data_obada1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H50 Cl N O P2 Ru' _chemical_formula_sum 'C27 H50 Cl N O P2 Ru' _chemical_formula_weight 603.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.119(3) _cell_length_b 14.860(3) _cell_length_c 11.625(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.00(3) _cell_angle_gamma 90.00 _cell_volume 2946.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 39322 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 27.22 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.183 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.751 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8787 _exptl_absorpt_correction_T_max 0.9702 _exptl_absorpt_process_details empirical _exptl_special_details ; 'X-SHAPE 2.07 (03-Aug-2005) Stoe & Cie, Darmstadt, Germany' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40503 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.84 _reflns_number_total 6267 _reflns_number_gt 5119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+2.7620P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6267 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.210090(14) 0.487404(14) 0.36695(2) 0.01299(7) Uani 1 1 d . . . P1 P 0.27342(5) 0.55124(5) 0.54168(7) 0.01606(16) Uani 1 1 d . . . Cl1 Cl 0.11645(5) 0.41354(5) 0.48398(7) 0.02670(18) Uani 1 1 d . . . O1 O 0.29845(14) 0.59396(15) 0.2152(2) 0.0229(5) Uani 1 1 d . . . N1 N 0.55640(16) 0.06889(16) 0.4352(3) 0.0222(6) Uani 1 1 d . . . H1A H 0.5480 0.0330 0.4931 0.027 Uiso 1 1 calc R . . H1B H 0.5940 0.0566 0.3907 0.027 Uiso 1 1 calc R . . C1 C 0.28926(18) 0.3880(2) 0.3747(3) 0.0182(6) Uani 1 1 d . . . H1C H 0.2723 0.3368 0.4147 0.022 Uiso 1 1 calc R . . P2 P 0.12800(4) 0.43761(5) 0.20087(7) 0.01407(16) Uani 1 1 d . . . C2 C 0.35992(18) 0.3761(2) 0.3375(3) 0.0193(6) Uani 1 1 d . . . H2A H 0.3791 0.4216 0.2899 0.023 Uiso 1 1 calc R . . C3 C 0.41102(18) 0.29676(19) 0.3647(3) 0.0176(6) Uani 1 1 d . . . C4 C 0.40166(18) 0.2409(2) 0.4598(3) 0.0175(6) Uani 1 1 d . . . H4A H 0.3616 0.2540 0.5090 0.021 Uiso 1 1 calc R . . C5 C 0.44994(18) 0.16650(19) 0.4836(3) 0.0175(6) Uani 1 1 d . . . H5A H 0.4420 0.1293 0.5480 0.021 Uiso 1 1 calc R . . C6 C 0.50969(17) 0.14606(19) 0.4139(3) 0.0163(6) Uani 1 1 d . . . C7 C 0.52000(18) 0.2021(2) 0.3199(3) 0.0196(6) Uani 1 1 d . . . H7A H 0.5608 0.1898 0.2717 0.024 Uiso 1 1 calc R . . C8 C 0.47134(18) 0.2750(2) 0.2965(3) 0.0188(6) Uani 1 1 d . . . H8A H 0.4792 0.3117 0.2316 0.023 Uiso 1 1 calc R . . C9 C 0.26765(19) 0.5547(2) 0.2732(3) 0.0264(8) Uani 1 1 d . . . C10 C 0.19541(19) 0.5992(2) 0.6253(3) 0.0208(7) Uani 1 1 d . . . H10A H 0.1699 0.5467 0.6607 0.025 Uiso 1 1 calc R . . C11 C 0.1310(2) 0.6452(2) 0.5467(3) 0.0264(7) Uani 1 1 d . . . H11A H 0.0910 0.6694 0.5936 0.040 Uiso 1 1 calc R . . H11B H 0.1069 0.6014 0.4915 0.040 Uiso 1 1 calc R . . H11C H 0.1538 0.6945 0.5046 0.040 Uiso 1 1 calc R . . C12 C 0.2233(2) 0.6615(2) 0.7255(3) 0.0292(8) Uani 1 1 d . . . H12A H 0.1779 0.6827 0.7639 0.044 Uiso 1 1 calc R . . H12B H 0.2508 0.7132 0.6958 0.044 Uiso 1 1 calc R . . H12C H 0.2589 0.6285 0.7811 0.044 Uiso 1 1 calc R . . C13 C 0.34583(19) 0.6426(2) 0.5272(3) 0.0214(7) Uani 1 1 d . . . H13A H 0.3639 0.6629 0.6071 0.026 Uiso 1 1 calc R . . C14 C 0.3114(2) 0.7250(2) 0.4622(3) 0.0261(7) Uani 1 1 d . . . H14A H 0.3523 0.7707 0.4579 0.039 Uiso 1 1 calc R . . H14B H 0.2686 0.7498 0.5031 0.039 Uiso 1 1 calc R . . H14C H 0.2913 0.7073 0.3840 0.039 Uiso 1 1 calc R . . C15 C 0.4180(2) 0.6066(2) 0.4729(3) 0.0265(7) Uani 1 1 d . . . H15A H 0.4556 0.6556 0.4662 0.040 Uiso 1 1 calc R . . H15B H 0.4020 0.5823 0.3961 0.040 Uiso 1 1 calc R . . H15C H 0.4424 0.5589 0.5218 0.040 Uiso 1 1 calc R . . C16 C 0.33160(19) 0.4702(2) 0.6374(3) 0.0211(7) Uani 1 1 d . . . H16A H 0.3675 0.4390 0.5869 0.025 Uiso 1 1 calc R . . C17 C 0.3847(2) 0.5099(2) 0.7378(3) 0.0339(8) Uani 1 1 d . . . H17A H 0.4121 0.4610 0.7814 0.051 Uiso 1 1 calc R . . H17B H 0.3528 0.5437 0.7889 0.051 Uiso 1 1 calc R . . H17C H 0.4233 0.5502 0.7074 0.051 Uiso 1 1 calc R . . C18 C 0.2803(2) 0.3963(2) 0.6832(3) 0.0261(7) Uani 1 1 d . . . H18A H 0.3131 0.3554 0.7327 0.039 Uiso 1 1 calc R . . H18B H 0.2544 0.3626 0.6182 0.039 Uiso 1 1 calc R . . H18C H 0.2406 0.4237 0.7281 0.039 Uiso 1 1 calc R . . C19 C 0.04636(17) 0.5214(2) 0.1762(3) 0.0175(6) Uani 1 1 d . . . H19A H 0.0241 0.5155 0.0941 0.021 Uiso 1 1 calc R . . C20 C 0.0779(2) 0.6170(2) 0.1930(3) 0.0226(7) Uani 1 1 d . . . H20A H 0.0347 0.6600 0.1799 0.034 Uiso 1 1 calc R . . H20B H 0.1170 0.6285 0.1379 0.034 Uiso 1 1 calc R . . H20C H 0.1024 0.6238 0.2719 0.034 Uiso 1 1 calc R . . C21 C -0.02027(18) 0.5052(2) 0.2532(3) 0.0250(7) Uani 1 1 d . . . H21A H -0.0611 0.5508 0.2368 0.038 Uiso 1 1 calc R . . H21B H 0.0001 0.5093 0.3345 0.038 Uiso 1 1 calc R . . H21C H -0.0425 0.4453 0.2377 0.038 Uiso 1 1 calc R . . C22 C 0.16457(19) 0.4276(2) 0.0548(3) 0.0212(7) Uani 1 1 d . . . H22A H 0.1236 0.3935 0.0060 0.025 Uiso 1 1 calc R . . C23 C 0.1766(2) 0.5164(2) -0.0083(3) 0.0291(7) Uani 1 1 d . . . H23A H 0.1955 0.5038 -0.0839 0.044 Uiso 1 1 calc R . . H23B H 0.2153 0.5532 0.0375 0.044 Uiso 1 1 calc R . . H23C H 0.1267 0.5489 -0.0190 0.044 Uiso 1 1 calc R . . C24 C 0.2396(2) 0.3709(3) 0.0585(3) 0.0361(9) Uani 1 1 d . . . H24A H 0.2572 0.3666 -0.0193 0.054 Uiso 1 1 calc R . . H24B H 0.2289 0.3104 0.0870 0.054 Uiso 1 1 calc R . . H24C H 0.2806 0.3993 0.1103 0.054 Uiso 1 1 calc R . . C25 C 0.07514(18) 0.32967(19) 0.2181(3) 0.0182(6) Uani 1 1 d . . . H25A H 0.0409 0.3396 0.2824 0.022 Uiso 1 1 calc R . . C26 C 0.0203(2) 0.3022(2) 0.1134(3) 0.0286(8) Uani 1 1 d . . . H26A H -0.0053 0.2452 0.1294 0.043 Uiso 1 1 calc R . . H26B H 0.0506 0.2951 0.0462 0.043 Uiso 1 1 calc R . . H26C H -0.0196 0.3489 0.0973 0.043 Uiso 1 1 calc R . . C27 C 0.1306(2) 0.2524(2) 0.2575(4) 0.0283(8) Uani 1 1 d . . . H27A H 0.1001 0.1973 0.2655 0.042 Uiso 1 1 calc R . . H27B H 0.1586 0.2677 0.3320 0.042 Uiso 1 1 calc R . . H27C H 0.1684 0.2429 0.2000 0.042 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 0.01263(11) 0.01148(10) 0.01471(12) -0.00032(10) 0.00041(8) 0.00022(10) P1 0.0177(4) 0.0138(3) 0.0161(4) 0.0008(3) -0.0021(3) -0.0011(3) Cl1 0.0270(4) 0.0290(4) 0.0244(4) -0.0031(3) 0.0039(3) -0.0034(3) O1 0.0285(13) 0.0201(11) 0.0186(12) 0.0007(9) -0.0066(10) -0.0011(10) N1 0.0229(14) 0.0161(13) 0.0279(16) 0.0036(11) 0.0047(12) 0.0048(10) C1 0.0173(15) 0.0167(14) 0.0197(17) -0.0014(12) -0.0030(13) 0.0015(11) P2 0.0136(4) 0.0133(3) 0.0153(4) -0.0015(3) 0.0012(3) 0.0011(3) C2 0.0198(16) 0.0185(15) 0.0192(17) -0.0004(12) -0.0005(13) -0.0006(12) C3 0.0154(15) 0.0174(14) 0.0194(17) -0.0009(12) -0.0025(12) -0.0004(11) C4 0.0139(14) 0.0191(14) 0.0199(17) -0.0052(12) 0.0032(13) -0.0014(11) C5 0.0202(15) 0.0171(14) 0.0151(16) 0.0011(11) 0.0014(13) -0.0025(11) C6 0.0149(15) 0.0126(13) 0.0207(17) -0.0025(11) -0.0020(12) -0.0026(11) C7 0.0181(16) 0.0220(15) 0.0189(17) -0.0031(12) 0.0029(13) 0.0010(12) C8 0.0207(16) 0.0192(15) 0.0166(16) 0.0026(12) 0.0018(13) -0.0008(12) C9 0.0150(15) 0.0293(17) 0.033(2) -0.0156(16) -0.0100(15) 0.0064(14) C10 0.0239(17) 0.0177(15) 0.0207(17) -0.0016(12) 0.0010(14) -0.0009(12) C11 0.0284(18) 0.0249(17) 0.0254(19) -0.0046(14) -0.0001(15) 0.0081(14) C12 0.038(2) 0.0263(17) 0.023(2) -0.0043(14) 0.0003(16) 0.0009(15) C13 0.0234(17) 0.0167(15) 0.0226(18) 0.0039(12) -0.0063(14) -0.0055(12) C14 0.0342(19) 0.0175(15) 0.0250(19) 0.0046(13) -0.0071(15) -0.0032(13) C15 0.0217(17) 0.0277(17) 0.029(2) 0.0057(14) -0.0024(15) -0.0071(13) C16 0.0243(16) 0.0167(15) 0.0215(17) 0.0048(12) -0.0033(13) 0.0017(12) C17 0.038(2) 0.0263(17) 0.033(2) 0.0087(15) -0.0191(16) -0.0029(16) C18 0.0319(19) 0.0217(16) 0.0244(18) 0.0083(13) 0.0004(15) 0.0007(14) C19 0.0174(14) 0.0167(13) 0.0182(15) -0.0003(12) -0.0007(12) 0.0023(12) C20 0.0272(18) 0.0131(14) 0.0265(19) -0.0015(13) -0.0031(14) 0.0018(12) C21 0.0214(15) 0.0235(17) 0.0310(18) 0.0041(13) 0.0068(14) 0.0080(13) C22 0.0232(17) 0.0238(16) 0.0171(17) -0.0028(12) 0.0040(13) 0.0022(13) C23 0.0278(17) 0.0363(18) 0.0243(18) 0.0049(16) 0.0081(14) 0.0031(15) C24 0.036(2) 0.047(2) 0.028(2) 0.0029(17) 0.0149(17) 0.0214(18) C25 0.0178(15) 0.0150(14) 0.0220(18) -0.0012(12) 0.0025(13) -0.0028(11) C26 0.0294(19) 0.0258(17) 0.030(2) -0.0020(14) -0.0041(16) -0.0105(14) C27 0.0234(17) 0.0152(15) 0.046(2) 0.0002(14) 0.0004(16) 0.0003(12) _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 C9 1.829(4) . ? Ru1 C1 2.002(3) . ? Ru1 P2 2.4035(11) . ? Ru1 P1 2.4120(10) . ? Ru1 Cl1 2.4506(10) . ? P1 C13 1.856(3) . ? P1 C10 1.860(3) . ? P1 C16 1.868(3) . ? O1 C9 1.066(4) . ? N1 C6 1.408(4) . ? N1 H1A 0.8800 . ? N1 H1B 0.8800 . ? C1 C2 1.332(4) . ? C1 H1C 0.9500 . ? P2 C25 1.861(3) . ? P2 C22 1.867(3) . ? P2 C19 1.875(3) . ? C2 C3 1.485(4) . ? C2 H2A 0.9500 . ? C3 C8 1.393(4) . ? C3 C4 1.404(4) . ? C4 C5 1.393(4) . ? C4 H4A 0.9500 . ? C5 C6 1.392(4) . ? C5 H5A 0.9500 . ? C6 C7 1.398(4) . ? C7 C8 1.380(4) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C10 C11 1.531(5) . ? C10 C12 1.532(5) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.529(4) . ? C13 C15 1.531(5) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.529(4) . ? C16 C17 1.534(5) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.526(4) . ? C19 C21 1.529(4) . ? C19 H19A 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.531(5) . ? C22 C24 1.534(5) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.527(5) . ? C25 C27 1.534(4) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 C9 Ru1 C1 91.86(14) . . ? C9 Ru1 P2 89.84(11) . . ? C1 Ru1 P2 98.93(9) . . ? C9 Ru1 P1 93.50(11) . . ? C1 Ru1 P1 89.96(9) . . ? P2 Ru1 P1 170.40(3) . . ? C9 Ru1 Cl1 171.14(10) . . ? C1 Ru1 Cl1 96.75(9) . . ? P2 Ru1 Cl1 86.74(3) . . ? P1 Ru1 Cl1 88.65(3) . . ? C13 P1 C10 106.42(15) . . ? C13 P1 C16 101.55(15) . . ? C10 P1 C16 107.79(15) . . ? C13 P1 Ru1 117.77(12) . . ? C10 P1 Ru1 107.46(11) . . ? C16 P1 Ru1 115.17(11) . . ? C6 N1 H1A 120.0 . . ? C6 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C2 C1 Ru1 135.6(2) . . ? C2 C1 H1C 112.2 . . ? Ru1 C1 H1C 112.2 . . ? C25 P2 C22 103.55(15) . . ? C25 P2 C19 103.05(14) . . ? C22 P2 C19 102.61(14) . . ? C25 P2 Ru1 115.76(11) . . ? C22 P2 Ru1 122.44(11) . . ? C19 P2 Ru1 107.10(10) . . ? C1 C2 C3 124.8(3) . . ? C1 C2 H2A 117.6 . . ? C3 C2 H2A 117.6 . . ? C8 C3 C4 116.9(3) . . ? C8 C3 C2 121.0(3) . . ? C4 C3 C2 122.1(3) . . ? C5 C4 C3 121.3(3) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C6 C5 C4 120.7(3) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C5 C6 C7 118.3(3) . . ? C5 C6 N1 120.7(3) . . ? C7 C6 N1 120.9(3) . . ? C8 C7 C6 120.4(3) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C7 C8 C3 122.3(3) . . ? C7 C8 H8A 118.8 . . ? C3 C8 H8A 118.8 . . ? O1 C9 Ru1 176.9(3) . . ? C11 C10 C12 110.1(3) . . ? C11 C10 P1 111.9(2) . . ? C12 C10 P1 116.0(2) . . ? C11 C10 H10A 106.0 . . ? C12 C10 H10A 106.0 . . ? P1 C10 H10A 106.