# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name ? _publ_contact_author_name 'Dr Victorio Cadierno' _publ_contact_author_email VCM@UNIOVI.ES _publ_section_title ; Novel ruthenium(II) complexes containing the N-phosphorylated iminophosphorane-phosphine ligand Ph2PCH2P{=NP(=O)(OEt)2}Ph2: A new coordination mode of its methanide anion ; # Attachment '6_8a_9a.cif' #=============================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 690029' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H51 N2 O3 P3 Ru, 0.5(C6 H14), 2(F6 Sb)' _chemical_formula_sum 'C47 H58 F12 N2 O3 P3 Ru Sb2' _chemical_formula_weight 1364.43 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 '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/a' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 22.1651(10) _cell_length_b 11.7056(4) _cell_length_c 21.9561(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.646(2) _cell_angle_gamma 90.00 _cell_volume 5397.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2708 _exptl_absorpt_coefficient_mu 11.682 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2540 _exptl_absorpt_correction_T_max 0.7270 _exptl_absorpt_process_details 'SADABS (Sheldrick,G.M.,1997-2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20594 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 71.24 _reflns_number_total 8523 _reflns_number_gt 5648 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0767P)^2^+57.7166P] 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 8523 _refine_ls_number_parameters 654 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1231 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2137 _refine_ls_wR_factor_gt 0.1943 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.048 _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 C1 C 0.2127(5) -0.0001(9) 0.3102(6) 0.042(3) Uani 1 1 d . . . C2 C 0.1806(6) -0.0529(11) 0.2528(6) 0.050(3) Uani 1 1 d . . . H2 H 0.1439 -0.0206 0.2247 0.060 Uiso 1 1 calc R . . C3 C 0.2042(6) -0.1556(12) 0.2376(7) 0.062(4) Uani 1 1 d . . . H3 H 0.1825 -0.1918 0.1991 0.074 Uiso 1 1 calc R . . C4 C 0.2591(6) -0.2055(12) 0.2782(7) 0.058(4) Uani 1 1 d . . . H4 H 0.2742 -0.2738 0.2669 0.070 Uiso 1 1 calc R . . C5 C 0.2914(6) -0.1515(10) 0.3361(7) 0.052(3) Uani 1 1 d . . . H5 H 0.3283 -0.1837 0.3639 0.062 Uiso 1 1 calc R . . C6 C 0.2683(5) -0.0507(10) 0.3520(6) 0.045(3) Uani 1 1 d . . . H6 H 0.2897 -0.0153 0.3908 0.054 Uiso 1 1 calc R . . C7 C 0.2014(5) 0.1285(10) 0.4161(6) 0.043(3) Uani 1 1 d . . . C8 C 0.1864(5) 0.0308(11) 0.4426(6) 0.045(3) Uani 1 1 d . . . H8 H 0.1720 -0.0329 0.4167 0.054 Uiso 1 1 calc R . . C9 C 0.1923(5) 0.0256(12) 0.5069(6) 0.052(3) Uani 1 1 d . . . H9 H 0.1817 -0.0404 0.5248 0.062 Uiso 1 1 calc R . . C10 C 0.2146(7) 0.1216(13) 0.5442(6) 0.061(4) Uani 1 1 d . . . H10 H 0.2182 0.1205 0.5876 0.074 Uiso 1 1 calc R . . C11 C 0.2313(7) 0.2180(12) 0.5183(7) 0.060(4) Uani 1 1 d . . . H11 H 0.2477 0.2804 0.5446 0.072 Uiso 1 1 calc R . . C12 C 0.2243(5) 0.2233(10) 0.4545(6) 0.045(3) Uani 1 1 d . . . H12 H 0.2347 0.2897 0.4368 0.054 Uiso 1 1 calc R . . C13 C 0.2486(5) 0.2387(9) 0.3250(6) 0.041(3) Uani 1 1 d . . . H13A H 0.2326 0.3158 0.3253 0.049 Uiso 1 1 calc R . . H13B H 0.2845 0.2297 0.3639 0.049 Uiso 1 1 calc R . . C14 C 0.3375(5) 0.1176(11) 0.2729(7) 0.049(3) Uani 1 1 d . . . C15 C 0.3365(6) 0.0378(11) 0.2258(7) 0.054(4) Uani 1 1 d . . . H15 H 0.3033 0.0392 0.1870 0.065 Uiso 1 1 calc R . . C16 C 0.3836(7) -0.0436(12) 0.2353(8) 0.066(4) Uani 1 1 d . . . H16 H 0.3837 -0.0933 0.2023 0.080 Uiso 1 1 calc R . . C17 C 0.4303(7) -0.0507(12) 0.2939(9) 0.070(4) Uani 1 1 d . . . H17 H 0.4601 -0.1093 0.3012 0.084 Uiso 1 1 calc R . . C18 C 0.4342(6) 0.0272(12) 0.3423(7) 0.057(4) Uani 1 1 d . . . H18 H 0.4674 0.0242 0.3810 0.068 Uiso 1 1 calc R . . C19 C 0.3863(5) 0.1114(11) 0.3316(7) 0.053(4) Uani 1 1 d . . . H19 H 0.3874 0.1632 0.3640 0.063 Uiso 1 1 calc R . . C20 C 0.3162(6) 0.3631(12) 0.2570(8) 0.057(4) Uani 1 1 d . . . C21 C 0.3204(7) 0.4021(13) 0.1998(10) 0.078(5) Uani 1 1 d . . . H21 H 0.3037 0.3593 0.1625 0.093 Uiso 1 1 calc R . . C22 C 0.3502(8) 0.5070(16) 0.1977(11) 0.089(6) Uani 1 1 d . . . H22 H 0.3523 0.5345 0.1586 0.107 Uiso 1 1 calc R . . C23 C 0.3764(7) 0.5699(15) 0.2529(14) 0.102(8) Uani 1 1 d . . . H23 H 0.3968 0.6388 0.2515 0.122 Uiso 1 1 calc R . . C24 C 0.3721(7) 0.5314(14) 0.3072(11) 0.087(6) Uani 1 1 d . . . H24 H 0.3889 0.5750 0.3441 0.104 Uiso 1 1 calc R . . C25 C 0.3434(6) 0.4272(12) 0.3118(9) 0.072(5) Uani 1 1 d . . . H25 H 0.3425 0.4010 0.3515 0.086 Uiso 1 1 calc R . . C26 C 0.1270(13) 0.114(2) 0.0658(12) 0.137(9) Uani 1 1 d U . . H26A H 0.1117 0.1631 0.0284 0.164 Uiso 1 1 calc R . . H26B H 0.1729 0.1082 0.0772 0.164 Uiso 1 1 calc R . . C27 C 0.103(2) 0.020(2) 0.0538(16) 0.277(19) Uani 1 1 d U . . H27A H 0.1132 -0.0119 0.0180 0.415 Uiso 1 1 calc R . . H27B H 0.0577 0.0267 0.0432 0.415 Uiso 1 1 calc R . . H27C H 0.1193 -0.0284 0.0906 0.415 Uiso 1 1 calc R . . C28 C 0.1024(9) 0.427(2) 0.0856(12) 0.114(7) Uani 1 1 d . . . H28A H 0.0716 0.3817 0.0534 0.137 Uiso 1 1 calc R . . H28B H 0.0826 0.4523 0.1168 0.137 Uiso 1 1 calc R . . C29 C 0.1181(15) 0.515(3) 0.0586(14) 0.216(19) Uani 1 1 d . . . H29C H 0.0808 0.5593 0.0377 0.324 Uiso 1 1 calc R . . H29A H 0.1374 0.4902 0.0275 0.324 Uiso 1 1 calc R . . H29B H 0.1478 0.5609 0.0906 0.324 Uiso 1 1 calc R . . C30 C 0.1135(6) 0.4590(12) 0.2933(7) 0.061(4) Uani 1 1 d . . . H30 H 0.1142 0.4561 0.2512 0.073 Uiso 1 1 calc R . . C31 C 0.1204(7) 0.5634(13) 0.3247(11) 0.083(6) Uani 1 1 d . . . H31 H 0.1237 0.6295 0.3025 0.099 Uiso 1 1 calc R . . C32 C 0.1223(7) 0.5710(15) 0.3858(10) 0.081(5) Uani 1 1 d . . . H32 H 0.1298 0.6404 0.4076 0.097 Uiso 1 1 calc R . . C33 C 0.1128(6) 0.4713(14) 0.4157(9) 0.075(5) Uani 1 1 d . . . H33 H 0.1120 0.4729 0.4578 0.089 Uiso 1 1 calc R . . C34 C 0.1044(5) 0.3687(12) 0.3818(7) 0.054(4) Uani 1 1 d . . . H34 H 0.0974 0.3025 0.4020 0.065 Uiso 1 1 calc R . . C35 C 0.0222(5) 0.0889(11) 0.3123(6) 0.045(3) Uani 1 1 d . . . C36 C 0.0341(5) 0.0348(10) 0.2597(7) 0.050(4) Uani 1 1 d . . . H36 H 0.0534 -0.0367 0.2650 0.060 Uiso 1 1 calc R . . C37 C 0.0168(5) 0.0888(10) 0.1992(6) 0.047(3) Uani 1 1 d . . . H37 H 0.0255 0.0532 0.1651 0.057 Uiso 1 1 calc R . . C38 C -0.0140(6) 0.1971(11) 0.1896(6) 0.048(3) Uani 1 1 d . . . C39 C -0.0245(5) 0.2527(10) 0.2415(6) 0.043(3) Uani 1 1 d . . . H39 H -0.0436 0.3244 0.2363 0.052 Uiso 1 1 calc R . . C40 C -0.0057(5) 0.1982(11) 0.3024(6) 0.044(3) Uani 1 1 d . . . H40 H -0.0120 0.2361 0.3371 0.053 Uiso 1 1 calc R . . C41 C 0.0351(7) 0.0311(14) 0.3752(7) 0.080(5) Uani 1 1 d . . . H41B H 0.0540 -0.0422 0.3737 0.120 Uiso 1 1 calc R . . H41A H -0.0041 0.0211 0.3844 0.120 Uiso 1 1 calc R . . H41C H 0.0638 0.0768 0.4082 0.120 Uiso 1 1 calc R . . C42 C -0.0337(7) 0.2518(12) 0.1227(7) 0.066(4) Uani 1 1 d . . . H42 H 0.0018 0.2421 0.1056 0.079 Uiso 1 1 calc R . . C43 C -0.0893(7) 0.1854(16) 0.0803(7) 0.090(6) Uani 1 1 d . . . H43B H -0.0783 0.1060 0.0815 0.135 Uiso 1 1 calc R . . H43C H -0.0999 0.2131 0.0370 0.135 Uiso 1 1 calc R . . H43A H -0.1252 0.1949 0.0953 0.135 Uiso 1 1 calc R . . C44 C -0.0475(8) 0.3765(13) 0.1226(7) 0.085(5) Uani 1 1 d . . . H44B H -0.0108 0.4157 0.1499 0.127 Uiso 1 1 calc R . . H44A H -0.0829 0.3886 0.1381 0.127 Uiso 1 1 calc R . . H44C H -0.0578 0.4056 0.0795 0.127 Uiso 1 1 calc R . . N1 N 0.2249(5) 0.1975(9) 0.1915(5) 0.057(3) Uani 1 1 d . . . N2 N 0.1059(4) 0.3614(8) 0.3229(5) 0.045(3) Uani 1 1 d . . . O1 O 0.1222(4) 0.2860(8) 0.2092(4) 0.055(2) Uani 1 1 d . . . O2 O 0.1623(5) 0.3522(10) 0.1199(5) 0.086(4) Uani 1 1 d . . . O3 O 0.1104(5) 0.1616(10) 0.1179(5) 0.080(3) Uani 1 1 d . . . P3 P 0.15542(16) 0.2488(3) 0.16300(18) 0.0591(10) Uani 1 1 d . . . P2 P 0.27799(15) 0.2271(3) 0.25750(17) 0.0486(8) Uani 1 1 d . . . P1 P 0.18506(13) 0.1381(2) 0.32984(15) 0.0387(7) Uani 1 1 d . . . Ru1 Ru 0.08046(4) 0.20581(8) 0.27137(5) 0.0403(3) Uani 1 1 d . . . F12 F 1.0021(5) 0.7288(8) 0.0508(4) 0.093(3) Uani 1 1 d . . . F11 F 0.9347(4) 0.8680(7) 0.1009(4) 0.076(2) Uani 1 1 d . . . F8 F 0.9847(5) 0.7678(8) 0.2120(4) 0.090(3) Uani 1 1 d . . . F10 F 0.9254(5) 0.6438(8) 0.1091(5) 0.103(3) Uani 1 1 d . . . F7 F 1.0531(4) 0.6304(7) 0.1646(4) 0.085(3) Uani 1 1 d . . . F9 F 1.0601(4) 0.8543(7) 0.1520(4) 0.080(3) Uani 1 1 d . . . F2 F 0.0851(9) 0.7971(12) 0.4400(10) 0.195(8) Uani 1 1 d . . . F3 F 0.0707(14) 0.6261(12) 0.5080(11) 0.283(15) Uani 1 1 d . . . F4 F -0.0046(6) 0.7306(11) 0.5514(5) 0.126(4) Uani 1 1 d . . . F5 F -0.0265(10) 0.8802(14) 0.4632(8) 0.206(8) Uani 1 1 d . . . F6 F 0.0910(11) 0.831(3) 0.5458(14) 0.373(18) Uani 1 1 d . . . Sb1 Sb 0.9894(4) 0.7465(6) 0.1378(4) 0.0348(12) Uani 0.50 1 d P A 1 Sb2 Sb 0.04331(10) 0.7592(3) 0.49391(17) 0.0519(7) Uani 0.50 1 d P B 1 F1 F 0.0013(17) 0.683(4) 0.420(2) 0.23(2) Uani 0.50 1 d P B 1 Sb2A Sb 0.01178(19) 0.7583(3) 0.48228(17) 0.0790(10) Uani 0.50 1 d P B 2 F1A F -0.057(3) 0.704(5) 0.437(2) 0.40(5) Uani 0.50 1 d P B 2 Sb1A Sb 0.9983(4) 0.7482(7) 0.1248(4) 0.049(2) Uani 0.50 1 d P A 2 C47 C 0.2587(15) 0.534(2) 0.0231(13) 0.078(9) Uiso 0.50 1 d PD C -1 H47A H 0.3047 0.5298 0.0365 0.094 Uiso 0.50 1 calc PR C -1 H47B H 0.2436 0.5006 0.0560 0.094 Uiso 0.50 1 calc PR C -1 C48 C 0.2286(17) 0.479(3) -0.0413(14) 0.089(10) Uiso 0.50 1 d PD C -1 H48A H 0.2490 0.4991 -0.0728 0.107 Uiso 0.50 1 calc PR C -1 H48B H 0.1830 0.4907 -0.0584 0.107 Uiso 0.50 1 calc PR C -1 C51 C 0.242(2) 0.271(4) -0.1106(19) 0.141(13) Uiso 0.50 1 d PD C -1 H51A H 0.2407 0.2009 -0.1333 0.211 Uiso 0.50 1 calc PR C -1 H51B H 0.2828 0.3065 -0.1024 0.211 Uiso 0.50 1 calc PR C -1 H51C H 0.2095 0.3218 -0.1362 0.211 Uiso 0.50 1 calc PR C -1 C49 C 0.247(3) 0.361(3) -0.0129(19) 0.19(2) Uiso 0.50 1 d PD C -1 H49A H 0.2292 0.3549 0.0224 0.223 Uiso 0.50 1 calc PR C -1 H49B H 0.2925 0.3615 0.0064 0.223 Uiso 0.50 1 calc PR C -1 C50 C 0.231(3) 0.249(3) -0.049(2) 0.141(13) Uiso 0.50 1 d PD C -1 H50A H 0.2578 0.1875 -0.0260 0.169 Uiso 0.50 1 calc PR C -1 H50B H 0.1865 0.2276 -0.0564 0.169 Uiso 0.50 1 calc PR C -1 C46 C 0.236(2) 0.656(3) 0.009(2) 0.118(14) Uiso 0.50 1 d PD C -1 H46A H 0.2045 0.6597 -0.0334 0.178 Uiso 0.50 1 calc PR C -1 H46B H 0.2710 0.7046 0.0100 0.178 Uiso 0.50 1 calc PR C -1 H46C H 0.2168 0.6814 0.0400 0.178 Uiso 0.50 1 calc PR C -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(5) 0.039(7) 0.054(8) -0.006(5) 0.017(6) 0.006(5) C2 0.043(6) 0.054(8) 0.058(8) -0.007(6) 0.021(6) -0.004(6) C3 0.060(8) 0.064(9) 0.061(9) -0.022(7) 0.019(7) 0.010(7) C4 0.064(8) 0.058(8) 0.067(9) -0.002(7) 0.043(8) 0.020(7) C5 0.051(7) 0.048(7) 0.064(9) 0.009(6) 0.029(7) 0.015(6) C6 0.041(6) 0.051(7) 0.049(8) 0.004(6) 0.022(6) 0.004(5) C7 0.039(6) 0.045(7) 0.045(7) 0.002(5) 0.014(6) 0.005(5) C8 0.029(5) 0.060(8) 0.044(8) 0.003(6) 0.009(5) 0.007(5) C9 0.034(6) 0.072(9) 0.048(9) 0.011(7) 0.010(6) 0.005(6) C10 0.066(9) 0.093(12) 0.027(7) -0.006(7) 0.017(7) 0.009(8) C11 0.078(9) 0.054(9) 0.048(9) -0.009(6) 0.019(7) 0.002(7) C12 0.041(6) 0.043(7) 0.051(8) -0.004(5) 0.013(6) 0.001(5) C13 0.030(5) 0.045(7) 0.054(8) 0.000(5) 0.022(5) 0.004(5) C14 0.030(6) 0.049(7) 0.074(10) 0.005(6) 0.025(6) 0.009(5) C15 0.037(6) 0.064(9) 0.075(10) -0.003(7) 0.038(7) 0.002(6) C16 0.057(8) 0.061(9) 0.090(12) -0.004(8) 0.036(9) -0.004(7) C17 0.052(8) 0.055(9) 0.113(14) 0.014(9) 0.040(9) 0.009(7) C18 0.041(7) 0.061(9) 0.074(10) 0.012(7) 0.026(7) -0.002(6) C19 0.034(6) 0.049(7) 0.082(10) 0.002(7) 0.029(7) 0.003(5) C20 0.034(6) 0.064(9) 0.088(11) 0.008(8) 0.040(7) -0.001(6) C21 0.061(9) 0.056(9) 0.128(15) 0.030(10) 0.046(10) 0.014(7) C22 0.062(10) 0.082(13) 0.150(19) 0.050(12) 0.070(12) 0.026(9) C23 0.045(8) 0.053(11) 0.22(3) 0.025(14) 0.052(13) 0.004(7) C24 0.050(9) 0.057(10) 0.16(2) -0.001(11) 0.044(11) -0.002(7) C25 0.046(7) 0.056(9) 0.128(15) -0.008(9) 0.050(9) -0.008(6) C26 0.17(2) 0.119(17) 0.133(19) -0.026(17) 0.071(19) 0.032(16) C27 0.61(6) 0.12(2) 0.23(3) -0.05(2) 0.33(4) -0.08(3) C28 