# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email wt67751726@126.com _publ_contact_author_name 'Wang Tao' loop_ _publ_author_name 'Tao Wang' 'Xin-Qi Hao' 'Xiao-Xue Zhang' 'Jun-Fang Gong' 'Mao-Ping Song' data_a _database_code_depnum_ccdc_archive 'CCDC 800253' #TrackingRef '(CCDC-800253).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H17 Cl N2 Pd' _chemical_formula_weight 415.20 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TETRAGONAL _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 14.309(2) _cell_length_b 14.309(2) _cell_length_c 16.961(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3472.8(10) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 489 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.222 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7921 _exptl_absorpt_correction_T_max 0.8100 _exptl_absorpt_process_details SADABS(2009) _chemical_absolute_configuration r _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 R-AXIS-IV _diffrn_measurement_method 'Oscillation frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13831 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3977 _reflns_number_gt 3547 _reflns_threshold_expression >2sigma(I) _computing_data_collection raxis _computing_cell_refinement raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics texsan _computing_publication_material texsan _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^)+(0.0506P)^2^+1.5750P] 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 SHELXL _refine_ls_extinction_coef 0.0034(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.55(6) _refine_ls_number_reflns 3977 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 Pd1 Pd 0.53595(3) 0.36789(3) 0.01861(2) 0.05999(14) Uani 1 1 d . . . Cl1 Cl 0.62535(11) 0.46396(13) 0.09831(9) 0.0829(4) Uani 1 1 d . . . N1 N 0.4581(3) 0.2873(3) -0.0482(2) 0.0628(10) Uani 1 1 d . . . N2 N 0.5779(4) 0.4222(4) -0.1001(3) 0.0665(11) Uani 1 1 d . . . C1 C 0.4710(4) 0.2981(4) 0.1047(3) 0.0684(13) Uani 1 1 d . . . C2 C 0.4796(5) 0.3069(5) 0.1860(3) 0.0776(16) Uani 1 1 d . . . H2A H 0.5215 0.3497 0.2073 0.093 Uiso 1 1 calc R . . C3 C 0.4254(5) 0.2518(5) 0.2354(4) 0.0935(19) Uani 1 1 d . . . H3A H 0.4315 0.2582 0.2897 0.112 Uiso 1 1 calc R . . C4 C 0.3635(6) 0.1883(6) 0.2060(4) 0.101(2) Uani 1 1 d . . . H4A H 0.3284 0.1515 0.2402 0.122 Uiso 1 1 calc R . . C5 C 0.3527(6) 0.1787(5) 0.1254(4) 0.091(2) Uani 1 1 d . . . H5A H 0.3097 0.1361 0.1053 0.109 Uiso 1 1 calc R . . C6 C 0.4063(4) 0.2326(4) 0.0746(3) 0.0680(13) Uani 1 1 d . . . C7 C 0.3988(4) 0.2273(4) -0.0123(3) 0.0687(12) Uani 1 1 d . . . C8 C 0.3404(5) 0.1733(5) -0.0567(4) 0.093(2) Uani 1 1 d . . . H8A H 0.2989 0.1325 -0.0323 0.112 Uiso 1 1 calc R . . C9 C 0.3433(6) 0.1794(6) -0.1378(4) 0.103(2) Uani 1 1 d . . . H9A H 0.3043 0.1419 -0.1682 0.123 Uiso 1 1 calc R . . C10 C 0.4035(5) 0.2409(5) -0.1737(4) 0.0880(19) Uani 1 1 d . . . H10A H 0.4058 0.2454 -0.2284 0.106 Uiso 1 1 calc R . . C11 C 0.4601(4) 0.2953(4) -0.1277(3) 0.0665(12) Uani 1 1 d . . . C12 C 0.5246(5) 0.3674(5) -0.1602(3) 0.0849(17) Uani 1 1 d . . . H12A H 0.4884 0.4106 -0.1920 0.102 Uiso 1 1 calc R . . H12B H 0.5690 0.3367 -0.1949 0.102 Uiso 1 1 calc R . . C13 C 0.6760(4) 0.4366(4) -0.1165(3) 0.0621(13) Uani 1 1 d . . . C14 C 0.7319(5) 0.3674(7) -0.1444(3) 0.0889(18) Uani 1 1 d . . . H14A H 0.7071 0.3082 -0.1533 0.107 Uiso 1 1 calc R . . C15 C 0.8261(6) 0.3843(10) -0.1597(4) 0.124(4) Uani 1 1 d . . . H15A H 0.8631 0.3366 -0.1801 0.148 Uiso 1 1 calc R . . C16 C 0.8648(6) 0.4694(12) -0.1455(5) 0.140(5) Uani 1 1 d . . . C17 C 0.8082(6) 0.5377(9) -0.1152(4) 0.119(3) Uani 1 1 d . . . H17A H 0.8332 0.5962 -0.1040 0.143 Uiso 1 1 calc R . . C18 C 0.7142(5) 0.5210(5) -0.1008(4) 0.0846(18) Uani 1 1 d . . . H18A H 0.6771 0.5685 -0.0802 0.102 Uiso 1 1 calc R . . C19 C 0.9683(6) 0.4934(14) -0.1634(6) 0.233(8) Uani 1 1 d . . . H19A H 0.9803 0.5572 -0.1494 0.350 Uiso 1 1 calc R . . H19B H 0.9803 0.4846 -0.2186 0.350 Uiso 1 1 calc R . . H19C H 1.0083 0.4531 -0.1332 0.350 Uiso 1 1 calc R . . H2 H 0.547(5) 0.474(5) -0.100(4) 0.09(2) 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 Pd1 0.0594(2) 0.0691(3) 0.05145(19) 0.00128(17) 0.00237(18) 0.00129(18) Cl1 0.0762(9) 0.0995(11) 0.0729(8) -0.0069(8) -0.0112(7) -0.0077(8) N1 0.061(2) 0.066(3) 0.062(2) -0.002(2) 0.006(2) 0.004(2) N2 0.068(3) 0.087(4) 0.045(2) 0.003(2) 0.008(2) -0.005(2) C1 0.068(3) 0.077(4) 0.061(3) 0.013(3) 0.001(3) 0.007(3) C2 0.076(4) 0.107(5) 0.050(3) 0.018(3) 0.003(3) 0.004(3) C3 0.105(5) 0.110(5) 0.065(3) 0.023(4) 0.006(4) 0.004(4) C4 0.114(6) 0.111(6) 0.079(4) 0.033(4) 0.016(4) -0.001(5) C5 0.101(5) 0.085(4) 0.086(4) 0.020(4) 0.007(4) -0.020(4) C6 0.070(4) 0.070(4) 0.064(3) 0.007(3) 0.002(3) 0.001(3) C7 0.070(3) 0.068(3) 0.068(3) -0.002(3) 0.006(3) -0.004(2) C8 0.103(5) 0.087(4) 0.088(4) 0.000(4) -0.003(4) -0.033(4) C9 0.107(6) 0.113(6) 0.089(5) -0.018(4) -0.007(4) -0.034(4) C10 0.098(5) 0.104(5) 0.063(3) -0.020(3) -0.001(3) -0.015(4) C11 0.067(3) 0.073(3) 0.060(3) -0.007(3) 0.008(3) 0.002(3) C12 0.089(4) 0.118(5) 0.048(2) 0.000(3) -0.003(3) -0.019(4) C13 0.061(3) 0.085(4) 0.040(2) 0.008(2) 0.004(2) 0.005(3) C14 0.082(4) 0.129(6) 0.056(3) 0.002(4) -0.003(3) 0.021(4) C15 0.087(6) 0.228(12) 0.055(4) 0.007(6) 0.000(4) 0.060(7) C16 0.058(4) 0.295(16) 0.065(4) 0.032(7) -0.003(3) 0.002(7) C17 0.096(6) 0.183(9) 0.080(4) 0.021(6) -0.008(4) -0.050(7) C18 0.079(4) 0.092(5) 0.083(4) -0.001(4) 0.001(3) -0.015(4) C19 0.058(5) 0.51(3) 0.132(7) 0.042(13) 0.009(5) -0.014(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 Pd1 N1 1.964(4) . ? Pd1 C1 1.999(5) . ? Pd1 N2 2.241(5) . ? Pd1 Cl1 2.3138(16) . ? N1 C7 1.352(7) . ? N1 C11 1.353(6) . ? N2 C13 1.445(7) . ? N2 C12 1.495(8) . ? N2 H2 0.85(6) . ? C1 C2 1.390(7) . ? C1 C6 1.414(8) . ? C2 C3 1.388(9) . ? C2 H2A 0.9300 . ? C3 C4 1.363(10) . ? C3 H3A 0.9300 . ? C4 C5 1.384(9) . ? C4 H4A 0.9300 . ? C5 C6 1.387(8) . ? C5 H5A 0.9300 . ? C6 C7 1.479(8) . ? C7 C8 1.365(8) . ? C8 C9 1.380(10) . ? C8 H8A 0.9300 . ? C9 C10 1.374(10) . ? C9 H9A 0.9300 . ? C10 C11 1.369(8) . ? C10 H10A 0.9300 . ? C11 C12 1.490(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.352(8) . ? C13 C14 1.358(9) . ? C14 C15 1.395(12) . ? C14 H14A 0.9300 . ? C15 C16 1.359(16) . ? C15 H15A 0.9300 . ? C16 C17 1.369(16) . ? C16 C19 1.550(12) . ? C17 C18 1.388(10) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 C1 82.2(2) . . ? N1 Pd1 N2 80.61(18) . . ? C1 Pd1 N2 162.7(2) . . ? N1 Pd1 Cl1 179.00(14) . . ? C1 Pd1 Cl1 97.28(18) . . ? N2 Pd1 Cl1 99.84(15) . . ? C7 N1 C11 121.1(5) . . ? C7 N1 Pd1 117.9(3) . . ? C11 N1 Pd1 120.9(4) . . ? C13 N2 C12 116.1(5) . . ? C13 N2 Pd1 118.9(3) . . ? C12 N2 Pd1 107.1(3) . . ? C13 N2 H2 112(5) . . ? C12 N2 H2 101(5) . . ? Pd1 N2 H2 99(5) . . ? C2 C1 C6 118.5(5) . . ? C2 C1 Pd1 129.7(5) . . ? C6 C1 Pd1 111.8(4) . . ? C3 C2 C1 119.8(6) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C4 C3 C2 121.5(6) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 120.0(6) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 119.8(7) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C5 C6 C1 120.4(5) . . ? C5 C6 C7 123.4(6) . . ? C1 C6 C7 116.2(5) . . ? N1 C7 