Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Zhong-Ning Chen' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter, CAS Yangqiao Xilu 155 Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email 'CZN@FJIRSM.AC.CN; CHENZN08@GMAIL.COM' _publ_section_title ; Syntheses, characterisation and redox properties of oxo-centred triruthenium cluster dimers and trimers Linked by ortho-metallated polypyridyl ligands ; loop_ _publ_author_name 'Zhong-Ning Chen' 'Jing-Lin Chen' 'Feng-Rong Dai' 'Heng-Yun Ye' ; Li-Yi Zhang ; # Attachment 'Compound 4.CIF' data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 671376' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H42 Cl4 F6 N6 O11 P Ru3' _chemical_formula_weight 1444.84 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.211(3) _cell_length_b 16.784(5) _cell_length_c 16.968(5) _cell_angle_alpha 83.902(6) _cell_angle_beta 78.696(6) _cell_angle_gamma 87.115(8) _cell_volume 2834.0(15) _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 Prism _exptl_crystal_colour Gray _exptl_crystal_size_max 0.5500 _exptl_crystal_size_mid 0.4000 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1434 _exptl_absorpt_coefficient_mu 1.085 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7392 _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 'RIGAKU MERCURY CCD' _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 21942 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12808 _reflns_number_gt 10755 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0856P)^2^+2.9090P] 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 12808 _refine_ls_number_parameters 698 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1488 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.004 _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 1.15847(3) 0.28204(2) 0.112917(19) 0.03631(10) Uani 1 1 d . . . Ru2 Ru 1.33155(3) 0.232170(19) 0.252076(18) 0.03448(9) Uani 1 1 d . . . Ru3 Ru 1.10507(3) 0.38324(2) 0.27850(2) 0.03946(10) Uani 1 1 d . . . Cl1 Cl 0.4851(4) 0.48634(19) 0.12294(19) 0.1499(11) Uani 1 1 d . . . Cl2 Cl 0.7438(3) 0.5074(2) 0.1632(2) 0.1621(13) Uani 1 1 d . . . Cl3 Cl -0.3543(11) 0.2878(5) 0.4860(5) 0.384(6) Uani 1 1 d D . . Cl4 Cl -0.6433(10) 0.2488(11) 0.6137(10) 0.43(2) Uani 0.30 1 d PD . . Cl4' Cl -0.6025(6) 0.2325(4) 0.5335(4) 0.186(2) Uani 0.70 1 d PD . . P1 P 0.6513(2) 0.25389(11) -0.22454(12) 0.0821(5) Uani 1 1 d . . . F1 F 0.7120(7) 0.3168(3) -0.1819(4) 0.147(2) Uani 1 1 d . . . F2 F 0.6172(14) 