Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'David Milstein' _publ_contact_author_address ; Department of Organic Chemistry The Weizmann Institute of Science Rehovot 76100 76100 ISRAEL ; _publ_contact_author_email DAVID.MILSTEIN@WEIZMANN.AC.IL _publ_section_title ;Electron-Rich, Bulky PNN- type Ruthenium Complexes: Synthesis, Characterization and Catalysis of Acceptorless Alcohol Dehydrogenation ; loop_ _publ_author_name D.Milstein L.Shimon 'Jing Zhang.' data_m394new _database_code_depnum_ccdc_archive 'CCDC 620162' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H80 Cl4 N6 P2 Ru2' _chemical_formula_weight 1087.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.296(4) _cell_length_b 11.907(2) _cell_length_c 23.054(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.87(3) _cell_angle_gamma 90.00 _cell_volume 5277.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11763 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9181 _exptl_absorpt_correction_T_max 0.9181 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '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 11997 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.46 _reflns_number_total 11997 _reflns_number_gt 9283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect package (Bruker Nonius)' _computing_cell_refinement HKL _computing_data_reduction HKL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+28.2925P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11997 _refine_ls_number_parameters 520 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.112542(18) 0.45005(3) 0.152701(16) 0.02362(11) Uani 1 1 d . . . Cl1 Cl 0.13964(6) 0.56206(10) 0.06980(5) 0.0279(2) Uani 1 1 d . . . Cl2 Cl 0.07941(6) 0.32435(12) 0.22735(5) 0.0350(3) Uani 1 1 d . . . P1 P 0.11633(6) 0.59785(13) 0.21823(5) 0.0287(3) Uani 1 1 d . . . N1 N 0.01022(19) 0.4900(4) 0.14277(17) 0.0246(8) Uani 1 1 d . . . C1 C 0.0249(2) 0.5861(5) 0.2363(2) 0.0309(11) Uani 1 1 d . . . H1A H 0.0217 0.5307 0.2679 0.037 Uiso 1 1 calc R . . H1B H 0.0087 0.6596 0.2500 0.037 Uiso 1 1 calc R . . C2 C -0.0206(2) 0.5496(4) 0.1834(2) 0.0276(10) Uani 1 1 d . . . C3 C -0.0916(3) 0.5738(5) 0.1756(2) 0.0311(11) Uani 1 1 d . . . H3 H -0.1129 0.6180 0.2034 0.037 Uiso 1 1 calc R . . C4 C -0.1306(3) 0.5330(5) 0.1273(2) 0.0319(11) Uani 1 1 d . . . H4 H -0.1789 0.5490 0.1217 0.038 Uiso 1 1 calc R . . C5 C -0.0988(3) 0.4685(5) 0.0869(2) 0.0318(11) Uani 1 1 d . . . H5 H -0.1254 0.4387 0.0539 0.038 Uiso 1 1 calc R . . C6 C -0.0278(2) 0.4480(4) 0.0952(2) 0.0258(10) Uani 1 1 d . . . C7 C 0.0130(2) 0.3864(4) 0.0527(2) 0.0287(10) Uani 1 1 d . . . H7A H -0.0184 0.3349 0.0293 0.034 Uiso 1 1 calc R . . H7B H 0.0318 0.4411 0.0258 0.034 Uiso 1 1 calc R . . N2 N 0.0719(2) 0.3200(3) 0.08238(18) 0.0272(9) Uani 1 1 d . . . C8 C 0.1686(3) 0.5914(6) 0.2917(2) 0.0399(14) Uani 1 1 d . . . C9 C 0.1334(3) 0.6541(7) 0.3397(2) 0.0523(18) Uani 1 1 d . . . H9A H 0.0874 0.6216 0.3435 0.078 Uiso 1 1 calc R . . H9B H 0.1285 0.7337 0.3293 0.078 Uiso 1 1 calc R . . H9C H 0.1620 0.6468 0.3767 0.078 Uiso 1 1 calc R . . C10 C 0.2420(3) 0.6392(7) 0.2866(3) 0.0518(17) Uani 1 1 d . . . H10A H 0.2718 0.6211 0.3219 0.078 Uiso 1 1 calc R . . H10B H 0.2392 0.7209 0.2819 0.078 Uiso 1 1 calc R . . H10C H 0.2617 0.6060 0.2527 0.078 Uiso 1 1 calc R . . C11 C 0.1774(3) 0.4715(6) 0.3121(2) 0.0459(15) Uani 1 1 d . . . H11A H 0.1979 0.4270 0.2822 0.069 Uiso 1 1 calc R . . H11B H 0.1318 0.4402 0.3192 0.069 Uiso 1 1 calc R . . H11C H 0.2080 0.4692 0.3482 0.069 Uiso 1 1 calc R . . C12 C 0.1215(3) 0.7478(5) 0.1897(2) 0.0364(12) Uani 1 1 d . . . C13 C 0.1143(3) 0.8392(6) 0.2360(3) 0.0454(14) Uani 1 1 d . . . H13A H 0.1544 0.8361 0.2650 0.068 Uiso 1 1 calc R . . H13B H 0.0715 0.8265 0.2552 0.068 Uiso 1 1 calc R . . H13C H 0.1122 0.9132 0.2173 0.068 Uiso 1 1 calc R . . C14 C 0.0597(3) 0.7639(5) 0.1432(2) 0.0388(13) Uani 1 1 d . . . H14A H 0.0640 0.8367 0.1240 0.058 Uiso 1 1 calc R . . H14B H 0.0160 0.7615 0.1618 0.058 Uiso 1 1 calc R . . H14C H 0.0600 0.7038 0.1142 0.058 Uiso 1 1 calc R . . C15 C 0.1906(3) 0.7646(5) 0.1621(3) 0.0416(14) Uani 1 1 d . . . H15A H 0.1894 0.8362 0.1410 0.062 Uiso 1 1 calc R . . H15B H 0.1973 0.7030 0.1349 0.062 Uiso 1 1 calc R . . H15C H 0.2290 0.7654 0.1927 0.062 Uiso 1 1 calc R . . C16 C 0.0963(3) 0.1311(5) 0.1294(3) 0.0474(15) Uani 1 1 d . . . H16A H 0.1197 0.0977 0.0975 0.071 Uiso 1 1 calc R . . H16B H 0.0736 0.0719 0.1504 0.071 Uiso 1 1 calc R . . H16C H 0.1306 0.1697 0.1562 0.071 Uiso 1 1 calc R . . C17 C 0.1237(3) 0.2936(5) 0.0393(2) 0.0323(11) Uani 1 1 d . . . H17A H 0.1622 0.2501 0.0596 0.039 Uiso 1 1 calc R . . H17B H 0.1435 0.3653 0.0265 0.039 Uiso 1 1 calc R . . C18 C 0.0965(3) 0.2285(6) -0.0144(2) 0.0441(14) Uani 1 1 d . . . H18A H 0.0794 0.1551 -0.0028 0.066 Uiso 1 1 calc R . . H18B H 0.1340 0.2180 -0.0400 0.066 Uiso 1 1 calc R . . H18C H 0.0583 0.2704 -0.0353 0.066 Uiso 1 1 calc R . . C19 C 0.0420(3) 0.2151(5) 0.1048(3) 0.0370(12) Uani 1 1 d . . . H19A H 0.0127 0.1787 0.0728 0.044 Uiso 1 1 calc R . . H19B H 0.0115 0.2349 0.1357 0.044 Uiso 1 1 calc R . . N3 N 0.2666(2) 0.3787(4) 0.16535(19) 0.0293(9) Uani 1 1 d . . . N4 N 0.2106(2) 0.4048(4) 0.16249(17) 0.0263(9) Uani 1 1 d . . . Ru2 Ru 0.36140(2) 0.32626(3) 0.156964(19) 0.02845(12) Uani 1 1 d . . . Cl3 Cl 0.41827(6) 0.47395(11) 0.21354(6) 0.0332(3) Uani 1 1 d . . . Cl4 Cl 0.30751(8) 0.18925(13) 0.09029(9) 0.0595(5) Uani 1 1 d . . . P2 P 0.37986(7) 0.20742(14) 0.23703(8) 0.0440(4) Uani 1 1 d . . . N5 N 0.3791(2) 0.4287(4) 0.07418(19) 0.0353(10) Uani 1 1 d . . . N6 N 0.4588(2) 0.2764(4) 0.1420(2) 0.0314(9) Uani 1 1 d . . . C20 C 0.4258(3) 0.3500(6) 0.0451(3) 0.0479(16) Uani 1 1 d . . . H20A H 0.4491 0.3910 0.0148 0.058 Uiso 1 1 calc R . . H20B H 0.3977 0.2889 0.0259 0.058 Uiso 1 1 calc R . . C21 C 0.4803(3) 0.3002(5) 0.0890(2) 0.0395(13) Uani 1 1 d . . . C22 C 0.5468(3) 0.2723(6) 0.0757(3) 0.0478(16) Uani 1 1 d . . . H22 H 0.5618 0.2896 0.0385 0.057 Uiso 1 1 calc R . . C23 C 0.5914(3) 0.2187(6) 0.1175(3) 0.0448(14) Uani 1 1 d . . . H23 H 0.6369 0.1978 0.1089 0.054 Uiso 1 1 calc R . . C24 C 0.5693(3) 0.1961(5) 0.1713(3) 0.0371(12) Uani 1 1 d . . . H24 H 0.5994 0.1593 0.2001 0.044 Uiso 1 1 calc R . . C25 C 0.5025(2) 0.2277(4) 0.1835(2) 0.0318(11) Uani 1 1 d . . . C26 C 0.4758(3) 0.2137(5) 0.2425(3) 0.0369(12) Uani 1 1 d . . . H26A H 0.4918 0.2776 0.2677 0.044 Uiso 1 1 calc R . . H26B H 0.4950 0.1439 0.2608 0.044 Uiso 1 1 calc R . . C27 C 0.3616(3) 0.0518(6) 0.2269(5) 0.072(3) Uani 1 1 d . . . C28 C 0.3808(4) -0.0242(8) 0.2789(5) 0.100(4) Uani 1 1 d . . . H28A H 0.3736 -0.1028 0.2673 0.149 Uiso 1 1 calc R . . H28B H 0.3514 -0.0061 0.3102 0.149 Uiso 1 1 calc R . . H28C H 0.4298 -0.0125 0.2925 0.149 Uiso 1 1 calc R . . C29 C 0.2826(4) 0.0346(7) 0.2078(6) 0.098(4) Uani 1 1 d . . . H29A H 0.2758 -0.0383 0.1885 0.147 Uiso 1 1 calc R . . H29B H 0.2665 0.0946 0.1808 0.147 Uiso 1 1 calc R . . H29C H 0.2560 0.0370 0.2422 0.147 Uiso 1 1 calc R . . C30 C 0.4041(4) 0.0121(6) 0.1783(4) 0.074(3) Uani 1 1 d . . . H30A H 0.4536 0.0117 0.1921 0.111 Uiso 1 1 calc R . . H30B H 0.3966 0.0629 0.1449 0.111 Uiso 1 1 calc R . . H30C H 0.3897 -0.0640 0.1665 0.111 Uiso 1 1 calc R . . C31 C 0.3574(3) 0.2471(8) 0.3147(3) 0.065(2) Uani 1 1 d . . . C32 C 0.4101(4) 0.1965(9) 0.3618(4) 0.083(3) Uani 1 1 d . . . H32A H 0.4562 0.2293 0.3583 0.124 Uiso 1 1 calc R . . H32B H 0.4124 0.1150 0.3565 0.124 Uiso 1 1 calc R . . H32C H 0.3952 0.2132 0.4004 0.124 Uiso 1 1 calc R . . C33 C 0.3580(4) 0.3739(7) 0.3226(3) 0.060(2) Uani 1 1 d . . . H33A H 0.3425 0.3925 0.3608 0.091 Uiso 1 1 calc R . . H33B H 0.3266 0.4085 0.2920 0.091 Uiso 1 1 calc R . . H33C H 0.4053 0.4023 0.3200 0.091 Uiso 1 1 calc R . . C34 C 0.2833(4) 0.2045(9) 0.3237(5) 0.093(4) Uani 1 1 d . . . H34A H 0.2671 0.2395 0.3586 0.139 Uiso 1 1 calc R . . H34B H 0.2842 0.1227 0.3286 0.139 Uiso 1 1 calc R . . H34C H 0.2516 0.2241 0.2897 0.139 Uiso 1 1 calc R . . C35 C 0.4152(3) 0.5366(5) 0.0828(3) 0.0430(14) Uani 1 1 d . . . H35A H 0.4335 0.5590 0.0457 0.052 Uiso 1 1 calc