C8 119.7(5) . . ? N1 C7 C6 111.8(5) . . ? C8 C7 C6 128.5(6) . . ? C7 C8 C9 119.8(6) . . ? C7 C8 H8A 120.1 . . ? C9 C8 H8A 120.1 . . ? C10 C9 C8 120.1(6) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C11 C10 C9 118.8(6) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? N1 C11 C10 120.5(5) . . ? N1 C11 C12 116.2(5) . . ? C10 C11 C12 123.3(5) . . ? C11 C12 N2 115.2(4) . . ? C11 C12 H12A 108.5 . . ? N2 C12 H12A 108.5 . . ? C11 C12 H12B 108.5 . . ? N2 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C18 C13 C14 118.8(6) . . ? C18 C13 N2 118.9(6) . . ? C14 C13 N2 122.3(6) . . ? C13 C14 C15 120.5(9) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C16 C15 C14 121.1(9) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C15 C16 C17 117.7(8) . . ? C15 C16 C19 123.5(13) . . ? C17 C16 C19 118.7(14) . . ? C16 C17 C18 121.1(10) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C13 C18 C17 120.7(8) . . ? C13 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pd1 N1 C7 1.4(4) . . . . ? N2 Pd1 N1 C7 -176.5(5) . . . . ? Cl1 Pd1 N1 C7 -59(8) . . . . ? C1 Pd1 N1 C11 177.8(5) . . . . ? N2 Pd1 N1 C11 -0.1(5) . . . . ? Cl1 Pd1 N1 C11 117(8) . . . . ? N1 Pd1 N2 C13 -134.2(5) . . . . ? C1 Pd1 N2 C13 -141.0(8) . . . . ? Cl1 Pd1 N2 C13 46.7(5) . . . . ? N1 Pd1 N2 C12 -0.2(4) . . . . ? C1 Pd1 N2 C12 -7.0(11) . . . . ? Cl1 Pd1 N2 C12 -179.3(4) . . . . ? N1 Pd1 C1 C2 -179.3(7) . . . . ? N2 Pd1 C1 C2 -172.5(7) . . . . ? Cl1 Pd1 C1 C2 -0.1(7) . . . . ? N1 Pd1 C1 C6 -0.9(4) . . . . ? N2 Pd1 C1 C6 5.9(11) . . . . ? Cl1 Pd1 C1 C6 178.3(4) . . . . ? C6 C1 C2 C3 0.3(10) . . . . ? Pd1 C1 C2 C3 178.6(6) . . . . ? C1 C2 C3 C4 0.1(12) . . . . ? C2 C3 C4 C5 -0.8(13) . . . . ? C3 C4 C5 C6 1.1(13) . . . . ? C4 C5 C6 C1 -0.7(11) . . . . ? C4 C5 C6 C7 -179.5(7) . . . . ? C2 C1 C6 C5 0.0(10) . . . . ? Pd1 C1 C6 C5 -178.6(6) . . . . ? C2 C1 C6 C7 178.9(6) . . . . ? Pd1 C1 C6 C7 0.3(8) . . . . ? C11 N1 C7 C8 0.5(9) . . . . ? Pd1 N1 C7 C8 176.9(5) . . . . ? C11 N1 C7 C6 -178.0(5) . . . . ? Pd1 N1 C7 C6 -1.6(7) . . . . ? C5 C6 C7 N1 179.6(6) . . . . ? C1 C6 C7 N1 0.8(9) . . . . ? C5 C6 C7 C8 1.3(13) . . . . ? C1 C6 C7 C8 -177.6(7) . . . . ? N1 C7 C8 C9 0.9(12) . . . . ? C6 C7 C8 C9 179.1(8) . . . . ? C7 C8 C9 C10 -1.1(14) . . . . ? C8 C9 C10 C11 0.0(13) . . . . ? C7 N1 C11 C10 -1.6(10) . . . . ? Pd1 N1 C11 C10 -177.9(5) . . . . ? C7 N1 C11 C12 176.8(6) . . . . ? Pd1 N1 C11 C12 0.4(8) . . . . ? C9 C10 C11 N1 1.3(11) . . . . ? C9 C10 C11 C12 -176.9(8) . . . . ? N1 C11 C12 N2 -0.6(9) . . . . ? C10 C11 C12 N2 177.7(7) . . . . ? C13 N2 C12 C11 136.0(6) . . . . ? Pd1 N2 C12 C11 0.5(7) . . . . ? C12 N2 C13 C18 139.3(6) . . . . ? Pd1 N2 C13 C18 -90.6(6) . . . . ? C12 N2 C13 C14 -43.2(7) . . . . ? Pd1 N2 C13 C14 86.9(6) . . . . ? C18 C13 C14 C15 -2.7(9) . . . . ? N2 C13 C14 C15 179.7(6) . . . . ? C13 C14 C15 C16 1.6(11) . . . . ? C14 C15 C16 C17 0.3(13) . . . . ? C14 C15 C16 C19 -178.3(7) . . . . ? C15 C16 C17 C18 -1.1(12) . . . . ? C19 C16 C17 C18 177.6(8) . . . . ? C14 C13 C18 C17 1.9(9) . . . . ? N2 C13 C18 C17 179.5(6) . . . . ? C16 C17 C18 C13 0.0(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 Cl1 0.85(6) 2.48(6) 3.334(6) 178(7) 7 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.328 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.067 data_20101124b _database_code_depnum_ccdc_archive 'CCDC 804174' #TrackingRef '(CCDC-804174).cif' _audit_creation_date 2011-04-11 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H39 Cl N2 P2 Ru, C H2 Cl2' _chemical_formula_sum 'C41 H41 Cl3 N2 P2 Ru' _chemical_formula_weight 831.12 _chemical_melting_point ? _chemical_oxdiff_formula 'C11 H10 S O2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.1716(3) _cell_length_b 11.2294(6) _cell_length_c 19.1796(9) _cell_angle_alpha 104.722(4) _cell_angle_beta 90.241(4) _cell_angle_gamma 95.615(4) _cell_volume 1900.46(15) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8792 _cell_measurement_temperature 292.15 _cell_measurement_theta_max 29.1044 _cell_measurement_theta_min 3.0599 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.84763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 852 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_unetI/netI 0.0428 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 15657 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 3.07 _diffrn_ambient_temperature 292.15 _diffrn_detector_area_resol_mean 16.2312 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -7.00 90.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 77.0000 90.0000 97 #__ type_ start__ end____ width___ exp.time_ 2 omega -9.00 31.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 77.0000 -150.0000 40 #__ type_ start__ end____ width___ exp.time_ 3 omega -52.00 39.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 -37.0000 -180.0000 91 #__ type_ start__ end____ width___ exp.time_ 4 omega -1.00 63.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 -123.0000 -32.0000 64 #__ type_ start__ end____ width___ exp.time_ 5 omega -46.00 50.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 -77.0000 -30.0000 96 #__ type_ start__ end____ width___ exp.time_ 6 omega -53.00 2.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 -37.0000 60.0000 55 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0002190000 _diffrn_orient_matrix_UB_12 -0.0627373000 _diffrn_orient_matrix_UB_13 0.0009036000 _diffrn_orient_matrix_UB_21 -0.0776934000 _diffrn_orient_matrix_UB_22 -0.0062333000 _diffrn_orient_matrix_UB_23 0.0002298000 _diffrn_orient_matrix_UB_31 -0.0028100000 _diffrn_orient_matrix_UB_32 -0.0183166000 _diffrn_orient_matrix_UB_33 -0.0382433000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6396 _reflns_number_total 7742 _reflns_odcompleteness_completeness 99.68 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 0.667 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.072 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 457 _refine_ls_number_reflns 7742 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0404 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+1.0643P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.0976 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1566(3) 0.5472(3) 0.69213(16) 0.0335(7) Uani 1 1 d . . . C2 C 1.2881(4) 0.6126(3) 0.72522(18) 0.0404(7) Uani 1 1 d . . . H2 H 1.2887 0.6515 0.7742 0.049 Uiso 1 1 calc R . . C3 C 1.4164(4) 0.6220(3) 0.6885(2) 0.0501(9) Uani 1 1 d . . . H3 H 1.4998 0.6676 0.7128 0.060 Uiso 1 1 calc R . . C4 C 1.4219(4) 0.5645(4) 0.6161(2) 0.0565(10) Uani 1 1 d . . . H4 H 1.5083 0.5712 0.5916 0.068 Uiso 1 1 calc R . . C5 C 1.2977(4) 0.4970(3) 0.58071(19) 0.0502(9) Uani 1 1 d . . . H5 H 1.3007 0.4572 0.5320 0.060 Uiso 1 1 calc R . . C6 C 1.1670(4) 0.4875(3) 0.61726(16) 0.0378(7) Uani 1 1 d . . . C7 C 1.0337(4) 0.4148(3) 0.58122(16) 0.0384(7) Uani 1 1 d . . . C8 C 1.0133(5) 0.3527(3) 0.50878(18) 0.0531(10) Uani 1 1 d . . . H8 H 1.0905 0.3526 0.4775 0.064 Uiso 1 1 calc R . . C9 C 0.8795(6) 0.2918(4) 0.4837(2) 0.0648(12) Uani 1 1 d . . . H9 H 0.8658 0.2506 0.4351 0.078 Uiso 1 1 calc R . . C10 C 0.7649(5) 0.2911(3) 0.5298(2) 0.0598(11) Uani 1 1 d . . . H10 H 0.6736 0.2501 0.5128 0.072 Uiso 1 1 