# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_cc01emm1n _database_code_depnum_ccdc_archive 'CCDC 831082' #TrackingRef 'web_deposit_cif_file_0_UrbanoDiaz_ #1308743264.ccdc_depost datos1.cif' _audit_creation_date 2011-03-27T21:28:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common EM247 _chemical_formula_moiety 'C41 H40 Cl2 N2 O Ru, 0.59(C2 H5 O), 0.41(C H2 Cl2)' _chemical_formula_sum 'C42.59 H43.77 Cl2.82 N2 O1.59 Ru' _chemical_formula_weight 810.06 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 20.7100(5) _cell_length_b 10.3621(3) _cell_length_c 18.7711(4) _cell_angle_alpha 90 _cell_angle_beta 107.433(1) _cell_angle_gamma 90 _cell_volume 3843.23(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7997 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 32.27 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672.8 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7846 _exptl_absorpt_correction_T_max 0.8959 _exptl_absorpt_process_details 'BRUKER AXS - SADABS' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Bruker X8 kappa APEXII CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_unetI/netI 0.0203 _diffrn_reflns_number 76624 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 11645 _reflns_number_gt 10381 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 v2011.2-3 (Bruker AXS, 2011)' _computing_cell_refinement 'APEX2 v2011.2-3 (Bruker AXS, 2011)' _computing_data_reduction 'APEX2 v2011.2-3 (Bruker AXS, 2011)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0248P)^2^+3.1946P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11645 _refine_ls_number_parameters 589 _refine_ls_number_restraints 375 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.001 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.156638(5) 0.013353(10) 0.234740(6) 0.01104(3) Uani 1 1 d . . . Cl2 Cl 0.187580(17) -0.15170(3) 0.166828(19) 0.01826(7) Uani 1 1 d . . . Cl3 Cl 0.130584(16) 0.11543(3) 0.334532(18) 0.01730(7) Uani 1 1 d . . . C1 C 0.24621(6) 0.09800(13) 0.25569(7) 0.0128(2) Uani 1 1 d . A . N2 N 0.26895(5) 0.20906(11) 0.23070(6) 0.0131(2) Uani 1 1 d . . . C3 C 0.33786(7) 0.22384(13) 0.26363(8) 0.0154(2) Uani 1 1 d . . . C4 C 0.35953(7) 0.12140(13) 0.30987(8) 0.0154(2) Uani 1 1 d . A . N5 N 0.30410(6) 0.04453(11) 0.30510(7) 0.0140(2) Uani 1 1 d . . . C6 C 0.39358(7) 0.31289(14) 0.26817(8) 0.0174(3) Uani 1 1 d . . . C7 C 0.40343(8) 0.42876(15) 0.23783(9) 0.0226(3) Uani 1 1 d . . . H7 H 0.3671 0.4715 0.2025 0.027 Uiso 1 1 calc R . . C8 C 0.46972(8) 0.48354(16) 0.26064(11) 0.0286(4) Uani 1 1 d . . . H8 H 0.4768 0.5645 0.2405 0.034 Uiso 1 1 calc R . . C9 C 0.52357(8) 0.42369(17) 0.31054(11) 0.0288(4) Uani 1 1 d . . . H9 H 0.5670 0.4628 0.3235 0.035 Uiso 1 1 calc R . . C10 C 0.51480(7) 0.30337(16) 0.34312(9) 0.0238(3) Uani 1 1 d . . . C11 C 0.56464(8) 0.22971(18) 0.39652(10) 0.0302(4) Uani 1 1 d . . . H11 H 0.6100 0.2598 0.4134 0.036 Uiso 1 1 calc R . . C12 C 0.54785(8) 0.11625(19) 0.42376(10) 0.0310(4) Uani 1 1 d . . . H12 H 0.5822 0.0695 0.4593 0.037 Uiso 1 1 calc R . . C13 C 0.48057(7) 0.06518(17) 0.40082(9) 0.0242(3) Uani 1 1 d . A . H13 H 0.4701 -0.0136 0.4208 0.029 Uiso 1 1 calc R . . C14 C 0.43180(7) 0.13368(14) 0.34910(8) 0.0179(3) Uani 1 1 d . . . C15 C 0.44965(7) 0.25201(14) 0.32109(8) 0.0184(3) Uani 1 1 d . A . C16 C 0.22843(6) 0.29969(13) 0.17782(8) 0.0133(2) Uani 1 1 d . . . C17 C 0.21993(7) 0.27917(13) 0.10219(8) 0.0154(2) Uani 1 1 d . . . C18 C 0.17798(7) 0.36428(15) 0.05139(8) 0.0194(3) Uani 1 1 d . . . H18 H 0.1702 0.3510 -0.0006 0.023 Uiso 1 1 calc R . . C19 C 0.14728(8) 0.46833(15) 0.07539(9) 0.0218(3) Uani 1 1 d . . . C20 C 0.15902(8) 0.48752(14) 0.15167(9) 0.0205(3) Uani 1 1 d . . . H20 H 0.1392 0.5599 0.1682 0.025 Uiso 1 1 calc R . . C21 C 0.19922(7) 0.40309(13) 0.20442(8) 0.0158(3) Uani 1 1 d . . . C22 C 0.25351(8) 0.16617(15) 0.07721(8) 0.0205(3) Uani 1 1 d . . . H22A H 0.3025 0.1707 0.1010 0.031 Uiso 1 1 calc R . . H22B H 0.2438 0.1688 0.0228 0.031 Uiso 1 1 calc R . . H22C H 0.2360 0.0856 0.0916 0.031 Uiso 1 1 calc R . . C23 C 0.10281(10) 0.56046(19) 0.01930(11) 0.0361(4) Uani 1 1 d . . . H23A H 0.0697 0.5998 0.0406 0.054 Uiso 1 1 calc R . . H23B H 0.0790 0.5132 -0.0262 0.054 Uiso 1 1 calc R . . H23C H 0.1309 0.6281 0.0072 0.054 Uiso 1 1 calc R . . C24 C 0.20915(8) 0.42009(15) 0.28659(8) 0.0216(3) Uani 1 1 d . . . H24A H 0.1926 0.5054 0.2955 0.032 Uiso 1 1 calc R . . H24B H 0.2574 0.4128 0.3140 0.032 Uiso 1 1 calc R . . H24C H 0.1839 0.3532 0.3038 0.032 Uiso 1 1 calc R . . C26 C 0.3010(9) -0.0577(8) 0.3541(6) 0.0144(13) Uani 0.61(2) 1 d PDU A 1 C27 C 0.2899(6) -0.0252(7) 0.4224(4) 0.0153(9) Uani 0.61(2) 1 d PDU A 1 C28 C 0.2784(4) -0.1265(7) 0.4660(4) 0.0234(10) Uani 0.61(2) 1 d PDU A 1 H28 H 0.2675 -0.1071 0.5105 0.028 Uiso 0.61(2) 1 calc PR A 1 C29 C 0.2823(3) -0.2541(7) 0.4465(4) 0.0262(12) Uani 0.61(2) 1 d PDU A 1 C30 C 0.3032(5) -0.2817(7) 0.3847(5) 0.0276(12) Uani 0.61(2) 1 d PDU A 1 H30 H 0.3109 -0.3690 0.3741 0.033 Uiso 0.61(2) 1 calc PR A 1 C31 C 0.3133(6) -0.1847(8) 0.3373(5) 0.0209(12) Uani 0.61(2) 1 d PDU A 1 C32 C 0.2946(6) 0.1117(7) 0.4486(5) 0.0214(11) Uani 0.61(2) 1 d PDU A 1 H32A H 0.2929 0.1143 0.5002 0.032 Uiso 0.61(2) 1 calc PR A 1 H32B H 0.2566 0.1612 0.4166 0.032 Uiso 0.61(2) 1 calc PR A 1 H32C H 0.3373 0.1494 0.4463 0.032 Uiso 0.61(2) 1 calc PR A 1 C33 C 0.2648(3) -0.3627(8) 0.4915(4) 0.0441(16) Uani 0.61(2) 1 d PDU A 1 H33A H 0.2598 -0.3281 0.5381 0.066 Uiso 0.61(2) 1 calc PR A 1 H33B H 0.3011 -0.4272 0.5029 0.066 Uiso 0.61(2) 1 calc PR A 1 H33C H 0.2223 -0.4031 0.4625 0.066 Uiso 0.61(2) 1 calc PR A 1 C34 C 0.3414(7) -0.2176(12) 0.2740(6) 0.0271(13) Uani 0.61(2) 1 d PDU A 1 H34A H 0.3350 -0.1442 0.2397 0.041 Uiso 0.61(2) 1 calc PR A 1 H34B H 0.3177 -0.2931 0.2471 0.041 Uiso 0.61(2) 1 calc PR A 1 H34C H 0.3898 -0.2369 0.2942 0.041 Uiso 0.61(2) 1 calc PR A 1 C76 C 0.3053(14) -0.0740(14) 0.3504(10) 0.018(2) Uani 0.39(2) 1 d PDU A 2 C77 C 0.2914(10) -0.0563(14) 0.4182(8) 0.026(2) Uani 0.39(2) 1 d PDU A 2 C78 C 0.2847(7) -0.1672(17) 0.4573(7) 0.035(2) Uani 0.39(2) 1 d PDU A 2 H78 H 0.2743 -0.1589 0.5031 0.042 Uiso 0.39(2) 1 calc PR A 2 C79 C 0.2925(9) -0.2870(14) 0.4316(7) 0.042(3) Uani 0.39(2) 1 d PDU A 2 C80 C 0.3117(10) -0.2987(12) 0.3678(9) 0.038(3) Uani 0.39(2) 1 d PDU A 2 H80 H 0.3199 -0.3827 0.3521 0.046 Uiso 0.39(2) 1 calc PR A 2 C81 C 0.3195(9) -0.1928(9) 0.3248(8) 0.019(2) Uani 0.39(2) 1 d PDU A 2 C82 C 0.2906(9) 0.0761(16) 0.4497(9) 0.031(2) Uani 0.39(2) 1 d PDU A 2 H82A H 0.3346 0.1174 0.4568 0.046 Uiso 0.39(2) 1 calc PR A 2 H82B H 0.2814 0.0699 0.4978 0.046 Uiso 0.39(2) 1 calc PR A 2 H82C H 0.2551 0.1276 0.4151 0.046 Uiso 0.39(2) 1 calc PR A 2 C83 C 0.2834(12) -0.4063(17) 0.4746(8) 0.084(6) Uani 0.39(2) 1 d PDU A 2 H83A H 0.2795 -0.3805 0.5234 0.126 Uiso 0.39(2) 1 calc PR A 2 H83B H 0.3225 -0.4633 0.4817 0.126 Uiso 0.39(2) 1 calc PR A 2 H83C H 0.2422 -0.4519 0.4464 0.126 Uiso 0.39(2) 1 calc PR A 2 C84 C 0.3446(11) -0.2072(19) 0.2584(10) 0.031(2) Uani 0.39(2) 1 d PDU A 2 H84A H 0.3186 -0.1504 0.2183 0.047 Uiso 0.39(2) 1 calc PR A 2 H84B H 0.3389 -0.2970 0.2411 0.047 Uiso 0.39(2) 1 calc PR A 2 H84C H 0.3926 -0.1838 0.2721 0.047 Uiso 0.39(2) 1 calc PR A 2 C35 C 0.10536(6) 0.11125(13) 0.15686(7) 0.0137(2) Uani 1 1 d . . . H35 H 0.1235 0.1865 0.1412 0.016 Uiso 1 1 calc R . . C36 C 0.03650(6) 0.07096(13) 0.11989(7) 0.0129(2) Uani 1 1 d . . . C37 C -0.00561(7) 0.13284(14) 0.05625(8) 0.0161(3) Uani 1 1 d . . . H37 H 0.0102 0.2070 0.0368 0.019 Uiso 1 1 calc R . . C38 C -0.07010(7) 0.08633(15) 0.02170(8) 0.0195(3) Uani 1 1 d . . . H38 H -0.0986 0.1284 -0.0213 0.023 Uiso 1 1 calc R . . C39 C -0.09286(7) -0.02239(15) 0.05039(8) 0.0207(3) Uani 1 1 d . . . H39 H -0.1369 -0.0545 0.0260 0.025 Uiso 1 1 calc R . . C40 C -0.05295(7) -0.08568(14) 0.11387(8) 0.0184(3) Uani 1 1 d . . . H40 H -0.0693 -0.1594 0.1332 0.022 Uiso 1 1 calc R . . C41 C 0.01148(7) -0.03736(13) 0.14795(7) 0.0143(2) Uani 1 1 d . . . O42 O 0.05755(5) -0.08929(9) 0.21007(5) 0.01471(18) Uani 1 1 d . . . C43 C 0.03430(7) -0.18315(14) 0.25599(8) 0.0178(3) Uani 1 1 d . . . H43 H 0.0074 -0.2524 0.2231 0.021 Uiso 1 1 calc R . . C44 C 0.09801(8) -0.24144(15) 0.30854(9) 0.0222(3) Uani 1 1 d . . . H44A H 0.1261 -0.2768 0.2795 0.033 Uiso 1 1 calc R . . H44B H 0.0857 -0.3106 0.3377 0.033 Uiso 1 1 calc R . . H44C H 0.1234 -0.1746 0.3424 0.033 Uiso 1 1 calc R . . C45 C -0.00999(8) -0.11495(16) 0.29564(9) 0.0230(3) Uani 1 1 d . . . H45A H 0.0167 -0.0491 0.3292 0.035 Uiso 1 1 calc R . . H45B H -0.0270 -0.1779 0.3246 0.035 Uiso 1 1 calc R . . H45C H -0.0482 -0.0739 0.2587 0.035 Uiso 1 1 calc R . . C50 C 0.4767(5) 0.1601(9) 0.0434(6) 0.050(2) Uani 0.4015(18) 1 d PU B 1 H50A H 0.5096 0.0950 0.0714 0.060 Uiso 0.4015(18) 1 calc PR B 1 H50B H 0.4996 0.2150 0.0151 0.060 Uiso 0.4015(18) 1 calc PR B 1 Cl51 Cl 0.44911(7) 0.25719(12) 0.10709(7) 0.0406(4) Uani 0.4015(18) 1 d PU B 1 Cl52 Cl 0.40586(9) 0.08127(17) -0.01973(9) 0.0580(5) Uani 0.4015(18) 1 d PU B 1 O60 O 0.5000 0.0000 0.0000 0.0792(14) Uani 0.5985(18) 2 d SPDU B -2 C61 C 0.5240(5) 0.1082(11) 0.0491(5) 0.076(2) Uani 0.2992(9) 1 d PDU B -2 H61A H 0.5478 0.0708 0.0985 0.091 