# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1364 data_global _publ_requested_journal ChemComm _publ_contact_author ; Sanshiro Komiya Department of Applied Chemistry, Faculty of technology, Tokyo University of Agriculture and Technology, 2-24-16 Nakacho, Koganei, Tokyo 184-8588, Japan ; _publ_contact_author_email komiya@cc.tuat.ac.jp _publ_section_title ; Regioselective 1,2-insertion of Ru into the C-S bond in 3-substituted thiophenes Paper NO. 9/05748J ; data_1 #---------------------------------------------- _audit_creation_date 'Tue Jul 6 09:01:04 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #--------------------------------------------- _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #--------------------------------------------- _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 625.71 _chemical_formula_analytical ? _chemical_formula_sum 'C25 H52 O P4 S Ru ' _chemical_formula_moiety 'C25 H52 O P4 S Ru ' _chemical_formula_structural ? _chemical_melting_point ? #---------------------------------------------- _cell_length_a 10.638(5) _cell_length_b 15.753(5) _cell_length_c 18.502(4) _cell_angle_alpha 90 _cell_angle_beta 99.22(2) _cell_angle_gamma 90 _cell_volume 3060(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.5 #--------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_meas 'not measured' _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.895 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #----------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.46 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -1 2 2 -1 0 2 0 0 _diffrn_reflns_number 7391 _reflns_number_total 7017 _reflns_number_gt 3792 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_av_sigmaI/netI 0.105 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.06572 _diffrn_orient_matrix_UB_12 0.04140 _diffrn_orient_matrix_UB_13 -0.01090 _diffrn_orient_matrix_UB_21 -0.04879 _diffrn_orient_matrix_UB_22 0.04739 _diffrn_orient_matrix_UB_23 0.01845 _diffrn_orient_matrix_UB_31 0.04867 _diffrn_orient_matrix_UB_32 -0.00839 _diffrn_orient_matrix_UB_33 0.05039 #-------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ru' 'Ru' -1.259 0.836 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------ 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru(1) Ru 0.10114(4) 0.20957(3) 0.27812(2) 0.0395(1) Uani 1.00 d . . . S(1) S 0.1605(2) 0.3444(1) 0.22987(9) 0.0609(5) Uani 1.00 d . . . P(1) P 0.0385(2) 0.2828(1) 0.37648(8) 0.0531(5) Uani 1.00 d . . . P(2) P 0.3225(2) 0.1948(1) 0.32887(9) 0.0554(5) Uani 1.00 d . . . P(3) P 0.0424(2) 0.0899(1) 0.33733(8) 0.0508(5) Uani 1.00 d . . . P(4) P 0.1628(2) 0.1439(1) 0.17522(8) 0.0550(5) Uani 1.00 d . . . O(1) O -0.3390(7) 0.3091(6) 0.0989(4) 0.158(3) Uani 1.00 d . . . C(1) C -0.0797(6) 0.2220(4) 0.2212(3) 0.056(2) Uani 1.00 d . . . C(2) C -0.1362(6) 0.2796(5) 0.1706(3) 0.068(2) Uani 1.00 d . . . C(3) C -0.0774(9) 0.3530(6) 0.1434(4) 0.082(3) Uani 1.00 d . . . C(4) C 0.0395(9) 0.3822(5) 0.1654(4) 0.075(3) Uani 1.00 d . . . C(5) C -0.2702(8) 0.2649(6) 0.1417(5) 0.099(3) Uani 1.00 d . . . C(6) C -0.076(1) 0.4409(7) 0.3311(5) 0.109(4) Uani 1.00 d . . . C(7) C -0.0974(7) 0.3562(6) 0.3610(4) 0.078(3) Uani 1.00 d . . . C(8) C 0.1594(7) 0.3425(5) 0.4369(4) 0.070(2) Uani 1.00 d . . . C(9) C 0.1147(9) 0.3916(6) 0.5006(5) 0.099(3) Uani 1.00 d . . . C(10) C -0.0244(7) 0.2064(5) 0.4375(4) 0.073(2) Uani 1.00 d . . . C(11) C 0.0366(7) 0.1188(5) 0.4334(3) 0.065(2) Uani 1.00 d . . . C(12) C -0.1147(9) 0.0405(7) 0.3096(5) 0.105(4) Uani 1.00 d . . . C(13) C -0.217(1) 0.051(1) 0.3380(7) 0.236(8) Uani 1.00 d . . . C(14) C 0.1377(8) -0.0655(5) 0.4103(4) 0.089(3) Uani 1.00 d . . . C(15) C 0.1395(9) -0.0067(5) 0.3453(5) 0.094(3) Uani 1.00 d . . . C(16) C 0.5126(8) 0.1170(6) 0.4388(4) 0.088(3) Uani 1.00 d . . . C(17) C 0.3789(8) 0.1442(7) 0.4201(4) 0.100(3) Uani 1.00 d . . . C(18) C 0.4238(7) 0.2896(5) 0.3356(5) 0.093(3) Uani 1.00 d . . . C(19) C 0.5434(9) 0.2945(7) 0.3094(6) 0.124(4) Uani 1.00 d . . . C(20) C 0.3950(7) 0.1232(5) 0.2680(4) 0.076(3) Uani 1.00 d . . . C(21) C 0.3384(8) 0.1380(7) 0.1901(4) 0.104(3) Uani 1.00 d . . . C(22) C 0.1335(8) 0.2018(5) 0.0876(3) 0.075(2) Uani 1.00 d . . . C(23) C 0.1977(10) 0.1667(6) 0.0261(4) 0.106(3) Uani 1.00 d . . . C(24) C -0.023(1) 0.0306(7) 0.1118(6) 0.135(5) Uani 1.00 d . . . C(25) C 0.114(1) 0.0377(5) 0.1467(4) 0.094(3) Uani 1.00 d . . . H H 0.046(7) 0.350(5) 0.527(4) 0.097(6) Uiso 1.00 d . . . H(1) H -0.1289 0.1729 0.2230 0.0768 Uiso 1.00 calc . . . H(2) H 0.000(8) 0.465(5) 0.363(4) 0.104(4) Uiso 1.00 calc . . . H(3) H -0.1296 0.3873 0.1068 0.0841 Uiso 1.00 calc . . . H(4) H 0.0631 0.4319 0.1386 0.0863 Uiso 1.00 calc . . . H(5) H -0.3084 0.2085 0.1602 0.1191 Uiso 1.00 calc . . . H(6) H -0.0937 0.4335 0.2781 0.1290 Uiso 1.00 calc . . . H(7) H -0.1458 0.4761 0.3429 0.1290 Uiso 1.00 calc . . . H(8) H -0.1659 0.3273 0.3291 0.0863 Uiso 1.00 calc . . . H(9) H -0.1266 0.3644 0.4071 0.0863 Uiso 1.00 calc . . . H(10) H 0.2225 0.3020 0.4595 0.0841 Uiso 1.00 calc . . . H(11) H 0.2019 0.3788 0.4065 0.0841 Uiso 1.00 calc . . . H(12) H 0.1961 0.4114 0.5325 0.1303 Uiso 1.00 calc . . . H(13) H 0.0833 0.4478 0.4777 0.1303 Uiso 1.00 calc . . . H(14) H -0.0056 0.2267 0.4874 0.0825 Uiso 1.00 calc . . . H(15) H -0.1135 0.2011 0.4244 0.0825 Uiso 1.00 calc . . . H(16) H -0.0105 0.0766 0.4556 0.0713 Uiso 1.00 calc . . . H(17) H 0.1223 0.1190 0.4610 0.0713 Uiso 1.00 calc . . . H(18) H -0.1321 0.0395 0.2570 0.1197 Uiso 1.00 calc . . . H(19) H -0.1006 -0.0228 0.3223 0.1197 Uiso 1.00 calc . . . H(20) H -0.2350 0.1206 0.3235 0.1791 Uiso 1.00 calc . . . H(21) H -0.2908 0.0294 0.3158 0.1791 Uiso 1.00 calc . . . H(22) H -0.2052 0.0569 0.3879 0.1791 Uiso 1.00 calc . . . H(23) H 0.0537 -0.0858 0.4127 0.0972 Uiso 1.00 calc . . . H(24) H 0.1925 -0.1136 0.4093 0.0972 Uiso 1.00 calc . . . H(25) H 0.1669 -0.0355 0.4559 0.0972 Uiso 1.00 calc . . . H(26) H 0.1122 -0.0400 0.3018 0.1025 Uiso 1.00 calc . . . H(27) H 0.2258 0.0100 0.3448 0.1025 Uiso 1.00 calc . . . H(28) H 0.5296 0.0909 0.4861 0.1015 Uiso 1.00 calc . . . H(29) H 0.5323 0.0761 0.4035 0.1015 Uiso 1.00 calc . . . H(30) H 0.5674 0.1644 0.4381 0.1015 Uiso 1.00 calc . . . H(31) H 0.3623 0.1817 0.4581 0.1082 Uiso 1.00 calc . . . H(32) H 0.3271 0.0933 0.4239 0.1082 Uiso 1.00 calc . . . H(33) H 0.3702 0.3361 0.3122 0.1039 Uiso 1.00 calc . . . H(34) H 0.4406 0.3053 0.3876 0.1039 Uiso 1.00 calc . . . H(35) H 0.6013 0.2514 0.3310 0.1377 Uiso 1.00 calc . . . H(36) H 0.5317 0.2854 0.2565 0.1377 Uiso 1.00 calc . . . H(37) H 0.5859 0.3484 0.3181 0.1377 Uiso 1.00 calc . . . H(38) H 0.4865 0.1289 0.2776 0.0895 Uiso 1.00 calc . . . H(39) H 0.3785 0.0637 0.2813 0.0895 Uiso 1.00 calc . . . H(40) H 0.3666 0.0973 0.1589 0.1042 Uiso 1.00 calc . . . H(41) H 0.3718 0.1937 0.1763 0.1042 Uiso 1.00 calc . . . H(42) H 0.0428 0.2026 0.0705 0.0820 Uiso 1.00 calc . . . H(43) H 0.1597 0.2601 0.0964 0.0820 Uiso 1.00 calc . . . H(44) H 0.1729 0.1089 0.0157 0.1111 Uiso 1.00 calc . . . H(45) H 0.1811 0.1990 -0.0171 0.1111 Uiso 1.00 calc . . . H(46) H 0.2902 0.1659 0.0420 0.1111 Uiso 1.00 calc . . . H(47) H -0.0747 0.0492 0.1470 0.1340 Uiso 1.00 calc . . . H(48) H -0.0381 0.0673 0.0706 0.1340 Uiso 1.00 calc . . . H(49) H -0.0452 -0.0255 0.0977 0.1340 Uiso 1.00 calc . . . H(50) H 0.1664 0.0166 0.1115 0.1010 Uiso 1.00 calc . . . H(51) H 0.1297 -0.0011 0.1879 0.1010 Uiso 1.00 calc . . . 