calc R . . C11 C 0.7882(4) 0.3527(3) 0.60200(18) 0.0448(8) Uani 1 1 d . . . C12 C 0.6744(4) 0.3572(4) 0.6587(2) 0.0536(9) Uani 1 1 d . . . H12A H 0.5778 0.3545 0.6372 0.064 Uiso 1 1 calc R . . H12B H 0.6760 0.2859 0.6784 0.064 Uiso 1 1 calc R . . C13 C 1.0740(4) 0.2385(3) 0.69774(16) 0.0373(7) Uani 1 1 d . . . C14 C 1.2134(4) 0.2412(3) 0.66934(19) 0.0486(9) Uani 1 1 d . . . H14 H 1.2826 0.3080 0.6885 0.058 Uiso 1 1 calc R . . C15 C 1.2504(5) 0.1464(4) 0.6133(2) 0.0669(12) Uani 1 1 d . . . H15 H 1.3444 0.1492 0.5954 0.080 Uiso 1 1 calc R . . C16 C 1.1492(6) 0.0477(4) 0.5838(2) 0.0797(14) Uani 1 1 d . . . H16 H 1.1742 -0.0159 0.5457 0.096 Uiso 1 1 calc R . . C17 C 1.0115(6) 0.0434(4) 0.6106(2) 0.0795(14) Uani 1 1 d . . . H17 H 0.9433 -0.0240 0.5912 0.095 Uiso 1 1 calc R . . C18 C 0.9730(4) 0.1386(4) 0.6666(2) 0.0578(10) Uani 1 1 d . . . H18 H 0.8782 0.1357 0.6835 0.069 Uiso 1 1 calc R . . C19 C 0.8989(3) 0.2887(3) 0.82276(16) 0.0364(7) Uani 1 1 d . . . C20 C 0.9328(4) 0.1829(3) 0.84161(19) 0.0503(9) Uani 1 1 d . . . H20 H 1.0208 0.1506 0.8276 0.060 Uiso 1 1 calc R . . C21 C 0.8369(5) 0.1253(4) 0.8809(2) 0.0591(11) Uani 1 1 d . . . H21 H 0.8620 0.0555 0.8940 0.071 Uiso 1 1 calc R . . C22 C 0.7042(5) 0.1699(4) 0.90116(19) 0.0595(11) Uani 1 1 d . . . H22 H 0.6395 0.1296 0.9269 0.071 Uiso 1 1 calc R . . C23 C 0.6689(4) 0.2737(4) 0.88292(19) 0.0530(9) Uani 1 1 d . . . H23 H 0.5798 0.3044 0.8963 0.064 Uiso 1 1 calc R . . C24 C 0.7658(4) 0.3335(3) 0.84446(17) 0.0417(8) Uani 1 1 d . . . H24 H 0.7413 0.4048 0.8330 0.050 Uiso 1 1 calc R . . C25 C 1.1982(3) 0.3921(3) 0.82607(17) 0.0398(7) Uani 1 1 d . . . H25A H 1.2336 0.3116 0.8200 0.048 Uiso 1 1 calc R . . H25B H 1.2701 0.4415 0.8055 0.048 Uiso 1 1 calc R . . C26 C 1.1972(4) 0.4520(3) 0.90672(17) 0.0465(8) Uani 1 1 d . . . H26A H 1.1218 0.4063 0.9277 0.056 Uiso 1 1 calc R . . H26B H 1.2906 0.4439 0.9280 0.056 Uiso 1 1 calc R . . C27 C 1.1707(4) 0.5880(3) 0.92766(19) 0.0478(8) Uani 1 1 d . . . H27A H 1.2284 0.6302 0.8972 0.057 Uiso 1 1 calc R . . H27B H 1.2058 0.6238 0.9770 0.057 Uiso 1 1 calc R . . C28 C 1.0106(4) 0.6127(3) 0.92156(16) 0.0383(7) Uani 1 1 d . . . H28A H 0.9893 0.6763 0.9639 0.046 Uiso 1 1 calc R . . H28B H 0.9487 0.5379 0.9222 0.046 Uiso 1 1 calc R . . C29 C 0.7788(3) 0.7140(3) 0.86847(16) 0.0340(7) Uani 1 1 d . . . C30 C 0.6926(4) 0.6659(3) 0.91634(19) 0.0469(8) Uani 1 1 d . . . H30 H 0.7269 0.6062 0.9363 0.056 Uiso 1 1 calc R . . C31 C 0.5558(4) 0.7060(4) 0.9348(2) 0.0604(11) Uani 1 1 d . . . H31 H 0.4994 0.6723 0.9666 0.073 Uiso 1 1 calc R . . C32 C 0.5036(4) 0.7943(4) 0.9066(2) 0.0547(10) Uani 1 1 d . . . H32 H 0.4131 0.8222 0.9200 0.066 Uiso 1 1 calc R . . C33 C 0.5864(4) 0.8415(3) 0.8582(2) 0.0492(9) Uani 1 1 d . . . H33 H 0.5506 0.9001 0.8379 0.059 Uiso 1 1 calc R . . C34 C 0.7227(4) 0.8020(3) 0.83952(17) 0.0417(8) Uani 1 1 d . . . H34 H 0.7776 0.8351 0.8070 0.050 Uiso 1 1 calc R . . C35 C 1.0714(3) 0.8134(3) 0.85711(17) 0.0362(7) Uani 1 1 d . . . C36 C 1.1030(4) 0.8885(3) 0.92658(19) 0.0454(8) Uani 1 1 d . . . H36 H 1.0639 0.8636 0.9659 0.055 Uiso 1 1 calc R . . C37 C 1.1912(4) 0.9989(3) 0.9380(2) 0.0583(10) Uani 1 1 d . . . H37 H 1.2117 1.0473 0.9847 0.070 Uiso 1 1 calc R . . C38 C 1.2490(4) 1.0376(3) 0.8803(3) 0.0625(11) Uani 1 1 d . . . H38 H 1.3102 1.1111 0.8879 0.075 Uiso 1 1 calc R . . C39 C 1.2157(4) 0.9669(4) 0.8115(2) 0.0590(11) Uani 1 1 d . . . H39 H 1.2524 0.9942 0.7725 0.071 Uiso 1 1 calc R . . C40 C 1.1273(4) 0.8544(3) 0.7991(2) 0.0467(8) Uani 1 1 d . . . H40 H 1.1059 0.8071 0.7522 0.056 Uiso 1 1 calc R . . C41 C 0.5793(9) -0.1036(6) 0.6478(3) 0.137(3) Uani 1 1 d D . . H41A H 0.6641 -0.1467 0.6522 0.165 Uiso 1 1 calc R A 1 H41B H 0.4919 -0.1595 0.6482 0.165 Uiso 1 1 calc R A 1 Cl1 Cl 0.86733(10) 0.68527(8) 0.67238(4) 0.0450(2) Uani 1 1 d . . . Cl2 Cl 0.5792(6) 0.0292(4) 0.72086(19) 0.1055(9) Uani 0.728(5) 1 d PD B 1 Cl3 Cl 0.5840(3) -0.0590(4) 0.56685(13) 0.1204(11) Uani 0.728(5) 1 d PD B 1 N1 N 0.9203(3) 0.4112(2) 0.62578(13) 0.0347(6) Uani 1 1 d . . . N2 N 0.7042(3) 0.4719(3) 0.71703(17) 0.0460(7) Uani 1 1 d . . . P1 P 1.02551(8) 0.36919(7) 0.77066(4) 0.03063(17) Uani 1 1 d . . . P2 P 0.96005(8) 0.66169(7) 0.84073(4) 0.03030(17) Uani 1 1 d . . . Ru1 Ru 0.94857(3) 0.52334(2) 0.729439(12) 0.02906(8) Uani 1 1 d . . . Cl3A Cl 0.6295(10) -0.1362(11) 0.5593(4) 0.1204(11) Uani 0.272(5) 1 d PD B 2 Cl2A Cl 0.570(2) 0.0454(13) 0.7014(6) 0.1055(9) Uani 0.272(5) 1 d PD B 2 H2A H 0.680(4) 0.538(3) 0.7000(18) 0.044(10) Uiso 1 1 d . . . H2B H 0.650(5) 0.474(4) 0.751(2) 0.071(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0380(17) 0.0325(16) 0.0336(16) 0.0126(13) 0.0062(13) 0.0095(13) C2 0.0375(18) 0.0403(18) 0.0448(18) 0.0110(15) 0.0073(14) 0.0101(14) C3 0.0333(18) 0.054(2) 0.067(2) 0.0216(19) 0.0083(17) 0.0071(16) C4 0.042(2) 0.067(3) 0.068(3) 0.028(2) 0.0237(19) 0.0153(19) C5 0.061(2) 0.055(2) 0.0404(19) 0.0167(17) 0.0202(18) 0.0225(19) C6 0.0453(19) 0.0388(18) 0.0339(16) 0.0143(14) 0.0083(14) 0.0132(14) C7 0.054(2) 0.0352(17) 0.0299(16) 0.0124(13) 0.0069(14) 0.0138(15) C8 0.081(3) 0.047(2) 0.0315(18) 0.0059(16) 0.0061(18) 0.015(2) C9 0.107(4) 0.051(2) 0.0318(19) 0.0017(17) -0.010(2) 0.008(2) C10 0.075(3) 0.047(2) 0.050(2) 0.0044(18) -0.024(2) -0.002(2) C11 0.054(2) 0.0377(18) 0.0425(19) 0.0110(15) -0.0124(16) 0.0027(16) C12 0.041(2) 0.056(2) 0.063(2) 0.0176(19) -0.0107(17) -0.0048(17) C13 0.0418(18) 0.0360(17) 0.0339(16) 0.0055(13) -0.0004(14) 0.0123(14) C14 0.046(2) 0.045(2) 0.052(2) 0.0067(16) 0.0056(16) 0.0101(16) C15 0.070(3) 0.060(3) 0.066(3) 0.002(2) 0.025(2) 0.021(2) C16 0.099(4) 0.057(3) 0.070(3) -0.013(2) 0.024(3) 0.019(3) C17 0.084(3) 0.056(3) 0.075(3) -0.019(2) 0.004(3) -0.009(2) C18 0.050(2) 0.054(2) 0.059(2) -0.0044(19) 0.0028(18) 0.0029(18) C19 0.0392(18) 0.0353(17) 0.0346(16) 0.0101(13) -0.0014(13) 0.0005(14) C20 0.055(2) 0.046(2) 0.054(2) 0.0196(17) -0.0007(17) 0.0061(17) C21 0.083(3) 0.046(2) 0.052(2) 0.0246(18) -0.006(2) -0.005(2) C22 0.075(3) 0.056(2) 0.043(2) 0.0142(18) 0.0063(19) -0.020(2) C23 0.050(2) 0.062(2) 0.045(2) 0.0128(18) 0.0117(17) -0.0034(18) C24 0.0432(19) 0.0436(19) 0.0389(18) 0.0121(15) 0.0027(14) 0.0037(15) C25 0.0341(17) 0.0444(19) 0.0442(18) 0.0144(15) -0.0004(14) 0.0116(14) C26 0.045(2) 0.059(2) 0.0390(18) 0.0175(16) -0.0116(15) 0.0061(17) C27 0.046(2) 0.054(2) 0.0402(19) 0.0077(16) -0.0143(15) 0.0027(17) C28 0.0443(19) 0.0398(18) 0.0302(16) 0.0077(13) 0.0019(13) 0.0043(14) C29 0.0285(15) 0.0367(17) 0.0318(15) 0.0001(13) 0.0023(12) 0.0026(13) C30 0.043(2) 0.049(2) 0.052(2) 0.0164(16) 0.0165(16) 0.0078(16) C31 0.040(2) 0.069(3) 0.072(3) 0.019(2) 0.0251(19) 0.0009(19) C32 0.0300(18) 0.054(2) 0.073(3) 0.004(2) 0.0126(18) 0.0062(16) C33 0.0363(19) 0.048(2) 0.061(2) 0.0067(17) -0.0012(16) 0.0100(16) C34 0.0338(17) 0.049(2) 0.0413(18) 0.0085(15) 0.0038(14) 0.0051(15) C35 0.0265(15) 0.0338(17) 0.0463(18) 0.0050(14) 0.0039(13) 0.0070(13) C36 0.0414(19) 0.0410(19) 0.050(2) 0.0048(16) 0.0008(16) 0.0042(15) C37 0.049(2) 0.043(2) 0.073(3) -0.0023(19) -0.008(2) 0.0027(17) C38 0.040(2) 0.037(2) 0.105(4) 0.010(2) -0.008(2) -0.0022(16) C39 0.045(2) 0.050(2) 0.089(3) 0.030(2) 0.018(2) 0.0053(18) C40 0.043(2) 0.043(2) 0.053(2) 0.0113(16) 