# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Masayoshi Onishi' _publ_contact_author_email ONISHI@NAGASAKI-U.AC.JP _publ_section_title ; Vinylidene rutheniums with an electrostructurally flexible NO ligand and their ruthenacyclobutene formation ; loop_ _publ_author_name 'Masayoshi Onishi' 'Yasuhiro Arikawa' 'Yoshimasa Nishimura' 'Keisuke Umakoshi' 'Mamoru Yamaguchi' # Attachment '710364.cif' data_0459 _database_code_depnum_ccdc_archive 'CCDC 710364' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C47 H42 Cl5 N O P2 Ru ' _chemical_formula_moiety 'C45 H38 Cl N O P2 Ru, C2 H4 Cl4 ' _chemical_formula_weight 977.14 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/m 1' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z -x,-y,-z x,1/2-y,z _cell_length_a 9.523(3) _cell_length_b 22.815(7) _cell_length_c 10.988(2) _cell_angle_alpha 90 _cell_angle_beta 103.112(4) _cell_angle_gamma 90 _cell_volume 2324.9(11) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4004 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.1 _cell_measurement_temperature 298(1) #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.060 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.723 _exptl_absorpt_correction_T_max 0.957 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method ? _diffrn_ambient_temperature 298(1) _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19792 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9679 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9679 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). Each asymmetric unit contains a half molecule and one CH2Cl2 solvent molecule, and one of the chloride atom of the solvent molecule is disordered with occupancy factors of 0.5 / 0.5. Hydrogen atoms of CH2Cl2 solvent molecules were not located. ; _reflns_number_total 5302 _reflns_number_gt 2441 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1348 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.1910 _refine_ls_wR_factor_gt 0.1711 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5301 _refine_ls_number_parameters 266 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[?^2^(Fo^2^) + (0.02000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 1.16 _refine_diff_density_min -1.19 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;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) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Ru 0.87182(8) 0.2500 0.02940(7) 0.0467(2) Uani 1.00 d S . . Cl(1) Cl 1.0349(3) 0.2500 0.2382(2) 0.0713(7) Uani 1.00 d S . . Cl(2) Cl 1.1870(6) 0.1603(2) -0.3662(5) 0.247(2) Uiso 1.00 d . . . Cl(3a) Cl 1.1366(9) 0.0743(4) -0.5220(8) 0.199(3) Uiso 0.50 d P . . Cl(3b) Cl 1.2753(8) 0.0914(3) -0.5528(7) 0.162(2) Uiso 0.50 d P . . P P 0.9030(2) 0.14641(6) 0.0210(1) 0.0457(4) Uani 1.00 d . . . O O 0.5677(8) 0.2500 -0.0229(8) 0.095(3) Uani 1.00 d S . . N N 0.6804(8) 0.2500 0.0353(7) 0.054(2) Uani 1.00 d S . . C(1) C 0.8829(9) 0.2500 -0.1325(8) 0.050(2) Uani 1.00 d S . . C(2) C 0.895(1) 0.2500 -0.2488(8) 0.060(2) Uani 1.00 d S . . C(3) C 0.778(1) 0.2500 -0.3607(8) 0.058(2) Uani 1.00 d S . . C(4) C 0.635(1) 0.2500 -0.3537(10) 0.079(3) Uani 1.00 d S . . C(5) C 0.525(1) 0.2500 -0.463(1) 0.096(4) Uani 1.00 d S . . C(6) C 0.553(1) 0.2500 -0.581(1) 0.097(3) Uani 1.00 d S . . C(7) C 0.696(1) 0.2500 -0.5856(10) 0.087(3) Uani 1.00 d S . . C(8) C 0.803(1) 0.2500 -0.4784(10) 0.082(3) Uani 1.00 d S . . C(9) C 0.437(2) 0.2500 -0.698(1) 0.139(6) Uani 1.00 d S . . C(10) C 0.8156(6) 0.1133(2) -0.1265(5) 0.049(1) Uani 1.00 d . . . C(11) C 0.6685(7) 0.1181(3) -0.1654(7) 0.073(2) Uani 1.00 d . . . C(12) C 0.5931(8) 0.0948(3) -0.2788(7) 0.077(2) Uani 1.00 d . . . C(13) C 0.6659(10) 0.0677(3) -0.3535(7) 0.085(2) Uani 1.00 d . . . C(14) C 0.8088(10) 0.0648(4) -0.3225(7) 0.091(2) Uani 1.00 d . . . C(15) C 0.8888(8) 0.0861(3) -0.2053(6) 0.070(2) Uani 1.00 d . . . C(16) C 1.0919(6) 0.1266(2) 0.0444(6) 0.054(2) Uani 1.00 d . . . C(17) C 1.1777(7) 0.1583(3) -0.0182(8) 0.082(2) Uani 1.00 d . . . C(18) C 1.3223(8) 0.1452(3) -0.0067(9) 0.095(3) Uani 1.00 d . . . C(19) C 1.3821(8) 0.1003(4) 0.0716(8) 0.087(3) Uani 1.00 d . . . C(20) C 1.2987(8) 0.0685(3) 0.1348(8) 0.094(3) Uani 1.00 d . . . C(21) C 1.1566(7) 0.0820(3) 0.1218(7) 0.073(2) Uani 1.00 d . . . C(22) C 0.8313(6) 0.1027(2) 0.1330(5) 0.051(2) Uani 1.00 d . . . C(23) C 0.8030(7) 0.0438(3) 0.1143(6) 0.065(2) Uani 1.00 d . . . C(24) C 0.7498(8) 0.0115(3) 0.1995(7) 0.077(2) Uani 1.00 d . . . C(25) C 0.7198(9) 0.0378(3) 0.3018(7) 0.084(2) Uani 1.00 d . . . C(26) C 0.7453(9) 0.0967(3) 0.3222(6) 0.085(2) Uani 1.00 d . . . C(27) C 0.8026(8) 0.1283(3) 0.2373(6) 0.068(2) Uani 1.00 d . . . C(28) C 1.164(2) 0.1508(3) -0.530(2) 0.266(8) Uiso 1.00 d . . . H(1) H 0.9927 0.2500 -0.2621 0.0720 Uiso 1.00 calc S . . H(2) H 0.6104 0.2500 -0.2727 0.0942 Uiso 1.00 calc S . . H(3) H 0.4253 0.2500 -0.4560 0.1157 Uiso 1.00 calc S . . H(4) H 0.7213 0.2500 -0.6661 0.1047 Uiso 1.00 calc S . . H(5) H 0.9022 0.2500 -0.4867 0.0988 Uiso 1.00 calc S . . H(6) H 0.4808 0.2500 -0.7696 0.1664 Uiso 1.00 calc S . . H(7) H 0.3781 0.2153 -0.7000 0.1664 Uiso 1.00 calc . . . H(8) H 0.6154 0.1382 -0.1124 0.0874 Uiso 1.00 calc . . . H(9) H 0.4890 0.0983 -0.3034 0.0921 Uiso 1.00 calc . . . H(10) H 0.6137 0.0500 -0.4309 0.1016 Uiso 1.00 calc . . . H(11) H 0.8599 0.0477 -0.3809 0.1091 Uiso 1.00 calc . . . H(12) H 0.9927 0.0816 -0.1817 0.0844 Uiso 1.00 calc . . . H(13) H 1.1354 0.1905 -0.0716 0.0987 Uiso 1.00 calc . . . H(14) H 1.3801 0.1673 -0.0528 0.1135 Uiso 1.00 calc . . . H(15) H 1.4836 0.0909 0.0822 0.1039 Uiso 1.00 calc . . . H(16) H 1.3409 0.0365 0.1888 0.1129 Uiso 1.00 calc . . . H(17) H 1.0996 0.0597 0.1683 0.0876 Uiso 1.00 calc . . . H(18) H 0.8209 0.0249 0.0403 0.0777 Uiso 1.00 calc . . . H(19) H 0.7336 -0.0302 0.1866 0.0921 Uiso 1.00 calc . . . H(20) H 0.6803 0.0149 0.3605 0.1010 Uiso 1.00 calc . . . H(21) H 0.7235 0.1158 0.3946 0.1022 Uiso 1.00 calc . . . H(22) H 0.8230 0.1697 0.2522 0.0817 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 0.0529(4) 0.0392(3) 0.0497(4) 0.0000 0.0151(3) 0.0000 Cl(1) 0.076(2) 0.062(1) 0.068(1) 0.0000 -0.002(1) 0.0000 P 0.0502(9) 0.0376(7) 0.0510(9) 0.0001(6) 0.0149(8) 0.0020(7) O 0.059(3) 0.099(6) 0.129(7) 0.0000 0.024(4) 0.0000 N 0.058(2) 0.041(3) 0.068(5) 0.0000 0.026(3) 0.0000 C(1) 0.054(5) 0.046(4) 0.050(2) 0.0000 0.014(4) 0.0000 C(2) 0.072(6) 0.059(5) 0.051(3) 0.0000 0.020(3) 0.0000 C(3) 0.074(4) 0.044(4) 0.054(4) 0.0000 0.014(3) 0.0000 C(4) 0.079(5) 0.098(7) 0.067(6) 0.0000 0.034(4) 0.0000 C(5) 0.061(7) 0.15(1) 0.085(6) 0.0000 0.026(4) 0.0000 C(6) 0.115(7) 0.102(8) 0.065(5) 0.0000 0.003(5) 0.0000 C(7) 0.120(7) 0.091(8) 0.051(5) 0.0000 0.020(5) 0.0000 C(8) 0.096(8) 0.098(8) 0.059(4) 0.0000 0.030(4) 0.0000 C(9) 0.11(1) 0.22(2) 0.075(8) 0.0000 -0.004(6) 0.0000 C(10) 0.058(3) 0.038(3) 0.053(3) -0.003(2) 0.017(2) 0.004(2) C(11) 0.063(3) 0.074(4) 0.077(4) 0.003(4) 0.006(3) -0.021(4) C(12) 0.069(5) 0.077(5) 0.074(4) -0.009(3) -0.005(3) -0.002(3) C(13) 0.113(5) 0.083(5) 0.055(4) -0.022(5) 0.013(4) -0.015(4) C(14) 0.113(5) 0.100(6) 0.069(4) -0.020(5) 0.040(4) -0.036(4) C(15) 0.076(5) 0.073(4) 0.070(4) 0.000(4) 0.035(3) -0.019(3) C(16) 0.051(2) 0.046(3) 0.065(4) 0.003(2) 0.014(3) -0.009(2) C(17) 0.056(3) 0.072(4) 0.132(7) 0.010(3) 0.049(4) 0.038(4) C(18) 0.053(3) 0.093(6) 0.141(8) 0.004(4) 0.029(5) 0.018(4) C(19) 0.052(4) 0.102(6) 0.105(6) 0.016(4) 0.017(4) -0.006(4) C(20) 0.061(4) 0.094(6) 0.124(7) 0.026(4) 0.015(4) 0.039(5) C(21) 0.061(3) 0.070(4) 0.091(5) 0.014(3) 0.021(4) 0.026(3) C(22) 0.053(4) 0.047(2) 0.052(3) -0.001(3) 0.013(3) 0.009(2) C(23) 0.087(5) 0.048(3) 0.069(4) 0.003(3) 0.036(4) -0.001(3) C(24) 0.106(6) 0.051(4) 0.081(5) -0.009(4) 0.038(4) 0.015(3) C(25) 0.114(6) 0.078(4) 0.073(5) -0.012(4) 0.047(5) 0.026(3) C(26) 0.127(7) 0.084(4) 0.057(4) -0.025(5) 0.048(4) 0.004(4) C(27) 0.098(5) 0.057(4) 0.056(4) -0.010(3) 0.030(4) 0.000(3) #------------------------------------------------------------------------------ _computing_data_collection D*TREK _computing_cell_refinement D*TREK _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cl(1) 2.461(3) . . yes Ru P 2.387(1) . . yes Ru P 2.387(1) . 