# ic025727y.cif data_js0018 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H106 N4 P2 Ru' _chemical_formula_weight 1526.90 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' _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 11.1136(5) _cell_length_b 12.4931(5) _cell_length_c 16.7167(7) _cell_angle_alpha 71.554(2) _cell_angle_beta 73.964(2) _cell_angle_gamma 73.214(2) _cell_volume 2063.81(15) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 10146 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 11339 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.02 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.986 _reflns_number_total 7184 _reflns_number_gt 6175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement '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^)+(0.0000P)^2^+5.6321P] 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 7184 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1312 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.200 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.321 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.075 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 0.5000 0.5000 0.5000 0.01731(13) Uani 1 2 d S . . P1 P 0.70144(10) 0.48148(9) 0.53045(6) 0.0223(2) Uani 1 1 d . . . N1 N 0.4250(3) 0.4437(3) 0.62941(18) 0.0187(7) Uani 1 1 d . . . N2 N 0.4443(3) 0.6650(3) 0.51725(19) 0.0197(7) Uani 1 1 d . . . C1 C 0.4825(4) 0.2374(3) 0.6336(2) 0.0228(8) Uani 1 1 d . . . H1 H 0.4776 0.1631 0.6714 0.027 Uiso 1 1 calc R . . C2 C 0.4317(4) 0.3292(3) 0.6715(2) 0.0214(8) Uani 1 1 d . . . C3 C 0.3769(4) 0.3166(3) 0.7620(2) 0.0247(9) Uani 1 1 d . . . C4 C 0.3364(4) 0.4243(3) 0.7750(2) 0.0260(9) Uani 1 1 d . . . C5 C 0.3659(4) 0.5063(3) 0.6908(2) 0.0213(8) Uani 1 1 d . . . C6 C 0.3449(4) 0.6273(3) 0.6719(2) 0.0213(8) Uani 1 1 d . . . C7 C 0.3800(4) 0.7025(3) 0.5912(2) 0.0212(8) Uani 1 1 d . . . C8 C 0.3541(4) 0.8290(3) 0.5687(2) 0.0234(9) Uani 1 1 d . . . C9 C 0.4060(4) 0.8638(3) 0.4837(2) 0.0236(9) Uani 1 1 d . . . C10 C 0.4606(4) 0.7614(3) 0.4516(2) 0.0221(8) Uani 1 1 d . . . C11 C 0.2786(5) 0.4468(4) 0.8627(3) 0.0418(12) Uani 1 1 d . . . H11A H 0.2808 0.3729 0.9067 0.063 Uiso 1 1 calc R . . H11B H 0.1895 0.4902 0.8642 0.063 Uiso 1 1 calc R . . H11C H 0.3280 0.4919 0.8742 0.063 Uiso 1 1 calc R . . C12 C 0.2783(4) 0.9113(4) 0.6232(3) 0.0330(10) Uani 1 1 d . . . H12A H 0.2723 0.9911 0.5876 0.050 Uiso 1 1 calc R . . H12B H 0.3213 0.8997 0.6701 0.050 Uiso 1 1 calc R . . H12C H 0.1918 0.8966 0.6474 0.050 Uiso 1 1 calc R . . C13 C 0.3748(5) 0.2025(4) 0.8279(3) 0.0352(11) Uani 1 1 d . . . H13A H 0.3643 0.1465 0.8010 0.042 Uiso 1 1 calc R . . H13B H 0.2998 0.2126 0.8755 0.042 Uiso 1 1 calc R . . C14 C 0.4956(7) 0.1534(5) 0.8645(4) 0.072(2) Uani 1 1 d . . . H14A H 0.5698 0.1391 0.8182 0.108 Uiso 1 1 calc R . . H14B H 0.4880 0.0806 0.9083 0.108 Uiso 1 1 calc R . . H14C H 0.5072 0.2088 0.8907 0.108 Uiso 1 1 calc R . . C15 C 0.4072(4) 0.9849(3) 0.4274(3) 0.0302(10) Uani 1 1 d . . . H15A H 0.4926 0.9856 0.3888 0.036 Uiso 1 1 calc R . . H15B H 0.3935 1.0374 0.4643 0.036 Uiso 1 1 calc R . . C16 C 0.3047(5) 1.0306(4) 0.3728(3) 0.0439(12) Uani 1 1 d . . . H16A H 0.3203 0.9814 0.3339 0.066 Uiso 1 1 calc R . . H16B H 0.3083 1.1100 0.3389 0.066 Uiso 1 1 calc R . . H16C H 0.2198 1.0298 0.4105 0.066 Uiso 1 1 calc R . . C17 C 0.2789(4) 0.6817(3) 0.7461(2) 0.0228(8) Uani 1 1 d . . . C18 C 0.1474(4) 0.7028(3) 0.7736(2) 0.0265(9) Uani 1 1 d . . . H18 H 0.0972 0.6845 0.7442 0.032 Uiso 1 1 calc R . . C19 C 0.0861(4) 0.7502(4) 0.8433(2) 0.0263(9) Uani 1 1 d . . . C20 C 0.1630(4) 0.7779(3) 0.8843(2) 0.0258(9) Uani 1 1 d . . . H20 H 0.1229 0.8105 0.9320 0.031 Uiso 1 1 calc R . . C21 C 0.2959(4) 0.7593(3) 0.8578(2) 0.0228(8) Uani 1 1 d . . . C22 C 0.3534(4) 0.7098(3) 0.7885(2) 0.0239(9) Uani 1 1 d . . . H22 H 0.4441 0.6950 0.7699 0.029 Uiso 1 1 calc R . . C23 C -0.0603(4) 0.7709(4) 0.8724(3) 0.0337(10) Uani 1 1 d . . . C24 C -0.1002(5) 0.6542(5) 0.8988(4) 0.0575(15) Uani 1 1 d . . . H24A H -0.0605 0.6019 0.9466 0.086 Uiso 1 1 calc R . . H24B H -0.0717 0.6198 0.8496 0.086 Uiso 1 1 calc R . . H24C H -0.1939 0.6668 0.9168 0.086 Uiso 1 1 calc R . . C25 C -0.1121(5) 0.8235(5) 0.9493(3) 0.0517(14) Uani 1 1 d . . . H25A H -0.0896 0.8987 0.9342 0.077 Uiso 1 1 calc R . . H25B H -0.0744 0.7717 0.9982 0.077 Uiso 1 1 calc R . . H25C H -0.2057 0.8338 0.9650 0.077 Uiso 1 1 calc R . . C26 C -0.1227(5) 0.8513(6) 0.7985(3) 0.0622(17) Uani 1 1 d . . . H26A H -0.2162 0.8628 0.8168 0.093 Uiso 1 1 calc R . . H26B H -0.0938 0.8170 0.7493 0.093 Uiso 1 1 calc R . . H26C H -0.0984 0.9260 0.7818 0.093 Uiso 1 1 calc R . . C27 C 0.3801(4) 0.7873(4) 0.9045(3) 0.0305(10) Uani 1 1 d . . . C28 C 0.4458(6) 0.6729(5) 0.9590(3) 0.0522(14) Uani 1 1 d . . . H28A H 0.3806 0.6350 1.0019 0.078 Uiso 1 1 calc R . . H28B H 0.5018 0.6882 0.9883 0.078 Uiso 1 1 calc R . . H28C H 0.4972 0.6223 0.9216 0.078 Uiso 1 1 calc R . . C29 C 0.4825(5) 0.8478(5) 0.8388(3) 0.0462(13) Uani 1 1 d . . . H29A H 0.5355 0.8651 0.8693 0.069 Uiso 1 1 calc R . . H29B H 0.4406 0.9200 0.8029 0.069 Uiso 1 1 calc R . . H29C H 0.5370 0.7971 0.8023 0.069 Uiso 1 1 calc R . . C30 C 0.3017(5) 0.8667(5) 0.9632(3) 0.0440(12) Uani 1 1 d . . . H30A H 0.2419 0.8265 1.0097 0.066 Uiso 1 1 calc R . . H30B H 0.2534 0.9372 0.9295 0.066 Uiso 1 1 calc R . . H30C H 0.3598 0.8872 0.9877 0.066 Uiso 1 1 calc R . . C55 C 0.9882(6) 0.8600(5) 0.1540(4) 0.0683(18) Uani 1 1 d . . . H55 H 1.0217 0.9105 0.1019 0.082 Uiso 1 1 calc R . . C56 C 0.8926(6) 0.9044(5) 0.2162(4) 0.0524(14) Uani 1 1 d . . . H56 H 0.8612 0.9856 0.2071 0.063 Uiso 1 1 calc R . . C57 C 0.8445(5) 0.8325(4) 0.2889(3) 0.0364(11) Uani 1 1 d . . . H57 H 0.7778 0.8638 0.3304 0.044 Uiso 1 1 calc R . . C58 C 0.8901(4) 0.7129(4) 0.3052(3) 0.0380(11) Uani 1 1 d . . . C59 C 0.9839(6) 0.6677(5) 0.2415(4) 0.076(2) Uani 1 1 d . . . H59 H 1.0125 0.5865 0.2488 0.092 Uiso 1 1 calc R . . C60 C 1.0335(7) 0.7430(6) 0.1684(4) 0.094(3) Uani 1 1 d . . . H60 H 1.1011 0.7131 0.1268 0.112 Uiso 1 1 calc R . . C69 C 0.8366(4) 0.6365(4) 0.3834(3) 0.0369(11) Uani 1 1 d . . . C70 C 0.7894(4) 0.5739(4) 0.4480(3) 0.0306(10) Uani 1 1 d . . . C71 C 0.8167(4) 0.3418(3) 0.5339(3) 0.0242(9) Uani 1 1 d . . . C72 C 0.8804(5) 0.3133(4) 0.4570(3) 0.0427(12) Uani 1 1 d . . . H72 H 0.8664 0.3673 0.4040 0.051 Uiso 1 1 calc R . . C73 C 0.9642(5) 0.2072(5) 0.4566(3) 0.0535(14) Uani 1 1 d . . . H73 H 1.0058 0.1882 0.4035 0.064 Uiso 1 1 calc R . . C74 C 0.9875(5) 0.1288(4) 0.5329(3) 0.0428(12) Uani 1 1 d . . . H74 H 1.0474 0.0571 0.5326 0.051 Uiso 1 1 calc R . . C75 C 0.9240(6) 0.1553(4) 0.6084(3) 0.0508(14) Uani 1 1 d . . . H75 H 0.9377 0.1006 0.6612 0.061 Uiso 1 1 calc R . . C76 C 0.8391(5) 0.2611(4) 0.6098(3) 0.0472(13) Uani 1 1 d . . . H76 H 0.7961 0.2783 0.6634 0.057 Uiso 1 1 calc R . . C77 C 0.7085(4) 0.5157(4) 0.6275(3) 0.0282(9) Uani 1 1 d . . . C78 C 0.7723(5) 0.5987(4) 0.6237(3) 0.0423(12) Uani 1 1 d . . . H78 H 0.8126 0.6405 0.5697 0.051 Uiso 1 1 calc R . . C79 C 0.7766(6) 0.6196(5) 0.6996(4) 0.0546(15) Uani 1 1 d . . . H79 H 0.8190 0.6771 0.6969 0.066 Uiso 1 1 calc R . . C80 C 0.7208(5) 0.5591(5) 0.7780(4) 0.0545(15) Uani 1 1 d . . . H80 H 0.7260 0.5738 0.8292 0.065 Uiso 1 1 calc R . . C81 C 0.6571(5) 0.4767(5) 0.7831(3) 0.0480(14) Uani 1 1 d . . . H81 H 0.6182 0.4348 0.8375 0.058 Uiso 1 1 calc R . . C82 C 0.6501(4) 0.4552(4) 0.7072(3) 0.0360(11) Uani 1 1 d . . . H82 H 0.6054 0.3993 0.7102 0.043 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 0.0206(3) 0.0188(2) 0.0122(2) -0.00456(17) -0.00141(17) - 0.00517(18) P1 0.0246(6) 0.0233(5) 0.0195(5) -0.0053(4) -0.0034(4) -0.0074(4) N1 0.0223(17) 0.0202(16) 0.0134(15) -0.0058(13) -0.0022(13) -0.0042(13) N2 0.0228(18) 0.0215(16) 0.0145(15) -0.0038(13) -0.0019(13) -0.0068(14) C1 0.031(2) 0.0197(19) 0.0171(19) -0.0008(16) -0.0058(17) -0.0088(17) C2 0.026(2) 0.023(2) 0.0149(18) -0.0034(16) -0.0036(16) -0.0064(17) C3 0.032(2) 0.027(2) 0.0148(19) -0.0036(16) -0.0012(17) -0.0115(18) C4 0.032(2) 0.028(2) 0.0156(19) -0.0044(17) -0.0010(17) -0.0093(18) C5 0.023(2) 0.026(2) 0.0153(18) -0.0071(16) -0.0011(16) -0.0065(17) C6 0.022(2) 0.026(2) 0.0172(19) -0.0076(16) -0.0022(16) -0.0065(16) C7 0.023(2) 0.022(2) 0.0201(19) -0.0077(16) -0.0041(16) -0.0051(16) C8 0.027(2) 0.022(2) 0.022(2) -0.0085(16) -0.0038(17) -0.0048(17) C9 0.026(2) 0.021(2) 0.024(2) -0.0067(16) -0.0039(17) -0.0057(17) C10 0.026(2) 0.022(2) 0.0190(19) -0.0058(16) -0.0052(16) -0.0057(17) C11 0.070(4) 0.030(2) 0.018(2) -0.0058(19) 0.003(2) -0.012(2) C12 0.044(3) 0.025(2) 0.026(2) -0.0110(18) 0.000(2) -0.002(2) C13 0.057(3) 0.028(2) 0.019(2) -0.0047(18) -0.001(2) -0.014(2) C14 0.125(6) 0.041(3) 0.066(4) 0.013(3) -0.067(4) -0.024(3) C15 0.041(3) 0.022(2) 0.025(2) -0.0065(17) -0.0032(19) -0.0060(19) C16 0.042(3) 0.034(3) 0.040(3) 0.002(2) -0.003(2) -0.001(2) C17 0.027(2) 0.022(2) 0.0161(19) -0.0039(16) -0.0016(16) -0.0038(17) C18 0.028(2) 0.031(2) 0.020(2) -0.0077(17) -0.0009(17) -0.0091(18) C19 0.026(2) 0.031(2) 0.020(2) -0.0075(17) 0.0011(17) -0.0088(18) C20 0.029(2) 0.030(2) 0.0176(19) -0.0108(17) 0.0001(17) -0.0041(18) C21 0.025(2) 0.026(2) 0.0169(19) -0.0052(16) -0.0030(16) -0.0071(17) C22 0.025(2) 0.025(2) 0.020(2) -0.0071(16) -0.0033(17) -0.0041(17) C23 0.026(2) 0.050(3) 0.025(2) -0.013(2) 0.0019(18) -0.011(2) C24 0.046(3) 0.077(4) 0.057(3) -0.028(3) 0.014(3) -0.035(3) C25 0.033(3) 0.081(4) 0.044(3) -0.033(3) 0.010(2) -0.015(3) C26 0.031(3) 0.100(5) 0.042(3) -0.014(3) -0.007(2) 0.003(3) C27 0.032(2) 0.042(3) 0.023(2) -0.0160(19) -0.0059(18) -0.007(2) C28 0.061(4) 0.055(3) 0.048(3) -0.017(3) -0.031(3) -0.001(3) C29 0.043(3) 0.064(3) 0.044(3) -0.026(3) 0.004(2) -0.030(3) C30 0.041(3) 0.063(3) 0.042(3) -0.033(3) -0.007(2) -0.012(2) C55 0.078(5) 0.052(4) 0.049(3) 0.011(3) 0.003(3) -0.019(3) C56 0.057(4) 0.038(3) 0.058(3) -0.002(3) -0.013(3) -0.015(3) C57 0.040(3) 0.031(2) 0.037(3) -0.008(2) -0.006(2) -0.008(2) C58 0.030(3) 0.041(3) 0.037(3) -0.001(2) -0.003(2) -0.013(2) C59 0.058(4) 0.041(3) 0.071(4) 0.010(3) 0.034(3) 0.006(3) C60 0.082(5) 0.066(4) 0.066(4) 0.009(3) 0.032(4) 0.009(4) C69 0.034(3) 0.039(3) 0.036(3) -0.010(2) -0.005(2) -0.008(2) C70 0.029(2) 0.031(2) 0.031(2) -0.002(2) -0.0063(19) -0.0108(19) C71 0.021(2) 0.027(2) 0.026(2) -0.0079(17) -0.0047(17) -0.0063(17) C72 0.053(3) 0.040(3) 0.028(2) -0.010(2) -0.008(2) 0.003(2) C73 0.057(4) 0.051(3) 0.042(3) -0.022(3) -0.004(3) 0.010(3) C74 0.036(3) 0.035(3) 0.059(3) -0.019(2) -0.015(2) 0.001(2) C75 0.069(4) 0.031(3) 0.044(3) -0.002(2) -0.023(3) 0.004(2) C76 0.065(4) 0.035(3) 0.030(3) -0.007(2) -0.006(2) 0.001(2) C77 0.029(2) 0.030(2) 0.027(2) -0.0120(18) -0.0120(18) 0.0015(18) C78 0.050(3) 0.034(3) 0.052(3) -0.015(2) -0.024(2) -0.006(2) C79 0.063(4) 0.046(3) 0.075(4) -0.031(3) -0.041(3) 0.001(3) C80 0.046(3) 0.077(4) 0.054(4) -0.046(3) -0.025(3) 0.012(3) C81 0.035(3) 0.081(4) 0.032(3) -0.029(3) -0.011(2) 0.001(3) C82 0.026(2) 0.055(3) 0.031(2) -0.019(2) -0.0065(19) -0.005(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 N1 2.061(3) . ? Ru1 N1 2.061(3) 2_666 ? Ru1 N2 2.063(3) . ? Ru1 N2 2.063(3) 2_666 ? Ru1 P1 2.3623(10) . ? Ru1 P1 2.3623(10) 2_666 ? P1 C70 1.757(4) . ? P1 C77 1.830(4) . ? P1 C71 1.837(4) . ? N1 C2 1.370(5) . ? N1 C5 1.392(5) . ? N2 C10 1.367(5) . ? N2 C7 1.395(5) . ? C1 C2 1.386(5) . ? C1 C10 1.387(5) 2_666 ? C1 H1 0.9500 . ? C2 C3 1.443(5) . ? C3 C4 1.357(6) . ? C3 C13 1.502(5) . ? C4 C5 1.472(5) . ? C4 C11 1.509(5) . ? C5 C6 1.404(5) . ? C6 C7 1.404(5) . ? C6 C17 1.511(5) . ? C7 C8 1.465(5) . ? C8 C9 1.357(5) . ? C8 C12 1.504(5) . ? C9 C10 1.448(5) . ? C9 C15 1.510(5) . ? C10 C1 1.387(5) 2_666 ? 