0.0138(16) 0.0060(15) C41 0.187(8) 0.097(5) 0.128(6) 0.046(4) -0.001(5) -0.027(5) Cl1 0.0564(5) 0.0465(5) 0.0371(4) 0.0150(4) 0.0049(4) 0.0170(4) Cl2 0.1144(15) 0.1252(19) 0.077(2) 0.0391(14) 0.007(2) -0.0251(14) Cl3 0.108(2) 0.173(3) 0.0709(11) 0.0153(17) 0.0070(11) 0.0118(19) N1 0.0427(15) 0.0336(14) 0.0286(13) 0.0089(11) -0.0053(11) 0.0057(11) N2 0.0364(16) 0.061(2) 0.0425(17) 0.0160(15) 0.0009(13) 0.0086(14) P1 0.0293(4) 0.0317(4) 0.0309(4) 0.0074(3) 0.0010(3) 0.0049(3) P2 0.0285(4) 0.0337(4) 0.0282(4) 0.0064(3) 0.0050(3) 0.0044(3) Ru1 0.02933(13) 0.03252(14) 0.02571(13) 0.00717(9) 0.00224(9) 0.00574(9) Cl3A 0.108(2) 0.173(3) 0.0709(11) 0.0153(17) 0.0070(11) 0.0118(19) Cl2A 0.1144(15) 0.1252(19) 0.077(2) 0.0391(14) 0.007(2) -0.0251(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.407(4) . ? C1 C6 1.430(4) . ? C1 Ru1 2.057(3) . ? C2 H2 0.9300 . ? C2 C3 1.384(4) . ? C3 H3 0.9300 . ? C3 C4 1.376(5) . ? C4 H4 0.9300 . ? C4 C5 1.378(5) . ? C5 H5 0.9300 . ? C5 C6 1.400(4) . ? C6 C7 1.466(5) . ? C7 C8 1.390(4) . ? C7 N1 1.353(4) . ? C8 H8 0.9300 . ? C8 C9 1.367(6) . ? C9 H9 0.9300 . ? C9 C10 1.377(6) . ? C10 H10 0.9300 . ? C10 C11 1.388(5) . ? C11 C12 1.506(5) . ? C11 N1 1.340(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 N2 1.477(5) . ? C13 C14 1.392(5) . ? C13 C18 1.388(5) . ? C13 P1 1.843(3) . ? C14 H14 0.9300 . ? C14 C15 1.377(5) . ? C15 H15 0.9300 . ? C15 C16 1.374(6) . ? C16 H16 0.9300 . ? C16 C17 1.367(6) . ? C17 H17 0.9300 . ? C17 C18 1.383(5) . ? C18 H18 0.9300 . ? C19 C20 1.388(5) . ? C19 C24 1.391(5) . ? C19 P1 1.852(3) . ? C20 H20 0.9300 . ? C20 C21 1.379(5) . ? C21 H21 0.9300 . ? C21 C22 1.381(6) . ? C22 H22 0.9300 . ? C22 C23 1.367(6) . ? C23 H23 0.9300 . ? C23 C24 1.387(5) . ? C24 H24 0.9300 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 C26 1.523(4) . ? C25 P1 1.863(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 C27 1.521(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 C28 1.530(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 P2 1.843(3) . ? C29 C30 1.391(4) . ? C29 C34 1.388(5) . ? C29 P2 1.852(3) . ? C30 H30 0.9300 . ? C30 C31 1.391(5) . ? C31 H31 0.9300 . ? C31 C32 1.366(6) . ? C32 H32 0.9300 . ? C32 C33 1.378(5) . ? C33 H33 0.9300 . ? C33 C34 1.386(5) . ? C34 H34 0.9300 . ? C35 C36 1.396(4) . ? C35 C40 1.390(4) . ? C35 P2 1.852(3) . ? C36 H36 0.9300 . ? C36 C37 1.380(5) . ? C37 H37 0.9300 . ? C37 C38 1.378(6) . ? C38 H38 0.9300 . ? C38 C39 1.372(6) . ? C39 H39 0.9300 . ? C39 C40 1.399(5) . ? C40 H40 0.9300 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 Cl2 1.768(8) . ? C41 Cl3 1.748(6) . ? C41 Cl3A 1.718(9) . ? C41 Cl2A 1.738(14) . ? Cl1 Ru1 2.5157(8) . ? N1 Ru1 2.065(2) . ? N2 Ru1 2.255(3) . ? N2 H2A 0.93(4) . ? N2 H2B 0.82(4) . ? P1 Ru1 2.2470(8) . ? P2 Ru1 2.2938(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 114.5(3) . . ? C2 C1 Ru1 132.7(2) . . ? C6 C1 Ru1 112.8(2) . . ? C1 C2 H2 118.4 . . ? C3 C2 C1 123.2(3) . . ? C3 C2 H2 118.4 . . ? C2 C3 H3 119.7 . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3 119.7 . . ? C3 C4 H4 120.5 . . ? C3 C4 C5 119.1(3) . . ? C5 C4 H4 120.5 . . ? C4 C5 H5 119.6 . . ? C4 C5 C6 120.8(3) . . ? C6 C5 H5 119.6 . . ? C1 C6 C7 116.3(3) . . ? C5 C6 C1 121.8(3) . . ? C5 C6 C7 122.0(3) . . ? C8 C7 C6 127.5(3) . . ? N1 C7 C6 113.7(3) . . ? N1 C7 C8 118.8(3) . . ? C7 C8 H8 120.1 . . ? C9 C8 C7 119.8(4) . . ? C9 C8 H8 120.1 . . ? C8 C9 H9 119.8 . . ? C8 C9 C10 120.4(3) . . ? C10 C9 H9 119.8 . . ? C9 C10 H10 120.6 . . ? C9 C10 C11 118.8(4) . . ? C11 C10 H10 120.6 . . ? C10 C11 C12 124.6(3) . . ? N1 C11 C10 120.0(3) . . ? N1 C11 C12 115.4(3) . . ? C11 C12 H12A 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N2 C12 C11 110.0(3) . . ? N2 C12 H12A 109.7 . . ? N2 C12 H12B 109.7 . . ? C14 C13 P1 120.0(3) . . ? C18 C13 C14 117.7(3) . . ? C18 C13 P1 122.1(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 C13 121.0(4) . . ? C15 C14 H14 119.5 . . ? C14 C15 H15 119.8 . . ? C16 C15 C14 120.3(4) . . ? C16 C15 H15 119.8 . . ? C15 C16 H16 120.2 . . ? C17 C16 C15 119.7(4) . . ? C17 C16 H16 120.2 . . ? C16 C17 H17 119.8 . . ? C16 C17 C18 120.4(4) . . ? C18 C17 H17 119.8 . . ? C13 C18 H18 119.6 . . ? C17 C18 C13 120.8(4) . . ? C17 C18 H18 119.6 . . ? C20 C19 C24 117.9(3) . . ? C20 C19 P1 121.7(3) . . ? C24 C19 P1 120.4(2) . . ? C19 C20 H20 119.8 . . ? C21 C20 C19 120.5(4) . . ? C21 C20 H20 119.8 . . ? C20 C21 H21 119.5 . . ? C20 C21 C22 120.9(4) . . ? C22 C21 H21 119.5 . . ? C21 C22 H22 120.3 . . ? C23 C22 C21 119.3(3) . . ? C23 C22 H22 120.3 . . ? C22 C23 H23 119.9 . . ? C22 C23 C24 120.1(4) . . ? C24 C23 H23 119.9 . . ? C19 C24 H24 119.4 . . ? C23 C24 C19 121.2(3) . . ? C23 C24 H24 119.4 . . ? H25A C25 H25B 106.9 . . ? C26 C25 H25A 107.4 . . ? C26 C25 H25B 107.4 . . ? C26 C25 P1 119.7(2) . . ? P1 C25 H25A 107.4 . . ? P1 C25 H25B 107.4 . . ? C25 C26 H26A 108.4 . . ? C25 C26 H26B 108.4 . . ? H26A C26 H26B 107.4 . . ? C27 C26 C25 115.6(3) . . ? C27 C26 H26A 108.4 . . ? C27 C26 H26B 108.4 . . ? C26 C27 H27A 108.5 . . ? C26 C27 H27B 108.5 . . ? C26 C27 C28 114.9(3) . . ? H27A C27 H27B 107.5 . . ? C28 C27 H27A 108.5 . . ? C28 C27 H27B 108.5 . . ? C27 C28 H28A 108.4 . . ? C27 C28 H28B 108.4 . . ? C27 C28 P2 115.7(2) . . ? H28A C28 H28B 107.4 . . ? P2 C28 H28A 108.4 . . ? P2 C28 H28B 108.4 . . ? C30 C29 P2 122.6(3) . . ? C34 C29 C30 117.6(3) . . ? C34 C29 P2 119.8(2) . . ? C29 C30 H30 119.6 . . ? C29 C30 C31 120.9(4) . . ? C31 C30 H30 119.6 . . ? C30 C31 H31 119.7 . . ? C32 C31 C30 120.7(3) . . ? C32 C31 H31 119.7 . . ? C31 C32 H32 120.4 . . ? C31 C32 C33 119.3(3) . . ? C33 C32 H32 120.4 . . ? C32 C33 H33 119.8 . . ? C32 C33 C34 120.4(4) . . ? C34 C33 H33 119.8 . . ? C29 C34 H34 119.4 . . ? C33 C34 C29 121.2(3) . . ? C33 C34 H34 119.4 . . ? C36 C35 P2 121.9(2) . . ? C40 C35 C36 118.4(3) . . ? C40 C35 P2 119.7(2) . . ? C35 C36 H36 119.4 . . ? C37 C36 C35 121.2(3) . . ? C37 C36 H36 119.4 . . ? C36 C37 H37 119.9 . . ? C38 C37 C36 120.1(4) . . ? C38 C37 H37 119.9 . . ? C37 C38 H38 120.2 . . ? C39 C38 C37 119.6(3) . . ? C39 C38 H38 120.2 . . ? C38 C39 H39 119.5 . . ? C38 C39 C40 121.0(4) . . ? C40 C39 H39 119.5 . . ? C35 C40 C39 119.7(3) . . ? C35 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? H41A C41 H41B 108.2 . . ? Cl2 C41 H41A 109.8 . . ? Cl2 C41 H41B 109.8 . . ? Cl3 C41 H41A 109.8 . . ? Cl3 C41 H41B 109.8 . . ? Cl3 C41 Cl2 109.4(4) . . ? Cl3A C41 H41A 81.5 . . ? Cl3A C41 H41B 105.0 . . ? Cl3A C41 Cl2 137.0(5) . . ? Cl3A C41 Cl3 32.7(3) . . ? Cl3A C41 Cl2A 123.9(6) . . ? Cl2A C41 H41A 119.7 . . ? Cl2A C41 H41B 113.8 . . ? Cl2A C41 Cl2 15.3(4) . . ? Cl2A C41 Cl3 94.5(4) . . ? C7 N1 Ru1 116.9(2) . . ? C11 N1 C7 122.2(3) . . ? C11 N1 Ru1 120.2(2) . . ? C12 N2 Ru1 108.8(2) . . ? C12 N2 H2A 109(2) . . ? C12 N2 H2B 113(3) . . ? Ru1 N2 H2A 98(2) . . ? Ru1 N2 H2B 124(3) . . ? H2A N2 H2B 103(4) . . ? C13 P1 C19 101.36(14) . . ? C13 P1 C25 97.49(15) . . ? C13 P1 Ru1 112.84(10) . . ? C19 P1 C25 101.09(15) . . ? C19 P1 Ru1 119.10(11) . . ? C25 P1 Ru1 121.23(11) . . ? C28 P2 C29 98.97(14) . . ? C28 P2 C35 100.68(15) . . ? C28 P2 Ru1 120.09(11) . . ? C29 P2 C35 99.89(14) . . ? C29 P2 Ru1 112.21(10) . . ? C35 P2 Ru1 121.11(10) . . ? C1 Ru1 Cl1 90.67(8) . . ? C1 Ru1 N1 79.76(11) . . ? C1 Ru1 N2 154.49(12) . . ? C1 Ru1 P1 86.90(8) . . ? C1 Ru1 P2 103.27(9) . . ? N1 Ru1 Cl1 83.42(7) . . ? N1 Ru1 N2 76.30(11) . . ? N1 Ru1 P1 91.82(7) . . ? N1 Ru1 P2 173.20(7) . . ? N2 Ru1 Cl1 78.03(9) . . ? N2 Ru1 P2 99.65(8) . . ? P1 Ru1 Cl1 174.98(3) . . ? P1 Ru1 N2 102.44(9) . . ? P1 Ru1 P2 94.41(3) . . ? P2 Ru1 Cl1 90.42(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A Cl1 0.93(4) 2.42(3) 3.010(4) 122(3) . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 -1.1(5) . . . . ? C1 C6 C7 C8 177.1(3) . . . . ? C1 C6 C7 N1 -2.5(4) . . . . ? C2 C1 C6 C5 -1.3(4) . . . . ? C2 C1 C6 C7 178.1(3) . . . . ? C2 C1 Ru1 Cl1 100.4(3) . . . . ? C2 C1 Ru1 N1 -176.4(3) . . . . ? C2 C1 Ru1 N2 163.2(3) . . . . ? C2 C1 Ru1 P1 -84.0(3) . . . . ? C2 C1 Ru1 P2 9.8(3) . . . . ? C2 C3 C4 C5 -0.2(6) . . . . ? C3 C4 C5 C6 0.6(6) . . . . ? C4 C5 C6 C1 0.2(5) . . . . ? C4 C5 C6 C7 -179.1(3) . . . . ? C5 C6 C7 C8 -3.5(5) . . . . ? C5 C6 C7 N1 176.9(3) . . . . ? C6 C1 C2 C3 1.7(5) . . . . ? C6 C1 Ru1 Cl1 -77.7(2) . . . . ? C6 C1 Ru1 N1 5.5(2) . . . . ? C6 C1 Ru1 N2 -14.9(4) . . . . ? C6 C1 Ru1 P1 97.9(2) . . . . ? C6 C1 Ru1 P2 -168.3(2) . . . . ? C6 C7 C8 C9 -178.2(3) . . . . ? C6 C7 N1 C11 177.7(3) . . . . ? C6 C7 N1 Ru1 7.3(3) . . . . ? C7 C8 C9 C10 -0.3(6) . . . . ? C7 N1 Ru1 C1 -7.3(2) . . . . ? C7 N1 Ru1 Cl1 84.6(2) . . . . ? C7 N1 Ru1 N2 163.8(2) . . . . ? C7 N1 Ru1 P1 -93.8(2) . . . . ? C7 N1 Ru1 P2 109.8(6) . . . . ? C8 C7 N1 C11 -1.9(5) . . . . ? C8 C7 N1 Ru1 -172.3(2) . . . . ? C8 C9 C10 C11 -0.3(6) . . . . ? C9 C10 C11 C12 -178.5(4) . . . . ? C9 C10 C11 N1 -0.1(6) . . . . ? C10 C11 C12 N2 -152.3(3) . . . . ? C10 C11 N1 C7 1.3(5) . . . . ? C10 C11 N1 Ru1 171.4(3) . . . . ? C11 C12 N2 Ru1 -32.5(3) . . . . ? C11 N1 Ru1 C1 -177.9(3) . . . . ? C11 N1 Ru1 Cl1 -86.0(2) . . . . ? C11 N1 Ru1 N2 -6.8(2) . . . . ? C11 N1 Ru1 P1 95.6(2) . . . . ? C11 N1 Ru1 P2 -60.8(7) . . . . ? C12 C11 N1 C7 179.8(3) . . . . ? C12 C11 N1 Ru1 -10.1(4) . . . . ? C12 N2 Ru1 C1 42.4(4) . . . . ? C12 N2 Ru1 Cl1 107.8(2) . . . . ? C12 N2 Ru1 N1 21.8(2) . . . . ? C12 N2 Ru1 P1 -67.1(2) . . . . ? C12 N2 Ru1 P2 -163.8(2) . . . . ? C13 C14 C15 C16 0.8(7) . . . . ? C13 P1 Ru1 C1 -64.89(15) . . . . ? C13 P1 Ru1 Cl1 -3.7(4) . . . . ? C13 P1 Ru1 N1 14.75(14) . . . . ? C13 P1 Ru1 N2 91.12(14) . . . . ? C13 P1 Ru1 P2 -167.97(12) . . . . ? C14 C13 C18 C17 1.9(6) . . . . ? C14 C13 P1 C19 -146.6(3) . . . . ? C14 C13 P1 C25 -43.6(3) . . . . ? C14 C13 P1 Ru1 84.9(3) . . . . ? C14 C15 C16 C17 -0.5(8) . . . . ? C15 C16 C17 C18 1.0(8) . . . . ? C16 C17 C18 C13 -1.7(7) . . . . ? C18 C13 C14 C15 -1.5(6) . . . . ? C18 C13 P1 C19 37.1(3) . . . . ? C18 C13 P1 C25 140.1(3) . . . . ? C18 C13 P1 Ru1 -91.4(3) . . . . ? C19 C20 C21 C22 1.3(6) . . . . ? C19 P1 Ru1 C1 176.49(14) . . . . ? C19 P1 Ru1 Cl1 -122.3(4) . . . . ? C19 P1 Ru1 N1 -103.87(14) . . . . ? C19 P1 Ru1 N2 -27.50(14) . . . . ? C19 P1 Ru1 P2 73.41(12) . . . . ? C20 C19 C24 C23 -0.8(5) . . . . ? C20 C19 P1 C13 47.2(3) . . . . ? C20 C19 P1 C25 -52.9(3) . . . . ? C20 C19 P1 Ru1 171.6(2) . . . . ? C20 C21 C22 C23 -1.1(6) . . . . ? C21 C22 C23 C24 0.0(6) . . . . ? C22 C23 C24 C19 1.0(5) . . . . ? C24 C19 C20 C21 -0.3(5) . . . . ? C24 C19 P1 C13 -133.0(3) . . . . ? C24 C19 P1 C25 126.9(3) . . . . ? C24 C19 P1 Ru1 -8.6(3) . . . . ? C25 C26 C27 C28 78.3(4) . . . . ? C25 P1 Ru1 C1 49.99(15) . . . . ? C25 P1 Ru1 Cl1 111.2(4) . . . . ? C25 P1 Ru1 N1 129.63(14) . . . . ? C25 P1 Ru1 N2 -154.00(14) . . . . ? C25 P1 Ru1 P2 -53.10(12) . . . . ? C26 C25 P1 C13 -155.0(3) . . . . ? C26 C25 P1 C19 -51.9(3) . . . . ? C26 C25 P1 Ru1 82.4(3) . . . . ? C26 C27 C28 P2 -101.2(3) . . . . ? C27 C28 P2 C29 -167.4(2) . . . . ? C27 C28 P2 C35 -65.4(3) . . . . ? C27 C28 P2 Ru1 70.4(3) . . . . ? C28 P2 Ru1 C1 -91.09(15) . . . . ? C28 P2 Ru1 Cl1 178.12(12) . . . . ? C28 P2 Ru1 N1 153.1(6) . . . . ? C28 P2 Ru1 N2 100.19(15) . . . . ? C28 P2 Ru1 P1 -3.24(12) . . . . ? C29 C30 C31 C32 -0.5(6) . . . . ? C29 P2 Ru1 C1 153.36(14) . . . . ? C29 P2 Ru1 Cl1 62.58(11) . . . . ? C29 P2 Ru1 N1 37.6(6) . . . . ? C29 P2 Ru1 N2 -15.35(14) . . . . ? C29 P2 Ru1 P1 -118.78(11) . . . . ? C30 C29 C34 C33 0.6(5) . . . . ? C30 C29 P2 C28 -27.3(3) . . . . ? C30 C29 P2 C35 -129.9(3) . . . . ? C30 C29 P2 Ru1 100.5(3) . . . . ? C30 C31 C32 C33 1.6(6) . . . . ? C31 C32 C33 C34 -1.5(6) . . . . ? C32 C33 C34 C29 0.4(5) . . . . ? C34 C29 C30 C31 -0.6(5) . . . . ? C34 C29 P2 C28 154.5(3) . . . . ? C34 C29 P2 C35 51.9(3) . . . . ? C34 C29 P2 Ru1 -77.7(3) . . . . ? C35 C36 C37 C38 0.5(6) . . . . ? C35 P2 Ru1 C1 35.78(15) . . . . ? C35 P2 Ru1 Cl1 -55.01(12) . . . . ? C35 P2 Ru1 N1 -80.0(6) . . . . ? C35 P2 Ru1 N2 -132.94(15) . . . . ? C35 P2 Ru1 P1 123.63(12) . . . . ? C36 C35 C40 C39 1.5(5) . . . . ? C36 C35 P2 C28 -32.2(3) . . . . ? C36 C35 P2 C29 69.0(3) . . . . ? C36 C35 P2 Ru1 -167.4(2) . . . . ? C36 C37 C38 C39 1.4(6) . . . . ? C37 C38 C39 C40 -1.9(6) . . . . ? C38 C39 C40 C35 0.4(6) . . . . ? C40 C35 C36 C37 -2.0(5) . . . . ? C40 C35 P2 C28 147.1(3) . . . . ? C40 C35 P2 C29 -111.7(3) . . . . ? C40 C35 P2 Ru1 11.9(3) . . . . ? N1 C7 C8 C9 1.4(5) . . . . ? N1 C11 C12 N2 29.3(4) . . . . ? P1 C13 C14 C15 -177.9(3) . . . . ? P1 C13 C18 C17 178.3(4) . . . . ? P1 C19 C20 C21 179.5(3) . . . . ? P1 C19 C24 C23 179.4(3) . . . . ? P1 C25 C26 C27 -67.7(4) . . . . ? P2 C29 C30 C31 -178.8(3) . . . . ? P2 C29 C34 C33 178.9(3) . . . . ? P2 C35 C36 C37 177.3(3) . . . . ? P2 C35 C40 C39 -177.8(3) . . . . ? Ru1 C1 C2 C3 -176.4(3) . . . . ? Ru1 C1 C6 C5 177.2(3) . . . . ? Ru1 C1 C6 C7 -3.4(3) . . . . ? data_20101143 _database_code_depnum_ccdc_archive 'CCDC 804175' #TrackingRef '20101143.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H45 Cl N2 P2 Ru' _chemical_formula_weight 836.31 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.4744(2) _cell_length_b 13.7238(3) _cell_length_c 29.0038(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.250(2) _cell_angle_gamma 90.00 _cell_volume 4002.69(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8316 _cell_measurement_theta_min 2.9203 _cell_measurement_theta_max 26.3144 _exptl_crystal_description prismatic _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8938 _exptl_absorpt_correction_T_max 0.8938 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18008 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8161 _reflns_number_gt 6643 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.9748P] 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 8161 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.487328(17) 0.208516(13) 0.393419(6) 0.02751(6) Uani 1 1 d . . . Cl1 Cl 0.53066(6) 0.25667(5) 0.47915(2) 0.03598(14) Uani 1 1 d . . . P1 P 0.64421(6) 0.32158(5) 0.38647(2) 0.03214(14) Uani 1 1 d . . . P2 P 0.44432(6) 0.15833(5) 0.31661(2) 0.03444(15) Uani 1 1 d . . . N1 N 0.34759(17) 0.11306(14) 0.40846(6) 0.0306(4) Uani 1 1 d . . . N2 N 0.28394(18) 0.30790(14) 0.39573(7) 0.0372(5) Uani 1 1 d . . . H2 H 0.3233 0.2997 0.4262 0.045 Uiso 1 1 d R . . C1 C 0.5966(2) 0.44960(17) 0.39306(9) 0.0346(5) Uani 1 1 d . . . C2 C 0.5277(3) 0.50447(19) 0.35373(9) 0.0461(6) Uani 1 1 d . . . H2A H 0.5022 0.4757 0.3235 0.055 Uiso 1 1 calc R . . C3 C 0.4963(3) 