0.3204(4) -0.2864(6) 0.249(6) Uani 1 1 d . . . F3 F 0.5931(10) 0.1897(4) -0.2629(5) 0.205(4) Uani 1 1 d . . . F4 F 0.6927(11) 0.1891(4) -0.1649(6) 0.226(5) Uani 1 1 d . . . F5 F 0.7692(12) 0.2447(9) -0.2821(8) 0.307(7) Uani 1 1 d . . . F6 F 0.5213(7) 0.2718(8) -0.1720(9) 0.292(7) Uani 1 1 d . . . O1 O 1.2010(2) 0.30257(16) 0.21400(16) 0.0351(6) Uani 1 1 d . . . O2 O 1.1293(3) 0.4072(2) 0.0750(2) 0.0540(8) Uani 1 1 d . . . O3 O 1.1157(4) 0.4699(2) 0.1868(2) 0.0541(8) Uani 1 1 d . . . O4 O 1.0805(3) 0.3100(2) 0.38405(19) 0.0529(8) Uani 1 1 d . . . O5 O 1.2013(3) 0.19729(19) 0.35686(17) 0.0451(7) Uani 1 1 d . . . O6 O 1.3549(3) 0.2967(2) 0.05643(17) 0.0479(7) Uani 1 1 d . . . O7 O 1.4756(3) 0.26243(19) 0.15310(17) 0.0433(7) Uani 1 1 d . . . O8 O 1.4099(3) 0.3164(2) 0.31118(19) 0.0483(7) Uani 1 1 d . . . O9 O 1.2725(3) 0.4244(2) 0.3047(2) 0.0538(8) Uani 1 1 d . . . O10 O 0.9243(3) 0.3497(2) 0.2645(2) 0.0507(8) Uani 1 1 d . . . O11 O 0.9610(3) 0.2721(2) 0.16166(19) 0.0488(7) Uani 1 1 d . . . N1 N 1.0031(4) 0.4714(3) 0.3488(3) 0.0553(10) Uani 1 1 d . . . N2 N 1.1108(4) 0.2635(2) -0.0001(2) 0.0474(8) Uani 1 1 d . . . N3 N 2.2425(5) -0.0832(4) 0.8511(4) 0.0812(15) Uani 1 1 d . . . N4 N 2.0912(5) 0.0764(3) 0.7376(3) 0.0652(12) Uani 1 1 d . . . N5 N 1.4409(3) 0.1339(2) 0.2947(2) 0.0400(7) Uani 1 1 d . . . N6 N 1.2750(3) 0.1464(2) 0.19465(19) 0.0358(7) Uani 1 1 d . . . C1 C 1.8775(5) 0.0356(4) 0.5954(3) 0.0603(13) Uani 1 1 d . . . C01 C 0.6157(11) 0.5477(6) 0.1131(7) 0.142(4) Uani 1 1 d . . . H01A H 0.5829 0.5980 0.1343 0.171 Uiso 1 1 calc R . . H01B H 0.6531 0.5594 0.0562 0.171 Uiso 1 1 calc R . . C2 C 1.8066(5) 0.0450(4) 0.5465(3) 0.0640(14) Uani 1 1 d . . . C02 C -0.4688(11) 0.2574(13) 0.5760(6) 0.241(8) Uiso 1 1 d D . . C3 C 1.7259(5) 0.0546(4) 0.4898(3) 0.0616(13) Uani 1 1 d . . . C4 C 1.6562(5) 0.0623(4) 0.4408(3) 0.0589(13) Uani 1 1 d . . . C11 C 1.9635(5) 0.0222(3) 0.6520(3) 0.0517(11) Uani 1 1 d . . . C12 C 2.0023(5) -0.0541(3) 0.6786(3) 0.0566(12) Uani 1 1 d . . . H12A H 1.9730 -0.0981 0.6587 0.068 Uiso 1 1 calc R . . C13 C 2.0838(5) -0.0655(3) 0.7342(3) 0.0520(11) Uani 1 1 d . . . H13A H 2.1099 -0.1169 0.7526 0.062 Uiso 1 1 calc R . . C14 C 2.1263(5) 0.0010(3) 0.7625(3) 0.0487(10) Uani 1 1 d . . . C15 C 2.0101(6) 0.0870(4) 0.6840(3) 0.0672(14) Uani 1 1 d . . . H15A H 1.9835 0.1389 0.6674 0.081 Uiso 1 1 calc R . . C16 C 2.2147(5) -0.0092(3) 0.8233(3) 0.0527(11) Uani 1 1 d . . . C17 C 2.2665(6) 0.0549(4) 0.8482(4) 0.0748(16) Uani 1 1 d . . . H17A H 2.2458 