.0015(10) -0.0033(9) -0.0001(10) N1 0.0175(13) 0.0284(15) 0.0114(13) -0.0057(12) -0.0016(10) 0.0029(11) N2 0.0250(15) 0.0320(16) 0.0148(14) -0.0040(12) -0.0015(11) -0.0005(13) N3 0.0156(13) 0.0289(15) 0.0214(15) 0.0040(12) -0.0041(11) 0.0008(12) C1 0.0116(14) 0.0266(17) 0.0155(17) 0.0062(14) -0.0020(12) -0.0012(13) C2 0.0204(16) 0.0237(16) 0.0150(16) 0.0017(13) -0.0025(12) -0.0003(14) C3 0.026(2) 0.044(2) 0.041(2) 0.0035(19) -0.0065(17) 0.0151(18) C4 0.0235(18) 0.032(2) 0.033(2) 0.0071(16) -0.0140(15) -0.0044(15) C5 0.0232(17) 0.0346(19) 0.0149(16) -0.0104(14) 0.0015(13) -0.0118(15) C6 0.0222(17) 0.0284(18) 0.0183(17) -0.0074(15) 0.0006(13) -0.0090(15) C7 0.0236(19) 0.035(2) 0.033(2) -0.0081(17) -0.0036(15) 0.0060(16) C8 0.024(2) 0.046(2) 0.040(2) -0.014(2) 0.0014(17) -0.0004(18) C9 0.0277(19) 0.045(2) 0.031(2) -0.0095(18) 0.0041(16) -0.0035(17) C10 0.0252(18) 0.039(2) 0.0154(17) -0.0095(15) 0.0055(13) -0.0111(16) C11 0.035(2) 0.044(2) 0.0164(17) -0.0084(16) 0.0072(15) -0.0144(17) C12 0.043(2) 0.033(2) 0.0177(18) 0.0018(15) -0.0003(15) -0.0056(17) C13 0.0262(18) 0.037(2) 0.0143(16) -0.0036(15) -0.0020(13) -0.0041(15) _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 O1 2.005(2) . ? Ru1 O1 2.005(2) 5_777 ? Ru1 N2 2.076(3) . ? Ru1 N2 2.076(3) 5_777 ? Ru1 C1 2.084(3) . ? Ru1 C1 2.084(3) 5_777 ? Mn1 O2 2.155(2) . ? Mn1 O2 2.155(2) 2_756 ? Mn1 N1 2.157(3) . ? Mn1 N1 2.157(3) 2_756 ? Mn1 Cl1 2.3821(13) . ? O1 C6 1.336(4) . ? O2 C2 1.238(4) . ? N1 C1 1.127(5) . ? N2 C13 1.300(5) . ? N2 C5 1.355(5) . ? N3 C2 1.313(4) . ? N3 C3 1.454(5) . ? N3 C4 1.455(5) . ? C2 H2 0.9300 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.413(5) . ? C5 C6 1.454(5) . ? C6 C7 1.372(5) . ? C7 C8 1.404(6) . ? C7 H7 0.9300 . ? C8 C9 1.357(7) . ? C8 H8 0.9300 . ? C9 C10 1.399(6) . ? C9 H9 0.9300 . ? C10 C11 1.427(6) . ? C11 C12 1.378(6) . ? C11 H11 0.9300 . ? C12 C13 1.418(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? 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 O1 Ru1 O1 180.000(1) . 5_777 ? O1 Ru1 N2 81.06(11) . . ? O1 Ru1 N2 98.94(11) 5_777 . ? O1 Ru1 N2 98.94(11) . 5_777 ? O1 Ru1 N2 81.06(11) 5_777 5_777 ? N2 Ru1 N2 180.00(14) . 5_777 ? O1 Ru1 C1 90.88(11) . . ? O1 Ru1 C1 89.12(11) 5_777 . ? N2 Ru1 C1 90.83(12) . . ? N2 Ru1 C1 89.17(12) 5_777 . ? O1 Ru1 C1 89.12(11) . 5_777 ? O1 Ru1 C1 90.88(11) 5_777 5_777 ? N2 Ru1 C1 89.17(12) . 5_777 ? N2 Ru1 C1 90.83(12) 5_777 5_777 ? C1 Ru1 C1 180.000(1) . 5_777 ? O2 Mn1 O2 172.24(14) . 2_756 ? O2 Mn1 N1 84.98(10) . . ? O2 Mn1 N1 91.17(10) 2_756 . ? O2 Mn1 N1 91.17(10) . 2_756 ? O2 Mn1 N1 84.98(10) 2_756 2_756 ? N1 Mn1 N1 120.60(16) . 2_756 ? O2 Mn1 Cl1 93.88(7) . . ? O2 Mn1 Cl1 93.88(7) 2_756 . ? N1 Mn1 Cl1 119.70(8) . . ? N1 Mn1 Cl1 119.70(8) 2_756 . ? C6 O1 Ru1 114.2(2) . . ? C2 O2 Mn1 128.9(2) . . ? C1 N1 Mn1 173.8(3) . . ? C13 N2 C5 119.1(3) . . ? C13 N2 Ru1 129.3(2) . . ? C5 N2 Ru1 111.5(2) . . ? C2 N3 C3 121.6(3) . . ? C2 N3 C4 121.0(3) . . ? C3 N3 C4 117.3(3) . . ? N1 C1 Ru1 178.9(3) . . ? O2 C2 N3 123.8(3) . . ? O2 C2 H2 118.1 . . ? N3 C2 H2 118.1 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C10 123.3(4) . . ? N2 C5 C6 116.1(3) . . ? C10 C5 C6 120.6(3) . . ? O1 C6 C7 125.2(4) . . ? O1 C6 C5 116.8(3) . . ? C7 C6 C5 117.9(3) . . ? C6 C7 C8 120.1(4) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 122.6(4) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C8 C9 C10 120.2(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C5 118.6(4) . . ? C9 C10 C11 124.9(3) . . ? C5 C10 C11 116.5(3) . . ? C12 C11 C10 119.1(3) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C13 119.1(4) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? N2 C13 C12 122.9(4) . . ? N2 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 66.95 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.124 _refine_diff_density_min -1.088 _refine_diff_density_rms 0.113 data_0318a_abs_corr _database_code_depnum_ccdc_archive 'CCDC 903914' #TrackingRef 'web_deposit_cif_file_0_WaiLunMan_1349106073.total.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H40 Mn N6 O6 Ru' _chemical_formula_weight 880.81 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' Mn Mn 0.3368 0.7283 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.568(4) _cell_length_b 13.049(4) _cell_length_c 13.520(3) _cell_angle_alpha 82.23(2) _cell_angle_beta 74.24(2) _cell_angle_gamma 63.88(3) _cell_volume 1915.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20780 _diffrn_reflns_av_R_equivalents 0.1525 _diffrn_reflns_av_sigmaI/netI 0.4503 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 26.24 _reflns_number_total 7382 _reflns_number_gt 2118 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7382 _refine_ls_number_parameters 434 _refine_ls_number_restraints 190 _refine_ls_R_factor_all 0.2324 _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.2155 _refine_ls_wR_factor_gt 0.1831 _refine_ls_goodness_of_fit_ref 0.751 _refine_ls_restrained_S_all 0.742 _refine_ls_shift/su_max 0.003 _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 Ru1 Ru 0.5000 0.0000 0.5000 0.0323(5) Uani 1 2 d S . . Ru2 Ru 0.0000 0.0000 0.0000 0.0302(4) Uani 1 2 d S . . Mn1 Mn 0.29269(17) -0.09206(16) 0.25350(13) 0.0272(5) Uani 1 1 d . . . O2 O 0.4027(7) -0.2123(7) 0.1638(6) 0.041(2) Uani 1 1 d . . . O3 O 0.2664(7) -0.1938(6) 0.3600(6) 0.034(2) Uani 1 1 d . . . N2 N 0.3078(9) 0.0266(8) 0.1488(6) 0.029(3) Uani 1 1 d . . . N1 N -0.0775(11) 0.1715(10) 0.0278(8) 0.0575(14) Uani 1 1 d DU . . N6 N 0.4573(13) 0.1689(11) 0.4520(8) 0.054(3) Uani 1 1 d . . . O1 O -0.1339(8) -0.0332(8) 0.0825(6) 0.0575(14) Uani 1 1 d DU . . N4 N 0.1381(9) -0.0730(8) 0.1839(7) 0.039(3) Uani 1 1 d . . . N5 N 0.4356(9) -0.0739(8) 0.3174(7) 0.038(3) Uani 1 1 d . . . N3 N 0.1778(8) 0.0415(9) 0.3391(7) 0.035(3) Uani 1 1 d . . . O4 O 0.6720(9) -0.0631(9) 0.4357(6) 0.0628(15) Uani 1 1 d U . . C13 C 0.0893(12) 0.2581(11) 0.3349(10) 0.048(4) Uani 1 1 d . . . H13A H 0.1452 0.2562 0.3732 0.058 Uiso 1 1 calc R . . H13B H 0.0144 0.2635 0.3834 0.058 Uiso 1 1 calc R . . C32 C 0.3523(11) 0.0097(12) 0.0515(9) 0.038(4) Uani 1 1 d . . . H32 H 0.3499 0.0716 0.0076 0.046 Uiso 1 1 calc R . . C25 C 0.1355(11) 0.0421(11) 0.4364(9) 0.034(3) Uani 1 1 d . . . H25 H 0.0857 0.1118 0.4686 0.041 Uiso 1 1 calc R . . C39 C -0.0007(13) 0.2182(12) -0.0266(10) 0.0575(14) Uani 1 1 d DU . . C33 C 0.0874(10) -0.0483(10) 0.1224(8) 0.025(3) Uani 1 1 d . . . C9 C 0.4586(10) -0.0431(11) 0.3785(9) 0.034(3) Uani 1 1 d . . . C17 C 0.1454(12) 0.1503(11) 0.2732(9) 0.036(3) Uani 1 1 d . . . H17 H 0.0864 0.1536 0.2367 0.043 Uiso 1 1 calc R . . C26 C 0.4253(11) -0.2052(13) 0.0608(9) 0.038(3) Uani 1 1 d . . . C19 C 0.2230(12) -0.1706(13) 0.4622(9) 0.042(3) Uani 1 1 d . . . C40 C -0.1143(13) -0.1409(12) 0.0910(10) 0.0575(14) Uani 1 1 d DU . . C14 C 0.2317(12) 0.2402(10) 0.1192(9) 0.037(3) Uani 1 1 d . . . H14A H 0.3054 0.2330 0.0679 0.045 Uiso 1 1 calc R . . H14B H 0.1727 0.2420 0.0844 0.045 Uiso 1 1 calc R . . C27 C 0.4068(11) -0.1045(12) 0.0079(8) 0.034(3) Uani 1 1 d . . . C5 C 0.3410(16) 0.2364(15) 0.4874(11) 0.0628(15) Uani 1 1 d U . . C20 C 0.1622(12) -0.0615(14) 0.4982(9) 0.040(3) Uani 1 1 d . . . C11 C 0.7274(15) -0.1771(14) 0.4490(10) 0.0628(15) Uani 1 1 d U . . C21 C 0.1194(11) -0.0460(13) 0.6071(9) 0.048(4) Uani 1 1 d . . . H21 H 0.0788 0.0272 0.6335 0.058 Uiso 1 1 calc R . . C18 C 0.2603(12) 0.1382(11) 0.1954(9) 0.044(4) Uani 1 1 d . . . H18 H 0.3191 0.1380 0.2305 0.053 Uiso 1 1 calc R . . C22 C 0.1379(12) -0.1377(15) 0.6713(10) 0.053(4) Uani 1 1 d . . . H22 H 0.1093 -0.1264 0.7418 0.064 Uiso 1 1 calc R . . C28 C 0.4873(13) -0.2020(16) -0.1499(10) 0.060(4) Uani 1 1 d . . . H28 H 0.5101 -0.2013 -0.2214 0.072 Uiso 1 1 calc R . . C23 C 0.2397(12) -0.2648(12) 0.5284(9) 0.047(4) Uani 1 1 d . . . H23 H 0.2779 -0.3381 0.5022 0.057 Uiso 1 1 calc R . . C29 C 0.4383(11) -0.1066(14) -0.1024(10) 0.053(4) Uani 1 1 d . . . H29 H 0.4232 -0.0385 -0.1400 0.064 Uiso 1 1 calc R . . C10 C 0.8544(14) -0.2531(13) 0.4060(10) 0.0628(15) Uani 1 1 d U . . H10 H 0.9066 -0.2242 0.3627 0.075 Uiso 1 1 calc R . . C4 C 0.2924(15) 0.3602(14) 0.4657(11) 0.0628(15) Uani 1 1 d U . . C38 C -0.1801(13) 0.2329(12) 0.0805(10) 0.0575(14) Uani 1 1 d DU . . H38 H -0.2308 0.1989 0.1165 0.069 Uiso 1 1 calc R . . C30 C 0.4787(12) -0.3085(13) 0.0085(9) 0.056(4) Uani 1 1 d . . . H30 H 0.4947 -0.3772 0.0451 0.067 Uiso 1 1 calc R . . C24 C 0.1986(14) -0.2486(14) 0.6350(10) 0.057(4) Uani 1 1 d . . . H24 H 0.2117 -0.3108 0.6804 0.068 Uiso 1 1 calc R . . C34 C -0.2228(13) 0.3535(12) 0.0879(10) 0.0575(14) Uani 1 1 d U . . H34 H -0.3000 0.3964 0.1277 0.069 Uiso 1 1 calc R . . C6 C 0.5338(16) 0.2084(15) 0.3962(11) 0.062(4) Uani 1 1 d . . . H6 H 0.6150 0.1593 0.3705 0.074 Uiso 1 1 calc R . . C8 C 0.3742(17) 0.3969(15) 0.4072(10) 0.058(4) Uani 1 1 d . . . H8 H 0.3465 0.4740 0.3890 0.070 Uiso 1 1 calc R . . C41 C -0.1894(14) -0.1921(15) 0.1516(12) 0.079(5) Uani 1 1 d D . . H41 H -0.2632 -0.1463 0.1944 0.095 Uiso 1 1 calc R . . C42 C -0.1569(15) -0.3091(15) 0.1496(13) 0.072(5) Uani 1 1 d D . . H42 H -0.2077 -0.3401 0.1917 0.087 Uiso 1 1 calc R . . C31 C 0.5073(13) -0.3074(15) -0.0968(11) 0.063(5) Uani 1 1 d . . . H31 H 0.5393 -0.3746 -0.1326 0.076 Uiso 1 1 calc R . . C35 C -0.1485(13) 0.4065(13) 0.0353(10) 0.0575(14) Uani 1 1 d U . . H35 H -0.1742 0.4845 0.0410 0.069 Uiso 1 1 calc R . . C12 C 0.8970(14) -0.3691(13) 0.4304(10) 0.0628(15) Uani 1 1 d U . . H12 H 0.9785 -0.4156 0.4023 0.075 Uiso 1 1 calc R . . C36 C -0.0322(14) 0.3390(11) -0.0274(10) 0.0575(14) Uani 1 1 d DU . . C15 C 0.0618(13) 0.3634(10) 0.2600(9) 0.049(4) Uani 1 1 d . . . H15A H -0.0002 0.3697 0.2268 0.059 Uiso 1 1 calc R . . H15B H 0.0317 0.4326 0.2979 0.059 Uiso 1 1 calc R . . C7 C 0.4897(18) 0.3319(16) 0.3745(11) 0.066(5) Uani 1 1 d . . . H7 H 0.5433 0.3628 0.3380 0.079 Uiso 1 1 calc R . . C16 C 0.1807(12) 0.3481(12) 0.1784(11) 0.059(4) Uani 1 1 d . . . H16A H 0.1642 0.4130 0.1310 0.071 Uiso 1 1 calc