# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Hai-Bin Song' 'Zheng-Zhi Zhang' 'Thomas C. W. Mak' _publ_contact_author_name 'Prof Thomas C W Mak' _publ_contact_author_address ; Prof Thomas C W Mak The Chinese University of Hong Kong Department of Chemistry Shatin New Territories Hong Kong SAR, P R CHINA ; _publ_contact_author_email 'TCWMAK@CUHK.EDU.HK' _publ_section_title ; Hetero-binuclear complexes containing a Ru(0)-M(n+) bond bridged by P,N-phosphine ligands: convenient synthesis of tridentate organometallic ligand trans-Ru(CO)3(L)2 (L = phosphine bearing a N-donor substituent) ; data_compound3 _database_code_CSD 169883 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H28 Ag F3 N2 O6 P2 Ru S' _chemical_formula_weight 968.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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 11.1704(16) _cell_length_b 11.4301(17) _cell_length_c 18.240(3) _cell_angle_alpha 75.620(3) _cell_angle_beta 74.322(3) _cell_angle_gamma 64.449(3) _cell_volume 1999.5(5) _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 prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 1.060 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.6450 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14093 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.03 _reflns_number_total 9437 _reflns_number_gt 4764 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9437 _refine_ls_number_parameters 487 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1287 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1501 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.001 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 Ag1 Ag 0.66227(5) 0.83598(5) 0.25151(3) 0.05710(18) Uani 1 1 d . . . Ru1 Ru 0.90600(5) 0.67168(5) 0.28892(3) 0.03807(15) Uani 1 1 d . . . P1 P 0.75717(15) 0.58917(16) 0.38293(9) 0.0399(4) Uani 1 1 d . . . P2 P 0.96767(17) 0.80201(16) 0.17554(9) 0.0445(4) Uani 1 1 d . . . C1 C 0.8380(7) 0.8227(7) 0.3416(4) 0.0547(17) Uani 1 1 d . . . O1 O 0.8055(5) 0.9091(5) 0.3743(3) 0.0726(15) Uani 1 1 d . . . C2 C 1.0748(7) 0.5713(7) 0.3242(4) 0.0515(16) Uani 1 1 d . . . O2 O 1.1751(5) 0.5102(5) 0.3453(3) 0.0799(16) Uani 1 1 d . . . C3 C 0.9047(7) 0.5655(7) 0.2228(4) 0.0545(17) Uani 1 1 d . . . O3 O 0.9052(6) 0.5040(5) 0.1821(3) 0.0878(18) Uani 1 1 d . . . S1 S 0.3590(3) 1.0675(3) 0.24485(15) 0.0996(8) Uani 1 1 d D . . O4 O 0.4823(6) 1.0301(6) 0.2724(4) 0.118(2) Uani 1 1 d . . . O5 O 0.3741(7) 1.0003(6) 0.1843(4) 0.121(2) Uani 1 1 d . . . O6 O 0.2351(7) 1.0992(11) 0.3007(4) 0.188(4) Uani 1 1 d . . . F1 F 0.2196(9) 1.2823(8) 0.1707(5) 0.245(6) Uani 1 1 d D . . F2 F 0.3359(9) 1.3011(6) 0.2414(4) 0.210(4) Uani 1 1 d D . . F3 F 0.4402(9) 1.2135(9) 0.1361(5) 0.204(4) Uani 1 1 d D . . C38 C 0.3379(9) 1.2252(8) 0.1965(5) 0.159(6) Uani 1 1 d D . . N1 N 0.5710(5) 0.6724(6) 0.2923(3) 0.0556(14) Uani 1 1 d . . . N2 N 0.7514(6) 0.8506(6) 0.1155(3) 0.0617(16) Uani 1 1 d . . . C4 C 0.8289(6) 0.4272(6) 0.4395(3) 0.0446(15) Uani 1 1 d . . . C5 C 0.7656(7) 0.3936(7) 0.5130(4) 0.0578(18) Uani 1 1 d . . . H5A H 0.6857 0.4553 0.5355 0.069 Uiso 1 1 calc R . . C6 C 0.8198(8) 0.2696(7) 0.5532(4) 0.070(2) Uani 1 1 d . . . H6A H 0.7765 0.2487 0.6028 0.084 Uiso 1 1 calc R . . C7 C 0.9350(8) 0.1779(7) 0.5216(4) 0.068(2) Uani 1 1 d . . . H7A H 0.9699 0.0943 0.5494 0.081 Uiso 1 1 calc R . . C8 C 1.0010(7) 0.2072(7) 0.4490(5) 0.069(2) Uani 1 1 d . . . H8A H 1.0804 0.1441 0.4273 0.083 Uiso 1 1 calc R . . C9 C 0.9477(7) 0.3326(7) 0.4080(4) 0.0583(18) Uani 1 1 d . . . H9A H 0.9925 0.3531 0.3588 0.070 Uiso 1 1 calc R . . C10 C 0.6505(6) 0.6938(6) 0.4563(3) 0.0409(14) Uani 1 1 d . . . C11 C 0.7138(7) 0.7100(6) 0.5073(3) 0.0507(16) Uani 1 1 d . . . H11A H 0.8065 0.6651 0.5044 0.061 Uiso 1 1 calc R . . C12 C 0.6405(8) 0.7913(7) 0.5614(4) 0.0597(18) Uani 1 1 d . . . H12A H 0.6836 0.8009 0.5953 0.072 Uiso 1 1 calc R . . C13 C 0.5033(8) 0.8590(7) 0.5661(4) 0.064(2) Uani 1 1 d . . . H13A H 0.4539 0.9148 0.6026 0.077 Uiso 1 1 calc R . . C14 C 0.4398(7) 0.8439(7) 0.5167(4) 0.069(2) Uani 1 1 d . . . H14A H 0.3470 0.8892 0.5198 0.083 Uiso 1 1 calc R . . C15 C 0.5137(6) 0.7610(6) 0.4621(4) 0.0513(16) Uani 1 1 d . . . H15A H 0.4698 0.7508 0.4290 0.062 Uiso 1 1 calc R . . C16 C 0.6335(6) 0.5684(6) 0.3420(3) 0.0459(15) Uani 1 1 d . . . C17 C 0.6088(7) 0.4550(7) 0.3586(4) 0.0575(18) Uani 1 1 d . . . H17A H 0.6531 0.3838 0.3928 0.069 Uiso 1 1 calc R . . C18 C 0.5170(8) 0.4501(9) 0.3230(4) 0.074(2) Uani 1 1 d . . . H18A H 0.4979 0.3753 0.3339 0.089 Uiso 1 1 calc R . . C19 C 0.4551(8) 0.5522(9) 0.2729(5) 0.078(2) Uani 1 1 d . . . H19A H 0.3953 0.5486 0.2474 0.094 Uiso 1 1 calc R . . C20 C 0.4826(7) 0.6633(9) 0.2601(4) 0.071(2) Uani 1 1 d . . . H20A H 0.4366 0.7358 0.2271 0.085 Uiso 1 1 calc R . . C21 C 1.1450(7) 0.7480(7) 0.1277(3) 0.0535(17) Uani 1 1 d . . . C22 C 1.2238(7) 0.6156(8) 0.1304(4) 0.070(2) Uani 1 1 d . . . H22A H 1.1864 0.5549 0.1572 0.084 Uiso 1 1 calc R . . C23 C 1.3572(8) 0.5720(10) 0.0938(5) 0.087(3) Uani 1 1 d . . . H23A H 1.4083 0.4824 0.0961 0.105 Uiso 1 1 calc R . . C24 C 1.4149(9) 0.6567(12) 0.0548(5) 0.094(3) Uani 1 1 d . . . H24A H 1.5045 0.6261 0.0297 0.112 Uiso 1 1 calc R . . C25 C 1.3405(10) 0.7877(12) 0.0525(5) 0.107(3) Uani 1 1 d . . . H25A H 1.3802 0.8469 0.0266 0.129 Uiso 1 1 calc R . . C26 C 1.2050(8) 0.8344(8) 0.0887(5) 0.080(2) Uani 1 1 d . . . H26A H 1.1551 0.9243 0.0865 0.096 Uiso 1 1 calc R . . C27 C 0.9234(7) 0.9710(7) 0.1860(4) 0.0551(18) Uani 1 1 d . . . C28 C 0.8161(9) 1.0744(8) 0.1599(5) 0.083(3) Uani 1 1 d . . . H28A H 0.7674 1.0612 0.1309 0.100 Uiso 1 1 calc R . . C29 C 0.7796(11) 1.1978(9) 0.1761(8) 0.131(5) Uani 1 1 d . . . H29A H 0.7059 1.2667 0.1580 0.157 Uiso 1 1 calc R . . C30 C 0.8471(12) 1.2213(11) 0.2171(8) 0.132(5) Uani 1 1 d . . . H30A H 0.8197 1.3055 0.2279 0.159 Uiso 1 1 calc R . . C31 C 0.9577(13) 1.1201(12) 0.2436(6) 0.110(4) Uani 1 1 d . . . H31A H 1.0059 1.1355 0.2719 0.132 Uiso 1 1 calc R . . C32 C 0.9957(9) 0.9958(9) 0.2272(4) 0.079(2) Uani 1 1 d . . . H32A H 1.0710 0.9275 0.2441 0.094 Uiso 1 1 calc R . . C33 C 0.8852(7) 0.8175(6) 0.0957(4) 0.0525(17) Uani 1 1 d . . . C34 C 0.9538(8) 0.7947(8) 0.0222(4) 0.075(2) Uani 1 1 d . . . H34A H 1.0464 0.7736 0.0090 0.090 Uiso 1 1 calc R . . C35 C 0.8816(11) 0.8040(11) -0.0321(5) 0.105(3) Uani 1 1 d . . . H35A H 0.9256 0.7856 -0.0815 0.125 Uiso 1 1 calc R . . C36 C 0.7470(12) 0.8401(11) -0.0115(5) 0.110(4) Uani 1 1 d . . . H36A H 0.6967 0.8496 -0.0472 0.132 Uiso 1 1 calc R . . C37 C 0.6850(9) 0.8626(9) 0.0614(5) 0.085(3) Uani 1 1 d . . . H37A H 0.5918 0.8877 0.0744 0.102 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0511(3) 0.0549(4) 0.0590(3) 0.0031(3) -0.0194(3) -0.0159(3) Ru1 0.0417(3) 0.0389(3) 0.0327(3) -0.0031(2) -0.0074(2) -0.0158(2) P1 0.0415(8) 0.0408(9) 0.0357(8) -0.0037(7) -0.0065(7) -0.0160(8) P2 0.0546(10) 0.0454(10) 0.0358(8) -0.0029(7) -0.0078(7) -0.0238(9) C1 0.058(4) 0.057(5) 0.042(4) 0.000(3) 0.001(3) -0.026(4) O1 0.099(4) 0.058(3) 0.060(3) -0.026(3) 0.004(3) -0.032(3) C2 0.056(4) 0.054(4) 0.047(4) -0.007(3) -0.010(3) -0.025(4) O2 0.054(3) 0.084(4) 0.090(4) 0.001(3) -0.035(3) -0.011(3) C3 0.073(5) 0.051(4) 0.042(4) -0.002(3) 0.003(3) -0.038(4) O3 0.142(5) 0.084(4) 0.067(4) -0.024(3) -0.014(3) -0.068(4) S1 0.0978(18) 0.097(2) 0.0896(18) -0.0282(15) -0.0350(15) -0.0075(15) O4 0.094(4) 0.097(5) 0.151(6) -0.058(4) -0.074(4) 0.025(4) O5 0.164(6) 0.088(5) 0.112(5) -0.035(4) -0.067(5) -0.015(5) O6 0.086(5) 0.349(14) 0.112(6) -0.080(7) 0.037(4) -0.079(7) F1 0.333(11) 0.134(6) 0.234(9) -0.071(6) -0.225(9) 0.066(7) F2 0.383(12) 0.077(4) 0.167(7) -0.031(4) -0.158(8) -0.017(6) F3 0.301(11) 0.235(10) 0.116(6) -0.001(6) -0.018(7) -0.167(9) C38 0.29(2) 0.099(9) 0.090(9) -0.032(7) -0.087(11) -0.044(12) N1 0.056(3) 0.070(4) 0.049(3) 0.002(3) -0.017(3) -0.034(3) N2 0.075(4) 0.071(4) 0.051(3) 0.005(3) -0.033(3) -0.034(4) C4 0.052(4) 0.042(4) 0.039(3) -0.004(3) -0.011(3) -0.017(3) C5 0.060(4) 0.050(4) 0.048(4) -0.002(3) -0.004(3) -0.013(4) C6 0.091(6) 0.057(5) 0.048(4) 0.005(4) -0.010(4) -0.024(5) C7 0.084(6) 0.043(4) 0.070(5) 0.009(4) -0.029(4) -0.020(4) C8 0.059(5) 0.042(4) 0.089(6) -0.011(4) -0.004(4) -0.008(4) C9 