4_555 yes Ru N 1.839(8) . . yes Ru C(1) 1.803(9) . . yes Cl(2) C(28) 1.78(2) . . yes Cl(3a) Cl(3b) 1.488(12) . . yes Cl(3a) C(28) 1.770(12) . . yes Cl(3b) C(28) 1.773(16) . . yes P C(10) 1.806(6) . . yes P C(16) 1.816(6) . . yes P C(22) 1.827(6) . . yes O N 1.111(10) . . yes C(1) C(2) 1.32(1) . . yes C(2) C(3) 1.46(1) . . yes C(3) C(4) 1.381(14) . . yes C(3) C(8) 1.37(1) . . yes C(4) C(5) 1.41(2) . . yes C(5) C(6) 1.39(2) . . yes C(6) C(7) 1.36(2) . . yes C(6) C(9) 1.493(17) . . yes C(7) C(8) 1.37(2) . . yes C(10) C(11) 1.370(9) . . yes C(10) C(15) 1.378(8) . . yes C(11) C(12) 1.394(9) . . yes C(12) C(13) 1.35(1) . . yes C(13) C(14) 1.33(1) . . yes C(14) C(15) 1.425(10) . . yes C(16) C(17) 1.387(9) . . yes C(16) C(21) 1.373(9) . . yes C(17) C(18) 1.382(10) . . yes C(18) C(19) 1.375(12) . . yes C(19) C(20) 1.375(11) . . yes C(20) C(21) 1.363(10) . . yes C(22) C(23) 1.375(8) . . yes C(22) C(27) 1.374(8) . . yes C(23) C(24) 1.385(9) . . yes C(24) C(25) 1.356(10) . . yes C(25) C(26) 1.37(1) . . yes C(26) C(27) 1.385(10) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ru P 88.78(4) . . . yes Cl(1) Ru P 88.78(4) . . 4_555 yes Cl(1) Ru N 112.6(3) . . . yes Cl(1) Ru C(1) 138.7(3) . . . yes P Ru P 164.04(8) . . 4_555 yes P Ru N 97.75(4) . . . yes P Ru C(1) 85.73(5) . . . yes P Ru N 97.75(4) 4_555 . . yes P Ru C(1) 85.73(5) 4_555 . . yes N Ru C(1) 108.6(4) . . . yes Cl(3b) Cl(3a) C(28) 65.3(8) . . . yes Cl(3a) Cl(3b) C(28) 65.1(7) . . . yes Ru P C(10) 114.2(2) . . . yes Ru P C(16) 111.7(2) . . . yes Ru P C(22) 116.5(2) . . . yes C(10) P C(16) 105.3(3) . . . yes C(10) P C(22) 102.1(3) . . . yes C(16) P C(22) 106.0(3) . . . yes Ru N O 144.3(8) . . . yes Ru C(1) C(2) 178.3(8) . . . yes C(1) C(2) C(3) 126.4(9) . . . yes C(2) C(3) C(4) 122.6(9) . . . yes C(2) C(3) C(8) 121.5(9) . . . yes C(4) C(3) C(8) 115.9(10) . . . yes C(3) C(4) C(5) 121.1(10) . . . yes C(4) C(5) C(6) 122(1) . . . yes C(5) C(6) C(7) 116(1) . . . yes C(5) C(6) C(9) 123.1(10) . . . yes C(7) C(6) C(9) 122(1) . . . yes C(6) C(7) C(8) 122(1) . . . yes C(3) C(8) C(7) 123.9(9) . . . yes P C(10) C(11) 118.6(5) . . . yes P C(10) C(15) 123.9(5) . . . yes C(11) C(10) C(15) 117.4(6) . . . yes C(10) C(11) C(12) 122.5(7) . . . yes C(11) C(12) C(13) 119.0(7) . . . yes C(12) C(13) C(14) 120.3(7) . . . yes C(13) C(14) C(15) 121.9(7) . . . yes C(10) C(15) C(14) 118.8(7) . . . yes P C(16) C(17) 118.7(5) . . . yes P C(16) C(21) 124.2(5) . . . yes C(17) C(16) C(21) 117.0(6) . . . yes C(16) C(17) C(18) 121.7(7) . . . yes C(17) C(18) C(19) 118.6(7) . . . yes C(18) C(19) C(20) 120.1(7) . . . yes C(19) C(20) C(21) 120.4(7) . . . yes C(16) C(21) C(20) 121.3(7) . . . yes P C(22) C(23) 121.5(5) . . . yes P C(22) C(27) 120.1(4) . . . yes C(23) C(22) C(27) 118.3(5) . . . yes C(22) C(23) C(24) 120.7(6) . . . yes C(23) C(24) C(25) 120.4(6) . . . yes C(24) C(25) C(26) 120.4(6) . . . yes C(25) C(26) C(27) 118.9(7) . . . yes C(22) C(27) C(26) 121.3(6) . . . yes Cl(2) C(28) Cl(3a) 93.2(9) . . . yes Cl(2) C(28) Cl(3b) 107.2(10) . . . yes Cl(3a) C(28) Cl(3b) 49.7(4) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru P C(10) C(11) -61.3(5) . . . . yes Ru P C(10) C(15) 115.9(5) . . . . yes Ru P C(16) C(17) -44.9(6) . . . . yes Ru P C(16) C(21) 134.7(6) . . . . yes Ru P C(22) C(23) 160.2(5) . . . . yes Ru P C(22) C(27) -18.6(6) . . . . yes Ru P C(16) C(17) 44.9(6) . 4_555 4_555 4_555 yes Ru P C(16) C(21) -134.7(6) . 4_555 4_555 4_555 yes Ru C(1) C(2) C(3) 180.0000(1) . . . . yes Cl(1) Ru P C(10) -175.4(2) . . . . yes Cl(1) Ru P C(16) -56.0(2) . . . . yes Cl(1) Ru P C(22) 65.9(2) . . . . yes Cl(1) Ru P C(10) 175.4(2) . . 4_555 4_555 yes Cl(1) Ru P C(16) 56.0(2) . . 4_555 4_555 yes Cl(1) Ru P C(22) -65.9(2) . . 4_555 4_555 yes Cl(1) Ru N O 180.0000(1) . . . . yes Cl(1) Ru C(1) C(2) 0.0 . . . . yes Cl(2) C(28) Cl(3a) Cl(3b) -110.0(9) . . . . yes Cl(2) C(28) Cl(3b) Cl(3a) 79.2(8) . . . . yes P Ru P C(10) 94.1(4) . . 4_555 4_555 yes P Ru P C(16) -25.2(4) . . 4_555 4_555 yes P Ru P C(22) -147.2(3) . . 4_555 4_555 yes P Ru N O -88.09(6) . . . . yes P Ru C(1) C(2) -83.25(4) . . . . yes P C(10) C(11) C(12) 178.9(6) . . . . yes P C(10) C(15) C(14) -176.7(6) . . . . yes P C(16) C(17) C(18) -179.2(7) . . . . yes P C(16) C(21) C(20) 179.3(7) . . . . yes P C(22) C(23) C(24) -179.9(6) . . . . yes P C(22) C(27) C(26) 178.2(6) . . . . yes O N Ru C(1) 0.0000(1) . . . . yes N Ru P C(10) 71.9(3) . . . . yes N Ru P C(16) -168.7(3) . . . . yes N Ru P C(22) -46.8(3) . . . . yes N Ru P C(10) -71.9(3) . . 4_555 4_555 yes N Ru P C(16) 168.7(3) . . 4_555 4_555 yes N Ru P C(22) 46.8(3) . . 4_555 4_555 yes N Ru C(1) C(2) 180.0 . . . . yes C(1) Ru P C(10) -36.3(3) . . . . yes C(1) Ru P C(16) 83.0(3) . . . . yes C(1) Ru P C(22) -155.0(3) . . . . yes C(1) Ru P C(10) 36.3(3) . . 4_555 4_555 yes C(1) Ru P C(16) -83.0(3) . . 4_555 4_555 yes C(1) Ru P C(22) 155.0(3) . . 4_555 4_555 yes C(1) C(2) C(3) C(4) 0.0000(2) . . . . yes C(1) C(2) C(3) C(8) 180.0 . . . . yes C(2) C(3) C(4) C(5) 180.0000(2) . . . . yes C(2) C(3) C(8) C(7) 180.0000(2) . . . . yes C(3) C(4) C(5) C(6) 0.0 . . . . yes C(3) C(8) C(7) C(6) 0.0000(3) . . . . yes C(4) C(3) C(8) C(7) 0.0000(1) . . . . yes C(4) C(5) C(6) C(7) 0.0 . . . . yes C(4) C(5) C(6) C(9) 180.0000(1) . . . . yes C(5) C(4) C(3) C(8) 0.0000(2) . . . . yes C(5) C(6) C(7) C(8) 0.0 . . . . yes C(8) C(7) C(6) C(9) 180.0000(4) . . . . yes C(10) P C(16) C(17) 79.5(6) . . . . yes C(10) P C(16) C(21) -100.9(6) . . . . yes C(10) P C(22) C(23) 35.1(6) . . . . yes C(10) P C(22) C(27) -143.7(6) . . . . yes C(10) C(11) C(12) C(13) 0(1) . . . . yes C(10) C(15) C(14) C(13) -3(1) . . . . yes C(11) C(10) P C(16) 175.9(5) . . . . yes C(11) C(10) P C(22) 65.4(6) . . . . yes C(11) C(10) C(15) C(14) 0.5(10) . . . . yes C(11) C(12) C(13) C(14) -2.5(11) . . . . yes C(12) C(11) C(10) C(15) 2.1(9) . . . . yes C(12) C(13) C(14) C(15) 5.0(12) . . . . yes C(15) C(10) P C(16) -7.0(6) . . . . yes C(15) C(10) P C(22) -117.5(6) . . . . yes C(16) P C(22) C(23) -74.9(6) . . . . yes C(16) P C(22) C(27) 106.3(6) . . . . yes C(16) C(17) C(18) C(19) -1(1) . . . . yes C(16) C(21) C(20) C(19) 1(1) . . . . yes C(17) C(16) P C(22) -172.8(6) . . . . yes C(17) C(16) C(21) C(20) -1(1) . . . . yes C(17) C(18) C(19) C(20) 1(1) . . . . yes C(18) C(17) C(16) C(21) 1(1) . . . . yes C(18) C(19) C(20) C(21) -1(1) . . . . yes C(21) C(16) P C(22) 6.8(7) . . . . yes C(22) C(23) C(24) C(25) 2.2(11) . . . . yes C(22) C(27) C(26) C(25) 1(1) . . . . yes C(23) C(22) C(27) C(26) 0(1) . . . . yes C(23) C(24) C(25) C(26) -1.4(12) . . . . yes C(24) C(23) C(22) C(27) -1(1) . . . . yes C(24) C(25) C(26) C(27) 0(1) . . . . yes C(24) C(25) C(26) C(27) 0(1) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(3a) C(25) 3.573(12) . 3_755 ? Cl(3b) C(21) 3.50(1) . 1_554 ? Cl(3b) C(20) 3.52(1) . 1_554 ? O C(18) 3.376(9) . 1_455 ? O C(18) 3.376(9) . 