R . . H16B H 0.2408 0.3458 0.2120 0.071 Uiso 1 1 calc R . . C37 C 0.0522(17) 0.3767(16) -0.0867(12) 0.077(5) Uani 1 1 d D . . H37 H 0.0358 0.4531 -0.0830 0.093 Uiso 1 1 calc R . . C3 C 0.1729(14) 0.4197(14) 0.5072(10) 0.0628(15) Uani 1 1 d U . . H3 H 0.1365 0.4976 0.4930 0.075 Uiso 1 1 calc R . . O6 O 0.1716(13) 0.6567(12) 0.3235(9) 0.107(4) Uani 1 1 d . . . H6A H 0.2000 0.7017 0.3262 0.160 Uiso 1 1 calc R . . O5 O 0.5504(17) 0.5749(11) 0.2516(10) 0.141(6) Uani 1 1 d . . . H5 H 0.5524 0.6235 0.2066 0.211 Uiso 1 1 calc R . . C1 C 0.194(2) 0.6297(17) 0.2228(13) 0.123(8) Uani 1 1 d . . . H1A H 0.1515 0.6966 0.1856 0.184 Uiso 1 1 calc R . . H1B H 0.1674 0.5721 0.2200 0.184 Uiso 1 1 calc R . . H1C H 0.2805 0.6014 0.1925 0.184 Uiso 1 1 calc R . . C2 C 0.5775(17) 0.5979(15) 0.3375(13) 0.100(6) Uani 1 1 d . . . H2A H 0.6021 0.6594 0.3213 0.150 Uiso 1 1 calc R . . H2B H 0.6426 0.5310 0.3565 0.150 Uiso 1 1 calc R . . H2C H 0.5065 0.6191 0.3937 0.150 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 Ru1 0.0296(10) 0.0450(11) 0.0219(9) -0.0012(8) -0.0164(7) -0.0092(9) Ru2 0.0366(10) 0.0414(10) 0.0152(8) 0.0038(7) -0.0150(7) -0.0149(9) Mn1 0.0316(12) 0.0376(12) 0.0136(10) 0.0012(9) -0.0099(8) -0.0135(10) O2 0.043(6) 0.065(6) 0.017(5) -0.005(4) -0.014(4) -0.019(5) O3 0.053(6) 0.038(5) 0.021(5) 0.010(4) -0.022(4) -0.023(5) N2 0.042(7) 0.045(7) 0.008(5) -0.008(5) -0.008(5) -0.021(6) N1 0.067(4) 0.075(4) 0.044(3) 0.000(3) -0.042(3) -0.026(3) N6 0.070(10) 0.090(10) 0.025(7) 0.003(7) -0.034(6) -0.043(9) O1 0.067(4) 0.075(4) 0.044(3) 0.000(3) -0.042(3) -0.026(3) N4 0.056(7) 0.047(7) 0.022(6) 0.010(5) -0.023(5) -0.024(6) N5 0.033(6) 0.051(7) 0.030(6) -0.002(5) -0.019(5) -0.011(6) N3 0.031(6) 0.073(8) 0.009(5) 0.016(5) -0.013(5) -0.027(6) O4 0.071(4) 0.091(4) 0.039(3) 0.003(3) -0.036(3) -0.033(4) C13 0.033(9) 0.065(10) 0.047(9) -0.003(8) -0.006(7) -0.024(8) C32 0.031(8) 0.079(11) 0.017(7) 0.022(7) -0.017(6) -0.033(8) C25 0.026(7) 0.060(10) 0.023(7) 0.003(7) -0.012(6) -0.021(7) C39 0.067(4) 0.075(4) 0.044(3) 0.000(3) -0.042(3) -0.026(3) C33 0.032(7) 0.038(8) 0.012(6) -0.008(6) 0.000(5) -0.021(7) C9 0.027(7) 0.051(9) 0.022(7) 0.004(6) -0.017(6) -0.011(7) C17 0.051(9) 0.056(9) 0.026(7) 0.010(7) -0.031(7) -0.035(8) C26 0.033(8) 0.079(11) 0.014(6) -0.014(7) -0.003(6) -0.030(8) C19 0.043(9) 0.067(10) 0.019(7) 0.006(7) -0.019(6) -0.022(8) C40 0.067(4) 0.075(4) 0.044(3) 0.000(3) -0.042(3) -0.026(3) C14 0.059(10) 0.029(8) 0.019(7) 0.005(6) -0.012(6) -0.014(7) C27 0.043(8) 0.063(10) 0.011(6) -0.004(7) 0.001(6) -0.039(8) C5 0.071(4) 0.091(4) 0.039(3) 0.003(3) -0.036(3) -0.033(4) C20 0.037(8) 0.085(11) 0.009(6) 0.001(7) -0.004(6) -0.038(9) C11 0.071(4) 0.091(4) 0.039(3) 0.003(3) -0.036(3) -0.033(4) C21 0.041(9) 0.094(12) 0.017(7) 0.001(8) -0.006(6) -0.036(9) C18 0.041(9) 0.061(10) 0.025(7) -0.024(7) 0.024(7) -0.029(8) C22 0.052(10) 0.099(13) 0.032(8) 0.011(9) -0.017(7) -0.052(10) C28 0.064(11) 0.107(14) 0.015(7) -0.008(9) 0.000(7) -0.045(11) C23 0.070(10) 0.051(9) 0.029(8) 0.007(7) -0.020(7) -0.030(8) C29 0.036(9) 0.081(12) 0.035(8) -0.024(8) -0.007(7) -0.013(9) C10 0.071(4) 0.091(4) 0.039(3) 0.003(3) -0.036(3) -0.033(4) C4 0.071(4) 0.091(4) 0.039(3) 0.003(3) -0.036(3) -0.033(4) C38 0.067(4) 0.075(4) 0.044(3) 0.000(3) -0.042(3) -0.026(3) C30 0.067(10) 0.074(11) 0.023(7) -0.017(7) -0.005(7) -0.026(9) C24 0.088(12) 0.077(12) 0.033(8) 0.026(8) -0.035(8) -0.054(11) C34 0.067(4) 0.075(4) 0.044(3) 0.000(3) -0.042(3) -0.026(3) C6 0.079(13) 0.080(14) 0.035(9) -0.015(9) -0.041(9) -0.021(11) C8 0.082(12) 0.082(12) 0.026(8) 0.011(8) -0.032(8) -0.042(12) C41 0.063(11) 0.110(15) 0.098(14) 0.041(11) -0.048(10) -0.063(12) C42 0.043(11) 0.104(15) 0.061(11) 0.045(11) -0.016(9) -0.035(11) C31 0.048(10) 0.101(14) 0.047(10) -0.056(10) -0.001(8) -0.029(10) C35 0.067(4) 0.075(4) 0.044(3) 0.000(3) -0.042(3) -0.026(3) C12 0.071(4) 0.091(4) 0.039(3) 0.003(3) -0.036(3) -0.033(4) C36 0.067(4) 0.075(4) 0.044(3) 0.000(3) -0.042(3) -0.026(3) C15 0.070(11) 0.030(8) 0.039(8) -0.002(7) -0.022(8) -0.009(8) C7 0.082(14) 0.085(14) 0.044(10) -0.003(9) -0.033(9) -0.035(12) C16 0.049(10) 0.063(11) 0.054(10) 0.020(9) -0.009(8) -0.020(9) C37 0.096(14) 0.130(16) 0.060(11) 0.032(11) -0.056(10) -0.084(14) C3 0.071(4) 0.091(4) 0.039(3) 0.003(3) -0.036(3) -0.033(4) O6 0.147(12) 0.145(12) 0.094(10) 0.032(8) -0.058(9) -0.113(10) O5 0.185(15) 0.090(10) 0.086(10) -0.002(8) -0.075(11) 0.019(10) C1 0.23(2) 0.16(2) 0.060(12) 0.029(12) -0.087(14) -0.13(2) C2 0.127(17) 0.120(16) 0.068(12) -0.001(11) -0.058(12) -0.044(14) _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 O4 1.926(9) 2_656 ? Ru1 O4 1.926(9) . ? Ru1 C9 2.063(12) 2_656 ? Ru1 C9 2.063(12) . ? Ru1 N6 2.080(13) 2_656 ? Ru1 N6 2.080(13) . ? Ru2 O1 1.938(9) . ? Ru2 O1 1.938(9) 2 ? Ru2 N1 2.051(12) . ? Ru2 N1 2.051(12) 2 ? Ru2 C33 2.106(12) . ? Ru2 C33 2.106(12) 2 ? Mn1 O2 1.881(8) . ? Mn1 O3 1.885(7) . ? Mn1 N3 1.970(10) . ? Mn1 N2 1.990(9) . ? Mn1 N4 2.286(10) . ? Mn1 N5 2.302(10) . ? O2 C26 1.343(12) . ? O3 C19 1.362(13) . ? N2 C32 1.289(13) . ? N2 C18 1.467(14) . ? N1 C38 1.248(12) . ? N1 C39 1.363(13) . ? N6 C6 1.302(16) . ? N6 C5 1.320(18) . ? O1 C40 1.311(12) . ? N4 C33 1.113(13) . ? N5 C9 1.118(13) . ? N3 C25 1.278(13) . ? N3 C17 1.524(14) . ? O4 C11 1.347(17) . ? C13 C17 1.515(16) . ? C13 C15 1.558(17) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C32 C27 1.468(17) . ? C32 H32 0.9300 . ? C25 C20 1.444(17) . ? C25 H25 0.9300 . ? C39 C36 1.445(14) . ? C39 C40 1.461(18) 2 ? C17 C18 1.495(15) . ? C17 H17 0.9800 . ? C26 C27 1.363(17) . ? C26 C30 1.403(17) . ? C19 C20 1.369(17) . ? C19 C23 1.391(16) . ? C40 C41 1.413(13) . ? C40 C39 1.461(18) 2 ? C14 C16 1.504(16) . ? C14 C18 1.539(16) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C27 C29 1.436(16) . ? C5 C11 1.442(19) 2_656 ? C5 C4 1.47(2) . ? C20 C21 1.433(15) . ? C11 C5 1.442(19) 2_656 ? C11 C10 1.46(2) . ? C21 C22 1.351(17) . ? C21 H21 0.9300 . ? C18 H18 0.9800 . ? C22 C24 1.390(18) . ? C22 H22 0.9300 . ? C28 C29 1.292(17) . ? C28 C31 1.413(19) . ? C28 H28 0.9300 . ? C23 C24 1.404(16) . ? C23 H23 0.9300 . ? C29 H29 0.9300 . ? C10 C12 1.390(18) . ? C10 H10 0.9300 . ? C4 C8 1.342(18) . ? C4 C3 1.344(19) . ? C38 C34 1.429(18) . ? C38 H38 0.9300 . ? C30 C31 1.370(17) . ? C30 H30 0.9300 . ? C24 H24 0.9300 . ? C34 C35 1.389(16) . ? C34 H34 0.9300 . ? C6 C7 1.47(2) . ? C6 H6 0.9300 . ? C8 C7 1.300(19) . ? C8 H8 0.9300 . ? C41 C42 1.397(15) . ? C41 H41 0.9300 . ? C42 C37 1.344(19) 2 ? C42 H42 0.9300 . ? C31 H31 0.9300 . ? C35 C36 1.423(18) . ? C35 H35 0.9300 . ? C12 C3 1.369(17) 2_656 ? C12 H12 0.9300 . ? C36 C37 1.379(13) . ? C15 C16 1.547(16) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C7 H7 0.9300 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C37 C42 1.344(19) 2 ? C37 H37 0.9300 . ? C3 C12 1.369(17) 2_656 ? C3 H3 0.9300 . ? O6 C1 1.374(17) . ? O6 H6A 0.8200 . ? O5 C2 1.399(18) . ? O5 H5 0.8200 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 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 O4 Ru1 O4 180.000(1) 2_656 . ? O4 Ru1 C9 92.5(4) 2_656 2_656 ? O4 Ru1 C9 87.5(4) . 2_656 ? O4 Ru1 C9 87.5(4) 2_656 . ? O4 Ru1 C9 92.5(4) . . ? C9 Ru1 C9 180.000(1) 2_656 . ? O4 Ru1 N6 98.0(5) 2_656 2_656 ? O4 Ru1 N6 82.0(5) . 2_656 ? C9 Ru1 N6 95.0(4) 2_656 2_656 ? C9 Ru1 N6 85.0(4) . 2_656 ? O4 Ru1 N6 82.0(5) 2_656 . ? O4 Ru1 N6 98.0(5) . . ? C9 Ru1 N6 85.0(4) 2_656 . ? C9 Ru1 N6 95.0(4) . . ? N6 Ru1 N6 180.0(6) 2_656 . ? O1 Ru2 O1 180.0(7) . 2 ? O1 Ru2 N1 97.7(4) . . ? O1 Ru2 N1 82.3(4) 2 . ? O1 Ru2 N1 82.3(4) . 2 ? O1 Ru2 N1 97.7(4) 2 2 ? N1 Ru2 N1 180.0(7) . 2 ? O1 Ru2 C33 91.2(4) . . ? O1 Ru2 C33 88.8(4) 2 . ? N1 Ru2 C33 94.8(4) . . ? N1 Ru2 C33 85.2(4) 2 . ? O1 Ru2 C33 88.8(4) . 2 ? O1 Ru2 C33 91.2(4) 2 2 ? N1 Ru2 C33 85.2(4) . 2 ? N1 Ru2 C33 94.8(4) 2 2 ? C33 Ru2 C33 180.0(6) . 2 ? O2 Mn1 O3 92.2(3) . . ? O2 Mn1 N3 175.9(4) . . ? O3 Mn1 N3 91.8(4) . . ? O2 Mn1 N2 92.8(4) . . ? O3 Mn1 N2 174.8(4) . . ? N3 Mn1 N2 83.1(4) . . ? O2 Mn1 N4 89.9(4) . . ? O3 Mn1 N4 95.3(3) . . ? N3 Mn1 N4 89.0(4) . . ? N2 Mn1 N4 83.7(4) . . ? O2 Mn1 N5 96.9(4) . . ? O3 Mn1 N5 93.1(3) . . ? N3 Mn1 N5 83.5(4) . . ? N2 Mn1 N5 87.3(4) . . ? N4 Mn1 N5 168.9(4) . . ? C26 O2 Mn1 125.4(9) . . ? C19 O3 Mn1 126.2(8) . . ? C32 N2 C18 123.2(11) . . ? C32 N2 Mn1 125.1(9) . . ? C18 N2 Mn1 111.7(7) . . ? C38 N1 C39 120.5(14) . . ? C38 N1 Ru2 129.9(11) . . ? C39 N1 Ru2 109.6(9) . . ? C6 N6 C5 121.7(15) . . ? C6 N6 Ru1 126.0(11) . . ? C5 N6 Ru1 112.3(11) . . ? C40 O1 Ru2 116.2(9) . . ? C33 N4 Mn1 154.2(9) . . ? C9 N5 Mn1 149.6(10) . . ? C25 N3 C17 122.4(11) . . ? C25 N3 Mn1 127.1(9) . . ? C17 N3 Mn1 110.5(7) . . ? C11 O4 Ru1 112.7(9) . . ? C17 C13 C15 109.0(11) . . ? C17 C13 H13A 109.9 . . ? C15 C13 H13A 109.9 . . ? C17 C13 H13B 109.9 . . ? C15 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N2 C32 C27 122.0(11) . . ? N2 C32 H32 119.0 . . ? C27 C32 H32 119.0 . . ? N3 C25 C20 122.3(12) . . ? N3 C25 H25 118.9 . . ? C20 C25 H25 118.9 . . ? N1 C39 C36 122.9(13) . . ? N1 C39 C40 116.6(12) . 2 ? C36 C39 C40 120.4(13) . 2 ? N4 C33 Ru2 176.6(10) . . ? N5 C9 Ru1 174.4(11) . . ? C18 C17 C13 112.4(9) . . ? C18 C17 N3 106.3(11) . . ? C13 C17 N3 113.4(10) . . ? C18 C17 H17 108.2 . . ? C13 C17 H17 108.2 . . ? N3 C17 H17 108.2 . . ? O2 C26 C27 122.4(12) . . ? O2 C26 C30 116.7(12) . . ? C27 C26 C30 120.7(11) . . ? O3 C19 C20 122.5(11) . . ? O3 C19 C23 115.9(12) . . ? C20 C19 C23 121.6(12) . . ? O1 C40 C41 129.3(14) . . ? O1 C40 C39 114.9(12) . 2 ? C41 C40 C39 115.8(13) . 2 ? C16 C14 C18 108.4(10) . . ? C16 C14 H14A 110.0 . . ? C18 C14 H14A 110.0 . . ? C16 C14 H14B 110.0 . . ? C18 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? C26 C27 C29 118.2(12) . . ? C26 C27 C32 126.9(11) . . ? C29 C27 C32 114.8(12) . . ? N6 C5 C11 113.2(16) . 2_656 ? N6 C5 C4 121.2(15) . . ? C11 C5 C4 125.6(16) 2_656 . ? C19 C20 C21 118.3(13) . . ? C19 C20 C25 126.2(11) . . ? C21 C20 C25 115.5(13) . . ? O4 C11 C5 119.7(14) . 