R . . H35B H 0.4555 0.5261 0.1119 0.052 Uiso 1 1 calc R . . C36 C 0.3710(3) 0.6306(6) 0.1029(3) 0.0509(16) Uani 1 1 d . . . H36A H 0.3378 0.6543 0.0707 0.076 Uiso 1 1 calc R . . H36B H 0.4008 0.6942 0.1155 0.076 Uiso 1 1 calc R . . H36C H 0.3457 0.6047 0.1355 0.076 Uiso 1 1 calc R . . C37 C 0.3127(3) 0.4417(6) 0.0353(3) 0.0452(15) Uani 1 1 d . . . H37A H 0.2802 0.4884 0.0560 0.054 Uiso 1 1 calc R . . H37B H 0.2913 0.3666 0.0294 0.054 Uiso 1 1 calc R . . C38 C 0.3198(4) 0.4941(8) -0.0245(3) 0.067(2) Uani 1 1 d . . . H38A H 0.3344 0.5726 -0.0196 0.100 Uiso 1 1 calc R . . H38B H 0.2749 0.4908 -0.0477 0.100 Uiso 1 1 calc R . . H38C H 0.3546 0.4525 -0.0444 0.100 Uiso 1 1 calc R . . C39 C 0.7255(4) 0.1651(7) 0.0327(3) 0.069(2) Uani 1 1 d . . . H39A H 0.7302 0.1562 0.0755 0.083 Uiso 1 1 calc R . . H39B H 0.6801 0.2008 0.0212 0.083 Uiso 1 1 calc R . . C40 C 0.7769(4) 0.2277(7) 0.0157(4) 0.069(2) Uani 1 1 d . . . H40A H 0.7935 0.2797 0.0474 0.083 Uiso 1 1 calc R . . H40B H 0.7599 0.2731 -0.0186 0.083 Uiso 1 1 calc R . . C41 C 0.8345(5) 0.1561(9) 0.0006(4) 0.087(3) Uani 1 1 d . . . H41A H 0.8714 0.1503 0.0331 0.104 Uiso 1 1 calc R . . H41B H 0.8550 0.1830 -0.0348 0.104 Uiso 1 1 calc R . . C42 C 0.7941(10) 0.0405(16) -0.0105(8) 0.166(6) Uiso 1 1 d . . . H42A H 0.7908 0.0190 -0.0521 0.199 Uiso 1 1 calc R . . H42B H 0.8162 -0.0211 0.0132 0.199 Uiso 1 1 calc R . . C43 C 0.7295(14) 0.069(2) 0.0077(12) 0.239(11) Uiso 1 1 d . . . H43A H 0.6951 0.0672 -0.0267 0.287 Uiso 1 1 calc R . . H43B H 0.7159 0.0102 0.0350 0.287 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01712(18) 0.0295(2) 0.02378(19) 0.00284(15) -0.00106(13) 0.00131(15) Cl1 0.0316(6) 0.0267(6) 0.0254(5) 0.0007(5) 0.0022(4) -0.0009(5) Cl2 0.0278(6) 0.0430(8) 0.0338(6) 0.0145(6) 0.0013(5) -0.0009(5) P1 0.0196(6) 0.0412(8) 0.0248(6) -0.0045(5) -0.0015(4) 0.0012(5) N1 0.0195(19) 0.028(2) 0.0262(19) 0.0015(17) -0.0015(15) 0.0010(16) C1 0.021(2) 0.043(3) 0.028(2) -0.001(2) -0.0015(18) 0.002(2) C2 0.023(2) 0.031(3) 0.029(2) 0.000(2) -0.0012(18) 0.003(2) C3 0.023(2) 0.038(3) 0.032(3) 0.000(2) 0.0002(19) 0.004(2) C4 0.019(2) 0.036(3) 0.040(3) 0.002(2) -0.0032(19) 0.002(2) C5 0.027(3) 0.032(3) 0.035(3) 0.002(2) -0.006(2) 0.000(2) C6 0.022(2) 0.027(3) 0.028(2) 0.004(2) -0.0019(18) 0.0011(19) C7 0.024(2) 0.030(3) 0.031(2) 0.001(2) -0.0053(19) 0.001(2) N2 0.022(2) 0.025(2) 0.033(2) 0.0035(17) -0.0050(16) 0.0011(16) C8 0.028(3) 0.061(4) 0.029(3) -0.010(3) -0.007(2) 0.003(3) C9 0.043(3) 0.085(5) 0.028(3) -0.017(3) -0.003(2) 0.010(3) C10 0.027(3) 0.089(5) 0.037(3) -0.011(3) -0.008(2) -0.002(3) C11 0.035(3) 0.069(5) 0.032(3) 0.003(3) -0.007(2) 0.013(3) C12 0.029(3) 0.040(3) 0.040(3) -0.010(2) 0.001(2) -0.002(2) C13 0.042(3) 0.048(4) 0.046(3) -0.013(3) 0.002(3) -0.002(3) C14 0.040(3) 0.036(3) 0.040(3) 0.001(2) 0.000(2) 0.000(2) C15 0.037(3) 0.041(3) 0.047(3) -0.010(3) 0.002(2) -0.011(3) C16 0.050(4) 0.034(3) 0.059(4) 0.009(3) 0.007(3) 0.009(3) C17 0.029(3) 0.034(3) 0.034(3) -0.005(2) 0.002(2) 0.005(2) C18 0.046(3) 0.047(4) 0.038(3) -0.009(3) 0.002(2) 0.004(3) C19 0.036(3) 0.032(3) 0.044(3) 0.006(2) 0.006(2) -0.004(2) N3 0.022(2) 0.028(2) 0.038(2) 0.0028(19) -0.0004(17) -0.0004(17) N4 0.024(2) 0.026(2) 0.028(2) 0.0026(17) -0.0008(15) -0.0009(17) Ru2 0.01778(19) 0.0237(2) 0.0429(2) -0.00149(17) -0.00285(15) 0.00139(15) Cl3 0.0277(6) 0.0331(7) 0.0377(6) -0.0045(5) -0.0025(5) -0.0009(5) Cl4 0.0413(8) 0.0346(8) 0.0970(13) -0.0256(8) -0.0263(8) 0.0060(6) P2 0.0188(6) 0.0391(9) 0.0740(11) 0.0213(8) 0.0036(6) 0.0022(6) N5 0.026(2) 0.042(3) 0.037(2) -0.004(2) -0.0010(18) 0.0134(19) N6 0.022(2) 0.026(2) 0.046(3) -0.0057(19) -0.0018(17) 0.0023(17) C20 0.043(3) 0.062(4) 0.038(3) -0.008(3) -0.001(2) 0.021(3) C21 0.035(3) 0.042(3) 0.042(3) -0.007(3) 0.000(2) 0.010(2) C22 0.037(3) 0.062(4) 0.045(3) 0.001(3) 0.006(2) 0.019(3) C23 0.029(3) 0.052(4) 0.053(4) -0.005(3) 0.005(2) 0.010(3) C24 0.028(3) 0.030(3) 0.051(3) 0.003(2) -0.004(2) 0.003(2) C25 0.021(2) 0.023(3) 0.051(3) -0.001(2) 0.000(2) 0.0028(19) C26 0.021(2) 0.036(3) 0.053(3) 0.008(3) 0.003(2) 0.005(2) C27 0.028(3) 0.042(4) 0.146(8) 0.033(5) 0.000(4) -0.001(3) C28 0.045(4) 0.062(5) 0.190(11) 0.072(7) 0.002(5) 0.000(4) C29 0.037(4) 0.040(4) 0.214(12) 0.029(6) -0.007(5) -0.013(3) C30 0.042(4) 0.027(3) 0.148(8) 0.001(4) -0.025(4) -0.002(3) C31 0.032(3) 0.092(6) 0.072(5) 0.045(4) 0.019(3) 0.014(3) C32 0.059(5) 0.123(8) 0.068(5) 0.057(5) 0.020(4) 0.036(5) C33 0.049(4) 0.088(6) 0.046(4) 0.015(4) 0.018(3) 0.016(4) C34 0.039(4) 0.113(8) 0.132(8) 0.071(7) 0.040(5) 0.022(4) C35 0.033(3) 0.052(4) 0.043(3) 0.009(3) -0.001(2) 0.003(3) C36 0.046(4) 0.039(4) 0.064(4) 0.006(3) -0.013(3) 0.007(3) C37 0.034(3) 0.054(4) 0.044(3) -0.009(3) -0.011(2) 0.014(3) C38 0.057(4) 0.103(6) 0.038(3) -0.004(4) -0.008(3) 0.041(4) C39 0.057(4) 0.084(6) 0.071(5) -0.047(4) 0.041(4) -0.029(4) C40 0.065(5) 0.068(5) 0.072(5) 0.016(4) -0.015(4) 0.004(4) C41 0.091(7) 0.122(9) 0.050(4) 0.026(5) 0.027(4) 0.016(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N4 1.961(4) . ? Ru1 N1 2.025(4) . ? Ru1 P1 2.3165(14) . ? Ru1 N2 2.329(4) . ? Ru1 Cl2 2.4079(13) . ? Ru1 Cl1 2.4238(13) . ? P1 C1 1.852(5) . ? P1 C8 1.899(5) . ? P1 C12 1.908(6) . ? N1 C2 1.354(6) . ? N1 C6 1.361(6) . ? C1 C2 1.503(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.395(7) . ? C3 C4 1.378(7) . ? C3 H3 0.9500 . ? C4 C5 1.389(8) . ? C4 H4 0.9500 . ? C5 C6 1.389(7) . ? C5 H5 0.9500 . ? C6 C7 1.501(7) . ? C7 N2 1.500(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? N2 C19 1.488(7) . ? N2 C17 1.501(6) . ? C8 C11 1.509(9) . ? C8 C9 1.539(8) . ? C8 C10 1.540(8) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.539(8) . ? C12 C13 1.540(8) . ? C12 C14 1.545(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C19 1.523(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.517(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? N3 N4 1.121(6) . ? N3 Ru2 1.958(4) . ? Ru2 N6 2.028(4) . ? Ru2 N5 2.315(5) . ? Ru2 P2 2.3291(17) . ? Ru2 Cl3 2.3988(14) . ? Ru2 Cl4 2.4154(16) . ? P2 C26 1.847(5) . ? P2 C27 1.897(8) . ? P2 C31 1.935(8) . ? N5 C35 1.466(8) . ? N5 C20 1.498(7) . ? N5 C37 1.507(7) . ? N6 C25 1.351(7) . ? N6 C21 1.355(7) . ? C20 C21 1.516(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.384(8) . ? C22 C23 1.393(8) . ? C22 H22 0.9500 . ? C23 C24 1.372(9) . ? C23 H23 0.9500 . ? C24 C25 1.395(7) . ? C24 H24 0.9500 . ? C25 C26 1.504(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C30 1.520(13) . ? C27 C28 1.521(12) . ? C27 C29 1.563(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.520(12) . ? C31 C32 1.546(9) . ? C31 C34 1.549(10) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.503(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.529(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C43 1.29(2) . ? C39 C40 1.326(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.465(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.592(19) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.39(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 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 N4 Ru1 N1 177.65(17) . . ? N4 Ru1 P1 99.02(13) . . ? N1 Ru1 P1 82.63(12) . . ? N4 Ru1 N2 99.33(16) . . ? N1 Ru1 N2 79.05(15) . . ? P1 Ru1 N2 161.64(10) . . ? N4 Ru1 Cl2 93.39(12) . . ? N1 Ru1 Cl2 84.91(12) . . ? P1 Ru1 Cl2 90.10(5) . . ? N2 Ru1 Cl2 89.44(11) . . ? N4 Ru1 Cl1 88.35(12) . . ? N1 Ru1 Cl1 93.16(12) . . ? P1 Ru1 Cl1 95.70(5) . . ? N2 Ru1 Cl1 84.22(11) . . ? Cl2 Ru1 Cl1 173.62(5) . . ? C1 P1 C8 103.9(2) . . ? C1 P1 C12 103.1(3) . . ? C8 P1 C12 107.8(3) . . ? C1 P1 Ru1 96.37(18) . . ? C8 P1 Ru1 122.4(2) . . ? C12 P1 Ru1 119.05(17) . . ? C2 N1 C6 120.7(4) . . ? C2 N1 Ru1 121.8(3) . . ? C6 N1 Ru1 117.3(3) . . ? C2 C1 P1 110.0(3) . . ? C2 C1 H1A 109.7 . . ? P1 C1 H1A 109.7 . . ? C2 C1 H1B 109.7 . . ? P1 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N1 C2 C3 120.2(4) . . ? N1 C2 C1 116.8(4) . . ? C3 C2 C1 123.0(4) . . ? C4 C3 C2 119.6(5) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 119.7(5) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 119.4(5) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? N1 C6 C5 120.3(5) . . ? N1 C6 C7 115.4(4) . . ? C5 C6 C7 124.2(4) . . ? N2 C7 C6 112.3(4) . . ? N2 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N2 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C19 N2 C7 107.4(4) . . ? C19 N2 C17 110.7(4) . . ? C7 N2 C17 109.3(4) . . ? C19 N2 Ru1 115.7(3) . . ? C7 N2 Ru1 99.5(3) . . ? C17 N2 Ru1 113.3(3) . . ? C11 C8 C9 106.2(5) . . ? C11 C8 C10 107.1(5) . . ? C9 C8 C10 110.0(5) . . ? C11 C8 P1 110.6(4) . . ? C9 C8 P1 112.8(4) . . ? C10 C8 P1 109.8(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C13 109.1(5) . . ? C15 C12 C14 109.9(5) . . ? C13 C12 C14 106.5(5) . . ? C15 C12 P1 109.7(4) . . ? C13 C12 P1 114.3(4) . . ? C14 C12 P1 107.2(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C16 H16A 109.5 . . ? C19 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C19 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 C18 116.3(4) . . ? N2 C17 H17A 108.2 . . ? C18 C17 H17A 108.2 . . ? N2 C17 H17B 108.2 . . ? C18 C17 H17B 108.2 . . ? H17A C17 H17B 107.