# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Zhong-Ning Chen.' 'Feng-Rong Dai.' 'Bin Li.' 'Heng-Yun Ye.' 'Li-Yi Zhang.' _publ_contact_author_name 'Zhong-Ning Chen' _publ_contact_author_email CZN@FJIRSM.AC.CN _publ_section_title ; Low-valence oxo-centred triruthenium complexes by bridging acetate substitution with pyrazolydiazine or pyridinyltetrazine ligands ; # Attachment 'compound 3.cif' data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 730666' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H30 Cl N6 O11 Ru3, 0.5(C6 H14), C H2 Cl2, F6 P' _chemical_formula_sum 'C31 H39 Cl3 F6 N6 O11 P Ru3' _chemical_formula_weight 1226.21 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 8.293(3) _cell_length_b 16.948(6) _cell_length_c 17.245(5) _cell_angle_alpha 71.464(9) _cell_angle_beta 78.345(12) _cell_angle_gamma 79.469(11) _cell_volume 2232.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4585 _cell_measurement_theta_min 3.0218 _cell_measurement_theta_max 27.4680 _exptl_crystal_description Platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1214 _exptl_absorpt_coefficient_mu 1.302 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5747 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU SATURN70' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14364 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0893 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7741 _reflns_number_gt 5681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0637P)^2^+4.0093P] 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 7741 _refine_ls_number_parameters 578 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.062 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.17903(7) 0.29306(3) 0.39792(3) 0.01910(16) Uani 1 1 d . . . Ru2 Ru 0.41658(7) 0.31309(3) 0.22241(3) 0.01892(16) Uani 1 1 d . . . Ru3 Ru 0.24632(7) 0.13450(4) 0.31494(3) 0.02110(16) Uani 1 1 d . . . Cl1 Cl 0.8113(2) 0.34522(12) 0.23885(11) 0.0307(4) Uani 1 1 d . . . O1 O 0.2737(6) 0.2435(3) 0.3101(3) 0.0201(10) Uani 1 1 d . . . O2 O 0.0607(6) 0.4002(3) 0.3272(3) 0.0250(11) Uani 1 1 d . . . O3 O 0.2387(6) 0.4168(3) 0.2077(3) 0.0223(11) Uani 1 1 d . . . O4 O 0.2838(6) 0.1920(3) 0.4830(3) 0.0254(11) Uani 1 1 d . . . O5 O 0.2777(7) 0.0821(3) 0.4379(3) 0.0300(12) Uani 1 1 d . . . O6 O -0.0412(6) 0.2393(3) 0.4294(3) 0.0258(12) Uani 1 1 d . . . O7 O -0.0040(6) 0.1484(3) 0.3544(3) 0.0281(12) Uani 1 1 d . . . O8 O 0.3225(6) 0.2886(3) 0.1315(3) 0.0267(12) Uani 1 1 d . . . O9 O 0.2022(7) 0.1701(3) 0.1954(3) 0.0325(13) Uani 1 1 d . . . O10 O 0.6080(6) 0.2192(3) 0.2159(3) 0.0263(11) Uani 1 1 d . . . O11 O 0.4955(6) 0.0995(3) 0.2797(3) 0.0312(12) Uani 1 1 d . . . N1 N 0.1259(8) 0.3484(4) 0.4913(4) 0.0260(14) Uani 1 1 d . . . N2 N 0.2670(8) 0.3779(4) 0.4979(4) 0.0274(14) Uani 1 1 d . . . N3 N 0.3815(7) 0.3439(4) 0.3795(4) 0.0240(13) Uani 1 1 d . . . N4 N 0.5028(7) 0.3424(3) 0.3111(3) 0.0223(13) Uani 1 1 d . . . N5 N 0.5579(7) 0.3912(4) 0.1237(3) 0.0191(12) Uani 1 1 d . . . N6 N 0.2176(8) 0.0111(4) 0.3173(4) 0.0269(14) Uani 1 1 d . . . C1 C 0.6504(9) 0.3613(5) 0.3141(4) 0.0253(16) Uani 1 1 d . . . C2 C 0.6810(10) 0.3901(5) 0.3766(5) 0.0301(18) Uani 1 1 d . . . H2A H 0.7854 0.4038 0.3750 0.036 Uiso 1 1 calc R . . C3 C 0.5566(9) 0.3978(5) 0.4398(5) 0.0281(18) Uani 1 1 d . . . H3A H 0.5720 0.4179 0.4818 0.034 Uiso 1 1 calc R . . C4 C 0.4059(10) 0.3742(5) 0.4384(4) 0.0279(17) Uani 1 1 d . . . C5 C 0.2350(11) 0.4124(6) 0.5615(5) 0.042(2) Uani 1 1 d . . . H5A H 0.3103 0.4350 0.5790 0.050 Uiso 1 1 calc R . . C6 C 0.0716(12) 0.4077(7) 0.5949(6) 0.052(3) Uani 1 1 d . . . H6A H 0.0125 0.4279 0.6381 0.063 Uiso 1 1 calc R . . C7 C 0.0118(10) 0.3659(5) 0.5501(5) 0.0308(18) Uani 1 1 d . . . H7A H -0.0958 0.3522 0.5610 0.037 Uiso 1 1 calc R . . C8 C 0.5595(9) 0.4723(4) 0.1184(5) 0.0250(16) Uani 1 1 d . . . H8A H 0.4938 0.4936 0.1595 0.030 Uiso 1 1 calc R . . C9 C 0.6531(9) 0.5246(5) 0.0553(4) 0.0285(17) Uani 1 1 d . . . H9A H 0.6498 0.5802 0.0539 0.034 Uiso 1 1 calc R . . C10 C 0.7511(10) 0.4950(5) -0.0055(4) 0.0315(19) Uani 1 1 d . . . H10A H 0.8158 0.5298 -0.0487 0.038 Uiso 1 1 calc R . . C11 C 0.7524(10) 0.4113(5) -0.0015(5) 0.0322(18) Uani 1 1 d . . . H11A H 0.8191 0.3888 -0.0417 0.039 Uiso 1 1 calc R . . C12 C 0.6537(9) 0.3631(5) 0.0625(4) 0.0286(17) Uani 1 1 d . . . H12A H 0.6526 0.3079 0.0640 0.034 Uiso 1 1 calc R . . C13 C 0.3060(12) -0.0210(5) 0.2588(6) 0.044(2) Uani 1 1 d . . . H13A H 0.3800 0.0105 0.2179 0.053 Uiso 1 1 calc R . . C14 C 0.2910(13) -0.1000(6) 0.2570(6) 0.056(3) Uani 1 1 d . . . H14A H 0.3546 -0.1209 0.2152 0.068 Uiso 1 1 calc R . . C15 C 0.1846(13) -0.1474(6) 0.3157(6) 0.050(2) Uani 1 1 d . . . H15A H 0.1756 -0.2012 0.3155 0.060 Uiso 1 1 calc R . . C16 C 0.0896(10) -0.1136(5) 0.3758(5) 0.0336(19) Uani 1 1 d . . . H16A H 0.0131 -0.1439 0.4162 0.040 Uiso 1 1 calc R . . C17 C 0.1093(10) -0.0350(5) 0.3753(5) 0.0300(18) Uani 1 1 d . . . H17A H 0.0459 -0.0127 0.4163 0.036 Uiso 1 1 calc R . . C18 C 0.1121(9) 0.4390(5) 0.2529(4) 0.0236(16) Uani 1 1 d . . . C19 C 0.0089(10) 0.5203(4) 0.2148(5) 0.0288(17) Uani 1 1 d . . . H19A H 0.0587 0.5441 0.1586 0.043 Uiso 1 1 calc R . . H19B H 0.0037 0.5589 0.2459 0.043 Uiso 1 1 calc R . . H19C H -0.1012 0.5096 0.2156 0.043 Uiso 1 1 calc R . . C20 C 0.2392(10) 0.2328(5) 0.1334(4) 0.0298(18) Uani 1 1 d U . . C21 C 0.1671(12) 0.2427(6) 0.0586(5) 0.047(3) Uani 1 1 d U . . H21A H 0.2007 0.2918 0.0161 0.071 Uiso 1 1 calc R . . H21B H 0.0483 0.2486 0.0718 0.071 Uiso 1 1 calc R . . H21C H 0.2056 0.1942 0.0394 0.071 Uiso 1 1 calc R . . C22 C 0.6142(9) 0.1409(5) 0.2415(4) 0.0223(16) Uani 1 1 d . . . C23 C 0.7815(10) 0.0913(5) 0.2259(5) 0.0324(19) Uani 1 1 d . . . H23A H 0.8616 0.1290 0.1964 0.049 Uiso 1 1 calc R . . H23B H 0.7745 0.0555 0.1936 0.049 Uiso 1 1 calc R . . H23C H 0.8150 0.0576 0.2778 0.049 Uiso 1 1 calc R . . C24 C 0.3056(9) 0.1140(4) 0.4893(4) 0.0236(16) Uani 1 1 d . . . C25 C 0.3604(10) 0.0558(5) 0.5685(4) 0.0317(19) Uani 1 1 d . . . H25A H 0.3719 -0.0012 0.5674 0.047 Uiso 1 1 calc R . . H25B H 0.2790 0.0632 0.6148 0.047 Uiso 1 1 calc R . . H25C H 0.4651 0.0685 0.5739 0.047 Uiso 1 1 calc R . . C26 C -0.0894(9) 0.1873(4) 0.4036(4) 0.0217(16) Uani 1 1 d . . . C27 C -0.2645(9) 0.1682(5) 0.4350(5) 0.0350(19) Uani 1 1 d . . . H27A H -0.3178 0.2009 0.4716 0.052 Uiso 1 1 calc R . . H27B H -0.2638 0.1096 0.4643 0.052 Uiso 1 1 calc R . . H27C H -0.3239 0.1819 0.3891 0.052 Uiso 1 1 calc R . . P1 P 0.5873(3) 0.37867(15) -0.27718(15) 0.0406(6) Uani 1 1 d . . . F1 F 0.5672(9) 0.3595(4) -0.1807(3) 0.084(2) Uani 1 1 d . . . F2 F 0.4015(7) 0.4224(4) -0.2772(4) 0.0734(18) Uani 1 1 d . . . F3 F 0.6080(8) 0.3990(5) -0.3760(4) 0.076(2) Uani 1 1 d . . . F4 F 0.7756(6) 0.3364(3) -0.2805(3) 0.0536(14) Uani 1 1 d . . . F5 F 0.5306(8) 0.2911(4) -0.2644(6) 0.108(3) Uani 1 1 d . . . F6 F 0.6435(7) 0.4663(3) -0.2898(3) 0.0525(14) Uani 1 1 d . . . C03 C 0.497(3) 0.0469(5) -0.006(3) 0.387(18) Uani 1 1 d DU . . H03A H 0.4814 0.0786 -0.0624 0.464 Uiso 1 1 calc R . . H03B H 0.4053 0.0655 0.0315 0.464 Uiso 1 1 calc R . . C04 C 0.661(3) 0.0598(11) 0.011(2) 0.375(18) Uani 1 1 d DU . . H04A H 0.6774 0.0272 0.0674 0.450 Uiso 1 1 calc R . . H04B H 0.7525 0.0418 -0.0267 0.450 Uiso 1 1 calc R . . C05 C 0.656(4) 0.1522(11) 0.0010(19) 0.344(18) Uani 1 1 d DU . . H05A H 0.7666 0.1645 -0.0028 0.515 Uiso 1 1 calc R . . H05B H 0.5869 0.1661 0.0478 0.515 Uiso 1 1 calc R . . H05C H 0.6121 0.1846 -0.0486 0.515 Uiso 1 1 calc R . . C01 C 0.225(3) 0.197(2) -0.193(2) 0.17(4) Uani 0.408(13) 1 d PD A 1 H01A H 0.2210 0.1864 -0.2445 0.208 Uiso 0.408(13) 1 calc PR A 1 H01B H 0.3053 0.2354 -0.2035 0.208 Uiso 0.408(13) 1 calc PR A 1 Cl11 Cl 0.029(2) 0.2413(9) -0.1551(13) 0.194(9) Uani 0.408(13) 1 d PD A 1 Cl12 Cl 0.288(2) 0.1019(12) -0.1206(14) 0.248(12) Uani 0.408(13) 1 d PD A 1 C02 C 0.152(4) 0.2282(18) -0.2052(16) 0.23(3) Uani 0.592(13) 1 d PD A 2 H02A H 0.0814 0.2805 -0.2248 0.274 Uiso 0.592(13) 1 calc PR A 2 H02B H 0.2416 0.2403 -0.1841 0.274 Uiso 0.592(13) 1 calc PR A 2 Cl13 Cl 0.2347(13) 0.1861(8) -0.2882(10) 0.203(7) Uani 0.592(13) 1 d PD A 2 Cl14 Cl 0.036(4) 0.158(2) -0.1251(11) 0.72(5) Uani 0.592(13) 1 d PD A 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 0.0191(3) 0.0170(3) 0.0203(3) -0.0035(2) -0.0013(2) -0.0055(2) Ru2 0.0199(3) 0.0167(3) 0.0187(3) -0.0031(2) -0.0009(2) -0.0047(2) Ru3 0.0231(3) 0.0170(3) 0.0222(3) -0.0041(2) -0.0018(3) -0.0050(2) Cl1 0.0241(10) 0.0374(11) 0.0309(10) -0.0105(9) -0.0012(8) -0.0070(8) O1 0.024(3) 0.016(2) 0.016(2) 0.002(2) -0.004(2) -0.004(2) O2 0.024(3) 0.026(3) 0.024(3) -0.002(2) -0.002(2) -0.009(2) O3 0.023(3) 0.019(3) 0.020(2) -0.001(2) -0.002(2) 0.001(2) O4 0.027(3) 0.028(3) 0.021(2) -0.005(2) -0.005(2) -0.006(2) O5 0.039(3) 0.021(3) 0.028(3) -0.003(2) -0.001(3) -0.008(2) O6 0.034(3) 0.021(3) 0.026(3) -0.008(2) -0.001(2) -0.013(2) O7 0.028(3) 0.019(3) 0.039(3) -0.010(2) -0.003(3) -0.008(2) O8 0.031(3) 0.023(3) 0.027(3) -0.006(2) -0.004(2) -0.006(2) O9 0.041(3) 0.029(3) 0.029(3) -0.001(2) -0.009(3) -0.020(3) O10 0.027(3) 0.015(3) 0.035(3) -0.005(2) -0.002(2) -0.006(2) O11 0.028(3) 0.025(3) 0.037(3) -0.007(2) 0.001(3) -0.007(2) N1 0.026(4) 0.021(3) 0.032(3) -0.007(3) -0.004(3) -0.008(3) N2 0.024(3) 0.031(4) 0.029(3) -0.015(3) 0.003(3) -0.004(3) N3 0.023(3) 0.022(3) 0.027(3) -0.008(3) 0.000(3) -0.005(3) N4 0.026(3) 0.012(3) 0.024(3) -0.002(2) -0.002(3) 0.001(2) N5 0.022(3) 0.018(3) 0.018(3) -0.006(2) -0.002(3) -0.004(2) N6 0.028(4) 0.021(3) 0.027(3) -0.005(3) -0.004(3) 0.001(3) C1 0.024(4) 0.025(4) 0.026(4) -0.005(3) -0.004(3) -0.003(3) C2 0.025(4) 0.030(4) 0.037(4) -0.011(4) -0.004(4) -0.007(3) C3 0.027(4) 0.026(4) 0.039(4) -0.011(3) -0.013(4) -0.010(3) C4 0.031(4) 0.024(4) 0.025(4) -0.004(3) -0.001(3) -0.004(3) C5 0.041(5) 0.057(6) 0.040(5) -0.035(5) 0.012(4) -0.022(4) C6 0.057(6) 0.070(7) 0.042(5) -0.037(5) 0.011(5) -0.022(5) C7 0.025(4) 0.034(5) 0.033(4) -0.015(4) 0.010(4) -0.008(3) C8 0.025(4) 0.017(4) 0.029(4) -0.003(3) -0.001(3) -0.001(3) C9 0.027(4) 0.023(4) 0.028(4) 0.002(3) -0.001(3) -0.006(3) C10 0.039(5) 0.032(5) 0.019(4) 0.002(3) -0.004(4) -0.011(4) C11 0.029(4) 0.036(5) 0.022(4) -0.004(3) 0.006(3) -0.001(4) C12 0.026(4) 0.029(4) 0.028(4) -0.011(3) 0.004(3) -0.003(3) C13 0.054(6) 0.031(5) 0.048(5) -0.020(4) 0.013(5) -0.013(4) C14 0.071(7) 0.035(5) 0.069(6) -0.038(5) 0.027(6) -0.023(5) C15 0.067(7) 0.027(5) 0.059(6) -0.024(5) 0.002(5) -0.007(5) C16 0.034(5) 0.020(4) 0.044(5) -0.006(4) -0.002(4) -0.009(3) C17 0.032(5) 0.021(4) 0.037(4) -0.009(3) -0.005(4) -0.003(3) C18 0.024(4) 0.025(4) 0.026(4) -0.008(3) -0.006(3) -0.008(3) C19 0.031(4) 0.019(4) 0.030(4) 0.001(3) -0.012(4) 0.006(3) C20 0.037(5) 0.034(4) 0.016(3) 0.002(3) -0.008(3) -0.012(4) C21 0.063(6) 0.063(6) 0.018(4) 0.014(4) -0.028(4) -0.034(5) C22 0.021(4) 0.026(4) 0.022(3) -0.005(3) -0.007(3) -0.003(3) C23 0.028(4) 0.024(4) 0.034(4) -0.001(3) 0.003(4) 0.003(3) C24 0.021(4) 0.015(4) 