# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Thibault E. Schmid' 'Xavier Bantreil' 'Alexandra M. Z. Slawin' 'Catherine S. J. Cazin' _publ_contact_author_name 'Catherine S. J. Cazin' _publ_contact_author_email cc111@st-andrews.ac.uk data_1A _database_code_depnum_ccdc_archive 'CCDC 811896' #TrackingRef '4121_web_deposit_cif_file_0_CatherineSJCazin_1297030467.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H53 Cl2 N2 O3 P Ru' _chemical_formula_sum 'C37 H53 Cl2 N2 O3 P Ru' _chemical_formula_weight 776.75 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.851(3) _cell_length_b 12.613(3) _cell_length_c 14.996(3) _cell_angle_alpha 90.595(2) _cell_angle_beta 104.238(4) _cell_angle_gamma 106.350(4) _cell_volume 1901.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 5592 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.8 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8413 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19402 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.36 _reflns_number_total 6900 _reflns_number_gt 6356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1075P)^2^+1.6568P] 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 6900 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1674 _refine_ls_wR_factor_gt 0.1606 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.005 _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 0.12663(3) 0.28138(2) 0.263526(18) 0.01993(14) Uani 1 1 d . . . Cl1 Cl 0.02149(10) 0.27578(8) 0.10504(6) 0.0271(2) Uani 1 1 d . . . Cl2 Cl 0.24736(10) 0.32405(8) 0.42306(6) 0.0289(2) Uani 1 1 d . . . C1 C -0.0217(4) 0.3396(3) 0.2981(2) 0.0212(8) Uani 1 1 d . . . N2 N -0.0195(3) 0.4472(3) 0.2928(2) 0.0245(7) Uani 1 1 d . . . C3 C -0.1201(4) 0.4746(3) 0.3320(3) 0.0320(9) Uani 1 1 d . . . H3A H -0.1725 0.5145 0.2889 0.038 Uiso 1 1 calc R . . H3B H -0.0784 0.5201 0.3917 0.038 Uiso 1 1 calc R . . C4 C -0.2060(4) 0.3605(3) 0.3446(3) 0.0298(9) Uani 1 1 d . . . H4A H -0.2225 0.3578 0.4068 0.036 Uiso 1 1 calc R . . H4B H -0.2922 0.3390 0.2972 0.036 Uiso 1 1 calc R . . N5 N -0.1231(3) 0.2889(3) 0.3331(2) 0.0239(7) Uani 1 1 d . . . C6 C 0.0627(4) 0.5290(3) 0.2503(3) 0.0234(8) Uani 1 1 d . . . C7 C 0.1850(4) 0.5976(3) 0.3020(3) 0.0265(8) Uani 1 1 d . . . C8 C 0.2610(4) 0.6766(3) 0.2570(3) 0.0306(9) Uani 1 1 d . . . H8A H 0.3451 0.7231 0.2911 0.037 Uiso 1 1 calc R . . C9 C 0.2166(5) 0.6888(4) 0.1640(3) 0.0330(9) Uani 1 1 d . . . C10 C 0.0918(5) 0.6218(4) 0.1156(3) 0.0321(9) Uani 1 1 d . . . H10A H 0.0605 0.6298 0.0518 0.039 Uiso 1 1 calc R . . C11 C 0.0123(4) 0.5442(3) 0.1573(3) 0.0280(9) Uani 1 1 d . . . C12 C 0.2356(4) 0.5916(4) 0.4039(3) 0.0318(9) Uani 1 1 d . . . H12A H 0.1690 0.5358 0.4257 0.048 Uiso 1 1 calc R . . H12B H 0.2524 0.6640 0.4364 0.048 Uiso 1 1 calc R . . H12C H 0.3184 0.5709 0.4159 0.048 Uiso 1 1 calc R . . C13 C 0.3001(5) 0.7753(4) 0.1164(4) 0.0482(12) Uani 1 1 d . . . H13A H 0.2733 0.8433 0.1166 0.072 Uiso 1 1 calc R . . H13B H 0.2868 0.7471 0.0525 0.072 Uiso 1 1 calc R . . H13C H 0.3942 0.7915 0.1493 0.072 Uiso 1 1 calc R . . C14 C -0.1285(4) 0.4820(4) 0.1038(3) 0.0354(10) Uani 1 1 d . . . H14A H -0.1919 0.5075 0.1284 0.053 Uiso 1 1 calc R . . H14B H -0.1439 0.4023 0.1098 0.053 Uiso 1 1 calc R . . H14C H -0.1406 0.4959 0.0384 0.053 Uiso 1 1 calc R . . C15 C -0.1728(4) 0.1733(3) 0.3427(3) 0.0244(8) Uani 1 1 d . . . C16 C -0.2541(4) 0.1020(3) 0.2647(3) 0.0256(8) Uani 1 1 d . . . C17 C -0.3072(4) -0.0084(3) 0.2778(3) 0.0310(9) Uani 1 1 d . . . H17A H -0.3633 -0.0577 0.2261 0.037 Uiso 1 1 calc R . . C18 C -0.2813(4) -0.0497(4) 0.3634(3) 0.0343(10) Uani 1 1 d . . . C19 C -0.2008(4) 0.0237(4) 0.4396(3) 0.0314(9) Uani 1 1 d . . . H19A H -0.1837 -0.0034 0.4988 0.038 Uiso 1 1 calc R . . C20 C -0.1455(4) 0.1352(3) 0.4304(3) 0.0273(8) Uani 1 1 d . . . C21 C -0.2802(4) 0.1429(4) 0.1699(3) 0.0327(9) Uani 1 1 d . . . H21A H -0.3048 0.2116 0.1727 0.049 Uiso 1 1 calc R . . H21B H -0.3531 0.0865 0.1275 0.049 Uiso 1 1 calc R . . H21C H -0.1998 0.1570 0.1477 0.049 Uiso 1 1 calc R . . C22 C -0.3373(5) -0.1718(4) 0.3728(4) 0.0466(12) Uani 1 1 d . . . H22A H -0.4247 -0.1855 0.3854 0.070 Uiso 1 1 calc R . . H22B H -0.2771 -0.1946 0.4239 0.070 Uiso 1 1 calc R . . H22C H -0.3464 -0.2144 0.3154 0.070 Uiso 1 1 calc R . . C23 C -0.0567(5) 0.2119(4) 0.5129(3) 0.0335(9) Uani 1 1 d . . . H23A H 0.0365 0.2217 0.5139 0.050 Uiso 1 1 calc R . . H23B H -0.0743 0.1801 0.5694 0.050 Uiso 1 1 calc R . . H23C H -0.0745 0.2840 0.5091 0.050 Uiso 1 1 calc R . . C24 C 0.0638(4) 0.1352(3) 