Uiso 0.2992(9) 1 calc PR B -2 H61B H 0.5591 0.1504 0.0312 0.091 Uiso 0.2992(9) 1 calc PR B -2 C62 C 0.4885(9) 0.1965(17) 0.0612(13) 0.098(5) Uani 0.2992(9) 1 d PDU B -2 H62A H 0.4451 0.1982 0.0216 0.147 Uiso 0.2992(9) 1 calc PR B -2 H62B H 0.5118 0.2791 0.0622 0.147 Uiso 0.2992(9) 1 calc PR B -2 H62C H 0.4804 0.1822 0.1094 0.147 Uiso 0.2992(9) 1 calc PR B -2 C63 C 0.5432(5) -0.0962(11) -0.0118(7) 0.073(2) Uani 0.2992(9) 1 d PDU B -2 H63A H 0.5831 -0.0469 -0.0153 0.087 Uiso 0.2992(9) 1 calc PR B -2 H63B H 0.5584 -0.1409 0.0370 0.087 Uiso 0.2992(9) 1 calc PR B -2 C64 C 0.5387(9) -0.187(2) -0.0583(13) 0.083(4) Uani 0.2992(9) 1 d PDU B -2 H64A H 0.5530 -0.2679 -0.0314 0.124 Uiso 0.2992(9) 1 calc PR B -2 H64B H 0.5678 -0.1678 -0.0896 0.124 Uiso 0.2992(9) 1 calc PR B -2 H64C H 0.4916 -0.1946 -0.0898 0.124 Uiso 0.2992(9) 1 calc PR B -2 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 0.00854(5) 0.01182(5) 0.01193(5) 0.00140(4) 0.00179(3) 0.00060(3) Cl2 0.01682(15) 0.01774(15) 0.01873(15) -0.00295(12) 0.00305(12) 0.00321(11) Cl3 0.01548(14) 0.02041(16) 0.01615(14) -0.00178(12) 0.00496(12) 0.00102(11) C1 0.0106(5) 0.0139(6) 0.0134(6) -0.0004(5) 0.0030(5) 0.0020(4) N2 0.0096(5) 0.0128(5) 0.0155(5) 0.0009(4) 0.0017(4) 0.0006(4) C3 0.0100(6) 0.0152(6) 0.0198(6) -0.0003(5) 0.0028(5) -0.0003(5) C4 0.0097(6) 0.0165(6) 0.0190(6) 0.0002(5) 0.0026(5) 0.0000(5) N5 0.0101(5) 0.0148(5) 0.0160(5) 0.0025(4) 0.0021(4) 0.0005(4) C6 0.0123(6) 0.0165(6) 0.0233(7) -0.0021(5) 0.0053(5) -0.0010(5) C7 0.0170(7) 0.0183(7) 0.0318(8) 0.0004(6) 0.0063(6) -0.0013(5) C8 0.0223(7) 0.0203(7) 0.0445(10) 0.0003(7) 0.0119(7) -0.0070(6) C9 0.0156(7) 0.0271(8) 0.0431(10) -0.0042(7) 0.0079(7) -0.0074(6) C10 0.0126(6) 0.0259(8) 0.0316(8) -0.0044(6) 0.0045(6) -0.0030(5) C11 0.0108(6) 0.0372(9) 0.0371(9) -0.0016(7) -0.0011(6) -0.0029(6) C12 0.0124(7) 0.0400(10) 0.0336(9) 0.0045(7) -0.0037(6) 0.0016(6) C13 0.0140(6) 0.0285(8) 0.0265(8) 0.0043(6) 0.0008(6) 0.0007(6) C14 0.0104(6) 0.0208(7) 0.0214(7) -0.0007(5) 0.0028(5) 0.0001(5) C15 0.0118(6) 0.0194(7) 0.0230(7) -0.0023(5) 0.0038(5) -0.0007(5) C16 0.0096(5) 0.0116(6) 0.0173(6) 0.0024(5) 0.0019(5) 0.0000(4) C17 0.0131(6) 0.0144(6) 0.0193(6) 0.0010(5) 0.0054(5) -0.0015(5) C18 0.0175(6) 0.0217(7) 0.0184(7) 0.0050(5) 0.0043(5) -0.0013(5) C19 0.0190(7) 0.0194(7) 0.0260(7) 0.0100(6) 0.0051(6) 0.0031(5) C20 0.0194(7) 0.0137(6) 0.0290(8) 0.0038(5) 0.0084(6) 0.0038(5) C21 0.0132(6) 0.0127(6) 0.0210(7) -0.0003(5) 0.0045(5) -0.0005(4) C22 0.0206(7) 0.0213(7) 0.0203(7) -0.0029(5) 0.0072(6) 0.0014(5) C23 0.0353(9) 0.0337(10) 0.0357(10) 0.0178(8) 0.0056(8) 0.0138(8) C24 0.0223(7) 0.0190(7) 0.0229(7) -0.0044(6) 0.0059(6) 0.0022(5) C26 0.007(3) 0.0117(17) 0.021(2) 0.0027(15) -0.0011(15) 0.0009(15) C27 0.0082(14) 0.023(2) 0.0135(16) 0.0065(17) 0.0010(11) 0.002(2) C28 0.0105(14) 0.037(3) 0.0208(18) 0.0090(18) 0.0021(11) -0.0004(18) C29 0.0133(15) 0.031(3) 0.029(3) 0.014(2) -0.0021(14) -0.0059(18) C30 0.0226(18) 0.0185(19) 0.033(4) 0.007(2) -0.004(2) -0.0036(15) C31 0.0115(19) 0.026(2) 0.022(2) -0.0012(15) 0.0012(16) 0.0012(13) C32 0.0182(18) 0.026(2) 0.0190(19) -0.006(2) 0.0041(13) 0.000(2) C33 0.026(2) 0.048(3) 0.049(3) 0.026(2) -0.0022(16) -0.0157(18) C34 0.026(2) 0.023(2) 0.029(3) -0.001(2) 0.002(2) 0.0086(17) C76 0.009(3) 0.023(5) 0.021(4) 0.015(3) 0.004(3) 0.003(4) C77 0.011(3) 0.030(5) 0.033(4) 0.003(3) -0.001(2) 0.000(4) C78 0.021(4) 0.058(6) 0.021(3) 0.021(4) -0.003(2) -0.013(5) C79 0.044(6) 0.036(5) 0.029(5) 0.017(4) -0.014(3) -0.025(4) C80 0.042(7) 0.022(4) 0.031(5) 0.010(3) -0.018(3) -0.013(3) C81 0.016(4) 0.005(3) 0.029(5) 0.009(2) -0.004(3) -0.002(2) C82 0.018(3) 0.050(6) 0.022(3) 0.004(5) 0.001(2) 0.005(5) C83 0.116(11) 0.065(7) 0.044(5) 0.034(5) -0.018(6) -0.061(7) C84 0.026(3) 0.021(4) 0.042(7) -0.006(4) 0.004(4) 0.009(3) C35 0.0114(6) 0.0143(6) 0.0152(6) 0.0013(5) 0.0039(5) 0.0005(4) C36 0.0109(5) 0.0145(6) 0.0130(6) -0.0009(5) 0.0029(5) 0.0015(4) C37 0.0164(6) 0.0170(6) 0.0143(6) 0.0006(5) 0.0038(5) 0.0042(5) C38 0.0166(6) 0.0230(7) 0.0149(6) -0.0027(5) -0.0013(5) 0.0059(5) C39 0.0125(6) 0.0250(7) 0.0210(7) -0.0056(6) -0.0004(5) -0.0002(5) C40 0.0131(6) 0.0193(7) 0.0214(7) -0.0021(5) 0.0031(5) -0.0024(5) C41 0.0114(6) 0.0164(6) 0.0140(6) 0.0000(5) 0.0022(5) 0.0014(5) O42 0.0102(4) 0.0167(5) 0.0155(4) 0.0045(4) 0.0013(3) -0.0018(3) C43 0.0156(6) 0.0160(6) 0.0222(7) 0.0052(5) 0.0060(5) -0.0029(5) C44 0.0204(7) 0.0209(7) 0.0252(7) 0.0091(6) 0.0068(6) 0.0028(5) C45 0.0191(7) 0.0276(8) 0.0247(7) 0.0069(6) 0.0102(6) 0.0004(6) C50 0.065(5) 0.037(4) 0.069(5) -0.011(3) 0.052(4) -0.021(3) Cl51 0.0434(7) 0.0288(6) 0.0456(7) -0.0058(5) 0.0070(5) 0.0037(5) Cl52 0.0629(10) 0.0589(10) 0.0529(9) -0.0203(7) 0.0185(7) -0.0073(7) O60 0.075(3) 0.077(3) 0.077(3) 0.040(2) 0.011(2) -0.006(2) C61 0.057(4) 0.107(5) 0.052(4) 0.030(3) -0.003(3) 0.002(3) C62 0.094(11) 0.059(6) 0.116(9) 0.043(5) -0.007(9) 0.011(7) C63 0.053(4) 0.082(4) 0.079(5) 0.037(3) 0.013(4) -0.018(3) C64 0.066(8) 0.089(8) 0.086(9) 0.032(5) 0.010(8) -0.006(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C35 1.8341(13) . ? Ru1 C1 1.9820(13) . ? Ru1 O42 2.2333(9) . ? Ru1 Cl2 2.3346(3) . ? Ru1 Cl3 2.3504(3) . ? C1 N2 1.3778(17) . ? C1 N5 1.3923(16) . ? N2 C3 1.3832(16) . ? N2 C16 1.4397(16) . ? C3 C4 1.3595(19) . ? C3 C6 1.4601(19) . ? C4 N5 1.3780(17) . ? C4 C14 1.4621(18) . ? N5 C26 1.417(10) . ? N5 C76 1.490(14) . ? C6 C7 1.370(2) . ? C6 C15 1.429(2) . ? C7 C8 1.428(2) . ? C7 H7 0.9500 . ? C8 C9 1.371(2) . ? C8 H8 0.9500 . ? C9 C10 1.424(2) . ? C9 H9 0.9500 . ? C10 C15 1.3930(19) . ? C10 C11 1.426(2) . ? C11 C12 1.368(3) . ? C11 H11 0.9500 . ? C12 C13 1.431(2) . ? C12 H12 0.9500 . ? C13 C14 1.371(2) . ? C13 H13 0.9500 . ? C14 C15 1.426(2) . ? C16 C17 1.3935(19) . ? C16 C21 1.3944(19) . ? C17 C18 1.3948(19) . ? C17 C22 1.507(2) . ? C18 C19 1.393(2) . ? C18 H18 0.9500 . ? C19 C20 1.393(2) . ? C19 C23 1.512(2) . ? C20 C21 1.395(2) . ? C20 H20 0.9500 . ? C21 C24 1.504(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 C31 1.395(7) . ? C26 C27 1.409(7) . ? C27 C28 1.396(6) . ? C27 C32 1.495(6) . ? C28 C29 1.382(6) . ? C28 H28 0.9500 . ? C29 C30 1.384(6) . ? C29 C33 1.515(6) . ? C30 C31 1.399(7) . ? C30 H30 0.9500 . ? C31 C34 1.509(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C76 C81 1.384(10) . ? C76 C77 1.397(11) . ? C77 C78 1.394(10) . ? C77 C82 1.496(10) . ? C78 C79 1.359(10) . ? C78 H78 0.9500 . ? C79 C80 1.374(10) . ? C79 C83 1.519(9) . ? C80 C81 1.400(10) . ? C80 H80 0.9500 . ? C81 C84 1.496(10) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C35 C36 1.4480(18) . ? C35 H35 0.9500 . ? C36 C41 1.4033(19) . ? C36 C37 1.4051(18) . ? C37 C38 1.385(2) . ? C37 H37 0.9500 . ? C38 C39 1.390(2) . ? C38 H38 0.9500 . ? C39 C40 1.394(2) . ? C39 H39 0.9500 . ? C40 C41 1.3889(18) . ? C40 H40 0.9500 . ? C41 O42 1.3758(16) . ? O42 C43 1.4728(16) . ? C43 C44 1.516(2) . ? C43 C45 1.518(2) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C50 Cl51 1.782(7) . ? C50 Cl52 1.784(9) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? O60 C63 1.401(12) . ? O60 C61 1.441(11) . ? C61 C62 1.237(15) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.265(15) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? 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 C35 Ru1 C1 101.38(6) . . ? C35 Ru1 O42 79.72(5) . . ? C1 Ru1 O42 177.71(5) . . ? C35 Ru1 Cl2 99.09(4) . . ? C1 Ru1 Cl2 92.22(4) . . ? O42 Ru1 Cl2 85.61(3) . . ? C35 Ru1 Cl3 99.79(4) . . ? C1 Ru1 Cl3 93.87(4) . . ? O42 Ru1 Cl3 87.91(3) . . ? Cl2 Ru1 Cl3 158.585(13) . . ? N2 C1 N5 104.19(11) . . ? N2 C1 Ru1 134.20(9) . . ? N5 C1 Ru1 121.60(10) . . ? C1 N2 C3 110.64(11) . . ? C1 N2 C16 126.26(11) . . ? C3 N2 C16 123.10(11) . . ? C4 C3 N2 107.33(12) . . ? C4 C3 C6 110.62(12) . . ? N2 C3 C6 141.97(13) . . ? C3 C4 N5 107.49(11) . . ? C3 C4 C14 110.24(12) . . ? N5 C4 C14 142.20(13) . . ? C4 N5 C1 110.34(11) . . ? C4 N5 C26 126.1(7) . . ? C1 N5 C26 122.2(7) . . ? C4 N5 C76 124.6(11) . . ? C1 N5 C76 124.9(11) . . ? C26 N5 C76 7.9(9) . . ? C7 C6 C15 119.00(13) . . ? C7 C6 C3 137.99(14) . . ? C15 C6 C3 103.00(12) . . ? C6 C7 C8 118.24(15) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? C9 C8 C7 122.51(15) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C8 C9 C10 120.47(14) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C15 C10 C9 116.35(14) . . ? C15 C10 C11 115.92(15) . . ? C9 C10 C11 127.73(14) . . ? C12 C11 C10 120.75(14) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 122.62(15) . . ? C11 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C14 C13 C12 117.79(15) . . ? C14 C13 H13 121.1 . . ? C12 C13 H13 121.1 . . ? C13 C14 C15 119.27(13) . . ? C13 C14 C4 137.53(14) . . ? C15 C14 C4 103.20(12) . . ? C10 C15 C14 123.65(14) . . ? C10 C15 C6 123.42(14) . . ? C14 C15 C6 112.93(12) . . ? C17 C16 C21 123.10(12) . . ? C17 C16 N2 118.20(12) . . ? C21 C16 N2 118.70(12) . . ? C16 C17 C18 117.56(13) . . ? C16 C17 C22 120.43(12) . . ? C18 C17 C22 121.99(13) . . ? C19 C18 C17 121.29(14) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C20 C19 C18 119.13(13) . . ? C20 C19 C23 120.52(15) . . ? C18 C19 C23 120.34(15) . . ? C19 C20 