0.089(14) 0.14(2) 0.132(19) 0.042(16) 0.069(14) 0.027(13) C29 0.24(4) 0.28(4) 0.18(3) 0.14(3) 0.13(3) 0.19(3) C30 0.052(7) 0.056(9) 0.074(10) 0.001(7) 0.019(7) 0.002(6) C31 0.050(8) 0.048(9) 0.144(18) -0.004(10) 0.022(10) -0.005(6) C32 0.062(9) 0.069(11) 0.106(15) -0.034(10) 0.019(10) -0.012(8) C33 0.049(8) 0.081(12) 0.095(13) -0.020(10) 0.023(8) -0.002(7) C34 0.034(6) 0.064(9) 0.060(10) 0.006(7) 0.009(6) 0.001(6) C35 0.023(5) 0.058(8) 0.056(8) 0.019(6) 0.018(6) -0.005(5) C36 0.036(6) 0.035(7) 0.077(10) 0.002(6) 0.013(7) -0.004(5) C37 0.032(6) 0.054(8) 0.054(8) -0.007(6) 0.010(6) -0.007(5) C38 0.048(7) 0.052(7) 0.041(7) 0.010(6) 0.011(6) -0.001(6) C39 0.027(5) 0.049(7) 0.055(8) 0.007(6) 0.013(5) 0.012(5) C40 0.023(5) 0.067(8) 0.046(7) 0.005(6) 0.017(5) -0.005(5) C41 0.056(8) 0.092(12) 0.086(12) 0.040(9) 0.014(8) -0.011(8) C42 0.058(8) 0.078(10) 0.052(9) 0.005(7) 0.005(7) -0.009(7) C43 0.076(10) 0.140(16) 0.039(9) 0.019(9) -0.003(8) -0.043(10) C44 0.096(12) 0.086(12) 0.060(10) 0.033(9) 0.008(9) 0.021(9) N1 0.066(7) 0.060(7) 0.050(7) 0.012(5) 0.024(6) 0.013(6) N2 0.029(4) 0.041(6) 0.060(7) 0.000(5) 0.008(5) -0.001(4) O1 0.045(4) 0.071(6) 0.052(5) 0.003(4) 0.021(4) 0.006(4) O2 0.065(6) 0.124(9) 0.070(7) 0.051(7) 0.024(6) 0.012(6) O3 0.077(7) 0.120(9) 0.042(6) -0.007(6) 0.019(5) -0.010(6) P3 0.0455(17) 0.083(3) 0.050(2) 0.0145(19) 0.0178(17) 0.0023(17) P2 0.0399(15) 0.052(2) 0.060(2) 0.0030(15) 0.0254(16) 0.0024(13) P1 0.0314(13) 0.0436(17) 0.0417(18) 0.0016(13) 0.0126(13) 0.0036(12) Ru1 0.0305(4) 0.0437(5) 0.0463(6) 0.0063(4) 0.0117(4) 0.0025(4) F12 0.127(8) 0.082(6) 0.063(6) -0.003(5) 0.019(6) 0.016(5) F11 0.071(5) 0.077(6) 0.076(6) 0.007(4) 0.020(5) 0.003(4) F8 0.131(8) 0.087(7) 0.066(6) 0.009(5) 0.051(6) -0.001(6) F10 0.103(7) 0.077(6) 0.122(8) -0.007(6) 0.026(6) -0.034(5) F7 0.102(7) 0.077(6) 0.064(5) 0.000(4) 0.012(5) 0.017(5) F9 0.059(5) 0.071(5) 0.104(7) -0.017(5) 0.018(5) -0.020(4) F2 0.239(19) 0.114(10) 0.29(2) 0.077(12) 0.163(17) 0.045(11) F3 0.61(4) 0.107(11) 0.31(2) 0.086(13) 0.39(3) 0.123(17) F4 0.110(8) 0.210(13) 0.081(7) 0.053(8) 0.062(7) 0.032(8) F5 0.33(2) 0.180(15) 0.178(14) 0.088(12) 0.176(17) 0.056(15) F6 0.25(2) 0.47(4) 0.43(4) -0.10(3) 0.15(2) -0.30(3) Sb1 0.0463(13) 0.0383(13) 0.035(3) 0.0000(14) 0.0338(16) -0.0026(10) Sb2 0.0444(10) 0.0583(13) 0.0539(16) -0.0088(9) 0.0169(11) -0.0113(11) F1 0.14(3) 0.34(5) 0.21(4) -0.22(4) 0.05(3) -0.01(3) Sb2A 0.145(3) 0.0467(13) 0.059(2) -0.0005(12) 0.052(2) 0.001(2) F1A 0.34(7) 0.47(8) 0.18(4) -0.17(5) -0.19(4) 0.14(6) Sb1A 0.067(3) 0.0563(16) 0.028(3) -0.0015(15) 0.020(2) -0.0230(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.380(16) . ? C1 C6 1.409(15) . ? C1 P1 1.830(11) . ? C2 C3 1.393(17) . ? C2 H2 0.9300 . ? C3 C4 1.387(17) . ? C3 H3 0.9300 . ? C4 C5 1.396(18) . ? C4 H4 0.9300 . ? C5 C6 1.375(16) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.371(16) . ? C7 C12 1.389(15) . ? C7 P1 1.814(13) . ? C8 C9 1.378(18) . ? C8 H8 0.9300 . ? C9 C10 1.385(18) . ? C9 H9 0.9300 . ? C10 C11 1.367(19) . ? C10 H10 0.9300 . ? C11 C12 1.361(18) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 P2 1.805(13) . ? C13 P1 1.865(11) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.389(18) . ? C14 C19 1.395(17) . ? C14 P2 1.792(11) . ? C15 C16 1.379(18) . ? C15 H15 0.9300 . ? C16 C17 1.37(2) . ? C16 H16 0.9300 . ? C17 C18 1.38(2) . ? C17 H17 0.9300 . ? C18 C19 1.411(17) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.37(2) . ? C20 C25 1.38(2) . ? C20 P2 1.805(14) . ? C21 C22 1.40(2) . ? C21 H21 0.9300 . ? C22 C23 1.38(3) . ? C22 H22 0.9300 . ? C23 C24 1.31(3) . ? C23 H23 0.9300 . ? C24 C25 1.39(2) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.21(3) . ? C26 O3 1.42(2) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.29(3) . ? C28 O2 1.57(2) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C30 N2 1.351(16) . ? C30 C31 1.39(2) . ? C30 H30 0.9300 . ? C31 C32 1.33(2) . ? C31 H31 0.9300 . ? C32 C33 1.39(2) . ? C32 H32 0.9300 . ? C33 C34 1.394(19) . ? C33 H33 0.9300 . ? C34 N2 1.308(17) . ? C34 H34 0.9300 . ? C35 C40 1.407(17) . ? C35 C36 1.415(18) . ? C35 C41 1.480(18) . ? C35 Ru1 2.257(11) . ? C36 C37 1.408(17) . ? C36 Ru1 2.228(11) . ? C36 H36 0.9300 . ? C37 C38 1.423(17) . ? C37 Ru1 2.225(11) . ? C37 H37 0.9300 . ? C38 C39 1.394(17) . ? C38 C42 1.532(18) . ? C38 Ru1 2.283(11) . ? C39 C40 1.419(16) . ? C39 Ru1 2.273(10) . ? C39 H39 0.9300 . ? C40 Ru1 2.225(11) . ? C40 H40 0.9300 . ? C41 H41B 0.9600 . ? C41 H41A 0.9600 . ? C41 H41C 0.9600 . ? C42 C44 1.49(2) . ? C42 C43 1.502(17) . ? C42 H42 0.9800 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C43 H43A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44A 0.9600 . ? C44 H44C 0.9600 . ? N1 P3 1.583(11) . ? N1 P2 1.585(11) . ? N2 Ru1 2.123(10) . ? O1 P3 1.496(10) . ? O1 Ru1 2.099(9) . ? O2 P3 1.573(10) . ? O3 P3 1.545(11) . ? P1 Ru1 2.398(3) . ? F12 Sb1A 1.669(12) . ? F12 Sb1 2.030(12) . ? F11 Sb1 1.877(11) . ? F11 Sb1A 1.939(11) . ? F8 Sb1 1.682(12) . ? F8 Sb1A 2.043(12) . ? F10 Sb1 1.812(12) . ? F10 Sb1A 1.968(12) . ? F7 Sb1A 1.860(11) . ? F7 Sb1 1.912(11) . ? F9 Sb1A 1.803(11) . ? F9 Sb1 1.959(11) . ? F2 Sb2 1.777(17) . ? F2 Sb2A 2.162(16) . ? F3 Sb2 1.665(14) . ? F3 Sb2A 1.987(18) . ? F4 Sb2A 1.702(11) . ? F4 Sb2 1.922(11) . ? F5 Sb2A 1.644(16) . ? F5 Sb2 2.046(17) . ? F6 Sb2 1.53(2) . ? F6 Sb2A 2.05(2) . ? Sb2 F1 1.83(3) . ? Sb2A F1A 1.67(5) . ? C47 C48 1.505(19) . ? C47 C46 1.513(19) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.51(2) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C51 C50 1.47(2) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C49 C50 1.52(2) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.7(11) . . ? C2 C1 P1 119.9(9) . . ? C6 C1 P1 120.4(9) . . ? C1 C2 C3 118.8(11) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 122.0(12) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 118.9(12) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 119.7(11) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 120.9(12) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C8 C7 C12 120.0(12) . . ? C8 C7 P1 120.0(9) . . ? C12 C7 P1 119.8(10) . . ? C7 C8 C9 121.0(12) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C10 118.0(13) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? C11 C10 C9 121.1(13) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 120.6(13) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C7 119.2(12) . . ? C11 C12 H12 120.4 . . ? C7 C12 H12 120.4 . . ? P2 C13 P1 118.5(6) . . ? P2 C13 H13A 107.7 . . ? P1 C13 H13A 107.7 . . ? P2 C13 H13B 107.7 . . ? P1 C13 H13B 107.7 . . ? H13A C13 H13B 107.1 . . ? C15 C14 C19 118.4(11) . . ? C15 C14 P2 120.4(9) . . ? C19 C14 P2 121.2(10) . . ? C16 C15 C14 121.4(13) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C15 119.4(15) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 121.6(13) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C18 C19 118.3(13) . . ? C17 C18 H18 120.9 . . ? C19 C18 H18 120.9 . . ? C14 C19 C18 120.7(13) . . ? C14 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C25 118.7(14) . . ? C21 C20 P2 118.0(12) . . ? C25 C20 P2 123.3(12) . . ? C20 C21 C22 119.6(19) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.6(19) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 119.1(18) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 122(2) . . ? C23 C24 H24 118.8 . . ? C25 C24 H24 118.8 . . ? C20 C25 C24 119.5(18) . . ? C20 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C27 C26 O3 109(3) . . ? C27 C26 H26A 109.9 . . ? O3 C26 H26A 109.9 . . ? C27 C26 H26B 109.9 . . ? O3 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? 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 . . ? C29 C28 O2 110.8(19) . . ? C29 C28 H28A 109.5 . . ? O2 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? O2 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C28 C29 H29C 109.5 . . ? C28 C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29C C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N2 C30 C31 121.1(16) . . ? N2 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C32 C31 C30 121.5(17) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C31 C32 C33 117.4(16) . . ? C31 C32 H32 121.3 . . ? C33 C32 H32 121.3 . . ? C32 C33 C34 119.1(17) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? N2 C34 C33 122.9(14) . . ? N2 C34 H34 118.5 . . ? C33 C34 H34 118.5 . . ? C40 C35 C36 117.9(11) . . ? C40 C35 C41 120.3(14) . . ? C36 C35 C41 121.7(12) . . ? C40 C35 Ru1 70.5(6) . . ? C36 C35 Ru1 70.5(7) . . ? C41 C35 Ru1 133.1(8) . . ? C37 C36 C35 120.2(11) . . ? C37 C36 Ru1 71.5(7) . . ? C35 C36 Ru1 72.7(7) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? Ru1 C36 H36 128.1 . . ? C36 C37 C38 120.9(12) . . ? C36 C37 Ru1 71.7(6) . . ? C38 C37 Ru1 73.8(7) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? Ru1 C37 H37 126.9 . . ? C39 C38 C37 119.5(11) . . ? C39 C38 C42 121.2(12) . . ? C37 C38 C42 119.4(13) . . ? C39 C38 Ru1 71.8(6) . . ? C37 C38 Ru1 69.4(6) . . ? C42 C38 Ru1 130.0(9) . . ? C38 C39 C40 119.0(11) . . ? C38 C39 Ru1 72.6(6) . . ? C40 C39 Ru1 69.8(6) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? Ru1 C39 H39 129.5 . . ? C35 C40 C39 122.5(12) . . ? C35 C40 Ru1 72.9(7) . . ? C39 C40 Ru1 73.5(7) . . ? C35 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? Ru1 C40 H40 126.9 . . ? C35 C41 H41B 109.5 . . ? C35 C41 H41A 109.5 . . ? H41B C41 H41A 109.5 . . ? C35 C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? C44 C42 C43 112.2(13) . . ? C44 C42 C38 114.0(13) . . ? C43 C42 C38 107.7(12) . . ? C44 C42 H42 107.6 . . ? C43 C42 H42 107.6 . . ? C38 C42 H42 107.6 . . ? C42 C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C43 H43A 109.5 . . ? H43B C43 H43A 109.5 . . ? H43C C43 H43A 109.5 . . ? C42 C44 H44B 109.5 . . ? C42 C44 H44A 109.5 . . ? H44B C44 H44A 109.5 . . ? C42 C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? P3 N1 P2 128.5(8) . . ? C34 N2 C30 117.8(12) . . ? C34 N2 Ru1 119.8(9) . . ? C30 N2 Ru1 121.5(10) . . ? P3 O1 Ru1 136.5(6) . . ? C28 O2 P3 119.3(10) . . ? C26 O3 P3 119.6(14) . . ? O1 P3 O3 105.7(6) . . ? O1 P3 O2 110.3(6) . . ? O3 P3 O2 106.9(6) . . ? O1 P3 N1 118.0(5) . . ? O3 P3 N1 110.5(6) . . ? O2 P3 N1 105.1(6) . . ? N1 P2 C14 107.6(6) . . ? N1 P2 C13 114.2(6) . . ? C14 P2 C13 109.7(6) . . ? N1 P2 C20 113.6(7) . . ? C14 P2 C20 108.2(6) . . ? C13 P2 C20 103.4(6) . . ? C7 P1 C1 102.8(6) . . ? C7 P1 C13 101.3(5) . . ? C1 P1 C13 103.2(5) . . ? C7 P1 Ru1 114.5(4) . . ? C1 P1 Ru1 120.4(4) . . ? C13 P1 Ru1 112.3(4) . . ? O1 Ru1 N2 82.3(4) . . ? O1 Ru1 C37 97.1(4) . . ? N2 Ru1 C37 155.2(4) . . ? O1 Ru1 C40 144.8(4) . . ? N2 Ru1 C40 88.8(4) . . ? C37 Ru1 C40 77.4(5) . . ? O1 Ru1 C36 127.6(5) . . ? N2 Ru1 C36 150.1(5) . . ? C37 Ru1 C36 36.9(5) . . ? C40 Ru1 C36 65.8(5) . . ? O1 Ru1 C35 163.2(4) . . ? N2 Ru1 C35 113.4(5) . . ? C37 Ru1 C35 66.2(5) . . ? C40 Ru1 C35 36.6(4) . . ? C36 Ru1 C35 36.8(5) . . ? O1 Ru1 C39 109.1(4) . . ? N2 Ru1 C39 91.1(4) . . ? C37 Ru1 C39 65.5(4) . . ? C40 Ru1 C39 36.8(4) . . ? C36 Ru1 C39 78.0(4) . . ? C35 Ru1 C39 66.3(4) . . ? O1 Ru1 C38 89.6(4) . . ? N2 Ru1 C38 118.6(4) . . ? C37 Ru1 C38 36.8(4) . . ? C40 Ru1 C38 65.0(4) . . ? C36 Ru1 C38 66.2(4) . . ? C35 Ru1 C38 77.8(4) . . ? C39 Ru1 C38 35.6(4) . . ? O1 Ru1 P1 86.8(2) . . ? N2 Ru1 P1 87.2(2) . . ? C37 Ru1 P1 117.6(3) . . ? C40 Ru1 P1 126.9(3) . . ? C36 Ru1 P1 95.5(3) . . ? C35 Ru1 P1 99.5(3) . . ? C39 Ru1 P1 163.6(3) . . ? C38 Ru1 P1 153.2(4) . . ? Sb1A F12 Sb1 5.2(5) . . ? Sb1 F11 Sb1A 11.8(5) . . ? Sb1 F8 Sb1A 5.1(5) . . ? Sb1 F10 Sb1A 11.1(5) . . ? Sb1A F7 Sb1 12.0(5) . . ? Sb1A F9 Sb1 11.2(5) . . ? Sb2 F2 Sb2A 15.8(2) . . ? Sb2 F3 Sb2A 18.3(3) . . ? Sb2A F4 Sb2 19.91(18) . . ? Sb2A F5 Sb2 16.5(3) . . ? Sb2 F6 Sb2A 13.6(4) . . ? F8 Sb1 F10 98.7(6) . . ? F8 Sb1 F11 94.3(5) . . ? F10 Sb1 F11 91.5(5) . . ? F8 Sb1 F7 94.4(5) . . ? F10 Sb1 F7 93.1(5) . . ? F11 Sb1 F7 169.4(6) . . ? F8 