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) 0.0411(2) 0.0457(2) 0.0325(2) -0.0018(2) 0.0085(2) -0.0022(2) S(1) 0.075(1) 0.0482(9) 0.063(1) -0.0029(8) 0.0203(9) 0.0055(8) P(1) 0.0526(9) 0.066(1) 0.0409(8) 0.0073(9) 0.0082(7) -0.0095(8) P(2) 0.0447(9) 0.063(1) 0.0573(9) 0.0000(8) 0.0052(7) -0.0036(9) P(3) 0.061(1) 0.0529(10) 0.0425(8) -0.0095(8) 0.0190(7) -0.0017(7) P(4) 0.071(1) 0.059(1) 0.0365(8) 0.0123(9) 0.0114(7) -0.0021(8) O(1) 0.122(6) 0.199(9) 0.123(5) 0.054(6) -0.071(5) -0.012(6) C(1) 0.051(4) 0.063(4) 0.055(3) -0.003(3) 0.007(3) -0.012(3) C(2) 0.065(4) 0.090(6) 0.044(3) 0.024(4) -0.005(3) -0.012(4) C(3) 0.110(7) 0.091(6) 0.039(4) 0.037(5) -0.006(4) 0.011(4) C(4) 0.114(7) 0.056(4) 0.056(4) 0.020(5) 0.020(4) 0.015(4) C(5) 0.079(6) 0.129(8) 0.076(5) 0.026(5) -0.027(4) -0.021(5) C(6) 0.146(10) 0.112(8) 0.068(6) 0.052(7) 0.017(6) 0.004(6) C(7) 0.074(5) 0.093(6) 0.067(5) 0.021(5) 0.011(4) -0.012(4) C(8) 0.080(5) 0.065(5) 0.061(4) 0.000(4) 0.002(4) -0.017(4) C(9) 0.118(8) 0.096(7) 0.073(5) 0.010(6) -0.008(5) -0.044(5) C(10) 0.084(5) 0.086(5) 0.055(4) -0.004(5) 0.033(3) -0.013(4) C(11) 0.077(5) 0.076(5) 0.047(4) -0.010(4) 0.026(3) -0.001(3) C(12) 0.101(7) 0.139(9) 0.077(6) -0.063(6) 0.016(5) 0.004(6) C(13) 0.096(9) 0.48(3) 0.14(1) -0.13(1) 0.049(8) -0.10(1) C(14) 0.107(7) 0.084(6) 0.087(6) 0.025(5) 0.048(5) 0.033(5) C(15) 0.129(8) 0.066(5) 0.103(6) 0.018(5) 0.066(6) 0.027(5) C(16) 0.083(6) 0.103(7) 0.071(5) 0.015(5) -0.009(4) 0.005(5) C(17) 0.077(6) 0.146(9) 0.075(5) 0.028(6) 0.003(4) 0.019(6) C(18) 0.051(4) 0.079(5) 0.144(8) -0.008(4) 0.001(5) -0.008(6) C(19) 0.097(7) 0.117(8) 0.17(1) -0.028(6) 0.058(7) -0.022(8) C(20) 0.063(5) 0.090(6) 0.078(5) 0.008(4) 0.021(4) -0.013(5) C(21) 0.096(6) 0.166(9) 0.054(4) 0.056(6) 0.028(4) 0.003(5) C(22) 0.116(6) 0.069(5) 0.044(3) 0.011(5) 0.030(4) 0.003(4) C(23) 0.147(9) 0.131(8) 0.052(4) 0.031(7) 0.047(5) 0.007(5) C(24) 0.18(1) 0.132(9) 0.097(7) -0.073(9) 0.033(8) -0.039(7) C(25) 0.170(10) 0.063(5) 0.050(4) -0.001(6) 0.019(5) -0.002(4) #----------------------------------------- _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3792 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0449 _refine_ls_wR_factor_gt 0.0449 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_shift/su_max 0.3600 _refine_ls_shift/su_mean 0.0160 _refine_diff_density_min -0.39 _refine_diff_density_max 0.64 #------------------------------------------------- _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) S(1) 2.427(2) 1_555 1_555 yes Ru(1) P(1) 2.340(2) 1_555 1_555 yes Ru(1) P(2) 2.403(2) 1_555 1_555 yes Ru(1) P(3) 2.316(2) 1_555 1_555 yes Ru(1) P(4) 2.351(2) 1_555 1_555 yes Ru(1) C(1) 2.049(6) 1_555 1_555 yes S(1) C(4) 1.715(8) 1_555 1_555 yes P(1) C(7) 1.837(8) 1_555 1_555 yes P(1) C(8) 1.824(7) 1_555 1_555 yes P(1) C(10) 1.847(7) 1_555 1_555 yes P(2) C(17) 1.876(8) 1_555 1_555 yes P(2) C(18) 1.834(8) 1_555 1_555 yes P(2) C(20) 1.848(7) 1_555 1_555 yes P(3) C(11) 1.845(6) 1_555 1_555 yes P(3) C(12) 1.840(8) 1_555 1_555 yes P(3) C(15) 1.832(8) 1_555 1_555 yes P(4) C(21) 1.846(9) 1_555 1_555 yes P(4) C(22) 1.843(7) 1_555 1_555 yes P(4) C(25) 1.805(9) 1_555 1_555 yes O(1) C(5) 1.210(10) 1_555 1_555 yes C(1) C(2) 1.371(9) 1_555 1_555 yes C(1) H(1) 0.938 1_555 1_555 no C(2) C(3) 1.44(1) 1_555 1_555 yes C(2) C(5) 1.46(1) 1_555 1_555 yes C(3) C(4) 1.33(1) 1_555 1_555 yes C(3) H(3) 0.968 1_555 1_555 no C(4) H(4) 0.980 1_555 1_555 no C(5) H(5) 1.056 1_555 1_555 no C(6) C(7) 1.48(1) 1_555 1_555 yes C(6) H(2) 0.99(8) 1_555 1_555 no C(6) H(6) 0.975 1_555 1_555 no C(6) H(7) 0.982 1_555 1_555 no C(7) H(8) 0.974 1_555 1_555 no C(7) H(9) 0.962 1_555 1_555 no C(8) C(9) 1.548(10) 1_555 1_555 yes C(8) H(10) 0.971 1_555 1_555 no C(8) H(11) 0.964 1_555 1_555 no C(9) H 1.14(7) 1_555 1_555 yes C(9) H(12) 1.016 1_555 1_555 no C(9) H(13) 1.015 1_555 1_555 no C(10) C(11) 1.53(1) 1_555 1_555 yes C(10) H(14) 0.967 1_555 1_555 no C(10) H(15) 0.943 1_555 1_555 no C(11) H(16) 0.963 1_555 1_555 no C(11) H(17) 0.971 1_555 1_555 no C(12) C(13) 1.29(1) 1_555 1_555 yes C(12) H(18) 0.961 1_555 1_555 no C(12) H(19) 1.030 1_555 1_555 no C(13) H(20) 1.140 1_555 1_555 no C(13) H(21) 0.892 1_555 1_555 no C(13) H(22) 0.917 1_555 1_555 no C(14) C(15) 1.521(10) 1_555 1_555 yes C(14) H(23) 0.957 1_555 1_555 no C(14) H(24) 0.958 1_555 1_555 no C(14) H(25) 0.973 1_555 1_555 no C(15) H(26) 0.966 1_555 1_555 no C(15) H(27) 0.957 1_555 1_555 no C(16) C(17) 1.47(1) 1_555 1_555 yes C(16) H(28) 0.958 1_555 1_555 no C(16) H(29) 0.964 1_555 1_555 no C(16) H(30) 0.948 1_555 1_555 no C(17) H(31) 0.956 1_555 1_555 no C(17) H(32) 0.982 1_555 1_555 no C(18) C(19) 1.44(1) 1_555 1_555 yes C(18) H(33) 0.984 1_555 1_555 no C(18) H(34) 0.980 1_555 1_555 no C(19) H(35) 0.959 1_555 1_555 no C(19) H(36) 0.977 1_555 1_555 no C(19) H(37) 0.964 1_555 1_555 no C(20) C(21) 1.49(1) 1_555 1_555 yes C(20) H(38) 0.965 1_555 1_555 no C(20) H(39) 0.993 1_555 1_555 no C(21) H(40) 0.944 1_555 1_555 no C(21) H(41) 0.995 1_555 1_555 no C(22) C(23) 1.521(9) 1_555 1_555 yes C(22) H(42) 0.966 1_555 1_555 no C(22) H(43) 0.966 1_555 1_555 no C(23) H(44) 0.959 1_555 1_555 no C(23) H(45) 0.940 1_555 1_555 no C(23) H(46) 0.982 1_555 1_555 no C(24) C(25) 1.51(1) 1_555 1_555 yes C(24) H(47) 0.959 1_555 1_555 no C(24) H(48) 0.950 1_555 1_555 no C(24) H(49) 0.940 1_555 1_555 no C(25) H(50) 0.979 1_555 1_555 no C(25) H(51) 0.971 1_555 1_555 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 S(1) Ru(1) P(1) 88.73(6) 1_555 1_555 1_555 yes S(1) Ru(1) P(2) 86.09(7) 1_555 1_555 1_555 yes S(1) Ru(1) P(3) 172.92(6) 1_555 1_555 1_555 yes S(1) Ru(1) P(4) 87.95(6) 1_555 1_555 1_555 yes S(1) Ru(1) C(1) 90.3(2) 1_555 1_555 1_555 yes P(1) Ru(1) P(2) 