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 C16 113.9(5) . . ? N2 C19 H19A 108.8 . . ? C16 C19 H19A 108.8 . . ? N2 C19 H19B 108.8 . . ? C16 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? N4 N3 Ru2 170.7(4) . . ? N3 N4 Ru1 176.8(4) . . ? N3 Ru2 N6 175.68(18) . . ? N3 Ru2 N5 96.76(16) . . ? N6 Ru2 N5 79.10(17) . . ? N3 Ru2 P2 101.34(13) . . ? N6 Ru2 P2 82.82(14) . . ? N5 Ru2 P2 161.88(11) . . ? N3 Ru2 Cl3 95.78(13) . . ? N6 Ru2 Cl3 85.39(13) . . ? N5 Ru2 Cl3 88.24(12) . . ? P2 Ru2 Cl3 88.99(6) . . ? N3 Ru2 Cl4 85.56(13) . . ? N6 Ru2 Cl4 92.81(13) . . ? N5 Ru2 Cl4 85.23(13) . . ? P2 Ru2 Cl4 97.04(7) . . ? Cl3 Ru2 Cl4 173.45(6) . . ? C26 P2 C27 102.9(3) . . ? C26 P2 C31 103.2(3) . . ? C27 P2 C31 107.4(4) . . ? C26 P2 Ru2 96.57(19) . . ? C27 P2 Ru2 118.8(3) . . ? C31 P2 Ru2 123.6(2) . . ? C35 N5 C20 108.2(5) . . ? C35 N5 C37 111.1(5) . . ? C20 N5 C37 108.2(4) . . ? C35 N5 Ru2 116.8(3) . . ? C20 N5 Ru2 100.1(4) . . ? C37 N5 Ru2 111.5(4) . . ? C25 N6 C21 120.5(4) . . ? C25 N6 Ru2 122.5(4) . . ? C21 N6 Ru2 116.8(3) . . ? N5 C20 C21 110.9(5) . . ? N5 C20 H20A 109.5 . . ? C21 C20 H20A 109.5 . . ? N5 C20 H20B 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 108.0 . . ? N6 C21 C22 120.7(5) . . ? N6 C21 C20 115.8(5) . . ? C22 C21 C20 123.3(6) . . ? C21 C22 C23 119.1(6) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 119.7(5) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 119.5(5) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? N6 C25 C24 120.4(5) . . ? N6 C25 C26 116.5(4) . . ? C24 C25 C26 123.1(5) . . ? C25 C26 P2 111.2(4) . . ? C25 C26 H26A 109.4 . . ? P2 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? P2 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C30 C27 C28 106.6(7) . . ? C30 C27 C29 109.0(8) . . ? C28 C27 C29 108.1(7) . . ? C30 C27 P2 106.8(5) . . ? C28 C27 P2 116.9(7) . . ? C29 C27 P2 109.2(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C32 107.8(8) . . ? C33 C31 C34 107.9(6) . . ? C32 C31 C34 109.7(6) . . ? C33 C31 P2 110.7(4) . . ? C32 C31 P2 111.7(5) . . ? C34 C31 P2 109.0(7) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N5 C35 C36 114.8(5) . . ? N5 C35 H35A 108.6 . . ? C36 C35 H35A 108.6 . . ? N5 C35 H35B 108.6 . . ? C36 C35 H35B 108.6 . . ? H35A C35 H35B 107.6 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 C38 116.2(5) . . ? N5 C37 H37A 108.2 . . ? C38 C37 H37A 108.2 . . ? N5 C37 H37B 108.2 . . ? C38 C37 H37B 108.2 . . ? H37A C37 H37B 107.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C43 C39 C40 107.0(13) . . ? C43 C39 H39A 110.3 . . ? C40 C39 H39A 110.3 . . ? C43 C39 H39B 110.3 . . ? C40 C39 H39B 110.3 . . ? H39A C39 H39B 108.6 . . ? C39 C40 C41 110.2(8) . . ? C39 C40 H40A 109.6 . . ? C41 C40 H40A 109.6 . . ? C39 C40 H40B 109.6 . . ? C41 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? C40 C41 C42 99.8(10) . . ? C40 C41 H41A 111.8 . . ? C42 C41 H41A 111.8 . . ? C40 C41 H41B 111.8 . . ? C42 C41 H41B 111.8 . . ? H41A C41 H41B 109.5 . . ? C43 C42 C41 100.5(17) . . ? C43 C42 H42A 111.7 . . ? C41 C42 H42A 111.7 . . ? C43 C42 H42B 111.7 . . ? C41 C42 H42B 111.7 . . ? H42A C42 H42B 109.5 . . ? C39 C43 C42 116(2) . . ? C39 C43 H43A 108.3 . . ? C42 C43 H43A 108.3 . . ? C39 C43 H43B 108.3 . . ? C42 C43 H43B 108.3 . . ? H43A C43 H43B 107.4 . . ? 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 N4 Ru1 P1 C1 -151.7(2) . . . . ? N1 Ru1 P1 C1 26.6(2) . . . . ? N2 Ru1 P1 C1 30.3(4) . . . . ? Cl2 Ru1 P1 C1 -58.22(18) . . . . ? Cl1 Ru1 P1 C1 119.11(18) . . . . ? N4 Ru1 P1 C8 -40.7(3) . . . . ? N1 Ru1 P1 C8 137.6(3) . . . . ? N2 Ru1 P1 C8 141.3(4) . . . . ? Cl2 Ru1 P1 C8 52.8(2) . . . . ? Cl1 Ru1 P1 C8 -129.9(2) . . . . ? N4 Ru1 P1 C12 99.5(2) . . . . ? N1 Ru1 P1 C12 -82.2(2) . . . . ? N2 Ru1 P1 C12 -78.5(4) . . . . ? Cl2 Ru1 P1 C12 -167.04(19) . . . . ? Cl1 Ru1 P1 C12 10.28(19) . . . . ? N4 Ru1 N1 C2 114(4) . . . . ? P1 Ru1 N1 C2 -20.2(4) . . . . ? N2 Ru1 N1 C2 161.0(4) . . . . ? Cl2 Ru1 N1 C2 70.6(4) . . . . ? Cl1 Ru1 N1 C2 -115.5(4) . . . . ? N4 Ru1 N1 C6 -61(4) . . . . ? P1 Ru1 N1 C6 164.2(4) . . . . ? N2 Ru1 N1 C6 -14.6(3) . . . . ? Cl2 Ru1 N1 C6 -105.1(3) . . . . ? Cl1 Ru1 N1 C6 68.8(3) . . . . ? C8 P1 C1 C2 -160.3(4) . . . . ? C12 P1 C1 C2 87.3(4) . . . . ? Ru1 P1 C1 C2 -34.5(4) . . . . ? C6 N1 C2 C3 -3.3(7) . . . . ? Ru1 N1 C2 C3 -178.8(4) . . . . ? C6 N1 C2 C1 176.1(5) . . . . ? Ru1 N1 C2 C1 0.6(6) . . . . ? P1 C1 C2 N1 26.0(6) . . . . ? P1 C1 C2 C3 -154.6(4) . . . . ? N1 C2 C3 C4 2.4(8) . . . . ? C1 C2 C3 C4 -177.0(5) . . . . ? C2 C3 C4 C5 -0.1(8) . . . . ? C3 C4 C5 C6 -1.3(8) . . . . ? C2 N1 C6 C5 1.9(7) . . . . ? Ru1 N1 C6 C5 177.5(4) . . . . ? C2 N1 C6 C7 178.4(4) . . . . ? Ru1 N1 C6 C7 -6.0(6) . . . . ? C4 C5 C6 N1 0.5(8) . . . . ? C4 C5 C6 C7 -175.7(5) . . . . ? N1 C6 C7 N2 36.5(6) . . . . ? C5 C6 C7 N2 -147.1(5) . . . . ? C6 C7 N2 C19 78.9(5) . . . . ? C6 C7 N2 C17 -161.0(4) . . . . ? C6 C7 N2 Ru1 -42.0(4) . . . . ? N4 Ru1 N2 C19 93.7(3) . . . . ? N1 Ru1 N2 C19 -84.5(3) . . . . ? P1 Ru1 N2 C19 -88.2(5) . . . . ? Cl2 Ru1 N2 C19 0.4(3) . . . . ? Cl1 Ru1 N2 C19 -178.9(3) . . . . ? N4 Ru1 N2 C7 -151.6(3) . . . . ? N1 Ru1 N2 C7 30.1(3) . . . . ? P1 Ru1 N2 C7 26.4(5) . . . . ? Cl2 Ru1 N2 C7 115.1(3) . . . . ? Cl1 Ru1 N2 C7 -64.2(3) . . . . ? N4 Ru1 N2 C17 -35.7(3) . . . . ? N1 Ru1 N2 C17 146.0(3) . . . . ? P1 Ru1 N2 C17 142.3(3) . . . . ? Cl2 Ru1 N2 C17 -129.1(3) . . . . ? Cl1 Ru1 N2 C17 51.6(3) . . . . ? C1 P1 C8 C11 80.9(4) . . . . ? C12 P1 C8 C11 -170.1(4) . . . . ? Ru1 P1 C8 C11 -26.1(5) . . . . ? C1 P1 C8 C9 -38.0(6) . . . . ? C12 P1 C8 C9 71.0(5) . . . . ? Ru1 P1 C8 C9 -145.0(4) . . . . ? C1 P1 C8 C10 -161.0(5) . . . . ? C12 P1 C8 C10 -52.0(5) . . . . ? Ru1 P1 C8 C10 91.9(5) . . . . ? C1 P1 C12 C15 -169.6(4) . . . . ? C8 P1 C12 C15 80.9(4) . . . . ? Ru1 P1 C12 C15 -64.5(4) . . . . ? C1 P1 C12 C13 67.5(4) . . . . ? C8 P1 C12 C13 -42.0(5) . . . . ? Ru1 P1 C12 C13 172.6(3) . . . . ? C1 P1 C12 C14 -50.3(4) . . . . ? C8 P1 C12 C14 -159.8(4) . . . . ? Ru1 P1 C12 C14 54.8(4) . . . . ? C19 N2 C17 C18 59.9(6) . . . . ? C7 N2 C17 C18 -58.2(6) . . . . ? Ru1 N2 C17 C18 -168.1(4) . . . . ? C7 N2 C19 C16 172.6(5) . . . . ? C17 N2 C19 C16 53.3(6) . . . . ? Ru1 N2 C19 C16 -77.4(5) . . . . ? Ru2 N3 N4 Ru1 -14(9) . . . . ? N1 Ru1 N4 N3 91(8) . . . . ? P1 Ru1 N4 N3 -135(7) . . . . ? N2 Ru1 N4 N3 44(7) . . . . ? Cl2 Ru1 N4 N3 134(7) . . . . ? Cl1 Ru1 N4 N3 -39(7) . . . . ? N4 N3 Ru2 N6 34(4) . . . . ? N4 N3 Ru2 N5 51(3) . . . . ? N4 N3 Ru2 P2 -130(3) . . . . ? N4 N3 Ru2 Cl3 140(3) . . . . ? N4 N3 Ru2 Cl4 -34(3) . . . . ? N3 Ru2 P2 C26 -157.1(2) . . . . ? N6 Ru2 P2 C26 24.0(2) . . . . ? N5 Ru2 P2 C26 19.8(5) . . . . ? Cl3 Ru2 P2 C26 -61.4(2) . . . . ? Cl4 Ru2 P2 C26 116.0(2) . . . . ? N3 Ru2 P2 C27 94.2(3) . . . . ? N6 Ru2 P2 C27 -84.6(3) . . . . ? N5 Ru2 P2 C27 -88.8(5) . . . . ? Cl3 Ru2 P2 C27 -170.1(3) . . . . ? Cl4 Ru2 P2 C27 7.4(3) . . . . ? N3 Ru2 P2 C31 -46.5(3) . . . . ? N6 