0.030(4) -0.002(3) -0.004(3) 0.000(3) C25 0.044(5) 0.028(4) 0.022(4) 0.000(3) -0.018(4) 0.000(4) C26 0.014(4) 0.023(4) 0.026(4) -0.004(3) -0.004(3) -0.003(3) C27 0.022(4) 0.036(5) 0.045(5) -0.008(4) -0.004(4) -0.005(4) P1 0.0362(13) 0.0346(13) 0.0531(14) -0.0203(11) 0.0029(12) -0.0068(10) F1 0.110(6) 0.061(4) 0.043(3) 0.006(3) 0.015(3) 0.018(4) F2 0.037(3) 0.070(4) 0.105(5) -0.028(4) 0.002(3) 0.002(3) F3 0.060(4) 0.121(6) 0.067(4) -0.060(4) -0.019(3) 0.008(4) F4 0.034(3) 0.057(4) 0.069(4) -0.022(3) -0.006(3) 0.002(3) F5 0.066(5) 0.059(4) 0.213(9) -0.072(5) 0.017(5) -0.026(4) F6 0.072(4) 0.032(3) 0.060(3) -0.011(3) -0.018(3) -0.014(3) C03 0.62(5) 0.27(3) 0.34(3) -0.13(3) -0.30(3) 0.10(4) C04 0.61(5) 0.27(3) 0.33(2) -0.14(3) -0.31(3) 0.10(3) C05 0.59(5) 0.23(3) 0.31(3) -0.15(3) -0.32(3) 0.11(3) C01 0.04(2) 0.12(4) 0.37(11) -0.08(6) -0.07(4) 0.02(2) Cl11 0.164(16) 0.119(12) 0.23(2) -0.010(12) 0.025(14) 0.008(10) Cl12 0.27(3) 0.25(3) 0.20(2) -0.040(18) -0.033(18) -0.03(2) C02 0.06(2) 0.32(7) 0.25(6) -0.09(5) 0.00(3) 0.10(3) Cl13 0.135(9) 0.235(13) 0.330(18) -0.209(13) -0.059(10) 0.006(8) Cl14 1.38(14) 0.30(4) 0.53(6) 0.04(4) -0.66(8) 0.01(6) _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 1.924(5) . ? Ru1 N3 1.950(6) . ? Ru1 O2 2.042(5) . ? Ru1 N1 2.047(6) . ? Ru1 O4 2.053(5) . ? Ru1 O6 2.086(5) . ? Ru2 O1 1.933(4) . ? Ru2 N4 2.038(6) . ? Ru2 O10 2.045(5) . ? Ru2 O3 2.061(5) . ? Ru2 O8 2.066(5) . ? Ru2 N5 2.086(6) . ? Ru3 O1 1.876(5) . ? Ru3 O7 2.044(5) . ? Ru3 O9 2.045(5) . ? Ru3 O11 2.065(5) . ? Ru3 O5 2.072(5) . ? Ru3 N6 2.134(6) . ? Cl1 C1 1.712(8) . ? O2 C18 1.266(8) . ? O3 C18 1.250(9) . ? O4 C24 1.273(8) . ? O5 C24 1.251(8) . ? O6 C26 1.259(8) . ? O7 C26 1.265(9) . ? O8 C20 1.259(8) . ? O9 C20 1.277(8) . ? O10 C22 1.253(8) . ? O11 C22 1.262(8) . ? N1 C7 1.308(9) . ? N1 N2 1.391(8) . ? N2 C5 1.361(9) . ? N2 C4 1.386(10) . ? N3 C4 1.337(9) . ? N3 N4 1.391(8) . ? N4 C1 1.335(9) . ? N5 C12 1.347(9) . ? N5 C8 1.352(9) . ? N6 C13 1.326(10) . ? N6 C17 1.348(10) . ? C1 C2 1.398(10) . ? C2 C3 1.363(11) . ? C2 H2A 0.9300 . ? C3 C4 1.387(10) . ? C3 H3A 0.9300 . ? C5 C6 1.367(12) . ? C5 H5A 0.9300 . ? C6 C7 1.407(11) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.367(10) . ? C8 H8A 0.9300 . ? C9 C10 1.360(11) . ? C9 H9A 0.9300 . ? C10 C11 1.398(11) . ? C10 H10A 0.9300 . ? C11 C12 1.364(10) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.376(11) . ? C13 H13A 0.9300 . ? C14 C15 1.353(13) . ? C14 H14A 0.9300 . ? C15 C16 1.381(12) . ? C15 H15A 0.9300 . ? C16 C17 1.369(10) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.512(10) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.478(9) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.507(10) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.509(9) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.500(10) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? P1 F1 1.570(6) . ? P1 F5 1.574(6) . ? P1 F6 1.574(5) . ? P1 F2 1.583(6) . ? P1 F4 1.592(5) . ? P1 F3 1.607(6) . ? C03 C04 1.523(10) . ? C03 C03 1.527(10) 2_655 ? C03 H03A 0.9700 . ? C03 H03B 0.9700 . ? C04 C05 1.511(7) . ? C04 H04A 0.9700 . ? C04 H04B 0.9700 . ? C05 H05A 0.9600 . ? C05 H05B 0.9600 . ? C05 H05C 0.9600 . ? C01 Cl12 1.756(10) . ? C01 Cl11 1.756(10) . ? C01 H01A 0.9700 . ? C01 H01B 0.9700 . ? C02 Cl13 1.762(10) . ? C02 Cl14 1.757(10) . ? C02 H02A 0.9700 . ? C02 H02B 0.9700 . ? 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 N3 89.3(2) . . ? O1 Ru1 O2 97.02(19) . . ? N3 Ru1 O2 92.3(2) . . ? O1 Ru1 N1 168.6(2) . . ? N3 Ru1 N1 79.9(2) . . ? O2 Ru1 N1 87.1(2) . . ? O1 Ru1 O4 91.18(19) . . ? N3 Ru1 O4 87.9(2) . . ? O2 Ru1 O4 171.8(2) . . ? N1 Ru1 O4 84.9(2) . . ? O1 Ru1 O6 95.77(19) . . ? N3 Ru1 O6 174.4(2) . . ? O2 Ru1 O6 89.45(19) . . ? N1 Ru1 O6 94.9(2) . . ? O4 Ru1 O6 89.58(19) . . ? O1 Ru2 N4 88.0(2) . . ? O1 Ru2 O10 95.6(2) . . ? N4 Ru2 O10 92.9(2) . . ? O1 Ru2 O3 93.16(19) . . ? N4 Ru2 O3 92.1(2) . . ? O10 Ru2 O3 170.11(19) . . ? O1 Ru2 O8 92.50(19) . . ? N4 Ru2 O8 177.4(2) . . ? O10 Ru2 O8 89.6(2) . . ? O3 Ru2 O8 85.35(19) . . ? O1 Ru2 N5 176.3(2) . . ? N4 Ru2 N5 94.6(2) . . ? O10 Ru2 N5 86.9(2) . . ? O3 Ru2 N5 84.2(2) . . ? O8 Ru2 N5 84.8(2) . . ? O1 Ru3 O7 94.8(2) . . ? O1 Ru3 O9 93.14(19) . . ? O7 Ru3 O9 89.4(2) . . ? O1 Ru3 O11 94.5(2) . . ? O7 Ru3 O11 170.47(19) . . ? O9 Ru3 O11 91.9(2) . . ? O1 Ru3 O5 95.12(19) . . ? O7 Ru3 O5 87.9(2) . . ? O9 Ru3 O5 171.50(19) . . ? O11 Ru3 O5 89.5(2) . . ? O1 Ru3 N6 178.6(2) . . ? O7 Ru3 N6 85.9(2) . . ? O9 Ru3 N6 85.7(2) . . ? O11 Ru3 N6 84.8(2) . . ? O5 Ru3 N6 86.1(2) . . ? Ru3 O1 Ru1 123.0(2) . . ? Ru3 O1 Ru2 123.7(3) . . ? Ru1 O1 Ru2 113.0(2) . . ? C18 O2 Ru1 125.9(5) . . ? C18 O3 Ru2 134.3(4) . . ? C24 O4 Ru1 130.9(4) . . ? C24 O5 Ru3 131.2(5) . . ? C26 O6 Ru1 131.8(5) . . ? C26 O7 Ru3 130.4(4) . . ? C20 O8 Ru2 132.3(5) . . ? C20 O9 Ru3 132.0(5) . . ? C22 O10 Ru2 131.8(5) . . ? C22 O11 Ru3 132.8(5) . . ? C7 N1 N2 105.3(6) . . ? C7 N1 Ru1 145.1(5) . . ? N2 N1 Ru1 109.6(4) . . ? C5 N2 N1 110.3(6) . . ? C5 N2 C4 131.3(7) . . ? N1 N2 C4 118.2(6) . . ? C4 N3 N4 120.9(6) . . ? C4 N3 Ru1 117.6(5) . . ? N4 N3 Ru1 121.2(4) . . ? C1 N4 N3 116.0(6) . . ? C1 N4 Ru2 131.8(5) . . ? N3 N4 Ru2 112.1(4) . . ? C12 N5 C8 116.5(6) . . ? C12 N5 Ru2 121.8(5) . . ? C8 N5 Ru2 121.7(5) . . ? C13 N6 C17 118.4(7) . . ? C13 N6 Ru3 119.3(5) . . ? C17 N6 Ru3 122.3(5) . . ? N4 C1 C2 123.6(7) . . ? N4 C1 Cl1 117.4(5) . . ? C2 C1 Cl1 118.9(6) . . ? C3 C2 C1 119.5(7) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 116.6(7) . . ? C2 C3 H3A 121.7 . . ? C4 C3 H3A 121.7 . . ? N3 C4 C3 122.9(7) . . ? N3 C4 N2 113.1(6) . . ? C3 C4 N2 124.0(7) . . ? C6 C5 N2 107.3(7) . . ? C6 C5 H5A 126.4 . . ? N2 C5 H5A 126.4 . . ? C5 C6 C7 105.4(8) . . ? C5 C6 H6A 127.3 . . ? C7 C6 H6A 127.3 . . ? N1 C7 C6 111.8(7) . . ? N1 C7 H7A 124.1 . . ? C6 C7 H7A 124.1 . . ? N5 C8 C9 123.0(7) . . ? N5 C8 H8A 118.5 . . ? C9 C8 H8A 118.5 . . ? C8 C9 C10 119.8(7) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C9 C10 C11 118.5(7) . . ? C9 C10 H10A 120.7 . . ? C11 C10 H10A 120.7 . . ? C12 C11 C10 118.5(7) . . ? C12 C11 H11A 120.7 . . ? C10 C11 H11A 120.7 . . ? N5 C12 C11 123.7(7) . . ? N5 C12 H12A 118.2 . . ? C11 C12 H12A 118.2 . . ? N6 C13 C14 121.7(8) . . ? N6 C13 H13A 119.2 . . ? C14 C13 H13A 119.2 . . ? C15 C14 C13 120.5(9) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 118.1(8) . . ? C14 C15 H15A 120.9 . . ? C16 C15 H15A 120.9 . . ? C17 C16 C15 119.3(8) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? N6 C17 C16 122.0(8) . . ? N6 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? O3 C18 O2 126.8(7) . . ? O3 C18 C19 116.7(6) . . ? O2 C18 C19 116.5(7) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O8 C20 O9 126.5(6) . . ? O8 C20 C21 117.5(7) . . ? O9 C20 C21 115.9(7) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O11 C22 O10 126.8(7) . . ? O11 C22 C23 116.8(7) . . ? O10 C22 C23 116.5(6) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O5 C24 O4 125.8(6) . . ? O5 C24 C25 118.1(6) . . ? O4 C24 C25 116.0(6) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O7 C26 O6 126.4(7) . . ? O7 C26 C27 116.3(6) . . ? O6 C26 C27 117.3(7) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? F1 P1 F5 89.4(5) . . ? F1 P1 F6 90.5(3) . . ? F5 P1 F6 179.8(5) . . ? F1 P1 F2 90.9(4) . . ? F5 P1 F2 90.9(4) . . ? F6 P1 F2 89.0(3) . . ? F1 P1 F4 90.9(3) . . ? F5 P1 F4 89.9(4) . . ? F6 P1 F4 90.3(3) . . ? F2 P1 F4 178.0(4) . . ? F1 P1 F3 179.6(4) . . ? F5 P1 F3 91.1(5) . . ? F6 P1 F3 89.0(3) . . ? F2 P1 F3 89.0(4) . . ? F4 P1 F3 89.2(3) . . ? C04 C03 C03 107.1(10) . 2_655 ? C04 C03 H03A 110.3 . . ? C03 C03 H03A 110.3 2_655 . ? C04 C03 H03B 110.3 . . ? C03 C03 H03B 110.3 2_655 . ? H03A C03 H03B 108.5 . . ? C05 C04 C03 107.9(9) . . ? C05 C04 H04A 110.1 . . ? C03 C04 H04A 110.1 . . ? C05 C04 H04B 110.1 . . ? C03 C04 H04B 110.1 . . ? H04A C04 H04B 108.4 . . ? C04 C05 H05A 109.5 . . ? C04 C05 H05B 109.5 . . ? H05A C05 H05B 109.5 . . ? C04 C05 H05C 109.5 . . ? H05A C05 H05C 109.5 . . ? H05B C05 H05C 109.5 . . ? Cl12 C01 Cl11 110.4(9) . . ? Cl12 C01 H01A 109.7 . . ? Cl11 C01 H01A 109.7 . . ? Cl12 C01 H01B 109.5 . . ? Cl11 C01 H01B 109.5 . . ? H01A C01 H01B 108.1 . . ? Cl13 C02 Cl14 111.1(9) . . ? Cl13 C02 H02A 109.4 . . ? Cl14 C02 H02A 109.4 . . ? Cl13 C02 H02B 109.4 . . ? Cl14 C02 H02B 109.4 . . ? H02A C02 H02B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.084 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.147 # Attachment 'compound 4.cif' data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 730667' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H34 Cl N6 O11 Ru3, F6 P, C H2 Cl2' _chemical_formula_sum 'C30 H36 Cl3 F6 N6 O11 P Ru3' _chemical_formula_weight 1211.18 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 8.010(4) _cell_length_b 13.998(6) _cell_length_c 20.935(11) _cell_angle_alpha 106.470(11) _cell_angle_beta 97.90(2) _cell_angle_gamma 96.716(17) _cell_volume 2199.5(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 3.0066 _cell_measurement_theta_max 27.4217 _exptl_crystal_description Chip _exptl_crystal_colour Brown _exptl_crystal_size_max 0.5000 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 1.320 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5124 _exptl_absorpt_correction_T_max 0.9120 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU SATURN70' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13422 _diffrn_reflns_av_R_equivalents 0.1486 _diffrn_reflns_av_sigmaI/netI 0.2651 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7542 _reflns_number_gt 3338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0866P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0089(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7542 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1660 _refine_ls_R_factor_gt 0.1186 _refine_ls_wR_factor_ref 0.2654 _refine_ls_wR_factor_gt 0.2389 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.25510(17) 0.63896(9) 0.83571(6) 0.0207(4) Uani 1 1 d . . . Ru2 Ru 0.16971(17) 0.51248(9) 0.67629(6) 0.0210(4) Uani 1 1 d . . . Ru3 Ru 0.06878(18) 0.74634(9) 0.72683(6) 0.0229(4) Uani 1 1 d . . . Cl1 Cl -0.1014(6) 0.2845(3) 0.6493(2) 0.0387(11) Uani 1 1 d . . . N1 N 0.3018(19) 0.6092(10) 0.9287(6) 0.032(4) Uani 1 1 d . . . N2 N 0.227(2) 0.5139(10) 0.9237(7) 0.036(4) Uani 1 1 d . . . N3 N 0.1563(16) 0.4920(9) 0.8108(6) 0.022(3) Uani 1 1 d . . . N4 N 0.0918(16) 0.4393(9) 0.7423(6) 0.022(3) Uani 1 1 d . . . N5 N 0.2017(17) 0.3838(9) 0.6000(6) 0.025(3) Uani 1 1 d . . . N6 N -0.060(2) 0.8623(10) 0.7048(6) 0.031(4) Uani 1 1 d . . . O1 O 0.1650(13) 0.6384(7) 0.7453(5) 0.021(2) Uani 1 1 d . . . O2 O 0.4898(14) 0.6062(8) 0.8203(5) 0.028(3) Uani 1 1 d . . . O3 O 0.4210(15) 0.5075(8) 0.7124(5) 0.032(3) Uani 1 1 d . . . O4 O 0.3689(16) 0.7917(8) 0.8664(6) 0.035(3) Uani 1 1 d . . . O5 O 0.2752(15) 0.8512(7) 0.7807(6) 0.031(3) Uani 1 1 d . . . O6 O 0.0413(15) 0.6804(8) 