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 1.514(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.524(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.378(6) . ? C17 C22 1.400(5) . ? C18 C19 1.391(5) . ? C18 H18 0.9500 . ? C19 C20 1.402(6) . ? C19 C23 1.533(6) . ? C20 C21 1.392(6) . ? C20 H20 0.9500 . ? C21 C22 1.397(5) . ? C21 C27 1.539(5) . ? C22 H22 0.9500 . ? C23 C26 1.516(7) . ? C23 C25 1.524(6) . ? C23 C24 1.542(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.532(7) . ? C27 C30 1.532(6) . ? C27 C29 1.535(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C55 C60 1.366(9) . ? C55 C56 1.390(8) . ? C55 H55 0.9500 . ? C56 C57 1.341(7) . ? C56 H56 0.9500 . ? C57 C58 1.394(6) . ? C57 H57 0.9500 . ? C58 C59 1.403(7) . ? C58 C69 1.443(6) . ? C59 C60 1.372(8) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C69 C70 1.201(6) . ? C71 C76 1.381(6) . ? C71 C72 1.385(6) . ? C72 C73 1.384(7) . ? C72 H72 0.9500 . ? C73 C74 1.378(7) . ? C73 H73 0.9500 . ? C74 C75 1.355(7) . ? C74 H74 0.9500 . ? C75 C76 1.387(7) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C82 1.391(6) . ? C77 C78 1.392(6) . ? C78 C79 1.389(7) . ? C78 H78 0.9500 . ? C79 C80 1.368(8) . ? C79 H79 0.9500 . ? C80 C81 1.379(8) . ? C80 H80 0.9500 . ? C81 C82 1.403(6) . ? C81 H81 0.9500 . ? C82 H82 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 N1 180.000(1) . 2_666 ? N1 Ru1 N2 86.91(11) . . ? N1 Ru1 N2 93.09(11) 2_666 . ? N1 Ru1 N2 93.09(11) . 2_666 ? N1 Ru1 N2 86.91(11) 2_666 2_666 ? N2 Ru1 N2 180.00(16) . 2_666 ? N1 Ru1 P1 90.62(9) . . ? N1 Ru1 P1 89.38(9) 2_666 . ? N2 Ru1 P1 89.28(9) . . ? N2 Ru1 P1 90.72(9) 2_666 . ? N1 Ru1 P1 89.38(9) . 2_666 ? N1 Ru1 P1 90.62(9) 2_666 2_666 ? N2 Ru1 P1 90.72(9) . 2_666 ? N2 Ru1 P1 89.28(9) 2_666 2_666 ? P1 Ru1 P1 180.000(1) . 2_666 ? C70 P1 C77 102.6(2) . . ? C70 P1 C71 100.7(2) . . ? C77 P1 C71 102.84(18) . . ? C70 P1 Ru1 110.77(15) . . ? C77 P1 Ru1 119.65(14) . . ? C71 P1 Ru1 117.70(13) . . ? C2 N1 C5 106.9(3) . . ? C2 N1 Ru1 123.1(2) . . ? C5 N1 Ru1 129.9(2) . . ? C10 N2 C7 107.1(3) . . ? C10 N2 Ru1 123.2(2) . . ? C7 N2 Ru1 129.7(2) . . ? C2 C1 C10 129.2(4) . 2_666 ? C2 C1 H1 115.4 . . ? C10 C1 H1 115.4 2_666 . ? N1 C2 C1 125.7(3) . . ? N1 C2 C3 110.3(3) . . ? C1 C2 C3 124.1(3) . . ? C4 C3 C2 107.4(3) . . ? C4 C3 C13 128.2(4) . . ? C2 C3 C13 124.4(4) . . ? C3 C4 C5 107.1(3) . . ? C3 C4 C11 123.2(4) . . ? C5 C4 C11 129.6(4) . . ? N1 C5 C6 123.4(3) . . ? N1 C5 C4 108.4(3) . . ? C6 C5 C4 128.2(3) . . ? C5 C6 C7 126.6(3) . . ? C5 C6 C17 116.6(3) . . ? C7 C6 C17 116.8(3) . . ? N2 C7 C6 123.5(3) . . ? N2 C7 C8 108.7(3) . . ? C6 C7 C8 127.8(3) . . ? C9 C8 C7 106.8(3) . . ? C9 C8 C12 123.6(4) . . ? C7 C8 C12 129.5(3) . . ? C8 C9 C10 107.8(3) . . ? C8 C9 C15 129.1(4) . . ? C10 C9 C15 123.2(3) . . ? N2 C10 C1 125.7(3) . 2_666 ? N2 C10 C9 109.7(3) . . ? C1 C10 C9 124.6(3) 2_666 . ? C4 C11 H11A 109.5 . . ? C4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 C14 112.8(4) . . ? C3 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? C3 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? 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 . . ? C9 C15 C16 113.0(4) . . ? C9 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? C9 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 119.4(3) . . ? C18 C17 C6 121.5(3) . . ? C22 C17 C6 119.1(3) . . ? C17 C18 C19 121.9(4) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C18 C19 C20 117.5(4) . . ? C18 C19 C23 120.1(4) . . ? C20 C19 C23 122.4(3) . . ? C21 C20 C19 122.4(3) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 118.1(4) . . ? C20 C21 C27 122.1(3) . . ? C22 C21 C27 119.8(4) . . ? C21 C22 C17 120.8(4) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? C26 C23 C25 108.3(4) . . ? C26 C23 C19 109.6(4) . . ? C25 C23 C19 113.5(4) . . ? C26 C23 C24 109.0(4) . . ? C25 C23 C24 107.5(4) . . ? C19 C23 C24 108.9(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C30 109.2(4) . . ? C28 C27 C29 109.4(4) . . ? C30 C27 C29 107.8(4) . . ? C28 C27 C21 107.9(4) . . ? C30 C27 C21 112.4(4) . . ? C29 C27 C21 110.3(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C60 C55 C56 119.3(5) . . ? C60 C55 H55 120.4 . . ? C56 C55 H55 120.4 . . ? C57 C56 C55 120.0(5) . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C56 C57 C58 121.6(5) . . ? C56 C57 H57 119.2 . . ? C58 C57 H57 119.2 . . ? C57 C58 C59 118.5(4) . . ? C57 C58 C69 121.0(4) . . ? C59 C58 C69 120.4(4) . . ? C60 C59 C58 118.7(5) . . ? C60 C59 H59 120.6 . . ? C58 C59 H59 120.6 . . ? C55 C60 C59 121.7(6) . . ? C55 C60 H60 119.1 . . ? C59 C60 H60 119.1 . . ? C70 C69 C58 178.5(5) . . ? C69 C70 P1 169.1(4) . . ? C76 C71 C72 118.1(4) . . ? C76 C71 P1 123.1(3) . . ? C72 C71 P1 118.8(3) . . ? C73 C72 C71 120.8(4) . . ? C73 C72 H72 119.6 . . ? C71 C72 H72 119.6 . . ? C74 C73 C72 120.3(5) . . ? C74 C73 H73 119.8 . . ? C72 C73 H73 119.8 . . ? C75 C74 C73 119.2(5) . . ? C75 C74 H74 120.4 . . ? C73 C74 H74 120.4 . . ? C74 C75 C76 121.1(5) . . ? C74 C75 H75 119.5 . . ? C76 C75 H75 119.5 . . ? C71 C76 C75 120.5(4) . . ? C71 C76 H76 119.8 . . ? C75 C76 H76 119.8 . . ? C82 C77 C78 119.5(4) . . ? C82 C77 P1 118.6(3) . . ? C78 C77 P1 121.9(3) . . ? C79 C78 C77 119.4(5) . . ? C79 C78 H78 120.3 . . ? C77 C78 H78 120.3 . . ? C80 C79 C78 121.2(5) . . ? C80 C79 H79 119.4 . . ? C78 C79 H79 119.4 . . ? C79 C80 C81 120.2(5) . . ? C79 C80 H80 119.9 . . ? C81 C80 H80 119.9 . . ? C80 C81 C82 119.6(5) . . ? C80 C81 H81 120.2 . . ? C82 C81 H81 120.2 . . ? C77 C82 C81 120.1(5) . . ? C77 C82 H82 119.9 . . ? C81 C82 H82 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ru1 P1 C70 -155.12(18) . . . . ? N1 Ru1 P1 C70 24.88(18) 2_666 . . . ? N2 Ru1 P1 C70 -68.22(18) . . . . ? N2 Ru1 P1 C70 111.78(18) 2_666 . . . ? N1 Ru1 P1 C77 -36.11(18) . . . . ? N1 Ru1 P1 C77 143.89(18) 2_666 . . . ? N2 Ru1 P1 C77 50.79(18) . . . . ? N2 Ru1 P1 C77 -129.21(18) 2_666 . . . ? N1 Ru1 P1 C71 89.87(17) . . . . ? N1 Ru1 P1 C71 -90.13(17) 2_666 . . . ? N2 Ru1 P1 C71 176.77(17) . . . . ? N2 Ru1 P1 C71 -3.23(17) 2_666 . . . ? N2 Ru1 N1 C2 -177.0(3) . . . . ? N2 Ru1 N1 C2 3.0(3) 2_666 . . . ? P1 Ru1 N1 C2 -87.7(3) . . . . ? P1 Ru1 N1 C2 92.3(3) 2_666 . . . ? N2 Ru1 N1 C5 -0.1(3) . . . . ? N2 Ru1 N1 C5 179.9(3) 2_666 . . . ? P1 Ru1 N1 C5 89.1(3) . . . . ? P1 Ru1 N1 C5 -90.9(3) 2_666 . . . ? N1 Ru1 N2 C10 -177.9(3) . . . . ? N1 Ru1 N2 C10 2.1(3) 2_666 . . . ? P1 Ru1 N2 C10 91.4(3) . . . . ? P1 Ru1 N2 C10 -88.6(3) 2_666 . . . ? N1 Ru1 N2 C7 -1.8(3) . . . . ? N1 Ru1 N2 C7 178.2(3) 2_666 . . . ? P1 Ru1 N2 C7 -92.4(3) . . . . ? P1 Ru1 N2 C7 87.6(3) 2_666 . . . ? C5 N1 C2 C1 179.1(4) . . . . ? Ru1 N1 C2 C1 -3.4(5) . . . . ? C5 N1 C2 C3 -0.4(4) . . . . ? Ru1 N1 C2 C3 177.0(3) . . . . ? C10 C1 C2 N1 1.9(7) 2_666 . . . ? C10 C1 C2 C3 -178.6(4) 2_666 . . . ? N1 C2 C3 C4 0.2(5) . . . . ? C1 C2 C3 C4 -179.4(4) . . . . ? N1 C2 C3 C13 -176.6(4) . . . . ? C1 C2 C3 C13 3.8(7) . . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C13 C3 C4 C5 176.8(4) . . . . ? C2 C3 C4 C11 -177.2(4) . . . . ? C13 C3 C4 C11 -0.6(7) . . . . ? C2 N1 C5 C6 178.5(4) . . . . ? Ru1 N1 C5 C6 1.3(6) . . . . ? C2 N1 C5 C4 0.5(4) . . . . ? Ru1 N1 C5 C4 -176.7(3) . . . . ? C3 C4 C5 N1 -0.4(5) . . . . ? C11 C4 C5 N1 176.8(4) . . . . ? C3 C4 C5 C6 -178.3(4) . . . . ? C11 C4 C5 C6 -1.1(7) . . . . ? N1 C5 C6 C7 -0.8(6) . . . . ? C4 C5 C6 C7 176.7(4) . . . . ? N1 C5 C6 C17 179.7(3) . . . . ? C4 C5 C6 C17 -2.7(6) . . . . ? C10 N2 C7 C6 179.2(4) . . . . ? Ru1 N2 C7 C6 2.6(5) . . . . ? C10 N2 C7 C8 0.9(4) . . . . ? Ru1 N2 C7 C8 -175.7(3) . . . . ? C5 C6 C7 N2 -1.1(6) . . . . ? C17 C6 C7 N2 178.3(3) . . . . ? C5 C6 C7 C8 176.9(4) . . . . ? C17 C6 C7 C8 -3.7(6) . . . . ? N2 C7 C8 C9 -1.7(4) . . . . ? C6 C7 C8 C9 -180.0(4) . . . . ? N2 C7 C8 C12 174.4(4) . . . . ? C6 C7 C8 C12 -3.8(7) . . . . ? C7 C8 C9 C10 1.8(4) . . . . ? C12 C8 C9 C10 -174.6(4) . . . . ? C7 C8 C9 C15 179.9(4) . . . . ? C12 C8 C9 C15 3.5(7) . . . . ? C7 N2 C10 C1 -178.2(4) . . . 2_666 ? Ru1 N2 C10 C1 -1.3(5) . . . 2_666 ? C7 N2 C10 C9 0.2(4) . . . . ? Ru1 N2 C10 C9 177.1(2) . . . . ? C8 C9 C10 N2 -1.3(5) . . . . ? C15 C9 C10 N2 -179.6(4) . . . . ? C8 C9 C10 C1 177.1(4) . . . 2_666 ? C15 C9 C10 C1 -1.1(6) . . . 2_666 ? C4 C3 C13 C14 -89.2(6) . . . . ? C2 C3 C13 C14 86.8(5) . . . . ? C8 C9 C15 C16 -99.7(5) . . . . ? C10 C9 C15 C16 78.1(5) . . . . ? C5 C6 C17 C18 -81.4(5) . . . . ? C7 C6 C17 C18 99.1(4) . . . . ? C5 C6 C17 C22 97.8(4) . . . . ? C7 C6 C17 C22 -81.7(5) . . . . ? C22 C17 C18 C19 -0.8(6) . . . . ? C6 C17 C18 C19 178.3(4) . . . . ? C17 C18 C19 C20 1.0(6) . . . . ? C17 C18 C19 C23 -179.3(4) . . . . ? C18 C19 C20 C21 -0.1(6) . . . . ? C23 C19 C20 C21 -179.9(4) . . . . ? C19 C20 C21 C22 -0.9(6) . . . . ? C19 C20 C21 C27 -178.6(4) . . . . ? C20 C21 C22 C17 1.1(6) . . . . ? C27 C21 C22 C17 178.8(4) . . . . ? C18 C17 C22 C21 -0.3(6) . . . . ? C6 C17 C22 C21 -179.5(3) . . . . ? C18 C19 C23 C26 -58.7(6) . . . . ? C20 C19 C23 C26 121.1(5) . . . . ? C18 C19 C23 C25 -179.9(4) . . . . ? C20 C19 C23 C25 -0.2(6) . . . . ? C18 C19 C23 C24 60.5(5) . . . . ? C20 C19 C23 C24 -119.8(4) . . . . ? C20 C21 C27 C28 104.0(5) . . . . ? C22 C21 C27 C28 -73.6(5) . . . . ? C20 C21 C27 C30 -16.3(6) . . . . ? C22 C21 C27 C30 166.1(4) . . . . ? C20 C21 C27 C29 -136.6(4) . . . . ? C22 C21 C27 C29 45.8(5) . . . . ? C60 C55 C56 C57 -0.9(10) . . . . ? C55 C56 C57 C58 1.4(8) . . . . ? C56 C57 C58 C59 -3.3(8) . . . . ? C56 C57 C58 C69 -179.4(5) . . . . ? C57 C58 C59 C60 4.6(10) . . . . ? C69 C58 C59 C60 -179.3(7) . . . . ? C56 C55 C60 C59 2.4(13) . . . . ? C58 C59 C60 C55 -4.2(13) . . . . ? C77 P1 C70 C69 -151(2) . . . . ? C71 P1 C70 C69 103(2) . . . . ? Ru1 P1 C70 C69 -22(2) . . . . ? C70 P1 C71 C76 137.5(4) . . . . ? C77 P1 C71 C76 31.8(4) . . . . ? Ru1 P1 C71 C76 -102.0(4) . . . . ? C70 P1 C71 C72 -45.4(4) . . . . ? C77 P1 C71 C72 -151.1(4) . . . . ? Ru1 P1 C71 C72 75.1(4) . . . . ? C76 C71 C72 C73 -0.2(7) . . . . ? P1 C71 C72 C73 -177.4(4) . . . . ? C71 C72 C73 C74 -1.3(8) . . . . ? C72 C73 C74 C75 2.4(8) . . . . ? C73 C74 C75 C76 -2.0(8) . . . . ? C72 C71 C76 C75 0.5(8) . . . . ? P1 C71 C76 C75 177.7(4) . . . . ? C74 C75 C76 C71 0.5(9) . . . . ? C70 P1 C77 C82 -178.4(3) . . . . ? C71 P1 C77 C82 -74.2(4) . . . . ? Ru1 P1 C77 C82 58.5(4) . . . . ? C70 P1 C77 C78 0.4(4) . . . . ? C71 P1 C77 C78 104.6(4) . . . . ? Ru1 P1 C77 C78 -122.7(3) . . . . ? C82 C77 C78 C79 0.0(7) . . . . ? P1 C77 C78 C79 -178.8(4) . . . . ? C77 C78 C79 C80 1.0(8) . . . . ? C78 C79 C80 C81 -1.0(8) . . . . ? C79 C80 C81 C82 0.1(8) . . . . ? C78 C77 C82 C81 -0.9(7) . . . . ? P1 C77 C82 C81 178.0(4) . . . . ? C80 C81 C82 C77 0.8(7) . . . . ? #===END ## Synthesis of phosphine and phosphonite complexes of a Ru(II) porphyrin ## ## E. Stulz, M. Maue, N. Feeder, S. Teat, Y.