0.6014(2) 0.35874(11) 0.0567(8) Uani 1 1 d . . . H3 H 0.4492 0.6369 0.3321 0.068 Uiso 1 1 calc R . . C4 C 0.5350(3) 0.6448(2) 0.40318(12) 0.0540(7) Uani 1 1 d . . . H4 H 0.5161 0.7102 0.4065 0.065 Uiso 1 1 calc R . . C5 C 0.6011(3) 0.5919(2) 0.44244(11) 0.0495(7) Uani 1 1 d . . . H5 H 0.6259 0.6212 0.4725 0.059 Uiso 1 1 calc R . . C6 C 0.6316(2) 0.4942(2) 0.43777(9) 0.0419(6) Uani 1 1 d . . . H6 H 0.6758 0.4587 0.4648 0.050 Uiso 1 1 calc R . . C7 C 0.8096(2) 0.32199(18) 0.43100(9) 0.0363(6) Uani 1 1 d . . . C8 C 0.9035(2) 0.3928(2) 0.42911(10) 0.0488(7) Uani 1 1 d . . . H8 H 0.8849 0.4376 0.4040 0.059 Uiso 1 1 calc R . . C9 C 1.0239(3) 0.3970(2) 0.46420(12) 0.0603(9) Uani 1 1 d . . . H9 H 1.0853 0.4451 0.4628 0.072 Uiso 1 1 calc R . . C10 C 1.0535(3) 0.3310(3) 0.50089(13) 0.0678(9) Uani 1 1 d . . . H10 H 1.1344 0.3344 0.5245 0.081 Uiso 1 1 calc R . . C11 C 0.9638(3) 0.2602(2) 0.50275(12) 0.0606(8) Uani 1 1 d . . . H11 H 0.9850 0.2139 0.5271 0.073 Uiso 1 1 calc R . . C12 C 0.8409(2) 0.2566(2) 0.46846(10) 0.0445(6) Uani 1 1 d . . . H12 H 0.7793 0.2095 0.4709 0.053 Uiso 1 1 calc R . . C13 C 0.6911(3) 0.3344(2) 0.32989(9) 0.0445(6) Uani 1 1 d . . . H13A H 0.6109 0.3477 0.3043 0.053 Uiso 1 1 calc R . . H13B H 0.7482 0.3911 0.3328 0.053 Uiso 1 1 calc R . . C14 C 0.7620(3) 0.2478(2) 0.31455(10) 0.0500(7) Uani 1 1 d . . . H14A H 0.8323 0.2724 0.3019 0.060 Uiso 1 1 calc R . . H14B H 0.8032 0.2089 0.3427 0.060 Uiso 1 1 calc R . . C15 C 0.6711(3) 0.1823(2) 0.27676(10) 0.0516(7) Uani 1 1 d . . . H15A H 0.7268 0.1444 0.2618 0.062 Uiso 1 1 calc R . . H15B H 0.6159 0.2239 0.2521 0.062 Uiso 1 1 calc R . . C16 C 0.5794(3) 0.1114(2) 0.29310(9) 0.0449(6) Uani 1 1 d . . . H16A H 0.6354 0.0702 0.3178 0.054 Uiso 1 1 calc R . . H16B H 0.5388 0.0695 0.2660 0.054 Uiso 1 1 calc R . . C17 C 0.3332(3) 0.0518(2) 0.30404(9) 0.0464(7) Uani 1 1 d . . . C18 C 0.3822(4) -0.0418(2) 0.31558(10) 0.0628(9) Uani 1 1 d . . . H18 H 0.4734 -0.0519 0.3273 0.075 Uiso 1 1 calc R . . C19 C 0.2959(5) -0.1202(3) 0.30969(13) 0.0896(13) Uani 1 1 d . . . H19 H 0.3297 -0.1826 0.3175 0.107 Uiso 1 1 calc R . . C20 C 0.1612(6) -0.1066(4) 0.29248(15) 0.1106(19) Uani 1 1 d . . . H20 H 0.1036 -0.1594 0.2888 0.133 Uiso 1 1 calc R . . C21 C 0.1128(4) -0.0153(4) 0.28082(13) 0.0991(15) Uani 1 1 d . . . H21 H 0.0215 -0.0060 0.2689 0.119 Uiso 1 1 calc R . . C22 C 0.1966(3) 0.0634(3) 0.28641(11) 0.0673(9) Uani 1 1 d . . . H22 H 0.1614 0.1253 0.2783 0.081 Uiso 1 1 calc R . . C23 C 0.3575(2) 0.2406(2) 0.26785(9) 0.0403(6) Uani 1 1 d . . . C24 C 0.3320(3) 0.2164(2) 0.21957(10) 0.0577(8) Uani 1 1 d . . . H24 H 0.3568 0.1554 0.2110 0.069 Uiso 1 1 calc R . . C25 C 0.2704(3) 0.2819(3) 0.18436(11) 0.0721(10) Uani 1 1 d . . . H25 H 0.2559 0.2656 0.1522 0.086 Uiso 1 1 calc R . . C26 C 0.2304(3) 0.3708(3) 0.19644(12) 0.0715(10) Uani 1 1 d . . . H26 H 0.1885 0.4144 0.1724 0.086 Uiso 1 1 calc R . . C27 C 0.2518(3) 0.3961(2) 0.24395(12) 0.0622(8) Uani 1 1 d . . . H27 H 0.2241 0.4564 0.2522 0.075 Uiso 1 1 calc R . . C28 C 0.3155(2) 0.3302(2) 0.27938(10) 0.0453(6) Uani 1 1 d . . . H28 H 0.3300 0.3470 0.3115 0.054 Uiso 1 1 calc R . . C29 C 0.5996(2) 0.08538(17) 0.41113(8) 0.0310(5) Uani 1 1 d . . . C30 C 0.7302(2) 0.06334(19) 0.41048(9) 0.0401(6) Uani 1 1 d . . . H30 H 0.7779 0.1103 0.3992 0.048 Uiso 1 1 calc R . . C31 C 0.7910(2) -0.0247(2) 0.42583(10) 0.0484(7) Uani 1 1 d . . . H31 H 0.8777 -0.0355 0.4247 0.058 Uiso 1 1 calc R . . C32 C 0.7243(3) -0.0968(2) 0.44287(10) 0.0517(7) Uani 1 1 d . . . H32 H 0.7654 -0.1562 0.4532 0.062 Uiso 1 1 calc R . . C33 C 0.5961(2) -0.07961(19) 0.44440(10) 0.0435(6) Uani 1 1 d . . . H33 H 0.5505 -0.1275 0.4560 0.052 Uiso 1 1 calc R . . C34 C 0.5341(2) 0.00889(17) 0.42872(8) 0.0321(5) Uani 1 1 d . . . C35 C 0.3958(2) 0.02634(17) 0.42783(8) 0.0333(5) Uani 1 1 d . . . C36 C 0.3146(3) -0.0371(2) 0.44461(10) 0.0458(7) Uani 1 1 d . . . H36 H 0.3476 -0.0967 0.4581 0.055 Uiso 1 1 calc R . . C37 C 0.1862(3) -0.0109(2) 0.44095(11) 0.0594(8) Uani 1 1 d . . . H37 H 0.1311 -0.0528 0.4518 0.071 Uiso 1 1 calc R . . C38 C 0.1384(3) 0.0781(2) 0.42106(11) 0.0549(8) Uani 1 1 d . . . H38 H 0.0515 0.0969 0.4186 0.066 Uiso 1 1 calc R . . C39 C 0.2217(2) 0.13842(18) 0.40497(9) 0.0391(6) Uani 1 1 d . . . C40 C 0.1768(2) 0.23491(19) 0.38214(11) 0.0468(7) Uani 1 1 d . . . H40A H 0.1492 0.2276 0.3475 0.056 Uiso 1 1 calc R . . H40B H 0.1008 0.2574 0.3921 0.056 Uiso 1 1 calc R . . C41 C 0.2383(2) 0.40675(18) 0.38854(9) 0.0376(6) Uani 1 1 d . . . C42 C 0.1325(3) 0.4345(2) 0.35043(10) 0.0531(7) Uani 1 1 d . . . H42 H 0.0907 0.3892 0.3273 0.064 Uiso 1 1 calc R . . C43 C 0.0887(3) 0.5309(2) 0.34693(11) 0.0653(9) Uani 1 1 d . . . H43 H 0.0178 0.5490 0.3210 0.078 Uiso 1 1 calc R . . C44 C 0.1471(3) 0.6002(2) 0.38054(12) 0.0618(8) Uani 1 1 d . . . C45 C 0.2532(3) 0.5714(2) 0.41831(11) 0.0533(7) Uani 1 1 d . . . H45 H 0.2947 0.6168 0.4415 0.064 Uiso 1 1 calc R . . C46 C 0.2986(2) 0.4766(2) 0.42221(9) 0.0425(6) Uani 1 1 d . . . H46 H 0.3707 0.4592 0.4478 0.051 Uiso 1 1 calc R . . C47 C 0.0958(5) 0.7046(3) 0.37677(16) 0.1043(15) Uani 1 1 d . . . H47A H 0.0281 0.7101 0.3931 0.156 Uiso 1 1 calc R . . H47B H 0.0592 0.7215 0.3436 0.156 Uiso 1 1 calc R . . H47C H 0.1677 0.7480 0.3913 0.156 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 0.02828(10) 0.02477(11) 0.02907(10) -0.00024(8) 0.00733(7) -0.00171(8) Cl1 0.0396(3) 0.0359(3) 0.0313(3) -0.0013(3) 0.0081(2) -0.0011(3) P1 0.0354(3) 0.0302(3) 0.0320(3) -0.0007(3) 0.0113(3) -0.0055(3) P2 0.0385(3) 0.0320(4) 0.0315(3) -0.0029(3) 0.0078(3) -0.0015(3) N1 0.0311(10) 0.0280(11) 0.0328(10) -0.0024(9) 0.0091(8) -0.0031(8) N2 0.0342(10) 0.0371(12) 0.0382(11) 0.0030(10) 0.0068(9) 0.0008(9) C1 0.0368(12) 0.0311(13) 0.0397(13) 0.0002(11) 0.0168(11) -0.0080(11) C2 0.0648(17) 0.0369(15) 0.0390(14) 0.0021(13) 0.0186(13) -0.0024(13) C3 0.081(2) 0.0374(16) 0.0559(18) 0.0134(15) 0.0255(16) 0.0061(15) C4 0.0641(18) 0.0303(15) 0.076(2) -0.0016(15) 0.0330(16) -0.0020(14) C5 0.0485(15) 0.0467(17) 0.0555(17) -0.0193(15) 0.0183(14) -0.0107(13) C6 0.0405(13) 0.0431(16) 0.0421(14) -0.0042(13) 0.0116(11) -0.0023(12) C7 0.0302(11) 0.0378(14) 0.0428(14) -0.0068(12) 0.0132(11) -0.0046(11) C8 0.0418(14) 0.0483(17) 0.0611(17) -0.0025(15) 0.0224(13) -0.0086(13) C9 0.0340(14) 0.062(2) 0.088(2) -0.0208(19) 0.0216(15) -0.0195(14) C10 0.0340(15) 0.074(2) 0.085(2) -0.009(2) -0.0011(15) -0.0063(16) C11 0.0415(15) 0.061(2) 0.069(2) 0.0030(17) -0.0013(15) 0.0004(15) C12 0.0337(13) 0.0424(16) 0.0551(16) -0.0015(14) 0.0084(12) -0.0065(12) C13 0.0558(16) 0.0424(16) 0.0410(14) -0.0012(13) 0.0226(13) -0.0101(13) C14 0.0509(16) 0.0559(18) 0.0507(16) -0.0062(14) 0.0266(14) -0.0046(14) C15 0.0565(16) 0.0574(19) 0.0477(16) -0.0104(14) 0.0259(14) 0.0009(14) C16 0.0503(15) 0.0443(16) 0.0399(14) -0.0116(13) 0.0121(12) 0.0034(13) C17 0.0608(17) 0.0443(17) 0.0322(13) -0.0087(13) 0.0097(12) -0.0178(14) C18 0.099(2) 0.0407(18) 0.0471(17) -0.0114(15) 0.0184(17) -0.0120(17) C19 0.166(4) 0.044(2) 0.060(2) -0.0109(18) 0.034(3) -0.031(3) C20 0.154(5) 0.107(4) 0.062(3) -0.008(3) 0.015(3) -0.087(4) C21 0.086(3) 0.131(4) 0.067(2) 0.006(3) 0.000(2) -0.066(3) C22 0.0627(19) 0.076(2) 0.0556(19) 0.0020(18) 0.0049(16) -0.0280(18) C23 