C21 121.57(14) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C16 C21 C20 117.29(13) . . ? C16 C21 C24 121.10(12) . . ? C20 C21 C24 121.59(13) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C31 C26 C27 121.5(7) . . ? C31 C26 N5 120.7(6) . . ? C27 C26 N5 117.6(6) . . ? C28 C27 C26 117.2(6) . . ? C28 C27 C32 121.7(5) . . ? C26 C27 C32 121.0(6) . . ? C29 C28 C27 122.0(5) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C30 118.6(5) . . ? C28 C29 C33 121.3(5) . . ? C30 C29 C33 120.1(5) . . ? C29 C30 C31 121.9(5) . . ? C29 C30 H30 119.0 . . ? C31 C30 H30 119.0 . . ? C26 C31 C30 117.5(6) . . ? C26 C31 C34 122.1(7) . . ? C30 C31 C34 120.3(7) . . ? C81 C76 C77 123.7(10) . . ? C81 C76 N5 120.3(9) . . ? C77 C76 N5 116.0(9) . . ? C78 C77 C76 116.9(9) . . ? C78 C77 C82 122.2(10) . . ? C76 C77 C82 120.7(10) . . ? C79 C78 C77 121.6(8) . . ? C79 C78 H78 119.2 . . ? C77 C78 H78 119.2 . . ? C78 C79 C80 119.1(8) . . ? C78 C79 C83 120.4(9) . . ? C80 C79 C83 120.4(9) . . ? C79 C80 C81 123.1(9) . . ? C79 C80 H80 118.5 . . ? C81 C80 H80 118.5 . . ? C76 C81 C80 115.1(9) . . ? C76 C81 C84 122.8(10) . . ? C80 C81 C84 122.1(9) . . ? C77 C82 H82A 109.5 . . ? C77 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C77 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C79 C83 H83A 109.5 . . ? C79 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C79 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C81 C84 H84A 109.5 . . ? C81 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C81 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C36 C35 Ru1 118.33(10) . . ? C36 C35 H35 120.8 . . ? Ru1 C35 H35 120.8 . . ? C41 C36 C37 118.63(12) . . ? C41 C36 C35 118.17(12) . . ? C37 C36 C35 123.17(13) . . ? C38 C37 C36 120.34(13) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 119.46(13) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C38 C39 C40 121.95(13) . . ? C38 C39 H39 119.0 . . ? C40 C39 H39 119.0 . . ? C41 C40 C39 117.77(14) . . ? C41 C40 H40 121.1 . . ? C39 C40 H40 121.1 . . ? O42 C41 C40 125.16(13) . . ? O42 C41 C36 113.00(11) . . ? C40 C41 C36 121.82(13) . . ? C41 O42 C43 119.28(10) . . ? C41 O42 Ru1 110.50(8) . . ? C43 O42 Ru1 129.37(8) . . ? O42 C43 C44 105.70(11) . . ? O42 C43 C45 109.33(11) . . ? C44 C43 C45 113.72(13) . . ? O42 C43 H43 109.3 . . ? C44 C43 H43 109.3 . . ? C45 C43 H43 109.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Cl51 C50 Cl52 109.8(4) . . ? Cl51 C50 H50A 109.7 . . ? Cl52 C50 H50A 109.7 . . ? Cl51 C50 H50B 109.7 . . ? Cl52 C50 H50B 109.7 . . ? H50A C50 H50B 108.2 . . ? C63 O60 C61 122.7(6) . . ? C62 C61 O60 125.7(12) . . ? C62 C61 H61A 105.9 . . ? O60 C61 H61A 105.9 . . ? C62 C61 H61B 105.9 . . ? O60 C61 H61B 105.9 . . ? H61A C61 H61B 106.2 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 O60 135.9(12) . . ? C64 C63 H63A 103.2 . . ? O60 C63 H63A 103.2 . . ? C64 C63 H63B 103.2 . . ? O60 C63 H63B 103.2 . . ? H63A C63 H63B 105.2 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 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 C35 Ru1 C1 N2 8.25(14) . . . . ? O42 Ru1 C1 N2 126.8(11) . . . . ? Cl2 Ru1 C1 N2 107.99(13) . . . . ? Cl3 Ru1 C1 N2 -92.56(13) . . . . ? C35 Ru1 C1 N5 -171.20(11) . . . . ? O42 Ru1 C1 N5 -52.7(12) . . . . ? Cl2 Ru1 C1 N5 -71.46(10) . . . . ? Cl3 Ru1 C1 N5 88.00(10) . . . . ? N5 C1 N2 C3 -0.33(15) . . . . ? Ru1 C1 N2 C3 -179.85(11) . . . . ? N5 C1 N2 C16 179.68(12) . . . . ? Ru1 C1 N2 C16 0.2(2) . . . . ? C1 N2 C3 C4 0.19(16) . . . . ? C16 N2 C3 C4 -179.82(12) . . . . ? C1 N2 C3 C6 -176.04(18) . . . . ? C16 N2 C3 C6 3.9(3) . . . . ? N2 C3 C4 N5 0.04(16) . . . . ? C6 C3 C4 N5 177.56(12) . . . . ? N2 C3 C4 C14 -177.61(12) . . . . ? C6 C3 C4 C14 -0.09(17) . . . . ? C3 C4 N5 C1 -0.25(16) . . . . ? C14 C4 N5 C1 176.14(18) . . . . ? C3 C4 N5 C26 -166.8(4) . . . . ? C14 C4 N5 C26 9.5(5) . . . . ? C3 C4 N5 C76 -176.3(7) . . . . ? C14 C4 N5 C76 0.1(7) . . . . ? N2 C1 N5 C4 0.36(15) . . . . ? Ru1 C1 N5 C4 179.95(10) . . . . ? N2 C1 N5 C26 167.6(4) . . . . ? Ru1 C1 N5 C26 -12.8(4) . . . . ? N2 C1 N5 C76 176.4(7) . . . . ? Ru1 C1 N5 C76 -4.0(7) . . . . ? C4 C3 C6 C7 -178.67(18) . . . . ? N2 C3 C6 C7 -2.5(3) . . . . ? C4 C3 C6 C15 0.30(16) . . . . ? N2 C3 C6 C15 176.46(18) . . . . ? C15 C6 C7 C8 0.0(2) . . . . ? C3 C6 C7 C8 178.90(17) . . . . ? C6 C7 C8 C9 1.0(3) . . . . ? C7 C8 C9 C10 -1.2(3) . . . . ? C8 C9 C10 C15 0.3(3) . . . . ? C8 C9 C10 C11 -178.78(18) . . . . ? C15 C10 C11 C12 -0.4(3) . . . . ? C9 C10 C11 C12 178.71(18) . . . . ? C10 C11 C12 C13 0.1(3) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? C12 C13 C14 C15 -0.5(2) . . . . ? C12 C13 C14 C4 179.60(17) . . . . ? C3 C4 C14 C13 179.71(18) . . . . ? N5 C4 C14 C13 3.4(4) . . . . ? C3 C4 C14 C15 -0.16(16) . . . . ? N5 C4 C14 C15 -176.50(19) . . . . ? C9 C10 C15 C14 -178.95(15) . . . . ? C11 C10 C15 C14 0.2(2) . . . . ? C9 C10 C15 C6 0.8(2) . . . . ? C11 C10 C15 C6 179.97(15) . . . . ? C13 C14 C15 C10 0.2(2) . . . . ? C4 C14 C15 C10 -179.87(15) . . . . ? C13 C14 C15 C6 -179.53(14) . . . . ? C4 C14 C15 C6 0.37(17) . . . . ? C7 C6 C15 C10 -1.0(2) . . . . ? C3 C6 C15 C10 179.82(14) . . . . ? C7 C6 C15 C14 178.80(14) . . . . ? C3 C6 C15 C14 -0.42(17) . . . . ? C1 N2 C16 C17 -89.04(16) . . . . ? C3 N2 C16 C17 90.98(16) . . . . ? C1 N2 C16 C21 90.54(16) . . . . ? C3 N2 C16 C21 -89.45(16) . . . . ? C21 C16 C17 C18 -2.5(2) . . . . ? N2 C16 C17 C18 177.06(12) . . . . ? C21 C16 C17 C22 179.37(13) . . . . ? N2 C16 C17 C22 -1.07(19) . . . . ? C16 C17 C18 C19 1.9(2) . . . . ? C22 C17 C18 C19 179.99(14) . . . . ? C17 C18 C19 C20 0.2(2) . . . . ? C17 C18 C19 C23 179.10(15) . . . . ? C18 C19 C20 C21 -1.8(2) . . . . ? C23 C19 C20 C21 179.27(15) . . . . ? C17 C16 C21 C20 1.0(2) . . . . ? N2 C16 C21 C20 -178.60(12) . . . . ? C17 C16 C21 C24 179.18(13) . . . . ? N2 C16 C21 C24 -0.37(19) . . . . ? C19 C20 C21 C16 1.3(2) . . . . ? C19 C20 C21 C24 -176.97(14) . . . . ? C4 N5 C26 C31 -94.4(14) . . . . ? C1 N5 C26 C31 100.4(14) . . . . ? C76 N5 C26 C31 -12(12) . . . . ? C4 N5 C26 C27 81.1(14) . . . . ? C1 N5 C26 C27 -84.0(13) . . . . ? C76 N5 C26 C27 163(14) . . . . ? C31 C26 C27 C28 -12(2) . . . . ? N5 C26 C27 C28 172.1(10) . . . . ? C31 C26 C27 C32 164.0(13) . . . . ? N5 C26 C27 C32 -11.5(19) . . . . ? C26 C27 C28 C29 4.6(15) . . . . ? C32 C27 C28 C29 -171.8(8) . . . . ? C27 C28 C29 C30 4.8(12) . . . . ? C27 C28 C29 C33 -175.6(8) . . . . ? C28 C29 C30 C31 -7.0(14) . . . . ? C33 C29 C30 C31 173.5(9) . . . . ? C27 C26 C31 C30 10(2) . . . . ? N5 C26 C31 C30 -174.2(12) . . . . ? C27 C26 C31 C34 -165.1(13) . . . . ? N5 C26 C31 C34 10(2) . . . . ? C29 C30 C31 C26 -0.5(18) . . . . ? C29 C30 C31 C34 175.1(10) . . . . ? C4 N5 C76 C81 -89(2) . . . . ? C1 N5 C76 C81 95(2) . . . . ? C26 N5 C76 C81 167(15) . . . . ? C4 N5 C76 C77 91(2) . . . . ? C1 N5 C76 C77 -85(2) . . . . ? C26 N5 C76 C77 -13(11) . . . . ? C81 C76 C77 C78 -7(4) . . . . ? N5 C76 C77 C78 172.9(17) . . . . ? C81 C76 C77 C82 167(2) . . . . ? N5 C76 C77 C82 -13(3) . . . . ? C76 C77 C78 C79 1(3) . . . . ? C82 C77 C78 C79 -173.1(14) . . . . ? C77 C78 C79 C80 4(2) . . . . ? C77 C78 C79 C83 -178.7(14) . . . . ? C78 C79 C80 C81 -4(2) . . . . ? C83 C79 C80 C81 178.6(14) . . . . ? C77 C76 C81 C80 7(3) . . . . ? N5 C76 C81 C80 -173.0(18) . . . . ? C77 C76 C81 C84 -170(2) . . . . ? N5 C76 C81 C84 10(3) . . . . ? C79 C80 C81 C76 -1(3) . . . . ? C79 C80 C81 C84 176.1(17) . . . . ? C1 Ru1 C35 C36 173.82(10) . . . . ? O42 Ru1 C35 C36 -4.14(10) . . . . ? Cl2 Ru1 C35 C36 79.67(10) . . . . ? Cl3 Ru1 C35 C36 -90.18(10) . . . . ? Ru1 C35 C36 C41 3.10(17) . . . . ? Ru1 C35 C36 C37 -175.08(10) . . . . ? C41 C36 C37 C38 -0.8(2) . . . . ? C35 C36 C37 C38 177.36(13) . . . . ? C36 C37 C38 C39 -0.1(2) . . . . ? C37 C38 C39 C40 0.9(2) . . . . ? C38 C39 C40 C41 -0.6(2) . . . . ? C39 C40 C41 O42 -178.94(13) . . . . ? C39 C40 C41 C36 -0.4(2) . . . . ? C37 C36 C41 O42 179.80(12) . . . . ? C35 C36 C41 O42 1.54(18) . . . . ? C37 C36 C41 C40 1.1(2) . . . . ? C35 C36 C41 C40 -177.18(13) . . . . ? C40 C41 O42 C43 -15.4(2) . . . . ? C36 C41 O42 C43 165.97(12) . . . . ? C40 C41 O42 Ru1 174.21(12) . . . . ? C36 C41 O42 Ru1 -4.45(14) . . . . ? C35 Ru1 O42 C41 4.88(9) . . . . ? C1 Ru1 O42 C41 -114.0(11) . . . . ? Cl2 Ru1 O42 C41 -95.20(8) . . . . ? Cl3 Ru1 O42 C41 105.23(8) . . . . ? C35 Ru1 O42 C43 -164.29(12) . . . . ? C1 Ru1 O42 C43 76.8(12) . . . . ? Cl2 Ru1 O42 C43 95.63(11) . . . . ? Cl3 Ru1 O42 C43 -63.95(11) . . . . ? C41 O42 C43 C44 168.28(12) . . . . ? Ru1 O42 C43 C44 -23.36(16) . . . . ? C41 O42 C43 C45 -68.94(15) . . . . ? Ru1 O42 C43 C45 99.42(12) . . . . ? C63 O60 C61 C62 179.3(18) . . . . ? C61 O60 C63 C64 -166(2) . . . . ? data_cc06evy1n _database_code_depnum_ccdc_archive 'CCDC 831083' #TrackingRef 'web_deposit_cif_file_1_UrbanoDiaz_ #1308743264.ccdc_depost datos2.cif' _audit_creation_date 2010-11-27T19:27:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common EPH200-20 _chemical_formula_moiety '3(C29 H32 Cl2 N2 O Ru), 0.25(O)' _chemical_formula_sum 'C87 H93 Cl6 N6 O3.25 Ru3' _chemical_formula_weight 1790.6578 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.0768(6) _cell_length_b 17.4168(6) _cell_length_c 17.9705(6) _cell_angle_alpha 108.116(3) _cell_angle_beta 97.210(3) _cell_angle_gamma 119.219(2) _cell_volume 4178.