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 111.5(3) . . ? C14 C13 P1 113.5(2) . . ? C15 C13 P1 110.5(2) . . ? C14 C13 H13A 107.0 . . ? C15 C13 H13A 107.0 . . ? P1 C13 H13A 107.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 109.3(3) . . ? C18 C16 P1 112.2(2) . . ? C17 C16 P1 117.1(2) . . ? C18 C16 H16A 105.8 . . ? C17 C16 H16A 105.8 . . ? P1 C16 H16A 105.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 110.2(3) . . ? C20 C19 P2 110.4(2) . . ? C21 C19 P2 113.0(2) . . ? C20 C19 H19A 107.7 . . ? C21 C19 H19A 107.7 . . ? P2 C19 H19A 107.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C24 109.9(3) . . ? C23 C22 P2 115.9(2) . . ? C24 C22 P2 111.3(2) . . ? C23 C22 H22A 106.4 . . ? C24 C22 H22A 106.4 . . ? P2 C22 H22A 106.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 111.1(3) . . ? C26 C25 P2 114.5(2) . . ? C27 C25 P2 112.6(2) . . ? C26 C25 H25A 106.0 . . ? C27 C25 H25A 106.0 . . ? P2 C25 H25A 106.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.84 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.877 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.083 #===END data_obada2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H54 F3 N O2 P2 Ru' _chemical_formula_sum 'C37 H54 F3 N O2 P2 Ru' _chemical_formula_weight 764.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 44.471(9) _cell_length_b 9.0287(18) _cell_length_c 18.372(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.18(3) _cell_angle_gamma 90.00 _cell_volume 7282(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 40820 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 27.23 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.267 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3200 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6703 _exptl_absorpt_correction_T_max 0.8494 _exptl_absorpt_process_details empirical _exptl_special_details ; 'X-SHAPE 2.07 (03-Aug-2005) Stoe & Cie, Darmstadt, Germany' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47906 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.90 _reflns_number_total 7732 _reflns_number_gt 6228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+18.7516P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7732 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.616971(5) 0.28177(2) 0.914088(12) 0.01369(6) Uani 1 1 d . . . P1 P 0.578108(15) 0.22276(8) 0.98880(4) 0.01525(14) Uani 1 1 d . . . O1 O 0.59007(4) 0.1350(2) 0.83155(11) 0.0174(4) Uani 1 1 d . . . N1 N 0.58234(5) 0.3778(3) 0.82800(12) 0.0156(5) Uani 1 1 d . . . C1 C 0.64469(6) 0.1279(3) 0.97039(15) 0.0166(5) Uani 1 1 d . . . H1A H 0.6445 0.0367 0.9446 0.020 Uiso 1 1 calc R . . F1 F 0.76732(5) -0.3021(3) 1.20673(13) 0.0492(6) Uani 1 1 d . . . P2 P 0.656488(16) 0.31790(8) 0.83876(4) 0.01606(15) Uani 1 1 d . . . O2 O 0.64426(5) 0.5142(2) 1.01906(12) 0.0254(5) Uani 1 1 d . . . F2 F 0.76562(5) -0.3727(3) 1.09527(13) 0.0509(6) Uani 1 1 d . . . C2 C 0.66328(6) 0.1250(3) 1.03602(16) 0.0193(6) Uani 1 1 d . . . H2A H 0.6632 0.2100 1.0664 0.023 Uiso 1 1 calc R . . F3 F 0.73473(5) -0.4642(2) 1.16081(14) 0.0432(5) Uani 1 1 d . . . C3 C 0.68368(6) 0.0032(3) 1.06511(16) 0.0194(6) Uani 1 1 d . . . C4 C 0.70616(7) 0.0280(3) 1.12656(16) 0.0221(6) Uani 1 1 d . . . H4A H 0.7072 0.1219 1.1502 0.027 Uiso 1 1 calc R . . C5 C 0.72689(7) -0.0812(4) 1.15375(17) 0.0249(6) Uani 1 1 d . . . H5A H 0.7420 -0.0617 1.1954 0.030 Uiso 1 1 calc R . . C6 C 0.72557(6) -0.2187(4) 1.12002(17) 0.0237(6) Uani 1 1 d . . . C7 C 0.70286(8) -0.2476(3) 1.06020(19) 0.0313(8) Uani 1 1 d . . . H7A H 0.7016 -0.3424 1.0375 0.038 Uiso 1 1 calc R . . C8 C 0.68219(7) -0.1382(4) 1.03383(18) 0.0309(7) Uani 1 1 d . . . H8A H 0.6666 -0.1597 0.9935 0.037 Uiso 1 1 calc R . . C9 C 0.74807(7) -0.3369(4) 1.14545(18) 0.0291(7) Uani 1 1 d . . . C10 C 0.63359(6) 0.4226(3) 0.97722(15) 0.0184(6) Uani 1 1 d . . . C11 C 0.57395(6) 0.2442(3) 0.80021(15) 0.0167(6) Uani 1 1 d . . . C12 C 0.54866(6) 0.2267(3) 0.74159(15) 0.0186(5) Uani 1 1 d . . . H12A H 0.5425 0.1309 0.7236 0.022 Uiso 1 1 calc R . . C13 C 0.53374(6) 0.3489(3) 0.71233(15) 0.0196(6) Uani 1 1 d . . . H13A H 0.5169 0.3387 0.6738 0.024 Uiso 1 1 calc R . . C14 C 0.54307(6) 0.4930(3) 0.73881(15) 0.0179(6) Uani 1 1 d . . . C15 C 0.52885(7) 0.6242(3) 0.70886(16) 0.0224(6) Uani 1 1 d . . . H15A H 0.5122 0.6181 0.6696 0.027 Uiso 1 1 calc R . . C16 C 0.53878(7) 0.7602(3) 0.73564(17) 0.0227(6) Uani 1 1 d . . . H16A H 0.5292 0.8478 0.7148 0.027 Uiso 1 1 calc R . . C17 C 0.56343(7) 0.7698(3) 0.79454(17) 0.0240(6) Uani 1 1 d . . . H17A H 0.5705 0.8642 0.8125 0.029 Uiso 1 1 calc R . . C18 C 0.57724(7) 0.6441(3) 0.82618(16) 0.0198(6) Uani 1 1 d . . . H18A H 0.5932 0.6520 0.8669 0.024 Uiso 1 1 calc R . . C19 C 0.56767(6) 0.5031(3) 0.79816(15) 0.0164(5) Uani 1 1 d . . . C20 C 0.57605(7) 0.3466(3) 1.06819(15) 0.0204(6) Uani 1 1 d . . . H20A H 0.5577 0.3162 1.0895 0.024 Uiso 1 1 calc R . . C21 C 0.57103(7) 0.5091(3) 1.04329(18) 0.0251(7) Uani 1 1 d . . . H21A H 0.5699 0.5717 1.0863 0.038 Uiso 1 1 calc R . . H21B H 0.5520 0.5171 1.0084 0.038 Uiso 1 1 calc R . . H21C H 0.5881 0.5417 1.0193 0.038 Uiso 1 1 calc R . . C22 C 0.60341(7) 0.3336(4) 1.13024(16) 0.0258(6) Uani 1 1 d . . . H22A H 0.6007 0.4015 1.1703 0.039 Uiso 1 1 calc R . . H22B H 0.6221 0.3594 1.1111 0.039 Uiso 1 1 calc R . . H22C H 0.6049 0.2318 1.1489 0.039 Uiso 1 1 calc R . . C23 C 0.53737(6) 0.2286(3) 0.94008(15) 0.0181(5) Uani 1 1 d . . . H23A H 0.5366 0.3082 0.9020 0.022 Uiso 1 1 calc R . . C24 C 0.51294(6) 0.2690(4) 0.98767(16) 0.0228(6) Uani 1 1 d . . . H24A H 0.4928 0.2693 0.9568 0.034 Uiso 1 1 calc R . . H24B H 0.5173 0.3675 1.0092 0.034 Uiso 1 1 calc R . . H24C H 0.5132 0.1958 1.0272 0.034 Uiso 1 1 calc R . . C25 C 0.52758(7) 0.0848(3) 0.89781(16) 0.0217(6) Uani 1 1 d . . . H25A H 0.5064 0.0939 0.8735 0.033 Uiso 1 1 calc R . . H25B H 0.5294 0.0014 0.9324 0.033 Uiso 1 1 calc R . . H25C H 0.5407 0.0676 0.8606 0.033 Uiso 1 1 calc R . . C26 C 0.58443(7) 0.0376(3) 1.03377(15) 0.0190(6) Uani 1 1 d . . . H26A H 0.6048 0.0452 1.0658 0.023 Uiso 1 1 calc R . . C27 C 0.58766(7) -0.0906(3) 0.98069(16) 0.0217(6) Uani 1 1 d . . . H27A H 0.5909 -0.1834 1.0085 0.033 Uiso 1 1 calc R . . H27B H 0.6051 -0.0721 0.9554 0.033 Uiso 1 1 calc R . . H27C H 0.5691 -0.0983 0.9442 0.033 Uiso 1 1 calc R . . C28 C 0.56235(7) -0.0039(3) 1.08628(17) 0.0240(6) Uani 1 1 d . . . H28A H 0.5675 -0.1024 1.1070 0.036 Uiso 1 1 calc R . . H28B H 0.5415 -0.0047 1.0592 0.036 Uiso 1 1 calc R . . H28C H 0.5639 0.0689 1.1263 0.036 Uiso 1 1 calc R . . C29 C 0.69566(6) 0.2749(4) 0.88751(17) 0.0234(6) Uani 1 1 d . . . H29A H 0.6936 0.1784 0.9129 0.028 Uiso 1 1 calc R . . C30 C 0.70739(7) 0.3835(4) 0.94949(19) 0.0315(7) Uani 1 1 d . . . H30A H 0.7279 0.3542 0.9726 0.047 Uiso 1 1 calc R . . H30B H 0.6938 0.3822 0.9864 0.047 Uiso 1 1 calc R . . H30C H 0.7080 0.4835 0.9291 0.047 Uiso 1 1 calc R . . C31 C 0.72019(7) 0.2479(4) 0.83971(19) 0.0283(7) Uani 1 1 d . . . H31A H 0.7396 0.2258 0.8713 0.043 Uiso 1 1 calc R . . H31B H 0.7225 0.3365 0.8103 0.043 Uiso 1 1 calc R . . H31C H 0.7143 0.1639 0.8067 0.043 Uiso 1 1 calc R . . C32 C 0.65551(7) 0.5056(3) 0.79668(17) 0.0205(6) Uani 1 1 d . . . H32A H 0.6343 0.5169 0.7694 0.025 Uiso 1 1 calc R . . C33 C 0.67633(7) 0.5311(4) 0.73840(18) 0.0277(7) Uani 1 1 d . . . H33A H 0.6739 0.6330 0.7201 0.042 Uiso 1 1 calc R . . H33B H 0.6708 0.4619 0.6974 0.042 Uiso 1 1 calc R . . H33C H 0.6976 0.5146 0.7607 0.042 Uiso 1 1 calc R . . C34 C 0.65969(8) 0.6343(3) 0.85189(19) 0.0292(7) Uani 1 1 d . . . H34A H 0.6588 0.7284 0.8251 0.044 Uiso 1 1 calc R . . H34B H 0.6795 0.6252 0.8837 0.044 Uiso 1 1 calc R . . H34C H 0.6434 0.6314 0.8822 0.044 Uiso 1 1 calc R . . C35 C 0.65450(7) 0.1933(3) 0.75653(16) 0.0223(6) Uani 1 1 d . . . H35A H 0.6737 0.2099 0.7357 0.027 Uiso 1 1 calc R . . C36 C 0.65450(7) 0.0314(3) 0.77868(18) 0.0271(7) Uani 1 1 d . . . H36A H 0.6535 -0.0309 0.7347 0.041 Uiso 1 1 calc R . . H36B H 0.6368 0.0114 0.8028 0.041 Uiso 1 1 calc R . . H36C H 0.6732 0.0091 0.8129 0.041 Uiso 1 1 calc R . . C37 C 0.62802(7) 0.2268(4) 0.69408(16) 0.0270(7) Uani 1 1 d . . . H37A H 0.6286 0.1572 0.6534 0.041 Uiso 1 1 calc R . . H37B H 0.6300 0.3283 0.6765 0.041 Uiso 1 1 calc R . . H37C H 0.6086 0.2163 0.7126 0.041 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 0.01479(10) 0.01188(10) 0.01400(10) 0.00037(9) 0.00108(7) -0.00024(9) P1 0.0173(3) 0.0145(3) 0.0137(3) 0.0004(3) 0.0017(2) -0.0006(3) O1 0.0204(10) 0.0114(10) 0.0203(10) 0.0012(8) 0.0033(8) 0.0001(7) N1 0.0168(11) 0.0148(12) 0.0153(11) 0.0010(9) 0.0031(9) 0.0009(9) C1 0.0170(13) 0.0157(14) 0.0174(13) 0.0014(11) 0.0037(10) 0.0006(10) F1 0.0424(12) 0.0445(14) 0.0524(14) 0.0055(11) -0.0181(10) 0.0144(10) P2 0.0159(3) 0.0139(3) 0.0183(3) 0.0011(3) 0.0027(3) 0.0000(3) O2 0.0277(11) 0.0228(11) 0.0258(11) -0.0073(9) 0.0046(9) -0.0072(9) F2 0.0439(13) 0.0647(16) 0.0496(13) 0.0213(12) 0.0238(10) 0.0300(11) C2 0.0202(14) 0.0170(14) 0.0206(14) -0.0007(11) 0.0025(11) 0.0000(11) F3 0.0317(11) 0.0268(11) 0.0712(16) 0.0208(10) 0.0089(10) 0.0074(8) C3 0.0182(14) 0.0201(15) 0.0194(14) 0.0027(11) 0.0011(11) -0.0001(11) C4 0.0233(15) 0.0208(15) 0.0213(15) -0.0015(12) 0.0009(12) -0.0001(12) C5 0.0202(14) 0.0293(17) 0.0233(15) 0.0035(13) -0.0023(12) -0.0006(12) C6 0.0190(14) 0.0251(15) 0.0266(15) 0.0078(13) 0.0028(11) 0.0012(13) C7 0.0343(18) 0.0199(17) 0.0359(18) -0.0030(13) -0.0054(14) 0.0043(13) C8 0.0303(17) 0.0260(17) 0.0311(17) -0.0004(14) -0.0117(14) 0.0022(13) C9 0.0221(15) 0.0315(17) 0.0336(18) 0.0092(14) 0.0040(13) 0.0029(13) C10 0.0176(13) 0.0193(15) 0.0182(14) 0.0018(11) 0.0033(11) 0.0006(11) C11 0.0187(13) 0.0177(15) 0.0149(13) 0.0010(10) 0.0063(10) 0.0000(10) C12 0.0214(13) 0.0185(13) 0.0162(13) -0.0027(11) 0.0040(10) -0.0025(11) C13 0.0182(13) 0.0260(15) 0.0139(13) -0.0001(11) 0.0007(10) -0.0020(11) C14 0.0193(14) 0.0189(14) 0.0161(13) 0.0020(11) 0.0050(11) 0.0009(11) C15 0.0208(14) 0.0257(16) 0.0207(14) 0.0056(12) 0.0040(11) 0.0033(12) C16 0.0254(14) 0.0186(15) 0.0256(15) 0.0072(11) 0.0083(12) 0.0065(11) C17 0.0295(16) 0.0173(14) 0.0268(15) -0.0011(12) 0.0098(12) 0.0012(12) C18 0.0241(15) 0.0155(14) 0.0200(14) -0.0008(11) 0.0036(11) 0.0010(11) C19 0.0171(13) 0.0174(14) 0.0162(13) 0.0020(11) 0.0070(11) 0.0007(10) C20 0.0247(15) 0.0202(15) 0.0170(14) -0.0026(11) 0.0057(11) -0.0030(12) C21 0.0274(16) 0.0209(15) 0.0280(16) -0.0058(13) 0.0072(13) -0.0006(12) C22 0.0306(16) 0.0285(16) 0.0180(14) -0.0058(12) 0.0031(12) -0.0045(13) C23 0.0182(13) 0.0181(13) 0.0177(13) 0.0030(11) 0.0019(10) -0.0009(11) C24 0.0193(14) 0.0256(15) 0.0239(14) 0.0018(12) 0.0049(11) 0.0014(12) C25 0.0208(14) 0.0214(15) 0.0216(14) 0.0018(12) -0.0004(11) -0.0040(11) C26 0.0214(14) 0.0198(14) 0.0157(13) 0.0028(11) 0.0023(11) -0.0008(11) C27 0.0267(15) 0.0152(14) 0.0231(15) 0.0032(11) 0.0038(12) 0.0000(11) C28 0.0295(16) 0.0227(15) 0.0207(15) 0.0053(12) 0.0070(12) 0.0000(12) C29 0.0182(13) 0.0239(15) 0.0276(15) 