0.8714(6) 0.036(3) Uani 1 1 d . . . O7 O -0.0463(16) 0.7801(8) 0.8104(6) 0.037(3) Uani 1 1 d . . . O8 O -0.0739(13) 0.5004(8) 0.6247(5) 0.025(2) Uani 1 1 d . . . O9 O -0.1522(14) 0.6517(7) 0.6690(5) 0.026(3) Uani 1 1 d . . . O10 O 0.2566(14) 0.5882(7) 0.6114(5) 0.027(3) Uani 1 1 d . . . O11 O 0.1805(15) 0.7415(8) 0.6424(5) 0.029(3) Uani 1 1 d . . . C1 C -0.003(2) 0.3493(12) 0.7336(9) 0.040(5) Uani 1 1 d . . . C2 C -0.030(2) 0.3090(13) 0.7814(8) 0.032(4) Uani 1 1 d . . . H2A H -0.1007 0.2451 0.7707 0.038 Uiso 1 1 calc R . . C3 C 0.042(2) 0.3589(13) 0.8451(10) 0.041(5) Uani 1 1 d . . . H3A H 0.0259 0.3300 0.8802 0.049 Uiso 1 1 calc R . . C4 C 0.138(2) 0.4489(12) 0.8596(8) 0.025(4) Uani 1 1 d . . . C5 C 0.243(3) 0.5028(13) 0.9903(9) 0.048(6) Uani 1 1 d . . . C6 C 0.338(3) 0.5921(15) 1.0309(10) 0.056(6) Uani 1 1 d . . . H6A H 0.3802 0.6062 1.0779 0.067 Uiso 1 1 calc R . . C7 C 0.364(3) 0.6601(14) 0.9941(8) 0.043(5) Uani 1 1 d . . . C8 C 0.189(4) 0.4079(14) 1.0015(9) 0.075(8) Uani 1 1 d . . . H8A H 0.2175 0.4152 1.0499 0.113 Uiso 1 1 calc R . . H8B H 0.2469 0.3560 0.9759 0.113 Uiso 1 1 calc R . . H8C H 0.0650 0.3881 0.9864 0.113 Uiso 1 1 calc R . . C9 C 0.447(3) 0.7682(13) 1.0173(9) 0.048(5) Uani 1 1 d . . . H9A H 0.4363 0.7954 0.9789 0.072 Uiso 1 1 calc R . . H9B H 0.5678 0.7736 1.0358 0.072 Uiso 1 1 calc R . . H9C H 0.3901 0.8067 1.0524 0.072 Uiso 1 1 calc R . . C10 C 0.129(2) 0.3683(11) 0.5351(8) 0.031(4) Uani 1 1 d . . . H10A H 0.0582 0.4139 0.5253 0.038 Uiso 1 1 calc R . . C11 C 0.154(2) 0.2884(12) 0.4814(9) 0.037(5) Uani 1 1 d . . . H11A H 0.1007 0.2801 0.4363 0.044 Uiso 1 1 calc R . . C12 C 0.259(2) 0.2213(13) 0.4951(9) 0.038(5) Uani 1 1 d . . . H12A H 0.2809 0.1674 0.4596 0.046 Uiso 1 1 calc R . . C13 C 0.331(3) 0.2356(13) 0.5631(9) 0.044(5) Uani 1 1 d . . . H13A H 0.3986 0.1898 0.5751 0.053 Uiso 1 1 calc R . . C14 C 0.300(2) 0.3169(12) 0.6112(8) 0.036(4) Uani 1 1 d . . . H14A H 0.3531 0.3272 0.6566 0.043 Uiso 1 1 calc R . . C15 C -0.229(2) 0.8606(11) 0.7067(7) 0.021(3) Uani 1 1 d . . . H15A H -0.2901 0.8038 0.7146 0.025 Uiso 1 1 calc R . . C16 C -0.312(3) 0.9312(13) 0.6984(9) 0.047(5) Uani 1 1 d . . . H16A H -0.4300 0.9263 0.7016 0.057 Uiso 1 1 calc R . . C17 C -0.226(3) 1.0187(14) 0.6840(9) 0.048(6) Uani 1 1 d . . . H17A H -0.2855 1.0701 0.6760 0.057 Uiso 1 1 calc R . . C18 C -0.054(3) 1.0236(13) 0.6827(10) 0.045(5) Uani 1 1 d . . . H18A H 0.0096 1.0790 0.6740 0.054 Uiso 1 1 calc R . . C19 C 0.027(2) 0.9432(12) 0.6947(8) 0.035(4) Uani 1 1 d . . . H19A H 0.1470 0.9469 0.6957 0.041 Uiso 1 1 calc R . . C20 C 0.524(2) 0.5443(11) 0.7692(8) 0.027(4) Uani 1 1 d . . . C21 C 0.697(2) 0.5127(14) 0.7713(9) 0.034(4) Uani 1 1 d . . . H21A H 0.7661 0.5451 0.8165 0.051 Uiso 1 1 calc R . . H21B H 0.7540 0.5333 0.7376 0.051 Uiso 1 1 calc R . . H21C H 0.6843 0.4392 0.7611 0.051 Uiso 1 1 calc R . . C22 C 0.375(2) 0.8566(10) 0.8336(8) 0.019(3) Uani 1 1 d . . . C23 C 0.517(2) 0.9460(12) 0.8651(9) 0.035(4) Uani 1 1 d . . . H23A H 0.5824 0.9380 0.9058 0.052 Uiso 1 1 calc R . . H23B H 0.4675 1.0082 0.8773 0.052 Uiso 1 1 calc R . . H23C H 0.5925 0.9498 0.8326 0.052 Uiso 1 1 calc R . . C24 C -0.046(2) 0.7448(12) 0.8602(8) 0.027(4) Uani 1 1 d . . . C25 C -0.172(2) 0.7821(12) 0.9085(8) 0.031(4) Uani 1 1 d . . . H25A H -0.1608 0.7515 0.9452 0.046 Uiso 1 1 calc R . . H25B H -0.2896 0.7625 0.8831 0.046 Uiso 1 1 calc R . . H25C H -0.1458 0.8558 0.9275 0.046 Uiso 1 1 calc R . . C26 C -0.181(2) 0.5605(12) 0.6303(8) 0.027(4) Uani 1 1 d . . . C27 C -0.359(2) 0.5231(11) 0.5876(8) 0.028(4) Uani 1 1 d . . . H27A H -0.3660 0.4532 0.5595 0.042 Uiso 1 1 calc R . . H27B H -0.3813 0.5657 0.5585 0.042 Uiso 1 1 calc R . . H27C H -0.4437 0.5264 0.6174 0.042 Uiso 1 1 calc R . . C28 C 0.251(2) 0.6763(11) 0.6082(8) 0.022(4) Uani 1 1 d . . . C29 C 0.334(3) 0.7065(14) 0.5547(9) 0.045(5) Uani 1 1 d . . . H29A H 0.3219 0.7763 0.5576 0.067 Uiso 1 1 calc R . . H29B H 0.2788 0.6617 0.5098 0.067 Uiso 1 1 calc R . . H29C H 0.4558 0.7011 0.5621 0.067 Uiso 1 1 calc R . . P1 P 0.4348(7) 0.2119(4) 0.7713(2) 0.0363(12) Uani 1 1 d . . . F1 F 0.4249(18) 0.0917(9) 0.7456(7) 0.077(4) Uani 1 1 d . . . F2 F 0.6037(14) 0.2196(9) 0.8232(6) 0.059(3) Uani 1 1 d . . . F3 F 0.3219(16) 0.2009(10) 0.8282(6) 0.064(4) Uani 1 1 d . . . F4 F 0.2618(14) 0.2042(8) 0.7199(5) 0.048(3) Uani 1 1 d . . . F5 F 0.5461(15) 0.2236(9) 0.7153(6) 0.054(3) Uani 1 1 d . . . F6 F 0.4405(16) 0.3313(7) 0.7977(6) 0.060(3) Uani 1 1 d . . . C01 C 0.078(3) 1.0330(16) 0.8726(9) 0.051(6) Uani 1 1 d . . . H01A H 0.1674 1.0616 0.8520 0.062 Uiso 1 1 calc R . . H01B H 0.0171 0.9688 0.8393 0.062 Uiso 1 1 calc R . . Cl01 Cl -0.0673(8) 1.1173(4) 0.8902(3) 0.0647(17) Uani 1 1 d . . . Cl02 Cl 0.1753(8) 1.0077(4) 0.9456(3) 0.0578(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0279(9) 0.0139(7) 0.0150(7) -0.0014(5) 0.0003(6) 0.0012(5) Ru2 0.0259(8) 0.0158(7) 0.0161(7) -0.0025(5) 0.0011(6) 0.0038(5) Ru3 0.0333(9) 0.0161(7) 0.0161(7) -0.0006(5) 0.0039(6) 0.0060(6) Cl1 0.048(3) 0.026(2) 0.029(2) -0.0037(18) 0.003(2) -0.006(2) N1 0.055(11) 0.024(7) 0.013(7) 0.003(6) -0.003(7) 0.014(7) N2 0.061(11) 0.029(8) 0.012(7) 0.005(6) -0.006(7) 0.002(8) N3 0.024(8) 0.021(7) 0.020(7) 0.003(5) 0.002(6) 0.006(6) N4 0.023(8) 0.017(7) 0.020(7) -0.004(5) 0.003(6) 0.004(6) N5 0.043(9) 0.014(7) 0.014(7) -0.003(5) 0.003(6) 0.017(6) N6 0.054(11) 0.024(7) 0.012(7) -0.001(5) -0.004(7) 0.016(7) O1 0.035(7) 0.009(5) 0.019(6) 0.003(4) 0.002(5) 0.007(5) O2 0.033(7) 0.024(6) 0.018(6) 0.001(5) -0.006(5) 0.003(5) O3 0.047(8) 0.017(6) 0.021(6) -0.005(5) 0.006(6) -0.003(5) O4 0.055(9) 0.015(6) 0.029(7) 0.005(5) -0.007(6) 0.003(6) O5 0.042(8) 0.017(6) 0.027(7) 0.000(5) 0.003(6) 0.003(5) O6 0.043(8) 0.029(7) 0.035(7) 0.007(6) 0.005(6) 0.015(6) O7 0.052(9) 0.025(6) 0.033(7) 0.006(5) 0.016(7) 0.006(6) O8 0.023(7) 0.024(6) 0.017(6) -0.004(4) -0.003(5) -0.006(5) O9 0.042(8) 0.010(5) 0.025(6) 0.008(4) 0.005(6) -0.006(5) O10 0.041(7) 0.014(5) 0.026(6) 0.006(4) 0.012(6) 0.002(5) O11 0.041(8) 0.024(6) 0.023(6) 0.005(5) 0.007(6) 0.009(5) C1 0.044(12) 0.021(9) 0.031(11) -0.018(8) -0.013(9) -0.002(9) C2 0.046(12) 0.021(9) 0.030(10) 0.008(7) 0.017(9) -0.001(8) C3 0.042(13) 0.028(10) 0.044(12) -0.002(8) 0.006(10) 0.005(9) C4 0.033(11) 0.022(8) 0.023(9) 0.008(7) 0.013(8) -0.004(7) C5 0.082(17) 0.033(11) 0.015(9) 0.000(8) -0.019(10) 0.000(10) C6 0.080(17) 0.042(12) 0.030(11) 0.006(9) 0.001(11) -0.027(11) C7 0.068(15) 0.041(11) 0.011(9) 0.005(8) -0.008(9) 0.006(10) C8 0.16(3) 0.035(11) 0.015(10) 0.005(8) -0.012(13) -0.023(14) C9 0.083(17) 0.024(10) 0.027(10) 0.000(8) 0.006(11) -0.007(10) C10 0.058(13) 0.005(7) 0.029(9) -0.001(6) 0.012(9) 0.002(8) C11 0.058(14) 0.028(9) 0.023(9) 0.005(7) 0.010(9) 0.009(9) C12 0.055(13) 0.031(10) 0.025(10) -0.001(8) 0.005(9) 0.016(9) C13 0.067(15) 0.023(9) 0.043(12) 0.005(8) 0.012(11) 0.024(10) C14 0.058(13) 0.025(9) 0.017(9) -0.006(7) 0.004(9) 0.008(9) C15 0.029(10) 0.016(8) 0.016(8) 0.003(6) 0.012(7) -0.005(7) C16 0.073(16) 0.032(11) 0.029(10) -0.006(8) 0.008(11) 0.016(11) C17 0.080(17) 0.028(10) 0.034(11) 0.006(8) 0.002(11) 0.027(11) C18 0.055(15) 0.022(10) 0.056(13) 0.015(9) -0.003(11) 0.002(9) C19 0.041(12) 0.021(9) 0.029(10) -0.001(7) -0.015(9) 0.002(8) C20 0.034(11) 0.011(8) 0.031(10) 0.005(7) 0.003(8) -0.011(7) C21 0.014(9) 0.046(11) 0.034(10) 0.003(8) -0.005(8) 0.003(8) C22 0.029(10) 0.003(7) 0.023(8) -0.004(6) 0.013(8) -0.004(6) C23 0.047(12) 0.021(9) 0.035(10) 0.015(8) 0.002(9) -0.008(8) C24 0.026(10) 0.022(8) 0.022(9) 0.002(7) -0.009(8) -0.014(7) C25 0.036(11) 0.024(9) 0.026(9) 0.000(7) 0.002(8) 0.003(8) C26 0.031(10) 0.027(9) 0.016(8) -0.008(7) 0.006(8) 0.010(8) C27 0.030(10) 0.017(8) 0.028(9) -0.004(7) -0.001(8) 0.002(7) C28 0.019(9) 0.016(8) 0.027(9) 0.001(7) 0.004(7) 0.002(7) C29 0.068(15) 0.049(12) 0.031(10) 0.021(9) 0.030(11) 0.015(11) P1 0.040(3) 0.038(3) 0.034(3) 0.014(2) 0.006(2) 0.008(2) F1 0.092(11) 0.040(7) 0.107(12) 0.031(7) 0.017(9) 0.023(7) F2 0.035(7) 0.085(9) 0.060(8) 0.030(7) -0.003(6) 0.008(6) F3 0.066(9) 0.090(10) 0.052(8) 0.040(7) 0.026(7) 0.010(7) F4 0.047(7) 0.049(7) 0.045(7) 0.019(5) -0.007(6) 0.000(6) F5 0.058(8) 0.062(8) 0.054(8) 0.029(6) 0.025(7) 0.012(6) F6 0.082(9) 0.022(6) 0.069(9) 0.004(5) 0.019(7) 0.005(6) C01 0.065(16) 0.061(14) 0.020(10) 0.005(9) 0.009(10) -0.005(11) Cl01 0.061(4) 0.044(3) 0.088(5) 0.016(3) 0.019(4) 0.003(3) Cl02 0.074(4) 0.054(3) 0.033(3) -0.006(2) 0.010(3) 0.010(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 1.928(10) . ? Ru1 N3 2.007(13) . ? Ru1 O2 2.033(11) . ? Ru1 O6 2.041(11) . ? Ru1 N1 2.098(12) . ? Ru1 O4 2.102(11) . ? Ru2 O1 1.945(9) . ? Ru2 O8 2.059(11) . ? Ru2 N4 2.058(13) . ? Ru2 O3 2.066(12) . ? Ru2 O10 2.087(10) . ? Ru2 N5 2.110(11) . ? Ru3 O1 1.884(9) . ? Ru3 O5 2.035(12) . ? Ru3 O7 2.053(11) . ? Ru3 O11 2.076(10) . ? Ru3 O9 2.076(11) . ? Ru3 N6 2.144(12) . ? Cl1 C1 1.761(17) . ? N1 C7 1.34(2) . ? N1 N2 1.366(19) . ? N2 C4 1.42(2) . ? N2 C5 1.43(2) . ? N3 C4 1.341(18) . ? N3 N4 1.406(17) . ? N4 C1 1.34(2) . ? N5 C14 1.341(19) . ? N5 C10 1.35(2) . ? N6 C19 1.34(2) . ? N6 C15 1.36(2) . ? O2 C20 1.255(18) . ? O3 C20 1.282(19) . ? O4 C22 1.285(17) . ? O5 C22 1.251(18) . ? O6 C24 1.258(18) . ? O7 C24 1.274(18) . ? O8 C26 1.265(17) . ? O9 C26 1.278(18) . ? O10 C28 1.259(16) . ? O11 C28 1.238(16) . ? C1 C2 1.31(2) . ? C2 C3 1.33(2) . ? C2 H2A 0.9500 . ? C3 C4 1.33(2) . ? C3 H3A 0.9500 . ? C5 C6 1.36(3) . ? C5 C8 1.44(2) . ? C6 C7 1.40(2) . ? C6 H6A 0.9500 . ? C7 C9 1.49(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.40(2) . ? C10 H10A 0.9500 . ? C11 C12 1.39(2) . ? C11 H11A 0.9500 . ? C12 C13 1.41(2) . ? C12 H12A 0.9500 . ? C13 C14 1.36(2) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.29(2) . ? C15 H15A 0.9500 . ? C16 C17 1.46(3) . ? C16 H16A 0.9500 . ? C17 C18 1.38(3) . ? C17 H17A 0.9500 . ? C18 C19 1.43(2) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.51(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.51(2) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.55(2) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.52(2) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.51(2) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 F2 1.588(12) . ? P1 F6 1.597(11) . ? P1 F5 1.599(11) . ? P1 F1 1.604(12) . ? P1 F4 1.606(11) . ? P1 F3 1.621(11) . ? C01 Cl01 1.75(2) . ? C01 Cl02 1.764(19) . ? C01 H01A 0.9900 . ? C01 H01B 0.9900 . ? 