0.2844(3) 0.0262(8) Uani 1 1 d . . . H24A H 0.0515 0.1264 0.3447 0.031 Uiso 1 1 calc R . . C25 C 0.0283(4) 0.0294(3) 0.2297(3) 0.0259(8) Uani 1 1 d . . . C26 C -0.0284(4) -0.0663(3) 0.2692(3) 0.0302(9) Uani 1 1 d . . . H26A H -0.0406 -0.0601 0.3295 0.036 Uiso 1 1 calc R . . C27 C -0.0673(5) -0.1703(4) 0.2212(4) 0.0396(11) Uani 1 1 d . . . H27A H -0.1071 -0.2347 0.2479 0.048 Uiso 1 1 calc R . . C28 C -0.0471(4) -0.1788(4) 0.1337(3) 0.0372(10) Uani 1 1 d . . . H28A H -0.0745 -0.2495 0.1002 0.045 Uiso 1 1 calc R . . C29 C 0.0125(4) -0.0858(4) 0.0952(3) 0.0330(9) Uani 1 1 d . . . H29A H 0.0284 -0.0928 0.0362 0.040 Uiso 1 1 calc R . . C30 C 0.0493(4) 0.0183(4) 0.1424(3) 0.0291(9) Uani 1 1 d . . . H30A H 0.0890 0.0823 0.1151 0.035 Uiso 1 1 calc R . . P1 P 0.31316(10) 0.25212(8) 0.22616(7) 0.0241(2) Uani 1 1 d . . . O31 O 0.4491(3) 0.3506(2) 0.26642(19) 0.0273(6) Uani 1 1 d . . . C31 C 0.4445(4) 0.4642(3) 0.2767(3) 0.0306(9) Uani 1 1 d . . . H31A H 0.3534 0.4632 0.2804 0.037 Uiso 1 1 calc R . . C32 C 0.5438(5) 0.5160(4) 0.3676(3) 0.0359(10) Uani 1 1 d . . . H32A H 0.5192 0.4735 0.4181 0.054 Uiso 1 1 calc R . . H32B H 0.5433 0.5927 0.3782 0.054 Uiso 1 1 calc R . . H32C H 0.6330 0.5154 0.3651 0.054 Uiso 1 1 calc R . . C33 C 0.4743(6) 0.5237(4) 0.1943(3) 0.0433(11) Uani 1 1 d . . . H33A H 0.4064 0.4868 0.1382 0.065 Uiso 1 1 calc R . . H33B H 0.5619 0.5221 0.1887 0.065 Uiso 1 1 calc R . . H33C H 0.4740 0.6008 0.2023 0.065 Uiso 1 1 calc R . . O34 O 0.2993(3) 0.2379(2) 0.11876(18) 0.0282(6) Uani 1 1 d . . . C34 C 0.4020(4) 0.2146(4) 0.0797(3) 0.0398(11) Uani 1 1 d . . . H34A H 0.4868 0.2282 0.1292 0.048 Uiso 1 1 calc R . . C35 C 0.4226(6) 0.2935(5) 0.0061(4) 0.0577(15) Uani 1 1 d . . . H35A H 0.4546 0.3700 0.0342 0.087 Uiso 1 1 calc R . . H35B H 0.3382 0.2827 -0.0406 0.087 Uiso 1 1 calc R . . H35C H 0.4885 0.2791 -0.0230 0.087 Uiso 1 1 calc R . . C36 C 0.3537(5) 0.0951(4) 0.0422(3) 0.0476(13) Uani 1 1 d . . . H36A H 0.3428 0.0476 0.0927 0.071 Uiso 1 1 calc R . . H36B H 0.4188 0.0786 0.0134 0.071 Uiso 1 1 calc R . . H36C H 0.2682 0.0811 -0.0039 0.071 Uiso 1 1 calc R . . O37 O 0.3648(3) 0.1487(2) 0.25840(19) 0.0276(6) Uani 1 1 d . . . C37 C 0.3679(4) 0.1054(3) 0.3483(3) 0.0272(8) Uani 1 1 d . . . H37A H 0.2939 0.1187 0.3712 0.033 Uiso 1 1 calc R . . C38 C 0.5002(4) 0.1638(4) 0.4165(3) 0.0350(10) Uani 1 1 d . . . H38A H 0.5092 0.2431 0.4245 0.052 Uiso 1 1 calc R . . H38B H 0.5731 0.1539 0.3928 0.052 Uiso 1 1 calc R . . H38C H 0.5034 0.1321 0.4761 0.052 Uiso 1 1 calc R . . C39 C 0.3458(5) -0.0184(4) 0.3337(3) 0.0388(10) Uani 1 1 d . . . H39A H 0.2591 -0.0524 0.2901 0.058 Uiso 1 1 calc R . . H39B H 0.3480 -0.0512 0.3928 0.058 Uiso 1 1 calc R . . H39C H 0.4161 -0.0316 0.3086 0.058 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 0.0194(2) 0.0225(2) 0.0186(2) 0.00027(13) 0.00254(14) 0.00932(14) Cl1 0.0289(5) 0.0363(5) 0.0190(5) 0.0020(4) 0.0024(4) 0.0174(4) Cl2 0.0278(5) 0.0372(5) 0.0202(5) -0.0028(4) -0.0011(4) 0.0136(4) C1 0.0227(19) 0.0252(19) 0.0156(16) -0.0022(14) 0.0000(14) 0.0116(15) N2 0.0260(17) 0.0229(16) 0.0294(17) 0.0011(13) 0.0097(14) 0.0127(13) C3 0.037(2) 0.029(2) 0.040(2) 0.0036(18) 0.0171(19) 0.0177(19) C4 0.030(2) 0.033(2) 0.032(2) 0.0044(17) 0.0102(18) 0.0157(18) N5 0.0223(16) 0.0258(17) 0.0261(16) 0.0038(13) 0.0073(13) 0.0099(13) C6 0.030(2) 0.0227(19) 0.0234(18) 0.0008(15) 0.0085(16) 0.0155(16) C7 0.030(2) 0.0224(19) 0.029(2) 0.0004(16) 0.0062(17) 0.0130(16) C8 0.029(2) 0.027(2) 0.037(2) 0.0031(17) 0.0087(18) 0.0099(17) C9 0.039(2) 0.030(2) 0.039(2) 0.0098(18) 0.020(2) 0.0161(19) C10 0.042(3) 0.036(2) 0.026(2) 0.0072(17) 0.0092(18) 0.024(2) C11 0.033(2) 0.027(2) 0.027(2) 0.0005(16) 0.0041(17) 0.0168(17) C12 0.031(2) 0.036(2) 0.028(2) -0.0027(17) 0.0020(17) 0.0126(18) C13 0.053(3) 0.044(3) 0.060(3) 0.022(2) 0.032(3) 0.018(2) C14 0.033(2) 0.040(2) 0.034(2) -0.0008(18) 0.0022(18) 0.0166(19) C15 0.0203(19) 0.0244(19) 0.028(2) 0.0024(15) 0.0045(16) 0.0078(15) C16 0.0177(19) 0.031(2) 0.030(2) 0.0033(16) 0.0064(16) 0.0102(16) C17 0.019(2) 0.032(2) 0.039(2) -0.0012(18) 0.0036(17) 0.0076(17) C18 0.028(2) 0.029(2) 0.048(3) 0.0091(19) 0.0121(19) 0.0097(18) C19 0.028(2) 0.035(2) 0.036(2) 0.0124(18) 0.0118(18) 0.0129(18) C20 0.022(2) 0.035(2) 0.027(2) 0.0027(17) 0.0070(16) 0.0110(17) C21 0.025(2) 0.036(2) 0.029(2) -0.0005(18) -0.0026(17) 0.0054(17) C22 0.043(3) 0.036(3) 0.055(3) 0.014(2) 0.008(2) 0.006(2) C23 0.035(2) 0.039(2) 0.026(2) 0.0029(18) 0.0057(18) 0.0135(19) C24 0.0230(19) 0.035(2) 0.0235(18) 0.0045(16) 0.0044(15) 