0.0014(13) 0.0022(11) 0.0031(12) C30 0.0208(15) 0.0376(19) 0.0339(18) -0.0067(15) -0.0024(13) -0.0001(13) C31 0.0203(15) 0.0292(18) 0.0358(18) 0.0032(13) 0.0054(13) 0.0048(12) C32 0.0196(14) 0.0188(14) 0.0235(15) 0.0041(12) 0.0041(12) -0.0003(11) C33 0.0282(16) 0.0250(16) 0.0314(17) 0.0076(13) 0.0095(13) -0.0006(13) C34 0.0375(18) 0.0152(15) 0.0359(18) 0.0018(13) 0.0089(14) -0.0017(13) C35 0.0204(14) 0.0228(16) 0.0250(15) -0.0035(12) 0.0076(12) 0.0019(11) C36 0.0313(17) 0.0202(16) 0.0313(17) -0.0064(13) 0.0092(14) -0.0025(13) C37 0.0267(15) 0.0341(17) 0.0204(14) -0.0060(13) 0.0042(12) -0.0026(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C10 1.799(3) . ? Ru1 C1 2.028(3) . ? Ru1 N1 2.202(2) . ? Ru1 O1 2.216(2) . ? Ru1 P2 2.4263(10) . ? Ru1 P1 2.4315(9) . ? P1 C20 1.852(3) . ? P1 C26 1.866(3) . ? P1 C23 1.889(3) . ? O1 C11 1.299(3) . ? N1 C11 1.339(4) . ? N1 C19 1.375(4) . ? C1 C2 1.349(4) . ? C1 H1A 0.9500 . ? F1 C9 1.338(4) . ? P2 C32 1.860(3) . ? P2 C29 1.868(3) . ? P2 C35 1.875(3) . ? O2 C10 1.176(4) . ? F2 C9 1.339(4) . ? C2 C3 1.471(4) . ? C2 H2A 0.9500 . ? F3 C9 1.343(4) . ? C3 C8 1.398(4) . ? C3 C4 1.401(4) . ? C4 C5 1.387(4) . ? C4 H4A 0.9500 . ? C5 C6 1.385(5) . ? C5 H5A 0.9500 . ? C6 C7 1.393(4) . ? C6 C9 1.486(4) . ? C7 C8 1.383(4) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C11 C12 1.437(4) . ? C12 C13 1.354(4) . ? C12 H12A 0.9500 . ? C13 C14 1.427(4) . ? C13 H13A 0.9500 . ? C14 C15 1.413(4) . ? C14 C19 1.419(4) . ? C15 C16 1.370(4) . ? C15 H15A 0.9500 . ? C16 C17 1.415(4) . ? C16 H16A 0.9500 . ? C17 C18 1.374(4) . ? C17 H17A 0.9500 . ? C18 C19 1.413(4) . ? C18 H18A 0.9500 . ? C20 C22 1.533(4) . ? C20 C21 1.542(4) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C25 1.539(4) . ? C23 C24 1.543(4) . ? C23 H23A 1.0000 . ? 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 C28 1.529(4) . ? C26 C27 1.535(4) . ? C26 H26A 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.525(4) . ? C29 C30 1.529(4) . ? C29 H29A 1.0000 . ? 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 C34 1.534(4) . ? C32 C33 1.541(4) . ? C32 H32A 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.517(4) . ? C35 C37 1.537(4) . ? C35 H35A 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 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 C10 Ru1 C1 90.09(12) . . ? C10 Ru1 N1 110.68(11) . . ? C1 Ru1 N1 159.19(10) . . ? C10 Ru1 O1 170.34(10) . . ? C1 Ru1 O1 99.04(10) . . ? N1 Ru1 O1 60.30(8) . . ? C10 Ru1 P2 90.70(9) . . ? C1 Ru1 P2 86.93(8) . . ? N1 Ru1 P2 91.40(6) . . ? O1 Ru1 P2 92.93(5) . . ? C10 Ru1 P1 92.69(9) . . ? C1 Ru1 P1 89.48(8) . . ? N1 Ru1 P1 90.76(6) . . ? O1 Ru1 P1 84.29(5) . . ? P2 Ru1 P1 175.07(3) . . ? C20 P1 C26 102.43(13) . . ? C20 P1 C23 101.08(13) . . ? C26 P1 C23 107.47(13) . . ? C20 P1 Ru1 116.19(10) . . ? C26 P1 Ru1 112.07(9) . . ? C23 P1 Ru1 116.15(9) . . ? C11 O1 Ru1 92.77(16) . . ? C11 N1 C19 120.2(2) . . ? C11 N1 Ru1 92.27(16) . . ? C19 N1 Ru1 147.48(19) . . ? C2 C1 Ru1 134.8(2) . . ? C2 C1 H1A 112.6 . . ? Ru1 C1 H1A 112.6 . . ? C32 P2 C29 110.29(14) . . ? C32 P2 C35 102.53(14) . . ? C29 P2 C35 100.50(14) . . ? C32 P2 Ru1 112.86(10) . . ? C29 P2 Ru1 113.80(10) . . ? C35 P2 Ru1 115.70(10) . . ? C1 C2 C3 126.4(3) . . ? C1 C2 H2A 116.8 . . ? C3 C2 H2A 116.8 . . ? C8 C3 C4 117.3(3) . . ? C8 C3 C2 123.2(3) . . ? C4 C3 C2 119.5(3) . . ? C5 C4 C3 121.6(3) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C6 C5 C4 119.9(3) . . ? C6 C5 H5A 120.1 . . ? C4 C5 H5A 120.1 . . ? C5 C6 C7 119.6(3) . . ? C5 C6 C9 121.7(3) . . ? C7 C6 C9 118.7(3) . . ? C8 C7 C6 120.0(3) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C3 121.5(3) . . ? C7 C8 H8A 119.2 . . ? C3 C8 H8A 119.2 . . ? F1 C9 F2 105.7(3) . . ? F1 C9 F3 105.6(3) . . ? F2 C9 F3 105.3(3) . . ? F1 C9 C6 113.8(3) . . ? F2 C9 C6 113.2(3) . . ? F3 C9 C6 112.5(3) . . ? O2 C10 Ru1 179.2(3) . . ? O1 C11 N1 114.5(2) . . ? O1 C11 C12 124.0(3) . . ? N1 C11 C12 121.5(3) . . ? C13 C12 C11 118.9(3) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? C12 C13 C14 120.7(3) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C15 C14 C19 119.2(3) . . ? C15 C14 C13 123.0(3) . . ? C19 C14 C13 117.8(3) . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 119.7(3) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 C16 120.8(3) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C17 C18 C19 120.1(3) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? N1 C19 C18 120.0(3) . . ? N1 C19 C14 120.8(3) . . ? C18 C19 C14 119.2(3) . . ? C22 C20 C21 110.7(2) . . ? C22 C20 P1 114.0(2) . . ? C21 C20 P1 111.3(2) . . ? C22 C20 H20A 106.8 . . ? C21 C20 H20A 106.8 . . ? P1 C20 H20A 106.8 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C23 C24 108.5(2) . . ? C25 C23 P1 112.84(19) . . ? C24 C23 P1 116.53(19) . . ? C25 C23 H23A 106.1 . . ? C24 C23 H23A 106.1 . . ? P1 C23 H23A 106.1 . . ? 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 . . ? C28 C26 C27 110.5(2) . . ? C28 C26 P1 115.6(2) . . ? C27 C26 P1 114.65(19) . . ? C28 C26 H26A 104.9 . . ? C27 C26 H26A 104.9 . . ? P1 C26 H26A 104.9 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C30 109.9(3) . . ? C31 C29 P2 117.1(2) . . ? C30 C29 P2 113.9(2) . . ? C31 C29 H29A 104.9 . . ? C30 C29 H29A 104.9 . . ? P2 C29 H29A 104.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C33 108.9(2) . . ? C34 C32 P2 115.0(2) . . ? C33 C32 P2 116.6(2) . . ? C34 C32 H32A 105.0 . . ? C33 C32 H32A 105.0 . . ? P2 C32 H32A 105.0 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C37 110.9(3) . . ? C36 C35 P2 111.4(2) . . ? C37 C35 P2 114.5(2) . . ? C36 C35 H35A 106.5 . . ? C37 C35 H35A 106.5 . . ? P2 C35 H35A 106.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.90 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.695 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.077 #===END data_obada3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H61 N O4 P2 Ru' _chemical_formula_weight 782.91 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 10.538(2) _cell_length_b 14.021(3) _cell_length_c 15.444(3) _cell_angle_alpha 63.61(3) _cell_angle_beta 81.98(3) _cell_angle_gamma 75.88(3) _cell_volume 1981.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18968 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 27.22 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 0.516 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6620 _exptl_absorpt_correction_T_max 0.9135 _exptl_absorpt_process_details empirical _exptl_special_details ; 'X-SHAPE 2.07 (03-Aug-2005) Stoe & Cie, Darmstadt, Germany' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26621 _diffrn_reflns_av_R_equivalents 0.1687 _diffrn_reflns_av_sigmaI/netI 0.1662 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.93 _reflns_number_total 8396 _reflns_number_gt 5265 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0069P)^2^+27.5418P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8396 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1734 _refine_ls_R_factor_gt 0.1129 _refine_ls_wR_factor_ref 0.2322 _refine_ls_wR_factor_gt 0.2106 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.82763(9) 0.69300(7) 0.72022(7) 0.0170(2) Uani 1 1 d . . . O1 O 0.7686(7) 0.7953(6) 0.5698(5) 0.0267(16) Uani 1 1 d . . . N1 N 0.7231(8) 0.6315(6) 0.6456(6) 0.0213(17) Uani 1 1 d . . . C1 C 0.9183(10) 0.7968(8) 0.7345(8) 0.025(2) Uani 1 1 d . . . H1A H 0.9198 0.8616 0.6769 0.030 Uiso 1 1 calc R . . P1 P 1.0334(3) 0.6150(2) 0.6658(2) 0.0295(7) Uani 1 1 d . . . P2 P 0.6240(3) 0.7757(3) 0.7775(2) 0.0334(7) Uani 1 1 d . . . C2 C 0.9770(10) 0.7937(8) 0.8080(8) 0.025(2) Uani 1 1 d . . . H2A H 0.9788 0.7303 0.8673 0.030 Uiso 1 1 calc R . . O2 O 0.8778(8) 0.5252(6) 0.9215(6) 0.0362(18) Uani 1 1 d . . . C3 C 1.0389(9) 0.8787(8) 0.8061(8) 0.024(2) Uani 1 1 d . . . O3 O 1.2217(9) 1.1177(7) 0.7982(6) 0.043(2) Uani 1 1 d . . . O4 O 0.5264(7) 0.6657(5) 0.4162(5) 0.0263(16) Uani 1 1 d . . . C4 C 1.0615(10) 0.8836(8) 0.8908(8) 0.026(2) Uani 1 1 d . . . H4A H 1.0364 0.8300 0.9508 0.032 Uiso 1 1 calc R . . C5 C 1.1182(11) 0.9620(8) 0.8924(7) 0.027(2) Uani 1 1 d . . . H5A H 1.1282 0.9644 0.9516 0.032 Uiso 1 1 calc R . . C6 C 1.1604(11) 1.0378(9) 0.8039(8) 0.029(2) Uani 1 1 d . . . C7 C 1.1412(12) 1.0363(9) 0.7193(9) 0.037(3) Uani 1 1 d . . . H7A H 1.1691 1.0892 0.6600 0.044 Uiso 1 1 calc R . . C8 C 1.0818(11) 0.9595(8) 0.7179(8) 0.028(2) Uani 1 1 d . . . H8A H 1.0693 0.9603 0.6578 0.034 Uiso 1 1 calc R . . C9 C 1.2430(14) 1.1217(11) 0.8866(10) 0.049(3) Uani 1 1 d . . . H9A H 1.2862 1.1821 0.8714 0.073 Uiso 1 1 calc R . . H9B H 1.2986 1.0532 0.9281 0.073 Uiso 1 1 calc R . . H9C H 1.1587 1.1327 0.9204 0.073 Uiso 1 1 calc R . . C10 C 0.8581(10) 0.5921(9) 0.8435(9) 0.031(2) Uani 1 1 d . . . C11 C 0.7132(10) 0.7252(8) 0.5652(8) 0.024(2) Uani 1 1 d . . . C12 C 0.6484(9) 0.7424(8) 0.4840(7) 0.024(2) Uani 1 1 d . . . H12A H 0.6411 0.8095 0.4277 0.029 Uiso 1 1 calc R . . C13 C 0.5960(9) 0.6592(8) 0.4885(7) 0.023(2) Uani 1 1 d . . . C14 C 0.6106(10) 0.5579(8) 0.5713(7) 0.024(2) Uani 1 1 d . . . H14A H 0.5789 0.4987 0.5741 0.029 Uiso 1 1 calc R . . C15 C 0.6732(10) 0.5501(8) 0.6471(7) 0.025(2) Uani 1 1 d . . . H15A H 0.6822 0.4837 0.7041 0.030 Uiso 1 1 calc R . . C16 C 0.5068(12) 0.7682(9) 0.3315(8) 0.036(3) Uani 1 1 d . . . H16A H 0.5921 0.7822 0.2980 0.043 Uiso 1 1 calc R . . H16B H 0.4664 0.8279 0.3507 0.043 Uiso 1 1 calc R . . C17 C 0.4197(10) 0.7646(8) 0.2654(8) 0.027(2) Uani 1 1 d . . . C18 C 0.4628(12) 0.7047(9) 0.2116(8) 0.035(3) Uani 1 1 d . . . H18A H 0.5484 0.6605 0.2212 0.042 Uiso 1 1 calc R . . C19 C 0.3882(12) 0.7065(10) 0.1462(8) 0.037(3) Uani 1 1 d . . . H19A H 0.4221 0.6654 0.1100 0.045 Uiso 1 1 calc R . . C20 C 0.2620(12) 0.7686(10) 0.1322(9) 0.042(3) Uani 1 1 d . . . H20A H 0.2065 0.7662 0.0901 0.050 Uiso 1 1 calc R . . C21 C 0.2186(10) 0.8329(9) 0.1795(9) 0.033(3) Uani 1 1 d . . . H21A H 0.1366 0.8824 0.1648 0.040 Uiso 1 1 calc R . . C22 C 0.2955(11) 0.8258(9) 0.2500(9) 0.037(3) Uani 1 1 d . . . H22A H 0.2604 0.8646 0.2880 0.045 Uiso 1 1 calc R . . C23 C 1.1779(12) 0.6040(10) 0.7289(9) 0.040(3) Uani 1 1 d . . . H23A H 1.1606 0.6727 0.7375 0.048 Uiso 1 1 calc R . . C24 C 1.1911(12) 0.5111(10) 0.8332(9) 0.039(3) Uani 1 1 d . . . H24A H 1.2688 0.5103 0.8619 0.059 Uiso 1 1 calc R . . H24B H 1.1997 0.4411 0.8308 0.059 Uiso 1 1 calc R . . H24C H 1.1130 0.5232 0.8726 0.059 Uiso 1 1 calc R . . C25 C 1.3126(11) 0.6004(10) 0.6742(9) 0.041(3) Uani 1 1 d . . . H25A H 1.3803 0.5947 0.7147 0.062 Uiso 1 1 calc R . . H25B H 1.3095 0.6671 0.6139 0.062 Uiso 1 1 calc R . . H25C H 1.3333 0.5372 0.6591 0.062 Uiso 1 1 calc R . . C26 C 1.0331(11) 0.4792(9) 0.6724(9) 0.034(3) Uani 1 1 d . . . H26A H 0.9710 0.4934 0.6226 0.040 Uiso 1 1 calc R . . C27 C 0.9776(12) 0.4029(9) 0.7688(8) 0.036(3) Uani 1 1 d . . . H27A H 0.9799 0.3333 0.7674 0.054 Uiso 1 1 calc R . . H27B H 0.8869 0.4361 0.7790 0.054 Uiso 1 1 calc R . . H27C H 1.0304 0.3906 0.8217 0.054 Uiso 