Sb1 F9 92.6(6) . . ? F10 Sb1 F9 168.7(7) . . ? F11 Sb1 F9 87.3(5) . . ? F7 Sb1 F9 86.2(5) . . ? F8 Sb1 F12 175.0(7) . . ? F10 Sb1 F12 86.2(6) . . ? F11 Sb1 F12 86.3(5) . . ? F7 Sb1 F12 84.6(5) . . ? F9 Sb1 F12 82.5(5) . . ? F6 Sb2 F3 104.5(17) . . ? F6 Sb2 F2 88.7(11) . . ? F3 Sb2 F2 96.9(7) . . ? F6 Sb2 F1 164.5(17) . . ? F3 Sb2 F1 76.0(17) . . ? F2 Sb2 F1 75.9(16) . . ? F6 Sb2 F4 90.1(10) . . ? F3 Sb2 F4 87.7(7) . . ? F2 Sb2 F4 175.4(6) . . ? F1 Sb2 F4 105.5(15) . . ? F6 Sb2 F5 97.8(14) . . ? F3 Sb2 F5 154.4(12) . . ? F2 Sb2 F5 96.2(6) . . ? F1 Sb2 F5 86.0(16) . . ? F4 Sb2 F5 79.6(5) . . ? F5 Sb2A F1A 83(2) . . ? F5 Sb2A F4 98.8(7) . . ? F1A Sb2A F4 93(3) . . ? F5 Sb2A F3 170.7(11) . . ? F1A Sb2A F3 105(2) . . ? F4 Sb2A F3 84.6(6) . . ? F5 Sb2A F6 94.2(12) . . ? F1A Sb2A F6 173(3) . . ? F4 Sb2A F6 81.5(9) . . ? F3 Sb2A F6 77.7(13) . . ? F5 Sb2A F2 96.0(7) . . ? F1A Sb2A F2 120(3) . . ? F4 Sb2A F2 145.8(7) . . ? F3 Sb2A F2 76.7(6) . . ? F6 Sb2A F2 66.8(9) . . ? F12 Sb1A F9 98.4(6) . . ? F12 Sb1A F7 97.4(6) . . ? F9 Sb1A F7 92.5(5) . . ? F12 Sb1A F11 95.4(6) . . ? F9 Sb1A F11 90.1(5) . . ? F7 Sb1A F11 166.5(6) . . ? F12 Sb1A F10 92.2(6) . . ? F9 Sb1A F10 168.7(7) . . ? F7 Sb1A F10 89.9(5) . . ? F11 Sb1A F10 85.2(5) . . ? F12 Sb1A F8 174.5(7) . . ? F9 Sb1A F8 86.4(5) . . ? F7 Sb1A F8 85.0(5) . . ? F11 Sb1A F8 81.9(5) . . ? F10 Sb1A F8 82.8(5) . . ? C48 C47 C46 101(3) . . ? C48 C47 H47A 111.6 . . ? C46 C47 H47A 111.6 . . ? C48 C47 H47B 111.6 . . ? C46 C47 H47B 111.6 . . ? H47A C47 H47B 109.4 . . ? C47 C48 C49 92(2) . . ? C47 C48 H48A 113.3 . . ? C49 C48 H48A 113.3 . . ? C47 C48 H48B 113.3 . . ? C49 C48 H48B 113.3 . . ? H48A C48 H48B 110.7 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C49 C50 126(3) . . ? C48 C49 H49A 105.9 . . ? C50 C49 H49A 105.9 . . ? C48 C49 H49B 105.9 . . ? C50 C49 H49B 105.9 . . ? H49A C49 H49B 106.2 . . ? C51 C50 C49 104.2(18) . . ? C51 C50 H50A 110.9 . . ? C49 C50 H50A 110.9 . . ? C51 C50 H50B 110.9 . . ? C49 C50 H50B 110.9 . . ? H50A C50 H50B 108.9 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0(2) . . . . ? P1 C1 C2 C3 177.2(11) . . . . ? C1 C2 C3 C4 -1(2) . . . . ? C2 C3 C4 C5 1(2) . . . . ? C3 C4 C5 C6 0(2) . . . . ? C4 C5 C6 C1 -1(2) . . . . ? C2 C1 C6 C5 0.5(19) . . . . ? P1 C1 C6 C5 -176.6(10) . . . . ? C12 C7 C8 C9 1.4(17) . . . . ? P1 C7 C8 C9 -173.4(9) . . . . ? C7 C8 C9 C10 -0.7(17) . . . . ? C8 C9 C10 C11 -1(2) . . . . ? C9 C10 C11 C12 2(2) . . . . ? C10 C11 C12 C7 -2(2) . . . . ? C8 C7 C12 C11 -0.2(18) . . . . ? P1 C7 C12 C11 174.6(10) . . . . ? C19 C14 C15 C16 -2(2) . . . . ? P2 C14 C15 C16 176.6(11) . . . . ? C14 C15 C16 C17 4(2) . . . . ? C15 C16 C17 C18 -5(2) . . . . ? C16 C17 C18 C19 4(2) . . . . ? C15 C14 C19 C18 1.2(19) . . . . ? P2 C14 C19 C18 -177.8(10) . . . . ? C17 C18 C19 C14 -2(2) . . . . ? C25 C20 C21 C22 -2(2) . . . . ? P2 C20 C21 C22 -179.6(10) . . . . ? C20 C21 C22 C23 1(2) . . . . ? C21 C22 C23 C24 -1(3) . . . . ? C22 C23 C24 C25 2(3) . . . . ? C21 C20 C25 C24 2(2) . . . . ? P2 C20 C25 C24 179.9(11) . . . . ? C23 C24 C25 C20 -2(2) . . . . ? N2 C30 C31 C32 3(2) . . . . ? C30 C31 C32 C33 -4(2) . . . . ? C31 C32 C33 C34 3(2) . . . . ? C32 C33 C34 N2 1(2) . . . . ? C40 C35 C36 C37 -1.6(16) . . . . ? C41 C35 C36 C37 175.2(11) . . . . ? Ru1 C35 C36 C37 -55.5(9) . . . . ? C40 C35 C36 Ru1 53.9(9) . . . . ? C41 C35 C36 Ru1 -129.3(11) . . . . ? C35 C36 C37 C38 -1.2(16) . . . . ? Ru1 C36 C37 C38 -57.4(10) . . . . ? C35 C36 C37 Ru1 56.1(9) . . . . ? C36 C37 C38 C39 2.9(17) . . . . ? Ru1 C37 C38 C39 -53.4(10) . . . . ? C36 C37 C38 C42 -178.4(11) . . . . ? Ru1 C37 C38 C42 125.2(11) . . . . ? C36 C37 C38 Ru1 56.3(9) . . . . ? C37 C38 C39 C40 -1.7(17) . . . . ? C42 C38 C39 C40 179.7(11) . . . . ? Ru1 C38 C39 C40 -53.9(9) . . . . ? C37 C38 C39 Ru1 52.3(10) . . . . ? C42 C38 C39 Ru1 -126.3(12) . . . . ? C36 C35 C40 C39 2.9(15) . . . . ? C41 C35 C40 C39 -173.9(11) . . . . ? Ru1 C35 C40 C39 56.8(9) . . . . ? C36 C35 C40 Ru1 -53.9(9) . . . . ? C41 C35 C40 Ru1 129.3(10) . . . . ? C38 C39 C40 C35 -1.3(16) . . . . ? Ru1 C39 C40 C35 -56.5(9) . . . . ? C38 C39 C40 Ru1 55.3(10) . . . . ? C39 C38 C42 C44 15.6(19) . . . . ? C37 C38 C42 C44 -163.0(13) . . . . ? Ru1 C38 C42 C44 -76.2(18) . . . . ? C39 C38 C42 C43 -109.5(15) . . . . ? C37 C38 C42 C43 71.8(17) . . . . ? Ru1 C38 C42 C43 158.7(12) . . . . ? C33 C34 N2 C30 -2.7(17) . . . . ? C33 C34 N2 Ru1 -171.9(9) . . . . ? C31 C30 N2 C34 0.9(18) . . . . ? C31 C30 N2 Ru1 169.9(10) . . . . ? C29 C28 O2 P3 173(2) . . . . ? C27 C26 O3 P3 152(3) . . . . ? Ru1 O1 P3 O3 52.6(8) . . . . ? Ru1 O1 P3 O2 167.7(7) . . . . ? Ru1 O1 P3 N1 -71.6(9) . . . . ? C26 O3 P3 O1 176.7(14) . . . . ? C26 O3 P3 O2 59.2(16) . . . . ? C26 O3 P3 N1 -54.6(16) . . . . ? C28 O2 P3 O1 -49.5(15) . . . . ? C28 O2 P3 O3 64.9(15) . . . . ? C28 O2 P3 N1 -177.7(14) . . . . ? P2 N1 P3 O1 -30.9(12) . . . . ? P2 N1 P3 O3 -152.6(9) . . . . ? P2 N1 P3 O2 92.5(10) . . . . ? P3 N1 P2 C14 165.3(9) . . . . ? P3 N1 P2 C13 43.3(11) . . . . ? P3 N1 P2 C20 -74.9(11) . . . . ? C15 C14 P2 N1 9.7(13) . . . . ? C19 C14 P2 N1 -171.4(11) . . . . ? C15 C14 P2 C13 134.4(11) . . . . ? C19 C14 P2 C13 -46.7(12) . . . . ? C15 C14 P2 C20 -113.5(12) . . . . ? C19 C14 P2 C20 65.4(13) . . . . ? P1 C13 P2 N1 37.7(9) . . . . ? P1 C13 P2 C14 -83.1(7) . . . . ? P1 C13 P2 C20 161.6(7) . . . . ? C21 C20 P2 N1 -29.3(13) . . . . ? C25 C20 P2 N1 153.2(11) . . . . ? C21 C20 P2 C14 90.2(12) . . . . ? C25 C20 P2 C14 -87.3(12) . . . . ? C21 C20 P2 C13 -153.5(11) . . . . ? C25 C20 P2 C13 29.0(12) . . . . ? C8 C7 P1 C1 -44.4(11) . . . . ? C12 C7 P1 C1 140.7(9) . . . . ? C8 C7 P1 C13 -151.0(9) . . . . ? C12 C7 P1 C13 34.1(10) . . . . ? C8 C7 P1 Ru1 87.9(10) . . . . ? C12 C7 P1 Ru1 -86.9(10) . . . . ? C2 C1 P1 C7 144.4(11) . . . . ? C6 C1 P1 C7 -38.4(12) . . . . ? C2 C1 P1 C13 -110.5(11) . . . . ? C6 C1 P1 C13 66.7(11) . . . . ? C2 C1 P1 Ru1 15.6(12) . . . . ? C6 C1 P1 Ru1 -167.2(8) . . . . ? P2 C13 P1 C7 151.1(6) . . . . ? P2 C13 P1 C1 44.9(8) . . . . ? P2 C13 P1 Ru1 -86.2(6) . . . . ? P3 O1 Ru1 N2 152.3(7) . . . . ? P3 O1 Ru1 C37 -52.7(8) . . . . ? P3 O1 Ru1 C40 -130.9(8) . . . . ? P3 O1 Ru1 C36 -29.8(9) . . . . ? P3 O1 Ru1 C35 -48.1(16) . . . . ? P3 O1 Ru1 C39 -119.2(7) . . . . ? P3 O1 Ru1 C38 -88.8(8) . . . . ? P3 O1 Ru1 P1 64.7(7) . . . . ? C34 N2 Ru1 O1 -166.7(9) . . . . ? C30 N2 Ru1 O1 24.5(9) . . . . ? C34 N2 Ru1 C37 103.1(13) . . . . ? C30 N2 Ru1 C37 -65.7(15) . . . . ? C34 N2 Ru1 C40 47.5(9) . . . . ? C30 N2 Ru1 C40 -121.3(9) . . . . ? C34 N2 Ru1 C36 16.7(13) . . . . ? C30 N2 Ru1 C36 -152.1(9) . . . . ? C34 N2 Ru1 C35 19.6(9) . . . . ? C30 N2 Ru1 C35 -149.2(9) . . . . ? C34 N2 Ru1 C39 84.2(9) . . . . ? C30 N2 Ru1 C39 -84.6(9) . . . . ? C34 N2 Ru1 C38 108.0(9) . . . . ? C30 N2 Ru1 C38 -60.8(10) . . . . ? C34 N2 Ru1 P1 -79.5(8) . . . . ? C30 N2 Ru1 P1 111.7(9) . . . . ? C36 C37 Ru1 O1 149.1(7) . . . . ? C38 C37 Ru1 O1 -79.7(8) . . . . ? C36 C37 Ru1 N2 -123.9(11) . . . . ? C38 C37 Ru1 N2 7.3(16) . . . . ? C36 C37 Ru1 C40 -66.3(8) . . . . ? C38 C37 Ru1 C40 64.9(8) . . . . ? C38 C37 Ru1 C36 131.2(12) . . . . ? C36 C37 Ru1 C35 -29.5(7) . . . . ? C38 C37 Ru1 C35 101.7(8) . . . . ? C36 C37 Ru1 C39 -103.1(8) . . . . ? C38 C37 Ru1 C39 28.1(7) . . . . ? C36 C37 Ru1 C38 -131.2(12) . . . . ? C36 C37 Ru1 P1 59.0(8) . . . . ? C38 C37 Ru1 P1 -169.8(6) . . . . ? C35 C40 Ru1 O1 151.3(7) . . . . ? C39 C40 Ru1 O1 18.8(11) . . . . ? C35 C40 Ru1 N2 -133.9(7) . . . . ? C39 C40 Ru1 N2 93.5(7) . . . . ? C35 C40 Ru1 C37 66.8(7) . . . . ? C39 C40 Ru1 C37 -65.7(7) . . . . ? C35 C40 Ru1 C36 29.8(7) . . . . ? C39 C40 Ru1 C36 -102.8(8) . . . . ? C39 C40 Ru1 C35 -132.6(11) . . . . ? C35 C40 Ru1 C39 132.6(11) . . . . ? C35 C40 Ru1 C38 103.6(8) . . . . ? C39 C40 Ru1 C38 -29.0(7) . . . . ? C35 C40 Ru1 P1 -48.3(8) . . . . ? C39 C40 Ru1 P1 179.1(6) . . . . ? C37 C36 Ru1 O1 -40.0(9) . . . . ? C35 C36 Ru1 O1 -171.3(5) . . . . ? C37 C36 Ru1 N2 135.8(8) . . . . ? C35 C36 Ru1 N2 4.5(11) . . . . ? C35 C36 Ru1 C37 -131.3(10) . . . . ? C37 C36 Ru1 C40 101.6(8) . . . . ? C35 C36 Ru1 C40 -29.7(6) . . . . ? C37 C36 Ru1 C35 131.3(10) . . . . ? C37 C36 Ru1 C39 65.0(8) . . . . ? C35 C36 Ru1 C39 -66.3(7) . . . . ? C37 C36 Ru1 C38 29.5(7) . . . . ? C35 C36 Ru1 C38 -101.8(7) . . . . ? C37 C36 Ru1 P1 -130.2(7) . . . . ? C35 C36 Ru1 P1 98.5(6) . . . . ? C40 C35 Ru1 O1 -106.2(14) . . . . ? C36 C35 Ru1 O1 24.5(16) . . . . ? C41 C35 Ru1 O1 140.2(14) . . . . ? C40 C35 Ru1 N2 51.7(8) . . . . ? C36 C35 Ru1 N2 -177.6(6) . . . . ? C41 C35 Ru1 N2 -62.0(15) . . . . ? C40 C35 Ru1 C37 -101.2(7) . . . . ? C36 C35 Ru1 C37 29.5(6) . . . . ? C41 C35 Ru1 C37 145.1(16) . . . . ? C36 C35 Ru1 C40 130.8(10) . . . . ? C41 C35 Ru1 C40 -113.6(18) . . . . ? C40 C35 Ru1 C36 -130.8(10) . . . . ? C41 C35 Ru1 C36 115.6(17) . . . . ? C40 C35 Ru1 C39 -28.8(7) . . . . ? C36 C35 Ru1 C39 102.0(7) . . . . ? C41 C35 Ru1 C39 -142.4(16) . . . . ? C40 C35 Ru1 C38 -64.4(7) . . . . ? C36 C35 Ru1 C38 66.4(7) . . . . ? C41 C35 Ru1 C38 -178.0(16) . . . . ? C40 C35 Ru1 P1 142.7(6) . . . . ? C36 C35 Ru1 P1 -86.5(6) . . . . ? C41 C35 Ru1 P1 29.1(15) . . . . ? C38 C39 Ru1 O1 60.2(8) . . . . ? C40 C39 Ru1 O1 -168.7(7) . . . . ? C38 C39 Ru1 N2 142.4(8) . . . . ? C40 C39 Ru1 N2 -86.5(8) . . . . ? C38 C39 Ru1 C37 -29.0(7) . . . . ? C40 C39 Ru1 C37 102.1(8) . . . . ? C38 C39 Ru1 C40 -131.1(11) . . . . ? C38 C39 Ru1 C36 -65.7(8) . . . . ? C40 C39 Ru1 C36 65.4(8) . . . . ? C38 C39 Ru1 C35 -102.4(8) . . . . ? C40 C39 Ru1 C35 28.7(7) . . . . ? C40 C39 Ru1 C38 131.1(11) . . . . ? C38 C39 Ru1 P1 -133.6(10) . . . . ? C40 C39 Ru1 P1 -2.5(16) . . . . ? C39 C38 Ru1 O1 -124.9(7) . . . . ? C37 C38 Ru1 O1 102.5(8) . . . . ? C42 C38 Ru1 O1 -9.1(13) . . . . ? C39 C38 Ru1 N2 -43.9(9) . . . . ? C37 C38 Ru1 N2 -176.5(7) . . . . ? C42 C38 Ru1 N2 71.9(14) . . . . ? C39 C38 Ru1 C37 132.6(11) . . . . ? C42 C38 Ru1 C37 -111.6(16) . . . . ? C39 C38 Ru1 C40 29.8(7) . . . . ? C37 C38 Ru1 C40 -102.8(9) . . . . ? C42 C38 Ru1 C40 145.6(14) . . . . ? C39 C38 Ru1 C36 103.0(8) . . . . ? C37 C38 Ru1 C36 -29.6(8) . . . . ? C42 C38 Ru1 C36 -141.2(14) . . . . ? C39 C38 Ru1 C35 66.2(8) . . . . ? C37 C38 Ru1 C35 -66.4(8) . . . . ? C42 C38 Ru1 C35 -178.0(14) . . . . ? C37 C38 Ru1 C39 -132.6(11) . . . . ? C42 C38 Ru1 C39 115.8(15) . . . . ? C39 C38 Ru1 P1 153.0(7) . . . . ? C37 C38 Ru1 P1 20.4(13) . . . . ? C42 C38 Ru1 P1 -91.2(14) . . . . ? C7 P1 Ru1 O1 145.3(5) . . . . ? C1 P1 Ru1 O1 -91.3(6) . . . . ? C13 P1 Ru1 O1 30.5(5) . . . . ? C7 P1 Ru1 N2 62.9(5) . . . . ? C1 P1 Ru1 N2 -173.7(6) . . . . ? C13 P1 Ru1 N2 -51.9(5) . . . . ? C7 P1 Ru1 C37 -118.3(6) . . . . ? C1 P1 Ru1 C37 5.1(6) . . . . ? C13 P1 Ru1 C37 126.8(6) . . . . ? C7 P1 Ru1 C40 -23.5(6) . . . . ? C1 P1 Ru1 C40 99.9(6) . . . . ? C13 P1 Ru1 C40 -138.3(6) . . . . ? C7 P1 Ru1 C36 -87.2(6) . . . . ? C1 P1 Ru1 C36 36.2(6) . . . . ? C13 P1 Ru1 C36 158.0(6) . . . . ? C7 P1 Ru1 C35 -50.3(6) . . . . ? C1 P1 Ru1 C35 73.1(6) . . . . ? C13 P1 Ru1 C35 -165.2(6) . . . . ? C7 P1 Ru1 C39 -21.6(12) . . . . ? C1 P1 Ru1 C39 101.8(12) . . . . ? C13 P1 Ru1 C39 -136.5(12) . . . . ? C7 P1 Ru1 C38 -131.9(8) . . . . ? C1 P1 Ru1 C38 -8.5(9) . . . . ? C13 P1 Ru1 C38 113.2(8) . . . . ? Sb1A F8 Sb1 F10 163(5) . . . . ? Sb1A F8 Sb1 F11 -105(5) . . . . ? Sb1A F8 Sb1 F7 69(5) . . . . ? Sb1A F8 Sb1 F9 -18(5) . . . . ? Sb1A F8 Sb1 F12 -9(4) . . . . ? Sb1A F10 Sb1 F8 -172(3) . . . . ? Sb1A F10 Sb1 F11 94(2) . . . . ? Sb1A F10 Sb1 F7 -77(2) . . . . ? Sb1A F10 Sb1 F9 10(2) . . . . ? Sb1A F10 Sb1 F12 7(2) . . . . ? Sb1A F11 Sb1 F8 154(3) . . . . ? Sb1A F11 Sb1 F10 -108(2) . . . . ? Sb1A F11 Sb1 F7 9(2) . . . . ? Sb1A F11 Sb1 F9 61(2) . . . . ? Sb1A F11 Sb1 F12 -21(2) . . . . ? Sb1A F7 Sb1 F8 -154(3) . . . . ? Sb1A F7 Sb1 F10 107(2) . . . . ? Sb1A F7 Sb1 F11 -9(2) . . . . ? Sb1A F7 Sb1 F9 -62(2) . . . . ? Sb1A F7 Sb1 F12 21(2) . . . . ? Sb1A F9 Sb1 F8 171(3) . . . . ? Sb1A F9 Sb1 F10 -10(2) . . . . ? Sb1A F9 Sb1 F11 -95(2) . . . . ? Sb1A F9 Sb1 F7 