0.0145(17) C25 0.0196(19) 0.0250(19) 0.032(2) 0.0028(16) 0.0003(16) 0.0097(15) C26 0.028(2) 0.031(2) 0.034(2) 0.0018(17) 0.0081(18) 0.0134(18) C27 0.033(2) 0.028(2) 0.056(3) 0.005(2) 0.008(2) 0.0083(19) C28 0.033(2) 0.031(2) 0.044(3) -0.0107(19) -0.0046(19) 0.0154(19) C29 0.030(2) 0.034(2) 0.034(2) -0.0042(18) -0.0004(18) 0.0146(18) C30 0.028(2) 0.031(2) 0.028(2) -0.0017(16) 0.0017(16) 0.0118(17) P1 0.0215(5) 0.0266(5) 0.0245(5) -0.0005(4) 0.0035(4) 0.0100(4) O31 0.0212(14) 0.0267(14) 0.0331(15) -0.0018(12) 0.0035(11) 0.0087(11) C31 0.029(2) 0.024(2) 0.039(2) 0.0019(17) 0.0071(18) 0.0093(17) C32 0.034(2) 0.029(2) 0.040(2) -0.0051(18) 0.0067(19) 0.0044(18) C33 0.056(3) 0.037(3) 0.041(3) 0.006(2) 0.014(2) 0.019(2) O34 0.0250(14) 0.0406(16) 0.0231(13) -0.0019(12) 0.0073(11) 0.0152(12) C34 0.026(2) 0.061(3) 0.037(2) -0.011(2) 0.0102(19) 0.019(2) C35 0.052(3) 0.071(4) 0.055(3) -0.002(3) 0.030(3) 0.012(3) C36 0.045(3) 0.060(3) 0.043(3) -0.012(2) 0.006(2) 0.029(3) O37 0.0280(15) 0.0283(15) 0.0280(14) -0.0008(11) 0.0048(12) 0.0129(12) C37 0.0215(19) 0.036(2) 0.027(2) 0.0041(17) 0.0068(16) 0.0122(17) C38 0.032(2) 0.037(2) 0.034(2) 0.0029(18) 0.0016(18) 0.0147(19) C39 0.037(2) 0.033(2) 0.049(3) 0.010(2) 0.009(2) 0.0156(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 C24 1.836(4) . ? Ru1 C1 2.114(4) . ? Ru1 P1 2.3496(11) . ? Ru1 Cl1 2.3605(10) . ? Ru1 Cl2 2.4008(10) . ? C1 N5 1.338(5) . ? C1 N2 1.354(5) . ? N2 C6 1.429(5) . ? N2 C3 1.476(5) . ? C3 C4 1.521(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N5 1.478(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N5 C15 1.427(5) . ? C6 C7 1.394(6) . ? C6 C11 1.403(5) . ? C7 C8 1.397(6) . ? C7 C12 1.502(6) . ? C8 C9 1.385(6) . ? C8 H8A 0.9500 . ? C9 C10 1.390(6) . ? C9 C13 1.516(6) . ? C10 C11 1.378(6) . ? C10 H10A 0.9500 . ? C11 C14 1.517(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 C20 1.397(6) . ? C15 C16 1.406(6) . ? C16 C17 1.386(6) . ? C16 C21 1.506(6) . ? C17 C18 1.384(6) . ? C17 H17A 0.9500 . ? C18 C19 1.399(6) . ? C18 C22 1.510(6) . ? C19 C20 1.388(6) . ? C19 H19A 0.9500 . ? C20 C23 1.502(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.461(5) . ? C24 H24A 0.9500 . ? C25 C30 1.395(6) . ? C25 C26 1.400(6) . ? C26 C27 1.391(6) . ? C26 H26A 0.9500 . ? C27 C28 1.391(7) . ? C27 H27A 0.9500 . ? C28 C29 1.378(6) . ? C28 H28A 0.9500 . ? C29 C30 1.390(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? P1 O34 1.584(3) . ? P1 O37 1.594(3) . ? P1 O31 1.611(3) . ? O31 C31 1.456(5) . ? C31 C33 1.508(6) . ? C31 C32 1.519(6) . ? C31 H31A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O34 C34 1.474(5) . ? C34 C36 1.502(7) . ? C34 C35 1.509(7) . ? C34 H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? O37 C37 1.456(5) . ? C37 C39 1.517(6) . ? C37 C38 1.521(6) . ? C37 H37A 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Ru1 C1 98.47(16) . . ? C24 Ru1 P1 92.05(12) . . ? C1 Ru1 P1 169.23(11) . . ? C24 Ru1 Cl1 100.59(12) . . ? C1 Ru1 Cl1 90.22(10) . . ? P1 Ru1 Cl1 90.13(4) . . ? C24 Ru1 Cl2 90.13(12) . . ? C1 Ru1 Cl2 87.09(10) . . ? P1 Ru1 Cl2 90.57(4) . . ? Cl1 Ru1 Cl2 169.23(4) . . ? N5 C1 N2 107.5(3) . . ? N5 C1 Ru1 131.1(3) . . ? N2 C1 Ru1 121.3(3) . . ? C1 N2 C6 126.6(3) . . ? C1 N2 C3 112.9(3) . . ? C6 N2 C3 120.4(3) . . ? N2 C3 C4 102.2(3) . . ? N2 C3 H3A 111.3 . . ? C4 C3 H3A 111.3 . . ? N2 C3 H3B 111.3 . . ? C4 C3 H3B 111.3 . . ? H3A C3 H3B 109.2 . . ? N5 C4 C3 102.2(3) . . ? N5 C4 H4A 111.3 . . ? C3 C4 H4A 111.3 . . ? N5 C4 H4B 111.3 . . ? C3 C4 H4B 111.3 . . ? H4A C4 H4B 109.2 . . ? C1 N5 C15 127.8(3) . . ? C1 N5 C4 113.2(3) . . ? C15 N5 C4 117.8(3) . . ? C7 C6 C11 121.1(4) . . ? C7 C6 N2 120.6(3) . . ? C11 C6 N2 118.1(4) . . ? C6 C7 C8 118.2(4) . . ? C6 C7 C12 122.5(4) . . ? C8 C7 C12 119.3(4) . . ? C9 C8 C7 121.6(4) . . ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C8 C9 C10 118.5(4) . . ? C8 C9 C13 120.9(4) . . ? C10 C9 C13 120.6(4) . . ? C11 C10 C9 122.0(4) . . ? C11 C10 H10A 119.0 . . ? C9 C10 H10A 119.0 . . ? C10 C11 C6 118.4(4) . . ? C10 C11 C14 119.6(4) . . ? C6 C11 C14 121.9(4) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 121.8(4) . . ? C20 C15 N5 118.9(4) . . ? C16 C15 N5 119.2(3) . . ? C17 C16 C15 117.6(4) . . ? C17 C16 C21 120.8(4) . . ? C15 C16 C21 121.6(4) . . ? C18 C17 C16 122.4(4) . . ? C18 C17 H17A 118.8 . . ? C16 C17 H17A 118.8 . . ? C17 C18 C19 118.5(4) . . ? C17 C18 C22 120.1(4) . . ? C19 C18 C22 121.4(4) . . ? C20 C19 C18 121.5(4) . . ? C20 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? C19 C20 C15 118.3(4) . . ? C19 