0.1065 0.8272 0.090 Uiso 1 1 calc R . . C18 C 2.3476(7) 0.0446(5) 0.9032(4) 0.088(2) Uani 1 1 d . . . H18A H 2.3824 0.0883 0.9205 0.106 Uiso 1 1 calc R . . C19 C 2.3766(7) -0.0312(5) 0.9320(4) 0.087(2) Uani 1 1 d . . . H19A H 2.4323 -0.0409 0.9694 0.104 Uiso 1 1 calc R . . C20 C 2.3229(8) -0.0921(5) 0.9053(5) 0.098(2) Uani 1 1 d . . . H20A H 2.3430 -0.1440 0.9257 0.117 Uiso 1 1 calc R . . C21 C 1.5745(4) 0.0626(3) 0.3816(3) 0.0512(11) Uani 1 1 d . . . C22 C 1.5468(5) -0.0083(3) 0.3555(3) 0.0605(13) Uani 1 1 d . . . H22A H 1.5834 -0.0563 0.3755 0.073 Uiso 1 1 calc R . . C23 C 1.4646(5) -0.0086(3) 0.2996(3) 0.0554(11) Uani 1 1 d . . . H23A H 1.4451 -0.0566 0.2821 0.066 Uiso 1 1 calc R . . C24 C 1.4120(4) 0.0635(3) 0.2702(3) 0.0424(9) Uani 1 1 d . . . C26 C 1.5194(4) 0.1330(3) 0.3496(3) 0.0461(10) Uani 1 1 d . . . H26A H 1.5376 0.1813 0.3669 0.055 Uiso 1 1 calc R . . C27 C 1.3210(4) 0.0703(3) 0.2128(3) 0.0414(9) Uani 1 1 d . . . C28 C 1.2825(5) 0.0076(3) 0.1779(3) 0.0506(10) Uani 1 1 d . . . H28A H 1.3119 -0.0446 0.1910 0.061 Uiso 1 1 calc R . . C29 C 1.1584(5) 0.1006(3) 0.1026(3) 0.0482(10) Uani 1 1 d . . . H29A H 1.1038 0.1104 0.0645 0.058 Uiso 1 1 calc R . . C30 C 1.1989(5) 0.0237(3) 0.1226(3) 0.0533(11) Uani 1 1 d . . . H30A H 1.1703 -0.0182 0.0990 0.064 Uiso 1 1 calc R . . C31 C 1.1971(4) 0.1657(3) 0.1383(2) 0.0373(8) Uani 1 1 d . . . C32 C 1.1231(4) 0.4681(3) 0.1113(3) 0.0495(10) Uani 1 1 d . . . C33 C 1.1204(7) 0.5490(4) 0.0644(4) 0.0748(16) Uani 1 1 d . . . H33A H 1.1254 0.5425 0.0083 0.112 Uiso 1 1 calc R . . H33B H 1.1952 0.5788 0.0703 0.112 Uiso 1 1 calc R . . H33C H 1.0388 0.5775 0.0845 0.112 Uiso 1 1 calc R . . C34 C 1.1178(4) 0.2384(3) 0.4004(3) 0.0448(9) Uani 1 1 d . . . C35 C 1.0566(7) 0.1997(4) 0.4824(3) 0.0732(17) Uani 1 1 d . . . H35A H 1.0902 0.1454 0.4886 0.110 Uiso 1 1 calc R . . H35B H 0.9612 0.2000 0.4878 0.110 Uiso 1 1 calc R . . H35C H 1.0793 0.2289 0.5233 0.110 Uiso 1 1 calc R . . C36 C 1.4608(4) 0.2875(3) 0.0826(3) 0.0432(9) Uani 1 1 d . . . C37 C 1.5881(5) 0.3087(4) 0.0234(3) 0.0720(17) Uani 1 1 d . . . H37A H 1.5674 0.3265 -0.0286 0.108 Uiso 1 1 calc R . . H37B H 1.6472 0.2624 0.0190 0.108 Uiso 1 1 calc R . . H37C H 1.6307 0.3508 0.0421 0.108 Uiso 1 1 calc R . . C38 C 1.3794(4) 0.3877(3) 0.3187(3) 0.0469(10) Uani 1 1 d . . . C39 C 1.4728(6) 0.4389(4) 0.3479(4) 0.0722(16) Uani 1 1 d . . . H39A H 1.5505 0.4073 0.3570 0.108 Uiso 1 1 calc R . . H39B H 1.4286 0.4590 0.3975 0.108 Uiso 1 1 calc R . . H39C H 1.4991 0.4830 0.3080 0.108 