77(2) . . . . ? Sb1A F9 Sb1 F12 -8(2) . . . . ? Sb1A F12 Sb1 F8 11(5) . . . . ? Sb1A F12 Sb1 F10 -161(5) . . . . ? Sb1A F12 Sb1 F11 107(5) . . . . ? Sb1A F12 Sb1 F7 -68(5) . . . . ? Sb1A F12 Sb1 F9 19(5) . . . . ? Sb2A F6 Sb2 F3 -135.9(17) . . . . ? Sb2A F6 Sb2 F2 127.3(15) . . . . ? Sb2A F6 Sb2 F1 134(8) . . . . ? Sb2A F6 Sb2 F4 -48.2(14) . . . . ? Sb2A F6 Sb2 F5 31.3(13) . . . . ? Sb2A F3 Sb2 F6 147.5(13) . . . . ? Sb2A F3 Sb2 F2 -122.1(11) . . . . ? Sb2A F3 Sb2 F1 -48.5(15) . . . . ? Sb2A F3 Sb2 F4 58.0(8) . . . . ? Sb2A F3 Sb2 F5 -1.9(13) . . . . ? Sb2A F2 Sb2 F6 -139.4(15) . . . . ? Sb2A F2 Sb2 F3 116.2(13) . . . . ? Sb2A F2 Sb2 F1 42.5(18) . . . . ? Sb2A F2 Sb2 F4 -66(10) . . . . ? Sb2A F2 Sb2 F5 -41.7(9) . . . . ? Sb2A F4 Sb2 F6 141.6(15) . . . . ? Sb2A F4 Sb2 F3 -113.9(12) . . . . ? Sb2A F4 Sb2 F2 68(10) . . . . ? Sb2A F4 Sb2 F1 -39.1(18) . . . . ? Sb2A F4 Sb2 F5 43.7(8) . . . . ? Sb2A F5 Sb2 F6 -147.6(13) . . . . ? Sb2A F5 Sb2 F3 2.6(18) . . . . ? Sb2A F5 Sb2 F2 122.9(11) . . . . ? Sb2A F5 Sb2 F1 47.6(18) . . . . ? Sb2A F5 Sb2 F4 -59.0(9) . . . . ? Sb2 F5 Sb2A F1A -163(3) . . . . ? Sb2 F5 Sb2A F4 105.5(10) . . . . ? Sb2 F5 Sb2A F3 -6(4) . . . . ? Sb2 F5 Sb2A F6 23.5(10) . . . . ? Sb2 F5 Sb2A F2 -43.6(9) . . . . ? Sb2 F4 Sb2A F5 -121.1(10) . . . . ? Sb2 F4 Sb2A F1A 155(2) . . . . ? Sb2 F4 Sb2A F3 50.3(10) . . . . ? Sb2 F4 Sb2A F6 -28.1(11) . . . . ? Sb2 F4 Sb2A F2 -6.3(10) . . . . ? Sb2 F3 Sb2A F5 6(5) . . . . ? Sb2 F3 Sb2A F1A 163(3) . . . . ? Sb2 F3 Sb2A F4 -106.0(10) . . . . ? Sb2 F3 Sb2A F6 -23.5(10) . . . . ? Sb2 F3 Sb2A F2 45.3(9) . . . . ? Sb2 F6 Sb2A F5 -140.0(17) . . . . ? Sb2 F6 Sb2A F1A 153(20) . . . . ? Sb2 F6 Sb2A F4 121.6(17) . . . . ? Sb2 F6 Sb2A F3 35.3(15) . . . . ? Sb2 F6 Sb2A F2 -45.3(14) . . . . ? Sb2 F2 Sb2A F5 124.1(11) . . . . ? Sb2 F2 Sb2A F1A -150(2) . . . . ? Sb2 F2 Sb2A F4 8.5(13) . . . . ? Sb2 F2 Sb2A F3 -50.1(11) . . . . ? Sb2 F2 Sb2A F6 32.0(13) . . . . ? Sb1 F12 Sb1A F9 -159(5) . . . . ? Sb1 F12 Sb1A F7 108(5) . . . . ? Sb1 F12 Sb1A F11 -68(5) . . . . ? Sb1 F12 Sb1A F10 17(5) . . . . ? Sb1 F12 Sb1A F8 -8(4) . . . . ? Sb1 F9 Sb1A F12 170(3) . . . . ? Sb1 F9 Sb1A F7 -92(2) . . . . ? Sb1 F9 Sb1A F11 74(2) . . . . ? Sb1 F9 Sb1A F10 10(2) . . . . ? Sb1 F9 Sb1A F8 -7(2) . . . . ? Sb1 F7 Sb1A F12 -154(3) . . . . ? Sb1 F7 Sb1A F9 107(2) . . . . ? Sb1 F7 Sb1A F11 6.8(16) . . . . ? Sb1 F7 Sb1A F10 -61(2) . . . . ? Sb1 F7 Sb1A F8 21(2) . . . . ? Sb1 F11 Sb1A F12 154(3) . . . . ? Sb1 F11 Sb1A F9 -108(2) . . . . ? Sb1 F11 Sb1A F7 -7.0(17) . . . . ? Sb1 F11 Sb1A F10 62(2) . . . . ? Sb1 F11 Sb1A F8 -22(2) . . . . ? Sb1 F10 Sb1A F12 -171(3) . . . . ? Sb1 F10 Sb1A F9 -10(2) . . . . ? Sb1 F10 Sb1A F7 92(2) . . . . ? Sb1 F10 Sb1A F11 -76(2) . . . . ? Sb1 F10 Sb1A F8 7(2) . . . . ? Sb1 F8 Sb1A F12 10(5) . . . . ? Sb1 F8 Sb1A F9 161(5) . . . . ? Sb1 F8 Sb1A F7 -106(5) . . . . ? Sb1 F8 Sb1A F11 70(5) . . . . ? Sb1 F8 Sb1A F10 -16(5) . . . . ? C46 C47 C48 C49 -170(4) . . . . ? C47 C48 C49 C50 178(5) . . . . ? C48 C49 C50 C51 42(7) . . . . ? _diffrn_measured_fraction_theta_max 0.813 _diffrn_reflns_theta_full 71.24 _diffrn_measured_fraction_theta_full 0.813 _refine_diff_density_max 1.253 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.133 #==END #=============================================================================== data_8a _database_code_depnum_ccdc_archive 'CCDC 690030' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H48 N5 O3 P3 Ru, 2(F6 Sb), 2(C H2 Cl2)' _chemical_formula_sum 'C51 H52 Cl4 F12 N5 O3 P3 Ru Sb2' _chemical_formula_weight 1590.26 _chemical_compound_source synthesis 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4217(2) _cell_length_b 34.9367(6) _cell_length_c 15.9704(3) _cell_angle_alpha 90.00 _cell_angle_beta 120.276(1) _cell_angle_gamma 90.00 _cell_volume 5985.42(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9887 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.350 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 1.487 _exptl_absorpt_correction_type 'Multi scan' _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.772 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95 mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39556 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.08 _reflns_number_total 10433 _reflns_number_gt 8145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collet (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowki & Minor 1997)' _computing_data_reduction 'HKL Denzo and scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR 92 (Altomare A., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0857P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10433 _refine_ls_number_parameters 732 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6004(5) 0.67638(15) 0.9708(4) 0.0194(11) Uani 1 1 d . . . C2 C 0.4932(5) 0.66123(16) 0.8935(4) 0.0229(12) Uani 1 1 d . . . H2 H 0.4954 0.6368 0.8714 0.027 Uiso 1 1 calc R . . C3 C 0.3815(5) 0.68212(18) 0.8478(4) 0.0296(14) Uani 1 1 d . . . H3 H 0.3104 0.6716 0.7958 0.035 Uiso 1 1 calc R . . C4 C 0.3779(6) 0.71836(18) 0.8808(4) 0.0325(14) Uani 1 1 d . . . H4 H 0.3044 0.7324 0.8508 0.039 Uiso 1 1 calc R . . C5 C 0.4835(6) 0.73360(17) 0.9582(4) 0.0327(14) Uani 1 1 d . . . H5 H 0.4812 0.7581 0.9800 0.039 Uiso 1 1 calc R . . C6 C 0.5934(6) 0.71264(16) 1.0039(4) 0.0282(13) Uani 1 1 d . . . H6 H 0.6633 0.7230 1.0574 0.034 Uiso 1 1 calc R . . C7 C 0.7670(5) 0.64543(14) 1.1550(4) 0.0178(11) Uani 1 1 d . . . C8 C 0.6623(5) 0.63764(16) 1.1639(4) 0.0240(12) Uani 1 1 d . . . H8 H 0.5834 0.6371 1.1089 0.029 Uiso 1 1 calc R . . C9 C 0.6760(6) 0.63073(17) 1.2545(5) 0.0325(14) Uani 1 1 d . . . H9 H 0.6066 0.6255 1.2602 0.039 Uiso 1 1 calc R . . C10 C 0.7930(7) 0.63172(18) 1.3359(4) 0.0361(16) Uani 1 1 d . . . H10 H 0.8021 0.6269 1.3964 0.043 Uiso 1 1 calc R . . C11 C 0.8971(6) 0.63973(17) 1.3286(4) 0.0325(15) Uani 1 1 d . . . H11 H 0.9757 0.6404 1.3840 0.039 Uiso 1 1 calc R . . C12 C 0.8840(5) 0.64670(15) 1.2391(4) 0.0242(12) Uani 1 1 d . . . H12 H 0.9541 0.6523 1.2345 0.029 Uiso 1 1 calc R . . C13 C 0.8709(5) 0.68237(15) 1.0532(4) 0.0200(11) Uani 1 1 d . . . H13A H 0.8606 0.7047 1.0845 0.024 Uiso 1 1 calc R . . H13B H 0.9494 0.6706 1.0997 0.024 Uiso 1 1 calc R . . C14 C 0.7579(5) 0.72894(16) 0.8728(4) 0.0222(12) Uani 1 1 d . . . C15 C 0.7266(6) 0.76088(17) 0.9079(5) 0.0355(15) Uani 1 1 d . . . H15 H 0.7724 0.7666 0.9736 0.043 Uiso 1 1 calc R . . C16 C 0.6281(7) 0.7843(2) 0.8461(6) 0.0473(19) Uani 1 1 d . . . H16 H 0.6082 0.8057 0.8704 0.057 Uiso 1 1 calc R . . C17 C 0.5611(6) 0.7760(2) 0.7504(6) 0.0480(19) Uani 1 1 d . . . H17 H 0.4946 0.7915 0.7090 0.058 Uiso 1 1 calc R . . C18 C 0.5907(6) 0.7446(2) 0.7139(5) 0.048(2) Uani 1 1 d . . . H18 H 0.5439 0.7393 0.6479 0.058 Uiso 1 1 calc R . . C19 C 0.6902(6) 0.72061(18) 0.7744(4) 0.0334(15) Uani 1 1 d . . . H19 H 0.7105 0.6996 0.7493 0.040 Uiso 1 1 calc R . . C20 C 1.0225(5) 0.73114(16) 1.0071(4) 0.0254(13) Uani 1 1 d . . . C21 C 1.1271(5) 0.72297(17) 1.0963(4) 0.0294(14) Uani 1 1 d . . . H21 H 1.1271 0.7018 1.1314 0.035 Uiso 1 1 calc R . . C22 C 1.2302(6) 0.7461(2) 1.1326(5) 0.0420(17) Uani 1 1 d . . . H22 H 1.2994 0.7406 1.1927 0.050 Uiso 1 1 calc R . . C23 C 1.2320(7) 0.7767(2) 1.0816(6) 0.060(2) Uani 1 1 d . . . H23 H 1.3014 0.7926 1.1076 0.071 Uiso 1 1 calc R . . C24 C 1.1324(8) 0.7843(3) 0.9923(8) 0.096(4) Uani 1 1 d . . . H24 H 1.1363 0.8046 0.9561 0.116 Uiso 1 1 calc R . . C25 C 1.0268(7) 0.7625(2) 0.9555(6) 0.072(3) Uani 1 1 d . . . H25 H 0.9578 0.7687 0.8958 0.086 Uiso 1 1 calc R . . C26 C 0.9463(6) 0.56823(17) 0.8060(4) 0.0298(14) Uani 1 1 d . . . H26A H 0.9225 0.5511 0.8418 0.036 Uiso 1 1 calc R . . H26B H 1.0354 0.5659 0.8322 0.036 Uiso 1 1 calc R . . C27 C 0.8782(7) 0.5579(2) 0.7012(5) 0.0463(18) Uani 1 1 d . . . H27A H 0.9007 0.5753 0.6661 0.069 Uiso 1 1 calc R . . H27B H 0.7900 0.5593 0.6765 0.069 Uiso 1 1 calc R . . H27C H 0.9000 0.5323 0.6935 0.069 Uiso 1 1 calc R . . C28 C 1.1808(5) 0.64785(17) 0.9490(4) 0.0276(13) Uani 1 1 d . . . H28A H 1.1474 0.6736 0.9324 0.033 Uiso 1 1 calc R . . H28B H 1.1804 0.6367 0.8933 0.033 Uiso 1 1 calc R . . C29 C 1.3106(6) 0.6488(2) 1.0340(5) 0.0404(17) Uani 1 1 d . . . H29A H 1.3436 0.6232 1.0484 0.061 Uiso 1 1 calc R . . H29B H 1.3094 0.6591 1.0892 0.061 Uiso 1 1 calc R . . H29C H 1.3619 0.6645 1.0189 0.061 Uiso 1 1 calc R . . C30 C 0.8413(5) 0.50301(15) 0.9804(4) 0.0214(12) Uani 1 1 d . . . H30 H 0.8967 0.5072 1.0460 0.026 Uiso 1 1 calc R . . C31 C 0.8371(5) 0.46724(16) 0.9419(4) 0.0255(13) Uani 1 1 d . . . H31 H 0.8896 0.4478 0.9811 0.031 Uiso 1 1 calc R . . C32 C 0.7551(5) 0.46056(16) 0.8456(4) 0.0278(13) Uani 1 1 d . . . H32 H 0.7494 0.4364 0.8191 0.033 Uiso 1 1 calc R . . C33 C 0.6810(5) 0.49021(16) 0.7886(4) 0.0255(13) Uani 1 1 d . . . H33 H 0.6254 0.4864 0.7229 0.031 Uiso 1 1 calc R . . C34 C 0.6905(5) 0.52589(15) 0.8303(4) 0.0193(11) Uani 1 1 d . . . C35 C 0.6264(5) 0.56056(16) 0.7738(4) 0.0203(12) Uani 1 1 d . . . C36 C 0.5534(5) 0.56020(17) 0.6748(4) 0.0287(13) Uani 1 1 d . . . H36 H 0.5353 0.5370 0.6417 0.034 Uiso 1 1 calc R . . C37 C 0.5061(6) 0.59398(18) 0.6232(4) 0.0336(15) Uani 1 1 d . . . H37 H 0.4543 0.5938 0.5562 0.040 Uiso 1 1 calc R . . C38 C 0.5385(5) 0.62790(17) 0.6748(4) 0.0278(13) Uani 1 1 d . . . H38 H 0.5125 0.6513 0.6429 0.033 Uiso 1 1 calc R . . C39 C 0.6106(5) 0.62641(16) 0.7753(4) 0.0219(12) Uani 1 1 d . . . H39 H 0.6310 0.6494 0.8094 0.026 Uiso 1 1 calc R . . C40 C 0.4972(5) 0.56419(15) 0.9318(4) 0.0202(12) Uani 1 1 d . . . H40 H 0.4712 0.5723 0.8690 0.024 Uiso 1 1 calc R . . C41 C 0.4092(5) 0.55065(16) 0.9524(4) 0.0275(13) Uani 1 1 d . . . H41 H 0.3254 0.5499 0.9047 0.033 Uiso 1 1 calc R . . C42 C 0.4482(5) 0.53805(17) 1.0463(4) 0.0295(14) Uani 1 1 d . . . H42 H 0.3908 0.5293 1.0629 0.035 Uiso 1 1 calc R . . C43 C 0.5727(5) 0.53886(16) 1.1134(4) 0.0263(13) Uani 1 1 d . . . H43 H 0.6007 0.5299 1.1758 0.032 Uiso 1 1 calc R . . C44 C 0.6569(5) 0.55293(15) 1.0889(4) 0.0194(11) Uani 1 1 d . . . C45 C 0.7918(5) 0.55407(14) 1.1571(4) 0.0176(11) Uani 1 1 d . . . C46 C 0.8506(5) 0.54033(16) 1.2510(4) 0.0242(12) Uani 1 1 d . . . H46 H 0.8040 0.5293 1.2755 0.029 Uiso 1 1 calc R . . C47 C 0.9778(5) 0.54294(17) 1.3082(4) 0.0281(14) Uani 1 1 d . . . H47 H 1.0177 0.5337 1.3715 0.034 Uiso 1 1 calc R . . C48 C 1.0463(5) 0.55953(16) 1.2708(4) 0.0257(13) Uani 1 1 d . . . H48 H 1.1325 0.5620 1.3086 0.031 Uiso 1 1 calc R . . C49 C 0.9838(5) 0.57221(15) 1.1770(4) 0.0198(11) Uani 1 1 d . . . H49 H 1.0296 0.5829 1.1514 0.024 Uiso 1 1 calc R . . C50 C 0.2805(7) 0.4816(2) 0.5291(5) 0.056(2) Uani 1 1 d . . . H50A H 0.2738 0.4979 0.5755 0.067 Uiso 1 1 calc R . . H50B H 0.1984 0.4713 0.4851 0.067 Uiso 1 1 calc R . . C51 C 0.0816(10) 0.1737(3) -0.1630(8) 0.085(3) Uani 1 1 d . . . H51A H 0.0523 0.1574 -0.2196 0.102 Uiso 1 1 calc R . . H51B H 0.0401 0.1656 -0.1283 0.102 Uiso 1 1 calc R . . F1 F 0.6539(4) 0.09473(12) 0.1428(3) 0.0582(12) Uani 1 1 d . . . F2 F 0.5942(5) 0.1521(2) 0.2190(4) 0.112(3) Uani 1 1 d . . . F3 F 0.5484(5) 0.15788(14) 0.0397(3) 0.0772(17) Uani 1 1 d . . . F4 F 0.7248(7) 0.19828(13) 0.1785(4) 0.116(3) Uani 1 1 d . . . F5 F 0.7842(5) 0.14091(15) 0.1025(4) 0.0788(16) Uani 1 1 d . . . F6 F 0.8266(4) 0.13664(11) 0.2802(3) 0.0535(11) Uani 1 1 d . . . F7 F 0.2914(4) 0.53593(14) 0.7041(3) 0.0645(13) Uani 1 1 d . . . F8 F 0.1565(4) 0.5790(2) 0.7527(3) 0.090(2) Uani 1 1 d . . . F9 F 0.0482(5) 0.53854(16) 0.5902(4) 0.0799(16) Uani 1 1 d . . . F10 F 0.0554(5) 0.61421(17) 0.5854(4) 0.0886(18) Uani 1 1 d . . . F11 F 0.1913(4) 0.57182(13) 0.5351(3) 0.0562(12) Uani 1 1 d . . . F12 F 0.3037(5) 0.61006(15) 0.7016(4) 0.0788(16) Uani 1 1 d . . . N1 N 0.9013(4) 0.66634(13) 0.8914(3) 0.0242(10) Uani 1 1 d . . . N2 N 0.7678(4) 0.53207(12) 0.9263(3) 0.0166(9) Uani 1 1 d . . . N3 N 0.6527(4) 0.59366(12) 0.8262(3) 0.0179(9) Uani 1 1 d . . . N4 N 0.6190(4) 0.56628(11) 0.9983(3) 0.0151(9) Uani 1 1 d . . . N5 N 0.8589(4) 0.56990(11) 