2_656 ? O4 C11 C10 127.4(14) . . ? C5 C11 C10 112.9(15) 2_656 . ? C22 C21 C20 120.0(14) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? N2 C18 C17 105.6(9) . . ? N2 C18 C14 114.6(10) . . ? C17 C18 C14 109.2(11) . . ? N2 C18 H18 109.1 . . ? C17 C18 H18 109.1 . . ? C14 C18 H18 109.1 . . ? C21 C22 C24 121.8(13) . . ? C21 C22 H22 119.1 . . ? C24 C22 H22 119.1 . . ? C29 C28 C31 122.0(13) . . ? C29 C28 H28 119.0 . . ? C31 C28 H28 119.0 . . ? C19 C23 C24 119.6(13) . . ? C19 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C28 C29 C27 120.7(15) . . ? C28 C29 H29 119.7 . . ? C27 C29 H29 119.7 . . ? C12 C10 C11 119.5(15) . . ? C12 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C8 C4 C3 129.6(18) . . ? C8 C4 C5 115.1(16) . . ? C3 C4 C5 115.4(16) . . ? N1 C38 C34 122.8(15) . . ? N1 C38 H38 118.6 . . ? C34 C38 H38 118.6 . . ? C31 C30 C26 119.5(14) . . ? C31 C30 H30 120.2 . . ? C26 C30 H30 120.2 . . ? C22 C24 C23 118.7(12) . . ? C22 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C35 C34 C38 119.8(14) . . ? C35 C34 H34 120.1 . . ? C38 C34 H34 120.1 . . ? N6 C6 C7 119.0(15) . . ? N6 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C7 C8 C4 124.3(18) . . ? C7 C8 H8 117.8 . . ? C4 C8 H8 117.8 . . ? C42 C41 C40 122.3(15) . . ? C42 C41 H41 118.8 . . ? C40 C41 H41 118.8 . . ? C37 C42 C41 120.1(15) 2 . ? C37 C42 H42 120.0 2 . ? C41 C42 H42 120.0 . . ? C30 C31 C28 118.7(13) . . ? C30 C31 H31 120.6 . . ? C28 C31 H31 120.6 . . ? C34 C35 C36 118.7(14) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C3 C12 C10 124.5(15) 2_656 . ? C3 C12 H12 117.7 2_656 . ? C10 C12 H12 117.7 . . ? C37 C36 C35 126.9(15) . . ? C37 C36 C39 117.7(14) . . ? C35 C36 C39 115.4(13) . . ? C16 C15 C13 108.8(11) . . ? C16 C15 H15A 109.9 . . ? C13 C15 H15A 109.9 . . ? C16 C15 H15B 109.9 . . ? C13 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C8 C7 C6 118.7(16) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C14 C16 C15 111.5(11) . . ? C14 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? C14 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C42 C37 C36 123.5(16) 2 . ? C42 C37 H37 118.3 2 . ? C36 C37 H37 118.3 . . ? C4 C3 C12 122.0(17) . 2_656 ? C4 C3 H3 119.0 . . ? C12 C3 H3 119.0 2_656 . ? C1 O6 H6A 109.5 . . ? C2 O5 H5 109.5 . . ? O6 C1 H1A 109.5 . . ? O6 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O6 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O5 C2 H2A 109.5 . . ? O5 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O5 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 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 O3 Mn1 O2 C26 153.1(9) . . . . ? N3 Mn1 O2 C26 -18(6) . . . . ? N2 Mn1 O2 C26 -26.0(9) . . . . ? N4 Mn1 O2 C26 57.7(9) . . . . ? N5 Mn1 O2 C26 -113.6(9) . . . . ? O2 Mn1 O3 C19 158.9(9) . . . . ? N3 Mn1 O3 C19 -21.7(9) . . . . ? N2 Mn1 O3 C19 -32(4) . . . . ? N4 Mn1 O3 C19 -110.9(9) . . . . ? N5 Mn1 O3 C19 61.9(9) . . . . ? O2 Mn1 N2 C32 16.5(10) . . . . ? O3 Mn1 N2 C32 -153(4) . . . . ? N3 Mn1 N2 C32 -162.9(10) . . . . ? N4 Mn1 N2 C32 -73.1(10) . . . . ? N5 Mn1 N2 C32 113.3(10) . . . . ? O2 Mn1 N2 C18 -164.2(8) . . . . ? O3 Mn1 N2 C18 26(4) . . . . ? N3 Mn1 N2 C18 16.4(8) . . . . ? N4 Mn1 N2 C18 106.1(8) . . . . ? N5 Mn1 N2 C18 -67.4(8) . . . . ? O1 Ru2 N1 C38 -1.1(12) . . . . ? O1 Ru2 N1 C38 178.9(12) 2 . . . ? N1 Ru2 N1 C38 100(100) 2 . . . ? C33 Ru2 N1 C38 -92.9(12) . . . . ? C33 Ru2 N1 C38 87.1(12) 2 . . . ? O1 Ru2 N1 C39 -177.7(8) . . . . ? O1 Ru2 N1 C39 2.3(8) 2 . . . ? N1 Ru2 N1 C39 -77(100) 2 . . . ? C33 Ru2 N1 C39 90.4(8) . . . . ? C33 Ru2 N1 C39 -89.6(8) 2 . . . ? O4 Ru1 N6 C6 179.3(10) 2_656 . . . ? O4 Ru1 N6 C6 -0.7(10) . . . . ? C9 Ru1 N6 C6 86.1(10) 2_656 . . . ? C9 Ru1 N6 C6 -93.9(10) . . . . ? N6 Ru1 N6 C6 -13(100) 2_656 . . . ? O4 Ru1 N6 C5 1.3(9) 2_656 . . . ? O4 Ru1 N6 C5 -178.7(9) . . . . ? C9 Ru1 N6 C5 -91.9(9) 2_656 . . . ? C9 Ru1 N6 C5 88.1(9) . . . . ? N6 Ru1 N6 C5 169(100) 2_656 . . . ? O1 Ru2 O1 C40 66(100) 2 . . . ? N1 Ru2 O1 C40 -174.7(8) . . . . ? N1 Ru2 O1 C40 5.3(8) 2 . . . ? C33 Ru2 O1 C40 -79.6(8) . . . . ? C33 Ru2 O1 C40 100.4(8) 2 . . . ? O2 Mn1 N4 C33 -72(2) . . . . ? O3 Mn1 N4 C33 -164(2) . . . . ? N3 Mn1 N4 C33 104(2) . . . . ? N2 Mn1 N4 C33 21(2) . . . . ? N5 Mn1 N4 C33 56(3) . . . . ? O2 Mn1 N5 C9 -160.5(19) . . . . ? O3 Mn1 N5 C9 -67.9(19) . . . . ? N3 Mn1 N5 C9 23.6(19) . . . . ? N2 Mn1 N5 C9 106.9(19) . . . . ? N4 Mn1 N5 C9 71(3) . . . . ? O2 Mn1 N3 C25 -174(5) . . . . ? O3 Mn1 N3 C25 15.1(10) . . . . ? N2 Mn1 N3 C25 -165.8(10) . . . . ? N4 Mn1 N3 C25 110.4(10) . . . . ? N5 Mn1 N3 C25 -77.8(10) . . . . ? O2 Mn1 N3 C17 5(6) . . . . ? O3 Mn1 N3 C17 -166.2(7) . . . . ? N2 Mn1 N3 C17 12.9(7) . . . . ? N4 Mn1 N3 C17 -70.9(7) . . . . ? N5 Mn1 N3 C17 100.9(7) . . . . ? O4 Ru1 O4 C11 88(100) 2_656 . . . ? C9 Ru1 O4 C11 98.4(8) 2_656 . . . ? C9 Ru1 O4 C11 -81.6(8) . . . . ? N6 Ru1 O4 C11 3.0(8) 2_656 . . . ? N6 Ru1 O4 C11 -177.0(8) . . . . ? C18 N2 C32 C27 175.8(11) . . . . ? Mn1 N2 C32 C27 -5.0(15) . . . . ? C17 N3 C25 C20 177.3(10) . . . . ? Mn1 N3 C25 C20 -4.1(16) . . . . ? C38 N1 C39 C36 -0.4(19) . . . . ? Ru2 N1 C39 C36 176.6(9) . . . . ? C38 N1 C39 C40 -176.3(12) . . . 2 ? Ru2 N1 C39 C40 0.7(13) . . . 2 ? Mn1 N4 C33 Ru2 10(21) . . . . ? O1 Ru2 C33 N4 176(19) . . . . ? O1 Ru2 C33 N4 -4(19) 2 . . . ? N1 Ru2 C33 N4 -86(19) . . . . ? N1 Ru2 C33 N4 94(19) 2 . . . ? C33 Ru2 C33 N4 25(100) 2 . . . ? Mn1 N5 C9 Ru1 78(12) . . . . ? O4 Ru1 C9 N5 -80(11) 2_656 . . . ? O4 Ru1 C9 N5 100(11) . . . . ? C9 Ru1 C9 N5 -48(100) 2_656 . . . ? N6 Ru1 C9 N5 19(11) 2_656 . . . ? N6 Ru1 C9 N5 -161(11) . . . . ? C15 C13 C17 C18 58.5(14) . . . . ? C15 C13 C17 N3 179.1(9) . . . . ? C25 N3 C17 C18 139.9(11) . . . . ? Mn1 N3 C17 C18 -38.8(10) . . . . ? C25 N3 C17 C13 15.9(15) . . . . ? Mn1 N3 C17 C13 -162.9(8) . . . . ? Mn1 O2 C26 C27 24.5(15) . . . . ? Mn1 O2 C26 C30 -160.6(9) . . . . ? Mn1 O3 C19 C20 18.2(16) . . . . ? Mn1 O3 C19 C23 -164.3(8) . . . . ? Ru2 O1 C40 C41 174.5(11) . . . . ? Ru2 O1 C40 C39 -7.1(13) . . . 2 ? O2 C26 C27 C29 177.6(10) . . . . ? C30 C26 C27 C29 2.8(18) . . . . ? O2 C26 C27 C32 -5(2) . . . . ? C30 C26 C27 C32 -179.9(11) . . . . ? N2 C32 C27 C26 -4.6(19) . . . . ? N2 C32 C27 C29 172.7(11) . . . . ? C6 N6 C5 C11 -177.6(11) . . . 2_656 ? Ru1 N6 C5 C11 0.5(14) . . . 2_656 ? C6 N6 C5 C4 -0.3(19) . . . . ? Ru1 N6 C5 C4 177.8(9) . . . . ? O3 C19 C20 C21 179.6(10) . . . . ? C23 C19 C20 C21 2.2(19) . . . . ? O3 C19 C20 C25 0(2) . . . . ? C23 C19 C20 C25 -177.4(11) . . . . ? N3 C25 C20 C19 -7(2) . . . . ? N3 C25 C20 C21 173.3(10) . . . . ? Ru1 O4 C11 C5 -4.3(14) . . . 2_656 ? Ru1 O4 C11 C10 176.1(11) . . . . ? C19 C20 C21 C22 -0.9(18) . . . . ? C25 C20 C21 C22 178.8(11) . . . . ? C32 N2 C18 C17 137.6(11) . . . . ? Mn1 N2 C18 C17 -41.7(12) . . . . ? C32 N2 C18 C14 17.4(17) . . . . ? Mn1 N2 C18 C14 -161.9(8) . . . . ? C13 C17 C18 N2 175.5(10) . . . . ? N3 C17 C18 N2 50.9(12) . . . . ? C13 C17 C18 C14 -60.8(14) . . . . ? N3 C17 C18 C14 174.5(9) . . . . ? C16 C14 C18 N2 178.4(9) . . . . ? C16 C14 C18 C17 60.2(14) . . . . ? C20 C21 C22 C24 0.3(19) . . . . ? O3 C19 C23 C24 179.5(11) . . . . ? C20 C19 C23 C24 -3(2) . . . . ? C31 C28 C29 C27 3(2) . . . . ? C26 C27 C29 C28 -2.7(19) . . . . ? C32 C27 C29 C28 179.7(12) . . . . ? O4 C11 C10 C12 178.3(11) . . . . ? C5 C11 C10 C12 -1.3(17) 2_656 . . . ? N6 C5 C4 C8 0.9(18) . . . . ? C11 C5 C4 C8 177.7(12) 2_656 . . . ? N6 C5 C4 C3 -179.2(13) . . . . ? C11 C5 C4 C3 -2.3(19) 2_656 . . . ? C39 N1 C38 C34 -0.4(19) . . . . ? Ru2 N1 C38 C34 -176.7(8) . . . . ? O2 C26 C30 C31 -178.1(11) . . . . ? C27 C26 C30 C31 -3.1(19) . . . . ? C21 C22 C24 C23 -1(2) . . . . ? C19 C23 C24 C22 2.3(19) . . . . ? N1 C38 C34 C35 -0.4(19) . . . . ? C5 N6 C6 C7 1.6(18) . . . . ? Ru1 N6 C6 C7 -176.2(8) . . . . ? C3 C4 C8 C7 177.1(15) . . . . ? C5 C4 C8 C7 -3(2) . . . . ? O1 C40 C41 C42 177.8(14) . . . . ? C39 C40 C41 C42 -1(2) 2 . . . ? C40 C41 C42 C37 -2(2) . . . 2 ? C26 C30 C31 C28 3(2) . . . . ? C29 C28 C31 C30 -3(2) . . . . ? C38 C34 C35 C36 1.9(17) . . . . ? C11 C10 C12 C3 0.4(19) . . . 2_656 ? C34 C35 C36 C37 178.4(12) . . . . ? C34 C35 C36 C39 -2.5(17) . . . . ? N1 C39 C36 C37 -179.0(11) . . . . ? C40 C39 C36 C37 -3.2(18) 2 . . . ? N1 C39 C36 C35 1.8(18) . . . . ? C40 C39 C36 C35 177.7(11) 2 . . . ? C17 C13 C15 C16 -55.2(14) . . . . ? C4 C8 C7 C6 4(2) . . . . ? N6 C6 C7 C8 -3.5(19) . . . . ? C18 C14 C16 C15 -60.5(15) . . . . ? C13 C15 C16 C14 58.5(15) . . . . ? C35 C36 C37 C42 -175.3(14) . . . 2 ? C39 C36 C37 C42 6(2) . . . 2 ? C8 C4 C3 C12 -176.8(13) . . . 2_656 ? C5 C4 C3 C12 3.3(19) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 26.24 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 2.743 _refine_diff_density_min -1.397 _refine_diff_density_rms 0.161 data_wy2044wm _database_code_depnum_ccdc_archive 'CCDC 903915' #TrackingRef 'web_deposit_cif_file_0_WaiLunMan_1349106073.total.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H44 Cu N12 O8 Ru2' _chemical_formula_weight 1254.69 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' Cu Cu 0.3201 1.2651 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9277(12) _cell_length_b 20.948(3) _cell_length_c 15.023(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.175(2) _cell_angle_gamma 90.00 _cell_volume 2723.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1266 _exptl_absorpt_coefficient_mu 0.