# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2065 data_6c _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C28 H31 Cl N2 O P Ru.Cl.[C H Cl3]0.5' _chemical_formula_structural 'C28.50 H31.50 Cl3.50 N2 O P Ru' _chemical_formula_analytical 'C28.50 H31.50 Cl3.50 N2 O P Ru' _chemical_formula_sum 'C28.50 H31.50 Cl3.50 N2 O P Ru' _chemical_formula_weight 674.17 _chemical_melting_point - _chemical_compound_source - loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0689(7) _cell_length_b 12.2999(8) _cell_length_c 23.989(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.8250(10) _cell_angle_gamma 90.00 _cell_volume 3184.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 84 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method - _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 0.859 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.856166 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; - ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 18840 _diffrn_reflns_av_R_equivalents 0.1712 _diffrn_reflns_av_sigmaI/netI 0.2870 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.70 _reflns_number_total 7483 _reflns_number_observed 2761 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 56 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7427 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2119 _refine_ls_R_factor_obs 0.0710 _refine_ls_wR_factor_all 0.2502 _refine_ls_wR_factor_obs 0.1391 _refine_ls_goodness_of_fit_all 0.852 _refine_ls_goodness_of_fit_obs 1.118 _refine_ls_restrained_S_all 1.213 _refine_ls_restrained_S_obs 1.118 _refine_ls_shift/esd_max 0.050 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.42489(6) 0.85660(5) 0.19935(3) 0.0370(2) Uani 1 d . . Cl1 Cl 0.2595(2) 0.7713(2) 0.23178(10) 0.0581(6) Uani 1 d . . N1 N 0.3484(6) 0.7711(5) 0.1208(3) 0.043(2) Uani 1 d . . C2 C 0.4038(8) 0.7015(6) 0.0932(3) 0.046(2) Uani 1 d . . C3 C 0.3602(10) 0.6835(7) 0.0329(4) 0.057(2) Uani 1 d . . O3 O 0.4333(7) 0.6141(6) 0.0103(3) 0.083(2) Uani 1 d . . H3 H 0.3939(34) 0.5905(72) -0.0204(24) 0.124 Uiso 1 calc R . C4 C 0.2571(9) 0.7305(7) 0.0047(4) 0.065(3) Uani 1 d . . H4A H 0.2287(9) 0.7200(7) -0.0344(4) 0.078 Uiso 1 calc R . C5 C 0.1917(9) 0.7969(7) 0.0357(4) 0.070(3) Uani 1 d . . H5A H 0.1164(9) 0.8278(7) 0.0178(4) 0.084 Uiso 1 calc R . C6 C 0.2393(9) 0.8150(7) 0.0916(4) 0.062(3) Uani 1 d . . H6A H 0.1956(9) 0.8598(7) 0.1113(4) 0.074 Uiso 1 calc R . N7 N 0.5039(6) 0.6441(5) 0.1217(3) 0.049(2) Uani 1 d . . H7 H 0.5654(6) 0.6338(5) 0.1059(3) 0.059 Uiso 1 calc R . C8 C 0.5090(8) 0.6003(6) 0.1778(3) 0.049(2) Uani 1 d . . H8A H 0.5718(8) 0.5440(6) 0.1860(3) 0.059 Uiso 1 calc R . H8B H 0.4298(8) 0.5675(6) 0.1789(3) 0.059 Uiso 1 calc R . P1 P 0.5450(2) 0.70682(15) 0.23222(8) 0.0380(5) Uani 1 d . . C9 C 0.5224(7) 0.6423(6) 0.2977(3) 0.041(2) Uani 1 d . . C10 C 0.4925(9) 0.7041(7) 0.3411(3) 0.059(3) Uani 1 d . . H10A H 0.4839(9) 0.7791(7) 0.3371(3) 0.071 Uiso 1 calc R . C11 C 0.4757(9) 0.6540(8) 0.3897(3) 0.061(3) Uani 1 d . . H11A H 0.4535(9) 0.6962(8) 0.4180(3) 0.073 Uiso 1 calc R . C12 C 0.4899(9) 0.5466(8) 0.3983(4) 0.065(3) Uani 1 d . . H12A H 0.4791(9) 0.5149(8) 0.4320(4) 0.078 Uiso 1 calc R . C13 C 0.5210(8) 0.4842(7) 0.3556(4) 0.059(2) Uani 1 d . . H13A H 0.5300(8) 0.4094(7) 0.3604(4) 0.071 Uiso 1 calc R . C14 C 0.5385(8) 0.5310(6) 0.3068(3) 0.050(2) Uani 1 d . . H14A H 0.5616(8) 0.4881(6) 0.2790(3) 0.060 Uiso 1 calc R . C15 C 0.7113(8) 0.7266(6) 0.2455(4) 0.046(2) Uani 1 d . . C16 C 0.7738(8) 0.7717(6) 0.2971(4) 0.052(2) Uani 1 d . . H16A H 0.7306(8) 0.7874(6) 0.3253(4) 0.063 Uiso 1 calc R . C17 C 0.8973(9) 0.7931(6) 0.3069(4) 0.059(2) Uani 1 d . . H17A H 0.9385(9) 0.8215(6) 0.3419(4) 0.071 Uiso 1 calc R . C18 C 0.9618(9) 0.7725(7) 0.2645(5) 0.071(3) Uani 1 d . . H18A H 1.0458(9) 0.7888(7) 0.2710(5) 0.085 Uiso 1 calc R . C19 C 0.9032(9) 0.7287(7) 0.2137(5) 0.061(3) Uani 1 d . . H19A H 0.9480(9) 0.7130(7) 0.1861(5) 0.073 Uiso 1 calc R . C20 C 0.7776(9) 0.7073(6) 0.2027(4) 0.055(2) Uani 1 d . . H20A H 0.7370(9) 0.6804(6) 0.1672(4) 0.066 Uiso 1 calc R . C21 C 0.4295(9) 0.9966(6) 0.2607(3) 0.048(2) Uani 1 d . . C22 C 0.5513(7) 0.9685(5) 0.2568(3) 0.041(2) Uani 1 d . . H22A H 0.6102(7) 0.9538(5) 0.2901(3) 0.049 Uiso 1 calc R . C23 C 0.5854(8) 0.9623(5) 0.2039(3) 0.042(2) Uani 1 d . . H23A H 0.6656(8) 0.9414(5) 0.2028(3) 0.050 Uiso 1 calc R . C24 C 0.4996(8) 0.9873(6) 0.1516(3) 0.046(2) Uani 1 d . . C25 C 0.3798(8) 1.0210(6) 0.1564(3) 0.049(2) Uani 1 d . . H25A H 0.3228(8) 1.0421(6) 0.1236(3) 0.059 Uiso 1 calc R . C26 C 0.3457(8) 1.0235(6) 0.2071(3) 0.046(2) Uani 1 d . . H26A H 0.2648(8) 1.0434(6) 0.2075(3) 0.055 Uiso 1 calc R . C27 C 0.3911(9) 0.9981(7) 0.3159(4) 0.066(3) Uani 1 d . . H27A H 0.3056(9) 1.0191(7) 0.3097(4) 0.099 Uiso 1 calc R . H27B H 0.4412(9) 1.0494(7) 0.3412(4) 0.099 Uiso 1 calc R . H27C H 0.4017(9) 0.9270(7) 0.3327(4) 0.099 Uiso 1 calc R . C28 C 0.5328(9) 0.9837(7) 0.0934(3) 0.061(3) Uani 1 d . . H28A H 0.4586(9) 0.9612(7) 0.0652(3) 0.073 Uiso 1 calc R . C29 C 0.6348(11) 0.9050(9) 0.0898(4) 0.100(4) Uani 1 d . . H29A H 0.6507(11) 0.9071(9) 0.0520(4) 0.150 Uiso 1 calc R . H29B H 0.6102(11) 0.8328(9) 0.0978(4) 0.150 Uiso 1 calc R . H29C H 0.7086(11) 0.9247(9) 0.1172(4) 0.150 Uiso 1 calc R . C30 C 0.5636(18) 1.0996(9) 0.0790(5) 0.161(8) Uani 1 d . . H30A H 0.4962(18) 1.1468(9) 0.0818(5) 0.241 Uiso 1 calc R . H30B H 0.5766(18) 1.1020(9) 0.0407(5) 0.241 Uiso 1 calc R . H30C H 0.6375(18) 1.1231(9) 0.1053(5) 0.241 Uiso 1 calc R . Cl2 Cl 0.7198(2) 0.4742(2) 0.09929(9) 0.0660(7) Uani 1 d . . C40 C 0.7775(22) 0.6329(15) -0.0091(8) 0.086(8) Uani 0.50 d P . H40A H 0.7346(22) 0.5892(15) 0.0147(8) 0.104 Uiso 0.50 calc PR . Cl3 Cl 0.8435(11) 0.7365(8) 0.0244(4) 0.217(6) Uani 0.50 d P . Cl4 Cl 0.6833(9) 0.6577(11) -0.0774(5) 0.218(5) Uani 0.50 d P . Cl5 Cl 0.8805(11) 0.5617(6) -0.0326(4) 0.211(6) Uani 0.50 d P . 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 0.0370(4) 0.0328(3) 0.0426(4) -0.0065(3) 0.0119(3) 0.0003(3) Cl1 0.0437(14) 0.0555(13) 0.082(2) -0.0062(12) 0.0290(13) -0.0078(10) N1 0.035(4) 0.044(4) 0.049(4) -0.013(3) 0.003(4) -0.002(3) C2 0.042(6) 0.048(5) 0.047(5) -0.003(4) 0.004(5) 0.009(4) C3 0.067(7) 0.062(6) 0.040(6) -0.008(4) 0.009(6) 0.014(5) O3 0.084(5) 0.110(6) 0.051(4) -0.031(4) 0.008(4) 0.034(4) C4 0.070(8) 0.078(7) 0.041(5) -0.015(5) -0.001(6) 0.022(6) C5 0.059(7) 0.073(7) 0.064(7) -0.013(5) -0.018(6) 0.020(5) C6 0.057(7) 0.065(6) 0.055(6) -0.022(5) -0.006(6) 0.013(5) N7 0.049(5) 0.063(4) 0.036(4) -0.014(4) 0.011(4) 0.010(4) C8 0.069(7) 0.041(5) 0.042(5) -0.009(4) 0.019(5) 0.006(4) P1 0.0401(14) 0.0333(11) 0.0427(12) -0.0048(9) 0.0135(11) 0.0004(9) C9 0.038(5) 0.044(5) 0.041(4) 0.002(4) 0.007(4) -0.006(4) C10 0.079(8) 0.057(6) 0.043(5) 0.001(4) 0.016(5) 0.019(5) C11 0.075(7) 0.075(7) 0.036(5) -0.007(5) 0.016(5) 0.010(5) C12 0.069(7) 0.064(7) 0.064(6) 0.014(5) 0.019(6) -0.008(5) C13 0.064(7) 0.048(5) 0.061(6) 0.007(5) 0.004(5) -0.006(4) C14 0.062(6) 0.041(5) 0.050(5) -0.003(4) 0.020(5) -0.004(4) C15 0.052(6) 0.031(4) 0.059(5) 0.011(4) 0.024(5) 0.013(4) C16 0.049(6) 0.053(5) 0.057(6) -0.004(5) 0.016(5) -0.003(4) C17 0.047(6) 0.051(5) 0.076(7) 0.003(5) 0.007(6) -0.011(4) C18 0.052(7) 0.038(5) 0.130(10) 0.023(6) 0.038(8) 0.007(5) C19 0.059(7) 0.045(6) 0.090(8) 0.005(5) 0.042(7) 0.009(5) C20 0.054(6) 0.052(5) 0.064(6) 0.009(4) 0.024(5) 0.022(4) C21 0.079(7) 0.021(4) 0.046(5) -0.003(4) 0.017(5) -0.003(4) C22 0.037(5) 0.033(4) 0.049(5) -0.007(4) 0.002(4) -0.001(4) C23 0.043(5) 0.034(4) 0.052(5) 0.004(4) 0.020(5) -0.006(4) C24 0.051(6) 0.039(5) 0.045(5) -0.003(4) 0.006(5) -0.005(4) C25 0.059(6) 0.039(5) 0.048(5) 0.008(4) 0.007(5) 0.008(4) C26 0.050(6) 0.033(4) 0.053(5) 0.003(4) 0.007(5) 0.005(4) C27 0.093(8) 0.053(5) 0.059(6) -0.013(5) 0.030(6) 0.009(5) C28 0.072(7) 0.071(6) 0.041(5) 0.002(5) 0.018(5) -0.013(5) C29 0.106(10) 0.130(10) 0.082(8) -0.001(7) 0.056(8) 0.020(7) C30 0.320(24) 0.084(9) 0.110(10) 0.001(8) 0.113(14) -0.043(11) Cl2 0.084(2) 0.068(2) 0.0441(13) -0.0079(11) 0.0099(13) 0.0218(13) C40 0.150(22) 0.057(12) 0.080(14) 0.031(11) 0.085(16) -0.002(12) Cl3 0.303(13) 0.234(10) 0.169(7) -0.129(7) 0.169(9) -0.200(10) Cl4 0.088(7) 0.368(15) 0.177(9) 0.105(10) -0.017(6) -0.049(7) Cl5 0.386(15) 0.122(6) 0.194(8) 0.044(6) 0.211(10) 0.107(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.160(6) . ? Ru1 C23 2.184(7) . ? Ru1 C22 2.213(7) . ? Ru1 C24 2.236(7) . ? Ru1 C26 2.256(7) . ? Ru1 C21 2.258(7) . ? Ru1 C25 2.274(7) . ? Ru1 P1 2.306(2) . ? Ru1 Cl1 2.385(2) . ? N1 C2 1.315(9) . ? N1 C6 1.365(10) . ? C2 N7 1.363(10) . ? C2 C3 1.436(11) . ? C3 C4 1.324(11) . ? C3 O3 1.370(9) . ? C4 C5 1.408(11) . ? C5 C6 1.345(11) . ? N7 C8 1.439(9) . ? C8 P1 1.830(7) . ? P1 C15 1.813(9) . ? P1 C9 1.826(7) . ? C9 C10 1.386(10) . ? C9 C14 1.392(10) . ? C10 C11 1.368(11) . ? C11 C12 1.341(11) . ? C12 C13 1.384(11) . ? C13 C14 1.356(10) . ? C15 C16 1.393(11) . ? C15 C20 1.409(10) . ? C16 C17 1.360(11) . ? C17 C18 1.390(12) . ? C18 C19 1.359(12) . ? C19 C20 1.382(12) . ? C21 C22 1.415(11) . ? C21 C26 1.447(11) . ? C21 C27 1.478(10) . ? C22 C23 1.406(10) . ? C23 C24 1.429(10) . ? C24 C25 1.418(11) . ? C24 C28 1.522(10) . ? C25 C26 1.350(10) . ? C28 C29 1.504(13) . ? C28 C30 1.524(12) . ? C40 Cl3 1.59(2) . ? C40 Cl5 1.63(2) . ? C40 Cl4 1.76(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 C23 119.4(2) . . ? N1 Ru1 C22 156.6(2) . . ? C23 Ru1 C22 37.3(3) . . ? N1 Ru1 C24 91.2(3) . . ? C23 Ru1 C24 37.7(3) . . ? C22 Ru1 C24 67.5(3) . . ? N1 Ru1 C26 115.5(3) . . ? C23 Ru1 C26 77.3(3) . . ? C22 Ru1 C26 65.6(3) . . ? C24 Ru1 C26 65.3(3) . . ? N1 Ru1 C21 152.5(3) . . ? C23 Ru1 C21 67.3(3) . . ? C22 Ru1 C21 36.9(3) . . ? C24 Ru1 C21 80.1(3) . . ? C26 Ru1 C21 37.4(3) . . ? N1 Ru1 C25 91.9(3) . . ? C23 Ru1 C25 65.6(3) . . ? C22 Ru1 C25 76.9(3) . . ? C24 Ru1 C25 36.6(3) . . ? C26 Ru1 C25 34.7(3) . . ? C21 Ru1 C25 65.7(3) . . ? N1 Ru1 P1 89.7(2) . . ? C23 Ru1 P1 93.3(2) . . ? C22 Ru1 P1 92.7(2) . . ? C24 Ru1 P1 119.9(2) . . ? C26 Ru1 P1 154.7(2) . . ? C21 Ru1 P1 117.3(2) . . ? C25 Ru1 P1 156.5(2) . . ? N1 Ru1 Cl1 83.7(2) . . ? C23 Ru1 Cl1 156.9(2) . . ? C22 Ru1 Cl1 119.7(2) . . ? C24 Ru1 Cl1 151.8(2) . . ? C26 Ru1 Cl1 91.9(2) . . ? C21 Ru1 Cl1 91.8(2) . . ? C25 Ru1 Cl1 115.6(2) . . ? P1 Ru1 Cl1 87.89(7) . . ? C2 N1 C6 117.2(7) . . ? C2 N1 Ru1 128.3(6) . . ? C6 N1 Ru1 112.7(5) . . ? N1 C2 N7 120.2(7) . . ? N1 C2 C3 121.1(8) . . ? N7 C2 C3 118.7(7) . . ? C4 C3 O3 126.0(8) . . ? C4 C3 C2 120.4(8) . . ? O3 C3 C2 113.6(8) . . ? C3 C4 C5 118.0(8) . . ? C6 C5 C4 119.2(9) . . ? C5 C6 N1 123.6(8) . . ? C2 N7 C8 121.5(6) . . ? N7 C8 P1 110.8(5) . . ? C15 P1 C9 103.6(4) . . ? C15 P1 C8 105.9(4) . . ? C9 P1 C8 104.6(3) . . ? C15 P1 Ru1 116.0(2) . . ? C9 P1 Ru1 117.5(3) . . ? C8 P1 Ru1 108.1(3) . . ? C10 C9 C14 117.7(7) . . ? C10 C9 P1 120.6(6) . . ? C14 C9 P1 121.7(6) . . ? C11 C10 C9 119.6(8) . . ? C12 C11 C10 122.7(8) . . ? C11 C12 C13 118.3(8) . . ? C14 C13 C12 120.6(8) . . ? C13 C14 C9 121.0(8) . . ? C16 C15 C20 118.6(8) . . ? C16 C15 P1 119.6(6) . . ? C20 C15 P1 121.4(7) . . ? C17 C16 C15 120.8(8) . . ? C16 C17 C18 119.9(9) . . ? C19 C18 C17 120.6(9) . . ? C18 C19 C20 120.4(8) . . ? C19 C20 C15 119.5(9) . . ? C22 C21 C26 115.5(7) . . ? C22 C21 C27 121.9(8) . . ? C26 C21 C27 122.6(8) . . ? C22 C21 Ru1 69.8(4) . . ? C26 C21 Ru1 71.2(4) . . ? C27 C21 Ru1 128.6(5) . . ? C23 C22 C21 121.5(8) . . ? C23 C22 Ru1 70.3(4) . . ? C21 C22 Ru1 73.3(4) . . ? C22 C23 C24 121.5(7) . . ? C22 C23 Ru1 72.5(4) . . ? C24 C23 Ru1 73.1(5) . . ? C25 C24 C23 116.2(7) . . ? C25 C24 C28 120.3(8) . . ? C23 C24 C28 123.4(7) . . ? C25 C24 Ru1 73.1(4) . . ? C23 C24 Ru1 69.2(4) . . ? C28 C24 Ru1 129.9(5) . . ? C26 C25 C24 122.2(8) . . ? C26 C25 Ru1 71.9(4) . . ? C24 C25 Ru1 70.2(4) . . ? C25 C26 C21 122.8(8) . . ? C25 C26 Ru1 73.4(4) . . ? C21 C26 Ru1 71.4(4) . . ? C29 C28 C24 114.1(8) . . ? C29 C28 C30 112.4(10) . . ? C24 C28 C30 107.0(7) . . ? Cl3 C40 Cl5 109.0(15) . . ? Cl3 C40 Cl4 116.1(11) . . ? Cl5 C40 Cl4 94.9(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C23 Ru1 N1 C2 58.5(7) . . . . ? C22 Ru1 N1 C2 60.9(10) . . . . ? C24 Ru1 N1 C2 84.9(7) . . . . ? C26 Ru1 N1 C2 148.0(6) . . . . ? C21 Ru1 N1 C2 155.5(6) . . . . ? C25 Ru1 N1 C2 121.5(7) . . . . ? P1 Ru1 N1 C2 -35.0(6) . . . . ? Cl1 Ru1 N1 C2 -123.0(7) . . . . ? C23 Ru1 N1 C6 -105.7(6) . . . . ? C22 Ru1 N1 C6 -103.3(8) . . . . ? C24 Ru1 N1 C6 -79.3(6) . . . . ? C26 Ru1 N1 C6 -16.3(6) . . . . ? C21 Ru1 N1 C6 -8.7(9) . . . . ? C25 Ru1 N1 C6 -42.7(6) . . . . ? P1 Ru1 N1 C6 160.7(6) . . . . ? Cl1 Ru1 N1 C6 72.8(6) . . . . ? C6 N1 C2 N7 -171.4(8) . . . . ? Ru1 N1 C2 N7 25.0(11) . . . . ? C6 N1 C2 C3 8.0(12) . . . . ? Ru1 N1 C2 C3 -155.6(6) . . . . ? N1 C2 C3 C4 -5.4(14) . . . . ? N7 C2 C3 C4 174.1(9) . . . . ? N1 C2 C3 O3 175.9(8) . . . . ? N7 C2 C3 O3 -4.7(12) . . . . ? O3 C3 C4 C5 177.8(9) . . . . ? C2 C3 C4 C5 -0.8(15) . . . . ? C3 C4 C5 C6 3.7(15) . . . . ? C4 C5 C6 N1 -0.9(15) . . . . ? C2 N1 C6 C5 -5.0(13) . . . . ? Ru1 N1 C6 C5 161.1(8) . . . . ? N1 C2 N7 C8 40.1(11) . . . . ? C3 C2 N7 C8 -139.4(8) . . . . ? C2 N7 C8 P1 -77.3(9) . . . . ? N7 C8 P1 C15 -80.0(6) . . . . ? N7 C8 P1 C9 170.9(6) . . . . ? N7 C8 P1 Ru1 44.9(6) . . . . ? N1 Ru1 P1 C15 117.0(3) . . . . ? C23 Ru1 P1 C15 -2.4(4) . . . . ? C22 Ru1 P1 C15 -39.7(4) . . . . ? C24 Ru1 P1 C15 25.8(4) . . . . ? C26 Ru1 P1 C15 -69.4(6) . . . . ? C21 Ru1 P1 C15 -68.5(4) . . . . ? C25 Ru1 P1 C15 22.9(6) . . . . ? Cl1 Ru1 P1 C15 -159.4(3) . . . . ? N1 Ru1 P1 C9 -119.7(3) . . . . ? C23 Ru1 P1 C9 120.9(4) . . . . ? C22 Ru1 P1 C9 83.6(3) . . . . ? C24 Ru1 P1 C9 149.1(4) . . . . ? C26 Ru1 P1 C9 53.9(6) . . . . ? C21 Ru1 P1 C9 54.8(4) . . . . ? C25 Ru1 P1 C9 146.2(6) . . . . ? Cl1 Ru1 P1 C9 -36.1(3) . . . . ? N1 Ru1 P1 C8 -1.7(3) . . . . ? C23 Ru1 P1 C8 -121.1(3) . . . . ? C22 Ru1 P1 C8 -158.4(3) . . . . ? C24 Ru1 P1 C8 -92.9(4) . . . . ? C26 Ru1 P1 C8 171.9(5) . . . . ? C21 Ru1 P1 C8 172.9(3) . . . . ? C25 Ru1 P1 C8 -95.8(6) . . . . ? Cl1 Ru1 P1 C8 82.0(3) . . . . ? C15 P1 C9 C10 95.3(7) . . . . ? C8 P1 C9 C10 -154.0(7) . . . . ? Ru1 P1 C9 C10 -34.1(8) . . . . ? C15 P1 C9 C14 -82.5(7) . . . . ? C8 P1 C9 C14 28.3(8) . . . . ? Ru1 P1 C9 C14 148.1(6) . . . . ? C14 C9 C10 C11 -2.3(13) . . . . ? P1 C9 C10 C11 179.8(7) . . . . ? C9 C10 C11 C12 1.7(15) . . . . ? C10 C11 C12 C13 -1.0(15) . . . . ? C11 C12 C13 C14 1.0(14) . . . . ? C12 C13 C14 C9 -1.8(13) . . . . ? C10 C9 C14 C13 2.4(12) . . . . ? P1 C9 C14 C13 -179.8(7) . . . . ? C9 P1 C15 C16 -47.4(7) . . . . ? C8 P1 C15 C16 -157.2(6) . . . . ? Ru1 P1 C15 C16 82.9(6) . . . . ? C9 P1 C15 C20 138.9(6) . . . . ? C8 P1 C15 C20 29.1(7) . . . . ? Ru1 P1 C15 C20 -90.7(6) . . . . ? C20 C15 C16 C17 -2.4(11) . . . . ? P1 C15 C16 C17 -176.2(6) . . . . ? C15 C16 C17 C18 1.7(12) . . . . ? C16 C17 C18 C19 -1.5(13) . . . . ? C17 C18 C19 C20 2.2(13) . . . . ? C18 C19 C20 C15 -2.9(12) . . . . ? C16 C15 C20 C19 3.0(11) . . . . ? P1 C15 C20 C19 176.7(6) . . . . ? N1 Ru1 C21 C22 -138.7(6) . . . . ? C23 Ru1 C21 C22 -28.5(4) . . . . ? C22 Ru1 C21 C22 0.000(1) . . . . ? C24 Ru1 C21 C22 -65.5(5) . . . . ? C26 Ru1 C21 C22 -127.5(6) . . . . ? C25 Ru1 C21 C22 -100.9(5) . . . . ? P1 Ru1 C21 C22 53.1(5) . . . . ? Cl1 Ru1 C21 C22 141.7(4) . . . . ? N1 Ru1 C21 C26 -11.2(8) . . . . ? C23 Ru1 C21 C26 99.1(5) . . . . ? C22 Ru1 C21 C26 127.5(6) . . . . ? C24 Ru1 C21 C26 62.0(5) . . . . ? C26 Ru1 C21 C26 0.000(4) . . . . ? C25 Ru1 C21 C26 26.6(4) . . . . ? P1 Ru1 C21 C26 -179.4(4) . . . . ? Cl1 Ru1 C21 C26 -90.8(4) . . . . ? N1 Ru1 C21 C27 106.0(9) . . . . ? C23 Ru1 C21 C27 -143.8(9) . . . . ? C22 Ru1 C21 C27 -115.3(10) . . . . ? C24 Ru1 C21 C27 179.2(9) . . . . ? C26 Ru1 C21 C27 117.2(10) . . . . ? C25 Ru1 C21 C27 143.8(9) . . . . ? P1 Ru1 C21 C27 -62.2(9) . . . . ? Cl1 Ru1 C21 C27 26.4(8) . . . . ? C26 C21 C22 C23 -3.0(10) . . . . ? C27 C21 C22 C23 177.0(7) . . . . ? Ru1 C21 C22 C23 53.3(6) . . . . ? C26 C21 C22 Ru1 -56.3(6) . . . . ? C27 C21 C22 Ru1 123.7(7) . . . . ? Ru1 C21 C22 Ru1 0.0 . . . . ? N1 Ru1 C22 C23 -3.5(9) . . . . ? C23 Ru1 C22 C23 0.000(1) . . . . ? C24 Ru1 C22 C23 -29.5(4) . . . . ? C26 Ru1 C22 C23 -101.5(5) . . . . ? C21 Ru1 C22 C23 -133.5(7) . . . . ? C25 Ru1 C22 C23 -66.8(5) . . . . ? P1 Ru1 C22 C23 91.9(4) . . . . ? Cl1 Ru1 C22 C23 -179.0(4) . . . . ? N1 Ru1 C22 C21 130.0(6) . . . . ? C23 Ru1 C22 C21 133.5(7) . . . . ? C24 Ru1 C22 C21 104.0(5) . . . . ? C26 Ru1 C22 C21 31.9(4) . . . . ? C21 Ru1 C22 C21 0.000(1) . . . . ? C25 Ru1 C22 C21 66.7(5) . . . . ? P1 Ru1 C22 C21 -134.6(4) . . . . ? Cl1 Ru1 C22 C21 -45.5(5) . . . . ? C21 C22 C23 C24 1.9(10) . . . . ? Ru1 C22 C23 C24 56.6(6) . . . . ? C21 C22 C23 Ru1 -54.7(6) . . . . ? Ru1 C22 C23 Ru1 0.0 . . . . ? N1 Ru1 C23 C22 178.4(4) . . . . ? C22 Ru1 C23 C22 0.000(1) . . . . ? C24 Ru1 C23 C22 132.0(7) . . . . ? C26 Ru1 C23 C22 66.1(5) . . . . ? C21 Ru1 C23 C22 28.2(4) . . . . ? C25 Ru1 C23 C22 100.7(5) . . . . ? P1 Ru1 C23 C22 -90.1(4) . . . . ? Cl1 Ru1 C23 C22 2.2(8) . . . . ? N1 Ru1 C23 C24 46.5(5) . . . . ? C22 Ru1 C23 C24 -132.0(6) . . . . ? C24 Ru1 C23 C24 0.000(1) . . . . ? C26 Ru1 C23 C24 -65.8(4) . . . . ? C21 Ru1 C23 C24 -103.8(5) . . . . ? C25 Ru1 C23 C24 -31.3(4) . . . . ? P1 Ru1 C23 C24 137.9(4) . . . . ? Cl1 Ru1 C23 C24 -129.7(5) . . . . ? C22 C23 C24 C25 1.5(10) . . . . ? Ru1 C23 C24 C25 57.7(6) . . . . ? C22 C23 C24 C28 178.9(7) . . . . ? Ru1 C23 C24 C28 -124.9(7) . . . . ? C22 C23 C24 Ru1 -56.3(6) . . . . ? Ru1 C23 C24 Ru1 0.0 . . . . ? N1 Ru1 C24 C25 91.6(5) . . . . ? C23 Ru1 C24 C25 -127.6(7) . . . . ? C22 Ru1 C24 C25 -98.4(5) . . . . ? C26 Ru1 C24 C25 -26.0(5) . . . . ? C21 Ru1 C24 C25 -62.2(5) . . . . ? C25 Ru1 C24 C25 0.000(2) . . . . ? P1 Ru1 C24 C25 -178.1(4) . . . . ? Cl1 Ru1 C24 C25 12.8(7) . . . . ? N1 Ru1 C24 C23 -140.8(4) . . . . ? C23 Ru1 C24 C23 0.000(1) . . . . ? C22 Ru1 C24 C23 29.2(4) . . . . ? C26 Ru1 C24 C23 101.6(5) . . . . ? C21 Ru1 C24 C23 65.4(5) . . . . ? C25 Ru1 C24 C23 127.6(7) . . . . ? P1 Ru1 C24 C23 -50.5(4) . . . . ? Cl1 Ru1 C24 C23 140.4(4) . . . . ? N1 Ru1 C24 C28 -24.1(8) . . . . ? C23 Ru1 C24 C28 116.7(10) . . . . ? C22 Ru1 C24 C28 145.9(9) . . . . ? C26 Ru1 C24 C28 -141.7(9) . . . . ? C21 Ru1 C24 C28 -177.9(9) . . . . ? C25 Ru1 C24 C28 -115.7(10) . . . . ? P1 Ru1 C24 C28 66.2(9) . . . . ? Cl1 Ru1 C24 C28 -102.8(8) . . . . ? C23 C24 C25 C26 -3.7(11) . . . . ? C28 C24 C25 C26 178.8(7) . . . . ? Ru1 C24 C25 C26 52.0(7) . . . . ? C23 C24 C25 Ru1 -55.7(6) . . . . ? C28 C24 C25 Ru1 126.8(7) . . . . ? Ru1 C24 C25 Ru1 0.000(1) . . . . ? N1 Ru1 C25 C26 135.1(5) . . . . ? C23 Ru1 C25 C26 -103.4(6) . . . . ? C22 Ru1 C25 C26 -65.7(5) . . . . ? C24 Ru1 C25 C26 -135.5(8) . . . . ? C26 Ru1 C25 C26 0.000(4) . . . . ? C21 Ru1 C25 C26 -28.5(5) . . . . ? P1 Ru1 C25 C26 -131.3(5) . . . . ? Cl1 Ru1 C25 C26 51.2(6) . . . . ? N1 Ru1 C25 C24 -89.4(5) . . . . ? C23 Ru1 C25 C24 32.1(4) . . . . ? C22 Ru1 C25 C24 69.8(5) . . . . ? C24 Ru1 C25 C24 0.000(2) . . . . ? C26 Ru1 C25 C24 135.5(8) . . . . ? C21 Ru1 C25 C24 107.0(5) . . . . ? P1 Ru1 C25 C24 4.2(9) . . . . ? Cl1 Ru1 C25 C24 -173.3(4) . . . . ? C24 C25 C26 C21 2.7(12) . . . . ? Ru1 C25 C26 C21 53.9(6) . . . . ? C24 C25 C26 Ru1 -51.2(7) . . . . ? Ru1 C25 C26 Ru1 0.000(2) . . . . ? C22 C21 C26 C25 0.8(10) . . . . ? C27 C21 C26 C25 -179.2(7) . . . . ? Ru1 C21 C26 C25 -54.8(7) . . . . ? C22 C21 C26 Ru1 55.6(5) . . . . ? C27 C21 C26 Ru1 -124.4(7) . . . . ? Ru1 C21 C26 Ru1 0.000(2) . . . . ? N1 Ru1 C26 C25 -51.4(6) . . . . ? C23 Ru1 C26 C25 65.3(5) . . . . ? C22 Ru1 C26 C25 102.7(6) . . . . ? C24 Ru1 C26 C25 27.4(5) . . . . ? C21 Ru1 C26 C25 134.2(7) . . . . ? C25 Ru1 C26 C25 0.000(4) . . . . ? P1 Ru1 C26 C25 135.6(5) . . . . ? Cl1 Ru1 C26 C25 -135.3(5) . . . . ? N1 Ru1 C26 C21 174.3(4) . . . . ? C23 Ru1 C26 C21 -69.0(5) . . . . ? C22 Ru1 C26 C21 -31.5(4) . . . . ? C24 Ru1 C26 C21 -106.9(5) . . . . ? C21 Ru1 C26 C21 0.000(4) . . . . ? C25 Ru1 C26 C21 -134.2(7) . . . . ? P1 Ru1 C26 C21 1.3(8) . . . . ? Cl1 Ru1 C26 C21 90.4(4) . . . . ? C25 C24 C28 C29 -154.9(9) . . . . ? C23 C24 C28 C29 27.7(12) . . . . ? Ru1 C24 C28 C29 -62.1(12) . . . . ? C25 C24 C28 C30 80.1(11) . . . . ? C23 C24 C28 C30 -97.2(11) . . . . ? Ru1 C24 C28 C30 173.0(9) . . . . ? _refine_diff_density_max 1.298 _refine_diff_density_min -0.910 _refine_diff_density_rms 0.131 #---END data_6d #------------------------------------------------------------------------------ _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 10.980(2) _cell_length_b 12.228(3) _cell_length_c 24.194(3) _cell_angle_alpha 90 _cell_angle_beta 101.96(2) _cell_angle_gamma 90 _cell_volume 3178(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.0 _cell_measurement_theta_max 8.3 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 717.89 _chemical_formula_analytical 'C29 H32 Cl5 N2 P Ru ' _chemical_formula_sum 'C29 H32 Cl5 N2 P Ru ' _chemical_formula_moiety 'C28 H31 Cl N2 P Ru.Cl.C H Cl3' _chemical_formula_structural 'C29 H32 Cl5 N2 P Ru ' _chemical_compound_source - _exptl_crystal_F_000 1456.00 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.833 _exptl_special_details ; The scan width was (0.79+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 12). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.09 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 -3 -1 -2 -3 -3 -4 -2 0 _diffrn_reflns_number 6198 _reflns_number_total 5873 _reflns_number_gt 2570 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04346 _diffrn_reflns_av_sigmaI/netI 0.130 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.08448 _diffrn_orient_matrix_UB_12 0.02677 _diffrn_orient_matrix_UB_13 -0.01884 _diffrn_orient_matrix_UB_21 0.01636 _diffrn_orient_matrix_UB_22 -0.02239 _diffrn_orient_matrix_UB_23 -0.03754 _diffrn_orient_matrix_UB_31 -0.03553 _diffrn_orient_matrix_UB_32 -0.07396 _diffrn_orient_matrix_UB_33 0.00455 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 116 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 128 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 20 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 4 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.22490(6) 0.34592(5) 0.80022(3) 0.0359(2) 1.000 . Uani d ? Cl(1) 0.0269(2) 0.2617(2) 0.7694(1) 0.0586(7) 1.000 . Uani d ? Cl(2) 0.6240(2) -0.0232(2) 0.8999(1) 0.0741(9) 1.000 . Uani d ? Cl(3) 0.3219(6) -0.1415(4) 0.9555(2) 0.246(3) 1.000 . Uani d ? Cl(4) 0.1770(4) -0.2385(5) 1.0232(2) 0.259(3) 1.000 . Uani d ? Cl(5) 0.0807(5) -0.0702(4) 0.9506(2) 0.247(3) 1.000 . Uani d ? P(1) 0.3121(2) 0.1979(2) 0.76468(9) 0.0397(6) 1.000 . Uani d ? N(1) 0.2272(6) 0.2557(5) 0.8771(3) 0.047(2) 1.000 . Uani d ? N(7) 0.3861(6) 0.1307(5) 0.8736(3) 0.053(2) 1.000 . Uani d ? C(2) 0.3137(7) 0.1861(6) 0.9037(4) 0.050(3) 1.000 . Uani d ? C(3) 0.3339(8) 0.1723(8) 0.9628(4) 0.068(3) 1.000 . Uani d ? C(4) 0.259(1) 0.2214(9) 0.9932(4) 0.081(4) 1.000 . Uani d ? C(5) 0.160(1) 0.2832(9) 0.9640(4) 0.085(4) 1.000 . Uani d ? C(6) 0.1465(8) 0.2993(8) 0.9072(4) 0.070(3) 1.000 . Uani d ? C(8) 0.3331(7) 0.0901(6) 0.8180(4) 0.049(3) 1.000 . Uani d ? C(9) 0.2253(7) 0.1346(6) 0.7009(3) 0.042(2) 1.000 . Uani d ? C(10) 0.2311(7) 0.0219(6) 0.6919(4) 0.052(3) 1.000 . Uani d ? C(11) 0.1640(9) -0.0251(7) 0.6427(5) 0.070(4) 1.000 . Uani d ? C(12) 0.0942(9) 0.0390(8) 0.6017(4) 0.066(3) 1.000 . Uani d ? C(13) 0.0884(9) 0.1477(9) 0.6090(4) 0.077(4) 1.000 . Uani d ? C(14) 0.1538(8) 0.1952(7) 0.6583(4) 0.061(3) 1.000 . Uani d ? C(15) 0.4661(7) 0.2198(6) 0.7490(3) 0.043(3) 1.000 . Uani d ? C(16) 0.5736(7) 0.2010(6) 0.7898(4) 0.051(3) 1.000 . Uani d ? C(17) 0.6885(8) 0.2264(7) 0.7772(4) 0.065(3) 1.000 . Uani d ? C(18) 0.6964(9) 0.2695(8) 0.7260(5) 0.072(4) 1.000 . Uani d ? C(19) 0.5897(9) 0.2886(7) 0.6863(4) 0.064(3) 1.000 . Uani d ? C(20) 0.4745(7) 0.2645(6) 0.6971(4) 0.052(3) 1.000 . Uani d ? C(21) 0.1714(7) 0.4874(6) 0.7422(3) 0.043(3) 1.000 . Uani d ? C(22) 0.2977(7) 0.4615(6) 0.7449(3) 0.042(3) 1.000 . Uani d ? C(23) 0.3815(6) 0.4543(6) 0.7973(3) 0.039(2) 1.000 . Uani d ? C(24) 0.3455(7) 0.4751(6) 0.8483(3) 0.043(3) 1.000 . Uani d ? C(25) 0.2199(8) 0.5082(6) 0.8451(3) 0.047(3) 1.000 . Uani d ? C(26) 0.1354(7) 0.5135(6) 0.7940(4) 0.046(3) 1.000 . Uani d ? C(27) 0.0812(8) 0.4921(7) 0.6874(4) 0.058(3) 1.000 . Uani d ? C(28) 0.4324(8) 0.4696(7) 0.9059(4) 0.057(3) 1.000 . Uani d ? C(29) 0.5446(8) 0.3983(8) 0.9080(4) 0.079(4) 1.000 . Uani d ? C(30) 0.471(1) 0.5849(9) 0.9245(4) 0.117(5) 1.000 . Uani d ? C(40) 0.208(1) -0.121(1) 0.9932(5) 0.106(5) 1.000 . Uani d ? H(3) 0.4009 0.1280 0.9814 0.081 1.000 . Uiso c ? H(4) 0.2735 0.2138 1.0331 0.097 1.000 . Uiso c ? H(5) 0.1017 0.3142 0.9836 0.102 1.000 . Uiso c ? H(6) 0.0787 0.3421 0.8879 0.084 1.000 . Uiso c ? H(7n) 0.4612 0.0875 0.8988 0.070 1.000 . Uiso c ? H(8b) 0.3869 0.0359 0.8082 0.059 1.000 . Uiso c ? H(8a) 0.2543 0.0584 0.8185 0.059 1.000 . Uiso c ? H(10) 0.2815 -0.0228 0.7197 0.063 1.000 . Uiso c ? H(11) 0.1665 -0.1020 0.6376 0.084 1.000 . Uiso c ? H(12) 0.0497 0.0065 0.5678 0.079 1.000 . Uiso c ? H(13) 0.0395 0.1918 0.5805 0.092 1.000 . Uiso c ? H(14) 0.1492 0.2722 0.6629 0.074 1.000 . Uiso c ? H(16) 0.5687 0.1714 0.8256 0.061 1.000 . Uiso c ? H(17) 0.7625 0.2134 0.8047 0.078 1.000 . Uiso c ? H(18) 0.7752 0.2862 0.7179 0.086 1.000 . Uiso c ? H(19) 0.5954 0.3191 0.6508 0.076 1.000 . Uiso c ? H(20) 0.4013 0.2782 0.6693 0.063 1.000 . Uiso c ? H(22) 0.3265 0.4490 0.7110 0.050 1.000 . Uiso c ? H(23) 0.4654 0.4345 0.7980 0.047 1.000 . Uiso c ? H(25) 0.1934 0.5272 0.8788 0.057 1.000 . Uiso c ? H(26) 0.0520 0.5349 0.7934 0.055 1.000 . Uiso c ? H(27a) 0.0515 0.5649 0.6806 0.069 1.000 . Uiso c ? H(27b) 0.1210 0.4698 0.6580 0.069 1.000 . Uiso c ? H(27c) 0.0132 0.4447 0.6886 0.069 1.000 . Uiso c ? H(28) 0.3867 0.4407 0.9318 0.068 1.000 . Uiso c ? H(29b) 0.5188 0.3246 0.9006 0.094 1.000 . Uiso c ? H(29c) 0.5972 0.4030 0.9444 0.094 1.000 . Uiso c ? H(29a) 0.5888 0.4220 0.8804 0.094 1.000 . Uiso c ? H(30b) 0.5408 0.5823 0.9553 0.140 1.000 . Uiso c ? H(30c) 0.4040 0.6211 0.9360 0.140 1.000 . Uiso c ? H(30a) 0.4934 0.6236 0.8940 0.140 1.000 . Uiso c ? H(40) 0.2367 -0.0693 1.0222 0.127 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0364(3) 0.0326(3) 0.0408(4) 0.0037(4) 0.0123(3) 0.0070(4) Cl(1) 0.040(1) 0.056(1) 0.080(2) -0.007(1) 0.013(1) 0.007(1) Cl(2) 0.083(2) 0.083(2) 0.049(2) 0.027(1) 0.000(1) 0.005(1) Cl(3) 0.321(7) 0.223(6) 0.235(6) 0.037(5) 0.155(5) -0.069(5) Cl(4) 0.183(5) 0.254(6) 0.288(7) -0.091(4) -0.070(4) 0.143(5) Cl(5) 0.235(5) 0.169(5) 0.256(6) 0.034(4) -0.138(5) -0.013(4) P(1) 0.040(1) 0.033(1) 0.046(1) 0.0032(9) 0.009(1) 0.004(1) N(1) 0.048(4) 0.046(4) 0.049(5) 0.008(3) 0.017(4) 0.015(4) N(7) 0.056(4) 0.051(5) 0.049(5) 0.018(4) 0.003(4) 0.011(4) C(2) 0.053(5) 0.039(5) 0.056(6) 0.002(4) 0.006(5) 0.018(4) C(3) 0.077(7) 0.070(7) 0.051(6) 0.007(6) 0.001(5) 0.019(6) C(4) 0.116(9) 0.083(8) 0.052(7) 0.013(7) 0.038(7) 0.022(6) C(5) 0.104(9) 0.091(8) 0.075(8) 0.031(7) 0.052(7) 0.028(7) C(6) 0.072(6) 0.075(7) 0.075(7) 0.026(5) 0.044(6) 0.029(6) C(8) 0.050(5) 0.038(5) 0.060(6) 0.005(4) 0.014(4) 0.007(5) C(9) 0.040(4) 0.037(5) 0.052(5) -0.001(4) 0.016(4) -0.001(4) C(10) 0.055(5) 0.038(5) 0.062(6) 0.000(4) 0.008(5) 0.004(5) C(11) 0.073(7) 0.052(6) 0.087(8) -0.019(5) 0.016(6) -0.019(6) C(12) 0.069(7) 0.071(7) 0.058(7) -0.015(6) 0.013(5) -0.014(6) C(13) 0.087(7) 0.086(8) 0.051(6) 0.012(7) -0.002(5) 0.007(7) C(14) 0.078(7) 0.044(5) 0.059(7) 0.003(5) 0.007(5) 0.007(5) C(15) 0.039(5) 0.038(5) 0.053(6) 0.005(4) 0.014(4) -0.007(4) C(16) 0.047(5) 0.040(5) 0.069(6) 0.005(4) 0.019(5) -0.001(5) C(17) 0.044(6) 0.053(6) 0.091(8) 0.005(5) -0.002(5) -0.019(6) C(18) 0.058(7) 0.056(7) 0.110(9) -0.007(5) 0.036(7) -0.024(7) C(19) 0.061(6) 0.059(6) 0.080(7) -0.007(5) 0.037(6) -0.010(6) C(20) 0.047(5) 0.049(5) 0.064(6) 0.000(4) 0.016(5) -0.009(5) C(21) 0.060(5) 0.027(4) 0.044(5) 0.006(4) 0.010(4) 0.008(4) C(22) 0.054(5) 0.034(5) 0.044(5) -0.006(4) 0.025(4) 0.002(4) C(23) 0.038(4) 0.034(5) 0.044(5) -0.005(4) 0.005(4) 0.004(4) C(24) 0.050(5) 0.036(5) 0.047(5) -0.004(4) 0.021(4) -0.004(4) C(25) 0.065(6) 0.044(5) 0.036(5) 0.010(4) 0.016(4) 0.000(4) C(26) 0.051(5) 0.028(4) 0.061(6) 0.011(4) 0.017(5) 0.003(4) C(27) 0.066(6) 0.044(5) 0.057(6) -0.001(5) -0.002(5) 0.008(5) C(28) 0.064(6) 0.056(6) 0.048(6) 0.001(5) 0.007(5) -0.003(5) C(29) 0.068(7) 0.099(9) 0.064(7) 0.005(6) 0.002(5) 0.010(6) C(30) 0.18(1) 0.081(9) 0.060(8) -0.015(8) -0.038(8) -0.004(7) C(40) 0.102(9) 0.11(1) 0.10(1) -0.007(8) -0.015(7) -0.007(8) #------------------------------------------------------------------------------ _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.00000002(2) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 2570 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_all 0.0382 _refine_ls_wR_factor_ref 0.0382 _refine_ls_goodness_of_fit_all 1.635 _refine_ls_goodness_of_fit_ref 1.635 _refine_ls_shift/esd_max 0.0130 _refine_ls_shift/esd_mean 0.0130 _refine_diff_density_min -0.60 _refine_diff_density_max 0.84 #------------------------------------------------------------------------------ _geom_special_details ; - ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) Cl(1) 2.382(2) . . yes Ru(1) P(1) 2.296(2) . . yes Ru(1) N(1) 2.158(6) . . yes Ru(1) C(21) 2.229(7) . . yes Ru(1) C(22) 2.208(7) . . yes Ru(1) C(23) 2.184(7) . . yes Ru(1) C(24) 2.228(7) . . yes Ru(1) C(25) 2.268(7) . . yes Ru(1) C(26) 2.264(7) . . yes Cl(3) C(40) 1.72(1) . . yes Cl(4) C(40) 1.67(1) . . yes Cl(5) C(40) 1.67(1) . . yes P(1) C(8) 1.825(8) . . yes P(1) C(9) 1.811(8) . . yes P(1) C(15) 1.828(7) . . yes N(1) C(2) 1.337(9) . . yes N(1) C(6) 1.367(9) . . yes N(7) C(2) 1.364(9) . . yes N(7) C(8) 1.439(9) . . yes N(7) H(7n) 1.06 . . no C(2) C(3) 1.41(1) . . yes C(3) C(4) 1.35(1) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.39(1) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.37(1) . . yes C(5) H(5) 0.95 . . no C(6) H(6) 0.95 . . no C(8) H(8b) 0.95 . . no C(8) H(8a) 0.95 . . no C(9) C(10) 1.40(1) . . yes C(9) C(14) 1.38(1) . . yes C(10) C(11) 1.39(1) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.37(1) . . yes C(11) H(11) 0.95 . . no C(12) C(13) 1.34(1) . . yes C(12) H(12) 0.95 . . no C(13) C(14) 1.39(1) . . yes C(13) H(13) 0.95 . . no C(14) H(14) 0.95 . . no C(15) C(16) 1.39(1) . . yes C(15) C(20) 1.39(1) . . yes C(16) C(17) 1.39(1) . . yes C(16) H(16) 0.95 . . no C(17) C(18) 1.37(1) . . yes C(17) H(17) 0.95 . . no C(18) C(19) 1.37(1) . . yes C(18) H(18) 0.95 . . no C(19) C(20) 1.38(1) . . yes C(19) H(19) 0.95 . . no C(20) H(20) 0.95 . . no C(21) C(22) 1.41(1) . . yes C(21) C(26) 1.43(1) . . yes C(21) C(27) 1.48(1) . . yes C(22) C(23) 1.41(1) . . yes C(22) H(22) 0.95 . . no C(23) C(24) 1.395(9) . . yes C(23) H(23) 0.95 . . no C(24) C(25) 1.42(1) . . yes C(24) C(28) 1.52(1) . . yes C(25) C(26) 1.38(1) . . yes C(25) H(25) 0.95 . . no C(26) H(26) 0.95 . . no C(27) H(27a) 0.95 . . no C(27) H(27b) 0.95 . . no C(27) H(27c) 0.95 . . no C(28) C(29) 1.50(1) . . yes C(28) C(30) 1.51(1) . . yes C(28) H(28) 0.95 . . no C(29) H(29b) 0.95 . . no C(29) H(29c) 0.95 . . no C(29) H(29a) 0.95 . . no C(30) H(30b) 0.95 . . no C(30) H(30c) 0.95 . . no C(30) H(30a) 0.95 . . no C(40) H(40) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ru(1) P(1) 88.06(8) . . . yes Cl(1) Ru(1) N(1) 84.0(2) . . . yes Cl(1) Ru(1) C(21) 92.0(2) . . . yes Cl(1) Ru(1) C(22) 120.6(2) . . . yes Cl(1) Ru(1) C(23) 157.9(2) . . . yes Cl(1) Ru(1) C(24) 151.1(2) . . . yes Cl(1) Ru(1) C(25) 114.7(2) . . . yes Cl(1) Ru(1) C(26) 90.9(2) . . . yes P(1) Ru(1) N(1) 89.3(2) . . . yes P(1) Ru(1) C(21) 116.9(2) . . . yes P(1) Ru(1) C(22) 92.6(2) . . . yes P(1) Ru(1) C(23) 94.3(2) . . . yes P(1) Ru(1) C(24) 120.4(2) . . . yes P(1) Ru(1) C(25) 157.3(2) . . . yes P(1) Ru(1) C(26) 153.8(2) . . . yes N(1) Ru(1) C(21) 153.4(3) . . . yes N(1) Ru(1) C(22) 155.4(3) . . . yes N(1) Ru(1) C(23) 118.0(3) . . . yes N(1) Ru(1) C(24) 90.7(3) . . . yes N(1) Ru(1) C(25) 91.8(3) . . . yes N(1) Ru(1) C(26) 116.6(3) . . . yes C(21) Ru(1) C(22) 37.1(3) . . . yes C(21) Ru(1) C(23) 67.4(3) . . . yes C(21) Ru(1) C(24) 80.2(3) . . . yes C(21) Ru(1) C(25) 66.0(3) . . . yes C(21) Ru(1) C(26) 37.0(3) . . . yes C(22) Ru(1) C(23) 37.4(3) . . . yes C(22) Ru(1) C(24) 67.2(3) . . . yes C(22) Ru(1) C(25) 77.2(3) . . . yes C(22) Ru(1) C(26) 65.6(3) . . . yes C(23) Ru(1) C(24) 36.9(2) . . . yes C(23) Ru(1) C(25) 65.3(3) . . . yes C(23) Ru(1) C(26) 77.4(3) . . . yes C(24) Ru(1) C(25) 36.9(3) . . . yes C(24) Ru(1) C(26) 66.2(3) . . . yes C(25) Ru(1) C(26) 35.6(3) . . . yes Ru(1) P(1) C(8) 107.8(3) . . . yes Ru(1) P(1) C(9) 118.0(2) . . . yes Ru(1) P(1) C(15) 115.9(2) . . . yes C(8) P(1) C(9) 105.1(4) . . . yes C(8) P(1) C(15) 105.4(4) . . . yes C(9) P(1) C(15) 103.4(3) . . . yes Ru(1) N(1) C(2) 128.4(5) . . . yes Ru(1) N(1) C(6) 111.5(5) . . . yes C(2) N(1) C(6) 117.8(7) . . . yes C(2) N(7) C(8) 120.2(7) . . . yes C(2) N(7) H(7n) 114.3 . . . no C(8) N(7) H(7n) 118.8 . . . no N(1) C(2) N(7) 119.6(8) . . . yes N(1) C(2) C(3) 120.7(8) . . . yes N(7) C(2) C(3) 119.7(8) . . . yes C(2) C(3) C(4) 120.9(9) . . . yes C(2) C(3) H(3) 119.6 . . . no C(4) C(3) H(3) 119.6 . . . no C(3) C(4) C(5) 117.6(9) . . . yes C(3) C(4) H(4) 121.1 . . . no C(5) C(4) H(4) 121.3 . . . no C(4) C(5) C(6) 120.0(9) . . . yes C(4) C(5) H(5) 120.0 . . . no C(6) C(5) H(5) 120.1 . . . no N(1) C(6) C(5) 122.2(8) . . . yes N(1) C(6) H(6) 118.9 . . . no C(5) C(6) H(6) 118.9 . . . no P(1) C(8) N(7) 112.3(5) . . . yes P(1) C(8) H(8b) 108.7 . . . no P(1) C(8) H(8a) 108.8 . . . no N(7) C(8) H(8b) 108.8 . . . no N(7) C(8) H(8a) 108.8 . . . no H(8b) C(8) H(8a) 109.5 . . . no P(1) C(9) C(10) 121.4(6) . . . yes P(1) C(9) C(14) 121.7(6) . . . yes C(10) C(9) C(14) 116.9(8) . . . yes C(9) C(10) C(11) 120.6(8) . . . yes C(9) C(10) H(10) 119.7 . . . no C(11) C(10) H(10) 119.7 . . . no C(10) C(11) C(12) 120.2(8) . . . yes C(10) C(11) H(11) 119.9 . . . no C(12) C(11) H(11) 119.9 . . . no C(11) C(12) C(13) 120.3(9) . . . yes C(11) C(12) H(12) 119.8 . . . no C(13) C(12) H(12) 119.9 . . . no C(12) C(13) C(14) 119.9(9) . . . yes C(12) C(13) H(13) 120.0 . . . no C(14) C(13) H(13) 120.1 . . . no C(9) C(14) C(13) 122.1(8) . . . yes C(9) C(14) H(14) 118.9 . . . no C(13) C(14) H(14) 119.0 . . . no P(1) C(15) C(16) 121.0(6) . . . yes P(1) C(15) C(20) 118.8(6) . . . yes C(16) C(15) C(20) 120.0(7) . . . yes C(15) C(16) C(17) 118.9(8) . . . yes C(15) C(16) H(16) 120.5 . . . no C(17) C(16) H(16) 120.6 . . . no C(16) C(17) C(18) 121.0(9) . . . yes C(16) C(17) H(17) 119.5 . . . no C(18) C(17) H(17) 119.5 . . . no C(17) C(18) C(19) 119.7(9) . . . yes C(17) C(18) H(18) 120.2 . . . no C(19) C(18) H(18) 120.1 . . . no C(18) C(19) C(20) 121.1(9) . . . yes C(18) C(19) H(19) 119.5 . . . no C(20) C(19) H(19) 119.4 . . . no C(15) C(20) C(19) 119.4(8) . . . yes C(15) C(20) H(20) 120.3 . . . no C(19) C(20) H(20) 120.3 . . . no Ru(1) C(21) C(22) 70.6(4) . . . yes Ru(1) C(21) C(26) 72.8(4) . . . yes Ru(1) C(21) C(27) 129.3(6) . . . yes C(22) C(21) C(26) 117.3(7) . . . yes C(22) C(21) C(27) 121.2(7) . . . yes C(26) C(21) C(27) 121.4(7) . . . yes Ru(1) C(22) C(21) 72.3(4) . . . yes Ru(1) C(22) C(23) 70.4(4) . . . yes Ru(1) C(22) H(22) 130.3 . . . no C(21) C(22) C(23) 120.6(7) . . . yes C(21) C(22) H(22) 119.7 . . . no C(23) C(22) H(22) 119.7 . . . no Ru(1) C(23) C(22) 72.2(4) . . . yes Ru(1) C(23) C(24) 73.3(4) . . . yes Ru(1) C(23) H(23) 127.7 . . . no C(22) C(23) C(24) 122.3(7) . . . yes C(22) C(23) H(23) 118.9 . . . no C(24) C(23) H(23) 118.9 . . . no Ru(1) C(24) C(23) 69.9(4) . . . yes Ru(1) C(24) C(25) 73.1(4) . . . yes Ru(1) C(24) C(28) 129.8(6) . . . yes C(23) C(24) C(25) 116.9(7) . . . yes C(23) C(24) C(28) 124.3(7) . . . yes C(25) C(24) C(28) 118.8(7) . . . yes Ru(1) C(25) C(24) 70.0(4) . . . yes Ru(1) C(25) C(26) 72.0(4) . . . yes Ru(1) C(25) H(25) 131.9 . . . no C(24) C(25) C(26) 121.6(7) . . . yes C(24) C(25) H(25) 119.2 . . . no C(26) C(25) H(25) 119.2 . . . no Ru(1) C(26) C(21) 70.1(4) . . . yes Ru(1) C(26) C(25) 72.4(4) . . . yes Ru(1) C(26) H(26) 130.9 . . . no C(21) C(26) C(25) 121.2(7) . . . yes C(21) C(26) H(26) 119.4 . . . no C(25) C(26) H(26) 119.4 . . . no C(21) C(27) H(27a) 109.4 . . . no C(21) C(27) H(27b) 109.5 . . . no C(21) C(27) H(27c) 109.4 . . . no H(27a) C(27) H(27b) 109.5 . . . no H(27a) C(27) H(27c) 109.5 . . . no H(27b) C(27) H(27c) 109.5 . . . no C(24) C(28) C(29) 114.4(7) . . . yes C(24) C(28) C(30) 108.5(7) . . . yes C(24) C(28) H(28) 107.7 . . . no C(29) C(28) C(30) 110.6(8) . . . yes C(29) C(28) H(28) 107.7 . . . no C(30) C(28) H(28) 107.7 . . . no C(28) C(29) H(29b) 109.5 . . . no C(28) C(29) H(29c) 109.5 . . . no C(28) C(29) H(29a) 109.5 . . . no H(29b) C(29) H(29c) 109.5 . . . no H(29b) C(29) H(29a) 109.4 . . . no H(29c) C(29) H(29a) 109.5 . . . no C(28) C(30) H(30b) 109.5 . . . no C(28) C(30) H(30c) 109.5 . . . no C(28) C(30) H(30a) 109.5 . . . no H(30b) C(30) H(30c) 109.5 . . . no H(30b) C(30) H(30a) 109.4 . . . no H(30c) C(30) H(30a) 109.5 . . . no Cl(3) C(40) Cl(4) 109.9(7) . . . yes Cl(3) C(40) Cl(5) 109.6(8) . . . yes Cl(3) C(40) H(40) 108.5 . . . no Cl(4) C(40) Cl(5) 111.7(7) . . . yes Cl(4) C(40) H(40) 108.6 . . . no Cl(5) C(40) H(40) 108.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(18) 3.56(1) . 1_455 no Cl(2) N(7) 3.175(6) . . no Cl(2) C(40) 3.35(1) . 3_657 no Cl(2) C(20) 3.517(9) . 2_646 no Cl(2) C(4) 3.58(1) . 3_657 no Cl(5) C(27) 3.525(9) . 2_546 no C(16) C(22) 3.43(1) . 2_646 no C(17) C(22) 3.29(1) . 2_646 no C(17) C(21) 3.38(1) . 2_646 no #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A 'N(7)' 'H(7n)' 'Cl(2)' '1.06' '2.24' '3.175(6)' '146.5' '.' #---END data_ms1335a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H17 N2 O2 P' _chemical_formula_weight 324.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 8.7043(6) _cell_length_b 10.8681(8) _cell_length_c 17.2011(11) _cell_angle_alpha 90.024(4) _cell_angle_beta 91.491(4) _cell_angle_gamma 100.777(4) _cell_volume 1597.95(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description trapezoid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.183 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.9643 _exptl_absorpt_correction_T_max 0.9819 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 KappaCCD _diffrn_measurement_method '2o phi + omega frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9398 _diffrn_reflns_av_R_equivalents 0.0850 _diffrn_reflns_av_sigmaI/netI 0.1221 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5614 _reflns_number_gt 3657 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _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^)+(0.0450P)^2^+0.4264P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0038(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5614 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 P1 P 0.64656(9) 0.78553(7) 0.13333(4) 0.0217(2) Uani 1 1 d . . . O1 O 0.7537(2) 0.72253(18) 0.18254(11) 0.0265(5) Uani 1 1 d . . . N1 N 0.7307(3) 1.0104(2) 0.20437(15) 0.0252(6) Uani 1 1 d . . . C1 C 0.5932(4) 0.9179(3) 0.18239(18) 0.0249(7) Uani 1 1 d . . . H1A H 0.523(4) 0.962(3) 0.1504(17) 0.036(9) Uiso 1 1 d . . . H1B H 0.538(4) 0.882(3) 0.2287(18) 0.036(9) Uiso 1 1 d . . . P2 P 0.34551(9) 0.23782(7) 0.36670(4) 0.0209(2) Uani 1 1 d . . . O2 O 0.9722(3) 1.16134(19) 0.27095(12) 0.0287(5) Uani 1 1 d . . . H2O H 1.0514 1.2152 0.2835 0.065(14) Uiso 1 1 calc R . . N2 N 0.6279(3) 1.1789(2) 0.15431(14) 0.0278(6) Uani 1 1 d . . . C2 C 0.7392(3) 1.1375(3) 0.19583(16) 0.0222(7) Uani 1 1 d . . . O3 O 0.2345(2) 0.30024(17) 0.31926(11) 0.0247(5) Uani 1 1 d . . . N3 N 0.2603(3) 0.0167(2) 0.29304(15) 0.0250(6) Uani 1 1 d . . . C3 C 0.8663(3) 1.2181(3) 0.23114(16) 0.0222(7) Uani 1 1 d . . . O4 O 0.0201(2) -0.13709(18) 0.22486(12) 0.0261(5) Uani 1 1 d . . . H4O H -0.0549 -0.1920 0.2085 0.035(10) Uiso 1 1 calc R . . N4 N 0.3457(3) -0.1496(2) 0.35602(14) 0.0247(6) Uani 1 1 d . . . C4 C 0.8752(4) 1.3455(3) 0.22543(19) 0.0288(8) Uani 1 1 d . . . H4 H 0.958(3) 1.398(3) 0.2489(15) 0.012(7) Uiso 1 1 d . . . C5 C 0.7573(4) 1.3901(3) 0.18339(19) 0.0328(8) Uani 1 1 d . . . H5 H 0.761(4) 1.480(3) 0.1759(17) 0.033(9) Uiso 1 1 d . . . C6 C 0.6387(4) 1.3053(3) 0.14943(19) 0.0329(8) Uani 1 1 d . . . H6 H 0.556(4) 1.332(3) 0.1187(17) 0.032(9) Uiso 1 1 d . . . C7 C 0.7327(3) 0.8397(3) 0.04314(15) 0.0221(7) Uani 1 1 d . . . C8 C 0.7230(4) 0.9561(3) 0.01094(18) 0.0289(8) Uani 1 1 d . . . H8 H 0.662(4) 1.015(3) 0.0405(16) 0.029(8) Uiso 1 1 d . . . C9 C 0.8010(4) 0.9942(3) -0.05714(18) 0.0323(8) Uani 1 1 d . . . H9 H 0.795(4) 1.074(3) -0.0809(17) 0.038(9) Uiso 1 1 d . . . C10 C 0.8876(4) 0.9176(3) -0.09306(17) 0.0297(8) Uani 1 1 d . . . H10 H 0.943(4) 0.944(3) -0.1419(17) 0.031(8) Uiso 1 1 d . . . C11 C 0.8955(4) 0.8021(3) -0.0621(2) 0.0409(9) Uani 1 1 d . . . H11 H 0.960(4) 0.752(3) -0.090(2) 0.052(11) Uiso 1 1 d . . . C12 C 0.8188(4) 0.7623(3) 0.00554(19) 0.0368(9) Uani 1 1 d . . . H12 H 0.817(4) 0.674(3) 0.0264(19) 0.053(10) Uiso 1 1 d . . . C13 C 0.4622(3) 0.6838(3) 0.11381(16) 0.0226(7) Uani 1 1 d . . . C14 C 0.3594(4) 0.7099(3) 0.05528(19) 0.0323(8) Uani 1 1 d . . . H14 H 0.391(4) 0.780(3) 0.0210(17) 0.035(9) Uiso 1 1 d . . . C15 C 0.2124(4) 0.6366(3) 0.0468(2) 0.0395(9) Uani 1 1 d . . . H15 H 0.143(5) 0.656(4) 0.004(2) 0.082(14) Uiso 1 1 d . . . C16 C 0.1673(4) 0.5360(3) 0.0949(2) 0.0371(9) Uani 1 1 d . . . H16 H 0.063(5) 0.483(3) 0.0869(19) 0.054(11) Uiso 1 1 d . . . C17 C 0.2692(4) 0.5058(3) 0.1519(2) 0.0388(9) Uani 1 1 d . . . H17 H 0.241(4) 0.441(3) 0.1824(18) 0.033(9) Uiso 1 1 d . . . C18 C 0.4162(4) 0.5805(3) 0.16149(19) 0.0304(8) Uani 1 1 d . . . H18 H 0.492(4) 0.565(3) 0.2020(19) 0.042(10) Uiso 1 1 d . . . C19 C 0.3983(4) 0.1069(3) 0.31621(19) 0.0246(7) Uani 1 1 d . . . H19A H 0.458(3) 0.141(3) 0.2707(16) 0.025(8) Uiso 1 1 d . . . H19B H 0.463(3) 0.066(3) 0.3504(15) 0.017(7) Uiso 1 1 d . . . C20 C 0.2427(3) -0.1097(3) 0.30834(16) 0.0214(7) Uani 1 1 d . . . C21 C 0.1151(3) -0.1910(3) 0.27318(16) 0.0212(7) Uani 1 1 d . . . C22 C 0.0930(4) -0.3155(3) 0.28957(18) 0.0268(7) Uani 1 1 d . . . H22 H 0.009(3) -0.372(2) 0.2659(14) 0.011(7) Uiso 1 1 d . . . C23 C 0.1999(4) -0.3588(3) 0.34053(19) 0.0315(8) Uani 1 1 d . . . H23 H 0.185(4) -0.445(3) 0.3538(17) 0.037(9) Uiso 1 1 d . . . C24 C 0.3211(4) -0.2740(3) 0.37097(18) 0.0291(8) Uani 1 1 d . . . H24 H 0.390(4) -0.298(3) 0.4065(17) 0.029(8) Uiso 1 1 d . . . C25 C 0.2592(3) 0.1791(2) 0.45658(16) 0.0199(6) Uani 1 1 d . . . C26 C 0.3385(4) 0.1196(3) 0.51248(18) 0.0278(8) Uani 1 1 d . . . H26 H 0.443(4) 0.114(3) 0.5066(19) 0.045(10) Uiso 1 1 d . . . C27 C 0.2642(4) 0.0751(3) 0.58018(18) 0.0297(8) Uani 1 1 d . . . H27 H 0.326(4) 0.033(3) 0.6183(18) 0.036(9) Uiso 1 1 d . . . C28 C 0.1127(4) 0.0891(3) 0.59274(18) 0.0261(7) Uani 1 1 d . . . H28 H 0.067(4) 0.058(3) 0.6377(17) 0.029(8) Uiso 1 1 d . . . C29 C 0.0339(4) 0.1480(3) 0.53778(18) 0.0270(7) Uani 1 1 d . . . H29 H -0.070(4) 0.157(2) 0.5461(15) 0.021(8) Uiso 1 1 d . . . C30 C 0.1067(4) 0.1923(3) 0.47009(17) 0.0250(7) Uani 1 1 d . . . H30 H 0.053(3) 0.231(3) 0.4315(15) 0.019(7) Uiso 1 1 d . . . C31 C 0.5274(3) 0.3443(3) 0.38717(16) 0.0198(6) Uani 1 1 d . . . C32 C 0.6590(4) 0.3071(3) 0.42031(19) 0.0313(8) Uani 1 1 d . . . H32 H 0.656(4) 0.219(3) 0.4335(17) 0.036(9) Uiso 1 1 d . . . C33 C 0.7946(4) 0.3944(3) 0.43479(19) 0.0327(8) Uani 1 1 d . . . H33 H 0.891(4) 0.360(3) 0.4607(19) 0.049(10) Uiso 1 1 d . . . C34 C 0.8003(4) 0.5176(3) 0.41541(19) 0.0325(8) Uani 1 1 d . . . H34 H 0.898(4) 0.578(3) 0.4252(17) 0.034(9) Uiso 1 1 d . . . C35 C 0.6738(4) 0.5561(3) 0.3803(2) 0.0395(9) Uani 1 1 d . . . H35 H 0.683(4) 0.644(3) 0.3623(19) 0.048(10) Uiso 1 1 d . . . C36 C 0.5369(4) 0.4686(3) 0.3662(2) 0.0339(8) Uani 1 1 d . . . H36 H 0.447(4) 0.495(3) 0.3366(18) 0.042(10) Uiso 1 1 d . . . H3N H 0.200(5) 0.031(4) 0.256(2) 0.064(13) Uiso 1 1 d . . . H1N H 0.806(4) 0.994(3) 0.2361(18) 0.031(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0194(5) 0.0211(4) 0.0231(4) 0.0028(3) -0.0002(3) -0.0005(3) O1 0.0231(12) 0.0266(12) 0.0275(11) 0.0043(9) -0.0045(9) -0.0004(9) N1 0.0200(15) 0.0243(15) 0.0299(15) -0.0001(12) -0.0058(12) 0.0016(11) C1 0.0165(17) 0.0265(17) 0.0295(17) -0.0009(14) 0.0007(14) -0.0019(13) P2 