97.32(6) 1_555 1_555 1_555 yes P(1) Ru(1) P(3) 84.33(6) 1_555 1_555 1_555 yes P(1) Ru(1) P(4) 176.46(7) 1_555 1_555 1_555 yes P(1) Ru(1) C(1) 89.5(2) 1_555 1_555 1_555 yes P(2) Ru(1) P(3) 93.35(6) 1_555 1_555 1_555 yes P(2) Ru(1) P(4) 83.71(6) 1_555 1_555 1_555 yes P(2) Ru(1) C(1) 172.2(2) 1_555 1_555 1_555 yes P(3) Ru(1) P(4) 99.01(6) 1_555 1_555 1_555 yes P(3) Ru(1) C(1) 91.1(2) 1_555 1_555 1_555 yes P(4) Ru(1) C(1) 89.3(2) 1_555 1_555 1_555 yes Ru(1) S(1) C(4) 110.4(3) 1_555 1_555 1_555 yes Ru(1) P(1) C(7) 120.3(2) 1_555 1_555 1_555 yes Ru(1) P(1) C(8) 118.0(2) 1_555 1_555 1_555 yes Ru(1) P(1) C(10) 109.3(2) 1_555 1_555 1_555 yes C(7) P(1) C(8) 103.3(3) 1_555 1_555 1_555 yes C(7) P(1) C(10) 98.7(4) 1_555 1_555 1_555 yes C(8) P(1) C(10) 104.5(3) 1_555 1_555 1_555 yes Ru(1) P(2) C(17) 123.0(3) 1_555 1_555 1_555 yes Ru(1) P(2) C(18) 118.4(3) 1_555 1_555 1_555 yes Ru(1) P(2) C(20) 107.4(2) 1_555 1_555 1_555 yes C(17) P(2) C(18) 100.7(4) 1_555 1_555 1_555 yes C(17) P(2) C(20) 100.6(4) 1_555 1_555 1_555 yes C(18) P(2) C(20) 104.0(4) 1_555 1_555 1_555 yes Ru(1) P(3) C(11) 108.0(2) 1_555 1_555 1_555 yes Ru(1) P(3) C(12) 121.0(3) 1_555 1_555 1_555 yes Ru(1) P(3) C(15) 121.5(3) 1_555 1_555 1_555 yes C(11) P(3) C(12) 101.8(4) 1_555 1_555 1_555 yes C(11) P(3) C(15) 103.4(4) 1_555 1_555 1_555 yes C(12) P(3) C(15) 98.4(5) 1_555 1_555 1_555 yes Ru(1) P(4) C(21) 108.0(3) 1_555 1_555 1_555 yes Ru(1) P(4) C(22) 117.7(2) 1_555 1_555 1_555 yes Ru(1) P(4) C(25) 122.7(3) 1_555 1_555 1_555 yes C(21) P(4) C(22) 100.4(4) 1_555 1_555 1_555 yes C(21) P(4) C(25) 103.5(5) 1_555 1_555 1_555 yes C(22) P(4) C(25) 101.6(3) 1_555 1_555 1_555 yes Ru(1) C(1) C(2) 133.4(5) 1_555 1_555 1_555 yes Ru(1) C(1) H(1) 112.7(5) 1_555 1_555 1_555 no C(2) C(1) H(1) 112.5(6) 1_555 1_555 1_555 no C(1) C(2) C(3) 126.9(7) 1_555 1_555 1_555 yes C(1) C(2) C(5) 116.2(8) 1_555 1_555 1_555 yes C(3) C(2) C(5) 116.9(7) 1_555 1_555 1_555 yes C(2) C(3) C(4) 127.4(7) 1_555 1_555 1_555 yes C(2) C(3) H(3) 117.3(9) 1_555 1_555 1_555 no C(4) C(3) H(3) 115.2(10) 1_555 1_555 1_555 no S(1) C(4) C(3) 130.9(6) 1_555 1_555 1_555 yes S(1) C(4) H(4) 113.9(7) 1_555 1_555 1_555 no C(3) C(4) H(4) 115.1(8) 1_555 1_555 1_555 no O(1) C(5) C(2) 127(1) 1_555 1_555 1_555 yes O(1) C(5) H(5) 118.2(9) 1_555 1_555 1_555 no C(2) C(5) H(5) 114.8(8) 1_555 1_555 1_555 no C(7) C(6) H(2) 105(5) 1_555 1_555 1_555 no C(7) C(6) H(6) 104.6(10) 1_555 1_555 1_555 no C(7) C(6) H(7) 104.8(10) 1_555 1_555 1_555 no H(2) C(6) H(6) 130(5) 1_555 1_555 1_555 no H(2) C(6) H(7) 103(5) 1_555 1_555 1_555 no H(6) C(6) H(7) 104.9(9) 1_555 1_555 1_555 no P(1) C(7) C(6) 117.4(6) 1_555 1_555 1_555 yes P(1) C(7) H(8) 107.1(6) 1_555 1_555 1_555 no P(1) C(7) H(9) 107.8(6) 1_555 1_555 1_555 no C(6) C(7) H(8) 109.9(8) 1_555 1_555 1_555 no C(6) C(7) H(9) 107.6(7) 1_555 1_555 1_555 no H(8) C(7) H(9) 106.4(8) 1_555 1_555 1_555 no P(1) C(8) C(9) 116.9(6) 1_555 1_555 1_555 yes P(1) C(8) H(10) 107.3(5) 1_555 1_555 1_555 no P(1) C(8) H(11) 107.4(5) 1_555 1_555 1_555 no C(9) C(8) H(10) 106.0(6) 1_555 1_555 1_555 no C(9) C(8) H(11) 112.2(7) 1_555 1_555 1_555 no H(10) C(8) H(11) 106.6(7) 1_555 1_555 1_555 no C(8) C(9) H 109(3) 1_555 1_555 1_555 yes C(8) C(9) H(12) 105.0(8) 1_555 1_555 1_555 no C(8) C(9) H(13) 103.9(7) 1_555 1_555 1_555 no H C(9) H(12) 118(3) 1_555 1_555 1_555 no H C(9) H(13) 119(4) 1_555 1_555 1_555 no H(12) C(9) H(13) 99.6(8) 1_555 1_555 1_555 no P(1) C(10) C(11) 111.0(4) 1_555 1_555 1_555 yes P(1) C(10) H(14) 109.2(6) 1_555 1_555 1_555 no P(1) C(10) H(15) 110.4(6) 1_555 1_555 1_555 no C(11) C(10) H(14) 108.7(7) 1_555 1_555 1_555 no C(11) C(10) H(15) 108.9(7) 1_555 1_555 1_555 no H(14) C(10) H(15) 108.6(6) 1_555 1_555 1_555 no P(3) C(11) C(10) 110.4(5) 1_555 1_555 1_555 yes P(3) C(11) H(16) 109.9(5) 1_555 1_555 1_555 no P(3) C(11) H(17) 109.5(5) 1_555 1_555 1_555 no C(10) C(11) H(16) 110.3(6) 1_555 1_555 1_555 no C(10) C(11) H(17) 109.9(6) 1_555 1_555 1_555 no H(16) C(11) H(17) 106.7(7) 1_555 1_555 1_555 no P(3) C(12) C(13) 128.2(9) 1_555 1_555 1_555 yes P(3) C(12) H(18) 108.0(6) 1_555 1_555 1_555 no P(3) C(12) H(19) 104.7(7) 1_555 1_555 1_555 no C(13) C(12) H(18) 112(1) 1_555 1_555 1_555 no C(13) C(12) H(19) 97(1) 1_555 1_555 1_555 no H(18) C(12) H(19) 102.4(9) 1_555 1_555 1_555 no C(12) C(13) H(20) 98(1) 1_555 1_555 1_555 no C(12) C(13) H(21) 120(1) 1_555 1_555 1_555 no C(12) C(13) H(22) 115(1) 1_555 1_555 1_555 no H(20) C(13) H(21) 98(1) 1_555 1_555 1_555 no H(20) C(13) H(22) 97(1) 1_555 1_555 1_555 no H(21) C(13) H(22) 118(1) 1_555 1_555 1_555 no C(15) C(14) H(23) 111.7(8) 1_555 1_555 1_555 no C(15) C(14) H(24) 112.3(7) 1_555 1_555 1_555 no C(15) C(14) H(25) 110.3(8) 1_555 1_555 1_555 no H(23) C(14) H(24) 108.2(8) 1_555 1_555 1_555 no H(23) C(14) H(25) 107.0(7) 1_555 1_555 1_555 no H(24) C(14) H(25) 106.9(8) 1_555 1_555 1_555 no P(3) C(15) C(14) 119.4(5) 1_555 1_555 1_555 yes P(3) C(15) H(26) 107.0(7) 1_555 1_555 1_555 no P(3) C(15) H(27) 107.5(6) 1_555 1_555 1_555 no C(14) C(15) H(26) 106.8(7) 1_555 1_555 1_555 no C(14) C(15) H(27) 108.0(8) 1_555 1_555 1_555 no H(26) C(15) H(27) 107.6(7) 1_555 1_555 1_555 no C(17) C(16) H(28) 111.9(8) 1_555 1_555 1_555 no C(17) C(16) H(29) 110.0(7) 1_555 1_555 1_555 no C(17) C(16) H(30) 109.9(8) 1_555 1_555 1_555 no H(28) C(16) H(29) 107.6(8) 1_555 1_555 1_555 no H(28) C(16) H(30) 108.9(8) 1_555 1_555 1_555 no H(29) C(16) H(30) 108.4(8) 1_555 1_555 1_555 no P(2) C(17) C(16) 119.5(6) 1_555 1_555 1_555 yes P(2) C(17) H(31) 109.2(7) 1_555 1_555 1_555 no P(2) C(17) H(32) 108.0(6) 1_555 1_555 1_555 no C(16) C(17) H(31) 107.0(8) 1_555 1_555 1_555 no C(16) C(17) H(32) 106.1(8) 1_555 1_555 1_555 no H(31) C(17) H(32) 106.3(8) 1_555 1_555 1_555 no P(2) C(18) C(19) 124.3(7) 1_555 1_555 1_555 yes P(2) C(18) H(33) 106.4(5) 1_555 1_555 1_555 no P(2) C(18) H(34) 106.6(7) 1_555 1_555 1_555 no C(19) C(18) H(33) 107.1(9) 1_555 1_555 1_555 no C(19) C(18) H(34) 106.6(7) 1_555 1_555 1_555 no H(33) C(18) H(34) 104.3(8) 1_555 1_555 1_555 no C(18) C(19) H(35) 111.6(9) 1_555 1_555 1_555 no C(18) C(19) H(36) 110.7(9) 1_555 1_555 1_555 no C(18) C(19) H(37) 114.1(9) 1_555 1_555 1_555 no H(35) C(19) H(36) 106.5(10) 1_555 1_555 1_555 no H(35) C(19) H(37) 107.5(10) 1_555 1_555 1_555 no H(36) C(19) H(37) 106.1(10) 1_555 1_555 1_555 no P(2) C(20) C(21) 110.5(6) 1_555 1_555 1_555 yes P(2) C(20) H(38) 109.8(6) 1_555 1_555 1_555 no P(2) C(20) H(39) 108.5(5) 1_555 1_555 1_555 no C(21) C(20) H(38) 113.8(7) 1_555 1_555 1_555 no C(21) C(20) H(39) 109.2(8) 1_555 1_555 1_555 no H(38) C(20) H(39) 104.8(7) 1_555 1_555 1_555 no