1 1 calc R . . C28 C 1.1644(12) 0.4224(11) 0.6442(12) 0.053(4) Uani 1 1 d . . . H28A H 1.1562 0.3519 0.6493 0.080 Uiso 1 1 calc R . . H28B H 1.2314 0.4110 0.6878 0.080 Uiso 1 1 calc R . . H28C H 1.1896 0.4678 0.5775 0.080 Uiso 1 1 calc R . . C29 C 1.0836(12) 0.6918(9) 0.5374(8) 0.036(3) Uani 1 1 d . . . H29A H 1.1778 0.6587 0.5311 0.043 Uiso 1 1 calc R . . C30 C 1.0804(13) 0.8116(9) 0.5152(8) 0.040(3) Uani 1 1 d . . . H30A H 1.1079 0.8505 0.4475 0.060 Uiso 1 1 calc R . . H30B H 1.1401 0.8134 0.5575 0.060 Uiso 1 1 calc R . . H30C H 0.9913 0.8466 0.5266 0.060 Uiso 1 1 calc R . . C31 C 1.0159(13) 0.6825(11) 0.4645(9) 0.045(3) Uani 1 1 d . . . H31A H 1.0499 0.7250 0.3996 0.068 Uiso 1 1 calc R . . H31B H 0.9217 0.7103 0.4694 0.068 Uiso 1 1 calc R . . H31C H 1.0314 0.6060 0.4762 0.068 Uiso 1 1 calc R . . C32 C 0.6422(13) 0.8235(11) 0.8678(9) 0.045(3) Uani 1 1 d . . . H32A H 0.7200 0.8583 0.8420 0.054 Uiso 1 1 calc R . . C33 C 0.6881(14) 0.7295(12) 0.9665(9) 0.053(4) Uani 1 1 d . . . H33A H 0.6968 0.7598 1.0111 0.080 Uiso 1 1 calc R . . H33B H 0.7729 0.6866 0.9572 0.080 Uiso 1 1 calc R . . H33C H 0.6236 0.6828 0.9934 0.080 Uiso 1 1 calc R . . C34 C 0.5411(15) 0.9101(12) 0.8841(9) 0.055(4) Uani 1 1 d . . . H34A H 0.5696 0.9242 0.9343 0.082 Uiso 1 1 calc R . . H34B H 0.4578 0.8858 0.9049 0.082 Uiso 1 1 calc R . . H34C H 0.5297 0.9769 0.8238 0.082 Uiso 1 1 calc R . . C35 C 0.5030(11) 0.6912(10) 0.8170(11) 0.045(3) Uani 1 1 d . . . H35A H 0.4726 0.6967 0.7561 0.055 Uiso 1 1 calc R . . C36 C 0.5556(11) 0.5706(10) 0.8756(8) 0.039(3) Uani 1 1 d . . . H36A H 0.4841 0.5312 0.8930 0.058 Uiso 1 1 calc R . . H36B H 0.5937 0.5595 0.9346 0.058 Uiso 1 1 calc R . . H36C H 0.6231 0.5432 0.8370 0.058 Uiso 1 1 calc R . . C37 C 0.3758(12) 0.7262(13) 0.8699(13) 0.064(5) Uani 1 1 d . . . H37A H 0.3180 0.6749 0.8863 0.097 Uiso 1 1 calc R . . H37B H 0.3307 0.7994 0.8274 0.097 Uiso 1 1 calc R . . H37C H 0.3987 0.7263 0.9292 0.097 Uiso 1 1 calc R . . C38 C 0.5332(13) 0.9077(12) 0.6841(11) 0.056(4) Uani 1 1 d . . . H38A H 0.4717 0.9434 0.7216 0.068 Uiso 1 1 calc R . . C39 C 0.6314(15) 0.9842(10) 0.6291(10) 0.053(4) Uani 1 1 d . . . H39A H 0.5851 1.0530 0.5806 0.079 Uiso 1 1 calc R . . H39B H 0.7008 0.9491 0.5971 0.079 Uiso 1 1 calc R . . H39C H 0.6702 0.9985 0.6752 0.079 Uiso 1 1 calc R . . C40 C 0.4478(17) 0.8972(16) 0.6183(13) 0.085(6) Uani 1 1 d . . . H40A H 0.4054 0.9698 0.5727 0.128 Uiso 1 1 calc R . . H40B H 0.3807 0.8566 0.6574 0.128 Uiso 1 1 calc R . . H40C H 0.5023 0.8584 0.5824 0.128 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 0.0188(4) 0.0146(4) 0.0189(4) -0.0080(3) -0.0046(3) -0.0018(3) O1 0.027(4) 0.027(4) 0.031(4) -0.014(3) -0.013(3) -0.003(3) N1 0.024(4) 0.021(4) 0.023(4) -0.012(4) 0.003(3) -0.007(4) C1 0.024(5) 0.020(5) 0.027(5) -0.007(4) 0.000(4) -0.004(4) P1 0.0287(16) 0.0253(15) 0.0344(17) -0.0130(13) -0.0016(13) -0.0048(13) P2 0.0317(17) 0.0368(17) 0.0380(18) -0.0245(15) -0.0098(14) 0.0035(14) C2 0.032(6) 0.018(5) 0.030(6) -0.013(4) 0.001(5) -0.010(4) O2 0.034(4) 0.033(4) 0.036(5) -0.013(4) -0.006(4) 0.001(4) C3 0.018(5) 0.020(5) 0.033(6) -0.012(4) -0.007(4) 0.001(4) O3 0.050(5) 0.038(5) 0.051(5) -0.022(4) -0.006(4) -0.019(4) O4 0.030(4) 0.021(4) 0.026(4) -0.006(3) -0.004(3) -0.009(3) C4 0.030(6) 0.020(5) 0.030(6) -0.009(4) -0.010(5) -0.005(4) C5 0.039(6) 0.026(5) 0.020(5) -0.012(4) -0.006(5) -0.010(5) C6 0.025(6) 0.024(5) 0.042(7) -0.019(5) -0.004(5) -0.004(5) C7 0.043(7) 0.029(6) 0.039(7) -0.010(5) 0.000(5) -0.018(5) C8 0.037(6) 0.022(5) 0.030(6) -0.012(4) -0.008(5) -0.007(5) C9 0.058(9) 0.047(8) 0.062(9) -0.034(7) 0.013(7) -0.035(7) C10 0.015(5) 0.030(6) 0.046(7) -0.015(5) -0.012(5) 0.001(4) C11 0.020(5) 0.019(5) 0.033(6) -0.014(4) -0.005(4) 0.004(4) C12 0.019(5) 0.026(5) 0.026(5) -0.009(4) -0.002(4) -0.003(4) C13 0.014(5) 0.031(6) 0.025(5) -0.016(4) 0.003(4) -0.003(4) C14 0.026(5) 0.024(5) 0.020(5) -0.006(4) -0.003(4) -0.005(4) C15 0.027(6) 0.020(5) 0.025(5) -0.008(4) 0.002(4) -0.008(4) C16 0.040(7) 0.030(6) 0.037(6) -0.013(5) -0.017(5) -0.002(5) C17 0.021(5) 0.023(5) 0.031(6) -0.007(4) -0.011(4) 0.001(4) C18 0.044(7) 0.028(6) 0.036(6) -0.017(5) -0.012(5) -0.003(5) C19 0.042(7) 0.048(7) 0.029(6) -0.018(5) -0.002(5) -0.017(6) C20 0.046(7) 0.044(7) 0.038(7) -0.007(6) -0.017(6) -0.023(6) C21 0.019(5) 0.040(6) 0.048(7) -0.022(6) -0.008(5) -0.008(5) C22 0.026(6) 0.038(7) 0.053(8) -0.026(6) -0.001(5) -0.003(5) C23 0.038(7) 0.042(7) 0.040(7) -0.017(6) -0.007(6) -0.007(6) C24 0.031(6) 0.041(7) 0.040(7) -0.014(6) -0.005(5) 0.000(6) C25 0.032(6) 0.041(7) 0.048(8) -0.014(6) -0.008(6) -0.008(6) C26 0.027(6) 0.025(6) 0.046(7) -0.016(5) 0.002(5) -0.002(5) C27 0.037(6) 0.028(6) 0.041(7) -0.017(5) -0.004(5) 0.002(5) C28 0.035(7) 0.055(9) 0.086(11) -0.048(8) 0.005(7) -0.006(6) C29 0.044(7) 0.039(6) 0.023(6) -0.014(5) 0.010(5) -0.012(6) C30 0.047(7) 0.031(6) 0.032(6) -0.001(5) 0.005(6) -0.017(6) C31 0.052(8) 0.048(8) 0.036(7) -0.018(6) 0.006(6) -0.015(7) C32 0.041(7) 0.051(8) 0.045(7) -0.028(6) -0.009(6) 0.005(6) C33 0.055(9) 0.062(9) 0.039(8) -0.026(7) -0.012(7) 0.012(7) C34 0.087(11) 0.068(9) 0.031(7) -0.037(7) -0.014(7) -0.014(8) C35 0.027(6) 0.045(7) 0.073(9) -0.034(7) 0.003(6) -0.005(6) C36 0.026(6) 0.048(7) 0.025(6) -0.003(5) 0.001(5) -0.003(5) C37 0.025(7) 0.074(10) 0.114(14) -0.065(10) 0.013(8) -0.005(7) C38 0.041(8) 0.073(10) 0.066(10) -0.048(8) -0.027(7) 0.019(7) C39 0.076(10) 0.034(7) 0.045(8) -0.016(6) -0.014(7) 0.001(7) C40 0.070(11) 0.120(16) 0.073(12) -0.065(12) -0.035(10) 0.034(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C10 1.812(12) . ? Ru1 C1 2.025(10) . ? Ru1 O1 2.202(7) . ? Ru1 N1 2.233(8) . ? Ru1 P1 2.399(3) . ? Ru1 P2 2.429(4) . ? O1 C11 1.290(11) . ? N1 C11 1.341(12) . ? N1 C15 1.359(12) . ? C1 C2 1.346(14) . ? C1 H1A 0.9500 . ? P1 C23 1.859(12) . ? P1 C29 1.860(11) . ? P1 C26 1.863(11) . ? P2 C35 1.811(12) . ? P2 C32 1.844(12) . ? P2 C38 1.890(15) . ? C2 C3 1.480(12) . ? C2 H2A 0.9500 . ? O2 C10 1.160(13) . ? C3 C4 1.396(14) . ? C3 C8 1.432(14) . ? O3 C6 1.388(12) . ? O3 C9 1.442(14) . ? O4 C13 1.377(12) . ? O4 C16 1.442(12) . ? C4 C5 1.384(13) . ? C4 H4A 0.9500 . ? C5 C6 1.403(14) . ? C5 H5A 0.9500 . ? C6 C7 1.359(15) . ? C7 C8 1.380(14) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.410(14) . ? C12 C13 1.381(13) . ? C12 H12A 0.9500 . ? C13 C14 1.418(14) . ? C14 C15 1.372(14) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.489(14) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.365(15) . ? C17 C18 1.389(14) . ? C18 C19 1.352(15) . ? C18 H18A 0.9500 . ? C19 C20 1.386(17) . ? C19 H19A 0.9500 . ? C20 C21 1.358(17) . ? C20 H20A 0.9500 . ? C21 C22 1.402(15) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C25 1.550(17) . ? C23 C24 1.555(16) . ? C23 H23A 1.0000 . ? 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 C28 1.530(15) . ? C26 C27 1.532(15) . ? C26 H26A 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.481(16) . ? C29 C30 1.550(15) . ? C29 H29A 1.0000 . ? 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 C34 1.496(18) . ? C32 C33 1.549(18) . ? C32 H32A 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.520(17) . ? C35 C37 1.560(17) . ? C35 H35A 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C40 1.523(19) . ? C38 C39 1.56(2) . ? C38 H38A 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 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 C10 Ru1 C1 93.0(4) . . ? C10 Ru1 O1 169.2(4) . . ? C1 Ru1 O1 97.7(3) . . ? C10 Ru1 N1 109.7(4) . . ? C1 Ru1 N1 157.3(4) . . ? O1 Ru1 N1 59.7(3) . . ? C10 Ru1 P1 90.7(4) . . ? C1 Ru1 P1 88.6(3) . . ? O1 Ru1 P1 90.8(2) . . ? N1 Ru1 P1 89.8(2) . . ? C10 Ru1 P2 88.9(4) . . ? C1 Ru1 P2 89.1(3) . . ? O1 Ru1 P2 90.0(2) . . ? N1 Ru1 P2 92.5(2) . . ? P1 Ru1 P2 177.67(12) . . ? C11 O1 Ru1 94.6(6) . . ? C11 N1 C15 118.8(8) . . ? C11 N1 Ru1 91.8(6) . . ? C15 N1 Ru1 149.4(7) . . ? C2 C1 Ru1 133.8(8) . . ? C2 C1 H1A 113.1 . . ? Ru1 C1 H1A 113.1 . . ? C23 P1 C29 101.0(6) . . ? C23 P1 C26 109.1(6) . . ? C29 P1 C26 102.8(5) . . ? C23 P1 Ru1 114.7(4) . . ? C29 P1 Ru1 116.1(4) . . ? C26 P1 Ru1 112.0(4) . . ? C35 P2 C32 111.7(6) . . ? C35 P2 C38 102.0(6) . . ? C32 P2 C38 98.8(6) . . ? C35 P2 Ru1 112.3(4) . . ? C32 P2 Ru1 115.0(4) . . ? C38 P2 Ru1 115.6(5) . . ? C1 C2 C3 126.8(9) . . ? C1 C2 H2A 116.6 . . ? C3 C2 H2A 116.6 . . ? C4 C3 C8 115.8(9) . . ? C4 C3 C2 121.8(9) . . ? C8 C3 C2 122.4(9) . . ? C6 O3 C9 118.6(9) . . ? C13 O4 C16 116.3(7) . . ? C5 C4 C3 123.8(10) . . ? C5 C4 H4A 118.1 . . ? C3 C4 H4A 118.1 . . ? C4 C5 C6 117.8(9) . . ? C4 C5 H5A 121.1 . . ? C6 C5 H5A 121.1 . . ? C7 C6 O3 117.2(10) . . ? C7 C6 C5 120.6(9) . . ? O3 C6 C5 122.1(10) . . ? C6 C7 C8 121.3(10) . . ? C6 C7 H7A 119.3 . . ? C8 C7 H7A 119.3 . . ? C7 C8 C3 120.6(10) . . ? C7 C8 H8A 119.7 . . ? C3 C8 H8A 119.7 . . ? O3 C9 H9A 109.5 . . ? O3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 Ru1 178.0(10) . . ? O1 C11 N1 113.9(9) . . ? O1 C11 C12 124.4(9) . . ? N1 C11 C12 121.6(9) . . ? C13 C12 C11 118.2(9) . . ? C13 C12 H12A 120.9 . . ? C11 C12 H12A 120.9 . . ? O4 C13 C12 124.6(9) . . ? O4 C13 C14 114.5(8) . . ? C12 C13 C14 120.9(9) . . ? C15 C14 C13 116.4(9) . . ? C15 C14 H14A 121.8 . . ? C13 C14 H14A 121.8 . . ? N1 C15 C14 124.0(9) . . ? N1 C15 H15A 118.0 . . ? C14 C15 H15A 118.0 . . ? O4 C16 C17 109.2(8) . . ? O4 C16 H16A 109.8 . . ? C17 C16 H16A 109.8 . . ? O4 C16 H16B 109.8 . . ? C17 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? C22 C17 C18 116.5(10) . . ? C22 C17 C16 121.3(10) . . ? C18 C17 C16 122.1(10) . . ? C19 C18 C17 122.9(11) . . ? C19 C18 H18A 118.5 . . ? C17 C18 H18A 118.5 . . ? C18 C19 C20 119.6(11) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? C21 C20 C19 119.3(10) . . ? C21 C20 H20A 120.3 . . ? C19 C20 H20A 120.3 . . ? C20 C21 C22 119.6(11) . . ? C20 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? C17 C22 C21 121.6(11) . . ? C17 C22 H22A 119.2 . . ? C21 C22 H22A 119.2 . . ? C25 C23 C24 109.3(10) . . ? C25 C23 P1 117.3(9) . . ? C24 C23 P1 114.1(8) . . ? C25 C23 H23A 105.0 . . ? C24 C23 H23A 105.0 . . ? P1 C23 H23A 105.0 . . ? 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 . . ? C28 C26 C27 111.3(10) . . ? C28 C26 P1 114.4(8) . . ? C27 C26 P1 113.7(8) . . ? C28 C26 H26A 105.5 . . ? C27 C26 H26A 105.5 . . ? P1 C26 H26A 105.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C30 112.6(10) . . ? C31 C29 P1 115.9(8) . . ? C30 C29 P1 110.7(7) . . ? C31 C29 H29A 105.6 . . ? C30 C29 H29A 105.6 . . ? P1 C29 H29A 105.6 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C33 109.7(11) . . ? C34 C32 P2 122.2(9) . . ? C33 C32 P2 113.2(9) . . ? C34 C32 H32A 103.1 . . ? C33 C32 H32A 103.1 . . ? P2 C32 H32A 103.1 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C37 108.1(11) . . ? C36 C35 P2 115.0(8) . . ? C37 C35 P2 117.5(9) . . ? C36 C35 H35A 104.9 . . ? C37 C35 H35A 104.9 . . ? P2 C35 H35A 104.