4_455 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ # Attachment '710365.cif' data_0530 _database_code_depnum_ccdc_archive 'CCDC 710365' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C56 H56 Cl3 N O3 P2 Ru ' _chemical_formula_moiety 'C55 H54 Cl N O3 P2 Ru, C H2 Cl2' _chemical_formula_weight 1060.44 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.957(1) _cell_length_b 15.466(1) _cell_length_c 17.537(2) _cell_angle_alpha 78.638(2) _cell_angle_beta 71.9489(9) _cell_angle_gamma 71.3085(8) _cell_volume 2660.7(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9630 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.1 _cell_measurement_temperature 296(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour amber _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.030 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_T_max 0.984 _exptl_special_details ; Low data completeness is due to low quality of the crystal. ; #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method \w _diffrn_ambient_temperature 296(1) _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23134 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9304 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9304 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). Hydrogen atoms of CH2Cl2 solvent molecules were not located. Because of low quality of the crystal, some crystal solvent cannot be located. ; _reflns_number_total 11356 _reflns_number_gt 6974 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1164 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 11314 _refine_ls_number_parameters 595 _refine_ls_goodness_of_fit_ref 1.397 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.02000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0004 _refine_diff_density_max 1.46 _refine_diff_density_min -1.13 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;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) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Ru 0.14823(3) 0.29508(2) 0.23464(2) 0.03892(9) Uani 1.00 d . . . Cl(1) Cl -0.07181(10) 0.37676(6) 0.21146(6) 0.0457(3) Uani 1.00 d . . . Cl(2) Cl -0.4602(6) 0.6497(4) 0.2138(5) 0.382(4) Uani 1.00 d . . . Cl(3) Cl -0.2209(7) 0.6197(4) 0.0986(4) 0.318(3) Uani 1.00 d . . . P(1) P 0.11093(10) 0.15285(6) 0.22230(6) 0.0382(3) Uani 1.00 d . . . P(2) P 0.16319(10) 0.44230(6) 0.25222(6) 0.0364(3) Uani 1.00 d . . . O(1) O 0.3675(4) 0.2796(3) 0.0867(2) 0.091(1) Uani 1.00 d . . . O(2) O 0.4754(4) 0.1309(3) 0.3442(3) 0.101(1) Uani 1.00 d . . . O(3) O 0.4885(3) 0.1765(2) 0.2131(2) 0.070(1) Uani 1.00 d . . . N N 0.2711(3) 0.2908(2) 0.1399(2) 0.049(1) Uani 1.00 d . . . C(1) C 0.6293(5) 0.1277(4) 0.1940(5) 0.109(2) Uani 1.00 d . . . C(2) C 0.4225(5) 0.1716(3) 0.2906(4) 0.065(2) Uani 1.00 d . . . C(3) C 0.2787(4) 0.2221(3) 0.3048(3) 0.046(1) Uani 1.00 d . . . C(4) C 0.1932(4) 0.2247(3) 0.3774(3) 0.051(1) Uani 1.00 d . . . C(5) C 0.0665(4) 0.2743(2) 0.3608(2) 0.041(1) Uani 1.00 d . . . C(6) C -0.0561(4) 0.2926(3) 0.4086(3) 0.047(1) Uani 1.00 d . . . C(7) C -0.0981(4) 0.2702(3) 0.4981(3) 0.047(1) Uani 1.00 d . . . C(8) C -0.2160(5) 0.2460(3) 0.5347(3) 0.056(1) Uani 1.00 d . . . C(9) C -0.2538(5) 0.2236(3) 0.6167(3) 0.066(2) Uani 1.00 d . . . C(10) C -0.1767(6) 0.2236(3) 0.6658(3) 0.065(2) Uani 1.00 d . . . C(11) C -0.0626(5) 0.2495(3) 0.6298(3) 0.064(2) Uani 1.00 d . . . C(12) C -0.0226(5) 0.2727(3) 0.5472(3) 0.058(1) Uani 1.00 d . . . C(13) C -0.2202(8) 0.1988(5) 0.7559(3) 0.106(2) Uani 1.00 d . . . C(14) C -0.0134(4) 0.1115(2) 0.3043(2) 0.040(1) Uani 1.00 d . . . C(15) C -0.1455(4) 0.1648(3) 0.3173(3) 0.048(1) Uani 1.00 d . . . C(16) C -0.2456(4) 0.1384(3) 0.3770(3) 0.056(1) Uani 1.00 d . . . C(17) C -0.2192(5) 0.0589(3) 0.4277(3) 0.063(2) Uani 1.00 d . . . C(18) C -0.0879(6) 0.0045(4) 0.4155(3) 0.080(2) Uani 1.00 d . . . C(19) C 0.0137(5) 0.0307(3) 0.3544(3) 0.063(1) Uani 1.00 d . . . C(20) C -0.3313(6) 0.0328(5) 0.4948(4) 0.110(2) Uani 1.00 d . . . C(21) C 0.2638(4) 0.0589(3) 0.2044(3) 0.051(1) Uani 1.00 d . . . C(22) C 0.3281(5) 0.0179(3) 0.2646(3) 0.062(1) Uani 1.00 d . . . C(23) C 0.4521(5) -0.0468(3) 0.2483(4) 0.084(2) Uani 1.00 d . . . C(24) C 0.5143(6) -0.0729(4) 0.1732(5) 0.105(2) Uani 1.00 d . . . C(25) C 0.4499(7) -0.0351(4) 0.1139(4) 0.118(2) Uani 1.00 d . . . C(26) C 0.3251(5) 0.0309(4) 0.1293(3) 0.084(2) Uani 1.00 d . . . C(27) C 0.6533(8) -0.1388(6) 0.1558(6) 0.178(4) Uani 1.00 d . . . C(28) C 0.0495(4) 0.1594(3) 0.1349(3) 0.047(1) Uani 1.00 d . . . C(29) C -0.0088(5) 0.0946(3) 0.1297(3) 0.062(2) Uani 1.00 d . . . C(30) C -0.0493(5) 0.0957(4) 0.0627(4) 0.075(2) Uani 1.00 d . . . C(31) C -0.0322(6) 0.1616(4) -0.0023(4) 0.083(2) Uani 1.00 d . . . C(32) C 0.0270(6) 0.2266(4) 0.0023(3) 0.078(2) Uani 1.00 d . . . C(33) C 0.0668(5) 0.2261(3) 0.0697(3) 0.059(1) Uani 1.00 d . . . C(34) C -0.0782(9) 0.1673(5) -0.0771(5) 0.139(3) Uani 1.00 d . . . C(35) C 0.2865(4) 0.4465(2) 0.2997(2) 0.038(1) Uani 1.00 d . . . C(36) C 0.2652(4) 0.5132(3) 0.3487(3) 0.049(1) Uani 1.00 d . . . C(37) C 0.3664(4) 0.5190(3) 0.3771(3) 0.057(1) Uani 1.00 d . . . C(38) C 0.4923(4) 0.4591(3) 0.3575(3) 0.053(1) Uani 1.00 d . . . C(39) C 0.5149(4) 0.3931(3) 0.3081(3) 0.052(1) Uani 1.00 d . . . C(40) C 0.4139(4) 0.3865(3) 0.2798(3) 0.047(1) Uani 1.00 d . . . C(41) C 0.6035(5) 0.4658(4) 0.3873(4) 0.083(2) Uani 1.00 d . . . C(42) C 0.2112(4) 0.5051(3) 0.1527(2) 0.044(1) Uani 1.00 d . . . C(43) C 0.3083(5) 0.5516(3) 0.1342(3) 0.058(1) Uani 1.00 d . . . C(44) C 0.3466(5) 0.5954(3) 0.0573(3) 0.071(2) Uani 1.00 d . . . C(45) C 0.2870(5) 0.5970(3) -0.0018(3) 0.061(1) Uani 1.00 d . . . C(46) C 0.1896(5) 0.5521(3) 0.0169(3) 0.058(1) Uani 1.00 d . . . C(47) C 0.1529(4) 0.5051(3) 0.0924(3) 0.052(1) Uani 1.00 d . . . C(48) C 0.3287(6) 0.6441(4) -0.0858(3) 0.094(2) Uani 1.00 d . . . C(49) C 0.0086(4) 0.5203(3) 0.3054(2) 0.041(1) Uani 1.00 d . . . C(50) C -0.0626(4) 0.5974(3) 0.2659(3) 0.056(1) Uani 1.00 d . . . C(51) C -0.1779(5) 0.6556(3) 0.3100(4) 0.074(2) Uani 1.00 d . . . C(52) C -0.2242(5) 0.6401(3) 0.3916(3) 0.065(2) Uani 1.00 d . . . C(53) C -0.1537(5) 0.5643(3) 0.4301(3) 0.060(1) Uani 1.00 d . . . C(54) C -0.0397(4) 0.5041(3) 0.3883(3) 0.050(1) Uani 1.00 d . . . C(55) C -0.3493(6) 0.7046(5) 0.4388(5) 0.111(2) Uani 1.00 d . . . C(56) C -0.330(1) 0.5813(7) 0.1638(9) 0.227(5) Uani 1.00 d . . . H(1) H 0.6402 0.0631 0.2130 0.1307 Uiso 1.00 calc . . . H(2) H 0.6672 0.1347 0.1361 0.1307 Uiso 1.00 calc . . . H(3) H 0.6747 0.1526 0.2202 0.1307 Uiso 1.00 calc . . . H(4) H 0.2114 0.1994 0.4292 0.0612 Uiso 1.00 calc . . . H(5) H -0.1272 0.3242 0.3826 0.0560 Uiso 1.00 calc . . . H(6) H -0.2725 0.2449 0.5021 0.0668 Uiso 1.00 calc . . . H(7) H -0.3370 0.2073 0.6409 0.0792 Uiso 1.00 calc . . . H(8) H -0.0077 0.2519 0.6630 0.0764 Uiso 1.00 calc . . . H(9) H 0.0593 0.2909 0.5237 0.0700 Uiso 1.00 calc . . . H(10) H -0.2326 0.2509 0.7834 0.1276 Uiso 1.00 calc . . . H(11) H -0.3037 0.1828 0.7699 0.1276 Uiso 1.00 calc . . . H(12) H -0.1522 0.1469 0.7723 0.1276 Uiso 1.00 calc . . . H(13) H -0.1673 0.2220 0.2832 0.0570 Uiso 1.00 calc . . . H(14) H -0.3370 0.1766 0.3836 0.0673 Uiso 1.00 calc . . . H(15) H -0.0668 -0.0523 0.4501 0.0957 Uiso 1.00 calc . . . H(16) H 0.1048 -0.0081 0.3467 0.0762 Uiso 1.00 calc . . . H(17) H -0.3728 0.0803 0.5309 0.1317 Uiso 1.00 calc . . . H(18) H -0.3973 0.0261 0.4718 0.1317 Uiso 1.00 calc . . . H(19) H -0.2955 -0.0249 0.5245 0.1317 Uiso 1.00 calc . . . H(20) H 0.2857 0.0347 0.3191 0.0750 Uiso 1.00 calc . . . H(21) H 0.4950 -0.0739 0.2915 0.1006 Uiso 1.00 calc . . . H(22) H 0.4912 -0.0543 0.0601 0.1414 Uiso 1.00 calc . . . H(23) H 0.2818 0.0569 0.0860 0.1002 Uiso 1.00 calc . . . H(24) H 0.6521 -0.1961 0.1901 0.2139 Uiso 1.00 calc . . . H(25) H 0.6824 -0.1503 0.0997 0.2139 Uiso 1.00 calc . . . H(26) H 0.7146 -0.1122 0.1666 0.2139 Uiso 1.00 calc . . . H(27) H -0.0214 0.0471 0.1743 0.0742 Uiso 1.00 calc . . . H(28) H -0.0906 0.0494 0.0611 0.0906 Uiso 1.00 calc . . . H(29) H 0.0408 0.2733 -0.0428 0.0935 Uiso 1.00 calc . . . H(30) H 0.1072 0.2728 0.0717 0.0707 Uiso 1.00 calc . . . H(31) H -0.1429 0.2262 -0.0837 0.1667 Uiso 1.00 calc . . . H(32) H -0.0019 0.1611 -0.1241 0.1667 Uiso 1.00 calc . . . H(33) H -0.1189 0.1183 -0.0710 0.1667 Uiso 1.00 calc . . . H(34) H 0.1776 0.5566 0.3632 0.0583 Uiso 1.00 calc . . . H(35) H 0.3484 0.5662 0.4114 0.0688 Uiso 1.00 calc . . . H(36) H 0.6032 0.3506 0.2929 0.0620 Uiso 1.00 calc . . . H(37) H 0.4323 0.3392 0.2455 0.0559 Uiso 1.00 calc . . . H(38) H 0.6369 0.4084 0.4182 0.1000 Uiso 1.00 calc . . . H(39) H 0.6753 0.4779 0.3416 0.1000 Uiso 1.00 calc . . . H(40) H 0.5700 0.5153 0.4213 0.1000 Uiso 1.00 calc . . . H(41) H 0.3494 0.5535 0.1753 0.0691 Uiso 1.00 calc . . . H(42) H 0.4168 0.6254 0.0449 0.0849 Uiso 1.00 calc . . . H(43) H 0.1456 0.5534 -0.0237 0.0700 Uiso 1.00 calc . . . H(44) H 0.0863 0.4722 0.1034 0.0625 Uiso 1.00 calc . . . H(45) H 0.3980 0.6719 -0.0887 0.1133 Uiso 1.00 calc . . . H(46) H 0.3626 0.5994 -0.1245 0.1133 Uiso 1.00 calc . . . H(47) H 0.2521 0.6913 -0.0982 