-F. Ng, A. D. Bond, S. Darling & J. K. M. Sanders ## ## Denoted (DPAP)2Ru(DPP) (monoclinic form) in text ## data_js0016 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H106 N4 P2 Ru' _chemical_formula_weight 1526.90 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' _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 22.920(5) _cell_length_b 20.254(5) _cell_length_c 18.366(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.44(1) _cell_angle_gamma 90.00 _cell_volume 8326(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7233 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.37 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 0.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9836 _exptl_absorpt_correction_T_max 0.9945 _exptl_absorpt_process_details ; Correction applied by SADABS - note that the transmission factors are not real since they include corrections for beam decay and possibly crystal decay (the two cannot be distinguished). The numbers listed in the CIF are those calculated by SHELXL. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6929 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS, Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'Thin slice \w-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_reflns_number 13361 _diffrn_reflns_av_R_equivalents 0.2070 _diffrn_reflns_av_sigmaI/netI 0.1489 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 20.27 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 20.27 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 4335 _reflns_number_gt 2856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker AXS, 1994)' _computing_cell_refinement 'Bruker SAINT (Bruker AXS, 1994)' _computing_data_reduction 'Bruker SAINT (Bruker AXS, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1996)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4335 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2451 _refine_ls_R_factor_gt 0.2036 _refine_ls_wR_factor_ref 0.5064 _refine_ls_wR_factor_gt 0.4681 _refine_ls_goodness_of_fit_ref 1.822 _refine_ls_restrained_S_all 1.822 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 7.736 _refine_diff_density_min -7.001 _refine_diff_density_rms 0.293 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 0.2500 0.2500 0.0000 0.0176(9) Uiso 1 2 d S . . P1 P 0.2194(2) 0.1440(2) -0.0425(3) 0.0282(14) Uiso 1 1 d . . . N1 N 0.2146(6) 0.2848(6) -0.1061(8) 0.022(3) Uiso 1 1 d . . . N2 N 0.1687(6) 0.2627(6) 0.0310(8) 0.017(3) Uiso 1 1 d . . . C1 C 0.2416(7) 0.2892(8) -0.1680(10) 0.021(4) Uiso 1 1 d . . . C2 C 0.1993(8) 0.3158(9) -0.2283(11) 0.030(5) Uiso 1 1 d . . . C3 C 0.1471(7) 0.3265(8) -0.2067(10) 0.022(4) Uiso 1 1 d . . . C4 C 0.1581(7) 0.3060(8) -0.1288(10) 0.024(4) Uiso 1 1 d . . . C5 C 0.1146(8) 0.3059(8) -0.0851(10) 0.028(4) Uiso 1 1 d . . . H5A H 0.0767 0.3234 -0.1081 0.033 Uiso 1 1 calc R . . C6 C 0.1200(7) 0.2836(8) -0.0134(10) 0.019(4) Uiso 1 1 d . . . C7 C 0.0700(7) 0.2879(8) 0.0263(10) 0.026(4) Uiso 1 1 d . . . C8 C 0.0933(8) 0.2679(8) 0.0979(11) 0.024(4) Uiso 1 1 d . . . C9 C 0.1553(7) 0.2499(7) 0.1048(10) 0.019(4) Uiso 1 1 d . . . C10 C 0.1978(7) 0.2292(8) 0.1635(10) 0.020(4) Uiso 1 1 d . . . C11 C 0.2055(9) 0.3320(10) -0.3081(12) 0.047(6) Uiso 1 1 d . . . H11A H 0.1677 0.3498 -0.3365 0.071 Uiso 1 1 calc R . . H11B H 0.2156 0.2917 -0.3323 0.071 Uiso 1 1 calc R . . H11C H 0.2372 0.3648 -0.3063 0.071 Uiso 1 1 calc R . . C12 C 0.0566(10) 0.2656(11) 0.1578(13) 0.047(6) Uiso 1 1 d . . . H12A H 0.0158 0.2807 0.1367 0.070 Uiso 1 1 calc R . . H12B H 0.0749 0.2943 0.1994 0.070 Uiso 1 1 calc R . . H12C H 0.0554 0.2202 0.1758 0.070 Uiso 1 1 calc R . . C13 C 0.0891(9) 0.3574(9) -0.2485(12) 0.043(5) Uiso 1 1 d . . . H13A H 0.0548 0.3342 -0.2352 0.052 Uiso 1 1 calc R . . H13B H 0.0859 0.3525 -0.3028 0.052 Uiso 1 1 calc R . . C14 C 0.0872(11) 0.4310(11) -0.2286(15) 0.064(7) Uiso 1 1 d . . . H14A H 0.0497 0.4503 -0.2559 0.096 Uiso 1 1 calc R . . H14B H 0.1210 0.4538 -0.2423 0.096 Uiso 1 1 calc R . . H14C H 0.0898 0.4356 -0.1749 0.096 Uiso 1 1 calc R . . C15 C 0.0072(10) 0.3104(11) -0.0065(14) 0.054(6) Uiso 1 1 d . . . H15A H -0.0207 0.2880 0.0197 0.065 Uiso 1 1 calc R . . H15B H -0.0036 0.2974 -0.0597 0.065 Uiso 1 1 calc R . . C16 C 0.0002(13) 0.3859(14) -0.0002(18) 0.088(9) Uiso 1 1 d . . . H16A H -0.0410 0.3986 -0.0230 0.132 Uiso 1 1 calc R . . H16B H 0.0277 0.4083 -0.0262 0.132 Uiso 1 1 calc R . . H16C H 0.0094 0.3988 0.0524 0.132 Uiso 1 1 calc R . . C17 C 0.1784(8) 0.2263(8) 0.2370(11) 0.025(4) Uiso 1 1 d . . . C18 C 0.1831(8) 0.2807(9) 0.2803(11) 0.032(5) Uiso 1 1 d . . . H18A H 0.1975 0.3203 0.2627 0.039 Uiso 1 1 calc R . . C19 C 0.1678(8) 0.2815(9) 0.3499(10) 0.028(4) Uiso 1 1 d . . . C20 C 0.1478(8) 0.2233(9) 0.3732(12) 0.033(5) Uiso 1 1 d . . . H20A H 0.1401 0.2217 0.4220 0.040 Uiso 1 1 calc R . . C21 C 0.1379(8) 0.1664(9) 0.3299(12) 0.036(5) Uiso 1 1 d . . . C22 C 0.1539(7) 0.1695(9) 0.2592(10) 0.027(4) Uiso 1 1 d . . . H22A H 0.1477 0.1321 0.2271 0.033 Uiso 1 1 calc R . . C23 C 0.1739(10) 0.3452(11) 0.3978(13) 0.052(6) Uiso 1 1 d . . . C24 C 0.1704(10) 0.3334(12) 0.4781(13) 0.056(6) Uiso 1 1 d . . . H24A H 0.2062 0.3098 0.5039 0.084 Uiso 1 1 calc R . . H24B H 0.1349 0.3070 0.4796 0.084 Uiso 1 1 calc R . . H24C H 0.1678 0.3759 0.5027 0.084 Uiso 1 1 calc R . . C25 C 0.1204(19) 0.386(2) 0.361(3) 0.151(16) Uiso 1 1 d . . . H25A H 0.0836 0.3617 0.3618 0.226 Uiso 1 1 calc R . . H25B H 0.1224 0.3946 0.3086 0.226 Uiso 1 1 calc R . . H25C H 0.1204 0.4280 0.3871 0.226 Uiso 1 1 calc R . . C26 C 0.226(2) 0.385(2) 0.393(3) 0.155(16) Uiso 1 1 d . . . H26A H 0.2624 0.3616 0.4166 0.232 Uiso 1 1 calc R . . H26B H 0.2239 0.4274 0.4180 0.232 Uiso 1 1 calc R . . H26C H 0.2262 0.3930 0.3402 0.232 Uiso 1 1 calc R . . C27 C 0.1159(10) 0.1040(12) 0.3600(14) 0.058(6) Uiso 1 1 d . . . C28 C 0.1682(18) 0.081(2) 0.433(2) 0.149(16) Uiso 1 1 d . . . H28A H 0.1554 0.0400 0.4543 0.223 Uiso 1 1 calc R . . H28B H 0.1741 0.1155 0.4711 0.223 Uiso 1 1 calc R . . H28C H 0.2058 0.0725 0.4175 0.223 Uiso 1 1 calc R . . C29 C 0.1208(19) 0.0472(19) 0.319(2) 0.134(14) Uiso 1 1 d . . . H29A H 0.0926 0.0497 0.2706 0.201 Uiso 1 1 calc R . . H29B H 0.1118 0.0084 0.3463 0.201 Uiso 1 1 calc R . . H29C H 0.1616 0.0437 0.3108 0.201 Uiso 1 1 calc R . . C30 C 0.0713(16) 0.1152(18) 0.402(2) 0.110(11) Uiso 1 1 d . . . H30A H 0.0342 0.1295 0.3686 0.164 Uiso 1 1 calc R . . H30B H 0.0850 0.1495 0.4395 0.164 Uiso 1 1 calc R . . H30C H 0.0641 0.0742 0.4271 0.164 Uiso 1 1 calc R . . C31 C 0.1653(7) 0.1446(8) -0.1265(10) 0.025(4) Uiso 1 1 d . A . C32 C 0.1363(8) 0.1475(9) -0.1870(12) 0.037(5) Uiso 1 1 d . . . C33 C 0.1022(9) 0.1600(14) -0.2583(11) 0.021(9) Uiso 0.50 1 d PG A 1 C34 C 0.1270(8) 0.1408(15) -0.3176(14) 0.042(11) Uiso 0.50 1 d PG A 1 H34A H 0.1665 0.1236 -0.3085 0.051 Uiso 0.50 1 calc PR A 1 C35 C 0.0941(11) 0.1467(15) -0.3903(12) 0.038(10) Uiso 0.50 1 d PG A 1 H35A H 0.1110 0.1335 -0.4309 0.046 Uiso 0.50 1 calc PR A 1 C36 C 0.0363(10) 0.1718(15) -0.4036(11) 0.046(11) Uiso 0.50 1 d PG A 1 H36A H 0.0138 0.1758 -0.4533 0.056 Uiso 0.50 1 calc PR A 1 C37 C 0.0115(8) 0.1910(13) -0.3443(13) 0.044(11) Uiso 0.50 1 d PG A 1 H37A H -0.0280 0.2082 -0.3534 0.053 Uiso 0.50 1 calc PR A 1 C38 C 0.0444(9) 0.1851(12) -0.2716(12) 0.028(9) Uiso 0.50 1 d PG A 1 H38A H 0.0274 0.1982 -0.2310 0.033 Uiso 0.50 1 calc PR A 1 C33' C 0.0992(10) 0.1351(14) -0.2718(11) 0.033(11) Uiso 0.50 1 d PG A 2 C34' C 0.1175(10) 0.1743(14) -0.3248(15) 0.029(9) Uiso 0.50 1 d PG A 2 H34B H 0.1521 0.2011 -0.3110 0.034 Uiso 0.50 1 calc PR A 2 C35' C 0.0851(12) 0.1742(15) -0.3981(14) 0.066(16) Uiso 0.50 1 d PG A 2 H35B H 0.0977 0.2010 -0.4344 0.080 Uiso 0.50 1 calc PR A 2 C36' C 0.0345(12) 0.1350(15) -0.4184(11) 0.048(11) Uiso 0.50 1 d PG A 2 H36B H 0.0124 0.1349 -0.4685 0.057 Uiso 0.50 1 calc PR A 2 C37' C 0.0162(9) 0.0958(12) -0.3653(14) 0.037(9) Uiso 0.50 1 d PG A 2 H37B H -0.0185 0.0690 -0.3791 0.044 Uiso 0.50 1 calc PR A 2 C38' C 0.0485(10) 0.0959(13) -0.2920(13) 0.037(10) Uiso 0.50 1 d PG A 2 H38B H 0.0360 0.0691 -0.2557 0.045 Uiso 0.50 1 calc PR A 2 C39 C 0.2732(5) 0.0871(6) -0.0678(8) 0.026(4) Uiso 1 1 d G . . C40 C 0.2700(6) 0.0685(8) -0.1415(7) 0.076(8) Uiso 1 1 d G . . H40A H 0.2385 0.0846 -0.1797 0.092 Uiso 1 1 calc R . . C41 C 0.3127(8) 0.0262(9) -0.1590(7) 0.089(9) Uiso 1 1 d G . . H41A H 0.3104 0.0134 -0.2093 0.107 Uiso 1 1 calc R . . C42 C 0.3587(6) 0.0026(8) -0.1030(10) 0.062(7) Uiso 1 1 d G . . H42A H 0.3879 -0.0263 -0.1150 0.074 Uiso 1 1 calc R . . C43 C 0.3620(6) 0.0212(8) -0.0294(8) 0.080(8) Uiso 1 1 d G . . H43A H 0.3934 0.0051 0.0089 0.096 Uiso 1 1 calc R . . C44 C 0.3192(7) 0.0635(8) -0.0118(6) 0.074(8) Uiso 1 1 d G . . H44A H 0.3215 0.0763 0.0385 0.089 Uiso 1 1 calc R . . C45 C 0.1803(7) 0.0960(8) 0.0191(9) 0.053(6) Uiso 1 1 d G . . C46 C 0.1187(7) 0.0866(9) 0.0008(9) 0.083(8) Uiso 1 1 d G . . H46A H 0.0959 0.1044 -0.0443 0.099 Uiso 1 1 calc R . . C47 C 0.0907(6) 0.0512(11) 0.0484(12) 0.116(12) Uiso 1 1 d G . . H47A H 0.0487 0.0448 0.0359 0.139 Uiso 1 1 calc R . . C48 C 0.1242(9) 0.0252(10) 0.1143(11) 0.105(11) Uiso 1 1 d G . . H48A H 0.1051 0.0011 0.1469 0.126 Uiso 1 1 calc R . . C49 C 0.1857(8) 0.0346(9) 0.1326(9) 0.092(9) Uiso 1 1 d G . . H49A H 0.2086 0.0169 0.1777 0.110 Uiso 1 1 calc R . . C50 C 0.2137(6) 0.0700(8) 0.0850(9) 0.061(7) Uiso 1 1 d G . . H50A H 0.2558 0.0764 0.0975 0.073 Uiso 1 1 calc R . . _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 2.067(14) 7 ? Ru1 N1 2.067(14) . ? Ru1 N2 2.079(13) . ? Ru1 N2 2.079(13) 7 ? Ru1 P1 2.340(5) . ? Ru1 P1 2.340(5) 7 ? P1 C31 1.758(18) . ? P1 C39 1.820(11) . ? P1 C45 1.862(14) . ? N1 C4 1.34(2) . ? N1 C1 1.41(2) . ? N2 C6 1.30(2) . ? N2 C9 1.48(2) . ? C1 C2 1.41(2) . ? C1 C10 1.42(2) 7 ? C2 C3 1.36(2) . ? C2 C11 1.54(3) . ? C3 C4 1.46(2) . ? C3 C13 1.52(3) . ? C4 C5 1.41(3) . ? C5 C6 1.37(2) . ? C5 H5A 0.9500 . ? C6 C7 1.49(2) . ? C7 C8 1.37(3) . ? C7 C15 1.51(3) . ? C8 C9 1.45(2) . ? C8 C12 1.52(3) . ? C9 C10 1.36(2) . ? C10 C1 1.42(2) 7 ? C10 C17 1.51(3) . ? 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 1.54(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.54(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.35(3) . ? C17 C22 1.38(2) . ? C18 C19 1.40(3) . ? C18 H18A 0.9500 . ? C19 C20 1.37(3) . ? C19 C23 1.55(3) . ? C20 C21 1.39(3) . ? C20 H20A 0.9500 . ? C21 C22 1.42(3) . ? C21 C27 1.51(3) . ? C22 H22A 0.9500 . ? C23 C26 1.46(5) . ? C23 C24 1.51(3) . ? C23 C25 1.52(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.39(4) . ? C27 C30 1.43(4) . ? C27 C28 1.67(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.17(2) . ? C32 C33 1.40(3) . ? C32 C33' 1.62(3) . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C34 H34A 0.9500 . ? C35 C36 1.3900 . ? C35 H35A 0.9500 . ? C36 C37 1.3900 . ? C36 H36A 0.9500 . ? C37 C38 1.3900 . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C33' C34' 1.3900 . ? C33' C38' 1.3900 . ? C34' C35' 1.3900 . ? C34' H34B 0.9500 . ? C35' C36' 1.3900 . ? C35' H35B 0.9500 . ? C36' C37' 1.3900 . ? C36' H36B 0.9500 . ? C37' C38' 1.3900 . ? C37' H37B 0.9500 . ? C38' H38B 0.9500 . ? C39 C40 1.3900 . ? C39 C44 1.3900 . ? C40 C41 1.3900 . ? C40 H40A 0.9500 . ? C41 C42 1.3900 . ? C41 H41A 0.9500 . ? C42 C43 1.3900 . ? C42 H42A 0.9500 . ? C43 C44 1.3900 . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C46 C47 1.3900 . ? C46 H46A 0.9500 . ? C47 C48 1.3900 . ? C47 H47A 0.9500 . ? C48 C49 1.3900 . ? C48 H48A 0.9500 . ? C49 C50 1.3900 . ? C49 H49A 0.9500 . ? C50 H50A 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 N1 180.0(7) 7 . ? N1 Ru1 N2 88.7(5) 7 . ? N1 Ru1 N2 91.3(5) . . ? N1 Ru1 N2 91.3(5) 7 7 ? N1 Ru1 N2 88.7(5) . 7 ? N2 Ru1 N2 180.0(7) . 7 ? N1 Ru1 P1 91.7(4) 7 . ? N1 Ru1 P1 88.3(4) . . ? N2 Ru1 P1 89.0(3) . . ? N2 Ru1 P1 91.0(3) 7 . ? N1 Ru1 P1 88.3(4) 7 7 ? N1 Ru1 P1 91.7(4) . 7 ? N2 Ru1 P1 91.0(3) . 7 ? N2 Ru1 P1 89.0(3) 7 7 ? P1 Ru1 P1 180.00(9) . 7 ? C31 P1 C39 99.7(7) . . ? C31 P1 C45 101.3(8) . . ? C39 P1 C45 105.5(7) . . ? C31 P1 Ru1 113.0(6) . . ? C39 P1 Ru1 119.6(5) . . ? C45 P1 Ru1 115.2(6) . . ? C4 N1 C1 107.0(14) . . ? C4 N1 Ru1 123.9(12) . . ? C1 N1 Ru1 129.1(10) . . ? C6 N2 C9 108.2(13) . . ? C6 N2 Ru1 124.5(12) . . ? C9 N2 Ru1 127.3(10) . . ? N1 C1 C2 108.1(14) . . ? N1 C1 C10 122.0(15) . 7 ? C2 C1 C10 129.8(17) . 7 ? C3 C2 C1 109.3(16) . . ? C3 C2 C11 120.9(16) . . ? C1 C2 C11 129.9(16) . . ? C2 C3 C4 105.3(15) . . ? C2 C3 C13 130.4(17) . . ? C4 C3 C13 124.2(16) . . ? N1 C4 C5 125.2(17) . . ? N1 C4 C3 110.3(15) . . ? C5 C4 C3 124.4(16) . . ? C6 C5 C4 128.2(17) . . ? C6 C5 H5A 115.9 . . ? C4 C5 H5A 115.9 . . ? N2 C6 C5 126.6(16) . . ? N2 C6 C7 111.0(15) . . ? C5 C6 C7 122.1(15) . . ? C8 C7 C6 105.7(15) . . ? C8 C7 C15 128.0(18) . . ? C6 C7 C15 126.3(18) . . ? C7 C8 C9 109.4(16) . . ? C7 C8 C12 122.7(16) . . ? C9 C8 C12 127.9(17) . . ? C10 C9 C8 132.3(17) . . ? C10 C9 N2 122.0(14) . . ? C8 C9 N2 105.6(14) . . ? C9 C10 C1 130.7(17) . 7 ? C9 C10 C17 115.1(15) . . ? C1 C10 C17 114.2(15) 7 . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 C14 110.2(17) . . ? C3 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? C3 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? 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 . . ? C7 C15 C16 112.0(19) . . ? C7 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? C7 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 119.5(18) . . ? C18 C17 C10 119.6(16) . . ? C22 C17 C10 120.8(16) . . ? C17 C18 C19 123.1(18) . . ? C17 C18 H18A 118.5 . . ? C19 C18 H18A 118.5 . . ? C20 C19 C18 116.4(18) . . ? C20 C19 C23 122.3(18) . . ? C18 C19 C23 121.3(17) . . ? C19 C20 C21 124(2) . . ? C19 C20 H20A 118.0 . . ? C21 C20 H20A 118.0 . . ? C20 C21 C22 116.3(18) . . ? C20 C21 C27 120.7(19) . . ? C22 C21 C27 122.8(18) . . ? C17 C22 C21 120.4(17) . . ? C17 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C26 C23 C24 111(3) . . ? C26 C23 C25 105(3) . . ? C24 C23 C25 109(2) . . ? C26 C23 C19 114(3) . . ? C24 C23 C19 113.8(18) . . ? C25 C23 C19 103(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C30 125(3) . . ? C29 C27 C21 115(3) . . ? C30 C27 C21 114(2) . . ? C29 C27 C28 94(3) . . ? C30 C27 C28 95(3) . . ? C21 C27 C28 107(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 P1 170.1(17) . . ? C31 C32 C33 172(2) . . ? C31 C32 C33' 168(2) . . ? C33 C32 C33' 19.5(13) . . ? C34 C33 C38 120.0 . . ? C34 C33 C32 116.3(17) . . ? C38 C33 C32 123.5(16) . . ? C35 C34 C33 120.0 . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 H38A 120.0 . . ? C33 C38 H38A 120.0 . . ? C34' C33' C38' 120.0 . . ? C34' C33' C32 114.1(16) . . ? C38' C33' C32 125.4(16) . . ? C33' C34' C35' 120.0 . . ? C33' C34' H34B 120.0 . . ? C35' C34' H34B 120.0 . . ? C34' C35' C36' 120.0 . . ? C34' C35' H35B 120.0 . . ? C36' C35' H35B 120.0 . . ? C37' C36' C35' 120.0 . . ? C37' C36' H36B 120.0 . . ? C35' C36' H36B 120.0 . . ? C36' C37' C38' 120.0 . . ? C36' C37' H37B 120.0 . . ? C38' C37' H37B 120.0 . . ? C37' C38' C33' 120.0 . . ? C37' C38' H38B 120.0 . . ? C33' C38' H38B 120.0 . . ? C40 C39 C44 120.0 . . ? C40 C39 P1 121.5(8) . . ? C44 C39 P1 118.5(8) . . ? C41 C40 C39 120.0 . . ? C41 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C43 C42 C41 120.0 . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C43 C44 C39 120.0 . . ? C43 C44 H44A 120.0 . . ? C39 C44 H44A 120.0 . . ? C46 C45 C50 120.0 . . ? C46 C45 P1 121.4(10) . . ? C50 C45 P1 118.6(10) . . ? C47 C46 C45 120.0 . . ? C47 C46 H46A 120.0 . . ? C45 C46 H46A 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47A 120.0 . . ? C48 C47 H47A 120.0 . . ? C47 C48 C49 120.0 . . ? C47 C48 H48A 120.0 . . ? C49 C48 H48A 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49A 120.0 . . ? C48 C49 H49A 120.0 . . ? C49 C50 C45 120.0 . . ? C49 C50 H50A 120.0 . . ? C45 C50 H50A 120.0 . . ? #===END ## Synthesis of phosphine and phosphonite complexes of a Ru(II) porphyrin ## ## E. Stulz, M. Maue, N. Feeder, S. Teat, Y.-F. Ng, A. D. Bond, S. Darling & J. K. M. Sanders ## ## Denoted [(PA)3P]2Ru(DPP) in text ## data_js0007 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C108 H106 N4 P2 Ru, 4(C H Cl3)' _chemical_formula_sum 'C112 H110 Cl12 N4 P2 Ru' _chemical_formula_weight 2100.45 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' _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 13.8041(7) _cell_length_b 13.8388(8) _cell_length_c 14.7719(8) _cell_angle_alpha 87.730(2) _cell_angle_beta 83.010(2) _cell_angle_gamma 67.105(2) _cell_volume 2580.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20080 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 29.18 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9578 _exptl_absorpt_correction_T_max 0.9681 _exptl_absorpt_process_details ; Correction applied by SADABS - note that the transmission factors are not real since they include corrections for beam decay and possibly crystal decay (the two cannot be distinguished). The numbers listed in the CIF are those calculated by SHELXL. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6923 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS, Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'Thin slice \w-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_reflns_number 25065 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 29.44 _diffrn_measured_fraction_theta_max 0.856 _diffrn_reflns_theta_full 29.44 _diffrn_measured_fraction_theta_full 0.856 _reflns_number_total 13243 _reflns_number_gt 11428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker AXS, 1994)' _computing_cell_refinement 'Bruker SAINT (Bruker AXS, 1994)' _computing_data_reduction 'Bruker SAINT (Bruker AXS, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1996)' _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^)+(0.0869P)^2^+1.3889P] 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 13243 _refine_ls_number_parameters 604 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1365 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 1.021 _refine_diff_density_min -1.402 _refine_diff_density_rms 0.083 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 0.5000 0.5000 0.5000 0.01295(7) Uani 1 2 d S . . P1 P 0.62145(4) 0.57665(4) 0.47447(3) 0.01637(11) Uani 1 1 d . . . N1 N 0.50264(13) 0.51201(13) 0.63844(11) 0.0161(3) Uani 1 1 d . . . N2 N 0.38073(13) 0.64649(13) 0.49408(11) 0.0162(3) Uani 1 1 d . . . C1 C 0.43752(16) 0.59820(16) 0.68917(14) 0.0183(4) Uani 1 1 d . . . C2 C 0.35991(16) 0.68642(16) 0.65735(14) 0.0195(4) Uani 1 1 d . . . H2 H 0.3189 0.7380 0.7023 0.023 Uiso 1 1 calc R . . C3 C 0.33360(16) 0.71012(15) 0.56919(14) 0.0185(4) Uani 1 1 d . . . C4 C 0.25531(17) 0.80828(16) 0.54228(15) 0.0218(4) Uani 1 1 d . . . C5 C 0.25654(17) 0.80383(16) 0.45039(15) 0.0217(4) Uani 1 1 d . . . C6 C 0.33515(16) 0.70058(15) 0.41939(14) 0.0181(4) Uani 1 1 d . . . C7 C 0.36103(16) 0.65957(16) 0.33014(14) 0.0180(4) Uani 1 1 d . . . C8 C 0.43520(15) 0.55916(16) 0.30314(13) 0.0170(4) Uani 1 1 d . . . C9 C 0.46168(17) 0.51204(17) 0.21129(14) 0.0204(4) Uani 1 1 d . . . C10 C 0.53947(17) 0.41545(17) 0.21679(14) 0.0206(4) Uani 1 1 d . . . C11 C 0.1861(2) 0.89212(19) 0.39656(18) 0.0331(5) Uani 1 1 d . . . H11A H 0.1328 0.8716 0.3743 0.050 Uiso 1 1 calc R . . H11B H 0.2288 0.9078 0.3446 0.050 Uiso 1 1 calc R . . H11C H 0.1508 0.9545 0.4357 0.050 Uiso 1 1 calc R . . C12 C 0.41574(19) 0.55636(19) 0.12405(15) 0.0257(4) Uani 1 1 d . . . H12A H 0.4447 0.5023 0.0761 0.039 Uiso 1 1 calc R . . H12B H 0.4341 0.6165 0.1054 0.039 Uiso 1 1 calc R . . H12C H 0.3386 0.5791 0.1339 0.039 Uiso 1 1 calc R . . C13 C 0.18608(19) 0.89627(18) 0.60675(17) 0.0287(5) Uani 1 1 d . . . H13A H 0.1800 0.9639 0.5780 0.034 Uiso 1 1 calc R . . H13B H 0.2205 0.8900 0.6629 0.034 Uiso 1 1 calc R . . C14 C 0.0761(3) 0.8972(3) 0.6324(3) 0.0657(12) Uani 1 1 d . . . H14A H 0.0407 0.9054 0.5773 0.099 Uiso 1 1 calc R . . H14B H 0.0351 0.9557 0.6744 0.099 Uiso 1 1 calc R . . H14C H 0.0813 0.8310 0.6620 0.099 Uiso 1 1 calc R . . C15 C 0.59342(19) 0.33369(19) 0.14356(15) 0.0275(5) Uani 1 1 d . . . H15A H 0.5456 0.3457 0.0958 0.033 Uiso 1 1 calc R . . H15B H 0.6043 0.2640 0.1703 0.033 Uiso 1 1 calc R . . C16 C 0.6994(2) 0.3310(3) 0.0987(2) 0.0432(7) Uani 1 1 d . . . H16A H 0.6886 0.3960 0.0646 0.065 Uiso 1 1 calc R . . H16B H 0.7320 0.2709 0.0568 0.065 Uiso 1 1 calc R . . H16C H 0.7459 0.3246 0.1456 0.065 Uiso 1 1 calc R . . C17 C 0.30602(16) 0.72998(16) 0.25662(14) 0.0195(4) Uani 1 1 d . . . C18 C 0.35426(17) 0.79111(17) 0.20765(15) 0.0222(4) Uani 1 1 d . . . H18 H 0.4209 0.7874 0.2217 0.027 Uiso 1 1 calc R . . C19 C 0.30619(17) 0.85728(17) 0.13859(15) 0.0226(4) Uani 1 1 d D A . C20 C 0.20798(18) 0.85980(17) 0.11986(16) 0.0238(4) Uani 1 1 d . . . H20 H 0.1741 0.9046 0.0730 0.029 Uiso 1 1 calc R . . C21 C 0.15827(17) 0.79975(17) 0.16685(15) 0.0213(4) Uani 1 1 d . . . C22 C 0.20890(16) 0.73449(16) 0.23621(14) 0.0203(4) Uani 1 1 d . . . H22 H 0.1763 0.6929 0.2696 0.024 Uiso 1 1 calc R . . C23 C 0.05216(18) 0.80147(19) 0.14361(17) 0.0261(4) Uani 1 1 d . . . C24 C 0.0673(3) 0.6919(3) 0.1142(3) 0.0604(11) Uani 1 1 d . . . H24A H 0.0000 0.6925 0.0987 0.091 Uiso 1 1 calc R . . H24B H 0.0911 0.6428 0.1642 0.091 Uiso 1 1 calc R . . H24C H 0.1206 0.6697 0.0607 0.091 Uiso 1 1 calc R . . C25 C 0.0101(3) 0.8767(3) 0.0664(3) 0.0593(11) Uani 1 1 d . . . H25A H 0.0588 0.8524 0.0104 0.089 Uiso 1 1 calc R . . H25B H 0.0042 0.9470 0.0824 0.089 Uiso 1 1 calc R . . H25C H -0.0598 