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4563 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 19.68 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8243 _exptl_absorpt_correction_T_max 0.9281 _exptl_absorpt_process_details 'BRUKER AXS - SADABS' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Bruker X8 kappa APEXII CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.1310 _diffrn_reflns_av_unetI/netI 0.1416 _diffrn_reflns_number 105659 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 19099 _reflns_number_gt 10431 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 v2010.11-3 (Bruker AXS, 2010)' _computing_cell_refinement 'APEX2 v2010.11-3 (Bruker AXS, 2010)' _computing_data_reduction 'APEX2 v2010.11-3 (Bruker AXS, 2010)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0358P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 19099 _refine_ls_number_parameters 1043 _refine_ls_number_restraints 360 _refine_ls_R_factor_all 0.1415 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.161 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.144 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.09755(3) 0.32222(3) 0.60640(2) 0.01997(11) Uani 1 1 d . . . Cl2 Cl 0.07006(10) 0.21178(9) 0.66389(8) 0.0303(3) Uani 1 1 d . . . Cl3 Cl 0.14053(10) 0.39607(9) 0.51709(8) 0.0324(3) Uani 1 1 d . . . C4 C -0.0401(3) 0.2633(3) 0.5563(3) 0.0195(12) Uani 1 1 d . . . N5 N -0.0954(3) 0.1846(3) 0.4799(2) 0.0222(10) Uani 1 1 d . . . C6 C -0.1896(4) 0.1545(3) 0.4610(3) 0.0292(13) Uani 1 1 d . . . H6 H -0.2402 0.1024 0.4114 0.035 Uiso 1 1 calc R . . C7 C -0.1962(4) 0.2123(3) 0.5256(3) 0.0315(14) Uani 1 1 d . . . H7 H -0.2524 0.2087 0.5309 0.038 Uiso 1 1 calc R . . N8 N -0.1049(3) 0.2786(3) 0.5836(2) 0.0211(10) Uani 1 1 d . . . C11 C -0.0608(3) 0.1432(3) 0.4212(3) 0.0186(11) Uani 1 1 d . . . C12 C -0.0389(4) 0.1776(3) 0.3618(3) 0.0239(12) Uani 1 1 d . . . C13 C -0.0044(4) 0.1374(4) 0.3061(3) 0.0309(14) Uani 1 1 d . . . H13 H 0.0120 0.1602 0.2652 0.037 Uiso 1 1 calc R . . C14 C 0.0059(4) 0.0656(4) 0.3099(3) 0.0344(15) Uani 1 1 d . . . H14 H 0.0328 0.0417 0.2736 0.041 Uiso 1 1 calc R . . C15 C -0.0223(4) 0.0272(4) 0.3657(3) 0.0315(14) Uani 1 1 d . . . H15 H -0.0174 -0.0248 0.3659 0.038 Uiso 1 1 calc R . . C16 C -0.0579(3) 0.0647(3) 0.4218(3) 0.0236(12) Uani 1 1 d . . . C17 C -0.0586(4) 0.2494(3) 0.3514(3) 0.0341(14) Uani 1 1 d . . . H17A H -0.0238 0.2772 0.3172 0.051 Uiso 1 1 calc R . . H17B H -0.0378 0.3017 0.4061 0.051 Uiso 1 1 calc R . . H17C H -0.1270 0.2163 0.3243 0.051 Uiso 1 1 calc R . . C18 C -0.1011(4) 0.0156(3) 0.4747(3) 0.0353(15) Uani 1 1 d . . . H18A H -0.0716 0.0635 0.5329 0.053 Uiso 1 1 calc R . . H18B H -0.0903 -0.0360 0.4687 0.053 Uiso 1 1 calc R . . H18C H -0.1697 -0.0129 0.4569 0.053 Uiso 1 1 calc R . . C21 C -0.0857(3) 0.3582(3) 0.6579(3) 0.0207(12) Uani 1 1 d . . . C22 C -0.0920(4) 0.3454(3) 0.7292(3) 0.0262(13) Uani 1 1 d . . . C23 C -0.0768(4) 0.4226(4) 0.7979(3) 0.0317(14) Uani 1 1 d . . . H23 H -0.0786 0.4172 0.8487 0.038 Uiso 1 1 calc R . . C24 C -0.0591(4) 0.5063(4) 0.7928(3) 0.0338(15) Uani 1 1 d . . . H24 H -0.0505 0.5573 0.8399 0.041 Uiso 1 1 calc R . . C25 C -0.0535(4) 0.5176(4) 0.7202(3) 0.0301(14) Uani 1 1 d . . . H25 H -0.0407 0.5761 0.7178 0.036 Uiso 1 1 calc R . . C26 C -0.0667(3) 0.4429(3) 0.6513(3) 0.0224(12) Uani 1 1 d . . . C27 C -0.1123(4) 0.2527(4) 0.7338(3) 0.0349(15) Uani 1 1 d . . . H27A H -0.1664 0.1964 0.6851 0.052 Uiso 1 1 calc R . . H27B H -0.1274 0.2514 0.7844 0.052 Uiso 1 1 calc R . . H27C H -0.0561 0.2501 0.7348 0.052 Uiso 1 1 calc R . . C28 C -0.0594(4) 0.4535(4) 0.5719(3) 0.0296(13) Uani 1 1 d . . . H28A H -0.0498 0.5156 0.5776 0.044 Uiso 1 1 calc R . . H28B H -0.1182 0.3997 0.5259 0.044 Uiso 1 1 calc R . . H28C H -0.0054 0.4520 0.5604 0.044 Uiso 1 1 calc R . . C30 C 0.1293(3) 0.4269(3) 0.6984(3) 0.0213(12) Uani 1 1 d . . . H30 H 0.0860 0.4456 0.7057 0.026 Uiso 1 1 calc R . . C31 C 0.2226(3) 0.4813(3) 0.7606(3) 0.0210(12) Uani 1 1 d . . . C32 C 0.2871(3) 0.4565(3) 0.7434(3) 0.0217(12) Uani 1 1 d . . . C33 C 0.3737(4) 0.4990(4) 0.8001(3) 0.0284(13) Uani 1 1 d . . . H33 H 0.4158 0.4800 0.7876 0.034 Uiso 1 1 calc R . . C34 C 0.3980(4) 0.5712(4) 0.8771(3) 0.0324(14) Uani 1 1 d . . . H34 H 0.4575 0.6011 0.9180 0.039 Uiso 1 1 calc R . . C35 C 0.3391(4) 0.6008(3) 0.8960(3) 0.0297(14) Uani 1 1 d . . . H35 H 0.3586 0.6517 0.9487 0.036 Uiso 1 1 calc R . . C36 C 0.2503(4) 0.5557(3) 0.8376(3) 0.0264(13) Uani 1 1 d . . . H36 H 0.2089 0.5756 0.8502 0.032 Uiso 1 1 calc R . . O37 O 0.2519(2) 0.3841(2) 0.6642(2) 0.0276(9) Uani 1 1 d . . . C38 C 0.3145(4) 0.3613(4) 0.6293(4) 0.0407(16) Uani 1 1 d . . . H38 H 0.3511 0.3530 0.6705 0.049 Uiso 1 1 calc R . . C39 C 0.2518(4) 0.2658(4) 0.5525(4) 0.059(2) Uani 1 1 d . . . H39A H 0.2085 0.2152 0.5676 0.088 Uiso 1 1 calc R . . H39B H 0.2916 0.2472 0.5279 0.088 Uiso 1 1 calc R . . H39C H 0.2147 0.2728 0.5121 0.088 Uiso 1 1 calc R . . C40 C 0.3846(4) 0.4443(4) 0.6109(4) 0.0503(18) Uani 1 1 d . . . H40A H 0.3494 0.4521 0.5697 0.075 Uiso 1 1 calc R . . H40B H 0.4276 0.4290 0.5891 0.075 Uiso 1 1 calc R . . H40C H 0.4218 0.5049 0.6622 0.075 Uiso 1 1 calc R . . Ru41 Ru 0.23050(3) 0.34756(3) 0.13702(2) 0.01917(11) Uani 1 1 d . . . Cl42 Cl 0.06599(9) 0.26532(9) 0.10449(8) 0.0279(3) Uani 1 1 d . . . Cl43 Cl 0.38031(9) 0.37261(10) 0.17257(8) 0.0340(3) Uani 1 1 d . . . C44 C 0.2256(3) 0.3342(3) 0.0221(3) 0.0196(12) Uani 1 1 d . A . N45 N 0.2004(3) 0.2505(3) -0.0440(2) 0.0184(9) Uani 1 1 d . . . C46 C 0.1969(4) 0.2611(3) -0.1170(3) 0.0262(13) Uani 1 1 d . . . H46 H 0.1799 0.2126 -0.1703 0.031 Uiso 1 1 calc R . . C47 C 0.2220(4) 0.3525(3) -0.0989(3) 0.0257(13) Uani 1 1 d . A . H47 H 0.2271 0.3816 -0.1364 0.031 Uiso 1 1 calc R . . N48 N 0.2387(3) 0.3956(3) -0.0147(2) 0.0215(10) Uani 1 1 d . . . C51 C 0.1817(4) 0.1611(3) -0.0418(3) 0.0198(12) Uani 1 1 d . . . C52 C 0.2574(4) 0.1507(3) -0.0265(3) 0.0217(12) Uani 1 1 d . . . C53 C 0.2369(4) 0.0621(3) -0.0289(3) 0.0263(13) Uani 1 1 d . . . H53 H 0.2872 0.0535 -0.0175 0.032 Uiso 1 1 calc R . . C54 C 0.1449(4) -0.0130(4) -0.0475(3) 0.0288(14) Uani 1 1 d . . . H54 H 0.1322 -0.0727 -0.0480 0.035 Uiso 1 1 calc R . . C55 C 0.0706(4) -0.0027(3) -0.0655(3) 0.0280(13) Uani 1 1 d . . . H55 H 0.0073 -0.0559 -0.0790 0.034 Uiso 1 1 calc R . . C56 C 0.0869(4) 0.0838(3) -0.0643(3) 0.0212(12) Uani 1 1 d . . . C57 C 0.3574(3) 0.2285(3) -0.0144(3) 0.0320(14) Uani 1 1 d . . . H57A H 0.4024 0.2324 0.0287 0.048 Uiso 1 1 calc R . . H57B H 0.3645 0.2914 0.0027 0.048 Uiso 1 1 calc R . . H57C H 0.3705 0.2123 -0.0666 0.048 Uiso 1 1 calc R . . C58 C 0.0053(3) 0.0919(3) -0.0917(3) 0.0298(14) Uani 1 1 d . . . H58A H -0.0550 0.0301 -0.1066 0.045 Uiso 1 1 calc R . . H58B H 0.0083 0.1066 -0.1401 0.045 Uiso 1 1 calc R . . H58C H 0.0096 0.1442 -0.0463 0.045 Uiso 1 1 calc R . . C61A C 0.2813(7) 0.4991(6) 0.0286(8) 0.0265(19) Uani 0.655(6) 1 d PDU A 1 C62A C 0.2204(8) 0.5300(6) 0.0304(6) 0.033(2) Uani 0.655(6) 1 d PDU A 1 C63A C 0.2611(9) 0.6302(6) 0.0742(8) 0.045(2) Uani 0.655(6) 1 d PDU A 1 H63A H 0.2221 0.6547 0.0773 0.054 Uiso 0.655(6) 1 calc PR A 1 C64A C 0.3602(9) 0.6937(7) 0.1134(8) 0.049(2) Uani 0.655(6) 1 d PDU A 1 H64A H 0.3878 0.7614 0.1431 0.059 Uiso 0.655(6) 1 calc PR A 1 C65A C 0.4179(8) 0.6604(6) 0.1099(5) 0.048(2) Uani 0.655(6) 1 d PDU A 1 H65A H 0.4845 0.7058 0.1377 0.058 Uiso 0.655(6) 1 calc PR A 1 C66A C 0.3821(8) 0.5614(7) 0.0667(7) 0.034(2) Uani 0.655(6) 1 d PDU A 1 C67A C 0.1154(7) 0.4578(8) -0.0114(7) 0.043(3) Uani 0.655(6) 1 d PDU A 1 H67A H 0.1009 0.4291 -0.0717 0.064 Uiso 0.655(6) 1 calc PR A 1 H67B H 0.0826 0.4906 0.0023 0.064 Uiso 0.655(6) 1 calc PR A 1 H67C H 0.0937 0.4063 0.0078 0.064 Uiso 0.655(6) 1 calc PR A 1 C68A C 0.4437(6) 0.5246(6) 0.0599(5) 0.038(2) Uani 0.655(6) 1 d PDU A 1 H68A H 0.5105 0.5797 0.0823 0.057 Uiso 0.655(6) 1 calc PR A 1 H68B H 0.4282 0.4840 0.0014 0.057 Uiso 0.655(6) 1 calc PR A 1 H68C H 0.4333 0.4857 0.0915 0.057 Uiso 0.655(6) 1 calc PR A 1 C61B C 0.2441(12) 0.4895(12) 0.0201(17) 0.035(3) Uani 0.345(6) 1 d PDU A 2 C62B C 0.1627(15) 0.4898(12) 0.0061(14) 0.037(3) Uani 0.345(6) 1 d PDU A 2 C63B C 0.1766(13) 0.5812(10) 0.0366(10) 0.040(3) Uani 0.345(6) 1 d PDU A 2 H63B H 0.1244 0.5871 0.0255 0.048 Uiso 0.345(6) 1 calc PR A 2 C64B C 0.2690(14) 0.6644(11) 0.0840(15) 0.045(3) Uani 0.345(6) 1 d PDU A 2 H64B H 0.2777 0.7262 0.1070 0.054 Uiso 0.345(6) 1 calc PR A 2 C65B C 0.3451(17) 0.6596(12) 0.0977(16) 0.049(3) Uani 0.345(6) 1 d PDU A 2 H65B H 0.4056 0.7177 0.1319 0.058 Uiso 0.345(6) 1 calc PR A 2 C66B C 0.3378(13) 0.5709(10) 0.0627(11) 0.040(3) Uani 0.345(6) 1 d PDU A 2 C67B C 0.0670(12) 0.3963(12) -0.0425(10) 0.035(4) Uani 0.345(6) 1 d PDU A 2 H67D H 0.0684 0.3600 -0.0957 0.053 Uiso 0.345(6) 1 calc PR A 2 H67E H 0.0189 0.4106 -0.0526 0.053 Uiso 0.345(6) 1 calc PR A 2 H67F H 0.0510 0.3570 -0.0109 0.053 Uiso 0.345(6) 1 calc PR A 2 C68B C 0.4210(13) 0.5664(17) 0.0801(16) 0.047(5) Uani 0.345(6) 1 d PDU A 2 H68D H 0.4790 0.6324 0.1050 0.070 Uiso 0.345(6) 1 calc PR A 2 H68E H 0.4222 0.5271 0.0282 