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8003 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _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_type 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13104 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4741 _reflns_number_gt 3218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+1.6192P] 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 4741 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.2074 _refine_ls_wR_factor_gt 0.1868 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4888(8) 0.1633(3) 0.9335(5) 0.0272(16) Uani 1 1 d . . . C2 C 0.6047(9) 0.3199(4) 0.7935(6) 0.0360(18) Uani 1 1 d . . . C3 C 0.2264(11) 0.2388(4) 0.7313(7) 0.048(2) Uani 1 1 d . . . H3A H 0.2693 0.2104 0.6969 0.057 Uiso 1 1 calc R . . C4 C 0.0630(13) 0.2578(5) 0.6975(7) 0.060(3) Uani 1 1 d . . . H4A H 0.0052 0.2422 0.6417 0.072 Uiso 1 1 calc R . . C5 C -0.0034(11) 0.2983(4) 0.7480(6) 0.048(2) Uani 1 1 d . . . H5A H -0.1065 0.3106 0.7291 0.058 Uiso 1 1 calc R . . C6 C 0.0970(10) 0.3207(4) 0.8328(7) 0.048(2) Uani 1 1 d . . . C7 C 0.2523(11) 0.3013(4) 0.8571(7) 0.051(2) Uani 1 1 d . . . C8 C 0.3554(10) 0.3242(4) 0.9427(6) 0.043(2) Uani 1 1 d . . . C9 C 0.2970(15) 0.3663(5) 0.9932(8) 0.067(3) Uani 1 1 d . . . H9A H 0.3613 0.3820 1.0471 0.081 Uiso 1 1 calc R . . C10 C 0.1481(14) 0.3868(6) 0.9686(8) 0.070(3) Uani 1 1 d . . . H10A H 0.1126 0.4166 1.0045 0.084 Uiso 1 1 calc R . . C11 C 0.0530(13) 0.3640(5) 0.8925(7) 0.061(3) Uani 1 1 d . . . H11A H -0.0491 0.3777 0.8782 0.073 Uiso 1 1 calc R . . C12 C 0.8531(10) 0.2489(4) 1.0042(6) 0.042(2) Uani 1 1 d . . . H12A H 0.8032 0.2750 1.0379 0.050 Uiso 1 1 calc R . . C13 C 1.0201(16) 0.2347(5) 1.0437(8) 0.076(4) Uani 1 1 d . . . H13A H 1.0745 0.2513 1.0997 0.091 Uiso 1 1 calc R . . C14 C 1.0900(12) 0.1941(4) 0.9900(7) 0.055(3) Uani 1 1 d . . . H14A H 1.1935 0.1828 1.0097 0.066 Uiso 1 1 calc R . . C15 C 0.9990(8) 0.1718(4) 0.9070(6) 0.0364(19) Uani 1 1 d . . . C16 C 0.8405(12) 0.1900(4) 0.8778(7) 0.053(3) Uani 1 1 d . . . C17 C 0.7447(9) 0.1644(4) 0.7916(6) 0.043(2) Uani 1 1 d . . . C18 C 0.8059(13) 0.1250(5) 0.7395(8) 0.065(3) Uani 1 1 d . . . H18A H 0.7444 0.1076 0.6860 0.078 Uiso 1 1 calc R . . C19 C 0.9611(13) 0.1106(5) 0.7667(7) 0.061(3) Uani 1 1 d . . . H19A H 1.0042 0.0851 0.7287 0.073 Uiso 1 1 calc R . . C20 C 1.0523(11) 0.1320(4) 0.8458(7) 0.049(2) Uani 1 1 d . . . H20A H 1.1557 0.1200 0.8608 0.059 Uiso 1 1 calc R . . C21 C 0.8245(10) 0.0510(4) 0.0380(7) 0.052(2) Uani 1 1 d . . . H21A H 0.7854 0.0927 0.0152 0.063 Uiso 1 1 calc R . . H21B H 0.9268 0.0461 0.0275 0.063 Uiso 1 1 calc R . . C22 C 0.8347(10) 0.0473(4) 0.1380(7) 0.053(3) Uani 1 1 d . . . H22A H 0.9195 0.0741 0.1699 0.063 Uiso 1 1 calc R . . H22B H 0.8596 0.0037 0.1580 0.063 Uiso 1 1 calc R . . C23 C 0.6891(11) 0.0673(4) 0.1670(6) 0.050(2) Uani 1 1 d . . . H23A H 0.7124 0.0705 0.2334 0.061 Uiso 1 1 calc R . . H23B H 0.6568 0.1091 0.1418 0.061 Uiso 1 1 calc R . . C24 C 0.4166(11) 0.0412(4) 0.1596(6) 0.049(2) Uani 1 1 d . . . H24A H 0.4305 0.0392 0.2257 0.059 Uiso 1 1 calc R . . H24B H 0.3920 0.0848 0.1399 0.059 Uiso 1 1 calc R . . C25 C 0.2918(10) -0.0014(4) 0.1143(6) 0.049(2) Uani 1 1 d . . . H25A H 0.1953 0.0127 0.1266 0.059 Uiso 1 1 calc R . . H25B H 0.3129 -0.0443 0.1382 0.059 Uiso 1 1 calc R . . C26 C 0.3520(19) 0.0673(7) 0.6398(8) 0.103(5) Uani 1 1 d . . . C27 C 0.7010(14) 0.4791(5) 0.8480(8) 0.063(3) Uani 1 1 d . . . Cu1 Cu 0.5000 0.0000 0.0000 0.0316(4) Uani 1 2 d S . . N1 N 0.4606(7) 0.1170(3) 0.9665(4) 0.0371(16) Uani 1 1 d . . . N2 N 0.6415(9) 0.3622(4) 0.7566(5) 0.052(2) Uani 1 1 d . . . N3 N 0.3105(11) 0.2606(4) 0.8070(6) 0.055(2) Uani 1 1 d . . . N4 N 0.7744(9) 0.2278(3) 0.9275(5) 0.0489(19) Uani 1 1 d . . . N5 N 0.7224(8) 0.0014(3) -0.0119(5) 0.0409(17) Uani 1 1 d . . . N6 N 0.5590(8) 0.0206(3) 0.1349(5) 0.0422(17) Uani 1 1 d . . . O1 O 0.4995(8) 0.3018(3) 0.9608(5) 0.0582(17) Uani 1 1 d . . . O2 O 0.5943(7) 0.1837(3) 0.7715(4) 0.0531(16) Uani 1 1 d . . . O3 O 0.3756(8) 0.0854(3) 0.7326(4) 0.0565(17) Uani 1 1 d . . . O4 O 0.610(2) 0.4679(7) 0.9057(11) 0.214(8) Uani 1 1 d . . . Ru1 Ru 0.54515(7) 0.24313(3) 0.86640(4) 0.0298(2) Uani 1 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 C1 0.022(4) 0.030(4) 0.030(4) 0.003(3) 0.006(3) -0.001(3) C2 0.026(4) 0.030(4) 0.051(5) 0.008(4) 0.008(4) 0.001(3) C3 0.056(6) 0.039(5) 0.058(6) 0.015(4) 0.034(5) 0.009(4) C4 0.075(8) 0.051(6) 0.055(6) 0.015(5) 0.017(5) -0.018(5) C5 0.044(5) 0.043(5) 0.064(6) 0.025(5) 0.027(5) 0.008(4) C6 0.030(5) 0.044(5) 0.074(6) 0.032(5) 0.023(5) 0.016(4) C7 0.056(6) 0.035(5) 0.070(6) 0.018(5) 0.032(5) -0.001(4) C8 0.034(5) 0.036(5) 0.060(6) 0.018(4) 0.016(4) 0.003(4) C9 0.090(9) 0.050(6) 0.071(7) 0.003(5) 0.038(6) 0.008(6) C10 0.078(8) 0.068(7) 0.078(8) 0.018(6) 0.042(7) 0.017(6) C11 0.060(7) 0.063(7) 0.061(6) 0.019(5) 0.018(6) -0.007(5) C12 0.028(4) 0.043(5) 0.053(5) -0.007(4) 0.007(4) 0.002(4) C13 0.112(11) 0.057(7) 0.061(7) 0.009(5) 0.025(7) -0.028(7) C14 0.057(6) 0.041(5) 0.076(7) 0.014(5) 0.034(6) 0.006(4) C15 0.017(4) 0.035(4) 0.056(5) 0.011(4) 0.007(4) 0.000(3) C16 0.074(7) 0.029(4) 0.072(7) 0.012(4) 0.047(6) 0.003(4) C17 0.026(4) 0.041(5) 0.058(6) 0.027(4) 0.004(4) 0.004(4) C18 0.076(8) 0.043(6) 0.086(8) -0.007(5) 0.038(6) 0.002(5) C19 0.063(7) 0.059(6) 0.061(6) 0.010(5) 0.016(5) 0.005(5) C20 0.044(5) 0.039(5) 0.065(6) 0.008(4) 0.016(5) 0.000(4) C21 0.026(5) 0.047(5) 0.080(7) -0.002(5) 0.006(4) -0.006(4) C22 0.030(5) 0.035(5) 0.083(7) -0.005(5) -0.006(5) 0.004(4) C23 0.058(6) 0.037(5) 0.047(5) -0.015(4) -0.005(4) 0.001(4) C24 0.054(6) 0.047(5) 0.051(5) -0.007(4) 0.023(5) 0.001(4) C25 0.045(5) 0.045(5) 0.066(6) 0.012(4) 0.029(5) 0.007(4) C26 0.148(14) 0.099(10) 0.053(7) -0.021(7) 0.005(7) -0.051(10) C27 0.078(8) 0.044(6) 0.076(7) 0.002(5) 0.036(6) -0.017(5) Cu1 0.0258(7) 0.0339(8) 0.0367(7) -0.0055(6) 0.0107(6) -0.0073(5) N1 0.032(4) 0.038(4) 0.041(4) 0.002(3) 0.007(3) 0.003(3) N2 0.039(4) 0.045(5) 0.072(5) 0.020(4) 0.013(4) 0.008(3) N3 0.067(6) 0.043(5) 0.057(5) 0.011(4) 0.016(4) -0.007(4) N4 0.052(5) 0.043(4) 0.057(5) 0.005(4) 0.022(4) -0.006(4) N5 0.037(4) 0.032(4) 0.058(4) 0.001(3) 0.020(3) -0.002(3) N6 0.048(4) 0.033(4) 0.049(4) -0.005(3) 0.018(3) 0.001(3) O1 0.057(4) 0.046(4) 0.074(4) 0.001(3) 0.020(4) 0.007(3) O2 0.048(4) 0.055(4) 0.057(4) -0.001(3) 0.015(3) 0.004(3) O3 0.062(4) 0.044(4) 0.055(4) 0.002(3) -0.003(3) -0.005(3) O4 0.27(2) 0.135(12) 0.182(15) -0.074(11) -0.058(13) 0.033(13) Ru1 0.0262(4) 0.0233(4) 0.0416(4) 0.0035(3) 0.0115(3) 0.0022(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.145(9) . ? C1 Ru1 2.078(7) . ? C2 N2 1.136(10) . ? C2 Ru1 2.086(8) . ? C3 N3 1.283(13) . ? C3 C4 1.477(15) . ? C3 H3A 0.9300 . ? C4 C5 1.366(14) . ? C4 H4A 0.9300 . ? C5 C6 1.445(13) . ? C5 H5A 0.9300 . ? C6 C11 1.397(14) . ? C6 C7 1.404(12) . ? C7 N3 1.325(12) . ? C7 C8 1.467(13) . ? C8 O1 1.333(10) . ? C8 C9 1.349(13) . ? C9 C10 1.360(15) . ? C9 H9A 0.9300 . ? C10 C11 1.335(14) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 N4 1.273(11) . ? C12 C13 1.493(16) . ? C12 H12A 0.9300 . ? C13 C14 1.417(15) . ? C13 H13A 0.9300 . ? C14 C15 1.392(12) . ? C14 H14A 0.9300 . ? C15 C20 1.408(12) . ? C15 C16 1.427(12) . ? C16 N4 1.323(11) . ? C16 C17 1.467(13) . ? C17 C18 1.342(13) . ? C17 O2 1.363(10) . ? C18 C19 1.379(14) . ? C18 H18A 0.9300 . ? C19 C20 1.343(13) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 N5 1.463(10) . ? C21 C22 1.484(13) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.527(13) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N6 1.504(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.459(12) . ? C24 N6 1.474(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N5 1.512(11) 3_655 ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 O3 1.411(13) . ? C27 O4 1.35(2) . ? Cu1 N6 2.012(7) 3_655 ? Cu1 N6 2.012(7) . ? Cu1 N5 2.037(7) 3_655 ? Cu1 N5 2.037(7) . ? N3 Ru1 2.098(9) . ? N4 Ru1 2.053(8) . ? N5 C25 1.512(11) 3_655 ? O1 Ru1 1.992(7) . ? O2 Ru1 2.021(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 N1 C1 Ru1 175.7(7) . . ? N2 C2 Ru1 177.5(8) . . ? N3 C3 C4 121.6(9) . . ? N3 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C5 C4 C3 120.2(10) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 115.5(9) . . ? C4 C5 H5A 122.2 . . ? C6 C5 H5A 122.2 . . ? C11 C6 C7 115.8(10) . . ? C11 C6 C5 124.4(8) . . ? C7 C6 C5 119.7(9) . . ? N3 C7 C6 122.5(10) . . ? N3 C7 C8 117.3(9) . . ? C6 C7 C8 120.1(9) . . ? O1 C8 C9 127.0(10) . . ? O1 C8 C7 115.5(8) . . ? C9 C8 C7 117.4(9) . . ? C8 C9 C10 122.7(11) . . ? C8 C9 H9A 118.6 . . ? C10 C9 H9A 118.6 . . ? C11 C10 C9 119.6(11) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C6 124.2(11) . . ? C10 C11 H11A 117.9 . . ? C6 C11 H11A 117.9 . . ? N4 C12 C13 124.5(9) . . ? N4 C12 H12A 117.8 . . ? C13 C12 H12A 117.8 . . ? C14 C13 C12 115.4(10) . . ? C14 C13 H13A 122.3 . . ? C12 C13 H13A 122.3 . . ? C15 C14 C13 118.0(10) . . ? C15 C14 H14A 121.0 . . ? C13 C14 H14A 121.0 . . ? C14 C15 C20 124.6(8) . . ? C14 C15 C16 120.2(8) . . ? C20 C15 C16 115.2(8) . . ? N4 C16 C15 122.1(9) . . ? N4 C16 C17 118.2(9) . . ? C15 C16 C17 119.6(8) . . ? C18 C17 O2 124.9(9) . . ? C18 C17 C16 120.4(9) . . ? O2 C17 C16 114.7(8) . . ? C17 C18 C19 119.0(11) . . ? C17 C18 H18A 120.5 . . ? C19 C18 H18A 120.5 . . ? C20 C19 C18 122.4(11) . . ? C20 C19 H19A 118.8 . . ? C18 C19 H19A 118.8 . . ? C19 C20 C15 123.2(9) . . ? C19 C20 H20A 118.4 . . ? C15 C20 H20A 118.4 . . ? N5 C21 C22 111.0(8) . . ? N5 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? N5 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 115.4(7) . . ? C21 C22 H22A 108.4 . . ? C23 C22 H22A 108.4 . . ? C21 C22 H22B 108.4 . . ? C23 C22 H22B 108.4 . . ? H22A C22 H22B 107.5 . . ? N6 C23 C22 112.0(7) . . ? N6 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? N6 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C25 C24 N6 108.1(7) . . ? C25 C24 H24A 110.1 . . ? N6 C24 H24A 110.1 . . ? C25 C24 H24B 110.1 . . ? N6 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? C24 C25 N5 109.8(7) . 3_655 ? C24 C25 H25A 109.7 . . ? N5 C25 H25A 109.7 3_655 . ? C24 C25 H25B 109.7 . . ? N5 C25 H25B 109.7 3_655 . ? H25A C25 H25B 108.2 . . ? N6 Cu1 N6 180.0 3_655 . ? N6 Cu1 N5 93.7(3) 3_655 3_655 ? N6 Cu1 N5 86.3(3) . 3_655 ? N6 Cu1 N5 86.3(3) 3_655 . ? N6 Cu1 N5 93.7(3) . . ? N5 Cu1 N5 180.0(4) 3_655 . ? C3 N3 C7 120.4(9) . . ? C3 N3 Ru1 128.4(7) . . ? C7 N3 Ru1 111.1(7) . . ? C12 N4 C16 119.7(9) . . ? C12 N4 Ru1 128.3(7) . . ? C16 N4 Ru1 112.0(7) . . ? C21 N5 C25 114.1(7) . 