Uiso 1 1 calc R . . C40 C 0.8881(4) 0.3035(3) 0.2196(3) 0.0432(9) Uani 1 1 d . . . C41 C 0.7435(5) 0.2840(4) 0.2361(4) 0.0690(16) Uani 1 1 d . . . H41A H 0.6972 0.3107 0.2813 0.103 Uiso 1 1 calc R . . H41B H 0.7344 0.2271 0.2482 0.103 Uiso 1 1 calc R . . H41C H 0.7059 0.3016 0.1894 0.103 Uiso 1 1 calc R . . C42 C 0.8962(6) 0.4540(4) 0.4050(4) 0.0785(18) Uani 1 1 d . . . H42A H 0.8637 0.4025 0.4104 0.094 Uiso 1 1 calc R . . C43 C 0.8303(8) 0.5084(5) 0.4562(5) 0.106(3) Uani 1 1 d . . . H43A H 0.7558 0.4944 0.4954 0.127 Uiso 1 1 calc R . . C44 C 0.8811(10) 0.5854(5) 0.4460(6) 0.118(3) Uani 1 1 d . . . H44A H 0.8403 0.6237 0.4794 0.142 Uiso 1 1 calc R . . C45 C 0.9902(8) 0.6050(5) 0.3876(5) 0.096(2) Uani 1 1 d . . . H45A H 1.0231 0.6565 0.3793 0.116 Uiso 1 1 calc R . . C46 C 1.0501(6) 0.5450(4) 0.3408(4) 0.0717(16) Uani 1 1 d . . . H46A H 1.1266 0.5568 0.3023 0.086 Uiso 1 1 calc R . . C47 C 0.9862(6) 0.2445(4) -0.0059(4) 0.0718(17) Uani 1 1 d . . . H47A H 0.9218 0.2365 0.0411 0.086 Uiso 1 1 calc R . . C48 C 0.9511(7) 0.2366(5) -0.0794(4) 0.086(2) Uani 1 1 d . . . H48A H 0.8649 0.2230 -0.0820 0.103 Uiso 1 1 calc R . . C49 C 1.0470(8) 0.2494(4) -0.1488(4) 0.083(2) Uani 1 1 d . . . H49A H 1.0255 0.2461 -0.1992 0.099 Uiso 1 1 calc R . . C50 C 1.1717(8) 0.2666(5) -0.1429(4) 0.092(2) Uani 1 1 d . . . H50A H 1.2377 0.2747 -0.1890 0.111 Uiso 1 1 calc R . . C51 C 1.2007(7) 0.2722(4) -0.0675(3) 0.0717(16) Uani 1 1 d . . . H51A H 1.2880 0.2825 -0.0641 0.086 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 0.03337(16) 0.04146(19) 0.03539(17) -0.00683(13) -0.00838(12) -0.00013(13) Ru2 0.03249(16) 0.03817(18) 0.03353(16) -0.00486(12) -0.00693(12) -0.00327(12) Ru3 0.03705(17) 0.03963(19) 0.04217(19) -0.01117(14) -0.00463(13) -0.00239(13) Cl1 0.190(3) 0.115(2) 0.138(2) 0.0089(17) -0.021(2) -0.037(2) Cl2 0.130(2) 0.152(3) 0.176(3) 0.046(2) 0.002(2) 0.0071(19) Cl3 0.585(15) 0.332(9) 0.276(7) 0.098(6) -0.204(9) -0.217(10) Cl4 0.55(4) 0.48(4) 0.37(3) -0.32(3) -0.35(3) 0.40(4) Cl4' 0.182(5) 0.225(6) 0.184(5) -0.087(4) -0.090(4) 0.056(4) P1 0.0984(13) 0.0687(11) 0.0904(12) -0.0264(9) -0.0376(10) 0.0050(9) F1 0.204(6) 0.102(4) 0.164(5) -0.028(4) -0.091(5) -0.035(4) F2 0.461(18) 0.120(5) 0.238(9) 0.000(6) -0.252(12) -0.020(8) F3 0.377(12) 0.091(4) 0.210(7) -0.020(4) -0.196(8) -0.050(5) F4 0.402(13) 0.083(4) 0.262(9) 0.010(5) -0.249(10) -0.015(6) F5 0.250(11) 0.352(17) 0.272(12) -0.121(12) 0.110(10) 0.016(11) F6 0.101(5) 0.353(16) 0.415(18) -0.162(14) 0.039(7) -0.020(7) O1 