P(4) C(21) C(20) 113.3(5) 1_555 1_555 1_555 yes P(4) C(21) H(40) 110.9(8) 1_555 1_555 1_555 no P(4) C(21) H(41) 108.2(6) 1_555 1_555 1_555 no C(20) C(21) H(40) 111.6(8) 1_555 1_555 1_555 no C(20) C(21) H(41) 106.4(8) 1_555 1_555 1_555 no H(40) C(21) H(41) 106.2(7) 1_555 1_555 1_555 no P(4) C(22) C(23) 116.4(6) 1_555 1_555 1_555 yes P(4) C(22) H(42) 108.3(5) 1_555 1_555 1_555 no P(4) C(22) H(43) 108.6(5) 1_555 1_555 1_555 no C(23) C(22) H(42) 107.7(7) 1_555 1_555 1_555 no C(23) C(22) H(43) 108.6(7) 1_555 1_555 1_555 no H(42) C(22) H(43) 106.8(7) 1_555 1_555 1_555 no C(22) C(23) H(44) 110.7(8) 1_555 1_555 1_555 no C(22) C(23) H(45) 113.2(8) 1_555 1_555 1_555 no C(22) C(23) H(46) 109.3(7) 1_555 1_555 1_555 no H(44) C(23) H(45) 109.6(9) 1_555 1_555 1_555 no H(44) C(23) H(46) 106.2(9) 1_555 1_555 1_555 no H(45) C(23) H(46) 107.7(9) 1_555 1_555 1_555 no C(25) C(24) H(47) 107.8(9) 1_555 1_555 1_555 no C(25) C(24) H(48) 108.7(9) 1_555 1_555 1_555 no C(25) C(24) H(49) 111(1) 1_555 1_555 1_555 no H(47) C(24) H(48) 108(1) 1_555 1_555 1_555 no H(47) C(24) H(49) 109(1) 1_555 1_555 1_555 no H(48) C(24) H(49) 110.3(10) 1_555 1_555 1_555 no P(4) C(25) C(24) 114.0(7) 1_555 1_555 1_555 yes P(4) C(25) H(50) 110.0(7) 1_555 1_555 1_555 no P(4) C(25) H(51) 110.4(6) 1_555 1_555 1_555 no C(24) C(25) H(50) 107.9(8) 1_555 1_555 1_555 no C(24) C(25) H(51) 108.7(10) 1_555 1_555 1_555 no H(50) C(25) H(51) 105.4(9) 1_555 1_555 1_555 no #========================END data_2 #------------------------------------------ _audit_creation_date 'Tue Jul 6 08:57:41 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------- _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 974.00 _chemical_formula_analytical ? _chemical_formula_sum 'C51 H77 B O P4 S Ru ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------ _cell_length_a 11.485(5) _cell_length_b 24.678(5) _cell_length_c 18.369(4) _cell_angle_alpha 90 _cell_angle_beta 95.22(3) _cell_angle_gamma 90 _cell_volume 5184(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 #-------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? 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 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 1.100 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064.00 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.971 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.04 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -2 -2 2 -3 -1 1 -1 -3 _diffrn_reflns_number 12457 _reflns_number_total 11876 _reflns_number_gt 6755 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.084 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02092 _diffrn_orient_matrix_UB_12 -0.01953 _diffrn_orient_matrix_UB_13 -0.04707 _diffrn_orient_matrix_UB_21 -0.00314 _diffrn_orient_matrix_UB_22 0.03533 _diffrn_orient_matrix_UB_23 -0.02677 _diffrn_orient_matrix_UB_31 0.08484 _diffrn_orient_matrix_UB_32 -0.00351 _diffrn_orient_matrix_UB_33 -0.00747 #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ru' 'Ru' -1.259 0.836 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'B' 'B' 0.001 0.001 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------- 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru(1) Ru 0.08795(6) 0.09077(3) 0.20582(4) 0.0499(2) Uani 1.00 d . . . S(1) S 0.0611(2) 0.12252(8) 0.0806(1) 0.0548(6) Uani 1.00 d . . . P(1) P 0.2034(2) 0.16482(10) 0.2491(1) 0.0672(8) Uani 1.00 d . . . P(2) P 0.1076(2) 0.06326(10) 0.3277(1) 0.0642(7) Uani 1.00 d . . . P(3) P 0.2423(2) 0.03224(10) 0.1711(1) 0.0622(7) Uani 1.00 d . . . P(4) P -0.0320(2) 0.01695(9) 0.1638(1) 0.0599(7) Uani 1.00 d . . . O(1) O -0.0285(7) 0.1564(3) -0.0640(4) 0.091(3) Uani 1.00 d . . . C(1) C -0.0480(8) 0.1389(4) 0.2304(4) 0.061(3) Uani 1.00 d . . . C(2) C -0.1243(9) 0.1721(4) 0.1886(5) 0.072(3) Uani 1.00 d . . . C(3) C -0.1311(8) 0.1824(4) 0.1111(5) 0.068(3) Uani 1.00 d . . . C(4) C -0.0580(9) 0.1653(3) 0.0610(5) 0.066(3) Uani 1.00 d . . . C(5) C 0.1726(8) 0.1682(4) 0.0508(5) 0.074(3) Uani 1.00 d . . . C(6) C -0.0884(9) 0.1767(4) -0.0191(5) 0.074(3) Uani 1.00 d . . . C(7) C -0.184(1) 0.2162(5) -0.0418(6) 0.116(5) Uani 1.00 d . . . C(8) C 0.143(3) 0.2744(7) 0.274(1) 0.30(1) Uani 1.00 d . . . C(9) C 0.153(1) 0.2326(4) 0.2189(7) 0.102(4) Uani 1.00 d . . . C(10) C 0.354(1) 0.1662(5) 0.2322(8) 0.126(6) Uani 1.00 d . . . C(11) C 0.427(1) 0.2152(8) 0.2473(9) 0.164(8) Uani 1.00 d . . . C(12) C 0.200(1) 0.1663(5) 0.3476(6) 0.115(5) Uani 1.00 d . . . C(13) C 0.207(1) 0.1106(5) 0.3774(6) 0.120(5) Uani 1.00 d . . . C(14) C -0.026(1) 0.0620(5) 0.3755(6) 0.105(5) Uani 1.00 d . . . C(15) C -0.037(2) 0.093(1) 0.435(1) 0.22(1) Uani 1.00 d . . . C(16) C 0.222(2) -0.0090(5) 0.4336(7) 0.159(7) Uani 1.00 d . . . C(17) C 0.1692(10) -0.0023(4) 0.3559(6) 0.084(4) Uani 1.00 d . . . C(18) C 0.381(1) 0.0062(5) 0.0532(6) 0.100(4) Uani 1.00 d . . . C(19) C 0.2985(9) 0.0458(4) 0.0824(5) 0.078(3) Uani 1.00 d . . . C(20) C 0.378(1) 0.0194(5) 0.2289(6) 0.094(4) Uani 1.00 d . . . C(21) C 0.429(1) -0.0370(5) 0.2356(7) 0.107(5) Uani 1.00 d . . . C(22) C 0.1746(9) -0.0352(4) 0.1520(6) 0.079(3) Uani 1.00 d . . . C(23) C 0.0532(10) -0.0268(4) 0.1097(6) 0.080(3) Uani 1.00 d . . . C(24) C -0.089(1) -0.0319(4) 0.2265(6) 0.097(4) Uani 1.00 d . . . C(25) C -0.158(1) -0.0803(4) 0.1898(7) 0.106(5) Uani 1.00 d . . . C(26) C -0.270(1) 0.0475(5) 0.1362(8) 0.112(5) Uani 1.00 d . . . C(27) C -0.1621(9) 0.0297(4) 0.0991(5) 0.077(3) Uani 1.00 d . . . C(28) C 0.6280(9) 0.3291(4) 0.1067(6) 0.074(3) Uani 1.00 d . . . C(29) C 0.741(1) 0.3370(4) 0.0947(6) 0.083(4) Uani 1.00 d . . . C(30) C 0.831(1) 0.3386(5) 0.1525(9) 0.106(5) Uani 1.00 d . . . C(31) C 0.804(1) 0.3313(5) 0.2237(8) 0.109(5) Uani 1.00 d . . . C(32) C 0.693(1) 0.3245(5) 0.2371(6) 0.105(5) Uani 1.00 d . . . C(33) C 0.605(1) 0.3236(5) 0.1799(6) 0.093(4) Uani 1.00 d . . . C(34) C 0.5120(8) 0.2568(4) 0.0172(5) 0.068(3) Uani 1.00 d . . . C(35) C 0.5487(9) 0.2159(4) 0.0659(6) 0.083(4) Uani 1.00 d . . . C(36) C 0.533(1) 0.1613(5) 0.0468(9) 0.111(5) Uani 1.00 d . . . C(37) C 0.487(1) 0.1462(5) -0.0202(10) 0.115(6) Uani 1.00 d . . . C(38) C 0.449(1) 0.1848(5) -0.0696(7) 0.106(5) Uani 1.00 d . . . C(39) C 0.464(1) 0.2388(4) -0.0501(6) 0.092(4) Uani 1.00 d . . . C(40) C 0.3949(9) 0.3422(4) 0.0636(5) 0.065(3) Uani 1.00 d . . . C(41) C 0.2926(8) 0.3139(4) 0.0495(5) 0.068(3) Uani 1.00 d . . . C(42) C 0.1847(9) 0.3334(4) 0.0683(5) 0.075(3) Uani 1.00 d . . . C(43) C 0.1781(10) 0.3824(5) 0.1040(6) 0.084(4) Uani 1.00 d . . . C(44) C 0.2802(9) 0.4108(5) 0.1206(6) 0.084(4) Uani 1.00 d . . . C(45) C 0.3850(9) 