0.1133 Uiso 1.00 calc . . . H(48) H -0.0324 0.6107 0.2078 0.0666 Uiso 1.00 calc . . . H(49) H -0.2270 0.7090 0.2815 0.0884 Uiso 1.00 calc . . . H(50) H -0.1841 0.5522 0.4883 0.0720 Uiso 1.00 calc . . . H(51) H 0.0068 0.4500 0.4175 0.0603 Uiso 1.00 calc . . . H(52) H -0.3268 0.7297 0.4776 0.1331 Uiso 1.00 calc . . . H(53) H -0.3864 0.7543 0.4020 0.1331 Uiso 1.00 calc . . . H(54) H -0.4145 0.6712 0.4670 0.1331 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 0.0349(2) 0.0406(2) 0.0401(2) -0.0128(1) -0.0109(1) 0.0036(1) Cl(1) 0.0381(5) 0.0468(5) 0.0515(6) -0.0101(4) -0.0168(5) 0.0014(4) Cl(2) 0.255(6) 0.279(6) 0.56(1) -0.080(5) -0.060(7) 0.013(6) Cl(3) 0.361(7) 0.273(5) 0.341(7) -0.096(5) -0.058(6) -0.126(5) P(1) 0.0354(5) 0.0365(5) 0.0406(6) -0.0108(4) -0.0101(5) 0.0022(4) P(2) 0.0373(5) 0.0381(5) 0.0353(6) -0.0150(4) -0.0113(4) 0.0034(4) O(1) 0.053(2) 0.125(3) 0.067(2) -0.016(2) 0.013(2) -0.008(2) O(2) 0.067(2) 0.109(3) 0.128(4) -0.019(2) -0.064(3) 0.042(3) O(3) 0.039(2) 0.062(2) 0.094(3) -0.008(1) -0.008(2) 0.002(2) N 0.044(2) 0.053(2) 0.048(2) -0.016(2) -0.008(2) -0.001(2) C(1) 0.038(3) 0.084(4) 0.167(7) -0.004(3) -0.002(4) 0.010(4) C(2) 0.043(3) 0.060(3) 0.090(4) -0.023(2) -0.023(3) 0.016(3) C(3) 0.040(2) 0.043(2) 0.057(3) -0.016(2) -0.020(2) 0.009(2) C(4) 0.052(3) 0.054(2) 0.051(3) -0.017(2) -0.025(2) 0.007(2) C(5) 0.042(2) 0.044(2) 0.041(2) -0.019(2) -0.013(2) 0.003(2) C(6) 0.050(2) 0.050(2) 0.043(2) -0.018(2) -0.015(2) 0.001(2) C(7) 0.055(3) 0.047(2) 0.042(2) -0.017(2) -0.015(2) -0.002(2) C(8) 0.061(3) 0.069(3) 0.041(3) -0.028(2) -0.010(2) -0.002(2) C(9) 0.077(3) 0.080(3) 0.045(3) -0.040(3) -0.006(3) -0.002(2) C(10) 0.085(4) 0.064(3) 0.043(3) -0.023(3) -0.012(3) -0.002(2) C(11) 0.084(4) 0.070(3) 0.051(3) -0.027(3) -0.031(3) -0.007(2) C(12) 0.068(3) 0.062(3) 0.052(3) -0.027(2) -0.017(2) -0.006(2) C(13) 0.148(6) 0.137(6) 0.038(3) -0.058(5) -0.018(4) 0.001(3) C(14) 0.039(2) 0.041(2) 0.040(2) -0.016(2) -0.011(2) 0.001(2) C(15) 0.043(2) 0.047(2) 0.051(3) -0.015(2) -0.013(2) 0.003(2) C(16) 0.043(2) 0.064(3) 0.062(3) -0.024(2) -0.011(2) 0.004(2) C(17) 0.056(3) 0.074(3) 0.060(3) -0.036(2) -0.010(2) 0.010(2) C(18) 0.074(4) 0.072(3) 0.078(4) -0.031(3) -0.013(3) 0.032(3) C(19) 0.051(3) 0.055(3) 0.072(3) -0.017(2) -0.011(2) 0.017(2) C(20) 0.080(4) 0.138(5) 0.096(5) -0.059(4) -0.005(4) 0.041(4) C(21) 0.042(2) 0.040(2) 0.059(3) -0.009(2) -0.004(2) 0.002(2) C(22) 0.053(3) 0.047(2) 0.075(3) -0.015(2) -0.013(2) 0.017(2) C(23) 0.057(3) 0.054(3) 0.112(5) -0.003(2) -0.018(3) 0.025(3) C(24) 0.070(4) 0.072(4) 0.106(5) 0.023(3) 0.008(4) 0.019(3) C(25) 0.088(4) 0.102(5) 0.079(4) 0.029(4) 0.026(4) 0.011(4) C(26) 0.073(4) 0.070(3) 0.064(4) 0.010(3) 0.002(3) 0.008(3) C(27) 0.095(6) 0.142(7) 0.180(9) 0.059(5) 0.007(6) 0.025(6) C(28) 0.042(2) 0.047(2) 0.047(3) -0.002(2) -0.011(2) -0.014(2) C(29) 0.062(3) 0.070(3) 0.057(3) -0.021(2) -0.012(2) -0.019(2) C(30) 0.070(3) 0.090(4) 0.079(4) -0.018(3) -0.021(3) -0.043(3) C(31) 0.088(4) 0.082(4) 0.077(4) 0.020(3) -0.045(3) -0.042(3) C(32) 0.094(4) 0.069(3) 0.058(3) 0.012(3) -0.035(3) -0.013(3) C(33) 0.066(3) 0.058(3) 0.050(3) -0.007(2) -0.024(2) -0.005(2) C(34) 0.172(8) 0.137(6) 0.122(6) 0.032(5) -0.103(6) -0.070(5) C(35) 0.035(2) 0.041(2) 0.038(2) -0.013(2) -0.008(2) 0.000(2) C(36) 0.037(2) 0.053(2) 0.058(3) -0.009(2) -0.015(2) -0.014(2) C(37) 0.043(2) 0.071(3) 0.065(3) -0.012(2) -0.016(2) -0.026(2) C(38) 0.043(2) 0.068(3) 0.052(3) -0.017(2) -0.017(2) -0.008(2) C(39) 0.033(2) 0.055(3) 0.061(3) -0.007(2) -0.012(2) -0.003(2) C(40) 0.043(2) 0.046(2) 0.048(3) -0.014(2) -0.005(2) -0.009(2) C(41) 0.049(3) 0.122(4) 0.091(4) -0.018(3) -0.030(3) -0.031(3) C(42) 0.041(2) 0.042(2) 0.043(2) -0.013(2) -0.008(2) 0.003(2) C(43) 0.062(3) 0.062(3) 0.053(3) -0.034(2) -0.016(2) 0.014(2) C(44) 0.069(3) 0.075(3) 0.066(3) -0.042(3) -0.011(3) 0.020(3) C(45) 0.060(3) 0.055(3) 0.048(3) -0.015(2) 0.000(2) 0.012(2) C(46) 0.069(3) 0.062(3) 0.040(3) -0.021(2) -0.015(2) 0.007(2) C(47) 0.058(3) 0.056(2) 0.043(3) -0.026(2) -0.013(2) 0.008(2) C(48) 0.093(4) 0.107(4) 0.057(3) -0.035(3) 0.002(3) 0.027(3) C(49) 0.036(2) 0.047(2) 0.047(2) -0.017(2) -0.016(2) -0.001(2) C(50) 0.050(3) 0.058(3) 0.051(3) -0.002(2) -0.020(2) -0.002(2) C(51) 0.066(3) 0.061(3) 0.086(4) 0.006(2) -0.034(3) -0.009(3) C(52) 0.045(3) 0.072(3) 0.076(4) -0.009(2) -0.011(3) -0.024(3) C(53) 0.048(3) 0.076(3) 0.054(3) -0.025(2) 0.000(2) -0.014(2) C(54) 0.049(2) 0.051(2) 0.050(3) -0.018(2) -0.010(2) -0.003(2) C(55) 0.061(4) 0.117(5) 0.132(6) 0.005(3) 0.000(4) -0.054(4) C(56) 0.126(8) 0.138(8) 0.30(2) -0.026(6) 0.098(9) -0.035(9) #------------------------------------------------------------------------------ _computing_data_collection D*TREK _computing_cell_refinement D*TREK _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cl(1) 2.455(1) . . yes Ru P(1) 2.423(1) . . yes Ru P(2) 2.419(1) . . yes Ru N 1.783(4) . . yes Ru C(3) 2.084(4) . . yes Ru C(5) 2.116(4) . . yes Cl(2) C(56) 1.59(1) . . yes Cl(3) C(56) 1.56(1) . . yes P(1) C(14) 1.820(4) . . yes P(1) C(21) 1.819(4) . . yes P(1) C(28) 1.829(4) . . yes P(2) C(35) 1.816(4) . . yes P(2) C(42) 1.832(4) . . yes P(2) C(49) 1.830(4) . . yes O(1) N 1.162(4) . . yes O(2) C(2) 1.219(6) . . yes O(3) C(1) 1.448(6) . . yes O(3) C(2) 1.327(6) . . yes C(2) C(3) 1.483(6) . . yes C(3) C(4) 1.325(6) . . yes C(4) C(5) 1.442(5) . . yes C(5) C(6) 1.319(5) . . yes C(6) C(7) 1.495(6) . . yes C(7) C(8) 1.387(6) . . yes C(7) C(12) 1.380(6) . . yes C(8) C(9) 1.373(6) . . yes C(9) C(10) 1.380(7) . . yes C(10) C(11) 1.361(7) . . yes C(10) C(13) 1.512(7) . . yes C(11) C(12) 1.387(6) . . yes C(14) C(15) 1.390(5) . . yes C(14) C(19) 1.382(5) . . yes C(15) C(16) 1.368(6) . . yes C(16) C(17) 1.373(6) . . yes C(17) C(18) 1.389(7) . . yes C(17) C(20) 1.513(7) . . yes C(18) C(19) 1.390(6) . . yes C(21) C(22) 1.387(6) . . yes C(21) C(26) 1.366(7) . . yes C(22) C(23) 1.389(6) . . yes C(23) C(24) 1.356(9) . . yes C(24) C(25) 1.369(10) . . yes C(24) C(27) 1.514(8) . . yes C(25) C(26) 1.403(7) . . yes C(28) C(29) 1.380(6) . . yes C(28) C(33) 1.391(6) . . yes C(29) C(30) 1.374(7) . . yes C(30) C(31) 1.381(8) . . yes C(31) C(32) 1.385(8) . . yes C(31) C(34) 1.522(8) . . yes C(32) C(33) 1.380(7) . . yes C(35) C(36) 1.388(5) . . yes C(35) C(40) 1.388(5) . . yes C(36) C(37) 1.382(6) . . yes C(37) C(38) 1.375(6) . . yes C(38) C(39) 1.382(6) . . yes C(38) C(41) 1.505(6) . . yes C(39) C(40) 1.384(6) . . yes C(42) C(43) 1.393(6) . . yes C(42) C(47) 1.394(6) . . yes C(43) C(44) 1.387(6) . . yes C(44) C(45) 1.379(7) . . yes C(45) C(46) 1.378(7) . . yes C(45) C(48) 1.511(6) . . yes C(46) C(47) 1.386(6) . . yes C(49) C(50) 1.387(5) . . yes C(49) C(54) 1.387(6) . . yes C(50) C(51) 1.395(6) . . yes C(51) C(52) 1.363(7) . . yes C(52) C(53) 1.363(7) . . yes C(52) C(55) 1.518(7) . . yes C(53) C(54) 1.385(6) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ru P(1) 88.42(3) . . . yes Cl(1) Ru P(2) 87.04(3) . . . yes Cl(1) Ru N 108.6(1) . . . yes Cl(1) Ru C(3) 154.7(1) . . . yes Cl(1) Ru C(5) 92.5(1) . . . yes P(1) Ru P(2) 174.65(4) . . . yes P(1) Ru N 91.9(1) . . . yes P(1) Ru C(3) 89.6(1) . . . yes P(1) Ru C(5) 88.8(1) . . . yes P(2) Ru N 92.3(1) . . . yes P(2) Ru C(3) 93.3(1) . . . yes P(2) Ru C(5) 88.5(1) . . . yes N Ru C(3) 96.7(2) . . . yes N Ru C(5) 158.9(1) . . . yes C(3) Ru C(5) 62.3(2) . . . yes Ru P(1) C(14) 117.1(1) . . . yes Ru P(1) C(21) 112.9(1) . . . yes Ru P(1) C(28) 113.2(1) . . . yes C(14) P(1) C(21) 107.7(2) . . . yes C(14) P(1) C(28) 101.9(2) . . . yes C(21) P(1) C(28) 102.6(2) . . . yes Ru P(2) C(35) 119.5(1) . . . yes Ru P(2) C(42) 108.9(1) . . . yes Ru P(2) C(49) 116.3(1) . . . yes C(35) P(2) C(42) 102.3(2) . . . yes C(35) P(2) C(49) 103.6(2) . . . yes C(42) P(2) C(49) 104.5(2) . . . yes C(1) O(3) C(2) 116.2(4) . . . yes Ru N O(1) 167.4(3) . . . yes O(2) C(2) O(3) 123.4(5) . . . yes O(2) C(2) C(3) 123.9(5) . . . yes O(3) C(2) C(3) 112.8(4) . . . yes Ru C(3) C(2) 136.9(4) . . . yes Ru C(3) C(4) 99.8(3) . . . yes C(2) C(3) C(4) 123.2(4) . . . yes C(3) C(4) C(5) 103.3(4) . . . yes