0.0177(4) 0.0190(4) 0.0247(4) 0.0030(3) -0.0001(3) 0.0002(3) O2 0.0270(13) 0.0218(11) 0.0368(13) 0.0014(10) -0.0077(10) 0.0039(10) N2 0.0293(16) 0.0262(15) 0.0283(14) 0.0021(12) -0.0011(12) 0.0061(12) C2 0.0235(18) 0.0240(17) 0.0194(15) 0.0027(13) 0.0057(13) 0.0046(13) O3 0.0200(12) 0.0219(11) 0.0301(11) 0.0049(9) -0.0040(9) -0.0007(9) N3 0.0241(16) 0.0186(14) 0.0304(15) -0.0009(11) -0.0050(12) 0.0000(11) C3 0.0206(17) 0.0241(16) 0.0217(15) 0.0033(13) 0.0002(13) 0.0040(13) O4 0.0243(13) 0.0203(11) 0.0320(12) 0.0030(10) -0.0078(10) 0.0007(10) N4 0.0227(15) 0.0233(14) 0.0282(14) 0.0022(11) -0.0014(11) 0.0050(11) C4 0.028(2) 0.0235(18) 0.0333(18) 0.0004(15) 0.0036(16) 0.0010(15) C5 0.034(2) 0.0254(18) 0.0390(19) 0.0080(16) 0.0027(16) 0.0063(15) C6 0.033(2) 0.0301(19) 0.0374(19) 0.0075(16) -0.0019(16) 0.0107(16) C7 0.0227(17) 0.0223(16) 0.0186(15) -0.0007(13) -0.0013(13) -0.0023(13) C8 0.032(2) 0.0288(18) 0.0276(17) 0.0038(15) 0.0011(14) 0.0097(15) C9 0.038(2) 0.0302(19) 0.0285(18) 0.0077(15) 0.0011(15) 0.0052(16) C10 0.030(2) 0.0354(19) 0.0217(17) 0.0037(15) 0.0037(14) -0.0010(15) C11 0.046(2) 0.039(2) 0.041(2) 0.0078(17) 0.0202(18) 0.0126(18) C12 0.044(2) 0.0306(19) 0.038(2) 0.0085(16) 0.0126(17) 0.0112(16) C13 0.0191(17) 0.0233(16) 0.0239(16) -0.0007(13) 0.0012(13) -0.0004(13) C14 0.027(2) 0.0272(18) 0.040(2) 0.0062(16) -0.0041(15) -0.0011(14) C15 0.032(2) 0.041(2) 0.042(2) 0.0023(17) -0.0139(17) -0.0010(17) C16 0.026(2) 0.037(2) 0.043(2) -0.0027(17) -0.0006(16) -0.0073(16) C17 0.036(2) 0.037(2) 0.039(2) 0.0113(18) 0.0046(17) -0.0045(16) C18 0.0249(19) 0.0324(19) 0.0321(18) 0.0034(15) 0.0017(15) 0.0006(15) C19 0.0207(18) 0.0188(16) 0.0331(18) 0.0008(14) 0.0027(15) 0.0003(13) C20 0.0191(17) 0.0217(16) 0.0242(16) -0.0007(13) 0.0033(13) 0.0057(13) C21 0.0228(17) 0.0203(16) 0.0222(15) 0.0023(13) 0.0006(13) 0.0085(13) C22 0.0241(19) 0.0224(17) 0.0323(18) -0.0001(14) -0.0010(15) 0.0002(14) C23 0.036(2) 0.0206(17) 0.0392(19) 0.0092(15) 0.0017(16) 0.0084(15) C24 0.026(2) 0.0301(19) 0.0315(18) 0.0021(15) -0.0044(15) 0.0080(15) C25 0.0186(17) 0.0139(14) 0.0257(16) -0.0024(12) -0.0021(13) -0.0004(12) C26 0.0193(18) 0.0284(18) 0.0357(18) 0.0070(15) 0.0010(14) 0.0041(14) C27 0.030(2) 0.0321(19) 0.0271(17) 0.0049(15) -0.0026(15) 0.0061(14) C28 0.0305(19) 0.0228(17) 0.0240(17) 0.0006(14) 0.0044(14) 0.0018(14) C29 0.0208(19) 0.0286(18) 0.0319(18) -0.0009(14) 0.0025(14) 0.0047(14) C30 0.0229(18) 0.0238(17) 0.0284(17) 0.0025(14) -0.0005(14) 0.0044(13) C31 0.0169(16) 0.0199(16) 0.0213(15) -0.0006(12) -0.0010(12) 0.0000(12) C32 0.028(2) 0.0225(18) 0.042(2) 0.0064(15) -0.0041(15) 0.0009(14) C33 0.0217(19) 0.034(2) 0.041(2) 0.0004(16) -0.0039(15) 0.0018(15) C34 0.0221(19) 0.0267(19) 0.045(2) -0.0067(16) -0.0003(16) -0.0040(15) C35 0.029(2) 0.0214(18) 0.066(2) 0.0053(17) 0.0001(17) -0.0003(15) C36 0.028(2) 0.0269(19) 0.046(2) 0.0041(16) -0.0023(16) 0.0048(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O1 1.501(2) . ? P1 C7 1.792(3) . ? P1 C13 1.794(3) . ? P1 C1 1.807(3) . ? N1 C2 1.378(4) . ? N1 C1 1.453(4) . ? P2 O3 1.5047(19) . ? P2 C25 1.801(3) . ? P2 C19 1.804(3) . ? P2 C31 1.804(3) . ? O2 C3 1.371(3) . ? N2 C2 1.333(4) . ? N2 C6 1.362(4) . ? C2 C3 1.401(4) . ? N3 C20 1.380(4) . ? N3 C19 1.448(4) . ? C3 C4 1.376(4) . ? O4 C21 1.365(3) . ? N4 C20 1.331(4) . ? N4 C24 1.355(4) . ? C4 C5 1.400(4) . ? C5 C6 1.367(5) . ? C7 C12 1.396(4) . ? C7 C8 1.397(4) . ? C8 C9 1.393(4) . ? C9 C10 1.379(5) . ? C10 C11 1.377(4) . ? C11 C12 1.386(4) . ? C13 C14 1.394(4) . ? C13 C18 1.394(4) . ? C14 C15 1.379(5) . ? C15 C16 1.375(5) . ? C16 C17 1.385(5) . ? C17 C18 1.388(5) . ? C20 C21 1.406(4) . ? C21 C22 1.362(4) . ? C22 C23 1.406(4) . ? C23 C24 1.358(5) . ? C25 C30 1.387(4) . ? C25 C26 1.397(4) . ? C26 C27 1.390(4) . ? C27 C28 1.378(4) . ? C28 C29 1.381(4) . ? C29 C30 1.383(4) . ? C31 C36 1.387(4) . ? C31 C32 1.393(4) . ? C32 C33 1.386(4) . ? C33 C34 1.372(4) . ? C34 C35 1.374(5) . ? C35 C36 1.395(5) . ? 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 O1 P1 C7 111.90(13) . . ? O1 P1 C13 111.62(12) . . ? C7 P1 C13 109.25(14) . . ? O1 P1 C1 112.19(14) . . ? C7 P1 C1 107.89(14) . . ? C13 P1 C1 103.60(14) . . ? C2 N1 C1 123.4(3) . . ? N1 C1 P1 111.3(2) . . ? O3 P2 C25 110.90(12) . . ? O3 P2 C19 112.26(14) . . ? C25 P2 C19 107.16(13) . . ? O3 P2 C31 111.19(12) . . ? C25 P2 C31 109.60(13) . . ? C19 P2 C31 105.52(14) . . ? C2 N2 C6 117.1(3) . . ? N2 C2 N1 119.2(3) . . ? N2 C2 C3 122.7(3) . . ? N1 C2 C3 118.0(3) . . ? C20 N3 C19 123.3(3) . . ? O2 C3 C4 124.9(3) . . ? O2 C3 C2 115.9(3) . . ? C4 C3 C2 119.2(3) . . ? C20 N4 C24 116.8(3) . . ? C3 C4 C5 118.6(3) . . ? C6 C5 C4 118.6(3) . . ? N2 C6 C5 123.7(3) . . ? C12 C7 C8 119.2(3) . . ? C12 C7 P1 117.3(2) . . ? C8 C7 P1 123.5(2) . . ? C9 C8 C7 119.9(3) . . ? C10 C9 C8 120.4(3) . . ? C11 C10 C9 119.9(3) . . ? C10 C11 C12 120.7(3) . . ? C11 C12 C7 120.0(3) . . ? C14 C13 C18 119.1(3) . . ? C14 C13 P1 121.6(2) . . ? C18 C13 P1 119.2(2) . . ? C15 C14 C13 120.1(3) . . ? C16 C15 C14 120.4(3) . . ? C15 C16 C17 120.6(3) . . ? C16 C17 C18 119.2(3) . . ? C17 C18 C13 120.6(3) . . ? N3 C19 P2 110.9(2) . . ? N4 C20 N3 119.0(3) . . ? N4 C20 C21 122.8(3) . . ? N3 C20 C21 118.3(3) . . ? C22 C21 O4 124.6(3) . . ? C22 C21 C20 119.1(3) . . ? O4 C21 C20 116.4(2) . . ? C21 C22 C23 118.8(3) . . ? C24 C23 C22 118.2(3) . . ? N4 C24 C23 124.3(3) . . ? C30 C25 C26 118.9(3) . . ? C30 C25 P2 118.3(2) . . ? C26 C25 P2 122.8(2) . . ? C27 C26 C25 119.8(3) . . ? C28 C27 C26 120.6(3) . . ? C27 C28 C29 119.9(3) . . ? C28 C29 C30 120.0(3) . . ? C29 C30 C25 120.9(3) . . ? C36 C31 C32 118.8(3) . . ? C36 C31 P2 117.7(2) . . ? C32 C31 P2 123.4(2) . . ? C33 C32 C31 120.2(3) . . ? C34 C33 C32 120.0(3) . . ? C33 C34 C35 121.0(3) . . ? C34 C35 C36 119.1(3) . . ? C31 C36 C35 120.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 P1 137.5(2) . . . . ? O1 P1 C1 N1 58.3(2) . . . . ? C7 P1 C1 N1 -65.4(2) . . . . ? C13 P1 C1 N1 178.8(2) . . . . ? C6 N2 C2 N1 178.1(3) . . . . ? C6 N2 C2 C3 -2.3(4) . . . . ? C1 N1 C2 N2 -11.3(4) . . . . ? C1 N1 C2 C3 169.1(3) . . . . ? N2 C2 C3 O2 -179.1(2) . . . . ? N1 C2 C3 O2 0.5(4) . . . . ? N2 C2 C3 C4 2.3(4) . . . . ? N1 C2 C3 C4 -178.1(3) . . . . ? O2 C3 C4 C5 -179.3(3) . . . . ? C2 C3 C4 C5 -0.9(4) . . . . ? C3 C4 C5 C6 -0.3(5) . . . . ? C2 N2 C6 C5 1.0(5) . . . . ? C4 C5 C6 N2 0.3(5) . . . . ? O1 P1 C7 C12 39.7(3) . . . . ? C13 P1 C7 C12 -84.4(3) . . . . ? C1 P1 C7 C12 163.6(3) . . . . ? O1 P1 C7 C8 -137.6(3) . . . . ? C13 P1 C7 C8 98.3(3) . . . . ? C1 P1 C7 C8 -13.7(3) . . . . ? C12 C7 C8 C9 -1.1(5) . . . . ? P1 C7 C8 C9 176.2(3) . . . . ? C7 C8 C9 C10 0.1(5) . . . . ? C8 C9 C10 C11 0.9(5) . . . . ? C9 C10 C11 C12 -0.9(6) . . . . ? C10 C11 C12 C7 -0.1(6) . . . . ? C8 C7 C12 C11 1.1(5) . . . . ? P1 C7 C12 C11 -176.4(3) . . . . ? O1 P1 C13 C14 -164.6(2) . . . . ? C7 P1 C13 C14 -40.3(3) . . . . ? C1 P1 C13 C14 74.5(3) . . . . ? O1 P1 C13 C18 19.6(3) . . . . ? C7 P1 C13 C18 143.9(2) . . . . ? C1 P1 C13 C18 -101.3(3) . . . . ? C18 C13 C14 C15 2.2(5) . . . . ? P1 C13 C14 C15 -173.6(3) . . . . ? C13 C14 C15 C16 -1.3(5) . . . . ? C14 C15 C16 C17 -0.8(6) . . . . ? C15 C16 C17 C18 1.9(6) . . . . ? C16 C17 C18 C13 -0.9(5) . . . . ? C14 C13 C18 C17 -1.1(5) . . . . ? P1 C13 C18 C17 174.8(3) . . . . ? C20 N3 C19 P2 -129.6(2) . . . . ? O3 P2 C19 N3 -56.0(2) . . . . ? C25 P2 C19 N3 66.0(2) . . . . ? C31 P2 C19 N3 -177.2(2) . . . . ? C24 N4 C20 N3 178.2(3) . . . . ? C24 N4 C20 C21 -1.2(4) . . . . ? C19 N3 C20 N4 10.0(4) . . . . ? C19 N3 C20 C21 -170.6(3) . . . . ? N4 C20 C21 C22 1.5(4) . . . . ? N3 C20 C21 C22 -177.9(3) . . . . ? N4 C20 C21 O4 -179.2(2) . . . . ? N3 C20 C21 O4 1.4(4) . . . . ? O4 C21 C22 C23 -179.9(3) . . . . ? C20 C21 C22 C23 -0.7(4) . . . . ? C21 C22 C23 C24 -0.3(5) . . . . ? C20 N4 C24 C23 0.1(5) . . . . ? C22 C23 C24 N4 0.6(5) . . . . ? O3 P2 C25 C30 2.4(3) . . . . ? C19 P2 C25 C30 -120.4(2) . . . . ? C31 P2 C25 C30 125.6(2) . . . . ? O3 P2 C25 C26 -178.4(2) . . . . ? C19 P2 C25 C26 58.8(3) . . . . ? C31 P2 C25 C26 -55.2(3) . . . . ? C30 C25 C26 C27 0.0(5) . . . . ? P2 C25 C26 C27 -179.2(2) . . . . ? C25 C26 C27 C28 0.0(5) . . . . ? C26 C27 C28 C29 -0.1(5) . . . . ? C27 C28 C29 C30 0.3(5) . . . . ? C28 C29 C30 C25 -0.4(5) . . . . ? C26 C25 C30 C29 0.2(5) . . . . ? P2 C25 C30 C29 179.4(2) . . . . ? O3 P2 C31 C36 7.2(3) . . . . ? C25 P2 C31 C36 -115.8(2) . . . . ? C19 P2 C31 C36 129.2(3) . . . . ? O3 P2 C31 C32 -170.6(2) . . . . ? C25 P2 C31 C32 66.4(3) . . . . ? C19 P2 C31 C32 -48.6(3) . . . . ? C36 C31 C32 C33 2.6(5) . . . . ? P2 C31 C32 C33 -179.6(2) . . . . ? C31 C32 C33 C34 -1.0(5) . . . . ? C32 C33 C34 C35 -1.2(5) . . . . ? C33 C34 C35 C36 1.6(5) . . . . ? C32 C31 C36 C35 -2.2(5) . . . . ? P2 C31 C36 C35 179.9(3) . . . . ? C34 C35 C36 C31 0.1(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N O2 0.89(3) 2.18(3) 2.647(4) 112(2) . N1 H1N O4 0.89(3) 2.55(3) 3.241(3) 135(3) 1_665 O2 H2O O3 0.84 1.78 2.606(3) 167.3 1_665 O4 H4O O1 0.84 1.79 2.612(3) 163.8 1_445 N3 H3N O4 0.85(4) 2.23(4) 2.666(3) 112(3) . N3 H3N O2 0.85(4) 2.66(4) 3.214(3) 124(3) 1_445 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.262 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.066 #===END data_sd157a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H54 Cl2 N2 O5 P4 Pt' _chemical_formula_weight 1272.92 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' 'Pt' 'Pt' -1.7033 8.3905 '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 10.9899(5) _cell_length_b 15.8626(8) _cell_length_c 16.8562(11) _cell_angle_alpha 81.161(3) _cell_angle_beta 76.380(3) _cell_angle_gamma 77.645(3) _cell_volume 2773.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 2.793 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.4013 _exptl_absorpt_correction_T_max 0.7676 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 KappaCCD _diffrn_measurement_method '2o phi + omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20959 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12428 _reflns_number_gt 10080 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _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^)+(0.0000P)^2^+32.8860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12428 _refine_ls_number_parameters 689 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1387 _refine_ls_wR_factor_gt 0.1292 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Pt1 Pt 0.51365(3) 0.71778(2) 0.720301(18) 0.02453(11) Uani 1 1 d . . . Cl1 Cl 0.68163(16) 0.62034(12) 0.76797(11) 0.0300(4) Uani 1 1 d . . . P1 P 0.39664(17) 0.61495(13) 0.77808(12) 0.0256(4) Uani 1 1 d . . . O1 O 0.4821(5) 0.7615(4) 1.0060(3) 0.0320(12) Uani 1 1 d . . . N1 N 0.4303(6) 0.6419(4) 0.9261(4) 0.0300(15) Uani 1 1 d . . . C1 C 0.4258(7) 0.5727(5) 0.8816(4) 0.0290(17) Uani 1 1 d . . . H1A H 0.3571 0.5415 0.9123 0.035 Uiso 1 1 calc R . . H1B H 0.5075 0.5310 0.8768 0.035 Uiso 1 1 calc R . . Cl2 Cl 0.66361(16) 0.80665(12) 0.65914(11) 0.0288(4) Uani 1 1 d . . . P2 P 0.58283(19) 0.79648(14) 1.04287(12) 0.0299(4) Uani 1 1 d . . . O2 O 0.5307(6) 0.8401(4) 1.1173(3) 0.0412(14) Uani 1 1 d . . . N2 N 0.3034(6) 0.5867(5) 1.0456(4) 0.0354(16) Uani 1 1 d . . . C2 C 0.3795(7) 0.6425(5) 1.0093(5) 0.0313(18) Uani 1 1 d . . . P3 P 0.35617(17) 0.82198(13) 0.68430(11) 0.0243(4) Uani 1 1 d . . . O3 O 0.6483(5) 0.7787(3) 0.4145(3) 0.0287(12) Uani 1 1 d . . . N3 N 0.4873(6) 0.8653(4) 0.5316(4) 0.0311(15) Uani 1 1 d . . . H3N H 0.5481 0.8228 0.5393 0.037 Uiso 1 1 d R . . C3 C 0.4049(7) 0.7038(5) 1.0527(5) 0.0320(18) Uani 1 1 d . . . P4 P 0.79089(18) 0.74477(13) 0.36708(12) 0.0271(4) Uani 1 1 d . . . O4 O 0.8102(5) 0.7363(4) 0.2793(3) 0.0336(12) Uani 1 1 d . . . N4 N 0.3730(6) 0.9515(4) 0.4380(4) 0.0278(14) Uani 1 1 d . . . C4 C 0.3529(8) 0.7049(6) 1.1350(5) 0.043(2) Uani 1 1 d . . . H4 H 0.3705 0.7451 1.1653 0.051 Uiso 1 1 calc R . . C5 C 0.2746(8) 0.6466(7) 1.1732(5) 0.046(2) Uani 1 1 d . . . H5 H 0.2367 0.6460 1.2300 0.055 Uiso 1 1 calc R . . C6 C 0.2527(8) 0.5889(6) 1.1264(5) 0.043(2) Uani 1 1 d . . . H6 H 0.1990 0.5487 1.1527 0.052 Uiso 1 1 calc R . . C7 C 0.2240(7) 0.6370(5) 0.7955(5) 0.0278(17) Uani 1 1 d . . . C8 C 0.1639(7) 0.6056(5) 0.7446(4) 0.0267(16) Uani 1 1 d . . . H8 H 0.2129 0.5747 0.7000 0.032 Uiso 1 1 calc R . . C9 C 0.0301(7) 0.6202(5) 0.7602(5) 0.0323(18) Uani 1 1 d . . . H9 H -0.0118 0.6000 0.7255 0.039 Uiso 1 1 calc R . . C10 C -0.0402(7) 0.6635(6) 0.8252(5) 0.0350(19) Uani 1 1 d . . . H10 H -0.1306 0.6726 0.8359 0.042 Uiso 1 1 calc R . . C11 C 0.0198(7) 0.6943(6) 0.8758(5) 0.0362(19) Uani 1 1 d . . . H11 H -0.0296 0.7243 0.9208 0.043 Uiso 1 1 calc R . . C12 C 0.1521(7) 0.6812(5) 0.8605(5) 0.0331(18) Uani 1 1 d . . . H12 H 0.1931 0.7027 0.8949 0.040 Uiso 1 1 calc R . . C13 C 0.4443(6) 0.5210(5) 0.7216(4) 0.0251(15) Uani 1 1 d . . . C14 C 0.5114(7) 0.5249(5) 0.6412(5) 0.0295(17) Uani 1 1 d . . . H14 H 0.5366 0.5779 0.6154 0.035 Uiso 1 1 calc R . . C15 C 0.5428(7) 0.4541(6) 0.5975(5) 0.0346(18) Uani 1 1 d . . . H15 H 0.5880 0.4585 0.5420 0.042 Uiso 1 1 calc R . . C16 C 0.5075(7) 0.3753(6) 0.6353(5) 0.0369(19) Uani 1 1 d . . . H16 H 0.5288 0.3258 0.6059 0.044 Uiso 1 1 calc R . . C17 C 0.4410(8) 0.3704(6) 0.7166(5) 0.039(2) Uani 1 1 d . . . H17 H 0.4169 0.3173 0.7428 0.047 Uiso 1 1 calc R . . C18 C 0.4098(7) 0.4422(5) 0.7591(5) 0.0310(17) Uani 1 1 d . . . H18 H 0.3644 0.4380 0.8146 0.037 Uiso 1 1 calc R . . C19 C 0.7039(7) 0.7023(5) 1.0561(4) 0.0287(16) Uani 1 1 d . . . C20 C 0.7236(7) 0.6286(5) 1.0163(5) 0.0326(18) Uani 1 1 d . . . H20 H 0.6706 0.6256 0.9800 0.039 Uiso 1 1 calc R . . C21 C 0.8212(8) 0.5586(5) 1.0294(5) 0.0358(19) Uani 1 1 d . . . H21 H 0.8350 0.5085 1.0016 0.043 Uiso 1 1 calc R . . C22 C 0.8977(7) 0.5623(6) 1.0827(5) 0.0363(19) Uani 1 1 d . . . H22 H 0.9636 0.5147 1.0920 0.044 Uiso 1 1 calc R . . C23 C 0.8780(7) 0.6355(6) 1.1226(5) 0.037(2) Uani 1 1 d . . . H23 H 0.9309 0.6380 1.1590 0.044 Uiso 1 1 calc R . . C24 C 0.7816(7) 0.7052(5) 1.1099(5) 0.0315(17) Uani 1 1 d . . . H24 H 0.7684 0.7550 1.1379 0.038 Uiso 1 1 calc R . . C25 C 0.6506(7) 0.8638(5) 0.9559(5) 0.0327(18) Uani 1 1 d . . . C26 C 0.6700(10) 0.9426(6) 0.9683(6) 0.049(2) Uani 1 1 d . . . H26 H 0.6373 0.9636 1.0205 0.059 Uiso 1 1 calc R . . C27 C 0.7378(11) 0.9921(7) 0.9044(6) 0.057(3) Uani 1 1 d . . . H27 H 0.7502 1.0472 0.9132 0.068 Uiso 1 1 calc R . . C28 C 0.7863(9) 0.9626(6) 0.8298(5) 0.042(2) Uani 1 1 d . . . H28 H 0.8357 0.9956 0.7874 0.050 Uiso 1 1 calc R . . C29 C 0.7639(8) 0.8849(6) 0.8157(5) 0.0373(19) Uani 1 1 d . . . H29 H 0.7956 0.8649 0.7631 0.045 Uiso 1 1 calc R . . C30 C 0.6950(8) 0.8359(5) 0.8782(5) 0.0345(18) Uani 1 1 d . . . H30 H 0.6779 0.7828 0.8680 0.041 Uiso 1 1 calc R . . C31 C 0.4117(7) 0.9048(5) 0.6020(5) 0.0304(18) Uani 1 1 d . . . H31A H 0.3373 0.9458 0.5866 0.036 Uiso 1 1 calc R . . H31B H 0.4627 0.9380 0.6222 0.036 Uiso 1 1 calc R . . C32 C 0.4713(7) 0.8894(5) 0.4527(5) 0.0273(17) Uani 1 1 d . . . C33 C 0.5570(7) 0.8480(5) 0.3891(5) 0.0284(17) Uani 1 1 d . . . C34 C 0.5463(7) 0.8710(5) 0.3085(5) 0.0303(17) Uani 1 1 d . . . H34 H 0.6052 0.8433 0.2651 0.036 Uiso 1 1 calc R . . C35 C 0.4448(7) 0.9368(5) 0.2935(5) 0.0313(18) Uani 1 1 d . . . H35 H 0.4335 0.9562 0.2391 0.038 Uiso 1 1 calc R . . C36 C 0.3626(7) 0.9726(5) 0.3586(5) 0.0296(17) Uani 1 1 d . . . H36 H 0.2922 1.0157 0.3476 0.036 Uiso 1 1 calc R . . C37 C 0.2394(7) 0.7899(5) 0.6408(4) 0.0245(15) Uani 1 1 d . . . C38 C 0.2844(7) 0.7426(5) 0.5736(5) 0.0264(16) Uani 1 1 d . . . H38 H 0.3733 0.7220 0.5570 0.032 Uiso 1 1 calc R . . C39 C 0.2010(7) 0.7249(5) 0.5301(5) 0.0310(17) Uani 1 1 d . . . H39 H 0.2329 0.6928 0.4840 0.037 Uiso 1 1 calc R . . C40 C 0.0729(7) 0.7541(5) 0.5542(5) 0.0333(18) Uani 1 1 d . . . H40 H 0.0159 0.7431 0.5242 0.040 Uiso 1 1 calc R . . C41 C 0.0262(7) 0.7992(5) 0.6217(5) 0.0348(19) Uani 1 1 d . . . H41 H -0.0631 0.8173 0.6391 0.042 Uiso 1 1 calc R . . C42 C 0.1089(7) 0.8186(5) 0.6649(4) 0.0274(16) Uani 1 1 d . . . H42 H 0.0762 0.8514 0.7105 0.033 Uiso 1 1 calc R . . C43 C 0.2750(8) 0.8876(5) 0.7679(5) 0.0307(17) Uani 1 1 d . . . C44 C 0.1945(8) 0.9665(6) 0.7550(5) 0.039(2) Uani 1 1 d . . . H44 H 0.1772 0.9855 0.7019 0.047 Uiso 1 1 calc R . . C45 C 0.1393(12) 1.0176(6) 0.8176(6) 0.059(3) Uani 1 1 d . . . H45 H 0.0837 1.0711 0.8078 0.071 Uiso 1 1 calc R . . C46 C 0.1650(13) 0.9907(7) 0.8952(7) 0.073(4) Uani 1 1 d . . . H46 H 0.1269 1.0254 0.9389 0.088 Uiso 1 1 calc R . . C47 C 0.2464(14) 0.9132(7) 0.9083(7) 0.080(4) Uani 1 1 d . . . H47 H 0.2634 0.8945 0.9616 0.096 Uiso 1 1 calc R . . C48 C 0.3038(11) 0.8623(6) 0.8453(6) 0.054(3) Uani 1 1 d . . . H48 H 0.3626 0.8103 0.8546 0.065 Uiso 1 1 calc R . . C49 C 0.8826(7) 0.8186(5) 0.3847(4) 0.0259(16) Uani 1 1 d . . . C50 C 0.8337(7) 0.8826(5) 0.4365(5) 0.0298(17) Uani 1 1 d . . . H50 H 0.7489 0.8870 0.4678 0.036 Uiso 1 1 calc R . . C51 C 0.9085(7) 0.9411(5) 0.4431(5) 0.0309(17) Uani 1 1 d . . . H51 H 0.8739 0.9865 0.4774 0.037 Uiso 1 1 calc R . . C52 C 1.0324(8) 0.9328(6) 0.3997(5) 0.0360(19) Uani 1 1 d . . . H52 H 1.0835 0.9720 0.4051 0.043 Uiso 1 1 calc R . . C53 C 1.0835(8) 0.8688(6) 0.3488(5) 0.038(2) Uani 1 1 d . . . H53 H 1.1693 0.8637 0.3193 0.046 Uiso 1 1 calc R . . C54 C 1.0092(7) 0.8114(5) 0.3405(5) 0.0329(18) Uani 1 1 d . . . H54 H 1.0439 0.7673 0.3050 0.039 Uiso 1 1 calc R . . C55 C 0.8218(7) 0.6428(5) 0.4289(5) 0.0286(16) Uani 1 1 d . . . C56 C 0.8519(7) 0.5669(5) 0.3903(5) 0.0325(17) Uani 1 1 d . . . H56 H 0.8622 0.5695 0.3325 0.039 Uiso 1 1 calc R . . C57 C 0.8667(7) 0.4875(5) 0.4383(5) 0.0339(18) Uani 1 1 d . . . H57 H 0.8869 0.4354 0.4129 0.041 Uiso 1 1 calc R . . C58 C 0.8524(7) 0.4830(5) 0.5224(5) 0.0345(19) Uani 1 1 d . . . H58 H 0.8627 0.4281 0.5544 0.041 Uiso 1 1 calc R . . C59 C 0.8230(7) 0.5585(5) 0.5600(5) 0.0340(19) Uani 1 1 d . . . H59 H 0.8135 0.5554 0.6178 0.041 Uiso 1 1 calc R . . C60 C 0.8074(6) 0.6390(5) 0.5136(4) 0.0305(17) Uani 1 1 d . . . H60 H 0.7871 0.6908 0.5395 0.037 Uiso 1 1 calc R . . H1N H 0.5207 0.6558 0.9021 0.037 Uiso 1 1 d R . . O1S O 0.0068(6) 1.1332(5) 1.0300(4) 0.103(7) Uani 0.50 1 d PR . . O2S O -0.0851(6) 1.1754(5) 0.8759(4) 0.137(10) Uani 0.50 1 d PR . . 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 Pt1 0.02093(15) 0.03284(17) 0.02263(15) 0.00991(10) -0.01099(10) -0.01315(11) Cl1 0.0224(8) 0.0378(10) 0.0313(10) 0.0112(8) -0.0134(7) -0.0109(7) P1 0.0210(9) 0.0339(10) 0.0244(10) 0.0105(8) -0.0105(8) -0.0135(8) O1 0.026(3) 0.050(3) 0.021(3) 0.007(2) -0.008(2) -0.016(2) N1 0.027(3) 0.045(4) 0.020(3) 0.011(3) -0.007(3) -0.021(3) C1 0.028(4) 0.036(4) 0.025(4) 0.011(3) -0.012(3) -0.015(3) Cl2 0.0242(9) 0.0370(10) 0.0290(9) 0.0098(7) -0.0114(7) -0.0169(7) P2 0.0278(10) 0.0406(12) 0.0236(10) 0.0021(8) -0.0103(8) -0.0100(8) O2 0.042(3) 0.057(4) 0.024(3) 0.000(3) -0.011(3) -0.007(3) N2 0.026(3) 0.049(4) 0.028(4) 0.016(3) -0.010(3) -0.010(3) C2 0.025(4) 0.039(4) 0.028(4) 0.011(3) -0.014(3) -0.004(3) P3 0.0205(9) 0.0337(10) 0.0198(9) 0.0081(8) -0.0071(7) -0.0124(8) O3 0.022(3) 0.030(3) 0.033(3) 0.011(2) -0.012(2) -0.006(2) N3 0.028(3) 0.033(4) 0.030(4) 0.016(3) -0.013(3) -0.007(3) C3 0.024(4) 0.047(5) 0.025(4) 0.009(3) -0.012(3) -0.010(3) P4 0.0247(9) 0.0326(10) 0.0254(10) 0.0064(8) -0.0102(8) -0.0097(8) O4 0.032(3) 0.042(3) 0.028(3) 0.003(2) -0.012(2) -0.009(2) N4 0.025(3) 0.030(3) 0.030(3) 0.013(3) -0.013(3) -0.012(3) C4 0.037(5) 0.067(6) 0.024(4) 0.003(4) -0.004(4) -0.018(4) C5 0.036(5) 0.070(7) 0.025(4) 0.007(4) -0.002(4) -0.011(4) C6 0.031(4) 0.049(5) 0.040(5) 0.021(4) -0.004(4) -0.010(4) C7 0.023(4) 0.034(4) 0.030(4) 0.019(3) -0.016(3) -0.017(3) C8 0.027(4) 0.034(4) 0.022(4) 0.006(3) -0.010(3) -0.014(3) C9 0.022(4) 0.042(5) 0.037(5) 0.015(4) -0.019(3) -0.016(3) C10 0.024(4) 0.050(5) 0.031(4) 0.010(4) -0.011(3) -0.014(4) C11 0.024(4) 0.049(5) 0.031(4) 0.005(4) -0.004(3) -0.009(4) C12 0.026(4) 0.044(5) 0.030(4) 0.008(4) -0.010(3) -0.011(3) C13 0.017(3) 0.034(4) 0.027(4) 0.006(3) -0.008(3) -0.011(3) C14 0.026(4) 0.036(4) 0.029(4) 0.006(3) -0.011(3) -0.012(3) C15 0.026(4) 0.052(5) 0.025(4) 0.004(4) -0.001(3) -0.019(4) C16 0.028(4) 0.047(5) 0.039(5) 0.000(4) -0.007(4) -0.016(4) C17 0.033(4) 0.049(5) 0.037(5) 0.007(4) -0.005(4) -0.022(4) C18 0.030(4) 0.031(4) 0.031(4) 0.004(3) -0.005(3) -0.011(3) C19 0.028(4) 0.043(5) 0.016(3) 0.006(3) -0.005(3) -0.015(3) C20 0.028(4) 0.044(5) 0.028(4) 0.004(3) -0.004(3) -0.018(3) C21 0.035(4) 0.036(4) 0.032(4) 0.009(3) 0.005(3) -0.018(4) C22 0.028(4) 0.043(5) 0.029(4) 0.010(4) -0.002(3) -0.003(3) C23 0.026(4) 0.060(6) 0.023(4) 0.007(4) -0.010(3) -0.009(4) C24 0.035(4) 0.042(5) 0.021(4) 0.007(3) -0.012(3) -0.015(3) C25 0.033(4) 0.040(5) 0.027(4) 0.005(3) -0.014(3) -0.010(3) C26 0.069(7) 0.051(6) 0.031(5) -0.003(4) -0.009(5) -0.022(5) C27 0.088(8) 0.046(6) 0.043(6) 0.001(4) -0.011(5) -0.036(6) C28 0.046(5) 0.053(6) 0.030(5) 0.013(4) -0.015(4) -0.021(4) C29 0.040(5) 0.046(5) 0.026(4) 0.009(4) -0.011(4) -0.012(4) C30 0.038(4) 0.038(5) 0.030(4) 0.005(3) -0.009(4) -0.017(4) C31 0.028(4) 0.037(4) 0.028(4) 0.016(3) -0.013(3) -0.017(3) C32 0.021(4) 0.036(4) 0.028(4) 0.013(3) -0.010(3) -0.019(3) C33 0.025(4) 0.029(4) 0.033(4) 0.010(3) -0.015(3) -0.010(3) C34 0.030(4) 0.039(4) 0.024(4) 0.001(3) -0.009(3) -0.012(3) C35 0.035(4) 0.032(4) 0.032(4) 0.009(3) -0.024(4) -0.007(3) C36 0.025(4) 0.033(4) 0.033(4) 0.010(3) -0.014(3) -0.009(3) C37 0.023(3) 0.033(4) 0.019(3) 0.011(3) -0.010(3) -0.013(3) C38 0.021(3) 0.030(4) 0.029(4) 0.008(3) -0.010(3) -0.008(3) C39 0.038(4) 0.035(4) 0.025(4) 0.006(3) -0.013(3) -0.016(3) C40 0.030(4) 0.041(5) 0.034(4) 0.011(4) -0.018(4) -0.017(3) C41 0.023(4) 0.047(5) 0.035(5) 0.017(4) -0.013(3) -0.014(3) C42 0.026(4) 0.036(4) 0.021(4) 0.006(3) -0.005(3) -0.013(3) C43 0.041(4) 0.037(4) 0.021(4) -0.001(3) -0.009(3) -0.018(4) C44 0.043(5) 0.044(5) 0.028(4) 0.008(4) -0.015(4) -0.003(4) C45 0.094(8) 0.040(5) 0.044(6) -0.007(4) -0.032(6) 0.007(5) C46 0.120(11) 0.059(7) 0.042(6) -0.022(5) -0.039(7) 0.016(7) C47 0.147(12) 0.053(7) 0.043(6) -0.016(5) -0.053(8) 0.018(7) C48 0.085(8) 0.042(5) 0.039(5) 0.004(4) -0.032(5) -0.004(5) C49 0.021(3) 0.035(4) 0.023(4) 0.009(3) -0.011(3) -0.009(3) C50 0.027(4) 0.040(4) 0.025(4) 0.010(3) -0.013(3) -0.012(3) C51 0.038(4) 0.032(4) 0.027(4) 0.001(3) -0.016(3) -0.009(3) C52 0.034(4) 0.043(5) 0.036(5) 0.013(4) -0.017(4) -0.022(4) C53 0.030(4) 0.050(5) 0.033(5) 0.009(4) -0.007(4) -0.015(4) C54 0.027(4) 0.044(5) 0.026(4) 0.004(3) -0.006(3) -0.011(3) C55 0.020(3) 0.040(4) 0.028(4) 0.004(3) -0.010(3) -0.011(3) C56 0.029(4) 0.040(5) 0.031(4) 0.003(3) -0.011(3) -0.010(3) C57 0.031(4) 0.033(4) 0.041(5) 0.004(4) -0.014(4) -0.010(3) C58 0.024(4) 0.040(5) 0.041(5) 0.012(4) -0.011(3) -0.016(3) C59 0.023(4) 0.045(5) 0.034(4) 0.012(4) -0.011(3) -0.011(3) C60 0.017(3) 0.043(5) 0.034(4) 0.001(3) -0.011(3) -0.010(3) O1S 0.052(10) 0.136(17) 0.140(18) 0.007(14) -0.071(12) -0.018(10) O2S 0.133(18) 0.16(2) 0.069(13) 0.055(13) -0.042(13) 0.049(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P3 2.2489(19) . ? Pt1 P1 2.2543(18) . ? Pt1 Cl2 2.3482(16) . ? Pt1 Cl1 2.3534(17) . ? P1 C13 1.807(8) . ? P1 C7 1.815(7) . ? P1 C1 1.846(7) . ? O1 C3 1.405(9) . ? O1 P2 1.617(5) . ? N1 C2 1.383(10) . ? N1 C1 1.435(10) . ? P2 O2 1.463(6) . ? P2 C25 1.786(8) . ? P2 C19 1.800(8) . ? N2 C2 1.328(10) . ? N2 C6 1.347(11) . ? C2 C3 1.409(12) . ? P3 C37 1.812(7) . ? P3 C43 1.823(8) . ? P3 C31 1.846(7) . ? O3 C33 1.409(8) . ? O3 P4 1.601(5) . ? N3 C32 1.368(9) . ? N3 C31 1.425(10) . ? C3 C4 1.372(11) . ? P4 O4 1.468(6) . ? P4 C55 1.797(8) . ? P4 C49 1.797(7) . ? N4 C32 1.340(9) . ? N4 C36 1.353(9) . ? C4 C5 1.381(12) . ? C5 C6 1.386(14) . ? C7 C12 1.382(12) . ? C7 C8 1.401(10) . ? C8 C9 1.406(10) . ? C9 C10 1.370(12) . ? C10 C11 1.389(11) . ? C11 C12 1.391(10) . ? C13 C14 1.382(10) . ? C13 C18 1.398(10) . ? C14 C15 1.376(12) . ? C15 C16 1.402(11) . ? C16 C17 1.392(12) . ? C17 C18 1.377(12) . ? C19 C20 1.389(12) . ? C19 C24 1.395(10) . ? C20 C21 1.400(11) . ? C21 C22 1.383(12) . ? C22 C23 1.381(12) . ? C23 C24 1.387(11) . ? C25 C26 1.367(12) . ? C25 C30 1.390(12) . ? C26 C27 1.395(13) . ? C27 C28 1.359(14) . ? C28 C29 1.372(12) . ? C29 C30 1.383(11) . ? C32 C33 1.394(11) . ? C33 C34 1.377(10) . ? C34 C35 1.397(10) . ? C35 C36 1.359(11) . ? C37 C38 1.388(11) . ? C37 C42 1.390(10) . ? C38 C39 1.396(10) . ? C39 C40 1.368(11) . ? C40 C41 1.373(12) . ? C41 C42 1.397(10) . ? C43 C44 1.389(11) . ? C43 C48 1.393(11) . ? C44 C45 1.374(13) . ? C45 C46 1.387(13) . ? C46 C47 1.378(15) . ? C47 C48 1.382(15) . ? C49 C50 1.378(11) . ? C49 C54 1.405(10) . ? C50 C51 1.397(10) . ? C51 C52 1.375(11) . ? C52 C53 1.371(13) . ? C53 C54 1.387(11) . ? C55 C60 1.393(10) . ? C55 C56 1.397(11) . ? C56 C57 1.389(11) . ? C57 C58 1.381(11) . ? C58 C59 1.382(12) . ? C59 C60 1.390(10) . ? 