0.0308(12) 0.0386(15) 0.0358(13) -0.0048(11) -0.0051(10) -0.0044(11) O2 0.064(2) 0.0464(19) 0.0532(19) -0.0028(15) -0.0182(16) 0.0057(15) O3 0.067(2) 0.0422(18) 0.0528(19) -0.0062(14) -0.0093(16) 0.0000(15) O4 0.060(2) 0.054(2) 0.0402(16) -0.0085(14) 0.0029(14) 0.0007(16) O5 0.0475(16) 0.0464(17) 0.0385(15) -0.0040(13) -0.0005(12) -0.0032(13) O6 0.0378(15) 0.065(2) 0.0385(15) -0.0003(14) -0.0029(12) -0.0031(14) O7 0.0332(13) 0.0534(18) 0.0416(15) -0.0009(13) -0.0045(11) -0.0037(12) O8 0.0461(16) 0.0516(19) 0.0528(18) -0.0142(14) -0.0174(14) -0.0035(14) O9 0.0457(17) 0.0503(19) 0.069(2) -0.0191(16) -0.0112(15) -0.0078(14) O10 0.0353(14) 0.059(2) 0.0591(19) -0.0223(16) -0.0046(13) -0.0009(14) O11 0.0347(14) 0.062(2) 0.0523(18) -0.0177(15) -0.0077(13) -0.0028(14) N1 0.054(2) 0.053(2) 0.058(2) -0.0184(19) -0.0047(19) 0.0035(19) N2 0.053(2) 0.047(2) 0.046(2) -0.0100(16) -0.0176(16) 0.0039(17) N3 0.075(3) 0.085(4) 0.092(4) -0.002(3) -0.044(3) 0.010(3) N4 0.078(3) 0.058(3) 0.065(3) -0.002(2) -0.029(2) -0.008(2) N5 0.0351(16) 0.046(2) 0.0369(17) -0.0019(14) -0.0032(13) -0.0018(14) N6 0.0351(16) 0.0362(17) 0.0368(16) -0.0062(13) -0.0068(13) -0.0015(13) C1 0.051(3) 0.079(4) 0.050(3) 0.005(2) -0.012(2) -0.006(2) C01 0.160(10) 0.088(6) 0.154(9) 0.029(6) 0.004(8) 0.015(6) C2 0.052(3) 0.086(4) 0.052(3) 0.008(3) -0.013(2) -0.004(3) C3 0.049(3) 0.081(4) 0.051(3) 0.010(3) -0.009(2) -0.003(3) C4 0.047(2) 0.082(4) 0.042(2) 0.011(2) -0.005(2) 0.003(2) C11 0.046(2) 0.068(3) 0.042(2) -0.002(2) -0.0101(19) -0.010(2) C12 0.056(3) 0.058(3) 0.059(3) -0.010(2) -0.015(2) -0.008(2) C13 0.052(3) 0.048(3) 0.057(3) 0.000(2) -0.017(2) -0.002(2) C14 0.048(2) 0.057(3) 0.041(2) -0.0052(19) -0.0059(18) -0.005(2) C15 0.083(4) 0.064(4) 0.058(3) 0.003(3) -0.028(3) -0.008(3) C16 0.043(2) 0.069(3) 0.046(2) -0.010(2) -0.0083(19) 0.003(2) C17 0.082(4) 0.079(4) 0.073(4) -0.022(3) -0.030(3) 0.002(3) C18 0.089(5) 0.113(6) 0.079(4) -0.037(4) -0.039(4) 0.002(4) C19 0.069(4) 0.126(7) 0.074(4) -0.020(4) -0.033(3) 0.012(4) C20 0.090(5) 0.114(6) 0.098(5) 0.000(5) -0.051(4) 0.023(4) C21 0.037(2) 0.069(3) 0.043(2) 0.006(2) -0.0055(18) 0.003(2) C22 0.056(3) 0.062(3) 0.058(3) 0.012(2) -0.010(2) 0.012(2) C23 0.058(3) 0.047(3) 0.059(3) 0.000(2) -0.012(2) 0.004(2) C24 0.038(2) 0.042(2) 0.044(2) 0.0022(17) -0.0032(17) 0.0003(17) C26 0.040(2) 0.058(3) 0.040(2) 0.0003(19) -0.0090(17) -0.0013(19) C27 0.038(2) 0.043(2) 0.041(2) -0.0050(17) -0.0031(16) 0.0001(17) C28 0.055(3) 0.038(2) 0.058(3) -0.011(2) -0.007(2) 