Ru C(5) C(4) 94.6(3) . . . yes Ru C(5) C(6) 134.0(3) . . . yes C(4) C(5) C(6) 131.2(4) . . . yes C(5) C(6) C(7) 127.5(4) . . . yes C(6) C(7) C(8) 120.5(4) . . . yes C(6) C(7) C(12) 122.0(4) . . . yes C(8) C(7) C(12) 117.5(4) . . . yes C(7) C(8) C(9) 120.7(4) . . . yes C(8) C(9) C(10) 121.9(5) . . . yes C(9) C(10) C(11) 117.2(4) . . . yes C(9) C(10) C(13) 121.0(5) . . . yes C(11) C(10) C(13) 121.7(5) . . . yes C(10) C(11) C(12) 122.0(5) . . . yes C(7) C(12) C(11) 120.6(4) . . . yes P(1) C(14) C(15) 117.6(3) . . . yes P(1) C(14) C(19) 124.9(3) . . . yes C(15) C(14) C(19) 117.5(4) . . . yes C(14) C(15) C(16) 121.5(4) . . . yes C(15) C(16) C(17) 121.3(4) . . . yes C(16) C(17) C(18) 118.1(4) . . . yes C(16) C(17) C(20) 120.2(5) . . . yes C(18) C(17) C(20) 121.7(5) . . . yes C(17) C(18) C(19) 120.7(4) . . . yes C(14) C(19) C(18) 120.9(4) . . . yes P(1) C(21) C(22) 121.5(4) . . . yes P(1) C(21) C(26) 120.9(4) . . . yes C(22) C(21) C(26) 117.4(4) . . . yes C(21) C(22) C(23) 121.2(5) . . . yes C(22) C(23) C(24) 121.4(6) . . . yes C(23) C(24) C(25) 118.0(5) . . . yes C(23) C(24) C(27) 120.3(7) . . . yes C(25) C(24) C(27) 121.7(7) . . . yes C(24) C(25) C(26) 121.3(6) . . . yes C(21) C(26) C(25) 120.7(5) . . . yes P(1) C(28) C(29) 120.7(3) . . . yes P(1) C(28) C(33) 121.4(3) . . . yes C(29) C(28) C(33) 117.8(4) . . . yes C(28) C(29) C(30) 121.4(5) . . . yes C(29) C(30) C(31) 121.1(5) . . . yes C(30) C(31) C(32) 117.8(5) . . . yes C(30) C(31) C(34) 123.1(7) . . . yes C(32) C(31) C(34) 119.0(7) . . . yes C(31) C(32) C(33) 121.3(5) . . . yes C(28) C(33) C(32) 120.6(5) . . . yes P(2) C(35) C(36) 123.4(3) . . . yes P(2) C(35) C(40) 118.9(3) . . . yes C(36) C(35) C(40) 117.3(4) . . . yes C(35) C(36) C(37) 121.4(4) . . . yes C(36) C(37) C(38) 121.1(4) . . . yes C(37) C(38) C(39) 118.0(4) . . . yes C(37) C(38) C(41) 121.5(4) . . . yes C(39) C(38) C(41) 120.5(4) . . . yes C(38) C(39) C(40) 121.2(4) . . . yes C(35) C(40) C(39) 121.1(4) . . . yes P(2) C(42) C(43) 121.7(3) . . . yes P(2) C(42) C(47) 120.1(3) . . . yes C(43) C(42) C(47) 118.2(4) . . . yes C(42) C(43) C(44) 120.4(4) . . . yes C(43) C(44) C(45) 121.4(4) . . . yes C(44) C(45) C(46) 118.1(4) . . . yes C(44) C(45) C(48) 121.7(5) . . . yes C(46) C(45) C(48) 120.2(5) . . . yes C(45) C(46) C(47) 121.6(4) . . . yes C(42) C(47) C(46) 120.2(4) . . . yes P(2) C(49) C(50) 122.3(3) . . . yes P(2) C(49) C(54) 119.9(3) . . . yes C(50) C(49) C(54) 117.7(4) . . . yes C(49) C(50) C(51) 119.7(4) . . . yes C(50) C(51) C(52) 122.4(4) . . . yes C(51) C(52) C(53) 117.6(4) . . . yes C(51) C(52) C(55) 121.7(5) . . . yes C(53) C(52) C(55) 120.7(5) . . . yes C(52) C(53) C(54) 121.7(4) . . . yes C(49) C(54) C(53) 120.8(4) . . . yes Cl(2) C(56) Cl(3) 120.1(8) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru P(1) C(14) C(15) 64.7(3) . . . . yes Ru P(1) C(14) C(19) -115.6(4) . . . . yes Ru P(1) C(21) C(22) 71.7(4) . . . . yes Ru P(1) C(21) C(26) -103.2(4) . . . . yes Ru P(1) C(28) C(29) -163.4(3) . . . . yes Ru P(1) C(28) C(33) 20.5(4) . . . . yes Ru P(2) C(35) C(36) -145.8(3) . . . . yes Ru P(2) C(35) C(40) 41.4(3) . . . . yes Ru P(2) C(42) C(43) -135.6(3) . . . . yes Ru P(2) C(42) C(47) 42.7(3) . . . . yes Ru P(2) C(49) C(50) -106.5(3) . . . . yes Ru P(2) C(49) C(54) 74.7(3) . . . . yes Ru C(3) C(2) O(2) -177.4(4) . . . . yes Ru C(3) C(2) O(3) 3.4(6) . . . . yes Ru C(3) C(4) C(5) 1.0(3) . . . . yes Ru C(5) C(4) C(3) -1.0(3) . . . . yes Ru C(5) C(6) C(7) 177.7(3) . . . . yes Cl(1) Ru P(1) C(14) -71.2(1) . . . . yes Cl(1) Ru P(1) C(21) 163.0(2) . . . . yes Cl(1) Ru P(1) C(28) 47.0(1) . . . . yes Cl(1) Ru P(2) C(35) 163.8(1) . . . . yes Cl(1) Ru P(2) C(42) -79.4(1) . . . . yes Cl(1) Ru P(2) C(49) 38.2(1) . . . . yes Cl(1) Ru N O(1) 179(1) . . . . yes Cl(1) Ru C(3) C(2) 171.5(3) . . . . yes Cl(1) Ru C(3) C(4) -4.1(5) . . . . yes Cl(1) Ru C(5) C(4) 179.2(2) . . . . yes Cl(1) Ru C(5) C(6) 3.8(4) . . . . yes P(1) Ru P(2) C(35) 131.8(4) . . . . yes P(1) Ru P(2) C(42) -111.4(5) . . . . yes P(1) Ru P(2) C(49) 6.2(5) . . . . yes P(1) Ru N O(1) -91(1) . . . . yes P(1) Ru C(3) C(2) 86.0(4) . . . . yes P(1) Ru C(3) C(4) -89.6(3) . . . . yes P(1) Ru C(5) C(4) 90.8(2) . . . . yes P(1) Ru C(5) C(6) -84.5(4) . . . . yes P(1) C(14) C(15) C(16) 179.3(4) . . . . yes P(1) C(14) C(19) C(18) -179.9(4) . . . . yes P(1) C(21) C(22) C(23) -172.9(4) . . . . yes P(1) C(21) C(26) C(25) 173.5(5) . . . . yes P(1) C(28) C(29) C(30) -176.6(4) . . . . yes P(1) C(28) C(33) C(32) 176.1(4) . . . . yes P(2) Ru P(1) C(14) -39.2(5) . . . . yes P(2) Ru P(1) C(21) -165.1(4) . . . . yes P(2) Ru P(1) C(28) 79.0(5) . . . . yes P(2) Ru N O(1) 91(1) . . . . yes P(2) Ru C(3) C(2) -98.5(4) . . . . yes P(2) Ru C(3) C(4) 85.9(3) . . . . yes P(2) Ru C(5) C(4) -93.8(2) . . . . yes P(2) Ru C(5) C(6) 90.8(4) . . . . yes P(2) C(35) C(36) C(37) -173.6(4) . . . . yes P(2) C(35) C(40) C(39) 173.5(3) . . . . yes P(2) C(42) C(43) C(44) 177.3(4) . . . . yes P(2) C(42) C(47) C(46) -179.6(3) . . . . yes P(2) C(49) C(50) C(51) -178.3(4) . . . . yes P(2) C(49) C(54) C(53) 177.5(3) . . . . yes O(1) N Ru C(3) -2(1) . . . . yes O(1) N Ru C(5) 0(1) . . . . yes O(2) C(2) O(3) C(1) 1.8(7) . . . . yes O(2) C(2) C(3) C(4) -2.5(7) . . . . yes O(3) C(2) C(3) C(4) 178.4(4) . . . . yes N Ru P(1) C(14) -179.7(2) . . . . yes N Ru P(1) C(21) 54.4(2) . . . . yes N Ru P(1) C(28) -61.5(2) . . . . yes N Ru P(2) C(35) -87.7(2) . . . . yes N Ru P(2) C(42) 29.1(2) . . . . yes N Ru P(2) C(49) 146.7(2) . . . . yes N Ru C(3) C(2) -5.8(4) . . . . yes N Ru C(3) C(4) 178.5(3) . . . . yes N Ru C(5) C(4) -1.4(5) . . . . yes N Ru C(5) C(6) -176.7(4) . . . . yes C(1) O(3) C(2) C(3) -179.0(4) . . . . yes C(2) C(3) Ru C(5) 174.9(5) . . . . yes C(2) C(3) C(4) C(5) -175.5(4) . . . . yes C(3) Ru P(1) C(14) 83.6(2) . . . . yes C(3) Ru P(1) C(21) -42.3(2) . . . . yes C(3) Ru P(1) C(28) -158.2(2) . . . . yes C(3) Ru P(2) C(35) 9.1(2) . . . . yes C(3) Ru P(2) C(42) 125.9(2) . . . . yes C(3) Ru P(2) C(49) -116.5(2) . . . . yes C(3) Ru C(5) C(4) 0.7(2) . . . . yes C(3) Ru C(5) C(6) -174.7(5) . . . . yes C(3) C(4) C(5) C(6) 174.6(4) . . . . yes C(4) C(3) Ru C(5) -0.7(3) . . . . yes C(4) C(5) C(6) C(7) 3.9(7) . . . . yes C(5) Ru P(1) C(14) 21.4(2) . . . . yes C(5) Ru P(1) C(21) -104.5(2) . . . . yes C(5) Ru P(1) C(28) 139.5(2) . . . . yes C(5) Ru P(2) C(35) 71.2(2) . . . . yes C(5) Ru P(2) C(42) -172.0(2) . . . . yes C(5) Ru P(2) C(49) -54.4(2) . . . . yes C(5) C(6) C(7) C(8) -144.6(5) . . . . yes C(5) C(6) C(7) C(12) 35.5(6) . . . . yes C(6) C(7) C(8) C(9) 178.7(4) . . . . yes C(6) C(7) C(12) C(11) -178.5(4) . . . . yes C(7) C(8) C(9) C(10) -0.4(7) . . . . yes C(7) C(12) C(11) C(10) 0.0(7) . . . . yes C(8) C(7) C(12) C(11) 1.6(6) . . . . yes C(8) C(9) C(10) C(11) 1.9(7) . . . . yes C(8) C(9) C(10) C(13) 179.9(5) . . . . yes C(9) C(8) C(7) C(12) -1.4(7) . . . . yes C(9) C(10) C(11) C(12) -1.7(7) . . . . yes C(12) C(11) C(10) C(13) -179.7(5) . . . . yes C(14) P(1) C(21) C(22) -59.1(4) . . . . yes C(14) P(1) C(21) C(26) 126.0(4) . . . . yes C(14) P(1) C(28) C(29) -36.7(4) . . . . yes C(14) P(1) C(28) C(33) 147.1(3) . . . . yes C(14) C(15) C(16) C(17) 1.3(7) . . . . yes C(14) C(19) C(18) C(17) 0.1(9) . . . . yes C(15) C(14) P(1) C(21) -166.9(3) . . . . yes C(15) C(14) P(1) C(28) -59.3(3) . . . . yes C(15) C(14) C(19) C(18) -0.3(7) . . . . yes C(15) C(16) C(17) C(18) -1.5(8) . . . . yes C(15) C(16) C(17) C(20) 178.2(5) . . . . yes C(16) C(15) C(14) C(19) -0.4(6) . . . . yes C(16) C(17) C(18) C(19) 0.8(8) . . . . yes C(19) C(14) P(1) C(21) 12.8(4) . . . . yes C(19) C(14) P(1) C(28) 120.3(4) . . . . yes C(19) C(18) C(17) C(20) -178.9(6) . . . . yes C(21) P(1) C(28) C(29) 74.7(4) . . . . yes C(21) P(1) C(28) C(33) -101.5(4) . . . . yes C(21) C(22) C(23) C(24) -0.6(8) . . . . yes C(21) C(26) C(25) C(24) 0(1) . . . . yes C(22) C(21) P(1) C(28) -166.2(4) . . . . yes C(22) C(21) C(26) C(25) -1.6(8) . . . . yes C(22) C(23) C(24) C(25) -1(1) . . . . yes C(22) C(23) C(24) C(27) 176.0(6) . . . . yes C(23) C(22) C(21) C(26) 2.2(7) . . . . yes