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 P3 Pt1 P1 98.24(7) . . ? P3 Pt1 Cl2 90.48(6) . . ? P1 Pt1 Cl2 170.86(7) . . ? P3 Pt1 Cl1 173.17(7) . . ? P1 Pt1 Cl1 85.05(6) . . ? Cl2 Pt1 Cl1 86.58(6) . . ? C13 P1 C7 104.2(3) . . ? C13 P1 C1 104.4(3) . . ? C7 P1 C1 102.6(3) . . ? C13 P1 Pt1 111.3(2) . . ? C7 P1 Pt1 122.1(2) . . ? C1 P1 Pt1 110.5(2) . . ? C3 O1 P2 122.4(4) . . ? C2 N1 C1 122.3(6) . . ? N1 C1 P1 111.0(5) . . ? O2 P2 O1 116.2(3) . . ? O2 P2 C25 114.5(4) . . ? O1 P2 C25 101.0(3) . . ? O2 P2 C19 113.2(3) . . ? O1 P2 C19 104.2(3) . . ? C25 P2 C19 106.5(4) . . ? C2 N2 C6 118.0(8) . . ? N2 C2 N1 118.4(7) . . ? N2 C2 C3 121.7(7) . . ? N1 C2 C3 119.9(7) . . ? C37 P3 C43 109.6(4) . . ? C37 P3 C31 100.1(3) . . ? C43 P3 C31 101.9(4) . . ? C37 P3 Pt1 117.8(3) . . ? C43 P3 Pt1 111.8(3) . . ? C31 P3 Pt1 114.0(3) . . ? C33 O3 P4 128.6(5) . . ? C32 N3 C31 125.5(6) . . ? C4 C3 O1 124.5(8) . . ? C4 C3 C2 119.7(7) . . ? O1 C3 C2 115.8(7) . . ? O4 P4 O3 117.1(3) . . ? O4 P4 C55 113.6(4) . . ? O3 P4 C55 98.4(3) . . ? O4 P4 C49 111.5(3) . . ? O3 P4 C49 104.9(3) . . ? C55 P4 C49 110.3(3) . . ? C32 N4 C36 116.7(7) . . ? C3 C4 C5 118.8(9) . . ? C4 C5 C6 118.3(8) . . ? N2 C6 C5 123.5(8) . . ? C12 C7 C8 120.1(7) . . ? C12 C7 P1 120.4(5) . . ? C8 C7 P1 119.5(6) . . ? C7 C8 C9 119.2(8) . . ? C10 C9 C8 120.2(7) . . ? C9 C10 C11 120.5(7) . . ? C10 C11 C12 120.0(8) . . ? C7 C12 C11 120.0(8) . . ? C14 C13 C18 118.4(7) . . ? C14 C13 P1 122.0(6) . . ? C18 C13 P1 119.5(6) . . ? C15 C14 C13 121.7(7) . . ? C14 C15 C16 119.6(8) . . ? C17 C16 C15 119.1(8) . . ? C18 C17 C16 120.4(8) . . ? C17 C18 C13 120.7(8) . . ? C20 C19 C24 119.2(7) . . ? C20 C19 P2 124.0(6) . . ? C24 C19 P2 116.8(6) . . ? C19 C20 C21 120.2(7) . . ? C22 C21 C20 120.0(8) . . ? C23 C22 C21 119.8(8) . . ? C22 C23 C24 120.6(7) . . ? C23 C24 C19 120.2(8) . . ? C26 C25 C30 119.0(8) . . ? C26 C25 P2 118.1(7) . . ? C30 C25 P2 122.7(6) . . ? C25 C26 C27 119.9(9) . . ? C28 C27 C26 120.8(9) . . ? C27 C28 C29 119.8(8) . . ? C28 C29 C30 119.9(8) . . ? C29 C30 C25 120.5(8) . . ? N3 C31 P3 110.8(5) . . ? N4 C32 N3 119.6(7) . . ? N4 C32 C33 121.2(7) . . ? N3 C32 C33 119.2(7) . . ? C34 C33 C32 121.5(7) . . ? C34 C33 O3 123.6(7) . . ? C32 C33 O3 114.8(6) . . ? C33 C34 C35 117.0(8) . . ? C36 C35 C34 118.5(7) . . ? N4 C36 C35 125.1(7) . . ? C38 C37 C42 118.8(6) . . ? C38 C37 P3 117.5(5) . . ? C42 C37 P3 123.3(6) . . ? C37 C38 C39 121.0(7) . . ? C40 C39 C38 119.5(8) . . ? C39 C40 C41 120.4(7) . . ? C40 C41 C42 120.6(7) . . ? C37 C42 C41 119.7(8) . . ? C44 C43 C48 118.7(8) . . ? C44 C43 P3 121.9(6) . . ? C48 C43 P3 119.1(7) . . ? C45 C44 C43 121.4(8) . . ? C44 C45 C46 119.7(9) . . ? C47 C46 C45 119.4(10) . . ? C46 C47 C48 121.1(9) . . ? C47 C48 C43 119.6(9) . . ? C50 C49 C54 119.4(7) . . ? C50 C49 P4 123.4(6) . . ? C54 C49 P4 117.1(6) . . ? C49 C50 C51 120.1(7) . . ? C52 C51 C50 119.6(8) . . ? C53 C52 C51 121.1(7) . . ? C52 C53 C54 119.7(8) . . ? C53 C54 C49 120.0(8) . . ? C60 C55 C56 120.7(7) . . ? C60 C55 P4 121.2(6) . . ? C56 C55 P4 118.0(6) . . ? C57 C56 C55 118.5(8) . . ? C58 C57 C56 121.2(8) . . ? C57 C58 C59 119.8(7) . . ? C58 C59 C60 120.3(8) . . ? C59 C60 C55 119.4(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P3 Pt1 P1 C13 115.8(2) . . . . ? Cl2 Pt1 P1 C13 -46.5(5) . . . . ? Cl1 Pt1 P1 C13 -70.2(2) . . . . ? P3 Pt1 P1 C7 -8.0(3) . . . . ? Cl2 Pt1 P1 C7 -170.3(5) . . . . ? Cl1 Pt1 P1 C7 166.0(3) . . . . ? P3 Pt1 P1 C1 -128.6(3) . . . . ? Cl2 Pt1 P1 C1 69.1(6) . . . . ? Cl1 Pt1 P1 C1 45.4(3) . . . . ? C2 N1 C1 P1 142.1(6) . . . . ? C13 P1 C1 N1 162.2(5) . . . . ? C7 P1 C1 N1 -89.3(6) . . . . ? Pt1 P1 C1 N1 42.4(6) . . . . ? C3 O1 P2 O2 -56.4(7) . . . . ? C3 O1 P2 C25 179.2(6) . . . . ? C3 O1 P2 C19 68.8(6) . . . . ? C6 N2 C2 N1 -178.8(7) . . . . ? C6 N2 C2 C3 -1.5(11) . . . . ? C1 N1 C2 N2 -13.3(10) . . . . ? C1 N1 C2 C3 169.4(7) . . . . ? P1 Pt1 P3 C37 -41.8(3) . . . . ? Cl2 Pt1 P3 C37 135.4(3) . . . . ? Cl1 Pt1 P3 C37 -160.2(6) . . . . ? P1 Pt1 P3 C43 86.4(3) . . . . ? Cl2 Pt1 P3 C43 -96.4(3) . . . . ? Cl1 Pt1 P3 C43 -31.9(7) . . . . ? P1 Pt1 P3 C31 -158.7(3) . . . . ? Cl2 Pt1 P3 C31 18.5(3) . . . . ? Cl1 Pt1 P3 C31 82.9(6) . . . . ? P2 O1 C3 C4 36.0(10) . . . . ? P2 O1 C3 C2 -145.1(6) . . . . ? N2 C2 C3 C4 1.8(11) . . . . ? N1 C2 C3 C4 179.1(7) . . . . ? N2 C2 C3 O1 -177.1(6) . . . . ? N1 C2 C3 O1 0.2(10) . . . . ? C33 O3 P4 O4 -44.5(7) . . . . ? C33 O3 P4 C55 -166.6(6) . . . . ? C33 O3 P4 C49 79.7(6) . . . . ? O1 C3 C4 C5 177.6(7) . . . . ? C2 C3 C4 C5 -1.2(12) . . . . ? C3 C4 C5 C6 0.4(13) . . . . ? C2 N2 C6 C5 0.7(12) . . . . ? C4 C5 C6 N2 -0.1(13) . . . . ? C13 P1 C7 C12 155.6(6) . . . . ? C1 P1 C7 C12 47.0(7) . . . . ? Pt1 P1 C7 C12 -77.4(6) . . . . ? C13 P1 C7 C8 -21.6(6) . . . . ? C1 P1 C7 C8 -130.3(6) . . . . ? Pt1 P1 C7 C8 105.4(5) . . . . ? C12 C7 C8 C9 0.5(10) . . . . ? P1 C7 C8 C9 177.7(5) . . . . ? C7 C8 C9 C10 -1.0(11) . . . . ? C8 C9 C10 C11 0.8(11) . . . . ? C9 C10 C11 C12 0.0(12) . . . . ? C8 C7 C12 C11 0.2(11) . . . . ? P1 C7 C12 C11 -177.0(6) . . . . ? C10 C11 C12 C7 -0.5(12) . . . . ? C7 P1 C13 C14 113.8(6) . . . . ? C1 P1 C13 C14 -138.9(6) . . . . ? Pt1 P1 C13 C14 -19.6(6) . . . . ? C7 P1 C13 C18 -64.5(6) . . . . ? C1 P1 C13 C18 42.8(6) . . . . ? Pt1 P1 C13 C18 162.1(5) . . . . ? C18 C13 C14 C15 1.1(10) . . . . ? P1 C13 C14 C15 -177.2(6) . . . . ? C13 C14 C15 C16 -0.9(11) . . . . ? C14 C15 C16 C17 0.2(11) . . . . ? C15 C16 C17 C18 0.2(12) . . . . ? C16 C17 C18 C13 0.0(12) . . . . ? C14 C13 C18 C17 -0.7(11) . . . . ? P1 C13 C18 C17 177.7(6) . . . . ? O2 P2 C19 C20 146.7(6) . . . . ? O1 P2 C19 C20 19.6(7) . . . . ? C25 P2 C19 C20 -86.6(7) . . . . ? O2 P2 C19 C24 -33.4(7) . . . . ? O1 P2 C19 C24 -160.5(5) . . . . ? C25 P2 C19 C24 93.3(6) . . . . ? C24 C19 C20 C21 -0.7(11) . . . . ? P2 C19 C20 C21 179.2(6) . . . . ? C19 C20 C21 C22 0.7(11) . . . . ? C20 C21 C22 C23 -0.5(11) . . . . ? C21 C22 C23 C24 0.4(12) . . . . ? C22 C23 C24 C19 -0.4(12) . . . . ? C20 C19 C24 C23 0.6(11) . . . . ? P2 C19 C24 C23 -179.3(6) . . . . ? O2 P2 C25 C26 11.8(8) . . . . ? O1 P2 C25 C26 137.4(7) . . . . ? C19 P2 C25 C26 -114.1(7) . . . . ? O2 P2 C25 C30 -174.5(6) . . . . ? O1 P2 C25 C30 -48.9(7) . . . . ? C19 P2 C25 C30 59.6(7) . . . . ? C30 C25 C26 C27 -2.5(14) . . . . ? P2 C25 C26 C27 171.5(8) . . . . ? C25 C26 C27 C28 -0.7(16) . . . . ? C26 C27 C28 C29 2.9(15) . . . . ? C27 C28 C29 C30 -1.8(13) . . . . ? C28 C29 C30 C25 -1.4(12) . . . . ? C26 C25 C30 C29 3.5(12) . . . . ? P2 C25 C30 C29 -170.1(6) . . . . ? C32 N3 C31 P3 130.0(6) . . . . ? C37 P3 C31 N3 -71.7(5) . . . . ? C43 P3 C31 N3 175.6(5) . . . . ? Pt1 P3 C31 N3 55.0(5) . . . . ? C36 N4 C32 N3 179.8(6) . . . . ? C36 N4 C32 C33 -0.8(10) . . . . ? C31 N3 C32 N4 -4.2(10) . . . . ? C31 N3 C32 C33 176.4(6) . . . . ? N4 C32 C33 C34 1.8(11) . . . . ? N3 C32 C33 C34 -178.9(7) . . . . ? N4 C32 C33 O3 -174.4(6) . . . . ? N3 C32 C33 O3 5.0(9) . . . . ? P4 O3 C33 C34 34.1(10) . . . . ? P4 O3 C33 C32 -149.8(5) . . . . ? C32 C33 C34 C35 -0.7(11) . . . . ? O3 C33 C34 C35 175.1(6) . . . . ? C33 C34 C35 C36 -1.3(11) . . . . ? C32 N4 C36 C35 -1.3(11) . . . . ? C34 C35 C36 N4 2.3(12) . . . . ? C43 P3 C37 C38 177.1(5) . . . . ? C31 P3 C37 C38 70.6(6) . . . . ? Pt1 P3 C37 C38 -53.6(6) . . . . ? C43 P3 C37 C42 4.9(7) . . . . ? C31 P3 C37 C42 -101.6(6) . . . . ? Pt1 P3 C37 C42 134.2(5) . . . . ? C42 C37 C38 C39 0.8(10) . . . . ? P3 C37 C38 C39 -171.8(5) . . . . ? C37 C38 C39 C40 -0.4(11) . . . . ? C38 C39 C40 C41 -1.1(11) . . . . ? C39 C40 C41 C42 2.3(11) . . . . ? C38 C37 C42 C41 0.3(10) . . . . ? P3 C37 C42 C41 172.4(5) . . . . ? C40 C41 C42 C37 -1.9(11) . . . . ? C37 P3 C43 C44 -61.8(7) . . . . ? C31 P3 C43 C44 43.5(7) . . . . ? Pt1 P3 C43 C44 165.7(6) . . . . ? C37 P3 C43 C48 124.5(7) . . . . ? C31 P3 C43 C48 -130.1(7) . . . . ? Pt1 P3 C43 C48 -8.0(8) . . . . ? C48 C43 C44 C45 -2.7(14) . . . . ? P3 C43 C44 C45 -176.4(8) . . . . ? C43 C44 C45 C46 0.6(17) . . . . ? C44 C45 C46 C47 0(2) . . . . ? C45 C46 C47 C48 1(2) . . . . ? C46 C47 C48 C43 -3(2) . . . . ? C44 C43 C48 C47 3.7(15) . . . . ? P3 C43 C48 C47 177.6(9) . . . . ? O4 P4 C49 C50 134.0(6) . . . . ? O3 P4 C49 C50 6.3(7) . . . . ? C55 P4 C49 C50 -98.8(6) . . . . ? O4 P4 C49 C54 -43.7(6) . . . . ? O3 P4 C49 C54 -171.5(5) . . . . ? C55 P4 C49 C54 83.5(6) . . . . ? C54 C49 C50 C51 1.7(10) . . . . ? P4 C49 C50 C51 -175.9(5) . . . . ? C49 C50 C51 C52 -2.1(10) . . . . ? C50 C51 C52 C53 1.1(11) . . . . ? C51 C52 C53 C54 0.2(12) . . . . ? C52 C53 C54 C49 -0.5(11) . . . . ? C50 C49 C54 C53 -0.4(11) . . . . ? P4 C49 C54 C53 177.4(6) . . . . ? O4 P4 C55 C60 -179.6(5) . . . . ? O3 P4 C55 C60 -55.1(6) . . . . ? C49 P4 C55 C60 54.3(7) . . . . ? O4 P4 C55 C56 -4.1(7) . . . . ? O3 P4 C55 C56 120.5(6) . . . . ? C49 P4 C55 C56 -130.2(6) . . . . ? C60 C55 C56 C57 0.3(11) . . . . ? P4 C55 C56 C57 -175.3(6) . . . . ? C55 C56 C57 C58 -0.2(11) . . . . ? C56 C57 C58 C59 0.0(11) . . . . ? C57 C58 C59 C60 0.2(11) . . . . ? C58 C59 C60 C55 -0.1(10) . . . . ? C56 C55 C60 C59 -0.2(10) . . . . ? P4 C55 C60 C59 175.2(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N Cl1 1.04 2.58 3.356(7) 131.5 . N3 H3N Cl2 0.86 2.58 3.133(6) 122.9 . _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 6.377 _refine_diff_density_min -3.717 _refine_diff_density_rms 0.197 #===END data_ruppo _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Cl2 N2 O4 P2 Ru' _chemical_formula_weight 846.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3753(3) _cell_length_b 12.8896(3) _cell_length_c 20.6503(5) _cell_angle_alpha 106.031(2) _cell_angle_beta 99.091(2) _cell_angle_gamma 93.886(2) _cell_volume 1850.19(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.8728 _exptl_absorpt_correction_T_max 0.9333 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 KappaCCD _diffrn_measurement_method '2o phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15074 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8461 _reflns_number_gt 7150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed, (Barbour, 1999)' _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^)+(0.0080P)^2^+1.7108P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8461 _refine_ls_number_parameters 621 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.37193(2) 0.593347(13) 0.394667(8) 0.01189(6) Uani 1 1 d . . . Cl1 Cl 0.60138(8) 0.48317(4) 0.34763(3) 0.01611(12) Uani 1 1 d . . . P1 P 0.41295(8) 0.69332(4) 0.31813(3) 0.01216(12) Uani 1 1 d . . . O1 O 0.7412(2) 0.44816(12) 0.16516(8) 0.0209(4) Uani 1 1 d . . . N1 N 0.7210(3) 0.63688(16) 0.25969(9) 0.0159(4) Uani 1 1 d . . . C1 C 0.1654(3) 0.44753(18) 0.36327(12) 0.0191(5) Uani 1 1 d . . . Cl2 Cl 0.62516(7) 0.72044(4) 0.46939(3) 0.01587(12) Uani 1 1 d . . . P2 P 0.67918(9) 0.32438(5) 0.12563(3) 0.02059(14) Uani 1 1 d . . . O2 O 0.8015(3) 0.30538(13) 0.06778(9) 0.0278(4) Uani 1 1 d . . . N2 N 0.6885(3) 0.72901(15) 0.17670(10) 0.0194(4) Uani 1 1 d . . . C2 C 0.0815(3) 0.53589(19) 0.34994(12) 0.0183(5) Uani 1 1 d . . . H2 H 0.020(4) 0.5310(19) 0.3040(13) 0.022(7) Uiso 1 1 d . . . O3 O 0.7820(3) 0.27355(14) 0.17973(9) 0.0297(4) Uani 1 1 d . . . C3 C 0.0925(3) 0.63582(19) 0.40265(12) 0.0191(5) Uani 1 1 d . . . H3 H 0.043(3) 0.6933(19) 0.3918(12) 0.015(6) Uiso 1 1 d . . . O4 O 0.4833(2) 0.28968(13) 0.10176(9) 0.0273(4) Uani 1 1 d . . . C4 C 0.1891(3) 0.64788(18) 0.46994(11) 0.0178(5) Uani 1 1 d . . . C5 C 0.2675(3) 0.55512(19) 0.48307(12) 0.0187(5) Uani 1 1 d . . . H5 H 0.335(4) 0.562(2) 0.5292(13) 0.025(7) Uiso 1 1 d . . . C6 C 0.2561(3) 0.45909(19) 0.43154(12) 0.0201(5) Uani 1 1 d . . . H6 H 0.321(4) 0.401(2) 0.4423(13) 0.026(7) Uiso 1 1 d . . . C7 C 0.1587(4) 0.3422(2) 0.30745(14) 0.0272(6) Uani 1 1 d . . . H7A H 0.067(4) 0.292(2) 0.3157(14) 0.036(8) Uiso 1 1 d . . . H7B H 0.280(5) 0.310(3) 0.3107(16) 0.051(10) Uiso 1 1 d . . . H7C H 0.131(5) 0.345(2) 0.2610(17) 0.047(9) Uiso 1 1 d . . . C8 C 0.2124(4) 0.75252(19) 0.52856(12) 0.0209(5) Uani 1 1 d . . . H8 H 0.352(4) 0.767(2) 0.5489(13) 0.023(7) Uiso 1 1 d . . . C9 C 0.1493(4) 0.8488(2) 0.50625(14) 0.0255(6) Uani 1 1 d . . . H9A H 0.216(4) 0.864(2) 0.4717(13) 0.026(7) Uiso 1 1 d . . . H9B H 0.176(4) 0.915(2) 0.5481(15) 0.036(8) Uiso 1 1 d . . . H9C H 0.014(4) 0.837(2) 0.4891(14) 0.029(7) Uiso 1 1 d . . . C10 C 0.1121(4) 0.7339(2) 0.58458(13) 0.0238(5) Uani 1 1 d . . . H10A H -0.025(4) 0.721(2) 0.5684(13) 0.023(7) Uiso 1 1 d . . . H10B H 0.144(4) 0.803(2) 0.6261(13) 0.025(7) Uiso 1 1 d . . . H10C H 0.156(4) 0.674(2) 0.6012(13) 0.025(7) Uiso 1 1 d . . . C11 C 0.6582(3) 0.72424(18) 0.30905(11) 0.0155(5) Uani 1 1 d . . . H11A H 0.667(3) 0.7909(19) 0.2941(12) 0.014(6) Uiso 1 1 d . . . H11B H 0.725(4) 0.7365(19) 0.3526(13) 0.017(6) Uiso 1 1 d . . . C12 C 0.7040(3) 0.63546(17) 0.19219(11) 0.0148(4) Uani 1 1 d . . . C13 C 0.7082(3) 0.53803(17) 0.14082(12) 0.0169(5) Uani 1 1 d . . . C14 C 0.6883(3) 0.53644(19) 0.07348(12) 0.0206(5) Uani 1 1 d . . . H14 H 0.686(4) 0.470(2) 0.0404(13) 0.022(7) Uiso 1 1 d . . . C15 C 0.6666(4) 0.6335(2) 0.05741(12) 0.0222(5) Uani 1 1 d . . . H15 H 0.648(4) 0.636(2) 0.0115(14) 0.024(7) Uiso 1 1 d . . . C16 C 0.6695(4) 0.7257(2) 0.10992(12) 0.0224(5) Uani 1 1 d . . . H16 H 0.655(4) 0.795(2) 0.1009(12) 0.021(6) Uiso 1 1 d . . . C17 C 0.3328(3) 0.82668(17) 0.34278(11) 0.0151(4) Uani 1 1 d . . . C18 C 0.1499(3) 0.84152(19) 0.32072(12) 0.0191(5) Uani 1 1 d . . . H18 H 0.062(3) 0.7811(19) 0.2878(12) 0.014(6) Uiso 1 1 d . . . C19 C 0.0884(4) 0.9426(2) 0.34393(13) 0.0231(5) Uani 1 1 d . . . H19 H -0.028(4) 0.953(2) 0.3266(13) 0.022(7) Uiso 1 1 d . . . C20 C 0.2088(4) 1.0289(2) 0.38933(13) 0.0238(5) Uani 1 1 d . . . H20 H 0.169(4) 1.098(2) 0.4057(14) 0.031(7) Uiso 1 1 d . . . C21 C 0.3891(4) 1.01448(19) 0.41211(13) 0.0208(5) Uani 1 1 d . . . H21 H 0.470(4) 1.072(2) 0.4431(13) 0.026(7) Uiso 1 1 d . . . C22 C 0.4523(3) 0.91381(18) 0.38888(12) 0.0172(5) Uani 1 1 d . . . H22 H 0.574(4) 0.906(2) 0.4039(13) 0.023(7) Uiso 1 1 d . . . C23 C 0.3004(3) 0.63064(18) 0.22933(11) 0.0160(5) Uani 1 1 d . . . C24 C 0.2766(3) 0.51738(19) 0.20554(12) 0.0189(5) Uani 1 1 d . . . H24 H 0.315(3) 0.4771(19) 0.2374(12) 0.016(6) Uiso 1 1 d . . . C25 C 0.2032(4) 0.4641(2) 0.13748(12) 0.0248(5) Uani 1 1 d . . . H25 H 0.187(4) 0.388(2) 0.1234(14) 0.033(8) Uiso 1 1 d . . . C26 C 0.1528(4) 0.5232(2) 0.09269(13) 0.0295(6) Uani 1 1 d . . . H26 H 0.100(4) 0.486(2) 0.0467(14) 0.029(7) Uiso 1 1 d . . . C27 C 0.1773(4) 0.6355(2) 0.11489(13) 0.0295(6) Uani 1 1 d . . . H27 H 0.142(4) 0.676(2) 0.0869(14) 0.028(7) Uiso 1 1 d . . . C28 C 0.2515(3) 0.6900(2) 0.18314(12) 0.0231(5) Uani 1 1 d . . . H28 H 0.271(3) 0.7644(19) 0.2001(11) 0.009(6) Uiso 1 1 d . . . C29 C 0.7059(4) 0.18754(18) 0.20081(12) 0.0241(5) Uani 1 1 d . . . C30 C 0.5567(5) 0.1983(2) 0.23257(15) 0.0359(7) Uani 1 1 d . . . H30 H 0.507(5) 0.262(3) 0.2409(17) 0.054(10) Uiso 1 1 d . . . C31 C 0.4930(6) 0.1130(3) 0.25482(17) 0.0502(9) Uani 1 1 d . . . H31 H 0.387(6) 0.124(3) 0.275(2) 0.071(12) Uiso 1 1 d . . . C32 C 0.5795(6) 0.0201(3) 0.24507(17) 0.0543(11) Uani 1 1 d . . . H32 H 0.528(5) -0.038(3) 0.2610(19) 0.073(12) Uiso 1 1 d . . . C33 C 0.7299(6) 0.0110(2) 0.21315(16) 0.0457(9) Uani 1 1 d . . . H33 H 0.786(6) -0.044(3) 0.207(2) 0.072(13) Uiso 1 1 d . . . C34 C 0.7967(4) 0.0960(2) 0.19094(14) 0.0310(6) Uani 1 1 d . . . H34 H 0.903(4) 0.095(2) 0.1696(15) 0.037(8) Uiso 1 1 d . . . C35 C 0.8033(4) 0.20425(18) 0.01899(12) 0.0246(5) Uani 1 1 d . . . C36 C 0.9704(5) 0.1836(2) 0.00058(16) 0.0402(8) Uani 1 1 d . . . H36 H 1.073(5) 0.234(3) 0.0213(17) 0.057(10) Uiso 1 1 d . . . C37 C 0.8232(5) 0.0169(3) -0.08093(18) 0.0529(9) Uani 1 1 d . . . H37 H 0.832(5) -0.046(3) -0.1158(17) 0.054(10) Uiso 1 1 d . . . C38 C 0.9796(5) 0.0888(3) -0.05000(19) 0.0566(10) Uani 1 1 d . . . H38 H 1.102(5) 0.072(3) -0.0621(17) 0.059(10) Uiso 1 1 d . . . C39 C 0.6569(5) 0.0387(3) -0.06166(16) 0.0450(8) Uani 1 1 d . . . H39 H 0.550(6) -0.012(3) -0.0829(19) 0.067(11) Uiso 1 1 d . . . C40 C 0.6455(4) 0.1335(2) -0.01114(15) 0.0351(7) Uani 1 1 d . . . H40 H 0.537(5) 0.152(2) 0.0063(16) 0.044(9) Uiso 1 1 d . . . H1 H 0.709(4) 0.580(2) 0.2674(13) 0.017(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01056(10) 0.01387(10) 0.01191(9) 0.00555(7) 0.00107(6) 0.00075(6) Cl1 0.0159(3) 0.0160(3) 0.0187(3) 0.0076(2) 0.0041(2) 0.0043(2) P1 0.0114(3) 0.0138(3) 0.0120(3) 0.0051(2) 0.0018(2) 0.0017(2) O1 0.0278(10) 0.0149(8) 0.0221(8) 0.0073(7) 0.0058(7) 0.0056(7) N1 0.0174(11) 0.0159(10) 0.0175(10) 0.0082(8) 0.0060(8) 0.0044(8) C1 0.0139(12) 0.0202(11) 0.0234(12) 0.0077(10) 0.0044(9) -0.0043(9) Cl2 0.0142(3) 0.0183(3) 0.0138(2) 0.0048(2) -0.0005(2) -0.0011(2) P2 0.0212(3) 0.0159(3) 0.0261(3) 0.0080(2) 0.0051(3) 0.0024(2) O2 0.0327(11) 0.0161(8) 0.0333(10) 0.0009(7) 0.0145(8) 0.0006(7) N2 0.0245(11) 0.0187(10) 0.0189(10) 0.0083(8) 0.0091(8) 0.0048(8) C2 0.0111(11) 0.0288(13) 0.0152(11) 0.0084(10) 0.0008(9) -0.0011(9) O3 0.0261(10) 0.0254(9) 0.0422(11) 0.0207(8) 0.0012(8) 0.0019(8) C3 0.0112(12) 0.0228(12) 0.0273(13) 0.0129(10) 0.0048(9) 0.0028(9) O4 0.0243(10) 0.0245(9) 0.0340(10) 0.0102(8) 0.0054(8) 0.0022(7) C4 0.0116(11) 0.0234(12) 0.0185(11) 0.0051(9) 0.0067(9) -0.0018(9) C5 0.0164(12) 0.0276(12) 0.0153(11) 0.0116(10) 0.0038(9) -0.0002(10) C6 0.0161(12) 0.0226(12) 0.0247(12) 0.0135(10) 0.0023(10) -0.0012(10) C7 0.0285(16) 0.0241(13) 0.0256(14) 0.0044(11) 0.0041(11) -0.0073(11) C8 0.0179(13) 0.0250(12) 0.0209(12) 0.0075(10) 0.0060(10) 0.0014(10) C9 0.0279(15) 0.0228(13) 0.0298(14) 0.0093(11) 0.0137(12) 0.0027(11) C10 0.0246(15) 0.0255(13) 0.0234(13) 0.0077(11) 0.0092(11) 0.0048(11) C11 0.0163(12) 0.0184(11) 0.0119(11) 0.0044(9) 0.0035(9) 0.0009(9) C12 0.0110(11) 0.0176(11) 0.0175(11) 0.0066(9) 0.0053(9) 0.0018(8) C13 0.0160(12) 0.0158(11) 0.0212(11) 0.0080(9) 0.0053(9) 0.0014(9) C14 0.0221(13) 0.0206(12) 0.0187(12) 0.0043(10) 0.0066(10) -0.0002(10) C15 0.0246(14) 0.0275(13) 0.0174(12) 0.0106(10) 0.0057(10) 0.0026(10) C16 0.0278(14) 0.0209(12) 0.0235(12) 0.0132(10) 0.0069(10) 0.0038(10) C17 0.0174(12) 0.0168(11) 0.0141(10) 0.0083(9) 0.0043(9) 0.0033(9) C18 0.0169(12) 0.0218(12) 0.0197(11) 0.0087(10) 0.0013(9) 0.0025(10) C19 0.0184(13) 0.0274(13) 0.0265(13) 0.0121(11) 0.0021(10) 0.0097(10) C20 0.0284(15) 0.0177(12) 0.0300(13) 0.0100(10) 0.0114(11) 0.0093(10) C21 0.0222(13) 0.0165(11) 0.0253(12) 0.0068(10) 0.0079(10) 0.0017(10) C22 0.0164(13) 0.0180(11) 0.0188(11) 0.0075(9) 0.0042(9) 0.0016(9) C23 0.0120(11) 0.0246(12) 0.0121(10) 0.0066(9) 0.0020(8) 0.0017(9) C24 0.0146(12) 0.0239(12) 0.0167(11) 0.0040(10) 0.0029(9) 0.0008(9) C25 0.0188(13) 0.0301(14) 0.0188(12) -0.0020(10) 0.0008(10) 0.0008(10) C26 0.0204(14) 0.0495(17) 0.0131(12) 0.0013(11) 0.0004(10) 0.0054(12) C27 0.0232(14) 0.0533(18) 0.0168(12) 0.0181(12) 0.0016(10) 0.0087(12) C28 0.0209(14) 0.0287(14) 0.0219(12) 0.0111(11) 0.0038(10) 0.0022(10) C29 0.0349(15) 0.0153(11) 0.0214(12) 0.0080(10) -0.0006(11) 0.0012(10) C30 0.0462(19) 0.0287(15) 0.0350(16) 0.0075(12) 0.0172(14) 0.0049(13) C31 0.062(3) 0.053(2) 0.0416(19) 0.0208(16) 0.0191(18) -0.0034(18) C32 0.086(3) 0.0386(19) 0.0350(17) 0.0222(15) -0.0073(18) -0.0187(19) C33 0.077(3) 0.0174(14) 0.0333(16) 0.0074(12) -0.0174(17) 0.0077(15) C34 0.0393(18) 0.0243(13) 0.0265(14) 0.0057(11) -0.0016(12) 0.0100(12) C35 0.0370(16) 0.0152(11) 0.0222(12) 0.0053(10) 0.0063(11) 0.0062(10) C36 0.0403(19) 0.0250(14) 0.0495(18) -0.0046(13) 0.0223(15) -0.0051(13) C37 0.055(2) 0.0432(19) 0.0435(19) -0.0163(16) 0.0120(17) 0.0018(17) C38 