Ru2 P2 C31 134.7(3) . . . . ? N5 Ru2 P2 C31 130.4(5) . . . . ? Cl3 Ru2 P2 C31 49.2(3) . . . . ? Cl4 Ru2 P2 C31 -133.4(3) . . . . ? N3 Ru2 N5 C35 95.9(4) . . . . ? N6 Ru2 N5 C35 -85.3(4) . . . . ? P2 Ru2 N5 C35 -81.0(6) . . . . ? Cl3 Ru2 N5 C35 0.3(4) . . . . ? Cl4 Ru2 N5 C35 -179.1(4) . . . . ? N3 Ru2 N5 C20 -147.7(3) . . . . ? N6 Ru2 N5 C20 31.1(3) . . . . ? P2 Ru2 N5 C20 35.4(6) . . . . ? Cl3 Ru2 N5 C20 116.7(3) . . . . ? Cl4 Ru2 N5 C20 -62.7(3) . . . . ? N3 Ru2 N5 C37 -33.4(4) . . . . ? N6 Ru2 N5 C37 145.3(4) . . . . ? P2 Ru2 N5 C37 149.6(4) . . . . ? Cl3 Ru2 N5 C37 -129.0(4) . . . . ? Cl4 Ru2 N5 C37 51.5(4) . . . . ? N3 Ru2 N6 C25 178(51) . . . . ? N5 Ru2 N6 C25 161.3(4) . . . . ? P2 Ru2 N6 C25 -17.3(4) . . . . ? Cl3 Ru2 N6 C25 72.2(4) . . . . ? Cl4 Ru2 N6 C25 -114.1(4) . . . . ? N3 Ru2 N6 C21 2(3) . . . . ? N5 Ru2 N6 C21 -14.7(4) . . . . ? P2 Ru2 N6 C21 166.6(4) . . . . ? Cl3 Ru2 N6 C21 -103.8(4) . . . . ? Cl4 Ru2 N6 C21 69.8(4) . . . . ? C35 N5 C20 C21 80.0(6) . . . . ? C37 N5 C20 C21 -159.5(6) . . . . ? Ru2 N5 C20 C21 -42.7(6) . . . . ? C25 N6 C21 C22 1.8(9) . . . . ? Ru2 N6 C21 C22 177.9(5) . . . . ? C25 N6 C21 C20 177.4(5) . . . . ? Ru2 N6 C21 C20 -6.4(7) . . . . ? N5 C20 C21 N6 37.1(8) . . . . ? N5 C20 C21 C22 -147.4(6) . . . . ? N6 C21 C22 C23 0.4(10) . . . . ? C20 C21 C22 C23 -174.9(6) . . . . ? C21 C22 C23 C24 -1.1(10) . . . . ? C22 C23 C24 C25 -0.3(9) . . . . ? C21 N6 C25 C24 -3.2(8) . . . . ? Ru2 N6 C25 C24 -179.1(4) . . . . ? C21 N6 C25 C26 174.9(5) . . . . ? Ru2 N6 C25 C26 -1.1(6) . . . . ? C23 C24 C25 N6 2.4(8) . . . . ? C23 C24 C25 C26 -175.5(6) . . . . ? N6 C25 C26 P2 25.3(6) . . . . ? C24 C25 C26 P2 -156.6(5) . . . . ? C27 P2 C26 C25 89.4(5) . . . . ? C31 P2 C26 C25 -159.0(4) . . . . ? Ru2 P2 C26 C25 -32.2(4) . . . . ? C26 P2 C27 C30 -49.8(6) . . . . ? C31 P2 C27 C30 -158.3(5) . . . . ? Ru2 P2 C27 C30 55.2(5) . . . . ? C26 P2 C27 C28 69.4(7) . . . . ? C31 P2 C27 C28 -39.1(7) . . . . ? Ru2 P2 C27 C28 174.4(5) . . . . ? C26 P2 C27 C29 -167.6(7) . . . . ? C31 P2 C27 C29 83.9(8) . . . . ? Ru2 P2 C27 C29 -62.5(8) . . . . ? C26 P2 C31 C33 82.0(5) . . . . ? C27 P2 C31 C33 -169.7(5) . . . . ? Ru2 P2 C31 C33 -25.3(6) . . . . ? C26 P2 C31 C32 -38.1(7) . . . . ? C27 P2 C31 C32 70.2(7) . . . . ? Ru2 P2 C31 C32 -145.3(5) . . . . ? C26 P2 C31 C34 -159.5(5) . . . . ? C27 P2 C31 C34 -51.2(6) . . . . ? Ru2 P2 C31 C34 93.3(6) . . . . ? C20 N5 C35 C36 170.7(5) . . . . ? C37 N5 C35 C36 52.1(7) . . . . ? Ru2 N5 C35 C36 -77.4(5) . . . . ? C35 N5 C37 C38 55.7(7) . . . . ? C20 N5 C37 C38 -62.9(7) . . . . ? Ru2 N5 C37 C38 -172.0(5) . . . . ? C43 C39 C40 C41 -27.0(16) . . . . ? C39 C40 C41 C42 20.7(11) . . . . ? C40 C41 C42 C43 -7.4(17) . . . . ? C40 C39 C43 C42 22(3) . . . . ? C41 C42 C43 C39 -8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.774 _refine_diff_density_min -1.047 _refine_diff_density_rms 0.136 # Attachment 'compound2new.cif' data_m426new _database_code_depnum_ccdc_archive 'CCDC 620163' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H50 Cl F3 N2 O3 P2 Ru S' _chemical_formula_weight 870.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.357(3) _cell_length_b 16.863(3) _cell_length_c 19.073(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.09(3) _cell_angle_gamma 90.00 _cell_volume 3958.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 40442 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8811 _exptl_absorpt_correction_T_max 0.9379 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '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 8871 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.53 _reflns_number_total 8871 _reflns_number_gt 7331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect package (Bruker Nonius)' _computing_cell_refinement HKL _computing_data_reduction HKL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0109P)^2^+8.4379P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8871 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.302156(18) 0.059773(12) 0.169207(11) 0.01389(6) Uani 1 1 d . . . P1 P 0.12585(6) 0.05370(4) 0.19824(4) 0.01794(15) Uani 1 1 d . . . Cl1 Cl 0.27374(6) 0.06903(4) 0.04360(3) 0.02166(15) Uani 1 1 d . . . P2 P 0.33612(6) 0.19010(4) 0.18853(4) 0.01526(15) Uani 1 1 d . . . N1 N 0.33652(19) 0.02866(13) 0.27277(12) 0.0169(5) Uani 1 1 d . . . C2 C 0.4399(2) 0.00529(16) 0.29276(14) 0.0188(6) Uani 1 1 d . . . C3 C 0.4687(3) -0.02413(17) 0.35957(16) 0.0257(7) Uani 1 1 d . . . H3 H 0.5414 -0.0399 0.3727 0.031 Uiso 1 1 calc R . . C4 C 0.3911(3) -0.03036(18) 0.40705(16) 0.0297(7) Uani 1 1 d . . . H4 H 0.4097 -0.0508 0.4530 0.036 Uiso 1 1 calc R . . C5 C 0.2858(3) -0.00647(18) 0.38686(16) 0.0275(7) Uani 1 1 d . . . H5 H 0.2314 -0.0105 0.4189 0.033 Uiso 1 1 calc R . . C6 C 0.2599(3) 0.02349(17) 0.31949(15) 0.0225(6) Uani 1 1 d . . . C7 C 0.5209(2) 0.01976(16) 0.24018(14) 0.0184(6) Uani 1 1 d . . . H7A H 0.5473 0.0751 0.2446 0.022 Uiso 1 1 calc R . . H7B H 0.5840 -0.0159 0.2504 0.022 Uiso 1 1 calc R . . N2 N 0.47257(19) 0.00577(13) 0.16647(12) 0.0162(5) Uani 1 1 d . . . C8 C 0.4693(2) -0.08286(16) 0.15559(15) 0.0200(6) Uani 1 1 d . . . H8A H 0.4176 -0.1060 0.1867 0.024 Uiso 1 1 calc R . . H8B H 0.5421 -0.1048 0.1702 0.024 Uiso 1 1 calc R . . C9 C 0.4361(3) -0.10891(17) 0.07993(16) 0.0249(7) Uani 1 1 d . . . H9A H 0.3749 -0.0765 0.0603 0.037 Uiso 1 1 calc R . . H9B H 0.4145 -0.1648 0.0796 0.037 Uiso 1 1 calc R . . H9C H 0.4977 -0.1021 0.0515 0.037 Uiso 1 1 calc R . . C10 C 0.5441(2) 0.04231(16) 0.11583(15) 0.0208(6) Uani 1 1 d . . . H10A H 0.5492 0.0999 0.1255 0.025 Uiso 1 1 calc R . . H10B H 0.5086 0.0357 0.0676 0.025 Uiso 1 1 calc R . . C11 C 0.6585(3) 0.00898(19) 0.11764(17) 0.0292(7) Uani 1 1 d . . . H11A H 0.6937 0.0126 0.1656 0.044 Uiso 1 1 calc R . . H11B H 0.7003 0.0395 0.0857 0.044 Uiso 1 1 calc R . . H11C H 0.6552 -0.0467 0.1028 0.044 Uiso 1 1 calc R . . C12 C 0.1493(2) 0.05590(19) 0.29552(15) 0.0248(6) Uani 1 1 d . . . H12A H 0.1435 0.1112 0.3123 0.030 Uiso 1 1 calc R . . H12B H 0.0929 0.0239 0.3161 0.030 Uiso 1 1 calc R . . C13 C 0.0953(2) -0.05413(17) 0.17553(16) 0.0240(6) Uani 1 1 d . . . C14 C 0.0320(3) -0.06301(19) 0.10256(17) 0.0311(7) Uani 1 1 d . . . H14A H 0.0676 -0.0316 0.0680 0.047 Uiso 1 1 calc R . . H14B H -0.0426 -0.0441 0.1048 0.047 Uiso 1 1 calc R . . H14C H 0.0308 -0.1189 0.0886 0.047 Uiso 1 1 calc R . . C15 C 0.0383(3) -0.1011(2) 0.2308(2) 0.0383(9) Uani 1 1 d . . . H15A H 0.0284 -0.1562 0.2153 0.057 Uiso 1 1 calc R . . H15B H -0.0327 -0.0773 0.2365 0.057 Uiso 1 1 calc R . . H15C H 0.0829 -0.0998 0.2759 0.057 Uiso 1 1 calc R . . C16 C 0.2078(3) -0.09158(17) 0.17108(17) 0.0253(7) Uani 1 1 d . . . H16A H 0.2473 -0.0922 0.2180 0.038 Uiso 1 1 calc R . . H16B H 0.2487 -0.0604 0.1390 0.038 Uiso 1 1 calc R . . H16C H 0.1993 -0.1460 0.1534 0.038 Uiso 1 1 calc R . . C17 C -0.0037(2) 0.11265(18) 0.18021(17) 0.0254(7) Uani 1 1 d . . . C18 C 0.0137(3) 0.19638(18) 0.21139(18) 0.0273(7) Uani 1 1 d . . . H18A H -0.0521 0.2280 0.2005 0.041 Uiso 1 1 calc R . . H18B H 0.0749 0.2218 0.1909 0.041 Uiso 1 1 calc R . . H18C H 0.0294 0.1926 0.2626 0.041 Uiso 1 1 calc R . . C19 C -0.0970(3) 0.0745(2) 0.2166(2) 0.0349(8) Uani 1 1 d . . . H19A H -0.0747 0.0674 0.2668 0.052 Uiso 1 1 calc R . . H19B H -0.1149 0.0228 0.1951 0.052 Uiso 1 1 calc R . . H19C H -0.1611 0.1090 0.2110 0.052 Uiso 1 1 calc R . . C20 C -0.0366(3) 0.11955(19) 0.10034(18) 0.0319(8) Uani 1 1 d . . . H20A H -0.0746 0.1699 0.0905 0.048 Uiso 1 1 calc R . . H20B H -0.0846 0.0754 0.0852 0.048 Uiso 1 1 calc R . . H20C H 0.0287 0.1178 0.0747 0.048 Uiso 1 1 calc R . . C21 C 0.2573(2) 0.26594(16) 0.13639(16) 0.0213(6) Uani 1 1 d . . . C22 C 0.1803(2) 0.24659(18) 0.08260(16) 0.0242(6) Uani 1 1 d . . . H22 H 0.1651 0.1924 0.0722 0.029 Uiso 1 1 calc R . . C23 C 0.1243(3) 0.3058(2) 0.04303(19) 0.0354(8) Uani 1 1 d . . . H23 H 0.0719 0.2919 0.0056 0.043 Uiso 1 1 calc R . . C24 C 0.1453(3) 0.3845(2) 0.0586(2) 0.0416(9) Uani 1 1 d . . . H24 H 0.1060 0.4248 0.0324 0.050 Uiso 1 1 calc R . . C25 C 0.2236(3) 