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C40 C38 C39 114.1(14) . . ? C40 C38 P2 115.9(11) . . ? C39 C38 P2 108.9(9) . . ? C40 C38 H38A 105.7 . . ? C39 C38 H38A 105.7 . . ? P2 C38 H38A 105.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.93 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.455 _refine_diff_density_min -1.657 _refine_diff_density_rms 0.155 #===END data_obada4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H54 N2 O3 P2 Ru' _chemical_formula_sum 'C34 H54 N2 O3 P2 Ru' _chemical_formula_weight 701.80 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.720(3) _cell_length_b 20.513(4) _cell_length_c 23.998(8) _cell_angle_alpha 90.00 _cell_angle_beta 120.08(2) _cell_angle_gamma 90.00 _cell_volume 7122(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 42002 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 27.22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8736 _exptl_absorpt_correction_T_max 0.9898 _exptl_absorpt_process_details empirical _exptl_special_details ; 'X-SHAPE 2.07 (03-Aug-2005) Stoe & Cie, Darmstadt, Germany' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 101856 _diffrn_reflns_av_R_equivalents 0.1837 _diffrn_reflns_av_sigmaI/netI 0.1047 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.88 _reflns_number_total 15174 _reflns_number_gt 9782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+12.5867P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15174 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1292 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.1471 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.45423(4) 0.82155(2) 0.69828(2) 0.01483(11) Uani 1 1 d . . . P1 P 0.43011(11) 0.88598(7) 0.60797(7) 0.0177(3) Uani 1 1 d . . . P2 P 0.47978(11) 0.75709(7) 0.79006(7) 0.0175(3) Uani 1 1 d . . . O1 O 0.3619(3) 0.88429(19) 0.7139(2) 0.0204(9) Uani 1 1 d . . . O2 O 0.5911(3) 0.7412(2) 0.6845(2) 0.0257(9) Uani 1 1 d . . . O3 O 0.3257(3) 0.9888(2) 0.7690(2) 0.0287(10) Uani 1 1 d . . . N1 N 0.5119(3) 0.9082(2) 0.7621(2) 0.0176(10) Uani 1 1 d . . . N2 N 0.0546(5) 0.4545(3) 0.4608(3) 0.0418(16) Uani 1 1 d . . . C1 C 0.3567(4) 0.7571(3) 0.6398(3) 0.0162(11) Uani 1 1 d . . . H1A H 0.2967 0.7659 0.6332 0.019 Uiso 1 1 calc R . . C2 C 0.3610(4) 0.7038(3) 0.6084(3) 0.0201(12) Uani 1 1 d . . . H2A H 0.4183 0.6962 0.6102 0.024 Uiso 1 1 calc R . . C3 C 0.2863(4) 0.6554(3) 0.5713(3) 0.0210(12) Uani 1 1 d . . . C4 C 0.2977(4) 0.6127(3) 0.5304(3) 0.0230(13) Uani 1 1 d . . . H4A H 0.3496 0.6173 0.5246 0.028 Uiso 1 1 calc R . . C5 C 0.2339(5) 0.5639(3) 0.4983(3) 0.0248(13) Uani 1 1 d . . . H5A H 0.2411 0.5357 0.4696 0.030 Uiso 1 1 calc R . . C6 C 0.1590(5) 0.5561(3) 0.5081(3) 0.0259(14) Uani 1 1 d . . . C7 C 0.1451(5) 0.5996(3) 0.5475(3) 0.0274(14) Uani 1 1 d . . . H7A H 0.0925 0.5954 0.5526 0.033 Uiso 1 1 calc R . . C8 C 0.2093(5) 0.6490(3) 0.5791(3) 0.0243(13) Uani 1 1 d . . . H8A H 0.2006 0.6785 0.6062 0.029 Uiso 1 1 calc R . . C9 C 0.0981(5) 0.5005(3) 0.4805(3) 0.0327(15) Uani 1 1 d . . . C10 C 0.5397(4) 0.7732(3) 0.6908(3) 0.0177(12) Uani 1 1 d . . . C11 C 0.4278(5) 0.9233(3) 0.7528(3) 0.0215(13) Uani 1 1 d . . . C12 C 0.4149(4) 0.9784(3) 0.7845(3) 0.0212(13) Uani 1 1 d . . . C13 C 0.4913(5) 1.0147(3) 0.8251(3) 0.0253(14) Uani 1 1 d . . . H13A H 0.4853 1.0507 0.8476 0.030 Uiso 1 1 calc R . . C14 C 0.5788(5) 0.9987(3) 0.8335(3) 0.0314(16) Uani 1 1 d . . . H14A H 0.6316 1.0243 0.8607 0.038 Uiso 1 1 calc R . . C15 C 0.5859(5) 0.9457(3) 0.8017(3) 0.0238(13) Uani 1 1 d . . . H15A H 0.6448 0.9347 0.8074 0.029 Uiso 1 1 calc R . . C16 C 0.3094(5) 1.0415(3) 0.8013(4) 0.0339(16) Uani 1 1 d . . . H16A H 0.2431 1.0445 0.7863 0.051 Uiso 1 1 calc R . . H16B H 0.3305 1.0825 0.7919 0.051 Uiso 1 1 calc R . . H16C H 0.3435 1.0337 0.8479 0.051 Uiso 1 1 calc R . . C17 C 0.4150(5) 0.8385(3) 0.5370(3) 0.0234(13) Uani 1 1 d . . . H17A H 0.3820 0.7978 0.5368 0.028 Uiso 1 1 calc R . . C18 C 0.3559(5) 0.8684(3) 0.4699(3) 0.0280(14) Uani 1 1 d . . . H18A H 0.3536 0.8384 0.4373 0.042 Uiso 1 1 calc R . . H18B H 0.3832 0.9099 0.4676 0.042 Uiso 1 1 calc R . . H18C H 0.2931 0.8760 0.4618 0.042 Uiso 1 1 calc R . . C19 C 0.5063(5) 0.8155(3) 0.5429(3) 0.0352(16) Uani 1 1 d . . . H19A H 0.4933 0.7907 0.5043 0.053 Uiso 1 1 calc R . . H19B H 0.5394 0.7878 0.5810 0.053 Uiso 1 1 calc R . . H19C H 0.5445 0.8535 0.5470 0.053 Uiso 1 1 calc R . . C20 C 0.3247(4) 0.9377(3) 0.5708(3) 0.0212(13) Uani 1 1 d . . . H20A H 0.3168 0.9536 0.5289 0.025 Uiso 1 1 calc R . . C21 C 0.2396(5) 0.8963(3) 0.5544(3) 0.0285(15) Uani 1 1 d . . . H21A H 0.1843 0.9239 0.5346 0.043 Uiso 1 1 calc R . . H21B H 0.2468 0.8767 0.5939 0.043 Uiso 1 1 calc R . . H21C H 0.2333 0.8617 0.5243 0.043 Uiso 1 1 calc R . . C22 C 0.3269(5) 0.9986(3) 0.6089(3) 0.0283(14) Uani 1 1 d . . . H22A H 0.2683 1.0222 0.5849 0.042 Uiso 1 1 calc R . . H22B H 0.3780 1.0269 0.6153 0.042 Uiso 1 1 calc R . . H22C H 0.3358 0.9853 0.6509 0.042 Uiso 1 1 calc R . . C23 C 0.5253(4) 0.9460(3) 0.6324(3) 0.0235(13) Uani 1 1 d . . . H23A H 0.5207 0.9762 0.6634 0.028 Uiso 1 1 calc R . . C24 C 0.5182(6) 0.9894(3) 0.5781(3) 0.0357(17) Uani 1 1 d . . . H24A H 0.5707 1.0196 0.5954 0.054 Uiso 1 1 calc R . . H24B H 0.4604 1.0144 0.5593 0.054 Uiso 1 1 calc R . . H24C H 0.5188 0.9622 0.5448 0.054 Uiso 1 1 calc R . . C25 C 0.6229(5) 0.9154(3) 0.6698(3) 0.0311(15) Uani 1 1 d . . . H25A H 0.6696 0.9496 0.6815 0.047 Uiso 1 1 calc R . . H25B H 0.6299 0.8829 0.6427 0.047 Uiso 1 1 calc R . . H25C H 0.6310 0.8944 0.7090 0.047 Uiso 1 1 calc R . . C26 C 0.4941(5) 0.6680(3) 0.7790(3) 0.0258(14) Uani 1 1 d . . . H26A H 0.4555 0.6600 0.7316 0.031 Uiso 1 1 calc R . . C27 C 0.4583(5) 0.6202(3) 0.8104(4) 0.0337(16) Uani 1 1 d . . . H27A H 0.4683 0.5755 0.8010 0.051 Uiso 1 1 calc R . . H27B H 0.3921 0.6275 0.7932 0.051 Uiso 1 1 calc R . . H27C H 0.4915 0.6271 0.8571 0.051 Uiso 1 1 calc R . . C28 C 0.5922(5) 0.6489(3) 0.7968(3) 0.0302(15) Uani 1 1 d . . . H28A H 0.5944 0.6021 0.7894 0.045 Uiso 1 1 calc R . . H28B H 0.6346 0.6588 0.8423 0.045 Uiso 1 1 calc R . . H28C H 0.6107 0.6735 0.7701 0.045 Uiso 1 1 calc R . . C29 C 0.3881(4) 0.7580(3) 0.8119(3) 0.0238(13) Uani 1 1 d . . . H29A H 0.4023 0.7220 0.8436 0.029 Uiso 1 1 calc R . . C30 C 0.2933(5) 0.7426(3) 0.7525(3) 0.0311(15) Uani 1 1 d . . . H30A H 0.2456 0.7432 0.7649 0.047 Uiso 1 1 calc R . . H30B H 0.2952 0.6995 0.7357 0.047 Uiso 1 1 calc R . . H30C H 0.2787 0.7756 0.7191 0.047 Uiso 1 1 calc R . . C31 C 0.3812(5) 0.8212(3) 0.8436(3) 0.0318(15) Uani 1 1 d . . . H31A H 0.3314 0.8171 0.8537 0.048 Uiso 1 1 calc R . . H31B H 0.3678 0.8578 0.8139 0.048 Uiso 1 1 calc R . . H31C H 0.4399 0.8291 0.8833 0.048 Uiso 1 1 calc R . . C32 C 0.5810(4) 0.7848(3) 0.8669(3) 0.0188(12) Uani 1 1 d . . . H32A H 0.5647 0.8295 0.8746 0.023 Uiso 1 1 calc R . . C33 C 0.6707(4) 0.7935(3) 0.8631(3) 0.0234(13) Uani 1 1 d . . . H33A H 0.7209 0.8086 0.9049 0.035 Uiso 1 1 calc R . . H33B H 0.6599 0.8257 0.8299 0.035 Uiso 1 1 calc R . . H33C H 0.6878 0.7517 0.8523 0.035 Uiso 1 1 calc R . . C34 C 0.6000(5) 0.7449(3) 0.9261(3) 0.0271(14) Uani 1 1 d . . . H34A H 0.6539 0.7629 0.9643 0.041 Uiso 1 1 calc R . . H34B H 0.6123 0.6995 0.9201 0.041 Uiso 1 1 calc R . . H34C H 0.5460 0.7468 0.9318 0.041 Uiso 1 1 calc R . . Ru2 Ru 0.95814(4) 0.80643(2) 0.70376(2) 0.01548(11) Uani 1 1 d . . . P3 P 0.98574(11) 0.75382(7) 0.80166(7) 0.0187(3) Uani 1 1 d . . . P4 P 0.93353(11) 0.86288(7) 0.60830(7) 0.0180(3) Uani 1 1 d . . . O4 O 0.8750(3) 0.87862(18) 0.7175(2) 0.0200(9) Uani 1 1 d . . . O5 O 1.0743(3) 0.7072(2) 0.6866(2) 0.0275(10) Uani 1 1 d . . . O6 O 0.8481(3) 0.9908(2) 0.7667(2) 0.0277(10) Uani 1 1 d . . . N3 N 1.0262(4) 0.8971(2) 0.7613(2) 0.0184(10) Uani 1 1 d . . . N4 N 0.4008(4) 0.5534(3) 0.4434(3) 0.0317(13) Uani 1 1 d . . . C41 C 0.8491(4) 0.7483(3) 0.6510(3) 0.0165(11) Uani 1 1 d . . . H41A H 0.7946 0.7652 0.6486 0.020 Uiso 1 1 calc R . . C42 C 0.8320(4) 0.6918(3) 0.6180(3) 0.0188(12) Uani 1 1 d . . . H42A H 0.8828 0.6710 0.6181 0.023 Uiso 1 1 calc R . . C43 C 0.7414(4) 0.6598(3) 0.5820(3) 0.0189(12) Uani 1 1 d . . . C44 C 0.7227(5) 0.6146(3) 0.5330(3) 0.0257(13) Uani 1 1 d . . . H44A H 0.7703 0.6031 0.5242 0.031 Uiso 1 1 calc R . . C45 C 0.6363(5) 0.5867(3) 0.4973(3) 0.0249(13) Uani 1 1 d . . . H45A H 0.6253 0.5563 0.4644 0.030 Uiso 1 1 calc R . . C46 C 0.5654(4) 0.6025(3) 0.5091(3) 0.0230(13) Uani 1 1 d . . . C47 C 0.5822(4) 0.6467(3) 0.5579(3) 0.0223(13) Uani 1 1 d . . . H47A H 0.5343 0.6573 0.5667 0.027 Uiso 1 1 calc R . . C48 C 0.6688(4) 0.6752(3) 0.5936(3) 0.0213(12) Uani 1 1 d . . . H48A H 0.6794 0.7056 0.6264 0.026 Uiso 1 1 calc R . . C49 C 0.4743(5) 0.5744(3) 0.4722(3) 0.0259(14) Uani 1 1 d . . . C50 C 1.0310(4) 0.7470(3) 0.6942(3) 0.0222(13) Uani 1 1 d . . . C51 C 0.9437(5) 0.9170(3) 0.7523(3) 0.0214(13) Uani 1 1 d . . . C52 C 0.9357(4) 0.9770(3) 0.7797(3) 0.0207(13) Uani 1 1 d . . . C53 C 1.0133(5) 1.0135(3) 0.8145(3) 0.0266(14) Uani 1 1 d . . . H53A H 1.0096 1.0535 0.8329 0.032 Uiso 1 1 calc R . . C54 C 1.0983(5) 0.9923(3) 0.8232(3) 0.0253(14) Uani 1 1 d . . . H54A H 1.1524 1.0179 0.8472 0.030 Uiso 1 1 calc R . . C55 C 1.1026(5) 0.9339(3) 0.7963(3) 0.0258(14) Uani 1 1 d . . . H55A H 1.1604 0.9192 0.8026 0.031 Uiso 1 1 calc R . . C56 C 0.8384(6) 1.0437(4) 0.8017(4) 0.0415(19) Uani 1 1 d . . . H56A H 0.7730 1.0491 0.7886 0.062 Uiso 1 1 calc R . . H56B H 0.8614 1.0839 0.7926 0.062 Uiso 1 1 calc R . . H56C H 0.8740 1.0344 0.8480 0.062 Uiso 1 1 calc R . . C57 C 0.9130(5) 0.8084(3) 0.5396(3) 0.0238(13) Uani 1 1 d . . . H57A H 0.8760 0.7709 0.5413 0.029 Uiso 1 1 calc R . . C58 C 1.0016(6) 0.7782(4) 0.5466(3) 0.0363(17) Uani 1 1 d . . . H58A H 0.9858 0.7500 0.5095 0.054 Uiso 1 1 calc R . . H58B H 1.0323 0.7523 0.5862 0.054 Uiso 1 1 calc R . . H58C H 1.0431 0.8129 0.5486 0.054 Uiso 1 1 calc R . . C59 C 0.8563(5) 0.8367(3) 0.4716(3) 0.0328(15) Uani 1 1 d . . . H59A H 0.8493 0.8037 0.4399 0.049 Uiso 1 1 calc R . . H59B H 0.8881 0.8749 0.4674 0.049 Uiso 1 1 calc R . . H59C H 0.7951 0.8496 0.4639 0.049 Uiso 1 1 calc R . . C60 C 0.8309(5) 0.9173(3) 0.5687(3) 0.0233(13) Uani 1 1 d . . . H60A H 0.8225 0.9294 0.5257 0.028 Uiso 1 1 calc R . . C61 C 0.7434(5) 0.8818(3) 0.5563(3) 0.0307(15) Uani 1 1 d . . . H61A H 0.6905 0.9115 0.5352 0.046 Uiso 1 1 calc R . . H61B H 0.7503 0.8670 0.5973 0.046 Uiso 1 1 calc R . . H61C H 0.7331 0.8441 0.5284 0.046 Uiso 1 1 calc R . . C62 C 0.8392(5) 0.9817(3) 0.6047(3) 0.0302(15) Uani 1 1 d . . . H62A H 0.7823 1.0071 0.5803 0.045 Uiso 1 1 calc R . . H62B H 0.8917 1.0069 0.6088 0.045 Uiso 1 1 calc R . . H62C H 0.8488 0.9720 0.6476 0.045 Uiso 1 1 calc R . . C63 C 1.0313(4) 0.9192(3) 0.6267(3) 0.0233(13) Uani 1 1 d . . . H63A H 1.0299 0.9527 0.6565 0.028 Uiso 1 1 calc R . . C64 C 1.0221(5) 0.9577(3) 0.5691(3) 0.0299(15) Uani 1 1 d . . . H64A H 1.0758 0.9864 0.5834 0.045 Uiso 1 1 calc R . . H64B H 0.9656 0.9841 0.5505 0.045 Uiso 1 1 calc R . . H64C H 1.0190 0.9274 0.5365 0.045 Uiso 1 1 calc R . . C65 C 1.1266(5) 0.8863(3) 0.6649(3) 0.0310(15) Uani 1 1 d . . . H65A H 1.1751 0.9182 