0.050(2) 0.0432(19) 0.064(2) -0.0156(17) 0.0346(19) -0.0008(16) C39 0.042(2) 0.0364(17) 0.0395(17) -0.0081(14) -0.0062(15) -0.0020(15) C40 0.0299(17) 0.0318(15) 0.0367(16) 0.0009(12) 0.0006(13) 0.0079(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 C2 2.185(2) . ? Ru1 C3 2.187(2) . ? Ru1 C1 2.213(2) . ? Ru1 C4 2.217(2) . ? Ru1 C6 2.244(2) . ? Ru1 C5 2.249(2) . ? Ru1 P1 2.3396(6) . ? Ru1 Cl2 2.4149(5) . ? Ru1 Cl1 2.4305(6) . ? P1 C17 1.820(2) . ? P1 C23 1.820(2) . ? P1 C11 1.875(2) . ? O1 C13 1.405(3) . ? O1 P2 1.5763(16) . ? N1 C12 1.374(3) . ? N1 C11 1.452(3) . ? C1 C2 1.404(3) . ? C1 C6 1.425(3) . ? C1 C7 1.511(3) . ? P2 O4 1.4480(19) . ? P2 O3 1.5672(18) . ? P2 O2 1.5843(18) . ? O2 C35 1.413(3) . ? N2 C12 1.338(3) . ? N2 C16 1.352(3) . ? C2 C3 1.426(3) . ? O3 C29 1.412(3) . ? C3 C4 1.420(3) . ? C4 C5 1.435(3) . ? C4 C8 1.522(3) . ? C5 C6 1.379(3) . ? C8 C9 1.515(4) . ? C8 C10 1.531(3) . ? C12 C13 1.408(3) . ? C13 C14 1.369(3) . ? C14 C15 1.392(3) . ? C15 C16 1.366(3) . ? C17 C18 1.398(3) . ? C17 C22 1.398(3) . ? C18 C19 1.392(3) . ? C19 C20 1.389(4) . ? C20 C21 1.381(4) . ? C21 C22 1.393(3) . ? C23 C24 1.395(3) . ? C23 C28 1.399(3) . ? C24 C25 1.384(3) . ? C25 C26 1.376(4) . ? C26 C27 1.382(4) . ? C27 C28 1.392(3) . ? C29 C30 1.363(4) . ? C29 C34 1.378(4) . ? C30 C31 1.385(4) . ? C31 C32 1.376(5) . ? C32 C33 1.372(6) . ? C33 C34 1.390(4) . ? C35 C36 1.368(4) . ? C35 C40 1.374(4) . ? C36 C38 1.384(4) . ? C37 C39 1.372(5) . ? C37 C38 1.376(5) . ? C39 C40 1.389(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ru1 C3 38.08(9) . . ? C2 Ru1 C1 37.22(9) . . ? C3 Ru1 C1 68.06(9) . . ? C2 Ru1 C4 68.28(8) . . ? C3 Ru1 C4 37.60(9) . . ? C1 Ru1 C4 80.69(8) . . ? C2 Ru1 C6 66.42(9) . . ? C3 Ru1 C6 78.70(9) . . ? C1 Ru1 C6 37.27(8) . . ? C4 Ru1 C6 66.70(9) . . ? C2 Ru1 C5 78.59(9) . . ? C3 Ru1 C5 66.79(9) . . ? C1 Ru1 C5 66.48(8) . . ? C4 Ru1 C5 37.49(9) . . ? C6 Ru1 C5 35.74(9) . . ? C2 Ru1 P1 94.78(6) . . ? C3 Ru1 P1 93.95(6) . . ? C1 Ru1 P1 120.46(6) . . ? C4 Ru1 P1 118.98(6) . . ? C6 Ru1 P1 157.70(6) . . ? C5 Ru1 P1 156.36(6) . . ? C2 Ru1 Cl2 154.96(6) . . ? C3 Ru1 Cl2 116.93(6) . . ? C1 Ru1 Cl2 155.40(6) . . ? C4 Ru1 Cl2 90.42(6) . . ? C6 Ru1 Cl2 118.24(6) . . ? C5 Ru1 Cl2 92.61(6) . . ? P1 Ru1 Cl2 83.914(19) . . ? C2 Ru1 Cl1 117.36(6) . . ? C3 Ru1 Cl1 155.44(6) . . ? C1 Ru1 Cl1 90.30(6) . . ? C4 Ru1 Cl1 153.55(6) . . ? C6 Ru1 Cl1 91.17(7) . . ? C5 Ru1 Cl1 116.24(6) . . ? P1 Ru1 Cl1 87.045(19) . . ? Cl2 Ru1 Cl1 87.600(19) . . ? C17 P1 C23 105.54(10) . . ? C17 P1 C11 103.62(10) . . ? C23 P1 C11 101.82(10) . . ? C17 P1 Ru1 112.73(7) . . ? C23 P1 Ru1 116.12(7) . . ? C11 P1 Ru1 115.55(8) . . ? C13 O1 P2 127.39(15) . . ? C12 N1 C11 120.66(19) . . ? C2 C1 C6 118.1(2) . . ? C2 C1 C7 121.5(2) . . ? C6 C1 C7 120.4(2) . . ? C2 C1 Ru1 70.27(13) . . ? C6 C1 Ru1 72.54(13) . . ? C7 C1 Ru1 129.01(17) . . ? O4 P2 O3 117.04(10) . . ? O4 P2 O1 117.87(10) . . ? O3 P2 O1 98.64(9) . . ? O4 P2 O2 115.43(10) . . ? O3 P2 O2 103.85(10) . . ? O1 P2 O2 101.35(9) . . ? C35 O2 P2 124.34(15) . . ? C12 N2 C16 117.7(2) . . ? C1 C2 C3 121.0(2) . . ? C1 C2 Ru1 72.50(13) . . ? C3 C2 Ru1 71.06(13) . . ? C29 O3 P2 125.56(17) . . ? C4 C3 C2 120.5(2) . . ? C4 C3 Ru1 72.33(14) . . ? C2 C3 Ru1 70.86(13) . . ? C3 C4 C5 117.6(2) . . ? C3 C4 C8 123.9(2) . . ? C5 C4 C8 118.5(2) . . ? C3 C4 Ru1 70.07(13) . . ? C5 C4 Ru1 72.47(13) . . ? C8 C4 Ru1 128.83(15) . . ? C6 C5 C4 121.2(2) . . ? C6 C5 Ru1 71.94(13) . . ? C4 C5 Ru1 70.04(12) . . ? C5 C6 C1 121.5(2) . . ? C5 C6 Ru1 72.31(13) . . ? C1 C6 Ru1 70.19(13) . . ? C9 C8 C4 113.6(2) . . ? C9 C8 C10 110.9(2) . . ? C4 C8 C10 109.54(19) . . ? N1 C11 P1 113.02(15) . . ? N2 C12 N1 118.57(19) . . ? N2 C12 C13 120.8(2) . . ? N1 C12 C13 120.6(2) . . ? C14 C13 O1 124.8(2) . . ? C14 C13 C12 120.5(2) . . ? O1 C13 C12 114.66(19) . . ? C13 C14 C15 118.4(2) . . ? C16 C15 C14 118.1(2) . . ? N2 C16 C15 124.4(2) . . ? C18 C17 C22 119.4(2) . . ? C18 C17 P1 121.11(17) . . ? C22 C17 P1 119.29(18) . . ? C19 C18 C17 120.1(2) . . ? C20 C19 C18 120.0(2) . . ? C21 C20 C19 120.2(2) . . ? C20 C21 C22 120.2(2) . . ? C21 C22 C17 120.0(2) . . ? C24 C23 C28 119.0(2) . . ? C24 C23 P1 117.44(17) . . ? C28 C23 P1 123.31(18) . . ? C25 C24 C23 120.7(2) . . ? C26 C25 C24 119.8(2) . . ? C25 C26 C27 120.5(2) . . ? C26 C27 C28 120.2(2) . . ? C27 C28 C23 119.7(2) . . ? C30 C29 C34 122.6(3) . . ? C30 C29 O3 121.0(2) . . ? C34 C29 O3 116.3(2) . . ? C29 C30 C31 118.4(3) . . ? C32 C31 C30 120.4(4) . . ? C33 C32 C31 120.3(3) . . ? C32 C33 C34 120.2(3) . . ? C29 C34 C33 118.1(3) . . ? C36 C35 C40 121.8(2) . . ? C36 C35 O2 115.8(2) . . ? C40 C35 O2 122.3(2) . . ? C35 C36 C38 118.8(3) . . ? C39 C37 C38 120.1(3) . . ? C37 C38 C36 120.4(3) . . ? C37 C39 C40 120.2(3) . . ? C35 C40 C39 118.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Ru1 P1 C17 82.15(10) . . . . ? C3 Ru1 P1 C17 43.97(10) . . . . ? C1 Ru1 P1 C17 110.77(11) . . . . ? C4 Ru1 P1 C17 14.38(11) . . . . ? C6 Ru1 P1 C17 113.51(19) . . . . ? C5 Ru1 P1 C17 9.85(18) . . . . ? Cl2 Ru1 P1 C17 -72.72(8) . . . . ? Cl1 Ru1 P1 C17 -160.62(8) . . . . ? C2 Ru1 P1 C23 -39.78(11) . . . . ? C3 Ru1 P1 C23 -77.96(10) . . . . ? C1 Ru1 P1 C23 -11.16(11) . . . . ? C4 Ru1 P1 C23 -107.55(11) . . . . ? C6 Ru1 P1 C23 -8.4(2) . . . . ? C5 Ru1 P1 C23 -112.08(18) . . . . ? Cl2 Ru1 P1 C23 165.34(9) . . . . ? Cl1 Ru1 P1 C23 77.45(8) . . . . ? C2 Ru1 P1 C11 -158.94(10) . . . . ? C3 Ru1 P1 C11 162.87(10) . . . . ? C1 Ru1 P1 C11 -130.33(10) . . . . ? C4 Ru1 P1 C11 133.29(10) . . . . ? C6 Ru1 P1 C11 -127.58(19) . . . . ? C5 Ru1 P1 C11 128.75(17) . . . . ? Cl2 Ru1 P1 C11 46.18(8) . . . . ? Cl1 Ru1 P1 C11 -41.72(8) . . . . ? C3 Ru1 C1 C2 29.24(13) . . . . ? C4 Ru1 C1 C2 66.15(14) . . . . ? C6 Ru1 C1 C2 129.6(2) . . . . ? C5 Ru1 C1 C2 102.49(15) . . . . ? P1 Ru1 C1 C2 -52.09(14) . . . . ? Cl2 Ru1 C1 C2 136.28(14) . . . . ? Cl1 Ru1 C1 C2 -138.84(13) . . . . ? C2 Ru1 C1 C6 -129.6(2) . . . . ? C3 Ru1 C1 C6 -100.40(16) . . . . ? C4 Ru1 C1 C6 -63.48(15) . . . . ? C5 Ru1 C1 C6 -27.14(14) . . . . ? P1 Ru1 C1 C6 178.28(12) . . . . ? Cl2 Ru1 C1 C6 6.6(2) . . . . ? Cl1 Ru1 C1 C6 91.53(14) . . . . ? C2 Ru1 C1 C7 115.0(3) . . . . ? C3 Ru1 C1 C7 144.3(3) . . . . ? C4 Ru1 C1 C7 -178.8(2) . . . . ? C6 Ru1 C1 C7 -115.3(3) . . . . ? C5 Ru1 C1 C7 -142.5(3) . . . . ? P1 Ru1 C1 C7 63.0(2) . . . . ? Cl2 Ru1 C1 C7 -108.7(2) . . . . ? Cl1 Ru1 C1 C7 -23.8(2) . . . . ? C13 O1 P2 O4 -59.4(2) . . . . ? C13 O1 P2 O3 173.65(18) . . . . ? C13 O1 P2 O2 67.5(2) . . . . ? O4 P2 O2 C35 -53.9(2) . . . . ? O3 P2 O2 C35 75.5(2) . . . . ? O1 P2 O2 C35 177.50(19) . . . . ? C6 C1 C2 C3 2.3(3) . . . . ? C7 C1 C2 C3 -178.5(2) . . . . ? Ru1 C1 C2 C3 -54.12(19) . . . . ? C6 C1 C2 Ru1 56.42(19) . . . . ? C7 C1 C2 Ru1 -124.4(2) . . . . ? C3 Ru1 C2 C1 -132.7(2) . . . . ? C4 Ru1 C2 C1 -103.69(15) . . . . ? C6 Ru1 C2 C1 -30.59(13) . . . . ? C5 Ru1 C2 C1 -65.97(14) . . . . ? P1 Ru1 C2 C1 136.97(12) . . . . ? Cl2 Ru1 C2 C1 -137.18(14) . . . . ? Cl1 Ru1 C2 C1 47.83(14) . . . . ? C1 Ru1 C2 C3 132.7(2) . . . . ? C4 Ru1 C2 C3 29.04(13) . . . . ? C6 Ru1 C2 C3 102.14(15) . . . . ? C5 Ru1 C2 C3 66.76(14) . . . . ? P1 Ru1 C2 C3 -90.30(13) . . . . ? Cl2 Ru1 C2 C3 -4.5(2) . . . . ? Cl1 Ru1 C2 C3 -179.44(11) . . . . ? O4 P2 O3 C29 8.3(2) . . . . ? O1 P2 O3 C29 135.74(19) . . . . ? O2 P2 O3 C29 -120.2(2) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? Ru1 C2 C3 C4 -54.78(19) . . . . ? C1 C2 C3 Ru1 54.8(2) . . . . ? C2 Ru1 C3 C4 132.3(2) . . . . ? C1 Ru1 C3 C4 103.72(15) . . . . ? C6 Ru1 C3 C4 66.32(14) . . . . ? C5 Ru1 C3 C4 30.90(13) . . . . ? P1 Ru1 C3 C4 -134.94(12) . . . . ? Cl2 Ru1 C3 C4 -49.76(14) . . . . ? Cl1 Ru1 C3 C4 133.54(14) . . . . ? C1 Ru1 C3 C2 -28.62(13) . . . . ? C4 Ru1 C3 C2 -132.3(2) . . . . ? C6 Ru1 C3 C2 -66.03(14) . . . . ? C5 Ru1 C3 C2 -101.45(15) . . . . ? P1 Ru1 C3 C2 92.71(12) . . . . ? Cl2 Ru1 C3 C2 177.89(11) . . . . ? Cl1 Ru1 C3 C2 1.2(2) . . . . ? C2 C3 C4 C5 -2.5(3) . . . . ? Ru1 C3 C4 C5 -56.56(18) . . . . ? C2 C3 C4 C8 178.1(2) . . . . ? Ru1 C3 C4 C8 124.1(2) . . . . ? C2 C3 C4 Ru1 54.10(19) . . . . ? C2 Ru1 C4 C3 -29.38(13) . . . . ? C1 Ru1 C4 C3 -65.94(14) . . . . ? C6 Ru1 C4 C3 -102.09(15) . . . . ? C5 Ru1 C4 C3 -129.2(2) . . . . ? P1 Ru1 C4 C3 53.83(14) . . . . ? Cl2 Ru1 C4 C3 137.11(13) . . . . ? Cl1 Ru1 C4 C3 -137.43(14) . . . . ? C2 Ru1 C4 C5 99.77(15) . . . . ? C3 Ru1 C4 C5 129.2(2) . . . . ? C1 Ru1 C4 C5 63.21(14) . . . . ? C6 Ru1 C4 C5 27.06(13) . . . . ? P1 Ru1 C4 C5 -177.02(11) . . . . ? Cl2 Ru1 C4 C5 -93.74(13) . . . . ? Cl1 Ru1 C4 C5 -8.3(2) . . . . ? C2 Ru1 C4 C8 -147.3(2) . . . . ? C3 Ru1 C4 C8 -118.0(3) . . . . ? C1 Ru1 C4 C8 176.1(2) . . . . ? C6 Ru1 C4 C8 139.9(2) . . . . ? C5 Ru1 C4 C8 112.9(3) . . . . ? P1 Ru1 C4 C8 -64.1(2) . . . . ? Cl2 Ru1 C4 C8 19.1(2) . . . . ? Cl1 Ru1 C4 C8 104.6(2) . . . . ? C3 C4 C5 C6 2.7(3) . . . . ? C8 C4 C5 C6 -177.9(2) . . . . ? Ru1 C4 C5 C6 -52.7(2) . . . . ? C3 C4 C5 Ru1 55.35(18) . . . . ? C8 C4 C5 Ru1 -125.22(19) . . . . ? C2 Ru1 C5 C6 65.28(15) . . . . ? C3 Ru1 C5 C6 103.35(16) . . . . ? C1 Ru1 C5 C6 28.23(15) . . . . ? C4 Ru1 C5 C6 134.3(2) . . . . ? P1 Ru1 C5 C6 140.86(15) . . . . ? Cl2 Ru1 C5 C6 -138.38(14) . . . . ? Cl1 Ru1 C5 C6 -49.76(16) . . . . ? C2 Ru1 C5 C4 -69.06(14) . . . . ? C3 Ru1 C5 C4 -30.99(13) . . . . ? C1 Ru1 C5 C4 -106.11(15) . . . . ? C6 Ru1 C5 C4 -134.3(2) . . . . ? P1 Ru1 C5 C4 6.5(2) . . . . ? Cl2 Ru1 C5 C4 87.29(13) . . . . ? Cl1 Ru1 C5 C4 175.90(11) . . . . ? C4 C5 C6 C1 -0.4(3) . . . . ? Ru1 C5 C6 C1 -52.2(2) . . . . ? C4 C5 C6 Ru1 51.85(19) . . . . ? C2 C1 C6 C5 -2.1(3) . . . . ? C7 C1 C6 C5 178.6(2) . . . . ? Ru1 C1 C6 C5 53.2(2) . . . . ? C2 C1 C6 Ru1 -55.30(18) . . . . ? C7 C1 C6 Ru1 125.5(2) . . . . ? C2 Ru1 C6 C5 -103.71(16) . . . . ? C3 Ru1 C6 C5 -65.77(15) . . . . ? C1 Ru1 C6 C5 -134.3(2) . . . . ? C4 Ru1 C6 C5 -28.29(14) . . . . ? P1 Ru1 C6 C5 -138.17(16) . . . . ? Cl2 Ru1 C6 C5 48.87(16) . . . . ? Cl1 Ru1 C6 C5 136.77(14) . . . . ? C2 Ru1 C6 C1 30.55(14) . . . . ? C3 Ru1 C6 C1 68.50(15) . . . . ? C4 Ru1 C6 C1 105.97(16) . . . . ? C5 Ru1 C6 C1 134.3(2) . . . . ? P1 Ru1 C6 C1 -3.9(3) . . . . ? Cl2 Ru1 C6 C1 -176.87(12) . . . . ? Cl1 Ru1 C6 C1 -88.96(14) . . . . ? C3 C4 C8 C9 -9.2(3) . . . . ? C5 C4 C8 C9 171.4(2) . . . . ? Ru1 C4 C8 C9 81.6(3) . . . . ? C3 C4 C8 C10 115.5(2) . . . . ? C5 C4 C8 C10 -63.9(3) . . . . ? Ru1 C4 C8 C10 -153.76(19) . . . . ? C12 N1 C11 P1 91.9(2) . . . . ? C17 P1 C11 N1 -151.36(16) . . . . ? C23 P1 C11 N1 -41.95(18) . . . . ? Ru1 P1 C11 N1 84.82(16) . . . . ? C16 N2 C12 N1 -179.2(2) . . . . ? C16 N2 C12 C13 2.7(3) . . . . ? C11 N1 C12 N2 22.0(3) . . . . ? C11 N1 C12 C13 -159.8(2) . . . . ? P2 O1 C13 C14 -29.1(3) . . . . ? P2 O1 C13 C12 153.46(17) . . . . ? N2 C12 C13 C14 -2.9(3) . . . . ? N1 C12 C13 C14 178.9(2) . . . . ? N2 C12 C13 O1 174.7(2) . . . . ? N1 C12 C13 O1 -3.5(3) . . . . ? O1 C13 C14 C15 -176.4(2) . . . . ? C12 C13 C14 C15 1.0(4) . . . . ? C13 C14 C15 C16 1.1(4) . . . . ? C12 N2 C16 C15 -0.6(4) . . . . ? C14 C15 C16 N2 -1.3(4) . . . . ? C23 P1 C17 C18 38.8(2) . . . . ? C11 P1 C17 C18 145.46(18) . . . . ? Ru1 P1 C17 C18 -88.90(18) . . . . ? C23 P1 C17 C22 -146.25(17) . . . . ? C11 P1 C17 C22 -39.6(2) . . . . ? Ru1 P1 C17 C22 86.02(18) . . . . ? C22 C17 C18 C19 0.7(3) . . . . ? P1 C17 C18 C19 175.65(17) . . . . ? C17 C18 C19 C20 -0.2(4) . . . . ? C18 C19 C20 C21 -0.6(4) . . . . ? C19 C20 C21 C22 1.0(4) . . . . ? C20 C21 C22 C17 -0.5(3) . . . . ? C18 C17 C22 C21 -0.4(3) . . . . ? P1 C17 C22 C21 -175.36(17) . . . . ? C17 P1 C23 C24 -155.43(18) . . . . ? C11 P1 C23 C24 96.63(19) . . . . ? Ru1 P1 C23 C24 -29.8(2) . . . . ? C17 P1 C23 C28 30.0(2) . . . . ? C11 P1 C23 C28 -77.9(2) . . . . ? Ru1 P1 C23 C28 155.69(17) . . . . ? C28 C23 C24 C25 -1.0(3) . . . . ? P1 C23 C24 C25 -175.75(19) . . . . ? C23 C24 C25 C26 -0.1(4) . . . . ? C24 C25 C26 C27 1.0(4) . . . . ? C25 C26 C27 C28 -0.8(4) . . . . ? C26 C27 C28 C23 -0.3(4) . . . . ? C24 C23 C28 C27 1.2(4) . . . . ? P1 C23 C28 C27 175.60(19) . . . . ? P2 O3 C29 C30 -62.2(3) . . . . ? P2 O3 C29 C34 121.4(2) . . . . ? C34 C29 C30 C31 -1.0(5) . . . . ? O3 C29 C30 C31 -177.2(3) . . . . ? C29 C30 C31 C32 0.2(5) . . . . ? C30 C31 C32 C33 0.0(5) . . . . ? C31 C32 C33 C34 0.5(5) . . . . ? C30 C29 C34 C33 1.4(4) . . . . ? O3 C29 C34 C33 177.8(2) . . . . ? C32 C33 C34 C29 -1.2(4) . . . . ? P2 O2 C35 C36 -144.3(2) . . . . ? P2 O2 C35 C40 39.3(3) . . . . ? C40 C35 C36 C38 0.2(5) . . . . ? O2 C35 C36 C38 -176.2(3) . . . . ? C39 C37 C38 C36 -0.1(6) . . . . ? C35 C36 C38 C37 -0.1(6) . . . . ? C38 C37 C39 C40 0.3(6) . . . . ? C36 C35 C40 C39 0.0(5) . . . . ? O2 C35 C40 C39 176.2(3) . . . . ? C37 C39 C40 C35 -0.2(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl1 0.80(3) 2.52(3) 3.203(2) 145(2) . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.513 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.130 #===END data_rupyphos _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54.50 H66.50 Cl11.50 N2 O2 P2 Ru2' _chemical_formula_weight 1453.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2902(3) _cell_length_b 13.6623(4) _cell_length_c 21.4044(7) _cell_angle_alpha 93.695(2) _cell_angle_beta 104.682(2) _cell_angle_gamma 101.304(2) _cell_volume 3109.12(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1474 _exptl_absorpt_coefficient_mu 1.072 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.8141 _exptl_absorpt_correction_T_max 0.9003 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi + omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18624 _diffrn_reflns_av_R_equivalents 0.1074 _diffrn_reflns_av_sigmaI/netI 0.1195 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10808 _reflns_number_gt 8679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _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^)+(0.0592P)^2^+18.8848P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10808 _refine_ls_number_parameters 684 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1515 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.55567(4) 0.41716(3) 0.11986(2) 0.01798(13) Uani 1 1 d . . . Cl1 Cl 0.68242(14) 0.58615(10) 0.14489(7) 0.0252(3) Uani 1 1 d . . . P1 P 0.68780(13) 0.36577(10) 0.20667(7) 0.0161(3) Uani 1 1 d . . . O1 O 0.6399(3) 0.3663(3) 0.27309(18) 0.0178(8) Uani 1 1 d . . . N1 N 0.4875(4) 0.5091(3) 0.3646(2) 0.0213(10) Uani 1 1 d . . . C1 C 0.6164(5) 0.4513(4) 0.3031(3) 0.0177(11) Uani 1 1 d . . . Ru2 Ru 0.33761(4) 0.07122(3) 0.40141(2) 0.01626(13) Uani 1 1 d . . . Cl2 Cl 0.69478(13) 0.37420(11) 0.05790(7) 0.0247(3) Uani 1 1 d . . . P2 P 0.25292(13) 0.19399(10) 0.34488(7) 0.0162(3) Uani 1 1 d . . . N2 N 0.4446(4) 0.3379(3) 0.3270(2) 0.0180(10) Uani 1 1 d . . . C2 C 0.6859(5) 0.5471(4) 0.3077(3) 0.0220(12) Uani 1 1 d . . . H2 H 0.7535 0.5601 0.2883 0.026 Uiso 1 1 calc R . . Cl3 Cl 0.41634(13) 0.20529(10) 0.48994(6) 0.0219(3) Uani 1 1 d . . . C3 C 0.6553(6) 0.6248(4) 0.3412(3) 0.0249(13) Uani 1 1 d . . . H3 H 0.7019 0.6920 0.3454 0.030 Uiso 1 1 calc R . . Cl4 Cl 0.52826(12) 0.13351(10) 0.36965(7) 0.0219(3) Uani 1 1 d . . . C4 C 0.5556(6) 0.6025(4) 0.3683(3) 0.0251(13) Uani 1 1 d . . . H4 H 0.5344 0.6560 0.3908 0.030 Uiso 1 1 calc R . . C5 C 0.5174(5) 0.4340(4) 0.3328(3) 0.0170(11) Uani 1 1 d . . . C6 C 0.3448(5) 0.3242(4) 0.3604(3) 0.0186(11) Uani 1 1 d . . . H6A H 0.2883 0.3700 0.3454 0.022 Uiso 1 1 calc R . . H6B H 0.3828 0.3425 0.4078 0.022 Uiso 1 1 calc R . . C7 C 0.8542(5) 0.4224(4) 0.2367(3) 0.0178(11) Uani 1 1 d . . . C8 C 0.9238(6) 0.4734(4) 0.1986(3) 0.0258(13) Uani 1 1 d . . . H8 H 0.8838 0.4808 0.1549 0.031 Uiso 1 1 calc R . . C9 C 1.0522(6) 0.5136(5) 0.2246(3) 0.0293(14) Uani 1 1 d . . . H9 H 1.0992 0.5476 0.1984 0.035 Uiso 1 1 calc R . . C10 C 1.1116(6) 0.5041(4) 0.2885(3) 0.0282(14) Uani 1 1 d . . . H10 H 1.1989 0.5314 0.3059 0.034 Uiso 1 1 calc R . . C11 C 1.0424(5) 0.4544(4) 0.3265(3) 0.0247(13) Uani 1 1 d . . . H11 H 1.0826 0.4488 0.3705 0.030 Uiso 1 1 calc R . . C12 C 0.9160(5) 0.4129(4) 0.3014(3) 0.0204(12) Uani 1 1 d . . . H12 H 0.8702 0.3778 0.3278 0.025 Uiso 1 1 calc R . . C13 C 0.6849(5) 0.2325(4) 0.1973(3) 0.0187(11) Uani 1 1 d . . . C14 C 0.7688(6) 0.1972(4) 0.1684(3) 0.0244(13) Uani 1 1 d . . . H14 H 0.8304 0.2435 0.1557 0.029 Uiso 1 1 calc R . . C15 C 0.7626(6) 0.0945(5) 0.1582(3) 0.0299(14) Uani 1 1 d . . . H15 H 0.8207 0.0710 0.1391 0.036 Uiso 1 1 calc R . . C16 C 0.6724(6) 0.0266(5) 0.1758(3) 0.0282(14) Uani 1 1 d . . . H16 H 0.6680 -0.0435 0.1683 0.034 Uiso 1 1 calc R . . C17 C 0.5886(6) 0.0607(4) 0.2042(3) 0.0283(14) Uani 1 1 d . . . H17 H 0.5270 0.0136 0.2163 0.034 Uiso 1 1 calc R . . C18 C 0.5932(5) 0.1625(4) 0.2151(3) 0.0219(12) Uani 1 1 d . . . H18 H 0.5349 0.1851 0.2345 0.026 Uiso 1 1 calc R . . C19 C 0.1103(5) 0.2065(4) 0.3667(3) 0.0183(11) Uani 1 1 d . . . C20 C 0.1190(5) 0.2613(4) 0.4260(3) 0.0210(12) Uani 1 1 d . . . H20 H 0.1985 0.2973 0.4525 0.025 Uiso 1 1 calc R . . C21 C 0.0118(6) 0.2631(4) 0.4458(3) 0.0263(13) Uani 1 1 d . . . H21 H 0.0183 0.3009 0.4858 0.032 Uiso 1 1 calc R . . C22 C -0.1056(5) 0.2101(4) 0.4077(3) 0.0256(13) Uani 1 1 d . . . H22 H -0.1786 0.2107 0.4219 0.031 Uiso 1 1 calc R . . C23 C -0.1145(5) 0.1565(4) 0.3488(3) 0.0233(13) Uani 1 1 d . . . H23 H -0.1943 0.1209 0.3224 0.028 Uiso 1 1 calc R . . C24 C -0.0082(5) 0.1544(4) 0.3282(3) 0.0203(12) Uani 1 1 d . . . H24 H -0.0156 0.1175 0.2877 0.024 Uiso 1 1 calc R . . C25 C 0.2050(5) 0.1723(4) 0.2559(3) 0.0200(12) Uani 1 1 d . . . C26 C 0.1308(5) 0.2313(5) 0.2201(3) 0.0278(14) Uani 1 1 d . . . H26 H 0.1061 0.2837 0.2416 0.033 Uiso 1 1 calc R . . C27 C 0.0935(6) 0.2121(6) 0.1522(3) 0.0378(17) Uani 1 1 d . . . H27 H 0.0439 0.2522 0.1274 0.045 Uiso 1 1 calc R . . C28 C 0.1280(6) 0.1358(6) 0.1211(3) 0.0414(18) Uani 1 1 d . . . H28 H 0.0987 0.1212 0.0751 0.050 Uiso 1 1 calc R . . C29 C 0.2049(7) 0.0801(5) 0.1563(3) 0.0381(16) Uani 1 1 d . . . H29 H 0.2310 0.0290 0.1343 0.046 Uiso 1 1 calc R . . C30 C 0.2440(6) 0.0984(4) 0.2232(3) 0.0278(13) Uani 1 1 d . . . H30 H 0.2979 0.0604 0.2472 0.033 Uiso 1 1 calc R . . C31 C 0.3943(5) 0.4707(4) 0.1400(3) 0.0240(12) Uani 1 1 d . . . C32 C 0.3945(5) 0.3746(5) 0.1595(3) 0.0245(13) Uani 1 1 d . . . H32 H 0.3921 0.3642 0.2026 0.029 Uiso 1 1 calc R . . C33 C 0.3983(5) 0.2923(4) 0.1163(3) 0.0238(13) Uani 1 1 d . . . H33 H 0.4001 0.2284 0.1310 0.029 Uiso 1 1 calc R . . C34 C 0.3991(5) 0.3057(4) 0.0514(3) 0.0247(13) Uani 1 1 d . . . C35 C 0.3913(5) 0.4020(5) 0.0306(3) 0.0255(13) Uani 1 1 d . . . H35 H 0.3867 0.4114 -0.0135 0.031 Uiso 1 1 calc R . . C36 C 0.3903(5) 0.4823(5) 0.0735(3) 0.0245(13) Uani 1 1 d . . . H36 H 0.3869 0.5460 0.0585 0.029 Uiso 1 1 calc R . . C37 C 0.3947(6) 0.5594(5) 0.1855(3) 0.0325(15) Uani 1 1 d . . . H37A H 0.3136 0.5788 0.1724 0.049 Uiso 1 1 calc R . . H37B H 0.4619 0.6159 0.1839 0.049 Uiso 1 1 calc R . . H37C H 0.4088 0.5412 0.2300 0.049 Uiso 1 1 calc R . . C38 C 0.4016(6) 0.2200(5) 0.0025(3) 0.0320(14) Uani 1 1 d . . . H38 H 0.4556 0.2491 -0.0252 0.038 Uiso 1 1 calc R . . C39 C 0.4552(8) 0.1350(5) 0.0326(4) 0.0452(19) Uani 1 1 d . . . H39A H 0.4031 0.1037 0.0594 0.068 Uiso 1 1 calc R . . H39B H 0.5411 0.1618 0.0598 0.068 Uiso 1 1 calc R . . H39C H 0.4560 0.0846 -0.0020 0.068 Uiso 1 1 calc R . . C40 C 0.2675(7) 0.1827(6) -0.0419(3) 0.0430(18) Uani 1 1 d . . . H40A H 0.2666 0.1296 -0.0752 0.065 Uiso 1 1 calc R . . H40B H 0.2391 0.2388 -0.0630 0.065 Uiso 1 1 calc R . . H40C H 0.2114 0.1560 -0.0159 0.065 Uiso 1 1 calc R . . C41 C 0.2187(6) -0.0120(4) 0.4563(3) 0.0258(13) Uani 1 1 d . . . C42 C 0.3331(5) -0.0460(4) 0.4710(3) 0.0246(13) Uani 1 1 d . . . H42 H 0.3780 -0.0443 0.5152 0.029 Uiso 1 1 calc R . . C43 C 0.3802(6) -0.0815(4) 0.4224(3) 0.0255(13) Uani 1 1 d . . . H43 H 0.4566 -0.1038 0.4338 0.031 Uiso 1 1 calc R . . C44 C 0.3149(5) -0.0851(4) 0.3549(3) 0.0239(13) Uani 1 1 d . . . C45 C 0.1985(5) -0.0564(4) 0.3403(3) 0.0227(12) Uani 1 1 d . . . H45 H 0.1515 -0.0610 0.2962 0.027 Uiso 1 1 calc R . . C46 C 0.1504(5) -0.0208(4) 0.3904(3) 0.0225(12) Uani 1 1 d . . . H46 H 0.0713 -0.0028 0.3794 0.027 Uiso 1 1 calc R . . C47 C 0.1724(7) 0.0309(5) 0.5102(3) 0.0358(15) Uani 1 1 d . . . H47A H 0.1266 -0.0241 0.5280 0.054 Uiso 1 1 calc R . . H47B H 0.1164 0.0751 0.4929 0.054 Uiso 1 1 calc R . . H47C H 0.2442 0.0696 0.5448 0.054 Uiso 1 1 calc R . . C48 C 0.3619(6) -0.1310(4) 0.3020(3) 0.0303(14) Uani 1 1 d . . . H48 H 0.3388 -0.0961 0.2625 0.036 Uiso 1 1 calc R . . C49 C 0.5032(7) -0.1249(5) 0.3196(4) 0.0377(16) Uani 1 1 d . . . H49A H 0.5481 -0.0544 0.3312 0.057 Uiso 1 1 calc R . . H49B H 0.5254 -0.1541 0.2823 0.057 Uiso 1 1 calc R . . H49C H 0.5268 -0.1624 0.3567 0.057 Uiso 1 1 calc R . . C50 C 0.2924(8) -0.2424(5) 0.2852(4) 0.048(2) Uani 1 1 d . . . H50A H 0.3085 -0.2766 0.3244 0.072 Uiso 1 1 calc R . . H50B H 0.3226 -0.2747 0.2519 0.072 Uiso 1 1 calc R . . H50C H 0.2021 -0.2467 0.2687 0.072 Uiso 1 1 calc R . . Cl1S Cl -0.18792(16) 0.30487(11) 0.55237(8) 0.0320(3) Uani 1 1 d . . . C1S C -0.2807(6) 0.3703(5) 0.4982(3) 0.0264(13) Uani 1 1 d . . . H1S H -0.3474 0.3202 0.4653 0.032 Uiso 1 1 calc R . . Cl2S Cl -0.35314(14) 0.44315(11) 0.54119(8) 0.0320(4) Uani 1 1 d . . . C2S C 0.8673(7) 0.7845(6) 0.2558(4) 0.0459(19) Uani 1 1 d . . . H2S H 0.7908 0.7328 0.2315 0.055 Uiso 1 1 calc R . . Cl3S Cl -0.18785(17) 0.44667(13) 0.45756(8) 0.0391(4) Uani 1 1 d . . . C3S C 0.7619(11) 0.2033(8) -0.0547(6) 0.022(2) Uiso 0.50 1 d P . . H3S H 0.7532 0.2563 -0.0227 0.027 Uiso 0.50 1 calc PR A 1 Cl4S Cl 0.9417(3) 0.8363(3) 0.19919(11) 0.0996(12) Uani 1 1 d . . . C4S C 0.9358(10) 0.6233(8) 0.0614(5) 0.017(2) Uiso 0.50 1 d P . . Cl5S Cl 0.96409(15) 0.72561(12) 0.31069(10) 0.0442(4) Uani 1 1 d . . . C5S C 0.9417(14) 0.6457(11) -0.0210(7) 0.042(3) Uiso 0.50 1 d P . . Cl6S Cl 0.81883(19) 0.87846(14) 0.29746(12) 0.0587(6) Uani 1 1 d . . . O1S O 0.9458(7) 0.5539(7) -0.0604(4) 0.0171(17) Uiso 0.50 1 d P . . Cl7S Cl 0.6150(8) 0.1834(7) -0.1115(4) 0.045(2) Uiso 0.25 1 d P B 1 Cl8S Cl 0.8746(11) 0.2714(9) -0.0848(6) 0.080(3) Uiso 0.25 1 d P . 