0.3909(4) 0.1018(5) 0.076(3) Uani 1.00 d . . . C(46) C 0.5571(8) 0.3577(4) -0.0319(5) 0.069(3) Uani 1.00 d . . . C(47) C 0.5247(9) 0.4120(4) -0.0424(5) 0.077(3) Uani 1.00 d . . . C(48) C 0.559(1) 0.4437(4) -0.0990(7) 0.091(4) Uani 1.00 d . . . C(49) C 0.628(1) 0.4214(6) -0.1490(7) 0.102(5) Uani 1.00 d . . . C(50) C 0.662(1) 0.3687(6) -0.1423(6) 0.102(5) Uani 1.00 d . . . C(51) C 0.628(1) 0.3380(5) -0.0839(6) 0.093(4) Uani 1.00 d . . . B B 0.521(1) 0.3215(4) 0.0391(6) 0.069(3) Uani 1.00 d . . . H H 0.0819 0.2741 0.2971 0.2431 Uiso 1.00 d . . . H(1) H -0.0611 0.1389 0.2820 0.0734 Uiso 1.00 calc . . . H(2) H -0.1807 0.1916 0.2147 0.0826 Uiso 1.00 calc . . . H(3) H -0.1981 0.2042 0.0909 0.0792 Uiso 1.00 calc . . . H(4) H -0.1547 0.2475 -0.0638 0.1210 Uiso 1.00 calc . . . H(5) H -0.2421 0.1998 -0.0773 0.1210 Uiso 1.00 calc . . . H(6) H -0.2256 0.2272 -0.0011 0.1210 Uiso 1.00 calc . . . H(7) H 0.2489 0.1513 0.0573 0.0851 Uiso 1.00 calc . . . H(8) H 0.1574 0.1773 0.0004 0.0851 Uiso 1.00 calc . . . H(9) H 0.1766 0.2010 0.0788 0.0851 Uiso 1.00 calc . . . H(10) H 0.2167 0.2685 0.3109 0.2431 Uiso 1.00 calc . . . H(11) H 0.1627 0.3104 0.2546 0.2431 Uiso 1.00 calc . . . H(12) H 0.2020 0.2450 0.1798 0.1114 Uiso 1.00 calc . . . H(13) H 0.0747 0.2297 0.1931 0.1114 Uiso 1.00 calc . . . H(14) H 0.3953 0.1370 0.2604 0.1359 Uiso 1.00 calc . . . H(15) H 0.3610 0.1565 0.1811 0.1359 Uiso 1.00 calc . . . H(16) H 0.5051 0.2120 0.2352 0.1690 Uiso 1.00 calc . . . H(17) H 0.3918 0.2457 0.2186 0.1690 Uiso 1.00 calc . . . H(18) H 0.4275 0.2258 0.2976 0.1690 Uiso 1.00 calc . . . H(19) H 0.2627 0.1901 0.3694 0.1192 Uiso 1.00 calc . . . H(20) H 0.1278 0.1836 0.3603 0.1192 Uiso 1.00 calc . . . H(21) H 0.1970 0.1099 0.4287 0.1209 Uiso 1.00 calc . . . H(22) H 0.2895 0.0975 0.3745 0.1209 Uiso 1.00 calc . . . H(23) H -0.0911 0.0662 0.3393 0.1162 Uiso 1.00 calc . . . H(24) H -0.0327 0.0238 0.3933 0.1162 Uiso 1.00 calc . . . H(25) H 0.0205 0.0892 0.4724 0.2018 Uiso 1.00 calc . . . H(26) H -0.0343 0.1323 0.4181 0.2018 Uiso 1.00 calc . . . H(27) H -0.1137 0.0905 0.4527 0.2018 Uiso 1.00 calc . . . H(28) H 0.2563 -0.0440 0.4436 0.1576 Uiso 1.00 calc . . . H(29) H 0.2904 0.0168 0.4418 0.1576 Uiso 1.00 calc . . . H(30) H 0.1709 -0.0002 0.4678 0.1576 Uiso 1.00 calc . . . H(31) H 0.1089 -0.0299 0.3484 0.0981 Uiso 1.00 calc . . . H(32) H 0.2282 -0.0125 0.3225 0.0981 Uiso 1.00 calc . . . H(33) H 0.3472 -0.0280 0.0477 0.1141 Uiso 1.00 calc . . . H(34) H 0.4086 0.0177 0.0076 0.1141 Uiso 1.00 calc . . . H(35) H 0.4513 0.0033 0.0878 0.1141 Uiso 1.00 calc . . . H(36) H 0.2329 0.0511 0.0454 0.0950 Uiso 1.00 calc . . . H(37) H 0.3370 0.0824 0.0855 0.0950 Uiso 1.00 calc . . . H(38) H 0.4363 0.0438 0.2128 0.1095 Uiso 1.00 calc . . . H(39) H 0.3640 0.0314 0.2782 0.1095 Uiso 1.00 calc . . . H(40) H 0.3753 -0.0625 0.2524 0.1177 Uiso 1.00 calc . . . H(41) H 0.4501 -0.0497 0.1884 0.1177 Uiso 1.00 calc . . . H(42) H 0.4998 -0.0385 0.2683 0.1177 Uiso 1.00 calc . . . H(43) H 0.2236 -0.0572 0.1239 0.0910 Uiso 1.00 calc . . . H(44) H 0.1659 -0.0542 0.1969 0.0910 Uiso 1.00 calc . . . H(45) H 0.0123 -0.0614 0.1009 0.0926 Uiso 1.00 calc . . . H(46) H 0.0602 -0.0112 0.0623 0.0926 Uiso 1.00 calc . . . H(47) H -0.0249 -0.0463 0.2590 0.1074 Uiso 1.00 calc . . . H(48) H -0.1397 -0.0131 0.2582 0.1074 Uiso 1.00 calc . . . H(49) H -0.2253 -0.0670 0.1584 0.1164 Uiso 1.00 calc . . . H(50) H -0.1103 -0.1000 0.1582 0.1164 Uiso 1.00 calc . . . H(51) H -0.1866 -0.1050 0.2234 0.1164 Uiso 1.00 calc . . . H(52) H -0.2541 0.0804 0.1634 0.1217 Uiso 1.00 calc . . . H(53) H -0.3366 0.0541 0.1018 0.1217 Uiso 1.00 calc . . . H(54) H -0.2918 0.0204 0.1700 0.1217 Uiso 1.00 calc . . . H(55) H -0.1446 0.0571 0.0642 0.0903 Uiso 1.00 calc . . . H(56) H -0.1819 -0.0029 0.0711 0.0903 Uiso 1.00 calc . . . H(57) H 0.7588 0.3415 0.0444 0.1000 Uiso 1.00 calc . . . H(58) H 0.9136 0.3439 0.1433 0.1211 Uiso 1.00 calc . . . H(59) H 0.8654 0.3323 0.2633 0.1187 Uiso 1.00 calc . . . H(60) H 0.6755 0.3202 0.2875 0.1221 Uiso 1.00 calc . . . H(61) H 0.5229 0.3195 0.1906 0.1100 Uiso 1.00 calc . . . H(62) H 0.5838 0.2259 0.1160 0.0969 Uiso 1.00 calc . . . H(63) H 0.5577 0.1330 0.0822 0.1234 Uiso 1.00 calc . . . H(64) H 0.4797 0.1082 -0.0299 0.1278 Uiso 1.00 calc . . . H(65) H 0.4146 0.1730 -0.1191 0.1271 Uiso 1.00 calc . . . H(66) H 0.4381 0.2666 -0.0859 0.1096 Uiso 1.00 calc . . . H(67) H 0.2936 0.2792 0.0242 0.0789 Uiso 1.00 calc . . . H(68) H 0.1138 0.3121 0.0563 0.0877 Uiso 1.00 calc . . . H(69) H 0.1035 0.3958 0.1160 0.0982 Uiso 1.00 calc . . . H(70) H 0.2751 0.4455 0.1450 0.0984 Uiso 1.00 calc . . . H(71) H 0.4559 0.4117 0.1166 0.0920 Uiso 1.00 calc . . . H(72) H 0.4734 0.4288 -0.0074 0.0911 Uiso 1.00 calc . . . H(73) H 0.5364 0.4821 -0.1032 0.1047 Uiso 1.00 calc . . . H(74) H 0.6505 0.4444 -0.1889 0.1171 Uiso 1.00 calc . . . H(75) H 0.7119 0.3529 -0.1794 0.1253 Uiso 1.00 calc . . . H(76) H 0.6546 0.3000 -0.0792 0.1074 Uiso 1.00 calc . . . 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) 0.0590(4) 0.0432(3) 0.0480(3) 0.0004(3) 0.0075(3) 0.0006(3) S(1) 0.064(1) 0.048(1) 0.053(1) 0.0058(10) 0.0101(10) 0.0016(9) P(1) 0.087(2) 0.051(1) 0.064(1) -0.011(1) 0.012(1) -0.005(1) P(2) 0.086(2) 0.057(1) 0.050(1) -0.001(1) 0.004(1) 0.000(1) P(3) 0.067(2) 0.056(1) 0.064(1) 0.008(1) 0.008(1) 0.002(1) P(4) 0.071(2) 0.051(1) 0.058(1) -0.006(1) 0.007(1) 0.001(1) O(1) 0.135(7) 0.078(5) 0.061(4) 0.031(4) 0.016(4) 0.003(4) C(1) 0.065(6) 0.072(6) 0.047(5) -0.002(5) 0.004(4) -0.003(4) C(2) 0.079(7) 0.074(6) 0.064(6) 0.020(5) 0.022(5) -0.004(5) C(3) 0.079(7) 0.058(5) 0.069(6) 0.019(5) 0.013(5) 0.006(5) C(4) 0.094(7) 0.044(5) 0.060(5) 0.013(4) 0.015(5) 0.006(4) C(5) 0.063(6) 0.095(7) 0.065(6) -0.012(5) 0.005(5) 0.013(5) C(6) 0.092(8) 0.062(6) 0.070(6) 0.014(5) 0.010(5) 0.012(5) C(7) 0.14(1) 0.13(1) 0.075(7) 0.071(9) 0.005(7) 0.030(7) C(8) 0.57(5) 0.09(1) 0.20(2) 0.09(2) -0.09(3) -0.06(1) C(9) 0.108(9) 0.061(6) 0.13(1) -0.014(6) -0.007(8) -0.003(7) C(10) 0.11(1) 0.092(9) 0.17(1) -0.024(8) 0.005(10) -0.039(9) C(11) 0.14(1) 0.22(2) 0.14(1) -0.08(1) 0.02(1) 0.01(1) C(12) 0.18(1) 0.090(9) 0.070(7) -0.028(9) -0.016(8) -0.014(6) C(13) 0.21(2) 0.087(8) 0.056(6) -0.031(9) -0.024(8) -0.005(6) C(14) 0.13(1) 0.13(1) 0.061(6) 0.036(8) 0.013(7) 0.022(7) C(15) 0.13(2) 0.37(3) 0.15(2) -0.02(2) 0.00(1) -0.11(2) C(16) 0.28(2) 0.090(9) 0.095(10) 0.02(1) -0.05(1) 0.030(8) C(17) 0.092(8) 0.088(7) 0.071(6) 0.007(6) -0.001(6) 0.017(6) C(18) 0.091(8) 0.120(10) 0.090(8) 0.032(7) 0.019(7) -0.004(7) C(19) 0.079(7) 0.084(7) 0.073(6) 0.012(6) 0.014(5) -0.011(5) C(20) 