0.058(4) 0.045(4) 0.061(4) -0.003(3) -0.006(3) -0.016(4) C10 0.048(4) 0.035(3) 0.035(3) -0.001(3) -0.004(3) -0.016(3) C11 0.057(4) 0.051(4) 0.039(4) -0.008(3) -0.006(3) -0.018(4) C12 0.080(5) 0.055(5) 0.041(4) -0.006(3) -0.010(3) -0.026(4) C13 0.085(6) 0.044(4) 0.053(4) -0.014(3) 0.003(4) -0.021(4) C14 0.054(4) 0.069(5) 0.070(5) -0.020(4) 0.000(4) -0.012(4) C15 0.045(4) 0.049(4) 0.055(4) -0.009(3) -0.011(3) -0.012(3) C16 0.039(3) 0.054(4) 0.044(4) -0.009(3) -0.005(3) -0.019(3) C17 0.071(5) 0.062(5) 0.049(4) -0.007(3) -0.006(3) -0.039(4) C18 0.088(6) 0.099(7) 0.064(5) -0.010(5) -0.009(4) -0.068(5) C19 0.074(5) 0.122(8) 0.067(5) -0.016(5) -0.013(4) -0.064(6) C20 0.059(5) 0.097(6) 0.066(5) -0.002(4) -0.022(4) -0.038(5) C21 0.064(4) 0.058(5) 0.040(4) -0.007(3) -0.004(3) -0.029(4) C22 0.062(5) 0.080(6) 0.052(4) -0.017(4) 0.008(4) -0.020(5) C23 0.073(6) 0.101(7) 0.066(5) -0.030(5) 0.011(4) -0.019(6) C24 0.065(6) 0.138(9) 0.070(6) -0.038(6) 0.020(4) -0.039(7) C25 0.090(7) 0.138(10) 0.097(7) -0.031(7) 0.032(6) -0.069(7) C26 0.073(5) 0.077(6) 0.088(6) -0.017(5) 0.012(4) -0.039(5) C27 0.069(5) 0.056(5) 0.048(4) -0.009(3) 0.003(3) -0.040(4) C28 0.082(6) 0.051(5) 0.118(7) -0.009(5) -0.015(5) -0.030(5) C29 0.105(8) 0.046(6) 0.228(14) -0.037(7) -0.002(8) -0.026(6) C30 0.128(10) 0.087(9) 0.192(14) -0.077(9) 0.060(9) -0.074(8) C31 0.166(11) 0.127(9) 0.084(7) -0.055(7) 0.029(7) -0.110(9) C32 0.105(6) 0.087(6) 0.066(5) -0.017(4) -0.003(5) -0.062(6) C33 0.078(5) 0.046(4) 0.039(4) 0.005(3) -0.016(3) -0.032(4) C34 0.094(6) 0.093(6) 0.038(4) -0.002(4) -0.011(4) -0.041(5) C35 0.137(9) 0.139(9) 0.043(5) -0.012(5) -0.019(5) -0.060(8) C36 0.144(9) 0.149(10) 0.059(6) 0.000(6) -0.055(6) -0.065(9) C37 0.095(6) 0.110(7) 0.062(5) 0.006(5) -0.040(5) -0.048(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O4 2.295(6) . ? Ag1 N1 2.373(5) . ? Ag1 N2 2.404(6) . ? Ag1 Ru1 2.7132(7) . ? Ru1 C3 1.918(7) . ? Ru1 C2 1.926(7) . ? Ru1 C1 1.944(8) . ? Ru1 P2 2.3570(16) . ? Ru1 P1 2.3669(16) . ? P1 C10 1.829(6) . ? P1 C4 1.831(6) . ? P1 C16 1.857(6) . ? P2 C27 1.822(7) . ? P2 C21 1.828(7) . ? P2 C33 1.859(7) . ? C1 O1 1.152(8) . ? C2 O2 1.147(7) . ? C3 O3 1.141(8) . ? S1 O5 1.431(6) . ? S1 O6 1.441(6) . ? S1 O4 1.446(6) . ? S1 C38 1.744(8) . ? F1 C38 1.355(7) . ? F2 C38 1.322(7) . ? F3 C38 1.341(7) . ? N1 C20 1.327(8) . ? N1 C16 1.347(7) . ? N2 C37 1.336(8) . ? N2 C33 1.340(8) . ? C4 C5 1.381(8) . ? C4 C9 1.386(8) . ? C5 C6 1.378(9) . ? C6 C7 1.350(10) . ? C7 C8 1.369(9) . ? C8 C9 1.393(9) . ? C10 C15 1.370(8) . ? C10 C11 1.397(8) . ? C11 C12 1.368(9) . ? C12 C13 1.376(9) . ? C13 C14 1.369(10) . ? C14 C15 1.385(9) . ? C16 C17 1.384(9) . ? C17 C18 1.380(9) . ? C18 C19 1.338(10) . ? C19 C20 1.383(10) . ? C21 C26 1.377(9) . ? C21 C22 1.380(9) . ? C22 C23 1.379(10) . ? C23 C24 1.343(12) . ? C24 C25 1.360(12) . ? C25 C26 1.396(11) . ? C27 C28 1.367(10) . ? C27 C32 1.389(10) . ? C28 C29 1.374(12) . ? C29 C30 1.335(16) . ? C30 C31 1.382(15) . ? C31 C32 1.382(12) . ? C33 C34 1.378(9) . ? C34 C35 1.395(11) . ? C35 C36 1.344(12) . ? C36 C37 1.353(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ag1 N1 105.4(2) . . ? O4 Ag1 N2 107.6(2) . . ? N1 Ag1 N2 110.34(19) . . ? O4 Ag1 Ru1 144.00(15) . . ? N1 Ag1 Ru1 93.85(13) . . ? N2 Ag1 Ru1 93.18(14) . . ? C3 Ru1 C2 103.4(3) . . ? C3 Ru1 C1 156.5(3) . . ? C2 Ru1 C1 100.1(3) . . ? C3 Ru1 P2 86.63(18) . . ? C2 Ru1 P2 102.42(19) . . ? C1 Ru1 P2 88.03(18) . . ? C3 Ru1 P1 86.48(18) . . ? C2 Ru1 P1 102.02(19) . . ? C1 Ru1 P1 89.00(18) . . ? P2 Ru1 P1 155.53(6) . . ? C3 Ru1 Ag1 84.2(2) . . ? C2 Ru1 Ag1 172.4(2) . . ? C1 Ru1 Ag1 72.3(2) . . ? P2 Ru1 Ag1 78.10(4) . . ? P1 Ru1 Ag1 77.86(4) . . ? C10 P1 C4 103.4(3) . . ? C10 P1 C16 103.4(3) . . ? C4 P1 C16 101.6(3) . . ? C10 P1 Ru1 114.82(19) . . ? C4 P1 Ru1 118.4(2) . . ? C16 P1 Ru1 113.3(2) . . ? C27 P2 C21 103.6(3) . . ? C27 P2 C33 104.2(3) . . ? C21 P2 C33 100.9(3) . . ? C27 P2 Ru1 114.6(2) . . ? C21 P2 Ru1 118.6(2) . . ? C33 P2 Ru1 113.0(2) . . ? O1 C1 Ru1 175.6(7) . . ? O2 C2 Ru1 179.2(6) . . ? O3 C3 Ru1 178.4(6) . . ? O5 S1 O6 118.6(5) . . ? O5 S1 O4 114.3(4) . . ? O6 S1 O4 117.1(5) . . ? O5 S1 C38 102.5(4) . . ? O6 S1 C38 98.9(6) . . ? O4 S1 C38 100.6(5) . . ? S1 O4 Ag1 121.4(4) . . ? F2 C38 F3 110.5(8) . . ? F2 C38 F1 107.9(7) . . ? F3 C38 F1 109.1(8) . . ? F2 C38 S1 112.2(6) . . ? F3 C38 S1 107.3(6) . . ? F1 C38 S1 109.8(7) . . ? C20 N1 C16 117.5(6) . . ? C20 N1 Ag1 125.4(5) . . ? C16 N1 Ag1 115.9(4) . . ? C37 N2 C33 118.1(7) . . ? C37 N2 Ag1 125.0(5) . . ? C33 N2 Ag1 115.4(4) . . ? C5 C4 C9 117.9(6) . . ? C5 C4 P1 122.0(5) . . ? C9 C4 P1 120.1(5) . . ? C6 C5 C4 120.6(7) . . ? C7 C6 C5 120.9(7) . . ? C6 C7 C8 120.4(7) . . ? C7 C8 C9 119.3(7) . . ? C4 C9 C8 120.9(6) . . ? C15 C10 C11 118.4(6) . . ? C15 C10 P1 123.9(5) . . ? C11 C10 P1 117.7(5) . . ? C12 C11 C10 120.6(6) . . ? C11 C12 C13 120.4(7) . . ? C14 C13 C12 119.8(7) . . ? C13 C14 C15 120.0(7) . . ? C10 C15 C14 121.0(6) . . ? N1 C16 C17 121.7(6) . . ? N1 C16 P1 114.4(5) . . ? C17 C16 P1 123.8(5) . . ? C18 C17 C16 118.4(7) . . ? C19 C18 C17 120.4(7) . . ? C18 C19 C20 118.1(7) . . ? N1 C20 C19 123.7(7) . . ? C26 C21 C22 117.7(7) . . ? C26 C21 P2 122.7(6) . . ? C22 C21 P2 119.6(5) . . ? C23 C22 C21 120.9(8) . . ? C24 C23 C22 121.3(9) . . ? C23 C24 C25 119.2(8) . . ? C24 C25 C26 120.7(9) . . ? C21 C26 C25 120.3(8) . . ? C28 C27 C32 117.9(7) . . ? C28 C27 P2 123.2(6) . . ? C32 C27 P2 118.8(6) . . ? C27 C28 C29 120.5(10) . . ? C30 C29 C28 121.7(11) . . ? C29 C30 C31 119.7(10) . . ? C30 C31 C32 119.0(11) . . ? C31 C32 C27 121.1(10) . . ? N2 C33 C34 121.6(6) . . ? N2 C33 P2 114.5(5) . . ? C34 C33 P2 124.0(6) . . ? C33 C34 C35 118.7(8) . . ? C36 C35 C34 118.7(8) . . ? C35 C36 C37 120.0(8) . . ? N2 C37 C36 123.0(8) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.833 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.106 #==========================================END data_compound4 _database_code_CSD 169884 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H50 Hg I2 N2 O6 P2 Ru' _chemical_formula_weight 1284.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6934(8) _cell_length_b 12.7794(7) _cell_length_c 24.9176(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.4100(10) _cell_angle_gamma 90.00 _cell_volume 4677.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 5.033 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31692 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.03 _reflns_number_total 11260 _reflns_number_gt 7303 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11260 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0602 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.883 _refine_ls_shift/su_max 0.004 _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 Hg1 Hg 0.621464(12) 0.619312(15) 1.178943(7) 0.04498(6) Uani 1 1 d . . . I1 I 0.61496(2) 0.61083(3) 1.291585(11) 0.05583(9) Uani 1 1 d . . . I2 I 0.52439(2) 0.79773(3) 1.146996(13) 0.06118(10) Uani 1 1 d . . . Ru1 Ru 0.74607(2) 0.51207(3) 1.122563(12) 0.03260(8) Uani 1 1 d . . . P1 P 0.66746(7) 0.35745(9) 1.14864(4) 0.0351(2) Uani 1 1 d . . . P2 P 0.82652(7) 0.66666(9) 1.09814(4) 0.0345(2) Uani 1 1 d . . . C1 C 0.8105(3) 0.5152(3) 1.19189(17) 0.0422(10) Uani 1 1 d . . . O1 O 0.8507(2) 0.5157(3) 1.23102(12) 0.0644(10) Uani 1 1 d . . . C2 C 0.8277(3) 0.4258(4) 1.08165(19) 0.0523(12) Uani 1 1 d . . . O2 O 0.8748(3) 0.3744(3) 1.05844(16) 0.0840(12) Uani 1 1 d . . . C3 C 0.6529(3) 0.5458(4) 1.06844(17) 0.0480(11) Uani 1 1 d . . . O3 O 0.5994(2) 0.5667(3) 1.03662(13) 0.0660(10) Uani 1 1 d . . . C4 C 0.7391(3) 0.2747(3) 1.19197(17) 0.0390(10) Uani 1 1 d . . . C5 C 0.7463(3) 0.2902(4) 1.24738(17) 0.0525(12) Uani 1 1 d . . . H5A H 0.7129 0.3427 1.2636 0.063 Uiso 1 1 calc R . . C6 C 0.8044(4) 0.2263(5) 1.2782(2) 0.0669(16) Uani 1 1 d . . . H6A H 0.8095 0.2364 1.3151 0.080 Uiso 1 1 calc R . . C7 C 0.8536(4) 0.1489(5) 1.2545(3) 0.0730(17) Uani 1 1 d . . . H7A H 0.8905 0.1053 1.2755 0.088 Uiso 1 1 calc R . . C8 C 0.8490(3) 0.1353(4) 1.2004(2) 0.0684(15) Uani 1 1 d . . . H8A H 0.8836 0.0835 1.1844 0.082 Uiso 1 1 calc R . . C9 C 0.7927(3) 0.1989(4) 1.1691(2) 0.0535(12) Uani 1 1 d . . . H9A H 0.7909 0.1903 1.1320 0.064 Uiso 1 1 calc R . . C10 