1 Cl9S Cl 0.7888(8) 0.1088(5) -0.0041(3) 0.0296(16) Uiso 0.25 1 d P B 1 O2S O 0.9202(8) 0.5077(9) -0.0551(4) 0.0246(19) Uiso 0.50 1 d P . . C7S C 0.9411(17) 0.5244(13) 0.0107(9) 0.057(4) Uiso 0.50 1 d P . . C6S C 0.9092(11) 0.4504(11) -0.0637(6) 0.024(3) Uiso 0.50 1 d P . . H2N H 0.489(6) 0.288(5) 0.330(3) 0.019(15) Uiso 1 1 d . . . Cl10 Cl 0.6239(7) 0.1465(6) -0.1071(4) 0.0353(17) Uiso 0.25 1 d P B 2 Cl11 Cl 0.8431(10) 0.2023(8) -0.1216(5) 0.070(2) Uiso 0.25 1 d P B 2 Cl12 Cl 0.8337(8) 0.1251(5) -0.0067(3) 0.0292(16) Uiso 0.25 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0199(2) 0.0193(2) 0.0143(2) 0.00366(17) 0.00344(18) 0.00434(18) Cl1 0.0310(8) 0.0210(7) 0.0211(7) 0.0042(5) 0.0044(6) 0.0028(6) P1 0.0161(7) 0.0179(7) 0.0149(7) 0.0023(5) 0.0050(5) 0.0044(5) O1 0.0171(19) 0.0188(19) 0.019(2) 0.0029(15) 0.0059(15) 0.0047(15) N1 0.025(3) 0.017(2) 0.024(3) 0.0014(19) 0.010(2) 0.004(2) C1 0.021(3) 0.018(3) 0.014(3) -0.001(2) 0.003(2) 0.008(2) Ru2 0.0144(2) 0.0148(2) 0.0182(2) 0.00355(17) 0.00175(17) 0.00310(17) Cl2 0.0270(7) 0.0290(7) 0.0192(7) 0.0028(6) 0.0078(6) 0.0067(6) P2 0.0161(7) 0.0164(7) 0.0168(7) 0.0024(5) 0.0040(5) 0.0053(5) N2 0.018(2) 0.015(2) 0.026(3) 0.0056(19) 0.011(2) 0.0073(19) C2 0.023(3) 0.022(3) 0.024(3) 0.005(2) 0.010(2) 0.007(2) Cl3 0.0253(7) 0.0177(6) 0.0199(7) 0.0022(5) 0.0008(5) 0.0048(5) C3 0.025(3) 0.017(3) 0.031(3) 0.001(2) 0.009(3) -0.001(2) Cl4 0.0185(7) 0.0203(6) 0.0290(7) 0.0073(5) 0.0081(6) 0.0051(5) C4 0.033(3) 0.019(3) 0.026(3) -0.002(2) 0.012(3) 0.008(2) C5 0.017(3) 0.017(3) 0.016(3) 0.004(2) 0.003(2) 0.002(2) C6 0.019(3) 0.019(3) 0.020(3) 0.005(2) 0.007(2) 0.004(2) C7 0.018(3) 0.018(3) 0.019(3) 0.000(2) 0.006(2) 0.006(2) C8 0.026(3) 0.028(3) 0.022(3) 0.002(2) 0.007(2) 0.004(3) C9 0.021(3) 0.033(3) 0.036(4) 0.009(3) 0.013(3) 0.003(3) C10 0.018(3) 0.022(3) 0.042(4) -0.001(3) 0.005(3) 0.005(2) C11 0.024(3) 0.020(3) 0.029(3) 0.006(2) 0.002(3) 0.007(2) C12 0.023(3) 0.017(3) 0.022(3) 0.003(2) 0.006(2) 0.007(2) C13 0.018(3) 0.021(3) 0.017(3) 0.001(2) 0.002(2) 0.007(2) C14 0.025(3) 0.026(3) 0.025(3) 0.005(2) 0.010(2) 0.008(2) C15 0.032(3) 0.031(3) 0.032(3) 0.002(3) 0.011(3) 0.016(3) C16 0.036(4) 0.023(3) 0.027(3) 0.000(2) 0.007(3) 0.012(3) C17 0.037(4) 0.021(3) 0.026(3) 0.003(2) 0.010(3) 0.002(3) C18 0.024(3) 0.022(3) 0.022(3) 0.004(2) 0.009(2) 0.009(2) C19 0.021(3) 0.017(3) 0.022(3) 0.010(2) 0.009(2) 0.008(2) C20 0.020(3) 0.020(3) 0.023(3) 0.005(2) 0.006(2) 0.006(2) C21 0.028(3) 0.028(3) 0.027(3) 0.003(3) 0.013(3) 0.009(3) C22 0.019(3) 0.030(3) 0.036(3) 0.010(3) 0.015(3) 0.013(2) C23 0.017(3) 0.025(3) 0.032(3) 0.011(2) 0.008(2) 0.007(2) C24 0.023(3) 0.017(3) 0.025(3) 0.005(2) 0.010(2) 0.009(2) C25 0.017(3) 0.024(3) 0.015(3) 0.002(2) 0.002(2) -0.001(2) C26 0.022(3) 0.039(4) 0.024(3) 0.011(3) 0.006(2) 0.006(3) C27 0.023(3) 0.066(5) 0.024(3) 0.016(3) 0.002(3) 0.011(3) C28 0.029(4) 0.069(5) 0.019(3) 0.000(3) 0.006(3) -0.001(3) C29 0.041(4) 0.043(4) 0.027(4) -0.006(3) 0.015(3) -0.001(3) C30 0.030(3) 0.025(3) 0.030(3) 0.000(3) 0.013(3) 0.004(3) C31 0.015(3) 0.031(3) 0.023(3) -0.001(2) 0.002(2) 0.005(2) C32 0.019(3) 0.033(3) 0.023(3) 0.007(3) 0.007(2) 0.004(2) C33 0.021(3) 0.023(3) 0.023(3) 0.005(2) 0.002(2) 0.000(2) C34 0.023(3) 0.026(3) 0.020(3) -0.001(2) 0.000(2) 0.000(2) C35 0.021(3) 0.036(3) 0.016(3) 0.006(2) 0.000(2) 0.005(3) C36 0.021(3) 0.028(3) 0.025(3) 0.006(2) 0.003(2) 0.009(2) C37 0.032(4) 0.043(4) 0.025(3) 0.002(3) 0.005(3) 0.018(3) C38 0.035(4) 0.028(3) 0.028(3) -0.003(3) 0.003(3) 0.005(3) C39 0.061(5) 0.030(4) 0.037(4) -0.008(3) -0.003(4) 0.018(3) C40 0.048(4) 0.045(4) 0.026(4) -0.009(3) -0.001(3) 0.005(3) C41 0.029(3) 0.019(3) 0.030(3) 0.012(2) 0.010(3) 0.001(2) C42 0.025(3) 0.019(3) 0.027(3) 0.010(2) 0.002(2) 0.000(2) C43 0.024(3) 0.016(3) 0.034(3) 0.007(2) 0.004(3) 0.000(2) C44 0.024(3) 0.014(3) 0.032(3) 0.000(2) 0.008(3) 0.001(2) C45 0.023(3) 0.015(3) 0.024(3) -0.001(2) -0.001(2) -0.001(2) C46 0.018(3) 0.015(3) 0.033(3) 0.008(2) 0.004(2) 0.000(2) C47 0.035(4) 0.035(4) 0.039(4) 0.008(3) 0.017(3) 0.002(3) C48 0.037(4) 0.015(3) 0.039(4) 0.000(3) 0.013(3) 0.004(3) C49 0.043(4) 0.024(3) 0.055(5) 0.008(3) 0.024(4) 0.014(3) C50 0.048(4) 0.031(4) 0.067(5) -0.016(4) 0.024(4) 0.007(3) Cl1S 0.0428(9) 0.0298(8) 0.0297(8) 0.0100(6) 0.0156(7) 0.0130(7) C1S 0.025(3) 0.029(3) 0.025(3) 0.000(2) 0.006(3) 0.009(3) Cl2S 0.0261(8) 0.0312(8) 0.0398(9) -0.0079(7) 0.0132(7) 0.0070(6) C2S 0.035(4) 0.042(4) 0.044(4) 0.001(3) -0.005(3) -0.009(3) Cl3S 0.0502(10) 0.0467(10) 0.0341(9) 0.0186(7) 0.0233(8) 0.0231(8) Cl4S 0.0674(16) 0.163(3) 0.0297(11) 0.0130(14) -0.0073(10) -0.0387(18) Cl5S 0.0258(8) 0.0295(8) 0.0737(13) 0.0056(8) 0.0083(8) 0.0048(7) Cl6S 0.0432(11) 0.0312(9) 0.0913(17) 0.0069(10) -0.0006(10) 0.0090(8) _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 C33 2.191(6) . ? Ru1 C32 2.190(6) . ? Ru1 C31 2.218(6) . ? Ru1 C34 2.222(6) . ? Ru1 C36 2.256(6) . ? Ru1 C35 2.266(6) . ? Ru1 P1 2.3119(14) . ? Ru1 Cl1 2.4130(14) . ? Ru1 Cl2 2.4263(15) . ? P1 O1 1.644(4) . ? P1 C13 1.812(6) . ? P1 C7 1.815(5) . ? O1 C1 1.393(6) . ? N1 C5 1.339(7) . ? N1 C4 1.340(7) . ? C1 C2 1.372(8) . ? C1 C5 1.409(8) . ? Ru2 C46 2.184(5) . ? Ru2 C45 2.193(5) . ? Ru2 C41 2.201(6) . ? Ru2 C44 2.235(6) . ? Ru2 C42 2.259(5) . ? Ru2 C43 2.278(6) . ? Ru2 P2 2.3443(14) . ? Ru2 Cl3 2.4076(14) . ? Ru2 Cl4 2.4327(14) . ? P2 C19 1.821(6) . ? P2 C25 1.831(6) . ? P2 C6 1.838(5) . ? N2 C5 1.385(7) . ? N2 C6 1.468(7) . ? C2 C3 1.390(8) . ? C3 C4 1.386(8) . ? C7 C8 1.398(8) . ? C7 C12 1.410(8) . ? C8 C9 1.397(9) . ? C9 C10 1.388(9) . ? C10 C11 1.385(9) . ? C11 C12 1.380(8) . ? C13 C14 1.395(8) . ? C13 C18 1.411(8) . ? C14 C15 1.392(9) . ? C15 C16 1.381(9) . ? C16 C17 1.382(9) . ? C17 C18 1.384(8) . ? C19 C20 1.403(8) . ? C19 C24 1.403(8) . ? C20 C21 1.384(8) . ? C21 C22 1.395(9) . ? C22 C23 1.386(9) . ? C23 C24 1.385(8) . ? C25 C30 1.394(9) . ? C25 C26 1.399(8) . ? C26 C27 1.398(9) . ? C27 C28 1.373(11) . ? C28 C29 1.378(11) . ? C29 C30 1.378(9) . ? C31 C32 1.404(8) . ? C31 C36 1.432(8) . ? C31 C37 1.504(9) . ? C32 C33 1.423(9) . ? C33 C34 1.415(8) . ? C34 C35 1.428(8) . ? C34 C38 1.529(9) . ? C35 C36 1.388(9) . ? C38 C39 1.518(9) . ? C38 C40 1.536(9) . ? C41 C46 1.410(8) . ? C41 C42 1.425(9) . ? C41 C47 1.513(9) . ? C42 C43 1.384(9) . ? C43 C44 1.439(9) . ? C44 C45 1.409(8) . ? C44 C48 1.516(9) . ? C45 C46 1.417(9) . ? C48 C49 1.528(10) . ? C48 C50 1.542(9) . ? Cl1S C1S 1.768(6) . ? C1S Cl2S 1.757(6) . ? C1S Cl3S 1.760(6) . ? C2S Cl5S 1.743(8) . ? C2S Cl4S 1.752(8) . ? C2S Cl6S 1.765(9) . ? C3S Cl10 1.678(13) . ? C3S Cl12 1.706(13) . ? C3S Cl8S 1.712(16) . ? C3S Cl7S 1.750(14) . ? C3S Cl9S 1.759(13) . ? C3S Cl11 1.888(16) . ? C4S C7S 1.70(2) . ? C4S C5S 1.823(18) . ? C4S Cl8S 2.249(16) 2_765 ? C5S O1S 1.481(17) . ? C5S C7S 1.83(2) . ? C5S O2S 1.924(19) . ? O1S O2S 0.671(9) . ? O1S C6S 1.386(14) . ? O1S C7S 1.612(19) . ? Cl8S C4S 2.249(16) 2_765 ? O2S C6S 0.770(12) . ? O2S C7S 1.36(2) . ? O2S C7S 1.76(2) 2_765 ? C7S C6S 1.74(2) 2_765 ? C7S C6S 1.74(2) . ? C7S C7S 1.74(4) 2_765 ? C7S O2S 1.76(2) 2_765 ? C6S C7S 1.74(2) 2_765 ? 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 C33 Ru1 C32 37.9(2) . . ? C33 Ru1 C31 68.1(2) . . ? C32 Ru1 C31 37.1(2) . . ? C33 Ru1 C34 37.4(2) . . ? C32 Ru1 C34 67.7(2) . . ? C31 Ru1 C34 80.5(2) . . ? C33 Ru1 C36 78.6(2) . . ? C32 Ru1 C36 66.1(2) . . ? C31 Ru1 C36 37.3(2) . . ? C34 Ru1 C36 66.5(2) . . ? C33 Ru1 C35 66.3(2) . . ? C32 Ru1 C35 77.8(2) . . ? C31 Ru1 C35 66.4(2) . . ? C34 Ru1 C35 37.1(2) . . ? C36 Ru1 C35 35.7(2) . . ? C33 Ru1 P1 93.13(15) . . ? C32 Ru1 P1 91.88(16) . . ? C31 Ru1 P1 116.28(16) . . ? C34 Ru1 P1 120.24(16) . . ? C36 Ru1 P1 153.52(16) . . ? C35 Ru1 P1 157.27(16) . . ? C33 Ru1 Cl1 157.98(17) . . ? C32 Ru1 Cl1 120.38(17) . . ? C31 Ru1 Cl1 90.70(15) . . ? C34 Ru1 Cl1 148.30(15) . . ? C36 Ru1 Cl1 88.13(16) . . ? C35 Ru1 Cl1 111.70(16) . . ? P1 Ru1 Cl1 91.00(5) . . ? C33 Ru1 Cl2 113.07(17) . . ? C32 Ru1 Cl2 150.76(17) . . ? C31 Ru1 Cl2 158.33(16) . . ? C34 Ru1 Cl2 88.59(16) . . ? C36 Ru1 Cl2 121.03(16) . . ? C35 Ru1 Cl2 93.79(16) . . ? P1 Ru1 Cl2 85.39(5) . . ? Cl1 Ru1 Cl2 88.81(5) . . ? O1 P1 C13 96.2(2) . . ? O1 P1 C7 103.1(2) . . ? C13 P1 C7 103.0(2) . . ? O1 P1 Ru1 113.81(14) . . ? C13 P1 Ru1 113.71(18) . . ? C7 P1 Ru1 123.18(18) . . ? C1 O1 P1 123.5(3) . . ? C5 N1 C4 118.2(5) . . ? C2 C1 O1 124.4(5) . . ? C2 C1 C5 119.5(5) . . ? O1 C1 C5 116.0(5) . . ? C46 Ru2 C45 37.8(2) . . ? C46 Ru2 C41 37.5(2) . . ? C45 Ru2 C41 68.0(2) . . ? C46 Ru2 C44 67.7(2) . . ? C45 Ru2 C44 37.1(2) . . ? C41 Ru2 C44 80.5(2) . . ? C46 Ru2 C42 66.3(2) . . ? C45 Ru2 C42 78.1(2) . . ? C41 Ru2 C42 37.2(2) . . ? C44 Ru2 C42 66.2(2) . . ? C46 Ru2 C43 78.0(2) . . ? C45 Ru2 C43 66.0(2) . . ? C41 Ru2 C43 66.3(2) . . ? C44 Ru2 C43 37.2(2) . . ? C42 Ru2 C43 35.5(2) . . ? C46 Ru2 P2 91.37(15) . . ? C45 Ru2 P2 94.97(15) . . ? C41 Ru2 P2 114.71(16) . . ? C44 Ru2 P2 122.64(16) . . ? C42 Ru2 P2 151.74(16) . . ? C43 Ru2 P2 159.65(16) . . ? C46 Ru2 Cl3 117.19(17) . . ? C45 Ru2 Cl3 154.98(16) . . ? C41 Ru2 Cl3 89.89(17) . . ? C44 Ru2 Cl3 153.95(16) . . ? C42 Ru2 Cl3 91.58(16) . . ? C43 Ru2 Cl3 116.89(16) . . ? P2 Ru2 Cl3 83.38(5) . . ? C46 Ru2 Cl4 155.97(17) . . ? C45 Ru2 Cl4 118.43(16) . . ? C41 Ru2 Cl4 157.24(16) . . ? C44 Ru2 Cl4 93.04(15) . . ? C42 Ru2 Cl4 120.34(16) . . ? C43 Ru2 Cl4 95.44(16) . . ? P2 Ru2 Cl4 87.20(5) . . ? Cl3 Ru2 Cl4 86.49(5) . . ? C19 P2 C25 104.4(3) . . ? C19 P2 C6 102.6(2) . . ? C25 P2 C6 102.0(2) . . ? C19 P2 Ru2 109.22(17) . . ? C25 P2 Ru2 117.83(19) . . ? C6 P2 Ru2 118.93(18) . . ? C5 N2 C6 117.4(4) . . ? C1 C2 C3 118.6(5) . . ? C4 C3 C2 118.7(5) . . ? N1 C4 C3 123.2(5) . . ? N1 C5 N2 118.2(5) . . ? N1 C5 C1 121.8(5) . . ? N2 C5 C1 119.9(5) . . ? N2 C6 P2 111.8(4) . . ? C8 C7 C12 118.8(5) . . ? C8 C7 P1 123.1(4) . . ? C12 C7 P1 118.1(4) . . ? C9 C8 C7 120.0(6) . . ? C10 C9 C8 120.6(6) . . ? C11 C10 C9 119.4(6) . . ? C12 C11 C10 120.8(6) . . ? C11 C12 C7 120.4(5) . . ? C14 C13 C18 119.1(5) . . ? C14 C13 P1 120.1(4) . . ? C18 C13 P1 120.7(4) . . ? C15 C14 C13 120.2(5) . . ? C16 C15 C14 120.3(6) . . ? C15 C16 C17 120.0(6) . . ? C16 C17 C18 120.8(6) . . ? C17 C18 C13 119.6(6) . . ? C20 C19 C24 118.9(5) . . ? C20 C19 P2 119.7(4) . . ? C24 C19 P2 121.2(4) . . ? C21 C20 C19 120.0(5) . . ? C20 C21 C22 120.8(6) . . ? C23 C22 C21 119.3(5) . . ? C24 C23 C22 120.6(5) . . ? C23 C24 C19 120.4(5) . . ? C30 C25 C26 119.5(5) . . ? C30 C25 P2 120.4(4) . . ? C26 C25 P2 120.1(5) . . ? C27 C26 C25 119.0(6) . . ? C28 C27 C26 120.5(6) . . ? C27 C28 C29 120.4(6) . . ? C30 C29 C28 120.1(7) . . ? C29 C30 C25 120.4(6) . . ? C32 C31 C36 117.7(5) . . ? C32 C31 C37 122.5(5) . . ? C36 C31 C37 119.8(5) . . ? C32 C31 Ru1 70.4(3) . . ? C36 C31 Ru1 72.8(3) . . ? C37 C31 Ru1 129.0(4) . . ? C31 C32 C33 121.7(5) . . ? C31 C32 Ru1 72.5(3) . . ? C33 C32 Ru1 71.1(3) . . ? C34 C33 C32 120.1(5) . . ? C34 C33 Ru1 72.5(3) . . ? C32 C33 Ru1 71.0(3) . . ? C33 C34 C35 118.0(5) . . ? C33 C34 C38 122.5(5) . . ? C35 C34 C38 119.4(5) . . ? C33 C34 Ru1 70.1(3) . . ? C35 C34 Ru1 73.2(3) . . ? C38 C34 Ru1 130.4(4) . . ? C36 C35 C34 121.4(5) . . ? C36 C35 Ru1 71.7(3) . . ? C34 C35 Ru1 69.8(3) . . ? C35 C36 C31 121.0(5) . . ? C35 C36 Ru1 72.5(3) . . ? C31 C36 Ru1 69.9(3) . . ? C39 C38 C34 114.8(5) . . ? C39 C38 C40 112.1(6) . . ? C34 C38 C40 107.4(5) . . ? C46 C41 C42 117.9(6) . . ? C46 C41 C47 121.7(6) . . ? C42 C41 C47 120.4(6) . . ? C46 C41 Ru2 70.6(3) . . ? C42 C41 Ru2 73.6(3) . . ? C47 C41 Ru2 127.3(4) . . ? C43 C42 C41 121.5(5) . . ? C43 C42 Ru2 73.0(3) . . ? C41 C42 Ru2 69.2(3) . . ? C42 C43 C44 120.9(6) . . ? C42 C43 Ru2 71.5(3) . . ? C44 C43 Ru2 69.8(3) . . ? C45 C44 C43 117.6(5) . . ? C45 C44 C48 121.3(5) . . ? C43 C44 C48 120.6(5) . . ? C45 C44 Ru2 69.8(3) . . ? C43 C44 Ru2 73.0(3) . . ? C48 C44 Ru2 134.7(4) . . ? C44 C45 C46 121.1(5) . . ? C44 C45 Ru2 73.1(3) . . ? C46 C45 Ru2 70.8(3) . . ? C41 C46 C45 120.8(5) . . ? C41 C46 Ru2 71.9(3) . . ? C45 C46 Ru2 71.4(3) . . ? C44 C48 C49 115.1(6) . . ? C44 C48 C50 107.6(5) . . ? C49 C48 C50 109.0(5) . . ? Cl2S C1S Cl3S 110.6(3) . . ? Cl2S C1S Cl1S 109.9(3) . . ? Cl3S C1S Cl1S 110.3(3) . . ? Cl5S C2S Cl4S 111.6(5) . . ? Cl5S C2S Cl6S 110.5(4) . . ? Cl4S C2S Cl6S 110.2(4) . . ? Cl10 C3S Cl12 114.3(7) . . ? Cl10 C3S Cl8S 118.3(8) . . ? Cl12 C3S Cl8S 106.2(8) . . ? Cl10 C3S Cl7S 18.1(3) . . ? Cl12 C3S Cl7S 131.8(8) . . ? Cl8S C3S Cl7S 110.0(8) . . ? Cl10 C3S Cl9S 100.9(7) . . ? Cl12 C3S Cl9S 17.5(3) . . ? Cl8S C3S Cl9S 123.6(8) . . ? Cl7S C3S Cl9S 117.2(7) . . ? Cl10 C3S Cl11 91.0(7) . . ? Cl12 C3S Cl11 100.1(7) . . ? Cl8S C3S Cl11 36.0(5) . . ? Cl7S C3S Cl11 91.3(7) . . ? Cl9S C3S Cl11 112.7(7) . . ? C7S C4S C5S 62.5(9) . . ? C7S C4S Cl8S 106.5(9) . 2_765 ? C5S C4S Cl8S 80.9(7) . 2_765 ? O1S C5S C4S 112.4(10) . . ? O1S C5S C7S 57.1(8) . . ? C4S C5S C7S 55.4(8) . . ? O1S C5S O2S 17.2(4) . . ? C4S C5S O2S 97.2(8) . . ? C7S C5S O2S 42.5(7) . . ? O2S O1S C6S 17.1(10) . . ? O2S O1S C5S 122.1(14) . . ? C6S O1S C5S 139.2(10) . . ? O2S O1S C7S 56.7(12) . . ? C6S O1S C7S 70.8(9) . . ? C5S O1S C7S 72.4(9) . . ? C3S Cl8S C4S 146.4(8) . 2_765 ? O1S O2S C6S 148.0(19) . . ? O1S O2S C7S 99.0(15) . . ? C6S O2S C7S 106.3(15) . . ? O1S O2S C7S 98.2(12) . 2_765 ? C6S O2S C7S 75.1(13) . 2_765 ? C7S O2S C7S 66.3(12) . 2_765 ? O1S O2S C5S 40.7(11) . . ? C6S O2S C5S 170.9(14) . . ? C7S O2S C5S 65.0(10) . . ? C7S O2S C5S 102.8(9) 2_765 . ? O2S C7S O1S 24.3(5) . . ? O2S C7S C4S 133.1(14) . . ? O1S C7S C4S 112.6(11) . . ? O2S C7S C6S 122.2(13) . 2_765 ? O1S C7S C6S 110.8(11) . 2_765 ? C4S C7S C6S 78.7(10) . 2_765 ? O2S C7S C6S 25.0(6) . . ? O1S C7S C6S 48.6(7) . . ? C4S C7S C6S 155.9(13) . . ? C6S C7S C6S 119.8(11) 2_765 . ? O2S C7S C7S 67.9(12) . 2_765 ? O1S C7S C7S 72.0(12) . 2_765 ? C4S C7S C7S 135.8(17) . 2_765 ? C6S C7S C7S 60.2(11) 2_765 2_765 ? C6S C7S C7S 59.6(11) . 2_765 ? O2S C7S O2S 113.7(12) . 2_765 ? O1S C7S O2S 113.5(11) . 2_765 ? C4S C7S O2S 100.4(11) . 2_765 ? C6S C7S O2S 25.4(5) 2_765 2_765 ? C6S C7S O2S 101.6(10) . 2_765 ? C7S C7S O2S 45.8(9) 2_765 2_765 ? O2S C7S C5S 72.4(10) . . ? O1S C7S C5S 50.5(8) . . ? C4S C7S C5S 62.1(8) . . ? C6S C7S C5S 100.1(11) 2_765 . ? C6S C7S C5S 97.4(11) . . ? C7S C7S C5S 107.7(15) 2_765 . ? O2S C7S C5S 122.2(11) 2_765 . ? O2S C6S O1S 14.9(9) . . ? O2S C6S C7S 79.5(13) . 2_765 ? O1S C6S C7S 77.7(9) . 2_765 ? O2S C6S C7S 48.6(12) . . ? O1S C6S C7S 60.7(9) . . ? C7S C6S C7S 60.2(11) 2_765 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C33 Ru1 P1 O1 -62.4(2) . . . . ? C32 Ru1 P1 O1 -24.5(2) . . . . ? C31 Ru1 P1 O1 4.7(2) . . . . ? C34 Ru1 P1 O1 -89.6(2) . . . . ? C36 Ru1 P1 O1 8.2(4) . . . . ? C35 Ru1 P1 O1 -86.5(4) . . . . ? Cl1 Ru1 P1 O1 95.98(15) . . . . ? Cl2 Ru1 P1 O1 -175.29(16) . . . . ? C33 Ru1 P1 C13 46.5(3) . . . . ? C32 Ru1 P1 C13 84.4(3) . . . . ? C31 Ru1 P1 C13 113.6(3) . . . . ? C34 Ru1 P1 C13 19.2(3) . . . . ? C36 Ru1 P1 C13 117.0(4) . . . . ? C35 Ru1 P1 C13 22.3(5) . . . . ? Cl1 Ru1 P1 C13 -155.2(2) . . . . ? Cl2 Ru1 P1 C13 -66.4(2) . . . . ? C33 Ru1 P1 C7 171.9(3) . . . . ? C32 Ru1 P1 C7 -150.2(3) . . . . ? C31 Ru1 P1 C7 -121.0(3) . . . . ? C34 Ru1 P1 C7 144.7(3) . . . . ? C36 Ru1 P1 C7 -117.6(4) . . . . ? C35 Ru1 P1 C7 147.8(5) . . . . ? Cl1 Ru1 P1 C7 -29.7(2) . . . . ? Cl2 Ru1 P1 C7 59.0(2) . . . . ? C13 P1 O1 C1 -176.3(4) . . . . ? C7 P1 O1 C1 78.8(4) . . . . ? Ru1 P1 O1 C1 -56.9(4) . . . . ? P1 O1 C1 C2 -37.4(7) . . . . ? P1 O1 C1 C5 145.6(4) . . . . ? C46 Ru2 P2 C19 37.6(3) . . . . ? C45 Ru2 P2 C19 75.3(3) . . . . ? C41 Ru2 P2 C19 7.2(3) . . . . ? C44 Ru2 P2 C19 101.8(3) . . . . ? C42 Ru2 P2 C19 1.3(4) . . . . ? C43 Ru2 P2 C19 95.5(5) . . . . ? Cl3 Ru2 P2 C19 -79.6(2) . . . . ? Cl4 Ru2 P2 C19 -166.4(2) . . . . ? C46 Ru2 P2 C25 -81.2(3) . . . . ? C45 Ru2 P2 C25 -43.5(3) . . . . ? C41 Ru2 P2 C25 -111.6(3) . . . . ? C44 Ru2 P2 C25 -17.0(3) . . . . ? C42 Ru2 P2 C25 -117.5(4) . . . . ? C43 Ru2 P2 C25 -23.3(5) . . . . ? Cl3 Ru2 P2 C25 161.6(2) . . . . ? Cl4 Ru2 P2 C25 74.8(2) . . . . ? C46 Ru2 P2 C6 154.7(3) . . . . ? C45 Ru2 P2 C6 -167.6(3) . . . . ? C41 Ru2 P2 C6 124.3(3) . . . . ? C44 Ru2 P2 C6 -141.1(3) . . . . ? C42 Ru2 P2 C6 118.5(4) . . . . ? C43 Ru2 P2 C6 -147.4(5) . . . . ? Cl3 Ru2 P2 C6 37.5(2) . . . . ? Cl4 Ru2 P2 C6 -49.3(2) . . . . ? O1 C1 C2 C3 -177.5(5) . . . . ? C5 C1 C2 C3 -0.6(8) . . . . ? C1 C2 C3 C4 -0.3(9) . . . . ? C5 N1 C4 C3 -0.2(9) . . . . ? C2 C3 C4 N1 0.7(9) . . . . ? C4 N1 C5 N2 -178.0(5) . . . . ? C4 N1 C5 C1 -0.7(8) . . . . ? C6 N2 C5 N1 -4.2(7) . . . . ? C6 N2 C5 C1 178.5(5) . . . . ? C2 C1 C5 N1 1.2(8) . . . . ? O1 C1 C5 N1 178.3(5) . . . . ? C2 C1 C5 N2 178.3(5) . . . . ? O1 C1 C5 N2 -4.5(7) . . . . ? C5 N2 C6 P2 177.4(4) . . . . ? C19 P2 C6 N2 -161.6(4) . . . . ? C25 P2 C6 N2 -53.7(4) . . . . ? Ru2 P2 C6 N2 77.8(4) . . . . ? O1 P1 C7 C8 -153.8(5) . . . . ? C13 P1 C7 C8 106.6(5) . . . . ? Ru1 P1 C7 C8 -23.4(6) . . . . ? O1 P1 C7 C12 27.1(5) . . . . ? C13 P1 C7 C12 -72.5(5) . . . . ? Ru1 P1 C7 C12 157.4(3) . . . . ? C12 C7 C8 C9 0.3(9) . . . . ? P1 C7 C8 C9 -178.8(5) . . . . ? C7 C8 C9 C10 -0.6(9) . . . . ? C8 C9 C10 C11 -0.1(9) . . . . ? C9 C10 C11 C12 1.1(9) . . . . ? C10 C11 C12 C7 -1.4(9) . . . . ? C8 C7 C12 C11 0.7(8) . . . . ? P1 C7 C12 C11 179.8(4) . . . . ? O1 P1 C13 C14 -149.6(5) . . . . ? C7 P1 C13 C14 -44.6(5) . . . . ? Ru1 P1 C13 C14 90.9(5) . . . . ? O1 P1 C13 C18 34.4(5) . . . . ? C7 P1 C13 C18 139.4(5) . . . . ? Ru1 P1 C13 C18 -85.0(5) . . . . ? C18 C13 C14 C15 -0.7(9) . . . . ? P1 C13 C14 C15 -176.8(5) . . . . ? C13 C14 C15 C16 0.8(9) . . . . ? C14 C15 C16 C17 -0.7(9) . . . . ? C15 C16 C17 C18 0.4(9) . . . . ? C16 C17 C18 C13 -0.2(9) . . . . ? C14 C13 C18 C17 0.4(8) . . . . ? P1 C13 C18 C17 176.5(5) . . . . ? C25 P2 C19 C20 -154.7(4) . . . . ? C6 P2 C19 C20 -48.6(5) . . . . ? Ru2 P2 C19 C20 78.4(4) . . . . ? C25 P2 C19 C24 31.4(5) . . . . ? C6 P2 C19 C24 137.5(4) . . . . ? Ru2 P2 C19 C24 -95.5(4) . . . . ? C24 C19 C20 C21 0.3(8) . . . . ? P2 C19 C20 C21 -173.7(4) . . . . ? C19 C20 C21 C22 0.5(8) . . . . ? C20 C21 C22 C23 -1.1(9) . . . . ? C21 C22 C23 C24 0.8(8) . . . . ? C22 C23 C24 C19 0.1(8) . . . . ? C20 C19 C24 C23 -0.6(8) . . . . ? P2 C19 C24 C23 173.3(4) . . . . ? C19 P2 C25 C30 -135.8(5) . . . . ? C6 P2 C25 C30 117.6(5) . . . . ? Ru2 P2 C25 C30 -14.5(5) . . . . ? C19 P2 C25 C26 45.4(5) . . . . ? C6 P2 C25 C26 -61.2(5) . . . . ? Ru2 P2 C25 C26 166.7(4) . . . . ? C30 C25 C26 C27 2.4(8) . . . . ? P2 C25 C26 C27 -178.8(5) . . . . ? C25 C26 C27 C28 0.7(9) . . . . ? C26 C27 C28 C29 -3.1(10) . . . . ? C27 C28 C29 C30 2.4(10) . . . . ? C28 C29 C30 C25 0.8(10) . . . . ? C26 C25 C30 C29 -3.1(9) . . . . ? P2 C25 C30 C29 178.1(5) . . . . ? C33 Ru1 C31 C32 28.6(3) . . . . ? C34 Ru1 C31 C32 65.4(4) . . . . ? C36 Ru1 C31 C32 128.8(5) . . . . ? C35 Ru1 C31 C32 101.3(4) . . . . ? P1 Ru1 C31 C32 -53.8(4) . . . . ? Cl1 Ru1 C31 C32 -145.2(3) . . . . ? Cl2 Ru1 C31 C32 126.2(4) . . . . ? C33 Ru1 C31 C36 -100.2(4) . . . . ? C32 Ru1 C31 C36 -128.8(5) . . . . ? C34 Ru1 C31 C36 -63.4(3) . . . . ? C35 Ru1 C31 C36 -27.5(3) . . . . ? P1 Ru1 C31 C36 177.4(3) . . . . ? Cl1 Ru1 C31 C36 86.0(3) . . . . ? Cl2 Ru1 C31 C36 -2.6(6) . . . . ? C33 Ru1 C31 C37 145.0(6) . . . . ? C32 Ru1 C31 C37 116.4(7) . . . . ? C34 Ru1 C31 C37 -178.2(6) . . . . ? C36 Ru1 C31 C37 -114.8(7) . . . . ? C35 Ru1 C31 C37 -142.3(6) . . . . ? P1 Ru1 C31 C37 62.6(6) . . . . ? Cl1 Ru1 C31 C37 -28.8(5) . . . . ? Cl2 Ru1 C31 C37 -117.4(5) . . . . ? C36 C31 C32 C33 3.7(8) . . . . ? C37 C31 C32 C33 -177.9(5) . . . . ? Ru1 C31 C32 C33 -53.5(5) . . . . ? C36 C31 C32 Ru1 57.2(5) . . . . ? C37 C31 C32 Ru1 -124.4(5) . . . . ? C33 Ru1 C32 C31 -133.7(5) . . . . ? C34 Ru1 C32 C31 -104.3(4) . . . . ? C36 Ru1 C32 C31 -31.1(3) . . . . ? C35 Ru1 C32 C31 -66.8(3) . . . . ? P1 Ru1 C32 C31 133.7(3) . . . . ? Cl1 Ru1 C32 C31 41.4(4) . . . . ? Cl2 Ru1 C32 C31 -142.4(3) . . . . ? C31 Ru1 C32 C33 133.7(5) . . . . ? C34 Ru1 C32 C33 29.4(3) . . . . ? C36 Ru1 C32 C33 102.6(4) . . . . ? C35 Ru1 C32 C33 66.9(4) . . . . ? P1 Ru1 C32 C33 -92.7(3) . . . . ? Cl1 Ru1 C32 C33 175.1(3) . . . . ? Cl2 Ru1 C32 C33 -8.8(5) . . . . ? C31 C32 C33 C34 -1.4(9) . . . . ? Ru1 C32 C33 C34 -55.5(5) . . . . ? C31 C32 C33 Ru1 54.2(5) . . . . ? C32 Ru1 C33 C34 131.6(5) . . . . ? C31 Ru1 C33 C34 103.5(4) . . . . ? C36 Ru1 C33 C34 66.0(4) . . . . ? C35 Ru1 C33 C34 30.7(4) . . . . ? P1 Ru1 C33 C34 -139.4(3) . . . . ? Cl1 Ru1 C33 C34 120.2(4) . . . . ? Cl2 Ru1 C33 C34 -53.1(4) . . . . ? C31 Ru1 C33 C32 -28.1(3) . . . . ? C34 Ru1 C33 C32 -131.6(5) . . . . ? C36 Ru1 C33 C32 -65.6(3) . . . . ? C35 Ru1 C33 C32 -100.9(4) . . . . ? P1 Ru1 C33 C32 89.0(3) . . . . ? Cl1 Ru1 C33 C32 -11.4(6) . . . . ? Cl2 Ru1 C33 C32 175.4(3) . . . . ? C32 C33 C34 C35 -2.4(8) . . . . ? Ru1 C33 C34 C35 -57.2(5) . . . . ? C32 C33 C34 C38 -179.3(5) . . . . ? Ru1 C33 C34 C38 125.9(6) . . . . ? C32 C33 C34 Ru1 54.8(5) . . . . ? C32 Ru1 C34 C33 -29.8(3) . . . . ? C31 Ru1 C34 C33 -66.2(4) . . . . ? C36 Ru1 C34 C33 -102.4(4) . . . . ? C35 Ru1 C34 C33 -129.2(5) . . . . ? P1 Ru1 C34 C33 48.8(4) . . . . ? Cl1 Ru1 C34 C33 -141.9(3) . . . . ? Cl2 Ru1 C34 C33 132.6(3) . . . . ? C33 Ru1 C34 C35 129.2(5) . . . . ? C32 Ru1 C34 C35 99.4(4) . . . . ? C31 Ru1 C34 C35 63.0(4) . . . . ? C36 Ru1 C34 C35 26.8(3) . . . . ? P1 Ru1 C34 C35 178.0(3) . . . . ? Cl1 Ru1 C34 C35 -12.7(5) . . . . ? Cl2 Ru1 C34 C35 -98.2(3) . . . . ? C33 Ru1 C34 C38 -116.2(7) . . . . ? C32 Ru1 C34 C38 -146.0(6) . . . . ? C31 Ru1 C34 C38 177.6(6) . . . . ? C36 Ru1 C34 C38 141.4(6) . . . . ? C35 Ru1 C34 C38 114.6(7) . . . . ? P1 Ru1 C34 C38 -67.4(6) . . . . ? Cl1 Ru1 C34 C38 101.9(6) . . . . ? Cl2 Ru1 C34 C38 16.4(5) . . . . ? C33 C34 C35 C36 3.7(8) . . . . ? C38 C34 C35 C36 -179.2(5) . . . . ? Ru1 C34 C35 C36 -51.9(5) . . . . ? C33 C34 C35 Ru1 55.7(5) . . . . ? C38 C34 C35 Ru1 -127.3(5) . . . . ? C33 Ru1 C35 C36 104.0(4) . . . . ? C32 Ru1 C35 C36 65.9(4) . . . . ? C31 Ru1 C35 C36 28.6(3) . . . . ? C34 Ru1 C35 C36 135.0(5) . . . . ? P1 Ru1 C35 C36 130.5(4) . . . . ? Cl1 Ru1 C35 C36 -52.2(4) . . . . ? Cl2 Ru1 C35 C36 -142.4(3) . . . . ? C33 Ru1 C35 C34 -30.9(4) . . . . ? C32 Ru1 C35 C34 -69.1(4) . . . . ? C31 Ru1 C35 C34 -106.3(4) . . . . ? C36 Ru1 C35 C34 -135.0(5) . . . . ? P1 Ru1 C35 C34 -4.5(7) . . . . ? Cl1 Ru1 C35 C34 172.9(3) . . . . ? Cl2 