0.106(9) 0.093(8) 0.081(7) 0.026(7) -0.010(6) -0.010(6) C(21) 0.113(10) 0.093(8) 0.111(9) 0.043(7) -0.013(7) 0.004(7) C(22) 0.076(7) 0.063(6) 0.100(8) 0.015(5) 0.021(6) -0.003(5) C(23) 0.094(8) 0.059(6) 0.086(7) -0.008(5) 0.007(6) -0.023(5) C(24) 0.15(1) 0.067(6) 0.072(7) -0.038(7) 0.027(7) 0.001(5) C(25) 0.14(1) 0.069(7) 0.110(9) -0.035(7) 0.008(8) 0.006(6) C(26) 0.085(9) 0.098(9) 0.15(1) 0.014(7) 0.000(8) -0.028(8) C(27) 0.075(7) 0.076(7) 0.078(7) -0.013(5) -0.006(5) 0.003(5) C(28) 0.084(7) 0.060(6) 0.077(7) 0.003(5) 0.004(6) 0.013(5) C(29) 0.081(8) 0.074(7) 0.093(8) -0.009(6) 0.004(6) 0.009(6) C(30) 0.069(8) 0.092(9) 0.15(1) -0.005(6) -0.012(8) 0.005(9) C(31) 0.10(1) 0.096(9) 0.12(1) 0.008(8) -0.040(9) 0.000(8) C(32) 0.10(1) 0.13(1) 0.077(8) 0.011(8) -0.021(7) 0.012(7) C(33) 0.100(9) 0.101(9) 0.077(7) -0.001(7) -0.006(6) 0.016(6) C(34) 0.070(6) 0.058(5) 0.077(6) 0.006(5) 0.012(5) 0.013(5) C(35) 0.088(8) 0.068(6) 0.094(8) 0.013(5) 0.013(6) 0.027(6) C(36) 0.13(1) 0.070(8) 0.14(1) 0.026(8) 0.032(10) 0.041(8) C(37) 0.13(1) 0.059(7) 0.16(1) 0.007(7) 0.04(1) -0.007(9) C(38) 0.12(1) 0.077(8) 0.12(1) 0.001(7) 0.004(8) -0.013(8) C(39) 0.114(10) 0.063(6) 0.095(8) 0.014(6) -0.007(7) 0.006(6) C(40) 0.079(7) 0.058(5) 0.059(5) 0.001(5) 0.012(5) 0.013(4) C(41) 0.067(6) 0.062(6) 0.075(6) 0.003(5) 0.010(5) 0.017(5) C(42) 0.065(6) 0.081(7) 0.077(6) -0.009(5) 0.003(5) 0.019(5) C(43) 0.083(8) 0.090(8) 0.080(7) 0.016(6) 0.019(6) 0.008(6) C(44) 0.071(7) 0.092(7) 0.089(7) 0.006(6) 0.012(6) -0.013(6) C(45) 0.080(7) 0.073(6) 0.075(6) -0.007(5) 0.015(5) -0.005(5) C(46) 0.069(6) 0.062(6) 0.075(6) 0.004(5) 0.011(5) 0.014(5) C(47) 0.093(7) 0.063(6) 0.075(6) -0.003(5) 0.009(5) 0.016(5) C(48) 0.110(9) 0.066(7) 0.096(8) -0.010(6) 0.002(7) 0.025(6) C(49) 0.11(1) 0.104(10) 0.090(8) -0.019(8) 0.019(7) 0.033(7) C(50) 0.099(9) 0.12(1) 0.091(8) 0.008(8) 0.036(7) 0.025(8) C(51) 0.104(9) 0.088(8) 0.092(8) 0.023(7) 0.030(7) 0.024(6) B 0.095(9) 0.055(6) 0.058(6) 0.000(6) 0.006(6) 0.013(5) #----------------------------------------- _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6755 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.980 _refine_ls_shift/su_max 0.5280 _refine_ls_shift/su_mean 0.0090 _refine_diff_density_min -1.41 _refine_diff_density_max 1.10 #-------------------------------------------- _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) S(1) 2.423(2) 1_555 1_555 yes Ru(1) P(1) 2.353(3) 1_555 1_555 yes Ru(1) P(2) 2.330(2) 1_555 1_555 yes Ru(1) P(3) 2.417(3) 1_555 1_555 yes Ru(1) P(4) 2.370(3) 1_555 1_555 yes Ru(1) C(1) 2.044(9) 1_555 1_555 yes S(1) C(4) 1.739(9) 1_555 1_555 yes S(1) C(5) 1.825(9) 1_555 1_555 yes P(1) C(9) 1.83(1) 1_555 1_555 yes P(1) C(10) 1.79(1) 1_555 1_555 yes P(1) C(12) 1.81(1) 1_555 1_555 yes P(2) C(13) 1.82(1) 1_555 1_555 yes P(2) C(14) 1.83(1) 1_555 1_555 yes P(2) C(17) 1.82(1) 1_555 1_555 yes P(3) C(19) 1.84(1) 1_555 1_555 yes P(3) C(20) 1.83(1) 1_555 1_555 yes P(3) C(22) 1.86(1) 1_555 1_555 yes P(4) C(23) 1.81(1) 1_555 1_555 yes P(4) C(24) 1.826(10) 1_555 1_555 yes P(4) C(27) 1.85(1) 1_555 1_555 yes O(1) C(6) 1.23(1) 1_555 1_555 yes C(1) C(2) 1.38(1) 1_555 1_555 yes C(1) H(1) 0.973 1_555 1_555 no C(2) C(3) 1.44(1) 1_555 1_555 yes C(2) H(2) 0.970 1_555 1_555 no C(3) C(4) 1.37(1) 1_555 1_555 yes C(3) H(3) 0.984 1_555 1_555 no C(4) C(6) 1.51(1) 1_555 1_555 yes C(5) H(7) 0.970 1_555 1_555 no C(5) H(8) 0.953 1_555 1_555 no C(5) H(9) 0.959 1_555 1_555 no C(6) C(7) 1.50(1) 1_555 1_555 yes C(7) H(4) 0.948 1_555 1_555 no C(7) H(5) 0.976 1_555 1_555 no C(7) H(6) 0.965 1_555 1_555 no C(8) C(9) 1.48(2) 1_555 1_555 yes C(8) H 0.833 1_555 1_555 yes C(8) H(10) 1.057 1_555 1_555 no C(8) H(11) 1.019 1_555 1_555 no C(9) H(12) 0.974 1_555 1_555 no C(9) H(13) 0.981 1_555 1_555 no C(10) C(11) 1.48(2) 1_555 1_555 yes C(10) H(14) 0.980 1_555 1_555 no C(10) H(15) 0.982 1_555 1_555 no C(11) H(16) 0.950 1_555 1_555 no C(11) H(17) 0.986 1_555 1_555 no C(11) H(18) 0.959 1_555 1_555 no C(12) C(13) 1.48(2) 1_555 1_555 yes C(12) H(19) 0.986 1_555 1_555 no C(12) H(20) 0.976 1_555 1_555 no C(13) H(21) 0.961 1_555 1_555 no C(13) H(22) 1.003 1_555 1_555 no C(14) C(15) 1.36(2) 1_555 1_555 yes C(14) H(23) 0.956 1_555 1_555 no C(14) H(24) 0.985 1_555 1_555 no C(15) H(25) 0.936 1_555 1_555 no C(15) H(26) 0.993 1_555 1_555 no C(15) H(27) 0.978 1_555 1_555 no C(16) C(17) 1.51(2) 1_555 1_555 yes C(16) H(28) 0.960 1_555 1_555 no C(16) H(29) 1.009 1_555 1_555 no C(16) H(30) 0.925 1_555 1_555 no C(17) H(31) 0.975 1_555 1_555 no C(17) H(32) 0.986 1_555 1_555 no C(18) C(19) 1.49(1) 1_555 1_555 yes C(18) H(33) 0.928 1_555 1_555 no C(18) H(34) 0.967 1_555 1_555 no C(18) H(35) 0.987 1_555 1_555 no C(19) H(36) 0.975 1_555 1_555 no C(19) H(37) 1.005 1_555 1_555 no C(20) C(21) 1.51(1) 1_555 1_555 yes C(20) H(38) 0.971 1_555 1_555 no C(20) H(39) 0.978 1_555 1_555 no C(21) H(40) 0.951 1_555 1_555 no C(21) H(41) 0.977 1_555 1_555 no C(21) H(42) 0.968 1_555 1_555 no C(22) C(23) 1.55(1) 1_555 1_555 yes C(22) H(43) 0.962 1_555 1_555 no C(22) H(44) 0.964 1_555 1_555 no C(23) H(45) 0.978 1_555 1_555 no C(23) H(46) 0.963 1_555 1_555 no C(24) C(25) 1.56(1) 1_555 1_555 yes C(24) H(47) 0.969 1_555 1_555 no C(24) H(48) 0.980 1_555 1_555 no C(25) H(49) 0.976 1_555 1_555 no C(25) H(50) 0.966 1_555 1_555 no C(25) H(51) 0.948 1_555 1_555 no C(26) C(27) 1.53(2) 1_555 1_555 yes C(26) H(52) 0.963 1_555 1_555 no C(26) H(53) 0.956 1_555 1_555 no C(26) H(54) 0.961 1_555 1_555 no C(27) H(55) 0.967 1_555 1_555 no C(27) H(56) 0.971 1_555 1_555 no C(28) C(29) 1.35(1) 1_555 1_555 yes C(28) C(33) 1.40(1) 1_555 1_555 yes C(28) B 1.67(2) 1_555 1_555 yes C(29) C(30) 1.42(2) 1_555 1_555 yes C(29) H(57) 0.970 1_555 1_555 no C(30) C(31) 1.38(2) 1_555 1_555 yes C(30) H(58) 0.987 1_555 1_555 no C(31) C(32) 1.33(2) 1_555 1_555 yes C(31) H(59) 0.967 1_555 1_555 no C(32) C(33) 1.38(1) 1_555 1_555 yes C(32) H(60) 0.969 1_555 1_555 no C(33) H(61) 0.987 1_555 1_555 no C(34) C(35) 1.39(1) 1_555 1_555 yes C(34) C(39) 1.38(1) 1_555 1_555 yes C(34) B 1.65(1) 1_555 1_555 yes C(35) C(36) 1.40(2) 1_555 1_555 yes C(35) H(62) 0.999 1_555 1_555 no C(36) C(37) 1.35(2) 1_555 1_555 yes C(36) H(63) 0.978 1_555 1_555 no C(37) C(38) 1.36(2) 1_555 1_555 yes C(37) H(64) 0.956 1_555 1_555 no C(38) C(39) 1.38(1) 1_555 1_555 yes C(38) H(65) 1.003 1_555 1_555 no C(39) H(66) 0.975 1_555 1_555 no C(40) C(41) 1.37(1) 1_555 1_555 yes C(40) C(45) 1.40(1) 1_555 1_555 yes C(40) B 1.64(2) 1_555 1_555 yes C(41) C(42) 1.40(1) 1_555 1_555 yes C(41) H(67) 0.976 1_555 1_555 no C(42) C(43) 1.38(1) 1_555 1_555 yes C(42) H(68) 