3_655 ? C21 N5 Cu1 117.6(5) . . ? C25 N5 Cu1 104.4(5) 3_655 . ? C24 N6 C23 112.0(7) . . ? C24 N6 Cu1 106.7(5) . . ? C23 N6 Cu1 117.0(6) . . ? C8 O1 Ru1 115.3(6) . . ? C17 O2 Ru1 113.4(6) . . ? O1 Ru1 O2 179.3(3) . . ? O1 Ru1 N4 97.7(3) . . ? O2 Ru1 N4 81.6(3) . . ? O1 Ru1 C1 92.0(3) . . ? O2 Ru1 C1 88.1(3) . . ? N4 Ru1 C1 89.4(3) . . ? O1 Ru1 C2 91.2(3) . . ? O2 Ru1 C2 88.7(3) . . ? N4 Ru1 C2 90.1(3) . . ? C1 Ru1 C2 176.8(3) . . ? O1 Ru1 N3 80.7(3) . . ? O2 Ru1 N3 100.0(3) . . ? N4 Ru1 N3 178.4(3) . . ? C1 Ru1 N3 90.6(3) . . ? C2 Ru1 N3 89.9(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.938 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.144 data_ic13994 _database_code_depnum_ccdc_archive 'CCDC 903916' #TrackingRef 'web_deposit_cif_file_0_WaiLunMan_1349106073.total.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H60 N12 Ni O8 Ru2' _chemical_formula_weight 1265.99 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' Ni Ni 0.3393 1.1124 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9374(3) _cell_length_b 20.4558(10) _cell_length_c 15.3293(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.278(2) _cell_angle_gamma 90.00 _cell_volume 2716.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6508 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.958 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.652 _exptl_absorpt_correction_T_max 0.891 _exptl_absorpt_process_details ? _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 KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14376 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6160 _reflns_number_gt 4348 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0745P)^2^+3.2783P] 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 6160 _refine_ls_number_parameters 458 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1526 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.006 _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 Ru Ru 0.54875(4) 0.262613(18) 0.37242(3) 0.03839(14) Uani 1 1 d . . . Ni Ni 0.5000 0.5000 0.5000 0.0326(2) Uani 1 2 d S . . N1 N 0.4799(4) 0.39921(18) 0.4611(3) 0.0357(8) Uani 1 1 d . . . N2 N 0.6434(5) 0.1373(2) 0.2715(4) 0.0637(13) Uani 1 1 d . . . N3 N 0.4365(4) 0.52509(18) 0.3645(3) 0.0395(9) Uani 1 1 d . . . N4 N 0.7273(4) 0.50234(18) 0.4865(3) 0.0388(9) Uani 1 1 d . . . C1 C 0.4979(5) 0.3490(2) 0.4327(3) 0.0367(10) Uani 1 1 d . A . C2 C 0.6073(5) 0.1817(2) 0.3079(4) 0.0480(12) Uani 1 1 d . A . C3 C 0.3098(5) 0.5729(2) 0.3390(3) 0.0453(11) Uani 1 1 d . . . H3A H 0.2851 0.5798 0.2730 0.054 Uiso 1 1 calc R . . H3B H 0.3442 0.6153 0.3684 0.054 Uiso 1 1 calc R . . C4 C 0.8360(6) 0.4495(2) 0.6340(4) 0.0499(13) Uani 1 1 d . . . H4A H 0.8614 0.4943 0.6577 0.060 Uiso 1 1 calc R A . H4B H 0.9223 0.4207 0.6641 0.060 Uiso 1 1 calc R . . C5 C 0.8283(5) 0.4501(2) 0.5350(4) 0.0444(12) Uani 1 1 d . A . H5A H 0.9337 0.4561 0.5264 0.053 Uiso 1 1 calc R . . H5B H 0.7895 0.4073 0.5088 0.053 Uiso 1 1 calc R . . C6 C 0.7131(6) 0.5029(2) 0.3875(3) 0.0465(12) Uani 1 1 d . A . H6A H 0.6918 0.4582 0.3629 0.056 Uiso 1 1 calc R . . H6B H 0.8109 0.5182 0.3751 0.056 Uiso 1 1 calc R . . C7 C 0.5820(5) 0.5484(2) 0.3432(3) 0.0457(11) Uani 1 1 d . A . H7A H 0.6054 0.5935 0.3658 0.055 Uiso 1 1 calc R . . H7B H 0.5695 0.5487 0.2772 0.055 Uiso 1 1 calc R . . O1 O 0.5948(6) 0.3199(3) 0.2760(4) 0.0421(14) Uani 0.598(5) 1 d P A 1 O2 O 0.5012(6) 0.2058(3) 0.4678(4) 0.0475(15) Uani 0.598(5) 1 d P A 1 N5 N 0.7771(8) 0.2782(3) 0.4338(6) 0.0426(18) Uani 0.598(5) 1 d P A 1 N6 N 0.3123(8) 0.2436(3) 0.3121(6) 0.0427(19) Uani 0.598(5) 1 d P A 1 C8 C 0.860(2) 0.2571(9) 0.5146(11) 0.048(5) Uani 0.598(5) 1 d P A 1 H8 H 0.8135 0.2308 0.5518 0.058 Uiso 0.598(5) 1 calc PR A 1 C9 C 1.0163(12) 0.2745(5) 0.5429(7) 0.054(2) Uani 0.598(5) 1 d P A 1 H9 H 1.0766 0.2610 0.6001 0.064 Uiso 0.598(5) 1 calc PR A 1 C10 C 1.0854(17) 0.3138(6) 0.4832(11) 0.056(3) Uani 0.598(5) 1 d P A 1 H10 H 1.1917 0.3248 0.5025 0.067 Uiso 0.598(5) 1 calc PR A 1 C11 C 1.0017(12) 0.3356(6) 0.3994(9) 0.039(3) Uani 0.598(5) 1 d P A 1 C12 C 1.043(2) 0.3723(7) 0.3367(10) 0.050(4) Uani 0.598(5) 1 d P A 1 H12 H 1.1498 0.3837 0.3505 0.060 Uiso 0.598(5) 1 calc PR A 1 C13 C 0.9668(12) 0.3937(5) 0.2645(8) 0.056(3) Uani 0.598(5) 1 d P A 1 H13 H 1.0115 0.4201 0.2267 0.067 Uiso 0.598(5) 1 calc PR A 1 C14 C 0.8142(12) 0.3775(4) 0.2418(6) 0.044(2) Uani 0.598(5) 1 d P A 1 H14 H 0.7501 0.3938 0.1873 0.053 Uiso 0.598(5) 1 calc PR A 1 C15 C 0.7491(17) 0.3370(6) 0.2972(11) 0.038(3) Uani 0.598(5) 1 d P A 1 C16 C 0.8429(13) 0.3158(4) 0.3775(8) 0.0366(19) Uani 0.598(5) 1 d P A 1 C17 C 0.230(2) 0.2671(8) 0.2321(12) 0.061(6) Uani 0.598(5) 1 d P A 1 H17 H 0.2713 0.2958 0.1951 0.074 Uiso 0.598(5) 1 calc PR A 1 C18 C 0.0684(13) 0.2426(5) 0.2087(7) 0.051(2) Uani 0.598(5) 1 d P A 1 H18 H 0.0039 0.2564 0.1528 0.062 Uiso 0.598(5) 1 calc PR A 1 C19 C -0.0001(16) 0.1991(6) 0.2639(10) 0.044(3) Uani 0.598(5) 1 d P A 1 H19 H -0.1048 0.1853 0.2478 0.053 Uiso 0.598(5) 1 calc PR A 1 C20 C 0.1043(13) 0.1804(7) 0.3421(9) 0.037(3) Uani 0.598(5) 1 d P A 1 C21 C 0.0630(16) 0.1370(6) 0.4047(9) 0.056(3) Uani 0.598(5) 1 d P A 1 H21 H -0.0409 0.1220 0.3903 0.067 Uiso 0.598(5) 1 calc PR A 1 C22 C 0.1526(13) 0.1153(5) 0.4802(8) 0.069(3) Uani 0.598(5) 1 d P A 1 H22 H 0.1151 0.0854 0.5172 0.083 Uiso 0.598(5) 1 calc PR A 1 C23 C 0.3032(13) 0.1374(4) 0.5041(7) 0.052(2) Uani 0.598(5) 1 d P A 1 H23 H 0.3701 0.1226 0.5587 0.062 Uiso 0.598(5) 1 calc PR A 1 C24 C 0.3604(16) 0.1822(6) 0.4480(10) 0.039(3) Uani 0.598(5) 1 d P A 1 C25 C 0.2567(11) 0.2026(4) 0.3656(8) 0.0394(19) Uani 0.598(5) 1 d P A 1 O1' O 0.7051(9) 0.2362(4) 0.4858(6) 0.046(2) Uani 0.402(5) 1 d P A 2 O2' O 0.3971(9) 0.2892(4) 0.2594(6) 0.043(2) Uani 0.402(5) 1 d P A 2 N5' N 0.7481(14) 0.3093(5) 0.3500(10) 0.037(3) Uani 0.402(5) 1 d P A 2 N6' N 0.3684(12) 0.2115(6) 0.3974(9) 0.045(3) Uani 0.402(5) 1 d P A 2 C8' C 0.761(4) 0.3470(14) 0.2787(19) 0.045(7) Uiso 0.402(5) 1 d P A 2 H8' H 0.6745 0.3546 0.2294 0.054 Uiso 0.402(5) 1 calc PR A 2 C9' C 0.914(2) 0.3756(8) 0.2809(11) 0.049(4) Uiso 0.402(5) 1 d P A 2 H9' H 0.9261 0.4014 0.2315 0.058 Uiso 0.402(5) 1 calc PR A 2 C10' C 1.055(3) 0.3646(13) 0.3608(16) 0.035(5) Uiso 0.402(5) 1 d P A 2 H10' H 1.1548 0.3820 0.3641 0.042 Uiso 0.402(5) 1 calc PR A 2 C11' C 1.019(2) 0.3262(8) 0.4274(12) 0.020(4) Uiso 0.402(5) 1 d P A 2 C12' C 1.135(2) 0.3122(11) 0.5043(15) 0.048(6) Uiso 0.402(5) 1 d P A 2 H12' H 1.2370 0.3271 0.5072 0.057 Uiso 0.402(5) 1 calc PR A 2 C13' C 1.110(2) 0.2790(8) 0.5738(12) 0.061(4) Uiso 0.402(5) 1 d P A 2 H13' H 1.1915 0.2747 0.6264 0.074 Uiso 0.402(5) 1 calc PR A 2 C14' C 0.967(2) 0.2501(8) 0.5726(12) 0.055(4) Uiso 0.402(5) 1 d P A 2 H14' H 0.9514 0.2241 0.6208 0.066 Uiso 0.402(5) 1 calc PR A 2 C15' C 0.848(3) 0.2626(13) 0.4933(17) 0.028(5) Uiso 0.402(5) 1 d P A 2 C16' C 0.8730(15) 0.3005(7) 0.4227(10) 0.035(3) Uiso 0.402(5) 1 d P A 2 C17' C 0.352(3) 0.1710(12) 0.4648(17) 0.044(6) Uiso 0.402(5) 1 d P A 2 H17' H 0.4386 0.1627 0.5137 0.053 Uiso 0.402(5) 1 calc PR A 2 C18' C 0.215(2) 0.1422(10) 0.4636(13) 0.067(5) Uiso 0.402(5) 1 d P A 2 H18' H 0.2048 0.1146 0.5116 0.080 Uiso 0.402(5) 1 calc PR A 2 C19' C 0.078(3) 0.1548(13) 0.3836(19) 0.067(6) Uiso 0.402(5) 1 d P A 2 H19' H -0.0182 0.1347 0.3836 0.081 Uiso 0.402(5) 1 calc PR A 2 C20' C 0.085(4) 0.1894(19) 0.320(2) 0.067(6) Uiso 0.402(5) 1 d PD A 2 C21' C -0.014(3) 0.2078(14) 0.2363(16) 0.056(7) Uiso 0.402(5) 1 d PD A 2 H21' H -0.1127 0.1881 0.2270 0.067 Uiso 0.402(5) 1 calc PR A 2 C22' C -0.005(2) 0.2412(8) 0.1752(12) 0.054(4) Uiso 0.402(5) 1 d P A 2 H22' H -0.0918 0.2474 0.1259 0.065 Uiso 0.402(5) 1 calc PR A 2 C23' C 0.1311(19) 0.2707(7) 0.1764(11) 0.054(4) Uiso 0.402(5) 1 d P A 2 H23' H 0.1460 0.2987 0.1298 0.065 Uiso 0.402(5) 1 calc PR A 2 C24' C 0.243(3) 0.2563(10) 0.2501(17) 0.027(4) Uiso 0.402(5) 1 d P A 2 C25' C 0.242(2) 0.2213(9) 0.3208(12) 0.047(4) Uiso 0.402(5) 1 d P A 2 O5 O 0.3712(6) 0.4201(2) 0.2284(3) 0.0726(12) Uani 1 1 d . . . H5 H 0.4252 0.3862 0.2411 0.109 Uiso 1 1 calc R . . C29 C 0.3656(14) 0.4391(5) 0.1394(6) 0.137(4) Uani 1 1 d . . . H29A H 0.3208 0.4829 0.1285 0.205 Uiso 1 1 calc R . . H29B H 0.3017 0.4080 0.0974 0.205 Uiso 1 1 calc R . . H29C H 0.4703 0.4394 0.1303 0.205 Uiso 1 1 calc R . . O6 O 0.6966(9) 0.0160(3) 0.3592(6) 0.145(3) Uani 1 1 d . . . H6 H 0.6861 0.0439 0.3180 0.217 Uiso 1 1 d R . . C30 C 0.5851(18) 0.0283(6) 0.4114(9) 0.174(5) Uani 1 1 d . . . H30A H 0.5841 -0.0086 0.4521 0.261 Uiso 1 1 calc R . . H30B H 0.4823 0.0335 0.3708 0.261 Uiso 1 1 calc R . . H30C H 0.6132 0.0684 0.4467 0.261 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 Ru 0.0330(2) 0.0313(2) 0.0536(3) -0.00681(17) 0.01579(16) -0.00217(15) Ni 0.0310(4) 0.0271(4) 0.0424(5) 0.0008(3) 0.0141(3) 0.0008(3) N1 0.0346(19) 0.031(2) 0.045(2) -0.0018(16) 0.0166(17) 0.0001(15) N2 0.047(3) 0.051(3) 0.096(4) -0.027(3) 0.023(3) -0.006(2) N3 0.038(2) 0.035(2) 0.048(2) 0.0056(18) 0.0134(17) 0.0024(17) N4 0.036(2) 0.033(2) 0.051(2) 0.0009(17) 0.0201(18) 0.0025(16) C1 0.030(2) 0.035(2) 0.047(3) 0.001(2) 0.0131(19) -0.0057(19) C2 0.037(3) 0.040(3) 0.070(3) -0.012(3) 0.020(2) -0.006(2) C3 0.043(3) 0.041(3) 0.051(3) 0.008(2) 0.011(2) 0.003(2) C4 0.040(3) 0.035(3) 0.071(4) 0.008(2) 0.005(2) 0.000(2) C5 0.029(2) 0.035(2) 0.071(3) 0.000(2) 0.016(2) -0.0004(19) C6 0.047(3) 0.041(3) 0.058(3) -0.004(2) 0.026(2) -0.001(2) C7 0.046(3) 0.046(3) 0.049(3) 0.002(2) 0.018(2) -0.003(2) O1 0.035(3) 0.044(3) 0.048(3) -0.004(2) 0.010(2) -0.002(2) O2 0.039(3) 0.041(3) 0.064(4) -0.001(3) 0.015(3) -0.003(3) N5 0.033(4) 0.036(4) 0.061(5) -0.008(3) 0.017(4) -0.002(3) N6 0.029(3) 0.036(4) 0.066(6) -0.020(4) 0.018(4) -0.007(3) C8 0.059(9) 0.048(7) 0.043(10) 0.008(7) 0.022(9) 0.004(5) C9 0.047(6) 0.054(6) 0.056(6) -0.017(5) 0.004(5) 0.010(5) C10 0.044(7) 0.047(6) 0.073(10) -0.022(6) 0.010(7) 0.007(6) C11 0.041(6) 0.035(6) 0.036(7) -0.003(5) 0.003(5) 0.009(4) C12 