C 0.6345(3) 0.2668(3) 1.09440(17) 0.0414(10) Uani 1 1 d . . . C11 C 0.6446(3) 0.2907(4) 1.04096(18) 0.0554(13) Uani 1 1 d . . . H11A H 0.6708 0.3542 1.0315 0.067 Uiso 1 1 calc R . . C12 C 0.6164(4) 0.2220(5) 1.0012(2) 0.0737(17) Uani 1 1 d . . . H12A H 0.6230 0.2392 0.9653 0.088 Uiso 1 1 calc R . . C13 C 0.5784(4) 0.1281(5) 1.0154(2) 0.0830(19) Uani 1 1 d . . . H13A H 0.5592 0.0818 0.9886 0.100 Uiso 1 1 calc R . . C14 C 0.5685(4) 0.1015(4) 1.0678(2) 0.0776(17) Uani 1 1 d . . . H14A H 0.5436 0.0372 1.0770 0.093 Uiso 1 1 calc R . . C15 C 0.5961(3) 0.1719(4) 1.10747(19) 0.0545(13) Uani 1 1 d . . . H15A H 0.5886 0.1549 1.1434 0.065 Uiso 1 1 calc R . . C16 C 0.5642(3) 0.3703(4) 1.18897(16) 0.0427(10) Uani 1 1 d . . . H16A H 0.5325 0.3037 1.1886 0.051 Uiso 1 1 calc R . . H16B H 0.5827 0.3849 1.2259 0.051 Uiso 1 1 calc R . . N1 N 0.5009(2) 0.4511(3) 1.17109(13) 0.0402(8) Uani 1 1 d . . . C17 C 0.4293(3) 0.4617(4) 1.21164(17) 0.0510(12) Uani 1 1 d . . . H17A H 0.4572 0.4803 1.2460 0.061 Uiso 1 1 calc R . . H17B H 0.3983 0.3953 1.2157 0.061 Uiso 1 1 calc R . . C18 C 0.3625(3) 0.5433(5) 1.1952(2) 0.0659(15) Uani 1 1 d . . . H18A H 0.3162 0.5489 1.2222 0.079 Uiso 1 1 calc R . . H18B H 0.3931 0.6103 1.1930 0.079 Uiso 1 1 calc R . . O4 O 0.3199(2) 0.5195(3) 1.14430(16) 0.0740(11) Uani 1 1 d . . . C19 C 0.3864(3) 0.5080(5) 1.1051(2) 0.0652(15) Uani 1 1 d . . . H19A H 0.4174 0.5743 1.1005 0.078 Uiso 1 1 calc R . . H19B H 0.3568 0.4900 1.0711 0.078 Uiso 1 1 calc R . . C20 C 0.4553(3) 0.4252(4) 1.11947(17) 0.0500(12) Uani 1 1 d . . . H20A H 0.4254 0.3578 1.1221 0.060 Uiso 1 1 calc R . . H20B H 0.5001 0.4206 1.0916 0.060 Uiso 1 1 calc R . . C21 C 0.7905(3) 0.7110(3) 1.03083(16) 0.0400(10) Uani 1 1 d . . . C22 C 0.7195(3) 0.7779(4) 1.02360(19) 0.0600(14) Uani 1 1 d . . . H22A H 0.6900 0.8047 1.0532 0.072 Uiso 1 1 calc R . . C23 C 0.6907(4) 0.8068(5) 0.9720(2) 0.0763(17) Uani 1 1 d . . . H23A H 0.6433 0.8544 0.9674 0.092 Uiso 1 1 calc R . . C24 C 0.7318(4) 0.7656(5) 0.9284(2) 0.0747(17) Uani 1 1 d . . . H24A H 0.7123 0.7849 0.8940 0.090 Uiso 1 1 calc R . . C25 C 0.8012(4) 0.6966(5) 0.9351(2) 0.0743(17) Uani 1 1 d . . . H25A H 0.8286 0.6675 0.9054 0.089 Uiso 1 1 calc R . . C26 C 0.8311(4) 0.6693(4) 0.98640(17) 0.0592(14) Uani 1 1 d . . . H26A H 0.8791 0.6224 0.9909 0.071 Uiso 1 1 calc R . . C27 C 0.9497(3) 0.6523(3) 1.09313(14) 0.0366(10) Uani 1 1 d . . . C28 C 0.9982(3) 0.7302(4) 1.06703(16) 0.0494(12) Uani 1 1 d . . . H28A H 0.9674 0.7875 1.0524 0.059 Uiso 1 1 calc R . . C29 C 1.0921(3) 0.7233(5) 1.06259(19) 0.0618(14) Uani 1 1 d . . . H29A H 1.1239 0.7754 1.0450 0.074 Uiso 1 1 calc R . . C30 C 1.1377(3) 0.6385(5) 1.08458(19) 0.0620(15) Uani 1 1 d . . . H30A H 1.2005 0.6331 1.0814 0.074 Uiso 1 1 calc R . . C31 C 1.0908(3) 0.5624(4) 1.11106(18) 0.0551(13) Uani 1 1 d . . . H31A H 1.1220 0.5060 1.1263 0.066 Uiso 1 1 calc R . . C32 C 0.9974(3) 0.5691(4) 1.11512(16) 0.0456(11) Uani 1 1 d . . . H32A H 0.9662 0.5168 1.1329 0.055 Uiso 1 1 calc R . . C33 C 0.8125(3) 0.7862(3) 1.13804(15) 0.0416(10) Uani 1 1 d . . . H33A H 0.8481 0.8417 1.1223 0.050 Uiso 1 1 calc R . . H33B H 0.7491 0.8072 1.1359 0.050 Uiso 1 1 calc R . . N2 N 0.8399(2) 0.7751(3) 1.19475(13) 0.0420(9) Uani 1 1 d . . . C34 C 0.7818(3) 0.8389(4) 1.22887(17) 0.0546(13) Uani 1 1 d . . . H34A H 0.7189 0.8170 1.2242 0.065 Uiso 1 1 calc R . . H34B H 0.7860 0.9118 1.2184 0.065 Uiso 1 1 calc R . . C35 C 0.8113(3) 0.8269(5) 1.28662(18) 0.0699(16) Uani 1 1 d . . . H35A H 0.7712 0.8675 1.3089 0.084 Uiso 1 1 calc R . . H35B H 0.8060 0.7540 1.2970 0.084 Uiso 1 1 calc R . . O5 O 0.9018(2) 0.8603(3) 1.29561(13) 0.0702(11) Uani 1 1 d . . . C36 C 0.9596(4) 0.7996(5) 1.2636(2) 0.0808(19) Uani 1 1 d . . . H36A H 0.9560 0.7270 1.2747 0.097 Uiso 1 1 calc R . . H36B H 1.0219 0.8227 1.2694 0.097 Uiso 1 1 calc R . . C37 C 0.9349(3) 0.8074(5) 1.20438(18) 0.0602(14) Uani 1 1 d . . . H37A H 0.9429 0.8790 1.1923 0.072 Uiso 1 1 calc R . . H37B H 0.9750 0.7629 1.1841 0.072 Uiso 1 1 calc R . . C38 C -0.1253(8) 0.0047(10) 0.8675(4) 0.220(7) Uani 1 1 d . . . H38A H -0.1819 -0.0306 0.8599 0.331 Uiso 1 1 calc R . . H38B H -0.0968 0.0220 0.8344 0.331 Uiso 1 1 calc R . . H38C H -0.1367 0.0677 0.8873 0.331 Uiso 1 1 calc R . . C39 C -0.0685(7) -0.0600(9) 0.8976(4) 0.168(5) Uani 1 1 d . . . H39A H -0.0602 -0.1241 0.8774 0.202 Uiso 1 1 calc R . . H39B H -0.0997 -0.0784 0.9301 0.202 Uiso 1 1 calc R . . O6 O 0.0178(5) -0.0219(4) 0.9125(2) 0.1223(18) Uani 1 1 d . . . C40 C 0.0680(7) -0.0864(7) 0.9474(4) 0.134(3) Uani 1 1 d . . . H40A H 0.0756 -0.1548 0.9313 0.160 Uiso 1 1 calc R . . H40B H 0.0357 -0.0952 0.9806 0.160 Uiso 1 1 calc R . . C41 C 0.1599(7) -0.0385(7) 0.9593(3) 0.146(3) Uani 1 1 d . . . H41A H 0.1940 -0.0832 0.9833 0.218 Uiso 1 1 calc R . . H41B H 0.1522 0.0288 0.9756 0.218 Uiso 1 1 calc R . . H41C H 0.1921 -0.0307 0.9264 0.218 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.05220(11) 0.04039(11) 0.04249(10) -0.00314(8) 0.00390(7) 0.00526(10) I1 0.0655(2) 0.0645(2) 0.03750(16) -0.00727(15) 0.00049(14) -0.00185(18) I2 0.0720(2) 0.0477(2) 0.0631(2) 0.00266(16) -0.01154(17) 0.01457(18) Ru1 0.04204(19) 0.02882(18) 0.02686(16) -0.00023(14) -0.00050(13) -0.00183(16) P1 0.0419(6) 0.0310(6) 0.0322(5) 0.0015(4) -0.0014(4) -0.0015(5) P2 0.0433(6) 0.0314(6) 0.0289(5) 0.0023(5) -0.0010(4) 0.0006(5) C1 0.052(3) 0.038(3) 0.037(2) 0.005(2) -0.002(2) -0.003(2) O1 0.082(2) 0.068(2) 0.0420(19) 0.0053(17) -0.0201(17) -0.009(2) C2 0.068(3) 0.038(3) 0.052(3) -0.003(2) 0.004(2) -0.007(3) O2 0.092(3) 0.070(3) 0.091(3) -0.035(2) 0.032(2) 0.007(2) C3 0.061(3) 0.044(3) 0.038(2) 0.001(2) -0.003(2) -0.009(3) O3 0.068(2) 0.074(3) 0.055(2) 0.0101(19) -0.0260(17) -0.009(2) C4 0.037(2) 0.033(2) 0.046(2) 0.006(2) -0.0029(19) -0.006(2) C5 0.061(3) 0.054(3) 0.042(3) 0.006(2) -0.004(2) -0.005(3) C6 0.063(3) 0.081(4) 0.056(3) 0.029(3) -0.018(3) -0.014(3) C7 0.053(3) 0.069(4) 0.097(5) 0.038(4) -0.015(3) 0.006(3) C8 0.056(3) 0.056(4) 0.092(4) 0.018(3) -0.011(3) 0.011(3) C9 0.051(3) 0.049(3) 0.060(3) 0.005(2) 0.002(2) 0.006(3) C10 0.041(2) 0.035(3) 0.047(3) -0.005(2) -0.0092(19) -0.002(2) C11 0.077(3) 0.044(3) 0.045(3) -0.001(2) -0.010(2) -0.009(3) C12 0.108(5) 0.065(4) 0.048(3) -0.012(3) -0.016(3) -0.013(4) C13 0.102(5) 0.071(4) 0.075(4) -0.029(4) -0.018(3) -0.020(4) C14 0.094(4) 0.051(4) 0.087(4) -0.012(3) -0.011(3) -0.024(3) C15 0.061(3) 0.047(3) 0.055(3) -0.007(2) -0.006(2) -0.010(3) C16 0.045(2) 0.042(3) 0.041(2) 0.005(2) 0.0011(19) -0.001(2) N1 0.0342(19) 0.039(2) 0.047(2) 0.0059(17) -0.0024(15) -0.0056(18) C17 0.044(3) 0.060(3) 0.050(3) 0.002(2) 0.007(2) 0.000(3) C18 0.050(3) 0.070(4) 0.079(4) 0.002(3) 0.014(3) 0.003(3) O4 0.0428(19) 0.085(3) 0.093(3) 0.014(2) -0.0048(19) 0.007(2) C19 0.051(3) 0.078(4) 0.066(3) 0.013(3) -0.008(3) 0.011(3) C20 0.043(3) 0.060(3) 0.047(3) 0.001(2) -0.007(2) -0.007(3) C21 0.045(2) 0.039(3) 0.036(2) 0.0081(19) -0.0054(18) -0.008(2) C22 0.065(3) 0.066(4) 0.048(3) 0.011(3) -0.006(2) 0.013(3) C23 0.073(4) 0.085(5) 0.069(4) 0.022(3) -0.028(3) 0.010(4) C24 0.098(4) 0.078(4) 0.046(3) 0.015(3) -0.027(3) -0.023(4) C25 0.108(5) 0.075(4) 0.039(3) 0.007(3) -0.013(3) 0.008(4) C26 0.084(4) 0.055(3) 0.038(3) 0.002(2) -0.009(2) 0.011(3) C27 0.043(2) 0.042(3) 0.0247(19) -0.0010(18) -0.0036(17) 0.000(2) C28 0.053(3) 0.052(3) 0.043(3) 0.012(2) 0.000(2) 0.004(3) C29 0.054(3) 0.075(4) 0.056(3) 0.013(3) 0.007(2) -0.009(3) C30 0.047(3) 0.085(4) 0.054(3) -0.002(3) -0.002(2) 0.004(3) C31 0.054(3) 0.059(3) 0.052(3) -0.003(3) -0.010(2) 0.013(3) C32 0.053(3) 0.042(3) 0.041(2) 0.003(2) -0.001(2) 0.005(2) C33 0.048(3) 0.037(3) 0.039(2) 0.0009(19) -0.0017(19) 0.001(2) N2 0.050(2) 0.040(2) 0.0355(19) -0.0027(16) -0.0037(16) 0.0010(19) C34 0.048(3) 0.068(4) 0.048(3) -0.018(2) -0.001(2) 0.006(3) C35 0.063(3) 0.102(5) 0.045(3) -0.026(3) -0.004(2) 0.000(3) O5 0.059(2) 0.094(3) 0.057(2) -0.038(2) -0.0115(16) 0.013(2) C36 0.067(4) 0.109(5) 0.065(4) -0.037(3) -0.021(3) 0.026(4) C37 0.048(3) 0.079(4) 0.053(3) -0.018(3) -0.005(2) 0.008(3) C38 0.284(14) 0.260(15) 0.112(8) 0.045(8) -0.104(8) -0.145(13) C39 0.161(9) 0.210(13) 0.134(9) -0.020(8) 0.018(7) -0.110(10) O6 0.162(5) 0.105(4) 0.100(4) 0.006(3) 0.014(3) -0.025(4) C40 0.156(8) 0.099(7) 