C20 C23 120.5(4) . . ? C15 C20 C23 121.2(4) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 Ru1 134.9(3) . . ? C25 C24 H24A 112.6 . . ? Ru1 C24 H24A 112.6 . . ? C30 C25 C26 118.8(4) . . ? C30 C25 C24 124.1(4) . . ? C26 C25 C24 117.1(4) . . ? C27 C26 C25 120.8(4) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C28 119.3(4) . . ? C26 C27 H27A 120.4 . . ? C28 C27 H27A 120.4 . . ? C29 C28 C27 120.6(4) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C28 C29 C30 120.2(4) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C29 C30 C25 120.4(4) . . ? C29 C30 H30A 119.8 . . ? C25 C30 H30A 119.8 . . ? O34 P1 O37 99.96(15) . . ? O34 P1 O31 105.01(15) . . ? O37 P1 O31 99.26(15) . . ? O34 P1 Ru1 114.20(11) . . ? O37 P1 Ru1 121.84(11) . . ? O31 P1 Ru1 114.11(11) . . ? C31 O31 P1 119.7(2) . . ? O31 C31 C33 109.7(3) . . ? O31 C31 C32 106.4(3) . . ? C33 C31 C32 113.6(4) . . ? O31 C31 H31A 109.1 . . ? C33 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? 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 . . ? C34 O34 P1 123.5(3) . . ? O34 C34 C36 108.1(4) . . ? O34 C34 C35 106.9(4) . . ? C36 C34 C35 112.8(4) . . ? O34 C34 H34A 109.7 . . ? C36 C34 H34A 109.7 . . ? C35 C34 H34A 109.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C37 O37 P1 124.4(2) . . ? O37 C37 C39 106.5(3) . . ? O37 C37 C38 109.8(3) . . ? C39 C37 C38 112.5(3) . . ? O37 C37 H37A 109.3 . . ? C39 C37 H37A 109.3 . . ? C38 C37 H37A 109.3 . . ? 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 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 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 C24 Ru1 C1 N5 5.8(4) . . . . ? P1 Ru1 C1 N5 -161.5(3) . . . . ? Cl1 Ru1 C1 N5 106.6(3) . . . . ? Cl2 Ru1 C1 N5 -83.8(3) . . . . ? C24 Ru1 C1 N2 -179.5(3) . . . . ? P1 Ru1 C1 N2 13.1(7) . . . . ? Cl1 Ru1 C1 N2 -78.8(3) . . . . ? Cl2 Ru1 C1 N2 90.8(3) . . . . ? N5 C1 N2 C6 -172.7(3) . . . . ? Ru1 C1 N2 C6 11.6(5) . . . . ? N5 C1 N2 C3 3.8(4) . . . . ? Ru1 C1 N2 C3 -171.9(3) . . . . ? C1 N2 C3 C4 -11.5(4) . . . . ? C6 N2 C3 C4 165.2(3) . . . . ? N2 C3 C4 N5 13.5(4) . . . . ? N2 C1 N5 C15 173.1(3) . . . . ? Ru1 C1 N5 C15 -11.7(6) . . . . ? N2 C1 N5 C4 6.2(4) . . . . ? Ru1 C1 N5 C4 -178.6(3) . . . . ? C3 C4 N5 C1 -13.0(4) . . . . ? C3 C4 N5 C15 178.8(3) . . . . ? C1 N2 C6 C7 -93.0(5) . . . . ? C3 N2 C6 C7 90.7(5) . . . . ? C1 N2 C6 C11 92.0(5) . . . . ? C3 N2 C6 C11 -84.2(4) . . . . ? C11 C6 C7 C8 -4.8(6) . . . . ? N2 C6 C7 C8 -179.6(3) . . . . ? C11 C6 C7 C12 173.5(4) . . . . ? N2 C6 C7 C12 -1.3(6) . . . . ? C6 C7 C8 C9 1.0(6) . . . . ? C12 C7 C8 C9 -177.3(4) . . . . ? C7 C8 C9 C10 1.5(6) . . . . ? C7 C8 C9 C13 179.8(4) . . . . ? C8 C9 C10 C11 -0.2(6) . . . . ? C13 C9 C10 C11 -178.5(4) . . . . ? C9 C10 C11 C6 -3.5(6) . . . . ? C9 C10 C11 C14 173.6(4) . . . . ? C7 C6 C11 C10 6.0(6) . . . . ? N2 C6 C11 C10 -179.1(3) . . . . ? C7 C6 C11 C14 -171.0(4) . . . . ? N2 C6 C11 C14 3.9(5) . . . . ? C1 N5 C15 C20 105.9(5) . . . . ? C4 N5 C15 C20 -87.8(4) . . . . ? C1 N5 C15 C16 -77.8(5) . . . . ? C4 N5 C15 C16 88.5(4) . . . . ? C20 C15 C16 C17 0.1(6) . . . . ? N5 C15 C16 C17 -176.1(3) . . . . ? C20 C15 C16 C21 -178.3(4) . . . . ? N5 C15 C16 C21 5.5(6) . . . . ? C15 C16 C17 C18 -0.9(6) . . . . ? C21 C16 C17 C18 177.6(4) . . . . ? C16 C17 C18 C19 1.4(7) . . . . ? C16 C17 C18 C22 -177.5(4) . . . . ? C17 C18 C19 C20 -1.1(6) . . . . ? C22 C18 C19 C20 177.7(4) . . . . ? C18 C19 C20 C15 0.5(6) . . . . ? C18 C19 C20 C23 -178.5(4) . . . . ? C16 C15 C20 C19 0.1(6) . . . . ? N5 C15 C20 C19 176.3(4) . . . . ? C16 C15 C20 C23 179.0(4) . . . . ? N5 C15 C20 C23 -4.7(6) . . . . ? C1 Ru1 C24 C25 125.3(4) . . . . ? P1 Ru1 C24 C25 -57.0(4) . . . . ? Cl1 Ru1 C24 C25 33.5(4) . . . . ? Cl2 Ru1 C24 C25 -147.6(4) . . . . ? Ru1 C24 C25 C30 6.6(6) . . . . ? Ru1 C24 C25 C26 -174.4(3) . . . . ? C30 C25 C26 C27 -2.1(6) . . . . ? C24 C25 C26 C27 178.9(4) . . . . ? C25 C26 C27 C28 1.1(6) . . . . ? C26 C27 C28 C29 0.9(7) . . . . ? C27 C28 C29 C30 -2.0(6) . . . . ? C28 C29 C30 C25 1.0(6) . . . . ? C26 C25 C30 C29 1.0(6) . . . . ? C24 C25 C30 C29 180.0(4) . . . . ? C24 Ru1 P1 O34 99.32(17) . . . . ? C1 Ru1 P1 O34 -93.2(5) . . . . ? Cl1 Ru1 P1 O34 -1.28(13) . . . . ? Cl2 Ru1 P1 O34 -170.53(13) . . . . ? C24 Ru1 P1 O37 -20.84(18) . . . . ? C1 Ru1 P1 O37 146.7(5) . . . . ? Cl1 Ru1 P1 O37 -121.44(13) . . . . ? Cl2 Ru1 P1 O37 69.31(13) . . . . ? C24 Ru1 P1 O31 -139.88(17) . . . . ? C1 Ru1 P1 O31 27.6(5) . . . . ? Cl1 Ru1 P1 O31 119.52(12) . . . . ? Cl2 Ru1 P1 O31 -49.73(12) . . . . ? O34 P1 O31 C31 94.0(3) . . . . ? O37 P1 O31 C31 -163.0(3) . . . . ? Ru1 P1 O31 C31 -31.8(3) . . . . ? P1 O31 C31 C33 -97.1(4) . . . . ? P1 O31 C31 C32 139.8(3) . . . . ? O37 P1 O34 C34 -45.8(3) . . . . ? O31 P1 O34 C34 56.6(3) . . . . ? Ru1 P1 O34 C34 -177.6(3) . . . . ? P1 O34 C34 C36 105.5(4) . . . . ? P1 O34 C34 C35 -132.9(4) . . . . ? O34 P1 O37 C37 -166.1(3) . . . . ? O31 P1 O37 C37 86.8(3) . . . . ? Ru1 P1 O37 C37 -39.3(3) . . . . ? P1 O37 C37 C39 148.5(3) . . . . ? P1 O37 C37 C38 -89.