0.6735 0.046 Uiso 1 1 calc R . . H65B H 1.1305 0.8501 0.6398 0.046 Uiso 1 1 calc R . . H65C H 1.1349 0.8698 0.7058 0.046 Uiso 1 1 calc R . . C66 C 0.9861(5) 0.6624(3) 0.7951(3) 0.0249(14) Uani 1 1 d . . . H66A H 0.9432 0.6519 0.7487 0.030 Uiso 1 1 calc R . . C67 C 0.9516(6) 0.6224(3) 0.8336(3) 0.0359(17) Uani 1 1 d . . . H67A H 0.9547 0.5758 0.8259 0.054 Uiso 1 1 calc R . . H67B H 0.8875 0.6344 0.8197 0.054 Uiso 1 1 calc R . . H67C H 0.9906 0.6316 0.8797 0.054 Uiso 1 1 calc R . . C68 C 1.0813(5) 0.6362(3) 0.8109(4) 0.0340(17) Uani 1 1 d . . . H68A H 1.0785 0.5886 0.8067 0.051 Uiso 1 1 calc R . . H68B H 1.1273 0.6482 0.8552 0.051 Uiso 1 1 calc R . . H68C H 1.0988 0.6551 0.7811 0.051 Uiso 1 1 calc R . . C69 C 1.0960(4) 0.7800(3) 0.8740(3) 0.0199(12) Uani 1 1 d . . . H69A H 1.0859 0.8267 0.8806 0.024 Uiso 1 1 calc R . . C70 C 1.1799(5) 0.7806(3) 0.8653(3) 0.0257(14) Uani 1 1 d . . . H70A H 1.2342 0.7950 0.9054 0.039 Uiso 1 1 calc R . . H70B H 1.1690 0.8106 0.8304 0.039 Uiso 1 1 calc R . . H70C H 1.1907 0.7366 0.8545 0.039 Uiso 1 1 calc R . . C71 C 1.1165(5) 0.7462(3) 0.9358(3) 0.0256(14) Uani 1 1 d . . . H71A H 1.1750 0.7626 0.9714 0.038 Uiso 1 1 calc R . . H71B H 1.1214 0.6991 0.9313 0.038 Uiso 1 1 calc R . . H71C H 1.0665 0.7550 0.9448 0.038 Uiso 1 1 calc R . . C72 C 0.8995(5) 0.7675(3) 0.8281(3) 0.0259(14) Uani 1 1 d . . . H72A H 0.9126 0.7344 0.8623 0.031 Uiso 1 1 calc R . . C73 C 0.9039(5) 0.8349(4) 0.8580(4) 0.0357(17) Uani 1 1 d . . . H73A H 0.8566 0.8375 0.8706 0.054 Uiso 1 1 calc R . . H73B H 0.8929 0.8690 0.8264 0.054 Uiso 1 1 calc R . . H73C H 0.9651 0.8411 0.8961 0.054 Uiso 1 1 calc R . . C74 C 0.8017(5) 0.7540(4) 0.7728(3) 0.0325(15) Uani 1 1 d . . . H74A H 0.7573 0.7610 0.7875 0.049 Uiso 1 1 calc R . . H74B H 0.7976 0.7087 0.7584 0.049 Uiso 1 1 calc R . . H74C H 0.7875 0.7835 0.7369 0.049 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 0.0150(2) 0.0155(2) 0.0153(2) 0.00044(18) 0.00853(19) 0.00001(19) P1 0.0183(8) 0.0180(7) 0.0175(7) 0.0001(6) 0.0095(6) -0.0013(6) P2 0.0185(8) 0.0175(7) 0.0180(7) 0.0014(6) 0.0102(6) 0.0007(6) O1 0.019(2) 0.022(2) 0.021(2) -0.0006(16) 0.0113(19) 0.0011(17) O2 0.020(2) 0.035(2) 0.025(2) 0.0034(19) 0.0137(19) 0.0074(19) O3 0.028(3) 0.028(2) 0.031(3) -0.0066(19) 0.016(2) 0.0049(19) N1 0.016(3) 0.019(2) 0.018(2) 0.0019(18) 0.009(2) -0.0004(19) N2 0.051(4) 0.041(3) 0.043(4) -0.011(3) 0.031(3) -0.018(3) C1 0.017(3) 0.018(3) 0.019(3) -0.002(2) 0.013(2) -0.003(2) C2 0.018(3) 0.022(3) 0.021(3) 0.002(2) 0.011(3) 0.002(2) C3 0.026(3) 0.017(3) 0.017(3) 0.004(2) 0.008(3) 0.004(2) C4 0.022(3) 0.024(3) 0.022(3) -0.003(2) 0.010(3) -0.003(2) C5 0.028(4) 0.025(3) 0.022(3) -0.004(2) 0.012(3) 0.001(3) C6 0.030(4) 0.026(3) 0.021(3) 0.000(2) 0.012(3) -0.005(3) C7 0.027(4) 0.032(3) 0.029(3) 0.001(3) 0.019(3) -0.008(3) C8 0.028(4) 0.025(3) 0.019(3) -0.001(2) 0.011(3) -0.001(3) C9 0.032(4) 0.038(4) 0.031(4) -0.012(3) 0.018(3) -0.016(3) C10 0.018(3) 0.020(3) 0.012(3) 0.004(2) 0.005(2) 0.000(2) C11 0.022(3) 0.021(3) 0.015(3) 0.005(2) 0.005(3) 0.001(2) C12 0.023(3) 0.020(3) 0.021(3) 0.001(2) 0.011(3) 0.003(2) C13 0.038(4) 0.018(3) 0.023(3) -0.002(2) 0.017(3) 0.000(3) C14 0.039(4) 0.023(3) 0.025(3) -0.004(3) 0.010(3) -0.009(3) C15 0.025(3) 0.026(3) 0.018(3) 0.001(2) 0.009(3) 0.000(3) C16 0.043(5) 0.025(3) 0.041(4) -0.002(3) 0.027(4) 0.009(3) C17 0.031(4) 0.023(3) 0.022(3) 0.001(2) 0.017(3) -0.001(3) C18 0.031(4) 0.033(3) 0.022(3) -0.002(3) 0.015(3) -0.003(3) C19 0.044(4) 0.036(4) 0.034(4) 0.003(3) 0.026(3) 0.008(3) C20 0.025(3) 0.022(3) 0.015(3) 0.003(2) 0.008(3) 0.004(2) C21 0.019(4) 0.035(3) 0.025(3) 0.001(3) 0.006(3) 0.004(3) C22 0.034(4) 0.024(3) 0.028(3) 0.004(3) 0.016(3) 0.005(3) C23 0.023(3) 0.027(3) 0.021(3) 0.001(2) 0.011(3) -0.006(3) C24 0.049(5) 0.036(4) 0.030(4) 0.003(3) 0.026(4) -0.009(3) C25 0.022(4) 0.042(4) 0.030(4) 0.006(3) 0.014(3) -0.003(3) C26 0.034(4) 0.012(3) 0.023(3) -0.002(2) 0.008(3) -0.002(2) C27 0.034(4) 0.028(3) 0.037(4) 0.005(3) 0.016(3) 0.000(3) C28 0.042(4) 0.020(3) 0.037(4) 0.000(3) 0.025(3) 0.009(3) C29 0.020(3) 0.034(3) 0.021(3) 0.004(3) 0.013(3) -0.002(3) C30 0.026(4) 0.040(4) 0.036(4) 0.004(3) 0.022(3) -0.002(3) C31 0.029(4) 0.040(4) 0.036(4) -0.005(3) 0.023(3) -0.004(3) C32 0.020(3) 0.022(3) 0.014(3) 0.001(2) 0.008(2) 0.003(2) C33 0.018(3) 0.029(3) 0.022(3) 0.000(2) 0.009(3) -0.001(2) C34 0.028(4) 0.027(3) 0.020(3) 0.003(2) 0.008(3) 0.000(3) Ru2 0.0160(2) 0.0153(2) 0.0163(2) 0.00052(18) 0.0090(2) 0.00000(19) P3 0.0187(8) 0.0199(7) 0.0171(7) 0.0008(6) 0.0088(6) -0.0008(6) P4 0.0185(8) 0.0198(7) 0.0181(7) 0.0002(6) 0.0109(6) -0.0006(6) O4 0.020(2) 0.0178(19) 0.023(2) -0.0012(16) 0.0106(19) 0.0029(16) O5 0.027(3) 0.028(2) 0.034(2) 0.0022(19) 0.019(2) 0.0065(19) O6 0.026(3) 0.029(2) 0.034(3) -0.0066(19) 0.019(2) 0.0037(19) N3 0.021(3) 0.018(2) 0.019(2) 0.0043(19) 0.012(2) 0.0017(19) N4 0.030(3) 0.033(3) 0.028(3) -0.002(2) 0.012(3) -0.006(3) C41 0.018(3) 0.019(3) 0.017(3) 0.006(2) 0.011(2) 0.001(2) C42 0.017(3) 0.022(3) 0.022(3) 0.007(2) 0.014(2) 0.010(2) C43 0.021(3) 0.017(3) 0.021(3) 0.000(2) 0.012(3) -0.002(2) C44 0.028(4) 0.020(3) 0.030(3) -0.005(2) 0.016(3) 0.000(3) C45 0.028(4) 0.021(3) 0.028(3) -0.006(2) 0.015(3) -0.004(3) C46 0.024(3) 0.019(3) 0.017(3) 0.005(2) 0.003(3) -0.003(2) C47 0.023(3) 0.021(3) 0.025(3) 0.002(2) 0.014(3) -0.002(2) C48 0.026(3) 0.019(3) 0.019(3) -0.003(2) 0.012(3) -0.001(2) C49 0.033(4) 0.022(3) 0.024(3) 0.004(2) 0.016(3) 0.001(3) C50 0.017(3) 0.027(3) 0.022(3) 0.004(2) 0.009(3) -0.001(2) C51 0.025(4) 0.026(3) 0.020(3) -0.004(2) 0.017(3) -0.005(3) C52 0.023(3) 0.022(3) 0.024(3) 0.001(2) 0.016(3) -0.001(2) C53 0.040(4) 0.018(3) 0.024(3) -0.006(2) 0.017(3) 0.000(3) C54 0.024(4) 0.030(3) 0.017(3) -0.004(2) 0.007(3) -0.006(3) C55 0.023(3) 0.032(3) 0.024(3) -0.001(3) 0.014(3) -0.006(3) C56 0.040(5) 0.037(4) 0.058(5) -0.015(4) 0.032(4) 0.000(3) C57 0.034(4) 0.021(3) 0.023(3) -0.006(2) 0.018(3) -0.002(3) C58 0.051(5) 0.039(4) 0.033(4) 0.001(3) 0.032(4) 0.007(3) C59 0.036(4) 0.039(4) 0.023(3) -0.003(3) 0.015(3) -0.006(3) C60 0.026(4) 0.026(3) 0.020(3) 0.001(2) 0.014(3) 0.001(3) C61 0.019(4) 0.041(4) 0.030(4) 0.006(3) 0.011(3) 0.007(3) C62 0.033(4) 0.025(3) 0.027(3) 0.003(3) 0.011(3) 0.007(3) C63 0.022(3) 0.030(3) 0.019(3) -0.002(2) 0.011(3) -0.010(3) C64 0.030(4) 0.035(4) 0.024(3) 0.002(3) 0.013(3) -0.007(3) C65 0.019(3) 0.041(4) 0.032(4) 0.006(3) 0.013(3) -0.002(3) C66 0.029(4) 0.023(3) 0.016(3) 0.004(2) 0.006(3) 0.000(3) C67 0.045(5) 0.026(3) 0.032(4) 0.008(3) 0.016(3) -0.002(3) C68 0.041(4) 0.020(3) 0.035(4) 0.005(3) 0.015(3) 0.009(3) C69 0.022(3) 0.021(3) 0.015(3) -0.006(2) 0.008(3) -0.006(2) C70 0.021(3) 0.036(3) 0.020(3) 0.002(3) 0.010(3) -0.002(3) C71 0.024(4) 0.033(3) 0.019(3) 0.000(3) 0.011(3) -0.007(3) C72 0.022(3) 0.035(3) 0.028(3) 0.001(3) 0.018(3) -0.001(3) C73 0.038(4) 0.045(4) 0.036(4) 0.004(3) 0.028(4) 0.010(3) C74 0.025(4) 0.053(4) 0.027(3) 0.003(3) 0.018(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C10 1.820(6) . ? Ru1 C1 2.021(6) . ? Ru1 O1 2.182(4) . ? Ru1 N1 2.225(5) . ? Ru1 P1 2.3938(17) . ? Ru1 P2 2.4163(17) . ? P1 C20 1.858(6) . ? P1 C23 1.860(6) . ? P1 C17 1.865(6) . ? P2 C29 1.851(6) . ? P2 C32 1.860(6) . ? P2 C26 1.879(6) . ? O1 C11 1.302(7) . ? O2 C10 1.150(7) . ? O3 C12 1.362(8) . ? O3 C16 1.435(7) . ? N1 C11 1.345(8) . ? N1 C15 1.360(8) . ? N2 C9 1.141(9) . ? C1 C2 1.350(8) . ? C1 H1A 0.9500 . ? C2 C3 1.491(8) . ? C2 H2A 0.9500 . ? C3 C4 1.398(8) . ? C3 C8 1.398(9) . ? C4 C5 1.383(9) . ? C4 H4A 0.9500 . ? C5 C6 1.393(9) . ? C5 H5A 0.9500 . ? C6 C7 1.403(9) . ? C6 C9 1.449(9) . ? C7 C8 1.392(9) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C11 C12 1.437(8) . ? C12 C13 1.374(9) . ? C13 C14 1.411(10) . ? C13 H13A 0.9500 . ? C14 C15 1.368(9) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.535(9) . ? C17 C19 1.535(10) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.530(9) . ? C20 C22 1.537(8) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.534(8) . ? C23 C25 1.546(9) . ? C23 H23A 1.0000 . ? 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 C28 1.525(10) . ? C26 C27 1.529(9) . ? C26 H26A 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.538(9) . ? C29 C30 1.542(9) . ? C29 H29A 1.0000 . ? 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 C34 1.529(8) . ? C32 C33 1.557(9) . ? C32 H32A 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? Ru2 C50 1.817(6) . ? Ru2 C41 2.008(6) . ? Ru2 O4 2.166(4) . ? Ru2 N3 2.255(5) . ? Ru2 P3 2.4106(18) . ? Ru2 P4 2.4111(17) . ? P3 C72 1.866(7) . ? P3 C69 1.869(6) . ? P3 C66 1.883(6) . ? P4 C60 1.861(7) . ? P4 C63 1.864(6) . ? P4 C57 1.875(6) . ? O4 C51 1.295(7) . ? O5 C50 1.166(7) . ? O6 C52 1.365(8) . ? O6 C56 1.432(8) . ? N3 C51 1.349(8) . ? N3 C55 1.353(8) . ? N4 C49 1.150(9) . ? C41 C42 1.352(8) . ? C41 H41A 0.9500 . ? C42 C43 1.471(8) . ? C42 H42A 0.9500 . ? C43 C44 1.403(8) . ? C43 C48 1.409(8) . ? C44 C45 1.381(9) . ? C44 H44A 0.9500 . ? C45 C46 1.387(9) . ? C45 H45A 0.9500 . ? C46 C47 1.394(9) . ? C46 C49 1.443(9) . ? C47 C48 1.390(9) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C51 C52 1.433(8) . ? C52 C53 1.361(9) . ? C53 C54 1.399(10) . ? C53 H53A 0.9500 . ? C54 C55 1.379(9) . ? C54 H54A 0.9500 . ? C55 H55A 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C59 1.534(9) . ? C57 C58 1.535(10) . ? C57 H57A 1.0000 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.524(9) . ? C60 C62 1.546(9) . ? C60 H60A 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.532(8) . ? C63 C65 1.539(9) . ? C63 H63A 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C68 1.536(10) . ? C66 C67 1.549(9) . ? C66 H66A 1.0000 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C71 1.513(8) . ? C69 C70 1.519(9) . ? C69 H69A 1.0000 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C74 1.529(9) . ? C72 C73 1.543(9) . ? C72 H72A 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 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 C10 Ru1 C1 88.6(2) . . ? C10 Ru1 O1 175.0(2) . . ? C1 Ru1 O1 96.4(2) . . ? C10 Ru1 N1 114.3(2) . . ? C1 Ru1 N1 157.0(2) . . ? O1 Ru1 N1 60.69(17) . . ? C10 Ru1 P1 89.76(17) . . ? C1 Ru1 P1 91.23(16) . . ? O1 Ru1 P1 90.99(12) . . ? N1 Ru1 P1 90.04(13) . . ? C10 Ru1 P2 90.17(17) . . ? C1 Ru1 P2 89.28(16) . . ? O1 Ru1 P2 89.04(12) . . ? N1 Ru1 P2 89.53(13) . . ? P1 Ru1 P2 179.49(7) . . ? C20 P1 C23 103.2(3) . . ? C20 P1 C17 101.4(3) . . ? C23 P1 C17 109.6(3) . . ? C20 P1 Ru1 116.1(2) . . ? C23 P1 Ru1 110.5(2) . . ? C17 P1 Ru1 115.0(2) . . ? C29 P2 C32 100.8(3) . . ? C29 P2 C26 103.4(3) . . ? C32 P2 C26 108.7(3) . . ? C29 P2 Ru1 117.3(2) . . ? C32 P2 Ru1 113.16(19) . . ? C26 P2 Ru1 112.4(2) . . ? C11 O1 Ru1 93.9(4) . . ? C12 O3 C16 116.7(5) . . ? C11 N1 C15 119.7(5) . . ? C11 N1 Ru1 90.8(4) . . ? C15 N1 Ru1 149.5(4) . . ? C2 C1 Ru1 131.8(5) . . ? C2 C1 H1A 114.1 . . ? Ru1 C1 H1A 114.1 . . ? C1 C2 C3 127.5(6) . . ? C1 C2 H2A 116.3 . . ? C3 C2 H2A 116.3 . . ? C4 C3 C8 119.6(6) . . ? C4 C3 C2 117.9(6) . . ? C8 C3 C2 122.4(5) . . ? C5 C4 C3 120.5(6) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C5 C6 119.7(6) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C5 C6 C7 120.6(6) . . ? C5 C6 C9 119.9(6) . . ? C7 C6 C9 119.4(6) . . ? C8 C7 C6 119.1(6) . . ? C8 C7 H7A 120.4 . . ? C6 C7 H7A 120.4 . . ? C7 C8 C3 120.4(6) . . ? C7 C8 H8A 119.8 . . ? C3 C8 H8A 119.8 . . ? N2 C9 C6 175.9(9) . . ? O2 C10 Ru1 177.5(5) . . ? O1 C11 N1 114.5(5) . . ? O1 C11 C12 124.4(6) . . ? N1 C11 C12 121.0(6) . . ? O3 C12 C13 127.7(5) . . ? O3 C12 C11 114.4(5) . . ? C13 C12 C11 117.9(6) . . ? C12 C13 C14 120.3(6) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C15 C14 C13 118.6(6) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? N1 C15 C14 122.4(7) . . ? N1 C15 H15A 118.8 . . ? C14 C15 H15A 118.8 . . ? O3 C16 H16A 109.5 . . ? O3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 107.8(5) . . ? C18 C17 P1 118.1(4) . . ? C19 C17 P1 113.8(5) . . ? C18 C17 H17A 105.3 . . ? C19 C17 H17A 105.3 . . ? P1 C17 H17A 105.3 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 110.2(5) . . ? C21 C20 P1 110.0(4) . . ? C22 C20 P1 116.4(4) . . ? C21 C20 H20A 106.6 . . ? C22 C20 H20A 106.6 . . ? P1 C20 H20A 106.