1.1198(3) 0.0154(9) Uani 1 1 d . . . O1 O 0.9255(3) 0.60001(10) 0.9781(3) 0.0199(8) Uani 1 1 d . . . O2 O 0.9149(4) 0.60722(11) 0.8152(3) 0.0291(9) Uani 1 1 d . . . O3 O 1.1048(3) 0.62451(11) 0.9767(3) 0.0249(9) Uani 1 1 d . . . P1 P 0.74445(13) 0.64791(4) 1.03219(10) 0.0164(3) Uani 1 1 d . . . P2 P 0.88834(13) 0.69946(4) 0.95333(10) 0.0195(3) Uani 1 1 d . . . P3 P 0.95782(13) 0.62512(4) 0.91812(10) 0.0183(3) Uani 1 1 d . . . Ru1 Ru 0.75812(4) 0.586971(11) 0.97733(3) 0.01357(12) Uani 1 1 d . . . Sb1 Sb 0.68629(4) 0.146764(12) 0.15929(3) 0.03206(14) Uani 1 1 d . . . Sb2 Sb 0.17229(4) 0.575749(14) 0.64252(3) 0.03438(14) Uani 1 1 d . . . Cl1 Cl 0.33031(18) 0.50952(6) 0.46267(13) 0.0538(5) Uani 1 1 d . . . Cl2 Cl 0.3816(3) 0.44444(8) 0.5899(2) 0.1124(12) Uani 1 1 d . . . Cl3 Cl 0.2429(3) 0.16696(8) -0.08780(17) 0.0824(7) Uani 1 1 d . . . Cl4 Cl 0.0389(3) 0.22050(8) -0.2012(2) 0.1030(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(3) 0.016(3) 0.020(3) 0.002(2) 0.012(2) 0.002(2) C2 0.024(3) 0.020(3) 0.025(3) 0.000(2) 0.014(3) 0.004(2) C3 0.021(3) 0.036(4) 0.029(3) 0.003(3) 0.010(3) 0.003(3) C4 0.029(3) 0.035(4) 0.034(3) 0.009(3) 0.015(3) 0.012(3) C5 0.041(4) 0.023(3) 0.037(4) 0.004(3) 0.021(3) 0.013(3) C6 0.032(3) 0.021(3) 0.027(3) -0.001(2) 0.011(3) 0.002(3) C7 0.024(3) 0.012(3) 0.019(3) 0.001(2) 0.012(2) 0.002(2) C8 0.026(3) 0.022(3) 0.027(3) -0.002(2) 0.016(3) 0.000(2) C9 0.043(4) 0.025(3) 0.043(4) 0.002(3) 0.032(3) 0.003(3) C10 0.057(5) 0.034(4) 0.024(3) -0.001(3) 0.025(3) 0.004(3) C11 0.045(4) 0.026(3) 0.019(3) -0.002(2) 0.011(3) -0.001(3) C12 0.028(3) 0.019(3) 0.024(3) -0.003(2) 0.012(3) -0.001(2) C13 0.024(3) 0.015(3) 0.018(3) 0.000(2) 0.007(2) -0.001(2) C14 0.020(3) 0.021(3) 0.024(3) 0.010(2) 0.010(2) 0.001(2) C15 0.041(4) 0.026(3) 0.040(4) 0.010(3) 0.021(3) 0.005(3) C16 0.042(4) 0.036(4) 0.062(5) 0.026(4) 0.025(4) 0.019(3) C17 0.031(4) 0.041(4) 0.059(5) 0.030(4) 0.013(4) 0.008(3) C18 0.036(4) 0.055(5) 0.027(3) 0.020(3) -0.004(3) -0.014(4) C19 0.035(4) 0.030(3) 0.025(3) 0.006(3) 0.008(3) -0.005(3) C20 0.018(3) 0.019(3) 0.036(3) 0.005(2) 0.010(3) -0.003(2) C21 0.025(3) 0.033(3) 0.026(3) 0.003(3) 0.010(3) -0.004(3) C22 0.023(3) 0.052(4) 0.038(4) -0.006(3) 0.005(3) -0.009(3) C23 0.030(4) 0.040(4) 0.088(6) 0.006(4) 0.014(4) -0.015(3) C24 0.038(5) 0.066(6) 0.141(9) 0.064(6) 0.013(6) -0.017(4) C25 0.030(4) 0.059(5) 0.086(6) 0.048(5) -0.001(4) -0.014(4) C26 0.034(4) 0.029(3) 0.032(3) -0.004(3) 0.020(3) -0.003(3) C27 0.044(4) 0.051(5) 0.046(4) -0.020(3) 0.024(4) -0.010(4) C28 0.022(3) 0.033(3) 0.033(3) 0.005(3) 0.018(3) -0.008(3) C29 0.023(3) 0.050(4) 0.045(4) 0.002(3) 0.014(3) -0.010(3) C30 0.019(3) 0.020(3) 0.023(3) 0.004(2) 0.009(2) 0.002(2) C31 0.022(3) 0.020(3) 0.036(3) 0.001(2) 0.015(3) 0.005(2) C32 0.032(3) 0.016(3) 0.038(3) -0.009(2) 0.019(3) -0.002(2) C33 0.027(3) 0.025(3) 0.023(3) -0.007(2) 0.011(3) -0.006(3) C34 0.013(3) 0.023(3) 0.020(3) -0.002(2) 0.007(2) -0.001(2) C35 0.016(3) 0.024(3) 0.019(3) -0.001(2) 0.007(2) -0.001(2) C36 0.026(3) 0.030(3) 0.024(3) -0.006(3) 0.007(3) -0.004(3) C37 0.031(4) 0.042(4) 0.018(3) 0.001(3) 0.005(3) -0.004(3) C38 0.026(3) 0.032(3) 0.021(3) 0.010(2) 0.008(3) 0.003(3) C39 0.020(3) 0.023(3) 0.022(3) 0.002(2) 0.011(2) -0.002(2) C40 0.018(3) 0.020(3) 0.021(3) 0.002(2) 0.009(2) 0.001(2) C41 0.015(3) 0.026(3) 0.041(4) -0.004(3) 0.014(3) -0.005(2) C42 0.025(3) 0.032(3) 0.038(3) 0.003(3) 0.021(3) -0.006(3) C43 0.028(3) 0.026(3) 0.031(3) -0.001(3) 0.021(3) -0.005(3) C44 0.021(3) 0.015(3) 0.025(3) -0.002(2) 0.013(2) 0.001(2) C45 0.020(3) 0.013(3) 0.019(3) -0.001(2) 0.009(2) -0.001(2) C46 0.027(3) 0.024(3) 0.021(3) 0.006(2) 0.011(3) -0.001(2) C47 0.034(4) 0.025(3) 0.016(3) 0.006(2) 0.006(3) 0.005(3) C48 0.021(3) 0.022(3) 0.023(3) 0.000(2) 0.002(2) 0.000(2) C49 0.019(3) 0.014(3) 0.023(3) -0.002(2) 0.008(2) -0.004(2) C50 0.044(5) 0.074(6) 0.039(4) -0.010(4) 0.014(4) 0.006(4) C51 0.089(8) 0.072(7) 0.096(8) -0.014(6) 0.047(7) -0.006(6) F1 0.058(3) 0.039(2) 0.062(3) 0.000(2) 0.019(2) -0.014(2) F2 0.076(4) 0.210(8) 0.060(3) 0.015(4) 0.041(3) 0.077(4) F3 0.083(4) 0.073(3) 0.029(2) -0.006(2) -0.006(2) 0.040(3) F4 0.169(6) 0.025(3) 0.067(3) -0.009(2) -0.004(4) 0.017(3) F5 0.096(4) 0.086(4) 0.088(4) 0.011(3) 0.072(4) -0.001(3) F6 0.048(3) 0.043(2) 0.038(2) -0.0063(18) -0.0015(19) 0.019(2) F7 0.062(3) 0.071(3) 0.047(3) 0.009(2) 0.018(2) 0.014(2) F8 0.043(3) 0.198(7) 0.038(3) -0.012(3) 0.028(2) -0.002(3) F9 0.060(3) 0.089(4) 0.080(3) -0.012(3) 0.027(3) -0.043(3) F10 0.084(4) 0.096(4) 0.072(3) 0.002(3) 0.029(3) 0.049(3) F11 0.066(3) 0.072(3) 0.039(2) 0.002(2) 0.033(2) 0.001(2) F12 0.063(3) 0.082(4) 0.095(4) -0.048(3) 0.042(3) -0.039(3) N1 0.030(3) 0.019(2) 0.024(2) 0.004(2) 0.014(2) 0.000(2) N2 0.016(2) 0.016(2) 0.020(2) 0.0003(18) 0.0110(19) -0.0020(18) N3 0.014(2) 0.021(2) 0.019(2) 0.0000(18) 0.0085(19) -0.0012(19) N4 0.015(2) 0.011(2) 0.018(2) -0.0012(17) 0.0079(19) 0.0009(17) N5 0.018(2) 0.011(2) 0.016(2) -0.0018(17) 0.0077(19) -0.0016(17) O1 0.0163(19) 0.020(2) 0.0241(19) 0.0055(16) 0.0111(17) 0.0002(15) O2 0.037(2) 0.026(2) 0.025(2) -0.0022(17) 0.0162(19) 0.0012(19) O3 0.015(2) 0.029(2) 0.030(2) 0.0084(17) 0.0112(18) -0.0024(16) P1 0.0160(7) 0.0136(7) 0.0183(7) -0.0003(5) 0.0077(6) 0.0000(5) P2 0.0177(7) 0.0155(7) 0.0213(7) 0.0049(6) 0.0069(6) 0.0005(6) P3 0.0177(7) 0.0181(7) 0.0196(7) 0.0007(5) 0.0098(6) -0.0018(6) Ru1 0.0130(2) 0.0124(2) 0.0146(2) 0.00068(16) 0.00639(18) -0.00044(16) Sb1 0.0364(3) 0.0278(2) 0.0229(2) -0.00075(16) 0.00819(19) 0.01397(18) Sb2 0.0264(2) 0.0494(3) 0.0268(2) -0.00812(19) 0.01303(19) -0.0080(2) Cl1 0.0462(11) 0.0633(13) 0.0407(10) -0.0167(9) 0.0135(9) -0.0076(9) Cl2 0.0702(17) 0.0633(17) 0.132(3) 0.0306(16) -0.0022(17) 0.0016(14) Cl3 0.0916(19) 0.0898(19) 0.0637(14) -0.0078(13) 0.0375(14) 0.0184(15) Cl4 0.115(2) 0.0747(18) 0.101(2) -0.0206(15) 0.0408(19) 0.0198(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.386(8) . ? C1 C6 1.392(8) . ? C1 P1 1.839(5) . ? C2 C3 1.404(8) . ? C2 H2 0.9300 . ? C3 C4 1.381(9) . ? C3 H3 0.9300 . ? C4 C5 1.378(9) . ? C4 H4 0.9300 . ? C5 C6 1.388(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.397(8) . ? C7 C8 1.404(8) . ? C7 P1 1.838(5) . ? C8 C9 1.391(8) . ? C8 H8 0.9300 . ? C9 C10 1.377(9) . ? C9 H9 0.9300 . ? C10 C11 1.385(9) . ? C10 H10 0.9300 . ? C11 C12 1.377(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 P2 1.815(5) . ? C13 P1 1.870(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.389(8) . ? C14 C19 1.389(8) . ? C14 P2 1.800(5) . ? C15 C16 1.387(9) . ? C15 H15 0.9300 . ? C16 C17 1.354(10) . ? C16 H16 0.9300 . ? C17 C18 1.375(11) . ? C17 H17 0.9300 . ? C18 C19 1.400(9) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C25 1.388(8) . ? C20 C21 1.390(8) . ? C20 P2 1.815(6) . ? C21 C22 1.371(8) . ? C21 H21 0.9300 . ? C22 C23 1.35(1) . ? C22 H22 0.9300 . ? C23 C24 1.363(12) . ? C23 H23 0.9300 . ? C24 C25 1.368(10) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 O2 1.445(7) . ? C26 C27 1.490(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 O3 1.474(6) . ? C28 C29 1.495(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 N2 1.347(7) . ? C30 C31 1.382(8) . ? C30 H30 0.9300 . ? C31 C32 1.371(8) . ? C31 H31 0.9300 . ? C32 C33 1.380(8) . ? C32 H32 0.9300 . ? C33 C34 1.390(8) . ? C33 H33 0.9300 . ? C34 N2 1.354(6) . ? C34 C35 1.480(7) . ? C35 N3 1.367(7) . ? C35 C36 1.370(7) . ? C36 C37 1.389(8) . ? C36 H36 0.9300 . ? C37 C38 1.382(9) . ? C37 H37 0.9300 . ? C38 C39 1.390(7) . ? C38 H38 0.9300 . ? C39 N3 1.347(7) . ? C39 H39 0.9300 . ? C40 N4 1.342(7) . ? C40 C41 1.375(7) . ? C40 H40 0.9300 . ? C41 C42 1.394(8) . ? C41 H41 0.9300 . ? C42 C43 1.367(8) . ? C42 H42 0.9300 . ? C43 C44 1.378(7) . ? C43 H43 0.9300 . ? C44 N4 1.359(7) . ? C44 C45 1.468(7) . ? C45 N5 1.362(7) . ? C45 C46 1.382(7) . ? C46 C47 1.372(8) . ? C46 H46 0.9300 . ? C47 C48 1.390(8) . ? C47 H47 0.9300 . ? C48 C49 1.368(7) . ? C48 H48 0.9300 . ? C49 N5 1.349(7) . ? C49 H49 0.9300 . ? C50 Cl2 1.726(8) . ? C50 Cl1 1.766(8) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 Cl4 1.733(10) . ? C51 Cl3 1.757(10) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? F1 Sb1 1.852(4) . ? F2 Sb1 1.830(5) . ? F3 Sb1 1.853(4) . ? F4 Sb1 1.848(5) . ? F5 Sb1 1.859(5) . ? F6 Sb1 1.870(4) . ? F7 Sb2 1.904(4) . ? F8 Sb2 1.869(4) . ? F9 Sb2 1.861(4) . ? F10 Sb2 1.847(5) . ? F11 Sb2 1.852(4) . ? F12 Sb2 1.855(4) . ? N1 P3 1.564(5) . ? N1 P2 1.583(5) . ? N2 Ru1 2.112(4) . ? N3 Ru1 2.099(4) . ? N4 Ru1 2.050(4) . ? N5 Ru1 2.056(4) . ? O1 P3 1.496(4) . ? O1 Ru1 2.122(3) . ? O2 P3 1.578(4) . ? O3 P3 1.577(4) . ? P1 Ru1 2.3407(14) . ? 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 C2 C1 C6 118.0(5) . . ? C2 C1 P1 120.5(4) . . ? C6 C1 P1 121.3(4) . . ? C1 C2 C3 121.2(5) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 119.5(6) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 119.9(6) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.5(6) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.9(6) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C12 C7 C8 118.5(5) . . ? C12 C7 P1 123.3(4) . . ? C8 C7 P1 117.8(4) . . ? C9 C8 C7 120.3(6) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 119.7(6) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.7(6) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 119.8(6) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C7 120.9(6) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? P2 C13 P1 121.1(3) . . ? P2 C13 H13A 107.1 . . ? P1 C13 H13A 107.1 . . ? P2 C13 H13B 107.1 . . ? P1 C13 H13B 107.1 . . ? H13A C13 H13B 106.8 . . ? C15 C14 C19 119.5(5) . . ? C15 C14 P2 120.4(4) . . ? C19 C14 P2 120.1(5) . . ? C16 C15 C14 120.9(6) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C17 C16 C15 119.7(7) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.4(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C19 121.1(6) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C14 C19 C18 118.4(6) . . ? C14 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? C25 C20 C21 118.3(6) . . ? C25 C20 P2 120.1(5) . . ? C21 C20 P2 121.4(4) . . ? C22 C21 C20 120.3(6) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 120.5(6) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.3(7) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C25 120.6(8) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C20 120.0(7) . . ? C24 C25 H25 120.0 . . ? C20 C25 H25 120.0 . . ? O2 C26 C27 108.3(5) . . ? O2 C26 H26A 110.0 . . ? C27 C26 H26A 110.0 . . ? O2 C26 H26B 110.0 . . ? C27 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? 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 . . ? O3 C28 C29 107.5(5) . . ? O3 C28 H28A 110.2 . . ? C29 C28 H28A 110.2 . . ? O3 C28 H28B 110.2 . . ? C29 C28 H28B 110.2 . . ? H28A C28 H28B 108.5 . . ? 