0.070 Uiso 0.345(6) 1 calc PR A 2 H68F H 0.4175 0.5366 0.1188 0.070 Uiso 0.345(6) 1 calc PR A 2 C70 C 0.2631(4) 0.4723(3) 0.1876(3) 0.0304(14) Uani 1 1 d . . . H70 H 0.2725 0.5096 0.1567 0.037 Uiso 1 1 calc R . . C71 C 0.2747(4) 0.5144(3) 0.2740(3) 0.0248(13) Uani 1 1 d . . . C72 C 0.2579(4) 0.4565(3) 0.3159(3) 0.0229(12) Uani 1 1 d . . . C73 C 0.2640(3) 0.4915(4) 0.3993(3) 0.0258(13) Uani 1 1 d . . . H73 H 0.2510 0.4513 0.4278 0.031 Uiso 1 1 calc R . . C74 C 0.2894(4) 0.5865(4) 0.4390(3) 0.0295(14) Uani 1 1 d . . . H74 H 0.2930 0.6110 0.4954 0.035 Uiso 1 1 calc R . . C75 C 0.3096(4) 0.6463(4) 0.3992(3) 0.0305(14) Uani 1 1 d . . . H75 H 0.3298 0.7121 0.4285 0.037 Uiso 1 1 calc R . . C76 C 0.3001(4) 0.6095(3) 0.3164(3) 0.0304(14) Uani 1 1 d . . . H76 H 0.3110 0.6495 0.2879 0.036 Uiso 1 1 calc R . . O77 O 0.2357(2) 0.3653(2) 0.26875(18) 0.0216(8) Uani 1 1 d . . . C78 C 0.2358(4) 0.3043(3) 0.3086(3) 0.0245(12) Uani 1 1 d . . . H78 H 0.1919 0.2964 0.3417 0.029 Uiso 1 1 calc R . . C79 C 0.1976(4) 0.2066(3) 0.2390(3) 0.0308(14) Uani 1 1 d . . . H79A H 0.1345 0.1813 0.2028 0.046 Uiso 1 1 calc R . . H79B H 0.1928 0.1611 0.2622 0.046 Uiso 1 1 calc R . . H79C H 0.2408 0.2139 0.2066 0.046 Uiso 1 1 calc R . . C80 C 0.3352(4) 0.3498(4) 0.3657(3) 0.0402(16) Uani 1 1 d . . . H80A H 0.3793 0.3614 0.3341 0.060 Uiso 1 1 calc R . . H80B H 0.3344 0.3055 0.3889 0.060 Uiso 1 1 calc R . . H80C H 0.3560 0.4117 0.4109 0.060 Uiso 1 1 calc R . . Ru81 Ru 0.51212(3) 0.04034(3) 0.26869(2) 0.01843(11) Uani 1 1 d . . . Cl82 Cl 0.58685(9) 0.13956(8) 0.41047(7) 0.0253(3) Uani 1 1 d . . . Cl83 Cl 0.38621(10) -0.08437(9) 0.14853(8) 0.0371(4) Uani 1 1 d . . . C84 C 0.5053(4) 0.1430(3) 0.2483(3) 0.0233(12) Uani 1 1 d . . . N85 N 0.4380(3) 0.1620(3) 0.2636(2) 0.0236(10) Uani 1 1 d . . . C86 C 0.4494(4) 0.2377(4) 0.2454(3) 0.0333(14) Uani 1 1 d . . . H86 H 0.4111 0.2630 0.2502 0.040 Uiso 1 1 calc R . . C87 C 0.5251(4) 0.2683(4) 0.2196(3) 0.0389(16) Uani 1 1 d . . . H87 H 0.5509 0.3199 0.2031 0.047 Uiso 1 1 calc R . . N88 N 0.5584(3) 0.2108(3) 0.2216(2) 0.0236(10) Uani 1 1 d . . . C91 C 0.3625(4) 0.1099(3) 0.2924(3) 0.0240(12) Uani 1 1 d . . . C92 C 0.2749(4) 0.0294(4) 0.2336(3) 0.0279(13) Uani 1 1 d . . . C93 C 0.2037(4) -0.0220(4) 0.2615(4) 0.0360(15) Uani 1 1 d . . . H93 H 0.1445 -0.0784 0.2225 0.043 Uiso 1 1 calc R . . C94 C 0.2172(4) 0.0076(4) 0.3453(4) 0.0394(15) Uani 1 1 d . . . H94 H 0.1683 -0.0293 0.3639 0.047 Uiso 1 1 calc R . . C95 C 0.3009(4) 0.0900(4) 0.4014(4) 0.0359(15) Uani 1 1 d . . . H95 H 0.3084 0.1111 0.4588 0.043 Uiso 1 1 calc R . . C96 C 0.3762(4) 0.1442(4) 0.3769(3) 0.0292(14) Uani 1 1 d . . . C97 C 0.2545(4) 0.0029(4) 0.1418(3) 0.0384(15) Uani 1 1 d . . . H97A H 0.2360 0.0433 0.1280 0.058 Uiso 1 1 calc R . . H97B H 0.2024 -0.0660 0.1100 0.058 Uiso 1 1 calc R . . H97C H 0.3116 0.0143 0.1277 0.058 Uiso 1 1 calc R . . C98 C 0.4642(4) 0.2398(4) 0.4393(3) 0.0393(16) Uani 1 1 d . . . H98A H 0.5184 0.2527 0.4196 0.059 Uiso 1 1 calc R . . H98B H 0.4773 0.2369 0.4927 0.059 Uiso 1 1 calc R . . H98C H 0.4544 0.2922 0.4464 0.059 Uiso 1 1 calc R . . C101 C 0.6370(4) 0.2228(3) 0.1933(3) 0.0222(12) Uani 1 1 d . . . C102 C 0.7293(4) 0.2833(3) 0.2518(3) 0.0243(13) Uani 1 1 d . . . C103 C 0.8023(4) 0.2920(4) 0.2210(3) 0.0307(14) Uani 1 1 d . . . H103 H 0.8658 0.3327 0.2585 0.037 Uiso 1 1 calc R . . C104 C 0.7861(4) 0.2439(4) 0.1385(4) 0.0349(14) Uani 1 1 d . . . H104 H 0.8376 0.2498 0.1200 0.042 Uiso 1 1 calc R . . C105 C 0.6946(4) 0.1867(4) 0.0821(3) 0.0312(14) Uani 1 1 d . . . H105 H 0.6841 0.1553 0.0247 0.037 Uiso 1 1 calc R . . C106 C 0.6175(4) 0.1747(3) 0.1086(3) 0.0251(13) Uani 1 1 d . . . C107 C 0.7469(4) 0.3363(4) 0.3419(3) 0.0383(15) Uani 1 1 d . . . H10A H 0.7198 0.2893 0.3655 0.057 Uiso 1 1 calc R . . H10B H 0.7169 0.3726 0.3477 0.057 Uiso 1 1 calc R . . H10C H 0.8156 0.3818 0.3714 0.057 Uiso 1 1 calc R . . C108 C 0.5178(4) 0.1160(4) 0.0487(3) 0.0317(14) Uani 1 1 d . . . H10D H 0.4770 0.0612 0.0607 0.048 Uiso 1 1 calc R . . H10E H 0.5181 0.0912 -0.0082 0.048 Uiso 1 1 calc R . . H10F H 0.4934 0.1573 0.0545 0.048 Uiso 1 1 calc R . . C110 C 0.6114(3) 0.0499(3) 0.2340(3) 0.0211(12) Uani 1 1 d . . . H110 H 0.6416 0.0941 0.2107 0.025 Uiso 1 1 calc R . . C111 C 0.6433(3) -0.0110(3) 0.2428(3) 0.0190(12) Uani 1 1 d . . . C112 C 0.5960(3) -0.0767(3) 0.2755(3) 0.0191(12) Uani 1 1 d . . . C113 C 0.6242(4) -0.1359(4) 0.2863(3) 0.0264(13) Uani 1 1 d . . . H113 H 0.5911 -0.1810 0.3081 0.032 Uiso 1 1 calc R . . C114 C 0.7030(4) -0.1273(4) 0.2643(3) 0.0287(13) Uani 1 1 d . . . H114 H 0.7238 -0.1667 0.2722 0.034 Uiso 1 1 calc R . . C115 C 0.7505(4) -0.0639(4) 0.2317(3) 0.0280(13) Uani 1 1 d . . . H115 H 0.8038 -0.0594 0.2173 0.034 Uiso 1 1 calc R . . C116 C 0.7206(4) -0.0063(3) 0.2200(3) 0.0262(13) Uani 1 1 d . . . H116 H 0.7528 0.0369 0.1964 0.031 Uiso 1 1 calc R . . O117 O 0.5210(2) -0.0749(2) 0.29437(18) 0.0194(8) Uani 1 1 d . . . C118 C 0.4745(4) -0.1270(4) 0.3429(3) 0.0289(13) Uani 1 1 d . . . H118 H 0.4574 -0.1953 0.3164 0.035 Uiso 1 1 calc R . . C119 C 0.3837(4) -0.1295(4) 0.3358(3) 0.0316(14) Uani 1 1 d . . . H11A H 0.3998 -0.0628 0.3615 0.047 Uiso 1 1 calc R . . H11B H 0.3472 -0.1667 0.3642 0.047 Uiso 1 1 calc R . . H11C H 0.3454 -0.1606 0.2771 0.047 Uiso 1 1 calc R . . C120 C 0.5397(4) -0.0780(4) 0.4312(3) 0.0376(15) Uani 1 1 d . . . H12A H 0.5957 -0.0808 0.4315 0.056 Uiso 1 1 calc R . . H12B H 0.5058 -0.1116 0.4629 0.056 Uiso 1 1 calc R . . H12C H 0.5599 -0.0098 0.4565 0.056 Uiso 1 1 calc R . . O1W O 0.5058(10) 0.3729(10) 0.6957(9) 0.037(4) Uiso 0.25 1 d P . . 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 0.0201(2) 0.0171(2) 0.0200(2) 0.00773(17) 0.00572(19) 0.00901(19) Cl2 0.0344(8) 0.0222(6) 0.0318(8) 0.0142(6) 0.0056(6) 0.0140(6) Cl3 0.0313(8) 0.0303(7) 0.0262(7) 0.0152(6) 0.0111(6) 0.0089(6) C4 0.021(3) 0.019(2) 0.014(3) 0.008(2) 0.003(2) 0.008(2) N5 0.019(3) 0.022(2) 0.019(2) 0.0046(18) 0.0054(19) 0.010(2) C6 0.021(3) 0.025(3) 0.026(3) 0.002(2) 0.001(3) 0.009(3) C7 0.018(3) 0.027(3) 0.028(3) 0.000(2) 0.003(3) 0.006(3) N8 0.021(3) 0.022(2) 0.018(2) 0.0061(18) 0.0069(19) 0.011(2) C11 0.015(3) 0.015(2) 0.013(3) 0.003(2) 0.000(2) 0.003(2) C12 0.024(3) 0.021(3) 0.019(3) 0.007(2) 0.003(2) 0.010(2) C13 0.030(3) 0.033(3) 0.026(3) 0.014(3) 0.015(3) 0.013(3) C14 0.031(4) 0.039(3) 0.028(3) 0.005(3) 0.007(3) 0.022(3) C15 0.034(4) 0.029(3) 0.029(3) 0.005(3) 0.001(3) 0.022(3) C16 0.018(3) 0.019(3) 0.023(3) 0.009(2) -0.002(2) 0.005(2) C17 0.034(4) 0.023(3) 0.035(3) 0.016(3) 0.001(3) 0.009(3) C18 0.036(4) 0.019(3) 0.034(3) 0.011(2) 0.002(3) 0.006(3) C21 0.010(3) 0.017(2) 0.023(3) 0.005(2) 0.004(2) 0.002(2) C22 0.031(3) 0.027(3) 0.030(3) 0.017(2) 0.015(3) 0.018(3) C23 0.040(4) 0.033(3) 0.019(3) 0.010(2) 0.009(3) 0.020(3) C24 0.036(4) 0.028(3) 0.031(3) 0.003(3) 0.008(3) 0.020(3) C25 0.028(3) 0.024(3) 0.037(3) 0.013(3) 0.008(3) 0.015(3) C26 0.020(3) 0.028(3) 0.025(3) 0.014(2) 0.008(2) 0.014(2) C27 0.049(4) 0.033(3) 0.040(4) 0.027(3) 0.021(3) 0.026(3) C28 0.031(3) 0.036(3) 0.030(3) 0.022(3) 0.011(3) 0.020(3) C30 0.022(3) 0.023(3) 0.024(3) 0.013(2) 0.006(2) 0.015(2) C31 0.017(3) 0.018(2) 0.025(3) 0.012(2) 0.003(2) 0.007(2) C32 0.016(3) 0.020(3) 0.025(3) 0.015(2) 0.004(2) 0.005(2) C33 0.022(3) 0.033(3) 0.031(3) 0.023(3) 0.008(3) 0.010(3) C34 0.019(3) 0.034(3) 0.028(3) 0.022(3) 0.001(3) 0.000(3) C35 0.031(4) 0.020(3) 0.025(3) 0.010(2) 0.007(3) 0.005(3) C36 0.029(3) 0.021(3) 0.024(3) 0.012(2) 0.008(3) 0.009(3) O37 0.019(2) 0.0261(19) 0.032(2) 0.0093(16) 0.0093(17) 0.0103(17) C38 0.028(4) 0.044(4) 0.058(4) 0.017(3) 0.021(3) 0.027(3) C39 0.047(4) 0.040(4) 0.071(5) 0.000(3) 0.028(4) 0.024(3) C40 0.030(4) 0.053(4) 0.047(4) 0.011(3) 0.022(3) 0.014(3) Ru41 0.0234(3) 0.0153(2) 0.0157(2) 0.00695(17) 0.00619(19) 0.00857(19) Cl42 0.0239(8) 0.0261(7) 0.0273(7) 0.0074(6) 0.0065(6) 0.0126(6) Cl43 0.0217(8) 0.0488(8) 0.0267(7) 0.0185(6) 0.0098(6) 0.0149(7) C44 0.012(3) 0.017(2) 0.023(3) 0.008(2) 0.003(2) 0.005(2) N45 0.020(2) 0.019(2) 0.016(2) 0.0093(17) 0.0051(19) 0.0101(19) C46 0.039(4) 0.026(3) 0.015(3) 0.009(2) 0.009(3) 0.018(3) C47 0.039(4) 0.028(3) 0.016(3) 0.014(2) 0.013(3) 0.019(3) N48 0.029(3) 0.020(2) 0.017(2) 0.0104(18) 0.008(2) 0.014(2) C51 0.026(3) 0.013(2) 0.022(3) 0.008(2) 0.013(2) 0.011(2) C52 0.022(3) 0.023(3) 0.018(3) 0.010(2) 0.008(2) 0.011(2) C53 0.025(3) 0.027(3) 0.025(3) 0.010(2) 0.009(3) 0.014(3) C54 0.046(4) 0.022(3) 0.024(3) 0.015(2) 0.013(3) 0.020(3) C55 0.027(3) 0.020(3) 0.021(3) 0.005(2) 0.006(3) 0.006(3) C56 0.026(3) 0.019(3) 0.015(3) 0.005(2) 0.007(2) 0.011(2) C57 0.021(3) 0.029(3) 0.036(3) 0.009(3) 0.010(3) 0.011(3) C58 0.021(3) 0.024(3) 0.029(3) 0.005(2) 0.005(3) 0.007(3) C61A 0.053(4) 0.020(3) 0.016(4) 0.013(3) 0.016(4) 0.022(3) C62A 0.063(4) 0.024(3) 0.025(4) 0.017(3) 0.023(4) 0.028(3) C63A 0.084(4) 0.025(4) 0.032(4) 0.014(4) 0.030(4) 0.031(4) C64A 0.088(5) 0.022(4) 0.025(4) 0.012(4) 0.024(4) 0.020(4) C65A 0.072(5) 0.025(3) 0.025(4) 0.011(3) 0.014(4) 0.011(3) C66A 0.056(5) 0.024(3) 0.020(4) 0.018(3) 0.008(5) 0.019(4) C67A 0.059(6) 0.046(6) 0.040(6) 0.014(5) 0.016(6) 0.043(5) C68A 0.032(5) 0.033(5) 0.034(5) 0.021(4) 0.006(4) 0.006(4) C61B 0.060(5) 0.021(4) 