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 N3 89.5(5) . . ? O1 Ru1 O2 98.3(4) . . ? N3 Ru1 O2 91.7(5) . . ? O1 Ru1 O6 92.8(4) . . ? N3 Ru1 O6 91.5(5) . . ? O2 Ru1 O6 168.4(5) . . ? O1 Ru1 N1 165.5(5) . . ? N3 Ru1 N1 77.5(5) . . ? O2 Ru1 N1 88.6(5) . . ? O6 Ru1 N1 81.2(5) . . ? O1 Ru1 O4 93.7(4) . . ? N3 Ru1 O4 176.6(5) . . ? O2 Ru1 O4 86.6(5) . . ? O6 Ru1 O4 89.7(5) . . ? N1 Ru1 O4 99.5(5) . . ? O1 Ru2 O8 95.6(4) . . ? O1 Ru2 N4 87.1(4) . . ? O8 Ru2 N4 94.3(5) . . ? O1 Ru2 O3 93.8(4) . . ? O8 Ru2 O3 169.9(4) . . ? N4 Ru2 O3 89.7(5) . . ? O1 Ru2 O10 92.3(4) . . ? O8 Ru2 O10 87.6(4) . . ? N4 Ru2 O10 178.1(5) . . ? O3 Ru2 O10 88.6(4) . . ? O1 Ru2 N5 173.5(5) . . ? O8 Ru2 N5 88.6(5) . . ? N4 Ru2 N5 97.5(5) . . ? O3 Ru2 N5 81.7(5) . . ? O10 Ru2 N5 83.0(4) . . ? O1 Ru3 O5 93.5(4) . . ? O1 Ru3 O7 95.8(4) . . ? O5 Ru3 O7 88.9(5) . . ? O1 Ru3 O11 95.0(4) . . ? O5 Ru3 O11 86.4(5) . . ? O7 Ru3 O11 168.5(4) . . ? O1 Ru3 O9 92.6(4) . . ? O5 Ru3 O9 173.9(4) . . ? O7 Ru3 O9 90.9(5) . . ? O11 Ru3 O9 92.6(4) . . ? O1 Ru3 N6 175.5(6) . . ? O5 Ru3 N6 90.6(5) . . ? O7 Ru3 N6 82.3(5) . . ? O11 Ru3 N6 87.2(5) . . ? O9 Ru3 N6 83.4(5) . . ? C7 N1 N2 109.3(13) . . ? C7 N1 Ru1 138.5(12) . . ? N2 N1 Ru1 111.4(9) . . ? N1 N2 C4 119.3(12) . . ? N1 N2 C5 108.8(13) . . ? C4 N2 C5 131.7(15) . . ? C4 N3 N4 121.4(13) . . ? C4 N3 Ru1 119.9(11) . . ? N4 N3 Ru1 118.4(9) . . ? C1 N4 N3 112.6(13) . . ? C1 N4 Ru2 133.4(12) . . ? N3 N4 Ru2 113.9(9) . . ? C14 N5 C10 116.1(13) . . ? C14 N5 Ru2 123.7(10) . . ? C10 N5 Ru2 120.1(9) . . ? C19 N6 C15 118.2(14) . . ? C19 N6 Ru3 120.7(12) . . ? C15 N6 Ru3 120.9(11) . . ? Ru3 O1 Ru1 122.9(5) . . ? Ru3 O1 Ru2 123.5(5) . . ? Ru1 O1 Ru2 113.4(4) . . ? C20 O2 Ru1 126.8(11) . . ? C20 O3 Ru2 135.9(10) . . ? C22 O4 Ru1 130.9(10) . . ? C22 O5 Ru3 130.9(10) . . ? C24 O6 Ru1 129.8(11) . . ? C24 O7 Ru3 132.8(11) . . ? C26 O8 Ru2 132.1(10) . . ? C26 O9 Ru3 132.8(11) . . ? C28 O10 Ru2 132.3(10) . . ? C28 O11 Ru3 131.2(10) . . ? C2 C1 N4 126.2(17) . . ? C2 C1 Cl1 119.2(14) . . ? N4 C1 Cl1 114.6(14) . . ? C1 C2 C3 119.0(18) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C4 C3 C2 120.0(19) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 N3 120.4(17) . . ? C3 C4 N2 128.9(15) . . ? N3 C4 N2 110.7(14) . . ? C6 C5 N2 103.9(17) . . ? C6 C5 C8 133.1(17) . . ? N2 C5 C8 122.2(15) . . ? C5 C6 C7 110.8(19) . . ? C5 C6 H6A 124.6 . . ? C7 C6 H6A 124.6 . . ? N1 C7 C6 106.8(17) . . ? N1 C7 C9 122.8(15) . . ? C6 C7 C9 130.3(17) . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 C11 123.2(16) . . ? N5 C10 H10A 118.4 . . ? C11 C10 H10A 118.4 . . ? C12 C11 C10 118.9(17) . . ? C12 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? C11 C12 C13 118.1(15) . . ? C11 C12 H12A 120.9 . . ? C13 C12 H12A 120.9 . . ? C14 C13 C12 117.9(17) . . ? C14 C13 H13A 121.0 . . ? C12 C13 H13A 121.0 . . ? N5 C14 C13 125.8(17) . . ? N5 C14 H14A 117.1 . . ? C13 C14 H14A 117.1 . . ? C16 C15 N6 124.1(17) . . ? C16 C15 H15A 117.9 . . ? N6 C15 H15A 117.9 . . ? C15 C16 C17 120.1(19) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C18 C17 C16 117.2(16) . . ? C18 C17 H17A 121.4 . . ? C16 C17 H17A 121.4 . . ? C17 C18 C19 118.2(18) . . ? C17 C18 H18A 120.9 . . ? C19 C18 H18A 120.9 . . ? N6 C19 C18 122.1(18) . . ? N6 C19 H19A 119.0 . . ? C18 C19 H19A 119.0 . . ? O2 C20 O3 124.1(16) . . ? O2 C20 C21 120.1(16) . . ? O3 C20 C21 115.7(14) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O5 C22 O4 125.9(14) . . ? O5 C22 C23 120.2(13) . . ? O4 C22 C23 113.9(15) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O6 C24 O7 125.4(16) . . ? O6 C24 C25 118.5(14) . . ? O7 C24 C25 116.1(14) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O8 C26 O9 125.3(16) . . ? O8 C26 C27 118.3(13) . . ? O9 C26 C27 116.4(13) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O11 C28 O10 127.7(14) . . ? O11 C28 C29 114.8(13) . . ? O10 C28 C29 117.4(13) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? F2 P1 F6 91.4(7) . . ? F2 P1 F5 90.4(6) . . ? F6 P1 F5 90.9(6) . . ? F2 P1 F1 89.1(7) . . ? F6 P1 F1 178.5(8) . . ? F5 P1 F1 90.5(7) . . ? F2 P1 F4 178.9(6) . . ? F6 P1 F4 88.4(6) . . ? F5 P1 F4 90.7(6) . . ? F1 P1 F4 91.1(7) . . ? F2 P1 F3 89.6(7) . . ? F6 P1 F3 88.7(7) . . ? F5 P1 F3 179.6(7) . . ? F1 P1 F3 89.9(7) . . ? F4 P1 F3 89.2(6) . . ? Cl01 C01 Cl02 112.6(10) . . ? Cl01 C01 H01A 109.1 . . ? Cl02 C01 H01A 109.1 . . ? Cl01 C01 H01B 109.1 . . ? Cl02 C01 H01B 109.1 . . ? H01A C01 H01B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 2.217 _refine_diff_density_min -2.448 _refine_diff_density_rms 0.261 # Attachment 'compound 5.cif' data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 730668' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H28 N7 O11 Ru3, C H2 Cl2, F6 P' _chemical_formula_sum 'C26 H30 Cl2 F6 N7 O11 P Ru3' _chemical_formula_weight 1135.65 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.011(9) _cell_length_b 16.931(6) _cell_length_c 15.356(6) _cell_angle_alpha 90.00 _cell_angle_beta 116.807(5) _cell_angle_gamma 90.00 _cell_volume 3947(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8887 _cell_measurement_theta_min 2.4104 _cell_measurement_theta_max 27.4680 _exptl_crystal_description Prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2500 _exptl_crystal_size_min 0.1100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.911 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 1.399 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8243 _exptl_absorpt_correction_T_max 1.0000 _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 SATURN70' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25004 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6886 _reflns_number_gt 6071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0670P)^2^+46.3926P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0028(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6886 _refine_ls_number_parameters 571 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1780 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.124 _refine_ls_shift/su_mean 0.006 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 0.19007(5) -0.31607(4) 0.47858(5) 0.0360(2) Uani 1 1 d . A . Ru2 Ru 0.13405(5) -0.13262(4) 0.44317(5) 0.0367(2) Uani 1 1 d . A . Ru3 Ru 0.34429(5) -0.18170(4) 0.51260(6) 0.0382(2) Uani 1 1 d . A . P1 P 0.2017(4) 0.2616(3) 0.5570(4) 0.1076(16) Uani 1 1 d . . . F1 F 0.1917(16) 0.1868(9) 0.4890(14) 0.229(9) Uani 1 1 d . . . F2 F 0.1970(13) 0.3132(9) 0.4719(12) 0.199(7) Uani 1 1 d . . . F3 F 0.2115(12) 0.3373(9) 0.6130(11) 0.187(6) Uani 1 1 d . . . F4 F 0.2060(10) 0.2085(9) 0.6397(12) 0.183(7) Uani 1 1 d . . . F5 F 0.1019(10) 0.2699(12) 0.5175(15) 0.225(9) Uani 1 1 d . . . F6 F 0.3015(9) 0.2461(11) 0.5941(12) 0.191(7) Uani 1 1 d . . . N1 N 0.1265(6) -0.4258(5) 0.4464(6) 0.048(2) Uani 1 1 d . . . N2 N 0.0431(5) -0.4204(5) 0.3707(6) 0.050(2) Uani 1 1 d . . . N3 N 0.0729(5) -0.2897(5) 0.3794(5) 0.0409(18) Uani 1 1 d . . . N4 N 0.0495(5) -0.2117(5) 0.3637(6) 0.0426(18) Uani 1 1 d . . . N5 N -0.0512(6) -0.1132(6) 0.3103(7) 0.060(2) Uani 1 1 d . . . N6 N 0.0181(6) -0.0677(6) 0.3778(7) 0.056(2) Uani 1 1 d . . . N7 N 0.4751(5) -0.1523(5) 0.5423(7) 0.059(2) Uani 1 1 d D . . O1 O 0.2285(4) -0.2096(4) 0.4858(4) 0.0347(13) Uani 1 1 d . . . O2 O 0.1452(4) -0.2945(4) 0.5798(5) 0.0457(16) Uani 1 1 d . . . O3 O 0.1062(4) -0.1655(4) 0.5556(5) 0.0462(16) Uani 1 1 d . . . O4 O 0.3072(5) -0.3566(4) 0.5902(5) 0.0549(18) Uani 1 1 d . . . O5 O 0.3975(4) -0.2495(4) 0.6338(5) 0.0545(18) Uani 1 1 d . . . O6 O 0.2349(4) -0.3465(4) 0.3797(5) 0.0455(16) Uani 1 1 d . . . O7 O 0.3570(4) -0.2716(4) 0.4296(6) 0.0570(19) Uani 1 1 d . . . O8 O 0.1585(4) -0.0906(4) 0.3313(5) 0.0483(16) Uani 1 1 d . . . O9 O 0.3056(4) -0.1109(4) 0.3924(5) 0.0503(17) Uani 1 1 d . . . O10 O 0.2109(4) -0.0409(4) 0.5296(5) 0.0465(16) Uani 1 1 d . . . O11 O 0.3500(4) -0.0875(4) 0.5976(5) 0.0467(16) Uani 1 1 d . . . C1 C 0.1383(9) -0.5009(6) 0.4734(9) 0.064(3) Uani 1 1 d U . . H1A H 0.1891 -0.5215 0.5239 0.077 Uiso 1 1 calc R . . C2 C 0.0636(9) -0.5446(8) 0.4151(10) 0.079(3) Uani 1 1 d U . . H2A H 0.0555 -0.5985 0.4193 0.095 Uiso 1 1 calc R . . C3 C 0.0040(9) -0.4924(8) 0.3501(11) 0.075(3) Uani 1 1 d U . . H3A H -0.0521 -0.5041 0.3016 0.090 Uiso 1 1 calc R . . C4 C 0.0108(6) -0.3459(7) 0.3370(8) 0.048(2) Uani 1 1 d . . . C5 C -0.0758(7) -0.3265(8) 0.2714(8) 0.059(3) Uani 1 1 d . . . H5A H -0.1170 -0.3656 0.2382 0.071 Uiso 1 1 calc R . . C6 C -0.0982(7) -0.2478(8) 0.2575(8) 0.063(3) Uani 1 1 d . . . H6A H -0.1550 -0.2326 0.2140 0.076 Uiso 1 1 calc R . . C7 C -0.0364(6) -0.1926(7) 0.3079(7) 0.046(2) Uani 1 1 d . . . C8 C -0.1251(8) -0.0670(10) 0.2692(11) 0.084(4) Uani 1 1 d . . . H8A H -0.1803 -0.0836 0.2227 0.101 Uiso 1 1 calc R . . C9 C -0.1052(9) 0.0052(10) 0.3064(11) 0.084(4) Uani 1 1 d . . . H9A H -0.1431 0.0483 0.2899 0.101 Uiso 1 1 calc R . . C10 C -0.0150(9) 0.0043(8) 0.3763(12) 0.084(4) Uani 1 1 d . . . H10A H 0.0161 0.0468 0.4147 0.101 Uiso 1 1 calc R . . C11 C 0.1132(6) -0.2318(6) 0.5953(7) 0.044(2) Uani 1 1 d . A . C12 C 0.0822(9) -0.2371(8) 0.6745(9) 0.067(3) Uani 1 1 d . . . H12A H 0.0905 -0.2900 0.6996 0.101 Uiso 1 1 calc R A . H12B H 0.0209 -0.2235 0.6471 0.101 Uiso 1 1 calc R . . H12C H 0.1157 -0.2011 0.7264 0.101 Uiso 1 1 calc R . . C13 C 0.3752(7) -0.3193(7) 0.6464(8) 0.056(3) Uani 1 1 d . A . C14 C 0.4416(11) -0.3606(9) 0.7380(13) 0.124(8) Uani 1 1 d . . . H14A H 0.4202 -0.4122 0.7421 0.186 Uiso 1 1 calc R A . H14B H 0.4498 -0.3303 0.7943 0.186 Uiso 1 1 calc R . . H14C H 0.4968 -0.3652 0.7355 0.186 Uiso 1 1 calc R . . C15 C 0.3043(6) -0.3231(6) 0.3764(8) 0.046(2) Uani 1 1 d . A . C16 C 0.3250(8) -0.3586(9) 0.2978(10) 0.077(4) Uani 1 1 d . . . H16A H 0.3788 -0.3364 0.3029 0.116 Uiso 1 1 calc R A . H16B H 0.2778 -0.3470 0.2346 0.116 Uiso 1 1 calc R . . H16C H 0.3313 -0.4148 0.3064 0.116 Uiso 1 1 calc R . . C17 C 0.2322(7) -0.0859(6) 0.3282(7) 0.046(2) Uani 1 1 d . A . C18 C 0.2308(9) -0.0488(7) 0.2389(8) 0.064(3) Uani 1 1 d . . . H18A H 0.2894 -0.0480 0.2447 0.096 Uiso 1 1 calc R A . H18B H 0.2090 0.0043 0.2324 0.096 Uiso 1 1 calc R . . H18C H 0.1932 -0.0789 0.1824 0.096 Uiso 1 1 calc R . . C19 C 0.2917(7) -0.0373(6) 0.5890(7) 0.041(2) Uani 1 1 d . A . C20 C 0.3213(8) 0.0343(7) 0.6553(8) 0.057(3) Uani 1 1 d . . . H20A H 0.2716 0.0678 0.6417 0.085 Uiso 1 1 calc R A . H20B H 0.3646 0.0629 0.6441 0.085 Uiso 1 1 calc R . . H20C H 0.3465 0.0174 0.7221 0.085 Uiso 1 1 calc R . . C21 C 0.5371(9) -0.1344(16) 0.6357(9) 0.099(8) Uani 0.479(14) 1 d PDU A 1 H21A H 0.5215 -0.1335 0.6865 0.119 Uiso 0.479(14) 1 calc PR A 1 C22 C 0.6231(9) -0.1177(19) 0.6537(11) 0.126(8) Uani 0.479(14) 1 d PDU A 1 H22A H 0.6657 -0.1068 0.7168 0.151 Uiso 0.479(14) 1 calc PR A 1 C23 C 0.6451(7) -0.1173(9) 0.5767(15) 0.133(5) Uani 0.479(14) 1 d PDU A 1 H23A H 0.6991 -0.0972 0.5856 0.160 Uiso 0.479(14) 1 calc PR A 1 C24 C 0.5862(11) -0.147(2) 0.4868(14) 0.125(8) Uani 0.479(14) 1 d PDU A 1 H24A H 0.6046 -0.1584 0.4396 0.150 Uiso 0.479(14) 1 calc PR A 1 C25 C 0.4993(9) -0.1594(17) 0.4677(10) 0.114(8) Uani 0.479(14) 1 d PDU A 1 H25A H 0.4574 -0.1724 0.4050 0.136 Uiso 0.479(14) 1 calc PR A 1 C21' C 0.5398(9) -0.2095(9) 0.579(2) 0.138(10) Uani 0.521(14) 1 d PDU A 2 H21B H 0.5255 -0.2607 0.5891 0.166 Uiso 0.521(14) 1 calc PR A 2 C22' C 0.6263(8) -0.1903(12) 0.602(2) 0.140(8) Uani 0.521(14) 1 d PDU A 2 H22B H 0.6713 -0.2265 0.6348 0.168 Uiso 0.521(14) 1 calc PR A 2 C23' C 0.6451(7) -0.1173(9) 0.5767(15) 0.133(5) Uani 0.521(14) 1 d