C(23) C(24) C(25) C(26) 2(1) . . . . yes C(26) C(21) P(1) C(28) 18.9(5) . . . . yes C(26) C(25) C(24) C(27) -175.4(8) . . . . yes C(28) C(29) C(30) C(31) 0.5(8) . . . . yes C(28) C(33) C(32) C(31) 0.6(7) . . . . yes C(29) C(28) C(33) C(32) -0.2(6) . . . . yes C(29) C(30) C(31) C(32) -0.1(8) . . . . yes C(29) C(30) C(31) C(34) -178.5(5) . . . . yes C(30) C(29) C(28) C(33) -0.3(7) . . . . yes C(30) C(31) C(32) C(33) -0.5(8) . . . . yes C(33) C(32) C(31) C(34) 178.0(5) . . . . yes C(35) P(2) C(42) C(43) -8.2(4) . . . . yes C(35) P(2) C(42) C(47) 170.0(3) . . . . yes C(35) P(2) C(49) C(50) 120.3(4) . . . . yes C(35) P(2) C(49) C(54) -58.6(3) . . . . yes C(35) C(36) C(37) C(38) 0.4(7) . . . . yes C(35) C(40) C(39) C(38) 0.5(6) . . . . yes C(36) C(35) P(2) C(42) 94.0(4) . . . . yes C(36) C(35) P(2) C(49) -14.4(4) . . . . yes C(36) C(35) C(40) C(39) 0.3(6) . . . . yes C(36) C(37) C(38) C(39) 0.4(7) . . . . yes C(36) C(37) C(38) C(41) 179.2(5) . . . . yes C(37) C(36) C(35) C(40) -0.7(6) . . . . yes C(37) C(38) C(39) C(40) -0.8(7) . . . . yes C(40) C(35) P(2) C(42) -78.8(3) . . . . yes C(40) C(35) P(2) C(49) 172.8(3) . . . . yes C(40) C(39) C(38) C(41) -179.6(5) . . . . yes C(42) P(2) C(49) C(50) 13.5(4) . . . . yes C(42) P(2) C(49) C(54) -165.3(3) . . . . yes C(42) C(43) C(44) C(45) 2.4(8) . . . . yes C(42) C(47) C(46) C(45) 2.3(7) . . . . yes C(43) C(42) P(2) C(49) 99.5(4) . . . . yes C(43) C(42) C(47) C(46) -1.3(6) . . . . yes C(43) C(44) C(45) C(46) -1.4(8) . . . . yes C(43) C(44) C(45) C(48) -179.7(5) . . . . yes C(44) C(43) C(42) C(47) -1.0(7) . . . . yes C(44) C(45) C(46) C(47) -1.0(7) . . . . yes C(47) C(42) P(2) C(49) -82.2(4) . . . . yes C(47) C(46) C(45) C(48) 177.4(5) . . . . yes C(49) C(50) C(51) C(52) 0.3(8) . . . . yes C(49) C(54) C(53) C(52) 1.5(7) . . . . yes C(50) C(49) C(54) C(53) -1.4(6) . . . . yes C(50) C(51) C(52) C(53) -0.3(8) . . . . yes C(50) C(51) C(52) C(55) 179.5(5) . . . . yes C(51) C(50) C(49) C(54) 0.5(6) . . . . yes C(51) C(52) C(53) C(54) -0.6(7) . . . . yes C(54) C(53) C(52) C(55) 179.6(5) . . . . yes C(54) C(53) C(52) C(55) 179.6(5) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(2) C(13) 3.481(10) . 2_466 ? Cl(2) C(38) 3.543(8) . 1_455 ? Cl(2) C(37) 3.564(8) . 1_455 ? Cl(3) C(46) 3.520(7) . 2_565 ? Cl(3) C(32) 3.542(9) . 2_565 ? O(2) C(16) 3.322(6) . 1_655 ? C(1) C(30) 3.501(8) . 1_655 ? C(32) C(46) 3.506(6) . 2_565 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ # Attachment '710366.cif' data_0528 _database_code_depnum_ccdc_archive 'CCDC 710366' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C55 H54 Cl N O3 P2 Ru ' _chemical_formula_moiety 'C55 H54 Cl N O3 P2 Ru ' _chemical_formula_weight 975.51 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.712(2) _cell_length_b 12.742(1) _cell_length_c 15.986(2) _cell_angle_alpha 80.906(2) _cell_angle_beta 75.435(2) _cell_angle_gamma 88.018(2) _cell_volume 2474.6(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8253 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.1 _cell_measurement_temperature 296(1) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour amber _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.730 _exptl_absorpt_correction_T_max 0.909 _exptl_special_details ; Low data completeness is due to low quality of the crystal. ; #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC7' _diffrn_measurement_method \w _diffrn_ambient_temperature 296(1) _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21470 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9285 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9285 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 10553 _reflns_number_gt 6957 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0795 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 10507 _refine_ls_number_parameters 568 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.02000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0003 _refine_diff_density_max 0.97 _refine_diff_density_min -0.81 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;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) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Ru 0.21776(2) 0.06587(2) 0.21604(2) 0.02982(6) Uani 1.00 d . . . Cl Cl 0.22663(6) 0.05155(6) 0.37030(5) 0.0432(2) Uani 1.00 d . . . P(1) P 0.23119(6) -0.12598(5) 0.23625(5) 0.0310(2) Uani 1.00 d . . . P(2) P 0.22221(6) 0.25820(5) 0.19766(5) 0.0301(2) Uani 1.00 d . . . O(1) O -0.0143(2) 0.0625(2) 0.2279(2) 0.0634(8) Uani 1.00 d . . . O(2) O 0.0841(2) 0.0936(2) 0.0407(1) 0.0509(7) Uani 1.00 d . . . O(3) O 0.2357(2) 0.0654(2) -0.0598(1) 0.0559(7) Uani 1.00 d . . . N N 0.0758(2) 0.0628(2) 0.2314(2) 0.0360(7) Uani 1.00 d . . . C(1) C 0.1710(3) 0.0688(3) -0.1224(2) 0.074(1) Uani 1.00 d . . . C(2) C 0.1807(3) 0.0783(2) 0.0218(2) 0.0376(8) Uani 1.00 d . . . C(3) C 0.2511(2) 0.0732(2) 0.0813(2) 0.0317(7) Uani 1.00 d . . . C(4) C 0.3601(2) 0.0799(2) 0.0620(2) 0.0375(8) Uani 1.00 d . . . C(5) C 0.3888(2) 0.0784(2) 0.1439(2) 0.0327(8) Uani 1.00 d . . . C(6) C 0.4940(2) 0.0908(2) 0.1450(2) 0.0391(8) Uani 1.00 d . . . C(7) C 0.5487(2) 0.0891(2) 0.2152(2) 0.0383(8) Uani 1.00 d . . . C(8) C 0.5080(2) 0.0375(2) 0.2998(2) 0.0411(9) Uani 1.00 d . . . C(9) C 0.5650(3) 0.0349(2) 0.3628(2) 0.0491(10) Uani 1.00 d . . . C(10) C 0.6656(3) 0.0837(3) 0.3447(2) 0.055(1) Uani 1.00 d . . . C(11) C 0.7055(3) 0.1375(3) 0.2615(3) 0.070(1) Uani 1.00 d . . . C(12) C 0.6500(3) 0.1391(3) 0.1975(2) 0.058(1) Uani 1.00 d . . . C(13) C 0.7282(4) 0.0768(4) 0.4141(3) 0.092(2) Uani 1.00 d . . . C(14) C 0.3523(2) -0.1766(2) 0.2690(2) 0.0349(8) Uani 1.00 d . . . C(15) C 0.3494(2) -0.2057(2) 0.3561(2) 0.0331(8) Uani 1.00 d . . . C(16) C 0.4446(3) -0.2324(2) 0.3825(2) 0.055(1) Uani 1.00 d . . . C(17) C 0.5445(3) -0.2295(2) 0.3225(3) 0.057(1) Uani 1.00 d . . . C(18) C 0.5467(3) -0.2019(2) 0.2350(3) 0.055(1) Uani 1.00 d . . . C(19) C 0.4524(2) -0.1741(2) 0.2077(2) 0.0437(9) Uani 1.00 d . . . C(20) C 0.6473(3) -0.2540(3) 0.3524(3) 0.089(2) Uani 1.00 d . . . C(21) C 0.2218(2) -0.1905(2) 0.1446(2) 0.0369(8) Uani 1.00 d . . . C(22) C 0.2858(3) -0.2745(2) 0.1143(2) 0.0480(10) Uani 1.00 d . . . C(23) C 0.2617(3) -0.3255(2) 0.0519(2) 0.057(1) Uani 1.00 d . . . C(24) C 0.1750(3) -0.2967(2) 0.0163(2) 0.051(1) Uani 1.00 d . . . C(25) C 0.1120(3) -0.2124(2) 0.0454(2) 0.050(1) Uani 1.00 d . . . C(26) C 0.1352(2) -0.1609(2) 0.1082(2) 0.0436(9) Uani 1.00 d . . . C(27) C 0.1488(4) -0.3519(3) -0.0525(3) 0.080(2) Uani 1.00 d . . . C(28) C 0.1185(2) -0.1927(2) 0.3208(2) 0.0383(8) Uani 1.00 d . . . C(29) C 0.1034(3) -0.3018(2) 0.3261(2) 0.054(1) Uani 1.00 d . . . C(30) C 0.0175(3) -0.3541(3) 0.3865(3) 0.065(1) Uani 1.00 d . . . C(31) C -0.0575(3) -0.3014(3) 0.4440(2) 0.056(1) Uani 1.00 d . . . C(32) C -0.0419(3) -0.1934(3) 0.4391(2) 0.055(1) Uani 1.00 d . . . C(33) C 0.0454(3) -0.1402(2) 0.3792(2) 0.0480(10) Uani 1.00 d . . . C(34) C -0.1521(3) -0.3581(3) 0.5097(3) 0.086(2) Uani 1.00 d . . . C(35) C 0.2645(2) 0.3231(2) 0.0850(2) 0.0352(8) Uani 1.00 d . . . C(36) C 0.3686(3) 0.3639(2) 0.0506(2) 0.0453(9) Uani 1.00 d . . . C(37) C 0.4021(3) 0.4077(3) -0.0372(2) 0.058(1) Uani 1.00 d . . . C(38) C 0.3335(3) 0.4120(2) -0.0922(2) 0.056(1) Uani 1.00 d . . . C(39) C 0.2309(3) 0.3685(2) -0.0581(2) 0.054(1) Uani 1.00 d . . . C(40) C 0.1960(3) 0.3237(2) 0.0291(2) 0.0431(9) Uani 1.00 d . . . C(41) C 0.3690(4) 0.4638(3) -0.1858(3) 0.090(2) Uani 1.00 d . . . C(42) C 0.0872(2) 0.3096(2) 0.2436(2) 0.0378(8) Uani 1.00 d . . . C(43) C 0.0403(3) 0.3979(2) 0.2040(2) 0.053(1) Uani 1.00 d . . . C(44) C -0.0598(3) 0.4340(3) 0.2480(3) 0.071(1) Uani 1.00 d . . . C(45) C -0.1138(3) 0.3857(3) 0.3298(3) 0.064(1) Uani 1.00 d . . . C(46) C -0.0656(3) 0.2995(3) 0.3693(2) 0.056(1) Uani 1.00 d . . . C(47) C 0.0330(2) 0.2620(2) 0.3263(2) 0.0446(9) Uani 1.00 d . . . C(48) C -0.2245(4) 0.4238(4) 0.3761(3) 0.106(2) Uani 1.00 d . . . C(49) C 0.3032(2) 0.3251(2) 0.2534(2) 0.0341(8) Uani 1.00 d . . . C(50) C 0.2892(2) 0.4330(2) 0.2583(2) 0.0433(9) Uani 1.00 d . . . C(51) C 0.3429(3) 0.4812(2) 0.3066(2) 0.0442(9) Uani 1.00 d . . . C(52) C 0.4116(2) 0.4243(2) 0.3525(2) 0.0382(8) Uani 1.00 d . . . C(53) C 0.4278(2) 0.3183(2) 0.3442(2) 0.0437(9) Uani 1.00 d . . . C(54) C 0.3735(2) 0.2689(2) 0.2963(2) 0.0410(9) Uani 1.00 d . . . C(55) C 0.4632(3) 0.4759(2) 0.4096(2) 0.052(1) Uani 1.00 d . . . H(1) H 0.1353 0.1372 -0.1279 0.0893 Uiso 1.00 calc . . . H(2) H 0.2175 0.0587 -0.1788 0.0893 Uiso 1.00 calc . . . H(3) H 0.1166 0.0127 -0.1028 0.0893 Uiso 1.00 calc . . . H(4) H 0.4095 0.0849 0.0044 0.0450 Uiso 1.00 calc . . . H(5) H 0.5430 0.1035 0.0871 0.0470 Uiso 1.00 calc . . . H(6) H 0.4377 0.0023 0.3150 0.0493 Uiso 1.00 calc . . . H(7) H 0.5339 -0.0021 0.4213 0.0589 Uiso 1.00 calc . . . H(8) H 0.7743 0.1751 0.2476 0.0844 Uiso 1.00 calc . . . H(9) H 0.6817 0.1757 0.1390 0.0699 Uiso 1.00 calc . . . H(10) H 0.7429 0.0029 0.4332 0.1099 Uiso 1.00 calc . . . H(11) H 0.7963 0.1153 0.3901 0.1099 Uiso 1.00 calc . . . H(12) H 0.6856 0.1077 0.4635 0.1099 Uiso 1.00 calc . . . H(13) H 0.2804 -0.2078 0.3995 0.0397 Uiso 1.00 calc . . . H(14) H 0.4408 -0.2533 0.4443 0.0657 Uiso 1.00 calc . . . H(15) H 0.6154 -0.2019 0.1916 0.0654 Uiso 1.00 calc . . . H(16) H 0.4564 -0.1529 0.1460 0.0525 Uiso 1.00 calc . . . H(17) H 0.6426 -0.3252 0.3853 0.1071 Uiso 1.00 calc . . . H(18) H 0.7090 -0.2493 0.3019 0.1071 Uiso 1.00 calc . . . H(19) H 0.6564 -0.2031 0.3894 0.1071 Uiso 1.00 calc . . . H(20) H 0.3478 -0.2971 0.1376 0.0576 Uiso 1.00 calc . . . H(21) H 0.3073 -0.3838 0.0321 0.0683 Uiso 1.00 calc . . . H(22) H 0.0509 -0.1893 0.0211 0.0604 Uiso 1.00 calc . . . H(23) H 0.0896 -0.1023 0.1275 0.0523 Uiso 1.00 calc . . . H(24) H 0.0759 -0.3815 -0.0314 0.0955 Uiso 1.00 calc . . . H(25) H 0.1530 -0.3013 -0.1053 0.0955 Uiso 1.00 calc . . . H(26) H 0.2005 -0.4086 -0.0651 0.0955 Uiso 1.00 calc . . . H(27) H 0.1543 -0.3412 0.2866 0.0653 Uiso 1.00 calc . . . H(28) H 0.0092 -0.4300 0.3889 0.0779 Uiso 1.00 calc . . . H(29) H -0.0930 -0.1542 0.4785 0.0664 Uiso 1.00 calc . . . H(30) H 0.0552 -0.0648 0.3783 0.0577 Uiso 1.00 calc . . . H(31) H -0.1477 -0.3510 0.5682 0.1030 Uiso 1.00 calc . . . H(32) H -0.2195 -0.3272 0.4995 0.1030 Uiso 1.00 calc . . . H(33) H -0.1502 -0.4328 0.5037 0.1030 Uiso 1.00 calc . . . H(34) H 0.4183 0.3619 0.0880 0.0544 Uiso 1.00 calc . . . H(35) H 0.4754 0.4358 -0.0604 0.0700 Uiso 1.00 calc . . . H(36) H 0.1820 0.3694 -0.0960 0.0643 Uiso 1.00 calc . . . H(37) H 0.1239 0.2927 0.0513 0.0517 Uiso 1.00 calc . . . H(38) H 0.4430 0.4899 -0.1979 0.1081 Uiso 1.00 calc . . . H(39) H 0.3658 0.4124 -0.2238 0.1081 Uiso 1.00 calc . . . H(40) H 0.3213 0.5228 -0.1962 0.1081 Uiso 1.00 calc . . . H(41) H 0.0769 0.4338 0.1463 0.0640 Uiso 1.00 calc . . . H(42) H -0.0924 0.4953 0.2201 0.0853 Uiso 1.00 calc . . . H(43) H -0.1013 0.2652 0.4278 0.0672 Uiso 1.00 calc . . . H(44) H 0.0651 0.2007 0.3548 0.0535 Uiso 1.00 calc . . . H(45) H -0.2207 0.4438 0.4314 0.1266 Uiso 1.00 calc . . . H(46) H -0.2461 0.4849 0.3397 0.1266 Uiso 1.00 calc . . . H(47) H -0.2775 0.3672 0.3868 0.1266 Uiso 1.00 calc . . . H(48) H 0.2412 0.4744 0.2273 0.0519 Uiso 1.00 calc . . . H(49) H 0.3328 0.5566 0.3088 0.0530 Uiso 1.00 calc . . . H(50) H 0.4786 0.2777 0.3726 0.0524 Uiso 1.00 calc . . . H(51) H 0.3851 0.1939 0.2928 0.0492 Uiso 1.00 calc . . . H(52) H 0.4388 0.4407 0.4696 0.0630 Uiso 1.00 calc . . . H(53) H 0.5416 0.4704 0.3902 0.0630 Uiso 1.00 calc . . . H(54) H 0.4428 0.5502 0.4062 0.0630 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 0.0301(1) 0.0323(1) 0.0284(1) 0.00275(8) -0.00927(10) -0.00625(9) Cl 0.0489(5) 0.0535(4) 0.0293(4) 0.0029(3) -0.0134(3) -0.0072(3) P(1) 0.0316(4) 0.0308(4) 0.0298(4) 0.0040(3) -0.0065(3) -0.0050(3) P(2) 0.0319(4) 0.0311(4) 0.0290(4) 0.0016(3) -0.0095(3) -0.0064(3) O(1) 0.031(1) 0.095(2) 0.069(2) 0.003(1) -0.014(1) -0.024(1) O(2) 0.038(1) 0.075(1) 0.044(1) 0.006(1) -0.018(1) -0.012(1) O(3) 0.048(1) 0.095(2) 0.033(1) 0.003(1) -0.018(1) -0.023(1) N 0.030(1) 0.042(1) 0.037(1) 0.001(1) -0.007(1) -0.011(1) C(1) 0.077(3) 0.121(3) 0.040(2) -0.001(2) -0.034(2) -0.026(2) C(2) 0.042(2) 0.039(2) 0.034(2) 0.001(1) -0.013(1) -0.007(1) C(3) 0.036(2) 0.033(1) 0.027(2) 0.002(1) -0.007(1) -0.008(1) C(4) 0.038(2) 0.044(2) 0.030(2) 0.003(1) -0.007(1) -0.008(1) C(5) 0.031(2) 0.037(1) 0.033(2) 0.004(1) -0.011(1) -0.008(1) C(6) 0.035(2) 0.047(2) 0.035(2) 0.005(1) -0.010(1) -0.005(1) C(7) 0.029(2) 0.047(2) 0.040(2) 0.005(1) -0.011(1) -0.009(1) C(8) 0.036(2) 0.045(2) 0.045(2) 0.004(1) -0.016(1) -0.007(1) C(9) 0.054(2) 0.053(2) 0.044(2) 0.004(2) -0.020(2) -0.005(1) C(10) 0.049(2) 0.072(2) 0.053(2) 0.003(2) -0.026(2) -0.014(2) C(11) 0.041(2) 0.109(3) 0.065(3) -0.019(2) -0.022(2) -0.007(2) C(12) 0.036(2) 0.085(2) 0.051(2) -0.010(2) -0.013(2) 0.001(2) C(13) 0.083(3) 0.133(4) 0.076(3) -0.005(3) -0.051(3) -0.019(3) C(14) 0.038(2) 0.033(1) 0.034(2) 0.004(1) -0.012(1) -0.004(1) C(15) 0.033(2) 0.031(1) 0.035(2) -0.002(1) -0.009(1) 0.000(1) C(16) 0.064(2) 0.045(2) 0.059(2) -0.001(2) -0.031(2) 0.008(2) C(17) 0.056(2) 0.042(2) 0.080(3) 0.009(2) -0.035(2) -0.003(2) C(18) 0.035(2) 0.048(2) 0.077(3) 0.006(1) -0.009(2) -0.010(2) C(19) 0.041(2) 0.043(2) 0.046(2) 0.006(1) -0.009(2) -0.006(1) C(20) 0.064(3) 0.082(3) 0.135(4) 0.012(2) -0.058(3) -0.005(3) C(21) 0.040(2) 0.034(1) 0.037(2) 0.004(1) -0.010(1) -0.007(1) C(22) 0.052(2) 0.049(2) 0.049(2) 0.019(1) -0.019(2) -0.019(1) C(23) 0.068(2) 0.054(2) 0.059(2) 0.024(2) -0.024(2) -0.032(2) C(24) 0.064(2) 0.046(2) 0.049(2) 0.006(2) -0.021(2) -0.018(1) C(25) 0.053(2) 0.047(2) 0.061(2) 0.007(1) -0.030(2) -0.014(2) C(26) 0.045(2) 0.039(2) 0.053(2) 0.010(1) -0.019(2) -0.015(1) C(27) 0.100(3) 0.072(2) 0.086(3) 0.007(2) -0.043(3) -0.040(2) C(28) 0.035(2) 0.038(2) 0.041(2) 0.000(1) -0.009(1) -0.004(1) C(29) 0.054(2) 0.043(2) 0.057(2) -0.004(1) 0.002(2) -0.008(2) C(30) 0.071(3) 0.053(2) 0.063(3) -0.022(2) -0.005(2) -0.002(2) C(31) 0.048(2) 0.074(2) 0.044(2) -0.019(2) -0.008(2) 0.000(2) C(32) 0.049(2) 0.070(2) 0.039(2) -0.001(2) 0.002(2) -0.007(2) C(33) 0.049(2) 0.050(2) 0.040(2) -0.001(1) -0.002(2) -0.005(1) C(34) 0.073(3) 0.112(3) 0.063(3) -0.045(2) 0.001(2) -0.003(2) C(35) 0.040(2) 0.031(1) 0.034(2) 0.002(1) -0.006(1) -0.006(1) C(36) 0.042(2) 0.049(2) 0.043(2) -0.003(1) -0.007(2) -0.007(1) C(37) 0.056(2) 0.058(2) 0.049(2) -0.009(2) 0.009(2) -0.006(2) C(38) 0.075(3) 0.049(2) 0.034(2) 0.009(2) 0.000(2) -0.002(1) C(39) 0.074(3) 0.052(2) 0.037(2) 0.007(2) -0.021(2) -0.005(1) C(40) 0.049(2) 0.043(2) 0.038(2) 0.000(1) -0.014(2) -0.005(1) C(41) 0.115(4) 0.094(3) 0.040(2) 0.009(3) 0.006(2) 0.011(2) C(42) 0.036(2) 0.041(2) 0.042(2) 0.004(1) -0.016(1) -0.014(1) C(43) 0.057(2) 0.053(2) 0.051(2) 0.019(2) -0.016(2) -0.009(2) C(44) 0.067(3) 0.076(3) 0.075(3) 0.038(2) -0.028(2) -0.019(2) C(45) 0.048(2) 0.083(3) 0.067(3) 0.022(2) -0.017(2) -0.035(2) C(46) 0.045(2) 0.073(2) 0.050(2) 0.007(2) -0.008(2) -0.020(2) C(47) 0.040(2) 0.049(2) 0.045(2) 0.007(1) -0.009(2) -0.012(1) C(48) 0.063(3) 0.141(4) 0.109(4) 0.046(3) -0.008(3) -0.041(3) C(49) 0.035(2) 0.035(1) 0.033(2) -0.002(1) -0.009(1) -0.007(1) C(50) 0.049(2) 0.033(2) 0.052(2) 0.004(1) -0.024(2) -0.004(1) C(51) 0.054(2) 0.030(1) 0.053(2) -0.001(1) -0.019(2) -0.009(1) C(52) 0.036(2) 0.045(2) 0.034(2) -0.009(1) -0.005(1) -0.011(1) C(53) 0.042(2) 0.043(2) 0.053(2) 0.005(1) -0.023(2) -0.010(1) C(54) 0.041(2) 0.036(2) 0.053(2) 0.005(1) -0.020(2) -0.014(1) C(55) 0.060(2) 0.057(2) 0.047(2) -0.012(2) -0.020(2) -0.014(2) #------------------------------------------------------------------------------ _computing_data_collection D*TREK _computing_cell_refinement D*TREK _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cl 2.4746(7) . . yes Ru P(1) 2.4204(7) . . yes Ru P(2) 2.4225(7) . . yes Ru N 1.760(2) . . yes Ru C(3) 2.075(3) . . yes Ru C(5) 2.188(3) . . yes P(1) C(14) 1.813(3) . . yes P(1) C(21) 1.820(3) . . yes P(1) C(28) 1.830(3) . . yes P(2) C(35) 1.813(3) . . yes P(2) C(42) 1.831(3) . . yes P(2) C(49) 1.828(3) . . yes O(1) N 1.161(3) . . yes O(2) C(2) 1.206(3) . . yes O(3) C(1) 1.443(4) . . yes O(3) C(2) 