0.025(5) 0.013(4) 0.020(6) 0.021(4) C62B 0.067(6) 0.027(5) 0.027(5) 0.018(5) 0.023(6) 0.027(5) C63B 0.074(5) 0.030(4) 0.030(5) 0.021(4) 0.029(5) 0.031(4) C64B 0.087(5) 0.018(5) 0.031(5) 0.017(5) 0.030(5) 0.024(4) C65B 0.081(5) 0.022(4) 0.031(5) 0.014(5) 0.025(5) 0.018(4) C66B 0.065(5) 0.023(4) 0.025(4) 0.013(4) 0.019(5) 0.017(4) C67B 0.059(8) 0.040(7) 0.030(9) 0.024(7) 0.018(7) 0.038(6) C68B 0.054(7) 0.029(7) 0.033(8) 0.007(7) 0.020(8) 0.008(6) C70 0.047(4) 0.017(3) 0.021(3) 0.011(2) 0.011(3) 0.013(3) C71 0.031(3) 0.018(3) 0.019(3) 0.009(2) 0.012(2) 0.008(2) C72 0.024(3) 0.022(3) 0.014(3) 0.004(2) 0.006(2) 0.009(2) C73 0.024(3) 0.033(3) 0.022(3) 0.014(2) 0.011(2) 0.015(3) C74 0.031(3) 0.033(3) 0.016(3) 0.001(2) 0.008(3) 0.018(3) C75 0.031(3) 0.021(3) 0.028(3) 0.004(2) 0.004(3) 0.013(3) C76 0.038(4) 0.018(3) 0.024(3) 0.008(2) 0.006(3) 0.009(3) O77 0.031(2) 0.0190(17) 0.0170(18) 0.0107(14) 0.0091(16) 0.0138(17) C78 0.034(3) 0.029(3) 0.021(3) 0.017(2) 0.013(3) 0.020(3) C79 0.040(4) 0.028(3) 0.038(3) 0.023(3) 0.020(3) 0.020(3) C80 0.054(4) 0.053(4) 0.033(3) 0.022(3) 0.012(3) 0.041(4) Ru81 0.0213(2) 0.0182(2) 0.0164(2) 0.00848(17) 0.00671(18) 0.01075(19) Cl82 0.0280(8) 0.0273(7) 0.0184(7) 0.0064(5) 0.0052(6) 0.0166(6) Cl83 0.0426(9) 0.0252(7) 0.0262(8) 0.0041(6) -0.0065(7) 0.0155(7) C84 0.029(3) 0.025(3) 0.016(3) 0.009(2) 0.009(2) 0.015(3) N85 0.028(3) 0.024(2) 0.032(3) 0.019(2) 0.017(2) 0.017(2) C86 0.046(4) 0.036(3) 0.051(4) 0.037(3) 0.033(3) 0.030(3) C87 0.056(4) 0.035(3) 0.051(4) 0.030(3) 0.029(3) 0.033(3) N88 0.029(3) 0.021(2) 0.030(3) 0.0166(19) 0.014(2) 0.015(2) C91 0.029(3) 0.026(3) 0.033(3) 0.021(2) 0.019(3) 0.020(3) C92 0.036(4) 0.032(3) 0.034(3) 0.020(3) 0.016(3) 0.027(3) C93 0.029(4) 0.033(3) 0.049(4) 0.021(3) 0.010(3) 0.019(3) C94 0.038(4) 0.053(4) 0.060(4) 0.041(4) 0.036(4) 0.033(4) C95 0.055(5) 0.059(4) 0.039(4) 0.036(3) 0.034(3) 0.049(4) C96 0.037(4) 0.041(3) 0.027(3) 0.017(3) 0.013(3) 0.032(3) C97 0.041(4) 0.052(4) 0.035(3) 0.020(3) 0.015(3) 0.033(3) C98 0.050(4) 0.049(4) 0.036(3) 0.018(3) 0.018(3) 0.039(3) C101 0.027(3) 0.021(3) 0.030(3) 0.020(2) 0.017(3) 0.015(3) C102 0.031(3) 0.018(3) 0.023(3) 0.014(2) 0.008(3) 0.010(3) C103 0.021(3) 0.036(3) 0.036(3) 0.023(3) 0.008(3) 0.012(3) C104 0.030(4) 0.040(3) 0.052(4) 0.033(3) 0.024(3) 0.021(3) C105 0.043(4) 0.027(3) 0.027(3) 0.013(2) 0.017(3) 0.020(3) C106 0.028(3) 0.022(3) 0.025(3) 0.013(2) 0.008(3) 0.013(3) C107 0.037(4) 0.029(3) 0.029(3) 0.009(3) 0.003(3) 0.009(3) C108 0.036(4) 0.031(3) 0.028(3) 0.012(3) 0.009(3) 0.020(3) C110 0.027(3) 0.022(3) 0.020(3) 0.009(2) 0.013(2) 0.016(2) C111 0.016(3) 0.014(2) 0.015(3) 0.001(2) -0.004(2) 0.005(2) C112 0.017(3) 0.023(3) 0.015(3) 0.006(2) 0.006(2) 0.011(2) C113 0.032(3) 0.034(3) 0.022(3) 0.019(2) 0.009(3) 0.020(3) C114 0.031(3) 0.034(3) 0.028(3) 0.012(3) 0.012(3) 0.023(3) C115 0.022(3) 0.033(3) 0.026(3) 0.006(2) 0.009(3) 0.017(3) C116 0.029(3) 0.021(3) 0.022(3) 0.007(2) 0.012(3) 0.011(3) O117 0.021(2) 0.0252(18) 0.0205(18) 0.0147(15) 0.0119(16) 0.0150(16) C118 0.033(4) 0.033(3) 0.039(3) 0.027(3) 0.023(3) 0.021(3) C119 0.033(4) 0.036(3) 0.039(3) 0.026(3) 0.023(3) 0.020(3) C120 0.045(4) 0.057(4) 0.035(4) 0.032(3) 0.021(3) 0.035(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C30 1.813(4) . ? Ru1 C4 1.982(5) . ? Ru1 O37 2.243(3) . ? Ru1 Cl3 2.3297(14) . ? Ru1 Cl2 2.3374(13) . ? C4 N8 1.370(6) . ? C4 N5 1.376(5) . ? N5 C6 1.380(6) . ? N5 C11 1.443(6) . ? C6 C7 1.339(6) . ? C6 H6 0.9500 . ? C7 N8 1.391(6) . ? C7 H7 0.9500 . ? N8 C21 1.453(5) . ? C11 C12 1.385(6) . ? C11 C16 1.396(6) . ? C12 C13 1.396(7) . ? C12 C17 1.502(7) . ? C13 C14 1.364(7) . ? C13 H13 0.9500 . ? C14 C15 1.383(7) . ? C14 H14 0.9500 . ? C15 C16 1.394(7) . ? C15 H15 0.9500 . ? C16 C18 1.498(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 C22 1.375(7) . ? C21 C26 1.396(6) . ? C22 C23 1.393(6) . ? C22 C27 1.510(6) . ? C23 C24 1.373(7) . ? C23 H23 0.9500 . ? C24 C25 1.386(7) . ? C24 H24 0.9500 . ? C25 C26 1.385(6) . ? C25 H25 0.9500 . ? C26 C28 1.508(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 C31 1.452(6) . ? C30 H30 0.9500 . ? C31 C36 1.392(6) . ? C31 C32 1.400(7) . ? C32 C33 1.364(7) . ? C32 O37 1.380(5) . ? C33 C34 1.390(7) . ? C33 H33 0.9500 . ? C34 C35 1.369(7) . ? C34 H34 0.9500 . ? C35 C36 1.395(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? O37 C38 1.457(6) . ? C38 C39 1.510(7) . ? C38 C40 1.528(8) . ? C38 H38 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? Ru41 C70 1.822(4) . ? Ru41 C44 1.991(5) . ? Ru41 O77 2.274(3) . ? Ru41 Cl42 2.3289(14) . ? Ru41 Cl43 2.3389(14) . ? C44 N48 1.368(6) . ? C44 N45 1.380(5) . ? N45 C46 1.378(6) . ? N45 C51 1.442(6) . ? C46 C47 1.342(6) . ? C46 H46 0.9500 . ? C47 N48 1.382(6) . ? C47 H47 0.9500 . ? N48 C61A 1.447(9) . ? N48 C61B 1.510(18) . ? C51 C52 1.397(7) . ? C51 C56 1.402(6) . ? C52 C53 1.391(6) . ? C52 C57 1.504(7) . ? C53 C54 1.372(7) . ? C53 H53 0.9500 . ? C54 C55 1.377(7) . ? C54 H54 0.9500 . ? C55 C56 1.385(6) . ? C55 H55 0.9500 . ? C56 C58 1.505(7) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C61A C62A 1.383(12) . ? C61A C66A 1.424(13) . ? C62A C63A 1.404(11) . ? C62A C67A 1.495(12) . ? C63A C64A 1.405(18) . ? C63A H63A 0.9500 . ? C64A C65A 1.363(17) . ? C64A H64A 0.9500 . ? C65A C66A 1.404(12) . ? C65A H65A 0.9500 . ? C66A C68A 1.474(14) . ? C67A H67A 0.9800 . ? C67A H67B 0.9800 . ? C67A H67C 0.9800 . ? C68A H68A 0.9800 . ? C68A H68B 0.9800 . ? C68A H68C 0.9800 . ? C61B C62B 1.384(17) . ? C61B C66B 1.400(17) . ? C62B C63B 1.395(16) . ? C62B C67B 1.499(18) . ? C63B C64B 1.41(2) . ? C63B H63B 0.9500 . ? C64B C65B 1.34(3) . ? C64B H64B 0.9500 . ? C65B C66B 1.409(17) . ? C65B H65B 0.9500 . ? C66B C68B 1.462(19) . ? C67B H67D 0.9800 . ? C67B H67E 0.9800 . ? C67B H67F 0.9800 . ? C68B H68D 0.9800 . ? C68B H68E 0.9800 . ? C68B H68F 0.9800 . ? C70 C71 1.435(6) . ? C70 H70 0.9500 . ? C71 C72 1.383(7) . ? C71 C76 1.394(6) . ? C72 O77 1.370(5) . ? C72 C73 1.400(6) . ? C73 C74 1.387(6) . ? C73 H73 0.9500 . ? C74 C75 1.374(7) . ? C74 H74 0.9500 . ? C75 C76 1.377(7) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? O77 C78 1.454(5) . ? C78 C79 1.508(6) . ? C78 C80 1.519(7) . ? C78 H78 1.0000 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? Ru81 C110 1.829(5) . ? Ru81 C84 1.986(5) . ? Ru81 O117 2.263(3) . ? Ru81 Cl83 2.3156(13) . ? Ru81 Cl82 2.3237(12) . ? C84 N88 1.365(6) . ? C84 N85 1.378(6) . ? N85 C86 1.383(6) . ? N85 C91 1.440(6) . ? C86 C87 1.342(7) . ? C86 H86 0.9500 . ? C87 N88 1.379(6) . ? C87 H87 0.9500 . ? N88 C101 1.437(6) . ? C91 C96 1.388(7) . ? C91 C92 1.398(7) . ? C92 C93 1.379(7) . ? C92 C97 1.511(7) . ? C93 C94 1.379(7) . ? C93 H93 0.9500 . ? C94 C95 1.361(8) . ? C94 H94 0.9500 . ? C95 C96 1.397(7) . ? C95 H95 0.9500 . ? C96 C98 1.505(7) . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C101 C106 1.392(6) . ? C101 C102 1.405(7) . ? C102 C103 1.388(7) . ? C102 C107 1.497(6) . ? C103 C104 1.369(7) . ? C103 H103 0.9500 . ? C104 C105 1.384(7) . ? C104 H104 0.9500 . ? C105 C106 1.398(7) . ? C105 H105 0.9500 . ? C106 C108 1.503(7) . ? C107 H10A 0.9800 . ? C107 H10B 0.9800 . ? C107 H10C 0.9800 . ? C108 H10D 0.9800 . ? C108 H10E 0.9800 . ? C108 H10F 0.9800 . ? C110 C111 1.447(6) . ? C110 H110 0.9500 . ? C111 C112 1.393(6) . ? C111 C116 1.403(7) . ? C112 O117 1.378(5) . ? C112 C113 1.385(6) . ? C113 C114 1.401(7) . ? C113 H113 0.9500 . ? C114 C115 1.366(7) . ? C114 H114 0.9500 . ? C115 C116 1.385(7) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? O117 C118 1.475(6) . ? C118 C120 1.508(7) . ? C118 C119 1.517(7) . ? C118 H118 1.0000 . ? C119 H11A 0.9800 . ? C119 H11B 0.9800 . ? C119 H11C 0.9800 . ? C120 H12A 0.9800 . ? C120 H12B 0.9800 . ? C120 H12C 0.9800 . ? 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 C30 Ru1 C4 100.9(2) . . ? C30 Ru1 O37 79.82(18) . . ? C4 Ru1 O37 177.84(16) . . ? C30 Ru1 Cl3 99.53(15) . . ? C4 Ru1 Cl3 93.69(14) . . ? O37 Ru1 Cl3 88.16(10) . . ? C30 Ru1 Cl2 99.45(15) . . ? C4 Ru1 Cl2 93.14(14) . . ? O37 Ru1 Cl2 84.73(9) . . ? Cl3 Ru1 Cl2 158.20(5) . . ? N8 C4 N5 102.9(4) . . ? N8 C4 Ru1 134.0(3) . . ? N5 C4 Ru1 123.0(3) . . ? C4 N5 C6 111.7(4) . . ? C4 N5 C11 125.7(4) . . ? C6 N5 C11 122.3(4) . . ? C7 C6 N5 107.1(4) . . ? C7 C6 H6 126.4 . . ? N5 C6 H6 126.4 . . ? C6 C7 N8 106.8(5) . . ? C6 C7 H7 126.6 . . ? N8 C7 H7 126.6 . . ? C4 N8 C7 111.6(4) . . ? C4 N8 C21 127.5(4) . . ? C7 N8 C21 120.6(4) . . ? C12 C11 C16 122.0(4) . . ? C12 C11 N5 118.8(4) . . ? C16 C11 N5 119.0(4) . . ? C11 C12 C13 117.9(5) . . ? C11 C12 C17 122.0(5) . . ? C13 C12 C17 119.9(5) . . ? C14 C13 C12 120.7(5) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 121.0(5) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 120.0(5) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 118.0(5) . . ? C15 C16 C18 120.8(5) . . ? C11 C16 C18 120.9(5) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C21 C26 123.2(4) . . ? C22 C21 N8 119.5(4) . . ? C26 C21 N8 117.2(4) . . ? C21 C22 C23 117.3(5) . . ? C21 C22 C27 121.5(4) . . ? C23 C22 C27 121.2(5) . . ? C24 C23 C22 120.7(5) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 121.2(5) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C26 