PDU A 2 H23B H 0.7008 -0.1071 0.5820 0.160 Uiso 0.521(14) 1 calc PR A 2 C24' C 0.5807(10) -0.0586(10) 0.543(2) 0.115(7) Uani 0.521(14) 1 d PDU A 2 H24B H 0.5952 -0.0075 0.5331 0.137 Uiso 0.521(14) 1 calc PR A 2 C25' C 0.4950(9) -0.0770(8) 0.5235(18) 0.090(7) Uani 0.521(14) 1 d PDU A 2 H25B H 0.4510 -0.0389 0.4980 0.108 Uiso 0.521(14) 1 calc PR A 2 C01 C 0.365(4) -0.523(3) 0.496(3) 0.25(10) Uani 0.38(3) 1 d PD B 1 H01A H 0.3749 -0.4695 0.4806 0.298 Uiso 0.38(3) 1 calc PR B 1 H01B H 0.3074 -0.5254 0.4939 0.298 Uiso 0.38(3) 1 calc PR B 1 Cl1 Cl 0.3689(18) -0.5883(15) 0.409(2) 0.164(10) Uani 0.38(3) 1 d PD B 1 Cl2 Cl 0.446(3) -0.548(4) 0.614(3) 0.53(7) Uani 0.38(3) 1 d PD B 1 C02 C 0.414(2) -0.6191(16) 0.4980(16) 0.159(19) Uani 0.62(3) 1 d PD B 2 H02A H 0.3914 -0.6558 0.5303 0.191 Uiso 0.62(3) 1 calc PR B 2 H02B H 0.4773 -0.6224 0.5298 0.191 Uiso 0.62(3) 1 calc PR B 2 Cl3 Cl 0.3729(14) -0.6461(15) 0.3740(12) 0.228(12) Uani 0.62(3) 1 d PD B 2 Cl4 Cl 0.381(2) -0.5229(16) 0.510(3) 0.41(4) Uani 0.62(3) 1 d PD 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 0.0338(4) 0.0385(4) 0.0344(4) -0.0013(3) 0.0144(3) -0.0026(3) Ru2 0.0351(4) 0.0435(5) 0.0332(4) 0.0033(3) 0.0169(3) 0.0054(3) Ru3 0.0307(4) 0.0408(5) 0.0429(4) -0.0060(3) 0.0165(3) -0.0032(3) P1 0.129(4) 0.089(3) 0.128(4) 0.028(3) 0.079(4) 0.031(3) F1 0.36(3) 0.145(13) 0.192(16) -0.013(11) 0.133(19) 0.056(15) F2 0.32(2) 0.167(13) 0.180(14) 0.059(11) 0.175(16) 0.073(13) F3 0.260(19) 0.135(11) 0.146(12) -0.028(9) 0.074(12) 0.004(11) F4 0.214(14) 0.183(12) 0.232(15) 0.113(12) 0.171(13) 0.104(11) F5 0.117(11) 0.25(2) 0.26(2) 0.070(17) 0.050(12) 0.040(12) F6 0.142(11) 0.276(19) 0.200(15) 0.029(14) 0.117(11) 0.064(12) N1 0.054(5) 0.046(5) 0.046(5) -0.005(4) 0.025(4) -0.008(4) N2 0.044(5) 0.053(5) 0.051(5) -0.012(4) 0.021(4) -0.014(4) N3 0.039(4) 0.054(5) 0.036(4) -0.011(4) 0.023(3) -0.007(4) N4 0.040(4) 0.057(5) 0.038(4) 0.000(4) 0.024(4) 0.000(4) N5 0.038(5) 0.079(7) 0.059(6) 0.012(5) 0.017(4) 0.015(5) N6 0.054(5) 0.063(6) 0.053(5) 0.009(4) 0.025(4) 0.014(5) N7 0.044(5) 0.053(5) 0.078(7) -0.023(5) 0.026(5) -0.010(4) O1 0.030(3) 0.044(3) 0.031(3) -0.001(3) 0.015(2) 0.001(3) O2 0.055(4) 0.048(4) 0.037(4) -0.003(3) 0.024(3) -0.004(3) O3 0.048(4) 0.054(4) 0.046(4) -0.003(3) 0.029(3) 0.001(3) O4 0.043(4) 0.044(4) 0.059(5) 0.006(3) 0.007(3) -0.002(3) O5 0.044(4) 0.046(4) 0.057(4) 0.004(3) 0.007(3) -0.001(3) O6 0.038(3) 0.050(4) 0.053(4) -0.013(3) 0.024(3) -0.008(3) O7 0.045(4) 0.060(5) 0.070(5) -0.027(4) 0.030(4) -0.011(4) O8 0.053(4) 0.054(4) 0.042(4) 0.010(3) 0.024(3) 0.006(3) O9 0.042(4) 0.063(4) 0.047(4) 0.009(3) 0.022(3) -0.002(3) O10 0.044(4) 0.049(4) 0.045(4) -0.003(3) 0.019(3) 0.002(3) O11 0.048(4) 0.046(4) 0.044(4) -0.010(3) 0.020(3) -0.002(3) C1 0.087(7) 0.040(5) 0.062(6) -0.012(5) 0.032(5) -0.017(5) C2 0.090(7) 0.052(6) 0.080(7) -0.012(5) 0.025(6) -0.027(5) C3 0.078(7) 0.062(7) 0.079(7) -0.017(6) 0.029(6) -0.033(6) C4 0.041(5) 0.061(6) 0.049(6) -0.008(5) 0.027(5) -0.011(5) C5 0.038(5) 0.084(9) 0.044(6) -0.007(6) 0.009(5) -0.019(6) C6 0.038(6) 0.089(9) 0.053(7) 0.004(6) 0.012(5) -0.001(6) C7 0.037(5) 0.066(7) 0.038(5) 0.001(5) 0.019(4) 0.008(5) C8 0.043(7) 0.110(12) 0.080(9) 0.021(9) 0.010(6) 0.034(7) C9 0.071(9) 0.096(11) 0.087(10) 0.017(9) 0.038(8) 0.044(8) C10 0.080(9) 0.067(8) 0.102(11) 0.018(8) 0.039(8) 0.046(7) C11 0.036(5) 0.057(6) 0.037(5) -0.003(5) 0.014(4) -0.006(4) C12 0.095(9) 0.071(8) 0.057(7) -0.011(6) 0.053(7) -0.027(7) C13 0.051(6) 0.050(6) 0.055(6) 0.006(5) 0.011(5) 0.006(5) C14 0.093(11) 0.073(10) 0.113(13) 0.033(9) -0.035(10) -0.019(9) C15 0.043(5) 0.043(5) 0.052(6) -0.012(5) 0.020(5) 0.001(4) C16 0.067(8) 0.104(10) 0.087(9) -0.043(8) 0.058(8) -0.018(7) C17 0.057(6) 0.039(5) 0.046(6) -0.001(4) 0.029(5) -0.003(5) C18 0.091(9) 0.067(7) 0.046(6) 0.019(6) 0.042(6) 0.004(6) C19 0.057(6) 0.040(5) 0.034(5) -0.002(4) 0.028(5) -0.001(4) C20 0.063(7) 0.055(6) 0.053(6) -0.017(5) 0.027(5) -0.011(5) C21 0.044(11) 0.083(15) 0.16(2) -0.045(15) 0.043(13) -0.011(11) C22 0.058(11) 0.109(14) 0.198(18) -0.037(14) 0.046(12) -0.020(11) C23 0.066(7) 0.129(10) 0.223(14) -0.052(10) 0.081(8) -0.020(7) C24 0.069(11) 0.115(14) 0.227(18) -0.078(13) 0.099(12) -0.031(10) C25 0.076(13) 0.094(15) 0.22(2) -0.084(15) 0.116(14) -0.044(11) C21' 0.048(12) 0.121(17) 0.25(2) -0.065(17) 0.066(14) -0.006(12) C22' 0.061(10) 0.118(14) 0.245(19) -0.059(14) 0.071(12) -0.016(11) C23' 0.066(7) 0.129(10) 0.223(14) -0.052(10) 0.081(8) -0.020(7) C24' 0.081(11) 0.100(13) 0.182(17) -0.043(12) 0.076(12) -0.033(10) C25' 0.072(12) 0.080(14) 0.147(18) -0.036(13) 0.075(12) -0.033(11) C01 0.11(6) 0.06(4) 0.6(3) 0.08(9) 0.23(12) 0.04(4) Cl1 0.19(2) 0.118(15) 0.18(2) 0.033(14) 0.083(17) 0.027(15) Cl2 0.26(5) 0.52(9) 0.64(11) -0.42(9) 0.05(6) 0.04(5) C02 0.09(2) 0.13(3) 0.18(4) 0.03(3) -0.01(2) 0.01(2) Cl3 0.252(18) 0.25(3) 0.161(14) 0.117(16) 0.079(13) 0.029(18) Cl4 0.30(4) 0.18(2) 0.79(12) -0.09(4) 0.28(6) -0.06(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O1 1.904(6) . ? Ru1 N3 1.937(8) . ? Ru1 O6 2.049(6) . ? Ru1 O2 2.049(7) . ? Ru1 O4 2.073(7) . ? Ru1 N1 2.093(8) . ? Ru2 O1 1.938(6) . ? Ru2 N4 1.942(8) . ? Ru2 O3 2.062(7) . ? Ru2 O8 2.068(7) . ? Ru2 O10 2.077(7) . ? Ru2 N6 2.079(9) . ? Ru3 O1 1.882(6) . ? Ru3 O5 2.020(7) . ? Ru3 O11 2.035(6) . ? Ru3 O9 2.045(7) . ? Ru3 O7 2.059(7) . ? Ru3 N7 2.119(7) . ? P1 F3 1.510(14) . ? P1 F4 1.529(13) . ? P1 F5 1.529(15) . ? P1 F6 1.550(14) . ? P1 F2 1.544(14) . ? P1 F1 1.602(16) . ? N1 C1 1.325(14) . ? N1 N2 1.373(12) . ? N2 C3 1.355(14) . ? N2 C4 1.380(14) . ? N3 C4 1.351(12) . ? N3 N4 1.369(11) . ? N4 C7 1.357(12) . ? N5 C8 1.369(14) . ? N5 C7 1.370(14) . ? N5 N6 1.398(13) . ? N6 C10 1.338(15) . ? N7 C21 1.377(8) . ? N7 C21' 1.382(8) . ? N7 C25' 1.383(8) . ? N7 C25 1.387(8) . ? O2 C11 1.264(12) . ? O3 C11 1.257(12) . ? O4 C13 1.258(13) . ? O5 C13 1.282(13) . ? O6 C15 1.267(12) . ? O7 C15 1.253(12) . ? O8 C17 1.277(12) . ? O9 C17 1.265(12) . ? O10 C19 1.262(12) . ? O11 C19 1.268(11) . ? C1 C2 1.392(16) . ? C1 H1A 0.9300 . ? C2 C3 1.376(19) . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C4 C5 1.397(15) . ? C5 C6 1.377(17) . ? C5 H5A 0.9300 . ? C6 C7 1.359(16) . ? C6 H6A 0.9300 . ? C8 C9 1.33(2) . ? C8 H8A 0.9300 . ? C9 C10 1.42(2) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.531(14) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.520(16) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.525(14) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.499(13) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.515(13) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.390(8) . ? C21 H21A 0.9300 . ? C22 C23 1.392(8) . ? C22 H22A 0.9300 . ? C23 C24 1.383(9) . ? C23 H23A 0.9300 . ? C24 C25 1.387(8) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C21' C22' 1.389(9) . ? C21' H21B 0.9300 . ? C22' H22B 0.9300 . ? C24' C25' 1.387(8) . ? C24' H24B 0.9300 . ? C25' H25B 0.9300 . ? C01 Cl2 1.761(10) . ? C01 Cl1 1.759(10) . ? C01 H01A 0.9700 . ? C01 H01B 0.9700 . ? C02 Cl4 1.753(10) . ? C02 Cl3 1.767(10) . ? C02 H02A 0.9700 . ? C02 H02B 0.9700 . ? 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 N3 91.8(3) . . ? O1 Ru1 O6 92.8(3) . . ? N3 Ru1 O6 94.0(3) . . ? O1 Ru1 O2 91.3(3) . . ? N3 Ru1 O2 87.3(3) . . ? O6 Ru1 O2 175.7(3) . . ? O1 Ru1 O4 95.1(3) . . ? N3 Ru1 O4 172.1(3) . . ? O6 Ru1 O4 89.4(3) . . ? O2 Ru1 O4 88.8(3) . . ? O1 Ru1 N1 168.9(3) . . ? N3 Ru1 N1 77.3(3) . . ? O6 Ru1 N1 85.8(3) . . ? O2 Ru1 N1 90.5(3) . . ? O4 Ru1 N1 95.9(3) . . ? O1 Ru2 N4 90.9(3) . . ? O1 Ru2 O3 90.2(3) . . ? N4 Ru2 O3 87.4(3) . . ? O1 Ru2 O8 93.7(3) . . ? N4 Ru2 O8 94.9(3) . . ? O3 Ru2 O8 175.4(3) . . ? O1 Ru2 O10 95.7(3) . . ? N4 Ru2 O10 172.6(3) . . ? O3 Ru2 O10 89.0(3) . . ? O8 Ru2 O10 88.2(3) . . ? O1 Ru2 N6 168.4(3) . . ? N4 Ru2 N6 77.8(4) . . ? O3 Ru2 N6 91.2(3) . . ? O8 Ru2 N6 85.4(3) . . ? O10 Ru2 N6 95.8(3) . . ? O1 Ru3 O5 92.8(3) . . ? O1 Ru3 O11 94.6(3) . . ? O5 Ru3 O11 89.0(3) . . ? O1 Ru3 O9 94.0(3) . . ? O5 Ru3 O9 173.1(3) . . ? O11 Ru3 O9 91.3(3) . . ? O1 Ru3 O7 94.1(3) . . ? O5 Ru3 O7 91.2(3) . . ? O11 Ru3 O7 171.3(3) . . ? O9 Ru3 O7 87.5(3) . . ? O1 Ru3 N7 179.0(3) . . ? O5 Ru3 N7 86.8(3) . . ? O11 Ru3 N7 86.3(3) . . ? O9 Ru3 N7 86.3(3) . . ? O7 Ru3 N7 85.0(3) . . ? F3 P1 F4 94.3(10) . . ? F3 P1 F5 88.1(11) . . ? F4 P1 F5 90.8(10) . . ? F3 P1 F6 96.5(11) . . ? F4 P1 F6 87.7(8) . . ? F5 P1 F6 175.3(12) . . ? F3 P1 F2 87.3(9) . . ? F4 P1 F2 178.4(10) . . ? F5 P1 F2 89.3(10) . . ? F6 P1 F2 92.1(10) . . ? F3 P1 F1 174.1(10) . . ? F4 P1 F1 91.6(10) . . ? F5 P1 F1 92.4(13) . . ? F6 P1 F1 83.2(11) . . ? F2 P1 F1 86.8(9) . . ? C1 N1 N2 106.3(9) . . ? C1 N1 Ru1 142.1(8) . . ? N2 N1 Ru1 111.6(6) . . ? C3 N2 N1 110.4(10) . . ? C3 N2 C4 131.6(10) . . ? N1 N2 C4 117.6(8) . . ? C4 N3 N4 119.4(8) . . ? C4 N3 Ru1 121.4(7) . . ? N4 N3 Ru1 118.4(6) . . ? C7 N4 N3 119.2(8) . . ? C7 N4 Ru2 120.9(7) . . ? N3 N4 Ru2 118.7(6) . . ? C8 N5 C7 133.6(12) . . ? C8 N5 N6 108.6(11) . . ? C7 N5 N6 117.1(8) . . ? C10 N6 N5 106.4(10) . . ? C10 N6 Ru2 142.1(10) . . ? N5 N6 Ru2 111.5(7) . . ? C21 N7 C21' 68.4(18) . . ? C21 N7 C25' 82.5(11) . . ? C21' N7 C25' 120.6(6) . . ? C21 N7 C25 120.4(6) . . ? C21' N7 C25 78.6(11) . . ? C25' N7 C25 73.4(16) . . ? C21 N7 Ru3 120.8(7) . . ? C21' N7 Ru3 119.2(7) . . ? C25' N7 Ru3 120.2(7) . . ? C25 N7 Ru3 118.4(7) . . ? Ru3 O1 Ru1 123.2(3) . . ? Ru3 O1 Ru2 122.1(3) . . ? Ru1 O1 Ru2 114.0(3) . . ? C11 O2 Ru1 129.2(6) . . ? C11 O3 Ru2 129.8(6) . . ? C13 O4 Ru1 130.1(7) . . ? C13 O5 Ru3 128.5(7) . . ? C15 O6 Ru1 128.0(6) . . ? C15 O7 Ru3 132.4(6) . . ? C17 O8 Ru2 128.4(6) . . ? C17 O9 Ru3 134.6(6) . . ? C19 O10 Ru2 131.7(6) . . ? C19 O11 Ru3 130.6(6) . . ? N1 C1 C2 110.1(12) . . ? N1 C1 H1A 125.0 . . ? C2 C1 H1A 125.0 . . ? C1 C2 C3 106.6(11) . . ? C1 C2 H2A 126.7 . . ? C3 C2 H2A 126.7 . . ? N2 C3 C2 106.6(11) . . ? N2 C3 H3A 126.7 . . ? C2 C3 H3A 126.7 . . ? N3 C4 N2 111.7(9) . . ? N3 C4 C5 121.6(11) . . ? N2 C4 C5 126.6(10) . . ? C6 C5 C4 117.8(10) . . ? C6 C5 H5A 121.1 . . ? C4 C5 H5A 121.1 . . ? C7 C6 C5 119.3(10) . . ? C7 C6 H6A 120.3 . . ? C5 C6 H6A 120.3 . . ? N4 C7 C6 122.1(10) . . ? N4 C7 N5 112.1(9) . . ? C6 C7 N5 125.8(10) . . ? C9 C8 N5 108.9(13) . . ? C9 C8 H8A 125.5 . . ? N5 C8 H8A 125.5 . . ? C8 C9 C10 107.1(12) . . ? C8 C9 H9A 126.5 . . ? C10 C9 H9A 126.5 . . ? N6 C10 C9 109.0(14) . . ? N6 C10 H10A 125.5 . . ? C9 C10 H10A 125.5 . . ? O2 C11 O3 127.8(9) . . ? O2 C11 C12 115.7(9) . . ? O3 C11 C12 116.5(9) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 O5 127.0(10) . . ? O4 C13 C14 118.3(10) . . ? O5 C13 C14 114.6(10) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O7 C15 O6 126.6(9) . . ? O7 C15 C16 115.9(9) . . ? O6 C15 C16 117.4(9) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O9 C17 O8 126.2(9) . . ? O9 C17 C18 117.1(9) . . ? O8 C17 C18 116.7(10) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O10 C19 O11 126.0(9) . . ? O10 C19 C20 116.7(9) . . ? O11 