0.975 1_555 1_555 no C(43) C(44) 1.38(1) 1_555 1_555 yes C(43) H(69) 0.965 1_555 1_555 no C(44) C(45) 1.37(1) 1_555 1_555 yes C(44) H(70) 0.971 1_555 1_555 no C(45) H(71) 0.979 1_555 1_555 no C(46) C(47) 1.40(1) 1_555 1_555 yes C(46) C(51) 1.40(1) 1_555 1_555 yes C(46) B 1.66(1) 1_555 1_555 yes C(47) C(48) 1.38(1) 1_555 1_555 yes C(47) H(72) 1.000 1_555 1_555 no C(48) C(49) 1.38(2) 1_555 1_555 yes C(48) H(73) 0.984 1_555 1_555 no C(49) C(50) 1.36(2) 1_555 1_555 yes C(49) H(74) 0.980 1_555 1_555 no C(50) C(51) 1.40(1) 1_555 1_555 yes C(50) H(75) 1.007 1_555 1_555 no C(51) H(76) 0.986 1_555 1_555 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 S(1) Ru(1) P(1) 95.11(9) 1_555 1_555 1_555 yes S(1) Ru(1) P(2) 177.33(9) 1_555 1_555 1_555 yes S(1) Ru(1) P(3) 88.61(8) 1_555 1_555 1_555 yes S(1) Ru(1) P(4) 85.38(8) 1_555 1_555 1_555 yes S(1) Ru(1) C(1) 89.3(2) 1_555 1_555 1_555 yes P(1) Ru(1) P(2) 84.23(9) 1_555 1_555 1_555 yes P(1) Ru(1) P(3) 98.56(10) 1_555 1_555 1_555 yes P(1) Ru(1) P(4) 178.65(10) 1_555 1_555 1_555 yes P(1) Ru(1) C(1) 83.8(3) 1_555 1_555 1_555 yes P(2) Ru(1) P(3) 94.04(9) 1_555 1_555 1_555 yes P(2) Ru(1) P(4) 95.23(9) 1_555 1_555 1_555 yes P(2) Ru(1) C(1) 88.0(2) 1_555 1_555 1_555 yes P(3) Ru(1) P(4) 82.70(9) 1_555 1_555 1_555 yes P(3) Ru(1) C(1) 177.0(2) 1_555 1_555 1_555 yes P(4) Ru(1) C(1) 95.0(3) 1_555 1_555 1_555 yes Ru(1) S(1) C(4) 115.0(3) 1_555 1_555 1_555 yes Ru(1) S(1) C(5) 116.9(3) 1_555 1_555 1_555 yes C(4) S(1) C(5) 97.0(5) 1_555 1_555 1_555 yes Ru(1) P(1) C(9) 116.6(4) 1_555 1_555 1_555 yes Ru(1) P(1) C(10) 118.8(4) 1_555 1_555 1_555 yes Ru(1) P(1) C(12) 106.9(4) 1_555 1_555 1_555 yes C(9) P(1) C(10) 101.8(6) 1_555 1_555 1_555 yes C(9) P(1) C(12) 105.3(6) 1_555 1_555 1_555 yes C(10) P(1) C(12) 106.3(7) 1_555 1_555 1_555 yes Ru(1) P(2) C(13) 107.2(4) 1_555 1_555 1_555 yes Ru(1) P(2) C(14) 116.8(4) 1_555 1_555 1_555 yes Ru(1) P(2) C(17) 122.2(4) 1_555 1_555 1_555 yes C(13) P(2) C(14) 107.3(7) 1_555 1_555 1_555 yes C(13) P(2) C(17) 102.5(6) 1_555 1_555 1_555 yes C(14) P(2) C(17) 99.2(5) 1_555 1_555 1_555 yes Ru(1) P(3) C(19) 116.7(3) 1_555 1_555 1_555 yes Ru(1) P(3) C(20) 123.7(4) 1_555 1_555 1_555 yes Ru(1) P(3) C(22) 106.4(3) 1_555 1_555 1_555 yes C(19) P(3) C(20) 101.5(5) 1_555 1_555 1_555 yes C(19) P(3) C(22) 99.8(5) 1_555 1_555 1_555 yes C(20) P(3) C(22) 105.8(5) 1_555 1_555 1_555 yes Ru(1) P(4) C(23) 108.2(3) 1_555 1_555 1_555 yes Ru(1) P(4) C(24) 122.1(4) 1_555 1_555 1_555 yes Ru(1) P(4) C(27) 119.4(3) 1_555 1_555 1_555 yes C(23) P(4) C(24) 101.1(5) 1_555 1_555 1_555 yes C(23) P(4) C(27) 101.1(5) 1_555 1_555 1_555 yes C(24) P(4) C(27) 101.7(5) 1_555 1_555 1_555 yes Ru(1) C(1) C(2) 132.8(6) 1_555 1_555 1_555 yes Ru(1) C(1) H(1) 114.0(7) 1_555 1_555 1_555 no C(2) C(1) H(1) 113.2(9) 1_555 1_555 1_555 no C(1) C(2) C(3) 129.1(8) 1_555 1_555 1_555 yes C(1) C(2) H(2) 116.0(9) 1_555 1_555 1_555 no C(3) C(2) H(2) 114.9(9) 1_555 1_555 1_555 no C(2) C(3) C(4) 128.9(9) 1_555 1_555 1_555 yes C(2) C(3) H(3) 116.0(9) 1_555 1_555 1_555 no C(4) C(3) H(3) 115.1(9) 1_555 1_555 1_555 no S(1) C(4) C(3) 124.6(7) 1_555 1_555 1_555 yes S(1) C(4) C(6) 115.0(7) 1_555 1_555 1_555 yes C(3) C(4) C(6) 119.8(9) 1_555 1_555 1_555 yes S(1) C(5) H(7) 110.5(8) 1_555 1_555 1_555 no S(1) C(5) H(8) 111.6(7) 1_555 1_555 1_555 no S(1) C(5) H(9) 111.3(7) 1_555 1_555 1_555 no H(7) C(5) H(8) 107.6(9) 1_555 1_555 1_555 no H(7) C(5) H(9) 107.1(9) 1_555 1_555 1_555 no H(8) C(5) H(9) 108.5(10) 1_555 1_555 1_555 no O(1) C(6) C(4) 119.0(9) 1_555 1_555 1_555 yes O(1) C(6) C(7) 121.2(9) 1_555 1_555 1_555 yes C(4) C(6) C(7) 119.5(9) 1_555 1_555 1_555 yes C(6) C(7) H(4) 111(1) 1_555 1_555 1_555 no C(6) C(7) H(5) 111(1) 1_555 1_555 1_555 no C(6) C(7) H(6) 111.8(10) 1_555 1_555 1_555 no H(4) C(7) H(5) 107(1) 1_555 1_555 1_555 no H(4) C(7) H(6) 108(1) 1_555 1_555 1_555 no H(5) C(7) H(6) 106(1) 1_555 1_555 1_555 no C(9) C(8) H 120(2) 1_555 1_555 1_555 yes C(9) C(8) H(10) 103(1) 1_555 1_555 1_555 no C(9) C(8) H(11) 109(1) 1_555 1_555 1_555 no H C(8) H(10) 109(2) 1_555 1_555 1_555 no H C(8) H(11) 113(2) 1_555 1_555 1_555 no H(10) C(8) H(11) 96(1) 1_555 1_555 1_555 no P(1) C(9) C(8) 116(1) 1_555 1_555 1_555 yes P(1) C(9) H(12) 110.2(10) 1_555 1_555 1_555 no P(1) C(9) H(13) 109.9(8) 1_555 1_555 1_555 no C(8) C(9) H(12) 111(1) 1_555 1_555 1_555 no C(8) C(9) H(13) 102(1) 1_555 1_555 1_555 no H(12) C(9) H(13) 105(1) 1_555 1_555 1_555 no P(1) C(10) C(11) 121(1) 1_555 1_555 1_555 yes P(1) C(10) H(14) 108(1) 1_555 1_555 1_555 no P(1) C(10) H(15) 108(1) 1_555 1_555 1_555 no C(11) C(10) H(14) 105(1) 1_555 1_555 1_555 no C(11) C(10) H(15) 106(1) 1_555 1_555 1_555 no H(14) C(10) H(15) 104(1) 1_555 1_555 1_555 no C(10) C(11) H(16) 114(1) 1_555 1_555 1_555 no C(10) C(11) H(17) 109(1) 1_555 1_555 1_555 no C(10) C(11) H(18) 111(1) 1_555 1_555 1_555 no H(16) C(11) H(17) 106(1) 1_555 1_555 1_555 no H(16) C(11) H(18) 108(1) 1_555 1_555 1_555 no H(17) C(11) H(18) 105(1) 1_555 1_555 1_555 no P(1) C(12) C(13) 110.0(8) 1_555 1_555 1_555 yes P(1) C(12) H(19) 109(1) 1_555 1_555 1_555 no P(1) C(12) H(20) 110.1(10) 1_555 1_555 1_555 no C(13) C(12) H(19) 112(1) 1_555 1_555 1_555 no C(13) C(12) H(20) 109(1) 1_555 1_555 1_555 no H(19) C(12) H(20) 104(1) 1_555 1_555 1_555 no P(2) C(13) C(12) 113.5(9) 1_555 1_555 1_555 yes P(2) C(13) H(21) 110(1) 1_555 1_555 1_555 no P(2) C(13) H(22) 108.6(9) 1_555 1_555 1_555 no C(12) C(13) H(21) 111(1) 1_555 1_555 1_555 no C(12) C(13) H(22) 107(1) 1_555 1_555 1_555 no H(21) C(13) H(22) 104(1) 1_555 1_555 1_555 no P(2) C(14) C(15) 120(1) 1_555 1_555 1_555 yes P(2) C(14) H(23) 108.0(8) 1_555 1_555 1_555 no P(2) C(14) H(24) 106.6(9) 1_555 1_555 1_555 no C(15) C(14) H(23) 109(1) 1_555 1_555 1_555 no C(15) C(14) H(24) 105(1) 1_555 1_555 1_555 no H(23) C(14) H(24) 106(1) 1_555 1_555 1_555 no C(14) C(15) H(25) 114(1) 1_555 1_555 1_555 no C(14) C(15) H(26) 109(1) 1_555 1_555 1_555 no C(14) C(15) H(27) 112(1) 1_555 1_555 1_555 no H(25) C(15) H(26) 106(2) 1_555 1_555 1_555 no H(25) C(15) H(27) 108(2) 1_555 1_555 1_555 no H(26) C(15) H(27) 103(1) 1_555 1_555 1_555 no C(17) C(16) H(28) 113(1) 1_555 1_555 1_555 no C(17) C(16) H(29) 108(1) 1_555 1_555 1_555 no C(17) C(16) H(30) 112(1) 1_555 1_555 1_555 no H(28) C(16) H(29) 103(1) 1_555 1_555 1_555 no H(28) C(16) H(30) 110(1) 1_555 1_555 1_555 no H(29) C(16) H(30) 106(1) 1_555 1_555 1_555 no P(2) C(17) C(16) 118.6(9) 1_555 1_555 1_555 yes P(2) C(17) H(31) 109.1(8) 1_555 1_555 1_555 no P(2) C(17) H(32) 108.8(8) 1_555 1_555 1_555 no C(16) C(17) H(31) 106(1) 1_555 1_555 1_555 no C(16) C(17) H(32) 