0.4052(2) 0.1123(2) 0.0418(9) Uani 1 1 d . . . H25 H 0.2383 0.4594 0.1229 0.050 Uiso 1 1 calc R . . C26 C 0.2801(3) 0.34594(18) 0.15038(19) 0.0318(8) Uani 1 1 d . . . H26 H 0.3350 0.3598 0.1864 0.038 Uiso 1 1 calc R . . C27 C 0.4720(2) 0.22424(15) 0.16838(15) 0.0170(6) Uani 1 1 d . . . C28 C 0.4872(3) 0.23517(17) 0.09678(16) 0.0230(6) Uani 1 1 d . . . H28 H 0.4279 0.2276 0.0622 0.028 Uiso 1 1 calc R . . C29 C 0.5882(3) 0.25694(17) 0.07622(17) 0.0270(7) Uani 1 1 d . . . H29 H 0.5976 0.2649 0.0278 0.032 Uiso 1 1 calc R . . C30 C 0.6753(3) 0.26706(18) 0.12659(18) 0.0280(7) Uani 1 1 d . . . H30 H 0.7446 0.2811 0.1126 0.034 Uiso 1 1 calc R . . C31 C 0.6612(3) 0.25666(18) 0.19705(17) 0.0261(7) Uani 1 1 d . . . H31 H 0.7211 0.2633 0.2313 0.031 Uiso 1 1 calc R . . C32 C 0.5594(2) 0.23639(16) 0.21818(16) 0.0215(6) Uani 1 1 d . . . H32 H 0.5500 0.2309 0.2668 0.026 Uiso 1 1 calc R . . C33 C 0.3250(2) 0.22203(16) 0.27989(15) 0.0185(6) Uani 1 1 d . . . C34 C 0.3941(2) 0.19009(16) 0.33482(15) 0.0206(6) Uani 1 1 d . . . H34 H 0.4485 0.1532 0.3244 0.025 Uiso 1 1 calc R . . C35 C 0.3845(3) 0.21128(19) 0.40434(16) 0.0290(7) Uani 1 1 d . . . H35 H 0.4325 0.1894 0.4409 0.035 Uiso 1 1 calc R . . C36 C 0.3046(3) 0.2644(2) 0.42021(18) 0.0334(8) Uani 1 1 d . . . H36 H 0.2978 0.2792 0.4677 0.040 Uiso 1 1 calc R . . C37 C 0.2353(3) 0.2957(2) 0.36694(18) 0.0340(8) Uani 1 1 d . . . H37 H 0.1801 0.3317 0.3780 0.041 Uiso 1 1 calc R . . C38 C 0.2446(2) 0.27542(18) 0.29714(17) 0.0245(7) Uani 1 1 d . . . H38 H 0.1963 0.2978 0.2610 0.029 Uiso 1 1 calc R . . S1 S 0.28838(6) -0.35757(5) 0.10740(4) 0.02389(16) Uani 1 1 d . . . O1 O 0.3235(3) -0.27796(17) 0.12081(18) 0.0731(11) Uani 1 1 d . . . O2 O 0.3382(3) -0.3953(2) 0.05267(16) 0.0902(14) Uani 1 1 d . . . O3 O 0.27946(19) -0.40566(14) 0.16836(12) 0.0333(5) Uani 1 1 d . . . C100 C 0.1503(3) -0.3436(2) 0.0705(2) 0.0443(10) Uani 1 1 d . . . F1 F 0.1452(2) -0.30017(17) 0.01191(14) 0.0689(8) Uani 1 1 d . . . F2 F 0.0909(2) -0.3065(2) 0.11384(19) 0.1029(13) Uani 1 1 d . . . F3 F 0.1014(3) -0.41144(19) 0.0555(2) 0.1321(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01661(11) 0.01196(10) 0.01316(11) -0.00005(8) 0.00161(8) -0.00106(8) P1 0.0173(4) 0.0173(3) 0.0196(4) -0.0016(3) 0.0039(3) -0.0029(3) Cl1 0.0303(4) 0.0202(3) 0.0142(3) 0.0002(3) 0.0008(3) 0.0026(3) P2 0.0177(4) 0.0122(3) 0.0157(3) -0.0005(3) 0.0004(3) -0.0011(3) N1 0.0229(13) 0.0134(11) 0.0145(11) 0.0003(9) 0.0024(10) -0.0019(9) C2 0.0247(15) 0.0144(13) 0.0166(14) -0.0020(10) -0.0014(12) -0.0004(11) C3 0.0333(18) 0.0215(15) 0.0210(15) 0.0007(12) -0.0048(13) 0.0032(13) C4 0.048(2) 0.0246(16) 0.0165(15) 0.0039(12) 0.0011(14) 0.0006(14) C5 0.0396(19) 0.0268(16) 0.0175(15) 0.0023(12) 0.0102(14) -0.0041(14) C6 0.0319(17) 0.0183(14) 0.0180(15) -0.0029(11) 0.0060(13) -0.0047(12) C7 0.0177(15) 0.0194(14) 0.0176(14) -0.0027(11) -0.0021(11) 0.0011(11) N2 0.0207(13) 0.0132(11) 0.0150(11) -0.0002(9) 0.0025(9) -0.0004(9) C8 0.0250(16) 0.0143(13) 0.0204(15) 0.0001(11) 0.0010(12) 0.0020(11) C9 0.0314(18) 0.0186(14) 0.0249(16) -0.0035(12) 0.0028(13) -0.0004(12) C10 0.0235(16) 0.0184(14) 0.0210(15) 0.0000(11) 0.0057(12) 0.0002(11) C11 0.0243(17) 0.0348(18) 0.0292(17) -0.0036(14) 0.0066(14) -0.0001(14) C12 0.0247(16) 0.0287(16) 0.0222(15) -0.0021(13) 0.0079(12) -0.0022(13) C13 0.0255(16) 0.0167(14) 0.0302(16) -0.0010(12) 0.0050(13) -0.0082(12) C14 0.0327(18) 0.0222(15) 0.0373(19) -0.0069(14) -0.0035(15) -0.0055(14) C15 0.044(2) 0.0250(17) 0.048(2) 0.0048(15) 0.0116(18) -0.0119(15) C16 0.0303(17) 0.0140(13) 0.0314(17) 0.0007(12) 0.0020(14) -0.0018(12) C17 0.0187(16) 0.0239(15) 0.0340(18) -0.0064(13) 0.0049(13) -0.0034(12) C18 0.0216(16) 0.0247(16) 0.0358(18) -0.0086(13) 0.0035(14) 0.0019(12) C19 0.0178(16) 0.0374(19) 0.051(2) -0.0084(16) 0.0103(15) -0.0048(14) C20 0.0234(17) 0.0282(17) 0.042(2) -0.0045(14) -0.0066(15) 0.0018(13) C21 0.0211(15) 0.0169(14) 0.0261(16) 0.0048(11) 0.0027(13) 0.0007(11) C22 0.0223(16) 0.0244(15) 0.0258(16) 0.0018(12) 0.0007(13) 0.0029(12) C23 0.0302(19) 0.042(2) 0.0329(19) 0.0050(15) -0.0062(15) 0.0099(15) C24 0.037(2) 0.0328(19) 0.053(2) 0.0158(17) -0.0048(18) 0.0111(16) C25 0.038(2) 0.0217(17) 0.064(3) 0.0088(16) -0.0036(19) 0.0001(15) C26 0.0276(18) 0.0194(15) 0.047(2) 0.0055(14) -0.0077(15) -0.0030(13) C27 0.0203(15) 0.0104(12) 0.0205(14) 0.0000(10) 0.0028(12) -0.0016(10) C28 0.0263(17) 0.0209(14) 0.0217(15) 0.0026(11) 0.0012(13) 0.0009(12) C29 0.0343(19) 0.0227(15) 0.0252(16) 0.0026(12) 0.0097(14) -0.0019(13) C30 0.0229(17) 0.0238(15) 0.0389(19) -0.0019(13) 0.0113(14) -0.0043(13) C31 0.0197(16) 0.0260(16) 0.0325(18) -0.0055(13) 0.0018(13) -0.0028(12) C32 0.0237(16) 0.0183(14) 0.0222(15) -0.0032(11) 0.0013(12) -0.0008(12) C33 0.0199(15) 0.0149(13) 0.0209(15) -0.0054(11) 0.0034(12) -0.0037(11) C34 0.0232(16) 0.0169(13) 0.0218(15) -0.0037(11) 0.0029(12) -0.0025(11) C35 0.0323(18) 0.0337(17) 0.0206(16) -0.0036(13) 0.0001(14) -0.0050(14) C36 0.0301(19) 0.046(2) 0.0254(17) -0.0157(15) 0.0094(14) -0.0080(15) C37 0.0242(18) 0.0401(19) 0.038(2) -0.0210(15) 0.0050(15) -0.0003(14) C38 0.0189(16) 0.0268(16) 0.0275(17) -0.0080(13) 0.0002(13) -0.0008(12) S1 0.0216(4) 0.0280(4) 0.0220(4) 0.0057(3) 0.0020(3) 0.0008(3) O1 0.082(2) 0.0395(16) 0.088(2) 0.0272(16) -0.0474(19) -0.0327(16) O2 0.113(3) 0.125(3) 0.0383(18) 0.0182(18) 0.0379(19) 0.080(3) O3 0.0362(14) 0.0349(13) 0.0287(12) 0.0121(10) 0.0030(11) 0.0017(10) C100 0.029(2) 0.043(2) 0.058(3) 0.0218(19) -0.0082(18) -0.0002(16) F1 0.0511(15) 0.0877(19) 0.0634(17) 0.0418(15) -0.0200(13) 0.0017(14) F2 0.0567(18) 0.142(3) 0.117(3) 0.063(2) 0.0469(19) 0.058(2) F3 0.098(3) 0.078(2) 0.199(4) 0.055(2) -0.106(3) -0.0546(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 Ru1 N1 2.051(2) . ? Ru1 P2 2.2614(8) . ? Ru1 P1 2.2973(9) . ? Ru1 N2 2.299(2) . ? Ru1 Cl1 2.3953(9) . ? P1 C12 1.853(3) . ? P1 C17 1.890(3) . ? P1 C13 1.899(3) . ? P2 C33 1.841(3) . ? P2 C21 1.844(3) . ? P2 C27 1.848(3) . ? N1 C2 1.359(4) . ? N1 C6 1.360(4) . ? C2 C3 1.384(4) . ? C2 C7 1.498(4) . ? C3 C4 1.380(5) . ? C3 H3 0.9500 . ? C4 C5 1.383(5) . ? C4 H4 0.9500 . ? C5 C6 1.391(4) . ? C5 H5 0.9500 . ? C6 C12 1.504(4) . ? C7 N2 1.497(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? N2 C10 1.498(3) . ? N2 C8 1.509(3) . ? C8 C9 1.529(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.519(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C16 1.537(4) . ? C13 C15 1.539(4) . ? C13 C14 1.542(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.539(4) . ? C17 C18 1.540(4) . ? C17 C20 1.546(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.375(4) . ? C21 C26 1.399(4) . ? C22 C23 1.398(4) . ? C22 H22 0.9500 . ? C23 C24 1.380(5) . ? C23 H23 0.9500 . ? C24 C25 1.390(5) . ? C24 H24 0.9500 . ? C25 C26 1.387(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.389(4) . ? C27 C28 1.407(4) . ? C28 C29 1.390(4) . ? C28 H28 0.9500 . ? C29 C30 1.388(5) . ? C29 H29 0.9500 . ? C30 C31 1.382(4) . ? C30 H30 0.9500 . ? C31 C32 1.396(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.399(4) . ? C33 C38 1.402(4) . ? C34 C35 1.388(4) . ? C34 H34 0.9500 . ? C35 C36 1.387(5) . ? C35 H35 0.9500 . ? C36 C37 1.374(5) . ? C36 H36 0.9500 . ? C37 C38 1.389(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? S1 O2 1.410(3) . ? S1 O1 1.427(3) . ? S1 O3 1.430(2) . ? S1 C100 1.802(4) . ? C100 F2 1.312(5) . ? C100 F3 1.314(5) . ? C100 F1 1.333(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 P2 94.13(6) . . ? N1 Ru1 P1 82.89(7) . . ? P2 Ru1 P1 99.81(3) . . ? N1 Ru1 N2 78.98(9) . . ? P2 Ru1 N2 103.39(6) . . ? P1 Ru1 N2 151.39(6) . . ? N1 Ru1 Cl1 168.27(6) . . ? P2 Ru1 Cl1 96.22(3) . . ? P1 Ru1 Cl1 100.72(4) . . ? N2 Ru1 Cl1 93.23(6) . . ? C12 P1 C17 103.10(14) . . ? C12 P1 C13 104.95(14) . . ? C17 P1 C13 108.30(13) . . ? C12 P1 Ru1 99.96(10) . . ? C17 P1 Ru1 137.62(10) . . ? C13 P1 Ru1 99.29(10) . . ? C33 P2 C21 103.15(13) . . ? C33 P2 C27 104.54(13) . . ? C21 P2 C27 96.78(13) . . ? C33 P2 Ru1 114.22(9) . . ? C21 P2 Ru1 120.30(10) . . ? C27 P2 Ru1 115.33(9) . . ? C2 N1 C6 119.3(2) . . ? C2 N1 Ru1 116.96(18) . . ? C6 N1 Ru1 123.4(2) . . ? N1 C2 C3 121.3(3) . . ? N1 C2 C7 115.6(2) . . ? C3 C2 C7 122.9(3) . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? N1 C6 C5 120.8(3) . . ? N1 C6 C12 116.4(3) . . ? C5 C6 C12 122.8(3) . . ? N2 C7 C2 111.6(2) . . ? N2 C7 H7A 109.3 . . ? C2 C7 H7A 109.3 . . ? N2 C7 H7B 109.3 . . ? C2 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C7 N2 C10 109.4(2) . . ? C7 N2 C8 106.8(2) . . ? C10 N2 C8 109.2(2) . . ? C7 N2 Ru1 101.89(16) . . ? C10 N2 Ru1 116.46(16) . . ? C8 N2 Ru1 112.44(17) . . ? N2 C8 C9 114.6(2) . . ? N2 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? N2 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 115.7(2) . . ? N2 C10 H10A 108.3 . . ? C11 C10 H10A 108.3 . . ? N2 C10 H10B 108.3 . . ? C11 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C12 P1 110.8(2) . . ? C6 C12 H12A 109.5 . . ? P1 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C16 C13 C15 107.3(3) . . ? C16 C13 C14 107.4(3) . . ? C15 C13 C14 110.0(3) . . ? C16 C13 P1 104.08(19) . . ? C15 C13 P1 115.5(2) . . ? C14 C13 P1 111.9(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 107.1(3) . . ? C19 C17 C20 109.5(3) . . ? C18 C17 C20 109.1(3) . . ? C19 C17 P1 110.8(2) . . ? C18 C17 P1 109.0(2) . . ? C20 C17 P1 111.3(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 119.0(3) . . ? C22 C21 P2 122.3(2) . . ? C26 C21 P2 118.6(2) . . ? C21 C22 C23 120.7(3) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 119.8(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 120.3(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.4(3) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C21 120.7(3) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C32 C27 C28 118.8(3) . . ? C32 C27 P2 124.7(2) . . ? C28 C27 P2 116.4(2) . . ? C29 C28 C27 120.6(3) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 119.8(3) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C31 C30 C29 120.0(3) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.4(3) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C27 C32 C31 120.3(3) . . ? C27 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C38 118.0(3) . . ? C34 C33 P2 120.3(2) . . ? C38 C33 P2 121.6(2) . . ? C35 C34 C33 121.2(3) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C36 C35 C34 119.8(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 119.7(3) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 121.0(3) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C37 C38 C33 120.2(3) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? O2 S1 O1 114.3(3) . . ? O2 S1 O3 114.58(18) . . ? O1 S1 O3 115.61(17) . . ? O2 S1 C100 103.3(2) . . ? O1 S1 C100 102.10(18) . . ? O3 S1 C100 104.64(16) . . ? F2 C100 F3 106.2(4) . . ? F2 C100 F1 106.2(3) . . ? F3 C100 F1 108.0(4) . . ? F2 C100 S1 112.3(3) . . ? F3 C100 S1 111.9(3) . . ? F1 C100 S1 111.8(3) . . ? 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 N1 Ru1 P1 C12 16.24(12) . . . . ? P2 Ru1 P1 C12 -76.75(10) . . . . ? N2 Ru1 P1 C12 67.10(16) . . . . ? Cl1 Ru1 P1 C12 -175.06(10) . . . . ? N1 Ru1 P1 C17 138.50(16) . . . . ? P2 Ru1 P1 C17 45.51(15) . . . . ? N2 Ru1 P1 C17 -170.64(18) . . . . ? Cl1 Ru1 P1 C17 -52.80(15) . . . . ? N1 Ru1 P1 C13 -90.87(12) . . . . ? P2 Ru1 P1 C13 176.15(10) . . . . ? N2 Ru1 P1 C13 -40.00(16) . . . . ? Cl1 Ru1 P1 C13 77.83(10) . . . . ? N1 Ru1 P2 C33 -22.57(12) . . . . ? P1 Ru1 P2 C33 60.91(11) . . . . ? N2 Ru1 P2 C33 -102.21(12) . . . . ? Cl1 Ru1 P2 C33 162.96(11) . . . . ? N1 Ru1 P2 C21 -146.07(13) . . . . ? P1 Ru1 P2 C21 -62.58(12) . . . . ? N2 Ru1 P2 C21 134.29(13) . . . . ? Cl1 Ru1 P2 C21 39.46(12) . . . . ? N1 Ru1 P2 C27 98.60(12) . . . . ? P1 Ru1 P2 C27 -177.92(10) . . . . ? N2 Ru1 P2 C27 18.96(12) . . . . ? Cl1 Ru1 P2 C27 -75.87(11) . . . . ? P2 Ru1 N1 C2 -93.04(18) . . . . ? P1 Ru1 N1 C2 167.58(19) . . . . ? N2 Ru1 N1 C2 9.81(18) . . . . ? Cl1 Ru1 N1 C2 58.8(4) . . . . ? P2 Ru1 N1 C6 93.2(2) . . . . ? P1 Ru1 N1 C6 -6.2(2) . . . . ? N2 Ru1 N1 C6 -164.0(2) . . . . ? Cl1 Ru1 N1 C6 -115.0(3) . . . . ? C6 N1 C2 C3 0.4(4) . . . . ? Ru1 N1 C2 C3 -173.7(2) . . . . ? C6 N1 C2 C7 -174.8(2) . . . . ? Ru1 N1 C2 C7 11.1(3) . . . . ? N1 C2 C3 C4 0.3(4) . . . . ? C7 C2 C3 C4 175.1(3) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? C3 C4 C5 C6 -0.2(5) . . . . ? C2 N1 C6 C5 -1.0(4) . . . . ? Ru1 N1 C6 C5 172.7(2) . . . . ? C2 N1 C6 C12 175.7(2) . . . . ? Ru1 N1 C6 C12 -10.6(3) . . . . ? C4 C5 C6 N1 0.9(4) . . . . ? C4 C5 C6 C12 -175.6(3) . . . . ? N1 C2 C7 N2 -37.6(3) . . . . ? C3 C2 C7 N2 147.3(3) . . . . ? C2 C7 N2 C10 164.1(2) . . . . ? C2 C7 N2 C8 -77.8(3) . . . . ? C2 C7 N2 Ru1 40.3(2) . . . . ? N1 Ru1 N2 C7 -26.96(15) . . . . ? P2 Ru1 N2 C7 64.71(15) . . . . ? P1 Ru1 N2 C7 -78.61(19) . . . . ? Cl1 Ru1 N2 C7 161.88(15) . . . . ? N1 Ru1 N2 C10 -145.89(19) . . . . ? P2 Ru1 N2 C10 -54.22(18) . . . . ? P1 Ru1 N2 C10 162.47(14) . . . . ? Cl1 Ru1 N2 C10 42.96(18) . . . . ? N1 Ru1 N2 C8 87.02(18) . . . . ? P2 Ru1 N2 C8 178.69(16) . . . . ? P1 Ru1 N2 C8 35.4(2) . . . . ? Cl1 Ru1 N2 C8 -84.13(17) . . . . ? C7 N2 C8 C9 -172.3(2) . . . . ? C10 N2 C8 C9 -54.1(3) . . . . ? Ru1 N2 C8 C9 76.7(3) . . . . ? C7 N2 C10 C11 61.9(3) . . . . ? C8 N2 C10 C11 -54.6(3) . . . . ? Ru1 N2 C10 C11 176.70(19) . . . . ? N1 C6 C12 P1 25.5(3) . . . . ? C5 C6 C12 P1 -157.9(2) . . . . ? C17 P1 C12 C6 -170.3(2) . . . . ? C13 P1 C12 C6 76.4(2) . . . . ? Ru1 P1 C12 C6 -26.1(2) . . . . ? C12 P1 C13 C16 -86.2(2) . . . . ? C17 P1 C13 C16 164.2(2) . . . . ? Ru1 P1 C13 C16 16.8(2) . . . . ? C12 P1 C13 C15 31.1(3) . . . . ? C17 P1 C13 C15 -78.5(3) . . . . ? Ru1 P1 C13 C15 134.1(2) . . . . ? C12 P1 C13 C14 158.1(2) . . . . ? C17 P1 C13 C14 48.5(3) . . . . ? Ru1 P1 C13 C14 -98.9(2) . . . . ? C12 P1 C17 C19 -59.2(2) . . . . ? C13 P1 C17 C19 51.6(3) . . . . ? Ru1 P1 C17 C19 179.58(16) . . . . ? C12 P1 C17 C18 58.4(2) . . . . ? C13 P1 C17 C18 169.2(2) . . . . ? Ru1 P1 C17 C18 -62.9(3) . . . . ? C12 P1 C17 C20 178.7(2) . . . . ? C13 P1 C17 C20 -70.4(2) . . . . ? Ru1 P1 C17 C20 57.5(3) . . . . ? C33 P2 C21 C22 -131.9(3) . . . . ? C27 P2 C21 C22 121.4(3) . . . . ? Ru1 P2 C21 C22 -3.2(3) . . . . ? C33 P2 C21 C26 50.8(3) . . . . ? C27 P2 C21 C26 -55.9(3) . . . . ? Ru1 P2 C21 C26 179.4(2) . . . . ? C26 C21 C22 C23 -1.0(5) . . . . ? P2 C21 C22 C23 -178.3(2) . . . . ? C21 C22 C23 C24 -0.8(5) . . . . ? C22 C23 C24 C25 1.5(6) . . . . ? C23 C24 C25 C26 -0.3(6) . . . . ? C24 C25 C26 C21 -1.5(6) . . . . ? C22 C21 C26 C25 2.2(5) . . . . ? P2 C21 C26 C25 179.6(3) . . . . ? C33 P2 C27 C32 26.0(3) . . . . ? C21 P2 C27 C32 131.5(2) . . . . ? Ru1 P2 C27 C32 -100.3(2) . . . . ? C33 P2 C27 C28 -156.7(2) . . . . ? C21 P2 C27 C28 -51.2(2) . . . . ? Ru1 P2 C27 C28 77.0(2) . . . . ? C32 C27 C28 C29 0.7(4) . . . . ? P2 C27 C28 C29 -176.8(2) . . . . ? C27 C28 C29 C30 0.8(4) . . . . ? C28 C29 C30 C31 -1.0(5) . . . . ? C29 C30 C31 C32 -0.4(5) . . . . ? C28 C27 C32 C31 -2.0(4) . . . . ? P2 C27 C32 C31 175.2(2) . . . . ? C30 C31 C32 C27 1.9(4) . . . . ? C21 P2 C33 C34 -165.5(2) . . . . ? C27 P2 C33 C34 -64.8(2) . . . . ? Ru1 P2 C33 C34 62.2(2) . . . . ? C21 P2 C33 C38 17.8(3) . . . . ? C27 P2 C33 C38 118.5(2) . . . . ? Ru1 P2 C33 C38 -114.5(2) . . . . ? C38 C33 C34 C35 -0.9(4) . . . . ? P2 C33 C34 C35 -177.7(2) . . . . ? C33 C34 C35 C36 0.6(5) . . . . ? C34 C35 C36 C37 0.1(5) . . . . ? C35 C36 C37 C38 -0.6(5) . . . . ? C36 C37 C38 C33 0.4(5) . . . . ? C34 C33 C38 C37 0.4(4) . . . . ? P2 C33 C38 C37 177.1(2) . . . . ? O2 S1 C100 F2 -178.2(3) . . . . ? O1 S1 C100 F2 -59.3(3) . . . . ? O3 S1 C100 F2 61.6(3) . . . . ? O2 S1 C100 F3 62.4(4) . . . . ? O1 S1 C100 F3 -178.7(4) . . . . ? O3 S1 C100 F3 -57.8(4) . . . . ? O2 S1 C100 F1 -58.9(4) . . . . ? O1 S1 C100 F1 60.0(4) . . . . ? O3 S1 C100 F1 -179.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.740 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.087 # Attachment 'compound5new.cif' data_m562new _database_code_depnum_ccdc_archive 'CCDC 620164' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H43 B2 F8 N2 O3 P Ru' _chemical_formula_weight 701.