0.148(8) 0.031(6) 0.065(7) 0.018(7) C41 0.186(9) 0.123(8) 0.129(7) 0.028(6) 0.014(7) 0.032(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 Hg1 Ru1 2.7075(4) . ? Hg1 N1 2.789(3) . ? Hg1 I2 2.7948(4) . ? Hg1 I1 2.8128(4) . ? Ru1 C2 1.938(5) . ? Ru1 C3 1.947(5) . ? Ru1 C1 1.950(4) . ? Ru1 P1 2.3870(11) . ? Ru1 P2 2.3888(11) . ? P1 C4 1.826(4) . ? P1 C10 1.836(4) . ? P1 C16 1.848(4) . ? P2 C27 1.827(4) . ? P2 C21 1.836(4) . ? P2 C33 1.837(4) . ? C1 O1 1.128(5) . ? C2 O2 1.124(5) . ? C3 O3 1.134(5) . ? C4 C9 1.381(6) . ? C4 C5 1.396(6) . ? C5 C6 1.397(6) . ? C6 C7 1.368(8) . ? C7 C8 1.359(8) . ? C8 C9 1.386(6) . ? C10 C11 1.378(6) . ? C10 C15 1.380(6) . ? C11 C12 1.379(6) . ? C12 C13 1.374(8) . ? C13 C14 1.363(8) . ? C14 C15 1.389(7) . ? C16 N1 1.452(5) . ? N1 C20 1.473(5) . ? N1 C17 1.482(5) . ? C17 C18 1.484(6) . ? C18 O4 1.433(6) . ? O4 C19 1.406(5) . ? C19 C20 1.502(6) . ? C21 C22 1.358(6) . ? C21 C26 1.378(6) . ? C22 C23 1.392(6) . ? C23 C24 1.362(8) . ? C24 C25 1.355(7) . ? C25 C26 1.385(6) . ? C27 C32 1.380(6) . ? C27 C28 1.395(6) . ? C28 C29 1.389(6) . ? C29 C30 1.381(7) . ? C30 C31 1.371(7) . ? C31 C32 1.382(6) . ? C33 N2 1.467(5) . ? N2 C34 1.467(5) . ? N2 C37 1.469(5) . ? C34 C35 1.500(6) . ? C35 O5 1.409(5) . ? O5 C36 1.411(6) . ? C36 C37 1.515(6) . ? C38 C39 1.382(13) . ? C39 O6 1.400(9) . ? O6 C40 1.397(9) . ? C40 C41 1.504(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 Ru1 Hg1 N1 90.56(7) . . ? Ru1 Hg1 I2 127.740(12) . . ? N1 Hg1 I2 106.86(7) . . ? Ru1 Hg1 I1 122.566(12) . . ? N1 Hg1 I1 90.18(7) . . ? I2 Hg1 I1 106.618(12) . . ? C2 Ru1 C3 101.30(19) . . ? C2 Ru1 C1 100.63(19) . . ? C3 Ru1 C1 157.99(19) . . ? C2 Ru1 P1 88.99(14) . . ? C3 Ru1 P1 92.02(14) . . ? C1 Ru1 P1 90.20(13) . . ? C2 Ru1 P2 91.14(14) . . ? C3 Ru1 P2 89.10(14) . . ? C1 Ru1 P2 88.64(13) . . ? P1 Ru1 P2 178.83(4) . . ? C2 Ru1 Hg1 175.13(14) . . ? C3 Ru1 Hg1 76.94(13) . . ? C1 Ru1 Hg1 81.34(13) . . ? P1 Ru1 Hg1 86.55(3) . . ? P2 Ru1 Hg1 93.37(3) . . ? C4 P1 C10 102.0(2) . . ? C4 P1 C16 101.47(19) . . ? C10 P1 C16 104.6(2) . . ? C4 P1 Ru1 111.38(13) . . ? C10 P1 Ru1 116.26(15) . . ? C16 P1 Ru1 118.93(15) . . ? C27 P2 C21 103.44(18) . . ? C27 P2 C33 104.2(2) . . ? C21 P2 C33 101.8(2) . . ? C27 P2 Ru1 115.59(14) . . ? C21 P2 Ru1 110.77(14) . . ? C33 P2 Ru1 119.14(14) . . ? O1 C1 Ru1 177.3(4) . . ? O2 C2 Ru1 178.9(5) . . ? O3 C3 Ru1 178.9(4) . . ? C9 C4 C5 118.5(4) . . ? C9 C4 P1 119.3(3) . . ? C5 C4 P1 122.1(4) . . ? C4 C5 C6 119.4(5) . . ? C7 C6 C5 120.5(5) . . ? C8 C7 C6 120.4(5) . . ? C7 C8 C9 119.8(5) . . ? C4 C9 C8 121.2(5) . . ? C11 C10 C15 118.5(4) . . ? C11 C10 P1 122.6(4) . . ? C15 C10 P1 118.9(3) . . ? C10 C11 C12 121.0(5) . . ? C13 C12 C11 119.3(5) . . ? C14 C13 C12 121.2(5) . . ? C13 C14 C15 119.0(5) . . ? C10 C15 C14 121.0(5) . . ? N1 C16 P1 115.1(3) . . ? C16 N1 C20 112.5(3) . . ? C16 N1 C17 108.4(3) . . ? C20 N1 C17 107.5(3) . . ? C16 N1 Hg1 97.2(2) . . ? C20 N1 Hg1 120.6(3) . . ? C17 N1 Hg1 110.0(3) . . ? N1 C17 C18 110.6(4) . . ? O4 C18 C17 111.5(4) . . ? C19 O4 C18 110.0(4) . . ? O4 C19 C20 112.6(4) . . ? N1 C20 C19 109.9(4) . . ? C22 C21 C26 118.9(4) . . ? C22 C21 P2 121.3(3) . . ? C26 C21 P2 119.6(4) . . ? C21 C22 C23 120.3(5) . . ? C24 C23 C22 120.2(5) . . ? C25 C24 C23 120.0(5) . . ? C24 C25 C26 119.9(5) . . ? C21 C26 C25 120.7(5) . . ? C32 C27 C28 118.4(4) . . ? C32 C27 P2 123.0(3) . . ? C28 C27 P2 118.6(3) . . ? C29 C28 C27 120.7(4) . . ? C30 C29 C28 119.5(5) . . ? C31 C30 C29 120.2(5) . . ? C30 C31 C32 120.2(5) . . ? C27 C32 C31 121.0(5) . . ? N2 C33 P2 114.2(3) . . ? C33 N2 C34 110.8(3) . . ? C33 N2 C37 111.6(3) . . ? C34 N2 C37 108.2(3) . . ? N2 C34 C35 109.9(4) . . ? O5 C35 C34 111.7(4) . . ? C35 O5 C36 108.8(4) . . ? O5 C36 C37 112.4(4) . . ? N2 C37 C36 110.1(4) . . ? C38 C39 O6 117.8(10) . . ? C40 O6 C39 114.9(8) . . ? O6 C40 C41 109.9(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.853 _refine_diff_density_min -0.906 _refine_diff_density_rms 0.099 #==============================================END data_compound5 _database_code_CSD 169885 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H50 Cd I2 N2 O6 P2 Ru' _chemical_formula_weight 1196.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.682(3) _cell_length_b 12.739(3) _cell_length_c 24.921(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.54(3) _cell_angle_gamma 90.00 _cell_volume 4659.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 2.218 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.884 _exptl_absorpt_correction_T_max 1.037 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13197 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.54 _reflns_number_total 7730 _reflns_number_gt 6754 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0888P)^2^+0.0758P] 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 0.0024(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7730 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1688 _refine_ls_wR_factor_gt 0.1605 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.25589(3) 0.51156(4) 0.377838(18) 0.05652(18) Uani 1 1 d . . . P1 P 0.33253(12) 0.35698(13) 0.35115(6) 0.0586(4) Uani 1 1 d . . . P2 P 0.17627(11) 0.66574(13) 0.40304(6) 0.0573(4) Uani 1 1 d . . . C1 C 0.3493(5) 0.5469(5) 0.4307(3) 0.0720(17) Uani 1 1 d . . . O1 O 0.4020(4) 0.5673(4) 0.4628(2) 0.0873(15) Uani 1 1 d . . . C2 C 0.1717(5) 0.4253(6) 0.4170(3) 0.0735(18) Uani 1 1 d . . . O2 O 0.1251(5) 0.3723(5) 0.4407(3) 0.114(2) Uani 1 1 d . . . C3 C 0.1959(5) 0.5202(5) 0.3076(3) 0.0684(17) Uani 1 1 d . . . O3 O 0.1569(4) 0.5223(4) 0.26786(19) 0.0858(14) Uani 1 1 d . . . Cd1 Cd 0.39177(3) 0.60993(4) 0.321108(19) 0.06529(18) Uani 1 1 d . . . I1 I 0.47527(4) 0.79466(4) 0.35476(2) 0.0841(2) Uani 1 1 d . . . I2 I 0.38535(4) 0.61012(4) 0.209290(19) 0.0827(2) Uani 1 1 d . . . C4 C 0.2603(4) 0.2745(5) 0.3077(2) 0.0597(14) Uani 1 1 d . . . C5 C 0.2520(5) 0.2899(6) 0.2531(3) 0.0710(17) Uani 1 1 d . . . H5A H 0.2854 0.3425 0.2368 0.085 Uiso 1 1 calc R . . C6 C 0.1936(6) 0.2269(7) 0.2223(3) 0.089(2) Uani 1 1 d . . . H6A H 0.1872 0.2377 0.1855 0.107 Uiso 1 1 calc R . . C7 C 0.1452(5) 0.1479(7) 0.2468(4) 0.092(2) Uani 1 1 d . . . H7A H 0.1086 0.1032 0.2260 0.111 Uiso 1 1 calc R . . C8 C 0.1508(5) 0.1351(6) 0.3013(4) 0.089(2) Uani 1 1 d . . . H8A H 0.1158 0.0841 0.3177 0.107 Uiso 1 1 calc R . . C9 C 0.2067(5) 0.1963(6) 0.3310(3) 0.0773(19) Uani 1 1 d . . . H9A H 0.2101 0.1868 0.3680 0.093 Uiso 1 1 calc R . . C10 C 0.3675(4) 0.2665(5) 0.4044(3) 0.0641(15) Uani 1 1 d . . . C11 C 0.3572(6) 0.2890(6) 0.4584(3) 0.083(2) Uani 1 1 d . . . H11A H 0.3303 0.3520 0.4682 0.099 Uiso 1 1 calc R . . C12 C 0.3862(7) 0.2196(7) 0.4978(3) 0.101(3) Uani 1 1 d . . . H12A H 0.3807 0.2368 0.5338 0.121 Uiso 1 1 calc R . . C13 C 0.4231(7) 0.1253(8) 0.4834(4) 0.112(3) Uani 1 1 d . . . H13A H 0.4423 0.0779 0.5098 0.135 Uiso 1 1 calc R . . C14 C 0.4316(7) 0.1011(7) 0.4311(4) 0.104(3) Uani 1 1 d . . . H14A H 0.4556 0.0362 0.4217 0.124 Uiso 1 1 calc R . . C15 C 0.4057(5) 0.1700(6) 0.3915(3) 0.080(2) Uani 1 1 d . . . H15A H 0.4137 0.1524 0.3557 0.096 Uiso 1 1 calc R . . C16 C 0.4348(4) 0.3694(5) 0.3102(3) 0.0625(15) Uani 1 1 d . . . H16A H 0.4678 0.3035 0.3117 0.075 Uiso 1 1 calc R . . H16B H 0.4154 0.3809 0.2731 0.075 Uiso 1 1 calc R . . N1 N 0.4971(3) 0.4540(4) 0.3264(2) 0.0634(13) Uani 1 1 d . . . C17 C 0.5423(5) 0.4305(6) 0.3782(3) 0.0736(18) Uani 1 1 d . . . H17A H 0.5716 0.3623 0.3764 0.088 Uiso 1 1 calc R . . H17B H 0.4973 0.4276 0.4060 0.088 Uiso 1 1 calc R . . C18 C 0.6129(5) 0.5134(7) 0.3924(3) 0.086(2) Uani 1 1 d . . . H18A H 0.5829 0.5808 0.3960 0.103 Uiso 1 1 calc R . . H18B H 0.6417 0.4963 0.4268 0.103 Uiso 1 1 calc R . . O4 O 0.6796(4) 0.5210(5) 0.3535(3) 0.0968(17) Uani 1 1 d . . . C19 C 0.6377(5) 0.5430(7) 0.3028(4) 0.087(2) Uani 1 1 d . . . H19A H 0.6843 0.5476 0.2761 0.105 Uiso 1 1 calc R . . H19B H 0.6073 0.6105 0.3044 0.105 Uiso 1 1 calc R . . C20 C 0.5706(4) 0.4616(6) 0.2864(3) 0.0726(18) Uani 1 1 d . . . H20A H 0.6011 0.3943 0.2836 0.087 Uiso 1 1 calc R . . H20B H 0.5442 0.4791 0.2515 0.087 Uiso 1 1 calc R . . C21 C 0.0529(4) 0.6515(5) 0.4073(2) 0.0620(15) Uani 1 1 d . . . C22 C 0.0039(5) 0.7283(6) 0.4341(3) 0.0706(17) Uani 1 1 d . . . H22A H 0.0345 0.7850 0.4496 0.085 Uiso 1 1 calc R . . C23 C -0.0891(5) 0.7210(7) 0.4378(3) 0.088(2) Uani 1 1 d . . . H23A H -0.1208 0.7726 0.4560 0.105 Uiso 1 1 calc R . . C24 C -0.1365(5) 0.6365(7) 0.4145(3) 0.084(2) Uani 1 1 d . . . H24A H -0.1993 0.6309 0.4174 0.101 Uiso 1 1 calc R . . C25 C -0.0884(5) 0.5620(6) 0.3872(3) 0.0790(19) Uani 1 1 d . . . H25A H -0.1188 0.5058 0.3711 0.095 Uiso 1 1 calc R . . C26 C 0.0056(5) 0.5706(6) 0.3838(3) 0.0708(17) Uani 1 1 d . . . H26A H 0.0373 0.5198 0.3650 0.085 Uiso 1 1 calc R . . C27 C 0.2110(5) 0.7083(5) 0.4710(2) 0.0632(15) Uani 1 1 d . . . C28 C 0.2814(5) 0.7789(6) 0.4791(3) 0.082(2) Uani 1 1 d . . . H28A H 0.3099 0.8087 0.4499 0.098 Uiso 1 1 calc R . . C29 C 0.3091(6) 0.8050(8) 0.5303(4) 0.101(3) Uani 1 1 d . . . H29A H 0.3558 0.8534 0.5357 0.121 Uiso 1 1 calc R . . C30 C 0.2692(6) 0.7610(8) 0.5732(3) 0.094(2) Uani 1 1 d . . . H30A H 0.2890 0.7790 0.6077 0.112 Uiso 1 1 calc R . . C31 C 0.1999(7) 0.6903(7) 0.5659(3) 0.097(3) Uani 1 1 d . . . H31A H 0.1721 0.6606 0.5954 0.116 Uiso 1 1 calc R . . C32 C 0.1718(6) 0.6637(6) 0.5152(3) 0.082(2) Uani 1 1 d . . . H32A H 0.1254 0.6146 0.5103 0.098 Uiso 1 1 calc R . . C33 C 0.1899(5) 0.7861(5) 0.3630(2) 0.0633(15) Uani 1 1 d . . . H33A H 0.1551 0.8420 0.3792 0.076 Uiso 1 1 calc R . . H33B H 0.2536 0.8067 0.3647 0.076 Uiso 1 1 calc R . . N2 N 0.1616(4) 0.7768(4) 0.30744(19) 0.0624(12) Uani 1 1 d . . . C34 C 0.0672(5) 0.8116(7) 0.2969(3) 0.085(2) Uani 1 1 d . . . H34A H 0.0610 0.8838 0.3086 0.101 Uiso 1 1 calc R . . H34B H 0.0264 0.7689 0.3178 0.101 Uiso 1 1 calc R . . C35 C 0.0401(5) 0.8037(8) 0.2389(3) 0.094(3) Uani 1 1 d . . . H35A H 0.0401 0.7306 0.2280 0.113 Uiso 1 1 calc R . . H35B H -0.0213 0.8307 0.2335 0.113 Uiso 1 1 calc R . . O5 O 0.1006(4) 0.8613(5) 0.2065(2) 0.0900(16) Uani 1 1 d . . . C36 C 0.1893(6) 0.8262(8) 0.2149(3) 0.090(2) Uani 1 1 d . . . H36A H 0.2297 0.8661 0.1924 0.108 Uiso 1 1 calc R . . H36B H 0.1932 0.7530 0.2044 0.108 Uiso 1 1 calc R . . C37 C 0.2199(5) 0.8373(6) 0.2723(3) 0.0743(18) Uani 1 1 d . . . H37A H 0.2823 0.8130 0.2766 0.089 Uiso 1 1 calc R . . H37B H 0.2182 0.9108 0.2825 0.089 Uiso 1 1 calc R . . C38 C -0.1260(14) 0.9924(17) 0.3681(7) 0.236(11) Uani 1 1 d . . . H38A H -0.1820 1.0273 0.3583 0.353 Uiso 1 1 calc R . . H38B H -0.1386 0.9334 0.3906 0.353 Uiso 1 1 calc R . . H38C H -0.0970 0.9685 0.3362 0.353 Uiso 1 1 calc R . . C39 C -0.0663(13) 1.0646(15) 0.3967(8) 0.198(9) Uani 1 1 d . . . H39A H -0.0554 1.1247 0.3738 0.238 Uiso 1 1 calc R . . H39B H -0.0969 1.0896 0.4282 0.238 Uiso 1 1 calc R . . O6 O 0.0181(8) 1.0214(7) 0.4129(4) 0.153(3) Uani 1 1 d . . . C40 C 0.0671(12) 1.0833(12) 0.4473(7) 0.167(6) Uani 1 1 d . . . H40A H 0.0354 1.0901 0.4807 0.201 Uiso 1 1 calc R . . H40B H 0.0733 1.1529 0.4319 0.201 Uiso 1 1 calc R . . C41 C 0.1577(11) 1.0380(12) 0.4577(6) 0.174(6) Uani 1 1 d . . . H41A H 0.1919 1.0827 0.4818 0.261 Uiso 1 1 calc R . . H41B H 0.1891 1.0317 0.4246 0.261 Uiso 1 1 calc R . . H41C H 0.1514 0.9698 0.4736 0.261 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0708(3) 0.0503(3) 0.0486(3) -0.0002(2) 0.0026(2) 0.0018(2) P1 0.0704(10) 0.0496(9) 0.0555(8) -0.0017(7) -0.0006(7) 0.0014(7) P2 0.0701(10) 0.0513(9) 0.0506(8) -0.0019(7) 0.0033(7) 0.0012(7) C1 0.092(5) 0.056(4) 0.068(4) 0.000(3) 0.003(4) 0.011(4) O1 0.097(4) 0.092(4) 0.072(3) -0.010(3) -0.016(3) 0.007(3) C2 0.092(5) 0.060(4) 0.069(4) 0.006(4) 0.007(4) 0.009(4) O2 0.135(5) 0.099(4) 0.109(4) 0.033(4) 0.037(4) -0.010(4) C3 0.081(4) 0.058(4) 0.066(4) -0.009(3) 0.006(3) 0.007(3) O3 0.109(4) 0.085(4) 0.062(3) -0.004(3) -0.021(3) 0.007(3) Cd1 0.0765(3) 0.0589(3) 0.0606(3) 0.0016(2) 0.0032(2) -0.0038(2) I1 0.0984(4) 0.0677(3) 0.0857(3) -0.0028(2) -0.0089(3) -0.0114(2) I2 0.0957(4) 0.0893(4) 0.0630(3) 0.0086(2) 0.0036(2) 0.0018(3) C4 0.064(4) 0.048(3) 0.067(3) -0.005(3) -0.003(3) 0.004(3) C5 0.073(4) 0.071(4) 0.068(4) -0.016(3) -0.004(3) -0.002(3) C6 0.098(6) 0.095(6) 0.073(4) -0.025(5) -0.017(4) 0.018(5) C7 0.073(5) 0.085(6) 0.119(7) -0.035(6) -0.013(5) -0.002(4) C8 0.072(5) 0.072(5) 0.123(7) -0.016(5) -0.003(5) -0.008(4) C9 0.078(5) 0.064(4) 0.089(5) 0.000(4) 0.000(4) -0.001(3) C10 0.072(4) 0.057(4) 0.063(3) 0.007(3) -0.003(3) 0.004(3) C11 0.107(6) 0.069(5) 0.072(4) 0.002(4) -0.004(4) 0.002(4) C12 0.149(8) 0.085(6) 0.067(4) 0.016(4) -0.025(5) 0.012(5) C13 0.146(9) 0.094(7) 0.095(6) 0.035(6) -0.020(6) 0.022(6) C14 0.124(7) 0.068(5) 0.118(7) 0.021(5) -0.015(6) 0.020(5) C15 0.093(5) 0.067(4) 0.080(4) 0.003(4) -0.003(4) 0.018(4) C16 0.071(4) 0.053(3) 0.063(3) -0.008(3) 0.000(3) 0.003(3) N1 0.066(3) 0.062(3) 0.062(3) -0.004(3) -0.005(2) 0.002(2) C17 0.074(4) 0.081(5) 0.066(4) -0.003(4) -0.002(3) 0.001(4) C18 0.080(5) 0.084(5) 0.094(5) -0.016(4) -0.007(4) -0.009(4) O4 0.071(3) 0.107(4) 0.111(4) -0.011(4) -0.003(3) -0.007(3) C19 0.071(4) 0.086(5) 0.106(6) -0.005(5) 0.019(4) -0.006(4) C20 0.065(4) 0.071(4) 0.082(4) -0.007(4) 0.015(3) 0.001(3) C21 0.076(4) 0.057(4) 0.053(3) 0.000(3) 0.010(3) 0.001(3) C22 0.072(4) 0.070(4) 0.070(4) -0.009(3) 0.003(3) -0.002(3) C23 0.081(5) 0.106(6) 0.077(4) -0.010(5) 0.014(4) 0.013(5) C24 0.069(4) 0.113(7) 0.069(4) 0.008(5) 0.000(3) -0.017(4) C25 0.084(5) 0.078(5) 0.075(4) 0.003(4) -0.002(4) -0.012(4) C26 0.079(4) 0.068(4) 0.065(4) -0.005(3) -0.002(3) -0.004(3) C27 0.073(4) 0.058(4) 0.058(3) -0.005(3) -0.003(3) 0.002(3) C28 0.088(5) 0.083(5) 0.074(4) -0.013(4) -0.003(4) -0.009(4) C29 0.106(6) 0.108(7) 0.087(5) -0.030(5) -0.024(5) -0.012(5) C30 0.114(7) 0.102(6) 0.064(4) -0.016(5) -0.014(4) 0.011(5) C31 0.137(8) 0.099(6) 0.054(4) 0.001(4) -0.007(4) -0.011(6) C32 0.111(6) 0.076(5) 0.059(4) 0.000(4) -0.001(4) -0.005(4) C33 0.073(4) 0.057(4) 0.059(3) -0.004(3) 0.001(3) -0.003(3) N2 0.074(3) 0.057(3) 0.056(3) 0.006(2) -0.001(2) -0.006(2) C34 0.073(4) 0.095(5) 0.086(5) 0.022(4) 0.003(4) -0.003(4) C35 0.081(5) 0.113(7) 0.088(5) 0.029(5) -0.016(4) -0.017(5) O5 0.082(3) 0.108(4) 0.079(3) 0.032(3) -0.010(3) -0.011(3) C36 0.088(5) 0.118(7) 0.066(4) 0.012(5) 0.001(4) -0.013(5) C37 0.071(4) 0.083(5) 0.069(4) 0.011(4) 0.005(3) -0.008(4) C38 0.31(3) 0.22(2) 0.170(15) -0.021(15) -0.086(17) 0.10(2) C39 0.195(17) 0.193(19) 0.209(19) 0.047(15) 0.059(15) 0.103(15) O6 0.218(10) 0.114(6) 0.127(6) 0.008(5) 0.021(7) 0.026(7) C40 0.196(15) 0.121(10) 0.188(14) -0.059(11) 0.069(13) -0.026(11) C41 0.215(17) 0.142(12) 0.166(13) -0.004(10) 0.018(12) -0.001(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 C1 1.930(8) . ? Ru1 C2 1.937(7) . ? Ru1 C3 1.941(7) . ? Ru1 P1 2.3720(17) . ? Ru1 P2 2.3787(17) . ? Ru1 Cd1 2.7750(9) . ? P1 C10 1.822(6) . ? P1 C4 1.827(6) . ? P1 C16 1.845(6) . ? P2 C21 1.827(7) . ? P2 C27 1.836(6) . ? P2 C33 1.844(6) . ? C1 O1 1.129(8) . ? C2 O2 1.139(8) . ? C3 O3 1.131(8) . ? Cd1 N1 2.519(5) . ? Cd1 I1 2.7728(8) . ? Cd1 I2 2.7857(9) . ? C4 C5 1.377(9) . ? C4 C9 1.405(9) . ? C5 C6 1.389(10) . ? C6 C7 1.383(12) . ? C7 C8 1.368(13) . ? C8 C9 1.341(10) . ? C10 C11 1.388(10) . ? C10 C15 1.392(9) . ? C11 C12 1.378(10) . ? C12 C13 1.370(12) . ? C13 C14 1.350(14) . ? C14 C15 1.368(11) . ? C16 N1 1.464(8) . ? N1 C17 1.467(8) . ? N1 C20 1.492(8) . ? C17 C18 1.515(10) . ? C18 O4 1.400(9) . ? O4 C19 1.418(10) . ? C19 C20 1.480(10) . ? C21 C26 1.366(9) . ? C21 C22 1.394(9) . ? C22 C23 1.374(10) . ? C23 C24 1.400(11) . ? C24 C25 1.373(11) . ? C25 C26 1.391(9) . ? C27 C28 1.381(10) . ? C27 C32 1.381(9) . ? C28 C29 1.370(11) . ? C29 C30 1.353(12) . ? C30 C31 1.368(12) . ? C31 C32 1.361(10) . ? C33 N2 1.439(8) . ? N2 C37 1.460(8) . ? N2 C34 1.471(9) . ? C34 C35 1.494(11) . ? C35 O5 1.420(9) . ? O5 C36 1.387(9) . ? C36 C37 1.495(10) . ? C38 C39 1.45(2) . ? C39 O6 1.405(17) . ? O6 C40 1.356(15) . ? C40 C41 1.467(18) . ? 