0.000(2) C29 0.049(2) 0.053(3) 0.046(2) -0.015(2) -0.0106(19) -0.003(2) C30 0.062(3) 0.044(3) 0.056(3) -0.018(2) -0.009(2) -0.011(2) C31 0.0322(18) 0.046(2) 0.0336(18) -0.0091(16) -0.0036(14) -0.0028(16) C32 0.044(2) 0.042(2) 0.062(3) 0.000(2) -0.011(2) -0.0042(19) C33 0.096(4) 0.055(3) 0.070(4) 0.013(3) -0.017(3) -0.003(3) C34 0.048(2) 0.047(3) 0.039(2) -0.0080(18) -0.0042(18) -0.0104(19) C35 0.092(4) 0.070(4) 0.046(3) -0.002(2) 0.018(3) -0.013(3) C36 0.037(2) 0.046(2) 0.044(2) -0.0027(18) -0.0027(17) 0.0010(17) C37 0.045(3) 0.104(5) 0.058(3) 0.014(3) 0.001(2) -0.006(3) C38 0.043(2) 0.055(3) 0.046(2) -0.015(2) -0.0082(18) -0.012(2) C39 0.056(3) 0.074(4) 0.095(4) -0.035(3) -0.021(3) -0.014(3) C40 0.036(2) 0.042(2) 0.050(2) -0.0018(18) -0.0078(17) -0.0005(17) C41 0.037(2) 0.082(4) 0.091(4) -0.027(3) -0.008(2) -0.006(2) C42 0.065(3) 0.076(4) 0.091(4) -0.033(3) 0.006(3) 0.004(3) C43 0.095(5) 0.107(6) 0.107(6) -0.055(5) 0.020(4) 0.011(5) C44 0.141(8) 0.089(6) 0.119(7) -0.061(5) 0.012(6) 0.019(5) C45 0.108(6) 0.068(4) 0.117(6) -0.050(4) -0.015(5) 0.011(4) C46 0.079(4) 0.053(3) 0.083(4) -0.027(3) -0.005(3) -0.002(3) C47 0.054(3) 0.106(5) 0.064(3) -0.031(3) -0.025(3) 0.015(3) C48 0.082(4) 0.116(6) 0.075(4) -0.044(4) -0.044(4) 0.031(4) C49 0.119(6) 0.082(4) 0.062(4) -0.026(3) -0.050(4) 0.016(4) C50 0.119(6) 0.119(6) 0.044(3) -0.017(3) -0.015(3) -0.038(5) C51 0.083(4) 0.092(5) 0.044(3) -0.012(3) -0.011(3) -0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 1.919(3) . ? Ru1 C31 1.991(4) . ? Ru1 O11 2.032(3) . ? Ru1 O6 2.061(3) . ? Ru1 N2 2.126(4) . ? Ru1 O2 2.155(3) . ? Ru2 O1 1.899(3) . ? Ru2 N6 1.990(3) . ? Ru2 O7 2.042(3) . ? Ru2 O5 2.050(3) . ? Ru2 N5 2.090(4) . ? Ru2 O8 2.091(3) . ? Ru3 O1 1.937(3) . ? Ru3 O3 2.005(3) . ? Ru3 O9 2.020(3) . ? Ru3 O10 2.021(3) . ? Ru3 O4 2.041(3) . ? Ru3 N1 2.105(4) . ? Cl1 C01 1.698(12) . ? Cl2 C01 1.765(11) . ? Cl3 C02 1.777(5) . ? Cl4 Cl4' 1.395(15) . ? Cl4 C02 1.779(5) . ? Cl4' C02 1.751(5) . ? P1 F5 1.407(8) . ? P1 F6 1.482(8) . ? P1 F4 1.508(6) . ? P1 F3 1.518(5) . ? P1 F2 1.524(7) . ? P1 F1 1.558(5) . ? O2 C32 1.240(6) . ? O3 C32 1.272(6) . ? O4 C34 1.261(6) . ? O5 C34 1.246(5) . ? O6 C36 1.243(5) . ? O7 C36 1.261(5) . ? O8 C38 1.236(6) . ? O9 C38 1.276(6) . ? O10 C40 1.259(5) . ? O11 C40 1.258(5) . ? N1 C42 1.323(7) . ? N1 C46 1.331(7) . ? N2 C51 1.318(7) . ? N2 C47 1.351(7) . ? N3 C16 1.318(7) . ? N3 C20 1.340(8) . ? N4 C15 1.338(7) . ? N4 C14 1.344(7) . ? N5 C26 1.343(5) . ? N5 C24 1.356(6) . ? N6 C27 1.363(5) . ? N6 