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5300(3) _cell_length_b 16.7150(4) _cell_length_c 29.1060(6) _cell_angle_alpha 90.0000(10) _cell_angle_beta 90.0000(11) _cell_angle_gamma 90.0000(11) _cell_volume 6095.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 19430 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7829 _exptl_absorpt_correction_T_max 0.9384 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '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 6840 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6840 _reflns_number_gt 4817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect package (Bruker Nonius)' _computing_cell_refinement HKL _computing_data_reduction HKL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+11.3733P] 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 6840 _refine_ls_number_parameters 378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.47910(2) 0.144402(15) 0.130115(8) 0.01235(9) Uani 1 1 d . . . H1A H 0.485(4) 0.102(3) 0.0417(18) 0.046(17) Uiso 1 1 d . . . H1B H 0.477(4) 0.044(3) 0.0634(16) 0.038(16) Uiso 1 1 d . . . P2 P 0.66611(7) 0.15667(5) 0.12795(3) 0.01452(19) Uani 1 1 d . . . O2 O 0.4701(2) 0.02514(14) 0.15290(8) 0.0167(5) Uani 1 1 d . . . O3 O 0.4869(2) 0.08562(18) 0.06472(10) 0.0218(6) Uani 1 1 d . . . C1 C 0.4685(3) 0.1931(2) 0.18593(11) 0.0156(7) Uani 1 1 d . . . O1 O 0.4565(2) 0.22322(15) 0.22138(8) 0.0252(6) Uani 1 1 d . . . N1 N 0.4855(2) 0.24814(16) 0.09397(9) 0.0162(6) Uani 1 1 d . . . N2 N 0.3034(2) 0.16779(16) 0.11892(9) 0.0155(6) Uani 1 1 d . . . C10 C 0.6711(3) 0.2188(2) 0.07510(12) 0.0222(8) Uani 1 1 d . . . H10A H 0.7363 0.2523 0.0756 0.027 Uiso 1 1 calc R . . H10B H 0.6750 0.1835 0.0479 0.027 Uiso 1 1 calc R . . C11 C 0.3025(3) 0.2584(2) 0.11848(12) 0.0186(8) Uani 1 1 d . . . H11A H 0.2340 0.2777 0.1056 0.022 Uiso 1 1 calc R . . H11B H 0.3088 0.2787 0.1503 0.022 Uiso 1 1 calc R . . C12 C 0.7574(3) 0.0695(2) 0.11425(12) 0.0220(8) Uani 1 1 d . . . C13 C 0.7282(3) 0.2217(2) 0.17345(12) 0.0193(8) Uani 1 1 d . . . C14 C 0.6958(3) 0.0067(2) 0.08636(14) 0.0292(9) Uani 1 1 d . . . H14A H 0.7428 -0.0387 0.0796 0.044 Uiso 1 1 calc R . . H14B H 0.6711 0.0306 0.0575 0.044 Uiso 1 1 calc R . . H14C H 0.6342 -0.0119 0.1042 0.044 Uiso 1 1 calc R . . C15 C 0.8543(3) 0.0957(3) 0.08548(14) 0.0318(10) Uani 1 1 d . . . H15A H 0.9023 0.0501 0.0811 0.048 Uiso 1 1 calc R . . H15B H 0.8924 0.1386 0.1015 0.048 Uiso 1 1 calc R . . H15C H 0.8300 0.1152 0.0555 0.048 Uiso 1 1 calc R . . C16 C 0.7938(3) 0.0297(2) 0.15905(13) 0.0288(9) Uani 1 1 d . . . H16A H 0.7312 0.0131 0.1768 0.043 Uiso 1 1 calc R . . H16B H 0.8359 0.0678 0.1771 0.043 Uiso 1 1 calc R . . H16C H 0.8376 -0.0173 0.1519 0.043 Uiso 1 1 calc R . . C17 C 0.8487(3) 0.2352(3) 0.16684(14) 0.0304(9) Uani 1 1 d . . . H17A H 0.8745 0.2732 0.1900 0.046 Uiso 1 1 calc R . . H17B H 0.8619 0.2568 0.1361 0.046 Uiso 1 1 calc R . . H17C H 0.8865 0.1842 0.1703 0.046 Uiso 1 1 calc R . . C18 C 0.6753(3) 0.3051(2) 0.17094(12) 0.0223(8) Uani 1 1 d . . . H18A H 0.7000 0.3379 0.1968 0.033 Uiso 1 1 calc R . . H18B H 0.5976 0.2992 0.1725 0.033 Uiso 1 1 calc R . . H18C H 0.6949 0.3311 0.1420 0.033 Uiso 1 1 calc R . . C19 C 0.7099(3) 0.1859(2) 0.22157(11) 0.0226(8) Uani 1 1 d . . . H19A H 0.7618 0.1431 0.2271 0.034 Uiso 1 1 calc R . . H19B H 0.6375 0.1640 0.2234 0.034 Uiso 1 1 calc R . . H19C H 0.7188 0.2277 0.2448 0.034 Uiso 1 1 calc R . . C20 C 0.2369(3) 0.1377(2) 0.15794(12) 0.0199(8) Uani 1 1 d . . . H20A H 0.2680 0.1580 0.1869 0.024 Uiso 1 1 calc R . . H20B H 0.2423 0.0786 0.1586 0.024 Uiso 1 1 calc R . . C21 C 0.2583(3) 0.1414(2) 0.07352(11) 0.0200(8) Uani 1 1 d . . . H21A H 0.3078 0.1578 0.0487 0.024 Uiso 1 1 calc R . . H21B H 0.1895 0.1692 0.0683 0.024 Uiso 1 1 calc R . . C22 C 0.1197(3) 0.1601(3) 0.15689(14) 0.0310(10) Uani 1 1 d . . . H22A H 0.1127 0.2185 0.1574 0.046 Uiso 1 1 calc R . . H22B H 0.0838 0.1373 0.1838 0.046 Uiso 1 1 calc R . . H22C H 0.0870 0.1390 0.1288 0.046 Uiso 1 1 calc R . . C23 C 0.2402(3) 0.0519(2) 0.07045(13) 0.0273(9) Uani 1 1 d . . . H23A H 0.3031 0.0237 0.0823 0.041 Uiso 1 1 calc R . . H23B H 0.2283 0.0367 0.0383 0.041 Uiso 1 1 calc R . . H23C H 0.1776 0.0373 0.0888 0.041 Uiso 1 1 calc R . . C2 C 0.5744(3) 0.2719(2) 0.07130(11) 0.0179(8) Uani 1 1 d . . . C3 C 0.5721(3) 0.3402(2) 0.04429(13) 0.0264(9) Uani 1 1 d . . . H3 H 0.6345 0.3575 0.0286 0.032 Uiso 1 1 calc R . . C4 C 0.4779(4) 0.3828(2) 0.04037(13) 0.0294(9) Uani 1 1 d . . . H4 H 0.4756 0.4298 0.0220 0.035 Uiso 1 1 calc R . . C5 C 0.3870(4) 0.3573(2) 0.06310(13) 0.0284(9) Uani 1 1 d . . . H5 H 0.3217 0.3858 0.0601 0.034 Uiso 1 1 calc R . . C6 C 0.3932(3) 0.2897(2) 0.09013(11) 0.0178(8) Uani 1 1 d . . . C7 C 0.4515(3) -0.0145(2) 0.18778(12) 0.0169(8) Uani 1 1 d . . . C8 C 0.4650(4) -0.1027(2) 0.18610(13) 0.0280(9) Uani 1 1 d . . . H8A H 0.4845 -0.1190 0.1549 0.042 Uiso 1 1 calc R . . H8B H 0.3979 -0.1287 0.1949 0.042 Uiso 1 1 calc R . . H8C H 0.5215 -0.1188 0.2075 0.042 Uiso 1 1 calc R . . C9 C 0.4189(3) 0.0205(2) 0.23244(12) 0.0240(9) Uani 1 1 d . . . H9A H 0.4636 0.0672 0.2392 0.036 Uiso 1 1 calc R . . H9B H 0.4278 -0.0195 0.2568 0.036 Uiso 1 1 calc R . . H9C H 0.3439 0.0369 0.2309 0.036 Uiso 1 1 calc R . . B1 B 0.3442(4) 0.4249(3) 0.20038(16) 0.0275(11) Uani 1 1 d . . . F1 F 0.3464(2) 0.49319(15) 0.22815(9) 0.0430(7) Uani 1 1 d . . . F2 F 0.2784(2) 0.43835(14) 0.16293(8) 0.0385(6) Uani 1 1 d . . . F3 F 0.4458(2) 0.40606(17) 0.18580(10) 0.0502(7) Uani 1 1 d . . . F4 F 0.3018(2) 0.36149(15) 0.22543(9) 0.0481(7) Uani 1 1 d . . . B2 B 0.0294(5) 0.3447(3) 0.04530(15) 0.0340(12) Uani 1 1 d . . . F5A F 0.0277(5) 0.2937(3) 0.08166(17) 0.0333(12) Uiso 0.50 1 d P A 1 F5B F -0.0180(6) 0.3172(5) 0.0848(2) 0.072(2) Uiso 0.50 1 d P A 2 F6 F 0.1307(3) 0.3225(3) 0.02970(11) 0.0940(13) Uani 1 1 d . A . F7 F 0.0330(3) 0.42497(16) 0.05184(14) 0.0776(11) Uani 1 1 d . A . F8 F -0.0422(2) 0.32809(17) 0.01012(8) 0.0485(7) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01411(16) 0.01116(14) 0.01177(13) 0.00018(11) -0.00114(11) 0.00064(12) P2 0.0131(5) 0.0161(4) 0.0143(4) 0.0000(4) 0.0008(3) 0.0000(4) O2 0.0184(14) 0.0150(12) 0.0168(12) 0.0019(10) -0.0006(10) 0.0012(10) O3 0.0375(19) 0.0138(15) 0.0141(14) -0.0010(11) -0.0023(12) -0.0006(13) C1 0.017(2) 0.0131(17) 0.0170(17) 0.0031(14) -0.0017(14) 0.0012(15) O1 0.0283(17) 0.0271(14) 0.0203(13) -0.0057(11) 0.0012(11) 0.0031(12) N1 0.0234(18) 0.0115(14) 0.0138(13) -0.0001(12) -0.0054(12) -0.0025(13) N2 0.0154(17) 0.0118(13) 0.0194(14) -0.0044(11) -0.0030(12) 0.0028(12) C10 0.025(2) 0.026(2) 0.0154(17) 0.0013(15) 0.0048(15) -0.0023(17) C11 0.017(2) 0.0136(17) 0.0252(18) 0.0003(15) -0.0056(14) 0.0035(15) C12 0.017(2) 0.0233(19) 0.0256(18) -0.0059(16) 0.0057(15) 0.0037(16) C13 0.016(2) 0.0207(19) 0.0214(17) -0.0022(15) -0.0028(14) -0.0027(15) C14 0.029(3) 0.024(2) 0.034(2) -0.0086(18) 0.0019(18) 0.0050(18) C15 0.021(2) 0.042(2) 0.032(2) -0.005(2) 0.0075(17) 0.006(2) C16 0.029(2) 0.027(2) 0.031(2) -0.0013(17) -0.0020(17) 0.0086(18) C17 0.023(2) 0.032(2) 0.036(2) -0.0020(19) -0.0020(17) -0.0082(19) C18 0.031(2) 0.0166(18) 0.0197(18) -0.0028(15) -0.0033(16) -0.0050(17) C19 0.023(2) 0.025(2) 0.0194(17) -0.0002(16) -0.0062(15) 0.0004(17) C20 0.016(2) 0.0229(19) 0.0207(17) 0.0010(15) 0.0000(14) 0.0023(16) C21 0.021(2) 0.0199(18) 0.0186(17) -0.0005(15) -0.0061(14) -0.0001(16) C22 0.020(2) 0.037(2) 0.036(2) 0.0015(19) -0.0018(17) 0.0003(19) C23 0.035(3) 0.022(2) 0.0253(19) -0.0018(17) -0.0066(17) -0.0036(18) C2 0.024(2) 0.0181(18) 0.0117(16) 0.0007(14) -0.0027(14) -0.0057(16) C3 0.034(3) 0.025(2) 0.0204(18) 0.0059(16) 0.0000(17) -0.0075(18) C4 0.043(3) 0.0170(18) 0.028(2) 0.0084(16) -0.0082(19) -0.001(2) C5 0.035(3) 0.0168(19) 0.033(2) 0.0018(17) -0.0143(18) 0.0011(18) C6 0.022(2) 0.0139(17) 0.0176(17) 0.0001(14) -0.0061(14) 0.0014(15) C7 0.0103(19) 0.0178(18) 0.0225(18) 0.0014(15) -0.0001(13) 0.0004(14) C8 0.039(3) 0.0174(19) 0.027(2) 0.0030(16) 0.0059(18) 0.0034(18) C9 0.025(2) 0.025(2) 