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 C1 Ru1 C2 103.9(3) . . ? C1 Ru1 C3 154.1(3) . . ? C2 Ru1 C3 101.9(3) . . ? C1 Ru1 P1 93.0(2) . . ? C2 Ru1 P1 89.1(2) . . ? C3 Ru1 P1 90.10(19) . . ? C1 Ru1 P2 88.4(2) . . ? C2 Ru1 P2 90.6(2) . . ? C3 Ru1 P2 88.67(19) . . ? P1 Ru1 P2 178.64(6) . . ? C1 Ru1 Cd1 74.7(2) . . ? C2 Ru1 Cd1 171.9(2) . . ? C3 Ru1 Cd1 80.2(2) . . ? P1 Ru1 Cd1 83.05(5) . . ? P2 Ru1 Cd1 97.28(5) . . ? C10 P1 C4 102.5(3) . . ? C10 P1 C16 103.9(3) . . ? C4 P1 C16 100.9(3) . . ? C10 P1 Ru1 116.6(2) . . ? C4 P1 Ru1 111.8(2) . . ? C16 P1 Ru1 118.9(2) . . ? C21 P2 C27 103.1(3) . . ? C21 P2 C33 103.7(3) . . ? C27 P2 C33 102.8(3) . . ? C21 P2 Ru1 115.4(2) . . ? C27 P2 Ru1 111.1(2) . . ? C33 P2 Ru1 118.8(2) . . ? O1 C1 Ru1 177.9(6) . . ? O2 C2 Ru1 177.3(7) . . ? O3 C3 Ru1 176.1(6) . . ? N1 Cd1 I1 112.81(12) . . ? N1 Cd1 Ru1 93.77(12) . . ? I1 Cd1 Ru1 123.18(2) . . ? N1 Cd1 I2 93.29(12) . . ? I1 Cd1 I2 107.74(3) . . ? Ru1 Cd1 I2 120.30(3) . . ? C5 C4 C9 118.3(6) . . ? C5 C4 P1 122.6(5) . . ? C9 C4 P1 119.0(5) . . ? C4 C5 C6 120.0(7) . . ? C7 C6 C5 119.6(8) . . ? C8 C7 C6 120.4(8) . . ? C9 C8 C7 119.9(8) . . ? C8 C9 C4 121.7(8) . . ? C11 C10 C15 117.5(7) . . ? C11 C10 P1 122.7(5) . . ? C15 C10 P1 119.8(5) . . ? C12 C11 C10 121.2(8) . . ? C13 C12 C11 119.6(8) . . ? C14 C13 C12 120.0(8) . . ? C13 C14 C15 121.3(9) . . ? C14 C15 C10 120.3(8) . . ? N1 C16 P1 114.9(4) . . ? C16 N1 C17 111.0(5) . . ? C16 N1 C20 108.7(5) . . ? C17 N1 C20 106.4(5) . . ? C16 N1 Cd1 100.8(3) . . ? C17 N1 Cd1 118.1(4) . . ? C20 N1 Cd1 111.6(4) . . ? N1 C17 C18 110.7(6) . . ? O4 C18 C17 111.9(6) . . ? C18 O4 C19 109.6(6) . . ? O4 C19 C20 112.1(7) . . ? C19 C20 N1 110.4(6) . . ? C26 C21 C22 118.2(6) . . ? C26 C21 P2 122.9(5) . . ? C22 C21 P2 118.9(5) . . ? C23 C22 C21 120.7(7) . . ? C22 C23 C24 120.5(7) . . ? C25 C24 C23 118.7(7) . . ? C24 C25 C26 120.0(7) . . ? C21 C26 C25 121.8(7) . . ? C28 C27 C32 118.5(7) . . ? C28 C27 P2 121.1(5) . . ? C32 C27 P2 120.2(6) . . ? C29 C28 C27 119.8(8) . . ? C30 C29 C28 120.7(9) . . ? C29 C30 C31 120.3(8) . . ? C32 C31 C30 119.5(8) . . ? C31 C32 C27 121.1(8) . . ? N2 C33 P2 114.8(4) . . ? C33 N2 C37 112.0(5) . . ? C33 N2 C34 113.2(5) . . ? C37 N2 C34 107.4(5) . . ? N2 C34 C35 112.2(7) . . ? O5 C35 C34 111.1(6) . . ? C36 O5 C35 110.4(6) . . ? O5 C36 C37 111.7(7) . . ? N2 C37 C36 111.0(6) . . ? O6 C39 C38 114.3(16) . . ? C40 O6 C39 113.8(14) . . ? O6 C40 C41 110.2(12) . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 25.54 _diffrn_measured_fraction_theta_full 0.886 _refine_diff_density_max 1.250 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.129 #==============================================END data_compound61 _database_code_CSD 169886 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H42 Cl4 N2 O4 P2 Ru' _chemical_formula_weight 883.54 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0622(18) _cell_length_b 11.362(2) _cell_length_c 18.146(4) _cell_angle_alpha 95.479(17) _cell_angle_beta 94.424(17) _cell_angle_gamma 113.047(13) _cell_volume 2072.8(7) _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 colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type PSI-SCAN _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8671 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.1213 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7300 _reflns_number_gt 4132 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7300 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1363 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1531 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.33284(6) 0.50185(6) 1.25663(3) 0.04112(19) Uani 1 1 d . . . P1 P 0.2521(2) 0.3196(2) 1.15934(10) 0.0517(5) Uani 1 1 d . . . P2 P 0.43709(18) 0.67852(17) 1.35611(9) 0.0403(5) Uani 1 1 d . . . Cl1 Cl 0.52399(19) 0.59755(18) 1.19005(10) 0.0559(5) Uani 1 1 d . . . Cl2 Cl 0.44204(18) 0.37996(17) 1.31729(9) 0.0495(5) Uani 1 1 d . . . C1 C 0.2435(8) 0.5915(8) 1.2137(4) 0.061(2) Uani 1 1 d . . . O1 O 0.1879(6) 0.6494(6) 1.1904(3) 0.092(2) Uani 1 1 d . . . C2 C 0.1905(8) 0.4230(7) 1.3117(4) 0.052(2) Uani 1 1 d . . . O2 O 0.1064(6) 0.3724(6) 1.3438(3) 0.0774(18) Uani 1 1 d . . . C3 C 0.1774(8) 0.3420(10) 1.0722(4) 0.069(2) Uani 1 1 d . . . C4 C 0.2241(9) 0.4610(11) 1.0472(5) 0.084(3) Uani 1 1 d . . . H4A H 0.2894 0.5309 1.0777 0.100 Uiso 1 1 calc R . . C5 C 0.1771(12) 0.4800(14) 0.9783(5) 0.122(4) Uani 1 1 d . . . H5A H 0.2104 0.5611 0.9627 0.147 Uiso 1 1 calc R . . C6 C 0.0806(13) 0.3770(18) 0.9335(6) 0.156(7) Uani 1 1 d . . . H6A H 0.0486 0.3879 0.8868 0.187 Uiso 1 1 calc R . . C7 C 0.0312(11) 0.2584(15) 0.9568(6) 0.138(6) Uani 1 1 d . . . H7A H -0.0370 0.1901 0.9269 0.166 Uiso 1 1 calc R . . C8 C 0.0820(9) 0.2383(10) 1.0255(4) 0.094(3) Uani 1 1 d . . . H8B H 0.0519 0.1561 1.0395 0.113 Uiso 1 1 calc R . . C9 C 0.1285(9) 0.1772(8) 1.1875(4) 0.062(2) Uani 1 1 d . . . C10 C 0.1597(10) 0.0818(10) 1.2142(4) 0.082(3) Uani 1 1 d . . . H10A H 0.2461 0.0879 1.2149 0.098 Uiso 1 1 calc R . . C11 C 0.0664(16) -0.0232(12) 1.2403(6) 0.109(4) Uani 1 1 d . . . H11A H 0.0890 -0.0867 1.2584 0.131 Uiso 1 1 calc R . . C12 C -0.0606(17) -0.0297(12) 1.2384(6) 0.119(6) Uani 1 1 d . . . H12A H -0.1256 -0.1008 1.2536 0.143 Uiso 1 1 calc R . . C13 C -0.0935(12) 0.0651(13) 1.2149(6) 0.113(4) Uani 1 1 d . . . H13A H -0.1791 0.0604 1.2163 0.136 Uiso 1 1 calc R . . C14 C 0.0019(10) 0.1700(10) 1.1884(5) 0.083(3) Uani 1 1 d . . . H14A H -0.0206 0.2345 1.1716 0.100 Uiso 1 1 calc R . . C15 C 0.3937(8) 0.2739(7) 1.1317(4) 0.059(2) Uani 1 1 d . . . H15A H 0.4684 0.3501 1.1231 0.071 Uiso 1 1 calc R . . H15B H 0.4228 0.2355 1.1712 0.071 Uiso 1 1 calc R . . N1 N 0.3424(6) 0.1808(6) 1.0630(3) 0.0580(17) Uani 1 1 d . . . C16 C 0.3690(9) 0.0658(9) 1.0678(4) 0.080(3) Uani 1 1 d . . . H16A H 0.3288 0.0236 1.1091 0.096 Uiso 1 1 calc R . . H16B H 0.4638 0.0902 1.0773 0.096 Uiso 1 1 calc R . . C17 C 0.3137(11) -0.0272(9) 0.9957(5) 0.090(3) Uani 1 1 d . . . H17A H 0.3332 -0.1026 0.9997 0.108 Uiso 1 1 calc R . . H17B H 0.2182 -0.0554 0.9880 0.108 Uiso 1 1 calc R . . O3 O 0.3680(7) 0.0309(6) 0.9346(3) 0.0879(19) Uani 1 1 d . . . C18 C 0.3402(11) 0.1419(9) 0.9291(5) 0.097(3) Uani 1 1 d . . . H18A H 0.2450 0.1159 0.9207 0.116 Uiso 1 1 calc R . . H18B H 0.3775 0.1818 0.8866 0.116 Uiso 1 1 calc R . . C19 C 0.3950(10) 0.2376(8) 0.9973(5) 0.086(3) Uani 1 1 d . . . H19A H 0.4907 0.2683 1.0041 0.103 Uiso 1 1 calc R . . H19B H 0.3727 0.3110 0.9917 0.103 Uiso 1 1 calc R . . C20 C 0.3370(7) 0.6602(6) 1.4321(4) 0.0415(17) Uani 1 1 d . . . C21 C 0.3608(8) 0.6130(7) 1.4966(4) 0.054(2) Uani 1 1 d . . . H21A H 0.4361 0.5958 1.5043 0.065 Uiso 1 1 calc R . . C22 C 0.2744(8) 0.5909(7) 1.5501(4) 0.064(2) Uani 1 1 d . . . H22A H 0.2914 0.5579 1.5928 0.076 Uiso 1 1 calc R . . C23 C 0.1644(8) 0.6175(7) 1.5403(5) 0.064(2) Uani 1 1 d . . . H23A H 0.1077 0.6046 1.5768 0.076 Uiso 1 1 calc R . . C24 C 0.1381(8) 0.6629(7) 1.4768(5) 0.063(2) Uani 1 1 d . . . H24A H 0.0626 0.6798 1.4698 0.076 Uiso 1 1 calc R . . C25 C 0.2230(7) 0.6842(7) 1.4227(4) 0.0523(19) Uani 1 1 d . . . H25A H 0.2037 0.7148 1.3795 0.063 Uiso 1 1 calc R . . C26 C 0.4693(7) 0.8424(6) 1.3364(4) 0.0425(17) Uani 1 1 d . . . C27 C 0.4964(7) 0.8765(7) 1.2653(4) 0.053(2) Uani 1 1 d . . . H27A H 0.4908 0.8138 1.2267 0.064 Uiso 1 1 calc R . . C28 C 0.5314(8) 1.0026(8) 1.2524(5) 0.069(2) Uani 1 1 d . . . H28A H 0.5501 1.0247 1.2053 0.083 Uiso 1 1 calc R . . C29 C 0.5389(9) 1.0961(8) 1.3090(5) 0.072(2) Uani 1 1 d . . . H29A H 0.5625 1.1811 1.3004 0.086 Uiso 1 1 calc R . . C30 C 0.5110(8) 1.0619(8) 1.3781(5) 0.066(2) Uani 1 1 d . . . H30A H 0.5147 1.1244 1.4163 0.080 Uiso 1 1 calc R . . C31 C 0.4780(7) 0.9379(7) 1.3920(4) 0.0526(19) Uani 1 1 d . . . H31A H 0.4611 0.9176 1.4396 0.063 Uiso 1 1 calc R . . C32 C 0.6008(6) 0.6866(6) 1.3953(3) 0.0432(17) Uani 1 1 d . . . H32A H 0.5881 0.6067 1.4150 0.052 Uiso 1 1 calc R . . H32B H 0.6557 0.6937 1.3554 0.052 Uiso 1 1 calc R . . N2 N 0.6698(5) 0.7937(5) 1.4539(3) 0.0456(15) Uani 1 1 d . . . C33 C 0.7707(7) 0.9046(7) 1.4280(4) 0.060(2) Uani 1 1 d . . . H33A H 0.7305 0.9320 1.3873 0.072 Uiso 1 1 calc R . . H33B H 0.8386 0.8798 1.4095 0.072 Uiso 1 1 calc R . . C34 C 0.8324(8) 1.0146(8) 1.4910(6) 0.083(3) Uani 1 1 d . . . H34A H 0.9010 1.0860 1.4734 0.099 Uiso 1 1 calc R . . H34B H 0.7654 1.0439 1.5060 0.099 Uiso 1 1 calc R . . O4 O 0.8878(6) 0.9794(6) 1.5534(4) 0.0864(19) Uani 1 1 d . . . C35 C 0.7940(9) 0.8696(9) 1.5769(5) 0.078(3) Uani 1 1 d . . . H35A H 0.7245 0.8914 1.5955 0.094 Uiso 1 1 calc R . . H35B H 0.8364 0.8447 1.6177 0.094 Uiso 1 1 calc R . . C36 C 0.7334(8) 0.7577(7) 1.5166(4) 0.063(2) Uani 1 1 d . . . H36A H 0.8011 0.7311 1.4997 0.075 Uiso 1 1 calc R . . H36B H 0.6682 