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C25 109.8(6) . . ? C24 C23 P1 115.3(5) . . ? C25 C23 P1 113.7(4) . . ? C24 C23 H23A 105.7 . . ? C25 C23 H23A 105.7 . . ? P1 C23 H23A 105.7 . . ? 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 . . ? C28 C26 C27 109.3(5) . . ? C28 C26 P2 113.9(4) . . ? C27 C26 P2 116.4(5) . . ? C28 C26 H26A 105.4 . . ? C27 C26 H26A 105.4 . . ? P2 C26 H26A 105.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C30 109.4(6) . . ? C31 C29 P2 115.2(4) . . ? C30 C29 P2 110.5(4) . . ? C31 C29 H29A 107.1 . . ? C30 C29 H29A 107.1 . . ? P2 C29 H29A 107.1 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C33 110.9(5) . . ? C34 C32 P2 114.8(4) . . ? C33 C32 P2 113.7(4) . . ? C34 C32 H32A 105.5 . . ? C33 C32 H32A 105.5 . . ? P2 C32 H32A 105.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C50 Ru2 C41 88.6(3) . . ? C50 Ru2 O4 178.3(2) . . ? C41 Ru2 O4 93.0(2) . . ? C50 Ru2 N3 117.8(2) . . ? C41 Ru2 N3 153.6(2) . . ? O4 Ru2 N3 60.58(17) . . ? C50 Ru2 P3 90.53(19) . . ? C41 Ru2 P3 91.07(15) . . ? O4 Ru2 P3 88.97(12) . . ? N3 Ru2 P3 88.90(13) . . ? C50 Ru2 P4 90.50(19) . . ? C41 Ru2 P4 90.99(15) . . ? O4 Ru2 P4 89.94(12) . . ? N3 Ru2 P4 88.81(13) . . ? P3 Ru2 P4 177.72(6) . . ? C72 P3 C69 102.2(3) . . ? C72 P3 C66 102.3(3) . . ? C69 P3 C66 108.7(3) . . ? C72 P3 Ru2 117.5(2) . . ? C69 P3 Ru2 113.2(2) . . ? C66 P3 Ru2 111.8(2) . . ? C60 P4 C63 102.9(3) . . ? C60 P4 C57 101.1(3) . . ? C63 P4 C57 109.3(3) . . ? C60 P4 Ru2 116.6(2) . . ? C63 P4 Ru2 111.1(2) . . ? C57 P4 Ru2 114.7(2) . . ? C51 O4 Ru2 94.9(4) . . ? C52 O6 C56 116.6(5) . . ? C51 N3 C55 120.1(5) . . ? C51 N3 Ru2 89.4(4) . . ? C55 N3 Ru2 150.5(4) . . ? C42 C41 Ru2 137.5(5) . . ? C42 C41 H41A 111.3 . . ? Ru2 C41 H41A 111.3 . . ? C41 C42 C43 125.5(5) . . ? C41 C42 H42A 117.3 . . ? C43 C42 H42A 117.3 . . ? C44 C43 C48 117.5(5) . . ? C44 C43 C42 121.2(5) . . ? C48 C43 C42 121.3(5) . . ? C45 C44 C43 121.1(6) . . ? C45 C44 H44A 119.4 . . ? C43 C44 H44A 119.4 . . ? C44 C45 C46 120.9(6) . . ? C44 C45 H45A 119.6 . . ? C46 C45 H45A 119.6 . . ? C45 C46 C47 119.3(6) . . ? C45 C46 C49 122.0(6) . . ? C47 C46 C49 118.7(6) . . ? C48 C47 C46 120.0(6) . . ? C48 C47 H47A 120.0 . . ? C46 C47 H47A 120.0 . . ? C47 C48 C43 121.3(5) . . ? C47 C48 H48A 119.4 . . ? C43 C48 H48A 119.4 . . ? N4 C49 C46 178.1(7) . . ? O5 C50 Ru2 177.1(6) . . ? O4 C51 N3 115.1(5) . . ? O4 C51 C52 124.2(6) . . ? N3 C51 C52 120.7(6) . . ? C53 C52 O6 127.6(5) . . ? C53 C52 C51 118.3(6) . . ? O6 C52 C51 114.1(5) . . ? C52 C53 C54 120.4(6) . . ? C52 C53 H53A 119.8 . . ? C54 C53 H53A 119.8 . . ? C55 C54 C53 119.1(6) . . ? C55 C54 H54A 120.5 . . ? C53 C54 H54A 120.5 . . ? N3 C55 C54 121.4(6) . . ? N3 C55 H55A 119.3 . . ? C54 C55 H55A 119.3 . . ? O6 C56 H56A 109.5 . . ? O6 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O6 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C59 C57 C58 108.5(5) . . ? C59 C57 P4 117.0(4) . . ? C58 C57 P4 113.8(5) . . ? C59 C57 H57A 105.5 . . ? C58 C57 H57A 105.5 . . ? P4 C57 H57A 105.5 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C61 C60 C62 109.1(6) . . ? C61 C60 P4 111.2(4) . . ? C62 C60 P4 115.2(5) . . ? C61 C60 H60A 107.0 . . ? C62 C60 H60A 107.0 . . ? P4 C60 H60A 107.0 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C65 111.7(5) . . ? C64 C63 P4 115.2(4) . . ? C65 C63 P4 113.1(4) . . ? C64 C63 H63A 105.2 . . ? C65 C63 H63A 105.2 . . ? P4 C63 H63A 105.2 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C68 C66 C67 108.5(5) . . ? C68 C66 P3 112.0(4) . . ? C67 C66 P3 117.4(5) . . ? C68 C66 H66A 106.1 . . ? C67 C66 H66A 106.1 . . ? P3 C66 H66A 106.1 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C71 C69 C70 111.6(5) . . ? C71 C69 P3 114.3(4) . . ? C70 C69 P3 115.1(4) . . ? C71 C69 H69A 104.8 . . ? C70 C69 H69A 104.8 . . ? P3 C69 H69A 104.8 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C74 C72 C73 110.4(6) . . ? C74 C72 P3 110.5(4) . . ? C73 C72 P3 115.3(5) . . ? C74 C72 H72A 106.7 . . ? C73 C72 H72A 106.7 . . ? P3 C72 H72A 106.7 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.88 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.418 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.116 #===END data_obada5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H54 F3 N O P2 Ru S, C H2 Cl2' _chemical_formula_sum 'C38 H56 Cl2 F3 N O P2 Ru S' _chemical_formula_weight 865.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 9.5181(19) _cell_length_b 12.048(2) _cell_length_c 17.701(4) _cell_angle_alpha 83.19(3) _cell_angle_beta 85.91(3) _cell_angle_gamma 86.66(3) _cell_volume 2007.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 34123 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 27.23 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.267 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8014 _exptl_absorpt_correction_T_max 0.9255 _exptl_absorpt_process_details empirical _exptl_special_details ; 'X-SHAPE 2.07 (03-Aug-2005) Stoe & Cie, Darmstadt, Germany' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28542 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.86 _reflns_number_total 8492 _reflns_number_gt 6954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.6568P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8492 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.20438(2) 0.532790(15) 0.751467(11) 0.01094(5) Uani 1 1 d . . . S1 S -0.01687(6) 0.42838(5) 0.78902(3) 0.01556(12) Uani 1 1 d . . . O1 O 0.44505(18) 0.65574(15) 0.67109(11) 0.0222(4) Uani 1 1 d . . . C1 C 0.2083(2) 0.62531(19) 0.84103(13) 0.0151(5) Uani 1 1 d . . . H1A H 0.1351 0.6096 0.8795 0.018 Uiso 1 1 calc R . . P1 P 0.34373(6) 0.38920(5) 0.82781(3) 0.01369(12) Uani 1 1 d . . . N1 N 0.1661(2) 0.40308(15) 0.67806(11) 0.0139(4) Uani 1 1 d . . . F1 F 0.30891(19) 1.04136(14) 1.11215(10) 0.0355(4) Uani 1 1 d . . . P2 P 0.05276(6) 0.68122(5) 0.69085(3) 0.01319(12) Uani 1 1 d . . . C2 C 0.2934(3) 0.70386(19) 0.85653(14) 0.0161(5) Uani 1 1 d . . . H2A H 0.3704 0.7213 0.8207 0.019 Uiso 1 1 calc R . . F3 F 0.1906(2) 0.91308(14) 1.17771(9) 0.0373(4) Uani 1 1 d . . . C3 C 0.2779(2) 0.76506(19) 0.92395(14) 0.0157(5) Uani 1 1 d . . . F2 F 0.0880(2) 1.03286(16) 1.09758(12) 0.0462(5) Uani 1 1 d . . . C4 C 0.3424(3) 0.8678(2) 0.92153(14) 0.0189(5) Uani 1 1 d . . . H4A H 0.4007 0.8932 0.8778 0.023 Uiso 1 1 calc R . . C5 C 0.3229(3) 0.9322(2) 0.98131(15) 0.0208(5) Uani 1 1 d . . . H5A H 0.3663 1.0018 0.9781 0.025 Uiso 1 1 calc R . . C6 C 0.2394(3) 0.8952(2) 1.04647(15) 0.0201(5) Uani 1 1 d . . . C7 C 0.1793(3) 0.7918(2) 1.05173(15) 0.0208(5) Uani 1 1 d . . . H7A H 0.1251 0.7650 1.0967 0.025 Uiso 1 1 calc R . . C8 C 0.1986(3) 0.7282(2) 0.99135(15) 0.0201(5) Uani 1 1 d . . . H8A H 0.1571 0.6577 0.9956 0.024 Uiso 1 1 calc R . . C9 C 0.2073(3) 0.9696(2) 1.10759(16) 0.0258(6) Uani 1 1 d . . . C19 C 0.2358(3) 0.35197(19) 0.61928(13) 0.0159(5) Uani 1 1 d . . . C18 C 0.3629(3) 0.3936(2) 0.58425(14) 0.0193(5) Uani 1 1 d . . . H11A H 0.4003 0.4570 0.6013 0.023 Uiso 1 1 calc R . . C17 C 0.4331(3) 0.3434(2) 0.52573(15) 0.0236(5) Uani 1 1 d . . . H12A H 0.5184 0.3724 0.5025 0.028 Uiso 1 1 calc R . . C16 C 0.3788(3) 0.2485(2) 0.49993(15) 0.0246(6) Uani 1 1 d . . . H13A H 0.4276 0.2142 0.4593 0.030 Uiso 1 1 calc R . . C15 C 0.2567(3) 0.2064(2) 0.53330(15) 0.0226(5) Uani 1 1 d . . . H14A H 0.2215 0.1424 0.5159 0.027 Uiso 1 1 calc R . . C14 C 0.1814(3) 0.25653(19) 0.59345(14) 0.0189(5) Uani 1 1 d . . . C13 C 0.0527(3) 0.2158(2) 0.62978(15) 0.0213(5) Uani 1 1 d . . . H16A H 0.0124 0.1536 0.6127 0.026 Uiso 1 1 calc R . . C12 C -0.0123(3) 0.26572(19) 0.68867(15) 0.0191(5) Uani 1 1 d . . . H17A H -0.0973 0.2381 0.7134 0.023 Uiso 1 1 calc R . . C11 C 0.0480(2) 0.35998(19) 0.71300(14) 0.0152(5) Uani 1 1 d . . . C10 C 0.3557(3) 0.60540(19) 0.70368(14) 0.0174(5) Uani 1 1 d . . . C20 C 0.5383(2) 0.4024(2) 0.81508(14) 0.0184(5) Uani 1 1 d . . . H20A H 0.5821 0.3365 0.8463 0.022 Uiso 1 1 calc R . . C21 C 0.5959(3) 0.3966(2) 0.73211(15) 0.0216(5) Uani 1 1 d . . . H21A H 0.6988 0.3855 0.7304 0.032 Uiso 1 1 calc R . . H21B H 0.5699 0.4667 0.7011 0.032 Uiso 1 1 calc R . . H21C H 0.5555 0.3339 0.7120 0.032 Uiso 1 1 calc R . . C22 C 0.5878(3) 0.5071(2) 0.84437(17) 0.0239(6) Uani 1 1 d . . . H22A H 0.6903 0.5104 0.8346 0.036 Uiso 1 1 calc R . . H22B H 0.5638 0.5041 0.8993 0.036 Uiso 1 1 calc R . . H22C H 0.5413 0.5738 0.8180 0.036 Uiso 1 1 calc R . . C23 C 0.3121(3) 0.3950(2) 0.93244(14) 0.0172(5) Uani 1 1 d . . . H23A H 0.3394 0.4712 0.9410 0.021 Uiso 1 1 calc R . . C24 C 0.4051(3) 0.3133(2) 0.98288(15) 0.0232(5) Uani 1 1 d . . . H24A H 0.3923 0.3307 1.0357 0.035 Uiso 1 1 calc R . . H24B H 0.5043 0.3203 0.9647 0.035 Uiso 1 1 calc R . . H24C H 0.3783 0.2365 0.9804 0.035 Uiso 1 1 calc R . . C25 C 0.1576(3) 0.3883(2) 0.96334(14) 0.0204(5) Uani 1 1 d . . . H25A H 0.1452 0.4204 1.0119 0.031 Uiso 1 1 calc R . . H25B H 0.1324 0.3099 0.9713 0.031 Uiso 1 1 calc R . . H25C H 0.0965 0.4304 0.9265 0.031 Uiso 1 1 calc R . . C26 C 0.3281(3) 0.23994(19) 0.80923(15) 0.0181(5) Uani 1 1 d . . . H26A H 0.3159 0.2427 0.7534 0.022 Uiso 1 1 calc R . . C27 C 0.4571(3) 0.1599(2) 0.82542(15) 0.0216(5) Uani 1 1 d . . . H27A H 0.4389 0.0855 0.8122 0.032 Uiso 1 1 calc R . . H27B H 0.4747 0.1547 0.8796 0.032 Uiso 1 1 calc R . . H27C H 0.5398 0.1884 0.7947 0.032 Uiso 1 1 calc R . . C28 C 0.1974(3) 0.1852(2) 0.84970(16) 0.0226(5) Uani 1 1 d . . . H28A H 0.1822 0.1164 0.8276 0.034 Uiso 1 1 calc R . . H28B H 0.1148 0.2370 0.8432 0.034 Uiso 1 1 calc R . . H28C H 0.2118 0.1673 0.9041 0.034 Uiso 1 1 calc R . . C29 C 0.1294(3) 0.82375(18) 0.67713(14) 0.0167(5) Uani 1 1 d . . . H29A H 0.2340 0.8098 0.6713 0.020 Uiso 1 1 calc R . . C30 C 0.0891(3) 