0.8791 0.0567 0.089 Uiso 1 1 calc R . . C26 C -0.0287(2) 0.8341(4) 0.2278(3) 0.0593(10) Uani 1 1 d . . . H26A H -0.0960 0.8335 0.2136 0.089 Uiso 1 1 calc R . . H26B H -0.0394 0.9050 0.2467 0.089 Uiso 1 1 calc R . . H26C H -0.0029 0.7850 0.2773 0.089 Uiso 1 1 calc R . . C27 C 0.35680(18) 0.92594(18) 0.08483(16) 0.0280(5) Uani 1 1 d D . . C28 C 0.3488(5) 1.0154(4) 0.1431(4) 0.0471(14) Uiso 0.50 1 d PD A 1 H28A H 0.3777 1.0611 0.1071 0.071 Uiso 0.50 1 calc PR A 1 H28B H 0.3891 0.9881 0.1952 0.071 Uiso 0.50 1 calc PR A 1 H28C H 0.2744 1.0557 0.1653 0.071 Uiso 0.50 1 calc PR A 1 C29 C 0.3048(5) 0.9684(5) -0.0025(4) 0.0432(13) Uiso 0.50 1 d PD A 1 H29A H 0.2347 1.0237 0.0135 0.065 Uiso 0.50 1 calc PR A 1 H29B H 0.2974 0.9113 -0.0345 0.065 Uiso 0.50 1 calc PR A 1 H29C H 0.3490 0.9971 -0.0423 0.065 Uiso 0.50 1 calc PR A 1 C30 C 0.4741(4) 0.8575(5) 0.0537(4) 0.0476(14) Uiso 0.50 1 d PD A 1 H30A H 0.5067 0.8998 0.0171 0.071 Uiso 0.50 1 calc PR A 1 H30B H 0.4782 0.7983 0.0171 0.071 Uiso 0.50 1 calc PR A 1 H30C H 0.5117 0.8311 0.1074 0.071 Uiso 0.50 1 calc PR A 1 C28' C 0.4599(4) 0.9175(5) 0.1198(4) 0.0461(14) Uiso 0.50 1 d PD A 2 H28D H 0.4872 0.9655 0.0855 0.069 Uiso 0.50 1 calc PR A 2 H28E H 0.5123 0.8454 0.1114 0.069 Uiso 0.50 1 calc PR A 2 H28F H 0.4461 0.9363 0.1847 0.069 Uiso 0.50 1 calc PR A 2 C29' C 0.2790(5) 1.0417(4) 0.0979(5) 0.0492(15) Uiso 0.50 1 d PD A 2 H29D H 0.2665 1.0606 0.1627 0.074 Uiso 0.50 1 calc PR A 2 H29E H 0.2119 1.0508 0.0759 0.074 Uiso 0.50 1 calc PR A 2 H29F H 0.3095 1.0871 0.0633 0.074 Uiso 0.50 1 calc PR A 2 C30' C 0.3768(6) 0.8990(6) -0.0155(4) 0.0571(17) Uiso 0.50 1 d PD A 2 H30D H 0.3090 0.9207 -0.0406 0.086 Uiso 0.50 1 calc PR A 2 H30E H 0.4155 0.8232 -0.0238 0.086 Uiso 0.50 1 calc PR A 2 H30F H 0.4188 0.9358 -0.0473 0.086 Uiso 0.50 1 calc PR A 2 C31 C 0.65367(16) 0.60592(17) 0.36062(15) 0.0212(4) Uani 1 1 d . . . C32 C 0.67150(17) 0.62578(17) 0.28208(16) 0.0226(4) Uani 1 1 d . . . C33 C 0.69571(17) 0.64974(18) 0.18890(15) 0.0240(4) Uani 1 1 d . . . C34 C 0.75114(19) 0.7146(2) 0.16774(17) 0.0286(5) Uani 1 1 d . . . H34 H 0.7725 0.7436 0.2151 0.034 Uiso 1 1 calc R . . C35 C 0.7750(2) 0.7366(2) 0.07793(18) 0.0332(5) Uani 1 1 d . . . H35 H 0.8119 0.7816 0.0636 0.040 Uiso 1 1 calc R . . C36 C 0.7454(2) 0.6935(3) 0.00866(18) 0.0416(7) Uani 1 1 d . . . H36 H 0.7631 0.7080 -0.0531 0.050 Uiso 1 1 calc R . . C37 C 0.6901(3) 0.6292(3) 0.0292(2) 0.0480(8) Uani 1 1 d . . . H37 H 0.6698 0.5997 -0.0186 0.058 Uiso 1 1 calc R . . C38 C 0.6643(2) 0.6079(2) 0.11932(18) 0.0356(6) Uani 1 1 d . . . H38 H 0.6253 0.5647 0.1335 0.043 Uiso 1 1 calc R . . C39 C 0.58837(18) 0.69945(17) 0.52619(16) 0.0231(4) Uani 1 1 d . . . C40 C 0.56132(19) 0.78546(18) 0.55850(16) 0.0259(4) Uani 1 1 d . . . C41 C 0.52830(19) 0.88852(18) 0.59642(17) 0.0266(4) Uani 1 1 d . . . C42 C 0.4321(2) 0.9317(2) 0.6504(2) 0.0400(6) Uani 1 1 d . . . H42 H 0.3900 0.8915 0.6646 0.048 Uiso 1 1 calc R . . C43 C 0.3970(3) 1.0334(2) 0.6839(2) 0.0482(7) Uani 1 1 d . . . H43 H 0.3310 1.0628 0.7209 0.058 Uiso 1 1 calc R . . C44 C 0.4579(3) 1.0916(2) 0.6634(2) 0.0422(7) Uani 1 1 d . . . H44 H 0.4333 1.1615 0.6858 0.051 Uiso 1 1 calc R . . C45 C 0.5544(2) 1.0491(2) 0.6106(2) 0.0375(6) Uani 1 1 d . . . H45 H 0.5963 1.0896 0.5971 0.045 Uiso 1 1 calc R . . C46 C 0.5903(2) 0.94729(19) 0.57706(18) 0.0305(5) Uani 1 1 d . . . H46 H 0.6569 0.9178 0.5410 0.037 Uiso 1 1 calc R . . C47 C 0.74695(17) 0.50517(17) 0.50901(15) 0.0225(4) Uani 1 1 d . . . C48 C 0.83248(18) 0.44952(18) 0.53016(16) 0.0243(4) Uani 1 1 d . . . C49 C 0.93706(17) 0.38333(18) 0.54913(16) 0.0240(4) Uani 1 1 d . . . C50 C 0.99827(18) 0.4229(2) 0.59266(18) 0.0285(5) Uani 1 1 d . . . H50 H 0.9694 0.4938 0.6132 0.034 Uiso 1 1 calc R . . C51 C 1.10130(19) 0.3585(2) 0.60586(19) 0.0345(6) Uani 1 1 d . . . H51 H 1.1428 0.3854 0.6358 0.041 Uiso 1 1 calc R . . C52 C 1.1437(2) 0.2564(2) 0.5761(2) 0.0392(6) Uani 1 1 d . . . H52 H 1.2144 0.2129 0.5853 0.047 Uiso 1 1 calc R . . C53 C 1.0837(2) 0.2163(2) 0.5324(2) 0.0412(6) Uani 1 1 d . . . H53 H 1.1137 0.1457 0.5113 0.049 Uiso 1 1 calc R . . C54 C 0.9801(2) 0.2790(2) 0.51943(19) 0.0339(5) Uani 1 1 d . . . H54 H 0.9387 0.2511 0.4905 0.041 Uiso 1 1 calc R . . C60 C 0.2886(2) 0.3427(2) 0.27740(18) 0.0356(5) Uani 1 1 d . . . H60 H 0.3264 0.3649 0.3208 0.043 Uiso 1 1 calc R . . Cl1 Cl 0.21505(7) 0.45316(6) 0.21711(5) 0.04705(18) Uani 1 1 d . . . Cl2 Cl 0.20424(6) 0.29130(7) 0.34065(6) 0.0507(2) Uani 1 1 d . . . Cl3 Cl 0.38343(7) 0.24834(7) 0.20253(6) 0.0531(2) Uani 1 1 d . . . C61 C 0.9941(3) 0.3634(3) 0.1907(3) 0.0550(8) Uani 1 1 d . . . H61 H 1.0577 0.3670 0.2141 0.066 Uiso 1 1 calc R . . Cl4 Cl 0.89388(9) 0.39294(8) 0.28141(7) 0.0714(3) Uani 1 1 d . . . Cl5 Cl 1.02946(12) 0.23797(10) 0.14944(10) 0.0948(4) Uani 1 1 d . . . Cl6 Cl 0.95947(11) 0.45389(11) 0.10368(10) 0.0933(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01464(10) 0.01376(10) 0.01207(11) 0.00104(7) -0.00502(7) - 0.00632(8) P1 0.0183(2) 0.0178(2) 0.0160(2) 0.00153(18) -0.00591(18) -0.00915(19) N1 0.0178(7) 0.0168(7) 0.0160(8) 0.0018(6) -0.0061(6) -0.0082(6) N2 0.0189(8) 0.0181(7) 0.0142(7) 0.0016(6) -0.0068(6) -0.0087(6) C1 0.0208(9) 0.0217(9) 0.0150(9) -0.0002(7) -0.0052(7) -0.0099(8) C2 0.0215(9) 0.0186(9) 0.0182(9) -0.0026(7) -0.0040(7) -0.0069(7) C3 0.0197(9) 0.0163(8) 0.0201(9) -0.0006(7) -0.0052(7) -0.0067(7) C4 0.0228(10) 0.0173(9) 0.0245(10) 0.0002(8) -0.0076(8) -0.0056(8) C5 0.0238(10) 0.0166(9) 0.0249(10) 0.0016(7) -0.0087(8) -0.0065(8) C6 0.0187(9) 0.0160(8) 0.0204(9) 0.0033(7) -0.0074(7) -0.0065(7) C7 0.0194(9) 0.0208(9) 0.0178(9) 0.0049(7) -0.0080(7) -0.0107(7) C8 0.0193(9) 0.0212(9) 0.0149(9) 0.0031(7) -0.0066(7) -0.0114(7) C9 0.0236(10) 0.0271(10) 0.0153(9) 0.0016(8) -0.0060(7) -0.0140(8) C10 0.0251(10) 0.0252(10) 0.0140(9) -0.0002(7) -0.0047(7) -0.0118(8) C11 0.0412(13) 0.0214(10) 0.0283(12) 0.0017(9) -0.0163(10) 0.0005(10) C12 0.0316(11) 0.0309(11) 0.0150(9) 0.0019(8) -0.0084(8) -0.0109(9) C13 0.0306(11) 0.0205(10) 0.0309(12) -0.0048(9) -0.0097(9) -0.0032(9) C14 0.0323(15) 0.059(2) 0.099(3) -0.049(2) 0.0087(17) -0.0105(15) C15 0.0346(12) 0.0301(11) 0.0173(10) -0.0043(8) -0.0067(9) -0.0104(9) C16 0.0438(15) 0.0486(16) 0.0341(14) -0.0136(12) 0.0082(12) -0.0169(13) C17 0.0236(10) 0.0193(9) 0.0184(9) 0.0042(7) -0.0083(7) -0.0102(8) C18 0.0224(10) 0.0232(9) 0.0254(10) 0.0058(8) -0.0091(8) -0.0123(8) C19 0.0268(10) 0.0222(9) 0.0231(10) 0.0066(8) -0.0066(8) -0.0135(8) C20 0.0264(10) 0.0248(10) 0.0225(10) 0.0079(8) -0.0105(8) -0.0109(8) C21 0.0227(10) 0.0239(9) 0.0204(10) 0.0046(8) -0.0093(8) -0.0109(8) C22 0.0231(10) 0.0219(9) 0.0190(9) 0.0044(7) -0.0070(7) -0.0112(8) C23 0.0236(10) 0.0306(11) 0.0285(11) 0.0079(9) -0.0129(8) -0.0133(9) C24 0.0442(17) 0.0404(16) 0.105(3) -0.0083(18) -0.0410(19) -0.0155(14) C25 0.0487(18) 0.082(3) 0.066(2) 0.046(2) -0.0408(17) -0.0405(18) C26 0.0310(14) 0.104(3) 0.0485(19) -0.0151(19) -0.0024(13) -0.0320(18) C27 0.0309(11) 0.0295(11) 0.0305(12) 0.0129(9) -0.0099(9) -0.0186(9) C31 0.0216(9) 0.0228(9) 0.0237(10) 0.0021(8) -0.0048(8) -0.0131(8) C32 0.0222(9) 0.0238(10) 0.0249(11) 0.0014(8) -0.0048(8) -0.0118(8) C33 0.0230(10) 0.0295(11) 0.0211(10) 0.0029(8) -0.0032(8) -0.0118(9) C34 0.0295(11) 0.0345(12) 0.0280(12) 0.0031(9) -0.0068(9) -0.0183(10) C35 0.0320(12) 0.0443(14) 0.0312(13) 0.0102(11) -0.0064(10) -0.0234(11) C36 0.0454(15) 0.068(2) 0.0218(12) 0.0111(12) -0.0040(11) -0.0338(15) C37 0.064(2) 0.077(2) 0.0236(13) 0.0001(13) -0.0066(12) -0.0491(19) C38 0.0451(15) 0.0507(15) 0.0242(12) 0.0014(11) -0.0051(10) -0.0326(13) C39 0.0257(10) 0.0225(9) 0.0249(10) 0.0014(8) -0.0060(8) -0.0126(8) C40 0.0301(11) 0.0252(10) 0.0258(11) 0.0016(8) -0.0092(9) -0.0127(9) C41 0.0337(12) 0.0221(10) 0.0271(11) -0.0014(8) -0.0118(9) -0.0116(9) C42 0.0381(14) 0.0317(13) 0.0512(17) -0.0084(12) -0.0049(12) - 0.0139(11) C43 0.0439(16) 0.0354(14) 0.0572(19) -0.0147(13) 0.0017(14) -0.0075(13) C44 0.0537(17) 0.0223(11) 0.0480(17) -0.0079(11) -0.0177(13) - 0.0077(11) C45 0.0522(16) 0.0277(12) 0.0427(15) 0.0017(11) -0.0213(12) -0.0220(12) C46 0.0381(13) 0.0264(11) 0.0317(12) 0.0000(9) -0.0111(10) -0.0156(10) C47 0.0222(10) 0.0261(10) 0.0237(10) 0.0022(8) -0.0073(8) -0.0130(8) C48 0.0247(10) 0.0271(10) 0.0247(11) 0.0038(8) -0.0076(8) -0.0129(9) C49 0.0206(10) 0.0278(10) 0.0250(11) 0.0047(8) -0.0058(8) -0.0103(8) C50 0.0245(11) 0.0326(12) 0.0328(12) 0.0031(9) -0.0095(9) -0.0142(9) C51 0.0222(11) 0.0498(15) 0.0359(13) 0.0115(11) -0.0119(9) -0.0171(11) C52 0.0210(11) 0.0476(15) 0.0388(14) 0.0123(12) -0.0055(10) -0.0029(11) C53 0.0388(14) 0.0305(13) 0.0427(15) 0.0003(11) -0.0055(12) -0.0005(11) C54 0.0360(13) 0.0297(12) 0.0367(14) 0.0013(10) -0.0132(10) -0.0110(10) C60 0.0394(14) 0.0448(14) 0.0273(12) 0.0048(11) -0.0101(10) -0.0199(12) Cl1 0.0578(4) 0.0421(4) 0.0410(4) 0.0106(3) -0.0100(3) -0.0189(3) Cl2 0.0448(4) 0.0585(5) 0.0510(4) 0.0216(4) -0.0102(3) -0.0230(4) Cl3 0.0481(4) 0.0596(5) 0.0408(4) 0.0026(3) -0.0068(3) -0.0090(4) C61 0.0435(17) 0.061(2) 0.058(2) -0.0087(17) -0.0094(15) -0.0160(16) Cl4 0.0789(7) 0.0608(5) 0.0520(5) -0.0109(4) 0.0123(5) -0.0075(5) Cl5 0.1107(10) 0.0662(7) 0.0885(9) -0.0318(6) 0.0336(8) -0.0236(7) Cl6 0.0814(8) 0.0901(9) 0.0791(8) 0.0242(7) 0.0063(6) -0.0084(7) _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 N2 2.0621(17) 2_666 ? Ru1 N2 2.0621(16) . ? Ru1 N1 2.0642(17) 2_666 ? Ru1 N1 2.0642(17) . ? Ru1 P1 2.2970(5) 2_666 ? Ru1 P1 2.2970(5) . ? P1 C47 1.755(2) . ? P1 C39 1.759(2) . ? P1 C31 1.759(2) . ? N1 C1 1.366(3) . ? N1 C8 1.381(2) 2_666 ? N2 C3 1.373(3) . ? N2 C6 1.382(2) . ? C1 C2 1.385(3) . ? C1 C10 1.451(3) 2_666 ? C2 C3 1.387(3) . ? C2 H2 0.9500 . ? C3 C4 1.446(3) . ? C4 C5 1.359(3) . ? C4 C13 1.506(3) . ? C5 C6 1.467(3) . ? C5 C11 1.502(3) . ? C6 C7 1.405(3) . ? C7 C8 1.406(3) . ? C7 C17 1.499(3) . ? C8 N1 1.381(2) 2_666 ? C8 C9 1.471(3) . ? C9 C10 1.357(3) . ? C9 C12 1.508(3) . ? C10 C1 1.451(3) 2_666 ? C10 C15 1.500(3) . ? 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 1.515(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.518(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.387(3) . ? C17 C18 1.398(3) . ? C18 C19 1.392(3) . ? C18 H18 0.9500 . ? C19 C20 1.403(3) . ? C19 C27 1.531(3) . ? C20 C21 1.388(3) . ? C20 H20 0.9500 . ? C21 C22 1.401(3) . ? C21 C23 1.536(3) . ? C22 H22 0.9500 . ? C23 C26 1.520(4) . ? C23 C24 1.522(4) . ? C23 C25 1.523(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.498(5) . ? C27 C30' 1.509(6) . ? C27 C28' 1.533(5) . ? C27 C29 1.538(5) . ? C27 C30 1.545(5) . ? C27 C29' 1.547(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C28' H28D 0.9800 . ? C28' H28E 0.9800 . ? C28' H28F 0.9800 . ? C29' H29D 0.9800 . ? C29' H29E 0.9800 . ? C29' H29F 0.9800 . ? C30' H30D 0.9800 . ? C30' H30E 0.9800 . ? C30' H30F 0.9800 . ? C31 C32 1.200(3) . ? C32 C33 1.433(3) . ? C33 C38 1.390(3) . ? C33 C34 1.394(3) . ? C34 C35 1.379(3) . ? C34 H34 0.9500 . ? C35 C36 1.381(4) . ? C35 H35 0.9500 . ? C36 C37 1.384(4) . ? C36 H36 0.9500 . ? C37 C38 1.387(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.200(3) . ? C40 C41 1.432(3) . ? C41 C42 1.385(4) . ? C41 C46 1.392(3) . ? C42 C43 1.388(4) . ? C42 H42 0.9500 . ? C43 C44 1.375(5) . ? C43 H43 0.9500 . ? C44 C45 1.379(5) . ? C44 H44 0.9500 . ? C45 C46 1.389(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.203(3) . ? C48 C49 1.432(3) . ? C49 C50 1.395(3) . ? C49 C54 1.397(3) . ? C50 C51 1.387(3) . ? C50 H50 0.9500 . ? C51 C52 1.369(4) . ? C51 H51 0.9500 . ? C52 C53 1.387(5) . ? C52 H52 0.9500 . ? C53 C54 1.386(4) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C60 Cl2 1.749(3) . ? C60 Cl1 1.751(3) . ? C60 Cl3 1.754(3) . ? C60 H60 1.0000 . ? C61 Cl5 1.725(4) . ? C61 Cl6 1.734(4) . ? C61 Cl4 1.740(4) . ? C61 H61 1.0000 . ? 