0.6855 1.5356 0.075 Uiso 1 1 calc R . . C37 C 0.2375(11) 0.5157(13) 0.7677(6) 0.136(5) Uani 1 1 d . . . H37A H 0.2552 0.4769 0.8104 0.163 Uiso 1 1 calc R . . H37B H 0.3154 0.5414 0.7418 0.163 Uiso 1 1 calc R . . Cl3 Cl 0.2147(5) 0.6484(5) 0.7989(3) 0.236(3) Uani 1 1 d . . . Cl4 Cl 0.1033(4) 0.3979(5) 0.7073(2) 0.206(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0392(4) 0.0520(4) 0.0324(3) -0.0012(2) 0.0007(2) 0.0208(3) P1 0.0448(12) 0.0653(14) 0.0366(11) -0.0099(10) -0.0015(9) 0.0181(11) P2 0.0412(11) 0.0471(11) 0.0336(10) 0.0013(8) 0.0015(8) 0.0204(9) Cl1 0.0565(12) 0.0631(13) 0.0521(11) 0.0097(9) 0.0156(10) 0.0261(11) Cl2 0.0548(12) 0.0495(11) 0.0443(10) 0.0023(8) -0.0017(9) 0.0234(10) C1 0.058(5) 0.072(6) 0.056(5) -0.001(4) -0.001(4) 0.033(5) O1 0.098(5) 0.122(6) 0.080(4) 0.008(4) -0.015(4) 0.077(5) C2 0.043(5) 0.063(5) 0.043(4) -0.009(4) 0.003(4) 0.020(4) O2 0.057(4) 0.082(4) 0.076(4) -0.003(3) 0.029(3) 0.009(3) C3 0.054(5) 0.109(7) 0.035(4) -0.009(5) -0.002(4) 0.029(5) C4 0.080(7) 0.126(9) 0.048(5) 0.011(5) -0.006(5) 0.049(7) C5 0.114(10) 0.200(13) 0.057(6) 0.043(8) 0.006(7) 0.062(10) C6 0.078(9) 0.31(2) 0.056(7) 0.051(11) 0.007(7) 0.050(12) C7 0.059(7) 0.253(17) 0.046(6) 0.011(8) -0.007(6) 0.007(9) C8 0.061(6) 0.138(9) 0.047(5) -0.002(5) 0.002(5) 0.007(6) C9 0.063(6) 0.065(6) 0.043(5) -0.013(4) 0.002(4) 0.017(5) C10 0.089(8) 0.093(8) 0.049(5) -0.006(5) 0.015(5) 0.023(7) C11 0.141(12) 0.096(9) 0.073(7) 0.011(6) 0.012(8) 0.028(10) C12 0.144(13) 0.091(10) 0.056(7) 0.002(6) 0.018(8) -0.024(10) C13 0.079(8) 0.126(11) 0.098(9) 0.000(8) 0.034(7) 0.000(8) C14 0.062(6) 0.104(8) 0.062(6) -0.003(5) 0.007(5) 0.013(6) C15 0.085(6) 0.050(5) 0.046(4) -0.009(4) 0.028(4) 0.033(5) N1 0.060(4) 0.063(4) 0.049(4) -0.001(3) 0.017(3) 0.023(4) C16 0.086(7) 0.099(7) 0.062(6) -0.001(5) 0.021(5) 0.046(6) C17 0.119(9) 0.079(7) 0.075(6) 0.001(5) 0.033(6) 0.043(6) O3 0.114(5) 0.089(5) 0.065(4) -0.009(3) 0.028(4) 0.047(4) C18 0.143(10) 0.101(8) 0.064(6) 0.008(6) 0.044(6) 0.061(8) C19 0.117(8) 0.070(6) 0.067(6) -0.001(5) 0.034(6) 0.033(6) C20 0.048(5) 0.038(4) 0.037(4) -0.002(3) 0.006(3) 0.018(4) C21 0.052(5) 0.057(5) 0.045(4) 0.007(4) 0.009(4) 0.014(4) C22 0.065(6) 0.067(6) 0.049(5) 0.017(4) 0.016(4) 0.012(5) C23 0.058(6) 0.064(6) 0.057(5) 0.003(4) 0.026(5) 0.010(5) C24 0.038(5) 0.064(5) 0.083(6) 0.002(5) 0.019(5) 0.015(4) C25 0.052(5) 0.056(5) 0.051(4) 0.005(4) 0.003(4) 0.025(4) C26 0.049(4) 0.045(4) 0.039(4) 0.005(3) 0.002(3) 0.025(4) C27 0.059(5) 0.059(5) 0.044(4) 0.010(4) 0.005(4) 0.026(4) C28 0.080(7) 0.067(6) 0.070(6) 0.026(5) 0.012(5) 0.036(5) C29 0.078(7) 0.043(5) 0.094(7) 0.018(5) 0.009(6) 0.022(5) C30 0.076(6) 0.053(5) 0.073(6) 0.004(4) 0.013(5) 0.030(5) C31 0.062(5) 0.049(5) 0.051(5) 0.000(4) 0.010(4) 0.028(4) C32 0.044(4) 0.048(4) 0.043(4) 0.001(3) 0.002(3) 0.027(4) N2 0.040(4) 0.046(4) 0.045(3) -0.007(3) 0.002(3) 0.014(3) C33 0.043(5) 0.060(5) 0.074(6) 0.006(4) 0.000(4) 0.020(4) C34 0.048(6) 0.053(6) 0.135(9) -0.011(6) 0.013(6) 0.011(5) O4 0.050(4) 0.094(5) 0.087(5) -0.023(4) -0.006(4) 0.010(4) C35 0.050(5) 0.101(7) 0.063(6) -0.013(5) -0.006(5) 0.016(5) C36 0.048(5) 0.075(6) 0.047(4) 0.012(4) -0.008(4) 0.008(4) C37 0.077(8) 0.238(15) 0.135(10) 0.093(11) 0.035(8) 0.088(10) Cl3 0.261(6) 0.226(5) 0.359(7) 0.181(5) 0.192(5) 0.185(5) Cl4 0.105(3) 0.311(6) 0.173(4) 0.111(4) 0.019(3) 0.034(4) _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 C1 1.854(9) . ? Ru1 C2 1.894(8) . ? Ru1 P2 2.407(2) . ? Ru1 P1 2.411(2) . ? Ru1 Cl1 2.441(2) . ? Ru1 Cl2 2.4465(19) . ? P1 C9 1.811(9) . ? P1 C3 1.814(8) . ? P1 C15 1.919(7) . ? P2 C20 1.811(7) . ? P2 C26 1.830(7) . ? P2 C32 1.858(6) . ? C1 O1 1.149(8) . ? C2 O2 1.125(8) . ? C3 C4 1.381(11) . ? C3 C8 1.384(11) . ? C4 C5 1.386(11) . ? C5 C6 1.369(16) . ? C6 C7 1.364(18) . ? C7 C8 1.402(13) . ? C9 C14 1.372(11) . ? C9 C10 1.378(11) . ? C10 C11 1.390(14) . ? C11 C12 1.375(16) . ? C12 C13 1.358(16) . ? C13 C14 1.403(13) . ? C15 N1 1.472(8) . ? N1 C16 1.457(9) . ? N1 C19 1.461(9) . ? C16 C17 1.519(11) . ? C17 O3 1.400(9) . ? O3 C18 1.421(10) . ? C18 C19 1.481(11) . ? C20 C21 1.383(9) . ? C20 C25 1.392(9) . ? C21 C22 1.385(10) . ? C22 C23 1.367(11) . ? C23 C24 1.363(10) . ? C24 C25 1.384(10) . ? C26 C31 1.378(9) . ? C26 C27 1.403(9) . ? C27 C28 1.379(9) . ? C28 C29 1.378(10) . ? C29 C30 1.370(10) . ? C30 C31 1.364(9) . ? C32 N2 1.447(7) . ? N2 C36 1.464(8) . ? N2 C33 1.466(9) . ? C33 C34 1.509(10) . ? C34 O4 1.411(10) . ? O4 C35 1.403(9) . ? C35 C36 1.489(10) . ? C37 Cl3 1.677(13) . ? C37 Cl4 1.764(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 90.6(3) . . ? C1 Ru1 P2 90.1(2) . . ? C2 Ru1 P2 91.0(2) . . ? C1 Ru1 P1 96.0(2) . . ? C2 Ru1 P1 92.4(2) . . ? P2 Ru1 P1 173.05(7) . . ? C1 Ru1 Cl1 92.9(3) . . ? C2 Ru1 Cl1 176.5(2) . . ? P2 Ru1 Cl1 88.59(7) . . ? P1 Ru1 Cl1 87.70(7) . . ? C1 Ru1 Cl2 177.2(3) . . ? C2 Ru1 Cl2 86.6(2) . . ? P2 Ru1 Cl2 89.63(6) . . ? P1 Ru1 Cl2 84.49(7) . . ? Cl1 Ru1 Cl2 89.91(7) . . ? C9 P1 C3 105.3(4) . . ? C9 P1 C15 106.9(4) . . ? C3 P1 C15 104.4(4) . . ? C9 P1 Ru1 112.5(2) . . ? C3 P1 Ru1 116.2(3) . . ? C15 P1 Ru1 110.8(2) . . ? C20 P2 C26 103.3(3) . . ? C20 P2 C32 107.0(3) . . ? C26 P2 C32 104.7(3) . . ? C20 P2 Ru1 111.0(2) . . ? C26 P2 Ru1 118.6(2) . . ? C32 P2 Ru1 111.3(2) . . ? O1 C1 Ru1 176.8(7) . . ? O2 C2 Ru1 177.7(7) . . ? C4 C3 C8 118.1(8) . . ? C4 C3 P1 120.5(6) . . ? C8 C3 P1 121.1(8) . . ? C3 C4 C5 122.4(10) . . ? C6 C5 C4 118.7(12) . . ? C7 C6 C5 120.4(11) . . ? C6 C7 C8 120.8(12) . . ? C3 C8 C7 119.5(11) . . ? C14 C9 C10 118.9(9) . . ? C14 C9 P1 118.6(8) . . ? C10 C9 P1 122.3(8) . . ? C9 C10 C11 122.2(11) . . ? C12 C11 C10 117.5(13) . . ? C13 C12 C11 121.7(13) . . ? C12 C13 C14 119.9(13) . . ? C9 C14 C13 119.7(11) . . ? N1 C15 P1 107.2(5) . . ? C16 N1 C19 108.8(6) . . ? C16 N1 C15 112.6(6) . . ? C19 N1 C15 112.4(6) . . ? N1 C16 C17 110.5(7) . . ? O3 C17 C16 111.3(8) . . ? C17 O3 C18 109.3(7) . . ? O3 C18 C19 112.0(8) . . ? N1 C19 C18 110.9(7) . . ? C21 C20 C25 117.7(7) . . ? C21 C20 P2 123.7(6) . . ? C25 C20 P2 118.4(5) . . ? C20 C21 C22 121.0(8) . . ? C23 C22 C21 120.3(8) . . ? C24 C23 C22 119.7(8) . . ? C23 C24 C25 120.5(8) . . ? C24 C25 C20 120.8(7) . . ? C31 C26 C27 118.1(7) . . ? C31 C26 P2 121.2(5) . . ? C27 C26 P2 120.5(5) . . ? C28 C27 C26 120.2(7) . . ? C29 C28 C27 120.4(8) . . ? C30 C29 C28 119.1(8) . . ? C31 C30 C29 121.2(8) . . ? C30 C31 C26 120.9(7) . . ? N2 C32 P2 113.7(4) . . ? C32 N2 C36 112.8(5) . . ? C32 N2 C33 113.3(5) . . ? C36 N2 C33 108.0(6) . . ? N2 C33 C34 110.1(6) . . ? O4 C34 C33 112.5(7) . . ? C35 O4 C34 110.8(6) . . ? O4 C35 C36 113.4(7) . . ? N2 C36 C35 109.8(7) . . ? Cl3 C37 Cl4 114.9(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.834 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.088 #==================================================END data_compound62 _database_code_CSD 169887 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36.50 H41 Cl3 N2 O4 P2 Ru' _chemical_formula_weight 841.07 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 Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 20.928(2) _cell_length_b 20.928(2) _cell_length_c 17.798(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7795(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3448 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type Psi-Scans _exptl_absorpt_correction_T_min 0.917 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6595 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2914 _reflns_number_gt 1910 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+8.2071P] 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 2914 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1274 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 0.7500 0.32162(4) 0.0387(3) Uani 1 2 d S . . P1 P 0.44742(7) 0.64781(7) 0.33063(11) 0.0414(5) Uani 1 1 d . . . Cl1 Cl 0.42739(8) 0.78747(7) 0.41875(12) 0.0621(6) Uani 1 1 d . . . C1 C 0.5573(3) 0.7230(3) 0.2467(5) 0.0535(19) Uani 1 1 d . . . O1 O 0.5915(3) 0.7089(3) 0.2014(4) 0.091(2) Uani 1 1 d . . . C2 C 0.3749(3) 0.6436(3) 0.2727(5) 0.0487(19) Uani 1 1 d . . . C3 C 0.3772(4) 0.6225(4) 0.2006(5) 0.071(2) Uani 1 1 d . . . H3A H 0.4156 0.6072 0.1812 0.085 Uiso 1 1 calc