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.345 _refine_diff_density_min -1.272 _refine_diff_density_rms 0.146 # Attachment '4122_web_deposit_cif_file_1_CatherineSJCazin_1297030467.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 811897' #TrackingRef '4122_web_deposit_cif_file_1_CatherineSJCazin_1297030467.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H47 Cl2 N2 O3 P Ru' _chemical_formula_sum 'C34 H47 Cl2 N2 O3 P Ru' _chemical_formula_weight 734.68 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' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.973(3) _cell_length_b 14.976(3) _cell_length_c 15.679(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.436(6) _cell_angle_gamma 90.00 _cell_volume 3468.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 11534 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 28.5 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8543 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21173 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.33 _reflns_number_total 6276 _reflns_number_gt 5319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+4.6520P] 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 6276 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1112 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 Ru1 Ru 0.359382(18) 0.291467(18) 0.136512(18) 0.01916(11) Uani 1 1 d . . . Cl1 Cl 0.35818(6) 0.23414(6) 0.27804(6) 0.0253(2) Uani 1 1 d . . . Cl2 Cl 0.32656(6) 0.33761(6) -0.01182(6) 0.0274(2) Uani 1 1 d . . . C1 C 0.2936(2) 0.4086(2) 0.1711(2) 0.0203(7) Uani 1 1 d . . . N2 N 0.20399(19) 0.42276(19) 0.1621(2) 0.0256(7) Uani 1 1 d . . . C3 C 0.1798(3) 0.5099(3) 0.1957(3) 0.0359(10) Uani 1 1 d . . . H3A H 0.1506 0.5026 0.2476 0.043 Uiso 1 1 calc R . . H3B H 0.1388 0.5438 0.1513 0.043 Uiso 1 1 calc R . . C4 C 0.2712(2) 0.5556(3) 0.2180(3) 0.0324(9) Uani 1 1 d . . . H4A H 0.2768 0.6057 0.1781 0.039 Uiso 1 1 calc R . . H4B H 0.2812 0.5781 0.2782 0.039 Uiso 1 1 calc R . . N5 N 0.33463(19) 0.48264(19) 0.2070(2) 0.0230(7) Uani 1 1 d . . . C6 C 0.1299(2) 0.3656(2) 0.1265(3) 0.0257(8) Uani 1 1 d . . . C7 C 0.0925(2) 0.3068(2) 0.1810(3) 0.0256(8) Uani 1 1 d . . . C8 C 0.0138(3) 0.2607(3) 0.1468(3) 0.0297(9) Uani 1 1 d . . . H8A H -0.0111 0.2197 0.1827 0.036 Uiso 1 1 calc R . . C9 C -0.0296(3) 0.2726(3) 0.0619(3) 0.0320(9) Uani 1 1 d . . . C10 C 0.0094(2) 0.3307(3) 0.0100(3) 0.0308(9) Uani 1 1 d . . . H10A H -0.0184 0.3380 -0.0485 0.037 Uiso 1 1 calc R . . C11 C 0.0882(2) 0.3792(2) 0.0408(2) 0.0266(8) Uani 1 1 d . . . C12 C 0.1319(3) 0.2983(3) 0.2754(3) 0.0302(9) Uani 1 1 d . . . H12A H 0.1275 0.3558 0.3042 0.045 Uiso 1 1 calc R . . H12B H 0.1956 0.2805 0.2812 0.045 Uiso 1 1 calc R . . H12C H 0.0983 0.2530 0.3022 0.045 Uiso 1 1 calc R . . C13 C -0.1180(3) 0.2256(3) 0.0298(3) 0.0442(12) Uani 1 1 d . . . H13A H -0.1657 0.2509 0.0584 0.066 Uiso 1 1 calc R . . H13B H -0.1115 0.1618 0.0430 0.066 Uiso 1 1 calc R . . H13C H -0.1340 0.2338 -0.0329 0.066 Uiso 1 1 calc R . . C14 C 0.1220(3) 0.4474(3) -0.0171(3) 0.0357(10) Uani 1 1 d . . . H14A H 0.0953 0.5057 -0.0083 0.054 Uiso 1 1 calc R . . H14B H 0.1047 0.4293 -0.0776 0.054 Uiso 1 1 calc R . . H14C H 0.1881 0.4515 -0.0030 0.054 Uiso 1 1 calc R . . C15 C 0.4295(2) 0.5026(2) 0.2277(2) 0.0238(8) Uani 1 1 d . . . C16 C 0.4717(3) 0.5465(2) 0.1663(2) 0.0266(8) Uani 1 1 d . . . C17 C 0.5632(3) 0.5694(3) 0.1898(3) 0.0325(9) Uani 1 1 d . . . H17A H 0.5934 0.5984 0.1488 0.039 Uiso 1 1 calc R . . C18 C 0.6110(3) 0.5507(3) 0.2719(3) 0.0307(9) Uani 1 1 d . . . C19 C 0.5653(3) 0.5092(2) 0.3304(3) 0.0301(9) Uani 1 1 d . . . H19A H 0.5974 0.4968 0.3866 0.036 Uiso 1 1 calc R . . C20 C 0.4749(2) 0.4848(2) 0.3114(2) 0.0256(8) Uani 1 1 d . . . C21 C 0.4222(3) 0.5666(3) 0.0768(3) 0.0342(9) Uani 1 1 d . . . H21A H 0.3872 0.5142 0.0538 0.051 Uiso 1 1 calc R . . H21B H 0.4661 0.5817 0.0390 0.051 Uiso 1 1 calc R . . H21C H 0.3812 0.6172 0.0793 0.051 Uiso 1 1 calc R . . C22 C 0.7108(3) 0.5733(3) 0.2941(3) 0.0458(12) Uani 1 1 d . . . H22A H 0.7190 0.6232 0.3350 0.069 