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 N2 Ru1 N2 180.000(1) 2_666 . ? N2 Ru1 N1 93.04(7) 2_666 2_666 ? N2 Ru1 N1 86.96(7) . 2_666 ? N2 Ru1 N1 86.96(7) 2_666 . ? N2 Ru1 N1 93.04(7) . . ? N1 Ru1 N1 180.0 2_666 . ? N2 Ru1 P1 88.92(5) 2_666 2_666 ? N2 Ru1 P1 91.08(5) . 2_666 ? N1 Ru1 P1 88.93(5) 2_666 2_666 ? N1 Ru1 P1 91.07(5) . 2_666 ? N2 Ru1 P1 91.08(5) 2_666 . ? N2 Ru1 P1 88.92(5) . . ? N1 Ru1 P1 91.07(5) 2_666 . ? N1 Ru1 P1 88.93(5) . . ? P1 Ru1 P1 180.00(3) 2_666 . ? C47 P1 C39 101.66(11) . . ? C47 P1 C31 101.95(10) . . ? C39 P1 C31 100.12(10) . . ? C47 P1 Ru1 116.40(7) . . ? C39 P1 Ru1 117.28(8) . . ? C31 P1 Ru1 116.73(7) . . ? C1 N1 C8 107.32(17) . 2_666 ? C1 N1 Ru1 123.07(13) . . ? C8 N1 Ru1 129.61(14) 2_666 . ? C3 N2 C6 107.28(16) . . ? C3 N2 Ru1 123.26(13) . . ? C6 N2 Ru1 129.44(14) . . ? N1 C1 C2 125.95(18) . . ? N1 C1 C10 110.09(18) . 2_666 ? C2 C1 C10 123.96(19) . 2_666 ? C1 C2 C3 129.18(19) . . ? C1 C2 H2 115.4 . . ? C3 C2 H2 115.4 . . ? N2 C3 C2 125.43(18) . . ? N2 C3 C4 109.90(18) . . ? C2 C3 C4 124.61(19) . . ? C5 C4 C3 107.10(19) . . ? C5 C4 C13 128.0(2) . . ? C3 C4 C13 124.9(2) . . ? C4 C5 C6 107.22(18) . . ? C4 C5 C11 123.1(2) . . ? C6 C5 C11 129.7(2) . . ? N2 C6 C7 124.01(18) . . ? N2 C6 C5 108.48(18) . . ? C7 C6 C5 127.49(18) . . ? C6 C7 C8 126.00(18) . . ? C6 C7 C17 117.07(18) . . ? C8 C7 C17 116.92(18) . . ? N1 C8 C7 123.84(18) 2_666 . ? N1 C8 C9 108.53(17) 2_666 . ? C7 C8 C9 127.63(18) . . ? C10 C9 C8 107.11(18) . . ? C10 C9 C12 123.3(2) . . ? C8 C9 C12 129.57(19) . . ? C9 C10 C1 106.91(18) . 2_666 ? C9 C10 C15 129.1(2) . . ? C1 C10 C15 123.99(19) 2_666 . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C4 C13 C14 113.3(2) . . ? C4 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? C4 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? 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 . . ? C10 C15 C16 115.3(2) . . ? C10 C15 H15A 108.5 . . ? C16 C15 H15A 108.5 . . ? C10 C15 H15B 108.5 . . ? C16 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 119.85(18) . . ? C22 C17 C7 120.98(18) . . ? C18 C17 C7 119.17(18) . . ? C19 C18 C17 121.08(19) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 117.47(19) . . ? C18 C19 C27 122.04(19) . . ? C20 C19 C27 120.49(18) . . ? C21 C20 C19 122.87(19) . . ? C21 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? C20 C21 C22 117.98(19) . . ? C20 C21 C23 122.06(19) . . ? C22 C21 C23 119.95(19) . . ? C17 C22 C21 120.74(19) . . ? C17 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C26 C23 C24 109.1(3) . . ? C26 C23 C25 109.1(3) . . ? C24 C23 C25 108.2(3) . . ? C26 C23 C21 109.3(2) . . ? C24 C23 C21 109.0(2) . . ? C25 C23 C21 112.1(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C30' 137.1(4) . . ? C28 C27 C19 110.1(3) . . ? C30' C27 C19 110.8(3) . . ? C28 C27 C28' 64.3(3) . . ? C30' C27 C28' 109.9(4) . . ? C19 C27 C28' 112.5(3) . . ? C28 C27 C29 109.7(3) . . ? C30' C27 C29 41.6(3) . . ? C19 C27 C29 111.6(3) . . ? C28' C27 C29 134.4(4) . . ? C28 C27 C30 110.4(3) . . ? C30' C27 C30 67.3(4) . . ? C19 C27 C30 108.6(3) . . ? C28' C27 C30 48.0(3) . . ? C29 C27 C30 106.3(3) . . ? C28 C27 C29' 45.2(3) . . ? C30' C27 C29' 108.7(4) . . ? C19 C27 C29' 108.1(3) . . ? C28' C27 C29' 106.7(3) . . ? C29 C27 C29' 69.2(3) . . ? C30 C27 C29' 141.8(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? C27 C28' H28D 109.5 . . ? C27 C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? C27 C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? C27 C29' H29D 109.5 . . ? C27 C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? C27 C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? C27 C30' H30D 109.5 . . ? C27 C30' H30E 109.5 . . ? H30D C30' H30E 109.5 . . ? C27 C30' H30F 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? C32 C31 P1 177.10(19) . . ? C31 C32 C33 178.3(2) . . ? C38 C33 C34 119.8(2) . . ? C38 C33 C32 120.0(2) . . ? C34 C33 C32 120.2(2) . . ? C35 C34 C33 119.9(2) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.3(2) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C37 120.1(2) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C38 120.1(3) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C33 119.7(2) . . ? C37 C38 H38 120.1 . . ? C33 C38 H38 120.1 . . ? C40 C39 P1 176.4(2) . . ? C39 C40 C41 179.4(3) . . ? C42 C41 C46 119.6(2) . . ? C42 C41 C40 119.8(2) . . ? C46 C41 C40 120.6(2) . . ? C41 C42 C43 120.2(3) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 119.9(3) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.5(2) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C46 120.0(3) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 119.8(3) . . ? C45 C46 H46 120.1 . . ? C41 C46 H46 120.1 . . ? C48 C47 P1 175.1(2) . . ? C47 C48 C49 176.2(2) . . ? C50 C49 C54 119.6(2) . . ? C50 C49 C48 121.0(2) . . ? C54 C49 C48 119.3(2) . . ? C51 C50 C49 119.8(2) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C52 C51 C50 120.5(2) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C51 C52 C53 120.2(2) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C54 C53 C52 120.3(3) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C49 119.6(2) . . ? C53 C54 H54 120.2 . . ? C49 C54 H54 120.2 . . ? Cl2 C60 Cl1 110.20(15) . . ? Cl2 C60 Cl3 111.24(16) . . ? Cl1 C60 Cl3 110.44(15) . . ? Cl2 C60 H60 108.3 . . ? Cl1 C60 H60 108.3 . . ? Cl3 C60 H60 108.3 . . ? Cl5 C61 Cl6 110.4(2) . . ? Cl5 C61 Cl4 111.7(2) . . ? Cl6 C61 Cl4 111.7(2) . . ? Cl5 C61 H61 107.6 . . ? Cl6 C61 H61 107.6 . . ? Cl4 C61 H61 107.6 . . ? 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 N2 Ru1 P1 C47 -21.84(10) 2_666 . . . ? N2 Ru1 P1 C47 158.16(10) . . . . ? N1 Ru1 P1 C47 -114.91(10) 2_666 . . . ? N1 Ru1 P1 C47 65.09(10) . . . . ? N2 Ru1 P1 C39 -142.51(10) 2_666 . . . ? N2 Ru1 P1 C39 37.50(10) . . . . ? N1 Ru1 P1 C39 124.43(10) 2_666 . . . ? N1 Ru1 P1 C39 -55.57(10) . . . . ? N2 Ru1 P1 C31 98.74(9) 2_666 . . . ? N2 Ru1 P1 C31 -81.26(9) . . . . ? N1 Ru1 P1 C31 5.68(9) 2_666 . . . ? N1 Ru1 P1 C31 -174.32(9) . . . . ? N2 Ru1 N1 C1 179.86(16) 2_666 . . . ? N2 Ru1 N1 C1 -0.14(16) . . . . ? P1 Ru1 N1 C1 -91.28(15) 2_666 . . . ? P1 Ru1 N1 C1 88.72(15) . . . . ? N2 Ru1 N1 C8 -0.49(17) 2_666 . . 2_666 ? N2 Ru1 N1 C8 179.51(17) . . . 2_666 ? P1 Ru1 N1 C8 88.36(16) 2_666 . . 2_666 ? P1 Ru1 N1 C8 -91.64(16) . . . 2_666 ? N1 Ru1 N2 C3 178.61(16) 2_666 . . . ? N1 Ru1 N2 C3 -1.39(16) . . . . ? P1 Ru1 N2 C3 89.73(15) 2_666 . . . ? P1 Ru1 N2 C3 -90.27(15) . . . . ? N1 Ru1 N2 C6 -3.27(17) 2_666 . . . ? N1 Ru1 N2 C6 176.73(17) . . . . ? P1 Ru1 N2 C6 -92.15(16) 2_666 . . . ? P1 Ru1 N2 C6 87.85(16) . . . . ? C8 N1 C1 C2 -177.5(2) 2_666 . . . ? Ru1 N1 C1 C2 2.2(3) . . . . ? C8 N1 C1 C10 2.2(2) 2_666 . . 2_666 ? Ru1 N1 C1 C10 -178.13(13) . . . 2_666 ? N1 C1 C2 C3 -3.2(4) . . . . ? C10 C1 C2 C3 177.2(2) 2_666 . . . ? C6 N2 C3 C2 -177.4(2) . . . . ? Ru1 N2 C3 C2 1.1(3) . . . . ? C6 N2 C3 C4 0.0(2) . . . . ? Ru1 N2 C3 C4 178.43(13) . . . . ? C1 C2 C3 N2 1.3(4) . . . . ? C1 C2 C3 C4 -175.6(2) . . . . ? N2 C3 C4 C5 -0.7(2) . . . . ? C2 C3 C4 C5 176.6(2) . . . . ? N2 C3 C4 C13 178.5(2) . . . . ? C2 C3 C4 C13 -4.1(4) . . . . ? C3 C4 C5 C6 1.2(2) . . . . ? C13 C4 C5 C6 -178.1(2) . . . . ? C3 C4 C5 C11 -179.6(2) . . . . ? C13 C4 C5 C11 1.2(4) . . . . ? C3 N2 C6 C7 -178.23(19) . . . . ? Ru1 N2 C6 C7 3.4(3) . . . . ? C3 N2 C6 C5 0.8(2) . . . . ? Ru1 N2 C6 C5 -177.59(14) . . . . ? C4 C5 C6 N2 -1.2(2) . . . . ? C11 C5 C6 N2 179.6(2) . . . . ? C4 C5 C6 C7 177.7(2) . . . . ? C11 C5 C6 C7 -1.5(4) . . . . ? N2 C6 C7 C8 0.4(3) . . . . ? C5 C6 C7 C8 -178.4(2) . . . . ? N2 C6 C7 C17 -178.42(18) . . . . ? C5 C6 C7 C17 2.8(3) . . . . ? C6 C7 C8 N1 -3.3(3) . . . 2_666 ? C17 C7 C8 N1 175.48(17) . . . 2_666 ? C6 C7 C8 C9 177.6(2) . . . . ? C17 C7 C8 C9 -3.6(3) . . . . ? N1 C8 C9 C10 -0.9(2) 2_666 . . . ? C7 C8 C9 C10 178.3(2) . . . . ? N1 C8 C9 C12 179.1(2) 2_666 . . . ? C7 C8 C9 C12 -1.7(4) . . . . ? C8 C9 C10 C1 -0.4(2) . . . 2_666 ? C12 C9 C10 C1 179.63(19) . . . 2_666 ? C8 C9 C10 C15 178.5(2) . . . . ? C12 C9 C10 C15 -1.5(4) . . . . ? C5 C4 C13 C14 80.5(4) . . . . ? C3 C4 C13 C14 -98.7(3) . . . . ? C9 C10 C15 C16 97.9(3) . . . . ? C1 C10 C15 C16 -83.4(3) 2_666 . . . ? C6 C7 C17 C22 -87.6(2) . . . . ? C8 C7 C17 C22 93.5(2) . . . . ? C6 C7 C17 C18 93.0(2) . . . . ? C8 C7 C17 C18 -85.9(2) . . . . ? C22 C17 C18 C19 0.3(3) . . . . ? C7 C17 C18 C19 179.8(2) . . . . ? C17 C18 C19 C20 -0.3(3) . . . . ? C17 C18 C19 C27 179.2(2) . . . . ? C18 C19 C20 C21 0.0(3) . . . . ? C27 C19 C20 C21 -179.6(2) . . . . ? C19 C20 C21 C22 0.3(3) . . . . ? C19 C20 C21 C23 -178.4(2) . . . . ? C18 C17 C22 C21 0.0(3) . . . . ? C7 C17 C22 C21 -179.4(2) . . . . ? C20 C21 C22 C17 -0.3(3) . . . . ? C23 C21 C22 C17 178.4(2) . . . . ? C20 C21 C23 C26 -122.1(3) . . . . ? C22 C21 C23 C26 59.2(3) . . . . ? C20 C21 C23 C24 118.7(3) . . . . ? C22 C21 C23 C24 -59.9(3) . . . . ? C20 C21 C23 C25 -1.1(4) . . . . ? C22 C21 C23 C25 -179.8(3) . . . . ? C18 C19 C27 C28 -73.0(4) . . . . ? C20 C19 C27 C28 106.5(3) . . . . ? C18 C19 C27 C30' 120.1(4) . . . . ? C20 C19 C27 C30' -60.4(4) . . . . ? C18 C19 C27 C28' -3.4(4) . . . . ? C20 C19 C27 C28' 176.1(3) . . . . ? C18 C19 C27 C29 164.8(3) . . . . ? C20 C19 C27 C29 -15.6(4) . . . . ? C18 C19 C27 C30 48.0(4) . . . . ? C20 C19 C27 C30 -132.5(3) . . . . ? C18 C19 C27 C29' -121.0(3) . . . . ? C20 C19 C27 C29' 58.6(4) . . . . ? Ru1 P1 C31 C32 21(4) . . . . ? C38 C33 C34 C35 -0.3(4) . . . . ? C32 C33 C34 C35 179.4(2) . . . . ? C33 C34 C35 C36 -0.9(4) . . . . ? C34 C35 C36 C37 1.0(5) . . . . ? C35 C36 C37 C38 0.0(5) . . . . ? C36 C37 C38 C33 -1.1(5) . . . . ? C34 C33 C38 C37 1.3(4) . . . . ? C32 C33 C38 C37 -178.5(3) . . . . ? C46 C41 C42 C43 1.0(4) . . . . ? C40 C41 C42 C43 -176.9(3) . . . . ? C41 C42 C43 C44 0.0(5) . . . . ? C42 C43 C44 C45 -0.7(5) . . . . ? C43 C44 C45 C46 0.5(5) . . . . ? C44 C45 C46 C41 0.4(4) . . . . ? C42 C41 C46 C45 -1.2(4) . . . . ? C40 C41 C46 C45 176.7(2) . . . . ? C54 C49 C50 C51 0.2(4) . . . . ? C48 C49 C50 C51 -176.6(2) . . . . ? C49 C50 C51 C52 0.3(4) . . . . ? C50 C51 C52 C53 -0.1(4) . . . . ? C51 C52 C53 C54 -0.6(4) . . . . ? C52 C53 C54 C49 1.1(4) . . . . ? C50 C49 C54 C53 -0.9(4) . . . . ? C48 C49 C54 C53 175.9(2) . . . . ? #===END ## Synthesis of phosphine and phosphonite complexes of a Ru(II) porphyrin ## ## E. Stulz, M. Maue, N. Feeder, S. Teat, Y.