C19 C20 117.3(9) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N7 C21 C22 119.6(7) . . ? N7 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? C21 C22 C23 119.6(7) . . ? C21 C22 H22A 120.2 . . ? C23 C22 H22A 120.2 . . ? C24 C23 C22 119.7(7) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C23 C24 C25 119.3(7) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? N7 C25 C24 119.8(7) . . ? N7 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? N7 C21' C22' 119.7(7) . . ? N7 C21' H21B 120.1 . . ? C22' C21' H21B 120.1 . . ? C21' C22' H22B 120.2 . . ? C25' C24' H24B 120.2 . . ? N7 C25' C24' 119.7(7) . . ? N7 C25' H25B 120.2 . . ? C24' C25' H25B 120.2 . . ? Cl2 C01 Cl1 111.0(9) . . ? Cl2 C01 H01A 109.6 . . ? Cl1 C01 H01A 109.7 . . ? Cl2 C01 H01B 109.4 . . ? Cl1 C01 H01B 109.2 . . ? H01A C01 H01B 108.0 . . ? Cl4 C02 Cl3 111.2(9) . . ? Cl4 C02 H02A 109.2 . . ? Cl3 C02 H02A 109.4 . . ? Cl4 C02 H02B 109.5 . . ? Cl3 C02 H02B 109.4 . . ? H02A C02 H02B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.343 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.142 # Attachment 'compound 7.cif' data_compound_7 _database_code_depnum_ccdc_archive 'CCDC 730669' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C27 H28 N7 O11 Ru3), (F6 P), 1.5(C H2 Cl2)' _chemical_formula_sum 'C28.50 H31 Cl3 F6 N7 O11 P Ru3' _chemical_formula_weight 1202.13 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.278(18) _cell_length_b 8.539(3) _cell_length_c 30.424(13) _cell_angle_alpha 90.00 _cell_angle_beta 129.855(2) _cell_angle_gamma 90.00 _cell_volume 8432(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7848 _cell_measurement_theta_min 2.0508 _cell_measurement_theta_max 27.4835 _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 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4728 _exptl_absorpt_coefficient_mu 1.377 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7186 _exptl_absorpt_correction_T_max 1.0000 _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 SATURN70' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30876 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9636 _reflns_number_gt 8192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0845P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9636 _refine_ls_number_parameters 537 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1663 _refine_ls_wR_factor_gt 0.1568 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.839321(12) 0.43572(5) 0.920505(17) 0.02801(12) Uani 1 1 d . . . Ru2 Ru 0.928288(13) 0.27170(5) 1.010322(17) 0.02905(13) Uani 1 1 d . . . Ru3 Ru 0.877928(14) 0.38120(5) 1.056170(18) 0.03091(13) Uani 1 1 d . . . P1 P 0.87503(9) 0.1043(3) 0.78454(11) 0.0697(6) Uani 1 1 d . . . F1 F 0.8906(3) -0.0657(8) 0.8055(3) 0.126(3) Uani 1 1 d . . . F2 F 0.8593(4) 0.2722(8) 0.7630(4) 0.155(4) Uani 1 1 d . . . F3 F 0.9184(3) 0.1683(15) 0.8136(5) 0.180(5) Uani 1 1 d . . . F4 F 0.8304(2) 0.0456(12) 0.7545(4) 0.140(3) Uani 1 1 d . . . F5 F 0.8689(3) 0.0699(8) 0.7280(3) 0.122(3) Uani 1 1 d . . . F6 F 0.8818(2) 0.1423(8) 0.8411(3) 0.099(2) Uani 1 1 d . . . N1 N 0.80556(14) 0.5441(6) 0.83968(19) 0.0323(10) Uani 1 1 d . . . N2 N 0.89715(16) 0.5400(6) 0.8543(2) 0.0404(11) Uani 1 1 d . . . N3 N 0.88031(13) 0.4666(5) 0.91274(19) 0.0289(9) Uani 1 1 d . . . N4 N 0.91720(13) 0.3975(5) 0.94989(19) 0.0296(9) Uani 1 1 d . . . N5 N 0.93478(16) 0.4712(7) 0.8924(2) 0.0408(11) Uani 1 1 d . . . N6 N 0.97966(14) 0.2252(6) 1.0162(2) 0.0334(10) Uani 1 1 d . . . N7 N 0.87586(15) 0.4073(6) 1.1236(2) 0.0384(11) Uani 1 1 d . . . O1 O 0.88049(11) 0.3543(4) 0.99741(15) 0.0299(8) Uani 1 1 d . . . O2 O 0.83015(12) 0.2162(5) 0.88736(16) 0.0354(9) Uani 1 1 d . . . O3 O 0.89246(12) 0.0984(5) 0.95150(16) 0.0339(8) Uani 1 1 d . . . O4 O 0.78989(13) 0.3935(6) 0.91786(18) 0.0432(10) Uani 1 1 d . . . O5 O 0.81881(13) 0.2997(6) 1.00642(18) 0.0470(11) Uani 1 1 d . . . O6 O 0.84192(14) 0.6555(5) 0.94955(18) 0.0418(10) Uani 1 1 d . . . O7 O 0.85651(14) 0.6069(5) 1.03364(18) 0.0419(10) Uani 1 1 d . . . O8 O 0.94353(13) 0.1105(5) 1.07217(18) 0.0416(10) Uani 1 1 d . . . O9 O 0.89849(15) 0.1591(5) 1.08678(19) 0.0435(10) Uani 1 1 d . . . O10 O 0.96686(13) 0.4276(5) 1.07478(18) 0.0401(10) Uani 1 1 d . . . O11 O 0.93713(13) 0.4652(6) 1.11434(17) 0.0427(10) Uani 1 1 d . . . C1 C 0.7471(3) 0.2797(16) 0.9330(4) 0.092(4) Uani 1 1 d . . . H1A H 0.7494 0.2305 0.9633 0.138 Uiso 1 1 calc R . . H1B H 0.7354 0.2069 0.9020 0.138 Uiso 1 1 calc R . . H1C H 0.7295 0.3699 0.9197 0.138 Uiso 1 1 calc R . . C2 C 0.78883(19) 0.3290(9) 0.9547(3) 0.0466(15) Uani 1 1 d . . . C3 C 0.9378(3) -0.0724(9) 1.1245(4) 0.062(2) Uani 1 1 d . . . H3A H 0.9231 -0.0838 1.1385 0.092 Uiso 1 1 calc R . . H3B H 0.9669 -0.0718 1.1562 0.092 Uiso 1 1 calc R . . H3C H 0.9313 -0.1583 1.0995 0.092 Uiso 1 1 calc R . . C4 C 0.9257(2) 0.0787(7) 1.0921(2) 0.0389(13) Uani 1 1 d . . . C5 C 1.0042(2) 0.5649(10) 1.1611(3) 0.0569(19) Uani 1 1 d . . . H5B H 1.0009 0.5991 1.1880 0.085 Uiso 1 1 calc R . . H5C H 1.0086 0.6541 1.1464 0.085 Uiso 1 1 calc R . . H5D H 1.0274 0.4958 1.1798 0.085 Uiso 1 1 calc R . . C6 C 0.96589(17) 0.4797(7) 1.1124(2) 0.0351(12) Uani 1 1 d . . . C7 C 0.8367(3) 0.8608(9) 0.9959(3) 0.062(2) Uani 1 1 d . . . H7A H 0.8408 0.8782 1.0304 0.093 Uiso 1 1 calc R . . H7B H 0.8086 0.8832 0.9633 0.093 Uiso 1 1 calc R . . H7C H 0.8546 0.9281 0.9953 0.093 Uiso 1 1 calc R . . C8 C 0.84608(19) 0.6946(7) 0.9935(3) 0.0375(13) Uani 1 1 d . . . C9 C 0.8370(2) -0.0504(7) 0.8747(3) 0.0427(14) Uani 1 1 d . . . H9A H 0.8582 -0.1289 0.8934 0.064 Uiso 1 1 calc R . . H9B H 0.8268 -0.0357 0.8363 0.064 Uiso 1 1 calc R . . H9C H 0.8148 -0.0836 0.8737 0.064 Uiso 1 1 calc R . . C10 C 0.85445(17) 0.1016(6) 0.9071(2) 0.0312(11) Uani 1 1 d . . . C11 C 0.8638(2) 0.2924(9) 1.1388(3) 0.0474(16) Uani 1 1 d . . . H11A H 0.8537 0.2011 1.1171 0.057 Uiso 1 1 calc R . . C12 C 0.8655(2) 0.3016(11) 1.1856(3) 0.060(2) Uani 1 1 d . . . H12A H 0.8571 0.2175 1.1955 0.072 Uiso 1 1 calc R . . C13 C 0.8796(2) 0.4366(11) 1.2173(3) 0.060(2) Uani 1 1 d . . . H13A H 0.8809 0.4458 1.2489 0.072 Uiso 1 1 calc R . . C14 C 0.8918(2) 0.5570(10) 1.2020(3) 0.0581(19) Uani 1 1 d . . . H14A H 0.9013 0.6500 1.2227 0.070 Uiso 1 1 calc R . . C15 C 0.8897(2) 0.5391(9) 1.1550(3) 0.0463(15) Uani 1 1 d . . . H15A H 0.8982 0.6215 1.1448 0.056 Uiso 1 1 calc R . . C20 C 0.87124(18) 0.5297(6) 0.8642(2) 0.0321(11) Uani 1 1 d . . . C21 C 0.76584(18) 0.5868(7) 0.8053(2) 0.0384(13) Uani 1 1 d . . . H21A H 0.7502 0.5646 0.8163 0.046 Uiso 1 1 calc R . . C22 C 0.7473(2) 0.6639(8) 0.7535(3) 0.0486(16) Uani 1 1 d . . . H22A H 0.7198 0.6939 0.7305 0.058 Uiso 1 1 calc R . . C23 C 0.7703(2) 0.6950(9) 0.7369(3) 0.0506(17) Uani 1 1 d . . . H23A H 0.7581 0.7434 0.7019 0.061 Uiso 1 1 calc R . . C24 C 0.8110(2) 0.6546(8) 0.7717(2) 0.0417(14) Uani 1 1 d . . . H24A H 0.8270 0.6776 0.7615 0.050 Uiso 1 1 calc R . . C25 C 1.01291(18) 0.1395(8) 1.0563(3) 0.0419(14) Uani 1 1 d . . . H25A H 1.0139 0.0899 1.0843 0.050 Uiso 1 1 calc R . . C26 C 1.0459(2) 0.1232(9) 1.0570(3) 0.0490(16) Uani 1 1 d . . . H26A H 1.0686 0.0626 1.0849 0.059 Uiso 1 1 calc R . . C27 C 1.0447(2) 0.1981(9) 1.0157(3) 0.0518(17) Uani 1 1 d . . . H27A H 1.0663 0.1863 1.0152 0.062 Uiso 1 1 calc R . . C28 C 1.01122(19) 0.2905(8) 0.9752(3) 0.0439(14) Uani 1 1 d . . . H28A H 1.0102 0.3434 0.9476 0.053 Uiso 1 1 calc R . . C29 C 0.97924(16) 0.3027(7) 0.9765(2) 0.0340(12) Uani 1 1 d . . . C30 C 0.94256(17) 0.3981(7) 0.9365(2) 0.0327(11) Uani 1 1 d . . . C31 C 0.82770(18) 0.5788(7) 0.8225(2) 0.0344(12) Uani 1 1 d . . . C01 C 1.0000 0.908(4) 0.7500 0.164(11) Uani 1 2 d S . . Cl1 Cl 0.9730(2) 0.8284(13) 0.7633(3) 0.324(6) Uani 1 1 d . . . C02 C 0.7183(8) 0.769(3) 0.8775(9) 0.218(12) Uani 1 1 d . . . H02A H 0.6905 0.7362 0.8458 0.262 Uiso 1 1 calc R . . H02B H 0.7360 0.6793 0.8877 0.262 Uiso 1 1 calc R . . Cl3 Cl 0.73157(18) 0.9100(8) 0.8518(2) 0.186(2) Uani 1 1 d . . . Cl4 Cl 0.7198(3) 0.8007(15) 0.9292(3) 0.297(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0269(2) 0.0295(2) 0.0235(2) 0.00071(15) 0.01428(17) 0.00039(16) Ru2 0.0274(2) 0.0299(2) 0.0239(2) 0.00105(16) 0.01372(18) 0.00120(16) Ru3 0.0345(2) 0.0320(3) 0.0252(2) -0.00032(16) 0.01870(19) -0.00200(18) P1 0.1048(19) 0.0602(13) 0.0655(13) -0.0067(10) 0.0644(14) -0.0182(13) F1 0.171(7) 0.083(5) 0.088(5) 0.015(4) 0.066(5) 0.022(5) F2 0.308(13) 0.069(4) 0.116(6) 0.015(4) 0.149(8) 0.021(6) F3 0.165(8) 0.246(12) 0.194(9) -0.116(9) 0.146(8) -0.112(9) F4 0.095(5) 0.167(8) 0.132(7) -0.018(6) 0.060(5) -0.030(5) F5 0.213(8) 0.095(5) 0.093(5) -0.012(4) 0.115(6) -0.007(5) F6 0.155(6) 0.097(4) 0.082(4) -0.009(3) 0.093(4) -0.025(4) N1 0.029(2) 0.033(2) 0.027(2) -0.0007(18) 0.0144(19) 0.0008(19) N2 0.044(3) 0.043(3) 0.040(3) 0.004(2) 0.030(2) 0.001(2) N3 0.028(2) 0.025(2) 0.028(2) 0.0034(17) 0.0157(18) 0.0021(18) N4 0.026(2) 0.027(2) 0.031(2) -0.0043(18) 0.0162(18) -0.0046(18) N5 0.040(3) 0.043(3) 0.045(3) 0.005(2) 0.030(2) 0.001(2) N6 0.030(2) 0.037(3) 0.033(2) -0.0034(19) 0.020(2) 0.0030(19) N7 0.040(3) 0.047(3) 0.028(2) -0.002(2) 0.022(2) -0.001(2) O1 0.0278(17) 0.031(2) 0.0263(17) -0.0004(15) 0.0152(15) -0.0032(15) O2 0.037(2) 0.034(2) 0.0293(19) -0.0025(16) 0.0184(17) 0.0013(17) O3 0.0336(19) 0.028(2) 0.0324(19) -0.0043(15) 0.0175(17) -0.0011(16) O4 0.034(2) 0.058(3) 0.037(2) 0.004(2) 0.0229(19) -0.003(2) O5 0.039(2) 0.063(3) 0.035(2) 0.002(2) 0.0223(19) -0.008(2) O6 0.057(3) 0.030(2) 0.039(2) 0.0012(18) 0.031(2) 0.005(2) O7 0.053(3) 0.038(2) 0.038(2) 0.0066(18) 0.031(2) 0.010(2) O8 0.043(2) 0.040(2) 0.032(2) 0.0108(18) 0.0201(19) 0.0055(19) O9 0.059(3) 0.032(2) 0.046(2) 0.0035(19) 0.036(2) 0.000(2) O10 0.036(2) 0.044(2) 0.036(2) -0.0068(18) 0.0213(18) -0.0089(18) O11 0.039(2) 0.053(3) 0.029(2) -0.0081(19) 0.0180(18) -0.007(2) C1 0.051(4) 0.169(12) 0.051(5) -0.004(6) 0.030(4) -0.041(6) C2 0.033(3) 0.058(4) 0.046(4) -0.007(3) 0.024(3) -0.009(3) C3 0.071(5) 0.043(4) 0.064(5) 0.022(4) 0.040(4) 0.012(4) C4 0.051(3) 0.028(3) 0.031(3) 0.001(2) 0.023(3) -0.004(3) C5 0.046(4) 0.067(5) 0.040(4) -0.023(3) 0.019(3) -0.019(3) C6 0.030(3) 0.031(3) 0.030(3) 0.000(2) 0.012(2) -0.003(2) C7 0.086(6) 0.039(4) 0.050(4) -0.008(3) 0.039(4) 0.003(4) C8 0.040(3) 0.027(3) 0.045(3) -0.005(2) 0.027(3) -0.002(2) C9 0.049(3) 0.029(3) 0.033(3) -0.002(2) 0.019(3) -0.004(3) C10 0.037(3) 0.027(3) 0.029(3) -0.002(2) 0.021(2) -0.006(2) C11 0.046(3) 0.056(4) 0.051(4) -0.007(3) 0.036(3) -0.008(3) C12 0.067(5) 0.077(6) 0.055(4) 0.014(4) 0.048(4) 0.004(4) C13 0.056(4) 0.095(7) 0.041(4) 0.001(4) 0.036(3) 0.003(4) C14 0.061(4) 0.069(5) 0.047(4) -0.015(4) 0.036(4) -0.004(4) C15 0.056(4) 0.053(4) 0.037(3) -0.008(3) 0.033(3) -0.003(3) C20 0.044(3) 0.025(3) 0.028(3) -0.001(2) 0.023(2) -0.003(2) C21 0.031(3) 0.042(3) 0.029(3) 0.006(2) 0.013(2) 0.005(2) C22 0.037(3) 0.048(4) 0.032(3) 0.007(3) 0.009(3) 0.009(3) C23 0.055(4) 0.048(4) 0.032(3) 0.005(3) 0.020(3) 0.005(3) C24 0.053(4) 0.039(3) 0.024(3) 