C31 1.364(5) . ? C1 C2 1.196(7) . ? C1 C11 1.418(7) . ? C2 C3 1.378(7) . ? C3 C4 1.189(7) . ? C4 C21 1.425(7) . ? C11 C12 1.377(7) . ? C11 C15 1.409(8) . ? C12 C13 1.368(7) . ? C13 C14 1.382(7) . ? C14 C16 1.489(6) . ? C16 C17 1.364(8) . ? C17 C18 1.357(8) . ? C18 C19 1.354(11) . ? C19 C20 1.343(11) . ? C21 C22 1.374(8) . ? C21 C26 1.386(7) . ? C22 C23 1.385(7) . ? C23 C24 1.385(6) . ? C24 C27 1.465(6) . ? C27 C28 1.370(6) . ? C28 C30 1.386(7) . ? C29 C30 1.365(7) . ? C29 C31 1.412(6) . ? C32 C33 1.502(7) . ? C34 C35 1.503(6) . ? C36 C37 1.512(6) . ? C38 C39 1.500(6) . ? C40 C41 1.494(6) . ? C42 C43 1.385(9) . ? C43 C44 1.398(12) . ? C44 C45 1.366(12) . ? C45 C46 1.391(8) . ? C47 C48 1.385(8) . ? C48 C49 1.381(10) . ? C49 C50 1.345(10) . ? C50 C51 1.382(8) . ? 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 C31 89.55(14) . . ? O1 Ru1 O11 92.37(11) . . ? C31 Ru1 O11 92.89(15) . . ? O1 Ru1 O6 90.65(11) . . ? C31 Ru1 O6 89.82(14) . . ? O11 Ru1 O6 175.96(13) . . ? O1 Ru1 N2 178.11(13) . . ? C31 Ru1 N2 92.32(15) . . ? O11 Ru1 N2 87.76(14) . . ? O6 Ru1 N2 89.13(14) . . ? O1 Ru1 O2 93.68(12) . . ? C31 Ru1 O2 174.69(14) . . ? O11 Ru1 O2 91.19(14) . . ? O6 Ru1 O2 85.93(13) . . ? N2 Ru1 O2 84.44(14) . . ? O1 Ru2 N6 89.03(12) . . ? O1 Ru2 O7 93.19(11) . . ? N6 Ru2 O7 89.34(13) . . ? O1 Ru2 O5 92.07(12) . . ? N6 Ru2 O5 92.34(13) . . ? O7 Ru2 O5 174.51(12) . . ? O1 Ru2 N5 166.12(12) . . ? N6 Ru2 N5 79.47(14) . . ? O7 Ru2 N5 94.41(12) . . ? O5 Ru2 N5 80.76(12) . . ? O1 Ru2 O8 96.16(12) . . ? N6 Ru2 O8 174.20(13) . . ? O7 Ru2 O8 87.80(12) . . ? O5 Ru2 O8 90.06(13) . . ? N5 Ru2 O8 95.72(13) . . ? O1 Ru3 O3 95.37(13) . . ? O1 Ru3 O9 93.73(12) . . ? O3 Ru3 O9 89.03(15) . . ? O1 Ru3 O10 93.51(12) . . ? O3 Ru3 O10 92.46(15) . . ? O9 Ru3 O10 172.44(13) . . ? O1 Ru3 O4 94.39(12) . . ? O3 Ru3 O4 170.18(13) . . ? O9 Ru3 O4 89.20(15) . . ? O10 Ru3 O4 88.07(15) . . ? O1 Ru3 N1 179.28(14) . . ? O3 Ru3 N1 84.59(16) . . ? O9 Ru3 N1 85.55(15) . . ? O10 Ru3 N1 87.21(15) . . ? O4 Ru3 N1 85.64(16) . . ? Cl4' Cl4 C02 65.7(4) . . ? Cl4 Cl4' C02 67.8(4) . . ? F5 P1 F6 172.3(9) . . ? F5 P1 F4 93.4(8) . . ? F6 P1 F4 94.3(8) . . ? F5 P1 F3 87.1(7) . . ? F6 P1 F3 92.8(6) . . ? F4 P1 F3 88.5(4) . . ? F5 P1 F2 84.0(8) . . ? F6 P1 F2 88.3(7) . . ? F4 P1 F2 177.0(7) . . ? F3 P1 F2 92.9(4) . . ? F5 P1 F1 93.5(6) . . ? F6 P1 F1 87.0(5) . . ? F4 P1 F1 88.9(3) . . ? F3 P1 F1 177.4(4) . . ? F2 P1 F1 89.7(4) . . ? Ru2 O1 Ru1 115.85(14) . . ? Ru2 O1 Ru3 121.69(14) . . ? Ru1 O1 Ru3 122.20(14) . . ? C32 