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 . . ? N2 C30 C31 122.3(5) . . ? N2 C30 H30 118.8 . . ? C31 C30 H30 118.8 . . ? C32 C31 C30 119.5(5) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 118.9(5) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C32 C33 C34 119.3(5) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? N2 C34 C33 121.7(5) . . ? N2 C34 C35 114.6(5) . . ? C33 C34 C35 123.5(5) . . ? N3 C35 C36 122.0(5) . . ? N3 C35 C34 115.5(5) . . ? C36 C35 C34 122.4(5) . . ? C35 C36 C37 120.8(6) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C38 C37 C36 117.8(5) . . ? C38 C37 H37 121.1 . . ? C36 C37 H37 121.1 . . ? C37 C38 C39 118.7(5) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.6 . . ? N3 C39 C38 123.8(5) . . ? N3 C39 H39 118.1 . . ? C38 C39 H39 118.1 . . ? N4 C40 C41 123.0(5) . . ? N4 C40 H40 118.5 . . ? C41 C40 H40 118.5 . . ? C40 C41 C42 118.6(5) . . ? C40 C41 H41 120.7 . . ? C42 C41 H41 120.7 . . ? C43 C42 C41 118.6(5) . . ? C43 C42 H42 120.7 . . ? C41 C42 H42 120.7 . . ? C42 C43 C44 120.3(5) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? N4 C44 C43 121.3(5) . . ? N4 C44 C45 115.7(4) . . ? C43 C44 C45 123.0(5) . . ? N5 C45 C46 120.7(5) . . ? N5 C45 C44 114.1(4) . . ? C46 C45 C44 125.2(5) . . ? C47 C46 C45 120.1(5) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 119.4(5) . . ? C46 C47 H47 120.3 . . ? C48 C47 H47 120.3 . . ? C49 C48 C47 118.3(5) . . ? C49 C48 H48 120.9 . . ? C47 C48 H48 120.9 . . ? N5 C49 C48 123.1(5) . . ? N5 C49 H49 118.5 . . ? C48 C49 H49 118.5 . . ? Cl2 C50 Cl1 112.2(4) . . ? Cl2 C50 H50A 109.2 . . ? Cl1 C50 H50A 109.2 . . ? Cl2 C50 H50B 109.2 . . ? Cl1 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? Cl4 C51 Cl3 114.1(6) . . ? Cl4 C51 H51A 108.7 . . ? Cl3 C51 H51A 108.7 . . ? Cl4 C51 H51B 108.7 . . ? Cl3 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? P3 N1 P2 132.5(3) . . ? C30 N2 C34 118.1(5) . . ? C30 N2 Ru1 126.1(4) . . ? C34 N2 Ru1 115.8(3) . . ? C39 N3 C35 116.7(4) . . ? C39 N3 Ru1 128.0(4) . . ? C35 N3 Ru1 115.3(3) . . ? C40 N4 C44 118.1(4) . . ? C40 N4 Ru1 126.6(3) . . ? C44 N4 Ru1 115.3(3) . . ? C49 N5 C45 118.5(4) . . ? C49 N5 Ru1 125.6(3) . . ? C45 N5 Ru1 115.9(3) . . ? P3 O1 Ru1 134.5(2) . . ? C26 O2 P3 120.9(3) . . ? C28 O3 P3 122.6(3) . . ? C7 P1 C1 100.2(2) . . ? C7 P1 C13 100.2(2) . . ? C1 P1 C13 104.5(2) . . ? C7 P1 Ru1 110.83(16) . . ? C1 P1 Ru1 121.81(18) . . ? C13 P1 Ru1 116.08(18) . . ? N1 P2 C14 108.1(3) . . ? N1 P2 C13 113.8(2) . . ? C14 P2 C13 110.7(3) . . ? N1 P2 C20 112.5(3) . . ? C14 P2 C20 105.7(3) . . ? C13 P2 C20 105.8(3) . . ? O1 P3 N1 119.1(2) . . ? O1 P3 O3 102.5(2) . . ? N1 P3 O3 113.6(2) . . ? O1 P3 O2 112.1(2) . . ? N1 P3 O2 102.2(2) . . ? O3 P3 O2 107.2(2) . . ? N4 Ru1 N5 79.06(16) . . ? N4 Ru1 N3 97.97(16) . . ? N5 Ru1 N3 169.52(16) . . ? N4 Ru1 N2 87.69(16) . . ? N5 Ru1 N2 92.44(16) . . ? N3 Ru1 N2 77.35(16) . . ? N4 Ru1 O1 168.08(15) . . ? N5 Ru1 O1 90.42(15) . . ? N3 Ru1 O1 91.39(15) . . ? N2 Ru1 O1 87.17(15) . . ? N4 Ru1 P1 91.92(12) . . ? N5 Ru1 P1 88.18(12) . . ? N3 Ru1 P1 102.02(12) . . ? N2 Ru1 P1 179.20(13) . . ? O1 Ru1 P1 93.34(10) . . ? F2 Sb1 F4 89.5(3) . . ? F2 Sb1 F1 91.5(3) . . ? F4 Sb1 F1 177.9(3) . . ? F2 Sb1 F3 91.1(2) . . ? F4 Sb1 F3 89.7(2) . . ? F1 Sb1 F3 92.1(2) . . ? F2 Sb1 F5 178.2(2) . . ? F4 Sb1 F5 90.6(3) . . ? F1 Sb1 F5 88.3(2) . . ? F3 Sb1 F5 90.7(2) . . ? F2 Sb1 F6 89.1(2) . . ? F4 Sb1 F6 89.1(2) . . ? F1 Sb1 F6 89.07(18) . . ? F3 Sb1 F6 178.8(2) . . ? F5 Sb1 F6 89.1(2) . . ? F10 Sb2 F11 91.9(2) . . ? F10 Sb2 F12 93.0(3) . . ? F11 Sb2 F12 91.6(2) . . ? F10 Sb2 F9 91.1(3) . . ? F11 Sb2 F9 89.8(2) . . ? F12 Sb2 F9 175.6(3) . . ? F10 Sb2 F8 89.5(3) . . ? F11 Sb2 F8 178.6(2) . . ? F12 Sb2 F8 88.0(2) . . ? F9 Sb2 F8 90.5(2) . . ? F10 Sb2 F7 178.4(2) . . ? F11 Sb2 F7 89.7(2) . . ? F12 Sb2 F7 87.3(2) . . ? F9 Sb2 F7 88.5(2) . . ? F8 Sb2 F7 89.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.7(8) . . . . ? P1 C1 C2 C3 178.0(4) . . . . ? C1 C2 C3 C4 -0.3(9) . . . . ? C2 C3 C4 C5 -0.3(9) . . . . ? C3 C4 C5 C6 -0.6(9) . . . . ? C4 C5 C6 C1 2.0(9) . . . . ? C2 C1 C6 C5 -2.5(8) . . . . ? P1 C1 C6 C5 -178.8(4) . . . . ? C12 C7 C8 C9 -1.1(8) . . . . ? P1 C7 C8 C9 172.0(4) . . . . ? C7 C8 C9 C10 0.3(9) . . . . ? C8 C9 C10 C11 0.4(9) . . . . ? C9 C10 C11 C12 -0.2(9) . . . . ? C10 C11 C12 C7 -0.7(9) . . . . ? C8 C7 C12 C11 1.3(8) . . . . ? P1 C7 C12 C11 -171.4(4) . . . . ? C19 C14 C15 C16 0.6(9) . . . . ? P2 C14 C15 C16 178.5(5) . . . . ? C14 C15 C16 C17 0.2(10) . . . . ? C15 C16 C17 C18 -0.5(11) . . . . ? C16 C17 C18 C19 0.1(11) . . . . ? C15 C14 C19 C18 -1.0(9) . . . . ? P2 C14 C19 C18 -178.9(5) . . . . ? C17 C18 C19 C14 0.7(10) . . . . ? C25 C20 C21 C22 1.6(10) . . . . ? P2 C20 C21 C22 175.9(5) . . . . ? C20 C21 C22 C23 -0.9(11) . . . . ? C21 C22 C23 C24 -1.8(13) . . . . ? C22 C23 C24 C25 3.8(17) . . . . ? C23 C24 C25 C20 -3.1(17) . . . . ? C21 C20 C25 C24 0.4(14) . . . . ? P2 C20 C25 C24 -174.0(8) . . . . ? N2 C30 C31 C32 -0.6(8) . . . . ? C30 C31 C32 C33 1.9(8) . . . . ? C31 C32 C33 C34 -0.7(9) . . . . ? C32 C33 C34 N2 -2.1(8) . . . . ? C32 C33 C34 C35 172.7(5) . . . . ? N2 C34 C35 N3 -0.8(7) . . . . ? C33 C34 C35 N3 -176.0(5) . . . . ? N2 C34 C35 C36 174.2(5) . . . . ? C33 C34 C35 C36 -0.9(9) . . . . ? N3 C35 C36 C37 2.0(9) . . . . ? C34 C35 C36 C37 -172.7(5) . . . . ? C35 C36 C37 C38 2.1(9) . . . . ? C36 C37 C38 C39 -3.4(9) . . . . ? C37 C38 C39 N3 0.9(9) . . . . ? N4 C40 C41 C42 -0.8(8) . . . . ? C40 C41 C42 C43 -1.5(9) . . . . ? C41 C42 C43 C44 1.9(9) . . . . ? C42 C43 C44 N4 0.0(8) . . . . ? C42 C43 C44 C45 -179.1(5) . . . . ? N4 C44 C45 N5 2.4(6) . . . . ? C43 C44 C45 N5 -178.4(5) . . . . ? N4 C44 C45 C46 -176.8(5) . . . . ? C43 C44 C45 C46 2.3(8) . . . . ? N5 C45 C46 C47 0.7(8) . . . . ? C44 C45 C46 C47 180.0(5) . . . . ? C45 C46 C47 C48 0.1(9) . . . . ? C46 C47 C48 C49 -1.0(8) . . . . ? C47 C48 C49 N5 1.1(8) . . . . ? C31 C30 N2 C34 -2.1(8) . . . . ? C31 C30 N2 Ru1 176.5(4) . . . . ? C33 C34 N2 C30 3.4(7) . . . . ? C35 C34 N2 C30 -171.8(4) . . . . ? C33 C34 N2 Ru1 -175.3(4) . . . . ? C35 C34 N2 Ru1 9.4(6) . . . . ? C38 C39 N3 C35 3.1(8) . . . . ? C38 C39 N3 Ru1 -178.3(4) . . . . ? C36 C35 N3 C39 -4.5(8) . . . . ? C34 C35 N3 C39 170.5(5) . . . . ? C36 C35 N3 Ru1 176.8(4) . . . . ? C34 C35 N3 Ru1 -8.2(6) . . . . ? C41 C40 N4 C44 2.7(8) . . . . ? C41 C40 N4 Ru1 -178.5(4) . . . . ? C43 C44 N4 C40 -2.2(7) . . . . ? C45 C44 N4 C40 176.9(4) . . . . ? C43 C44 N4 Ru1 178.8(4) . . . . ? C45 C44 N4 Ru1 -2.1(6) . . . . ? C48 C49 N5 C45 -0.3(8) . . . . ? C48 C49 N5 Ru1 -178.4(4) . . . . ? C46 C45 N5 C49 -0.6(7) . . . . ? C44 C45 N5 C49 -179.9(4) . . . . ? C46 C45 N5 Ru1 177.6(4) . . . . ? C44 C45 N5 Ru1 -1.7(5) . . . . ? C27 C26 O2 P3 171.9(4) . . . . ? C29 C28 O3 P3 164.1(4) . . . . ? C12 C7 P1 C1 -143.2(4) . . . . ? C8 C7 P1 C1 44.0(4) . . . . ? C12 C7 P1 C13 -36.3(5) . . . . ? C8 C7 P1 C13 150.9(4) . . . . ? C12 C7 P1 Ru1 86.8(4) . . . . ? C8 C7 P1 Ru1 -85.9(4) . . . . ? C2 C1 P1 C7 -118.5(5) . . . . ? C6 C1 P1 C7 57.7(5) . . . . ? C2 C1 P1 C13 138.1(4) . . . . ? C6 C1 P1 C13 -45.8(5) . . . . ? C2 C1 P1 Ru1 4.0(5) . . . . ? C6 C1 P1 Ru1 -179.8(4) . . . . ? P2 C13 P1 C7 -175.2(3) . . . . ? P2 C13 P1 C1 -71.7(4) . . . . ? P2 C13 P1 Ru1 65.4(4) . . . . ? P3 N1 P2 C14 -154.1(4) . . . . ? P3 N1 P2 C13 -30.8(5) . . . . ? P3 N1 P2 C20 89.6(4) . . . . ? C15 C14 P2 N1 -178.6(5) . . . . ? C19 C14 P2 N1 -0.8(5) . . . . ? C15 C14 P2 C13 56.1(5) . . . . ? C19 C14 P2 C13 -126.0(5) . . . . ? C15 C14 P2 C20 -58.0(5) . . . . ? C19 C14 P2 C20 119.9(5) . . . . ? P1 C13 P2 N1 -55.0(4) . . . . ? P1 C13 P2 C14 67.0(4) . . . . ? P1 C13 P2 C20 -179.0(3) . . . . ? C25 C20 P2 N1 87.7(7) . . . . ? C21 C20 P2 N1 -86.6(5) . . . . ? C25 C20 P2 C14 -30.1(7) . . . . ? C21 C20 P2 C14 155.6(5) . . . . ? C25 C20 P2 C13 -147.5(6) . . . . ? C21 C20 P2 C13 38.2(6) . . . . ? Ru1 O1 P3 N1 44.0(4) . . . . ? Ru1 O1 P3 O3 170.4(3) . . . . ? Ru1 O1 P3 O2 -75.1(4) . . . . ? P2 N1 P3 O1 46.3(5) . . . . ? P2 N1 P3 O3 -74.6(5) . . . . ? P2 N1 P3 O2 170.3(4) . . . . ? C28 O3 P3 O1 -175.4(4) . . . . ? C28 O3 P3 N1 -45.6(5) . . . . ? C28 O3 P3 O2 66.5(5) . . . . ? C26 O2 P3 O1 -50.4(5) . . . . ? C26 O2 P3 N1 -179.1(4) . . . . ? C26 O2 P3 O3 61.2(5) . . . . ? C40 N4 Ru1 N5 -178.0(4) . . . . ? C44 N4 Ru1 N5 0.9(3) . . . . ? C40 N4 Ru1 N3 -8.1(4) . . . . ? C44 N4 Ru1 N3 170.7(3) . . . . ? C40 N4 Ru1 N2 -85.0(4) . . . . ? C44 N4 Ru1 N2 93.8(4) . . . . ? C40 N4 Ru1 O1 -149.6(6) . . . . ? C44 N4 Ru1 O1 29.3(9) . . . . ? C40 N4 Ru1 P1 94.3(4) . . . . ? C44 N4 Ru1 P1 -86.9(3) . . . . ? C49 N5 Ru1 N4 178.6(4) . . . . ? C45 N5 Ru1 N4 0.5(3) . . . . ? C49 N5 Ru1 N3 104.2(9) . . . . ? C45 N5 Ru1 N3 -73.9(10) . . . . ? C49 N5 Ru1 N2 91.4(4) . . . . ? C45 N5 Ru1 N2 -86.7(4) . . . . ? C49 N5 Ru1 O1 4.3(4) . . . . ? C45 N5 Ru1 O1 -173.9(3) . . . . ? C49 N5 Ru1 P1 -89.1(4) . . . . ? C45 N5 Ru1 P1 92.8(3) . . . . ? C39 N3 Ru1 N4 105.6(4) . . . . ? C35 N3 Ru1 N4 -75.8(4) . . . . ? C39 N3 Ru1 N5 178.3(8) . . . . ? C35 N3 Ru1 N5 -3.1(11) . . . . ? C39 N3 Ru1 N2 -168.6(5) . . . . ? C35 N3 Ru1 N2 10.0(4) . . . . ? C39 N3 Ru1 O1 -81.8(4) . . . . ? C35 N3 Ru1 O1 96.8(4) . . . . ? C39 N3 Ru1 P1 11.9(4) . . . . ? C35 N3 Ru1 P1 -169.5(3) . . . . ? C30 N2 Ru1 N4 -90.5(4) . . . . ? C34 N2 Ru1 N4 88.1(4) . . . . ? C30 N2 Ru1 N5 -11.6(4) . . . . ? C34 N2 Ru1 N5 167.1(4) . . . . ? C30 N2 Ru1 N3 170.8(4) . . . . ? C34 N2 Ru1 N3 -10.6(3) . . . . ? C30 N2 Ru1 O1 78.7(4) . . . . ? C34 N2 Ru1 O1 -102.6(4) . . . . ? C30 N2 Ru1 P1 -151(8) . . . . ? C34 N2 Ru1 P1 27(9) . . . . ? P3 O1 Ru1 N4 173.7(6) . . . . ? P3 O1 Ru1 N5 -158.4(3) . . . . ? P3 O1 Ru1 N3 31.9(3) . . . . ? P3 O1 Ru1 N2 109.1(3) . . . . ? P3 O1 Ru1 P1 -70.2(3) . . . . ? C7 P1 Ru1 N4 56.5(2) . . . . ? C1 P1 Ru1 N4 -60.9(2) . . . . ? C13 P1 Ru1 N4 169.9(2) . . . . ? C7 P1 Ru1 N5 -22.5(2) . . . . ? C1 P1 Ru1 N5 -139.8(2) . . . . ? C13 P1 Ru1 N5 90.9(2) . . . . ? C7 P1 Ru1 N3 155.1(2) . . . . ? C1 P1 Ru1 N3 37.7(2) . . . . ? C13 P1 Ru1 N3 -91.5(2) . . . . ? C7 P1 Ru1 N2 117(9) . . . . ? C1 P1 Ru1 N2 0(9) . . . . ? C13 P1 Ru1 N2 -129(9) . . . . ? C7 P1 Ru1 O1 -112.8(2) . . . . ? C1 P1 Ru1 O1 129.8(2) . . . . ? C13 P1 Ru1 O1 0.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.132 _refine_diff_density_min -1.268 _refine_diff_density_rms 0.240 #==END #=============================================================================== data_9a _database_code_depnum_ccdc_archive 'CCDC 690031' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H48 N5 O3 P3 Ru, Cl, 0.5(C H2 Cl2)' _chemical_formula_sum 'C49.50 H48 Cl2 N5 O3 P3 Ru' _chemical_formula_weight 1025.81 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1860(6) _cell_length_b 12.3134(7) _cell_length_c 21.3860(13) _cell_angle_alpha 96.780(5) _cell_angle_beta 100.137(5) _cell_angle_gamma 113.644(5) _cell_volume 2365.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6425 _cell_measurement_theta_min 3.9997 _cell_measurement_theta_max 73.6813 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1054 _exptl_absorpt_coefficient_mu 5.063 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.75605 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur Nova ; _diffrn_measurement_device ; 165 mm Onyx CCD detector in \k-geometry diffractometer ; _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.2640 _diffrn_standards_number 23986 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23986 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.1087 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 74.21 _reflns_number_total 8598 _reflns_number_gt 4612 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2007)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8598 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1667 _refine_ls_wR_factor_gt 0.1433 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0211(8) 0.7357(6) 0.2079(4) 0.055(2) Uani 1 1 d . . . C2 C 0.1422(9) 0.8374(5) 0.2468(4) 0.067(2) Uani 1 1 d . . . H2 H 0.2323 0.8323 0.2625 0.080 Uiso 1 1 calc R . . C3 C 0.1334(10) 0.9445(6) 0.2626(5) 0.089(3) Uani 1 1 d . . . H3 H 0.2166 1.0124 0.2900 0.106 Uiso 1 1 calc R . . C4 C 0.0065(10) 0.9553(7) 0.2394(6) 0.111(5) Uani 1 1 d . . . H4 H 0.0007 1.0300 0.2506 0.133 Uiso 1 1 calc R . . C5 C -0.1138(10) 0.8554(7) 0.1992(6) 0.091(3) Uani 1 1 d . . . H5 H -0.2023 0.8625 0.1828 0.109 Uiso 1 1 calc R . . C6 C -0.1081(8) 0.7463(6) 0.1826(5) 0.069(2) Uani 1 1 d . . . H6 H -0.1909 0.6792 0.1543 0.082 Uiso 1 1 calc R . . C7 C 0.1956(8) 0.6236(6) 0.1666(3) 0.0484(18) Uani 1 1 d . . . C8 C 0.1875(9) 0.5887(7) 0.1003(4) 0.063(2) Uani 1 1 d . . . H8 H 0.0941 0.5530 0.0697 0.076 Uiso 1 1 calc R . . C9 C 0.314(1) 0.6060(9) 0.0791(4) 0.080(3) Uani 1 1 d . . . H9 H 0.3065 0.5819 0.0343 0.096 Uiso 1 1 calc R . . C10 C 0.4487(10) 0.6571(9) 0.1220(5) 0.084(3) Uani 1 1 d . . . H10 H 0.5346 0.6675 0.1071 0.101 Uiso 1 1 calc R . . C11 C 0.4610(8) 0.6943(7) 0.1876(4) 0.070(2) Uani 1 1 d . . . H11 H 0.5555 0.7317 0.2173 0.084 Uiso 1 1 calc R . . C12 C 0.3343(8) 0.6765(7) 0.2097(4) 0.062(2) Uani 1 1 d . . . H12 H 0.3430 0.7009 