0.000(2) 0.020(3) -0.002(3) C25 0.033(3) 0.044(4) 0.040(3) 0.003(3) 0.019(3) 0.007(3) C26 0.033(3) 0.052(4) 0.051(4) -0.004(3) 0.021(3) 0.005(3) C27 0.039(3) 0.057(4) 0.060(4) -0.012(3) 0.032(3) 0.001(3) C28 0.044(3) 0.045(4) 0.050(4) 0.001(3) 0.033(3) 0.000(3) C29 0.028(2) 0.033(3) 0.037(3) -0.006(2) 0.019(2) -0.001(2) C30 0.035(3) 0.029(3) 0.036(3) -0.003(2) 0.024(2) -0.005(2) C31 0.039(3) 0.032(3) 0.026(3) 0.001(2) 0.018(2) 0.002(2) C01 0.108(16) 0.26(4) 0.130(19) 0.000 0.081(16) 0.000 Cl1 0.192(7) 0.381(13) 0.201(7) 0.052(8) 0.035(5) -0.147(8) C02 0.26(3) 0.30(3) 0.149(17) -0.043(18) 0.15(2) -0.10(2) Cl3 0.163(4) 0.222(6) 0.154(4) 0.022(4) 0.093(4) 0.011(4) Cl4 0.253(8) 0.496(16) 0.147(5) -0.003(8) 0.131(6) -0.064(9) _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 N3 1.911(5) . ? Ru1 O1 1.941(4) . ? Ru1 O2 2.044(4) . ? Ru1 O6 2.047(4) . ? Ru1 O4 2.071(4) . ? Ru1 N1 2.107(5) . ? Ru2 N4 1.910(5) . ? Ru2 O1 1.928(4) . ? Ru2 O10 2.044(4) . ? Ru2 O3 2.052(4) . ? Ru2 O8 2.073(4) . ? Ru2 N6 2.100(5) . ? Ru3 O1 1.873(4) . ? Ru3 O5 2.043(4) . ? Ru3 O9 2.045(5) . ? Ru3 O7 2.052(4) . ? Ru3 O11 2.058(4) . ? Ru3 N7 2.119(5) . ? P1 F2 1.539(8) . ? P1 F3 1.539(9) . ? P1 F1 1.552(7) . ? P1 F4 1.562(8) . ? P1 F6 1.586(6) . ? P1 F5 1.593(6) . ? N1 C21 1.340(7) . ? N1 C31 1.365(8) . ? N2 C20 1.313(7) . ? N2 N5 1.362(7) . ? N3 N4 1.341(6) . ? N3 C20 1.376(7) . ? N4 C30 1.370(7) . ? N5 C30 1.316(8) . ? N6 C25 1.342(8) . ? N6 C29 1.366(8) . ? N7 C11 1.319(9) . ? N7 C15 1.345(9) . ? O2 C10 1.258(7) . ? O3 C10 1.275(7) . ? O4 C2 1.274(8) . ? O5 C2 1.261(8) . ? O6 C8 1.277(7) . ? O7 C8 1.247(7) . ? O8 C4 1.263(8) . ? O9 C4 1.259(8) . ? O10 C6 1.254(7) . ? O11 C6 1.260(7) . ? C1 C2 1.496(10) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C3 C4 1.500(9) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C5 C6 1.507(8) . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C5 H5D 0.9600 . ? C7 C8 1.487(9) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C9 C10 1.506(8) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C11 C12 1.384(9) . ? C11 H11A 0.9300 . ? C12 C13 1.371(12) . ? C12 H12A 0.9300 . ? C13 C14 1.359(12) . ? C13 H13A 0.9300 . ? C14 C15 1.382(9) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C20 C31 1.477(8) . ? C21 C22 1.397(9) . ? C21 H21A 0.9300 . ? C22 C23 1.380(10) . ? C22 H22A 0.9300 . ? C23 C24 1.364(10) . ? C23 H23A 0.9300 . ? C24 C31 1.382(8) . ? C24 H24A 0.9300 . ? C25 C26 1.388(9) . ? C25 H25A 0.9300 . ? C26 C27 1.380(11) . ? C26 H26A 0.9300 . ? C27 C28 1.381(10) . ? C27 H27A 0.9300 . ? C28 C29 1.383(8) . ? C28 H28A 0.9300 . ? C29 C30 1.460(8) . ? C01 Cl1 1.588(15) . ? C01 Cl1 1.588(15) 2_756 ? C02 Cl4 1.559(19) . ? C02 Cl3 1.72(2) . ? C02 H02A 0.9700 . ? C02 H02B 0.9700 . ? 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 N3 Ru1 O1 90.84(17) . . ? N3 Ru1 O2 88.04(18) . . ? O1 Ru1 O2 90.36(16) . . ? N3 Ru1 O6 97.17(19) . . ? O1 Ru1 O6 92.83(17) . . ? O2 Ru1 O6 173.84(17) . . ? N3 Ru1 O4 172.56(18) . . ? O1 Ru1 O4 95.03(17) . . ? O2 Ru1 O4 87.35(18) . . ? O6 Ru1 O4 87.13(19) . . ? N3 Ru1 N1 77.59(18) . . ? O1 Ru1 N1 167.78(17) . . ? O2 Ru1 N1 93.13(17) . . ? O6 Ru1 N1 84.83(18) . . ? O4 Ru1 N1 96.83(18) . . ? N4 Ru2 O1 91.11(18) . . ? N4 Ru2 O10 96.32(19) . . ? O1 Ru2 O10 92.57(17) . . ? N4 Ru2 O3 88.70(18) . . ? O1 Ru2 O3 89.68(16) . . ? O10 Ru2 O3 174.45(17) . . ? N4 Ru2 O8 171.46(19) . . ? O1 Ru2 O8 95.93(17) . . ? O10 Ru2 O8 88.21(18) . . ? O3 Ru2 O8 86.52(17) . . ? N4 Ru2 N6 77.91(19) . . ? O1 Ru2 N6 168.02(18) . . ? O10 Ru2 N6 84.02(18) . . ? O3 Ru2 N6 94.77(17) . . ? O8 Ru2 N6 95.43(19) . . ? O1 Ru3 O5 92.45(17) . . ? O1 Ru3 O9 93.06(17) . . ? O5 Ru3 O9 89.0(2) . . ? O1 Ru3 O7 94.55(17) . . ? O5 Ru3 O7 90.2(2) . . ? O9 Ru3 O7 172.38(17) . . ? O1 Ru3 O11 94.65(17) . . ? O5 Ru3 O11 172.89(17) . . ? O9 Ru3 O11 90.22(19) . . ? O7 Ru3 O11 89.6(2) . . ? O1 Ru3 N7 178.75(19) . . ? O5 Ru3 N7 87.89(19) . . ? O9 Ru3 N7 85.7(2) . . ? O7 Ru3 N7 86.65(19) . . ? O11 Ru3 N7 85.00(18) . . ? F2 P1 F3 86.9(7) . . ? F2 P1 F1 179.3(7) . . ? F3 P1 F1 93.5(7) . . ? F2 P1 F4 91.1(6) . . ? F3 P1 F4 177.9(7) . . ? F1 P1 F4 88.5(5) . . ? F2 P1 F6 90.0(4) . . ? F3 P1 F6 89.1(4) . . ? F1 P1 F6 90.6(4) . . ? F4 P1 F6 90.6(4) . . ? F2 P1 F5 89.1(4) . . ? F3 P1 F5 89.8(5) . . ? F1 P1 F5 90.3(4) . . ? F4 P1 F5 90.5(5) . . ? F6 P1 F5 178.6(4) . . ? C21 N1 C31 117.8(5) . . ? C21 N1 Ru1 127.1(4) . . ? C31 N1 Ru1 115.1(4) . . ? C20 N2 N5 117.8(5) . . ? N4 N3 C20 116.8(5) . . ? N4 N3 Ru1 119.5(3) . . ? C20 N3 Ru1 122.4(4) . . ? N3 N4 C30 117.2(5) . . ? N3 N4 Ru2 119.6(3) . . ? C30 N4 Ru2 122.2(4) . . ? C30 N5 N2 117.7(5) . . ? C25 N6 C29 118.7(5) . . ? C25 N6 Ru2 127.1(4) . . ? C29 N6 Ru2 114.0(4) . . ? C11 N7 C15 117.6(6) . . ? C11 N7 Ru3 121.8(5) . . ? C15 N7 Ru3 120.5(4) . . ? Ru3 O1 Ru2 122.98(19) . . ? Ru3 O1 Ru1 123.4(2) . . ? Ru2 O1 Ru1 112.94(18) . . ? C10 O2 Ru1 129.7(4) . . ? C10 O3 Ru2 129.3(4) . . ? C2 O4 Ru1 130.1(4) . . ? C2 O5 Ru3 129.1(4) . . ? C8 O6 Ru1 128.7(4) . . ? C8 O7 Ru3 134.0(4) . . ? C4 O8 Ru2 130.2(4) . . ? C4 O9 Ru3 130.7(4) . . ? C6 O10 Ru2 129.4(4) . . ? C6 O11 Ru3 132.3(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O5 C2 O4 127.6(6) . . ? O5 C2 C1 116.9(7) . . ? O4 C2 C1 115.5(6) . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O9 C4 O8 126.7(5) . . ? O9 C4 C3 116.9(6) . . ? O8 C4 C3 116.3(6) . . ? C6 C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 C5 H5D 109.5 . . ? H5B C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? O10 C6 O11 127.2(5) . . ? O10 C6 C5 115.2(6) . . ? O11 C6 C5 117.6(6) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O7 C8 O6 126.4(6) . . ? O7 C8 C7 117.6(6) . . ? O6 C8 C7 116.0(6) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 O3 127.7(5) . . ? O2 C10 C9 116.8(5) . . ? O3 C10 C9 115.6(5) . . ? N7 C11 C12 122.9(7) . . ? N7 C11 H11A 118.5 . . ? C12 C11 H11A 118.5 . . ? C13 C12 C11 118.9(7) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? C14 C13 C12 119.1(7) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C13 C14 C15 118.9(7) . . ? C13 C14 H14A 120.5 . . ? C15 C14 H14A 120.5 . . ? N7 C15 C14 122.6(7) . . ? N7 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? N2 C20 N3 125.0(5) . . ? N2 C20 C31 123.3(5) . . ? N3 C20 C31 111.7(5) . . ? N1 C21 C22 121.7(6) . . ? N1 C21 H21A 119.2 . . ? C22 C21 H21A 119.2 . . ? C23 C22 C21 119.1(6) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? C24 C23 C22 120.0(6) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C31 118.4(6) . . ? C23 C24 H24A 120.8 . . ? C31 C24 H24A 120.8 . . ? N6 C25 C26 121.7(6) . . ? N6 C25 H25A 119.2 . . ? C26 C25 H25A 119.2 . . ? C27 C26 C25 119.2(6) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? C26 C27 C28 119.8(6) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C27 C28 C29 118.5(6) . . ? C27 C28 H28A 120.7 . . ? C29 C28 H28A 120.7 . . ? N6 C29 C28 122.0(5) . . ? N6 C29 C30 114.4(5) . . ? C28 C29 C30 123.6(6) . . ? N5 C30 N4 125.0(5) . . ? N5 C30 C29 123.6(5) . . ? N4 C30 C29 111.4(5) . . ? N1 C31 C24 123.0(6) . . ? N1 C31 C20 113.2(5) . . ? C24 C31 C20 123.8(6) . . ? Cl1 C01 Cl1 129(3) . 2_756 ? Cl4 C02 Cl3 121.7(16) . . ? Cl4 C02 H02A 106.9 . . ? Cl3 C02 H02A 106.9 . . ? Cl4 C02 H02B 106.9 . . ? Cl3 C02 H02B 106.9 . . ? H02A C02 H02B 106.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.288 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.143 # Attachment 'compound 8.cif' data_compound_8 _database_code_depnum_ccdc_archive 'CCDC 730670' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H23 N6 O12 Ru3, C H2 Cl2, 0.5(H2 O)' _chemical_formula_sum 'C24 H26 Cl2 N6 O12.50 Ru3' _chemical_formula_weight 972.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.6837(5) _cell_length_b 19.8341(7) _cell_length_c 15.8414(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.420(2) _cell_angle_gamma 90.00 _cell_volume 3538.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7793 _cell_measurement_theta_min 2.0801 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Gray _exptl_crystal_size_max 0.3500 _exptl_crystal_size_mid 0.2500 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 1.480 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7442 _exptl_absorpt_correction_T_max 1.0000 _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 SATURN70' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21799 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6219 _reflns_number_gt 5579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _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^)+(0.0822P)^2^+5.8648P] 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 6219 _refine_ls_number_parameters 443 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.131 _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 0.50668(3) 0.340631(19) 0.43593(3) 0.03034(14) Uani 1 1 d . . . Ru2 Ru 0.62101(3) 0.192909(19) 0.43129(3) 0.03075(14) Uani 1 1 d . . . Ru3 Ru 0.81014(4) 0.32362(2) 0.51698(3) 0.03619(14) Uani 1 1 d . . . N1 N 0.3359(4) 0.3803(2) 0.4249(3) 0.0347(9) Uani 1 1 d . . . N2 N 0.2303(4) 0.2121(2) 0.4420(4) 0.0507(12) Uani 1 1 d . . . N3 N 0.4162(3) 0.2619(2) 0.4469(3) 0.0321(9) Uani 1 1 d . . . N4 N 0.4644(4) 0.2004(2) 0.4442(3) 0.0326(9) Uani 1 1 d . . . N5 N 0.2784(4) 0.1491(2) 0.4363(4) 0.0495(12) Uani 1 1 d . . . N6 N 0.5595(4) 0.0934(2) 0.4102(3) 0.0354(9) Uani 1 1 d . . . O1 O 0.6510(3) 0.28772(17) 0.4570(2) 0.0330(7) Uani 1 1 d . . . O2 O 0.4761(3) 0.32227(18) 0.3043(2) 0.0382(8) Uani 1 1 d . . . O3 O 0.5544(3) 0.21764(18) 0.3017(2) 0.0391(8) Uani 1 1 d . . . O4 O 0.5864(3) 0.43013(19) 0.4131(3) 0.0431(9) Uani 1 1 d . . . O5 O 0.7800(4) 0.4050(2) 0.4313(3) 0.0466(9) Uani 1 1 d . . . O6 O 0.5385(3) 0.36907(19) 0.5636(2) 0.0399(8) Uani 1 1 d . . . O7 O 0.7390(3) 0.37388(19) 0.6066(2) 0.0431(9) Uani 1 1 d . . . O8 O 0.6977(3) 0.16399(19) 0.5581(3) 0.0434(9) Uani 1 1 d . . . O9 O 0.8415(3) 0.2421(2) 0.6046(3) 0.0487(10) Uani 1 1 d . . . O10 O 0.7810(3) 0.17513(19) 0.4029(3) 0.0448(9) Uani 1 1 d . . . O11 O 0.8824(3) 0.2732(2) 0.4275(3) 0.0480(10) Uani 1 1 d . . . O12 O 1.0364(5) 0.3926(4) 0.6080(4) 0.097(2) Uani 1 1 d . . . C1 C 0.6311(6) 0.4118(3) 0.7032(4) 0.0485(14) Uani 1 1 d . . . H1A H 0.7098 0.4208 0.7392 0.073 Uiso 1 1 calc R . . H1B H 0.5924 0.3804 0.7326 0.073 Uiso 1 1 calc R . . H1C H 0.5866 0.4531 0.6929 0.073 Uiso 1 1 calc R . . C2 C 0.6383(5) 0.3826(3) 0.6176(3) 0.0382(12) Uani 1 1 d . . . C3 C 0.8280(8) 0.1530(4) 0.6986(5) 0.080(3) Uani 1 1 d . . . H3A H 0.8940 0.1767 0.7358 0.120 Uiso 1 1 calc R . . H3B H 0.8523 0.1084 0.6877 0.120 Uiso 1 1 calc R . . H3C H 0.7647 0.1503 0.7267 0.120 Uiso 1 1 calc R . . C4 C 0.7854(5) 0.1902(3) 0.6130(4) 0.0442(13) Uani 1 1 d . . . C5 C 0.9337(6) 0.1927(4) 0.3342(5) 0.0631(18) Uani 1 1 d . . . H5B H 0.9910 0.2267 0.3311 0.095 Uiso 1 1 calc R . . H5C H 0.8826 0.1848 0.2767 0.095 Uiso 1 1 calc R . . H5D H 0.9740 0.1517 0.3567 0.095 Uiso 1 1 calc