R . . C4 C 0.3236(5) 0.6233(5) 0.1559(6) 0.103(3) Uani 1 1 d . . . H4A H 0.3259 0.6090 0.1065 0.123 Uiso 1 1 calc R . . C5 C 0.2672(5) 0.6449(5) 0.1838(8) 0.105(4) Uani 1 1 d . . . H5A H 0.2309 0.6447 0.1537 0.126 Uiso 1 1 calc R . . C6 C 0.2636(4) 0.6668(5) 0.2550(8) 0.096(3) Uani 1 1 d . . . H6A H 0.2249 0.6817 0.2739 0.115 Uiso 1 1 calc R . . C7 C 0.3180(3) 0.6669(4) 0.3001(5) 0.071(2) Uani 1 1 d . . . H7A H 0.3158 0.6828 0.3489 0.086 Uiso 1 1 calc R . . C8 C 0.4933(3) 0.5768(3) 0.3055(4) 0.0462(18) Uani 1 1 d . . . C9 C 0.4631(3) 0.5211(3) 0.2875(5) 0.067(2) Uani 1 1 d . . . H9A H 0.4188 0.5198 0.2846 0.080 Uiso 1 1 calc R . . C10 C 0.4988(4) 0.4664(3) 0.2734(5) 0.076(3) Uani 1 1 d . . . H10A H 0.4781 0.4283 0.2619 0.091 Uiso 1 1 calc R . . C11 C 0.5633(3) 0.4678(3) 0.2761(5) 0.073(2) Uani 1 1 d . . . H11A H 0.5867 0.4313 0.2648 0.087 Uiso 1 1 calc R . . C12 C 0.5938(3) 0.5225(3) 0.2953(5) 0.070(2) Uani 1 1 d . . . H12A H 0.6381 0.5231 0.2991 0.085 Uiso 1 1 calc R . . C13 C 0.5593(3) 0.5777(3) 0.3094(4) 0.058(2) Uani 1 1 d . . . H13A H 0.5805 0.6154 0.3215 0.070 Uiso 1 1 calc R . . C14 C 0.4211(3) 0.6311(3) 0.4268(4) 0.0548(19) Uani 1 1 d . . . H14A H 0.4582 0.6304 0.4594 0.066 Uiso 1 1 calc R . . H14B H 0.3936 0.6656 0.4434 0.066 Uiso 1 1 calc R . . N1 N 0.3865(2) 0.5705(2) 0.4352(3) 0.0572(16) Uani 1 1 d . . . C15 C 0.3259(3) 0.5778(3) 0.4741(5) 0.079(3) Uani 1 1 d . . . H15A H 0.3000 0.6094 0.4483 0.095 Uiso 1 1 calc R . . H15B H 0.3336 0.5930 0.5248 0.095 Uiso 1 1 calc R . . C16 C 0.2905(4) 0.5153(3) 0.4771(6) 0.092(3) Uani 1 1 d . . . H16A H 0.2504 0.5209 0.5036 0.110 Uiso 1 1 calc R . . H16B H 0.2811 0.5009 0.4265 0.110 Uiso 1 1 calc R . . O2 O 0.3286(3) 0.4685(3) 0.5148(4) 0.0939(19) Uani 1 1 d . . . C17 C 0.3886(4) 0.4600(3) 0.4781(6) 0.091(3) Uani 1 1 d . . . H17A H 0.3816 0.4437 0.4278 0.109 Uiso 1 1 calc R . . H17B H 0.4139 0.4290 0.5056 0.109 Uiso 1 1 calc R . . C18 C 0.4245(3) 0.5229(3) 0.4739(5) 0.074(2) Uani 1 1 d . . . H18A H 0.4343 0.5377 0.5242 0.088 Uiso 1 1 calc R . . H18B H 0.4645 0.5166 0.4473 0.088 Uiso 1 1 calc R . . C19 C 0.5000 0.2500 0.3750 0.227(19) Uani 1 4 d S . . Cl2 Cl 0.456(2) 0.3148(13) 0.3772(11) 0.111(6) Uani 0.25 1 d P . . Cl3 Cl 0.483(3) 0.1772(8) 0.3802(8) 0.126(7) Uani 0.25 1 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 0.0339(4) 0.0300(4) 0.0523(7) 0.000 0.000 0.0009(3) P1 0.0361(8) 0.0314(7) 0.0567(15) -0.0004(8) -0.0009(8) -0.0005(6) Cl1 0.0647(10) 0.0433(8) 0.0782(17) -0.0038(9) 0.0251(10) -0.0025(7) C1 0.057(4) 0.039(3) 0.065(6) -0.004(4) 0.006(4) -0.005(3) O1 0.098(4) 0.076(4) 0.099(6) -0.029(3) 0.047(4) -0.008(3) C2 0.043(3) 0.042(3) 0.061(7) 0.001(4) -0.006(3) -0.003(3) C3 0.061(5) 0.091(6) 0.061(7) 0.003(5) -0.008(4) -0.005(4) C4 0.087(7) 0.149(9) 0.072(8) 0.019(6) -0.026(6) -0.016(6) C5 0.077(7) 0.125(9) 0.114(12) 0.036(8) -0.048(7) -0.019(6) C6 0.043(4) 0.104(7) 0.141(11) 0.023(7) -0.017(6) 0.010(4) C7 0.059(4) 0.078(5) 0.076(7) 0.005(5) -0.008(4) 0.007(4) C8 0.044(3) 0.034(3) 0.060(5) -0.004(3) -0.002(3) 0.005(2) C9 0.050(4) 0.044(4) 0.106(7) -0.022(4) -0.002(4) -0.001(3) C10 0.077(5) 0.038(4) 0.112(8) -0.020(4) -0.014(5) 0.000(3) C11 0.065(5) 0.048(4) 0.105(8) -0.013(4) -0.004(5) 0.024(3) C12 0.050(4) 0.055(4) 0.107(7) -0.001(4) -0.007(4) 0.011(3) C13 0.049(4) 0.040(3) 0.086(6) -0.008(4) -0.004(4) 0.005(3) C14 0.059(4) 0.046(3) 0.060(6) -0.002(4) 0.005(4) -0.004(3) N1 0.054(3) 0.036(3) 0.082(5) 0.007(3) 0.008(3) -0.001(2) C15 0.063(5) 0.053(4) 0.121(8) 0.009(5) 0.023(5) -0.004(3) C16 0.071(5) 0.064(5) 0.140(9) 0.025(6) 0.002(6) -0.017(4) O2 0.104(5) 0.068(4) 0.109(6) 0.023(3) -0.001(4) -0.028(3) C17 0.084(6) 0.052(4) 0.136(9) 0.017(5) -0.001(6) 0.004(4) C18 0.070(5) 0.055(4) 0.095(7) 0.014(4) -0.003(5) -0.002(4) C19 0.124(13) 0.124(13) 0.43(6) 0.000 0.000 0.000 Cl2 0.195(19) 0.096(10) 0.042(9) 0.016(7) 0.026(10) 0.076(9) Cl3 0.29(2) 0.066(7) 0.018(8) 0.004(5) -0.012(13) -0.043(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 C1 1.880(9) . ? Ru1 C1 1.880(9) 6_564 ? Ru1 P1 2.4104(14) 6_564 ? Ru1 P1 2.4104(14) . ? Ru1 Cl1 2.4316(19) 6_564 ? Ru1 Cl1 2.4316(19) . ? P1 C8 1.825(5) . ? P1 C14 1.832(7) . ? P1 C2 1.836(7) . ? C1 O1 1.118(8) . ? C2 C3 1.358(10) . ? C2 C7 1.377(9) . ? C3 C4 1.376(11) . ? C4 C5 1.356(14) . ? C5 C6 1.349(13) . ? C6 C7 1.393(11) . ? C8 C9 1.364(8) . ? C8 C13 1.382(8) . ? C9 C10 1.390(9) . ? C10 C11 1.350(9) . ? C11 C12 1.356(10) . ? C12 C13 1.385(8) . ? C14 N1 1.467(7) . ? N1 C18 1.449(8) . ? N1 C15 1.452(8) . ? C15 C16 1.504(9) . ? C16 O2 1.429(9) . ? O2 C17 1.426(10) . ? C17 C18 1.517(9) . ? C19 Cl3 1.569(11) 6_554 ? C19 Cl3 1.569(11) 16_656 ? C19 Cl3 1.569(11) . ? C19 Cl3 1.569(11) 11_666 ? C19 Cl2 1.643(11) 16_656 ? C19 Cl2 1.643(11) 11_666 ? C19 Cl2 1.643(11) . ? C19 Cl2 1.643(11) 6_554 ? Cl2 Cl3 1.16(2) 11_666 ? Cl2 Cl3 1.30(2) 6_554 ? Cl2 Cl2 2.325(15) 16_656 ? Cl2 Cl2 2.325(15) 11_666 ? Cl3 Cl2 1.16(2) 16_656 ? Cl3 Cl2 1.304(19) 6_554 ? Cl3 Cl3 2.223(16) 16_656 ? Cl3 Cl3 2.223(16) 11_666 ? 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 C1 Ru1 C1 89.7(5) . 6_564 ? C1 Ru1 P1 91.32(18) . 6_564 ? C1 Ru1 P1 94.09(18) 6_564 6_564 ? C1 Ru1 P1 94.09(18) . . ? C1 Ru1 P1 91.32(18) 6_564 . ? P1 Ru1 P1 172.37(10) 6_564 . ? C1 Ru1 Cl1 90.5(2) . 6_564 ? C1 Ru1 Cl1 178.56(19) 6_564 6_564 ? P1 Ru1 Cl1 87.34(5) 6_564 6_564 ? P1 Ru1 Cl1 87.24(5) . 6_564 ? C1 Ru1 Cl1 178.56(19) . . ? C1 Ru1 Cl1 90.5(2) 6_564 . ? P1 Ru1 Cl1 87.24(5) 6_564 . ? P1 Ru1 Cl1 87.34(5) . . ? Cl1 Ru1 Cl1 89.37(10) 6_564 . ? C8 P1 C14 103.4(3) . . ? C8 P1 C2 105.0(3) . . ? C14 P1 C2 105.4(3) . . ? C8 P1 Ru1 117.8(2) . . ? C14 P1 Ru1 111.7(2) . . ? C2 P1 Ru1 112.5(2) . . ? O1 C1 Ru1 177.8(6) . . ? C3 C2 C7 118.7(7) . . ? C3 C2 P1 121.1(5) . . ? C7 C2 P1 119.9(6) . . ? C2 C3 C4 120.8(8) . . ? C5 C4 C3 120.1(10) . . ? C6 C5 C4 120.4(9) . . ? C5 C6 C7 119.7(9) . . ? C2 C7 C6 120.2(9) . . ? C9 C8 C13 119.1(5) . . ? C9 C8 P1 120.6(5) . . ? C13 C8 P1 120.1(4) . . ? C8 C9 C10 119.8(6) . . ? C11 C10 C9 120.8(6) . . ? C10 C11 C12 119.9(6) . . ? C11 C12 C13 120.3(6) . . ? C8 C13 C12 120.0(6) . . ? N1 C14 P1 114.1(5) . . ? C18 N1 C15 109.0(6) . . ? C18 N1 C14 111.8(5) . . ? C15 N1 C14 112.8(5) . . ? N1 C15 C16 110.8(6) . . ? O2 C16 C15 109.7(7) . . ? C17 O2 C16 111.2(7) . . ? O2 C17 C18 110.5(6) . . ? N1 C18 C17 110.3(6) . . ? Cl3 C19 Cl3 90.20(6) 6_554 16_656 ? Cl3 C19 Cl3 173.3(10) 6_554 . ? Cl3 C19 Cl3 90.20(6) 16_656 . ? Cl3 C19 Cl3 90.20(6) 6_554 11_666 ? Cl3 C19 Cl3 173.3(10) 16_656 11_666 ? Cl3 C19 Cl3 90.20(6) . 11_666 ? Cl3 C19 Cl2 137.8(8) 6_554 16_656 ? Cl3 C19 Cl2 132.0(8) 16_656 16_656 ? Cl3 C19 Cl2 42.4(7) . 16_656 ? Cl3 C19 Cl2 47.8(8) 11_666 16_656 ? Cl3 C19 Cl2 42.4(7) 6_554 11_666 ? Cl3 C19 Cl2 47.8(8) 16_656 11_666 ? Cl3 C19 Cl2 137.8(8) . 11_666 ? Cl3 C19 Cl2 132.0(8) 11_666 11_666 ? Cl2 C19 Cl2 177.3(14) 16_656 11_666 ? Cl3 C19 Cl2 47.8(8) 6_554 . ? Cl3 C19 Cl2 137.8(8) 16_656 . ? Cl3 C19 Cl2 132.0(8) . . ? Cl3 C19 Cl2 42.4(7) 11_666 . ? Cl2 C19 Cl2 90.03(4) 16_656 . ? Cl2 C19 Cl2 90.03(3) 11_666 . ? Cl3 C19 Cl2 132.0(8) 6_554 6_554 ? Cl3 C19 Cl2 42.4(7) 16_656 6_554 ? Cl3 C19 Cl2 47.8(8) . 6_554 ? Cl3 C19 Cl2 137.8(8) 11_666 6_554 ? Cl2 C19 Cl2 90.03(3) 16_656 6_554 ? Cl2 C19 Cl2 90.03(3) 11_666 6_554 ? Cl2 C19 Cl2 177.3(14) . 6_554 ? Cl3 Cl2 Cl3 128.4(15) 11_666 6_554 ? Cl3 Cl2 C19 65.4(9) 11_666 . ? Cl3 Cl2 C19 63.1(7) 6_554 . ? Cl3 Cl2 Cl2 20.8(10) 11_666 16_656 ? Cl3 Cl2 Cl2 108.1(7) 6_554 16_656 ? C19 Cl2 Cl2 44.984(18) . 16_656 ? Cl3 Cl2 Cl2 110.0(9) 11_666 11_666 ? Cl3 Cl2 Cl2 18.5(7) 6_554 11_666 ? C19 Cl2 Cl2 44.984(17) . 11_666 ? Cl2 Cl2 Cl2 89.94(6) 16_656 11_666 ? Cl2 Cl3 Cl2 140.7(16) 16_656 6_554 ? Cl2 Cl3 C19 72.2(9) 16_656 . ? Cl2 Cl3 C19 69.1(9) 6_554 . ? Cl2 Cl3 Cl3 116.6(9) 16_656 16_656 ? Cl2 Cl3 Cl3 24.2(9) 6_554 16_656 ? C19 Cl3 Cl3 44.90(3) . 16_656 ? Cl2 Cl3 Cl3 27.4(9) 16_656 11_666 ? Cl2 Cl3 Cl3 113.8(9) 6_554 11_666 ? C19 Cl3 Cl3 44.90(3) . 11_666 ? Cl3 Cl3 Cl3 89.61(12) 16_656 11_666 ? _diffrn_measured_fraction_theta_max 0.760 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.760 _refine_diff_density_max 0.550 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.084 #==========================================END