108(1) 1_555 1_555 1_555 no H(31) C(17) H(32) 104(1) 1_555 1_555 1_555 no C(19) C(18) H(33) 111(1) 1_555 1_555 1_555 no C(19) C(18) H(34) 112(1) 1_555 1_555 1_555 no C(19) C(18) H(35) 109(1) 1_555 1_555 1_555 no H(33) C(18) H(34) 109(1) 1_555 1_555 1_555 no H(33) C(18) H(35) 108(1) 1_555 1_555 1_555 no H(34) C(18) H(35) 105(1) 1_555 1_555 1_555 no P(3) C(19) C(18) 118.9(8) 1_555 1_555 1_555 yes P(3) C(19) H(36) 109.4(8) 1_555 1_555 1_555 no P(3) C(19) H(37) 107.6(7) 1_555 1_555 1_555 no C(18) C(19) H(36) 108.1(9) 1_555 1_555 1_555 no C(18) C(19) H(37) 108.6(10) 1_555 1_555 1_555 no H(36) C(19) H(37) 103.2(10) 1_555 1_555 1_555 no P(3) C(20) C(21) 120.8(9) 1_555 1_555 1_555 yes P(3) C(20) H(38) 107.1(8) 1_555 1_555 1_555 no P(3) C(20) H(39) 106.7(9) 1_555 1_555 1_555 no C(21) C(20) H(38) 108(1) 1_555 1_555 1_555 no C(21) C(20) H(39) 107(1) 1_555 1_555 1_555 no H(38) C(20) H(39) 105(1) 1_555 1_555 1_555 no C(20) C(21) H(40) 112(1) 1_555 1_555 1_555 no C(20) C(21) H(41) 110(1) 1_555 1_555 1_555 no C(20) C(21) H(42) 112(1) 1_555 1_555 1_555 no H(40) C(21) H(41) 107(1) 1_555 1_555 1_555 no H(40) C(21) H(42) 107(1) 1_555 1_555 1_555 no H(41) C(21) H(42) 105(1) 1_555 1_555 1_555 no P(3) C(22) C(23) 108.6(6) 1_555 1_555 1_555 yes P(3) C(22) H(43) 110.6(8) 1_555 1_555 1_555 no P(3) C(22) H(44) 110.5(8) 1_555 1_555 1_555 no C(23) C(22) H(43) 110.5(10) 1_555 1_555 1_555 no C(23) C(22) H(44) 109.4(9) 1_555 1_555 1_555 no H(43) C(22) H(44) 107.2(9) 1_555 1_555 1_555 no P(4) C(23) C(22) 108.1(7) 1_555 1_555 1_555 yes P(4) C(23) H(45) 109.8(8) 1_555 1_555 1_555 no P(4) C(23) H(46) 110.6(8) 1_555 1_555 1_555 no C(22) C(23) H(45) 111.3(9) 1_555 1_555 1_555 no C(22) C(23) H(46) 111.0(10) 1_555 1_555 1_555 no H(45) C(23) H(46) 106.1(9) 1_555 1_555 1_555 no P(4) C(24) C(25) 115.5(8) 1_555 1_555 1_555 yes P(4) C(24) H(47) 109.9(9) 1_555 1_555 1_555 no P(4) C(24) H(48) 109.3(8) 1_555 1_555 1_555 no C(25) C(24) H(47) 108.2(10) 1_555 1_555 1_555 no C(25) C(24) H(48) 107(1) 1_555 1_555 1_555 no H(47) C(24) H(48) 105.5(10) 1_555 1_555 1_555 no C(24) C(25) H(49) 110(1) 1_555 1_555 1_555 no C(24) C(25) H(50) 110(1) 1_555 1_555 1_555 no C(24) C(25) H(51) 113(1) 1_555 1_555 1_555 no H(49) C(25) H(50) 106(1) 1_555 1_555 1_555 no H(49) C(25) H(51) 107(1) 1_555 1_555 1_555 no H(50) C(25) H(51) 108(1) 1_555 1_555 1_555 no C(27) C(26) H(52) 110(1) 1_555 1_555 1_555 no C(27) C(26) H(53) 112(1) 1_555 1_555 1_555 no C(27) C(26) H(54) 110(1) 1_555 1_555 1_555 no H(52) C(26) H(53) 107(1) 1_555 1_555 1_555 no H(52) C(26) H(54) 107(1) 1_555 1_555 1_555 no H(53) C(26) H(54) 108(1) 1_555 1_555 1_555 no P(4) C(27) C(26) 113.8(8) 1_555 1_555 1_555 yes P(4) C(27) H(55) 109.8(8) 1_555 1_555 1_555 no P(4) C(27) H(56) 109.6(8) 1_555 1_555 1_555 no C(26) C(27) H(55) 108(1) 1_555 1_555 1_555 no C(26) C(27) H(56) 108.3(9) 1_555 1_555 1_555 no H(55) C(27) H(56) 106.3(10) 1_555 1_555 1_555 no C(29) C(28) C(33) 115(1) 1_555 1_555 1_555 yes C(29) C(28) B 123.0(10) 1_555 1_555 1_555 yes C(33) C(28) B 120.9(10) 1_555 1_555 1_555 yes C(28) C(29) C(30) 121(1) 1_555 1_555 1_555 yes C(28) C(29) H(57) 117(1) 1_555 1_555 1_555 no C(30) C(29) H(57) 120(1) 1_555 1_555 1_555 no C(29) C(30) C(31) 119(1) 1_555 1_555 1_555 yes C(29) C(30) H(58) 121(1) 1_555 1_555 1_555 no C(31) C(30) H(58) 119(1) 1_555 1_555 1_555 no C(30) C(31) C(32) 119(1) 1_555 1_555 1_555 yes C(30) C(31) H(59) 119(1) 1_555 1_555 1_555 no C(32) C(31) H(59) 120(1) 1_555 1_555 1_555 no C(31) C(32) C(33) 120(1) 1_555 1_555 1_555 yes C(31) C(32) H(60) 117(1) 1_555 1_555 1_555 no C(33) C(32) H(60) 121(1) 1_555 1_555 1_555 no C(28) C(33) C(32) 122(1) 1_555 1_555 1_555 yes C(28) C(33) H(61) 117(1) 1_555 1_555 1_555 no C(32) C(33) H(61) 119(1) 1_555 1_555 1_555 no C(35) C(34) C(39) 114.8(9) 1_555 1_555 1_555 yes C(35) C(34) B 122.2(9) 1_555 1_555 1_555 yes C(39) C(34) B 123.0(9) 1_555 1_555 1_555 yes C(34) C(35) C(36) 120(1) 1_555 1_555 1_555 yes C(34) C(35) H(62) 119(1) 1_555 1_555 1_555 no C(36) C(35) H(62) 119(1) 1_555 1_555 1_555 no C(35) C(36) C(37) 121(1) 1_555 1_555 1_555 yes C(35) C(36) H(63) 119(1) 1_555 1_555 1_555 no C(37) C(36) H(63) 118(1) 1_555 1_555 1_555 no C(36) C(37) C(38) 119(1) 1_555 1_555 1_555 yes C(36) C(37) H(64) 117(1) 1_555 1_555 1_555 no C(38) C(37) H(64) 123(1) 1_555 1_555 1_555 no C(37) C(38) C(39) 118(1) 1_555 1_555 1_555 yes C(37) C(38) H(65) 118(1) 1_555 1_555 1_555 no C(39) C(38) H(65) 122(1) 1_555 1_555 1_555 no C(34) C(39) C(38) 124(1) 1_555 1_555 1_555 yes C(34) C(39) H(66) 116(1) 1_555 1_555 1_555 no C(38) C(39) H(66) 118(1) 1_555 1_555 1_555 no C(41) C(40) C(45) 115.0(9) 1_555 1_555 1_555 yes C(41) C(40) B 123.9(9) 1_555 1_555 1_555 yes C(45) C(40) B 121.2(9) 1_555 1_555 1_555 yes C(40) C(41) C(42) 123.0(9) 1_555 1_555 1_555 yes C(40) C(41) H(67) 119.4(9) 1_555 1_555 1_555 no C(42) C(41) H(67) 117.5(10) 1_555 1_555 1_555 no C(41) C(42) C(43) 120.0(10) 1_555 1_555 1_555 yes C(41) C(42) H(68) 120(1) 1_555 1_555 1_555 no C(43) C(42) H(68) 119(1) 1_555 1_555 1_555 no C(42) C(43) C(44) 118.2(10) 1_555 1_555 1_555 yes C(42) C(43) H(69) 119(1) 1_555 1_555 1_555 no C(44) C(43) H(69) 122(1) 1_555 1_555 1_555 no C(43) C(44) C(45) 120(1) 1_555 1_555 1_555 yes C(43) C(44) H(70) 117(1) 1_555 1_555 1_555 no C(45) C(44) H(70) 121(1) 1_555 1_555 1_555 no C(40) C(45) C(44) 123.0(10) 1_555 1_555 1_555 yes C(40) C(45) H(71) 118(1) 1_555 1_555 1_555 no C(44) C(45) H(71) 117(1) 1_555 1_555 1_555 no C(47) C(46) C(51) 113.8(9) 1_555 1_555 1_555 yes C(47) C(46) B 122.7(9) 1_555 1_555 1_555 yes C(51) C(46) B 123.3(9) 1_555 1_555 1_555 yes C(46) C(47) C(48) 123(1) 1_555 1_555 1_555 yes C(46) C(47) H(72) 118.1(9) 1_555 1_555 1_555 no C(48) C(47) H(72) 118(1) 1_555 1_555 1_555 no C(47) C(48) C(49) 119(1) 1_555 1_555 1_555 yes C(47) C(48) H(73) 120(1) 1_555 1_555 1_555 no C(49) C(48) H(73) 119(1) 1_555 1_555 1_555 no C(48) C(49) C(50) 119(1) 1_555 1_555 1_555 yes C(48) C(49) H(74) 118(1) 1_555 1_555 1_555 no C(50) C(49) H(74) 121(1) 1_555 1_555 1_555 no C(49) C(50) C(51) 119(1) 1_555 1_555 1_555 yes C(49) C(50) H(75) 119(1) 1_555 1_555 1_555 no C(51) C(50) H(75) 121(1) 1_555 1_555 1_555 no C(46) C(51) C(50) 123(1) 1_555 1_555 1_555 yes C(46) C(51) H(76) 117(1) 1_555 1_555 1_555 no C(50) C(51) H(76) 118(1) 1_555 1_555 1_555 no C(28) B C(34) 108.6(8) 1_555 1_555 1_555 yes C(28) B C(40) 111.7(8) 1_555 1_555 1_555 yes C(28) B C(46) 107.7(8) 1_555 1_555 1_555 yes C(34) B C(40) 109.1(8) 1_555 1_555 1_555 yes C(34) B C(46) 110.1(8) 1_555 1_555 1_555 yes C(40) B C(46) 109.7(8) 1_555 1_555 1_555 yes #====================END