R . . C6 C 0.8609(5) 0.2162(3) 0.3936(4) 0.0419(12) Uani 1 1 d . . . C7 C 0.7026(6) 0.5049(3) 0.3562(5) 0.0611(17) Uani 1 1 d . . . H7A H 0.7831 0.5084 0.3526 0.092 Uiso 1 1 calc R . . H7B H 0.6840 0.5429 0.3876 0.092 Uiso 1 1 calc R . . H7C H 0.6499 0.5040 0.2983 0.092 Uiso 1 1 calc R . . C8 C 0.6881(5) 0.4409(3) 0.4037(4) 0.0418(12) Uani 1 1 d . . . C9 C 0.4840(7) 0.2763(3) 0.1692(4) 0.0568(16) Uani 1 1 d . . . H9A H 0.4350 0.3147 0.1476 0.085 Uiso 1 1 calc R . . H9B H 0.4442 0.2360 0.1431 0.085 Uiso 1 1 calc R . . H9C H 0.5581 0.2806 0.1544 0.085 Uiso 1 1 calc R . . C10 C 0.5066(5) 0.2723(3) 0.2668(3) 0.0375(11) Uani 1 1 d . . . C11 C 0.9550(6) 0.3633(4) 0.5737(4) 0.0534(15) Uani 1 1 d . . . C20 C 0.2983(4) 0.2648(3) 0.4420(4) 0.0365(11) Uani 1 1 d . . . C21 C 0.3028(5) 0.4449(3) 0.4137(4) 0.0444(13) Uani 1 1 d . . . H21A H 0.3588 0.4772 0.4098 0.053 Uiso 1 1 calc R . . C22 C 0.1868(6) 0.4650(3) 0.4076(4) 0.0538(15) Uani 1 1 d . . . H22A H 0.1659 0.5102 0.3994 0.065 Uiso 1 1 calc R . . C23 C 0.1044(5) 0.4185(3) 0.4135(5) 0.0559(16) Uani 1 1 d . . . H23A H 0.0264 0.4314 0.4084 0.067 Uiso 1 1 calc R . . C24 C 0.1376(5) 0.3512(3) 0.4273(4) 0.0500(15) Uani 1 1 d . . . H24A H 0.0831 0.3186 0.4335 0.060 Uiso 1 1 calc R . . C25 C 0.6192(5) 0.0396(3) 0.3938(3) 0.0416(12) Uani 1 1 d . . . H25A H 0.6979 0.0448 0.3927 0.050 Uiso 1 1 calc R . . C26 C 0.5672(6) -0.0237(3) 0.3784(4) 0.0552(15) Uani 1 1 d . . . H26A H 0.6103 -0.0601 0.3660 0.066 Uiso 1 1 calc R . . C27 C 0.4537(6) -0.0323(3) 0.3817(4) 0.0521(15) Uani 1 1 d . . . H27A H 0.4181 -0.0745 0.3716 0.062 Uiso 1 1 calc R . . C28 C 0.3913(5) 0.0222(3) 0.4001(4) 0.0474(14) Uani 1 1 d . . . H28A H 0.3133 0.0171 0.4030 0.057 Uiso 1 1 calc R . . C29 C 0.4464(5) 0.0846(3) 0.4143(3) 0.0359(11) Uani 1 1 d . . . C30 C 0.3895(5) 0.1462(3) 0.4333(3) 0.0368(11) Uani 1 1 d . . . C31 C 0.2532(5) 0.3339(3) 0.4316(4) 0.0376(11) Uani 1 1 d . . . Cl01 Cl 0.1695(5) 0.3528(4) 0.1793(5) 0.272(3) Uani 1 1 d DU . . Cl02 Cl 0.2224(6) 0.2139(4) 0.2173(4) 0.297(4) Uani 1 1 d DU . . C01 C 0.1315(12) 0.2709(6) 0.1426(10) 0.256(8) Uani 1 1 d DU . . H01A H 0.1434 0.2649 0.0847 0.307 Uiso 1 1 calc R . . H01B H 0.0485 0.2625 0.1389 0.307 Uiso 1 1 calc R . . O01 O 0.980(3) 0.4995(18) 0.065(3) 0.195(17) Uani 0.330(15) 1 d PU A 1 O02 O 0.971(3) 0.5196(13) 0.194(2) 0.075(12) Uani 0.170(15) 1 d PU A 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 0.0301(2) 0.0289(2) 0.0335(2) -0.00316(15) 0.01096(17) -0.00685(15) Ru2 0.0296(2) 0.0290(2) 0.0345(2) -0.00130(15) 0.01000(18) -0.00414(14) Ru3 0.0293(2) 0.0393(2) 0.0399(3) -0.00385(18) 0.00899(18) -0.00958(16) N1 0.035(2) 0.034(2) 0.035(2) -0.0026(17) 0.0099(18) -0.0041(17) N2 0.035(2) 0.040(3) 0.080(4) 0.003(2) 0.021(2) -0.007(2) N3 0.029(2) 0.031(2) 0.038(2) -0.0024(17) 0.0104(17) -0.0055(16) N4 0.032(2) 0.030(2) 0.037(2) -0.0028(17) 0.0108(18) -0.0052(16) N5 0.037(3) 0.037(2) 0.073(4) 0.003(2) 0.010(2) -0.010(2) N6 0.044(2) 0.033(2) 0.029(2) 0.0028(17) 0.0090(18) -0.0024(18) O1 0.0283(17) 0.0322(17) 0.0394(19) -0.0041(15) 0.0106(15) -0.0061(14) O2 0.043(2) 0.0358(19) 0.036(2) -0.0017(16) 0.0112(16) -0.0018(15) O3 0.051(2) 0.0349(19) 0.0325(19) -0.0051(15) 0.0124(16) 0.0008(16) O4 0.043(2) 0.037(2) 0.052(2) 0.0019(17) 0.0173(18) -0.0096(16) O5 0.046(2) 0.045(2) 0.052(2) 0.0031(18) 0.0185(19) -0.0126(18) O6 0.041(2) 0.045(2) 0.036(2) -0.0056(16) 0.0140(17) -0.0056(16) O7 0.045(2) 0.045(2) 0.040(2) -0.0086(17) 0.0112(17) -0.0105(17) O8 0.040(2) 0.044(2) 0.044(2) 0.0035(17) 0.0081(18) -0.0077(16) O9 0.041(2) 0.047(2) 0.050(2) 0.0056(18) -0.0024(18) -0.0067(18) O10 0.035(2) 0.045(2) 0.058(3) -0.0038(18) 0.0196(18) -0.0024(16) O11 0.036(2) 0.053(2) 0.059(3) -0.012(2) 0.0191(18) -0.0109(17) O12 0.056(3) 0.121(5) 0.104(5) -0.025(4) 0.003(3) -0.048(3) C1 0.064(4) 0.050(3) 0.033(3) -0.005(2) 0.015(3) -0.006(3) C2 0.049(3) 0.032(3) 0.034(3) 0.000(2) 0.012(2) -0.008(2) C3 0.091(6) 0.077(5) 0.053(4) 0.019(4) -0.014(4) -0.026(4) C4 0.042(3) 0.047(3) 0.040(3) 0.000(2) 0.004(3) -0.005(2) C5 0.047(4) 0.076(5) 0.075(5) -0.012(4) 0.033(4) -0.002(3) C6 0.033(3) 0.050(3) 0.044(3) 0.000(3) 0.012(2) 0.002(2) C7 0.062(4) 0.059(4) 0.061(4) 0.016(3) 0.014(3) -0.020(3) C8 0.050(3) 0.039(3) 0.036(3) -0.003(2) 0.010(2) -0.017(2) C9 0.083(5) 0.049(3) 0.040(3) 0.006(3) 0.019(3) 0.012(3) C10 0.042(3) 0.037(3) 0.034(3) -0.004(2) 0.010(2) -0.009(2) C11 0.043(3) 0.066(4) 0.053(4) -0.004(3) 0.015(3) -0.011(3) C20 0.033(3) 0.035(3) 0.045(3) -0.001(2) 0.015(2) -0.005(2) C21 0.046(3) 0.033(3) 0.055(3) 0.001(2) 0.014(3) -0.001(2) C22 0.058(4) 0.039(3) 0.064(4) -0.001(3) 0.014(3) 0.007(3) C23 0.041(3) 0.056(4) 0.073(4) -0.007(3) 0.019(3) 0.004(3) C24 0.037(3) 0.045(3) 0.072(4) 0.003(3) 0.021(3) -0.003(2) C25 0.054(3) 0.034(3) 0.038(3) 0.003(2) 0.015(3) 0.003(2) C26 0.076(4) 0.035(3) 0.056(4) 0.002(3) 0.021(3) 0.004(3) C27 0.069(4) 0.028(3) 0.056(4) 0.001(3) 0.011(3) -0.011(3) C28 0.051(3) 0.042(3) 0.046(3) 0.002(2) 0.006(3) -0.014(3) C29 0.038(3) 0.031(3) 0.036(3) 0.005(2) 0.005(2) -0.004(2) C30 0.037(3) 0.035(3) 0.040(3) 0.002(2) 0.012(2) -0.009(2) C31 0.032(3) 0.040(3) 0.043(3) -0.002(2) 0.013(2) -0.005(2) Cl01 0.140(4) 0.384(9) 0.295(8) -0.099(7) 0.064(5) -0.022(5) Cl02 0.254(7) 0.387(8) 0.203(6) 0.005(6) -0.018(5) -0.195(7) C01 0.074(8) 0.428(15) 0.231(17) -0.182(14) -0.022(10) -0.004(13) O01 0.20(2) 0.15(2) 0.22(2) 0.020(16) 0.032(17) 0.034(16) O02 0.079(17) 0.043(14) 0.082(18) 0.021(11) -0.016(12) -0.028(11) _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 N3 1.919(4) . ? Ru1 O1 1.939(3) . ? Ru1 O6 2.037(4) . ? Ru1 O2 2.052(4) . ? Ru1 O4 2.080(4) . ? Ru1 N1 2.109(4) . ? Ru2 N4 1.901(4) . ? Ru2 O1 1.936(3) . ? Ru2 O8 2.052(4) . ? Ru2 O3 2.052(4) . ? Ru2 O10 2.067(4) . ? Ru2 N6 2.097(4) . ? Ru3 C11 1.866(6) . ? Ru3 O1 1.981(3) . ? Ru3 O5 2.078(4) . ? Ru3 O7 2.080(4) . ? Ru3 O11 2.088(4) . ? Ru3 O9 2.100(4) . ? N1 C21 1.336(7) . ? N1 C31 1.359(7) . ? N2 C20 1.313(7) . ? N2 N5 1.382(7) . ? N3 N4 1.350(6) . ? N3 C20 1.360(6) . ? N4 C30 1.368(6) . ? N5 C30 1.313(7) . ? N6 C25 1.337(7) . ? N6 C29 1.351(7) . ? O2 C10 1.255(6) . ? O3 C10 1.277(6) . ? O4 C8 1.255(7) . ? O5 C8 1.264(7) . ? O6 C2 1.277(7) . ? O7 C2 1.247(7) . ? O8 C4 1.266(7) . ? O9 C4 1.246(7) . ? O10 C6 1.276(7) . ? O11 C6 1.248(7) . ? O12 C11 1.123(8) . ? C1 C2 1.498(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C3 C4 1.506(9) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C5 C6 1.501(8) . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C5 H5D 0.9600 . ? C7 C8 1.508(8) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C9 C10 1.500(8) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C20 C31 1.462(7) . ? C21 C22 1.391(8) . ? C21 H21A 0.9300 . ? C22 C23 1.354(9) . ? C22 H22A 0.9300 . ? C23 C24 1.391(9) . ? C23 H23A 0.9300 . ? C24 C31 1.377(8) . ? C24 H24A 0.9300 . ? C25 C26 1.389(8) . ? C25 H25A 0.9300 . ? C26 C27 1.351(9) . ? C26 H26A 0.9300 . ? C27 C28 1.376(9) . ? C27 H27A 0.9300 . ? C28 C29 1.386(7) . ? C28 H28A 0.9300 . ? C29 C30 1.460(8) . ? Cl01 C01 1.742(9) . ? Cl02 C01 1.772(9) . ? C01 H01A 0.9700 . ? C01 H01B 0.9700 . ? 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 N3 Ru1 O1 91.11(15) . . ? N3 Ru1 O6 95.44(16) . . ? O1 Ru1 O6 93.35(15) . . ? N3 Ru1 O2 89.78(16) . . ? O1 Ru1 O2 89.27(15) . . ? O6 Ru1 O2 174.11(14) . . ? N3 Ru1 O4 173.06(17) . . ? O1 Ru1 O4 94.74(15) . . ? O6 Ru1 O4 87.96(15) . . ? O2 Ru1 O4 86.57(15) . . ? N3 Ru1 N1 77.21(17) . . ? O1 Ru1 N1 167.72(15) . . ? O6 Ru1 N1 84.13(16) . . ? O2 Ru1 N1 94.40(16) . . ? O4 Ru1 N1 97.18(16) . . ? N4 Ru2 O1 91.58(15) . . ? N4 Ru2 O8 95.67(17) . . ? O1 Ru2 O8 93.34(15) . . ? N4 Ru2 O3 88.22(17) . . ? O1 Ru2 O3 88.71(14) . . ? O8 Ru2 O3 175.55(15) . . ? N4 Ru2 O10 171.74(17) . . ? O1 Ru2 O10 95.02(15) . . ? O8 Ru2 O10 88.91(17) . . ? O3 Ru2 O10 86.98(16) . . ? N4 Ru2 N6 77.96(17) . . ? O1 Ru2 N6 169.43(15) . . ? O8 Ru2 N6 86.27(15) . . ? O3 Ru2 N6 92.44(15) . . ? O10 Ru2 N6 95.53(16) . . ? C11 Ru3 O1 176.0(2) . . ? C11 Ru3 O5 87.8(2) . . ? O1 Ru3 O5 89.50(15) . . ? C11 Ru3 O7 86.8(2) . . ? O1 Ru3 O7 90.32(14) . . ? O5 Ru3 O7 92.55(16) . . ? C11 Ru3 O11 92.9(2) . . ? O1 Ru3 O11 89.96(14) . . ? O5 Ru3 O11 87.58(17) . . ? O7 Ru3 O11 179.69(16) . . ? C11 Ru3 O9 91.7(2) . . ? O1 Ru3 O9 90.96(15) . . ? O5 Ru3 O9 179.39(16) . . ? O7 Ru3 O9 87.05(17) . . ? O11 Ru3 O9 92.82(17) . . ? C21 N1 C31 118.2(5) . . ? C21 N1 Ru1 127.0(4) . . ? C31 N1 Ru1 114.7(3) . . ? C20 N2 N5 117.6(5) . . ? N4 N3 C20 117.4(4) . . ? N4 N3 Ru1 119.2(3) . . ? C20 N3 Ru1 122.4(3) . . ? N3 N4 C30 117.2(4) . . ? N3 N4 Ru2 119.7(3) . . ? C30 N4 Ru2 121.8(3) . . ? C30 N5 N2 117.7(4) . . ? C25 N6 C29 118.3(5) . . ? C25 N6 Ru2 127.4(4) . . ? C29 N6 Ru2 114.3(3) . . ? Ru2 O1 Ru1 112.88(16) . . ? Ru2 O1 Ru3 122.98(18) . . ? Ru1 O1 Ru3 123.39(17) . . ? C10 O2 Ru1 128.8(3) . . ? C10 O3 Ru2 130.0(3) . . ? C8 O4 Ru1 130.4(4) . . ? C8 O5 Ru3 130.0(3) . . ? C2 O6 Ru1 128.0(3) . . ? C2 O7 Ru3 136.4(3) . . ? C4 O8 Ru2 128.4(4) . . ? C4 O9 Ru3 134.6(4) . . ? C6 O10 Ru2 130.4(4) . . ? C6 O11 Ru3 130.9(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O7 C2 O6 127.2(5) . . ? O7 C2 C1 117.5(5) . . ? O6 C2 C1 115.3(5) . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O9 C4 O8 128.2(5) . . ? O9 C4 C3 116.3(5) . . ? O8 C4 C3 115.5(5) . . ? C6 C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 C5 H5D 109.5 . . ? H5B C5 H5D 109.5 . . ? H5C C5 H5D 109.5 . . ? O11 C6 O10 126.8(5) . . ? O11 C6 C5 117.9(5) . . ? O10 C6 C5 115.3(5) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O4 C8 O5 127.4(5) . . ? O4 C8 C7 115.9(6) . . ? O5 C8 C7 116.7(5) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 O3 127.7(5) . . ? O2 C10 C9 116.9(5) . . ? O3 C10 C9 115.3(5) . . ? O12 C11 Ru3 173.6(7) . . ? N2 C20 N3 124.8(5) . . ? N2 C20 C31 123.1(5) . . ? N3 C20 C31 112.0(4) . . ? N1 C21 C22 121.7(5) . . ? N1 C21 H21A 119.1 . . ? C22 C21 H21A 119.1 . . ? C23 C22 C21 119.8(6) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C22 C23 C24 119.4(6) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C31 C24 C23 118.4(5) . . ? C31 C24 H24A 120.8 . . ? C23 C24 H24A 120.8 . . ? N6 C25 C26 121.9(6) . . ? N6 C25 H25A 119.0 . . ? C26 C25 H25A 119.0 . . ? C27 C26 C25 119.6(6) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 119.4(5) . . ? C26 C27 H27A 120.3 . . ? C28 C27 H27A 120.3 . . ? C27 C28 C29 119.1(6) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? N6 C29 C28 121.7(5) . . ? N6 C29 C30 114.0(4) . . ? C28 C29 C30 124.3(5) . . ? N5 C30 N4 124.5(5) . . ? N5 C30 C29 123.6(5) . . ? N4 C30 C29 111.9(4) . . ? N1 C31 C24 122.4(5) . . ? N1 C31 C20 113.6(4) . . ? C24 C31 C20 123.9(5) . . ? Cl01 C01 Cl02 108.5(6) . . ? Cl01 C01 H01A 110.0 . . ? Cl02 C01 H01A 110.0 . . ? Cl01 C01 H01B 110.0 . . ? Cl02 C01 H01B 110.0 . . ? H01A C01 H01B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.157 _refine_diff_density_min -1.199 _refine_diff_density_rms 0.125