Uiso 1 1 calc R . . H22B H 0.7339 0.5901 0.2413 0.069 Uiso 1 1 calc R . . H22C H 0.7441 0.5211 0.3203 0.069 Uiso 1 1 calc R . . C23 C 0.4286(3) 0.4396(3) 0.3784(3) 0.0330(9) Uani 1 1 d . . . H23A H 0.4309 0.3747 0.3710 0.050 Uiso 1 1 calc R . . H23B H 0.3653 0.4590 0.3713 0.050 Uiso 1 1 calc R . . H23C H 0.4595 0.4557 0.4364 0.050 Uiso 1 1 calc R . . C24 C 0.4755(2) 0.3347(2) 0.1428(2) 0.0240(8) Uani 1 1 d . . . H24A H 0.4783 0.3807 0.1017 0.029 Uiso 1 1 calc R . . C25 C 0.5646(2) 0.3173(3) 0.1939(2) 0.0252(8) Uani 1 1 d . . . C26 C 0.6397(2) 0.3569(3) 0.1654(3) 0.0300(9) Uani 1 1 d . . . H26A H 0.6306 0.3935 0.1152 0.036 Uiso 1 1 calc R . . C27 C 0.7267(3) 0.3436(3) 0.2094(3) 0.0344(9) Uani 1 1 d . . . H27A H 0.7769 0.3695 0.1886 0.041 Uiso 1 1 calc R . . C28 C 0.7400(3) 0.2922(3) 0.2839(3) 0.0365(10) Uani 1 1 d . . . H28A H 0.7994 0.2840 0.3151 0.044 Uiso 1 1 calc R . . C29 C 0.6667(3) 0.2528(3) 0.3129(3) 0.0362(10) Uani 1 1 d . . . H29A H 0.6762 0.2178 0.3641 0.043 Uiso 1 1 calc R . . C30 C 0.5802(3) 0.2640(3) 0.2681(2) 0.0289(8) Uani 1 1 d . . . H30A H 0.5308 0.2353 0.2878 0.035 Uiso 1 1 calc R . . P1 P 0.40409(6) 0.15115(6) 0.09681(6) 0.0229(2) Uani 1 1 d . . . O31 O 0.32301(16) 0.07963(17) 0.08084(17) 0.0277(6) Uani 1 1 d . . . C31 C 0.2503(2) 0.0885(3) 0.0080(3) 0.0336(9) Uani 1 1 d . . . H31A H 0.2259 0.0286 -0.0093 0.040 Uiso 1 1 calc R . . H31B H 0.2746 0.1144 -0.0415 0.040 Uiso 1 1 calc R . . C32 C 0.1748(3) 0.1467(3) 0.0286(3) 0.0368(10) Uani 1 1 d . . . H32A H 0.1272 0.1507 -0.0222 0.055 Uiso 1 1 calc R . . H32B H 0.1983 0.2065 0.0445 0.055 Uiso 1 1 calc R . . H32C H 0.1497 0.1207 0.0770 0.055 Uiso 1 1 calc R . . O33 O 0.47236(16) 0.10047(16) 0.16881(16) 0.0260(6) Uani 1 1 d . . . C33 C 0.5050(3) 0.0102(2) 0.1540(3) 0.0324(9) Uani 1 1 d . . . H33A H 0.5449 0.0118 0.1095 0.039 Uiso 1 1 calc R . . H33B H 0.4533 -0.0298 0.1337 0.039 Uiso 1 1 calc R . . C34 C 0.5563(3) -0.0227(3) 0.2377(3) 0.0339(9) Uani 1 1 d . . . H34A H 0.5792 -0.0829 0.2298 0.051 Uiso 1 1 calc R . . H34B H 0.5161 -0.0243 0.2811 0.051 Uiso 1 1 calc R . . H34C H 0.6073 0.0174 0.2572 0.051 Uiso 1 1 calc R . . O35 O 0.44339(17) 0.13648(16) 0.00814(16) 0.0277(6) Uani 1 1 d . . . C35 C 0.5100(3) 0.1959(3) -0.0199(3) 0.0301(9) Uani 1 1 d . . . H35A H 0.5005 0.2572 0.0003 0.036 Uiso 1 1 calc R . . H35B H 0.5011 0.1968 -0.0839 0.036 Uiso 1 1 calc R . . C36 C 0.6054(3) 0.1668(3) 0.0146(3) 0.0381(10) Uani 1 1 d . . . H36A H 0.6482 0.2085 -0.0050 0.057 Uiso 1 1 calc R . . H36B H 0.6155 0.1067 -0.0066 0.057 Uiso 1 1 calc R . . H36C H 0.6146 0.1663 0.0780 0.057 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 0.01849(17) 0.01678(18) 0.02231(19) -0.00075(11) 0.00366(13) 0.00081(10) Cl1 0.0280(5) 0.0240(4) 0.0248(5) 0.0031(4) 0.0070(4) 0.0008(4) Cl2 0.0277(5) 0.0304(5) 0.0234(5) 0.0016(4) 0.0020(4) 0.0019(4) C1 0.0231(17) 0.0212(18) 0.0160(17) 0.0026(14) 0.0011(14) -0.0008(14) N2 0.0220(15) 0.0167(15) 0.0380(19) -0.0054(13) 0.0043(14) 0.0011(12) C3 0.025(2) 0.027(2) 0.054(3) -0.0127(19) 0.0036(19) 0.0040(16) C4 0.0251(19) 0.024(2) 0.048(3) -0.0122(18) 0.0067(18) 0.0029(16) N5 0.0203(14) 0.0179(15) 0.0309(17) -0.0038(13) 0.0041(13) 0.0019(12) C6 0.0203(17) 0.0211(19) 0.035(2) -0.0055(16) 0.0033(16) 0.0031(15) C7 0.0241(18) 0.0238(19) 0.029(2) -0.0028(16) 0.0043(16) 0.0038(15) C8 0.0267(19) 0.024(2) 0.040(2) -0.0045(18) 0.0128(18) -0.0019(16) C9 0.0255(19) 0.032(2) 0.040(2) -0.0111(18) 0.0077(19) 0.0014(17) C10 0.0230(18) 0.034(2) 0.035(2) -0.0068(18) 0.0027(17) 0.0047(16) C11 0.0239(18) 0.0238(19) 0.032(2) -0.0019(16) 0.0061(16) 0.0071(15) C12 0.028(2) 0.035(2) 0.028(2) 0.0014(17) 0.0065(18) 0.0020(16) C13 0.028(2) 0.046(3) 0.060(3) -0.018(2) 0.010(2) -0.0066(19) C14 0.033(2) 0.032(2) 0.043(2) 0.0096(19) 0.0091(19) 0.0074(17) C15 0.0221(17) 0.0186(18) 0.031(2) -0.0024(15) 0.0064(16) -0.0012(14) C16 0.032(2) 0.0159(18) 0.033(2) -0.0015(15) 0.0089(17) -0.0013(15) C17 0.033(2) 0.027(2) 0.041(2) 0.0009(18) 0.0159(19) -0.0019(17) C18 0.0260(19) 0.023(2) 0.043(2) -0.0042(17) 0.0035(18) -0.0021(15) C19 0.030(2) 0.0205(19) 0.038(2) -0.0028(17) -0.0001(18) -0.0021(16) C20 0.0303(19) 0.0160(18) 0.031(2) -0.0015(15) 0.0057(17) -0.0015(15) C21 0.041(2) 0.031(2) 0.031(2) 0.0039(17) 0.0035(19) 0.0001(18) C22 0.025(2) 0.044(3) 0.068(3) -0.006(2) 0.007(2) -0.0098(19) C23 0.040(2) 0.025(2) 0.033(2) 0.0015(17) 0.0038(19) -0.0074(17) C24 0.0277(18) 0.0177(18) 0.026(2) -0.0020(15) 0.0042(16) 0.0015(15) C25 0.0218(18) 0.0253(19) 0.028(2) -0.0060(16) 0.0014(16) 0.0003(15) C26 