0.2546 0.074 Uiso 1 1 calc R . . C13 C -0.1273(7) 0.4958(6) 0.1290(3) 0.0436(16) Uani 1 1 d . . . C14 C -0.1305(6) 0.2551(6) 0.0981(3) 0.0412(15) Uani 1 1 d . . . C15 C -0.1023(7) 0.1699(6) 0.1279(3) 0.0490(18) Uani 1 1 d . . . H15 H -0.1348 0.1526 0.1661 0.059 Uiso 1 1 calc R . . C16 C -0.0278(8) 0.1099(6) 0.1030(5) 0.080(3) Uani 1 1 d . . . H16 H -0.0079 0.0527 0.1243 0.096 Uiso 1 1 calc R . . C17 C 0.0178(9) 0.1336(8) 0.0469(6) 0.095(4) Uani 1 1 d . . . H17 H 0.0727 0.0950 0.0306 0.114 Uiso 1 1 calc R . . C18 C -0.0156(8) 0.2124(9) 0.0148(4) 0.083(3) Uani 1 1 d . . . H18 H 0.0122 0.2256 -0.0248 0.100 Uiso 1 1 calc R . . C19 C -0.0910(7) 0.2737(7) 0.0400(3) 0.0556(19) Uani 1 1 d . . . H19 H -0.1149 0.3279 0.0175 0.067 Uiso 1 1 calc R . . C20 C -0.3949(7) 0.2892(6) 0.0788(3) 0.0432(16) Uani 1 1 d . . . C21 C -0.4759(8) 0.3579(7) 0.0824(4) 0.059(2) Uani 1 1 d . . . H21 H -0.4379 0.4302 0.1147 0.071 Uiso 1 1 calc R . . C22 C -0.6119(8) 0.3202(8) 0.0387(4) 0.068(2) Uani 1 1 d . . . H22 H -0.6665 0.3669 0.0409 0.081 Uiso 1 1 calc R . . C23 C -0.6678(9) 0.2144(8) -0.0082(4) 0.067(2) Uani 1 1 d . . . H23 H -0.7608 0.1890 -0.0379 0.080 Uiso 1 1 calc R . . C24 C -0.5901(7) 0.1464(7) -0.0120(3) 0.0553(19) Uani 1 1 d . . . H24 H -0.6288 0.0737 -0.0440 0.066 Uiso 1 1 calc R . . C25 C -0.4532(7) 0.1855(7) 0.0317(3) 0.0480(17) Uani 1 1 d . . . H25 H -0.3988 0.1388 0.0287 0.058 Uiso 1 1 calc R . . C26 C -0.2544(12) 0.0832(9) 0.3074(6) 0.115(4) Uani 1 1 d . . . H26B H -0.1723 0.0600 0.3193 0.138 Uiso 1 1 calc R . . H26A H -0.2586 0.1289 0.3477 0.138 Uiso 1 1 calc R . . C27 C -0.3785(14) -0.0187(10) 0.2890(7) 0.189(8) Uani 1 1 d . . . H27A H -0.4611 -0.0020 0.2971 0.283 Uiso 1 1 calc R . . H27B H -0.3688 -0.0782 0.3138 0.283 Uiso 1 1 calc R . . H27C H -0.3972 -0.0511 0.2426 0.283 Uiso 1 1 calc R . . C28 C -0.5838(8) 0.0798(6) 0.1623(3) 0.0542(18) Uani 1 1 d . . . H28B H -0.6194 0.1315 0.1390 0.065 Uiso 1 1 calc R . . H28A H -0.6113 0.0800 0.2044 0.065 Uiso 1 1 calc R . . C29 C -0.6525(9) -0.0455(6) 0.1232(4) 0.066(2) Uani 1 1 d . . . H29C H -0.6222 -0.0453 0.0821 0.099 Uiso 1 1 calc R . . H29A H -0.7604 -0.0772 0.1141 0.099 Uiso 1 1 calc R . . H29B H -0.6204 -0.0970 0.1474 0.099 Uiso 1 1 calc R . . C30 C 0.1876(7) 0.3861(5) 0.2242(3) 0.0420(15) Uani 1 1 d . . . H30 H 0.1694 0.4182 0.1871 0.050 Uiso 1 1 calc R . . C31 C 0.2839(6) 0.3336(5) 0.2277(3) 0.0403(15) Uani 1 1 d . . . H31 H 0.3309 0.3301 0.1933 0.048 Uiso 1 1 calc R . . C32 C 0.3130(8) 0.2853(6) 0.2813(4) 0.0556(18) Uani 1 1 d . . . H32 H 0.3832 0.2523 0.2857 0.067 Uiso 1 1 calc R . . C33 C 0.2349(8) 0.2875(6) 0.3280(3) 0.0534(18) Uani 1 1 d . . . H33 H 0.2474 0.2509 0.3639 0.064 Uiso 1 1 calc R . . C34 C 0.1392(7) 0.3417(5) 0.3235(3) 0.0431(16) Uani 1 1 d . . . C35 C 0.0554(8) 0.3476(6) 0.3712(3) 0.054(2) Uani 1 1 d . . . C36 C 0.0677(8) 0.3015(8) 0.4274(3) 0.070(2) Uani 1 1 d . . . H36 H 0.1355 0.2673 0.4375 0.084 Uiso 1 1 calc R . . C37 C -0.0233(10) 0.3074(9) 0.4683(4) 0.088(3) Uani 1 1 d . . . H37 H -0.0185 0.2760 0.5067 0.106 Uiso 1 1 calc R . . C38 C -0.1184(10) 0.3577(7) 0.4536(4) 0.071(3) Uani 1 1 d . . . H38 H -0.1819 0.3598 0.4809 0.085 Uiso 1 1 calc R . . C39 C -0.1221(8) 0.4056(6) 0.3988(3) 0.0512(19) Uani 1 1 d . . . H39 H -0.1869 0.4428 0.3893 0.061 Uiso 1 1 calc R . . C40 C -0.2726(9) 0.5464(6) 0.2846(4) 0.060(2) Uani 1 1 d . . . H40 H -0.3304 0.4715 0.2545 0.072 Uiso 1 1 calc R . . C41 C -0.3426(10) 0.6132(7) 0.3071(4) 0.072(3) Uani 1 1 d . . . H41 H -0.4471 0.5831 0.2941 0.087 Uiso 1 1 calc R . . C42 C -0.2572(13) 0.7253(8) 0.3492(4) 0.083(3) Uani 1 1 d . . . H42 H -0.3013 0.7751 0.3639 0.099 Uiso 1 1 calc R . . C43 C -0.1114(12) 0.7607(7) 0.3683(4) 0.077(3) Uani 1 1 d . . . H43 H -0.0522 0.8365 0.3974 0.092 Uiso 1 1 calc R . . C44 C -0.0437(10) 0.6913(6) 0.3472(4) 0.060(2) Uani 1 1 d . . . C45 C 0.1111(10) 0.7203(5) 0.3695(4) 0.064(2) Uani 1 1 d . . . C46 C 0.2188(12) 0.8236(6) 0.4161(4) 0.092(4) Uani 1 1 d . . . H46 H 0.1917 0.8840 0.4336 0.110 Uiso 1 1 calc R . . C47 C 0.3567(12) 0.8374(8) 0.4359(5) 0.119(5) Uani 1 1 d . . . H47 H 0.4284 0.9089 0.4657 0.143 Uiso 1 1 calc R . . C48 C 0.3957(10) 0.7488(7) 0.4133(4) 0.098(4) Uani 1 1 d . . . H48 H 0.4932 0.7565 0.4284 0.118 Uiso 1 1 calc R . . C49 C 0.2908(9) 0.6478(6) 0.3682(4) 0.071(3) Uani 1 1 d . . . H49 H 0.3183 0.5866 0.3524 0.085 Uiso 1 1 calc R . . N1 N -0.2035(5) 0.3381(4) 0.2083(2) 0.0359(12) Uani 1 1 d . . . N2 N 0.1174(5) 0.3942(4) 0.2716(2) 0.0372(12) Uani 1 1 d . . . N3 N -0.0368(6) 0.4014(4) 0.3584(2) 0.0419(14) Uani 1 1 d . . . N4 N -0.1268(7) 0.5835(4) 0.3037(3) 0.0518(16) Uani 1 1 d . . . N5 N 0.1513(6) 0.6323(4) 0.3455(3) 0.0538(17) Uani 1 1 d . . . O1 O -0.3904(5) 0.2583(4) 0.2808(2) 0.0571(14) Uani 1 1 d . . . O2 O -0.2137(5) 0.1658(4) 0.2651(2) 0.0551(12) Uani 1 1 d . . . O3 O -0.4236(5) 0.1272(3) 0.1731(2) 0.0417(10) Uani 1 1 d . . . P1 P 0.02235(19) 0.58615(14) 0.19291(9) 0.0434(4) Uani 1 1 d . . . P2 P -0.21187(17) 0.34755(14) 0.13274(8) 0.0377(4) Uani 1 1 d . . . P3 P -0.31232(19) 0.22686(13) 0.23531(8) 0.0416(4) Uani 1 1 d . . . Ru1 Ru -0.01119(6) 0.48823(4) 0.27899(3) 0.04245(18) Uani 1 1 d . . . Cl1 Cl 0.2598(5) 0.1247(3) 0.46075(15) 0.1404(14) Uani 1 1 d . . . Cl2 Cl 0.5780(3) 0.4926(3) 0.44998(16) 0.1276(12) Uani 1 1 d . . . C50 C 0.534(3) 0.4510(18) 0.5114(9) 0.101(7) Uani 0.50 1 d P . -1 H50B H 0.6265 0.4720 0.5444 0.121 Uiso 0.50 1 calc PR . -1 H50A H 0.4806 0.3614 0.5004 0.121 Uiso 0.50 1 calc PR . -1 H13 H -0.152(7) 0.505(6) 0.081(3) 0.056(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.069(5) 0.032(3) 0.096(6) 0.043(4) 0.060(4) 0.028(3) C2 0.085(5) 0.022(3) 0.116(7) 0.035(4) 0.067(5) 0.022(3) C3 0.092(6) 0.019(3) 0.170(10) 0.031(5) 0.080(7) 0.016(4) C4 0.094(7) 0.040(5) 0.229(14) 0.033(7) 0.097(9) 0.035(5) C5 0.077(6) 0.047(5) 0.189(11) 0.061(6) 0.073(7) 0.041(4) C6 0.062(5) 0.029(3) 0.138(8) 0.041(4) 0.055(5) 0.025(3) C7 0.067(5) 0.035(3) 0.070(5) 0.035(4) 0.038(4) 0.034(3) C8 0.069(5) 0.087(6) 0.075(5) 0.054(5) 0.048(4) 0.053(5) C9 0.092(7) 0.135(9) 0.082(6) 0.075(6) 0.063(6) 0.086(7) C10 0.084(6) 0.127(8) 0.122(8) 0.099(7) 0.083(6) 0.081(6) C11 0.056(5) 0.073(5) 0.110(7) 0.063(5) 0.044(5) 0.034(4) C12 0.057(5) 0.063(5) 0.090(6) 0.049(5) 0.045(4) 0.030(4) C13 0.049(4) 0.051(4) 0.048(4) 0.028(3) 0.024(3) 0.028(3) C14 0.033(3) 0.053(4) 0.031(3) -0.009(3) 0.002(3) 0.019(3) C15 0.042(4) 0.044(4) 0.059(5) -0.007(3) 0.010(3) 0.023(3) C16 0.049(5) 0.033(4) 0.169(10) 0.013(5) 0.039(5) 0.025(3) C17 0.056(5) 0.057(5) 0.158(11) -0.029(6) 0.056(6) 0.013(4) C18 0.035(4) 0.119(8) 0.070(6) -0.030(6) 0.021(4) 0.019(5) C19 0.049(4) 0.085(5) 0.039(4) 0.007(4) 0.013(3) 0.036(4) C20 0.045(4) 0.064(4) 0.041(4) 0.028(3) 0.026(3) 0.033(3) C21 0.059(5) 0.076(5) 0.076(5) 0.035(4) 0.045(4) 0.044(4) C22 0.049(5) 0.092(6) 0.105(7) 0.056(6) 0.042(5) 0.053(5) C23 0.057(5) 0.101(7) 0.071(6) 0.040(5) 0.037(4) 0.049(5) C24 0.045(4) 0.075(5) 0.049(4) 0.018(4) 0.021(3) 0.023(4) C25 0.047(4) 0.077(5) 0.033(4) 0.016(4) 0.014(3) 0.037(4) C26 0.136(10) 0.084(7) 0.158(11) 0.098(8) 0.068(9) 0.047(7) C27 0.123(11) 0.100(9) 0.243(18) 0.091(11) -0.052(11) -0.028(8) C28 0.061(4) 0.049(4) 0.051(4) 0.011(3) 0.018(4) 0.019(3) C29 0.079(5) 0.045(4) 0.050(5) -0.005(4) -0.001(4) 0.014(4) C30 0.048(4) 0.042(3) 0.038(4) 0.007(3) 0.024(3) 0.016(3) C31 0.043(3) 0.030(3) 0.043(4) 0.010(3) 0.012(3) 0.009(3) C32 0.049(4) 0.046(4) 0.069(5) 0.014(4) 0.010(4) 0.019(3) C33 0.063(5) 0.035(4) 0.051(4) 0.021(3) 0.010(3) 0.008(3) C34 0.045(4) 0.030(3) 0.036(4) 0.003(3) 0.010(3) -0.001(3) C35 0.054(4) 0.048(4) 0.029(4) 0.000(3) 0.010(3) -0.006(3) C36 0.051(4) 0.092(6) 0.046(4) 0.027(4) 0.011(4) 0.008(4) C37 0.085(7) 0.096(7) 0.039(5) 0.024(5) 0.016(4) -0.010(5) C38 0.077(6) 0.069(5) 0.039(4) 0.006(4) 0.026(4) 0.002(4) C39 0.067(4) 0.039(3) 0.035(4) 0.006(3) 0.028(3) 0.004(3) C40 0.090(6) 0.029(3) 0.080(5) 0.020(4) 0.059(5) 0.026(4) C41 0.109(7) 0.066(5) 0.097(7) 0.047(5) 0.076(6) 0.064(5) C42 0.168(10) 0.072(6) 0.081(7) 0.050(5) 0.081(7) 0.094(7) C43 0.158(9) 0.044(4) 0.068(6) 0.032(4) 0.070(6) 0.061(6) C44 0.107(6) 0.031(3) 0.064(5) 0.017(3) 0.064(5) 0.031(4) C45 0.114(7) 0.018(3) 0.060(5) 0.007(3) 0.061(5) 0.012(3) C46 0.149(9) 0.020(3) 0.077(6) -0.005(4) 0.075(6) -0.008(4) C47 0.109(8) 0.065(6) 0.102(8) -0.037(5) 0.075(7) -0.048(5) C48 0.079(6) 0.063(5) 0.090(7) -0.037(5) 0.051(5) -0.030(4) C49 0.071(5) 0.045(4) 0.079(6) 0.003(4) 0.049(5) -0.002(4) N1 0.059(3) 0.022(2) 0.031(3) 0.007(2) 0.019(2) 0.018(2) N2 0.040(3) 0.036(3) 0.026(3) 0.004(2) 0.011(2) 0.006(2) N3 0.047(3) 0.025(2) 0.032(3) -0.010(2) 0.017(2) -0.004(2) N4 0.078(4) 0.033(3) 0.064(4) 0.021(3) 0.055(3) 0.025(3) N5 0.066(4) 0.020(2) 0.070(4) 0.006(3) 0.052(3) 0.000(2) O1 0.067(3) 0.041(2) 0.051(3) 0.002(2) 0.042(2) 0.002(2) O2 0.068(3) 0.040(3) 0.048(3) 0.013(2) 0.000(2) 0.019(2) O3 0.051(3) 0.028(2) 0.044(3) 0.0050(19) 0.014(2) 0.0152(18) P1 0.0573(10) 0.0298(8) 0.0634(11) 0.0274(8) 0.0401(9) 0.0237(7) P2 0.0461(9) 0.0413(9) 0.0390(9) 0.0135(7) 0.0217(7) 0.0259(7) P3 0.0569(10) 0.0240(7) 0.0398(9) 0.0084(7) 0.0181(8) 0.0104(7) Ru1 0.0555(3) 0.0258(2) 0.0482(3) 0.0096(2) 0.0325(2) 0.0111(2) Cl1 0.264(4) 0.112(2) 0.109(2) 0.043(2) 0.069(3) 0.130(3) Cl2 0.097(2) 0.131(3) 0.126(3) -0.025(2) 0.0125(19) 0.0403(18) C50 0.15(2) 0.085(14) 0.075(13) 0.041(11) 0.047(14) 0.048(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.391(10) . ? C1 C6 1.395(10) . ? C1 P1 1.837(6) . ? C2 C3 1.364(9) . ? C2 H2 0.9500 . ? C3 C4 1.364(13) . ? C3 H3 0.9500 . ? C4 C5 1.388(13) . ? C4 H4 0.9500 . ? C5 C6 1.375(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.39(1) . ? C7 C8 1.41(1) . ? C7 P1 1.844(6) . ? C8 C9 1.385(9) . ? C8 H8 0.9500 . ? C9 C10 1.359(12) . ? C9 H9 0.9500 . ? C10 C11 1.390(12) . ? C10 H10 0.9500 . ? C11 C12 1.397(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 P2 1.696(6) . ? C13 P1 1.725(7) . ? C13 H13 1.04(6) . ? C14 C19 1.387(9) . ? C14 C15 1.387(9) . ? C14 P2 1.819(6) . ? C15 C16 1.380(9) . ? C15 H15 0.9500 . ? C16 C17 1.382(13) . ? C16 H16 0.9500 . ? C17 C18 1.367(13) . ? C17 H17 0.9500 . ? C18 C19 1.402(10) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.369(9) . ? C20 C21 1.404(9) . ? C20 P2 1.815(7) . ? C21 C22 1.392(11) . ? C21 H21 0.9500 . ? C22 C23 1.386(11) . ? C22 H22 0.9500 . ? C23 C24 1.368(10) . ? C23 H23 0.9500 . ? C24 C25 1.395(9) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.328(13) . ? C26 O2 1.428(9) . ? C26 H26B 0.9900 . ? C26 H26A 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 O3 1.459(8) . ? C28 C29 1.481(9) . ? C28 H28B 0.9900 . ? C28 H28A 0.9900 . ? C29 H29C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N2 1.356(7) . ? C30 C31 1.371(8) . ? C30 H30 0.9500 . ? C31 C32 1.394(9) . ? C31 H31 0.9500 . ? C32 C33 1.387(9) . ? C32 H32 0.9500 . ? C33 C34 1.382(9) . ? C33 H33 0.9500 . ? C34 N2 1.377(8) . ? C34 C35 1.454(9) . ? C35 N3 1.358(9) . ? C35 C36 1.396(9) . ? C36 C37 1.399(11) . ? C36 H36 0.9500 . ? C37 C38 1.357(12) . ? C37 H37 0.9500 . ? C38 C39 1.374(10) . ? C38 H38 0.9500 . ? C39 N3 1.340(7) . ? C39 H39 0.9500 . ? C40 N4 1.334(9) . ? C40 C41 1.384(9) . ? C40 H40 0.9500 . ? C41 C42 1.392(12) . ? C41 H41 0.9500 . ? C42 C43 1.338(13) . ? C42 H42 0.9500 . ? C43 C44 1.378(10) . ? C43 H43 0.9500 . ? C44 N4 1.369(9) . ? C44 C45 1.444(11) . ? C45 N5 1.379(8) . ? C45 C46 1.419(10) . ? C46 C47 1.329(15) . ? C46 H46 0.9500 . ? C47 C48 1.369(13) . ? C47 H47 0.9500 . ? C48 C49 1.381(10) . ? C48 H48 0.9500 . ? C49 N5 1.345(10) . ? C49 H49 0.9500 . ? N1 P2 1.622(5) . ? N1 P3 1.623(5) . ? N1 Ru1 2.222(5) . ? N2 Ru1 2.080(5) . ? N3 Ru1 2.112(5) . ? N4 Ru1 2.055(5) . ? N5 Ru1 2.033(5) . ? O1 P3 1.469(4) . ? O2 P3 1.573(5) . ? O3 P3 1.590(4) . ? P1 Ru1 2.3183(17) . ? Cl2 C50 1.540(17) . ? Cl2 C50 1.82(2) 2_666 ? C50 Cl2 1.82(2) 2_666 ? C50 H50B 0.9900 . ? C50 H50A 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 C2 C1 C6 118.8(6) . . ? C2 C1 P1 