-F. Ng, A. D. Bond, S. Darling & J. K. M. Sanders ## ## Denoted [PAP(OEt)2]2Ru(DPP) in text ## data_js0020 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H106 N4 O4 P2 Ru' _chemical_formula_weight 1398.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 9.8043(2) _cell_length_b 10.7826(3) _cell_length_c 18.6293(6) _cell_angle_alpha 87.309(2) _cell_angle_beta 77.381(2) _cell_angle_gamma 84.103(2) _cell_volume 1911.06(9) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 12351 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 21731 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.986 _reflns_number_total 8637 _reflns_number_gt 7160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement '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^)+(0.0728P)^2^+1.7947P] 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 8637 _refine_ls_number_parameters 450 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.647 _refine_diff_density_min -1.187 _refine_diff_density_rms 0.155 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 1.0000 0.0000 1.0000 0.02617(11) Uani 1 2 d S . . P1 P 0.77446(8) 0.08009(7) 1.05351(4) 0.03609(19) Uani 1 1 d . . . O1 O 0.6627(2) -0.0192(2) 1.05978(14) 0.0535(6) Uani 1 1 d . . . O2 O 0.6985(3) 0.2124(3) 1.02750(17) 0.0713(8) Uani 1 1 d . . . N1 N 0.9336(2) -0.0712(2) 0.91364(12) 0.0266(5) Uani 1 1 d . . . N2 N 0.9594(2) -0.1578(2) 1.06542(12) 0.0283(5) Uani 1 1 d . . . C1 C 0.8801(3) -0.2725(3) 0.97419(15) 0.0310(6) Uani 1 1 d . . . H1 H 0.8490 -0.3504 0.9664 0.037 Uiso 1 1 calc R . . C2 C 0.8895(3) -0.1881(3) 0.91535(15) 0.0284(6) Uani 1 1 d . . . C3 C 0.8547(3) -0.2109(3) 0.84600(15) 0.0296(6) Uani 1 1 d . . . C4 C 0.8776(3) -0.1074(3) 0.80232(15) 0.0304(6) Uani 1 1 d . . . C5 C 0.9309(3) -0.0189(2) 0.84493(15) 0.0273(5) Uani 1 1 d . . . C6 C 0.9791(3) 0.0975(3) 0.82039(14) 0.0272(5) Uani 1 1 d . . . C7 C 1.0313(3) 0.1799(3) 0.86206(15) 0.0295(6) Uani 1 1 d . . . C8 C 1.0811(3) 0.3022(3) 0.83833(16) 0.0327(6) Uani 1 1 d . . . C9 C 1.1131(3) 0.3517(3) 0.89778(16) 0.0319(6) Uani 1 1 d . . . C10 C 0.9095(3) -0.2599(3) 1.04298(15) 0.0291(6) Uani 1 1 d . . . C11 C 0.8499(4) -0.0940(3) 0.72579(16) 0.0404(7) Uani 1 1 d . . . H11A H 0.7938 -0.0147 0.7208 0.061 Uiso 1 1 calc R . . H11B H 0.7986 -0.1631 0.7170 0.061 Uiso 1 1 calc R . . H11C H 0.9394 -0.0955 0.6898 0.061 Uiso 1 1 calc R . . C12 C 1.1013(4) 0.3679(3) 0.76410(18) 0.0484(8) Uani 1 1 d . . . H12A H 1.1608 0.3130 0.7270 0.073 Uiso 1 1 calc R . . H12B H 1.1465 0.4444 0.7658 0.073 Uiso 1 1 calc R . . H12C H 1.0098 0.3891 0.7512 0.073 Uiso 1 1 calc R . . C13 C 0.8015(3) -0.3296(3) 0.82842(16) 0.0336(6) Uani 1 1 d . . . H13A H 0.8448 -0.4005 0.8540 0.040 Uiso 1 1 calc R . . H13B H 0.8313 -0.3431 0.7748 0.040 Uiso 1 1 calc R . . C14 C 0.6425(3) -0.3280(3) 0.8510(2) 0.0502(9) Uani 1 1 d . . . H14A H 0.6142 -0.4085 0.8403 0.075 Uiso 1 1 calc R . . H14B H 0.5988 -0.2615 0.8234 0.075 Uiso 1 1 calc R . . H14C H 0.6120 -0.3130 0.9038 0.075 Uiso 1 1 calc R . . C15 C 1.1683(3) 0.4755(3) 0.90207(17) 0.0364(6) Uani 1 1 d . . . H15A H 1.1362 0.5055 0.9530 0.044 Uiso 1 1 calc R . . H15B H 1.1276 0.5365 0.8692 0.044 Uiso 1 1 calc R . . C16 C 1.3263(4) 0.4718(4) 0.8809(3) 0.0649(11) Uani 1 1 d . . . H16A H 1.3547 0.5555 0.8842 0.097 Uiso 1 1 calc R . . H16B H 1.3591 0.4430 0.8304 0.097 Uiso 1 1 calc R . . H16C H 1.3676 0.4144 0.9144 0.097 Uiso 1 1 calc R . . C17 C 0.9748(3) 0.1388(2) 0.74270(14) 0.0276(5) Uani 1 1 d . . . C18 C 1.0837(3) 0.1015(3) 0.68517(15) 0.0303(6) Uani 1 1 d . . . H18 H 1.1603 0.0469 0.6949 0.036 Uiso 1 1 calc R . . C19 C 1.0838(3) 0.1423(3) 0.61310(15) 0.0317(6) Uani 1 1 d . . . C20 C 0.9701(3) 0.2222(3) 0.60109(16) 0.0353(6) Uani 1 1 d . . . H20 H 0.9682 0.2502 0.5522 0.042 Uiso 1 1 calc R . . C21 C 0.8587(3) 0.2630(3) 0.65784(16) 0.0325(6) Uani 1 1 d . A . C22 C 0.8624(3) 0.2188(3) 0.72872(16) 0.0316(6) Uani 1 1 d . . . H22 H 0.7869 0.2436 0.7683 0.038 Uiso 1 1 calc R . . C23 C 1.2081(3) 0.1021(3) 0.55055(17) 0.0424(7) Uani 1 1 d . . . C24 C 1.2241(5) -0.0410(4) 0.5466(3) 0.0720(12) Uani 1 1 d . . . H24A H 1.3039 -0.0673 0.5069 0.108 Uiso 1 1 calc R . . H24B H 1.1382 -0.0694 0.5370 0.108 Uiso 1 1 calc R . . H24C H 1.2405 -0.0775 0.5936 0.108 Uiso 1 1 calc R . . C25 C 1.1899(4) 0.1523(5) 0.4752(2) 0.0722(13) Uani 1 1 d . . . H25A H 1.2716 0.1221 0.4377 0.108 Uiso 1 1 calc R . . H25B H 1.1813 0.2437 0.4748 0.108 Uiso 1 1 calc R . . H25C H 1.1049 0.1235 0.4646 0.108 Uiso 1 1 calc R . . C26 C 1.3404(4) 0.1464(6) 0.5666(2) 0.0791(14) Uani 1 1 d . . . H26A H 1.4201 0.1241 0.5260 0.119 Uiso 1 1 calc R . . H26B H 1.3585 0.1065 0.6124 0.119 Uiso 1 1 calc R . . H26C H 1.3279 0.2371 0.5717 0.119 Uiso 1 1 calc R . . C27 C 0.7386(3) 0.3552(3) 0.64178(18) 0.0430(7) Uani 1 1 d D . . C28 C 0.6498(6) 0.2904(6) 0.6017(4) 0.075(2) Uani 0.70 1 d PD A 1 H28A H 0.6118 0.2199 0.6320 0.112 Uiso 0.70 1 calc PR A 1 H28B H 0.7073 0.2600 0.5549 0.112 Uiso 0.70 1 calc PR A 1 H28C H 0.5722 0.3492 0.5922 0.112 Uiso 0.70 1 calc PR A 1 C29 C 0.6432(7) 0.4086(6) 0.7119(3) 0.0688(19) Uani 0.70 1 d PD A 1 H29A H 0.6990 0.4508 0.7393 0.103 Uiso 0.70 1 calc PR A 1 H29B H 0.5998 0.3408 0.7426 0.103 Uiso 0.70 1 calc PR A 1 H29C H 0.5698 0.4685 0.6989 0.103 Uiso 0.70 1 calc PR A 1 C30 C 0.7981(7) 0.4641(6) 0.5940(5) 0.098(3) Uani 0.70 1 d PD A 1 H30A H 0.8558 0.5071 0.6199 0.147 Uiso 0.70 1 calc PR A 1 H30B H 0.7207 0.5226 0.5839 0.147 Uiso 0.70 1 calc PR A 1 H30C H 0.8559 0.4327 0.5475 0.147 Uiso 0.70 1 calc PR A 1 C31 C 0.725(2) 0.4649(17) 0.6893(11) 0.109(4) Uiso 0.30 1 d PD A 2 H31A H 0.7112 0.4369 0.7409 0.164 Uiso 0.30 1 calc PR A 2 H31B H 0.6440 0.5220 0.6824 0.164 Uiso 0.30 1 calc PR A 2 H31C H 0.8104 0.5082 0.6758 0.164 Uiso 0.30 1 calc PR A 2 C32 C 0.756(2) 0.395(2) 0.5616(8) 0.109(4) Uiso 0.30 1 d PD A 2 H32A H 0.7717 0.3203 0.5314 0.164 Uiso 0.30 1 calc PR A 2 H32B H 0.8360 0.4443 0.5472 0.164 Uiso 0.30 1 calc PR A 2 H32C H 0.6703 0.4446 0.5543 0.164 Uiso 0.30 1 calc PR A 2 C33 C 0.6048(19) 0.2881(19) 0.6615(12) 0.109(4) Uiso 0.30 1 d PD A 2 H33A H 0.6139 0.2170 0.6293 0.164 Uiso 0.30 1 calc PR A 2 H33B H 0.5243 0.3459 0.6549 0.164 Uiso 0.30 1 calc PR A 2 H33C H 0.5903 0.2583 0.7129 0.164 Uiso 0.30 1 calc PR A 2 C55 C 0.6529(7) 0.3709(4) 1.4016(2) 0.0810(16) Uani 1 1 d . . . H55 H 0.6345 0.4161 1.4458 0.097 Uiso 1 1 calc R . . C56 C 0.7827(6) 0.3690(4) 1.3554(2) 0.0750(13) Uani 1 1 d . . . H56 H 0.8543 0.4117 1.3677 0.090 Uiso 1 1 calc R . . C57 C 0.8087(5) 0.3037(3) 1.2903(2) 0.0571(10) Uani 1 1 d . . . H57 H 0.8988 0.3012 1.2583 0.069 Uiso 1 1 calc R . . C58 C 0.7052(4) 0.2428(3) 1.27188(19) 0.0455(8) Uani 1 1 d . . . C59 C 0.5737(4) 0.2440(4) 1.3202(2) 0.0645(11) Uani 1 1 d . . . H59 H 0.5019 0.2008 1.3086 0.077 Uiso 1 1 calc R . . C60 C 0.5491(6) 0.3083(5) 1.3849(2) 0.0781(15) Uani 1 1 d . . . H60 H 0.4603 0.3092 1.4180 0.094 Uiso 1 1 calc R . . C69 C 0.7295(3) 0.1810(3) 1.2034(2) 0.0439(7) Uani 1 1 d . . . C70 C 0.7471(3) 0.1333(3) 1.1447(2) 0.0432(7) Uani 1 1 d . . . C83 C 0.5214(4) -0.0035(4) 1.1050(3) 0.0682(12) Uani 1 1 d . . . H83A H 0.4522 -0.0158 1.0750 0.082 Uiso 1 1 calc R . . H83B H 0.5015 0.0819 1.1243 0.082 Uiso 1 1 calc R . . C84 C 0.5096(5) -0.0960(5) 1.1667(3) 0.0869(15) Uani 1 1 d . . . H84A H 0.4144 -0.0863 1.1972 0.130 Uiso 1 1 calc R . . H84B H 0.5774 -0.0826 1.1965 0.130 Uiso 1 1 calc R . . H84C H 0.5293 -0.1803 1.1472 0.130 Uiso 1 1 calc R . . C85 C 0.6756(5) 0.2301(4) 0.9574(2) 0.0680(11) Uani 1 1 d . . . H85A H 0.5795 0.2103 0.9567 0.082 Uiso 1 1 calc R . . H85B H 0.7431 0.1732 0.9236 0.082 Uiso 1 1 calc R . . C86 C 0.6926(5) 0.3608(4) 0.9323(3) 0.0718(12) Uani 1 1 d . . . H86A H 0.6752 0.3726 0.8825 0.108 Uiso 1 1 calc R . . H86B H 0.7884 0.3796 0.9320 0.108 Uiso 1 1 calc R . . H86C H 0.6255 0.4168 0.9657 0.108 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 0.03361(18) 0.02796(18) 0.02002(17) 0.00236(11) -0.00773(12) - 0.01441(12) P1 0.0348(4) 0.0392(4) 0.0364(4) 0.0082(3) -0.0107(3) -0.0114(3) O1 0.0410(12) 0.0630(16) 0.0577(16) -0.0066(12) -0.0038(11) -0.0235(11) O2 0.0536(15) 0.088(2) 0.0679(19) 0.0297(16) -0.0150(14) 0.0038(14) N1 0.0333(11) 0.0288(12) 0.0205(11) 0.0020(9) -0.0073(9) -0.0132(9) N2 0.0360(12) 0.0286(12) 0.0230(11) 0.0020(9) -0.0080(9) -0.0133(9) C1 0.0386(15) 0.0303(14) 0.0276(14) 0.0000(11) -0.0088(11) -0.0168(11) C2 0.0340(14) 0.0302(14) 0.0235(13) -0.0013(11) -0.0070(11) -0.0123(11) C3 0.0334(14) 0.0322(14) 0.0255(14) -0.0029(11) -0.0069(11) -0.0121(11) C4 0.0346(14) 0.0350(15) 0.0241(14) -0.0022(11) -0.0089(11) -0.0084(11) C5 0.0306(13) 0.0294(14) 0.0234(13) -0.0006(10) -0.0069(10) -0.0078(10) C6 0.0316(13) 0.0301(14) 0.0212(13) 0.0021(10) -0.0073(10) -0.0062(10) C7 0.0339(14) 0.0305(14) 0.0250(14) 0.0027(11) -0.0056(11) -0.0100(11) C8 0.0407(15) 0.0309(15) 0.0287(15) 0.0043(11) -0.0105(12) -0.0100(12) C9 0.0343(14) 0.0314(15) 0.0316(15) 0.0049(11) -0.0078(11) -0.0113(11) C10 0.0348(14) 0.0293(14) 0.0257(14) 0.0025(11) -0.0081(11) -0.0135(11) C11 0.0596(19) 0.0408(17) 0.0283(16) 0.0019(13) -0.0197(14) -0.0184(14) C12 0.078(2) 0.0388(18) 0.0353(18) 0.0125(14) -0.0198(16) -0.0289(16) C13 0.0433(16) 0.0320(15) 0.0286(15) -0.0037(11) -0.0113(12) - 0.0092(12) C14 0.0449(18) 0.0377(18) 0.072(3) -0.0081(16) -0.0163(17) -0.0124(14) C15 0.0463(16) 0.0303(15) 0.0359(16) 0.0058(12) -0.0116(13) -0.0158(12) C16 0.049(2) 0.056(2) 0.089(3) -0.004(2) -0.003(2) -0.0249(18) C17 0.0352(14) 0.0275(13) 0.0224(13) 0.0020(10) -0.0091(11) -0.0082(10) C18 0.0304(13) 0.0327(14) 0.0284(14) 0.0029(11) -0.0080(11) -0.0037(11) C19 0.0358(14) 0.0334(15) 0.0254(14) 0.0007(11) -0.0052(11) -0.0049(11) C20 0.0468(16) 0.0373(16) 0.0240(14) 0.0033(12) -0.0124(12) -0.0052(12) C21 0.0382(15) 0.0322(15) 0.0285(15) -0.0023(11) -0.0109(12) - 0.0014(11) C22 0.0356(14) 0.0324(15) 0.0264(14) -0.0022(11) -0.0059(11) - 0.0024(11) C23 0.0389(16) 0.054(2) 0.0306(16) 0.0038(14) -0.0011(13) -0.0021(14) C24 0.074(3) 0.069(3) 0.059(3) -0.012(2) 0.012(2) 0.009(2) C25 0.060(2) 0.117(4) 0.0294(19) 0.007(2) 0.0044(17) 0.005(2) C26 0.043(2) 0.138(5) 0.054(3) -0.007(3) 0.0030(18) -0.023(2) C27 0.0511(18) 0.0428(18) 0.0345(17) -0.0012(14) -0.0145(14) 0.0099(14) C28 0.057(3) 0.082(4) 0.095(5) -0.022(4) -0.050(4) 0.025(3) C29 0.074(4) 0.081(4) 0.043(3) -0.011(3) -0.017(3) 0.049(3) C30 0.060(4) 0.069(4) 0.145(7) 0.072(5) -0.005(4) 0.017(3) C55 0.136(5) 0.053(3) 0.038(2) -0.0011(19) -0.004(3) 0.028(3) C56 0.128(4) 0.049(2) 0.049(2) -0.0024(19) -0.017(3) -0.018(2) C57 0.079(3) 0.042(2) 0.046(2) -0.0007(16) -0.0016(18) -0.0117(18) C58 0.0545(19) 0.0343(17) 0.0414(19) 0.0027(14) -0.0032(15) 0.0082(14) C59 0.053(2) 0.074(3) 0.057(2) 0.006(2) -0.0028(18) 0.0180(19) C60 0.085(3) 0.081(3) 0.048(2) 0.004(2) 0.009(2) 0.037(3) C69 0.0426(17) 0.0367(17) 0.048(2) 0.0010(15) -0.0045(14) 0.0019(13) C70 0.0384(16) 0.0372(17) 0.051(2) -0.0016(15) -0.0039(14) -0.0019(13) C83 0.042(2) 0.067(3) 0.092(3) -0.003(2) -0.003(2) -0.0149(18) C84 0.073(3) 0.095(4) 0.083(4) -0.001(3) 0.016(2) -0.037(3) C85 0.071(3) 0.074(3) 0.059(3) -0.004(2) -0.013(2) -0.009(2) C86 0.106(4) 0.048(2) 0.065(3) 0.006(2) -0.035(3) 0.005(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 N2 2.067(2) . ? Ru1 N2 2.067(2) 2_757 ? Ru1 N1 2.068(2) . ? Ru1 N1 2.068(2) 2_757 ? Ru1 P1 2.3140(8) 2_757 ? Ru1 P1 2.3140(8) . ? P1 O1 1.592(2) . ? P1 O2 1.643(3) . ? P1 C70 1.774(4) . ? O1 C83 1.453(5) . ? O2 C85 1.374(5) . ? N1 C2 1.372(3) . ? N1 C5 1.378(3) . ? N2 C10 1.367(3) . ? N2 C7 1.382(3) 2_757 ? C1 C2 1.385(4) . ? C1 C10 1.389(4) . ? C1 H1 0.9500 . ? C2 C3 1.444(4) . ? C3 C4 1.358(4) . ? C3 C13 1.507(4) . ? C4 C5 1.472(4) . ? C4 C11 1.506(4) . ? C5 C6 1.408(4) . ? C6 C7 1.409(4) . ? C6 C17 1.502(4) . ? C7 N2 1.382(3) 2_757 ? C7 C8 1.469(4) . ? C8 C9 1.361(4) . ? C8 C12 1.507(4) . ? C9 C10 1.443(4) 2_757 ? C9 C15 1.503(4) . ? C10 C9 1.443(4) 2_757 ? 