C25 C24 119.5(5) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C21 118.1(5) . . ? C25 C26 C28 120.9(5) . . ? C21 C26 C28 121.0(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C30 Ru1 118.1(4) . . ? C31 C30 H30 120.9 . . ? Ru1 C30 H30 120.9 . . ? C36 C31 C32 118.4(5) . . ? C36 C31 C30 122.9(5) . . ? C32 C31 C30 118.7(4) . . ? C33 C32 O37 124.9(5) . . ? C33 C32 C31 122.7(5) . . ? O37 C32 C31 112.4(4) . . ? C32 C33 C34 117.2(5) . . ? C32 C33 H33 121.4 . . ? C34 C33 H33 121.4 . . ? C35 C34 C33 122.4(5) . . ? C35 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? C34 C35 C36 119.6(5) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C31 C36 C35 119.6(5) . . ? C31 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C32 O37 C38 120.3(4) . . ? C32 O37 Ru1 109.8(3) . . ? C38 O37 Ru1 129.8(3) . . ? O37 C38 C39 107.1(4) . . ? O37 C38 C40 110.3(4) . . ? C39 C38 C40 112.7(5) . . ? O37 C38 H38 108.9 . . ? C39 C38 H38 108.9 . . ? C40 C38 H38 108.9 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C70 Ru41 C44 100.5(2) . . ? C70 Ru41 O77 78.39(18) . . ? C44 Ru41 O77 178.83(16) . . ? C70 Ru41 Cl42 99.19(17) . . ? C44 Ru41 Cl42 93.68(14) . . ? O77 Ru41 Cl42 86.08(9) . . ? C70 Ru41 Cl43 100.40(18) . . ? C44 Ru41 Cl43 94.08(14) . . ? O77 Ru41 Cl43 86.56(9) . . ? Cl42 Ru41 Cl43 157.20(5) . . ? N48 C44 N45 102.0(4) . . ? N48 C44 Ru41 133.0(3) . . ? N45 C44 Ru41 124.9(3) . . ? C46 N45 C44 111.8(4) . . ? C46 N45 C51 121.0(4) . . ? C44 N45 C51 127.2(4) . . ? C47 C46 N45 107.4(4) . . ? C47 C46 H46 126.3 . . ? N45 C46 H46 126.3 . . ? C46 C47 N48 106.0(4) . . ? C46 C47 H47 127.0 . . ? N48 C47 H47 127.0 . . ? C44 N48 C47 112.8(4) . . ? C44 N48 C61A 125.6(6) . . ? C47 N48 C61A 120.8(7) . . ? C44 N48 C61B 127.1(12) . . ? C47 N48 C61B 118.1(12) . . ? C52 C51 C56 122.0(4) . . ? C52 C51 N45 118.9(4) . . ? C56 C51 N45 118.7(4) . . ? C53 C52 C51 117.8(5) . . ? C53 C52 C57 119.7(5) . . ? C51 C52 C57 122.3(4) . . ? C54 C53 C52 120.7(5) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C53 C54 C55 120.7(5) . . ? C53 C54 H54 119.6 . . ? C55 C54 H54 119.6 . . ? C54 C55 C56 121.0(5) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C55 C56 C51 117.5(5) . . ? C55 C56 C58 120.9(5) . . ? C51 C56 C58 121.4(4) . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C62A C61A C66A 125.0(8) . . ? C62A C61A N48 117.2(8) . . ? C66A C61A N48 117.8(8) . . ? C61A C62A C63A 117.5(10) . . ? C61A C62A C67A 120.3(8) . . ? C63A C62A C67A 122.3(10) . . ? C62A C63A C64A 119.2(11) . . ? C62A C63A H63A 120.4 . . ? C64A C63A H63A 120.4 . . ? C65A C64A C63A 121.6(9) . . ? C65A C64A H64A 119.2 . . ? C63A C64A H64A 119.2 . . ? C64A C65A C66A 122.2(10) . . ? C64A C65A H65A 118.9 . . ? C66A C65A H65A 118.9 . . ? C65A C66A C61A 114.5(11) . . ? C65A C66A C68A 122.9(10) . . ? C61A C66A C68A 122.5(8) . . ? C62B C61B C66B 126.7(16) . . ? C62B C61B N48 120.9(13) . . ? C66B C61B N48 112.4(13) . . ? C61B C62B C63B 116.0(17) . . ? C61B C62B C67B 120.5(14) . . ? C63B C62B C67B 123.4(16) . . ? C62B C63B C64B 119.1(16) . . ? C62B C63B H63B 120.5 . . ? C64B C63B H63B 120.5 . . ? C65B C64B C63B 122.3(15) . . ? C65B C64B H64B 118.9 . . ? C63B C64B H64B 118.9 . . ? C64B C65B C66B 121.8(19) . . ? C64B C65B H65B 119.1 . . ? C66B C65B H65B 119.1 . . ? C61B C66B C65B 113.8(16) . . ? C61B C66B C68B 124.5(16) . . ? C65B C66B C68B 121.2(16) . . ? C62B C67B H67D 109.5 . . ? C62B C67B H67E 109.5 . . ? H67D C67B H67E 109.5 . . ? C62B C67B H67F 109.5 . . ? H67D C67B H67F 109.5 . . ? H67E C67B H67F 109.5 . . ? C66B C68B H68D 109.5 . . ? C66B C68B H68E 109.5 . . ? H68D C68B H68E 109.5 . . ? C66B C68B H68F 109.5 . . ? H68D C68B H68F 109.5 . . ? H68E C68B H68F 109.5 . . ? C71 C70 Ru41 120.3(4) . . ? C71 C70 H70 119.8 . . ? Ru41 C70 H70 119.8 . . ? C72 C71 C76 119.1(4) . . ? C72 C71 C70 117.7(4) . . ? C76 C71 C70 123.2(5) . . ? O77 C72 C71 114.2(4) . . ? O77 C72 C73 125.0(5) . . ? C71 C72 C73 120.8(4) . . ? C74 C73 C72 118.1(5) . . ? C74 C73 H73 120.9 . . ? C72 C73 H73 120.9 . . ? C75 C74 C73 121.9(5) . . ? C75 C74 H74 119.0 . . ? C73 C74 H74 119.0 . . ? C74 C75 C76 119.1(5) . . ? C74 C75 H75 120.4 . . ? C76 C75 H75 120.4 . . ? C75 C76 C71 120.9(5) . . ? C75 C76 H76 119.6 . . ? C71 C76 H76 119.6 . . ? C72 O77 C78 119.9(4) . . ? C72 O77 Ru41 109.3(3) . . ? C78 O77 Ru41 129.8(3) . . ? O77 C78 C79 105.9(4) . . ? O77 C78 C80 110.9(4) . . ? C79 C78 C80 112.4(4) . . ? O77 C78 H78 109.2 . . ? C79 C78 H78 109.2 . . ? C80 C78 H78 109.2 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C78 C80 H80A 109.5 . . ? C78 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C78 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C110 Ru81 C84 101.2(2) . . ? C110 Ru81 O117 79.07(17) . . ? C84 Ru81 O117 178.98(15) . . ? C110 Ru81 Cl83 99.62(14) . . ? C84 Ru81 Cl83 93.33(14) . . ? O117 Ru81 Cl83 87.59(8) . . ? C110 Ru81 Cl82 102.35(14) . . ? C84 Ru81 Cl82 91.63(13) . . ? O117 Ru81 Cl82 87.35(8) . . ? Cl83 Ru81 Cl82 156.06(5) . . ? N88 C84 N85 102.8(4) . . ? N88 C84 Ru81 134.3(4) . . ? N85 C84 Ru81 122.8(4) . . ? C84 N85 C86 111.5(4) . . ? C84 N85 C91 126.0(4) . . ? C86 N85 C91 122.5(4) . . ? C87 C86 N85 106.7(5) . . ? C87 C86 H86 126.7 . . ? N85 C86 H86 126.7 . . ? C86 C87 N88 107.1(5) . . ? C86 C87 H87 126.4 . . ? N88 C87 H87 126.4 . . ? C84 N88 C87 111.9(4) . . ? C84 N88 C101 127.6(4) . . ? C87 N88 C101 120.5(4) . . ? C96 C91 C92 121.7(5) . . ? C96 C91 N85 119.6(5) . . ? C92 C91 N85 118.6(5) . . ? C93 C92 C91 118.4(5) . . ? C93 C92 C97 119.7(5) . . ? C91 C92 C97 121.7(5) . . ? C94 C93 C92 120.8(5) . . ? C94 C93 H93 119.6 . . ? C92 C93 H93 119.6 . . ? C95 C94 C93 119.8(6) . . ? C95 C94 H94 120.1 . . ? C93 C94 H94 120.1 . . ? C94 C95 C96 121.9(5) . . ? C94 C95 H95 119.0 . . ? C96 C95 H95 119.0 . . ? C91 C96 C95 117.1(5) . . ? C91 C96 C98 122.0(5) . . ? C95 C96 C98 120.7(5) . . ? C92 C97 H97A 109.5 . . ? C92 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C92 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C96 C98 H98A 109.5 . . ? C96 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C96 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C106 C101 C102 123.3(5) . . ? C106 C101 N88 118.0(5) . . ? C102 C101 N88 118.7(4) . . ? C103 C102 C101 116.2(5) . . ? C103 C102 C107 122.5(5) . . ? C101 C102 C107 121.3(5) . . ? C104 C103 C102 122.4(5) . . ? C104 C103 H103 118.8 . . ? C102 C103 H103 118.8 . . ? C103 C104 C105 120.0(5) . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C104 C105 C106 120.8(5) . . ? C104 C105 H105 119.6 . . ? C106 C105 H105 119.6 . . ? C101 C106 C105 117.3(5) . . ? C101 C106 C108 120.6(5) . . ? C105 C106 C108 122.1(5) . . ? C102 C107 H10A 109.5 . . ? C102 C107 H10B 109.5 . . ? H10A C107 H10B 109.5 . . ? C102 C107 H10C 109.5 . . ? H10A C107 H10C 109.5 . . ? H10B C107 H10C 109.5 . . ? C106 C108 H10D 109.5 . . ? C106 C108 H10E 109.5 . . ? H10D C108 H10E 109.5 . . ? C106 C108 H10F 109.5 . . ? H10D C108 H10F 109.5 . . ? H10E C108 H10F 109.5 . . ? C111 C110 Ru81 118.8(4) . . ? C111 C110 H110 120.6 . . ? Ru81 C110 H110 120.6 . . ? C112 C111 C116 118.4(4) . . ? C112 C111 C110 119.1(5) . . ? C116 C111 C110 122.5(5) . . ? O117 C112 C113 125.8(5) . . ? O117 C112 C111 112.6(4) . . ? C113 C112 C111 121.6(5) . . ? C112 C113 C114 118.1(5) . . ? C112 C113 H113 121.0 . . ? C114 C113 H113 121.0 . . ? C115 C114 C113 121.7(5) . . ? C115 C114 H114 119.1 . . ? C113 C114 H114 119.1 . . ? C114 C115 C116 119.5(5) . . ? C114 C115 H115 120.2 . . ? C116 C115 H115 120.2 . . ? C115 C116 C111 120.7(5) . . ? C115 C116 H116 119.7 . . ? C111 C116 H116 119.7 . . ? C112 O117 C118 119.2(4) . . ? C112 O117 Ru81 110.3(3) . . ? C118 O117 Ru81 128.9(3) . . ? O117 C118 C120 111.1(4) . . ? O117 C118 C119 105.3(4) . . ? C120 C118 C119 113.5(4) . . ? O117 C118 H118 108.9 . . ? C120 C118 H118 108.9 . . ? C119 C118 H118 108.9 . . ? C118 C119 H11A 109.5 . . ? C118 C119 H11B 109.5 . . ? H11A C119 H11B 109.5 . . ? C118 C119 H11C 109.5 . . ? H11A C119 H11C 109.5 . . ? H11B C119 H11C 109.5 . . ? C118 C120 H12A 109.5 . . ? C118 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? C118 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 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 C30 Ru1 C4 N8 -11.3(5) . . . . ? Cl3 Ru1 C4 N8 -111.7(5) . . . . ? Cl2 Ru1 C4 N8 89.0(5) . . . . ? C30 Ru1 C4 N5 174.4(4) . . . . ? Cl3 Ru1 C4 N5 73.9(4) . . . . ? Cl2 Ru1 C4 N5 -85.4(4) . . . . ? N8 C4 N5 C6 1.0(5) . . . . ? Ru1 C4 N5 C6 176.9(3) . . . . ? N8 C4 N5 C11 174.8(4) . . . . ? Ru1 C4 N5 C11 -9.4(7) . . . . ? C4 N5 C6 C7 -1.1(6) . . . . ? C11 N5 C6 C7 -175.1(5) . . . . ? N5 C6 C7 N8 0.7(6) . . . . ? N5 C4 N8 C7 -0.6(5) . . . . ? Ru1 C4 N8 C7 -175.7(4) . . . . ? N5 C4 N8 C21 -173.9(4) . . . . ? Ru1 C4 N8 C21 10.9(8) . . . . ? C6 C7 N8 C4 0.0(6) . . . . ? C6 C7 N8 C21 173.8(4) . . . . ? C4 N5 C11 C12 -90.9(6) . . . . ? C6 N5 C11 C12 82.2(6) . . . . ? C4 N5 C11 C16 94.3(6) . . . . ? C6 N5 C11 C16 -92.6(6) . . . . ? C16 C11 C12 C13 -6.1(7) . . . . ? N5 C11 C12 C13 179.3(4) . . . . ? C16 C11 C12 C17 168.7(4) . . . . ? N5 C11 C12 C17 -5.8(7) . . . . ? C11 C12 C13 C14 0.9(8) . . . . ? C17 C12 C13 C14 -174.1(5) . . . . ? C12 C13 C14 C15 