Ru1 C35 C34 82.6(3) . . . . ? C34 C35 C36 C31 -1.4(9) . . . . ? Ru1 C35 C36 C31 -52.5(5) . . . . ? C34 C35 C36 Ru1 51.1(5) . . . . ? C32 C31 C36 C35 -2.3(8) . . . . ? C37 C31 C36 C35 179.3(5) . . . . ? Ru1 C31 C36 C35 53.6(5) . . . . ? C32 C31 C36 Ru1 -56.0(5) . . . . ? C37 C31 C36 Ru1 125.6(5) . . . . ? C33 Ru1 C36 C35 -65.0(4) . . . . ? C32 Ru1 C36 C35 -102.7(4) . . . . ? C31 Ru1 C36 C35 -133.6(5) . . . . ? C34 Ru1 C36 C35 -27.7(3) . . . . ? P1 Ru1 C36 C35 -138.8(3) . . . . ? Cl1 Ru1 C36 C35 132.7(3) . . . . ? Cl2 Ru1 C36 C35 45.3(4) . . . . ? C33 Ru1 C36 C31 68.7(4) . . . . ? C32 Ru1 C36 C31 31.0(3) . . . . ? C34 Ru1 C36 C31 105.9(4) . . . . ? C35 Ru1 C36 C31 133.6(5) . . . . ? P1 Ru1 C36 C31 -5.1(6) . . . . ? Cl1 Ru1 C36 C31 -93.6(3) . . . . ? Cl2 Ru1 C36 C31 178.9(3) . . . . ? C33 C34 C38 C39 -23.8(9) . . . . ? C35 C34 C38 C39 159.3(6) . . . . ? Ru1 C34 C38 C39 66.9(8) . . . . ? C33 C34 C38 C40 101.6(7) . . . . ? C35 C34 C38 C40 -75.3(7) . . . . ? Ru1 C34 C38 C40 -167.7(5) . . . . ? C45 Ru2 C41 C46 -29.1(3) . . . . ? C44 Ru2 C41 C46 -65.5(4) . . . . ? C42 Ru2 C41 C46 -128.4(5) . . . . ? C43 Ru2 C41 C46 -101.5(4) . . . . ? P2 Ru2 C41 C46 56.2(4) . . . . ? Cl3 Ru2 C41 C46 138.9(3) . . . . ? Cl4 Ru2 C41 C46 -140.5(4) . . . . ? C46 Ru2 C41 C42 128.4(5) . . . . ? C45 Ru2 C41 C42 99.3(4) . . . . ? C44 Ru2 C41 C42 62.9(4) . . . . ? C43 Ru2 C41 C42 26.9(3) . . . . ? P2 Ru2 C41 C42 -175.4(3) . . . . ? Cl3 Ru2 C41 C42 -92.8(3) . . . . ? Cl4 Ru2 C41 C42 -12.1(7) . . . . ? C46 Ru2 C41 C47 -115.6(7) . . . . ? C45 Ru2 C41 C47 -144.6(6) . . . . ? C44 Ru2 C41 C47 178.9(6) . . . . ? C42 Ru2 C41 C47 116.0(7) . . . . ? C43 Ru2 C41 C47 142.9(6) . . . . ? P2 Ru2 C41 C47 -59.4(6) . . . . ? Cl3 Ru2 C41 C47 23.3(5) . . . . ? Cl4 Ru2 C41 C47 103.9(6) . . . . ? C46 C41 C42 C43 3.6(8) . . . . ? C47 C41 C42 C43 -177.2(5) . . . . ? Ru2 C41 C42 C43 -53.1(5) . . . . ? C46 C41 C42 Ru2 56.8(4) . . . . ? C47 C41 C42 Ru2 -124.0(5) . . . . ? C46 Ru2 C42 C43 103.1(4) . . . . ? C45 Ru2 C42 C43 65.2(4) . . . . ? C41 Ru2 C42 C43 134.5(5) . . . . ? C44 Ru2 C42 C43 28.1(3) . . . . ? P2 Ru2 C42 C43 143.3(3) . . . . ? Cl3 Ru2 C42 C43 -137.7(3) . . . . ? Cl4 Ru2 C42 C43 -50.9(4) . . . . ? C46 Ru2 C42 C41 -31.4(4) . . . . ? C45 Ru2 C42 C41 -69.3(4) . . . . ? C44 Ru2 C42 C41 -106.4(4) . . . . ? C43 Ru2 C42 C41 -134.5(5) . . . . ? P2 Ru2 C42 C41 8.8(6) . . . . ? Cl3 Ru2 C42 C41 87.7(3) . . . . ? Cl4 Ru2 C42 C41 174.6(3) . . . . ? C41 C42 C43 C44 0.1(8) . . . . ? Ru2 C42 C43 C44 -51.3(5) . . . . ? C41 C42 C43 Ru2 51.4(5) . . . . ? C46 Ru2 C43 C42 -65.7(4) . . . . ? C45 Ru2 C43 C42 -103.5(4) . . . . ? C41 Ru2 C43 C42 -28.1(3) . . . . ? C44 Ru2 C43 C42 -134.4(5) . . . . ? P2 Ru2 C43 C42 -125.6(4) . . . . ? Cl3 Ru2 C43 C42 48.9(4) . . . . ? Cl4 Ru2 C43 C42 137.7(3) . . . . ? C46 Ru2 C43 C44 68.7(4) . . . . ? C45 Ru2 C43 C44 30.9(3) . . . . ? C41 Ru2 C43 C44 106.3(4) . . . . ? C42 Ru2 C43 C44 134.4(5) . . . . ? P2 Ru2 C43 C44 8.8(7) . . . . ? Cl3 Ru2 C43 C44 -176.7(3) . . . . ? Cl4 Ru2 C43 C44 -87.8(3) . . . . ? C42 C43 C44 C45 -3.4(8) . . . . ? Ru2 C43 C44 C45 -55.5(4) . . . . ? C42 C43 C44 C48 -175.5(5) . . . . ? Ru2 C43 C44 C48 132.4(5) . . . . ? C42 C43 C44 Ru2 52.1(5) . . . . ? C46 Ru2 C44 C45 29.1(3) . . . . ? C41 Ru2 C44 C45 65.9(4) . . . . ? C42 Ru2 C44 C45 102.0(4) . . . . ? C43 Ru2 C44 C45 128.9(5) . . . . ? P2 Ru2 C44 C45 -47.5(4) . . . . ? Cl3 Ru2 C44 C45 135.7(3) . . . . ? Cl4 Ru2 C44 C45 -136.1(3) . . . . ? C46 Ru2 C44 C43 -99.8(4) . . . . ? C45 Ru2 C44 C43 -128.9(5) . . . . ? C41 Ru2 C44 C43 -63.0(4) . . . . ? C42 Ru2 C44 C43 -27.0(3) . . . . ? P2 Ru2 C44 C43 -176.4(3) . . . . ? Cl3 Ru2 C44 C43 6.8(6) . . . . ? Cl4 Ru2 C44 C43 95.0(3) . . . . ? C46 Ru2 C44 C48 143.6(7) . . . . ? C45 Ru2 C44 C48 114.5(7) . . . . ? C41 Ru2 C44 C48 -179.6(6) . . . . ? C42 Ru2 C44 C48 -143.5(7) . . . . ? C43 Ru2 C44 C48 -116.6(7) . . . . ? P2 Ru2 C44 C48 67.1(6) . . . . ? Cl3 Ru2 C44 C48 -109.8(6) . . . . ? Cl4 Ru2 C44 C48 -21.5(6) . . . . ? C43 C44 C45 C46 2.9(8) . . . . ? C48 C44 C45 C46 175.0(5) . . . . ? Ru2 C44 C45 C46 -54.2(5) . . . . ? C43 C44 C45 Ru2 57.1(4) . . . . ? C48 C44 C45 Ru2 -130.8(5) . . . . ? C46 Ru2 C45 C44 -132.7(5) . . . . ? C41 Ru2 C45 C44 -103.8(4) . . . . ? C42 Ru2 C45 C44 -66.2(4) . . . . ? C43 Ru2 C45 C44 -31.0(3) . . . . ? P2 Ru2 C45 C44 141.5(3) . . . . ? Cl3 Ru2 C45 C44 -133.5(4) . . . . ? Cl4 Ru2 C45 C44 52.0(4) . . . . ? C41 Ru2 C45 C46 28.9(3) . . . . ? C44 Ru2 C45 C46 132.7(5) . . . . ? C42 Ru2 C45 C46 66.5(3) . . . . ? C43 Ru2 C45 C46 101.7(4) . . . . ? P2 Ru2 C45 C46 -85.8(3) . . . . ? Cl3 Ru2 C45 C46 -0.8(6) . . . . ? Cl4 Ru2 C45 C46 -175.3(3) . . . . ? C42 C41 C46 C45 -4.1(8) . . . . ? C47 C41 C46 C45 176.7(5) . . . . ? Ru2 C41 C46 C45 54.2(5) . . . . ? C42 C41 C46 Ru2 -58.3(4) . . . . ? C47 C41 C46 Ru2 122.5(5) . . . . ? C44 C45 C46 C41 0.8(8) . . . . ? Ru2 C45 C46 C41 -54.4(5) . . . . ? C44 C45 C46 Ru2 55.2(5) . . . . ? C45 Ru2 C46 C41 132.7(5) . . . . ? C44 Ru2 C46 C41 104.0(4) . . . . ? C42 Ru2 C46 C41 31.2(3) . . . . ? C43 Ru2 C46 C41 66.6(4) . . . . ? P2 Ru2 C46 C41 -131.0(3) . . . . ? Cl3 Ru2 C46 C41 -47.7(4) . . . . ? Cl4 Ru2 C46 C41 142.9(4) . . . . ? C41 Ru2 C46 C45 -132.7(5) . . . . ? C44 Ru2 C46 C45 -28.6(3) . . . . ? C42 Ru2 C46 C45 -101.5(4) . . . . ? C43 Ru2 C46 C45 -66.1(3) . . . . ? P2 Ru2 C46 C45 96.4(3) . . . . ? Cl3 Ru2 C46 C45 179.6(3) . . . . ? Cl4 Ru2 C46 C45 10.2(6) . . . . ? C45 C44 C48 C49 159.8(5) . . . . ? C43 C44 C48 C49 -28.3(8) . . . . ? Ru2 C44 C48 C49 67.9(8) . . . . ? C45 C44 C48 C50 -78.5(7) . . . . ? C43 C44 C48 C50 93.3(7) . . . . ? Ru2 C44 C48 C50 -170.4(5) . . . . ? C7S C4S C5S O1S 0.1(10) . . . . ? Cl8S C4S C5S O1S 114.2(10) 2_765 . . . ? Cl8S C4S C5S C7S 114.1(9) 2_765 . . . ? C7S C4S C5S O2S 8.2(8) . . . . ? Cl8S C4S C5S O2S 122.3(7) 2_765 . . . ? C4S C5S O1S O2S 28.4(19) . . . . ? C7S C5S O1S O2S 28.5(15) . . . . ? C4S C5S O1S C6S 26.3(19) . . . . ? C7S C5S O1S C6S 26.4(15) . . . . ? O2S C5S O1S C6S -2.1(13) . . . . ? C4S C5S O1S C7S -0.1(10) . . . . ? O2S C5S O1S C7S -28.5(15) . . . . ? Cl10 C3S Cl8S C4S 172.7(11) . . . 2_765 ? Cl12 C3S Cl8S C4S -57.3(17) . . . 2_765 ? Cl7S C3S Cl8S C4S 155.1(12) . . . 2_765 ? Cl9S C3S Cl8S C4S -59.4(18) . . . 2_765 ? Cl11 C3S Cl8S C4S -142.2(19) . . . 2_765 ? C5S O1S O2S C6S -175(3) . . . . ? C7S O1S O2S C6S -142(4) . . . . ? C6S O1S O2S C7S 142(4) . . . . ? C5S O1S O2S C7S -33.0(17) . . . . ? C6S O1S O2S C7S 75(3) . . . 2_765 ? C5S O1S O2S C7S -100.2(14) . . . 2_765 ? C7S O1S O2S C7S -67.2(13) . . . 2_765 ? C6S O1S O2S C5S 175(3) . . . . ? C7S O1S O2S C5S 33.0(17) . . . . ? C4S C5S O2S O1S -153.7(17) . . . . ? C7S C5S O2S O1S -143.6(19) . . . . ? O1S C5S O2S C6S 164(10) . . . . ? C4S C5S O2S C6S 10(9) . . . . ? C7S C5S O2S C6S 20(9) . . . . ? O1S C5S O2S C7S 143.6(19) . . . . ? C4S C5S O2S C7S -10.0(10) . . . . ? O1S C5S O2S C7S 87.7(16) . . . 2_765 ? C4S C5S O2S C7S -66.0(10) . . . 2_765 ? C7S C5S O2S C7S -55.9(13) . . . 2_765 ? C6S O2S C7S O1S 160(2) . . . . ? C7S O2S C7S O1S 95.1(15) 2_765 . . . ? C5S O2S C7S O1S -23.0(13) . . . . ? O1S O2S C7S C4S 38(2) . . . . ? C6S O2S C7S C4S -162.0(18) . . . . ? C7S O2S C7S C4S 133(2) 2_765 . . . ? C5S O2S C7S C4S 14.7(15) . . . . ? O1S O2S C7S C6S -67.9(17) . . . 2_765 ? C6S O2S C7S C6S 92.3(18) . . . 2_765 ? C7S O2S C7S C6S 27.2(7) 2_765 . . 2_765 ? C5S O2S C7S C6S -91.0(14) . . . 2_765 ? O1S O2S C7S C6S -160(2) . . . . ? C7S O2S C7S C6S -65.1(16) 2_765 . . . ? C5S O2S C7S C6S 176.7(15) . . . . ? O1S O2S C7S C7S -95.1(15) . . . 2_765 ? C6S O2S C7S C7S 65.1(16) . . . 2_765 ? C5S O2S C7S C7S -118.1(13) . . . 2_765 ? O1S O2S C7S O2S -95.1(15) . . . 2_765 ? C6S O2S C7S O2S 65.1(16) . . . 2_765 ? C7S O2S C7S O2S 0.000(1) 2_765 . . 2_765 ? C5S O2S C7S O2S -118.1(13) . . . 2_765 ? O1S O2S C7S C5S 23.0(12) . . . . ? C6S O2S C7S C5S -176.7(15) . . . . ? C7S O2S C7S C5S 118.1(13) 2_765 . . . ? C6S O1S C7S O2S -11.0(12) . . . . ? C5S O1S C7S O2S 151.1(16) . . . . ? O2S O1S C7S C4S -151.0(18) . . . . ? C6S O1S C7S C4S -162.0(13) . . . . ? C5S O1S C7S C4S 0.1(11) . . . . ? O2S O1S C7S C6S 123.0(16) . . . 2_765 ? C6S O1S C7S C6S 112.0(12) . . . 2_765 ? C5S O1S C7S C6S -85.9(12) . . . 2_765 ? O2S O1S C7S C6S 11.0(12) . . . . ? C5S O1S C7S C6S 162.1(10) . . . . ? O2S O1S C7S C7S 76.0(15) . . . 2_765 ? C6S O1S C7S C7S 65.0(11) . . . 2_765 ? C5S O1S C7S C7S -132.9(13) . . . 2_765 ? O2S O1S C7S O2S 95.7(15) . . . 2_765 ? C6S O1S C7S O2S 84.7(11) . . . 2_765 ? C5S O1S C7S O2S -113.2(13) . . . 2_765 ? O2S O1S C7S C5S -151.1(16) . . . . ? C6S O1S C7S C5S -162.1(10) . . . . ? C5S C4S C7S O2S -15.9(16) . . . . ? Cl8S C4S C7S O2S -86.0(18) 2_765 . . . ? C5S C4S C7S O1S -0.1(9) . . . . ? Cl8S C4S C7S O1S -70.2(12) 2_765 . . . ? C5S C4S C7S C6S 107.9(9) . . . 2_765 ? Cl8S C4S C7S C6S 37.8(9) 2_765 . . 2_765 ? C5S C4S C7S C6S -35(3) . . . . ? Cl8S C4S C7S C6S -105(3) 2_765 . . . ? C5S C4S C7S C7S 87(2) . . . 2_765 ? Cl8S C4S C7S C7S 17(3) 2_765 . . 2_765 ? C5S C4S C7S O2S 121.0(11) . . . 2_765 ? Cl8S C4S C7S O2S 51.0(10) 2_765 . . 2_765 ? Cl8S C4S C7S C5S -70.1(8) 2_765 . . . ? O1S C5S C7S O2S -12.0(6) . . . . ? C4S C5S C7S O2S 167.9(12) . . . . ? C4S C5S C7S O1S 179.9(11) . . . . ? O2S C5S C7S O1S 12.0(6) . . . . ? O1S C5S C7S C4S -179.9(11) . . . . ? O2S C5S C7S C4S -167.9(12) . . . . ? O1S C5S C7S C6S 108.7(11) . . . 2_765 ? C4S C5S C7S C6S -71.3(10) . . . 2_765 ? O2S C5S C7S C6S 120.8(13) . . . 2_765 ? O1S C5S C7S C6S -13.5(8) . . . . ? C4S C5S C7S C6S 166.5(12) . . . . ? O2S C5S C7S C6S -1.4(6) . . . . ? O1S C5S C7S C7S 47.0(14) . . . 2_765 ? C4S C5S C7S C7S -133.1(18) . . . 2_765 ? O2S C5S C7S C7S 59.0(13) . . . 2_765 ? O1S C5S C7S O2S 95.3(14) . . . 2_765 ? C4S C5S C7S O2S -84.8(13) . . . 2_765 ? O2S C5S C7S O2S 107.4(15) . . . 2_765 ? C7S O2S C6S O1S -141(4) . . . . ? C7S O2S C6S O1S -82(3) 2_765 . . . ? C5S O2S C6S O1S -160(12) . . . . ? O1S O2S C6S C7S 82(3) . . . 2_765 ? C7S O2S C6S C7S -59.3(14) . . . 2_765 ? C5S O2S C6S C7S -78(9) . . . 2_765 ? O1S O2S C6S C7S 141(4) . . . . ? C7S O2S C6S C7S 59.3(14) 2_765 . . . ? C5S O2S C6S C7S -19(8) . . . . ? C5S O1S C6S O2S 6(4) . . . . ? C7S O1S C6S O2S 33(3) . . . . ? O2S O1S C6S C7S -95(4) . . . 2_765 ? C5S O1S C6S C7S -89.2(15) . . . 2_765 ? C7S O1S C6S C7S -62.5(12) . . . 2_765 ? O2S O1S C6S C7S -33(3) . . . . ? C5S O1S C6S C7S -26.7(15) . . . . ? O1S C7S C6S O2S -10.7(12) . . . . ? C4S C7S C6S O2S 34(3) . . . . ? C6S C7S C6S O2S -103.0(18) 2_765 . . . ? C7S C7S C6S O2S -103.0(18) 2_765 . . . ? O2S C7S C6S O2S -122.0(16) 2_765 . . . ? C5S C7S C6S O2S 3.2(14) . . . . ? O2S C7S C6S O1S 10.7(12) . . . . ? C4S C7S C6S O1S 44(3) . . . . ? C6S C7S C6S O1S -92.3(12) 2_765 . . . ? C7S C7S C6S O1S -92.3(12) 2_765 . . . ? O2S C7S C6S O1S -111.3(10) 2_765 . . . ? C5S C7S C6S O1S 13.9(8) . . . . ? O2S C7S C6S C7S 103.0(18) . . . 2_765 ? O1S C7S C6S C7S 92.3(12) . . . 2_765 ? C4S C7S C6S C7S 137(4) . . . 2_765 ? C6S C7S C6S C7S 0.000(2) 2_765 . . 2_765 ? O2S C7S C6S C7S -19.0(6) 2_765 . . 2_765 ? C5S C7S C6S C7S 106.1(14) . . . 2_765 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N Cl4 0.92(7) 2.41(6) 3.233(5) 150(5) . C2S H2S Cl1 1.00 2.52 3.432(7) 151.1 . C32 H32 N2 0.95 2.64 3.570(7) 166.0 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.529 _refine_diff_density_min -1.399 _refine_diff_density_rms 0.140 #===END data_ms1376 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H57 Cl7 N2 O P2 Rh2' _chemical_formula_weight 1229.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Rh' 'Rh' -1.1178 0.9187 '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 9.6851(3) _cell_length_b 16.4272(7) _cell_length_c 16.6831(8) _cell_angle_alpha 99.178(3) _cell_angle_beta 91.764(3) _cell_angle_gamma 92.281(3) _cell_volume 2616.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 1.089 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 KappaCCD _diffrn_measurement_method '1.9o phi + omega frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 19114 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11885 _reflns_number_gt 9858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _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^)+(0.0099P)^2^+5.6081P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11885 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0858 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Rh1 Rh 0.37913(2) 0.642792(14) 0.263158(14) 0.01641(7) Uani 1 1 d . . . Cl1 Cl 0.42690(8) 0.75158(5) 0.18604(5) 0.02454(17) Uani 1 1 d . . . P1 P 0.39521(8) 0.74071(4) 0.37805(5) 0.01635(16) Uani 1 1 d . . . O1 O 0.3651(2) 0.70903(12) 0.46459(12) 0.0177(4) Uani 1 1 d . . . N1 N 0.3698(3) 0.65973(15) 0.60833(15) 0.0182(5) Uani 1 1 d . . . C1 C 0.4804(3) 0.54942(18) 0.32043(19) 0.0222(7) Uani 1 1 d . . . Rh2 Rh 0.48598(2) 0.826783(13) 0.817493(14) 0.01681(7) Uani 1 1 d . . . Cl2 Cl 0.13461(8) 0.65156(5) 0.22954(5) 0.02308(16) Uani 1 1 d . . . P2 P 0.31648(8) 0.72521(4) 0.77223(5) 0.01565(15) Uani 1 1 d . . . N2 N 0.1408(3) 0.60765(16) 0.59032(16) 0.0223(6) Uani 1 1 d . . . C2 C 0.5713(3) 0.57967(18) 0.26412(19) 0.0209(6) Uani 1 1 d . . . Cl3 Cl 0.55701(7) 0.81748(4) 0.67887(4) 0.02021(15) Uani 1 1 d . . . C3 C 0.5088(3) 0.55618(18) 0.18360(19) 0.0201(6) Uani 1 1 d . . . Cl4 Cl 0.62490(8) 0.71494(4) 0.84053(5) 0.02357(16) Uani 1 1 d . . . C4 C 0.3791(3) 0.51581(18) 0.19021(19) 0.0206(6) Uani 1 1 d . . . C5 C 0.3586(3) 0.51352(18) 0.2761(2) 0.0228(7) Uani 1 1 d . . . C6 C 0.5144(4) 0.5468(2) 0.40833(19) 0.0290(8) Uani 1 1 d . . . H6A H 0.4319 0.5537 0.4387 0.044 Uiso 1 1 calc R . . H6B H 0.5812 0.5904 0.4290 0.044 Uiso 1 1 calc R . . H6C H 0.5517 0.4945 0.4136 0.044 Uiso 1 1 calc R . . C7 C 0.7168(3) 0.6149(2) 0.2829(2) 0.0283(7) Uani 1 1 d . . . H7A H 0.7798 0.5708 0.2775 0.042 Uiso 1 1 calc R . . H7B H 0.7237 0.6443 0.3376 0.042 Uiso 1 1 calc R . . H7C H 0.7397 0.6519 0.2458 0.042 Uiso 1 1 calc R . . C8 C 0.5718(4) 0.5721(2) 0.1068(2) 0.0283(7) Uani 1 1 d . . . H8A H 0.6256 0.5263 0.0854 0.042 Uiso 1 1 calc R . . H8B H 0.6305 0.6214 0.1176 0.042 Uiso 1 1 calc R . . H8C H 0.5000 0.5789 0.0678 0.042 Uiso 1 1 calc R . . C9 C 0.2809(4) 0.4789(2) 0.1221(2) 0.0281(7) Uani 1 1 d . . . H9A H 0.3232 0.4814 0.0712 0.042 Uiso 1 1 calc R . . H9B H 0.1981 0.5093 0.1248 0.042 Uiso 1 1 calc R . . H9C H 0.2584 0.4224 0.1266 0.042 Uiso 1 1 calc R . . C10 C 0.2390(4) 0.4708(2) 0.3083(2) 0.0315(8) Uani 1 1 d . . . H10A H 0.2508 0.4124 0.2992 0.047 Uiso 1 1 calc R . . H10B H 0.1552 0.4825 0.2809 0.047 Uiso 1 1 calc R . . H10C H 0.2338 0.4901 0.3655 0.047 Uiso 1 1 calc R . . C11 C 0.5731(3) 0.77740(17) 0.40365(18) 0.0182(6) Uani 1 1 d . . . C12 C 0.6472(3) 0.75658(19) 0.47039(19) 0.0226(6) Uani 1 1 d . . . H12 H 0.6026 0.7275 0.5063 0.027 Uiso 1 1 calc R . . C13 C 0.7864(3) 0.7791(2) 0.4832(2) 0.0263(7) Uani 1 1 d . . . H13 H 0.8353 0.7639 0.5270 0.032 Uiso 1 1 calc R . . C14 C 0.8530(4) 0.8239(2) 0.4313(2) 0.0294(7) Uani 1 1 d . . . H14 H 0.9465 0.8388 0.4399 0.035 Uiso 1 1 calc R . . C15 C 0.7795(4) 0.8466(2) 0.3661(2) 0.0299(8) Uani 1 1 d . . . H15 H 0.8240 0.8776 0.3316 0.036 Uiso 1 1 calc R . . C16 C 0.6407(3) 0.82363(19) 0.3519(2) 0.0243(7) Uani 1 1 d . . . H16 H 0.5925 0.8389 0.3080 0.029 Uiso 1 1 calc R . . C17 C 0.3026(3) 0.83554(18) 0.39016(19) 0.0202(6) Uani 1 1 d . . . C18 C 0.2077(3) 0.85511(18) 0.3322(2) 0.0214(6) Uani 1 1 d . . . H18 H 0.1912 0.8198 0.2832 0.026 Uiso 1 1 calc R . . C19 C 0.1381(3) 0.9282(2) 0.3487(2) 0.0283(7) Uani 1 1 d . . . H19 H 0.0754 0.9419 0.3102 0.034 Uiso 1 1 calc R . . C20 C 0.1615(4) 0.9803(2) 0.4217(2) 0.0317(8) Uani 1 1 d . . . H20 H 0.1135 1.0286 0.4323 0.038 Uiso 1 1 calc R . . C21 C 0.2559(4) 0.9614(2) 0.4795(2) 0.0351(8) Uani 1 1 d . . . H21 H 0.2719 0.9970 0.5284 0.042 Uiso 1 1 calc R . . C22 C 0.3262(4) 0.8892(2) 0.4636(2) 0.0294(7) Uani 1 1 d . . . H22 H 0.3896 0.8763 0.5021 0.035 Uiso 1 1 calc R . . C23 C 0.2421(3) 0.67190(17) 0.48514(19) 0.0186(6) Uani 1 1 d . . . C24 C 0.2483(3) 0.64620(17) 0.56198(18) 0.0169(6) Uani 1 1 d . . . C25 C 0.1225(3) 0.66034(19) 0.4381(2) 0.0222(6) Uani 1 1 d . . . H25 H 0.1164 0.6779 0.3879 0.027 Uiso 1 1 calc R . . C26 C 0.0093(3) 0.6207(2) 0.4690(2) 0.0263(7) Uani 1 1 d . . . H26 H -0.0745 0.6116 0.4395 0.032 Uiso 1 1 calc R . . C27 C 0.0244(3) 0.5958(2) 0.5434(2) 0.0270(7) Uani 1 1 d . . . H27 H -0.0511 0.5689 0.5625 0.032 Uiso 1 1 calc R . . C28 C 0.3768(3) 0.64400(17) 0.69115(17) 0.0182(6) Uani 1 1 d . . . H28A H 0.4721 0.6340 0.7046 0.022 Uiso 1 1 calc R . . H28B H 0.3229 0.5934 0.6932 0.022 Uiso 1 1 calc R . . C29 C 0.4126(4) 0.9504(2) 0.8354(2) 0.0319(8) Uani 1 1 d . . . C30 C 0.3677(4) 0.9095(2) 0.8998(2) 0.0388(10) Uani 1 1 d . . . C31 C 0.4874(5) 0.8888(2) 0.9422(2) 0.0441(11) Uani 1 1 d . . . C32 C 0.6067(4) 0.9198(2) 0.9052(3) 0.0388(9) Uani 1 1 d . . . C33 C 0.5604(4) 0.95841(19) 0.8417(2) 0.0331(8) Uani 1 1 d . . . C34 C 0.3275(7) 0.9910(3) 0.7784(3) 0.083(2) Uani 1 1 d . . . H34A H 0.2325 0.9723 0.7794 0.124 Uiso 1 1 calc R . . H34B H 0.3600 0.9771 0.7244 0.124 Uiso 1 1 calc R . . H34C H 0.3353 1.0498 0.7949 0.124 Uiso 1 1 calc R . . C35 C 0.2209(6) 0.8963(3) 0.9222(5) 0.110(3) Uani 1 1 d . . . H35A H 0.1954 0.9422 0.9612 0.164 Uiso 1 1 calc R . . H35B H 0.2118 0.8465 0.9452 0.164 Uiso 1 1 calc R . . H35C H 0.1614 0.8917 0.8744 0.164 Uiso 1 1 calc R . . C36 C 0.4939(10) 0.8518(3) 1.0186(3) 0.113(3) Uani 1 1 d . . . H36A H 0.5200 0.8940 1.0638 0.169 Uiso 1 1 calc R . . H36B H 0.5612 0.8100 1.0138 0.169 Uiso 1 1 calc R . . H36C H 0.4049 0.8275 1.0273 0.169 Uiso 1 1 calc R . . C37 C 0.7537(6) 0.9092(3) 0.9340(5) 0.103(3) Uani 1 1 d . . . H37A H 0.8161 0.9422 0.9074 0.155 Uiso 1 1 calc R . . H37B H 0.7753 0.8522 0.9210 0.155 Uiso 1 1 calc R . . H37C H 0.7628 0.9266 0.9917 0.155 Uiso 1 1 calc R . . C38 C 0.6489(6) 1.0013(3) 0.7875(3) 0.0736(18) Uani 1 1 d . . . H38A H 0.6461 1.0599 0.8036 0.110 Uiso 1 1 calc R . . H38B H 0.6148 0.9865 0.7322 0.110 Uiso 1 1 calc R . . H38C H 0.7425 0.9849 0.7919 0.110 Uiso 1 1 calc R . . C39 C 0.1623(3) 0.76743(17) 0.73281(19) 0.0187(6) Uani 1 1 d . . . C40 C 0.1778(3) 0.81596(19) 0.67153(19) 0.0212(6) Uani 1 1 d . . . H40 H 0.2640 0.8230 0.6500 0.025 Uiso 1 1 calc R . . C41 C 0.0642(3) 0.8537(2) 0.6429(2) 0.0254(7) Uani 1 1 d . . . H41 H 0.0745 0.8850 0.6015 0.030 Uiso 1 1 calc R . . C42 C -0.0642(3) 0.8447(2) 0.6758(2) 0.0274(7) Uani 1 1 d . . . H42 H -0.1394 0.8708 0.6571 0.033 Uiso 1 1 calc R . . C43 C -0.0806(3) 0.7972(2) 0.7364(2) 0.0292(8) Uani 1 1 d . . . H43 H -0.1671 0.7908 0.7579 0.035 Uiso 1 1 calc R . . C44 C 0.0322(3) 0.7588(2) 0.7652(2) 0.0253(7) Uani 1 1 d . . . H44 H 0.0208 0.7272 0.8063 0.030 Uiso 1 1 calc R . . C45 C 0.2531(3) 0.66033(18) 0.84390(18) 0.0186(6) Uani 1 1 d . . . C46 C 0.1571(3) 0.59525(18) 0.8168(2) 0.0223(7) Uani 1 1 d . . . H46 H 0.1275 0.5845 0.7624 0.027 Uiso 1 1 calc R . . C47 C 0.1057(3) 0.5465(2) 0.8709(2) 0.0265(7) Uani 1 1 d . . . H47 H 0.0429 0.5026 0.8527 0.032 Uiso 1 1 calc R . . C48 C 0.1485(3) 0.5637(2) 0.9521(2) 0.0273(7) Uani 1 1 d . . . H48 H 0.1127 0.5317 0.9885 0.033 Uiso 1 1 calc R . . C49 C 0.2436(3) 0.6275(2) 0.9797(2) 0.0273(7) Uani 1 1 d . . . H49 H 0.2711 0.6387 1.0344 0.033 Uiso 1 1 calc R . . C50 C 0.2982(3) 0.67492(19) 0.92503(19) 0.0208(6) Uani 1 1 d . . . H50 H 0.3651 0.7166 0.9429 0.025 Uiso 1 1 calc R . . Cl1S Cl -0.06934(15) 0.73200(9) 0.00114(8) 0.0696(4) Uani 1 1 d . . . C1S C -0.0454(4) 0.7724(3) 0.1038(3) 0.0413(10) Uani 1 1 d . . . H1S H 0.005(5) 0.737(3) 0.126(3) 0.054(13) Uiso 1 1 d . . . Cl2S Cl -0.20652(16) 0.77997(7) 0.14864(8) 0.0696(4) Uani 1 1 d . . . Cl3S Cl 0.03892(18) 0.87091(10) 0.11514(10) 0.0868(5) Uani 1 1 d . . . H1 H 0.421(3) 0.700(2) 0.598(2) 0.019(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02063(13) 0.01522(11) 0.01428(13) 0.00451(9) 0.00035(9) 0.00345(9) Cl1 0.0319(4) 0.0235(4) 0.0210(4) 0.0109(3) 0.0038(3) 0.0036(3) P1 0.0186(4) 0.0147(3) 0.0166(4) 0.0047(3) 0.0011(3) 0.0024(3) O1 0.0208(11) 0.0203(10) 0.0129(10) 0.0054(8) 0.0010(8) -0.0003(8) N1 0.0222(13) 0.0170(12) 0.0154(13) 0.0034(10) 0.0004(10) -0.0003(10) C1 0.0340(18) 0.0164(14) 0.0173(16) 0.0034(12) 0.0003(13) 0.0117(13) Rh2 0.02102(13) 0.01331(11) 0.01636(13) 0.00330(9) 0.00037(9) 0.00046(9) Cl2 0.0225(4) 0.0233(4) 0.0238(4) 0.0058(3) -0.0046(3) 0.0017(3) P2 0.0181(4) 0.0147(3) 0.0150(4) 0.0048(3) 0.0012(3) 0.0023(3) N2 0.0223(14) 0.0217(13) 0.0234(14) 0.0055(11) 0.0025(11) -0.0031(11) C2 0.0263(16) 0.0175(14) 0.0192(16) 0.0021(12) 0.0000(12) 0.0101(12) Cl3 0.0208(4) 0.0207(3) 0.0194(4) 0.0040(3) 0.0035(3) -0.0011(3) C3 0.0267(16) 0.0165(14) 0.0176(16) 0.0021(11) 0.0005(12) 0.0097(12) Cl4 0.0255(4) 0.0202(3) 0.0258(4) 0.0065(3) -0.0051(3) 0.0030(3) C4 0.0274(16) 0.0154(14) 0.0193(16) 0.0036(12) -0.0013(12) 0.0036(12) C5 0.0312(17) 0.0158(14) 0.0226(17) 0.0052(12) 0.0007(13) 0.0059(13) C6 0.049(2) 0.0220(16) 0.0169(17) 0.0035(13) -0.0015(15) 0.0131(15) C7 0.0268(17) 0.0278(17) 0.0285(19) -0.0020(14) -0.0021(14) 0.0090(14) C8 0.0305(18) 0.0343(18) 0.0209(17) 0.0043(14) 0.0070(14) 0.0083(15) C9 0.0359(19) 0.0235(16) 0.0232(18) 0.0005(13) -0.0075(14) -0.0011(14) C10 0.038(2) 0.0214(16) 0.037(2) 0.0101(15) 0.0099(16) 0.0016(14) C11 0.0188(15) 0.0142(13) 0.0202(16) -0.0010(11) 0.0015(12) -0.0007(11) C12 0.0246(16) 0.0248(16) 0.0178(16) 0.0018(12) 0.0009(12) -0.0008(13) C13 0.0245(17) 0.0302(17) 0.0232(17) 0.0012(14) -0.0005(13) 0.0037(14) C14 0.0215(17) 0.0301(17) 0.034(2) -0.0024(15) 0.0014(14) -0.0042(14) C15 0.0305(18) 0.0267(17) 0.032(2) 0.0056(14) 0.0076(15) -0.0062(14) C16 0.0254(17) 0.0207(15) 0.0272(18) 0.0055(13) 0.0017(13) -0.0019(13) C17 0.0223(16) 0.0159(14) 0.0240(17) 0.0064(12) 0.0053(12) 0.0042(12) C18 0.0205(15) 0.0200(15) 0.0257(17) 0.0098(13) 0.0028(12) 0.0012(12) C19 0.0227(17) 0.0273(17) 0.039(2) 0.0167(15) 0.0033(14) 0.0051(13) C20 0.0339(19) 0.0224(16) 0.042(2) 0.0103(15) 0.0105(16) 0.0083(14) C21 0.050(2) 0.0230(17) 0.031(2) -0.0016(15) 0.0047(17) 0.0105(16) C22 0.0366(19) 0.0231(16) 0.0283(19) 0.0023(14) -0.0022(15) 0.0090(14) C23 0.0184(15) 0.0157(13) 0.0212(16) 0.0009(12) 0.0030(12) 0.0005(11) C24 