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 1.522(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.509(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.379(4) . ? C17 C22 1.391(4) . ? C18 C19 1.393(4) . ? C18 H18 0.9500 . ? C19 C20 1.388(4) . ? C19 C23 1.533(4) . ? C20 C21 1.395(4) . ? C20 H20 0.9500 . ? C21 C22 1.389(4) . ? C21 C27 1.533(4) . ? C22 H22 0.9500 . ? C23 C26 1.520(5) . ? C23 C25 1.521(5) . ? C23 C24 1.538(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C31 1.488(14) . ? C27 C28 1.504(6) . ? C27 C32 1.512(14) . ? C27 C30 1.526(6) . ? C27 C29 1.530(6) . ? C27 C33 1.530(14) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C55 C56 1.371(7) . ? C55 C60 1.374(8) . ? C55 H55 0.9500 . ? C56 C57 1.394(6) . ? C56 H56 0.9500 . ? C57 C58 1.373(5) . ? C57 H57 0.9500 . ? C58 C59 1.401(5) . ? C58 C69 1.430(5) . ? C59 C60 1.382(6) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C69 C70 1.201(5) . ? C83 C84 1.479(7) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 C86 1.479(6) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N2 180.000(1) . 2_757 ? N2 Ru1 N1 92.68(9) . . ? N2 Ru1 N1 87.32(8) 2_757 . ? N2 Ru1 N1 87.32(8) . 2_757 ? N2 Ru1 N1 92.68(9) 2_757 2_757 ? N1 Ru1 N1 180.000(1) . 2_757 ? N2 Ru1 P1 93.26(7) . 2_757 ? N2 Ru1 P1 86.74(7) 2_757 2_757 ? N1 Ru1 P1 87.89(6) . 2_757 ? N1 Ru1 P1 92.11(6) 2_757 2_757 ? N2 Ru1 P1 86.74(7) . . ? N2 Ru1 P1 93.26(7) 2_757 . ? N1 Ru1 P1 92.11(6) . . ? N1 Ru1 P1 87.89(6) 2_757 . ? P1 Ru1 P1 180.0 2_757 . ? O1 P1 O2 105.94(15) . . ? O1 P1 C70 103.35(15) . . ? O2 P1 C70 90.68(16) . . ? O1 P1 Ru1 112.69(10) . . ? O2 P1 Ru1 123.97(11) . . ? C70 P1 Ru1 116.71(11) . . ? C83 O1 P1 123.9(3) . . ? C85 O2 P1 121.2(3) . . ? C2 N1 C5 107.3(2) . . ? C2 N1 Ru1 123.32(17) . . ? C5 N1 Ru1 129.27(17) . . ? C10 N2 C7 107.3(2) . 2_757 ? C10 N2 Ru1 123.64(18) . . ? C7 N2 Ru1 128.94(18) 2_757 . ? C2 C1 C10 129.4(3) . . ? C2 C1 H1 115.3 . . ? C10 C1 H1 115.3 . . ? N1 C2 C1 125.6(2) . . ? N1 C2 C3 109.7(2) . . ? C1 C2 C3 124.8(2) . . ? C4 C3 C2 107.7(2) . . ? C4 C3 C13 128.0(3) . . ? C2 C3 C13 124.3(2) . . ? C3 C4 C5 106.5(2) . . ? C3 C4 C11 123.6(3) . . ? C5 C4 C11 129.9(3) . . ? N1 C5 C6 124.0(2) . . ? N1 C5 C4 108.8(2) . . ? C6 C5 C4 127.1(2) . . ? C5 C6 C7 126.0(2) . . ? C5 C6 C17 117.5(2) . . ? C7 C6 C17 116.5(2) . . ? N2 C7 C6 124.2(2) 2_757 . ? N2 C7 C8 108.5(2) 2_757 . ? C6 C7 C8 127.4(3) . . ? C9 C8 C7 106.9(2) . . ? C9 C8 C12 122.5(3) . . ? C7 C8 C12 130.5(3) . . ? C8 C9 C10 107.1(2) . 2_757 ? C8 C9 C15 127.7(3) . . ? C10 C9 C15 125.1(3) 2_757 . ? N2 C10 C1 125.4(2) . . ? N2 C10 C9 110.1(2) . 2_757 ? C1 C10 C9 124.6(2) . 2_757 ? C4 C11 H11A 109.5 . . ? C4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 C14 113.0(3) . . ? C3 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? C3 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? 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 . . ? C9 C15 C16 113.9(3) . . ? C9 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? C9 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 119.5(2) . . ? C18 C17 C6 120.6(2) . . ? C22 C17 C6 119.9(2) . . ? C17 C18 C19 121.4(3) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C20 C19 C18 117.6(3) . . ? C20 C19 C23 122.2(3) . . ? C18 C19 C23 120.2(3) . . ? C19 C20 C21 122.7(3) . . ? C19 C20 H20 118.6 . . ? C21 C20 H20 118.6 . . ? C22 C21 C20 117.6(3) . . ? C22 C21 C27 121.9(3) . . ? C20 C21 C27 120.5(3) . . ? C21 C22 C17 121.1(3) . . ? C21 C22 H22 119.4 . . ? C17 C22 H22 119.4 . . ? C26 C23 C25 109.2(3) . . ? C26 C23 C19 108.6(3) . . ? C25 C23 C19 113.5(3) . . ? C26 C23 C24 109.7(4) . . ? C25 C23 C24 106.6(4) . . ? C19 C23 C24 109.1(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C31 C27 C28 138.7(9) . . ? C31 C27 C32 111.3(11) . . ? C28 C27 C32 66.3(8) . . ? C31 C27 C30 71.6(9) . . ? C28 C27 C30 109.0(5) . . ? C32 C27 C30 44.4(8) . . ? C31 C27 C29 40.9(8) . . ? C28 C27 C29 107.9(4) . . ? C32 C27 C29 132.3(9) . . ? C30 C27 C29 107.8(5) . . ? C31 C27 C33 110.0(10) . . ? C28 C27 C33 42.7(8) . . ? C32 C27 C33 106.2(10) . . ? C30 C27 C33 140.1(9) . . ? C29 C27 C33 70.1(8) . . ? C31 C27 C21 108.4(9) . . ? C28 C27 C21 109.6(3) . . ? C32 C27 C21 113.8(9) . . ? C30 C27 C21 110.0(3) . . ? C29 C27 C21 112.4(3) . . ? C33 C27 C21 107.0(9) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C31 H31A 109.5 . . ? C27 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C27 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 H33A 109.5 . . ? C27 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C27 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C56 C55 C60 120.9(4) . . ? C56 C55 H55 119.6 . . ? C60 C55 H55 119.6 . . ? C55 C56 C57 119.3(5) . . ? C55 C56 H56 120.3 . . ? C57 C56 H56 120.3 . . ? C58 C57 C56 120.6(4) . . ? C58 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C57 C58 C59 119.5(4) . . ? C57 C58 C69 120.6(3) . . ? C59 C58 C69 119.9(4) . . ? C60 C59 C58 119.6(5) . . ? C60 C59 H59 120.2 . . ? C58 C59 H59 120.2 . . ? C55 C60 C59 120.2(4) . . ? C55 C60 H60 119.9 . . ? C59 C60 H60 119.9 . . ? C70 C69 C58 177.3(4) . . ? C69 C70 P1 173.5(3) . . ? O1 C83 C84 109.0(4) . . ? O1 C83 H83A 109.9 . . ? C84 C83 H83A 109.9 . . ? O1 C83 H83B 109.9 . . ? C84 C83 H83B 109.9 . . ? H83A C83 H83B 108.3 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? O2 C85 C86 110.1(4) . . ? O2 C85 H85A 109.6 . . ? C86 C85 H85A 109.6 . . ? O2 C85 H85B 109.6 . . ? C86 C85 H85B 109.6 . . ? H85A C85 H85B 108.2 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 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 N2 Ru1 P1 O1 -43.69(13) . . . . ? N2 Ru1 P1 O1 136.31(13) 2_757 . . . ? N1 Ru1 P1 O1 48.87(13) . . . . ? N1 Ru1 P1 O1 -131.13(13) 2_757 . . . ? N2 Ru1 P1 O2 -173.52(16) . . . . ? N2 Ru1 P1 O2 6.48(16) 2_757 . . . ? N1 Ru1 P1 O2 -80.96(16) . . . . ? N1 Ru1 P1 O2 99.04(16) 2_757 . . . ? N2 Ru1 P1 C70 75.68(14) . . . . ? N2 Ru1 P1 C70 -104.32(14) 2_757 . . . ? N1 Ru1 P1 C70 168.25(14) . . . . ? N1 Ru1 P1 C70 -11.75(14) 2_757 . . . ? O2 P1 O1 C83 -55.6(3) . . . . ? C70 P1 O1 C83 39.0(3) . . . . ? Ru1 P1 O1 C83 165.9(3) . . . . ? O1 P1 O2 C85 -71.3(3) . . . . ? C70 P1 O2 C85 -175.4(3) . . . . ? Ru1 P1 O2 C85 61.3(4) . . . . ? N2 Ru1 N1 C2 -2.2(2) . . . . ? N2 Ru1 N1 C2 177.8(2) 2_757 . . . ? P1 Ru1 N1 C2 91.0(2) 2_757 . . . ? P1 Ru1 N1 C2 -89.0(2) . . . . ? N2 Ru1 N1 C5 -178.5(2) . . . . ? N2 Ru1 N1 C5 1.5(2) 2_757 . . . ? P1 Ru1 N1 C5 -85.4(2) 2_757 . . . ? P1 Ru1 N1 C5 94.6(2) . . . . ? N1 Ru1 N2 C10 1.4(2) . . . . ? N1 Ru1 N2 C10 -178.6(2) 2_757 . . . ? P1 Ru1 N2 C10 -86.7(2) 2_757 . . . ? P1 Ru1 N2 C10 93.3(2) . . . . ? N1 Ru1 N2 C7 -175.1(2) . . . 2_757 ? N1 Ru1 N2 C7 4.9(2) 2_757 . . 2_757 ? P1 Ru1 N2 C7 96.9(2) 2_757 . . 2_757 ? P1 Ru1 N2 C7 -83.1(2) . . . 2_757 ? C5 N1 C2 C1 178.5(3) . . . . ? Ru1 N1 C2 C1 1.5(4) . . . . ? C5 N1 C2 C3 -1.1(3) . . . . ? Ru1 N1 C2 C3 -178.15(17) . . . . ? C10 C1 C2 N1 1.0(5) . . . . ? C10 C1 C2 C3 -179.4(3) . . . . ? N1 C2 C3 C4 -0.1(3) . . . . ? C1 C2 C3 C4 -179.8(3) . . . . ? N1 C2 C3 C13 -179.6(2) . . . . ? C1 C2 C3 C13 0.8(4) . . . . ? C2 C3 C4 C5 1.3(3) . . . . ? C13 C3 C4 C5 -179.3(3) . . . . ? C2 C3 C4 C11 -178.5(3) . . . . ? C13 C3 C4 C11 0.9(5) . . . . ? C2 N1 C5 C6 -175.1(2) . . . . ? Ru1 N1 C5 C6 1.7(4) . . . . ? C2 N1 C5 C4 1.9(3) . . . . ? Ru1 N1 C5 C4 178.69(18) . . . . ? C3 C4 C5 N1 -2.0(3) . . . . ? C11 C4 C5 N1 177.8(3) . . . . ? C3 C4 C5 C6 174.9(3) . . . . ? C11 C4 C5 C6 -5.3(5) . . . . ? N1 C5 C6 C7 -2.8(4) . . . . ? C4 C5 C6 C7 -179.2(3) . . . . ? N1 C5 C6 C17 177.4(2) . . . . ? C4 C5 C6 C17 0.9(4) . . . . ? C5 C6 C7 N2 -0.9(5) . . . 2_757 ? C17 C6 C7 N2 179.0(2) . . . 2_757 ? C5 C6 C7 C8 -179.4(3) . . . . ? C17 C6 C7 C8 0.4(4) . . . . ? N2 C7 C8 C9 -2.4(3) 2_757 . . . ? C6 C7 C8 C9 176.3(3) . . . . ? N2 C7 C8 C12 175.9(3) 2_757 . . . ? C6 C7 C8 C12 -5.5(5) . . . . ? C7 C8 C9 C10 2.7(3) . . . 2_757 ? C12 C8 C9 C10 -175.8(3) . . . 2_757 ? C7 C8 C9 C15 -179.9(3) . . . . ? C12 C8 C9 C15 1.6(5) . . . . ? C7 N2 C10 C1 177.4(3) 2_757 . . . ? Ru1 N2 C10 C1 0.3(4) . . . . ? C7 N2 C10 C9 -0.5(3) 2_757 . . 2_757 ? Ru1 N2 C10 C9 -177.65(18) . . . 2_757 ? C2 C1 C10 N2 -2.1(5) . . . . ? C2 C1 C10 C9 175.6(3) . . . 2_757 ? C4 C3 C13 C14 -91.3(4) . . . . ? C2 C3 C13 C14 88.0(4) . . . . ? C8 C9 C15 C16 -87.7(4) . . . . ? C10 C9 C15 C16 89.3(4) 2_757 . . . ? C5 C6 C17 C18 -85.4(3) . . . . ? C7 C6 C17 C18 94.7(3) . . . . ? C5 C6 C17 C22 96.9(3) . . . . ? C7 C6 C17 C22 -83.0(3) . . . . ? C22 C17 C18 C19 0.0(4) . . . . ? C6 C17 C18 C19 -177.8(3) . . . . ? C17 C18 C19 C20 0.1(4) . . . . ? C17 C18 C19 C23 178.4(3) . . . . ? C18 C19 C20 C21 0.6(4) . . . . ? C23 C19 C20 C21 -177.7(3) . . . . ? C19 C20 C21 C22 -1.3(4) . . . . ? C19 C20 C21 C27 177.6(3) . . . . ? C20 C21 C22 C17 1.3(4) . . . . ? C27 C21 C22 C17 -177.6(3) . . . . ? C18 C17 C22 C21 -0.7(4) . . . . ? C6 C17 C22 C21 177.0(3) . . . . ? C20 C19 C23 C26 118.6(4) . . . . ? C18 C19 C23 C26 -59.7(4) . . . . ? C20 C19 C23 C25 -3.1(5) . . . . ? C18 C19 C23 C25 178.6(3) . . . . ? C20 C19 C23 C24 -121.8(3) . . . . ? C18 C19 C23 C24 59.9(4) . . . . ? C22 C21 C27 C31 54.1(10) . . . . ? C20 C21 C27 C31 -124.7(9) . . . . ? C22 C21 C27 C28 -109.5(4) . . . . ? C20 C21 C27 C28 71.6(5) . . . . ? C22 C21 C27 C32 178.5(10) . . . . ? C20 C21 C27 C32 -0.3(10) . . . . ? C22 C21 C27 C30 130.7(5) . . . . ? C20 C21 C27 C30 -48.2(5) . . . . ? C22 C21 C27 C29 10.5(5) . . . . ? C20 C21 C27 C29 -168.4(4) . . . . ? C22 C21 C27 C33 -64.5(9) . . . . ? C20 C21 C27 C33 116.7(9) . . . . ? C60 C55 C56 C57 0.7(7) . . . . ? C55 C56 C57 C58 0.7(6) . . . . ? C56 C57 C58 C59 -1.7(6) . . . . ? C56 C57 C58 C69 176.9(4) . . . . ? C57 C58 C59 C60 1.3(6) . . . . ? C69 C58 C59 C60 -177.3(3) . . . . ? C56 C55 C60 C59 -1.2(7) . . . . ? C58 C59 C60 C55 0.2(6) . . . . ? P1 O1 C83 C84 -111.7(4) . . . . ? P1 O2 C85 C86 -144.8(3) . . . . ? #===END