O2 Ru1 131.9(3) . . ? C32 O3 Ru3 132.4(3) . . ? C34 O4 Ru3 132.0(3) . . ? C34 O5 Ru2 129.3(3) . . ? C36 O6 Ru1 131.6(3) . . ? C36 O7 Ru2 128.2(3) . . ? C38 O8 Ru2 131.2(3) . . ? C38 O9 Ru3 131.1(3) . . ? C40 O10 Ru3 133.2(3) . . ? C40 O11 Ru1 131.7(3) . . ? C42 N1 C46 118.6(5) . . ? C42 N1 Ru3 121.0(4) . . ? C46 N1 Ru3 120.2(4) . . ? C51 N2 C47 117.5(4) . . ? C51 N2 Ru1 121.2(3) . . ? C47 N2 Ru1 121.2(3) . . ? C16 N3 C20 116.9(6) . . ? C15 N4 C14 118.3(5) . . ? C26 N5 C24 119.3(4) . . ? C26 N5 Ru2 126.8(3) . . ? C24 N5 Ru2 113.4(3) . . ? C27 N6 C31 123.2(3) . . ? C27 N6 Ru2 117.0(3) . . ? C31 N6 Ru2 119.7(3) . . ? C2 C1 C11 178.1(7) . . ? Cl1 C01 Cl2 113.9(5) . . ? C1 C2 C3 179.0(7) . . ? Cl4' C02 Cl3 99.2(6) . . ? Cl4' C02 Cl4 46.5(5) . . ? Cl3 C02 Cl4 140.9(10) . . ? C4 C3 C2 179.6(7) . . ? C3 C4 C21 173.9(7) . . ? C12 C11 C15 117.8(5) . . ? C12 C11 C1 121.5(5) . . ? C15 C11 C1 120.7(5) . . ? C13 C12 C11 120.4(5) . . ? C12 C13 C14 118.5(5) . . ? N4 C14 C13 122.8(4) . . ? N4 C14 C16 117.3(4) . . ? C13 C14 C16 119.9(5) . . ? N4 C15 C11 122.1(5) . . ? N3 C16 C17 121.3(5) . . ? N3 C16 C14 117.1(5) . . ? C17 C16 C14 121.6(5) . . ? C18 C17 C16 120.9(7) . . ? C19 C18 C17 118.1(7) . . ? C20 C19 C18 118.5(6) . . ? N3 C20 C19 124.4(7) . . ? C22 C21 C26 118.1(4) . . ? C22 C21 C4 120.0(5) . . ? C26 C21 C4 121.9(5) . . ? C21 C22 C23 120.3(5) . . ? C24 C23 C22 118.9(5) . . ? N5 C24 C23 121.0(4) . . ? N5 C24 C27 115.3(4) . . ? C23 C24 C27 123.7(4) . . ? N5 C26 C21 122.4(5) . . ? N6 C27 C28 120.4(4) . . ? N6 C27 C24 114.5(4) . . ? C28 C27 C24 125.1(4) . . ? C27 C28 C30 118.5(4) . . ? C30 C29 C31 121.7(4) . . ? C29 C30 C28 120.3(4) . . ? N6 C31 C29 115.7(4) . . ? N6 C31 Ru1 116.3(3) . . ? C29 C31 Ru1 128.0(3) . . ? O2 C32 O3 126.5(4) . . ? O2 C32 C33 119.0(5) . . ? O3 C32 C33 114.5(5) . . ? O5 C34 O4 127.2(4) . . ? O5 C34 C35 116.9(4) . . ? O4 C34 C35 115.9(4) . . ? O6 C36 O7 127.9(4) . . ? O6 C36 C37 116.8(4) . . ? O7 C36 C37 115.3(4) . . ? O8 C38 O9 126.4(4) . . ? O8 C38 C39 119.3(5) . . ? O9 C38 C39 114.3(5) . . ? O11 C40 O10 126.7(4) . . ? O11 C40 C41 116.3(4) . . ? O10 C40 C41 117.0(4) . . ? N1 C42 C43 123.3(7) . . ? C42 C43 C44 116.9(7) . . ? C45 C44 C43 120.7(6) . . ? C44 C45 C46 117.4(7) . . ? N1 C46 C45 123.0(6) . . ? N2 C47 C48 122.2(6) . . ? C49 C48 C47 118.4(6) . . ? C50 C49 C48 119.3(5) . . ? C49 C50 C51 119.3(7) . . ? N2 C51 C50 123.2(6) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.882 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.103