3.5(8) . . . . ? C13 C14 C15 C16 -2.9(8) . . . . ? C14 C15 C16 C11 -2.2(7) . . . . ? C14 C15 C16 C18 171.5(5) . . . . ? C12 C11 C16 C15 6.7(7) . . . . ? N5 C11 C16 C15 -178.7(4) . . . . ? C12 C11 C16 C18 -166.9(5) . . . . ? N5 C11 C16 C18 7.6(7) . . . . ? C4 N8 C21 C22 -95.9(6) . . . . ? C7 N8 C21 C22 91.3(6) . . . . ? C4 N8 C21 C26 87.8(6) . . . . ? C7 N8 C21 C26 -85.0(6) . . . . ? C26 C21 C22 C23 -1.3(8) . . . . ? N8 C21 C22 C23 -177.5(4) . . . . ? C26 C21 C22 C27 -179.8(5) . . . . ? N8 C21 C22 C27 4.1(7) . . . . ? C21 C22 C23 C24 2.0(8) . . . . ? C27 C22 C23 C24 -179.5(5) . . . . ? C22 C23 C24 C25 -1.7(9) . . . . ? C23 C24 C25 C26 0.5(8) . . . . ? C24 C25 C26 C21 0.2(8) . . . . ? C24 C25 C26 C28 -178.9(5) . . . . ? C22 C21 C26 C25 0.2(8) . . . . ? N8 C21 C26 C25 176.5(4) . . . . ? C22 C21 C26 C28 179.3(5) . . . . ? N8 C21 C26 C28 -4.5(7) . . . . ? C4 Ru1 C30 C31 169.7(4) . . . . ? O37 Ru1 C30 C31 -8.3(4) . . . . ? Cl3 Ru1 C30 C31 -94.6(4) . . . . ? Cl2 Ru1 C30 C31 74.6(4) . . . . ? Ru1 C30 C31 C36 -172.5(4) . . . . ? Ru1 C30 C31 C32 6.1(6) . . . . ? C36 C31 C32 C33 3.2(7) . . . . ? C30 C31 C32 C33 -175.4(5) . . . . ? C36 C31 C32 O37 -178.1(4) . . . . ? C30 C31 C32 O37 3.3(6) . . . . ? O37 C32 C33 C34 179.9(4) . . . . ? C31 C32 C33 C34 -1.6(8) . . . . ? C32 C33 C34 C35 -1.0(8) . . . . ? C33 C34 C35 C36 1.8(8) . . . . ? C32 C31 C36 C35 -2.3(7) . . . . ? C30 C31 C36 C35 176.2(5) . . . . ? C34 C35 C36 C31 -0.1(8) . . . . ? C33 C32 O37 C38 -12.9(7) . . . . ? C31 C32 O37 C38 168.4(4) . . . . ? C33 C32 O37 Ru1 169.6(4) . . . . ? C31 C32 O37 Ru1 -9.0(5) . . . . ? C30 Ru1 O37 C32 9.9(3) . . . . ? Cl3 Ru1 O37 C32 109.9(3) . . . . ? Cl2 Ru1 O37 C32 -90.7(3) . . . . ? C30 Ru1 O37 C38 -167.2(4) . . . . ? Cl3 Ru1 O37 C38 -67.1(4) . . . . ? Cl2 Ru1 O37 C38 92.2(4) . . . . ? C32 O37 C38 C39 167.0(5) . . . . ? Ru1 O37 C38 C39 -16.2(7) . . . . ? C32 O37 C38 C40 -70.0(6) . . . . ? Ru1 O37 C38 C40 106.8(5) . . . . ? C70 Ru41 C44 N48 -1.9(5) . . . . ? Cl42 Ru41 C44 N48 98.2(5) . . . . ? Cl43 Ru41 C44 N48 -103.3(5) . . . . ? C70 Ru41 C44 N45 -177.7(4) . . . . ? Cl42 Ru41 C44 N45 -77.6(4) . . . . ? Cl43 Ru41 C44 N45 80.9(4) . . . . ? N48 C44 N45 C46 -1.2(5) . . . . ? Ru41 C44 N45 C46 175.7(3) . . . . ? N48 C44 N45 C51 177.1(4) . . . . ? Ru41 C44 N45 C51 -6.1(7) . . . . ? C44 N45 C46 C47 1.5(6) . . . . ? C51 N45 C46 C47 -176.9(4) . . . . ? N45 C46 C47 N48 -1.0(6) . . . . ? N45 C44 N48 C47 0.5(5) . . . . ? Ru41 C44 N48 C47 -175.9(4) . . . . ? N45 C44 N48 C61A -169.1(6) . . . . ? Ru41 C44 N48 C61A 14.4(9) . . . . ? N45 C44 N48 C61B 164.1(9) . . . . ? Ru41 C44 N48 C61B -12.4(11) . . . . ? C46 C47 N48 C44 0.3(6) . . . . ? C46 C47 N48 C61A 170.5(6) . . . . ? C46 C47 N48 C61B -164.9(9) . . . . ? C46 N45 C51 C52 89.6(6) . . . . ? C44 N45 C51 C52 -88.6(6) . . . . ? C46 N45 C51 C56 -83.4(6) . . . . ? C44 N45 C51 C56 98.5(6) . . . . ? C56 C51 C52 C53 -4.1(7) . . . . ? N45 C51 C52 C53 -176.9(4) . . . . ? C56 C51 C52 C57 171.1(4) . . . . ? N45 C51 C52 C57 -1.6(7) . . . . ? C51 C52 C53 C54 1.4(7) . . . . ? C57 C52 C53 C54 -174.0(5) . . . . ? C52 C53 C54 C55 1.0(8) . . . . ? C53 C54 C55 C56 -0.8(8) . . . . ? C54 C55 C56 C51 -1.8(7) . . . . ? C54 C55 C56 C58 174.3(4) . . . . ? C52 C51 C56 C55 4.3(7) . . . . ? N45 C51 C56 C55 177.0(4) . . . . ? C52 C51 C56 C58 -171.7(4) . . . . ? N45 C51 C56 C58 1.0(7) . . . . ? C44 N48 C61A C62A -103.1(10) . . . . ? C47 N48 C61A C62A 88.0(11) . . . . ? C61B N48 C61A C62A -1(4) . . . . ? C44 N48 C61A C66A 76.2(13) . . . . ? C47 N48 C61A C66A -92.7(12) . . . . ? C61B N48 C61A C66A 178(5) . . . . ? C66A C61A C62A C63A -0.9(18) . . . . ? N48 C61A C62A C63A 178.3(10) . . . . ? C66A C61A C62A C67A -179.5(12) . . . . ? N48 C61A C62A C67A -0.3(15) . . . . ? C61A C62A C63A C64A 0.1(18) . . . . ? C67A C62A C63A C64A 178.7(11) . . . . ? C62A C63A C64A C65A 0(2) . . . . ? C63A C64A C65A C66A 0.5(19) . . . . ? C64A C65A C66A C61A -1.1(17) . . . . ? C64A C65A C66A C68A 177.9(11) . . . . ? C62A C61A C66A C65A 1.4(19) . . . . ? N48 C61A C66A C65A -177.9(10) . . . . ? C62A C61A C66A C68A -177.6(11) . . . . ? N48 C61A C66A C68A 3.2(19) . . . . ? C44 N48 C61B C62B -89(3) . . . . ? C47 N48 C61B C62B 74(3) . . . . ? C61A N48 C61B C62B 177(7) . . . . ? C44 N48 C61B C66B 93(2) . . . . ? C47 N48 C61B C66B -103.7(19) . . . . ? C61A N48 C61B C66B 0(3) . . . . ? C66B C61B C62B C63B 1(4) . . . . ? N48 C61B C62B C63B -176(2) . . . . ? C66B C61B C62B C67B 179(2) . . . . ? N48 C61B C62B C67B 1(4) . . . . ? C61B C62B C63B C64B -5(3) . . . . ? C67B C62B C63B C64B 178(2) . . . . ? C62B C63B C64B C65B 3(4) . . . . ? C63B C64B C65B C66B 2(5) . . . . ? C62B C61B C66B C65B 4(4) . . . . ? N48 C61B C66B C65B -179(2) . . . . ? C62B C61B C66B C68B 176(3) . . . . ? N48 C61B C66B C68B -6(3) . . . . ? C64B C65B C66B C61B -6(4) . . . . ? C64B C65B C66B C68B -178(3) . . . . ? C44 Ru41 C70 C71 179.8(4) . . . . ? O77 Ru41 C70 C71 0.2(4) . . . . ? Cl42 Ru41 C70 C71 84.2(4) . . . . ? Cl43 Ru41 C70 C71 -84.1(4) . . . . ? Ru41 C70 C71 C72 -1.7(7) . . . . ? Ru41 C70 C71 C76 179.6(4) . . . . ? C76 C71 C72 O77 -178.5(5) . . . . ? C70 C71 C72 O77 2.7(7) . . . . ? C76 C71 C72 C73 1.5(8) . . . . ? C70 C71 C72 C73 -177.3(5) . . . . ? O77 C72 C73 C74 178.6(5) . . . . ? C71 C72 C73 C74 -1.5(8) . . . . ? C72 C73 C74 C75 -0.8(8) . . . . ? C73 C74 C75 C76 3.0(8) . . . . ? C74 C75 C76 C71 -3.0(8) . . . . ? C72 C71 C76 C75 0.8(8) . . . . ? C70 C71 C76 C75 179.5(5) . . . . ? C71 C72 O77 C78 167.2(4) . . . . ? C73 C72 O77 C78 -12.8(7) . . . . ? C71 C72 O77 Ru41 -2.3(5) . . . . ? C73 C72 O77 Ru41 177.7(4) . . . . ? C70 Ru41 O77 C72 1.2(3) . . . . ? Cl42 Ru41 O77 C72 -99.0(3) . . . . ? Cl43 Ru41 O77 C72 102.5(3) . . . . ? C70 Ru41 O77 C78 -166.9(4) . . . . ? Cl42 Ru41 O77 C78 92.8(4) . . . . ? Cl43 Ru41 O77 C78 -65.6(4) . . . . ? C72 O77 C78 C79 173.5(4) . . . . ? Ru41 O77 C78 C79 -19.4(6) . . . . ? C72 O77 C78 C80 -64.2(6) . . . . ? Ru41 O77 C78 C80 102.8(4) . . . . ? C110 Ru81 C84 N88 -4.0(5) . . . . ? Cl83 Ru81 C84 N88 -104.5(5) . . . . ? Cl82 Ru81 C84 N88 98.9(5) . . . . ? C110 Ru81 C84 N85 178.5(4) . . . . ? Cl83 Ru81 C84 N85 78.0(4) . . . . ? Cl82 Ru81 C84 N85 -78.6(4) . . . . ? N88 C84 N85 C86 0.9(5) . . . . ? Ru81 C84 N85 C86 179.1(3) . . . . ? N88 C84 N85 C91 179.2(4) . . . . ? Ru81 C84 N85 C91 -2.6(7) . . . . ? C84 N85 C86 C87 -0.9(6) . . . . ? C91 N85 C86 C87 -179.3(5) . . . . ? N85 C86 C87 N88 0.5(6) . . . . ? N85 C84 N88 C87 -0.6(5) . . . . ? Ru81 C84 N88 C87 -178.5(4) . . . . ? N85 C84 N88 C101 -177.1(4) . . . . ? Ru81 C84 N88 C101 5.0(8) . . . . ? C86 C87 N88 C84 0.1(6) . . . . ? C86 C87 N88 C101 176.9(5) . . . . ? C84 N85 C91 C96 93.9(6) . . . . ? C86 N85 C91 C96 -88.0(6) . . . . ? C84 N85 C91 C92 -90.2(6) . . . . ? C86 N85 C91 C92 87.9(6) . . . . ? C96 C91 C92 C93 -6.0(7) . . . . ? N85 C91 C92 C93 178.2(4) . . . . ? C96 C91 C92 C97 168.8(5) . . . . ? N85 C91 C92 C97 -7.0(7) . . . . ? C91 C92 C93 C94 2.4(8) . . . . ? C97 C92 C93 C94 -172.5(5) . . . . ? C92 C93 C94 C95 1.8(8) . . . . ? C93 C94 C95 C96 -2.6(8) . . . . ? C92 C91 C96 C95 5.1(7) . . . . ? N85 C91 C96 C95 -179.1(4) . . . . ? C92 C91 C96 C98 -169.7(5) . . . . ? N85 C91 C96 C98 6.0(7) . . . . ? C94 C95 C96 C91 -0.8(8) . . . . ? C94 C95 C96 C98 174.2(5) . . . . ? C84 N88 C101 C106 92.0(6) . . . . ? C87 N88 C101 C106 -84.3(6) . . . . ? C84 N88 C101 C102 -89.1(6) . . . . ? C87 N88 C101 C102 94.6(6) . . . . ? C106 C101 C102 C103 -1.3(7) . . . . ? N88 C101 C102 C103 179.9(4) . . . . ? C106 C101 C102 C107 177.7(5) . . . . ? N88 C101 C102 C107 -1.1(7) . . . . ? C101 C102 C103 C104 -0.6(7) . . . . ? C107 C102 C103 C104 -179.6(5) . . . . ? C102 C103 C104 C105 2.2(8) . . . . ? C103 C104 C105 C106 -2.0(8) . . . . ? C102 C101 C106 C105 1.4(7) . . . . ? N88 C101 C106 C105 -179.7(4) . . . . ? C102 C101 C106 C108 -176.2(4) . . . . ? N88 C101 C106 C108 2.7(7) . . . . ? C104 C105 C106 C101 0.3(7) . . . . ? C104 C105 C106 C108 177.8(5) . . . . ? C84 Ru81 C110 C111 176.8(3) . . . . ? O117 Ru81 C110 C111 -2.2(3) . . . . ? Cl83 Ru81 C110 C111 -87.8(3) . . . . ? Cl82 Ru81 C110 C111 82.7(3) . . . . ? Ru81 C110 C111 C112 1.5(6) . . . . ? Ru81 C110 C111 C116 -178.1(3) . . . . ? C116 C111 C112 O117 -179.3(4) . . . . ? C110 C111 C112 O117 1.0(6) . . . . ? C116 C111 C112 C113 0.5(7) . . . . ? C110 C111 C112 C113 -179.1(4) . . . . ? O117 C112 C113 C114 -179.5(4) . . . . ? C111 C112 C113 C114 0.7(7) . . . . ? C112 C113 C114 C115 -1.0(7) . . . . ? C113 C114 C115 C116 0.0(7) . . . . ? C114 C115 C116 C111 1.3(7) . . . . ? C112 C111 C116 C115 -1.5(7) . . . . ? C110 C111 C116 C115 178.1(4) . . . . ? C113 C112 O117 C118 10.8(7) . . . . ? C111 C112 O117 C118 -169.3(4) . . . . ? C113 C112 O117 Ru81 177.6(4) . . . . ? C111 C112 O117 Ru81 -2.5(4) . . . . ? C110 Ru81 O117 C112 2.7(3) . . . . ? Cl83 Ru81 O117 C112 102.9(3) . . . . ? Cl82 Ru81 O117 C112 -100.5(3) . . . . ? C110 Ru81 O117 C118 167.8(4) . . . . ? Cl83 Ru81 O117 C118 -91.9(3) . . . . ? Cl82 Ru81 O117 C118 64.7(3) . . . . ? C112 O117 C118 C120 69.0(5) . . . . ? Ru81 O117 C118 C120 -95.0(4) . . . . ? C112 O117 C118 C119 -167.7(4) . . . . ? Ru81 O117 C118 C119 28.3(5) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF