# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name dstephan@chem.utoronto.ca _publ_contact_author_email dstephan@chem.utoronto.ca loop_ _publ_author_name C.Brown D.Stephan data_ccb019_0m _database_code_depnum_ccdc_archive 'CCDC 869893' #TrackingRef '- All-cifs-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H78 Cl12 N2 P4 Ru2' _chemical_formula_weight 1938.96 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.477(2) _cell_length_b 12.7495(10) _cell_length_c 28.088(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.210(5) _cell_angle_gamma 90.00 _cell_volume 8882.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 0.819 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6862 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85843 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.68 _reflns_number_total 9338 _reflns_number_gt 6341 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 1.000 -0.154 0.250 125.4 17.5 2 1.000 0.153 0.750 125.4 17.7 3 0.500 0.346 0.250 125.4 17.5 4 0.500 0.653 0.750 125.4 17.7 _platon_squeeze_details ; During the refinement of the structure, electron density peaks were located that were believed to be highly disordered solvent molecules (possibly dichloromethane). Attempts made to model the solvent molecule were not successful. The SQUEEZE option in PLATON (Spek, 2003) indicated there was a large solvent cavity. In the final cycles of refinement, this contribution to the electron density was removed from the observed data. The density, the F(000) value, the molecular weight and the formula are given without taking into account the results obtained with the SQUEEZE option PLATON (Spek, 2003). Similar treatments of disordered solvent molecules were carried out by St\"ahler et al. (2001), Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005). References: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13 Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005). Acta Cryst. E61, m2014-m2017. Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M. (2003). Acta Cryst. E59, o975-o977. Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M. (2003). Acta Cryst. C59, m84-m86. St\"ahler, R., N\"ather, C. & Bensch, W. (2001). Acta Cryst. C57, 26-27. ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9338 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1546 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.002 _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 -0.260089(14) 0.24945(3) 0.931042(11) 0.01622(11) Uani 1 1 d . . . Cl2 Cl -0.24399(4) 0.12578(8) 1.00085(3) 0.0203(2) Uani 1 1 d . . . P1 P -0.25042(5) 0.12144(9) 0.87863(4) 0.0194(3) Uani 1 1 d . . . P2 P -0.27246(5) 0.39007(9) 0.87791(4) 0.0191(2) Uani 1 1 d . . . Cl1 Cl -0.35560(4) 0.21695(9) 0.92613(4) 0.0244(3) Uani 1 1 d . . . N1 N -0.17908(14) 0.2588(3) 0.94809(13) 0.0203(8) Uani 1 1 d . . . H1A H -0.1671 0.2866 0.9772 0.024 Uiso 1 1 calc R . . C4 C -0.31491(18) 0.4974(4) 0.89207(15) 0.0243(10) Uani 1 1 d . . . C20 C -0.1959(2) 0.1195(4) 0.80169(16) 0.0294(11) Uani 1 1 d . . . H20A H -0.2264 0.0819 0.7840 0.035 Uiso 1 1 calc R . . C37 C -0.22851(19) -0.0049(3) 0.90760(15) 0.0239(10) Uani 1 1 d . . . C11 C -0.17812(18) 0.4937(4) 0.92171(16) 0.0262(10) Uani 1 1 d . . . H11A H -0.1868 0.4707 0.9512 0.031 Uiso 1 1 calc R . . C24 C -0.14812(18) 0.2036(4) 0.87594(16) 0.0238(10) Uani 1 1 d . . . C19 C -0.19474(18) 0.1505(3) 0.84958(15) 0.0212(9) Uani 1 1 d . . . C12 C -0.21111(18) 0.4653(3) 0.87696(16) 0.0238(10) Uani 1 1 d . . . C35 C -0.3974(2) 0.0867(4) 0.78154(16) 0.0347(12) Uani 1 1 d . . . H35A H -0.4294 0.1266 0.7714 0.042 Uiso 1 1 calc R . . C18 C -0.30441(19) 0.3717(3) 0.81248(15) 0.0235(10) Uani 1 1 d . . . C31 C -0.30628(19) 0.0711(4) 0.83017(15) 0.0238(10) Uani 1 1 d . . . C13 C -0.2758(2) 0.3257(4) 0.78080(16) 0.0294(11) Uani 1 1 d . . . H13A H -0.2388 0.3085 0.7925 0.035 Uiso 1 1 calc R . . C25 C -0.08327(18) 0.2405(4) 0.95828(16) 0.0248(10) Uani 1 1 d . . . C7 C -0.1981(2) 0.5049(4) 0.83432(17) 0.0306(11) Uani 1 1 d . . . H7A H -0.2206 0.4890 0.8033 0.037 Uiso 1 1 calc R . . C8 C -0.1532(2) 0.5661(4) 0.83707(18) 0.0356(12) Uani 1 1 d . . . H8A H -0.1451 0.5917 0.8078 0.043 Uiso 1 1 calc R . . C15 C -0.3550(2) 0.3308(4) 0.71524(18) 0.0439(14) Uani 1 1 d . . . H15A H -0.3723 0.3175 0.6821 0.053 Uiso 1 1 calc R . . C43 C -0.13998(18) 0.2350(3) 0.92793(16) 0.0210(9) Uani 1 1 d . . . C36 C -0.35325(18) 0.1288(4) 0.81511(15) 0.0238(10) Uani 1 1 d . . . H36A H -0.3555 0.1974 0.8277 0.029 Uiso 1 1 calc R . . C21 C -0.1545(2) 0.1413(4) 0.77893(17) 0.0352(12) Uani 1 1 d . . . H21A H -0.1565 0.1189 0.7463 0.042 Uiso 1 1 calc R . . C33 C -0.3471(2) -0.0699(4) 0.77760(17) 0.0388(13) Uani 1 1 d . . . H33A H -0.3446 -0.1380 0.7646 0.047 Uiso 1 1 calc R . . C38 C -0.2647(2) -0.0605(4) 0.92879(16) 0.0302(11) Uani 1 1 d . . . H38A H -0.2981 -0.0292 0.9304 0.036 Uiso 1 1 calc R . . C32 C -0.3038(2) -0.0289(4) 0.81055(16) 0.0306(11) Uani 1 1 d . . . H32A H -0.2718 -0.0691 0.8202 0.037 Uiso 1 1 calc R . . C9 C -0.1199(2) 0.5909(4) 0.88084(19) 0.0377(13) Uani 1 1 d . . . H9A H -0.0884 0.6318 0.8821 0.045 Uiso 1 1 calc R . . C23 C -0.1069(2) 0.2265(4) 0.85216(18) 0.0323(12) Uani 1 1 d . . . H23A H -0.0760 0.2638 0.8693 0.039 Uiso 1 1 calc R . . C26 C -0.0485(2) 0.1564(4) 0.95990(18) 0.0375(13) Uani 1 1 d . . . H26A H -0.0598 0.0963 0.9403 0.045 Uiso 1 1 calc R . . C22 C -0.1099(2) 0.1961(4) 0.80428(18) 0.0370(13) Uani 1 1 d . . . H22A H -0.0815 0.2129 0.7889 0.044 Uiso 1 1 calc R . . C29 C -0.0140(2) 0.3308(5) 1.01564(19) 0.0426(14) Uani 1 1 d . . . H29A H -0.0019 0.3918 1.0344 0.051 Uiso 1 1 calc R . . C17 C -0.3584(2) 0.3962(4) 0.79464(16) 0.0309(11) Uani 1 1 d . . . H17A H -0.3784 0.4274 0.8156 0.037 Uiso 1 1 calc R . . C3 C -0.3131(2) 0.5959(4) 0.87001(19) 0.0360(12) Uani 1 1 d . . . H3A H -0.2871 0.6084 0.8512 0.043 Uiso 1 1 calc R . . C42 C -0.1800(2) -0.0525(4) 0.90601(18) 0.0384(13) Uani 1 1 d . . . H42A H -0.1544 -0.0161 0.8924 0.046 Uiso 1 1 calc R . . C1 C -0.3849(3) 0.6592(5) 0.9036(3) 0.0600(18) Uani 1 1 d . . . H1B H -0.4091 0.7137 0.9074 0.072 Uiso 1 1 calc R . . C10 C -0.1327(2) 0.5554(4) 0.92385(19) 0.0369(12) Uani 1 1 d . . . H10A H -0.1103 0.5734 0.9547 0.044 Uiso 1 1 calc R . . C14 C -0.3009(2) 0.3052(4) 0.73255(17) 0.0363(13) Uani 1 1 d . . . H14A H -0.2812 0.2738 0.7113 0.044 Uiso 1 1 calc R . . C34 C -0.3943(2) -0.0131(4) 0.76305(17) 0.0398(13) Uani 1 1 d . . . H34A H -0.4244 -0.0424 0.7406 0.048 Uiso 1 1 calc R . . C30 C -0.06610(19) 0.3268(4) 0.98700(18) 0.0337(12) Uani 1 1 d . . . H30A H -0.0900 0.3838 0.9872 0.040 Uiso 1 1 calc R . . C27 C 0.0022(2) 0.1593(5) 0.9896(2) 0.0453(15) Uani 1 1 d . . . H27A H 0.0253 0.1003 0.9915 0.054 Uiso 1 1 calc R . . C16 C -0.3834(2) 0.3752(4) 0.74611(19) 0.0411(13) Uani 1 1 d . . . H16A H -0.4205 0.3917 0.7343 0.049 Uiso 1 1 calc R . . C39 C -0.2528(3) -0.1594(4) 0.94718(18) 0.0435(14) Uani 1 1 d . . . H39A H -0.2775 -0.1959 0.9618 0.052 Uiso 1 1 calc R . . C2 C -0.3485(3) 0.6748(4) 0.8753(2) 0.0534(16) Uani 1 1 d . . . H2A H -0.3475 0.7401 0.8593 0.064 Uiso 1 1 calc R . . C28 C 0.0199(2) 0.2483(5) 1.0170(2) 0.0465(15) Uani 1 1 d . . . H28A H 0.0555 0.2515 1.0366 0.056 Uiso 1 1 calc R . . C5 C -0.35197(19) 0.4824(4) 0.92050(18) 0.0343(12) Uani 1 1 d . . . H5A H -0.3540 0.4167 0.9359 0.041 Uiso 1 1 calc R . . C6 C -0.3865(2) 0.5645(5) 0.9266(2) 0.0544(16) Uani 1 1 d . . . H6A H -0.4113 0.5545 0.9468 0.065 Uiso 1 1 calc R . . C41 C -0.1687(3) -0.1530(5) 0.9243(2) 0.0598(18) Uani 1 1 d . . . H41A H -0.1355 -0.1854 0.9228 0.072 Uiso 1 1 calc R . . C40 C -0.2048(3) -0.2057(5) 0.9443(2) 0.0614(19) Uani 1 1 d . . . H40A H -0.1968 -0.2749 0.9564 0.074 Uiso 1 1 calc R . . Cl11 Cl 0.08719(10) 0.42567(14) 0.94350(6) 0.0804(6) Uani 1 1 d . . . Cl13 Cl 0.00658(10) 0.4514(3) 0.85524(12) 0.1524(13) Uani 1 1 d . . . C100 C 0.0711(2) 0.4795(5) 0.8843(2) 0.0542(16) Uani 1 1 d . . . H10B H 0.0760 0.5565 0.8863 0.065 Uiso 1 1 calc R . . H10C H 0.0960 0.4509 0.8651 0.065 Uiso 1 1 calc R . . Cl4 Cl 0.00093(8) -0.26096(16) 0.83967(9) 0.0856(7) Uani 1 1 d . . . Cl6 Cl -0.02450(8) -0.06045(16) 0.87621(7) 0.0786(6) Uani 1 1 d . . . C90 C 0.0246(3) -0.1566(5) 0.8780(2) 0.0573(17) Uani 1 1 d . . . H90A H 0.0561 -0.1252 0.8683 0.069 Uiso 1 1 calc R . . H90B H 0.0368 -0.1827 0.9120 0.069 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 0.01882(19) 0.01737(18) 0.01332(17) -0.00129(14) 0.00544(12) -0.00054(14) Cl2 0.0280(6) 0.0189(5) 0.0153(5) -0.0008(4) 0.0073(4) -0.0008(4) P1 0.0245(6) 0.0189(6) 0.0156(5) -0.0025(4) 0.0064(4) -0.0006(5) P2 0.0229(6) 0.0190(6) 0.0154(5) -0.0005(4) 0.0041(4) -0.0008(5) Cl1 0.0202(6) 0.0325(6) 0.0220(5) -0.0035(4) 0.0075(4) -0.0025(5) N1 0.023(2) 0.020(2) 0.0182(17) -0.0028(15) 0.0067(15) -0.0029(16) C4 0.025(2) 0.024(2) 0.022(2) -0.0049(19) 0.0009(19) 0.0055(19) C20 0.040(3) 0.026(3) 0.025(2) -0.006(2) 0.012(2) 0.005(2) C37 0.037(3) 0.019(2) 0.017(2) -0.0027(18) 0.0076(19) 0.004(2) C11 0.033(3) 0.024(2) 0.022(2) 0.0039(19) 0.007(2) -0.001(2) C24 0.028(3) 0.021(2) 0.026(2) 0.0015(19) 0.014(2) 0.005(2) C19 0.027(2) 0.017(2) 0.023(2) 0.0023(18) 0.0108(19) 0.0039(19) C12 0.027(3) 0.020(2) 0.027(2) 0.0001(18) 0.0104(19) 0.0020(19) C35 0.032(3) 0.047(3) 0.022(2) 0.002(2) 0.002(2) -0.002(2) C18 0.033(3) 0.016(2) 0.020(2) 0.0030(18) 0.0045(19) -0.0032(19) C31 0.030(3) 0.025(2) 0.019(2) -0.0028(18) 0.0107(19) -0.005(2) C13 0.043(3) 0.022(2) 0.025(2) -0.0019(19) 0.011(2) -0.004(2) C25 0.022(2) 0.028(3) 0.028(2) 0.000(2) 0.0130(19) -0.001(2) C7 0.042(3) 0.028(3) 0.025(2) 0.002(2) 0.013(2) -0.011(2) C8 0.054(3) 0.028(3) 0.031(3) 0.005(2) 0.023(2) -0.009(2) C15 0.062(4) 0.036(3) 0.026(3) 0.001(2) -0.008(3) -0.010(3) C43 0.025(2) 0.013(2) 0.026(2) 0.0017(17) 0.0099(19) 0.0025(18) C36 0.030(3) 0.024(2) 0.019(2) 0.0004(18) 0.0085(19) -0.003(2) C21 0.051(3) 0.036(3) 0.026(3) 0.005(2) 0.025(2) 0.009(3) C33 0.060(4) 0.035(3) 0.022(2) -0.010(2) 0.011(2) -0.010(3) C38 0.045(3) 0.023(3) 0.023(2) 0.000(2) 0.009(2) -0.003(2) C32 0.040(3) 0.032(3) 0.019(2) -0.008(2) 0.005(2) -0.004(2) C9 0.037(3) 0.031(3) 0.050(3) 0.000(2) 0.020(3) -0.010(2) C23 0.036(3) 0.034(3) 0.031(3) 0.003(2) 0.016(2) 0.000(2) C26 0.035(3) 0.044(3) 0.036(3) -0.009(2) 0.011(2) 0.007(2) C22 0.038(3) 0.047(3) 0.034(3) 0.003(2) 0.024(2) 0.001(3) C29 0.031(3) 0.048(4) 0.042(3) -0.003(3) -0.004(2) -0.007(3) C17 0.037(3) 0.029(3) 0.023(2) 0.001(2) -0.001(2) 0.000(2) C3 0.041(3) 0.020(3) 0.046(3) 0.003(2) 0.009(2) 0.002(2) C42 0.044(3) 0.039(3) 0.031(3) 0.005(2) 0.007(2) 0.011(3) C1 0.059(4) 0.033(4) 0.088(5) -0.016(3) 0.017(4) 0.017(3) C10 0.041(3) 0.026(3) 0.040(3) 0.002(2) 0.003(2) -0.008(2) C14 0.057(4) 0.033(3) 0.021(2) -0.006(2) 0.014(2) -0.013(3) C34 0.046(3) 0.051(4) 0.023(3) -0.008(2) 0.007(2) -0.018(3) C30 0.025(3) 0.032(3) 0.043(3) -0.003(2) 0.004(2) -0.002(2) C27 0.024(3) 0.059(4) 0.054(4) 0.004(3) 0.009(3) 0.018(3) C16 0.042(3) 0.039(3) 0.037(3) -0.002(2) -0.003(2) 0.000(3) C39 0.077(4) 0.024(3) 0.033(3) 0.005(2) 0.019(3) -0.002(3) C2 0.057(4) 0.024(3) 0.077(4) 0.000(3) 0.008(3) 0.007(3) C28 0.019(3) 0.067(4) 0.052(3) 0.004(3) 0.003(2) -0.001(3) C5 0.032(3) 0.035(3) 0.038(3) -0.003(2) 0.012(2) 0.004(2) C6 0.047(4) 0.055(4) 0.065(4) -0.006(3) 0.020(3) 0.013(3) C41 0.071(5) 0.050(4) 0.061(4) 0.021(3) 0.023(4) 0.038(3) C40 0.104(6) 0.034(3) 0.051(4) 0.020(3) 0.027(4) 0.028(4) Cl11 0.151(2) 0.0480(10) 0.0522(10) 0.0026(8) 0.0430(11) 0.0034(11) Cl13 0.0795(17) 0.173(3) 0.174(3) 0.043(2) -0.0327(17) -0.0566(18) C100 0.052(4) 0.067(4) 0.045(3) 0.004(3) 0.013(3) -0.014(3) Cl4 0.0666(13) 0.0783(14) 0.1009(16) -0.0215(11) -0.0035(11) 0.0211(10) Cl6 0.0672(12) 0.0855(14) 0.0736(12) -0.0235(10) -0.0039(9) 0.0277(10) C90 0.048(4) 0.068(5) 0.056(4) 0.008(3) 0.013(3) 0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.013(4) . ? Ru1 P1 2.2489(11) . ? Ru1 P2 2.3078(12) . ? Ru1 Cl1 2.4409(11) . ? Ru1 Cl2 2.4720(10) 7_457 ? Ru1 Cl2 2.4761(10) . ? Cl2 Ru1 2.4719(10) 7_457 ? P1 C19 1.829(4) . ? P1 C37 1.833(5) . ? P1 C31 1.845(5) . ? P2 C12 1.839(5) . ? P2 C4 1.843(4) . ? P2 C18 1.847(4) . ? N1 C43 1.290(5) . ? C4 C5 1.382(6) . ? C4 C3 1.406(6) . ? C20 C21 1.382(6) . ? C20 C19 1.396(6) . ? C37 C42 1.388(7) . ? C37 C38 1.400(6) . ? C11 C10 1.388(6) . ? C11 C12 1.391(6) . ? C24 C23 1.399(6) . ? C24 C19 1.420(6) . ? C24 C43 1.482(6) . ? C12 C7 1.408(6) . ? C35 C34 1.383(7) . ? C35 C36 1.399(6) . ? C18 C17 1.388(7) . ? C18 C13 1.401(6) . ? C31 C36 1.386(6) . ? C31 C32 1.395(6) . ? C13 C14 1.385(6) . ? C25 C30 1.375(6) . ? C25 C26 1.386(7) . ? C25 C43 1.502(6) . ? C7 C8 1.372(7) . ? C8 C9 1.362(7) . ? C15 C16 1.372(7) . ? C15 C14 1.393(8) . ? C21 C22 1.383(8) . ? C33 C32 1.371(7) . ? C33 C34 1.383(8) . ? C38 C39 1.370(7) . ? C9 C10 1.398(7) . ? C23 C22 1.384(7) . ? C26 C27 1.368(7) . ? C29 C28 1.354(8) . ? C29 C30 1.387(7) . ? C17 C16 1.392(6) . ? C3 C2 1.382(7) . ? C42 C41 1.386(7) . ? C1 C2 1.368(9) . ? C1 C6 1.374(9) . ? C27 C28 1.387(8) . ? C39 C40 1.377(8) . ? C5 C6 1.403(7) . ? C41 C40 1.360(9) . ? Cl11 C100 1.760(6) . ? Cl13 C100 1.698(6) . ? Cl4 C90 1.731(7) . ? Cl6 C90 1.745(6) . ? 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 P1 86.49(10) . . ? N1 Ru1 P2 95.11(10) . . ? P1 Ru1 P2 99.19(4) . . ? N1 Ru1 Cl1 168.01(10) . . ? P1 Ru1 Cl1 95.55(4) . . ? P2 Ru1 Cl1 96.22(4) . . ? N1 Ru1 Cl2 85.32(10) . 7_457 ? P1 Ru1 Cl2 169.16(4) . 7_457 ? P2 Ru1 Cl2 88.62(4) . 7_457 ? Cl1 Ru1 Cl2 91.03(4) . 7_457 ? N1 Ru1 Cl2 82.75(10) . . ? P1 Ru1 Cl2 91.90(4) . . ? P2 Ru1 Cl2 168.58(4) . . ? Cl1 Ru1 Cl2 85.37(4) . . ? Cl2 Ru1 Cl2 80.03(4) 7_457 . ? Ru1 Cl2 Ru1 99.96(4) 7_457 . ? C19 P1 C37 100.8(2) . . ? C19 P1 C31 106.72(19) . . ? C37 P1 C31 97.3(2) . . ? C19 P1 Ru1 110.92(14) . . ? C37 P1 Ru1 114.50(14) . . ? C31 P1 Ru1 123.64(15) . . ? C12 P2 C4 99.1(2) . . ? C12 P2 C18 103.6(2) . . ? C4 P2 C18 99.3(2) . . ? C12 P2 Ru1 115.06(15) . . ? C4 P2 Ru1 115.93(15) . . ? C18 P2 Ru1 120.58(14) . . ? C43 N1 Ru1 137.3(3) . . ? C5 C4 C3 118.3(4) . . ? C5 C4 P2 122.3(4) . . ? C3 C4 P2 119.2(4) . . ? C21 C20 C19 122.6(5) . . ? C42 C37 C38 118.1(4) . . ? C42 C37 P1 123.6(4) . . ? C38 C37 P1 118.1(4) . . ? C10 C11 C12 120.8(4) . . ? C23 C24 C19 118.8(4) . . ? C23 C24 C43 117.6(4) . . ? C19 C24 C43 123.7(4) . . ? C20 C19 C24 117.9(4) . . ? C20 C19 P1 121.7(4) . . ? C24 C19 P1 120.4(3) . . ? C11 C12 C7 117.6(4) . . ? C11 C12 P2 117.6(3) . . ? C7 C12 P2 124.5(4) . . ? C34 C35 C36 120.1(5) . . ? C17 C18 C13 118.8(4) . . ? C17 C18 P2 120.4(3) . . ? C13 C18 P2 120.7(4) . . ? C36 C31 C32 118.5(4) . . ? C36 C31 P1 120.5(3) . . ? C32 C31 P1 120.8(4) . . ? C14 C13 C18 120.7(5) . . ? C30 C25 C26 119.0(5) . . ? C30 C25 C43 120.4(4) . . ? C26 C25 C43 120.5(4) . . ? C8 C7 C12 120.8(4) . . ? C9 C8 C7 121.5(4) . . ? C16 C15 C14 119.9(5) . . ? N1 C43 C24 123.2(4) . . ? N1 C43 C25 118.6(4) . . ? C24 C43 C25 118.1(4) . . ? C31 C36 C35 120.4(4) . . ? C20 C21 C22 119.2(4) . . ? C32 C33 C34 120.7(5) . . ? C39 C38 C37 121.1(5) . . ? C33 C32 C31 120.9(5) . . ? C8 C9 C10 118.9(5) . . ? C22 C23 C24 121.6(5) . . ? C27 C26 C25 120.4(5) . . ? C21 C22 C23 119.9(5) . . ? C28 C29 C30 120.4(5) . . ? C18 C17 C16 120.3(5) . . ? C2 C3 C4 121.0(5) . . ? C41 C42 C37 120.2(5) . . ? C2 C1 C6 119.8(5) . . ? C11 C10 C9 120.3(5) . . ? C13 C14 C15 119.7(5) . . ? C33 C34 C35 119.3(5) . . ? C25 C30 C29 120.2(5) . . ? C26 C27 C28 120.2(5) . . ? C15 C16 C17 120.6(5) . . ? C38 C39 C40 119.7(5) . . ? C1 C2 C3 120.2(6) . . ? C29 C28 C27 119.7(5) . . ? C4 C5 C6 119.9(5) . . ? C1 C6 C5 120.8(6) . . ? C40 C41 C42 120.5(6) . . ? C41 C40 C39 120.4(5) . . ? Cl13 C100 Cl11 111.2(3) . . ? Cl4 C90 Cl6 112.1(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.900 _refine_diff_density_min -1.291 _refine_diff_density_rms 0.100 #===end data_ccb101_0m _database_code_depnum_ccdc_archive 'CCDC 869894' #TrackingRef '- All-cifs-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H62 Cl4 N2 P4 Ru2' _chemical_formula_weight 1351.00 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0277(4) _cell_length_b 12.3376(5) _cell_length_c 14.2100(5) _cell_angle_alpha 98.147(2) _cell_angle_beta 110.240(2) _cell_angle_gamma 110.453(2) _cell_volume 1474.92(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9996 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 32.96 _exptl_crystal_description block _exptl_crystal_colour red _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 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8491 _exptl_absorpt_correction_T_max 0.9202 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42278 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 33.16 _reflns_number_total 11200 _reflns_number_gt 9527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0319P)^2^+0.5042P] 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 11200 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 0.399674(12) 0.397658(9) 0.360829(8) 0.01326(3) Uani 1 1 d . . . Cl2 Cl 0.54765(4) 0.39670(3) 0.53967(2) 0.01607(6) Uani 1 1 d . . . Cl1 Cl 0.65344(4) 0.47173(3) 0.35110(3) 0.01798(6) Uani 1 1 d . . . P1 P 0.33638(4) 0.20292(3) 0.29614(3) 0.01668(7) Uani 1 1 d . . . P2 P 0.26932(4) 0.42863(3) 0.20762(3) 0.01650(7) Uani 1 1 d . . . N1 N 0.21758(14) 0.34330(11) 0.40131(9) 0.0165(2) Uani 1 1 d . . . C1 C -0.0583(3) 0.1567(2) 0.57878(19) 0.0489(6) Uani 1 1 d . . . C2 C 0.2687(3) 0.76293(19) 0.19315(16) 0.0380(4) Uani 1 1 d . . . C3 C 0.0131(3) 0.15926(18) 0.51056(16) 0.0369(4) Uani 1 1 d . . . C4 C 0.4270(3) 0.83847(18) 0.24013(17) 0.0377(4) Uani 1 1 d . . . C5 C 0.4003(2) 0.15106(15) 0.20031(14) 0.0248(3) Uani 1 1 d . . . C6 C 0.3206(2) 0.35414(15) -0.10438(12) 0.0265(3) Uani 1 1 d . . . C7 C -0.1975(2) -0.04125(16) 0.16025(15) 0.0317(4) Uani 1 1 d . . . C8 C -0.0421(2) 0.25183(16) 0.08264(13) 0.0275(3) Uani 1 1 d . . . C9 C 0.4844(2) 0.66877(15) 0.26779(12) 0.0241(3) Uani 1 1 d . . . C10 C -0.1093(2) -0.06465(15) 0.11127(14) 0.0307(4) Uani 1 1 d . . . C11 C 0.1962(2) 0.37752(16) -0.10128(12) 0.0276(3) Uani 1 1 d . . . C12 C 0.01280(17) 0.23863(13) 0.44985(11) 0.0206(3) Uani 1 1 d . . . C13 C -0.12627(19) 0.05854(15) 0.24881(13) 0.0267(3) Uani 1 1 d . . . C14 C 0.12454(18) 0.11157(13) 0.23956(11) 0.0198(3) Uani 1 1 d . . . C15 C -0.2657(2) 0.2473(2) 0.11139(16) 0.0382(4) Uani 1 1 d . . . C16 C 0.03387(17) 0.13678(13) 0.28931(11) 0.0200(3) Uani 1 1 d . . . C17 C 0.28718(17) 0.39078(13) 0.08367(11) 0.0189(3) Uani 1 1 d . . . C18 C 0.4294(2) 0.35157(14) -0.01394(12) 0.0238(3) Uani 1 1 d . . . C19 C -0.0601(2) 0.31482(16) 0.45807(13) 0.0273(3) Uani 1 1 d . . . C20 C -0.1336(3) 0.2311(2) 0.58456(17) 0.0445(5) Uani 1 1 d . . . C21 C 0.4007(2) 0.12771(15) 0.39323(14) 0.0265(3) Uani 1 1 d . . . C22 C -0.0095(2) 0.40876(17) 0.22127(13) 0.0279(3) Uani 1 1 d . . . C23 C 0.09623(17) 0.24428(13) 0.38033(11) 0.0179(2) Uani 1 1 d . . . C24 C 0.41386(18) 0.37011(13) 0.08047(11) 0.0202(3) Uani 1 1 d . . . C25 C -0.1347(2) 0.30933(19) 0.52475(15) 0.0351(4) Uani 1 1 d . . . C26 C -0.2022(2) 0.1958(2) 0.05607(15) 0.0356(4) Uani 1 1 d . . . C27 C -0.1705(2) 0.3532(2) 0.19374(16) 0.0360(4) Uani 1 1 d . . . C28 C 0.5356(2) 0.79184(16) 0.27703(15) 0.0321(4) Uani 1 1 d . . . C29 C 0.05633(18) 0.36010(15) 0.16444(11) 0.0214(3) Uani 1 1 d . . . C30 C 0.1806(2) 0.39667(15) -0.00795(12) 0.0244(3) Uani 1 1 d . . . C31 C 0.2163(2) 0.63914(17) 0.18263(13) 0.0292(3) Uani 1 1 d . . . C32 C 0.32406(19) 0.59126(14) 0.22068(11) 0.0214(3) Uani 1 1 d . . . C33 C 0.0501(2) 0.01025(14) 0.15073(13) 0.0260(3) Uani 1 1 d . . . H1 H 0.243(2) 0.3997(18) 0.4594(16) 0.026(5) Uiso 1 1 d . . . H2 H 0.495(2) 0.3739(17) 0.1465(15) 0.020(4) Uiso 1 1 d . . . H3 H -0.152(2) -0.1346(19) 0.0535(16) 0.031(5) Uiso 1 1 d . . . H4 H 0.111(3) -0.0047(19) 0.1203(17) 0.032(5) Uiso 1 1 d . . . H5 H 0.054(2) 0.4790(18) 0.2787(15) 0.021(5) Uiso 1 1 d . . . H6 H 0.102(2) 0.5865(17) 0.1485(15) 0.023(5) Uiso 1 1 d . . . H32 H 0.092(2) 0.4114(18) -0.0051(16) 0.028(5) Uiso 1 1 d . . . H8 H -0.304(3) -0.094(2) 0.1335(19) 0.045(7) Uiso 1 1 d . . . H9 H 0.374(2) 0.0634(19) 0.1910(16) 0.029(5) Uiso 1 1 d . . . H10 H 0.505(3) 0.1939(19) 0.2318(16) 0.028(5) Uiso 1 1 d . . . H11 H 0.356(2) 0.0403(19) 0.3608(16) 0.030(5) Uiso 1 1 d . . . H12 H 0.124(2) 0.3822(18) -0.1631(16) 0.027(5) Uiso 1 1 d . . . H13 H 0.350(3) 0.163(2) 0.1392(18) 0.037(6) Uiso 1 1 d . . . H14 H 0.368(3) 0.143(2) 0.4467(19) 0.045(7) Uiso 1 1 d . . . H15 H -0.185(2) 0.0739(19) 0.2823(16) 0.031(5) Uiso 1 1 d . . . H16 H 0.648(3) 0.844(2) 0.3102(17) 0.035(6) Uiso 1 1 d . . . H17 H -0.209(3) 0.388(2) 0.2326(19) 0.047(7) Uiso 1 1 d . . . H18 H 0.330(2) 0.3421(19) -0.1722(16) 0.030(5) Uiso 1 1 d . . . H19 H 0.559(2) 0.6327(18) 0.2931(16) 0.029(5) Uiso 1 1 d . . . H20 H 0.502(3) 0.158(2) 0.4243(19) 0.043(6) Uiso 1 1 d . . . H21 H 0.001(3) 0.2167(19) 0.0434(17) 0.034(6) Uiso 1 1 d . . . H22 H -0.060(3) 0.370(2) 0.4192(19) 0.041(6) Uiso 1 1 d . . . H23 H 0.463(3) 0.915(2) 0.2435(19) 0.048(7) Uiso 1 1 d . . . H24 H 0.521(3) 0.3404(19) -0.0127(17) 0.034(6) Uiso 1 1 d . . . H25 H -0.182(3) 0.358(2) 0.5268(18) 0.037(6) Uiso 1 1 d . . . H26 H 0.065(3) 0.102(2) 0.506(2) 0.053(7) Uiso 1 1 d . . . H27 H -0.383(3) 0.208(2) 0.0916(19) 0.050(7) Uiso 1 1 d . . . H28 H 0.189(3) 0.791(2) 0.166(2) 0.063(8) Uiso 1 1 d . . . H29 H -0.058(3) 0.105(2) 0.618(2) 0.061(8) Uiso 1 1 d . . . H31 H -0.276(3) 0.119(2) -0.001(2) 0.056(7) Uiso 1 1 d . . . H30 H -0.182(3) 0.224(2) 0.624(2) 0.056(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01443(5) 0.01362(5) 0.01213(5) 0.00215(3) 0.00606(4) 0.00670(4) Cl2 0.01949(15) 0.01589(13) 0.01329(12) 0.00291(10) 0.00642(11) 0.00921(11) Cl1 0.01658(14) 0.02070(14) 0.01696(14) 0.00296(11) 0.00878(11) 0.00773(12) P1 0.01870(16) 0.01453(14) 0.01743(15) 0.00213(12) 0.00883(13) 0.00769(13) P2 0.01840(16) 0.01985(16) 0.01343(14) 0.00414(12) 0.00731(13) 0.01036(13) N1 0.0177(5) 0.0173(5) 0.0150(5) 0.0022(4) 0.0073(4) 0.0085(4) C1 0.0669(16) 0.0508(13) 0.0511(13) 0.0286(11) 0.0445(12) 0.0251(12) C2 0.0563(13) 0.0387(10) 0.0393(10) 0.0215(8) 0.0241(9) 0.0349(10) C3 0.0512(12) 0.0359(9) 0.0441(10) 0.0218(8) 0.0344(10) 0.0233(9) C4 0.0597(13) 0.0267(8) 0.0447(11) 0.0201(8) 0.0311(10) 0.0256(9) C5 0.0289(8) 0.0219(7) 0.0278(8) 0.0032(6) 0.0171(7) 0.0119(6) C6 0.0347(9) 0.0259(7) 0.0209(7) 0.0050(6) 0.0171(6) 0.0105(7) C7 0.0237(8) 0.0233(7) 0.0342(9) -0.0027(6) 0.0118(7) 0.0001(6) C8 0.0223(7) 0.0350(8) 0.0224(7) 0.0063(6) 0.0096(6) 0.0101(7) C9 0.0321(8) 0.0248(7) 0.0246(7) 0.0116(6) 0.0173(6) 0.0154(6) C10 0.0297(8) 0.0214(7) 0.0281(8) -0.0042(6) 0.0105(7) 0.0032(6) C11 0.0330(9) 0.0345(8) 0.0172(6) 0.0080(6) 0.0110(6) 0.0161(7) C12 0.0194(6) 0.0205(6) 0.0207(6) 0.0032(5) 0.0112(5) 0.0056(5) C13 0.0219(7) 0.0224(7) 0.0292(8) 0.0007(6) 0.0123(6) 0.0036(6) C14 0.0216(7) 0.0161(6) 0.0202(6) 0.0019(5) 0.0103(5) 0.0065(5) C15 0.0228(8) 0.0619(13) 0.0360(9) 0.0241(9) 0.0147(7) 0.0190(9) C16 0.0201(7) 0.0170(6) 0.0201(6) 0.0022(5) 0.0096(5) 0.0053(5) C17 0.0221(7) 0.0202(6) 0.0154(6) 0.0042(5) 0.0090(5) 0.0096(5) C18 0.0256(7) 0.0233(7) 0.0249(7) 0.0045(6) 0.0157(6) 0.0093(6) C19 0.0274(8) 0.0325(8) 0.0264(7) 0.0064(6) 0.0145(6) 0.0157(7) C20 0.0442(12) 0.0542(12) 0.0401(11) 0.0082(9) 0.0338(10) 0.0132(10) C21 0.0320(9) 0.0197(7) 0.0264(7) 0.0067(6) 0.0099(7) 0.0123(6) C22 0.0290(8) 0.0421(9) 0.0233(7) 0.0114(7) 0.0148(6) 0.0226(8) C23 0.0185(6) 0.0180(6) 0.0179(6) 0.0039(5) 0.0087(5) 0.0084(5) C24 0.0206(7) 0.0205(6) 0.0189(6) 0.0033(5) 0.0097(5) 0.0077(5) C25 0.0300(9) 0.0442(10) 0.0325(9) 0.0010(8) 0.0184(7) 0.0165(8) C26 0.0235(8) 0.0447(10) 0.0282(8) 0.0096(8) 0.0083(7) 0.0066(8) C27 0.0334(9) 0.0600(12) 0.0356(9) 0.0230(9) 0.0227(8) 0.0316(9) C28 0.0416(10) 0.0254(8) 0.0361(9) 0.0131(7) 0.0230(8) 0.0138(7) C29 0.0206(7) 0.0309(7) 0.0177(6) 0.0092(5) 0.0092(5) 0.0146(6) C30 0.0269(8) 0.0331(8) 0.0182(6) 0.0081(6) 0.0103(6) 0.0174(7) C31 0.0377(9) 0.0347(9) 0.0242(7) 0.0124(7) 0.0129(7) 0.0243(8) C32 0.0316(8) 0.0241(7) 0.0171(6) 0.0085(5) 0.0136(6) 0.0169(6) C33 0.0273(8) 0.0212(7) 0.0238(7) -0.0019(5) 0.0117(6) 0.0068(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 N1 2.0236(12) . ? Ru1 P1 2.2192(4) . ? Ru1 P2 2.2825(4) . ? Ru1 Cl1 2.4462(4) . ? Ru1 Cl2 2.4642(3) . ? Ru1 Cl2 2.4991(3) 2_666 ? Cl2 Ru1 2.4990(3) 2_666 ? P1 C14 1.8214(15) . ? P1 C5 1.8215(15) . ? P1 C21 1.8291(17) . ? P2 C29 1.8268(16) . ? P2 C17 1.8429(14) . ? P2 C32 1.8482(15) . ? N1 C23 1.2919(18) . ? N1 H1 0.89(2) . ? C1 C20 1.388(3) . ? C1 C3 1.389(3) . ? C1 H29 0.90(3) . ? C2 C4 1.375(3) . ? C2 C31 1.397(3) . ? C2 H28 0.96(3) . ? C3 C12 1.394(2) . ? C3 H26 1.02(3) . ? C4 C28 1.386(3) . ? C4 H23 0.87(2) . ? C5 H9 1.00(2) . ? C5 H10 0.90(2) . ? C5 H13 0.90(2) . ? C6 C18 1.382(2) . ? C6 C11 1.388(2) . ? C6 H18 1.00(2) . ? C7 C10 1.378(3) . ? C7 C13 1.391(2) . ? C7 H8 0.93(2) . ? C8 C26 1.389(2) . ? C8 C29 1.398(2) . ? C8 H21 0.96(2) . ? C9 C28 1.392(2) . ? C9 C32 1.395(2) . ? C9 H19 0.99(2) . ? C10 C33 1.387(2) . ? C10 H3 0.95(2) . ? C11 C30 1.386(2) . ? C11 H12 0.95(2) . ? C12 C19 1.393(2) . ? C12 C23 1.494(2) . ? C13 C16 1.401(2) . ? C13 H15 0.93(2) . ? C14 C33 1.401(2) . ? C14 C16 1.415(2) . ? C15 C27 1.382(3) . ? C15 C26 1.383(3) . ? C15 H27 1.01(3) . ? C16 C23 1.4823(19) . ? C17 C24 1.394(2) . ? C17 C30 1.400(2) . ? C18 C24 1.400(2) . ? C18 H24 0.97(2) . ? C19 C25 1.391(2) . ? C19 H22 0.93(2) . ? C20 C25 1.373(3) . ? C20 H30 0.85(3) . ? C21 H11 0.98(2) . ? C21 H14 0.95(2) . ? C21 H20 0.86(2) . ? C22 C27 1.394(3) . ? C22 C29 1.399(2) . ? C22 H5 0.94(2) . ? C24 H2 0.989(18) . ? C25 H25 0.89(2) . ? C26 H31 0.98(3) . ? C27 H17 0.92(2) . ? C28 H16 0.97(2) . ? C30 H32 0.98(2) . ? C31 C32 1.394(2) . ? C31 H6 0.989(19) . ? C33 H4 0.91(2) . ? 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 P1 87.27(3) . . ? N1 Ru1 P2 96.68(4) . . ? P1 Ru1 P2 97.771(14) . . ? N1 Ru1 Cl1 167.94(3) . . ? P1 Ru1 Cl1 95.217(13) . . ? P2 Ru1 Cl1 94.673(13) . . ? N1 Ru1 Cl2 82.47(3) . . ? P1 Ru1 Cl2 91.181(13) . . ? P2 Ru1 Cl2 170.966(12) . . ? Cl1 Ru1 Cl2 85.673(12) . . ? N1 Ru1 Cl2 83.12(3) . 2_666 ? P1 Ru1 Cl2 168.481(13) . 2_666 ? P2 Ru1 Cl2 89.672(12) . 2_666 ? Cl1 Ru1 Cl2 92.911(12) . 2_666 ? Cl2 Ru1 Cl2 81.295(12) . 2_666 ? Ru1 Cl2 Ru1 98.704(12) . 2_666 ? C14 P1 C5 105.40(7) . . ? C14 P1 C21 99.68(8) . . ? C5 P1 C21 99.95(8) . . ? C14 P1 Ru1 111.62(5) . . ? C5 P1 Ru1 121.90(6) . . ? C21 P1 Ru1 115.45(5) . . ? C29 P2 C17 102.31(7) . . ? C29 P2 C32 104.98(7) . . ? C17 P2 C32 96.16(6) . . ? C29 P2 Ru1 112.41(5) . . ? C17 P2 Ru1 126.04(5) . . ? C32 P2 Ru1 112.21(5) . . ? C23 N1 Ru1 137.59(10) . . ? C23 N1 H1 113.4(13) . . ? Ru1 N1 H1 107.1(13) . . ? C20 C1 C3 119.9(2) . . ? C20 C1 H29 120.4(18) . . ? C3 C1 H29 119.7(18) . . ? C4 C2 C31 120.37(18) . . ? C4 C2 H28 122.9(17) . . ? C31 C2 H28 116.7(17) . . ? C1 C3 C12 120.12(19) . . ? C1 C3 H26 118.8(15) . . ? C12 C3 H26 121.1(15) . . ? C2 C4 C28 120.00(17) . . ? C2 C4 H23 122.2(17) . . ? C28 C4 H23 117.6(17) . . ? P1 C5 H9 108.2(12) . . ? P1 C5 H10 103.5(13) . . ? H9 C5 H10 109.4(17) . . ? P1 C5 H13 108.7(14) . . ? H9 C5 H13 110.8(18) . . ? H10 C5 H13 115.7(19) . . ? C18 C6 C11 119.76(14) . . ? C18 C6 H18 121.9(12) . . ? C11 C6 H18 118.3(12) . . ? C10 C7 C13 119.66(16) . . ? C10 C7 H8 118.9(15) . . ? C13 C7 H8 121.4(15) . . ? C26 C8 C29 120.96(16) . . ? C26 C8 H21 119.4(13) . . ? C29 C8 H21 119.6(13) . . ? C28 C9 C32 120.53(16) . . ? C28 C9 H19 121.9(12) . . ? C32 C9 H19 117.5(12) . . ? C7 C10 C33 120.14(15) . . ? C7 C10 H3 122.3(13) . . ? C33 C10 H3 117.4(13) . . ? C30 C11 C6 119.93(15) . . ? C30 C11 H12 120.5(12) . . ? C6 C11 H12 119.6(12) . . ? C19 C12 C3 119.44(15) . . ? C19 C12 C23 121.00(14) . . ? C3 C12 C23 119.51(14) . . ? C7 C13 C16 121.38(15) . . ? C7 C13 H15 119.8(13) . . ? C16 C13 H15 118.8(13) . . ? C33 C14 C16 118.69(14) . . ? C33 C14 P1 120.87(12) . . ? C16 C14 P1 120.29(10) . . ? C27 C15 C26 120.44(18) . . ? C27 C15 H27 119.1(14) . . ? C26 C15 H27 120.4(14) . . ? C13 C16 C14 118.79(13) . . ? C13 C16 C23 117.09(13) . . ? C14 C16 C23 124.08(13) . . ? C24 C17 C30 118.64(13) . . ? C24 C17 P2 121.96(11) . . ? C30 C17 P2 118.98(11) . . ? C6 C18 C24 120.62(15) . . ? C6 C18 H24 121.6(13) . . ? C24 C18 H24 117.7(13) . . ? C25 C19 C12 119.93(17) . . ? C25 C19 H22 119.2(14) . . ? C12 C19 H22 120.8(14) . . ? C25 C20 C1 120.27(18) . . ? C25 C20 H30 121.7(18) . . ? C1 C20 H30 117.9(18) . . ? P1 C21 H11 111.0(12) . . ? P1 C21 H14 109.2(14) . . ? H11 C21 H14 109.0(19) . . ? P1 C21 H20 110.9(16) . . ? H11 C21 H20 110.8(19) . . ? H14 C21 H20 106(2) . . ? C27 C22 C29 120.59(17) . . ? C27 C22 H5 118.6(12) . . ? C29 C22 H5 120.8(12) . . ? N1 C23 C16 123.14(13) . . ? N1 C23 C12 118.46(12) . . ? C16 C23 C12 118.39(12) . . ? C17 C24 C18 119.97(14) . . ? C17 C24 H2 119.0(11) . . ? C18 C24 H2 120.9(11) . . ? C20 C25 C19 120.33(18) . . ? C20 C25 H25 122.3(15) . . ? C19 C25 H25 117.3(15) . . ? C15 C26 C8 119.74(19) . . ? C15 C26 H31 116.6(15) . . ? C8 C26 H31 123.6(15) . . ? C15 C27 C22 119.88(17) . . ? C15 C27 H17 122.3(16) . . ? C22 C27 H17 117.8(16) . . ? C4 C28 C9 120.02(19) . . ? C4 C28 H16 120.9(13) . . ? C9 C28 H16 119.1(13) . . ? C8 C29 C22 118.33(15) . . ? C8 C29 P2 121.60(12) . . ? C22 C29 P2 119.69(12) . . ? C11 C30 C17 121.02(15) . . ? C11 C30 H32 120.7(12) . . ? C17 C30 H32 118.2(12) . . ? C32 C31 C2 120.25(18) . . ? C32 C31 H6 120.7(11) . . ? C2 C31 H6 119.0(11) . . ? C31 C32 C9 118.82(15) . . ? C31 C32 P2 124.17(13) . . ? C9 C32 P2 116.96(11) . . ? C10 C33 C14 121.33(15) . . ? C10 C33 H4 121.4(14) . . ? C14 C33 H4 117.2(14) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 33.16 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.947 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.079 #===end data_ccb085_0m _database_code_depnum_ccdc_archive 'CCDC 869895' #TrackingRef '- All-cifs-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H55 Cl2 N5 P2 Ru' _chemical_formula_weight 1116.03 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 10.6627(5) _cell_length_b 17.9387(8) _cell_length_c 28.2348(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.259(2) _cell_angle_gamma 90.00 _cell_volume 5396.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 0.495 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8267 _exptl_absorpt_correction_T_max 0.8267 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 78203 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 33.00 _reflns_number_total 20332 _reflns_number_gt 15702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0525P)^2^+5.3658P] 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 20332 _refine_ls_number_parameters 662 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.037 _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 0.375844(13) 0.387573(8) 0.128148(5) 0.01549(4) Uani 1 1 d . . . Cl1 Cl 0.58740(4) 0.34479(3) 0.110999(18) 0.02450(10) Uani 1 1 d . . . Cl2 Cl 0.46224(4) 0.51404(2) 0.142888(17) 0.01967(9) Uani 1 1 d . . . P1 P 0.24652(5) 0.28798(3) 0.113202(18) 0.01859(9) Uani 1 1 d . . . P2 P 0.40680(4) 0.36860(3) 0.208973(17) 0.01538(9) Uani 1 1 d . . . N1 N 0.21204(15) 0.43952(9) 0.13629(6) 0.0177(3) Uani 1 1 d . . . C80 C 0.01908(17) 0.50497(11) 0.12449(7) 0.0195(3) Uani 1 1 d . . . N3 N 0.36248(15) 0.42030(10) 0.05397(6) 0.0220(3) Uani 1 1 d . . . C1 C 0.2936(2) 0.19678(12) 0.09039(8) 0.0263(4) Uani 1 1 d . . . C2 C 0.4164(2) 0.18545(14) 0.07694(10) 0.0353(5) Uani 1 1 d . . . H2 H 0.4762 0.2246 0.0801 0.042 Uiso 1 1 calc R . . C3 C 0.4515(3) 0.11659(17) 0.05884(14) 0.0551(9) Uani 1 1 d . . . H3 H 0.5354 0.1089 0.0498 0.066 Uiso 1 1 calc R . . C4 C 0.3652(3) 0.05962(17) 0.05391(14) 0.0591(9) Uani 1 1 d . . . H4 H 0.3894 0.0131 0.0410 0.071 Uiso 1 1 calc R . . C5 C 0.2432(3) 0.07011(15) 0.06770(12) 0.0471(7) Uani 1 1 d . . . H5 H 0.1842 0.0306 0.0648 0.056 Uiso 1 1 calc R . . C6 C 0.2074(2) 0.13833(13) 0.08573(9) 0.0325(5) Uani 1 1 d . . . H6 H 0.1235 0.1454 0.0950 0.039 Uiso 1 1 calc R . . C7 C 0.13429(18) 0.32292(11) 0.06695(7) 0.0212(4) Uani 1 1 d . . . C8 C 0.1066(2) 0.28148(13) 0.02602(8) 0.0294(4) Uani 1 1 d . . . H8 H 0.1441 0.2339 0.0224 0.035 Uiso 1 1 calc R . . C9 C 0.0246(2) 0.30875(15) -0.00978(8) 0.0347(5) Uani 1 1 d . . . H9 H 0.0076 0.2800 -0.0376 0.042 Uiso 1 1 calc R . . C10 C -0.0314(2) 0.37711(14) -0.00469(8) 0.0315(5) Uani 1 1 d . . . H10 H -0.0872 0.3957 -0.0290 0.038 Uiso 1 1 calc R . . C11 C -0.00651(19) 0.41906(12) 0.03586(7) 0.0247(4) Uani 1 1 d . . . H11 H -0.0471 0.4657 0.0394 0.030 Uiso 1 1 calc R . . C12 C 0.07758(17) 0.39364(11) 0.07160(7) 0.0193(3) Uani 1 1 d . . . C13 C 0.10629(17) 0.44400(10) 0.11209(7) 0.0183(3) Uani 1 1 d . . . C14 C -0.10992(18) 0.49466(12) 0.12818(7) 0.0237(4) Uani 1 1 d . . . H14 H -0.1463 0.4473 0.1215 0.028 Uiso 1 1 calc R . . C15 C -0.18500(19) 0.55345(13) 0.14155(8) 0.0279(4) Uani 1 1 d . . . H15 H -0.2724 0.5458 0.1449 0.033 Uiso 1 1 calc R . . C16 C -0.1335(2) 0.62349(13) 0.15013(9) 0.0300(5) Uani 1 1 d . . . H16 H -0.1857 0.6637 0.1589 0.036 Uiso 1 1 calc R . . C17 C -0.0053(2) 0.63462(13) 0.14585(9) 0.0283(4) Uani 1 1 d . . . H17 H 0.0301 0.6826 0.1514 0.034 Uiso 1 1 calc R . . C18 C 0.07053(19) 0.57548(11) 0.13349(8) 0.0231(4) Uani 1 1 d . . . H18 H 0.1583 0.5830 0.1311 0.028 Uiso 1 1 calc R . . C19 C 0.13749(18) 0.25719(11) 0.15881(7) 0.0212(4) Uani 1 1 d . . . C20 C 0.1718(2) 0.19821(11) 0.18926(8) 0.0243(4) Uani 1 1 d . . . H20 H 0.2502 0.1740 0.1860 0.029 Uiso 1 1 calc R . . C21 C 0.0924(2) 0.17477(12) 0.22420(8) 0.0282(4) Uani 1 1 d . . . H21 H 0.1168 0.1348 0.2446 0.034 Uiso 1 1 calc R . . C22 C -0.0227(2) 0.20975(13) 0.22936(8) 0.0300(5) Uani 1 1 d . . . H22 H -0.0760 0.1944 0.2537 0.036 Uiso 1 1 calc R . . C23 C -0.0594(2) 0.26678(13) 0.19911(8) 0.0288(4) Uani 1 1 d . . . H23 H -0.1386 0.2901 0.2023 0.035 Uiso 1 1 calc R . . C24 C 0.01981(19) 0.29011(12) 0.16390(8) 0.0244(4) Uani 1 1 d . . . H24 H -0.0066 0.3291 0.1430 0.029 Uiso 1 1 calc R . . C25 C 0.53916(17) 0.41380(10) 0.24205(7) 0.0185(3) Uani 1 1 d . . . C26 C 0.52764(19) 0.43127(12) 0.28989(7) 0.0235(4) Uani 1 1 d . . . H26 H 0.4525 0.4189 0.3051 0.028 Uiso 1 1 calc R . . C27 C 0.6244(2) 0.46643(13) 0.31565(8) 0.0285(4) Uani 1 1 d . . . H27 H 0.6146 0.4786 0.3480 0.034 Uiso 1 1 calc R . . C28 C 0.7348(2) 0.48359(13) 0.29402(8) 0.0301(5) Uani 1 1 d . . . H28 H 0.8004 0.5086 0.3113 0.036 Uiso 1 1 calc R . . C29 C 0.74946(19) 0.46417(13) 0.24699(8) 0.0270(4) Uani 1 1 d . . . H29 H 0.8264 0.4746 0.2325 0.032 Uiso 1 1 calc R . . C30 C 0.65225(18) 0.42945(11) 0.22086(7) 0.0217(4) Uani 1 1 d . . . H30 H 0.6630 0.4165 0.1887 0.026 Uiso 1 1 calc R . . C31 C 0.27650(17) 0.40845(11) 0.24101(7) 0.0189(3) Uani 1 1 d . . . C32 C 0.27431(19) 0.48653(12) 0.24459(8) 0.0244(4) Uani 1 1 d . . . H32 H 0.3402 0.5150 0.2319 0.029 Uiso 1 1 calc R . . C33 C 0.1769(2) 0.52255(14) 0.26640(9) 0.0333(5) Uani 1 1 d . . . H33 H 0.1767 0.5754 0.2689 0.040 Uiso 1 1 calc R . . C34 C 0.0802(2) 0.48139(16) 0.28454(10) 0.0403(6) Uani 1 1 d . . . H34 H 0.0144 0.5058 0.3002 0.048 Uiso 1 1 calc R . . C35 C 0.0795(2) 0.40493(16) 0.27986(10) 0.0372(6) Uani 1 1 d . . . H35 H 0.0118 0.3769 0.2916 0.045 Uiso 1 1 calc R . . C36 C 0.17719(19) 0.36812(13) 0.25806(8) 0.0251(4) Uani 1 1 d . . . H36 H 0.1755 0.3154 0.2549 0.030 Uiso 1 1 calc R . . C37 C 0.42909(17) 0.27340(10) 0.23051(7) 0.0194(3) Uani 1 1 d . . . C38 C 0.39796(18) 0.24993(12) 0.27566(8) 0.0241(4) Uani 1 1 d . . . H38 H 0.3651 0.2845 0.2974 0.029 Uiso 1 1 calc R . . C39 C 0.4151(2) 0.17571(13) 0.28870(9) 0.0302(5) Uani 1 1 d . . . H39 H 0.3926 0.1596 0.3193 0.036 Uiso 1 1 calc R . . C40 C 0.4647(2) 0.12516(12) 0.25743(10) 0.0316(5) Uani 1 1 d . . . H40 H 0.4727 0.0741 0.2660 0.038 Uiso 1 1 calc R . . C41 C 0.5026(2) 0.14912(12) 0.21372(9) 0.0311(5) Uani 1 1 d . . . H41 H 0.5408 0.1151 0.1929 0.037 Uiso 1 1 calc R . . C42 C 0.4850(2) 0.22304(11) 0.20015(8) 0.0252(4) Uani 1 1 d . . . H42 H 0.5110 0.2393 0.1701 0.030 Uiso 1 1 calc R . . C43 C 0.32556(19) 0.48993(13) 0.04227(8) 0.0257(4) Uani 1 1 d . . . H43 H 0.2978 0.5218 0.0666 0.031 Uiso 1 1 calc R . . C44 C 0.3262(2) 0.51736(15) -0.00376(8) 0.0334(5) Uani 1 1 d . . . H44 H 0.2992 0.5668 -0.0105 0.040 Uiso 1 1 calc R . . C45 C 0.3663(2) 0.47230(18) -0.03917(9) 0.0397(6) Uani 1 1 d . . . H45 H 0.3698 0.4902 -0.0707 0.048 Uiso 1 1 calc R . . C46 C 0.4015(2) 0.40011(18) -0.02804(8) 0.0392(6) Uani 1 1 d . . . H46 H 0.4273 0.3673 -0.0522 0.047 Uiso 1 1 calc R . . C47 C 0.3991(2) 0.37573(14) 0.01877(8) 0.0306(5) Uani 1 1 d . . . H47 H 0.4240 0.3261 0.0261 0.037 Uiso 1 1 calc R . . C48 C 0.8932(4) 0.06133(18) 0.09018(11) 0.0671(10) Uani 1 1 d D . . H48 H 0.9270 0.0202 0.1076 0.081 Uiso 1 1 calc R . . N4 N 0.8938(5) 0.0614(3) 0.04178(12) 0.1220(18) Uani 1 1 d D . . C50 C 0.8436(5) 0.1209(3) 0.01734(18) 0.110(2) Uani 1 1 d D . . H50 H 0.8426 0.1202 -0.0163 0.132 Uiso 1 1 calc R . . C51 C 0.7940(5) 0.1823(3) 0.03998(14) 0.110(2) Uani 1 1 d D . . H51 H 0.7608 0.2232 0.0222 0.132 Uiso 1 1 calc R . . C52 C 0.7937(3) 0.18263(19) 0.08914(14) 0.0725(12) Uani 1 1 d D . . H52 H 0.7605 0.2238 0.1057 0.087 Uiso 1 1 calc R . . C53 C 0.8430(4) 0.12159(17) 0.11364(12) 0.0690(11) Uani 1 1 d D . . H53 H 0.8424 0.1211 0.1473 0.083 Uiso 1 1 calc R . . C59 C 0.6790(3) 0.20402(16) 0.36803(13) 0.0490(7) Uani 1 1 d . . . H59 H 0.6256 0.1617 0.3690 0.059 Uiso 1 1 calc R . . C60 C 0.7043(2) 0.23748(16) 0.32527(11) 0.0426(6) Uani 1 1 d . . . H60 H 0.6706 0.2176 0.2963 0.051 Uiso 1 1 calc R . . C61 C 0.7776(3) 0.29893(16) 0.32551(11) 0.0417(6) Uani 1 1 d . . . H61 H 0.7952 0.3234 0.2967 0.050 Uiso 1 1 calc R . . C62 C 0.8266(3) 0.32559(17) 0.36793(12) 0.0489(7) Uani 1 1 d . . . H62 H 0.8775 0.3690 0.3674 0.059 Uiso 1 1 calc R . . C63 C 0.7325(3) 0.23316(19) 0.40882(12) 0.0529(8) Uani 1 1 d . . . H63 H 0.7167 0.2093 0.4380 0.063 Uiso 1 1 calc R . . N5 N 0.8067(3) 0.29420(17) 0.40960(10) 0.0581(7) Uani 1 1 d . . . C100 C 0.4102(3) 0.2795(2) 0.4275(2) 0.0934(16) Uani 1 1 d D . . H10A H 0.4657 0.2403 0.4369 0.112 Uiso 1 1 calc R . . C101 C 0.2817(3) 0.2695(2) 0.42111(19) 0.0916(15) Uani 1 1 d D . . H10B H 0.2488 0.2214 0.4274 0.110 Uiso 1 1 calc R . . C102 C 0.3712(4) 0.4101(3) 0.4066(2) 0.0993(17) Uani 1 1 d D . . H10C H 0.4027 0.4588 0.4014 0.119 Uiso 1 1 calc R . . C103 C 0.1975(4) 0.3245(2) 0.4062(2) 0.109(2) Uani 1 1 d D . . H10D H 0.1114 0.3139 0.3994 0.131 Uiso 1 1 calc R . . N6 N 0.2454(5) 0.3948(2) 0.4019(3) 0.176(3) Uani 1 1 d D . . C105 C 0.4507(5) 0.3515(2) 0.4192(3) 0.124(2) Uani 1 1 d D . . H10E H 0.5382 0.3614 0.4222 0.149 Uiso 1 1 calc R . . H90 H 0.214(2) 0.4730(14) 0.1577(9) 0.019(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01516(6) 0.01467(7) 0.01669(7) 0.00052(5) 0.00107(5) -0.00139(5) Cl1 0.0201(2) 0.0258(2) 0.0279(2) -0.00252(18) 0.00484(17) 0.00183(17) Cl2 0.01919(19) 0.01632(18) 0.0234(2) 0.00119(16) -0.00079(15) -0.00367(15) P1 0.0202(2) 0.0158(2) 0.0197(2) -0.00152(17) 0.00056(17) -0.00233(17) P2 0.01448(19) 0.01348(19) 0.0182(2) 0.00079(16) 0.00050(16) -0.00010(15) N1 0.0188(7) 0.0162(7) 0.0180(7) 0.0005(6) 0.0002(6) -0.0014(6) C80 0.0176(8) 0.0214(8) 0.0195(8) 0.0020(7) -0.0006(6) -0.0005(7) N3 0.0185(7) 0.0284(9) 0.0192(8) 0.0024(6) 0.0014(6) -0.0056(6) C1 0.0310(10) 0.0190(9) 0.0290(10) -0.0059(8) 0.0002(8) -0.0003(8) C2 0.0349(12) 0.0283(11) 0.0431(14) -0.0122(10) 0.0065(10) -0.0006(9) C3 0.0453(16) 0.0413(16) 0.080(2) -0.0284(16) 0.0149(15) 0.0056(13) C4 0.066(2) 0.0324(14) 0.080(2) -0.0290(15) 0.0065(18) 0.0054(14) C5 0.0561(17) 0.0245(11) 0.0606(19) -0.0177(12) 0.0030(14) -0.0065(11) C6 0.0383(12) 0.0218(10) 0.0375(13) -0.0074(9) 0.0007(10) -0.0041(9) C7 0.0218(8) 0.0228(9) 0.0189(9) -0.0003(7) 0.0007(7) -0.0054(7) C8 0.0337(11) 0.0291(11) 0.0250(10) -0.0065(8) -0.0032(8) -0.0033(9) C9 0.0386(12) 0.0419(13) 0.0230(10) -0.0072(9) -0.0071(9) -0.0029(10) C10 0.0321(11) 0.0407(13) 0.0211(10) 0.0016(9) -0.0079(8) -0.0040(9) C11 0.0232(9) 0.0284(10) 0.0222(9) 0.0037(8) -0.0026(7) -0.0027(8) C12 0.0177(8) 0.0220(9) 0.0182(8) 0.0022(7) -0.0002(6) -0.0058(7) C13 0.0173(8) 0.0185(8) 0.0189(8) 0.0039(7) -0.0005(6) -0.0030(6) C14 0.0194(9) 0.0260(9) 0.0256(10) 0.0013(8) -0.0008(7) -0.0013(7) C15 0.0182(9) 0.0349(11) 0.0306(11) 0.0012(9) 0.0017(8) 0.0026(8) C16 0.0259(10) 0.0303(11) 0.0339(12) -0.0042(9) 0.0024(8) 0.0072(8) C17 0.0266(10) 0.0237(9) 0.0346(12) -0.0041(8) -0.0003(8) 0.0008(8) C18 0.0200(8) 0.0212(9) 0.0279(10) 0.0001(7) -0.0008(7) -0.0007(7) C19 0.0222(9) 0.0177(8) 0.0237(9) 0.0004(7) -0.0002(7) -0.0065(7) C20 0.0256(9) 0.0191(9) 0.0279(10) 0.0006(7) -0.0026(8) -0.0051(7) C21 0.0359(11) 0.0207(9) 0.0279(11) 0.0049(8) -0.0005(9) -0.0076(8) C22 0.0340(11) 0.0277(10) 0.0286(11) 0.0016(9) 0.0066(9) -0.0121(9) C23 0.0252(10) 0.0292(10) 0.0323(11) -0.0004(9) 0.0058(8) -0.0053(8) C24 0.0244(9) 0.0224(9) 0.0267(10) 0.0026(8) 0.0020(7) -0.0045(7) C25 0.0170(8) 0.0153(8) 0.0228(9) 0.0018(7) -0.0027(6) 0.0002(6) C26 0.0206(9) 0.0266(9) 0.0232(9) 0.0001(8) -0.0001(7) -0.0004(7) C27 0.0291(10) 0.0312(11) 0.0249(10) -0.0047(8) -0.0040(8) -0.0004(8) C28 0.0241(10) 0.0326(11) 0.0328(12) -0.0013(9) -0.0085(8) -0.0048(8) C29 0.0183(9) 0.0303(10) 0.0322(11) 0.0034(9) -0.0019(8) -0.0033(8) C30 0.0173(8) 0.0236(9) 0.0242(9) 0.0023(7) -0.0006(7) 0.0006(7) C31 0.0158(8) 0.0204(8) 0.0201(8) -0.0017(7) -0.0018(6) 0.0018(6) C32 0.0225(9) 0.0217(9) 0.0291(10) -0.0014(8) 0.0004(8) 0.0041(7) C33 0.0295(11) 0.0282(11) 0.0421(13) -0.0083(10) -0.0016(9) 0.0102(9) C34 0.0218(10) 0.0478(15) 0.0519(16) -0.0160(12) 0.0072(10) 0.0093(10) C35 0.0193(9) 0.0454(14) 0.0475(15) -0.0105(12) 0.0086(9) -0.0031(9) C36 0.0192(9) 0.0284(10) 0.0276(10) -0.0034(8) 0.0011(7) -0.0026(7) C37 0.0167(8) 0.0158(8) 0.0254(9) 0.0035(7) -0.0024(7) -0.0012(6) C38 0.0196(9) 0.0239(9) 0.0287(10) 0.0058(8) -0.0010(7) 0.0001(7) C39 0.0220(9) 0.0279(10) 0.0402(13) 0.0159(9) -0.0046(9) -0.0028(8) C40 0.0253(10) 0.0182(9) 0.0505(15) 0.0097(9) -0.0077(9) -0.0001(7) C41 0.0297(11) 0.0180(9) 0.0453(14) -0.0005(9) -0.0032(9) 0.0040(8) C42 0.0259(9) 0.0185(9) 0.0310(11) 0.0014(8) 0.0000(8) 0.0016(7) C43 0.0211(9) 0.0321(11) 0.0239(10) 0.0076(8) -0.0014(7) -0.0048(8) C44 0.0218(9) 0.0479(14) 0.0301(11) 0.0175(10) -0.0035(8) -0.0062(9) C45 0.0234(10) 0.0729(19) 0.0223(10) 0.0138(11) -0.0034(8) -0.0118(11) C46 0.0296(11) 0.0677(18) 0.0207(10) -0.0062(11) 0.0063(8) -0.0105(12) C47 0.0263(10) 0.0412(13) 0.0244(10) -0.0052(9) 0.0038(8) -0.0057(9) C48 0.096(3) 0.0451(18) 0.059(2) -0.0021(16) -0.017(2) 0.0009(19) N4 0.123(4) 0.146(5) 0.096(4) -0.038(3) 0.000(3) -0.033(4) C50 0.130(5) 0.138(6) 0.062(3) 0.028(3) 0.001(3) -0.046(4) C51 0.122(5) 0.088(4) 0.117(5) 0.055(3) -0.051(4) -0.045(3) C52 0.052(2) 0.058(2) 0.106(3) -0.012(2) -0.016(2) 0.0004(17) C53 0.091(3) 0.067(2) 0.048(2) -0.0057(17) -0.0037(19) -0.009(2) C59 0.0309(13) 0.0346(14) 0.081(2) 0.0004(14) 0.0000(13) -0.0008(11) C60 0.0274(11) 0.0410(14) 0.0584(18) -0.0082(13) -0.0079(11) 0.0055(10) C61 0.0352(13) 0.0404(14) 0.0491(16) 0.0043(12) -0.0033(11) 0.0065(11) C62 0.0499(16) 0.0332(13) 0.063(2) -0.0004(13) -0.0084(14) -0.0018(12) C63 0.0516(17) 0.0530(18) 0.0541(19) 0.0140(15) 0.0023(14) 0.0068(14) N5 0.0643(18) 0.0558(17) 0.0532(17) -0.0046(13) -0.0112(14) 0.0002(14) C100 0.063(3) 0.073(3) 0.146(5) 0.014(3) 0.028(3) 0.009(2) C101 0.098(4) 0.065(3) 0.111(4) -0.001(3) 0.003(3) 0.000(3) C102 0.112(4) 0.084(3) 0.104(4) -0.001(3) 0.030(3) -0.023(3) C103 0.078(3) 0.070(3) 0.176(6) 0.046(3) -0.037(3) -0.015(2) N6 0.175(7) 0.096(4) 0.252(9) -0.011(5) -0.053(6) 0.014(4) C105 0.081(3) 0.101(4) 0.192(7) 0.058(5) 0.038(4) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.0008(16) . ? Ru1 N3 2.1744(17) . ? Ru1 P1 2.2860(5) . ? Ru1 P2 2.3180(5) . ? Ru1 Cl1 2.4490(5) . ? Ru1 Cl2 2.4776(5) . ? P1 C1 1.835(2) . ? P1 C7 1.846(2) . ? P1 C19 1.853(2) . ? P2 C37 1.8252(19) . ? P2 C31 1.833(2) . ? P2 C25 1.8487(19) . ? N1 C13 1.298(2) . ? N1 H90 0.85(3) . ? C80 C14 1.396(3) . ? C80 C18 1.398(3) . ? C80 C13 1.486(3) . ? N3 C47 1.345(3) . ? N3 C43 1.347(3) . ? C1 C2 1.393(3) . ? C1 C6 1.397(3) . ? C2 C3 1.394(3) . ? C2 H2 0.9500 . ? C3 C4 1.378(4) . ? C3 H3 0.9500 . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C6 1.385(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.396(3) . ? C7 C12 1.414(3) . ? C8 C9 1.399(3) . ? C8 H8 0.9500 . ? C9 C10 1.374(4) . ? C9 H9 0.9500 . ? C10 C11 1.387(3) . ? C10 H10 0.9500 . ? C11 C12 1.400(3) . ? C11 H11 0.9500 . ? C12 C13 1.480(3) . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.389(3) . ? C15 H15 0.9500 . ? C16 C17 1.391(3) . ? C16 H16 0.9500 . ? C17 C18 1.387(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.399(3) . ? C19 C20 1.403(3) . ? C20 C21 1.390(3) . ? C20 H20 0.9500 . ? C21 C22 1.391(3) . ? C21 H21 0.9500 . ? C22 C23 1.379(3) . ? C22 H22 0.9500 . ? C23 C24 1.394(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.396(3) . ? C25 C26 1.397(3) . ? C26 C27 1.390(3) . ? C26 H26 0.9500 . ? C27 C28 1.382(3) . ? C27 H27 0.9500 . ? C28 C29 1.388(3) . ? C28 H28 0.9500 . ? C29 C30 1.395(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.385(3) . ? C31 C32 1.405(3) . ? C32 C33 1.387(3) . ? C32 H32 0.9500 . ? C33 C34 1.383(4) . ? C33 H33 0.9500 . ? C34 C35 1.378(4) . ? C34 H34 0.9500 . ? C35 C36 1.396(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.395(3) . ? C37 C42 1.395(3) . ? C38 C39 1.392(3) . ? C38 H38 0.9500 . ? C39 C40 1.385(4) . ? C39 H39 0.9500 . ? C40 C41 1.382(4) . ? C40 H40 0.9500 . ? C41 C42 1.391(3) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.390(3) . ? C43 H43 0.9500 . ? C44 C45 1.367(4) . ? C44 H44 0.9500 . ? C45 C46 1.381(4) . ? C45 H45 0.9500 . ? C46 C47 1.393(3) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 N4 1.3670(10) . ? C48 C53 1.3861(10) . ? C48 H48 0.9500 . ? N4 C50 1.3684(10) . ? C50 C51 1.3880(10) . ? C50 H50 0.9500 . ? C51 C52 1.3882(10) . ? C51 H51 0.9500 . ? C52 C53 1.3875(10) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C59 C63 1.369(5) . ? C59 C60 1.384(5) . ? C59 H59 0.9500 . ? C60 C61 1.352(4) . ? C60 H60 0.9500 . ? C61 C62 1.373(4) . ? C61 H61 0.9500 . ? C62 N5 1.329(4) . ? C62 H62 0.9500 . ? C63 N5 1.351(4) . ? C63 H63 0.9500 . ? C100 C105 1.3861(10) . ? C100 C101 1.3865(10) . ? C100 H10A 0.9500 . ? C101 C103 1.3876(10) . ? C101 H10B 0.9500 . ? C102 N6 1.3701(10) . ? C102 C105 1.3872(10) . ? C102 H10C 0.9500 . ? C103 N6 1.3686(10) . ? C103 H10D 0.9500 . ? C105 H10E 0.9500 . ? 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 N3 87.74(7) . . ? N1 Ru1 P1 82.08(5) . . ? N3 Ru1 P1 90.98(5) . . ? N1 Ru1 P2 92.66(5) . . ? N3 Ru1 P2 171.61(5) . . ? P1 Ru1 P2 97.380(18) . . ? N1 Ru1 Cl1 169.62(5) . . ? N3 Ru1 Cl1 85.42(5) . . ? P1 Ru1 Cl1 105.795(18) . . ? P2 Ru1 Cl1 92.987(18) . . ? N1 Ru1 Cl2 82.80(5) . . ? N3 Ru1 Cl2 85.66(5) . . ? P1 Ru1 Cl2 164.632(18) . . ? P2 Ru1 Cl2 86.072(16) . . ? Cl1 Ru1 Cl2 88.905(17) . . ? C1 P1 C7 103.47(10) . . ? C1 P1 C19 99.56(10) . . ? C7 P1 C19 100.72(9) . . ? C1 P1 Ru1 126.16(7) . . ? C7 P1 Ru1 103.57(6) . . ? C19 P1 Ru1 119.68(6) . . ? C37 P2 C31 106.96(9) . . ? C37 P2 C25 98.93(8) . . ? C31 P2 C25 99.10(9) . . ? C37 P2 Ru1 118.49(7) . . ? C31 P2 Ru1 110.32(6) . . ? C25 P2 Ru1 120.61(6) . . ? C13 N1 Ru1 135.46(14) . . ? C13 N1 H90 108.9(16) . . ? Ru1 N1 H90 114.5(16) . . ? C14 C80 C18 119.15(19) . . ? C14 C80 C13 123.21(18) . . ? C18 C80 C13 117.63(17) . . ? C47 N3 C43 117.42(19) . . ? C47 N3 Ru1 122.76(16) . . ? C43 N3 Ru1 119.61(15) . . ? C2 C1 C6 119.2(2) . . ? C2 C1 P1 119.92(17) . . ? C6 C1 P1 120.92(18) . . ? C1 C2 C3 119.9(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.1(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 119.9(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.5(2) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C8 C7 C12 118.53(19) . . ? C8 C7 P1 120.99(17) . . ? C12 C7 P1 120.44(14) . . ? C7 C8 C9 121.2(2) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 119.9(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.1(2) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 121.0(2) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C7 119.30(18) . . ? C11 C12 C13 117.74(18) . . ? C7 C12 C13 122.92(17) . . ? N1 C13 C12 121.20(18) . . ? N1 C13 C80 117.41(17) . . ? C12 C13 C80 121.26(16) . . ? C15 C14 C80 120.1(2) . . ? C15 C14 H14 120.0 . . ? C80 C14 H14 120.0 . . ? C14 C15 C16 120.5(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 119.9(2) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 119.8(2) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C80 120.60(19) . . ? C17 C18 H18 119.7 . . ? C80 C18 H18 119.7 . . ? C24 C19 C20 117.93(19) . . ? C24 C19 P1 122.37(15) . . ? C20 C19 P1 119.69(16) . . ? C21 C20 C19 120.8(2) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 120.0(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0(2) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 121.2(2) . . ? C23 C24 H24 119.4 . . ? C19 C24 H24 119.4 . . ? C30 C25 C26 118.68(18) . . ? C30 C25 P2 121.80(15) . . ? C26 C25 P2 119.50(15) . . ? C27 C26 C25 121.07(19) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C28 C27 C26 119.8(2) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 119.8(2) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C29 C30 120.6(2) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C25 120.0(2) . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C36 C31 C32 118.74(19) . . ? C36 C31 P2 124.96(16) . . ? C32 C31 P2 116.08(15) . . ? C33 C32 C31 120.7(2) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 119.9(2) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 119.8(2) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.8(2) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C31 C36 C35 120.0(2) . . ? C31 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C42 119.27(18) . . ? C38 C37 P2 123.66(16) . . ? C42 C37 P2 117.02(15) . . ? C39 C38 C37 119.8(2) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 120.5(2) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C41 C40 C39 119.9(2) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.1(2) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C37 120.3(2) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? N3 C43 C44 123.0(2) . . ? N3 C43 H43 118.5 . . ? C44 C43 H43 118.5 . . ? C45 C44 C43 119.2(2) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C44 C45 C46 118.6(2) . . ? C44 C45 H45 120.7 . . ? C46 C45 H45 120.7 . . ? C45 C46 C47 119.7(2) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? N3 C47 C46 122.1(2) . . ? N3 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? N4 C48 C53 119.6(4) . . ? N4 C48 H48 120.2 . . ? C53 C48 H48 120.2 . . ? C48 N4 C50 119.2(4) . . ? N4 C50 C51 122.3(5) . . ? N4 C50 H50 118.8 . . ? C51 C50 H50 118.8 . . ? C52 C51 C50 118.7(4) . . ? C52 C51 H51 120.7 . . ? C50 C51 H51 120.7 . . ? C53 C52 C51 118.6(4) . . ? C53 C52 H52 120.7 . . ? C51 C52 H52 120.7 . . ? C48 C53 C52 121.5(3) . . ? C48 C53 H53 119.2 . . ? C52 C53 H53 119.2 . . ? C63 C59 C60 118.6(3) . . ? C63 C59 H59 120.7 . . ? C60 C59 H59 120.7 . . ? C61 C60 C59 118.8(3) . . ? C61 C60 H60 120.6 . . ? C59 C60 H60 120.6 . . ? C60 C61 C62 119.2(3) . . ? C60 C61 H61 120.4 . . ? C62 C61 H61 120.4 . . ? N5 C62 C61 123.8(3) . . ? N5 C62 H62 118.1 . . ? C61 C62 H62 118.1 . . ? N5 C63 C59 123.2(3) . . ? N5 C63 H63 118.4 . . ? C59 C63 H63 118.4 . . ? C62 N5 C63 116.3(3) . . ? C105 C100 C101 114.3(4) . . ? C105 C100 H10A 122.8 . . ? C101 C100 H10A 122.8 . . ? C100 C101 C103 124.8(4) . . ? C100 C101 H10B 117.6 . . ? C103 C101 H10B 117.6 . . ? N6 C102 C105 117.3(5) . . ? N6 C102 H10C 121.3 . . ? C105 C102 H10C 121.3 . . ? N6 C103 C101 116.3(4) . . ? N6 C103 H10D 121.8 . . ? C101 C103 H10D 121.8 . . ? C103 N6 C102 122.9(5) . . ? C100 C105 C102 123.9(5) . . ? C100 C105 H10E 118.0 . . ? C102 C105 H10E 118.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 33.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.272 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.092 #===end data_ccb093_0m _database_code_depnum_ccdc_archive 'CCDC 869896' #TrackingRef '- All-cifs-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H34 Cl2 N3 P Ru' _chemical_formula_weight 627.53 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)/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 9.0765(9) _cell_length_b 46.734(5) _cell_length_c 13.7877(14) _cell_angle_alpha 90.00 _cell_angle_beta 108.453(6) _cell_angle_gamma 90.00 _cell_volume 5547.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2312 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 21.42 _exptl_crystal_description needle _exptl_crystal_colour purple _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 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 0.839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8501 _exptl_absorpt_correction_T_max 0.9208 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49302 _diffrn_reflns_av_R_equivalents 0.1516 _diffrn_reflns_av_sigmaI/netI 0.1649 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -60 _diffrn_reflns_limit_k_max 56 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.57 _reflns_number_total 12733 _reflns_number_gt 7009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0381P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12733 _refine_ls_number_parameters 657 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1518 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Ru2 Ru 0.68359(6) 0.329424(10) 0.22078(4) 0.01868(13) Uani 1 1 d . . . Ru1 Ru 1.01732(5) 0.041394(10) 0.26865(3) 0.01258(11) Uani 1 1 d . . . Cl4 Cl 0.89197(18) 0.29516(3) 0.27970(12) 0.0273(4) Uani 1 1 d . . . Cl3 Cl 0.48785(17) 0.36631(3) 0.15450(11) 0.0230(3) Uani 1 1 d . . . Cl2 Cl 1.15315(16) 0.05204(3) 0.14634(10) 0.0186(3) Uani 1 1 d . . . Cl1 Cl 0.86598(15) 0.02706(3) 0.37773(10) 0.0180(3) Uani 1 1 d . . . P2 P 0.51191(19) 0.29424(3) 0.22060(12) 0.0226(4) Uani 1 1 d . . . P1 P 0.95671(17) 0.08817(3) 0.27892(11) 0.0151(3) Uani 1 1 d . . . N5 N 0.8575(5) 0.35944(10) 0.2047(4) 0.0205(12) Uani 1 1 d . . . N6 N 0.7303(6) 0.34742(10) 0.3698(4) 0.0200(11) Uani 1 1 d . . . N1 N 0.8282(5) 0.03938(10) 0.1469(3) 0.0145(10) Uani 1 1 d . . . H1 H 0.7809 0.0228 0.1434 0.017 Uiso 1 1 calc R . . N2 N 1.0492(5) -0.00450(10) 0.2482(3) 0.0154(11) Uani 1 1 d . . . N3 N 1.2315(5) 0.03829(9) 0.3936(3) 0.0136(10) Uani 1 1 d . . . C37 C 0.5566(7) 0.26278(13) 0.1531(5) 0.0218(14) Uani 1 1 d . . . C42 C 0.6091(7) 0.26593(13) 0.0672(5) 0.0251(15) Uani 1 1 d . . . C41 C 0.6379(7) 0.24129(14) 0.0190(5) 0.0311(16) Uani 1 1 d . . . H41 H 0.6723 0.2432 -0.0390 0.037 Uiso 1 1 calc R . . C40 C 0.6179(8) 0.21427(14) 0.0529(5) 0.0330(17) Uani 1 1 d . . . H40 H 0.6387 0.1978 0.0188 0.040 Uiso 1 1 calc R . . C39 C 0.5679(8) 0.21124(14) 0.1363(5) 0.0353(17) Uani 1 1 d . . . H39 H 0.5541 0.1927 0.1604 0.042 Uiso 1 1 calc R . . C38 C 0.5376(8) 0.23526(14) 0.1849(5) 0.0334(17) Uani 1 1 d . . . H38 H 0.5023 0.2329 0.2424 0.040 Uiso 1 1 calc R . . C43 C 0.6352(6) 0.29386(13) 0.0248(5) 0.0213(14) Uani 1 1 d . . . N4 N 0.6581(5) 0.31716(10) 0.0779(4) 0.0217(12) Uani 1 1 d . . . H4 H 0.6643 0.3320 0.0399 0.026 Uiso 1 1 calc R . . C44 C 0.6392(7) 0.29544(13) -0.0831(5) 0.0274(15) Uani 1 1 d . . . C49 C 0.7627(8) 0.30884(14) -0.1037(5) 0.0351(18) Uani 1 1 d . . . H49 H 0.8451 0.3168 -0.0495 0.042 Uiso 1 1 calc R . . C48 C 0.7658(9) 0.31061(15) -0.2040(6) 0.042(2) Uani 1 1 d . . . H48 H 0.8520 0.3193 -0.2173 0.050 Uiso 1 1 calc R . . C47 C 0.6464(10) 0.29995(17) -0.2834(5) 0.050(2) Uani 1 1 d . . . H47 H 0.6473 0.3020 -0.3518 0.061 Uiso 1 1 calc R . . C46 C 0.5244(9) 0.28620(17) -0.2631(5) 0.048(2) Uani 1 1 d . . . H46 H 0.4421 0.2784 -0.3178 0.058 Uiso 1 1 calc R . . C45 C 0.5210(9) 0.28365(15) -0.1648(5) 0.0423(19) Uani 1 1 d . . . H45 H 0.4376 0.2738 -0.1519 0.051 Uiso 1 1 calc R . . C35 C 0.3023(7) 0.30008(13) 0.1490(5) 0.0298(16) Uani 1 1 d . . . H35 H 0.2700 0.3175 0.1793 0.036 Uiso 1 1 calc R . . C34 C 0.2750(7) 0.30687(14) 0.0356(5) 0.0336(17) Uani 1 1 d . . . H34A H 0.3010 0.2901 0.0017 0.050 Uiso 1 1 calc R . . H34B H 0.3409 0.3230 0.0300 0.050 Uiso 1 1 calc R . . H34C H 0.1657 0.3119 0.0028 0.050 Uiso 1 1 calc R . . C36 C 0.1937(7) 0.27585(14) 0.1586(5) 0.0383(18) Uani 1 1 d . . . H36A H 0.0887 0.2795 0.1122 0.058 Uiso 1 1 calc R . . H36B H 0.1913 0.2750 0.2291 0.058 Uiso 1 1 calc R . . H36C H 0.2316 0.2576 0.1407 0.058 Uiso 1 1 calc R . . C32 C 0.5041(8) 0.27939(14) 0.3434(5) 0.0339(17) Uani 1 1 d . . . H32 H 0.4385 0.2618 0.3272 0.041 Uiso 1 1 calc R . . C33 C 0.4249(9) 0.30037(14) 0.3964(5) 0.041(2) Uani 1 1 d . . . H33A H 0.4129 0.2914 0.4576 0.062 Uiso 1 1 calc R . . H33B H 0.3225 0.3055 0.3495 0.062 Uiso 1 1 calc R . . H33C H 0.4887 0.3176 0.4160 0.062 Uiso 1 1 calc R . . C31 C 0.6640(8) 0.27055(16) 0.4140(5) 0.046(2) Uani 1 1 d . . . H31A H 0.7248 0.2877 0.4420 0.069 Uiso 1 1 calc R . . H31B H 0.7178 0.2594 0.3752 0.069 Uiso 1 1 calc R . . H31C H 0.6520 0.2589 0.4701 0.069 Uiso 1 1 calc R . . C54 C 0.8543(7) 0.38728(12) 0.2269(4) 0.0212(14) Uani 1 1 d . . . H54 H 0.7773 0.3938 0.2549 0.025 Uiso 1 1 calc R . . C53 C 0.9581(7) 0.40684(14) 0.2107(4) 0.0259(15) Uani 1 1 d . . . H53 H 0.9523 0.4265 0.2272 0.031 Uiso 1 1 calc R . . C52 C 1.0697(7) 0.39750(14) 0.1703(5) 0.0273(16) Uani 1 1 d . . . H52 H 1.1425 0.4106 0.1587 0.033 Uiso 1 1 calc R . . C51 C 1.0749(7) 0.36893(14) 0.1466(5) 0.0274(16) Uani 1 1 d . . . H51 H 1.1501 0.3621 0.1175 0.033 Uiso 1 1 calc R . . C50 C 0.9689(7) 0.35052(14) 0.1661(4) 0.0237(15) Uani 1 1 d . . . H50 H 0.9746 0.3307 0.1517 0.028 Uiso 1 1 calc R . . C55 C 0.8759(7) 0.34717(13) 0.4355(5) 0.0262(15) Uani 1 1 d . . . H55 H 0.9513 0.3358 0.4189 0.031 Uiso 1 1 calc R . . C56 C 0.9221(7) 0.36259(13) 0.5261(5) 0.0268(15) Uani 1 1 d . . . H56 H 1.0259 0.3614 0.5707 0.032 Uiso 1 1 calc R . . C57 C 0.8151(7) 0.37968(14) 0.5502(5) 0.0284(16) Uani 1 1 d . . . H57 H 0.8445 0.3908 0.6110 0.034 Uiso 1 1 calc R . . C58 C 0.6658(7) 0.38037(13) 0.4852(4) 0.0240(15) Uani 1 1 d . . . H58 H 0.5897 0.3919 0.5002 0.029 Uiso 1 1 calc R . . C59 C 0.6275(7) 0.36400(13) 0.3972(5) 0.0225(14) Uani 1 1 d . . . H59 H 0.5230 0.3644 0.3534 0.027 Uiso 1 1 calc R . . C2 C 1.1109(7) 0.11362(12) 0.3483(4) 0.0211(14) Uani 1 1 d . . . H2 H 1.0647 0.1332 0.3399 0.025 Uiso 1 1 calc R . . C1 C 1.1691(7) 0.10677(14) 0.4619(4) 0.0303(16) Uani 1 1 d . . . H1A H 1.2191 0.0879 0.4722 0.045 Uiso 1 1 calc R . . H1B H 1.0813 0.1066 0.4888 0.045 Uiso 1 1 calc R . . H1C H 1.2442 0.1213 0.4978 0.045 Uiso 1 1 calc R . . C3 C 1.2454(7) 0.11376(13) 0.3034(5) 0.0257(15) Uani 1 1 d . . . H3A H 1.3310 0.1253 0.3470 0.039 Uiso 1 1 calc R . . H3B H 1.2098 0.1219 0.2345 0.039 Uiso 1 1 calc R . . H3C H 1.2814 0.0941 0.3002 0.039 Uiso 1 1 calc R . . C5 C 0.7966(6) 0.09698(12) 0.3325(4) 0.0184(13) Uani 1 1 d . . . H5 H 0.8236 0.0875 0.4009 0.022 Uiso 1 1 calc R . . C4 C 0.6413(7) 0.08393(14) 0.2666(5) 0.0283(16) Uani 1 1 d . . . H4A H 0.5637 0.0861 0.3019 0.042 Uiso 1 1 calc R . . H4B H 0.6559 0.0636 0.2554 0.042 Uiso 1 1 calc R . . H4C H 0.6055 0.0938 0.2006 0.042 Uiso 1 1 calc R . . C6 C 0.7752(8) 0.12864(14) 0.3503(5) 0.0370(18) Uani 1 1 d . . . H6A H 0.7547 0.1390 0.2856 0.055 Uiso 1 1 calc R . . H6B H 0.8698 0.1361 0.4002 0.055 Uiso 1 1 calc R . . H6C H 0.6873 0.1311 0.3763 0.055 Uiso 1 1 calc R . . C7 C 0.8775(6) 0.10346(12) 0.1495(4) 0.0138(12) Uani 1 1 d . . . C8 C 0.8955(6) 0.13232(12) 0.1328(4) 0.0179(13) Uani 1 1 d . . . H8 H 0.9488 0.1440 0.1893 0.021 Uiso 1 1 calc R . . C9 C 0.8393(7) 0.14467(13) 0.0375(5) 0.0226(14) Uani 1 1 d . . . H9 H 0.8517 0.1646 0.0295 0.027 Uiso 1 1 calc R . . C10 C 0.7646(7) 0.12798(13) -0.0468(5) 0.0236(15) Uani 1 1 d . . . H10 H 0.7290 0.1362 -0.1132 0.028 Uiso 1 1 calc R . . C11 C 0.7431(6) 0.09936(12) -0.0326(4) 0.0166(13) Uani 1 1 d . . . H11 H 0.6909 0.0880 -0.0903 0.020 Uiso 1 1 calc R . . C12 C 0.7954(6) 0.08631(12) 0.0644(4) 0.0161(13) Uani 1 1 d . . . C13 C 0.7557(6) 0.05580(12) 0.0716(4) 0.0127(12) Uani 1 1 d . . . C14 C 0.6225(6) 0.04319(13) -0.0124(4) 0.0170(13) Uani 1 1 d . . . C19 C 0.6399(7) 0.01790(13) -0.0591(4) 0.0208(14) Uani 1 1 d . . . H19 H 0.7373 0.0084 -0.0384 0.025 Uiso 1 1 calc R . . C18 C 0.5160(8) 0.00620(15) -0.1364(5) 0.0326(17) Uani 1 1 d . . . H18 H 0.5285 -0.0113 -0.1680 0.039 Uiso 1 1 calc R . . C17 C 0.3751(8) 0.02016(16) -0.1666(5) 0.038(2) Uani 1 1 d . . . H17 H 0.2914 0.0126 -0.2208 0.045 Uiso 1 1 calc R . . C16 C 0.3545(7) 0.04514(16) -0.1185(5) 0.0363(19) Uani 1 1 d . . . H16 H 0.2561 0.0543 -0.1377 0.044 Uiso 1 1 calc R . . C15 C 0.4786(7) 0.05655(13) -0.0420(5) 0.0259(15) Uani 1 1 d . . . H15 H 0.4651 0.0738 -0.0093 0.031 Uiso 1 1 calc R . . C20 C 1.0405(6) -0.01517(12) 0.1564(4) 0.0173(13) Uani 1 1 d . . . H20 H 1.0292 -0.0023 0.1012 0.021 Uiso 1 1 calc R . . C21 C 1.0474(6) -0.04437(13) 0.1385(5) 0.0236(14) Uani 1 1 d . . . H21 H 1.0411 -0.0512 0.0724 0.028 Uiso 1 1 calc R . . C22 C 1.0634(6) -0.06333(13) 0.2177(5) 0.0236(15) Uani 1 1 d . . . H22 H 1.0675 -0.0834 0.2071 0.028 Uiso 1 1 calc R . . C23 C 1.0732(6) -0.05252(13) 0.3124(5) 0.0237(15) Uani 1 1 d . . . H23 H 1.0859 -0.0651 0.3687 0.028 Uiso 1 1 calc R . . C24 C 1.0644(6) -0.02331(12) 0.3249(4) 0.0181(13) Uani 1 1 d . . . H24 H 1.0694 -0.0162 0.3904 0.022 Uiso 1 1 calc R . . C29 C 1.2341(7) 0.03215(12) 0.4891(4) 0.0211(14) Uani 1 1 d . . . H29 H 1.1381 0.0296 0.5020 0.025 Uiso 1 1 calc R . . C28 C 1.3705(7) 0.02929(13) 0.5697(5) 0.0250(15) Uani 1 1 d . . . H28 H 1.3671 0.0246 0.6360 0.030 Uiso 1 1 calc R . . C27 C 1.5097(7) 0.03316(12) 0.5538(5) 0.0290(16) Uani 1 1 d . . . H27 H 1.6042 0.0317 0.6087 0.035 Uiso 1 1 calc R . . C26 C 1.5103(6) 0.03932(13) 0.4563(4) 0.0217(14) Uani 1 1 d . . . H26 H 1.6055 0.0420 0.4426 0.026 Uiso 1 1 calc R . . C25 C 1.3707(6) 0.04149(12) 0.3789(4) 0.0195(13) Uani 1 1 d . . . H25 H 1.3726 0.0454 0.3117 0.023 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 Ru2 0.0218(3) 0.0143(3) 0.0202(3) -0.0013(2) 0.0071(2) 0.0012(2) Ru1 0.0129(2) 0.0116(2) 0.0127(2) 0.0009(2) 0.00335(18) -0.0004(2) Cl4 0.0307(9) 0.0220(9) 0.0297(9) 0.0025(7) 0.0104(7) 0.0078(7) Cl3 0.0246(8) 0.0189(8) 0.0251(8) -0.0005(7) 0.0071(7) 0.0025(7) Cl2 0.0210(8) 0.0199(8) 0.0165(7) 0.0023(6) 0.0079(6) -0.0026(6) Cl1 0.0161(7) 0.0208(8) 0.0179(7) 0.0037(6) 0.0064(6) -0.0007(6) P2 0.0276(10) 0.0164(9) 0.0279(9) -0.0014(8) 0.0148(8) -0.0007(7) P1 0.0166(8) 0.0127(8) 0.0159(8) -0.0013(6) 0.0050(7) -0.0006(6) N5 0.020(3) 0.018(3) 0.022(3) -0.003(2) 0.005(2) 0.000(2) N6 0.024(3) 0.015(3) 0.022(3) 0.000(2) 0.008(2) 0.003(2) N1 0.014(2) 0.012(3) 0.019(3) -0.001(2) 0.008(2) -0.004(2) N2 0.014(2) 0.016(3) 0.018(3) 0.003(2) 0.008(2) -0.001(2) N3 0.012(2) 0.011(3) 0.016(2) -0.001(2) 0.001(2) 0.002(2) C37 0.022(3) 0.015(3) 0.028(4) -0.005(3) 0.006(3) 0.004(3) C42 0.025(4) 0.019(4) 0.031(4) -0.004(3) 0.009(3) 0.001(3) C41 0.034(4) 0.028(4) 0.030(4) -0.008(3) 0.008(3) 0.004(3) C40 0.039(4) 0.015(4) 0.045(4) -0.008(3) 0.013(4) 0.004(3) C39 0.042(4) 0.020(4) 0.049(5) 0.000(3) 0.022(4) -0.002(3) C38 0.051(5) 0.021(4) 0.036(4) -0.006(3) 0.024(4) 0.003(3) C43 0.017(3) 0.018(4) 0.029(4) -0.006(3) 0.008(3) 0.000(3) N4 0.027(3) 0.019(3) 0.019(3) -0.002(2) 0.007(2) -0.001(2) C44 0.035(4) 0.019(4) 0.029(4) -0.008(3) 0.012(3) 0.001(3) C49 0.053(5) 0.027(4) 0.027(4) -0.009(3) 0.015(4) -0.006(3) C48 0.068(6) 0.025(4) 0.045(5) -0.002(4) 0.036(4) -0.002(4) C47 0.082(7) 0.048(5) 0.022(4) 0.002(4) 0.017(4) 0.031(5) C46 0.049(5) 0.061(6) 0.025(4) -0.013(4) -0.002(4) 0.022(4) C45 0.043(5) 0.042(5) 0.040(5) -0.006(4) 0.010(4) 0.009(4) C35 0.029(4) 0.016(4) 0.046(4) -0.011(3) 0.014(3) -0.004(3) C34 0.026(4) 0.033(4) 0.040(4) -0.002(3) 0.008(3) 0.003(3) C36 0.031(4) 0.039(5) 0.052(5) -0.007(4) 0.022(4) -0.008(3) C32 0.049(5) 0.024(4) 0.037(4) -0.001(3) 0.025(4) -0.003(3) C33 0.068(5) 0.027(4) 0.043(4) -0.005(3) 0.038(4) -0.011(4) C31 0.058(5) 0.053(5) 0.029(4) 0.014(4) 0.015(4) 0.010(4) C54 0.021(3) 0.018(4) 0.024(3) -0.006(3) 0.005(3) 0.003(3) C53 0.028(4) 0.022(4) 0.020(3) 0.000(3) -0.002(3) -0.006(3) C52 0.024(4) 0.020(4) 0.032(4) 0.007(3) 0.001(3) -0.001(3) C51 0.015(3) 0.042(5) 0.028(4) 0.002(3) 0.010(3) 0.000(3) C50 0.018(3) 0.027(4) 0.023(3) 0.002(3) 0.002(3) 0.004(3) C55 0.023(4) 0.024(4) 0.030(4) -0.003(3) 0.006(3) -0.002(3) C56 0.022(3) 0.027(4) 0.024(4) 0.000(3) -0.003(3) -0.004(3) C57 0.025(4) 0.039(4) 0.020(3) -0.006(3) 0.007(3) -0.016(3) C58 0.029(4) 0.022(4) 0.027(4) -0.002(3) 0.018(3) -0.005(3) C59 0.022(3) 0.024(4) 0.025(3) 0.002(3) 0.012(3) 0.000(3) C2 0.026(3) 0.009(3) 0.028(4) -0.001(3) 0.009(3) -0.003(3) C1 0.034(4) 0.031(4) 0.017(3) -0.007(3) -0.005(3) 0.001(3) C3 0.021(3) 0.016(4) 0.037(4) -0.002(3) 0.004(3) -0.004(3) C5 0.022(3) 0.019(3) 0.016(3) -0.003(3) 0.007(3) 0.005(3) C4 0.020(3) 0.036(4) 0.032(4) 0.007(3) 0.012(3) 0.002(3) C6 0.046(4) 0.031(4) 0.038(4) -0.006(3) 0.020(4) 0.016(3) C7 0.015(3) 0.010(3) 0.016(3) 0.000(2) 0.004(3) 0.001(2) C8 0.017(3) 0.014(3) 0.020(3) -0.001(3) 0.002(3) -0.001(3) C9 0.023(3) 0.020(4) 0.029(4) 0.010(3) 0.013(3) 0.003(3) C10 0.021(3) 0.026(4) 0.022(3) 0.007(3) 0.003(3) -0.004(3) C11 0.018(3) 0.018(3) 0.015(3) 0.002(3) 0.006(3) 0.002(3) C12 0.016(3) 0.011(3) 0.021(3) 0.004(3) 0.007(3) 0.004(2) C13 0.013(3) 0.011(3) 0.014(3) -0.002(2) 0.005(2) 0.002(2) C14 0.019(3) 0.019(3) 0.012(3) 0.008(3) 0.004(2) -0.003(3) C19 0.023(3) 0.021(4) 0.016(3) 0.003(3) 0.003(3) -0.007(3) C18 0.041(4) 0.037(4) 0.020(4) -0.006(3) 0.010(3) -0.022(4) C17 0.034(4) 0.047(5) 0.021(4) 0.013(4) -0.005(3) -0.033(4) C16 0.021(3) 0.048(5) 0.028(4) 0.023(4) -0.009(3) -0.012(3) C15 0.021(3) 0.023(4) 0.032(4) 0.005(3) 0.006(3) -0.001(3) C20 0.020(3) 0.018(3) 0.016(3) 0.004(3) 0.010(3) 0.006(3) C21 0.024(3) 0.018(4) 0.031(4) -0.010(3) 0.012(3) 0.002(3) C22 0.013(3) 0.014(3) 0.040(4) -0.003(3) 0.002(3) 0.000(2) C23 0.014(3) 0.020(4) 0.033(4) 0.007(3) 0.003(3) 0.001(3) C24 0.012(3) 0.020(4) 0.022(3) 0.003(3) 0.005(3) 0.003(3) C29 0.016(3) 0.024(4) 0.024(3) 0.002(3) 0.006(3) -0.004(3) C28 0.029(4) 0.026(4) 0.019(3) 0.007(3) 0.006(3) -0.006(3) C27 0.017(3) 0.019(4) 0.039(4) 0.003(3) -0.009(3) 0.000(3) C26 0.015(3) 0.020(4) 0.029(4) 0.002(3) 0.006(3) 0.000(3) C25 0.023(3) 0.020(3) 0.018(3) -0.002(3) 0.010(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru2 N4 1.993(5) . ? Ru2 N6 2.135(5) . ? Ru2 N5 2.175(5) . ? Ru2 P2 2.2650(17) . ? Ru2 Cl4 2.4143(16) . ? Ru2 Cl3 2.4362(15) . ? Ru1 N1 1.987(4) . ? Ru1 N3 2.156(4) . ? Ru1 N2 2.194(5) . ? Ru1 P1 2.2697(16) . ? Ru1 Cl1 2.4301(14) . ? Ru1 Cl2 2.4345(14) . ? P2 C32 1.851(6) . ? P2 C37 1.852(6) . ? P2 C35 1.865(6) . ? P1 C7 1.844(5) . ? P1 C2 1.855(6) . ? P1 C5 1.873(6) . ? N5 C54 1.339(7) . ? N5 C50 1.349(7) . ? N6 C55 1.345(7) . ? N6 C59 1.355(7) . ? N1 C13 1.291(7) . ? N1 H1 0.8800 . ? N2 C20 1.340(7) . ? N2 C24 1.348(7) . ? N3 C29 1.341(7) . ? N3 C25 1.350(7) . ? C37 C38 1.387(8) . ? C37 C42 1.417(8) . ? C42 C41 1.396(8) . ? C42 C43 1.480(8) . ? C41 C40 1.379(9) . ? C41 H41 0.9500 . ? C40 C39 1.370(9) . ? C40 H40 0.9500 . ? C39 C38 1.380(9) . ? C39 H39 0.9500 . ? C38 H38 0.9500 . ? C43 N4 1.292(7) . ? C43 C44 1.501(8) . ? N4 H4 0.8800 . ? C44 C49 1.390(9) . ? C44 C45 1.399(9) . ? C49 C48 1.394(9) . ? C49 H49 0.9500 . ? C48 C47 1.368(10) . ? C48 H48 0.9500 . ? C47 C46 1.384(10) . ? C47 H47 0.9500 . ? C46 C45 1.371(10) . ? C46 H46 0.9500 . ? C45 H45 0.9500 . ? C35 C36 1.535(8) . ? C35 C34 1.537(9) . ? C35 H35 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C32 C31 1.527(9) . ? C32 C33 1.531(8) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C54 C53 1.381(8) . ? C54 H54 0.9500 . ? C53 C52 1.373(8) . ? C53 H53 0.9500 . ? C52 C51 1.379(8) . ? C52 H52 0.9500 . ? C51 C50 1.379(8) . ? C51 H51 0.9500 . ? C50 H50 0.9500 . ? C55 C56 1.386(8) . ? C55 H55 0.9500 . ? C56 C57 1.377(9) . ? C56 H56 0.9500 . ? C57 C58 1.368(8) . ? C57 H57 0.9500 . ? C58 C59 1.382(8) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C2 C1 1.520(8) . ? C2 C3 1.533(8) . ? C2 H2 1.0000 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C5 C6 1.522(8) . ? C5 C4 1.540(8) . ? C5 H5 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.386(7) . ? C7 C12 1.421(7) . ? C8 C9 1.377(8) . ? C8 H8 0.9500 . ? C9 C10 1.385(8) . ? C9 H9 0.9500 . ? C10 C11 1.375(8) . ? C10 H10 0.9500 . ? C11 C12 1.409(7) . ? C11 H11 0.9500 . ? C12 C13 1.482(7) . ? C13 C14 1.505(7) . ? C14 C19 1.379(8) . ? C14 C15 1.387(8) . ? C19 C18 1.393(8) . ? C19 H19 0.9500 . ? C18 C17 1.377(9) . ? C18 H18 0.9500 . ? C17 C16 1.384(10) . ? C17 H17 0.9500 . ? C16 C15 1.383(8) . ? C16 H16 0.9500 . ? C15 H15 0.9500 . ? C20 C21 1.392(8) . ? C20 H20 0.9500 . ? C21 C22 1.377(8) . ? C21 H21 0.9500 . ? C22 C23 1.377(8) . ? C22 H22 0.9500 . ? C23 C24 1.382(8) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C29 C28 1.384(7) . ? C29 H29 0.9500 . ? C28 C27 1.361(8) . ? C28 H28 0.9500 . ? C27 C26 1.377(8) . ? C27 H27 0.9500 . ? C26 C25 1.378(7) . ? C26 H26 0.9500 . ? C25 H25 0.9500 . ? 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 Ru2 N6 171.86(19) . . ? N4 Ru2 N5 86.89(19) . . ? N6 Ru2 N5 85.09(18) . . ? N4 Ru2 P2 85.74(15) . . ? N6 Ru2 P2 102.36(14) . . ? N5 Ru2 P2 171.68(13) . . ? N4 Ru2 Cl4 88.58(14) . . ? N6 Ru2 Cl4 92.38(13) . . ? N5 Ru2 Cl4 86.87(13) . . ? P2 Ru2 Cl4 89.10(6) . . ? N4 Ru2 Cl3 89.43(14) . . ? N6 Ru2 Cl3 88.94(13) . . ? N5 Ru2 Cl3 88.41(13) . . ? P2 Ru2 Cl3 95.37(6) . . ? Cl4 Ru2 Cl3 174.97(6) . . ? N1 Ru1 N3 172.37(17) . . ? N1 Ru1 N2 87.65(18) . . ? N3 Ru1 N2 85.11(16) . . ? N1 Ru1 P1 86.37(14) . . ? N3 Ru1 P1 100.95(12) . . ? N2 Ru1 P1 173.68(12) . . ? N1 Ru1 Cl1 90.17(13) . . ? N3 Ru1 Cl1 91.74(12) . . ? N2 Ru1 Cl1 86.16(12) . . ? P1 Ru1 Cl1 91.79(5) . . ? N1 Ru1 Cl2 85.20(13) . . ? N3 Ru1 Cl2 92.35(12) . . ? N2 Ru1 Cl2 89.70(12) . . ? P1 Ru1 Cl2 91.85(5) . . ? Cl1 Ru1 Cl2 173.92(5) . . ? C32 P2 C37 103.9(3) . . ? C32 P2 C35 102.2(3) . . ? C37 P2 C35 101.5(3) . . ? C32 P2 Ru2 119.8(2) . . ? C37 P2 Ru2 108.5(2) . . ? C35 P2 Ru2 118.7(2) . . ? C7 P1 C2 104.5(3) . . ? C7 P1 C5 100.5(3) . . ? C2 P1 C5 102.1(3) . . ? C7 P1 Ru1 109.92(18) . . ? C2 P1 Ru1 119.4(2) . . ? C5 P1 Ru1 118.03(19) . . ? C54 N5 C50 117.6(5) . . ? C54 N5 Ru2 122.3(4) . . ? C50 N5 Ru2 120.0(4) . . ? C55 N6 C59 115.7(5) . . ? C55 N6 Ru2 119.9(4) . . ? C59 N6 Ru2 123.3(4) . . ? C13 N1 Ru1 137.3(4) . . ? C13 N1 H1 111.4 . . ? Ru1 N1 H1 111.4 . . ? C20 N2 C24 117.4(5) . . ? C20 N2 Ru1 120.9(4) . . ? C24 N2 Ru1 121.4(4) . . ? C29 N3 C25 116.5(5) . . ? C29 N3 Ru1 122.0(4) . . ? C25 N3 Ru1 121.5(4) . . ? C38 C37 C42 118.0(6) . . ? C38 C37 P2 120.5(5) . . ? C42 C37 P2 121.5(5) . . ? C41 C42 C37 118.4(6) . . ? C41 C42 C43 117.5(6) . . ? C37 C42 C43 124.1(6) . . ? C40 C41 C42 122.0(6) . . ? C40 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? C39 C40 C41 119.6(6) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C40 C39 C38 119.6(6) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C38 C37 122.4(6) . . ? C39 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? N4 C43 C42 122.4(6) . . ? N4 C43 C44 118.1(6) . . ? C42 C43 C44 119.5(5) . . ? C43 N4 Ru2 138.6(4) . . ? C43 N4 H4 110.7 . . ? Ru2 N4 H4 110.7 . . ? C49 C44 C45 118.4(6) . . ? C49 C44 C43 119.9(6) . . ? C45 C44 C43 121.7(6) . . ? C44 C49 C48 120.0(7) . . ? C44 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C47 C48 C49 120.9(7) . . ? C47 C48 H48 119.6 . . ? C49 C48 H48 119.6 . . ? C48 C47 C46 119.3(7) . . ? C48 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? C45 C46 C47 120.7(7) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C46 C45 C44 120.7(7) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C36 C35 C34 109.8(5) . . ? C36 C35 P2 114.9(5) . . ? C34 C35 P2 112.2(4) . . ? C36 C35 H35 106.4 . . ? C34 C35 H35 106.4 . . ? P2 C35 H35 106.4 . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? 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 . . ? C31 C32 C33 111.4(6) . . ? C31 C32 P2 112.4(5) . . ? C33 C32 P2 110.9(5) . . ? C31 C32 H32 107.3 . . ? C33 C32 H32 107.3 . . ? P2 C32 H32 107.3 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N5 C54 C53 122.8(6) . . ? N5 C54 H54 118.6 . . ? C53 C54 H54 118.6 . . ? C52 C53 C54 118.9(6) . . ? C52 C53 H53 120.5 . . ? C54 C53 H53 120.5 . . ? C53 C52 C51 119.3(6) . . ? C53 C52 H52 120.4 . . ? C51 C52 H52 120.4 . . ? C50 C51 C52 118.6(6) . . ? C50 C51 H51 120.7 . . ? C52 C51 H51 120.7 . . ? N5 C50 C51 122.7(6) . . ? N5 C50 H50 118.6 . . ? C51 C50 H50 118.6 . . ? N6 C55 C56 123.7(6) . . ? N6 C55 H55 118.1 . . ? C56 C55 H55 118.1 . . ? C57 C56 C55 118.9(6) . . ? C57 C56 H56 120.5 . . ? C55 C56 H56 120.5 . . ? C58 C57 C56 118.9(6) . . ? C58 C57 H57 120.6 . . ? C56 C57 H57 120.6 . . ? C57 C58 C59 118.9(6) . . ? C57 C58 H58 120.5 . . ? C59 C58 H58 120.5 . . ? N6 C59 C58 123.8(6) . . ? N6 C59 H59 118.1 . . ? C58 C59 H59 118.1 . . ? C1 C2 C3 110.8(5) . . ? C1 C2 P1 110.8(4) . . ? C3 C2 P1 111.2(4) . . ? C1 C2 H2 107.9 . . ? C3 C2 H2 107.9 . . ? P1 C2 H2 107.9 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C5 C4 109.9(5) . . ? C6 C5 P1 115.6(4) . . ? C4 C5 P1 111.1(4) . . ? C6 C5 H5 106.6 . . ? C4 C5 H5 106.6 . . ? P1 C5 H5 106.6 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 118.0(5) . . ? C8 C7 P1 120.5(4) . . ? C12 C7 P1 121.5(4) . . ? C9 C8 C7 122.6(5) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C8 C9 C10 120.0(6) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 118.9(6) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 122.4(5) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C11 C12 C7 118.1(5) . . ? C11 C12 C13 117.6(5) . . ? C7 C12 C13 124.2(5) . . ? N1 C13 C12 123.6(5) . . ? N1 C13 C14 117.8(5) . . ? C12 C13 C14 118.6(5) . . ? C19 C14 C15 119.0(5) . . ? C19 C14 C13 120.8(5) . . ? C15 C14 C13 120.2(5) . . ? C14 C19 C18 120.6(6) . . ? C14 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C17 C18 C19 119.5(7) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C18 C17 C16 120.5(6) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C15 C16 C17 119.3(6) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C15 C14 121.0(6) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? N2 C20 C21 122.6(5) . . ? N2 C20 H20 118.7 . . ? C21 C20 H20 118.7 . . ? C22 C21 C20 119.4(6) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 118.3(6) . . ? C21 C22 H22 120.8 . . ? C23 C22 H22 120.8 . . ? C22 C23 C24 119.5(6) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? N2 C24 C23 122.8(6) . . ? N2 C24 H24 118.6 . . ? C23 C24 H24 118.6 . . ? N3 C29 C28 122.8(5) . . ? N3 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? C27 C28 C29 119.9(6) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C27 C26 118.4(6) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C26 C25 119.0(5) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? N3 C25 C26 123.4(5) . . ? N3 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.651 _refine_diff_density_min -0.960 _refine_diff_density_rms 0.142 #===end data_ccb092_0m _database_code_depnum_ccdc_archive 'CCDC 869897' #TrackingRef '- All-cifs-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 Cl4 N3 P Ru' _chemical_formula_weight 710.44 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 15.4539(12) _cell_length_b 18.3795(15) _cell_length_c 21.2573(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6037.8(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7019 _exptl_absorpt_correction_T_max 0.8324 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 78694 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 30.54 _reflns_number_total 9201 _reflns_number_gt 6419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0754P)^2^+19.0258P] 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 9201 _refine_ls_number_parameters 421 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _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 0.257517(19) -0.885306(15) 0.592658(13) 0.02150(9) Uani 1 1 d . . . Cl1 Cl 0.27838(8) -0.89623(6) 0.47896(4) 0.0367(2) Uani 1 1 d . . . Cl2 Cl 0.34064(7) -0.76791(5) 0.59213(5) 0.0377(2) Uani 1 1 d . . . P1 P 0.17669(6) -0.98620(5) 0.60836(4) 0.02259(19) Uani 1 1 d . . . N1 N 0.3788(2) -0.93748(19) 0.60573(16) 0.0297(7) Uani 1 1 d . . . N2 N 0.1473(2) -0.82063(17) 0.57256(16) 0.0293(7) Uani 1 1 d . . . C1 C 0.4008(3) -0.9826(2) 0.6530(2) 0.0394(10) Uani 1 1 d . . . H1 H 0.3591 -0.9912 0.6850 0.047 Uiso 1 1 calc R . . C2 C 0.4793(4) -1.0169(3) 0.6581(3) 0.0587(16) Uani 1 1 d . . . H2 H 0.4912 -1.0482 0.6926 0.070 Uiso 1 1 calc R . . C3 C 0.5411(4) -1.0048(4) 0.6117(4) 0.083(3) Uani 1 1 d . . . H3 H 0.5950 -1.0296 0.6122 0.099 Uiso 1 1 calc R . . C4 C 0.5218(4) -0.9564(5) 0.5655(3) 0.080(2) Uani 1 1 d . . . H4 H 0.5637 -0.9446 0.5344 0.096 Uiso 1 1 calc R . . C5 C 0.4414(3) -0.9247(3) 0.5639(2) 0.0520(13) Uani 1 1 d . . . H5 H 0.4295 -0.8913 0.5309 0.062 Uiso 1 1 calc R . . N3 N 0.2486(2) -0.86635(17) 0.68460(15) 0.0245(6) Uani 1 1 d . A . H6A H 0.2599 -0.8203 0.6926 0.029 Uiso 1 1 calc R . . C8 C 0.2185(3) -0.9808(2) 0.73912(18) 0.0334(9) Uani 1 1 d . A . C9 C 0.1998(3) -1.0252(2) 0.68626(17) 0.0284(8) Uani 1 1 d . . . C10 C 0.0561(3) -0.9751(2) 0.6155(2) 0.0356(9) Uani 1 1 d . . . H10 H 0.0355 -0.9524 0.5754 0.043 Uiso 1 1 calc R . . C11 C 0.0064(3) -1.0471(3) 0.6233(3) 0.0526(13) Uani 1 1 d . . . H11A H 0.0238 -1.0706 0.6627 0.079 Uiso 1 1 calc R . . H11B H 0.0196 -1.0794 0.5878 0.079 Uiso 1 1 calc R . . H11C H -0.0559 -1.0373 0.6242 0.079 Uiso 1 1 calc R . . C12 C 0.0306(3) -0.9239(3) 0.6689(3) 0.0476(12) Uani 1 1 d . . . H12A H -0.0310 -0.9118 0.6654 0.071 Uiso 1 1 calc R . . H12B H 0.0650 -0.8792 0.6661 0.071 Uiso 1 1 calc R . . H12C H 0.0415 -0.9477 0.7094 0.071 Uiso 1 1 calc R . . C13 C 0.1863(3) -1.0642(2) 0.55358(17) 0.0281(8) Uani 1 1 d . . . H13 H 0.1562 -1.1068 0.5731 0.034 Uiso 1 1 calc R . . C14 C 0.2810(3) -1.0849(2) 0.5439(2) 0.0369(10) Uani 1 1 d . . . H14A H 0.2845 -1.1297 0.5191 0.055 Uiso 1 1 calc R . . H14B H 0.3086 -1.0927 0.5849 0.055 Uiso 1 1 calc R . . H14C H 0.3109 -1.0456 0.5216 0.055 Uiso 1 1 calc R . . C15 C 0.1422(3) -1.0480(3) 0.49019(19) 0.0385(10) Uani 1 1 d . . . H15A H 0.1696 -1.0056 0.4706 0.058 Uiso 1 1 calc R . . H15B H 0.0807 -1.0379 0.4972 0.058 Uiso 1 1 calc R . . H15C H 0.1481 -1.0903 0.4624 0.058 Uiso 1 1 calc R . . C16 C 0.1980(4) -1.1006(2) 0.6949(2) 0.0445(12) Uani 1 1 d . . . H16 H 0.1863 -1.1313 0.6600 0.053 Uiso 1 1 calc R . . C17 C 0.2130(6) -1.1314(3) 0.7536(3) 0.070(2) Uani 1 1 d . . . H17 H 0.2109 -1.1827 0.7581 0.084 Uiso 1 1 calc R . . C18 C 0.2305(5) -1.0893(3) 0.8047(2) 0.071(2) Uani 1 1 d . . . H18 H 0.2412 -1.1109 0.8446 0.085 Uiso 1 1 calc R . . C19 C 0.2326(4) -1.0138(2) 0.7977(2) 0.0494(14) Uani 1 1 d . . . H19 H 0.2439 -0.9841 0.8334 0.059 Uiso 1 1 calc R . . C26 C 0.0941(3) -0.8345(3) 0.5234(2) 0.0386(10) Uani 1 1 d . . . H26 H 0.1064 -0.8755 0.4977 0.046 Uiso 1 1 calc R . . C27 C 0.0227(3) -0.7922(3) 0.5086(3) 0.0488(12) Uani 1 1 d . . . H27 H -0.0126 -0.8040 0.4734 0.059 Uiso 1 1 calc R . . C28 C 0.0036(3) -0.7326(3) 0.5457(3) 0.0521(14) Uani 1 1 d . . . H28 H -0.0458 -0.7034 0.5372 0.062 Uiso 1 1 calc R . . C29 C 0.0578(3) -0.7166(3) 0.5952(3) 0.0504(13) Uani 1 1 d . . . H29 H 0.0469 -0.6754 0.6210 0.061 Uiso 1 1 calc R . . C30 C 0.1287(3) -0.7612(2) 0.6071(2) 0.0382(10) Uani 1 1 d . . . H30 H 0.1657 -0.7491 0.6412 0.046 Uiso 1 1 calc R . . C7 C 0.2314(3) -0.9008(2) 0.73647(17) 0.0309(8) Uani 1 1 d . . . C20 C 0.2123(16) -0.8512(10) 0.7936(9) 0.033(4) Uani 0.41(2) 1 d PD A 1 C21 C 0.1284(15) -0.8368(14) 0.8147(13) 0.080(10) Uani 0.41(2) 1 d PD A 1 H21A H 0.0786 -0.8549 0.7937 0.096 Uiso 0.41(2) 1 calc PR A 1 C22 C 0.1225(17) -0.7935(14) 0.8694(14) 0.098(13) Uani 0.41(2) 1 d PD A 1 H22A H 0.0668 -0.7829 0.8858 0.117 Uiso 0.41(2) 1 calc PR A 1 C23 C 0.1927(18) -0.7666(10) 0.8996(9) 0.064(7) Uani 0.41(2) 1 d PD A 1 H23A H 0.1858 -0.7372 0.9360 0.077 Uiso 0.41(2) 1 calc PR A 1 C24 C 0.275(2) -0.7824(14) 0.8767(12) 0.066(10) Uani 0.41(2) 1 d PD A 1 H24A H 0.3246 -0.7635 0.8972 0.080 Uiso 0.41(2) 1 calc PR A 1 C25 C 0.284(2) -0.8258(19) 0.8236(14) 0.063(10) Uani 0.41(2) 1 d PD A 1 H25A H 0.3397 -0.8377 0.8083 0.075 Uiso 0.41(2) 1 calc PR A 1 C20A C 0.2398(11) -0.8630(7) 0.7979(7) 0.032(3) Uani 0.59(2) 1 d PD A 2 C23A C 0.2449(16) -0.7775(7) 0.9057(7) 0.073(6) Uani 0.59(2) 1 d PD A 2 H23B H 0.2462 -0.7488 0.9428 0.087 Uiso 0.59(2) 1 calc PR A 2 C25A C 0.3123(14) -0.8183(9) 0.8113(9) 0.054(5) Uani 0.59(2) 1 d PD A 2 H25B H 0.3607 -0.8176 0.7838 0.065 Uiso 0.59(2) 1 calc PR A 2 C22A C 0.1747(13) -0.8210(6) 0.8941(4) 0.065(4) Uani 0.59(2) 1 d PD A 2 H22B H 0.1279 -0.8231 0.9230 0.078 Uiso 0.59(2) 1 calc PR A 2 C24A C 0.3118(15) -0.7748(11) 0.8658(9) 0.070(7) Uani 0.59(2) 1 d PD A 2 H24B H 0.3592 -0.7435 0.8744 0.084 Uiso 0.59(2) 1 calc PR A 2 C21A C 0.1734(11) -0.8622(6) 0.8384(4) 0.049(3) Uani 0.59(2) 1 d PD A 2 H21B H 0.1236 -0.8905 0.8292 0.059 Uiso 0.59(2) 1 calc PR A 2 Cl4A Cl 0.4033(3) -1.1841(2) 0.7770(2) 0.1943(18) Uani 1 1 d . B 2 Cl5A Cl 0.5643(7) -1.2139(11) 0.7362(5) 0.322(9) Uani 0.50 1 d P B 2 C99A C 0.5031(10) -1.2367(7) 0.8096(7) 0.164(5) Uani 1 1 d . B 2 Cl5B Cl 0.5166(6) -1.3069(5) 0.7734(5) 0.194(4) Uani 0.50 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02843(16) 0.01765(14) 0.01841(14) 0.00167(9) 0.00514(10) 0.00087(10) Cl1 0.0549(6) 0.0360(5) 0.0192(4) 0.0039(4) 0.0075(4) 0.0034(5) Cl2 0.0452(6) 0.0251(5) 0.0429(5) -0.0009(4) 0.0170(5) -0.0103(4) P1 0.0275(5) 0.0190(4) 0.0213(4) 0.0000(3) 0.0031(3) -0.0002(3) N1 0.0294(17) 0.0275(16) 0.0323(16) -0.0082(13) 0.0028(13) 0.0004(13) N2 0.0364(18) 0.0210(15) 0.0306(16) 0.0045(12) 0.0025(13) 0.0019(13) C1 0.037(2) 0.033(2) 0.048(3) -0.0064(19) -0.0114(19) 0.0012(18) C2 0.050(3) 0.048(3) 0.077(4) -0.028(3) -0.034(3) 0.018(2) C3 0.038(3) 0.114(6) 0.096(5) -0.070(5) -0.029(3) 0.031(3) C4 0.033(3) 0.138(7) 0.070(4) -0.049(5) 0.006(3) 0.006(4) C5 0.036(3) 0.078(4) 0.043(3) -0.014(3) 0.011(2) -0.003(2) N3 0.0351(17) 0.0175(13) 0.0211(14) -0.0011(11) 0.0046(12) -0.0027(11) C8 0.057(3) 0.0219(17) 0.0214(17) 0.0003(14) 0.0083(17) -0.0020(17) C9 0.046(2) 0.0188(16) 0.0201(16) -0.0004(13) 0.0057(15) -0.0039(15) C10 0.030(2) 0.032(2) 0.045(2) -0.0042(18) 0.0080(17) -0.0030(16) C11 0.039(3) 0.044(3) 0.075(4) -0.004(3) 0.014(2) -0.011(2) C12 0.040(3) 0.040(3) 0.062(3) -0.005(2) 0.021(2) 0.000(2) C13 0.036(2) 0.0260(18) 0.0222(16) -0.0032(14) -0.0006(15) -0.0015(15) C14 0.047(3) 0.032(2) 0.032(2) -0.0107(17) 0.0051(18) 0.0089(19) C15 0.051(3) 0.037(2) 0.0273(19) -0.0057(17) -0.0101(18) -0.003(2) C16 0.089(4) 0.0194(18) 0.0252(19) 0.0012(15) 0.004(2) -0.005(2) C17 0.159(7) 0.022(2) 0.030(2) 0.0052(18) 0.008(3) 0.001(3) C18 0.162(7) 0.029(2) 0.022(2) 0.0075(18) 0.005(3) 0.004(3) C19 0.102(4) 0.027(2) 0.0191(17) -0.0004(16) 0.006(2) -0.003(2) C26 0.043(2) 0.034(2) 0.039(2) 0.0087(18) -0.0047(19) 0.0054(19) C27 0.046(3) 0.043(3) 0.057(3) 0.017(2) -0.007(2) 0.006(2) C28 0.038(3) 0.038(3) 0.080(4) 0.026(3) 0.002(2) 0.010(2) C29 0.048(3) 0.027(2) 0.077(4) 0.008(2) 0.017(3) 0.011(2) C30 0.038(2) 0.027(2) 0.050(3) 0.0042(18) 0.0061(19) 0.0053(17) C7 0.051(2) 0.0233(18) 0.0185(16) -0.0024(13) 0.0035(15) -0.0019(16) C20 0.075(13) 0.010(6) 0.015(5) 0.001(4) 0.009(7) 0.016(6) C21 0.062(12) 0.090(16) 0.088(16) -0.072(14) 0.048(11) -0.035(11) C22 0.095(17) 0.083(16) 0.11(2) -0.075(16) 0.074(16) -0.041(14) C23 0.13(2) 0.025(8) 0.038(9) -0.015(6) 0.037(11) -0.024(10) C24 0.14(3) 0.038(11) 0.024(8) -0.029(9) -0.023(13) 0.017(13) C25 0.072(17) 0.069(19) 0.047(11) -0.033(12) -0.020(10) 0.026(13) C20A 0.063(8) 0.008(4) 0.025(4) 0.002(3) -0.008(5) 0.009(4) C23A 0.160(19) 0.029(5) 0.028(5) -0.007(4) -0.029(10) 0.012(9) C25A 0.083(12) 0.024(4) 0.055(9) 0.000(5) -0.046(9) 0.004(7) C22A 0.121(13) 0.046(6) 0.029(4) -0.006(4) 0.017(6) 0.017(7) C24A 0.116(16) 0.039(6) 0.055(10) 0.010(6) -0.045(10) -0.014(8) C21A 0.074(9) 0.045(5) 0.027(4) -0.011(3) 0.010(4) -0.002(5) Cl4A 0.227(5) 0.156(3) 0.200(4) -0.018(3) -0.053(4) 0.029(3) Cl5A 0.183(9) 0.61(3) 0.171(9) -0.077(13) 0.018(8) -0.084(14) C99A 0.217(15) 0.104(9) 0.172(12) 0.017(9) 0.047(11) -0.004(9) Cl5B 0.196(8) 0.169(7) 0.217(9) -0.120(7) -0.007(7) -0.007(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 N3 1.990(3) . ? Ru1 N2 2.120(3) . ? Ru1 N1 2.124(3) . ? Ru1 P1 2.2606(10) . ? Ru1 Cl1 2.4466(10) . ? Ru1 Cl2 2.5111(10) . ? P1 C9 1.840(4) . ? P1 C13 1.853(4) . ? P1 C10 1.881(4) . ? N1 C5 1.333(6) . ? N1 C1 1.346(6) . ? N2 C30 1.348(5) . ? N2 C26 1.354(6) . ? C1 C2 1.372(7) . ? C1 H1 0.9500 . ? C2 C3 1.392(10) . ? C2 H2 0.9500 . ? C3 C4 1.357(11) . ? C3 H3 0.9500 . ? C4 C5 1.374(8) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? N3 C7 1.299(5) . ? N3 H6A 0.8800 . ? C8 C19 1.403(6) . ? C8 C9 1.419(5) . ? C8 C7 1.484(5) . ? C9 C16 1.397(5) . ? C10 C12 1.527(6) . ? C10 C11 1.538(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.526(6) . ? C13 C15 1.539(5) . ? C13 H13 1.0000 . ? 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 C17 1.388(7) . ? C16 H16 0.9500 . ? C17 C18 1.362(8) . ? C17 H17 0.9500 . ? C18 C19 1.396(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C26 C27 1.385(6) . ? C26 H26 0.9500 . ? C27 C28 1.382(8) . ? C27 H27 0.9500 . ? C28 C29 1.377(8) . ? C28 H28 0.9500 . ? C29 C30 1.391(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C7 C20A 1.485(15) . ? C7 C20 1.547(19) . ? C20 C25 1.36(3) . ? C20 C21 1.40(2) . ? C21 C22 1.411(18) . ? C21 H21A 0.9500 . ? C22 C23 1.35(3) . ? C22 H22A 0.9500 . ? C23 C24 1.39(3) . ? C23 H23A 0.9500 . ? C24 C25 1.39(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C20A C21A 1.341(18) . ? C20A C25A 1.42(2) . ? C23A C24A 1.34(2) . ? C23A C22A 1.37(2) . ? C23A H23B 0.9500 . ? C25A C24A 1.41(2) . ? C25A H25B 0.9500 . ? C22A C21A 1.404(12) . ? C22A H22B 0.9500 . ? C24A H24B 0.9500 . ? C21A H21B 0.9500 . ? Cl4A C99A 1.948(16) . ? Cl5A C99A 1.872(17) . ? Cl5A Cl5B 2.022(19) . ? C99A Cl5B 1.518(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ru1 N2 92.54(13) . . ? N3 Ru1 N1 90.66(13) . . ? N2 Ru1 N1 171.26(13) . . ? N3 Ru1 P1 87.74(9) . . ? N2 Ru1 P1 92.62(9) . . ? N1 Ru1 P1 95.63(10) . . ? N3 Ru1 Cl1 173.56(9) . . ? N2 Ru1 Cl1 87.29(10) . . ? N1 Ru1 Cl1 88.62(9) . . ? P1 Ru1 Cl1 98.70(4) . . ? N3 Ru1 Cl2 83.64(9) . . ? N2 Ru1 Cl2 85.89(10) . . ? N1 Ru1 Cl2 86.38(10) . . ? P1 Ru1 Cl2 171.17(4) . . ? Cl1 Ru1 Cl2 89.93(4) . . ? C9 P1 C13 104.38(17) . . ? C9 P1 C10 99.4(2) . . ? C13 P1 C10 102.33(19) . . ? C9 P1 Ru1 110.20(13) . . ? C13 P1 Ru1 119.85(13) . . ? C10 P1 Ru1 118.08(14) . . ? C5 N1 C1 115.0(4) . . ? C5 N1 Ru1 118.2(3) . . ? C1 N1 Ru1 126.7(3) . . ? C30 N2 C26 116.3(4) . . ? C30 N2 Ru1 121.1(3) . . ? C26 N2 Ru1 122.6(3) . . ? N1 C1 C2 124.5(5) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C1 C2 C3 118.4(6) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 117.9(5) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 C5 119.6(6) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 124.4(6) . . ? N1 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? C7 N3 Ru1 139.6(3) . . ? C7 N3 H6A 110.2 . . ? Ru1 N3 H6A 110.2 . . ? C19 C8 C9 119.1(4) . . ? C19 C8 C7 116.2(4) . . ? C9 C8 C7 124.6(3) . . ? C16 C9 C8 118.1(4) . . ? C16 C9 P1 120.1(3) . . ? C8 C9 P1 121.8(3) . . ? C12 C10 C11 108.8(4) . . ? C12 C10 P1 112.4(3) . . ? C11 C10 P1 114.2(3) . . ? C12 C10 H10 107.0 . . ? C11 C10 H10 107.0 . . ? P1 C10 H10 107.0 . . ? 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 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 110.8(3) . . ? C14 C13 P1 110.7(3) . . ? C15 C13 P1 111.4(3) . . ? C14 C13 H13 107.9 . . ? C15 C13 H13 107.9 . . ? P1 C13 H13 107.9 . . ? 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 . . ? C17 C16 C9 121.2(4) . . ? C17 C16 H16 119.4 . . ? C9 C16 H16 119.4 . . ? C18 C17 C16 121.3(4) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 118.9(4) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C18 C19 C8 121.4(4) . . ? C18 C19 H19 119.3 . . ? C8 C19 H19 119.3 . . ? N2 C26 C27 123.6(5) . . ? N2 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? C28 C27 C26 119.0(5) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C29 C28 C27 118.4(5) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? C28 C29 C30 119.5(5) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? N2 C30 C29 123.1(5) . . ? N2 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? N3 C7 C8 122.9(3) . . ? N3 C7 C20A 119.9(6) . . ? C8 C7 C20A 116.3(6) . . ? N3 C7 C20 114.7(8) . . ? C8 C7 C20 121.9(8) . . ? C20A C7 C20 18.3(8) . . ? C25 C20 C21 122.5(19) . . ? C25 C20 C7 114.6(17) . . ? C21 C20 C7 122.8(17) . . ? C20 C21 C22 115.5(17) . . ? C20 C21 H21A 122.2 . . ? C22 C21 H21A 122.2 . . ? C23 C22 C21 123.0(16) . . ? C23 C22 H22A 118.5 . . ? C21 C22 H22A 118.5 . . ? C22 C23 C24 119.3(15) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C25 C24 C23 120(2) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C20 C25 C24 120(2) . . ? C20 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C21A C20A C25A 117.9(14) . . ? C21A C20A C7 120.3(12) . . ? C25A C20A C7 121.2(14) . . ? C24A C23A C22A 121.3(13) . . ? C24A C23A H23B 119.3 . . ? C22A C23A H23B 119.3 . . ? C24A C25A C20A 119.4(18) . . ? C24A C25A H25B 120.3 . . ? C20A C25A H25B 120.3 . . ? C23A C22A C21A 118.5(12) . . ? C23A C22A H22B 120.8 . . ? C21A C22A H22B 120.8 . . ? C23A C24A C25A 120.3(17) . . ? C23A C24A H24B 119.8 . . ? C25A C24A H24B 119.8 . . ? C20A C21A C22A 122.5(13) . . ? C20A C21A H21B 118.8 . . ? C22A C21A H21B 118.8 . . ? C99A Cl5A Cl5B 45.7(6) . . ? Cl5B C99A Cl5A 72.4(9) . . ? Cl5B C99A Cl4A 110.5(10) . . ? Cl5A C99A Cl4A 89.6(8) . . ? C99A Cl5B Cl5A 61.9(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.230 _refine_diff_density_min -1.741 _refine_diff_density_rms 0.134 _vrf_PLAT213_ALERT_2_A ; PROBLEM:Check Atom C24 has ADP max/min Ratio ..... 14.4 prola RESPONSE: This is also an artifact of the disorder of the solvent and the phenyl ring ; #===end data_ccb011_0m _database_code_depnum_ccdc_archive 'CCDC 869898' #TrackingRef '- All-cifs-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C120 H107 Br3 Cl4 N2 P6 Ru2' _chemical_formula_weight 2346.57 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 17.1587(7) _cell_length_b 14.9111(6) _cell_length_c 20.5139(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.453(2) _cell_angle_gamma 90.00 _cell_volume 5177.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 1.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6701 _exptl_absorpt_correction_T_max 0.7451 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 110013 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.69 _reflns_number_total 8775 _reflns_number_gt 6840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0744P)^2^+21.1444P] 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 8775 _refine_ls_number_parameters 635 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.31306(2) 0.41342(2) 0.090292(17) 0.01315(12) Uani 1 1 d . . . P2 P 0.39642(7) 0.42357(8) 0.19608(6) 0.0156(3) Uani 1 1 d . . . Cl2 Cl 0.39781(6) 0.53249(7) 0.05266(5) 0.0155(2) Uani 1 1 d . . . P3 P 0.23524(7) 0.43725(8) -0.01641(6) 0.0164(3) Uani 1 1 d . . . Cl1 Cl 0.22276(7) 0.51060(8) 0.14041(5) 0.0187(3) Uani 1 1 d . . . C16 C 0.2803(3) 0.3807(3) -0.0803(2) 0.0198(11) Uani 1 1 d . . . N1 N 0.3855(2) 0.3319(3) 0.04952(18) 0.0159(8) Uani 1 1 d . . . H1A H 0.4034 0.3582 0.0165 0.019 Uiso 1 1 calc R . . C41 C 0.3551(3) 0.2977(3) 0.2890(2) 0.0236(11) Uani 1 1 d . . . H41A H 0.3878 0.2559 0.2712 0.028 Uiso 1 1 calc R . . C10 C 0.4611(3) 0.2128(3) 0.0109(2) 0.0198(10) Uani 1 1 d . . . C15 C 0.5195(3) 0.2643(3) -0.0105(2) 0.0225(11) Uani 1 1 d . . . H15A H 0.5304 0.3228 0.0069 0.027 Uiso 1 1 calc R . . C17 C 0.2580(3) 0.2950(4) -0.1029(2) 0.0236(11) Uani 1 1 d . . . H17A H 0.2126 0.2677 -0.0905 0.028 Uiso 1 1 calc R . . C51 C 0.3952(3) 0.6147(3) 0.1982(2) 0.0225(11) Uani 1 1 d . . . H51A H 0.3512 0.6118 0.1634 0.027 Uiso 1 1 calc R . . C39 C 0.5338(3) 0.3790(3) 0.1508(2) 0.0219(11) Uani 1 1 d . . . H39A H 0.5113 0.4143 0.1139 0.026 Uiso 1 1 calc R . . C38 C 0.6078(3) 0.3398(4) 0.1520(3) 0.0271(12) Uani 1 1 d . . . H38A H 0.6353 0.3481 0.1159 0.032 Uiso 1 1 calc R . . C29 C 0.0871(3) 0.4060(3) 0.0183(3) 0.0237(11) Uani 1 1 d . . . H29A H 0.1136 0.4161 0.0621 0.028 Uiso 1 1 calc R . . C40 C 0.3523(3) 0.3867(3) 0.2671(2) 0.0192(10) Uani 1 1 d . . . C6 C 0.4444(3) 0.0742(3) 0.1912(3) 0.0272(12) Uani 1 1 d . . . H6A H 0.4843 0.0325 0.2082 0.033 Uiso 1 1 calc R . . C50 C 0.4243(3) 0.6982(4) 0.2226(3) 0.0275(12) Uani 1 1 d . . . H50A H 0.4002 0.7516 0.2036 0.033 Uiso 1 1 calc R . . C5 C 0.3746(3) 0.0780(3) 0.2172(3) 0.0278(12) Uani 1 1 d . . . H5A H 0.3659 0.0377 0.2512 0.033 Uiso 1 1 calc R . . C26 C 0.2064(4) 0.7115(4) -0.0322(3) 0.0354(14) Uani 1 1 d . . . H26A H 0.2078 0.7614 -0.0033 0.042 Uiso 1 1 calc R . . C9 C 0.4130(3) 0.2503(3) 0.0590(2) 0.0182(10) Uani 1 1 d . . . C44 C 0.2630(3) 0.4187(4) 0.3440(3) 0.0328(13) Uani 1 1 d . . . H44A H 0.2321 0.4606 0.3636 0.039 Uiso 1 1 calc R . . C46 C 0.4304(3) 0.5371(3) 0.2246(2) 0.0199(10) Uani 1 1 d . . . C27 C 0.2248(3) 0.6259(3) -0.0061(3) 0.0259(12) Uani 1 1 d . . . H27A H 0.2383 0.6177 0.0403 0.031 Uiso 1 1 calc R . . C21 C 0.3469(3) 0.4193(4) -0.0996(2) 0.0245(11) Uani 1 1 d . . . H21A H 0.3631 0.4777 -0.0846 0.029 Uiso 1 1 calc R . . C20 C 0.3897(3) 0.3729(4) -0.1405(3) 0.0311(13) Uani 1 1 d . . . H20A H 0.4347 0.4000 -0.1538 0.037 Uiso 1 1 calc R . . C28 C 0.1297(3) 0.4059(3) -0.0335(2) 0.0197(10) Uani 1 1 d . . . C4 C 0.3185(3) 0.1402(3) 0.1936(2) 0.0237(11) Uani 1 1 d . . . H4A H 0.2711 0.1425 0.2119 0.028 Uiso 1 1 calc R . . C22 C 0.2232(3) 0.5532(3) -0.0485(2) 0.0202(11) Uani 1 1 d . . . C45 C 0.3059(3) 0.4468(4) 0.2958(2) 0.0243(11) Uani 1 1 d . . . H45A H 0.3034 0.5078 0.2822 0.029 Uiso 1 1 calc R . . C13 C 0.5457(4) 0.1455(4) -0.0825(3) 0.0327(13) Uani 1 1 d . . . H13A H 0.5747 0.1222 -0.1143 0.039 Uiso 1 1 calc R . . C11 C 0.4459(3) 0.1270(3) -0.0149(3) 0.0286(12) Uani 1 1 d . . . H11A H 0.4067 0.0907 -0.0003 0.034 Uiso 1 1 calc R . . C42 C 0.3112(3) 0.2693(4) 0.3363(3) 0.0279(12) Uani 1 1 d . . . H42A H 0.3128 0.2082 0.3497 0.033 Uiso 1 1 calc R . . C3 C 0.3283(3) 0.2009(3) 0.1431(2) 0.0196(10) Uani 1 1 d . . . C8 C 0.3981(3) 0.1940(3) 0.1150(2) 0.0196(10) Uani 1 1 d . . . C7 C 0.4556(3) 0.1313(3) 0.1404(3) 0.0244(11) Uani 1 1 d . . . H7A H 0.5031 0.1277 0.1225 0.029 Uiso 1 1 calc R . . C14 C 0.5619(3) 0.2307(4) -0.0571(3) 0.0295(13) Uani 1 1 d . . . H14A H 0.6019 0.2661 -0.0715 0.035 Uiso 1 1 calc R . . C34 C 0.4926(3) 0.3669(3) 0.2032(2) 0.0192(10) Uani 1 1 d . . . C30 C 0.0062(3) 0.3913(4) 0.0071(3) 0.0296(12) Uani 1 1 d . . . H30A H -0.0224 0.3915 0.0430 0.036 Uiso 1 1 calc R . . C12 C 0.4882(4) 0.0950(4) -0.0619(3) 0.0336(13) Uani 1 1 d . . . H12A H 0.4769 0.0369 -0.0801 0.040 Uiso 1 1 calc R . . C23 C 0.2032(3) 0.5675(4) -0.1164(3) 0.0270(12) Uani 1 1 d . . . H23A H 0.2020 0.5182 -0.1459 0.032 Uiso 1 1 calc R . . C43 C 0.2653(3) 0.3296(4) 0.3636(3) 0.0336(14) Uani 1 1 d . . . H43A H 0.2351 0.3103 0.3959 0.040 Uiso 1 1 calc R . . C25 C 0.1865(3) 0.7242(4) -0.0991(3) 0.0338(13) Uani 1 1 d . . . H25A H 0.1737 0.7826 -0.1161 0.041 Uiso 1 1 calc R . . C49 C 0.4869(3) 0.7038(4) 0.2733(3) 0.0323(13) Uani 1 1 d . . . H49A H 0.5059 0.7605 0.2899 0.039 Uiso 1 1 calc R . . C24 C 0.1850(3) 0.6523(4) -0.1415(3) 0.0316(13) Uani 1 1 d . . . H24A H 0.1714 0.6610 -0.1879 0.038 Uiso 1 1 calc R . . C32 C 0.0092(3) 0.3765(4) -0.1089(3) 0.0329(13) Uani 1 1 d . . . H32A H -0.0175 0.3667 -0.1527 0.039 Uiso 1 1 calc R . . C18 C 0.3021(3) 0.2490(4) -0.1436(3) 0.0311(13) Uani 1 1 d . . . H18A H 0.2866 0.1904 -0.1585 0.037 Uiso 1 1 calc R . . C48 C 0.5217(4) 0.6262(4) 0.2998(3) 0.0471(17) Uani 1 1 d . . . H48A H 0.5656 0.6293 0.3346 0.057 Uiso 1 1 calc R . . C47 C 0.4937(4) 0.5434(4) 0.2761(3) 0.0385(15) Uani 1 1 d . . . H47A H 0.5179 0.4903 0.2954 0.046 Uiso 1 1 calc R . . C33 C 0.0899(3) 0.3906(4) -0.0972(3) 0.0276(12) Uani 1 1 d . . . H33A H 0.1185 0.3898 -0.1331 0.033 Uiso 1 1 calc R . . C19 C 0.3672(3) 0.2876(4) -0.1621(3) 0.0350(14) Uani 1 1 d . . . H19A H 0.3970 0.2559 -0.1898 0.042 Uiso 1 1 calc R . . C31 C -0.0327(3) 0.3765(4) -0.0567(3) 0.0326(13) Uani 1 1 d . . . H31A H -0.0882 0.3664 -0.0646 0.039 Uiso 1 1 calc R . . P1 P 0.25370(7) 0.28514(9) 0.11266(6) 0.0189(3) Uani 1 1 d . . . C2 C 0.2018(3) 0.2161(4) 0.0453(3) 0.0295(12) Uani 1 1 d . . . H2A H 0.1795 0.1632 0.0637 0.044 Uiso 1 1 calc R . . H2B H 0.2389 0.1971 0.0164 0.044 Uiso 1 1 calc R . . H2C H 0.1591 0.2512 0.0196 0.044 Uiso 1 1 calc R . . C35 C 0.5285(3) 0.3185(4) 0.2582(3) 0.0283(12) Uani 1 1 d . . . H35A H 0.5027 0.3127 0.2956 0.034 Uiso 1 1 calc R . . C36 C 0.6017(3) 0.2789(4) 0.2588(3) 0.0350(14) Uani 1 1 d . . . H36A H 0.6250 0.2446 0.2959 0.042 Uiso 1 1 calc R . . C37 C 0.6409(3) 0.2892(4) 0.2056(3) 0.0365(14) Uani 1 1 d . . . H37A H 0.6907 0.2612 0.2059 0.044 Uiso 1 1 calc R . . C1 C 0.1839(3) 0.2846(4) 0.1702(3) 0.0285(12) Uani 1 1 d . . . H1B H 0.1639 0.2236 0.1740 0.043 Uiso 1 1 calc R . . H1C H 0.1397 0.3248 0.1540 0.043 Uiso 1 1 calc R . . H1D H 0.2103 0.3052 0.2136 0.043 Uiso 1 1 calc R . . Br1 Br 0.66947(7) 0.03546(8) 0.21548(5) 0.0875(3) Uani 1 1 d . . . C200 C 0.7219(4) 0.0266(4) 0.1416(3) 0.0507(18) Uani 1 1 d D . . C201 C 0.7932(4) -0.0207(5) 0.1483(4) 0.061(2) Uani 1 1 d D . . H20B H 0.8171 -0.0456 0.1894 0.073 Uiso 1 1 calc R . . C202 C 0.7226(4) 0.0556(6) 0.0256(3) 0.084(3) Uani 1 1 d D . . H20C H 0.6992 0.0813 -0.0153 0.101 Uiso 1 1 calc R . . C203 C 0.6868(4) 0.0652(5) 0.0818(3) 0.0554(19) Uani 1 1 d D . . H20D H 0.6389 0.0979 0.0794 0.067 Uiso 1 1 calc R . . C205 C 0.7934(5) 0.0076(5) 0.0305(4) 0.109(5) Uani 1 1 d D . . H20E H 0.8181 0.0000 -0.0072 0.131 Uiso 1 1 calc R . . C204 C 0.8276(5) -0.0293(6) 0.0913(4) 0.074(3) Uani 1 1 d D . . H20F H 0.8759 -0.0613 0.0939 0.089 Uiso 1 1 calc R . . C110 C 0.9692(4) 0.9854(6) 0.9447(4) 0.060(2) Uani 1 1 d . A -1 C111 C 0.9579(8) 1.0838(11) 0.9408(8) 0.053(4) Uani 0.50 1 d P A -1 C112 C 0.9843(11) 0.8865(14) 0.9538(10) 0.087(7) Uani 0.50 1 d P A -1 C113 C 1.0134(8) 0.8304(9) 0.9895(7) 0.026(3) Uiso 0.50 1 d P A -1 C114 C 0.9943(8) 1.0358(9) 0.9908(7) 0.041(3) Uani 0.50 1 d P A -1 Br5A Br 0.98080(11) 1.15667(14) 0.97011(15) 0.0807(6) Uani 0.50 1 d P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0119(2) 0.0145(2) 0.0136(2) -0.00099(15) 0.00377(14) -0.00037(15) P2 0.0150(6) 0.0174(6) 0.0144(6) 0.0007(5) 0.0023(5) -0.0005(5) Cl2 0.0157(6) 0.0138(5) 0.0169(6) 0.0012(4) 0.0029(4) -0.0019(4) P3 0.0150(6) 0.0195(6) 0.0145(6) -0.0021(5) 0.0023(5) -0.0002(5) Cl1 0.0165(6) 0.0236(6) 0.0166(6) -0.0040(5) 0.0047(5) 0.0045(5) C16 0.021(3) 0.025(3) 0.013(2) -0.002(2) 0.001(2) 0.004(2) N1 0.014(2) 0.019(2) 0.0149(19) -0.0004(16) 0.0047(16) -0.0037(16) C41 0.024(3) 0.024(3) 0.021(3) 0.002(2) -0.001(2) 0.000(2) C10 0.024(3) 0.017(2) 0.021(2) 0.004(2) 0.010(2) 0.007(2) C15 0.026(3) 0.018(2) 0.025(3) 0.001(2) 0.009(2) 0.003(2) C17 0.023(3) 0.030(3) 0.019(3) -0.002(2) 0.004(2) -0.003(2) C51 0.026(3) 0.024(3) 0.018(2) -0.005(2) 0.007(2) -0.002(2) C39 0.021(3) 0.022(3) 0.023(3) 0.000(2) 0.002(2) -0.001(2) C38 0.016(3) 0.032(3) 0.034(3) 0.002(2) 0.006(2) 0.001(2) C29 0.021(3) 0.023(3) 0.027(3) -0.001(2) 0.004(2) 0.003(2) C40 0.017(3) 0.024(3) 0.016(2) 0.002(2) 0.0005(19) -0.002(2) C6 0.035(3) 0.021(3) 0.024(3) 0.005(2) 0.002(2) 0.001(2) C50 0.037(3) 0.020(3) 0.030(3) -0.006(2) 0.018(3) 0.000(2) C5 0.042(3) 0.020(3) 0.022(3) 0.004(2) 0.008(2) -0.006(2) C26 0.040(4) 0.027(3) 0.037(3) -0.004(3) -0.002(3) 0.006(3) C9 0.020(3) 0.014(2) 0.021(2) 0.000(2) 0.007(2) -0.001(2) C44 0.030(3) 0.044(4) 0.026(3) 0.002(3) 0.010(2) 0.008(3) C46 0.020(3) 0.024(3) 0.017(2) 0.000(2) 0.006(2) -0.004(2) C27 0.028(3) 0.024(3) 0.024(3) -0.001(2) 0.000(2) 0.005(2) C21 0.025(3) 0.031(3) 0.018(3) -0.003(2) 0.005(2) -0.003(2) C20 0.028(3) 0.038(3) 0.030(3) -0.009(3) 0.011(2) -0.007(3) C28 0.015(2) 0.018(2) 0.025(3) 0.000(2) -0.002(2) 0.000(2) C4 0.030(3) 0.019(3) 0.024(3) -0.001(2) 0.011(2) -0.009(2) C22 0.013(2) 0.025(3) 0.022(3) 0.003(2) 0.002(2) 0.001(2) C45 0.029(3) 0.025(3) 0.020(3) 0.004(2) 0.007(2) 0.006(2) C13 0.043(4) 0.030(3) 0.030(3) 0.000(2) 0.021(3) 0.008(3) C11 0.040(3) 0.016(3) 0.033(3) 0.003(2) 0.016(3) 0.001(2) C42 0.027(3) 0.026(3) 0.028(3) 0.008(2) -0.002(2) -0.005(2) C3 0.024(3) 0.016(2) 0.020(2) -0.003(2) 0.006(2) -0.004(2) C8 0.024(3) 0.014(2) 0.021(3) 0.000(2) 0.006(2) -0.004(2) C7 0.027(3) 0.021(3) 0.026(3) 0.001(2) 0.008(2) 0.001(2) C14 0.031(3) 0.029(3) 0.034(3) 0.005(2) 0.018(2) 0.004(2) C34 0.019(3) 0.015(2) 0.022(3) -0.003(2) 0.000(2) -0.001(2) C30 0.021(3) 0.030(3) 0.038(3) -0.004(2) 0.008(2) -0.001(2) C12 0.048(4) 0.019(3) 0.037(3) -0.008(2) 0.017(3) 0.003(3) C23 0.033(3) 0.030(3) 0.018(3) -0.001(2) 0.001(2) 0.002(2) C43 0.029(3) 0.053(4) 0.021(3) 0.016(3) 0.010(2) 0.003(3) C25 0.031(3) 0.026(3) 0.042(3) 0.010(3) -0.002(3) 0.007(2) C49 0.029(3) 0.027(3) 0.043(3) -0.012(3) 0.012(3) -0.010(2) C24 0.027(3) 0.039(3) 0.027(3) 0.010(3) -0.002(2) 0.001(3) C32 0.023(3) 0.038(3) 0.032(3) -0.009(3) -0.013(2) 0.001(2) C18 0.034(3) 0.030(3) 0.028(3) -0.010(2) 0.003(2) 0.001(3) C48 0.041(4) 0.042(4) 0.050(4) -0.017(3) -0.017(3) -0.009(3) C47 0.039(4) 0.030(3) 0.039(3) -0.003(3) -0.016(3) -0.001(3) C33 0.026(3) 0.029(3) 0.027(3) -0.003(2) 0.003(2) 0.000(2) C19 0.034(3) 0.047(4) 0.026(3) -0.011(3) 0.010(3) 0.004(3) C31 0.018(3) 0.028(3) 0.050(4) -0.006(3) 0.002(3) -0.001(2) P1 0.0174(6) 0.0198(7) 0.0208(6) -0.0005(5) 0.0069(5) -0.0035(5) C2 0.032(3) 0.021(3) 0.034(3) -0.003(2) 0.001(2) -0.008(2) C35 0.021(3) 0.035(3) 0.028(3) 0.005(2) 0.001(2) 0.000(2) C36 0.025(3) 0.036(3) 0.043(3) 0.016(3) 0.001(3) 0.003(3) C37 0.018(3) 0.035(3) 0.055(4) 0.011(3) 0.003(3) 0.008(2) C1 0.025(3) 0.032(3) 0.032(3) 0.005(2) 0.014(2) -0.001(2) Br1 0.1032(8) 0.1103(8) 0.0559(5) 0.0164(5) 0.0338(5) 0.0175(6) C200 0.070(5) 0.044(4) 0.041(4) 0.003(3) 0.015(4) -0.014(4) C201 0.045(4) 0.054(5) 0.080(6) -0.002(4) -0.001(4) -0.005(4) C202 0.053(5) 0.105(7) 0.085(6) 0.068(6) -0.016(5) -0.039(5) C203 0.060(5) 0.050(4) 0.059(5) 0.015(4) 0.017(4) 0.002(4) C205 0.184(12) 0.041(5) 0.143(10) -0.020(6) 0.144(10) -0.026(6) C204 0.060(5) 0.069(6) 0.098(7) 0.006(5) 0.029(5) -0.005(4) C110 0.041(4) 0.088(6) 0.050(5) 0.021(4) 0.003(3) -0.011(4) C111 0.039(8) 0.061(10) 0.061(9) 0.021(8) 0.014(7) -0.007(7) C112 0.071(12) 0.091(15) 0.109(15) -0.063(13) 0.048(11) -0.063(11) C114 0.046(8) 0.033(6) 0.041(7) 0.007(6) 0.000(6) 0.003(6) Br5A 0.0547(11) 0.0581(12) 0.126(2) 0.0285(13) 0.0047(12) 0.0086(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.016(4) . ? Ru1 P1 2.2496(13) . ? Ru1 P3 2.3959(13) . ? Ru1 P2 2.3998(13) . ? Ru1 Cl1 2.4659(11) . ? Ru1 Cl2 2.4963(11) . ? P2 C40 1.833(5) . ? P2 C34 1.839(5) . ? P2 C46 1.854(5) . ? P3 C16 1.832(5) . ? P3 C28 1.847(5) . ? P3 C22 1.849(5) . ? C16 C17 1.391(7) . ? C16 C21 1.393(7) . ? N1 C9 1.307(6) . ? C41 C42 1.389(7) . ? C41 C40 1.400(7) . ? C10 C15 1.389(7) . ? C10 C11 1.392(7) . ? C10 C9 1.494(6) . ? C15 C14 1.386(7) . ? C17 C18 1.395(7) . ? C51 C46 1.375(7) . ? C51 C50 1.402(7) . ? C39 C34 1.392(7) . ? C39 C38 1.394(7) . ? C38 C37 1.376(8) . ? C29 C28 1.385(7) . ? C29 C30 1.386(7) . ? C40 C45 1.392(7) . ? C6 C7 1.382(7) . ? C6 C5 1.391(8) . ? C50 C49 1.371(8) . ? C5 C4 1.367(8) . ? C26 C25 1.371(8) . ? C26 C27 1.400(8) . ? C9 C8 1.480(7) . ? C44 C43 1.386(8) . ? C44 C45 1.391(7) . ? C46 C47 1.389(8) . ? C27 C22 1.387(7) . ? C21 C20 1.388(7) . ? C20 C19 1.380(8) . ? C28 C33 1.392(7) . ? C4 C3 1.405(7) . ? C22 C23 1.396(7) . ? C13 C12 1.362(8) . ? C13 C14 1.384(8) . ? C11 C12 1.382(7) . ? C42 C43 1.374(8) . ? C3 C8 1.415(7) . ? C3 P1 1.829(5) . ? C8 C7 1.396(7) . ? C34 C35 1.395(7) . ? C30 C31 1.385(8) . ? C23 C24 1.381(8) . ? C25 C24 1.379(8) . ? C49 C48 1.373(9) . ? C32 C33 1.382(8) . ? C32 C31 1.385(8) . ? C18 C19 1.366(8) . ? C48 C47 1.383(9) . ? P1 C1 1.814(5) . ? P1 C2 1.833(5) . ? C35 C36 1.385(8) . ? C36 C37 1.382(8) . ? Br1 C200 1.889(6) . ? C200 C201 1.3991(10) . ? C200 C203 1.3995(10) . ? C201 C204 1.3994(10) . ? C202 C205 1.3987(10) . ? C202 C203 1.4000(10) . ? C205 C204 1.3999(10) . ? C110 C114 1.229(15) . ? C110 C111 1.481(18) . ? C110 C112 1.50(2) . ? C111 Br5A 1.272(17) . ? C111 C114 1.320(19) . ? C112 C113 1.17(3) . ? C114 Br5A 1.857(12) . ? 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 P1 84.40(11) . . ? N1 Ru1 P3 89.97(11) . . ? P1 Ru1 P3 96.28(5) . . ? N1 Ru1 P2 95.55(11) . . ? P1 Ru1 P2 95.27(5) . . ? P3 Ru1 P2 167.64(4) . . ? N1 Ru1 Cl1 178.86(11) . . ? P1 Ru1 Cl1 94.48(4) . . ? P3 Ru1 Cl1 89.98(4) . . ? P2 Ru1 Cl1 84.72(4) . . ? N1 Ru1 Cl2 82.56(11) . . ? P1 Ru1 Cl2 166.94(4) . . ? P3 Ru1 Cl2 82.97(4) . . ? P2 Ru1 Cl2 86.78(4) . . ? Cl1 Ru1 Cl2 98.56(4) . . ? C40 P2 C34 106.3(2) . . ? C40 P2 C46 100.0(2) . . ? C34 P2 C46 99.4(2) . . ? C40 P2 Ru1 115.94(16) . . ? C34 P2 Ru1 115.91(16) . . ? C46 P2 Ru1 116.91(16) . . ? C16 P3 C28 105.3(2) . . ? C16 P3 C22 102.2(2) . . ? C28 P3 C22 96.9(2) . . ? C16 P3 Ru1 110.37(16) . . ? C28 P3 Ru1 121.16(16) . . ? C22 P3 Ru1 118.44(16) . . ? C17 C16 C21 118.5(5) . . ? C17 C16 P3 122.4(4) . . ? C21 C16 P3 118.4(4) . . ? C9 N1 Ru1 137.0(3) . . ? C42 C41 C40 121.3(5) . . ? C15 C10 C11 119.1(4) . . ? C15 C10 C9 120.4(4) . . ? C11 C10 C9 120.4(4) . . ? C14 C15 C10 120.4(5) . . ? C16 C17 C18 120.3(5) . . ? C46 C51 C50 119.9(5) . . ? C34 C39 C38 120.5(5) . . ? C37 C38 C39 120.0(5) . . ? C28 C29 C30 120.8(5) . . ? C45 C40 C41 117.8(5) . . ? C45 C40 P2 118.9(4) . . ? C41 C40 P2 122.9(4) . . ? C7 C6 C5 120.0(5) . . ? C49 C50 C51 120.9(5) . . ? C4 C5 C6 119.4(5) . . ? C25 C26 C27 120.8(5) . . ? N1 C9 C8 122.6(4) . . ? N1 C9 C10 118.4(4) . . ? C8 C9 C10 119.0(4) . . ? C43 C44 C45 120.1(5) . . ? C51 C46 C47 118.8(5) . . ? C51 C46 P2 123.3(4) . . ? C47 C46 P2 117.9(4) . . ? C22 C27 C26 119.5(5) . . ? C20 C21 C16 120.4(5) . . ? C19 C20 C21 120.4(5) . . ? C29 C28 C33 118.8(5) . . ? C29 C28 P3 118.6(4) . . ? C33 C28 P3 122.2(4) . . ? C5 C4 C3 122.4(5) . . ? C27 C22 C23 118.8(5) . . ? C27 C22 P3 121.2(4) . . ? C23 C22 P3 119.5(4) . . ? C44 C45 C40 120.9(5) . . ? C12 C13 C14 120.1(5) . . ? C12 C11 C10 119.8(5) . . ? C43 C42 C41 119.8(5) . . ? C4 C3 C8 117.7(5) . . ? C4 C3 P1 122.1(4) . . ? C8 C3 P1 120.2(4) . . ? C7 C8 C3 119.3(4) . . ? C7 C8 C9 118.0(4) . . ? C3 C8 C9 122.7(4) . . ? C6 C7 C8 121.1(5) . . ? C13 C14 C15 119.7(5) . . ? C39 C34 C35 118.7(5) . . ? C39 C34 P2 116.2(4) . . ? C35 C34 P2 125.0(4) . . ? C31 C30 C29 119.8(5) . . ? C13 C12 C11 120.9(5) . . ? C24 C23 C22 121.1(5) . . ? C42 C43 C44 120.1(5) . . ? C26 C25 C24 120.0(5) . . ? C50 C49 C48 119.1(5) . . ? C25 C24 C23 119.7(5) . . ? C33 C32 C31 120.0(5) . . ? C19 C18 C17 120.6(5) . . ? C49 C48 C47 120.6(6) . . ? C48 C47 C46 120.7(6) . . ? C32 C33 C28 120.7(5) . . ? C18 C19 C20 119.8(5) . . ? C30 C31 C32 119.9(5) . . ? C1 P1 C3 106.0(2) . . ? C1 P1 C2 101.3(3) . . ? C3 P1 C2 95.7(2) . . ? C1 P1 Ru1 120.38(19) . . ? C3 P1 Ru1 109.78(16) . . ? C2 P1 Ru1 120.26(18) . . ? C36 C35 C34 120.4(5) . . ? C37 C36 C35 120.3(5) . . ? C38 C37 C36 120.0(5) . . ? C201 C200 C203 122.5(6) . . ? C201 C200 Br1 118.8(4) . . ? C203 C200 Br1 118.7(4) . . ? C200 C201 C204 116.5(7) . . ? C205 C202 C203 119.1(6) . . ? C200 C203 C202 119.7(6) . . ? C202 C205 C204 119.8(7) . . ? C201 C204 C205 122.3(7) . . ? C114 C110 C111 57.4(9) . . ? C114 C110 C112 118.3(11) . . ? C111 C110 C112 175.7(12) . . ? Br5A C111 C114 91.5(12) . . ? Br5A C111 C110 142.5(12) . . ? C114 C111 C110 51.7(8) . . ? C113 C112 C110 145.7(16) . . ? C110 C114 C111 70.9(11) . . ? C110 C114 Br5A 113.8(9) . . ? C111 C114 Br5A 43.2(8) . . ? C111 Br5A C114 45.3(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.69 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.011 _refine_diff_density_min -1.841 _refine_diff_density_rms 0.120 #===end data_ccb063_0m _database_code_depnum_ccdc_archive 'CCDC 869899' #TrackingRef '- All-cifs-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H56 Cl2 N3 P Ru' _chemical_formula_weight 865.89 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 11.7266(7) _cell_length_b 19.7505(14) _cell_length_c 19.5819(14) _cell_angle_alpha 90.00 _cell_angle_beta 107.349(3) _cell_angle_gamma 90.00 _cell_volume 4329.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8966 _exptl_absorpt_correction_T_max 0.9463 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 38912 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.54 _reflns_number_total 9734 _reflns_number_gt 7315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0349P)^2^+1.1473P] 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 9734 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.002 _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 N3 N 0.10777(17) 0.60512(11) 0.29119(12) 0.0242(5) Uani 1 1 d . . . Ru1 Ru 0.343976(16) 0.667729(10) 0.289437(11) 0.01658(6) Uani 1 1 d . . . Cl2 Cl 0.26643(5) 0.71314(3) 0.17065(4) 0.02620(15) Uani 1 1 d . . . Cl1 Cl 0.41011(5) 0.60207(3) 0.39536(4) 0.02538(15) Uani 1 1 d . . . C14 C 0.7118(2) 0.60275(12) 0.37817(13) 0.0186(5) Uani 1 1 d . . . C42 C 0.1444(2) 0.89206(14) 0.33264(16) 0.0310(7) Uani 1 1 d . . . H42 H 0.1188 0.9280 0.2994 0.037 Uiso 1 1 calc R . . P1 P 0.52538(5) 0.64478(3) 0.26253(4) 0.01924(15) Uani 1 1 d . . . C15 C 0.8121(2) 0.62966(12) 0.43809(13) 0.0187(5) Uani 1 1 d . . . N1 N 0.64819(17) 0.64496(10) 0.33381(11) 0.0186(4) Uani 1 1 d . . . C46 C 0.2209(2) 0.78712(14) 0.43064(15) 0.0246(6) Uani 1 1 d . . . C21 C 0.6972(2) 0.52738(12) 0.37537(13) 0.0190(5) Uani 1 1 d . . . C10 C 0.6977(2) 0.68156(17) 0.19791(17) 0.0402(8) Uani 1 1 d . . . H10A H 0.7240 0.7137 0.1675 0.060 Uiso 1 1 calc R . . H10B H 0.6875 0.6367 0.1756 0.060 Uiso 1 1 calc R . . H10C H 0.7578 0.6792 0.2449 0.060 Uiso 1 1 calc R . . C8 C 0.5787(2) 0.70523(14) 0.20674(15) 0.0273(6) Uani 1 1 d . . . H8 H 0.5187 0.7060 0.1582 0.033 Uiso 1 1 calc R . . C31 C 0.0757(2) 0.55681(14) 0.17214(16) 0.0288(6) Uani 1 1 d . . . C13 C 0.4354(2) 0.51357(14) 0.23959(16) 0.0303(7) Uani 1 1 d . . . H13A H 0.3534 0.5297 0.2312 0.045 Uiso 1 1 calc R . . H13B H 0.4737 0.5081 0.2911 0.045 Uiso 1 1 calc R . . H13C H 0.4343 0.4699 0.2156 0.045 Uiso 1 1 calc R . . C35 C 0.1362(3) 0.38072(17) 0.1115(2) 0.0556(10) Uani 1 1 d . . . H35A H 0.0694 0.3501 0.1093 0.083 Uiso 1 1 calc R . . H35B H 0.2118 0.3565 0.1312 0.083 Uiso 1 1 calc R . . H35C H 0.1303 0.3969 0.0633 0.083 Uiso 1 1 calc R . . C44 C 0.2423(3) 0.97922(16) 0.4252(2) 0.0573(10) Uani 1 1 d . . . H44A H 0.2193 0.9894 0.4683 0.086 Uiso 1 1 calc R . . H44B H 0.2003 1.0099 0.3866 0.086 Uiso 1 1 calc R . . H44C H 0.3287 0.9853 0.4354 0.086 Uiso 1 1 calc R . . C11 C 0.5055(2) 0.56501(13) 0.20980(14) 0.0236(6) Uani 1 1 d . . . H11 H 0.5861 0.5457 0.2140 0.028 Uiso 1 1 calc R . . C47 C 0.2642(2) 0.73095(15) 0.48383(15) 0.0333(7) Uani 1 1 d . . . H47A H 0.3150 0.7498 0.5290 0.050 Uiso 1 1 calc R . . H47B H 0.3104 0.6984 0.4650 0.050 Uiso 1 1 calc R . . H47C H 0.1956 0.7080 0.4922 0.050 Uiso 1 1 calc R . . C12 C 0.4401(3) 0.57741(16) 0.13043(15) 0.0367(7) Uani 1 1 d . . . H12A H 0.4187 0.5339 0.1059 0.055 Uiso 1 1 calc R . . H12B H 0.4924 0.6025 0.1086 0.055 Uiso 1 1 calc R . . H12C H 0.3674 0.6038 0.1260 0.055 Uiso 1 1 calc R . . C1 C 0.3870(2) 0.75365(13) 0.32196(15) 0.0241(6) Uani 1 1 d . . . H1 H 0.3439 0.7869 0.2893 0.029 Uiso 1 1 calc R . . C16 C 0.8994(2) 0.58748(14) 0.48071(15) 0.0277(6) Uani 1 1 d . . . H16 H 0.8937 0.5399 0.4733 0.033 Uiso 1 1 calc R . . C30 C 0.1194(2) 0.54945(13) 0.24676(15) 0.0239(6) Uani 1 1 d . . . C29 C 0.0000(2) 0.60993(15) 0.31464(18) 0.0381(8) Uani 1 1 d . . . H29A H -0.0020 0.5734 0.3489 0.046 Uiso 1 1 calc R . . H29B H -0.0734 0.6076 0.2734 0.046 Uiso 1 1 calc R . . C9 C 0.5886(3) 0.77677(15) 0.23669(17) 0.0372(7) Uani 1 1 d . . . H9A H 0.6452 0.7773 0.2850 0.056 Uiso 1 1 calc R . . H9B H 0.5101 0.7919 0.2386 0.056 Uiso 1 1 calc R . . H9C H 0.6171 0.8072 0.2058 0.056 Uiso 1 1 calc R . . N2 N 0.12293(17) 0.70553(11) 0.33763(12) 0.0228(5) Uani 1 1 d . . . C19 C 0.9165(2) 0.72501(15) 0.50520(15) 0.0324(7) Uani 1 1 d . . . H19 H 0.9213 0.7724 0.5140 0.039 Uiso 1 1 calc R . . C45 C 0.2454(2) 0.85439(15) 0.45039(16) 0.0337(7) Uani 1 1 d . . . H45 H 0.2885 0.8644 0.4986 0.040 Uiso 1 1 calc R . . C3 C 0.4830(3) 0.85488(15) 0.38672(18) 0.0404(8) Uani 1 1 d . . . H3 H 0.4383 0.8806 0.3467 0.048 Uiso 1 1 calc R . . C40 C 0.1156(2) 0.82574(14) 0.30970(15) 0.0252(6) Uani 1 1 d . . . C33 C 0.0858(2) 0.50172(15) 0.12983(17) 0.0346(7) Uani 1 1 d . . . H33 H 0.0603 0.5067 0.0793 0.041 Uiso 1 1 calc R . . C7 C 0.5375(2) 0.74900(16) 0.44449(16) 0.0353(7) Uani 1 1 d . . . H7 H 0.5320 0.7010 0.4451 0.042 Uiso 1 1 calc R . . C34 C 0.1316(2) 0.44026(15) 0.15884(18) 0.0364(7) Uani 1 1 d . . . C6 C 0.6127(3) 0.78223(17) 0.50288(17) 0.0434(8) Uani 1 1 d . . . H6 H 0.6570 0.7570 0.5434 0.052 Uiso 1 1 calc R . . C5 C 0.6235(3) 0.85189(17) 0.50245(19) 0.0451(9) Uani 1 1 d . . . H5 H 0.6760 0.8747 0.5422 0.054 Uiso 1 1 calc R . . C38 C 0.1986(3) 0.47590(16) 0.35762(17) 0.0425(8) Uani 1 1 d . . . H38A H 0.1363 0.4503 0.3704 0.064 Uiso 1 1 calc R . . H38B H 0.2098 0.5198 0.3821 0.064 Uiso 1 1 calc R . . H38C H 0.2737 0.4504 0.3722 0.064 Uiso 1 1 calc R . . C18 C 1.0043(3) 0.68247(16) 0.54643(16) 0.0348(7) Uani 1 1 d . . . H18 H 1.0700 0.7006 0.5828 0.042 Uiso 1 1 calc R . . C4 C 0.5581(3) 0.88750(17) 0.4443(2) 0.0515(9) Uani 1 1 d . . . H4 H 0.5647 0.9354 0.4439 0.062 Uiso 1 1 calc R . . C20 C 0.8217(2) 0.69889(14) 0.45122(14) 0.0253(6) Uani 1 1 d . . . H20 H 0.7626 0.7286 0.4229 0.030 Uiso 1 1 calc R . . C43 C 0.2095(2) 0.90713(15) 0.40268(18) 0.0358(7) Uani 1 1 d . . . C37 C 0.1616(2) 0.48705(14) 0.27781(16) 0.0284(6) Uani 1 1 d . . . C32 C 0.0135(3) 0.62025(15) 0.13793(17) 0.0388(8) Uani 1 1 d . . . H32A H 0.0025 0.6188 0.0863 0.058 Uiso 1 1 calc R . . H32B H 0.0621 0.6597 0.1587 0.058 Uiso 1 1 calc R . . H32C H -0.0645 0.6235 0.1464 0.058 Uiso 1 1 calc R . . C2 C 0.4706(2) 0.78443(13) 0.38542(15) 0.0247(6) Uani 1 1 d . . . C17 C 0.9953(2) 0.61435(16) 0.53427(15) 0.0337(7) Uani 1 1 d . . . H17 H 1.0550 0.5850 0.5626 0.040 Uiso 1 1 calc R . . C36 C 0.1673(2) 0.43384(14) 0.23238(18) 0.0341(7) Uani 1 1 d . . . H36 H 0.1970 0.3913 0.2528 0.041 Uiso 1 1 calc R . . C41 C 0.0438(2) 0.81031(15) 0.23427(15) 0.0336(7) Uani 1 1 d . . . H41A H 0.0210 0.8527 0.2077 0.050 Uiso 1 1 calc R . . H41B H -0.0284 0.7853 0.2343 0.050 Uiso 1 1 calc R . . H41C H 0.0916 0.7828 0.2114 0.050 Uiso 1 1 calc R . . C39 C 0.1567(2) 0.77370(13) 0.35958(14) 0.0210(6) Uani 1 1 d . . . C27 C 0.1760(2) 0.66118(12) 0.30516(13) 0.0184(5) Uani 1 1 d . . . C28 C 0.0131(2) 0.67868(14) 0.35019(17) 0.0330(7) Uani 1 1 d . . . H28A H -0.0566 0.7079 0.3278 0.040 Uiso 1 1 calc R . . H28B H 0.0226 0.6745 0.4020 0.040 Uiso 1 1 calc R . . C26 C 0.7337(2) 0.48860(13) 0.32622(14) 0.0219(6) Uani 1 1 d . . . H26 H 0.7685 0.5101 0.2939 0.026 Uiso 1 1 calc R . . C22 C 0.6504(2) 0.49469(13) 0.42403(14) 0.0246(6) Uani 1 1 d . . . H22 H 0.6276 0.5203 0.4589 0.030 Uiso 1 1 calc R . . C25 C 0.7197(2) 0.41896(14) 0.32427(15) 0.0277(6) Uani 1 1 d . . . H25 H 0.7444 0.3929 0.2904 0.033 Uiso 1 1 calc R . . C23 C 0.6367(2) 0.42510(14) 0.42193(16) 0.0296(6) Uani 1 1 d . . . H23 H 0.6044 0.4031 0.4552 0.036 Uiso 1 1 calc R . . C24 C 0.6703(2) 0.38740(13) 0.37117(15) 0.0284(6) Uani 1 1 d . . . H24 H 0.6590 0.3397 0.3689 0.034 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 N3 0.0206(11) 0.0210(12) 0.0330(14) -0.0070(10) 0.0111(10) -0.0041(9) Ru1 0.01677(10) 0.01511(11) 0.01725(12) 0.00116(9) 0.00412(7) 0.00084(8) Cl2 0.0238(3) 0.0303(4) 0.0216(4) 0.0075(3) 0.0023(3) 0.0022(3) Cl1 0.0286(3) 0.0253(4) 0.0223(4) 0.0073(3) 0.0076(3) 0.0043(3) C14 0.0197(12) 0.0196(13) 0.0172(14) -0.0006(10) 0.0065(10) -0.0007(10) C42 0.0320(15) 0.0253(16) 0.0347(18) 0.0025(13) 0.0085(13) 0.0068(12) P1 0.0172(3) 0.0224(4) 0.0167(4) 0.0024(3) 0.0029(3) 0.0011(3) C15 0.0190(12) 0.0201(14) 0.0159(14) 0.0015(10) 0.0035(10) -0.0022(10) N1 0.0186(10) 0.0203(11) 0.0161(12) 0.0000(9) 0.0037(9) -0.0010(8) C46 0.0242(13) 0.0271(15) 0.0224(15) -0.0031(12) 0.0067(11) 0.0037(11) C21 0.0166(11) 0.0169(13) 0.0186(14) -0.0002(10) -0.0022(10) 0.0021(9) C10 0.0277(15) 0.064(2) 0.0315(19) 0.0107(16) 0.0131(13) -0.0011(14) C8 0.0207(13) 0.0393(17) 0.0198(15) 0.0100(13) 0.0027(11) -0.0013(11) C31 0.0253(13) 0.0238(15) 0.0358(18) -0.0039(13) 0.0066(12) -0.0040(11) C13 0.0278(14) 0.0312(16) 0.0304(17) -0.0090(13) 0.0062(12) -0.0017(12) C35 0.066(2) 0.039(2) 0.067(3) -0.0232(19) 0.028(2) -0.0017(17) C44 0.055(2) 0.0284(19) 0.076(3) -0.0156(18) -0.0004(19) 0.0021(16) C11 0.0184(12) 0.0317(16) 0.0192(15) -0.0049(12) 0.0032(10) 0.0046(11) C47 0.0322(15) 0.0405(18) 0.0261(17) 0.0049(14) 0.0069(13) 0.0046(13) C12 0.0402(17) 0.0426(19) 0.0216(16) -0.0088(14) 0.0005(13) 0.0054(14) C1 0.0233(13) 0.0186(14) 0.0303(16) 0.0035(12) 0.0080(11) 0.0034(10) C16 0.0277(14) 0.0276(16) 0.0240(16) 0.0017(12) 0.0020(12) -0.0027(11) C30 0.0196(12) 0.0208(14) 0.0314(17) -0.0052(12) 0.0080(11) -0.0042(10) C29 0.0296(15) 0.0333(18) 0.059(2) -0.0134(15) 0.0254(15) -0.0093(12) C9 0.0373(16) 0.0348(18) 0.0377(19) 0.0170(14) 0.0084(14) -0.0047(13) N2 0.0190(10) 0.0239(12) 0.0272(13) -0.0041(10) 0.0097(9) -0.0030(9) C19 0.0400(16) 0.0286(16) 0.0278(17) -0.0092(13) 0.0088(13) -0.0110(13) C45 0.0297(15) 0.0375(18) 0.0278(17) -0.0148(14) -0.0008(12) 0.0027(13) C3 0.0532(19) 0.0293(17) 0.0352(19) -0.0028(14) 0.0079(15) -0.0131(14) C40 0.0241(13) 0.0276(15) 0.0235(15) -0.0009(12) 0.0064(11) 0.0055(11) C33 0.0384(16) 0.0323(17) 0.0331(18) -0.0099(14) 0.0107(14) -0.0065(13) C7 0.0403(16) 0.0322(17) 0.0306(18) -0.0072(14) 0.0062(14) -0.0007(13) C34 0.0342(16) 0.0287(17) 0.049(2) -0.0158(15) 0.0166(15) -0.0074(13) C6 0.0478(19) 0.046(2) 0.0312(19) -0.0082(15) 0.0041(15) -0.0010(15) C5 0.051(2) 0.047(2) 0.039(2) -0.0208(17) 0.0154(16) -0.0226(16) C38 0.0514(19) 0.0340(18) 0.042(2) 0.0112(15) 0.0131(16) -0.0063(15) C18 0.0338(15) 0.049(2) 0.0190(16) -0.0051(13) 0.0038(12) -0.0175(14) C4 0.071(2) 0.0312(19) 0.051(2) -0.0096(17) 0.016(2) -0.0228(17) C20 0.0289(14) 0.0251(15) 0.0213(15) -0.0030(12) 0.0063(12) -0.0026(11) C43 0.0300(15) 0.0262(17) 0.047(2) -0.0085(14) 0.0045(14) 0.0015(12) C37 0.0245(13) 0.0235(15) 0.0378(18) -0.0009(13) 0.0103(12) -0.0062(11) C32 0.0385(16) 0.0286(17) 0.0388(19) -0.0011(14) -0.0046(14) -0.0039(13) C2 0.0239(13) 0.0245(15) 0.0280(16) -0.0056(12) 0.0112(12) -0.0047(11) C17 0.0274(14) 0.0439(19) 0.0229(16) 0.0079(14) -0.0030(12) -0.0007(13) C36 0.0293(15) 0.0185(15) 0.056(2) -0.0005(14) 0.0147(15) -0.0014(11) C41 0.0342(15) 0.0373(18) 0.0246(17) -0.0026(13) 0.0018(13) 0.0075(13) C39 0.0190(12) 0.0212(14) 0.0238(15) -0.0063(11) 0.0078(11) -0.0004(10) C27 0.0189(12) 0.0177(13) 0.0169(14) 0.0006(10) 0.0029(10) 0.0019(10) C28 0.0256(14) 0.0348(18) 0.045(2) -0.0096(14) 0.0201(13) -0.0074(12) C26 0.0155(11) 0.0259(15) 0.0206(15) -0.0009(11) -0.0003(10) -0.0001(10) C22 0.0304(14) 0.0217(14) 0.0199(15) 0.0034(11) 0.0049(11) 0.0045(11) C25 0.0254(13) 0.0240(15) 0.0269(16) -0.0078(12) -0.0025(12) 0.0053(11) C23 0.0326(15) 0.0237(15) 0.0293(17) 0.0092(12) 0.0041(12) 0.0011(12) C24 0.0288(14) 0.0158(14) 0.0326(17) 0.0002(12) -0.0029(12) 0.0005(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N3 C27 1.345(3) . ? N3 C30 1.433(3) . ? N3 C29 1.470(3) . ? Ru1 C1 1.830(3) . ? Ru1 C27 2.087(2) . ? Ru1 Cl1 2.3719(7) . ? Ru1 P1 2.3826(7) . ? Ru1 Cl2 2.4043(7) . ? C14 N1 1.273(3) . ? C14 C15 1.490(3) . ? C14 C21 1.498(3) . ? C42 C43 1.388(4) . ? C42 C40 1.393(4) . ? C42 H42 0.9500 . ? P1 N1 1.680(2) . ? P1 C8 1.849(3) . ? P1 C11 1.860(3) . ? C15 C16 1.389(3) . ? C15 C20 1.390(3) . ? C46 C45 1.389(4) . ? C46 C39 1.396(4) . ? C46 C47 1.503(4) . ? C21 C22 1.392(3) . ? C21 C26 1.394(3) . ? C10 C8 1.530(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C8 C9 1.521(4) . ? C8 H8 1.0000 . ? C31 C33 1.394(4) . ? C31 C30 1.404(4) . ? C31 C32 1.503(4) . ? C13 C11 1.528(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C35 C34 1.508(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C44 C43 1.506(4) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C11 C12 1.534(4) . ? C11 H11 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C1 C2 1.466(4) . ? C1 H1 0.9500 . ? C16 C17 1.394(4) . ? C16 H16 0.9500 . ? C30 C37 1.398(4) . ? C29 C28 1.513(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? N2 C27 1.340(3) . ? N2 C39 1.433(3) . ? N2 C28 1.480(3) . ? C19 C20 1.385(4) . ? C19 C18 1.386(4) . ? C19 H19 0.9500 . ? C45 C43 1.379(4) . ? C45 H45 0.9500 . ? C3 C4 1.368(4) . ? C3 C2 1.398(4) . ? C3 H3 0.9500 . ? C40 C39 1.401(4) . ? C40 C41 1.497(4) . ? C33 C34 1.379(4) . ? C33 H33 0.9500 . ? C7 C2 1.379(4) . ? C7 C6 1.383(4) . ? C7 H7 0.9500 . ? C34 C36 1.380(4) . ? C6 C5 1.382(4) . ? C6 H6 0.9500 . ? C5 C4 1.363(5) . ? C5 H5 0.9500 . ? C38 C37 1.508(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C18 C17 1.365(4) . ? C18 H18 0.9500 . ? C4 H4 0.9500 . ? C20 H20 0.9500 . ? C37 C36 1.391(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C17 H17 0.9500 . ? C36 H36 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C26 C25 1.384(4) . ? C26 H26 0.9500 . ? C22 C23 1.383(4) . ? C22 H22 0.9500 . ? C25 C24 1.373(4) . ? C25 H25 0.9500 . ? C23 C24 1.389(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? 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 C27 N3 C30 126.6(2) . . ? C27 N3 C29 113.4(2) . . ? C30 N3 C29 119.0(2) . . ? C1 Ru1 C27 100.39(10) . . ? C1 Ru1 Cl1 102.61(9) . . ? C27 Ru1 Cl1 85.06(7) . . ? C1 Ru1 P1 94.70(8) . . ? C27 Ru1 P1 164.86(7) . . ? Cl1 Ru1 P1 90.50(2) . . ? C1 Ru1 Cl2 88.64(9) . . ? C27 Ru1 Cl2 93.70(7) . . ? Cl1 Ru1 Cl2 168.73(2) . . ? P1 Ru1 Cl2 87.83(2) . . ? N1 C14 C15 117.9(2) . . ? N1 C14 C21 126.0(2) . . ? C15 C14 C21 116.0(2) . . ? C43 C42 C40 121.9(3) . . ? C43 C42 H42 119.0 . . ? C40 C42 H42 119.0 . . ? N1 P1 C8 97.61(11) . . ? N1 P1 C11 113.42(11) . . ? C8 P1 C11 103.15(13) . . ? N1 P1 Ru1 114.61(8) . . ? C8 P1 Ru1 119.30(9) . . ? C11 P1 Ru1 108.15(8) . . ? C16 C15 C20 118.3(2) . . ? C16 C15 C14 121.8(2) . . ? C20 C15 C14 119.9(2) . . ? C14 N1 P1 138.46(19) . . ? C45 C46 C39 117.7(3) . . ? C45 C46 C47 120.9(3) . . ? C39 C46 C47 121.4(2) . . ? C22 C21 C26 118.9(2) . . ? C22 C21 C14 120.0(2) . . ? C26 C21 C14 121.1(2) . . ? 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 . . ? C9 C8 C10 111.1(2) . . ? C9 C8 P1 111.88(19) . . ? C10 C8 P1 110.49(19) . . ? C9 C8 H8 107.7 . . ? C10 C8 H8 107.7 . . ? P1 C8 H8 107.7 . . ? C33 C31 C30 117.9(3) . . ? C33 C31 C32 120.1(3) . . ? C30 C31 C32 121.9(3) . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? 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 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C13 C11 C12 109.3(2) . . ? C13 C11 P1 110.12(18) . . ? C12 C11 P1 111.67(19) . . ? C13 C11 H11 108.6 . . ? C12 C11 H11 108.6 . . ? P1 C11 H11 108.6 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C2 C1 Ru1 136.5(2) . . ? C2 C1 H1 111.8 . . ? Ru1 C1 H1 111.8 . . ? C15 C16 C17 120.6(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C37 C30 C31 121.0(2) . . ? C37 C30 N3 119.9(3) . . ? C31 C30 N3 118.8(2) . . ? N3 C29 C28 102.9(2) . . ? N3 C29 H29A 111.2 . . ? C28 C29 H29A 111.2 . . ? N3 C29 H29B 111.2 . . ? C28 C29 H29B 111.2 . . ? H29A C29 H29B 109.1 . . ? 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 . . ? C27 N2 C39 129.1(2) . . ? C27 N2 C28 113.3(2) . . ? C39 N2 C28 117.6(2) . . ? C20 C19 C18 120.4(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C43 C45 C46 122.5(3) . . ? C43 C45 H45 118.7 . . ? C46 C45 H45 118.7 . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C42 C40 C39 117.7(3) . . ? C42 C40 C41 121.4(3) . . ? C39 C40 C41 120.9(2) . . ? C34 C33 C31 122.3(3) . . ? C34 C33 H33 118.9 . . ? C31 C33 H33 118.9 . . ? C2 C7 C6 121.0(3) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C33 C34 C36 118.1(3) . . ? C33 C34 C35 120.9(3) . . ? C36 C34 C35 120.9(3) . . ? C5 C6 C7 120.3(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C4 C5 C6 119.3(3) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? 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 . . ? C17 C18 C19 119.4(3) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C19 C20 C15 120.6(3) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? C45 C43 C42 118.3(3) . . ? C45 C43 C44 121.1(3) . . ? C42 C43 C44 120.6(3) . . ? C36 C37 C30 117.8(3) . . ? C36 C37 C38 119.9(3) . . ? C30 C37 C38 122.3(3) . . ? 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 . . ? C7 C2 C3 117.4(3) . . ? C7 C2 C1 124.7(3) . . ? C3 C2 C1 117.9(3) . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C34 C36 C37 122.7(3) . . ? C34 C36 H36 118.7 . . ? C37 C36 H36 118.7 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C46 C39 C40 121.8(2) . . ? C46 C39 N2 119.8(2) . . ? C40 C39 N2 118.3(2) . . ? N2 C27 N3 107.6(2) . . ? N2 C27 Ru1 128.46(18) . . ? N3 C27 Ru1 123.46(17) . . ? N2 C28 C29 102.7(2) . . ? N2 C28 H28A 111.2 . . ? C29 C28 H28A 111.2 . . ? N2 C28 H28B 111.2 . . ? C29 C28 H28B 111.2 . . ? H28A C28 H28B 109.1 . . ? C25 C26 C21 120.4(3) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C25 C26 120.2(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C22 C23 C24 119.9(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.685 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.076 #===end data_ccb057_0m _database_code_depnum_ccdc_archive 'CCDC 869900' #TrackingRef '- All-cifs-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H40 Cl2 N P2 Ru' _chemical_formula_weight 876.73 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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 12.1208(5) _cell_length_b 14.9206(6) _cell_length_c 22.2574(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4025.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1796 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6610 _exptl_absorpt_correction_T_max 0.7467 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68210 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 33.78 _reflns_number_total 16116 _reflns_number_gt 14219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0265P)^2^+0.3864P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.018(12) _refine_ls_number_reflns 16116 _refine_ls_number_parameters 500 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0640 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.887360(10) 0.538877(8) 0.904186(5) 0.01435(3) Uani 1 1 d . . . P1 P 0.69352(3) 0.54316(3) 0.928441(17) 0.01527(7) Uani 1 1 d . . . P2 P 1.07780(3) 0.53187(3) 0.878027(18) 0.01708(8) Uani 1 1 d . . . N1 N 0.92478(11) 0.53836(10) 0.99387(6) 0.0180(2) Uani 1 1 d . . . C1 C 0.92893(13) 0.46436(12) 1.02364(7) 0.0202(3) Uani 1 1 d . . . C2 C 0.90622(15) 0.38619(11) 0.98748(8) 0.0226(3) Uani 1 1 d . . . C3 C 0.90169(19) 0.29905(13) 1.00905(9) 0.0362(5) Uani 1 1 d . . . H3 H 0.9097 0.2876 1.0508 0.043 Uiso 1 1 calc R . . C4 C 0.8855(2) 0.22885(13) 0.96938(11) 0.0433(5) Uani 1 1 d . . . H4 H 0.8809 0.1690 0.9838 0.052 Uiso 1 1 calc R . . C5 C 0.87611(18) 0.24649(12) 0.90868(10) 0.0378(5) Uani 1 1 d . . . H5 H 0.8677 0.1980 0.8814 0.045 Uiso 1 1 calc R . . C6 C 0.87872(16) 0.33352(11) 0.88665(8) 0.0264(4) Uani 1 1 d . . . H6 H 0.8717 0.3438 0.8447 0.032 Uiso 1 1 calc R . . C7 C 0.89154(15) 0.40616(10) 0.92581(7) 0.0203(3) Uani 1 1 d . . . C8 C 0.96187(15) 0.46106(12) 1.08800(7) 0.0229(3) Uani 1 1 d . . . C9 C 0.88451(19) 0.45217(15) 1.13301(8) 0.0377(4) Uani 1 1 d . . . H9 H 0.8084 0.4479 1.1233 0.045 Uiso 1 1 calc R . . C10 C 0.9185(2) 0.44945(16) 1.19308(9) 0.0438(6) Uani 1 1 d . . . H10 H 0.8655 0.4451 1.2244 0.053 Uiso 1 1 calc R . . C11 C 1.0286(2) 0.45321(16) 1.20624(9) 0.0424(5) Uani 1 1 d . . . H11 H 1.0516 0.4503 1.2470 0.051 Uiso 1 1 calc R . . C12 C 1.1062(2) 0.46111(16) 1.16204(9) 0.0424(5) Uani 1 1 d . . . H12 H 1.1823 0.4634 1.1721 0.051 Uiso 1 1 calc R . . C13 C 1.07308(16) 0.46579(14) 1.10234(8) 0.0321(4) Uani 1 1 d . . . H13 H 1.1265 0.4722 1.0714 0.038 Uiso 1 1 calc R . . C14 C 0.61770(14) 0.64294(10) 0.90341(7) 0.0174(3) Uani 1 1 d . . . C15 C 0.52579(14) 0.67340(12) 0.93501(8) 0.0218(3) Uani 1 1 d . . . H15 H 0.5032 0.6433 0.9705 0.026 Uiso 1 1 calc R . . C16 C 0.46699(15) 0.74744(12) 0.91493(8) 0.0261(4) Uani 1 1 d . . . H16 H 0.4043 0.7677 0.9367 0.031 Uiso 1 1 calc R . . C17 C 0.49952(16) 0.79185(13) 0.86328(9) 0.0294(4) Uani 1 1 d . . . H17 H 0.4599 0.8430 0.8499 0.035 Uiso 1 1 calc R . . C18 C 0.59030(15) 0.76137(12) 0.83115(8) 0.0272(4) Uani 1 1 d . . . H18 H 0.6122 0.7914 0.7955 0.033 Uiso 1 1 calc R . . C19 C 0.64912(14) 0.68718(12) 0.85101(7) 0.0215(3) Uani 1 1 d . . . H19 H 0.7110 0.6665 0.8288 0.026 Uiso 1 1 calc R . . C20 C 0.60946(14) 0.45191(11) 0.89829(7) 0.0209(3) Uani 1 1 d . . . C21 C 0.63341(15) 0.36271(12) 0.91313(8) 0.0264(4) Uani 1 1 d . . . H21 H 0.6892 0.3499 0.9418 0.032 Uiso 1 1 calc R . . C22 C 0.57646(18) 0.29358(13) 0.88633(10) 0.0350(5) Uani 1 1 d . . . H22 H 0.5952 0.2334 0.8959 0.042 Uiso 1 1 calc R . . C23 C 0.4928(2) 0.31013(15) 0.84585(10) 0.0397(5) Uani 1 1 d . . . H23 H 0.4543 0.2618 0.8276 0.048 Uiso 1 1 calc R . . C24 C 0.4656(2) 0.39678(16) 0.83210(9) 0.0411(5) Uani 1 1 d . . . H24 H 0.4068 0.4086 0.8050 0.049 Uiso 1 1 calc R . . C25 C 0.52417(17) 0.46804(14) 0.85779(8) 0.0308(4) Uani 1 1 d . . . H25 H 0.5055 0.5279 0.8475 0.037 Uiso 1 1 calc R . . C26 C 0.66444(13) 0.54434(12) 1.00951(7) 0.0183(3) Uani 1 1 d . . . C27 C 0.69525(15) 0.62158(13) 1.04078(8) 0.0243(4) Uani 1 1 d . . . H27 H 0.7336 0.6680 1.0204 0.029 Uiso 1 1 calc R . . C28 C 0.67052(17) 0.63136(13) 1.10118(8) 0.0318(4) Uani 1 1 d . . . H28 H 0.6905 0.6848 1.1217 0.038 Uiso 1 1 calc R . . C29 C 0.61642(18) 0.56308(14) 1.13184(8) 0.0339(4) Uani 1 1 d . . . H29 H 0.5990 0.5698 1.1732 0.041 Uiso 1 1 calc R . . C30 C 0.58826(16) 0.48556(13) 1.10172(8) 0.0299(4) Uani 1 1 d . . . H30 H 0.5523 0.4384 1.1226 0.036 Uiso 1 1 calc R . . C31 C 0.61233(15) 0.47591(11) 1.04054(7) 0.0224(3) Uani 1 1 d . . . H31 H 0.5928 0.4222 1.0202 0.027 Uiso 1 1 calc R . . C32 C 1.13178(13) 0.61675(12) 0.82654(7) 0.0206(3) Uani 1 1 d . . . C33 C 1.24633(15) 0.62749(13) 0.82068(8) 0.0250(4) Uani 1 1 d . . . H33 H 1.2948 0.5898 0.8428 0.030 Uiso 1 1 calc R . . C34 C 1.28906(16) 0.69238(14) 0.78303(8) 0.0299(4) Uani 1 1 d . . . H34 H 1.3667 0.6984 0.7788 0.036 Uiso 1 1 calc R . . C35 C 1.22000(17) 0.74813(15) 0.75170(9) 0.0341(5) Uani 1 1 d . . . H35 H 1.2496 0.7934 0.7264 0.041 Uiso 1 1 calc R . . C36 C 1.10708(18) 0.73819(15) 0.75715(9) 0.0367(5) Uani 1 1 d . . . H36 H 1.0594 0.7767 0.7352 0.044 Uiso 1 1 calc R . . C37 C 1.06266(16) 0.67321(14) 0.79400(8) 0.0291(4) Uani 1 1 d . . . H37 H 0.9849 0.6670 0.7971 0.035 Uiso 1 1 calc R . . C38 C 1.17207(13) 0.54792(11) 0.94173(7) 0.0184(3) Uani 1 1 d . . . C39 C 1.15330(14) 0.62369(12) 0.97736(7) 0.0202(3) Uani 1 1 d . . . H39 H 1.0926 0.6618 0.9688 0.024 Uiso 1 1 calc R . . C40 C 1.22242(15) 0.64356(12) 1.02501(8) 0.0237(4) Uani 1 1 d . . . H40 H 1.2084 0.6947 1.0493 0.028 Uiso 1 1 calc R . . C41 C 1.31211(15) 0.58888(12) 1.03740(8) 0.0258(4) Uani 1 1 d . . . H41 H 1.3593 0.6021 1.0703 0.031 Uiso 1 1 calc R . . C42 C 1.33237(16) 0.51564(12) 1.00195(9) 0.0288(4) Uani 1 1 d . . . H42 H 1.3944 0.4787 1.0101 0.035 Uiso 1 1 calc R . . C43 C 1.26271(15) 0.49476(12) 0.95402(9) 0.0254(4) Uani 1 1 d . . . H43 H 1.2776 0.4438 0.9297 0.031 Uiso 1 1 calc R . . C44 C 1.12169(15) 0.42729(11) 0.84245(8) 0.0237(3) Uani 1 1 d . . . C45 C 1.13502(16) 0.42257(14) 0.78033(9) 0.0313(4) Uani 1 1 d . . . H45 H 1.1245 0.4745 0.7563 0.038 Uiso 1 1 calc R . . C46 C 1.16386(18) 0.34120(17) 0.75342(11) 0.0435(6) Uani 1 1 d . . . H46 H 1.1718 0.3382 0.7110 0.052 Uiso 1 1 calc R . . C47 C 1.18074(18) 0.26603(16) 0.78703(12) 0.0431(6) Uani 1 1 d . . . H47 H 1.2020 0.2115 0.7683 0.052 Uiso 1 1 calc R . . C48 C 1.16663(18) 0.26970(14) 0.84885(11) 0.0390(5) Uani 1 1 d . . . H48 H 1.1779 0.2174 0.8724 0.047 Uiso 1 1 calc R . . C49 C 1.13602(15) 0.34951(12) 0.87659(10) 0.0294(4) Uani 1 1 d . . . H49 H 1.1248 0.3511 0.9188 0.035 Uiso 1 1 calc R . . Cl2 Cl 0.84203(4) 0.51798(3) 0.802148(18) 0.02544(9) Uani 1 1 d . . . Cl1 Cl 0.89740(3) 0.70080(2) 0.913701(17) 0.02045(8) Uani 1 1 d . . . H100 H 0.9430(19) 0.5833(14) 1.0143(9) 0.029(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01418(5) 0.01545(5) 0.01341(5) -0.00123(4) -0.00004(4) 0.00127(5) P1 0.01424(17) 0.01635(18) 0.01522(16) -0.00050(16) 0.00024(13) -0.00026(16) P2 0.01443(17) 0.01895(19) 0.01786(18) -0.00306(16) 0.00075(14) 0.00161(16) N1 0.0174(6) 0.0185(6) 0.0179(6) 0.0007(6) -0.0003(5) -0.0001(6) C1 0.0181(7) 0.0215(8) 0.0209(7) 0.0024(7) -0.0016(6) 0.0007(7) C2 0.0233(9) 0.0176(7) 0.0269(8) 0.0020(6) -0.0045(7) 0.0015(7) C3 0.0448(13) 0.0247(9) 0.0390(10) 0.0100(8) -0.0094(10) 0.0008(10) C4 0.0531(14) 0.0158(8) 0.0610(14) 0.0053(9) -0.0105(13) 0.0007(10) C5 0.0402(12) 0.0195(8) 0.0536(12) -0.0115(9) -0.0048(11) 0.0020(8) C6 0.0252(9) 0.0224(8) 0.0314(8) -0.0086(7) 0.0002(8) 0.0013(8) C7 0.0169(7) 0.0185(7) 0.0254(7) -0.0008(6) -0.0023(7) 0.0022(7) C8 0.0285(8) 0.0203(7) 0.0199(7) 0.0036(7) -0.0041(6) 0.0007(7) C9 0.0328(10) 0.0530(13) 0.0272(9) 0.0073(9) 0.0016(8) 0.0052(12) C10 0.0529(14) 0.0538(14) 0.0249(9) 0.0083(9) 0.0067(9) 0.0094(12) C11 0.0642(15) 0.0404(12) 0.0225(9) 0.0008(9) -0.0096(9) 0.0117(12) C12 0.0421(12) 0.0504(12) 0.0346(10) 0.0014(10) -0.0191(10) -0.0012(13) C13 0.0291(9) 0.0414(11) 0.0258(9) 0.0043(9) -0.0059(7) -0.0025(9) C14 0.0150(6) 0.0179(6) 0.0193(6) -0.0016(6) -0.0019(7) 0.0000(6) C15 0.0177(8) 0.0237(8) 0.0239(8) -0.0011(7) -0.0007(6) -0.0018(7) C16 0.0182(8) 0.0278(9) 0.0322(10) -0.0057(7) -0.0027(7) 0.0048(7) C17 0.0254(10) 0.0242(9) 0.0385(10) 0.0030(8) -0.0103(8) 0.0049(8) C18 0.0247(10) 0.0298(9) 0.0271(9) 0.0084(7) -0.0057(7) 0.0014(7) C19 0.0199(8) 0.0240(8) 0.0207(7) 0.0009(6) -0.0015(6) 0.0014(7) C20 0.0202(7) 0.0225(7) 0.0202(7) -0.0036(6) 0.0033(7) -0.0041(7) C21 0.0223(9) 0.0235(8) 0.0333(10) -0.0009(7) 0.0024(7) -0.0019(6) C22 0.0367(11) 0.0214(9) 0.0470(12) -0.0051(8) 0.0100(9) -0.0069(8) C23 0.0474(13) 0.0335(11) 0.0382(11) -0.0104(9) 0.0033(10) -0.0231(10) C24 0.0481(13) 0.0417(13) 0.0336(11) -0.0009(9) -0.0157(10) -0.0170(11) C25 0.0374(10) 0.0277(10) 0.0272(9) 0.0012(8) -0.0101(7) -0.0077(9) C26 0.0155(7) 0.0219(8) 0.0174(7) 0.0005(6) 0.0001(5) -0.0003(7) C27 0.0270(9) 0.0255(9) 0.0204(8) -0.0015(7) 0.0015(7) -0.0029(8) C28 0.0389(11) 0.0343(10) 0.0222(9) -0.0063(8) -0.0009(8) 0.0017(9) C29 0.0329(10) 0.0497(12) 0.0192(8) 0.0005(7) 0.0039(8) 0.0043(10) C30 0.0268(9) 0.0381(10) 0.0247(9) 0.0084(7) 0.0053(7) -0.0011(7) C31 0.0178(7) 0.0265(8) 0.0228(7) 0.0023(6) 0.0008(7) -0.0005(8) C32 0.0172(8) 0.0252(8) 0.0193(7) -0.0028(6) 0.0031(6) -0.0007(7) C33 0.0197(8) 0.0265(9) 0.0288(9) -0.0003(7) 0.0006(7) -0.0003(7) C34 0.0214(9) 0.0407(11) 0.0276(9) -0.0025(8) 0.0042(7) -0.0067(8) C35 0.0314(11) 0.0450(12) 0.0258(10) 0.0112(8) 0.0053(8) -0.0044(9) C36 0.0277(10) 0.0527(12) 0.0297(9) 0.0196(9) 0.0034(9) 0.0016(10) C37 0.0215(9) 0.0424(11) 0.0234(9) 0.0067(8) 0.0018(7) -0.0008(8) C38 0.0149(7) 0.0184(8) 0.0217(7) -0.0008(6) -0.0005(5) -0.0001(6) C39 0.0169(7) 0.0201(8) 0.0236(8) -0.0015(6) -0.0001(6) 0.0018(7) C40 0.0214(9) 0.0237(8) 0.0260(8) -0.0029(7) -0.0029(7) -0.0025(7) C41 0.0226(9) 0.0239(9) 0.0310(9) 0.0017(7) -0.0091(7) -0.0057(7) C42 0.0207(9) 0.0209(9) 0.0449(11) 0.0035(8) -0.0118(8) 0.0024(7) C43 0.0213(9) 0.0198(8) 0.0351(10) -0.0032(7) -0.0040(7) 0.0039(7) C44 0.0165(8) 0.0236(8) 0.0309(9) -0.0097(7) 0.0021(7) 0.0024(7) C45 0.0252(10) 0.0358(10) 0.0330(10) -0.0135(8) 0.0037(8) -0.0001(8) C46 0.0298(11) 0.0560(15) 0.0447(12) -0.0299(11) 0.0065(10) 0.0005(10) C47 0.0263(10) 0.0356(12) 0.0676(16) -0.0303(11) 0.0041(10) 0.0043(9) C48 0.0258(10) 0.0246(10) 0.0667(15) -0.0136(10) 0.0006(10) 0.0042(8) C49 0.0213(9) 0.0237(9) 0.0431(11) -0.0091(8) 0.0017(8) 0.0023(7) Cl2 0.0243(2) 0.0352(2) 0.01682(17) -0.00578(15) -0.00220(15) 0.00184(18) Cl1 0.01949(18) 0.01666(16) 0.02520(18) 0.00037(13) -0.00002(16) 0.00161(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 C7 2.0384(16) . ? Ru1 N1 2.0470(13) . ? Ru1 Cl2 2.3573(4) . ? Ru1 P2 2.3828(4) . ? Ru1 P1 2.4115(4) . ? Ru1 Cl1 2.4283(4) . ? P1 C20 1.8282(17) . ? P1 C14 1.8361(15) . ? P1 C26 1.8386(15) . ? P2 C44 1.8289(16) . ? P2 C32 1.8290(18) . ? P2 C38 1.8367(16) . ? N1 C1 1.289(2) . ? N1 H100 0.84(2) . ? C1 C2 1.443(2) . ? C1 C8 1.488(2) . ? C2 C3 1.387(2) . ? C2 C7 1.416(2) . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.381(3) . ? C4 H4 0.9500 . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 C7 1.399(2) . ? C6 H6 0.9500 . ? C8 C9 1.379(3) . ? C8 C13 1.387(3) . ? C9 C10 1.400(3) . ? C9 H9 0.9500 . ? C10 C11 1.368(3) . ? C10 H10 0.9500 . ? C11 C12 1.366(3) . ? C11 H11 0.9500 . ? C12 C13 1.390(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.393(2) . ? C14 C15 1.394(2) . ? C15 C16 1.389(3) . ? C15 H15 0.9500 . ? C16 C17 1.384(3) . ? C16 H16 0.9500 . ? C17 C18 1.389(3) . ? C17 H17 0.9500 . ? C18 C19 1.389(2) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.393(2) . ? C20 C21 1.402(2) . ? C21 C22 1.377(3) . ? C21 H21 0.9500 . ? C22 C23 1.379(3) . ? C22 H22 0.9500 . ? C23 C24 1.369(3) . ? C23 H23 0.9500 . ? C24 C25 1.401(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.385(2) . ? C26 C27 1.397(2) . ? C27 C28 1.385(2) . ? C27 H27 0.9500 . ? C28 C29 1.391(3) . ? C28 H28 0.9500 . ? C29 C30 1.380(3) . ? C29 H29 0.9500 . ? C30 C31 1.400(2) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.391(3) . ? C32 C33 1.404(2) . ? C33 C34 1.381(3) . ? C33 H33 0.9500 . ? C34 C35 1.371(3) . ? C34 H34 0.9500 . ? C35 C36 1.382(3) . ? C35 H35 0.9500 . ? C36 C37 1.379(3) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C43 1.382(2) . ? C38 C39 1.400(2) . ? C39 C40 1.384(2) . ? C39 H39 0.9500 . ? C40 C41 1.387(3) . ? C40 H40 0.9500 . ? C41 C42 1.370(3) . ? C41 H41 0.9500 . ? C42 C43 1.396(3) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.394(3) . ? C44 C49 1.398(3) . ? C45 C46 1.398(3) . ? C45 H45 0.9500 . ? C46 C47 1.364(4) . ? C46 H46 0.9500 . ? C47 C48 1.388(3) . ? C47 H47 0.9500 . ? C48 C49 1.392(3) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? 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 C7 Ru1 N1 76.15(6) . . ? C7 Ru1 Cl2 96.01(5) . . ? N1 Ru1 Cl2 172.14(5) . . ? C7 Ru1 P2 89.48(5) . . ? N1 Ru1 P2 91.35(4) . . ? Cl2 Ru1 P2 89.116(15) . . ? C7 Ru1 P1 89.84(5) . . ? N1 Ru1 P1 89.87(4) . . ? Cl2 Ru1 P1 89.548(15) . . ? P2 Ru1 P1 178.429(16) . . ? C7 Ru1 Cl1 160.85(5) . . ? N1 Ru1 Cl1 84.70(5) . . ? Cl2 Ru1 Cl1 103.138(15) . . ? P2 Ru1 Cl1 90.941(15) . . ? P1 Ru1 Cl1 90.167(15) . . ? C20 P1 C14 102.33(7) . . ? C20 P1 C26 105.10(8) . . ? C14 P1 C26 101.19(7) . . ? C20 P1 Ru1 116.17(6) . . ? C14 P1 Ru1 116.18(5) . . ? C26 P1 Ru1 114.00(5) . . ? C44 P2 C32 102.44(8) . . ? C44 P2 C38 105.34(8) . . ? C32 P2 C38 99.83(8) . . ? C44 P2 Ru1 115.15(6) . . ? C32 P2 Ru1 117.99(5) . . ? C38 P2 Ru1 114.10(5) . . ? C1 N1 Ru1 120.88(12) . . ? C1 N1 H100 113.2(14) . . ? Ru1 N1 H100 125.8(14) . . ? N1 C1 C2 113.46(14) . . ? N1 C1 C8 122.26(16) . . ? C2 C1 C8 124.14(15) . . ? C3 C2 C7 121.86(16) . . ? C3 C2 C1 124.88(16) . . ? C7 C2 C1 113.23(14) . . ? C4 C3 C2 119.62(18) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 119.44(18) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.46(18) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C7 120.46(18) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C2 117.05(15) . . ? C6 C7 Ru1 127.06(13) . . ? C2 C7 Ru1 115.88(12) . . ? C9 C8 C13 119.91(16) . . ? C9 C8 C1 121.36(16) . . ? C13 C8 C1 118.73(15) . . ? C8 C9 C10 119.8(2) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 119.4(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 121.41(19) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 119.6(2) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C8 C13 C12 119.87(19) . . ? C8 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C19 C14 C15 119.11(15) . . ? C19 C14 P1 120.09(13) . . ? C15 C14 P1 120.76(13) . . ? C16 C15 C14 120.49(17) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 120.13(17) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.77(17) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C18 C19 120.25(17) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C14 120.25(16) . . ? C18 C19 H19 119.9 . . ? C14 C19 H19 119.9 . . ? C25 C20 C21 118.06(16) . . ? C25 C20 P1 121.51(13) . . ? C21 C20 P1 120.35(13) . . ? C22 C21 C20 120.36(18) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 121.18(19) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C24 C23 C22 119.49(19) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 120.2(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C20 C25 C24 120.63(19) . . ? C20 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C31 C26 C27 118.79(15) . . ? C31 C26 P1 124.73(13) . . ? C27 C26 P1 116.46(13) . . ? C28 C27 C26 120.83(17) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 120.09(18) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 119.49(17) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 120.48(17) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C26 C31 C30 120.28(16) . . ? C26 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C37 C32 C33 118.55(17) . . ? C37 C32 P2 122.00(13) . . ? C33 C32 P2 119.42(14) . . ? C34 C33 C32 120.49(18) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 120.34(18) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 119.67(19) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C37 C36 C35 120.94(19) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C36 C37 C32 120.01(18) . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C43 C38 C39 118.72(15) . . ? C43 C38 P2 124.91(13) . . ? C39 C38 P2 116.21(12) . . ? C40 C39 C38 120.60(16) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 120.06(17) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C42 C41 C40 119.69(17) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C41 C42 C43 120.65(17) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C38 C43 C42 120.26(17) . . ? C38 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C49 118.87(17) . . ? C45 C44 P2 120.42(15) . . ? C49 C44 P2 120.60(13) . . ? C44 C45 C46 119.9(2) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C47 C46 C45 121.1(2) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C48 119.54(19) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C47 C48 C49 120.4(2) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C48 C49 C44 120.1(2) . . ? C48 C49 H49 119.9 . . ? C44 C49 H49 119.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 33.78 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.572 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.069