0.071(8) 0.042(7) 0.041(9) -0.002(7) 0.021(7) 0.008(5) C13 0.053(6) 0.052(6) 0.074(7) -0.007(5) 0.037(6) -0.014(5) C14 0.053(6) 0.039(5) 0.047(5) -0.005(4) 0.024(5) -0.005(4) C15 0.044(6) 0.024(6) 0.052(9) -0.003(6) 0.023(6) 0.003(5) C16 0.032(5) 0.034(4) 0.045(6) -0.010(4) 0.011(4) 0.006(4) C17 0.089(12) 0.043(8) 0.062(12) 0.013(6) 0.039(9) 0.025(6) C18 0.048(6) 0.047(5) 0.052(6) -0.013(4) 0.002(5) 0.008(5) C19 0.065(8) 0.029(5) 0.049(8) -0.013(6) 0.033(8) 0.003(5) C20 0.021(5) 0.037(6) 0.056(8) -0.021(7) 0.014(4) 0.001(4) C21 0.079(8) 0.042(6) 0.057(8) 0.000(5) 0.037(7) 0.009(6) C22 0.081(8) 0.050(6) 0.091(9) 0.001(6) 0.050(7) -0.023(5) C23 0.059(6) 0.038(5) 0.064(6) 0.004(4) 0.028(5) -0.008(4) C24 0.053(7) 0.022(5) 0.051(8) 0.002(5) 0.028(6) -0.014(4) C25 0.042(6) 0.029(4) 0.051(6) -0.012(4) 0.018(4) 0.004(4) O1' 0.037(4) 0.039(5) 0.070(6) -0.004(4) 0.028(4) -0.005(4) O2' 0.042(5) 0.035(4) 0.055(5) -0.004(4) 0.020(4) -0.011(4) N5' 0.028(6) 0.027(5) 0.059(8) -0.005(6) 0.018(6) 0.002(5) N6' 0.027(6) 0.036(6) 0.071(8) -0.010(6) 0.011(6) 0.004(5) O5 0.092(3) 0.056(3) 0.062(3) -0.001(2) 0.003(2) 0.007(2) C29 0.186(11) 0.125(8) 0.083(6) 0.007(6) 0.004(6) 0.043(8) O6 0.185(7) 0.077(4) 0.187(7) 0.010(4) 0.074(6) 0.039(4) C30 0.261(16) 0.131(10) 0.147(11) 0.034(8) 0.081(11) 0.073(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru O2 1.994(6) . ? Ru O2' 1.993(9) . ? Ru O1 2.008(5) . ? Ru O1' 2.017(9) . ? Ru N6' 2.035(12) . ? Ru N5 2.050(7) . ? Ru C2 2.060(5) . ? Ru C1 2.095(5) . ? Ru N6 2.123(7) . ? Ru N5' 2.122(11) . ? Ni N3 2.078(4) 3_666 ? Ni N3 2.078(4) . ? Ni N4 2.093(3) 3_666 ? Ni N4 2.093(3) . ? Ni N1 2.141(4) 3_666 ? Ni N1 2.141(4) . ? N1 C1 1.143(5) . ? N2 C2 1.153(6) . ? N3 C3 1.474(6) . ? N3 C7 1.495(6) . ? N4 C5 1.476(6) . ? N4 C6 1.490(6) . ? C3 C4 1.532(7) 3_666 ? C4 C5 1.503(7) . ? C4 C3 1.532(7) 3_666 ? C6 C7 1.519(7) . ? O1 C15 1.382(16) . ? O2 C24 1.312(14) . ? N5 C8 1.349(19) . ? N5 C16 1.389(12) . ? N6 C17 1.352(19) . ? N6 C25 1.350(12) . ? C8 C9 1.40(2) . ? C9 C10 1.464(19) . ? C10 C11 1.392(17) . ? C11 C12 1.34(2) . ? C11 C16 1.434(16) . ? C12 C13 1.230(19) . ? C13 C14 1.363(14) . ? C14 C15 1.410(17) . ? C15 C16 1.377(19) . ? C17 C18 1.49(2) . ? C18 C19 1.462(18) . ? C19 C20 1.379(19) . ? C20 C25 1.397(16) . ? C20 C21 1.421(16) . ? C21 C22 1.311(18) . ? C22 C23 1.380(15) . ? C23 C24 1.435(14) . ? C24 C25 1.433(18) . ? O1' C15' 1.36(3) . ? O2' C24' 1.51(2) . ? N5' C8' 1.37(3) . ? N5' C16' 1.380(18) . ? N6' C17' 1.36(2) . ? N6' C25' 1.43(2) . ? C8' C9' 1.48(3) . ? C9' C10' 1.54(3) . ? C10' C11' 1.39(3) . ? C11' C16' 1.39(2) . ? C11' C12' 1.40(2) . ? C12' C13' 1.33(3) . ? C13' C14' 1.40(2) . ? C14' C15' 1.43(3) . ? C15' C16' 1.39(3) . ? C17' C18' 1.35(3) . ? C18' C19' 1.53(3) . ? C19' C20' 1.22(4) . ? C20' C21' 1.415(19) . ? C20' C25' 1.55(4) . ? C21' C22' 1.18(3) . ? C22' C23' 1.35(2) . ? C23' C24' 1.34(3) . ? C24' C25' 1.30(3) . ? O5 C29 1.408(10) . ? O6 C30 1.445(13) . ? 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 O2 Ru O2' 125.0(3) . . ? O2 Ru O1 179.5(2) . . ? O2' Ru O1 54.5(3) . . ? O2 Ru O1' 55.9(3) . . ? O2' Ru O1' 179.0(3) . . ? O1 Ru O1' 124.5(3) . . ? O2 Ru N6' 40.6(4) . . ? O2' Ru N6' 84.5(4) . . ? O1 Ru N6' 139.0(4) . . ? O1' Ru N6' 96.5(4) . . ? O2 Ru N5 97.0(3) . . ? O2' Ru N5 138.0(3) . . ? O1 Ru N5 83.4(3) . . ? O1' Ru N5 41.1(3) . . ? N6' Ru N5 137.6(5) . . ? O2 Ru C2 90.5(2) . . ? O2' Ru C2 90.0(3) . . ? O1 Ru C2 89.6(2) . . ? O1' Ru C2 89.7(3) . . ? N6' Ru C2 89.1(3) . . ? N5 Ru C2 90.2(2) . . ? O2 Ru C1 93.4(2) . . ? O2' Ru C1 88.8(3) . . ? O1 Ru C1 86.47(19) . . ? O1' Ru C1 91.4(3) . . ? N6' Ru C1 94.7(3) . . ? N5 Ru C1 88.1(2) . . ? C2 Ru C1 175.85(18) . . ? O2 Ru N6 81.0(3) . . ? O2' Ru N6 44.0(3) . . ? O1 Ru N6 98.6(3) . . ? O1' Ru N6 136.9(3) . . ? N6' Ru N6 40.4(4) . . ? N5 Ru N6 177.9(3) . . ? C2 Ru N6 89.3(2) . . ? C1 Ru N6 92.6(2) . . ? O2 Ru N5' 136.0(5) . . ? O2' Ru N5' 98.9(5) . . ? O1 Ru N5' 44.4(5) . . ? O1' Ru N5' 80.1(5) . . ? N6' Ru N5' 175.4(5) . . ? N5 Ru N5' 39.1(5) . . ? C2 Ru N5' 87.7(3) . . ? C1 Ru N5' 88.5(3) . . ? N6 Ru N5' 142.9(5) . . ? N3 Ni N3 180.000(1) 3_666 . ? N3 Ni N4 85.85(15) 3_666 3_666 ? N3 Ni N4 94.15(15) . 3_666 ? N3 Ni N4 94.15(15) 3_666 . ? N3 Ni N4 85.85(15) . . ? N4 Ni N4 180.000(1) 3_666 . ? N3 Ni N1 88.62(15) 3_666 3_666 ? N3 Ni N1 91.38(15) . 3_666 ? N4 Ni N1 90.64(13) 3_666 3_666 ? N4 Ni N1 89.36(13) . 3_666 ? N3 Ni N1 91.38(15) 3_666 . ? N3 Ni N1 88.62(15) . . ? N4 Ni N1 89.36(13) 3_666 . ? N4 Ni N1 90.64(13) . . ? N1 Ni N1 180.00(5) 3_666 . ? C1 N1 Ni 164.1(3) . . ? C3 N3 C7 112.5(4) . . ? C3 N3 Ni 115.6(3) . . ? C7 N3 Ni 105.0(3) . . ? C5 N4 C6 114.0(4) . . ? C5 N4 Ni 114.9(3) . . ? C6 N4 Ni 105.1(3) . . ? N1 C1 Ru 173.0(4) . . ? N2 C2 Ru 178.2(4) . . ? N3 C3 C4 112.2(4) . 3_666 ? C5 C4 C3 116.5(4) . 3_666 ? N4 C5 C4 112.6(4) . . ? N4 C6 C7 108.9(4) . . ? N3 C7 C6 108.9(4) . . ? C15 O1 Ru 110.4(8) . . ? C24 O2 Ru 114.2(7) . . ? C8 N5 C16 121.8(11) . . ? C8 N5 Ru 129.1(9) . . ? C16 N5 Ru 109.1(7) . . ? C17 N6 C25 125.0(12) . . ? C17 N6 Ru 126.0(9) . . ? C25 N6 Ru 109.0(7) . . ? N5 C8 C9 118.8(13) . . ? C8 C9 C10 119.2(12) . . ? C11 C10 C9 122.6(14) . . ? C12 C11 C10 131.2(14) . . ? C12 C11 C16 115.1(11) . . ? C10 C11 C16 113.7(13) . . ? C13 C12 C11 130.7(16) . . ? C12 C13 C14 116.3(12) . . ? C13 C14 C15 121.7(11) . . ? C16 C15 O1 118.9(13) . . ? C16 C15 C14 118.2(12) . . ? O1 C15 C14 122.9(13) . . ? C15 C16 N5 118.2(12) . . ? C15 C16 C11 117.9(11) . . ? N5 C16 C11 123.8(11) . . ? N6 C17 C18 112.0(13) . . ? C19 C18 C17 125.9(11) . . ? C20 C19 C18 112.5(12) . . ? C19 C20 C25 122.8(14) . . ? C19 C20 C21 121.8(12) . . ? C25 C20 C21 115.4(12) . . ? C22 C21 C20 127.1(13) . . ? C21 C22 C23 117.9(10) . . ? C22 C23 C24 121.2(11) . . ? O2 C24 C23 124.0(13) . . ? O2 C24 C25 118.1(11) . . ? C23 C24 C25 117.8(11) . . ? N6 C25 C20 121.8(12) . . ? N6 C25 C24 117.5(10) . . ? C20 C25 C24 120.6(11) . . ? C15' O1' Ru 113.6(12) . . ? C24' O2' Ru 111.8(10) . . ? C8' N5' C16' 120.6(18) . . ? C8' N5' Ru 128.5(17) . . ? C16' N5' Ru 110.8(9) . . ? C17' N6' C25' 119.8(18) . . ? C17' N6' Ru 134.0(15) . . ? C25' N6' Ru 106.0(11) . . ? N5' C8' C9' 118(2) . . ? C8' C9' C10' 122.0(19) . . ? C11' C10' C9' 112(2) . . ? C10' C11' C16' 124.0(19) . . ? C10' C11' C12' 118.6(19) . . ? C16' C11' C12' 117.4(16) . . ? C13' C12' C11' 122.8(19) . . ? C12' C13' C14' 122.7(18) . . ? C13' C14' C15' 114.9(18) . . ? O1' C15' C16' 119(2) . . ? O1' C15' C14' 119.2(19) . . ? C16' C15' C14' 122(2) . . ? N5' C16' C11' 123.7(14) . . ? N5' C16' C15' 116.4(17) . . ? C11' C16' C15' 119.9(18) . . ? C18' C17' N6' 121(2) . . ? C17' C18' C19' 119(2) . . ? C20' C19' C18' 123(3) . . ? C19' C20' C21' 137(4) . . ? C19' C20' C25' 118(3) . . ? C21' C20' C25' 105(3) . . ? C22' C21' C20' 137(4) . . ? C21' C22' C23' 119(2) . . ? C24' C23' C22' 113.2(18) . . ? C25' C24' C23' 132(2) . . ? C25' C24' O2' 111(2) . . ? C23' C24' O2' 117.1(18) . . ? C24' C25' N6' 126(2) . . ? C24' C25' C20' 115(2) . . ? N6' C25' C20' 118.8(18) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.707 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.174 data_ic13997 _database_code_depnum_ccdc_archive 'CCDC 903917' #TrackingRef 'web_deposit_cif_file_0_WaiLunMan_1349106073.total.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H52 N12 Ni O7 Ru2' _chemical_formula_weight 1205.90 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' Ni Ni 0.3393 1.1124 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7692(4) _cell_length_b 13.5116(4) _cell_length_c 17.1714(6) _cell_angle_alpha 95.113(2) _cell_angle_beta 96.982(2) _cell_angle_gamma 102.153(2) _cell_volume 2631.04(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11711 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description rod _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 0.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.832 _exptl_absorpt_process_details ? _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 KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31128 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11896 _reflns_number_gt 7215 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0764P)^2^+4.9385P] 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 11896 _refine_ls_number_parameters 649 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1683 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 1.0000 1.0000 0.0000 0.03325(15) Uani 1 2 d S . . Ru2 Ru 0.5000 0.5000 0.0000 0.03144(15) Uani 1 2 d S . . Ni Ni 0.74091(5) 0.81157(5) 0.19011(4) 0.03150(17) Uani 1 1 d . A . O2 O 0.5578(4) 0.4278(3) 0.0885(2) 0.0520(10) Uani 1 1 d D . . N1 N 0.8657(4) 0.8712(3) 0.1226(3) 0.0401(10) Uani 1 1 d . . . N2 N 0.6696(4) 0.7004(3) 0.0973(3) 0.0398(10) Uani 1 1 d . . . N3 N 0.6251(4) 0.9095(4) 0.1638(3) 0.0497(12) Uani 1 1 d . . . N4 N 0.8118(4) 0.9297(3) 0.2809(3) 0.0386(10) Uani 1 1 d . . . N5 N 0.8426(4) 0.7333(4) 0.2633(2) 0.0434(11) Uani 1 1 d . . . N6 N 0.6044(4) 0.7353(3) 0.2456(3) 0.0409(11) Uani 1 1 d . . . N8 N 0.3803(4) 0.5228(3) 0.0736(3) 0.0454(12) Uani 1 1 d D . . C1 C 0.9171(5) 0.9123(4) 0.0782(3) 0.0376(12) Uani 1 1 d . A . C2 C 0.6108(4) 0.6312(4) 0.0573(3) 0.0348(11) Uani 1 1 d . A . C3 C 0.6705(7) 1.0100(5) 0.2139(4) 0.0631(19) Uani 1 1 d . A . H3A H 0.6239 1.0141 0.2580 0.076 Uiso 1 1 calc R . . H3B H 0.6616 1.0660 0.1818 0.076 Uiso 1 1 calc R . . C4 C 0.8006(6) 1.0228(5) 0.2475(4) 0.0581(17) Uani 1 1 d . A . H4A H 0.8502 1.0339 0.2050 0.070 Uiso 1 1 calc R . . H4B H 0.8259 1.0821 0.2888 0.070 Uiso 1 1 calc R . . C5 C 0.9307(5) 0.9153(5) 0.3063(3) 0.0513(16) Uani 1 1 d . A . H5A H 0.9695 0.9648 0.3527 0.062 Uiso 1 1 calc R . . H5B H 0.9790 0.9255 0.2631 0.062 Uiso 1 1 calc R . . C6 C 0.9175(5) 0.8083(6) 0.3271(3) 0.0562(17) Uani 1 1 d . A . H6A H 0.9960 0.7924 0.3368 0.067 Uiso 1 1 calc R . . H6B H 0.8821 0.8029 0.3765 0.067 Uiso 1 1 calc R . . C7 C 0.7566(6) 0.6547(5) 0.2942(4) 0.0545(16) Uani 1 1 d . A . H7A H 0.7959 0.6311 0.3411 0.065 Uiso 1 1 calc R . . H7B H 0.7268 0.5953 0.2534 0.065 Uiso 1 1 calc R . . C8 C 0.6554(5) 0.6978(5) 0.3166(3) 0.0503(15) Uani 1 1 d . A . H8A H 0.5960 0.6445 0.3343 0.060 Uiso 1 1 calc R . . H8B H 0.6833 0.7543 0.3600 0.060 Uiso 1 1 calc R . . C9 C 0.5233(5) 0.8028(5) 0.2567(3) 0.0507(15) Uani 1 1 d . A . H9A H 0.5555 0.8544 0.3030 0.061 Uiso 1 1 calc R . . H9B H 0.4464 0.7629 0.2657 0.061 Uiso 1 1 calc R . . C10 C 0.5091(5) 0.8545(5) 0.1826(4) 0.0602(18) Uani 1 1 d . A . H10A H 0.4696 0.8027 0.1377 0.072 Uiso 1 1 calc R . . H10B H 0.4585 0.9037 0.1899 0.072 Uiso 1 1 calc R . . O1 O 0.8501(5) 1.0485(4) -0.0228(3) 0.0415(13) Uiso 0.67 1 d PD A 1 N7 N 1.0341(6) 1.1237(5) 0.0872(4) 0.0435(17) Uiso 0.67 1 d PD A 1 C11 C 1.1301(9) 1.1574(7) 0.1396(5) 0.057(2) Uiso 0.67 1 d PD A 1 H11A H 1.1947 1.1257 0.1379 0.068 Uiso 0.67 1 calc PR A 1 C12 C 1.1371(12) 1.2396(10) 0.1976(8) 0.080(5) Uiso 0.67 1 d PD A 1 H12A H 1.2074 1.2648 0.2336 0.096 Uiso 0.67 1 calc PR A 1 C13 C 1.0429(10) 1.2838(10) 0.2025(8) 0.074(4) Uiso 0.67 1 d PD A 1 H13A H 1.0468 1.3377 0.2429 0.088 Uiso 0.67 1 calc PR A 1 C14 C 0.9442(8) 1.2497(7) 0.1492(6) 0.061(3) Uiso 0.67 1 d PD A 1 C15 C 0.8414(9) 1.2896(9) 0.1467(7) 0.080(3) Uiso 0.67 1 d PD A 1 H15A H 0.8357 1.3428 0.1851 0.095 Uiso 0.67 1 calc PR A 1 C16 C 0.7521(12) 1.2494(8) 0.0878(6) 0.062(3) Uiso 0.67 1 d PD A 1 H16A H 0.6854 1.2786 0.0873 0.075 Uiso 0.67 1 calc PR A 1 C17 C 0.7443(10) 1.1703(9) 0.0274(7) 0.057(4) Uiso 0.67 1 d PD A 1 H17A H 0.6771 1.1468 -0.0116 0.068 Uiso 0.67 1 calc PR A 1 C18 C 0.8451(8) 1.1284(7) 0.0292(5) 0.050(2) Uiso 0.67 1 d PD A 1 C19 C 0.9369(11) 1.1679(10) 0.0872(8) 0.045(4) Uiso 0.67 1 d PD A 1 O1' O 1.1061(9) 1.0878(8) 0.0914(6) 0.042(3) Uiso 0.33 1 d PD A 2 N7' N 0.8991(11) 1.1037(10) 0.0250(8) 0.047(4) Uiso 0.33 1 d PD A 2 C11' C 0.7964(13) 1.1094(13) -0.0129(10) 0.047(4) Uiso 0.33 1 d PD A 2 H11B H 0.7585 1.0604 -0.0565 0.056 Uiso 0.33 1 calc PR A 2 C12' C 0.744(2) 1.189(2) 0.0119(16) 0.096(14) Uiso 0.33 1 d PD A 2 H12B H 0.6769 1.1992 -0.0199 0.115 Uiso 0.33 1 calc PR A 2 C13' C 0.789(2) 1.252(3) 0.0817(17) 0.127(17) Uiso 0.33 1 d PD A 2 H13B H 0.7509 1.3039 0.0990 0.152 Uiso 0.33 1 calc PR A 2 C14' C 0.8894(12) 1.2389(10) 0.1256(8) 0.033(3) Uiso 0.33 1 d PD A 2 C15' C 0.9421(15) 1.2976(14) 0.1974(10) 0.067(6) Uiso 0.33 1 d PD A 2 H15B H 0.9065 1.3474 0.2209 0.081 Uiso 0.33 1 calc PR A 2 C16' C 1.0457(16) 1.2814(15) 0.2327(12) 0.055(6) Uiso 0.33 1 d PD A 2 H16B H 1.0782 1.3198 0.2824 0.065 Uiso 0.33 1 calc PR A 2 C17' C 1.1073(16) 1.2145(14) 0.2029(10) 0.046(5) Uiso 0.33 1 d PD A 2 H17B H 1.1798 1.2079 0.2306 0.055 Uiso 0.33 1 calc PR A 2 C18' C 1.0588(13) 1.1558(12) 0.1294(9) 0.043(4) Uiso 0.33 1 d PD A 2 C19' C 0.9522(17) 1.1673(17) 0.0949(11) 0.028(7) Uiso 0.33 1 d PD A 2 C20 C 0.2917(5) 0.5684(5) 0.0632(4) 0.0549(16) Uani 1 1 d D . . H20 H 0.2765 0.5968 0.0153 0.066 Uiso 1 1 calc R . . C21 C 0.2196(6) 0.5754(6) 0.1222(4) 0.069(2) Uani 1 1 d D . . H21 H 0.1556 0.6078 0.1139 0.083 Uiso 1 1 calc R . . C22 C 0.2414(6) 0.5357(5) 0.1914(4) 0.0630(18) Uani 1 1 d D . . H22 H 0.1911 0.5393 0.2303 0.076 Uiso 1 1 calc R . . C23 C 0.3347(6) 0.4907(5) 0.2057(4) 0.0612(17) Uani 1 1 d D . . C24 C 0.3662(7) 0.4509(7) 0.2744(4) 0.079(2) Uani 1 1 d D . . H24 H 0.3212 0.4530 0.3166 0.095 Uiso 1 1 calc R . . C25 C 0.4635(8) 0.4078(7) 0.2819(5) 0.096(3) Uani 1 1 d D . . H25 H 0.4853 0.3836 0.3305 0.115 Uiso 1 1 calc R . . C26 C 0.5310(7) 0.3983(6) 0.2210(4) 0.081(2) Uani 1 1 d D . . H26 H 0.5961 0.3670 0.2278 0.097 Uiso 1 1 calc R . . C27 C 0.5006(5) 0.4360(5) 0.1499(3) 0.0532(15) Uani 1 1 d D . . C28 C 0.4060(5) 0.4831(4) 0.1437(3) 0.0454(14) Uani 1 1 d D . . Ru3 Ru 0.0000 0.5000 0.5000 0.03147(15) Uani 1 2 d S . . O3 O 0.1761(3) 0.5281(3) 0.5102(2) 0.0379(8) Uani 1 1 d . . . N9 N -0.0114(5) 0.5072(4) 0.3121(3) 0.0547(13) Uani 1 1 d . . . N10 N 0.0199(4) 0.3512(3) 0.4830(2) 0.0334(9) Uani 1 1 d . . . C29 C -0.0085(4) 0.5036(4) 0.3789(3) 0.0398(12) Uani 1 1 d . . . C30 C -0.0587(5) 0.2645(4) 0.4740(3) 0.0402(12) Uani 1 1 d . . . H30 H -0.1381 0.2660 0.4780 0.048 Uiso 1 1 calc R . . C31 C -0.0297(5) 0.1697(4) 0.4587(3) 0.0408(12) Uani 1 1 d . . . H31 H -0.0890 0.1086 0.4523 0.049 Uiso 1 1 calc R . . C32 C 0.0831(5) 0.1658(4) 0.4531(3) 0.0398(12) Uani 1 1 d . . . H32 H 0.1029 0.1019 0.4423 0.048 Uiso 1 1 calc R . . C33 C 0.1715(4) 0.2566(4) 0.4632(3) 0.0337(11) Uani 1 1 d . . . C34 C 0.2920(5) 0.2617(4) 0.4599(3) 0.0400(12) Uani 1 1 d . . . H34 H 0.3185 0.2011 0.4480 0.048 Uiso 1 1 calc R . . C35 C 0.3693(5) 0.3530(4) 0.4738(3) 0.0447(13) Uani 1 1 d . . . H35 H 0.4500 0.3550 0.4715 0.054 Uiso 1 1 calc R . . C36 C 0.3345(4) 0.4456(4) 0.4915(3) 0.0409(13) Uani 1 1 d . . . H36 H 0.3915 0.5081 0.5019 0.049 Uiso 1 1 calc R . . C37 C 0.2171(4) 0.4449(4) 0.4938(3) 0.0327(11) Uani 1 1 d . . . C38 C 0.1357(4) 0.3485(4) 0.4793(3) 0.0321(11) Uani 1 1 d . . . Ru4 Ru 0.5000 0.0000 0.5000 0.02440(13) Uani 1 2 d S . . O4 O 0.5441(3) -0.0673(3) 0.59568(19) 0.0343(8) Uani 1 1 d . . . N11 N 0.2660(4) 0.0390(3) 0.5642(2) 0.0381(10) Uani 1 1 d . . . N12 N 0.6095(3) 0.1246(3) 0.5685(2) 0.0291(9) Uani 1 1 d . . . C39 C 0.3512(4) 0.0261(3) 0.5439(3) 0.0289(10) Uani 1 1 d . . . C40 C 0.6387(5) 0.2204(4) 0.5536(3) 0.0378(12) Uani 1 1 d . . . H40 H 0.5992 0.2402 0.5080 0.045 Uiso 1 1 calc R . . C41 C 0.7258(5) 0.2934(4) 0.6029(4) 0.0503(15) Uani 1 1 d . . . H41 H 0.7451 0.3612 0.5900 0.060 Uiso 1 1 calc R . . C42 C 0.7833(5) 0.2681(5) 0.6693(4) 0.0510(16) Uani 1 1 d . . . H42 H 0.8442 0.3173 0.7018 0.061 Uiso 1 1 calc R . . C43 C 0.7510(5) 0.1675(5) 0.6895(3) 0.0464(14) Uani 1 1 d . . . C44 C 0.7995(5) 0.1331(7) 0.7579(4) 0.0613(19) Uani 1 1 d . . . H44 H 0.8576 0.1786 0.7952 0.074 Uiso 1 1 calc R . . C45 C 0.7631(6) 0.0350(8) 0.7704(4) 0.073(2) Uani 1 1 d . . . H45 H 0.7970 0.0131 0.8171 0.087 Uiso 1 1 calc R . . C46 C 0.6776(5) -0.0363(6) 0.7178(4) 0.0552(16) Uani 1 1 d . . . H46 H 0.6547 -0.1046 0.7291 0.066 Uiso 1 1 calc R . . C47 C 0.6263(4) -0.0060(4) 0.6483(3) 0.0377(12) Uani 1 1 d . . . C48 C 0.6632(4) 0.0970(4) 0.6361(3) 0.0327(11) Uani 1 1 d . . . O5 O 0.9754(4) 0.6097(3) 0.1774(2) 0.0524(10) Uani 1 1 d . . . H5 H 0.9713 0.5698 0.2123 0.079 Uiso 1 1 calc R . . C49 C 0.9020(7) 0.5596(7) 0.1060(4) 0.084(2) Uani 1 1 d . . . H49A H 0.8221 0.5339 0.1172 0.126 Uiso 1 1 calc R . . H49B H 0.9332 0.5026 0.0850 0.126 Uiso 1 1 calc R . . H49C H 0.9005 0.6082 0.0670 0.126 Uiso 1 1 calc R . . O6 O 0.6476(9) 0.3212(7) 0.3919(4) 0.149(3) Uani 1 1 d . . . H6 H 0.6864 0.3280 0.4372 0.223 Uiso 1 1 calc R . . C50 C 0.6765(7) 0.2435(5) 0.3441(4) 0.0678(19) Uani 1 1 d . . . H50A H 0.7412 0.2728 0.3162 0.102 Uiso 1 1 calc R . . H50B H 0.6079 0.2095 0.3055 0.102 Uiso 1 1 calc R . . H50C H 0.7006 0.1938 0.3770 0.102 Uiso 1 1 calc R . . O7 O 0.3878(9) 0.0695(8) 0.0121(6) 0.190(4) Uiso 1 1 d . . . H7 H 0.4398 0.0353 0.0136 0.285 Uiso 1 1 d R . . C51 C 0.4178(12) 0.1572(11) 0.0717(8) 0.167(5) Uiso 1 1 d . . . H51A H 0.4450 0.1364 0.1227 0.250 Uiso 1 1 calc R . . H51B H 0.3484 0.1855 0.0762 0.250 Uiso 1 1 calc R . . H51C H 0.4804 0.2090 0.0567 0.250 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 Ru1 0.0369(3) 0.0347(3) 0.0286(3) 0.0003(2) 0.0155(3) 0.0043(3) Ru2 0.0287(3) 0.0377(3) 0.0261(3) -0.0069(2) 0.0080(2) 0.0057(2) Ni 0.0283(3) 0.0397(4) 0.0254(3) -0.0028(3) 0.0108(3) 0.0038(3) O2 0.057(3) 0.061(3) 0.042(2) 0.008(2) 0.013(2) 0.018(2) N1 0.043(3) 0.040(2) 0.035(2) -0.003(2) 0.017(2) -0.001(2) N2 0.042(3) 0.043(3) 0.032(2) -0.002(2) 0.012(2) 0.002(2) N3 0.052(3) 0.055(3) 0.044(3) -0.001(2) 0.006(2) 0.020(2) N4 0.031(2) 0.044(3) 0.035(2) -0.009(2) 0.0094(19) 0.000(2) N5 0.039(3) 0.061(3) 0.032(2) 0.002(2) 0.008(2) 0.018(2) N6 0.029(2) 0.055(3) 0.041(3) 0.002(2) 0.017(2) 0.006(2) N8 0.038(3) 0.042(3) 0.052(3) -0.015(2) 0.013(2) 0.003(2) C1 0.045(3) 0.036(3) 0.030(3) -0.004(2) 0.014(2) 0.004(2) C2 0.030(3) 0.046(3) 0.027(3) -0.001(2) 0.011(2) 0.006(2) C3 0.094(5) 0.051(4) 0.053(4) 0.005(3) 0.017(4) 0.032(4) C4 0.072(5) 0.048(4) 0.052(4) -0.006(3) 0.028(3) 0.003(3) C5 0.027(3) 0.074(4) 0.041(3) -0.019(3) 0.008(2) -0.004(3) C6 0.037(3) 0.107(5) 0.029(3) -0.004(3) 0.006(2) 0.030(3) C7 0.070(4) 0.061(4) 0.039(3) 0.017(3) 0.020(3) 0.020(3) C8 0.048(3) 0.063(4) 0.043(3) 0.011(3) 0.026(3) 0.007(3) C9 0.031(3) 0.075(4) 0.046(3) -0.008(3) 0.016(3) 0.011(3) C10 0.044(4) 0.077(4) 0.060(4) -0.018(4) 0.002(3) 0.031(3) C20 0.045(4) 0.061(4) 0.058(4) -0.012(3) 0.013(3) 0.014(3) C21 0.053(4) 0.080(5) 0.076(5) -0.008(4) 0.025(4) 0.019(4) C22 0.050(4) 0.069(4) 0.070(5) -0.013(4) 0.023(4) 0.014(3) C23 0.059(4) 0.069(4) 0.051(4) -0.003(3) 0.015(3) 0.004(3) C24 0.081(6) 0.112(7) 0.043(4) 0.005(4) 0.016(4) 0.017(5) C25 0.113(7) 0.132(8) 0.053(5) 0.026(5) 0.018(5) 0.042(6) C26 0.093(6) 0.104(6) 0.055(4) 0.024(4) 0.015(4) 0.035(5) C27 0.057(4) 0.058(4) 0.041(3) -0.004(3) 0.009(3) 0.007(3) C28 0.051(3) 0.046(3) 0.037(3) -0.011(3) 0.021(3) 0.004(3) Ru3 0.0284(3) 0.0301(3) 0.0358(3) -0.0044(2) 0.0122(2) 0.0054(2) O3 0.0283(18) 0.0377(19) 0.048(2) -0.0024(17) 0.0114(16) 0.0073(15) N9 0.068(4) 0.055(3) 0.046(3) 0.002(3) 0.019(3) 0.019(3) N10 0.034(2) 0.033(2) 0.034(2) -0.0013(18) 0.0124(19) 0.0077(18) C29 0.034(3) 0.038(3) 0.048(3) -0.002(3) 0.012(3) 0.009(2) C30 0.036(3) 0.040(3) 0.044(3) -0.004(2) 0.014(2) 0.006(2) C31 0.037(3) 0.040(3) 0.041(3) -0.004(2) 0.008(2) 0.003(2) C32 0.052(3) 0.034(3) 0.034(3) -0.002(2) 0.007(3) 0.013(3) C33 0.035(3) 0.040(3) 0.027(3) -0.001(2) 0.006(2) 0.013(2) C34 0.038(3) 0.042(3) 0.043(3) 0.005(3) 0.012(2) 0.013(2) C35 0.036(3) 0.049(3) 0.055(4) 0.008(3) 0.017(3) 0.018(3) C36 0.032(3) 0.040(3) 0.051(3) 0.004(3) 0.010(2) 0.007(2) C37 0.035(3) 0.033(3) 0.030(3) 0.002(2) 0.012(2) 0.007(2) C38 0.034(3) 0.039(3) 0.024(2) -0.001(2) 0.008(2) 0.009(2) Ru4 0.0250(3) 0.0280(3) 0.0227(3) 0.0015(2) 0.0096(2) 0.0085(2) O4 0.0362(19) 0.041(2) 0.0317(18) 0.0113(16) 0.0110(16) 0.0157(16) N11 0.033(2) 0.049(3) 0.035(2) 0.001(2) 0.016(2) 0.010(2) N12 0.023(2) 0.033(2) 0.032(2) -0.0051(18) 0.0132(17) 0.0087(17) C39 0.032(3) 0.029(2) 0.027(2) 0.001(2) 0.010(2) 0.008(2) C40 0.040(3) 0.037(3) 0.042(3) 0.003(2) 0.021(2) 0.013(2) C41 0.044(3) 0.041(3) 0.064(4) -0.008(3) 0.029(3) 0.000(3) C42 0.029(3) 0.059(4) 0.057(4) -0.026(3) 0.016(3) 0.000(3) C43 0.031(3) 0.071(4) 0.038(3) -0.008(3) 0.012(2) 0.016(3) C44 0.033(3) 0.109(6) 0.040(4) -0.008(4) 0.003(3) 0.021(4) C45 0.045(4) 0.138(7) 0.044(4) 0.029(4) 0.007(3) 0.035(4) C46 0.045(3) 0.085(5) 0.047(4) 0.027(3) 0.011(3) 0.027(3) C47 0.030(3) 0.056(3) 0.035(3) 0.008(3) 0.015(2) 0.023(3) C48 0.021(2) 0.054(3) 0.026(2) -0.001(2) 0.007(2) 0.014(2) O5 0.046(2) 0.067(3) 0.045(2) -0.004(2) 0.008(2) 0.019(2) C49 0.067(5) 0.112(7) 0.072(5) -0.012(5) -0.003(4) 0.036(5) O6 0.218(9) 0.198(8) 0.093(5) 0.044(5) 0.055(6) 0.154(7) C50 0.077(5) 0.066(4) 0.063(4) 0.001(4) 0.017(4) 0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1' 1.999(11) . ? Ru1 O1' 1.999(11) 2_775 ? Ru1 O1 2.015(5) 2_775 ? Ru1 O1 2.015(5) . ? Ru1 C1 2.067(5) . ? Ru1 C1 2.067(5) 2_775 ? Ru1 N7' 2.068(13) 2_775 ? Ru1 N7' 2.068(13) . ? Ru1 N7 2.079(7) . ? Ru1 N7 2.079(7) 2_775 ? Ru2 O2 2.005(4) . ? Ru2 O2 2.005(4) 2_665 ? Ru2 C2 2.053(5) . ? Ru2 C2 2.053(5) 2_665 ? Ru2 N8 2.055(4) 2_665 ? Ru2 N8 2.055(4) . ? Ni N2 2.054(5) . ? Ni N1 2.057(4) . ? Ni N4 2.087(4) . ? Ni N6 2.099(4) . ? Ni N3 2.128(5) . ? Ni N5 2.129(4) . ? O2 C27 1.326(7) . ? N1 C1 1.141(6) . ? N2 C2 1.150(6) . ? N3 C10 1.498(8) . ? N3 C3 1.499(8) . ? N4 C4 1.451(8) . ? N4 C5 1.473(7) . ? N5 C6 1.482(7) . ? N5 C7 1.488(7) . ? N6 C9 1.470(7) . ? N6 C8 1.470(7) . ? N8 C20 1.320(7) . ? N8 C28 1.385(7) . ? C3 C4 1.537(9) . ? C5 C6 1.500(9) . ? C7 C8 1.507(8) . ? C9 C10 1.513(9) . ? O1 C18 1.355(9) . ? N7 C11 1.325(10) . ? N7 C19 1.397(11) . ? C11 C12 1.407(12) . ? C12 C13 1.373(13) . ? C13 C14 1.357(12) . ? C14 C15 1.423(11) . ? C14 C19 1.446(10) . ? C15 C16 1.350(12) . ? C16 C17 1.402(12) . ? C17 C18 1.416(12) . ? C18 C19 1.358(12) . ? O1' C18' 1.335(13) . ? N7' C11' 1.322(14) . ? N7' C19' 1.406(14) . ? C11' C12' 1.401(17) . ? C12' C13' 1.388(18) . ? C13' C14' 1.376(16) . ? C14' C15' 1.402(14) . ? C14' C19' 1.437(13) . ? C15' C16' 1.363(16) . ? C16' C17' 1.373(16) . ? C17' C18' 1.415(15) . ? C18' C19' 1.366(15) . ? C20 C21 1.409(8) . ? C21 C22 1.364(9) . ? C22 C23 1.370(8) . ? C23 C24 1.381(9) . ? C23 C28 1.443(7) . ? C24 C25 1.387(10) . ? C25 C26 1.401(10) . ? C26 C27 1.400(8) . ? C27 C28 1.392(8) . ? Ru3 O3 2.010(3) 2_566 ? Ru3 O3 2.010(3) . ? Ru3 N10 2.072(4) . ? Ru3 N10 2.072(4) 2_566 ? Ru3 C29 2.076(6) 2_566 ? Ru3 C29 2.076(6) . ? O3 C37 1.335(6) . ? N9 C29 1.149(7) . ? N10 C30 1.315(6) . ? N10 C38 1.381(6) . ? C30 C31 1.404(7) . ? C31 C32 1.355(7) . ? C32 C33 1.413(7) . ? C33 C38 1.408(7) . ? C33 C34 1.414(7) . ? C34 C35 1.352(7) . ? C35 C36 1.416(7) . ? C36 C37 1.385(7) . ? C37 C38 1.425(7) . ? Ru4 O4 2.013(3) . ? Ru4 O4 2.013(3) 2_656 ? Ru4 N12 2.060(4) . ? Ru4 N12 2.060(4) 2_656 ? Ru4 C39 2.072(5) 2_656 ? Ru4 C39 2.072(5) . ? O4 C47 1.325(6) . ? N11 C39 1.142(6) . ? N12 C40 1.324(6) . ? N12 C48 1.372(6) . ? C40 C41 1.399(8) . ? C41 C42 1.361(9) . ? C42 C43 1.417(9) . ? C43 C44 1.403(9) . ? C43 C48 1.420(7) . ? C44 C45 1.350(10) . ? C45 C46 1.405(10) . ? C46 C47 1.405(7) . ? C47 C48 1.411(7) . ? O5 C49 1.433(8) . ? O6 C50 1.399(8) . ? O7 C51 1.448(13) . ? 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 O1' Ru1 O1' 180.000(2) . 2_775 ? O1' Ru1 O1 69.3(3) . 2_775 ? O1' Ru1 O1 110.7(3) 2_775 2_775 ? O1' Ru1 O1 110.7(3) . . ? O1' Ru1 O1 69.3(3) 2_775 . ? O1 Ru1 O1 180.000(1) 2_775 . ? O1' Ru1 C1 89.4(3) . . ? O1' Ru1 C1 90.6(3) 2_775 . ? O1 Ru1 C1 93.2(2) 2_775 . ? O1 Ru1 C1 86.8(2) . . ? O1' Ru1 C1 90.6(3) . 2_775 ? O1' Ru1 C1 89.4(3) 2_775 2_775 ? O1 Ru1 C1 86.8(2) 2_775 2_775 ? O1 Ru1 C1 93.2(2) . 2_775 ? C1 Ru1 C1 180.000(1) . 2_775 ? O1' Ru1 N7' 99.8(4) . 2_775 ? O1' Ru1 N7' 80.2(4) 2_775 2_775 ? O1 Ru1 N7' 30.5(3) 2_775 2_775 ? O1 Ru1 N7' 149.5(3) . 2_775 ? C1 Ru1 N7' 92.5(4) . 2_775 ? C1 Ru1 N7' 87.5(4) 2_775 2_775 ? O1' Ru1 N7' 80.2(4) . . ? O1' Ru1 N7' 99.8(4) 2_775 . ? O1 Ru1 N7' 149.5(3) 2_775 . ? O1 Ru1 N7' 30.5(3) . . ? C1 Ru1 N7' 87.5(4) . . ? C1 Ru1 N7' 92.5(4) 2_775 . ? N7' Ru1 N7' 180.0(7) 2_775 . ? O1' Ru1 N7 30.1(3) . . ? O1' Ru1 N7 149.9(3) 2_775 . ? O1 Ru1 N7 99.3(2) 2_775 . ? O1 Ru1 N7 80.7(2) . . ? C1 Ru1 N7 88.0(2) . . ? C1 Ru1 N7 92.0(2) 2_775 . ? N7' Ru1 N7 129.8(4) 2_775 . ? N7' Ru1 N7 50.2(4) . . ? O1' Ru1 N7 149.9(3) . 2_775 ? O1' Ru1 N7 30.1(3) 2_775 2_775 ? O1 Ru1 N7 80.7(2) 2_775 2_775 ? O1 Ru1 N7 99.3(2) . 2_775 ? C1 Ru1 N7 92.0(2) . 2_775 ? C1 Ru1 N7 88.0(2) 2_775 2_775 ? N7' Ru1 N7 50.2(4) 2_775 2_775 ? N7' Ru1 N7 129.8(4) . 2_775 ? N7 Ru1 N7 180.0(3) . 2_775 ? O2 Ru2 O2 180.000(1) . 2_665 ? O2 Ru2 C2 87.34(18) . . ? O2 Ru2 C2 92.66(18) 2_665 . ? O2 Ru2 C2 92.66(18) . 2_665 ? O2 Ru2 C2 87.34(18) 2_665 2_665 ? C2 Ru2 C2 180.000(1) . 2_665 ? O2 Ru2 N8 97.75(18) . 2_665 ? O2 Ru2 N8 82.25(18) 2_665 2_665 ? C2 Ru2 N8 91.85(18) . 2_665 ? C2 Ru2 N8 88.15(18) 2_665 2_665 ? O2 Ru2 N8 82.25(18) . . ? O2 Ru2 N8 97.75(18) 2_665 . ? C2 Ru2 N8 88.15(18) . . ? C2 Ru2 N8 91.85(18) 2_665 . ? N8 Ru2 N8 180.0(2) 2_665 . ? N2 Ni N1 88.15(17) . . ? N2 Ni N4 177.24(19) . . ? N1 Ni N4 90.52(16) . . ? N2 Ni N6 83.95(17) . . ? N1 Ni N6 172.09(17) . . ? N4 Ni N6 97.38(17) . . ? N2 Ni N3 96.58(18) . . ? N1 Ni N3 96.97(19) . . ? N4 Ni N3 81.17(18) . . ? N6 Ni N3 84.06(19) . . ? N2 Ni N5 101.22(18) . . ? N1 Ni N5 98.96(18) . . ? N4 Ni N5 81.38(18) . . ? N6 Ni N5 82.54(18) . . ? N3 Ni N5 156.39(17) . . ? C27 O2 Ru2 112.0(4) . . ? C1 N1 Ni 166.2(5) . . ? C2 N2 Ni 163.7(4) . . ? C10 N3 C3 112.1(5) . . ? C10 N3 Ni 104.7(4) . . ? C3 N3 Ni 109.1(4) . . ? C4 N4 C5 118.2(5) . . ? C4 N4 Ni 105.6(3) . . ? C5 N4 Ni 104.2(3) . . ? C6 N5 C7 112.4(4) . . ? C6 N5 Ni 108.4(4) . . ? C7 N5 Ni 105.9(3) . . ? C9 N6 C8 117.1(4) . . ? C9 N6 Ni 108.1(4) . . ? C8 N6 Ni 108.9(3) . . ? C20 N8 C28 120.7(5) . . ? C20 N8 Ru2 130.0(4) . . ? C28 N8 Ru2 109.2(3) . . ? N1 C1 Ru1 173.4(5) . . ? N2 C2 Ru2 172.2(4) . . ? N3 C3 C4 110.6(5) . . ? N4 C4 C3 107.1(5) . . ? N4 C5 C6 107.1(4) . . ? N5 C6 C5 111.5(5) . . ? N5 C7 C8 110.4(5) . . ? N6 C8 C7 106.8(4) . . ? N6 C9 C10 107.7(4) . . ? N3 C10 C9 111.6(5) . . ? C18 O1 Ru1 112.5(5) . . ? C11 N7 C19 121.8(8) . . ? C11 N7 Ru1 127.6(6) . . ? C19 N7 Ru1 110.5(6) . . ? N7 C11 C12 120.5(10) . . ? C13 C12 C11 120.4(12) . . ? C14 C13 C12 119.4(11) . . ? C13 C14 C15 125.2(9) . . ? C13 C14 C19 121.0(9) . . ? C15 C14 C19 113.7(9) . . ? C16 C15 C14 117.8(10) . . ? C15 C16 C17 128.9(12) . . ? C16 C17 C18 114.4(10) . . ? O1 C18 C19 119.8(8) . . ? O1 C18 C17 122.0(8) . . ? C19 C18 C17 118.2(8) . . ? C18 C19 N7 116.3(8) . . ? C18 C19 C14 127.0(9) . . ? N7 C19 C14 116.7(9) . . ? C18' O1' Ru1 115.0(9) . . ? C11' N7' C19' 122.4(13) . . ? C11' N7' Ru1 128.1(11) . . ? C19' N7' Ru1 109.4(8) . . ? N7' C11' C12' 119.1(15) . . ? C13' C12' C11' 121.5(19) . . ? C14' C13' C12' 118.7(18) . . ? C13' C14' C15' 123.9(14) . . ? C13' C14' C19' 119.9(13) . . ? C15' C14' C19' 116.0(12) . . ? C16' C15' C14' 118.4(15) . . ? C15' C16' C17' 125.9(16) . . ? C16' C17' C18' 117.5(14) . . ? O1' C18' C19' 116.5(12) . . ? O1' C18' C17' 126.0(13) . . ? C19' C18' C17' 117.5(12) . . ? C18' C19' N7' 117.9(11) . . ? C18' C19' C14' 124.6(12) . . ? N7' C19' C14' 117.5(12) . . ? N8 C20 C21 120.6(6) . . ? C22 C21 C20 120.1(6) . . ? C21 C22 C23 121.2(6) . . ? C22 C23 C24 125.7(7) . . ? C22 C23 C28 117.5(6) . . ? C24 C23 C28 116.8(6) . . ? C23 C24 C25 120.1(7) . . ? C24 C25 C26 123.0(7) . . ? C25 C26 C27 118.6(7) . . ? O2 C27 C28 119.2(5) . . ? O2 C27 C26 122.5(6) . . ? C28 C27 C26 118.3(6) . . ? N8 C28 C27 117.1(5) . . ? N8 C28 C23 119.8(5) . . ? C27 C28 C23 123.1(6) . . ? O3 Ru3 O3 180.000(1) 2_566 . ? O3 Ru3 N10 98.83(15) 2_566 . ? O3 Ru3 N10 81.17(15) . . ? O3 Ru3 N10 81.17(15) 2_566 2_566 ? O3 Ru3 N10 98.83(15) . 2_566 ? N10 Ru3 N10 180.000(1) . 2_566 ? O3 Ru3 C29 89.58(17) 2_566 2_566 ? O3 Ru3 C29 90.42(17) . 2_566 ? N10 Ru3 C29 91.65(18) . 2_566 ? N10 Ru3 C29 88.35(18) 2_566 2_566 ? O3 Ru3 C29 90.42(17) 2_566 . ? O3 Ru3 C29 89.58(17) . . ? N10 Ru3 C29 88.35(18) . . ? N10 Ru3 C29 91.65(18) 2_566 . ? C29 Ru3 C29 180.000(1) 2_566 . ? C37 O3 Ru3 113.3(3) . . ? C30 N10 C38 118.6(4) . . ? C30 N10 Ru3 130.4(3) . . ? C38 N10 Ru3 111.0(3) . . ? N9 C29 Ru3 178.7(5) . . ? N10 C30 C31 122.6(5) . . ? C32 C31 C30 119.6(5) . . ? C31 C32 C33 120.2(5) . . ? C38 C33 C34 118.1(5) . . ? C38 C33 C32 116.7(4) . . ? C34 C33 C32 125.1(5) . . ? C35 C34 C33 119.8(5) . . ? C34 C35 C36 122.4(5) . . ? C37 C36 C35 119.9(5) . . ? O3 C37 C36 124.2(4) . . ? O3 C37 C38 118.3(4) . . ? C36 C37 C38 117.5(4) . . ? N10 C38 C33 122.2(4) . . ? N10 C38 C37 115.6(4) . . ? C33 C38 C37 122.1(4) . . ? O4 Ru4 O4 180.000(1) . 2_656 ? O4 Ru4 N12 80.97(15) . . ? O4 Ru4 N12 99.03(15) 2_656 . ? O4 Ru4 N12 99.03(15) . 2_656 ? O4 Ru4 N12 80.97(15) 2_656 2_656 ? N12 Ru4 N12 180.000(1) . 2_656 ? O4 Ru4 C39 89.27(16) . 2_656 ? O4 Ru4 C39 90.73(16) 2_656 2_656 ? N12 Ru4 C39 86.37(16) . 2_656 ? N12 Ru4 C39 93.63(16) 2_656 2_656 ? O4 Ru4 C39 90.73(16) . . ? O4 Ru4 C39 89.27(16) 2_656 . ? N12 Ru4 C39 93.63(16) . . ? N12 Ru4 C39 86.37(16) 2_656 . ? C39 Ru4 C39 180.0(2) 2_656 . ? C47 O4 Ru4 112.8(3) . . ? C40 N12 C48 118.9(5) . . ? C40 N12 Ru4 129.7(4) . . ? C48 N12 Ru4 111.2(3) . . ? N11 C39 Ru4 176.4(4) . . ? N12 C40 C41 122.0(5) . . ? C42 C41 C40 120.6(6) . . ? C41 C42 C43 119.2(5) . . ? C44 C43 C42 124.8(6) . . ? C44 C43 C48 118.1(6) . . ? C42 C43 C48 117.1(5) . . ? C45 C44 C43 119.7(6) . . ? C44 C45 C46 123.1(6) . . ? C47 C46 C45 119.6(6) . . ? O4 C47 C46 124.0(5) . . ? O4 C47 C48 118.9(4) . . ? C46 C47 C48 117.0(5) . . ? N12 C48 C47 115.5(4) . . ? N12 C48 C43 122.0(5) . . ? C47 C48 C43 122.4(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.559 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.119