122.1(6) . . ? C6 C1 P1 119.0(6) . . ? C3 C2 C1 120.9(8) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 120.8(9) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 118.8(8) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 121.6(9) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C1 118.9(8) . . ? C5 C6 H6 120.5 . . ? C1 C6 H6 120.5 . . ? C12 C7 C8 117.9(6) . . ? C12 C7 P1 123.0(5) . . ? C8 C7 P1 118.9(6) . . ? C9 C8 C7 120.8(8) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 120.6(8) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.2(7) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C12 119.9(8) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 120.6(8) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? P2 C13 P1 115.6(4) . . ? P2 C13 H13 110(4) . . ? P1 C13 H13 130(4) . . ? C19 C14 C15 118.8(6) . . ? C19 C14 P2 118.1(6) . . ? C15 C14 P2 123.1(5) . . ? C16 C15 C14 121.1(8) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 119.6(9) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 120.3(7) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.2(8) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C14 C19 C18 119.8(8) . . ? C14 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C25 C20 C21 118.4(6) . . ? C25 C20 P2 122.9(5) . . ? C21 C20 P2 118.5(6) . . ? C22 C21 C20 119.9(8) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.0(7) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.6(8) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.0(8) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C20 C25 C24 122.1(6) . . ? C20 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C27 C26 O2 121.2(11) . . ? C27 C26 H26B 107.0 . . ? O2 C26 H26B 107.0 . . ? C27 C26 H26A 107.0 . . ? O2 C26 H26A 107.0 . . ? H26B C26 H26A 106.8 . . ? 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 . . ? O3 C28 C29 108.7(6) . . ? O3 C28 H28B 109.9 . . ? C29 C28 H28B 109.9 . . ? O3 C28 H28A 109.9 . . ? C29 C28 H28A 109.9 . . ? H28B C28 H28A 108.3 . . ? C28 C29 H29C 109.5 . . ? C28 C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29C C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N2 C30 C31 122.7(6) . . ? N2 C30 H30 118.6 . . ? C31 C30 H30 118.6 . . ? C30 C31 C32 120.3(6) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 116.9(7) . . ? C33 C32 H32 121.6 . . ? C31 C32 H32 121.6 . . ? C34 C33 C32 121.5(7) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? N2 C34 C33 120.6(6) . . ? N2 C34 C35 115.5(6) . . ? C33 C34 C35 123.9(7) . . ? N3 C35 C36 121.0(7) . . ? N3 C35 C34 116.3(6) . . ? C36 C35 C34 122.6(8) . . ? C35 C36 C37 117.6(9) . . ? C35 C36 H36 121.2 . . ? C37 C36 H36 121.2 . . ? C38 C37 C36 120.5(8) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 119.4(7) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? N3 C39 C38 121.7(8) . . ? N3 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? N4 C40 C41 122.2(7) . . ? N4 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C40 C41 C42 118.9(9) . . ? C40 C41 H41 120.6 . . ? C42 C41 H41 120.6 . . ? C43 C42 C41 118.0(7) . . ? C43 C42 H42 121.0 . . ? C41 C42 H42 121.0 . . ? C42 C43 C44 122.4(9) . . ? C42 C43 H43 118.8 . . ? C44 C43 H43 118.8 . . ? N4 C44 C43 119.5(8) . . ? N4 C44 C45 115.4(6) . . ? C43 C44 C45 125.0(8) . . ? N5 C45 C46 118.7(9) . . ? N5 C45 C44 114.7(6) . . ? C46 C45 C44 126.4(7) . . ? C47 C46 C45 121.2(8) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C48 120.1(8) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C49 118.8(10) . . ? C47 C48 H48 120.6 . . ? C49 C48 H48 120.6 . . ? N5 C49 C48 122.9(8) . . ? N5 C49 H49 118.6 . . ? C48 C49 H49 118.6 . . ? P2 N1 P3 126.6(3) . . ? P2 N1 Ru1 114.8(2) . . ? P3 N1 Ru1 118.4(3) . . ? C30 N2 C34 117.8(6) . . ? C30 N2 Ru1 127.4(4) . . ? C34 N2 Ru1 114.7(4) . . ? C39 N3 C35 119.7(6) . . ? C39 N3 Ru1 126.1(5) . . ? C35 N3 Ru1 113.8(4) . . ? C40 N4 C44 118.8(6) . . ? C40 N4 Ru1 126.2(4) . . ? C44 N4 Ru1 114.9(5) . . ? C49 N5 C45 118.3(6) . . ? C49 N5 Ru1 126.1(4) . . ? C45 N5 Ru1 115.6(5) . . ? C26 O2 P3 123.9(6) . . ? C28 O3 P3 122.7(4) . . ? C13 P1 C1 107.0(4) . . ? C13 P1 C7 110.0(3) . . ? C1 P1 C7 101.1(3) . . ? C13 P1 Ru1 105.7(2) . . ? C1 P1 Ru1 113.7(2) . . ? C7 P1 Ru1 118.9(2) . . ? N1 P2 C13 108.7(3) . . ? N1 P2 C20 116.9(2) . . ? C13 P2 C20 105.5(3) . . ? N1 P2 C14 108.5(3) . . ? C13 P2 C14 113.8(3) . . ? C20 P2 C14 103.6(3) . . ? O1 P3 O2 112.7(3) . . ? O1 P3 O3 112.0(3) . . ? O2 P3 O3 103.3(2) . . ? O1 P3 N1 116.1(2) . . ? O2 P3 N1 105.4(3) . . ? O3 P3 N1 106.3(2) . . ? N5 Ru1 N4 79.3(2) . . ? N5 Ru1 N2 94.5(2) . . ? N4 Ru1 N2 169.8(2) . . ? N5 Ru1 N3 84.96(19) . . ? N4 Ru1 N3 93.0(2) . . ? N2 Ru1 N3 78.41(19) . . ? N5 Ru1 N1 174.5(2) . . ? N4 Ru1 N1 95.3(2) . . ? N2 Ru1 N1 90.90(18) . . ? N3 Ru1 N1 95.14(17) . . ? N5 Ru1 P1 93.94(15) . . ? N4 Ru1 P1 87.42(15) . . ? N2 Ru1 P1 101.09(13) . . ? N3 Ru1 P1 178.74(15) . . ? N1 Ru1 P1 86.02(13) . . ? C50 Cl2 C50 59.9(11) . 2_666 ? Cl2 C50 Cl2 120.1(11) . 2_666 ? Cl2 C50 H50B 107.3 . . ? Cl2 C50 H50B 107.3 2_666 . ? Cl2 C50 H50A 107.3 . . ? Cl2 C50 H50A 107.3 2_666 . ? H50B C50 H50A 106.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 3.0(11) . . . . ? P1 C1 C2 C3 -173.2(6) . . . . ? C1 C2 C3 C4 -1.5(13) . . . . ? C2 C3 C4 C5 -0.2(15) . . . . ? C3 C4 C5 C6 0.3(16) . . . . ? C4 C5 C6 C1 1.2(14) . . . . ? C2 C1 C6 C5 -2.9(11) . . . . ? P1 C1 C6 C5 173.5(6) . . . . ? C12 C7 C8 C9 0.6(11) . . . . ? P1 C7 C8 C9 -174.6(6) . . . . ? C7 C8 C9 C10 -0.1(13) . . . . ? C8 C9 C10 C11 -0.9(13) . . . . ? C9 C10 C11 C12 1.4(13) . . . . ? C8 C7 C12 C11 0.0(10) . . . . ? P1 C7 C12 C11 175.0(5) . . . . ? C10 C11 C12 C7 -1.0(11) . . . . ? C19 C14 C15 C16 4.1(10) . . . . ? P2 C14 C15 C16 -173.8(5) . . . . ? C14 C15 C16 C17 -0.9(11) . . . . ? C15 C16 C17 C18 -2.6(13) . . . . ? C16 C17 C18 C19 2.7(13) . . . . ? C15 C14 C19 C18 -3.9(10) . . . . ? P2 C14 C19 C18 174.1(5) . . . . ? C17 C18 C19 C14 0.5(12) . . . . ? C25 C20 C21 C22 0.0(9) . . . . ? P2 C20 C21 C22 175.4(5) . . . . ? C20 C21 C22 C23 0.4(10) . . . . ? C21 C22 C23 C24 -0.1(11) . . . . ? C22 C23 C24 C25 -0.4(10) . . . . ? C21 C20 C25 C24 -0.5(9) . . . . ? P2 C20 C25 C24 -175.7(5) . . . . ? C23 C24 C25 C20 0.7(10) . . . . ? N2 C30 C31 C32 0.2(9) . . . . ? C30 C31 C32 C33 3.3(9) . . . . ? C31 C32 C33 C34 -3.8(10) . . . . ? C32 C33 C34 N2 0.8(9) . . . . ? C32 C33 C34 C35 -179.5(6) . . . . ? N2 C34 C35 N3 1.4(8) . . . . ? C33 C34 C35 N3 -178.3(6) . . . . ? N2 C34 C35 C36 -178.3(6) . . . . ? C33 C34 C35 C36 1.9(10) . . . . ? N3 C35 C36 C37 3.0(11) . . . . ? C34 C35 C36 C37 -177.2(7) . . . . ? C35 C36 C37 C38 -0.7(13) . . . . ? C36 C37 C38 C39 -1.6(13) . . . . ? C37 C38 C39 N3 1.7(11) . . . . ? N4 C40 C41 C42 2.6(11) . . . . ? C40 C41 C42 C43 -3.0(12) . . . . ? C41 C42 C43 C44 0.9(12) . . . . ? C42 C43 C44 N4 1.9(11) . . . . ? C42 C43 C44 C45 -175.4(7) . . . . ? N4 C44 C45 N5 -2.5(8) . . . . ? C43 C44 C45 N5 174.8(6) . . . . ? N4 C44 C45 C46 -177.4(6) . . . . ? C43 C44 C45 C46 0.0(11) . . . . ? N5 C45 C46 C47 1.2(11) . . . . ? C44 C45 C46 C47 175.9(8) . . . . ? C45 C46 C47 C48 -2.8(14) . . . . ? C46 C47 C48 C49 2.4(14) . . . . ? C47 C48 C49 N5 -0.3(13) . . . . ? C31 C30 N2 C34 -3.3(9) . . . . ? C31 C30 N2 Ru1 172.1(4) . . . . ? C33 C34 N2 C30 2.8(8) . . . . ? C35 C34 N2 C30 -177.0(5) . . . . ? C33 C34 N2 Ru1 -173.2(5) . . . . ? C35 C34 N2 Ru1 7.1(6) . . . . ? C38 C39 N3 C35 0.6(9) . . . . ? C38 C39 N3 Ru1 -172.3(5) . . . . ? C36 C35 N3 C39 -3.0(9) . . . . ? C34 C35 N3 C39 177.2(5) . . . . ? C36 C35 N3 Ru1 170.7(5) . . . . ? C34 C35 N3 Ru1 -9.0(7) . . . . ? C41 C40 N4 C44 0.1(10) . . . . ? C41 C40 N4 Ru1 175.6(5) . . . . ? C43 C44 N4 C40 -2.4(9) . . . . ? C45 C44 N4 C40 175.2(6) . . . . ? C43 C44 N4 Ru1 -178.3(5) . . . . ? C45 C44 N4 Ru1 -0.8(7) . . . . ? C48 C49 N5 C45 -1.2(10) . . . . ? C48 C49 N5 Ru1 179.7(6) . . . . ? C46 C45 N5 C49 0.8(9) . . . . ? C44 C45 N5 C49 -174.5(6) . . . . ? C46 C45 N5 Ru1 180.0(5) . . . . ? C44 C45 N5 Ru1 4.7(7) . . . . ? C27 C26 O2 P3 58.0(16) . . . . ? C29 C28 O3 P3 -151.5(5) . . . . ? P2 C13 P1 C1 -145.1(3) . . . . ? P2 C13 P1 C7 106.0(4) . . . . ? P2 C13 P1 Ru1 -23.6(4) . . . . ? C2 C1 P1 C13 -166.4(5) . . . . ? C6 C1 P1 C13 17.3(6) . . . . ? C2 C1 P1 C7 -51.3(6) . . . . ? C6 C1 P1 C7 132.5(6) . . . . ? C2 C1 P1 Ru1 77.3(5) . . . . ? C6 C1 P1 Ru1 -99.0(6) . . . . ? C12 C7 P1 C13 -168.2(5) . . . . ? C8 C7 P1 C13 6.7(6) . . . . ? C12 C7 P1 C1 78.9(6) . . . . ? C8 C7 P1 C1 -106.1(6) . . . . ? C12 C7 P1 Ru1 -46.2(6) . . . . ? C8 C7 P1 Ru1 128.7(5) . . . . ? P3 N1 P2 C13 157.3(4) . . . . ? Ru1 N1 P2 C13 -27.9(4) . . . . ? P3 N1 P2 C20 38.1(5) . . . . ? Ru1 N1 P2 C20 -147.1(3) . . . . ? P3 N1 P2 C14 -78.5(4) . . . . ? Ru1 N1 P2 C14 96.4(3) . . . . ? P1 C13 P2 N1 34.0(4) . . . . ? P1 C13 P2 C20 160.1(3) . . . . ? P1 C13 P2 C14 -87.0(4) . . . . ? C25 C20 P2 N1 -109.5(5) . . . . ? C21 C20 P2 N1 75.3(5) . . . . ? C25 C20 P2 C13 129.6(5) . . . . ? C21 C20 P2 C13 -45.6(5) . . . . ? C25 C20 P2 C14 9.7(6) . . . . ? C21 C20 P2 C14 -165.5(5) . . . . ? C19 C14 P2 N1 -163.6(5) . . . . ? C15 C14 P2 N1 14.4(6) . . . . ? C19 C14 P2 C13 -42.4(6) . . . . ? C15 C14 P2 C13 135.5(5) . . . . ? C19 C14 P2 C20 71.6(5) . . . . ? C15 C14 P2 C20 -110.5(5) . . . . ? C26 O2 P3 O1 37.1(7) . . . . ? C26 O2 P3 O3 -83.9(7) . . . . ? C26 O2 P3 N1 164.7(7) . . . . ? C28 O3 P3 O1 3.3(5) . . . . ? C28 O3 P3 O2 124.8(5) . . . . ? C28 O3 P3 N1 -124.5(5) . . . . ? P2 N1 P3 O1 -122.9(4) . . . . ? Ru1 N1 P3 O1 62.4(4) . . . . ? P2 N1 P3 O2 111.6(4) . . . . ? Ru1 N1 P3 O2 -63.1(3) . . . . ? P2 N1 P3 O3 2.3(4) . . . . ? Ru1 N1 P3 O3 -172.3(2) . . . . ? C49 N5 Ru1 N4 175.2(6) . . . . ? C45 N5 Ru1 N4 -3.9(4) . . . . ? C49 N5 Ru1 N2 3.2(5) . . . . ? C45 N5 Ru1 N2 -175.9(4) . . . . ? C49 N5 Ru1 N3 81.2(5) . . . . ? C45 N5 Ru1 N3 -97.9(4) . . . . ? C49 N5 Ru1 N1 172.4(18) . . . . ? C45 N5 Ru1 N1 -7(2) . . . . ? C49 N5 Ru1 P1 -98.2(5) . . . . ? C45 N5 Ru1 P1 82.7(4) . . . . ? C40 N4 Ru1 N5 -173.1(6) . . . . ? C44 N4 Ru1 N5 2.5(4) . . . . ? C40 N4 Ru1 N2 -120.5(12) . . . . ? C44 N4 Ru1 N2 55.1(12) . . . . ? C40 N4 Ru1 N3 -88.8(5) . . . . ? C44 N4 Ru1 N3 86.8(4) . . . . ? C40 N4 Ru1 N1 6.7(5) . . . . ? C44 N4 Ru1 N1 -177.8(4) . . . . ? C40 N4 Ru1 P1 92.4(5) . . . . ? C44 N4 Ru1 P1 -92.0(4) . . . . ? C30 N2 Ru1 N5 -100.6(5) . . . . ? C34 N2 Ru1 N5 74.9(4) . . . . ? C30 N2 Ru1 N4 -152.1(10) . . . . ? C34 N2 Ru1 N4 23.4(13) . . . . ? C30 N2 Ru1 N3 175.5(5) . . . . ? C34 N2 Ru1 N3 -9.0(4) . . . . ? C30 N2 Ru1 N1 80.4(5) . . . . ? C34 N2 Ru1 N1 -104.0(4) . . . . ? C30 N2 Ru1 P1 -5.7(5) . . . . ? C34 N2 Ru1 P1 169.8(4) . . . . ? C39 N3 Ru1 N5 87.3(5) . . . . ? C35 N3 Ru1 N5 -85.9(4) . . . . ? C39 N3 Ru1 N4 8.4(5) . . . . ? C35 N3 Ru1 N4 -164.9(4) . . . . ? C39 N3 Ru1 N2 -177.0(5) . . . . ? C35 N3 Ru1 N2 9.7(4) . . . . ? C39 N3 Ru1 N1 -87.2(5) . . . . ? C35 N3 Ru1 N1 99.6(4) . . . . ? C39 N3 Ru1 P1 116(7) . . . . ? C35 N3 Ru1 P1 -57(7) . . . . ? P2 N1 Ru1 N5 102(2) . . . . ? P3 N1 Ru1 N5 -82(2) . . . . ? P2 N1 Ru1 N4 99.6(3) . . . . ? P3 N1 Ru1 N4 -85.1(3) . . . . ? P2 N1 Ru1 N2 -88.4(3) . . . . ? P3 N1 Ru1 N2 86.9(3) . . . . ? P2 N1 Ru1 N3 -166.9(3) . . . . ? P3 N1 Ru1 N3 8.4(3) . . . . ? P2 N1 Ru1 P1 12.6(2) . . . . ? P3 N1 Ru1 P1 -172.1(3) . . . . ? C13 P1 Ru1 N5 -168.5(3) . . . . ? C1 P1 Ru1 N5 -51.4(3) . . . . ? C7 P1 Ru1 N5 67.3(3) . . . . ? C13 P1 Ru1 N4 -89.5(3) . . . . ? C1 P1 Ru1 N4 27.6(3) . . . . ? C7 P1 Ru1 N4 146.4(3) . . . . ? C13 P1 Ru1 N2 96.1(3) . . . . ? C1 P1 Ru1 N2 -146.8(3) . . . . ? C7 P1 Ru1 N2 -28.0(3) . . . . ? C13 P1 Ru1 N3 162(7) . . . . ? C1 P1 Ru1 N3 -81(7) . . . . ? C7 P1 Ru1 N3 38(7) . . . . ? C13 P1 Ru1 N1 6.0(3) . . . . ? C1 P1 Ru1 N1 123.1(3) . . . . ? C7 P1 Ru1 N1 -118.1(3) . . . . ? C50 Cl2 C50 Cl2 0.000(2) 2_666 . . 2_666 ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 74.21 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 0.899 _refine_diff_density_min -1.417 _refine_diff_density_rms 0.101 #==END