0.0408(13) 0.0438(16) 0.0356(13) 0.0036(12) 0.0094(11) -0.0042(12) C24 0.0665(19) 0.068(2) 0.0374(15) 0.0016(15) 0.0126(14) 0.0011(16) C25 0.077(2) 0.101(3) 0.0351(16) 0.0111(19) 0.0103(16) -0.004(2) C26 0.064(2) 0.086(3) 0.057(2) 0.035(2) 0.0048(17) 0.0026(19) C27 0.0612(18) 0.054(2) 0.069(2) 0.0218(17) 0.0141(16) 0.0048(16) C28 0.0461(14) 0.0465(17) 0.0423(15) 0.0066(13) 0.0108(12) 0.0013(13) C29 0.0314(11) 0.0266(12) 0.0335(12) -0.0031(10) 0.0062(10) -0.0005(10) C30 0.0351(13) 0.0367(15) 0.0480(15) 0.0009(12) 0.0106(11) -0.0007(11) C31 0.0336(13) 0.0441(17) 0.0662(18) -0.0021(15) 0.0115(13) 0.0092(12) C32 0.0502(16) 0.0338(15) 0.0682(19) 0.0066(14) 0.0116(14) 0.0122(13) C33 0.0482(15) 0.0293(14) 0.0539(16) 0.0024(13) 0.0157(13) -0.0027(12) C34 0.0357(12) 0.0254(12) 0.0340(12) -0.0025(10) 0.0079(10) -0.0034(10) C35 0.0379(12) 0.0297(13) 0.0309(12) -0.0018(11) 0.0074(10) -0.0042(11) C36 0.0455(15) 0.0355(15) 0.0569(17) 0.0070(13) 0.0150(13) -0.0078(12) C37 0.0466(16) 0.0538(19) 0.083(2) 0.0130(17) 0.0262(16) -0.0143(14) C38 0.0337(13) 0.0501(18) 0.083(2) 0.0050(17) 0.0200(14) -0.0053(13) C39 0.0322(12) 0.0359(15) 0.0476(15) -0.0008(12) 0.0088(11) -0.0036(11) C40 0.0312(13) 0.0408(16) 0.0672(19) 0.0012(14) 0.0116(13) -0.0001(11) C41 0.0395(13) 0.0361(14) 0.0380(13) 0.0068(12) 0.0118(11) 0.0035(11) C42 0.0576(17) 0.0531(19) 0.0441(16) 0.0019(14) 0.0065(14) 0.0094(15) C43 0.072(2) 0.066(2) 0.0545(19) 0.0189(18) 0.0125(16) 0.0291(18) C44 0.080(2) 0.0446(19) 0.069(2) 0.0158(17) 0.0359(18) 0.0145(17) C45 0.0633(18) 0.0423(17) 0.0625(19) -0.0013(15) 0.0310(16) -0.0079(15) C46 0.0412(14) 0.0434(16) 0.0459(15) 0.0027(13) 0.0168(12) -0.0046(12) C47 0.147(4) 0.054(2) 0.122(4) 0.026(2) 0.056(3) 0.038(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C29 2.041(2) . ? Ru1 N1 2.0991(18) . ? Ru1 P2 2.2535(6) . ? Ru1 P1 2.3095(6) . ? Ru1 Cl1 2.4887(6) . ? Ru1 N2 2.5462(19) . ? P1 C13 1.848(2) . ? P1 C7 1.849(2) . ? P1 C1 1.851(2) . ? P2 C23 1.839(3) . ? P2 C17 1.840(3) . ? P2 C16 1.850(3) . ? N1 C39 1.340(3) . ? N1 C35 1.352(3) . ? N2 C41 1.434(3) . ? N2 C40 1.473(3) . ? N2 H2 0.8708 . ? C1 C6 1.388(3) . ? C1 C2 1.389(3) . ? C2 C3 1.387(4) . ? C2 H2A 0.9300 . ? C3 C4 1.374(4) . ? C3 H3 0.9300 . ? C4 C5 1.364(4) . ? C4 H4 0.9300 . ? C5 C6 1.393(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.377(4) . ? C7 C8 1.394(3) . ? C8 C9 1.383(4) . ? C8 H8 0.9300 . ? C9 C10 1.365(4) . ? C9 H9 0.9300 . ? C10 C11 1.363(4) . ? C10 H10 0.9300 . ? C11 C12 1.390(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.532(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.527(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.532(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C22 1.387(4) . ? C17 C18 1.390(4) . ? C18 C19 1.384(5) . ? C18 H18 0.9300 . ? C19 C20 1.371(6) . ? C19 H19 0.9300 . ? C20 C21 1.359(6) . ? C20 H20 0.9300 . ? C21 C22 1.373(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C28 1.379(4) . ? C23 C24 1.391(4) . ? C24 C25 1.378(4) . ? C24 H24 0.9300 . ? C25 C26 1.367(5) . ? C25 H25 0.9300 . ? C26 C27 1.377(5) . ? C26 H26 0.9300 . ? C27 C28 1.391(4) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.407(3) . ? C29 C34 1.424(3) . ? C30 C31 1.380(3) . ? C30 H30 0.9300 . ? C31 C32 1.381(4) . ? C31 H31 0.9300 . ? C32 C33 1.376(4) . ? C32 H32 0.9300 . ? C33 C34 1.392(3) . ? C33 H33 0.9300 . ? C34 C35 1.461(3) . ? C35 C36 1.397(3) . ? C36 C37 1.368(4) . ? C36 H36 0.9300 . ? C37 C38 1.383(4) . ? C37 H37 0.9300 . ? C38 C39 1.375(3) . ? C38 H38 0.9300 . ? C39 C40 1.496(3) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.382(3) . ? C41 C46 1.388(4) . ? C42 C43 1.395(4) . ? C42 H42 0.9300 . ? C43 C44 1.376(4) . ? C43 H43 0.9300 . ? C44 C45 1.382(4) . ? C44 C47 1.523(4) . ? C45 C46 1.380(4) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C29 Ru1 N1 79.46(8) . . ? C29 Ru1 P2 86.41(6) . . ? N1 Ru1 P2 93.24(5) . . ? C29 Ru1 P1 101.79(6) . . ? N1 Ru1 P1 172.73(5) . . ? P2 Ru1 P1 93.98(2) . . ? C29 Ru1 Cl1 92.13(6) . . ? N1 Ru1 Cl1 84.31(5) . . ? P2 Ru1 Cl1 177.35(2) . . ? P1 Ru1 Cl1 88.48(2) . . ? C29 Ru1 N2 149.81(8) . . ? N1 Ru1 N2 72.04(7) . . ? P2 Ru1 N2 104.62(5) . . ? P1 Ru1 N2 105.27(5) . . ? Cl1 Ru1 N2 75.61(5) . . ? C13 P1 C7 100.96(12) . . ? C13 P1 C1 98.47(12) . . ? C7 P1 C1 98.74(11) . . ? C13 P1 Ru1 120.93(9) . . ? C7 P1 Ru1 119.45(8) . . ? C1 P1 Ru1 114.19(7) . . ? C23 P2 C17 100.73(12) . . ? C23 P2 C16 101.23(12) . . ? C17 P2 C16 99.03(13) . . ? C23 P2 Ru1 119.44(9) . . ? C17 P2 Ru1 112.28(8) . . ? C16 P2 Ru1 120.59(9) . . ? C39 N1 C35 120.4(2) . . ? C39 N1 Ru1 123.43(16) . . ? C35 N1 Ru1 115.75(14) . . ? C41 N2 C40 113.97(19) . . ? C41 N2 Ru1 138.61(15) . . ? C40 N2 Ru1 102.06(14) . . ? C41 N2 H2 108.3 . . ? C40 N2 H2 107.0 . . ? Ru1 N2 H2 78.2 . . ? C6 C1 C2 118.0(2) . . ? C6 C1 P1 120.48(19) . . ? C2 C1 P1 121.54(19) . . ? C3 C2 C1 121.2(3) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C4 C3 C2 119.8(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 120.5(3) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C12 C7 C8 118.1(2) . . ? C12 C7 P1 121.27(18) . . ? C8 C7 P1 120.5(2) . . ? C9 C8 C7 120.5(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 120.5(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 119.7(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.5(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C7 C12 C11 120.6(3) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 P1 117.02(19) . . ? C14 C13 H13A 108.0 . . ? P1 C13 H13A 108.0 . . ? C14 C13 H13B 108.0 . . ? P1 C13 H13B 108.0 . . ? H13A C13 H13B 107.3 . . ? C15 C14 C13 114.2(2) . . ? C15 C14 H14A 108.7 . . ? C13 C14 H14A 108.7 . . ? C15 C14 H14B 108.7 . . ? C13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C14 C15 C16 118.1(2) . . ? C14 C15 H15A 107.8 . . ? C16 C15 H15A 107.8 . . ? C14 C15 H15B 107.8 . . ? C16 C15 H15B 107.8 . . ? H15A C15 H15B 107.1 . . ? C15 C16 P2 120.20(19) . . ? C15 C16 H16A 107.3 . . ? P2 C16 H16A 107.3 . . ? C15 C16 H16B 107.3 . . ? P2 C16 H16B 107.3 . . ? H16A C16 H16B 106.9 . . ? C22 C17 C18 117.9(3) . . ? C22 C17 P2 120.8(2) . . ? C18 C17 P2 121.1(2) . . ? C19 C18 C17 120.3(4) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C18 120.7(4) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 119.3(4) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 121.0(4) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C17 120.8(4) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? C28 C23 C24 118.2(3) . . ? C28 C23 P2 118.9(2) . . ? C24 C23 P2 122.8(2) . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 120.4(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 120.4(3) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C28 119.0(3) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C23 C28 C27 121.4(3) . . ? C23 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C30 C29 C34 114.4(2) . . ? C30 C29 Ru1 131.98(18) . . ? C34 C29 Ru1 113.55(16) . . ? C31 C30 C29 123.2(2) . . ? C31 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? C30 C31 C32 120.6(2) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C33 C32 C31 119.0(2) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C32 C33 C34 120.6(2) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C33 C34 C29 122.2(2) . . ? C33 C34 C35 121.2(2) . . ? C29 C34 C35 116.5(2) . . ? N1 C35 C36 120.0(2) . . ? N1 C35 C34 113.9(2) . . ? C36 C35 C34 126.1(2) . . ? C37 C36 C35 119.4(3) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C36 C37 C38 119.9(3) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C39 C38 C37 118.9(2) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? N1 C39 C38 121.5(2) . . ? N1 C39 C40 116.4(2) . . ? C38 C39 C40 122.2(2) . . ? N2 C40 C39 111.21(19) . . ? N2 C40 H40A 109.4 . . ? C39 C40 H40A 109.4 . . ? N2 C40 H40B 109.4 . . ? C39 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C42 C41 C46 118.6(2) . . ? C42 C41 N2 122.5(2) . . ? C46 C41 N2 118.9(2) . . ? C41 C42 C43 119.6(3) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C44 C43 C42 122.1(3) . . ? C44 C43 H43 118.9 . . ? C42 C43 H43 118.9 . . ? C43 C44 C45 117.6(3) . . ? C43 C44 C47 121.4(3) . . ? C45 C44 C47 121.0(3) . . ? C46 C45 C44 121.1(3) . . ? C46 C45 H45 119.4 . . ? C44 C45 H45 119.4 . . ? C45 C46 C41 121.0(3) . . ? C45 C46 H46 119.5 . . ? C41 C46 H46 119.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C29 Ru1 P1 C13 84.54(12) . . . . ? N1 Ru1 P1 C13 -176.2(4) . . . . ? P2 Ru1 P1 C13 -2.62(11) . . . . ? Cl1 Ru1 P1 C13 176.41(11) . . . . ? N2 Ru1 P1 C13 -108.96(12) . . . . ? C29 Ru1 P1 C7 -41.82(11) . . . . ? N1 Ru1 P1 C7 57.4(4) . . . . ? P2 Ru1 P1 C7 -128.98(9) . . . . ? Cl1 Ru1 P1 C7 50.04(9) . . . . ? N2 Ru1 P1 C7 124.67(10) . . . . ? C29 Ru1 P1 C1 -158.25(11) . . . . ? N1 Ru1 P1 C1 -59.0(4) . . . . ? P2 Ru1 P1 C1 114.59(9) . . . . ? Cl1 Ru1 P1 C1 -66.38(9) . . . . ? N2 Ru1 P1 C1 8.25(10) . . . . ? C29 Ru1 P2 C23 -171.18(11) . . . . ? N1 Ru1 P2 C23 109.61(11) . . . . ? P1 Ru1 P2 C23 -69.58(10) . . . . ? Cl1 Ru1 P2 C23 132.0(5) . . . . ? N2 Ru1 P2 C23 37.34(11) . . . . ? C29 Ru1 P2 C17 71.29(12) . . . . ? N1 Ru1 P2 C17 -7.92(12) . . . . ? P1 Ru1 P2 C17 172.88(11) . . . . ? Cl1 Ru1 P2 C17 14.5(5) . . . . ? N2 Ru1 P2 C17 -80.20(11) . . . . ? C29 Ru1 P2 C16 -44.77(12) . . . . ? N1 Ru1 P2 C16 -123.98(12) . . . . ? P1 Ru1 P2 C16 56.83(11) . . . . ? Cl1 Ru1 P2 C16 -101.6(5) . . . . ? N2 Ru1 P2 C16 163.75(11) . . . . ? C29 Ru1 N1 C39 -179.4(2) . . . . ? P2 Ru1 N1 C39 -93.66(18) . . . . ? P1 Ru1 N1 C39 80.0(5) . . . . ? Cl1 Ru1 N1 C39 87.35(18) . . . . ? N2 Ru1 N1 C39 10.66(18) . . . . ? C29 Ru1 N1 C35 8.41(16) . . . . ? P2 Ru1 N1 C35 94.16(15) . . . . ? P1 Ru1 N1 C35 -92.2(4) . . . . ? Cl1 Ru1 N1 C35 -84.83(15) . . . . ? N2 Ru1 N1 C35 -161.52(17) . . . . ? C29 Ru1 N2 C41 162.3(2) . . . . ? N1 Ru1 N2 C41 -177.7(2) . . . . ? P2 Ru1 N2 C41 -89.1(2) . . . . ? P1 Ru1 N2 C41 9.3(2) . . . . ? Cl1 Ru1 N2 C41 93.7(2) . . . . ? C29 Ru1 N2 C40 -47.2(2) . . . . ? N1 Ru1 N2 C40 -27.19(15) . . . . ? P2 Ru1 N2 C40 61.48(15) . . . . ? P1 Ru1 N2 C40 159.85(14) . . . . ? Cl1 Ru1 N2 C40 -115.80(15) . . . . ? C13 P1 C1 C6 -139.3(2) . . . . ? C7 P1 C1 C6 -36.8(2) . . . . ? Ru1 P1 C1 C6 91.14(19) . . . . ? C13 P1 C1 C2 39.3(2) . . . . ? C7 P1 C1 C2 141.9(2) . . . . ? Ru1 P1 C1 C2 -90.2(2) . . . . ? C6 C1 C2 C3 0.9(4) . . . . ? P1 C1 C2 C3 -177.8(2) . . . . ? C1 C2 C3 C4 0.8(4) . . . . ? C2 C3 C4 C5 -1.7(4) . . . . ? C3 C4 C5 C6 1.0(4) . . . . ? C2 C1 C6 C5 -1.6(4) . . . . ? P1 C1 C6 C5 177.07(19) . . . . ? C4 C5 C6 C1 0.7(4) . . . . ? C13 P1 C7 C12 -135.7(2) . . . . ? C1 P1 C7 C12 123.8(2) . . . . ? Ru1 P1 C7 C12 -0.4(2) . . . . ? C13 P1 C7 C8 48.2(2) . . . . ? C1 P1 C7 C8 -52.2(2) . . . . ? Ru1 P1 C7 C8 -176.50(18) . . . . ? C12 C7 C8 C9 -0.4(4) . . . . ? P1 C7 C8 C9 175.8(2) . . . . ? C7 C8 C9 C10 0.8(4) . . . . ? C8 C9 C10 C11 0.4(5) . . . . ? C9 C10 C11 C12 -2.1(5) . . . . ? C8 C7 C12 C11 -1.3(4) . . . . ? P1 C7 C12 C11 -177.4(2) . . . . ? C10 C11 C12 C7 2.6(5) . . . . ? C7 P1 C13 C14 68.8(2) . . . . ? C1 P1 C13 C14 169.4(2) . . . . ? Ru1 P1 C13 C14 -65.7(2) . . . . ? P1 C13 C14 C15 99.0(3) . . . . ? C13 C14 C15 C16 -76.6(3) . . . . ? C14 C15 C16 P2 65.3(3) . . . . ? C23 P2 C16 C15 53.2(2) . . . . ? C17 P2 C16 C15 156.1(2) . . . . ? Ru1 P2 C16 C15 -81.2(2) . . . . ? C23 P2 C17 C22 -35.6(3) . . . . ? C16 P2 C17 C22 -139.0(2) . . . . ? Ru1 P2 C17 C22 92.6(2) . . . . ? C23 P2 C17 C18 149.7(2) . . . . ? C16 P2 C17 C18 46.4(2) . . . . ? Ru1 P2 C17 C18 -82.1(2) . . . . ? C22 C17 C18 C19 -0.3(4) . . . . ? P2 C17 C18 C19 174.4(2) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C18 C19 C20 C21 0.5(6) . . . . ? C19 C20 C21 C22 -0.6(7) . . . . ? C20 C21 C22 C17 0.2(6) . . . . ? C18 C17 C22 C21 0.3(5) . . . . ? P2 C17 C22 C21 -174.5(3) . . . . ? C17 P2 C23 C28 120.7(2) . . . . ? C16 P2 C23 C28 -137.7(2) . . . . ? Ru1 P2 C23 C28 -2.6(2) . . . . ? C17 P2 C23 C24 -59.2(2) . . . . ? C16 P2 C23 C24 42.4(3) . . . . ? Ru1 P2 C23 C24 177.45(19) . . . . ? C28 C23 C24 C25 2.2(4) . . . . ? P2 C23 C24 C25 -177.9(2) . . . . ? C23 C24 C25 C26 -1.7(5) . . . . ? C24 C25 C26 C27 0.3(5) . . . . ? C25 C26 C27 C28 0.5(5) . . . . ? C24 C23 C28 C27 -1.4(4) . . . . ? P2 C23 C28 C27 178.7(2) . . . . ? C26 C27 C28 C23 0.1(4) . . . . ? N1 Ru1 C29 C30 175.4(2) . . . . ? P2 Ru1 C29 C30 81.4(2) . . . . ? P1 Ru1 C29 C30 -11.9(2) . . . . ? Cl1 Ru1 C29 C30 -100.8(2) . . . . ? N2 Ru1 C29 C30 -165.31(18) . . . . ? N1 Ru1 C29 C34 -6.77(16) . . . . ? P2 Ru1 C29 C34 -100.75(16) . . . . ? P1 Ru1 C29 C34 165.93(15) . . . . ? Cl1 Ru1 C29 C34 77.04(16) . . . . ? N2 Ru1 C29 C34 12.5(3) . . . . ? C34 C29 C30 C31 -0.4(4) . . . . ? Ru1 C29 C30 C31 177.45(19) . . . . ? C29 C30 C31 C32 0.1(4) . . . . ? C30 C31 C32 C33 -0.1(4) . . . . ? C31 C32 C33 C34 0.4(4) . . . . ? C32 C33 C34 C29 -0.8(4) . . . . ? C32 C33 C34 C35 176.8(2) . . . . ? C30 C29 C34 C33 0.7(3) . . . . ? Ru1 C29 C34 C33 -177.52(18) . . . . ? C30 C29 C34 C35 -177.0(2) . . . . ? Ru1 C29 C34 C35 4.8(3) . . . . ? C39 N1 C35 C36 -0.4(3) . . . . ? Ru1 N1 C35 C36 172.04(18) . . . . ? C39 N1 C35 C34 179.5(2) . . . . ? Ru1 N1 C35 C34 -8.1(2) . . . . ? C33 C34 C35 N1 -175.5(2) . . . . ? C29 C34 C35 N1 2.3(3) . . . . ? C33 C34 C35 C36 4.3(4) . . . . ? C29 C34 C35 C36 -177.9(2) . . . . ? N1 C35 C36 C37 0.4(4) . . . . ? C34 C35 C36 C37 -179.4(3) . . . . ? C35 C36 C37 C38 -0.4(4) . . . . ? C36 C37 C38 C39 0.4(5) . . . . ? C35 N1 C39 C38 0.4(4) . . . . ? Ru1 N1 C39 C38 -171.4(2) . . . . ? C35 N1 C39 C40 -178.8(2) . . . . ? Ru1 N1 C39 C40 9.3(3) . . . . ? C37 C38 C39 N1 -0.4(4) . . . . ? C37 C38 C39 C40 178.8(3) . . . . ? C41 N2 C40 C39 -161.0(2) . . . . ? Ru1 N2 C40 C39 39.9(2) . . . . ? N1 C39 C40 N2 -37.4(3) . . . . ? C38 C39 C40 N2 143.4(3) . . . . ? C40 N2 C41 C42 -35.8(3) . . . . ? Ru1 N2 C41 C42 112.5(3) . . . . ? C40 N2 C41 C46 141.3(2) . . . . ? Ru1 N2 C41 C46 -70.5(3) . . . . ? C46 C41 C42 C43 -0.4(4) . . . . ? N2 C41 C42 C43 176.7(3) . . . . ? C41 C42 C43 C44 -0.4(5) . . . . ? C42 C43 C44 C45 0.7(5) . . . . ? C42 C43 C44 C47 -178.5(3) . . . . ? C43 C44 C45 C46 -0.2(4) . . . . ? C47 C44 C45 C46 179.0(3) . . . . ? C44 C45 C46 C41 -0.6(4) . . . . ? C42 C41 C46 C45 0.9(4) . . . . ? N2 C41 C46 C45 -176.3(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 Cl1 0.87 2.36 3.087(2) 141.4 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.425 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.057