0.9014(2) 0.60538(15) 0.0225(5) Uani 1 1 d . . . H30A H 0.1396 0.9706 0.6021 0.034 Uiso 1 1 calc R . . H30B H -0.0127 0.9193 0.6086 0.034 Uiso 1 1 calc R . . H30C H 0.1150 0.8636 0.5599 0.034 Uiso 1 1 calc R . . C31 C 0.1015(3) 0.8912(2) 0.74586(15) 0.0216(5) Uani 1 1 d . . . H31A H 0.1615 0.9555 0.7393 0.032 Uiso 1 1 calc R . . H31B H 0.1230 0.8433 0.7927 0.032 Uiso 1 1 calc R . . H31C H 0.0022 0.9178 0.7493 0.032 Uiso 1 1 calc R . . C32 C 0.0138(3) 0.66393(19) 0.59137(13) 0.0166(5) Uani 1 1 d . . . H32A H -0.0332 0.7360 0.5698 0.020 Uiso 1 1 calc R . . C33 C 0.1519(3) 0.6474(2) 0.54244(14) 0.0199(5) Uani 1 1 d . . . H33A H 0.1323 0.6578 0.4884 0.030 Uiso 1 1 calc R . . H33B H 0.1927 0.5717 0.5556 0.030 Uiso 1 1 calc R . . H33C H 0.2185 0.7023 0.5521 0.030 Uiso 1 1 calc R . . C34 C -0.0873(3) 0.5715(2) 0.58489(15) 0.0219(5) Uani 1 1 d . . . H34A H -0.1017 0.5674 0.5310 0.033 Uiso 1 1 calc R . . H34B H -0.1780 0.5884 0.6120 0.033 Uiso 1 1 calc R . . H34C H -0.0469 0.4996 0.6075 0.033 Uiso 1 1 calc R . . C35 C -0.1286(2) 0.6968(2) 0.73690(14) 0.0167(5) Uani 1 1 d . . . H35A H -0.1742 0.6259 0.7310 0.020 Uiso 1 1 calc R . . C36 C -0.1340(3) 0.7029(2) 0.82312(14) 0.0186(5) Uani 1 1 d . . . H36A H -0.2325 0.7099 0.8429 0.028 Uiso 1 1 calc R . . H36B H -0.0843 0.7680 0.8333 0.028 Uiso 1 1 calc R . . H36C H -0.0886 0.6346 0.8483 0.028 Uiso 1 1 calc R . . C37 C -0.2237(3) 0.7907(2) 0.69806(16) 0.0222(5) Uani 1 1 d . . . H37A H -0.3212 0.7829 0.7190 0.033 Uiso 1 1 calc R . . H37B H -0.2188 0.7858 0.6431 0.033 Uiso 1 1 calc R . . H37C H -0.1917 0.8635 0.7074 0.033 Uiso 1 1 calc R . . Cl1 Cl 0.54541(8) 1.03357(7) 0.34604(6) 0.0442(2) Uani 1 1 d . . . Cl2 Cl 0.30641(9) 0.92990(7) 0.43254(5) 0.0473(2) Uani 1 1 d . . . C100 C 0.4304(3) 0.9238(2) 0.35407(18) 0.0334(7) Uani 1 1 d . . . H10A H 0.4857 0.8515 0.3600 0.040 Uiso 1 1 calc R . . H10B H 0.3800 0.9276 0.3067 0.040 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 0.01085(9) 0.01024(9) 0.01180(9) -0.00190(6) 0.00038(6) -0.00115(6) S1 0.0145(3) 0.0148(3) 0.0173(3) -0.0021(2) 0.0006(2) -0.0016(2) O1 0.0170(9) 0.0222(9) 0.0265(10) -0.0016(7) 0.0045(8) -0.0042(7) C1 0.0144(11) 0.0156(11) 0.0149(11) -0.0015(9) -0.0010(9) 0.0032(9) P1 0.0129(3) 0.0138(3) 0.0144(3) -0.0018(2) -0.0009(2) -0.0003(2) N1 0.0153(9) 0.0115(9) 0.0149(10) 0.0000(7) -0.0025(8) -0.0005(7) F1 0.0436(10) 0.0310(9) 0.0367(10) -0.0211(8) 0.0018(8) -0.0122(8) P2 0.0147(3) 0.0116(3) 0.0133(3) -0.0022(2) 0.0001(2) -0.0002(2) C2 0.0159(11) 0.0160(11) 0.0161(11) -0.0020(9) 0.0015(9) -0.0013(9) F3 0.0525(11) 0.0367(9) 0.0241(9) -0.0119(7) 0.0064(8) -0.0066(8) C3 0.0126(11) 0.0153(11) 0.0198(12) -0.0027(9) -0.0042(9) 0.0000(9) F2 0.0407(11) 0.0501(11) 0.0526(12) -0.0317(10) -0.0130(9) 0.0231(9) C4 0.0213(12) 0.0162(11) 0.0192(12) -0.0014(9) -0.0011(10) -0.0032(9) C5 0.0264(13) 0.0142(11) 0.0225(13) -0.0023(10) -0.0051(10) -0.0024(10) C6 0.0200(12) 0.0185(12) 0.0232(13) -0.0082(10) -0.0035(10) 0.0019(9) C7 0.0182(12) 0.0242(13) 0.0206(13) -0.0050(10) 0.0016(10) -0.0043(10) C8 0.0194(12) 0.0186(12) 0.0231(13) -0.0041(10) -0.0003(10) -0.0047(10) C9 0.0282(14) 0.0234(13) 0.0272(14) -0.0089(11) -0.0031(11) 0.0011(11) C19 0.0205(12) 0.0139(11) 0.0132(11) -0.0010(9) -0.0041(9) 0.0035(9) C18 0.0190(12) 0.0191(12) 0.0196(12) -0.0018(10) -0.0030(10) 0.0023(9) C17 0.0239(13) 0.0254(13) 0.0202(13) -0.0017(10) 0.0016(10) 0.0025(10) C16 0.0324(14) 0.0216(13) 0.0196(13) -0.0062(10) -0.0007(11) 0.0074(11) C15 0.0333(14) 0.0159(11) 0.0192(13) -0.0055(10) -0.0056(11) 0.0041(10) C14 0.0248(13) 0.0136(11) 0.0183(12) -0.0019(9) -0.0046(10) 0.0037(9) C13 0.0268(13) 0.0141(11) 0.0239(13) -0.0016(10) -0.0086(11) -0.0025(10) C12 0.0188(12) 0.0143(11) 0.0243(13) -0.0011(9) -0.0026(10) -0.0035(9) C11 0.0150(11) 0.0122(10) 0.0182(12) -0.0004(9) -0.0039(9) 0.0006(8) C10 0.0195(12) 0.0140(11) 0.0193(12) -0.0044(9) -0.0039(10) 0.0022(9) C20 0.0136(11) 0.0207(12) 0.0215(13) -0.0040(10) -0.0027(9) -0.0005(9) C21 0.0157(12) 0.0236(12) 0.0249(14) -0.0033(10) 0.0016(10) 0.0011(10) C22 0.0148(12) 0.0242(13) 0.0340(15) -0.0078(11) -0.0015(11) -0.0039(10) C23 0.0177(12) 0.0185(11) 0.0151(12) -0.0017(9) -0.0011(9) 0.0001(9) C24 0.0272(14) 0.0261(13) 0.0160(12) -0.0015(10) -0.0043(10) 0.0031(11) C25 0.0196(12) 0.0241(12) 0.0165(12) 0.0007(10) 0.0011(10) -0.0013(10) C26 0.0204(12) 0.0136(11) 0.0201(12) -0.0002(9) -0.0034(10) 0.0005(9) C27 0.0250(13) 0.0157(11) 0.0230(13) 0.0000(10) -0.0020(10) 0.0040(10) C28 0.0210(12) 0.0159(11) 0.0305(14) 0.0003(10) -0.0038(11) -0.0019(9) C29 0.0175(11) 0.0105(10) 0.0218(12) -0.0006(9) 0.0003(10) -0.0017(9) C30 0.0298(14) 0.0139(11) 0.0228(13) 0.0001(10) 0.0026(11) -0.0019(10) C31 0.0253(13) 0.0151(11) 0.0251(13) -0.0045(10) -0.0029(11) -0.0021(10) C32 0.0205(12) 0.0142(11) 0.0151(11) -0.0018(9) -0.0033(9) 0.0003(9) C33 0.0259(13) 0.0182(12) 0.0146(12) -0.0015(9) 0.0016(10) 0.0017(10) C34 0.0278(13) 0.0192(12) 0.0199(13) -0.0058(10) -0.0062(10) 0.0004(10) C35 0.0136(11) 0.0162(11) 0.0197(12) -0.0021(9) 0.0012(9) 0.0003(9) C36 0.0180(12) 0.0183(11) 0.0196(12) -0.0046(9) 0.0014(10) -0.0006(9) C37 0.0180(12) 0.0215(12) 0.0264(14) -0.0010(10) -0.0018(10) 0.0026(10) Cl1 0.0299(4) 0.0374(4) 0.0641(6) 0.0015(4) -0.0016(4) -0.0078(3) Cl2 0.0444(5) 0.0454(5) 0.0465(5) 0.0038(4) 0.0172(4) 0.0031(4) C100 0.0356(16) 0.0298(15) 0.0347(16) -0.0081(12) 0.0071(13) -0.0045(12) _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 C10 1.831(3) . ? Ru1 C1 2.047(2) . ? Ru1 N1 2.209(2) . ? Ru1 P2 2.4285(10) . ? Ru1 P1 2.4520(11) . ? Ru1 S1 2.5238(10) . ? S1 C11 1.719(2) . ? O1 C10 1.154(3) . ? C1 C2 1.345(3) . ? C1 H1A 0.9500 . ? P1 C20 1.863(2) . ? P1 C23 1.864(2) . ? P1 C26 1.882(2) . ? N1 C11 1.345(3) . ? N1 C19 1.381(3) . ? F1 C9 1.347(3) . ? P2 C32 1.863(3) . ? P2 C35 1.864(2) . ? P2 C29 1.887(2) . ? C2 C3 1.470(3) . ? C2 H2A 0.9500 . ? F3 C9 1.347(3) . ? C3 C8 1.405(3) . ? C3 C4 1.408(3) . ? F2 C9 1.341(3) . ? C4 C5 1.381(4) . ? C4 H4A 0.9500 . ? C5 C6 1.396(4) . ? C5 H5A 0.9500 . ? C6 C7 1.392(4) . ? C6 C9 1.489(3) . ? C7 C8 1.383(3) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C19 C18 1.411(3) . ? C19 C14 1.424(3) . ? C18 C17 1.374(3) . ? C18 H11A 0.9500 . ? C17 C16 1.417(4) . ? C17 H12A 0.9500 . ? C16 C15 1.363(4) . ? C16 H13A 0.9500 . ? C15 C14 1.416(3) . ? C15 H14A 0.9500 . ? C14 C13 1.428(4) . ? C13 C12 1.358(4) . ? C13 H16A 0.9500 . ? C12 C11 1.426(3) . ? C12 H17A 0.9500 . ? C20 C22 1.530(3) . ? C20 C21 1.539(3) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.534(3) . ? C23 C25 1.536(3) . ? C23 H23A 1.0000 . ? 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 C28 1.533(3) . ? C26 C27 1.538(3) . ? C26 H26A 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.541(3) . ? C29 C30 1.543(3) . ? C29 H29A 1.0000 . ? 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 C34 1.533(4) . ? C32 C33 1.538(3) . ? C32 H32A 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.534(3) . ? C35 C37 1.536(3) . ? C35 H35A 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? Cl1 C100 1.752(3) . ? Cl2 C100 1.763(3) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Ru1 C1 90.05(10) . . ? C10 Ru1 N1 104.78(9) . . ? C1 Ru1 N1 164.32(8) . . ? C10 Ru1 P2 87.98(8) . . ? C1 Ru1 P2 87.96(7) . . ? N1 Ru1 P2 97.46(6) . . ? C10 Ru1 P1 95.77(8) . . ? C1 Ru1 P1 85.97(7) . . ? N1 Ru1 P1 87.48(6) . . ? P2 Ru1 P1 172.86(2) . . ? C10 Ru1 S1 167.87(8) . . ? C1 Ru1 S1 100.62(7) . . ? N1 Ru1 S1 65.22(6) . . ? P2 Ru1 S1 86.67(3) . . ? P1 Ru1 S1 90.76(3) . . ? C11 S1 Ru1 80.26(9) . . ? C2 C1 Ru1 133.11(18) . . ? C2 C1 H1A 113.4 . . ? Ru1 C1 H1A 113.4 . . ? C20 P1 C23 101.22(12) . . ? C20 P1 C26 101.23(11) . . ? C23 P1 C26 107.76(11) . . ? C20 P1 Ru1 115.00(9) . . ? C23 P1 Ru1 113.13(8) . . ? C26 P1 Ru1 116.77(9) . . ? C11 N1 C19 119.6(2) . . ? C11 N1 Ru1 101.35(15) . . ? C19 N1 Ru1 138.32(16) . . ? C32 P2 C35 101.31(11) . . ? C32 P2 C29 101.23(11) . . ? C35 P2 C29 107.64(11) . . ? C32 P2 Ru1 114.75(8) . . ? C35 P2 Ru1 115.55(8) . . ? C29 P2 Ru1 114.63(8) . . ? C1 C2 C3 125.8(2) . . ? C1 C2 H2A 117.1 . . ? C3 C2 H2A 117.1 . . ? C8 C3 C4 117.1(2) . . ? C8 C3 C2 123.6(2) . . ? C4 C3 C2 119.2(2) . . ? C5 C4 C3 121.4(2) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C4 C5 C6 120.0(2) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C7 C6 C5 119.7(2) . . ? C7 C6 C9 120.3(2) . . ? C5 C6 C9 119.9(2) . . ? C8 C7 C6 119.8(2) . . ? C8 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? C7 C8 C3 121.8(2) . . ? C7 C8 H8A 119.1 . . ? C3 C8 H8A 119.1 . . ? F2 C9 F1 106.0(2) . . ? F2 C9 F3 105.8(2) . . ? F1 C9 F3 105.5(2) . . ? F2 C9 C6 112.4(2) . . ? F1 C9 C6 113.3(2) . . ? F3 C9 C6 113.2(2) . . ? N1 C19 C18 120.2(2) . . ? N1 C19 C14 120.8(2) . . ? C18 C19 C14 119.1(2) . . ? C17 C18 C19 120.6(2) . . ? C17 C18 H11A 119.7 . . ? C19 C18 H11A 119.7 . . ? C18 C17 C16 120.3(2) . . ? C18 C17 H12A 119.8 . . ? C16 C17 H12A 119.8 . . ? C15 C16 C17 120.0(2) . . ? C15 C16 H13A 120.0 . . ? C17 C16 H13A 120.0 . . ? C16 C15 C14 121.0(2) . . ? C16 C15 H14A 119.5 . . ? C14 C15 H14A 119.5 . . ? C15 C14 C19 118.9(2) . . ? C15 C14 C13 123.0(2) . . ? C19 C14 C13 118.1(2) . . ? C12 C13 C14 120.1(2) . . ? C12 C13 H16A 119.9 . . ? C14 C13 H16A 119.9 . . ? C13 C12 C11 119.4(2) . . ? C13 C12 H17A 120.3 . . ? C11 C12 H17A 120.3 . . ? N1 C11 C12 121.9(2) . . ? N1 C11 S1 113.05(17) . . ? C12 C11 S1 125.04(18) . . ? O1 C10 Ru1 175.7(2) . . ? C22 C20 C21 110.0(2) . . ? C22 C20 P1 113.47(17) . . ? C21 C20 P1 112.63(18) . . ? C22 C20 H20A 106.8 . . ? C21 C20 H20A 106.8 . . ? P1 C20 H20A 106.8 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C25 109.5(2) . . ? C24 C23 P1 115.42(17) . . ? C25 C23 P1 115.36(18) . . ? C24 C23 H23A 105.1 . . ? C25 C23 H23A 105.1 . . ? P1 C23 H23A 105.1 . . ? 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 . . ? C28 C26 C27 108.0(2) . . ? C28 C26 P1 113.83(17) . . ? C27 C26 P1 116.27(18) . . ? C28 C26 H26A 106.0 . . ? C27 C26 H26A 106.0 . . ? P1 C26 H26A 106.0 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C30 107.43(19) . . ? C31 C29 P2 114.53(17) . . ? C30 C29 P2 116.34(18) . . ? C31 C29 H29A 105.9 . . ? C30 C29 H29A 105.9 . . ? P2 C29 H29A 105.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C33 111.2(2) . . ? C34 C32 P2 114.54(17) . . ? C33 C32 P2 110.16(18) . . ? C34 C32 H32A 106.8 . . ? C33 C32 H32A 106.8 . . ? P2 C32 H32A 106.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C37 110.48(19) . . ? C36 C35 P2 114.58(17) . . ? C37 C35 P2 115.15(17) . . ? C36 C35 H35A 105.2 . . ? C37 C35 H35A 105.2 . . ? P2 C35 H35A 105.2 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Cl1 C100 Cl2 111.69(17) . . ? Cl1 C100 H10A 109.3 . . ? Cl2 C100 H10A 109.3 . . ? Cl1 C100 H10B 109.3 . . ? Cl2 C100 H10B 109.3 . . ? H10A C100 H10B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.86 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.464 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.070 #===END