0.0235(19) 0.031(2) 0.035(2) -0.0052(17) 0.0018(17) -0.0030(16) C27 0.0256(19) 0.034(2) 0.041(2) -0.0073(19) -0.0006(18) -0.0038(17) C28 0.026(2) 0.037(3) 0.042(3) -0.0062(19) -0.006(2) 0.0012(17) C29 0.034(2) 0.032(2) 0.039(2) -0.0008(19) -0.0048(19) 0.0029(18) C30 0.028(2) 0.030(2) 0.029(2) -0.0043(17) 0.0035(17) 0.0020(16) P1 0.0231(5) 0.0200(5) 0.0256(5) -0.0019(4) 0.0041(4) 0.0009(4) O31 0.0240(13) 0.0254(14) 0.0326(15) -0.0003(11) 0.0013(11) -0.0032(11) C31 0.0236(19) 0.037(2) 0.039(2) -0.0075(19) -0.0001(18) -0.0022(17) C32 0.032(2) 0.029(2) 0.049(3) 0.0050(19) 0.004(2) 0.0036(17) O33 0.0277(13) 0.0201(13) 0.0288(14) -0.0001(11) 0.0007(11) 0.0068(10) C33 0.036(2) 0.0203(19) 0.041(2) 0.0019(17) 0.0062(19) 0.0103(17) C34 0.0252(19) 0.032(2) 0.042(2) 0.0079(19) -0.0008(18) 0.0066(17) O35 0.0310(14) 0.0252(14) 0.0282(14) -0.0039(11) 0.0086(12) 0.0010(11) C35 0.035(2) 0.027(2) 0.031(2) -0.0034(17) 0.0138(18) -0.0012(16) C36 0.037(2) 0.039(2) 0.038(2) -0.0079(19) 0.008(2) -0.0006(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 C24 1.843(4) . ? Ru1 C1 2.125(3) . ? Ru1 P1 2.3213(10) . ? Ru1 Cl1 2.3820(10) . ? Ru1 Cl2 2.3985(11) . ? C1 N2 1.343(4) . ? C1 N5 1.346(4) . ? N2 C6 1.440(5) . ? N2 C3 1.475(5) . ? C3 C4 1.518(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N5 1.477(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N5 C15 1.435(4) . ? C6 C11 1.401(5) . ? C6 C7 1.406(5) . ? C7 C8 1.395(5) . ? C7 C12 1.505(5) . ? C8 C9 1.394(6) . ? C8 H8A 0.9500 . ? C9 C10 1.383(6) . ? C9 C13 1.510(6) . ? C10 C11 1.403(5) . ? C10 H10A 0.9500 . ? C11 C14 1.507(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 C16 1.400(5) . ? C15 C20 1.401(5) . ? C16 C17 1.402(5) . ? C16 C21 1.506(5) . ? C17 C18 1.394(6) . ? C17 H17A 0.9500 . ? C18 C19 1.379(5) . ? C18 C22 1.516(5) . ? C19 C20 1.387(5) . ? C19 H19A 0.9500 . ? C20 C23 1.510(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.462(5) . ? C24 H24A 0.9500 . ? C25 C30 1.399(5) . ? C25 C26 1.407(5) . ? C26 C27 1.385(5) . ? C26 H26A 0.9500 . ? C27 C28 1.386(6) . ? C27 H27A 0.9500 . ? C28 C29 1.386(6) . ? C28 H28A 0.9500 . ? C29 C30 1.380(5) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? P1 O33 1.586(3) . ? P1 O31 1.608(3) . ? P1 O35 1.611(3) . ? O31 C31 1.449(5) . ? C31 C32 1.503(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O33 C33 1.468(4) . ? C33 C34 1.491(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O35 C35 1.456(4) . ? C35 C36 1.507(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Ru1 C1 99.76(14) . . ? C24 Ru1 P1 91.20(11) . . ? C1 Ru1 P1 169.04(9) . . ? C24 Ru1 Cl1 103.18(12) . . ? C1 Ru1 Cl1 89.13(9) . . ? P1 Ru1 Cl1 88.28(3) . . ? C24 Ru1 Cl2 89.55(12) . . ? C1 Ru1 Cl2 88.86(9) . . ? P1 Ru1 Cl2 91.32(3) . . ? Cl1 Ru1 Cl2 167.27(3) . . ? N2 C1 N5 107.1(3) . . ? N2 C1 Ru1 126.9(3) . . ? N5 C1 Ru1 126.0(2) . . ? C1 N2 C6 129.8(3) . . ? C1 N2 C3 113.7(3) . . ? C6 N2 C3 116.5(3) . . ? N2 C3 C4 102.5(3) . . ? N2 C3 H3A 111.3 . . ? C4 C3 H3A 111.3 . . ? N2 C3 H3B 111.3 . . ? C4 C3 H3B 111.3 . . ? H3A C3 H3B 109.2 . . ? N5 C4 C3 102.3(3) . . ? N5 C4 H4A 111.3 . . ? C3 C4 H4A 111.3 . . ? N5 C4 H4B 111.3 . . ? C3 C4 H4B 111.3 . . ? H4A C4 H4B 109.2 . . ? C1 N5 C15 129.3(3) . . ? C1 N5 C4 113.6(3) . . ? C15 N5 C4 116.8(3) . . ? C11 C6 C7 121.1(3) . . ? C11 C6 N2 118.6(3) . . ? C7 C6 N2 119.6(3) . . ? C8 C7 C6 118.1(4) . . ? C8 C7 C12 120.4(3) . . ? C6 C7 C12 121.3(3) . . ? C7 C8 C9 122.4(4) . . ? C7 C8 H8A 118.8 . . ? C9 C8 H8A 118.8 . . ? C10 C9 C8 117.8(4) . . ? C10 C9 C13 121.9(4) . . ? C8 C9 C13 120.3(4) . . ? C9 C10 C11 122.4(4) . . ? C9 C10 H10A 118.8 . . ? C11 C10 H10A 118.8 . . ? C6 C11 C10 118.1(4) . . ? C6 C11 C14 122.4(3) . . ? C10 C11 C14 119.4(4) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 121.9(3) . . ? C16 C15 N5 119.0(3) . . ? C20 C15 N5 118.9(3) . . ? C15 C16 C17 117.8(4) . . ? C15 C16 C21 121.8(3) . . ? C17 C16 C21 120.4(3) . . ? C18 C17 C16 121.7(4) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C19 C18 C17 118.0(4) . . ? C19 C18 C22 121.7(4) . . ? C17 C18 C22 120.3(4) . . ? C18 C19 C20 123.3(4) . . ? C18 C19 H19A 118.4 . . ? C20 C19 H19A 118.4 . . ? C19 C20 C15 117.3(3) . . ? C19 C20 C23 120.8(4) . . ? C15 C20 C23 121.9(3) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 Ru1 137.3(3) . . ? C25 C24 H24A 111.3 . . ? Ru1 C24 H24A 111.3 . . ? C30 C25 C26 118.2(3) . . ? C30 C25 C24 124.7(3) . . ? C26 C25 C24 117.1(3) . . ? C27 C26 C25 121.1(4) . . ? C27 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C28 C27 C26 119.6(4) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C29 120.1(4) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 120.6(4) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 C25 120.5(4) . . ? C29 C30 H30A 119.8 . . ? C25 C30 H30A 119.8 . . ? O33 P1 O31 100.02(14) . . ? O33 P1 O35 105.36(13) . . ? O31 P1 O35 98.52(14) . . ? O33 P1 Ru1 115.01(10) . . ? O31 P1 Ru1 113.66(10) . . ? O35 P1 Ru1 121.14(10) . . ? C31 O31 P1 120.8(2) . . ? O31 C31 C32 112.2(3) . . ? O31 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? O31 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? 