0.0223(19) 0.0028(16) 0.0015(16) 0.0052(17) B1 0.032(3) 0.021(2) 0.029(2) -0.0003(19) -0.0016(19) 0.004(2) F1 0.0369(17) 0.0415(14) 0.0505(15) -0.0191(13) -0.0083(12) 0.0057(12) F2 0.0485(18) 0.0297(13) 0.0372(13) 0.0029(11) -0.0112(12) 0.0024(12) F3 0.0358(17) 0.0532(17) 0.0616(18) -0.0087(15) 0.0091(13) 0.0111(14) F4 0.057(2) 0.0395(15) 0.0473(16) 0.0172(13) 0.0030(13) 0.0000(14) B2 0.067(4) 0.022(2) 0.0130(19) -0.0036(17) 0.003(2) -0.003(2) F6 0.072(3) 0.144(3) 0.066(2) -0.041(2) -0.0199(19) 0.051(3) F7 0.073(3) 0.0246(15) 0.135(3) -0.0271(18) -0.003(2) 0.0004(15) F8 0.057(2) 0.0584(17) 0.0303(13) 0.0151(13) -0.0095(12) -0.0164(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.822(3) . ? Ru1 N1 2.030(3) . ? Ru1 O2 2.104(2) . ? Ru1 O3 2.144(3) . ? Ru1 N2 2.260(3) . ? Ru1 P2 2.3530(10) . ? P2 C10 1.857(3) . ? P2 C13 1.881(4) . ? P2 C12 1.895(4) . ? O2 C7 1.235(4) . ? O3 H1A 0.72(5) . ? O3 H1B 0.71(5) . ? C1 O1 1.158(4) . ? N1 C2 1.354(5) . ? N1 C6 1.353(5) . ? N2 C20 1.495(4) . ? N2 C21 1.503(4) . ? N2 C11 1.514(4) . ? C10 C2 1.507(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C6 1.499(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C16 1.533(5) . ? C12 C14 1.535(5) . ? C12 C15 1.539(5) . ? C13 C17 1.539(5) . ? C13 C19 1.540(5) . ? C13 C18 1.545(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.516(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C23 1.517(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C2 C3 1.387(5) . ? C3 C4 1.383(6) . ? C3 H3 0.9500 . ? C4 C5 1.385(6) . ? C4 H4 0.9500 . ? C5 C6 1.380(5) . ? C5 H5 0.9500 . ? C7 C9 1.483(5) . ? C7 C8 1.485(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? B1 F3 1.379(5) . ? B1 F2 1.385(5) . ? B1 F4 1.392(5) . ? B1 F1 1.398(5) . ? B2 F7 1.355(5) . ? B2 F5A 1.360(7) . ? B2 F5B 1.374(8) . ? B2 F8 1.390(6) . ? B2 F6 1.398(7) . ? 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 C1 Ru1 N1 94.79(12) . . ? C1 Ru1 O2 97.94(12) . . ? N1 Ru1 O2 167.14(10) . . ? C1 Ru1 O3 178.30(14) . . ? N1 Ru1 O3 85.96(11) . . ? O2 Ru1 O3 81.26(11) . . ? C1 Ru1 N2 88.89(13) . . ? N1 Ru1 N2 79.40(11) . . ? O2 Ru1 N2 99.04(10) . . ? O3 Ru1 N2 89.76(11) . . ? C1 Ru1 P2 93.28(12) . . ? N1 Ru1 P2 82.66(9) . . ? O2 Ru1 P2 98.30(7) . . ? O3 Ru1 P2 88.32(9) . . ? N2 Ru1 P2 162.05(8) . . ? C10 P2 C13 104.25(17) . . ? C10 P2 C12 103.59(16) . . ? C13 P2 C12 110.03(17) . . ? C10 P2 Ru1 96.01(13) . . ? C13 P2 Ru1 116.32(12) . . ? C12 P2 Ru1 122.68(13) . . ? C7 O2 Ru1 141.1(2) . . ? Ru1 O3 H1A 130(4) . . ? Ru1 O3 H1B 119(4) . . ? H1A O3 H1B 108(5) . . ? O1 C1 Ru1 176.7(3) . . ? C2 N1 C6 120.8(3) . . ? C2 N1 Ru1 122.4(2) . . ? C6 N1 Ru1 116.6(2) . . ? C20 N2 C21 111.1(3) . . ? C20 N2 C11 109.8(3) . . ? C21 N2 C11 106.4(3) . . ? C20 N2 Ru1 112.0(2) . . ? C21 N2 Ru1 116.2(2) . . ? C11 N2 Ru1 100.4(2) . . ? C2 C10 P2 111.3(2) . . ? C2 C10 H10A 109.4 . . ? P2 C10 H10A 109.4 . . ? C2 C10 H10B 109.4 . . ? P2 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C6 C11 N2 110.4(3) . . ? C6 C11 H11A 109.6 . . ? N2 C11 H11A 109.6 . . ? C6 C11 H11B 109.6 . . ? N2 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C16 C12 C14 107.6(3) . . ? C16 C12 C15 110.6(3) . . ? C14 C12 C15 107.7(3) . . ? C16 C12 P2 109.5(2) . . ? C14 C12 P2 109.5(3) . . ? C15 C12 P2 111.8(3) . . ? C17 C13 C19 108.5(3) . . ? C17 C13 C18 106.4(3) . . ? C19 C13 C18 109.3(3) . . ? C17 C13 P2 113.7(3) . . ? C19 C13 P2 110.7(2) . . ? C18 C13 P2 108.1(2) . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 C22 116.1(3) . . ? N2 C20 H20A 108.3 . . ? C22 C20 H20A 108.3 . . ? N2 C20 H20B 108.3 . . ? C22 C20 H20B 108.3 . . ? H20A C20 H20B 107.4 . . ? N2 C21 C23 113.4(3) . . ? N2 C21 H21A 108.9 . . ? C23 C21 H21A 108.9 . . ? N2 C21 H21B 108.9 . . ? C23 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C2 C3 120.0(3) . . ? N1 C2 C10 117.0(3) . . ? C3 C2 C10 122.9(3) . . ? C4 C3 C2 119.3(4) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 118.6(4) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N1 C6 C5 121.1(4) . . ? N1 C6 C11 115.0(3) . . ? C5 C6 C11 123.9(3) . . ? O2 C7 C9 124.1(3) . . ? O2 C7 C8 119.0(3) . . ? C9 C7 C8 116.9(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? F3 B1 F2 110.2(4) . . ? F3 B1 F4 109.8(4) . . ? F2 B1 F4 108.0(4) . . ? F3 B1 F1 110.3(4) . . ? F2 B1 F1 109.6(3) . . ? F4 B1 F1 109.1(3) . . ? F7 B2 F5A 120.8(4) . . ? F7 B2 F5B 103.2(5) . . ? F5A B2 F5B 29.7(4) . . ? F7 B2 F8 108.9(4) . . ? F5A B2 F8 116.0(4) . . ? F5B B2 F8 105.7(5) . . ? F7 B2 F6 106.2(4) . . ? F5A B2 F6 95.8(5) . . ? F5B B2 F6 125.1(6) . . ? F8 B2 F6 107.1(3) . . ? 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 C1 Ru1 P2 C10 -119.28(16) . . . . ? N1 Ru1 P2 C10 -24.86(14) . . . . ? O2 Ru1 P2 C10 142.20(13) . . . . ? O3 Ru1 P2 C10 61.28(15) . . . . ? N2 Ru1 P2 C10 -22.7(3) . . . . ? C1 Ru1 P2 C13 -10.12(16) . . . . ? N1 Ru1 P2 C13 84.30(15) . . . . ? O2 Ru1 P2 C13 -108.64(14) . . . . ? O3 Ru1 P2 C13 170.44(15) . . . . ? N2 Ru1 P2 C13 86.4(3) . . . . ? C1 Ru1 P2 C12 130.34(17) . . . . ? N1 Ru1 P2 C12 -135.24(16) . . . . ? O2 Ru1 P2 C12 31.82(15) . . . . ? O3 Ru1 P2 C12 -49.10(16) . . . . ? N2 Ru1 P2 C12 -133.1(3) . . . . ? C1 Ru1 O2 C7 8.9(4) . . . . ? N1 Ru1 O2 C7 -163.2(5) . . . . ? O3 Ru1 O2 C7 -169.5(4) . . . . ? N2 Ru1 O2 C7 -81.2(4) . . . . ? P2 Ru1 O2 C7 103.5(4) . . . . ? N1 Ru1 C1 O1 102(5) . . . . ? O2 Ru1 C1 O1 -77(5) . . . . ? O3 Ru1 C1 O1 -15(9) . . . . ? N2 Ru1 C1 O1 22(5) . . . . ? P2 Ru1 C1 O1 -175(100) . . . . ? C1 Ru1 N1 C2 112.3(3) . . . . ? O2 Ru1 N1 C2 -75.6(6) . . . . ? O3 Ru1 N1 C2 -69.3(3) . . . . ? N2 Ru1 N1 C2 -159.8(3) . . . . ? P2 Ru1 N1 C2 19.6(2) . . . . ? C1 Ru1 N1 C6 -73.4(3) . . . . ? O2 Ru1 N1 C6 98.8(5) . . . . ? O3 Ru1 N1 C6 105.1(2) . . . . ? N2 Ru1 N1 C6 14.6(2) . . . . ? P2 Ru1 N1 C6 -166.1(2) . . . . ? C1 Ru1 N2 C20 -52.8(2) . . . . ? N1 Ru1 N2 C20 -147.9(2) . . . . ? O2 Ru1 N2 C20 45.0(2) . . . . ? O3 Ru1 N2 C20 126.1(2) . . . . ? P2 Ru1 N2 C20 -150.1(2) . . . . ? C1 Ru1 N2 C21 178.0(2) . . . . ? N1 Ru1 N2 C21 82.9(2) . . . . ? O2 Ru1 N2 C21 -84.2(2) . . . . ? O3 Ru1 N2 C21 -3.1(2) . . . . ? P2 Ru1 N2 C21 80.7(3) . . . . ? C1 Ru1 N2 C11 63.7(2) . . . . ? N1 Ru1 N2 C11 -31.41(19) . . . . ? O2 Ru1 N2 C11 161.55(18) . . . . ? O3 Ru1 N2 C11 -117.3(2) . . . . ? P2 Ru1 N2 C11 -33.5(4) . . . . ? C13 P2 C10 C2 -87.2(3) . . . . ? C12 P2 C10 C2 157.7(3) . . . . ? Ru1 P2 C10 C2 32.0(3) . . . . ? C20 N2 C11 C6 162.2(3) . . . . ? C21 N2 C11 C6 -77.5(3) . . . . ? Ru1 N2 C11 C6 44.1(3) . . . . ? C10 P2 C12 C16 159.6(3) . . . . ? C13 P2 C12 C16 48.6(3) . . . . ? Ru1 P2 C12 C16 -94.0(3) . . . . ? C10 P2 C12 C14 -82.7(3) . . . . ? C13 P2 C12 C14 166.4(2) . . . . ? Ru1 P2 C12 C14 23.8(3) . . . . ? C10 P2 C12 C15 36.6(3) . . . . ? C13 P2 C12 C15 -74.4(3) . . . . ? Ru1 P2 C12 C15 143.0(2) . . . . ? C10 P2 C13 C17 -69.0(3) . . . . ? C12 P2 C13 C17 41.5(3) . . . . ? Ru1 P2 C13 C17 -173.2(2) . . . . ? C10 P2 C13 C19 168.6(3) . . . . ? C12 P2 C13 C19 -80.9(3) . . . . ? Ru1 P2 C13 C19 64.3(3) . . . . ? C10 P2 C13 C18 48.9(3) . . . . ? C12 P2 C13 C18 159.4(2) . . . . ? Ru1 P2 C13 C18 -55.3(3) . . . . ? C21 N2 C20 C22 -56.1(4) . . . . ? C11 N2 C20 C22 61.4(4) . . . . ? Ru1 N2 C20 C22 172.1(3) . . . . ? C20 N2 C21 C23 -53.1(4) . . . . ? C11 N2 C21 C23 -172.7(3) . . . . ? Ru1 N2 C21 C23 76.5(4) . . . . ? C6 N1 C2 C3 1.0(5) . . . . ? Ru1 N1 C2 C3 175.1(3) . . . . ? C6 N1 C2 C10 -175.9(3) . . . . ? Ru1 N1 C2 C10 -1.8(4) . . . . ? P2 C10 C2 N1 -23.7(4) . . . . ? P2 C10 C2 C3 159.4(3) . . . . ? N1 C2 C3 C4 -0.9(5) . . . . ? C10 C2 C3 C4 175.9(3) . . . . ? C2 C3 C4 C5 -0.2(6) . . . . ? C3 C4 C5 C6 1.1(6) . . . . ? C2 N1 C6 C5 -0.1(5) . . . . ? Ru1 N1 C6 C5 -174.5(3) . . . . ? C2 N1 C6 C11 -177.8(3) . . . . ? Ru1 N1 C6 C11 7.7(4) . . . . ? C4 C5 C6 N1 -1.0(5) . . . . ? C4 C5 C6 C11 176.6(3) . . . . ? N2 C11 C6 N1 -38.2(4) . . . . ? N2 C11 C6 C5 144.1(3) . . . . ? Ru1 O2 C7 C9 3.3(6) . . . . ? Ru1 O2 C7 C8 -174.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.653 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.176