0.0201(15) 0.0122(13) 0.0184(15) 0.0019(11) 0.0014(11) 0.0025(11) C25 0.0244(16) 0.0230(15) 0.0199(16) 0.0063(12) -0.0015(12) 0.0000(12) C26 0.0181(16) 0.0305(17) 0.0296(19) 0.0042(14) -0.0036(13) -0.0016(13) C27 0.0241(17) 0.0288(17) 0.0282(18) 0.0069(14) 0.0013(14) -0.0066(14) C28 0.0225(15) 0.0171(14) 0.0153(15) 0.0030(11) 0.0019(12) 0.0048(12) C29 0.046(2) 0.0172(15) 0.0291(19) -0.0057(13) -0.0051(16) 0.0083(15) C30 0.043(2) 0.0235(17) 0.043(2) -0.0172(16) 0.0208(18) -0.0090(16) C31 0.091(3) 0.0195(17) 0.0196(19) -0.0019(14) -0.001(2) -0.0013(19) C32 0.044(2) 0.0165(16) 0.049(2) -0.0118(16) -0.0172(19) 0.0022(15) C33 0.046(2) 0.0118(14) 0.039(2) -0.0024(14) 0.0135(17) -0.0057(14) C34 0.130(5) 0.032(2) 0.077(4) -0.018(2) -0.060(4) 0.040(3) C35 0.078(4) 0.058(3) 0.166(7) -0.070(4) 0.084(4) -0.031(3) C36 0.288(10) 0.032(2) 0.013(2) 0.0028(18) -0.022(4) -0.028(4) C37 0.072(4) 0.051(3) 0.160(7) -0.055(4) -0.075(4) 0.023(3) C38 0.110(4) 0.028(2) 0.078(4) -0.008(2) 0.057(3) -0.026(3) C39 0.0182(15) 0.0157(14) 0.0218(16) 0.0014(12) -0.0001(12) 0.0036(11) C40 0.0180(15) 0.0231(15) 0.0235(17) 0.0063(13) 0.0013(12) 0.0029(12) C41 0.0264(17) 0.0283(17) 0.0236(17) 0.0100(14) 0.0002(13) 0.0056(13) C42 0.0197(16) 0.0297(17) 0.033(2) 0.0065(15) -0.0041(14) 0.0080(13) C43 0.0172(16) 0.0328(18) 0.039(2) 0.0090(15) 0.0044(14) 0.0038(13) C44 0.0222(16) 0.0259(16) 0.0300(19) 0.0111(14) 0.0026(13) 0.0018(13) C45 0.0206(15) 0.0175(14) 0.0192(16) 0.0058(12) 0.0054(12) 0.0026(12) C46 0.0220(16) 0.0204(15) 0.0257(17) 0.0075(13) -0.0002(13) 0.0009(12) C47 0.0198(16) 0.0231(16) 0.039(2) 0.0136(14) 0.0021(14) -0.0005(13) C48 0.0233(16) 0.0301(17) 0.034(2) 0.0198(15) 0.0068(14) 0.0031(14) C49 0.0302(18) 0.0334(18) 0.0216(17) 0.0130(14) 0.0045(14) 0.0051(14) C50 0.0211(15) 0.0205(15) 0.0213(16) 0.0048(12) 0.0015(12) 0.0027(12) Cl1S 0.0831(9) 0.0775(9) 0.0439(7) -0.0109(6) 0.0038(6) 0.0332(7) C1S 0.041(2) 0.046(2) 0.040(2) 0.0181(19) -0.0079(18) 0.0045(19) Cl2S 0.0984(10) 0.0477(6) 0.0706(9) 0.0210(6) 0.0532(8) 0.0172(6) Cl3S 0.0970(11) 0.0816(10) 0.0832(10) 0.0371(8) -0.0348(9) -0.0470(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C2 2.167(3) . ? Rh1 C5 2.171(3) . ? Rh1 C1 2.181(3) . ? Rh1 C3 2.237(3) . ? Rh1 C4 2.241(3) . ? Rh1 P1 2.2944(11) . ? Rh1 Cl1 2.4015(10) . ? Rh1 Cl2 2.4320(9) . ? P1 O1 1.641(2) . ? P1 C17 1.815(3) . ? P1 C11 1.818(3) . ? O1 C23 1.394(3) . ? N1 C24 1.378(4) . ? N1 C28 1.446(4) . ? C1 C5 1.428(5) . ? C1 C2 1.438(4) . ? C1 C6 1.501(4) . ? Rh2 C29 2.158(3) . ? Rh2 C30 2.161(4) . ? Rh2 C31 2.166(4) . ? Rh2 C32 2.209(3) . ? Rh2 C33 2.222(3) . ? Rh2 P2 2.3136(11) . ? Rh2 Cl4 2.3925(10) . ? Rh2 Cl3 2.4163(9) . ? P2 C39 1.820(3) . ? P2 C45 1.828(3) . ? P2 C28 1.867(3) . ? N2 C24 1.335(4) . ? N2 C27 1.343(4) . ? C2 C3 1.444(4) . ? C2 C7 1.507(5) . ? C3 C4 1.412(4) . ? C3 C8 1.493(4) . ? C4 C5 1.459(4) . ? C4 C9 1.493(4) . ? C5 C10 1.489(4) . ? C11 C16 1.399(4) . ? C11 C12 1.401(4) . ? C12 C13 1.385(4) . ? C13 C14 1.382(5) . ? C14 C15 1.390(5) . ? C15 C16 1.385(5) . ? C17 C18 1.397(4) . ? C17 C22 1.398(5) . ? C18 C19 1.394(4) . ? C19 C20 1.380(5) . ? C20 C21 1.388(5) . ? C21 C22 1.385(5) . ? C23 C25 1.368(4) . ? C23 C24 1.413(4) . ? C25 C26 1.406(4) . ? C26 C27 1.373(5) . ? C29 C30 1.425(5) . ? C29 C33 1.431(5) . ? C29 C34 1.491(5) . ? C30 C31 1.421(6) . ? C30 C35 1.497(6) . ? C31 C32 1.441(6) . ? C31 C36 1.498(5) . ? C32 C33 1.390(5) . ? C32 C37 1.514(6) . ? C33 C38 1.501(5) . ? C39 C44 1.397(4) . ? C39 C40 1.401(4) . ? C40 C41 1.392(4) . ? C41 C42 1.387(5) . ? C42 C43 1.382(5) . ? C43 C44 1.394(4) . ? C45 C50 1.390(4) . ? C45 C46 1.398(4) . ? C46 C47 1.389(4) . ? C47 C48 1.386(5) . ? C48 C49 1.379(5) . ? C49 C50 1.394(4) . ? Cl1S C1S 1.740(4) . ? C1S Cl2S 1.751(5) . ? C1S Cl3S 1.763(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Rh1 C5 64.66(12) . . ? C2 Rh1 C1 38.64(12) . . ? C5 Rh1 C1 38.30(12) . . ? C2 Rh1 C3 38.25(11) . . ? C5 Rh1 C3 63.55(12) . . ? C1 Rh1 C3 63.55(11) . . ? C2 Rh1 C4 63.45(12) . . ? C5 Rh1 C4 38.57(11) . . ? C1 Rh1 C4 63.59(11) . . ? C3 Rh1 C4 36.77(11) . . ? C2 Rh1 P1 104.64(9) . . ? C5 Rh1 P1 118.85(9) . . ? C1 Rh1 P1 94.30(9) . . ? C3 Rh1 P1 141.22(8) . . ? C4 Rh1 P1 156.62(8) . . ? C2 Rh1 Cl1 104.13(9) . . ? C5 Rh1 Cl1 152.41(9) . . ? C1 Rh1 Cl1 141.87(9) . . ? C3 Rh1 Cl1 91.73(8) . . ? C4 Rh1 Cl1 113.99(8) . . ? P1 Rh1 Cl1 87.89(3) . . ? C2 Rh1 Cl2 153.93(8) . . ? C5 Rh1 Cl2 93.66(9) . . ? C1 Rh1 Cl2 128.50(9) . . ? C3 Rh1 Cl2 120.32(9) . . ? C4 Rh1 Cl2 90.63(9) . . ? P1 Rh1 Cl2 98.44(4) . . ? Cl1 Rh1 Cl2 88.50(4) . . ? O1 P1 C17 100.81(13) . . ? O1 P1 C11 96.40(13) . . ? C17 P1 C11 102.78(14) . . ? O1 P1 Rh1 116.93(8) . . ? C17 P1 Rh1 123.94(11) . . ? C11 P1 Rh1 111.74(11) . . ? C23 O1 P1 126.25(19) . . ? C24 N1 C28 121.2(3) . . ? C5 C1 C2 108.1(3) . . ? C5 C1 C6 125.6(3) . . ? C2 C1 C6 125.9(3) . . ? C5 C1 Rh1 70.45(17) . . ? C2 C1 Rh1 70.16(16) . . ? C6 C1 Rh1 130.5(2) . . ? C29 Rh2 C30 38.54(15) . . ? C29 Rh2 C31 64.23(14) . . ? C30 Rh2 C31 38.33(17) . . ? C29 Rh2 C32 63.42(14) . . ? C30 Rh2 C32 63.86(15) . . ? C31 Rh2 C32 38.43(16) . . ? C29 Rh2 C33 38.11(14) . . ? C30 Rh2 C33 63.39(13) . . ? C31 Rh2 C33 62.88(14) . . ? C32 Rh2 C33 36.55(14) . . ? C29 Rh2 P2 114.11(10) . . ? C30 Rh2 P2 99.67(10) . . ? C31 Rh2 P2 119.20(13) . . ? C32 Rh2 P2 157.48(12) . . ? C33 Rh2 P2 151.12(11) . . ? C29 Rh2 Cl4 157.69(10) . . ? C30 Rh2 Cl4 130.98(12) . . ? C31 Rh2 Cl4 97.16(12) . . ? C32 Rh2 Cl4 94.43(10) . . ? C33 Rh2 Cl4 123.71(11) . . ? P2 Rh2 Cl4 85.15(3) . . ? C29 Rh2 Cl3 99.39(11) . . ? C30 Rh2 Cl3 136.56(12) . . ? C31 Rh2 Cl3 151.62(11) . . ? C32 Rh2 Cl3 114.28(12) . . ? C33 Rh2 Cl3 89.72(10) . . ? P2 Rh2 Cl3 88.23(4) . . ? Cl4 Rh2 Cl3 92.03(4) . . ? C39 P2 C45 104.92(14) . . ? C39 P2 C28 107.90(14) . . ? C45 P2 C28 99.86(13) . . ? C39 P2 Rh2 112.01(10) . . ? C45 P2 Rh2 118.35(11) . . ? C28 P2 Rh2 112.67(10) . . ? C24 N2 C27 117.1(3) . . ? C1 C2 C3 107.7(3) . . ? C1 C2 C7 126.2(3) . . ? C3 C2 C7 125.2(3) . . ? C1 C2 Rh1 71.21(17) . . ? C3 C2 Rh1 73.50(17) . . ? C7 C2 Rh1 129.5(2) . . ? C4 C3 C2 108.5(3) . . ? C4 C3 C8 126.2(3) . . ? C2 C3 C8 125.3(3) . . ? C4 C3 Rh1 71.77(18) . . ? C2 C3 Rh1 68.25(17) . . ? C8 C3 Rh1 125.9(2) . . ? C3 C4 C5 107.9(3) . . ? C3 C4 C9 126.9(3) . . ? C5 C4 C9 125.2(3) . . ? C3 C4 Rh1 71.46(17) . . ? C5 C4 Rh1 68.10(16) . . ? C9 C4 Rh1 127.5(2) . . ? C1 C5 C4 107.7(3) . . ? C1 C5 C10 127.2(3) . . ? C4 C5 C10 124.7(3) . . ? C1 C5 Rh1 71.25(17) . . ? C4 C5 Rh1 73.33(16) . . ? C10 C5 Rh1 127.1(2) . . ? C16 C11 C12 119.0(3) . . ? C16 C11 P1 118.6(2) . . ? C12 C11 P1 122.3(2) . . ? C13 C12 C11 120.4(3) . . ? C14 C13 C12 120.2(3) . . ? C13 C14 C15 119.8(3) . . ? C16 C15 C14 120.6(3) . . ? C15 C16 C11 120.0(3) . . ? C18 C17 C22 119.7(3) . . ? C18 C17 P1 123.7(2) . . ? C22 C17 P1 116.5(2) . . ? C19 C18 C17 119.3(3) . . ? C20 C19 C18 120.5(3) . . ? C19 C20 C21 120.6(3) . . ? C22 C21 C20 119.4(3) . . ? C21 C22 C17 120.5(3) . . ? C25 C23 O1 125.5(3) . . ? C25 C23 C24 120.5(3) . . ? O1 C23 C24 114.0(3) . . ? N2 C24 N1 119.0(3) . . ? N2 C24 C23 121.9(3) . . ? N1 C24 C23 119.1(3) . . ? C23 C25 C26 117.2(3) . . ? C27 C26 C25 118.9(3) . . ? N2 C27 C26 124.4(3) . . ? N1 C28 P2 117.8(2) . . ? C30 C29 C33 107.5(3) . . ? C30 C29 C34 128.5(5) . . ? C33 C29 C34 123.3(4) . . ? C30 C29 Rh2 70.9(2) . . ? C33 C29 Rh2 73.37(19) . . ? C34 C29 Rh2 128.5(3) . . ? C31 C30 C29 107.7(3) . . ? C31 C30 C35 126.2(5) . . ? C29 C30 C35 125.9(5) . . ? C31 C30 Rh2 71.0(2) . . ? C29 C30 Rh2 70.6(2) . . ? C35 C30 Rh2 127.1(3) . . ? C30 C31 C32 107.8(3) . . ? C30 C31 C36 127.7(5) . . ? C32 C31 C36 124.0(5) . . ? C30 C31 Rh2 70.7(2) . . ? C32 C31 Rh2 72.4(2) . . ? C36 C31 Rh2 128.6(3) . . ? C33 C32 C31 107.9(3) . . ? C33 C32 C37 128.9(5) . . ? C31 C32 C37 123.1(5) . . ? C33 C32 Rh2 72.2(2) . . ? C31 C32 Rh2 69.1(2) . . ? C37 C32 Rh2 123.9(3) . . ? C32 C33 C29 108.9(3) . . ? C32 C33 C38 126.3(4) . . ? C29 C33 C38 124.7(4) . . ? C32 C33 Rh2 71.23(19) . . ? C29 C33 Rh2 68.51(18) . . ? C38 C33 Rh2 125.9(3) . . ? C44 C39 C40 119.0(3) . . ? C44 C39 P2 122.9(2) . . ? C40 C39 P2 118.0(2) . . ? C41 C40 C39 120.1(3) . . ? C42 C41 C40 120.3(3) . . ? C43 C42 C41 120.1(3) . . ? C42 C43 C44 120.0(3) . . ? C43 C44 C39 120.5(3) . . ? C50 C45 C46 119.4(3) . . ? C50 C45 P2 121.1(2) . . ? C46 C45 P2 119.5(2) . . ? C47 C46 C45 120.2(3) . . ? C48 C47 C46 119.6(3) . . ? C49 C48 C47 121.0(3) . . ? C48 C49 C50 119.5(3) . . ? C45 C50 C49 120.3(3) . . ? Cl1S C1S Cl2S 109.3(2) . . ? Cl1S C1S Cl3S 109.9(2) . . ? Cl2S C1S Cl3S 109.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Rh1 P1 O1 -78.49(13) . . . . ? C5 Rh1 P1 O1 -9.66(14) . . . . ? C1 Rh1 P1 O1 -40.68(13) . . . . ? C3 Rh1 P1 O1 -92.40(15) . . . . ? C4 Rh1 P1 O1 -22.5(2) . . . . ? Cl1 Rh1 P1 O1 177.46(9) . . . . ? Cl2 Rh1 P1 O1 89.28(10) . . . . ? C2 Rh1 P1 C17 154.96(14) . . . . ? C5 Rh1 P1 C17 -136.21(15) . . . . ? C1 Rh1 P1 C17 -167.22(15) . . . . ? C3 Rh1 P1 C17 141.05(17) . . . . ? C4 Rh1 P1 C17 -149.1(2) . . . . ? Cl1 Rh1 P1 C17 50.91(12) . . . . ? Cl2 Rh1 P1 C17 -37.26(12) . . . . ? C2 Rh1 P1 C11 31.22(13) . . . . ? C5 Rh1 P1 C11 100.05(15) . . . . ? C1 Rh1 P1 C11 69.03(14) . . . . ? C3 Rh1 P1 C11 17.31(17) . . . . ? C4 Rh1 P1 C11 87.2(2) . . . . ? Cl1 Rh1 P1 C11 -72.83(11) . . . . ? Cl2 Rh1 P1 C11 -161.01(10) . . . . ? C17 P1 O1 C23 76.4(2) . . . . ? C11 P1 O1 C23 -179.3(2) . . . . ? Rh1 P1 O1 C23 -60.9(2) . . . . ? C2 Rh1 C1 C5 -118.5(3) . . . . ? C3 Rh1 C1 C5 -80.0(2) . . . . ? C4 Rh1 C1 C5 -38.79(18) . . . . ? P1 Rh1 C1 C5 133.27(18) . . . . ? Cl1 Rh1 C1 C5 -134.66(17) . . . . ? Cl2 Rh1 C1 C5 28.9(2) . . . . ? C5 Rh1 C1 C2 118.5(3) . . . . ? C3 Rh1 C1 C2 38.51(17) . . . . ? C4 Rh1 C1 C2 79.76(19) . . . . ? P1 Rh1 C1 C2 -108.18(17) . . . . ? Cl1 Rh1 C1 C2 -16.1(2) . . . . ? Cl2 Rh1 C1 C2 147.47(15) . . . . ? C2 Rh1 C1 C6 120.8(4) . . . . ? C5 Rh1 C1 C6 -120.6(4) . . . . ? C3 Rh1 C1 C6 159.3(4) . . . . ? C4 Rh1 C1 C6 -159.4(4) . . . . ? P1 Rh1 C1 C6 12.7(3) . . . . ? Cl1 Rh1 C1 C6 104.7(3) . . . . ? Cl2 Rh1 C1 C6 -91.7(3) . . . . ? C29 Rh2 P2 C39 15.92(16) . . . . ? C30 Rh2 P2 C39 53.45(17) . . . . ? C31 Rh2 P2 C39 88.73(17) . . . . ? C32 Rh2 P2 C39 94.4(3) . . . . ? C33 Rh2 P2 C39 2.6(2) . . . . ? Cl4 Rh2 P2 C39 -175.77(11) . . . . ? Cl3 Rh2 P2 C39 -83.58(12) . . . . ? C29 Rh2 P2 C45 -106.34(16) . . . . ? C30 Rh2 P2 C45 -68.81(17) . . . . ? C31 Rh2 P2 C45 -33.53(18) . . . . ? C32 Rh2 P2 C45 -27.9(3) . . . . ? C33 Rh2 P2 C45 -119.6(2) . . . . ? Cl4 Rh2 P2 C45 61.97(12) . . . . ? Cl3 Rh2 P2 C45 154.16(11) . . . . ? C29 Rh2 P2 C28 137.79(15) . . . . ? C30 Rh2 P2 C28 175.32(16) . . . . ? C31 Rh2 P2 C28 -149.40(16) . . . . ? C32 Rh2 P2 C28 -143.8(3) . . . . ? C33 Rh2 P2 C28 124.5(2) . . . . ? Cl4 Rh2 P2 C28 -53.89(10) . . . . ? Cl3 Rh2 P2 C28 38.30(10) . . . . ? C5 C1 C2 C3 -4.4(3) . . . . ? C6 C1 C2 C3 168.8(3) . . . . ? Rh1 C1 C2 C3 -65.0(2) . . . . ? C5 C1 C2 C7 -173.8(3) . . . . ? C6 C1 C2 C7 -0.5(5) . . . . ? Rh1 C1 C2 C7 125.7(3) . . . . ? C5 C1 C2 Rh1 60.5(2) . . . . ? C6 C1 C2 Rh1 -126.2(3) . . . . ? C5 Rh1 C2 C1 -37.05(18) . . . . ? C3 Rh1 C2 C1 -115.8(3) . . . . ? C4 Rh1 C2 C1 -80.13(19) . . . . ? P1 Rh1 C2 C1 78.30(17) . . . . ? Cl1 Rh1 C2 C1 169.82(16) . . . . ? Cl2 Rh1 C2 C1 -73.2(3) . . . . ? C5 Rh1 C2 C3 78.73(19) . . . . ? C1 Rh1 C2 C3 115.8(3) . . . . ? C4 Rh1 C2 C3 35.65(17) . . . . ? P1 Rh1 C2 C3 -165.93(15) . . . . ? Cl1 Rh1 C2 C3 -74.40(17) . . . . ? Cl2 Rh1 C2 C3 42.5(3) . . . . ? C5 Rh1 C2 C7 -158.9(3) . . . . ? C1 Rh1 C2 C7 -121.8(4) . . . . ? C3 Rh1 C2 C7 122.4(4) . . . . ? C4 Rh1 C2 C7 158.0(3) . . . . ? P1 Rh1 C2 C7 -43.5(3) . . . . ? Cl1 Rh1 C2 C7 48.0(3) . . . . ? Cl2 Rh1 C2 C7 164.9(2) . . . . ? C1 C2 C3 C4 2.7(3) . . . . ? C7 C2 C3 C4 172.2(3) . . . . ? Rh1 C2 C3 C4 -60.7(2) . . . . ? C1 C2 C3 C8 -177.2(3) . . . . ? C7 C2 C3 C8 -7.7(5) . . . . ? Rh1 C2 C3 C8 119.4(3) . . . . ? C1 C2 C3 Rh1 63.5(2) . . . . ? C7 C2 C3 Rh1 -127.0(3) . . . . ? C2 Rh1 C3 C4 119.4(2) . . . . ? C5 Rh1 C3 C4 37.54(18) . . . . ? C1 Rh1 C3 C4 80.54(19) . . . . ? P1 Rh1 C3 C4 141.50(15) . . . . ? Cl1 Rh1 C3 C4 -129.71(16) . . . . ? Cl2 Rh1 C3 C4 -40.43(19) . . . . ? C5 Rh1 C3 C2 -81.89(19) . . . . ? C1 Rh1 C3 C2 -38.90(17) . . . . ? C4 Rh1 C3 C2 -119.4(2) . . . . ? P1 Rh1 C3 C2 22.1(2) . . . . ? Cl1 Rh1 C3 C2 110.86(17) . . . . ? Cl2 Rh1 C3 C2 -159.87(15) . . . . ? C2 Rh1 C3 C8 -118.6(3) . . . . ? C5 Rh1 C3 C8 159.5(3) . . . . ? C1 Rh1 C3 C8 -157.5(3) . . . . ? C4 Rh1 C3 C8 121.9(3) . . . . ? P1 Rh1 C3 C8 -96.6(3) . . . . ? Cl1 Rh1 C3 C8 -7.8(3) . . . . ? Cl2 Rh1 C3 C8 81.5(3) . . . . ? C2 C3 C4 C5 0.0(3) . . . . ? C8 C3 C4 C5 179.9(3) . . . . ? Rh1 C3 C4 C5 -58.6(2) . . . . ? C2 C3 C4 C9 -178.0(3) . . . . ? C8 C3 C4 C9 1.9(5) . . . . ? Rh1 C3 C4 C9 123.4(3) . . . . ? C2 C3 C4 Rh1 58.5(2) . . . . ? C8 C3 C4 Rh1 -121.6(3) . . . . ? C2 Rh1 C4 C3 -37.06(17) . . . . ? C5 Rh1 C4 C3 -119.0(3) . . . . ? C1 Rh1 C4 C3 -80.44(19) . . . . ? P1 Rh1 C4 C3 -100.7(2) . . . . ? Cl1 Rh1 C4 C3 57.31(18) . . . . ? Cl2 Rh1 C4 C3 145.96(16) . . . . ? C2 Rh1 C4 C5 81.9(2) . . . . ? C1 Rh1 C4 C5 38.52(18) . . . . ? C3 Rh1 C4 C5 119.0(3) . . . . ? P1 Rh1 C4 C5 18.2(3) . . . . ? Cl1 Rh1 C4 C5 176.27(16) . . . . ? Cl2 Rh1 C4 C5 -95.08(17) . . . . ? C2 Rh1 C4 C9 -159.7(3) . . . . ? C5 Rh1 C4 C9 118.4(4) . . . . ? C1 Rh1 C4 C9 156.9(3) . . . . ? C3 Rh1 C4 C9 -122.7(4) . . . . ? P1 Rh1 C4 C9 136.6(2) . . . . ? Cl1 Rh1 C4 C9 -65.4(3) . . . . ? Cl2 Rh1 C4 C9 23.3(3) . . . . ? C2 C1 C5 C4 4.4(3) . . . . ? C6 C1 C5 C4 -168.9(3) . . . . ? Rh1 C1 C5 C4 64.8(2) . . . . ? C2 C1 C5 C10 176.8(3) . . . . ? C6 C1 C5 C10 3.5(5) . . . . ? Rh1 C1 C5 C10 -122.8(3) . . . . ? C2 C1 C5 Rh1 -60.4(2) . . . . ? C6 C1 C5 Rh1 126.3(3) . . . . ? C3 C4 C5 C1 -2.7(3) . . . . ? C9 C4 C5 C1 175.3(3) . . . . ? Rh1 C4 C5 C1 -63.4(2) . . . . ? C3 C4 C5 C10 -175.4(3) . . . . ? C9 C4 C5 C10 2.7(5) . . . . ? Rh1 C4 C5 C10 124.0(3) . . . . ? C3 C4 C5 Rh1 60.7(2) . . . . ? C9 C4 C5 Rh1 -121.3(3) . . . . ? C2 Rh1 C5 C1 37.36(18) . . . . ? C3 Rh1 C5 C1 80.1(2) . . . . ? C4 Rh1 C5 C1 115.9(3) . . . . ? P1 Rh1 C5 C1 -56.0(2) . . . . ? Cl1 Rh1 C5 C1 108.5(2) . . . . ? Cl2 Rh1 C5 C1 -157.71(17) . . . . ? C2 Rh1 C5 C4 -78.51(19) . . . . ? C1 Rh1 C5 C4 -115.9(3) . . . . ? C3 Rh1 C5 C4 -35.81(18) . . . . ? P1 Rh1 C5 C4 -171.86(15) . . . . ? Cl1 Rh1 C5 C4 -7.4(3) . . . . ? Cl2 Rh1 C5 C4 86.42(17) . . . . ? C2 Rh1 C5 C10 160.3(3) . . . . ? C1 Rh1 C5 C10 122.9(4) . . . . ? C3 Rh1 C5 C10 -157.0(3) . . . . ? C4 Rh1 C5 C10 -121.2(4) . . . . ? P1 Rh1 C5 C10 66.9(3) . . . . ? Cl1 Rh1 C5 C10 -128.6(3) . . . . ? Cl2 Rh1 C5 C10 -34.8(3) . . . . ? O1 P1 C11 C16 -169.9(2) . . . . ? C17 P1 C11 C16 -67.3(3) . . . . ? Rh1 P1 C11 C16 67.7(3) . . . . ? O1 P1 C11 C12 14.2(3) . . . . ? C17 P1 C11 C12 116.8(3) . . . . ? Rh1 P1 C11 C12 -108.2(3) . . . . ? C16 C11 C12 C13 -2.2(5) . . . . ? P1 C11 C12 C13 173.7(2) . . . . ? C11 C12 C13 C14 1.5(5) . . . . ? C12 C13 C14 C15 0.2(5) . . . . ? C13 C14 C15 C16 -1.1(5) . . . . ? C14 C15 C16 C11 0.3(5) . . . . ? C12 C11 C16 C15 1.3(5) . . . . ? P1 C11 C16 C15 -174.7(3) . . . . ? O1 P1 C17 C18 -129.6(3) . . . . ? C11 P1 C17 C18 131.2(3) . . . . ? Rh1 P1 C17 C18 3.6(3) . . . . ? O1 P1 C17 C22 47.9(3) . . . . ? C11 P1 C17 C22 -51.2(3) . . . . ? Rh1 P1 C17 C22 -178.9(2) . . . . ? C22 C17 C18 C19 0.1(4) . . . . ? P1 C17 C18 C19 177.6(2) . . . . ? C17 C18 C19 C20 -0.6(5) . . . . ? C18 C19 C20 C21 0.8(5) . . . . ? C19 C20 C21 C22 -0.5(5) . . . . ? C20 C21 C22 C17 0.0(5) . . . . ? C18 C17 C22 C21 0.2(5) . . . . ? P1 C17 C22 C21 -177.4(3) . . . . ? P1 O1 C23 C25 -4.3(4) . . . . ? P1 O1 C23 C24 176.2(2) . . . . ? C27 N2 C24 N1 179.9(3) . . . . ? C27 N2 C24 C23 -1.5(4) . . . . ? C28 N1 C24 N2 -9.0(4) . . . . ? C28 N1 C24 C23 172.3(3) . . . . ? C25 C23 C24 N2 2.2(5) . . . . ? O1 C23 C24 N2 -178.3(3) . . . . ? C25 C23 C24 N1 -179.1(3) . . . . ? O1 C23 C24 N1 0.3(4) . . . . ? O1 C23 C25 C26 179.3(3) . . . . ? C24 C23 C25 C26 -1.3(5) . . . . ? C23 C25 C26 C27 -0.3(5) . . . . ? C24 N2 C27 C26 -0.1(5) . . . . ? C25 C26 C27 N2 1.0(5) . . . . ? C24 N1 C28 P2 -82.0(3) . . . . ? C39 P2 C28 N1 39.9(3) . . . . ? C45 P2 C28 N1 149.2(2) . . . . ? Rh2 P2 C28 N1 -84.3(2) . . . . ? C31 Rh2 C29 C30 -37.6(2) . . . . ? C32 Rh2 C29 C30 -80.7(2) . . . . ? C33 Rh2 C29 C30 -115.8(3) . . . . ? P2 Rh2 C29 C30 74.5(2) . . . . ? Cl4 Rh2 C29 C30 -73.3(4) . . . . ? Cl3 Rh2 C29 C30 166.8(2) . . . . ? C30 Rh2 C29 C33 115.8(3) . . . . ? C31 Rh2 C29 C33 78.2(2) . . . . ? C32 Rh2 C29 C33 35.2(2) . . . . ? P2 Rh2 C29 C33 -169.64(18) . . . . ? Cl4 Rh2 C29 C33 42.5(4) . . . . ? Cl3 Rh2 C29 C33 -77.4(2) . . . . ? C30 Rh2 C29 C34 -124.5(6) . . . . ? C31 Rh2 C29 C34 -162.1(5) . . . . ? C32 Rh2 C29 C34 154.9(5) . . . . ? C33 Rh2 C29 C34 119.7(6) . . . . ? P2 Rh2 C29 C34 -50.0(5) . . . . ? Cl4 Rh2 C29 C34 162.2(4) . . . . ? Cl3 Rh2 C29 C34 42.3(5) . . . . ? C33 C29 C30 C31 -3.1(4) . . . . ? C34 C29 C30 C31 -173.9(4) . . . . ? Rh2 C29 C30 C31 61.6(2) . . . . ? C33 C29 C30 C35 172.9(3) . . . . ? C34 C29 C30 C35 2.2(6) . . . . ? Rh2 C29 C30 C35 -122.3(4) . . . . ? C33 C29 C30 Rh2 -64.7(2) . . . . ? C34 C29 C30 Rh2 124.5(4) . . . . ? C29 Rh2 C30 C31 -117.6(3) . . . . ? C32 Rh2 C30 C31 -38.2(2) . . . . ? C33 Rh2 C30 C31 -79.1(2) . . . . ? P2 Rh2 C30 C31 125.6(2) . . . . ? Cl4 Rh2 C30 C31 33.6(3) . . . . ? Cl3 Rh2 C30 C31 -136.7(2) . . . . ? C31 Rh2 C30 C29 117.6(3) . . . . ? C32 Rh2 C30 C29 79.4(2) . . . . ? C33 Rh2 C30 C29 38.4(2) . . . . ? P2 Rh2 C30 C29 -116.8(2) . . . . ? Cl4 Rh2 C30 C29 151.20(18) . . . . ? Cl3 Rh2 C30 C29 -19.1(3) . . . . ? C29 Rh2 C30 C35 120.9(6) . . . . ? C31 Rh2 C30 C35 -121.6(6) . . . . ? C32 Rh2 C30 C35 -159.7(6) . . . . ? C33 Rh2 C30 C35 159.3(6) . . . . ? P2 Rh2 C30 C35 4.0(6) . . . . ? Cl4 Rh2 C30 C35 -87.9(6) . . . . ? Cl3 Rh2 C30 C35 101.8(5) . . . . ? C29 C30 C31 C32 2.0(4) . . . . ? C35 C30 C31 C32 -174.1(3) . . . . ? Rh2 C30 C31 C32 63.3(2) . . . . ? C29 C30 C31 C36 174.3(4) . . . . ? C35 C30 C31 C36 -1.7(6) . . . . ? Rh2 C30 C31 C36 -124.3(4) . . . . ? C29 C30 C31 Rh2 -61.4(2) . . . . ? C35 C30 C31 Rh2 122.6(4) . . . . ? C29 Rh2 C31 C30 37.8(2) . . . . ? C32 Rh2 C31 C30 116.8(3) . . . . ? C33 Rh2 C31 C30 80.6(2) . . . . ? P2 Rh2 C31 C30 -66.6(2) . . . . ? Cl4 Rh2 C31 C30 -155.1(2) . . . . ? Cl3 Rh2 C31 C30 97.0(3) . . . . ? C29 Rh2 C31 C32 -79.0(2) . . . . ? C30 Rh2 C31 C32 -116.8(3) . . . . ? C33 Rh2 C31 C32 -36.2(2) . . . . ? P2 Rh2 C31 C32 176.54(18) . . . . ? Cl4 Rh2 C31 C32 88.1(2) . . . . ? Cl3 Rh2 C31 C32 -19.8(4) . . . . ? C29 Rh2 C31 C36 161.2(6) . . . . ? C30 Rh2 C31 C36 123.4(7) . . . . ? C32 Rh2 C31 C36 -119.8(7) . . . . ? C33 Rh2 C31 C36 -156.1(6) . . . . ? P2 Rh2 C31 C36 56.7(6) . . . . ? Cl4 Rh2 C31 C36 -31.7(6) . . . . ? Cl3 Rh2 C31 C36 -139.6(5) . . . . ? C30 C31 C32 C33 0.0(4) . . . . ? C36 C31 C32 C33 -172.7(4) . . . . ? Rh2 C31 C32 C33 62.2(3) . . . . ? C30 C31 C32 C37 -179.8(3) . . . . ? C36 C31 C32 C37 7.5(6) . . . . ? Rh2 C31 C32 C37 -117.6(4) . . . . ? C30 C31 C32 Rh2 -62.2(2) . . . . ? C36 C31 C32 Rh2 125.1(4) . . . . ? C29 Rh2 C32 C33 -36.6(2) . . . . ? C30 Rh2 C32 C33 -79.9(3) . . . . ? C31 Rh2 C32 C33 -117.9(3) . . . . ? P2 Rh2 C32 C33 -125.8(3) . . . . ? Cl4 Rh2 C32 C33 146.1(2) . . . . ? Cl3 Rh2 C32 C33 51.9(2) . . . . ? C29 Rh2 C32 C31 81.3(2) . . . . ? C30 Rh2 C32 C31 38.1(2) . . . . ? C33 Rh2 C32 C31 117.9(3) . . . . ? P2 Rh2 C32 C31 -7.9(4) . . . . ? Cl4 Rh2 C32 C31 -95.9(2) . . . . ? Cl3 Rh2 C32 C31 169.8(2) . . . . ? C29 Rh2 C32 C37 -162.0(5) . . . . ? C30 Rh2 C32 C37 154.7(5) . . . . ? C31 Rh2 C32 C37 116.7(6) . . . . ? C33 Rh2 C32 C37 -125.4(6) . . . . ? P2 Rh2 C32 C37 108.8(5) . . . . ? Cl4 Rh2 C32 C37 20.7(5) . . . . ? Cl3 Rh2 C32 C37 -73.5(5) . . . . ? C31 C32 C33 C29 -1.9(4) . . . . ? C37 C32 C33 C29 177.9(4) . . . . ? Rh2 C32 C33 C29 58.3(2) . . . . ? C31 C32 C33 C38 178.5(3) . . . . ? C37 C32 C33 C38 -1.7(6) . . . . ? Rh2 C32 C33 C38 -121.3(4) . . . . ? C31 C32 C33 Rh2 -60.2(2) . . . . ? C37 C32 C33 Rh2 119.6(4) . . . . ? C30 C29 C33 C32 3.1(4) . . . . ? C34 C29 C33 C32 174.5(3) . . . . ? Rh2 C29 C33 C32 -60.0(2) . . . . ? C30 C29 C33 C38 -177.3(3) . . . . ? C34 C29 C33 C38 -5.9(6) . . . . ? Rh2 C29 C33 C38 119.6(4) . . . . ? C30 C29 C33 Rh2 63.1(2) . . . . ? C34 C29 C33 Rh2 -125.6(4) . . . . ? C29 Rh2 C33 C32 120.1(3) . . . . ? C30 Rh2 C33 C32 81.3(3) . . . . ? C31 Rh2 C33 C32 38.1(3) . . . . ? P2 Rh2 C33 C32 140.0(2) . . . . ? Cl4 Rh2 C33 C32 -41.9(3) . . . . ? Cl3 Rh2 C33 C32 -134.2(2) . . . . ? C30 Rh2 C33 C29 -38.9(2) . . . . ? C31 Rh2 C33 C29 -82.0(2) . . . . ? C32 Rh2 C33 C29 -120.1(3) . . . . ? P2 Rh2 C33 C29 19.9(3) . . . . ? Cl4 Rh2 C33 C29 -162.05(17) . . . . ? Cl3 Rh2 C33 C29 105.7(2) . . . . ? C29 Rh2 C33 C38 -118.1(5) . . . . ? C30 Rh2 C33 C38 -156.9(5) . . . . ? C31 Rh2 C33 C38 159.9(5) . . . . ? C32 Rh2 C33 C38 121.8(5) . . . . ? P2 Rh2 C33 C38 -98.2(4) . . . . ? Cl4 Rh2 C33 C38 79.9(4) . . . . ? Cl3 Rh2 C33 C38 -12.4(4) . . . . ? C45 P2 C39 C44 9.3(3) . . . . ? C28 P2 C39 C44 115.1(3) . . . . ? Rh2 P2 C39 C44 -120.3(3) . . . . ? C45 P2 C39 C40 -175.8(2) . . . . ? C28 P2 C39 C40 -70.0(3) . . . . ? Rh2 P2 C39 C40 54.6(3) . . . . ? C44 C39 C40 C41 -1.0(5) . . . . ? P2 C39 C40 C41 -176.2(2) . . . . ? C39 C40 C41 C42 1.2(5) . . . . ? C40 C41 C42 C43 -1.1(5) . . . . ? C41 C42 C43 C44 0.7(5) . . . . ? C42 C43 C44 C39 -0.5(5) . . . . ? C40 C39 C44 C43 0.6(5) . . . . ? P2 C39 C44 C43 175.6(3) . . . . ? C39 P2 C45 C50 -121.4(3) . . . . ? C28 P2 C45 C50 126.9(3) . . . . ? Rh2 P2 C45 C50 4.4(3) . . . . ? C39 P2 C45 C46 58.2(3) . . . . ? C28 P2 C45 C46 -53.5(3) . . . . ? Rh2 P2 C45 C46 -176.0(2) . . . . ? C50 C45 C46 C47 1.0(5) . . . . ? P2 C45 C46 C47 -178.6(2) . . . . ? C45 C46 C47 C48 1.0(5) . . . . ? C46 C47 C48 C49 -1.3(5) . . . . ? C47 C48 C49 C50 -0.5(5) . . . . ? C46 C45 C50 C49 -2.8(5) . . . . ? P2 C45 C50 C49 176.8(2) . . . . ? C48 C49 C50 C45 2.6(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1S H1S Cl2 0.89(5) 2.70(5) 3.573(4) 166(4) . N1 H1 Cl3 0.85(3) 2.48(3) 3.148(3) 136(3) . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.870 _refine_diff_density_min -1.505 _refine_diff_density_rms 0.165