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 . . ? C33 O33 P1 121.4(2) . . ? O33 C33 C34 107.6(3) . . ? O33 C33 H33A 110.2 . . ? C34 C33 H33A 110.2 . . ? O33 C33 H33B 110.2 . . ? C34 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35 O35 P1 122.8(2) . . ? O35 C35 C36 111.8(3) . . ? O35 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? O35 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? 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 . . ? 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 C24 Ru1 C1 N2 166.5(3) . . . . ? P1 Ru1 C1 N2 -13.9(7) . . . . ? Cl1 Ru1 C1 N2 -90.3(3) . . . . ? Cl2 Ru1 C1 N2 77.1(3) . . . . ? C24 Ru1 C1 N5 -14.0(3) . . . . ? P1 Ru1 C1 N5 165.6(3) . . . . ? Cl1 Ru1 C1 N5 89.3(3) . . . . ? Cl2 Ru1 C1 N5 -103.3(3) . . . . ? N5 C1 N2 C6 179.2(3) . . . . ? Ru1 C1 N2 C6 -1.2(5) . . . . ? N5 C1 N2 C3 -2.0(4) . . . . ? Ru1 C1 N2 C3 177.7(3) . . . . ? C1 N2 C3 C4 7.1(4) . . . . ? C6 N2 C3 C4 -173.9(3) . . . . ? N2 C3 C4 N5 -8.7(4) . . . . ? N2 C1 N5 C15 -178.0(3) . . . . ? Ru1 C1 N5 C15 2.3(5) . . . . ? N2 C1 N5 C4 -4.5(4) . . . . ? Ru1 C1 N5 C4 175.8(3) . . . . ? C3 C4 N5 C1 8.7(4) . . . . ? C3 C4 N5 C15 -177.0(3) . . . . ? C1 N2 C6 C11 -98.3(4) . . . . ? C3 N2 C6 C11 82.9(4) . . . . ? C1 N2 C6 C7 91.0(5) . . . . ? C3 N2 C6 C7 -87.8(4) . . . . ? C11 C6 C7 C8 1.6(5) . . . . ? N2 C6 C7 C8 172.0(3) . . . . ? C11 C6 C7 C12 -174.2(3) . . . . ? N2 C6 C7 C12 -3.7(5) . . . . ? C6 C7 C8 C9 -1.6(5) . . . . ? C12 C7 C8 C9 174.2(3) . . . . ? C7 C8 C9 C10 1.8(6) . . . . ? C7 C8 C9 C13 -175.9(4) . . . . ? C8 C9 C10 C11 -2.0(6) . . . . ? C13 C9 C10 C11 175.7(4) . . . . ? C7 C6 C11 C10 -1.7(5) . . . . ? N2 C6 C11 C10 -172.3(3) . . . . ? C7 C6 C11 C14 174.7(3) . . . . ? N2 C6 C11 C14 4.1(5) . . . . ? C9 C10 C11 C6 2.0(5) . . . . ? C9 C10 C11 C14 -174.5(3) . . . . ? C1 N5 C15 C16 91.7(5) . . . . ? C4 N5 C15 C16 -81.6(4) . . . . ? C1 N5 C15 C20 -94.0(4) . . . . ? C4 N5 C15 C20 92.7(4) . . . . ? C20 C15 C16 C17 2.5(5) . . . . ? N5 C15 C16 C17 176.7(3) . . . . ? C20 C15 C16 C21 -179.1(3) . . . . ? N5 C15 C16 C21 -5.0(5) . . . . ? C15 C16 C17 C18 -1.0(6) . . . . ? C21 C16 C17 C18 -179.3(4) . . . . ? C16 C17 C18 C19 -0.5(6) . . . . ? C16 C17 C18 C22 177.7(4) . . . . ? C17 C18 C19 C20 0.5(6) . . . . ? C22 C18 C19 C20 -177.7(4) . . . . ? C18 C19 C20 C15 0.9(6) . . . . ? C18 C19 C20 C23 -179.9(4) . . . . ? C16 C15 C20 C19 -2.5(5) . . . . ? N5 C15 C20 C19 -176.7(3) . . . . ? C16 C15 C20 C23 178.4(3) . . . . ? N5 C15 C20 C23 4.2(5) . . . . ? C1 Ru1 C24 C25 116.8(4) . . . . ? P1 Ru1 C24 C25 -63.1(4) . . . . ? Cl1 Ru1 C24 C25 25.4(4) . . . . ? Cl2 Ru1 C24 C25 -154.4(4) . . . . ? Ru1 C24 C25 C30 -10.7(6) . . . . ? Ru1 C24 C25 C26 168.8(3) . . . . ? C30 C25 C26 C27 0.1(6) . . . . ? C24 C25 C26 C27 -179.5(3) . . . . ? C25 C26 C27 C28 -1.6(6) . . . . ? C26 C27 C28 C29 1.5(6) . . . . ? C27 C28 C29 C30 0.2(6) . . . . ? C28 C29 C30 C25 -1.8(6) . . . . ? C26 C25 C30 C29 1.6(6) . . . . ? C24 C25 C30 C29 -178.8(4) . . . . ? C24 Ru1 P1 O33 65.82(16) . . . . ? C1 Ru1 P1 O33 -113.8(5) . . . . ? Cl1 Ru1 P1 O33 -37.33(11) . . . . ? Cl2 Ru1 P1 O33 155.40(11) . . . . ? C24 Ru1 P1 O31 -179.72(16) . . . . ? C1 Ru1 P1 O31 0.7(5) . . . . ? Cl1 Ru1 P1 O31 77.13(11) . . . . ? Cl2 Ru1 P1 O31 -90.14(11) . . . . ? C24 Ru1 P1 O35 -62.75(17) . . . . ? C1 Ru1 P1 O35 117.7(5) . . . . ? Cl1 Ru1 P1 O35 -165.89(12) . . . . ? Cl2 Ru1 P1 O35 26.83(12) . . . . ? O33 P1 O31 C31 -168.5(3) . . . . ? O35 P1 O31 C31 -61.2(3) . . . . ? Ru1 P1 O31 C31 68.4(3) . . . . ? P1 O31 C31 C32 -87.3(4) . . . . ? O31 P1 O33 C33 56.4(3) . . . . ? O35 P1 O33 C33 -45.4(3) . . . . ? Ru1 P1 O33 C33 178.5(2) . . . . ? P1 O33 C33 C34 -171.8(2) . . . . ? O33 P1 O35 C35 -87.9(3) . . . . ? O31 P1 O35 C35 169.2(3) . . . . ? Ru1 P1 O35 C35 44.8(3) . . . . ? P1 O35 C35 C36 89.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.938 _refine_diff_density_min -0.867 _refine_diff_density_rms 0.101