1.348(3) . . yes C(2) C(3) 1.454(4) . . yes C(3) C(4) 1.344(4) . . yes C(4) C(5) 1.441(4) . . yes C(5) C(6) 1.357(4) . . yes C(6) C(7) 1.458(4) . . yes C(7) C(8) 1.386(4) . . yes C(7) C(12) 1.400(4) . . yes C(8) C(9) 1.376(4) . . yes C(9) C(10) 1.386(4) . . yes C(10) C(11) 1.376(5) . . yes C(10) C(13) 1.510(5) . . yes C(11) C(12) 1.380(5) . . yes C(14) C(15) 1.375(4) . . yes C(14) C(19) 1.395(4) . . yes C(15) C(16) 1.394(4) . . yes C(16) C(17) 1.384(5) . . yes C(17) C(18) 1.380(5) . . yes C(17) C(20) 1.507(5) . . yes C(18) C(19) 1.391(4) . . yes C(21) C(22) 1.396(4) . . yes C(21) C(26) 1.384(4) . . yes C(22) C(23) 1.373(4) . . yes C(23) C(24) 1.376(4) . . yes C(24) C(25) 1.386(4) . . yes C(24) C(27) 1.503(4) . . yes C(25) C(26) 1.378(4) . . yes C(28) C(29) 1.396(4) . . yes C(28) C(33) 1.379(4) . . yes C(29) C(30) 1.373(4) . . yes C(30) C(31) 1.384(5) . . yes C(31) C(32) 1.384(4) . . yes C(31) C(34) 1.503(5) . . yes C(32) C(33) 1.386(4) . . yes C(35) C(36) 1.384(4) . . yes C(35) C(40) 1.395(4) . . yes C(36) C(37) 1.390(4) . . yes C(37) C(38) 1.379(5) . . yes C(38) C(39) 1.379(5) . . yes C(38) C(41) 1.499(5) . . yes C(39) C(40) 1.386(4) . . yes C(42) C(43) 1.394(4) . . yes C(42) C(47) 1.382(4) . . yes C(43) C(44) 1.392(5) . . yes C(44) C(45) 1.372(5) . . yes C(45) C(46) 1.382(5) . . yes C(45) C(48) 1.519(5) . . yes C(46) C(47) 1.379(4) . . yes C(49) C(50) 1.392(4) . . yes C(49) C(54) 1.374(4) . . yes C(50) C(51) 1.373(4) . . yes C(51) C(52) 1.391(4) . . yes C(52) C(53) 1.381(4) . . yes C(52) C(55) 1.489(4) . . yes C(53) C(54) 1.382(4) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Ru P(1) 86.13(3) . . . yes Cl Ru P(2) 91.58(2) . . . yes Cl Ru N 99.42(8) . . . yes Cl Ru C(3) 165.97(8) . . . yes Cl Ru C(5) 103.14(7) . . . yes P(1) Ru P(2) 174.40(3) . . . yes P(1) Ru N 92.88(7) . . . yes P(1) Ru C(3) 91.23(7) . . . yes P(1) Ru C(5) 89.92(7) . . . yes P(2) Ru N 92.54(7) . . . yes P(2) Ru C(3) 89.76(7) . . . yes P(2) Ru C(5) 85.62(7) . . . yes N Ru C(3) 94.5(1) . . . yes N Ru C(5) 157.4(1) . . . yes C(3) Ru C(5) 63.0(1) . . . yes Ru P(1) C(14) 114.02(9) . . . yes Ru P(1) C(21) 116.60(9) . . . yes Ru P(1) C(28) 113.45(9) . . . yes C(14) P(1) C(21) 107.0(1) . . . yes C(14) P(1) C(28) 104.6(1) . . . yes C(21) P(1) C(28) 99.6(1) . . . yes Ru P(2) C(35) 114.63(9) . . . yes Ru P(2) C(42) 110.29(9) . . . yes Ru P(2) C(49) 120.03(9) . . . yes C(35) P(2) C(42) 106.7(1) . . . yes C(35) P(2) C(49) 103.5(1) . . . yes C(42) P(2) C(49) 100.1(1) . . . yes C(1) O(3) C(2) 115.6(3) . . . yes Ru N O(1) 169.7(2) . . . yes O(2) C(2) O(3) 122.2(3) . . . yes O(2) C(2) C(3) 125.4(3) . . . yes O(3) C(2) C(3) 112.5(3) . . . yes Ru C(3) C(2) 132.0(2) . . . yes Ru C(3) C(4) 99.3(2) . . . yes C(2) C(3) C(4) 128.5(3) . . . yes C(3) C(4) C(5) 106.4(2) . . . yes Ru C(5) C(4) 91.3(2) . . . yes Ru C(5) C(6) 148.2(2) . . . yes C(4) C(5) C(6) 120.2(3) . . . yes C(5) C(6) C(7) 133.3(3) . . . yes C(6) C(7) C(8) 123.9(3) . . . yes C(6) C(7) C(12) 119.5(3) . . . yes C(8) C(7) C(12) 116.6(3) . . . yes C(7) C(8) C(9) 121.5(3) . . . yes C(8) C(9) C(10) 121.7(3) . . . yes C(9) C(10) C(11) 117.3(3) . . . yes C(9) C(10) C(13) 120.7(3) . . . yes C(11) C(10) C(13) 122.0(3) . . . yes C(10) C(11) C(12) 121.5(3) . . . yes C(7) C(12) C(11) 121.4(3) . . . yes P(1) C(14) C(15) 120.2(2) . . . yes P(1) C(14) C(19) 120.7(2) . . . yes C(15) C(14) C(19) 118.6(3) . . . yes C(14) C(15) C(16) 120.6(3) . . . yes C(15) C(16) C(17) 121.3(3) . . . yes C(16) C(17) C(18) 117.8(3) . . . yes C(16) C(17) C(20) 120.7(4) . . . yes C(18) C(17) C(20) 121.5(4) . . . yes C(17) C(18) C(19) 121.5(3) . . . yes C(14) C(19) C(18) 120.1(3) . . . yes P(1) C(21) C(22) 126.2(2) . . . yes P(1) C(21) C(26) 116.3(2) . . . yes C(22) C(21) C(26) 117.2(3) . . . yes C(21) C(22) C(23) 120.5(3) . . . yes C(22) C(23) C(24) 122.3(3) . . . yes C(23) C(24) C(25) 117.3(3) . . . yes C(23) C(24) C(27) 122.4(3) . . . yes C(25) C(24) C(27) 120.3(3) . . . yes C(24) C(25) C(26) 120.9(3) . . . yes C(21) C(26) C(25) 121.7(3) . . . yes P(1) C(28) C(29) 119.1(2) . . . yes P(1) C(28) C(33) 123.3(2) . . . yes C(29) C(28) C(33) 117.6(3) . . . yes C(28) C(29) C(30) 120.9(3) . . . yes C(29) C(30) C(31) 121.7(3) . . . yes C(30) C(31) C(32) 117.4(3) . . . yes C(30) C(31) C(34) 121.9(3) . . . yes C(32) C(31) C(34) 120.8(4) . . . yes C(31) C(32) C(33) 121.4(3) . . . yes C(28) C(33) C(32) 121.0(3) . . . yes P(2) C(35) C(36) 120.8(2) . . . yes P(2) C(35) C(40) 120.3(2) . . . yes C(36) C(35) C(40) 118.6(3) . . . yes C(35) C(36) C(37) 120.3(3) . . . yes C(36) C(37) C(38) 121.4(3) . . . yes C(37) C(38) C(39) 118.0(3) . . . yes C(37) C(38) C(41) 120.9(4) . . . yes C(39) C(38) C(41) 121.1(4) . . . yes C(38) C(39) C(40) 121.5(3) . . . yes C(35) C(40) C(39) 120.1(3) . . . yes P(2) C(42) C(43) 124.5(2) . . . yes P(2) C(42) C(47) 116.9(2) . . . yes C(43) C(42) C(47) 118.4(3) . . . yes C(42) C(43) C(44) 119.2(3) . . . yes C(43) C(44) C(45) 122.1(3) . . . yes C(44) C(45) C(46) 118.3(3) . . . yes C(44) C(45) C(48) 121.6(4) . . . yes C(46) C(45) C(48) 120.1(4) . . . yes C(45) C(46) C(47) 120.4(3) . . . yes C(42) C(47) C(46) 121.5(3) . . . yes P(2) C(49) C(50) 120.4(2) . . . yes P(2) C(49) C(54) 120.9(2) . . . yes C(50) C(49) C(54) 118.6(2) . . . yes C(49) C(50) C(51) 120.3(3) . . . yes C(50) C(51) C(52) 121.5(2) . . . yes C(51) C(52) C(53) 117.4(3) . . . yes C(51) C(52) C(55) 120.8(3) . . . yes C(53) C(52) C(55) 121.8(3) . . . yes C(52) C(53) C(54) 121.5(3) . . . yes C(49) C(54) C(53) 120.6(2) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru P(1) C(14) C(15) 93.7(2) . . . . yes Ru P(1) C(14) C(19) -78.1(2) . . . . yes Ru P(1) C(21) C(22) 137.9(2) . . . . yes Ru P(1) C(21) C(26) -49.7(3) . . . . yes Ru P(1) C(28) C(29) 166.2(2) . . . . yes Ru P(1) C(28) C(33) -12.4(3) . . . . yes Ru P(2) C(35) C(36) -102.5(2) . . . . yes Ru P(2) C(35) C(40) 71.3(2) . . . . yes Ru P(2) C(42) C(43) -137.9(2) . . . . yes Ru P(2) C(42) C(47) 47.6(2) . . . . yes Ru P(2) C(49) C(50) -166.7(2) . . . . yes Ru P(2) C(49) C(54) 8.9(3) . . . . yes Ru C(3) C(2) O(2) 10.6(4) . . . . yes Ru C(3) C(2) O(3) -170.3(2) . . . . yes Ru C(3) C(4) C(5) -0.1(2) . . . . yes Ru C(5) C(4) C(3) 0.1(2) . . . . yes Ru C(5) C(6) C(7) 10.4(6) . . . . yes Cl Ru P(1) C(14) -58.3(1) . . . . yes Cl Ru P(1) C(21) 176.2(1) . . . . yes Cl Ru P(1) C(28) 61.3(1) . . . . yes Cl Ru P(2) C(35) 159.7(1) . . . . yes Cl Ru P(2) C(42) -79.9(1) . . . . yes Cl Ru P(2) C(49) 35.5(1) . . . . yes Cl Ru N O(1) 178(1) . . . . yes Cl Ru C(3) C(2) 174.1(2) . . . . yes Cl Ru C(3) C(4) -10.3(4) . . . . yes Cl Ru C(5) C(4) 177.4(1) . . . . yes Cl Ru C(5) C(6) -9.3(4) . . . . yes P(1) Ru P(2) C(35) 93.8(3) . . . . yes P(1) Ru P(2) C(42) -145.7(3) . . . . yes P(1) Ru P(2) C(49) -30.3(3) . . . . yes P(1) Ru N O(1) -94(1) . . . . yes P(1) Ru C(3) C(2) 95.2(2) . . . . yes P(1) Ru C(3) C(4) -89.2(2) . . . . yes P(1) Ru C(5) C(4) 91.4(1) . . . . yes P(1) Ru C(5) C(6) -95.3(4) . . . . yes P(1) C(14) C(15) C(16) -172.1(2) . . . . yes P(1) C(14) C(19) C(18) 172.7(2) . . . . yes P(1) C(21) C(22) C(23) 171.5(3) . . . . yes P(1) C(21) C(26) C(25) -172.5(3) . . . . yes P(1) C(28) C(29) C(30) -177.6(3) . . . . yes P(1) C(28) C(33) C(32) 176.7(2) . . . . yes P(2) Ru P(1) C(14) 7.8(3) . . . . yes P(2) Ru P(1) C(21) -117.7(3) . . . . yes P(2) Ru P(1) C(28) 127.4(3) . . . . yes P(2) Ru N O(1) 86(1) . . . . yes P(2) Ru C(3) C(2) -90.4(2) . . . . yes P(2) Ru C(3) C(4) 85.3(2) . . . . yes P(2) Ru C(5) C(4) -92.0(1) . . . . yes P(2) Ru C(5) C(6) 81.3(4) . . . . yes P(2) C(35) C(36) C(37) 176.1(2) . . . . yes P(2) C(35) C(40) C(39) -176.7(2) . . . . yes P(2) C(42) C(43) C(44) -175.5(3) . . . . yes P(2) C(42) C(47) C(46) 175.3(2) . . . . yes P(2) C(49) C(50) C(51) 174.3(2) . . . . yes P(2) C(49) C(54) C(53) -174.8(2) . . . . yes O(1) N Ru C(3) -3(1) . . . . yes O(1) N Ru C(5) 2(1) . . . . yes O(2) C(2) O(3) C(1) -1.2(4) . . . . yes O(2) C(2) C(3) C(4) -163.9(3) . . . . yes O(3) C(2) C(3) C(4) 15.2(4) . . . . yes N Ru P(1) C(14) -157.6(1) . . . . yes N Ru P(1) C(21) 77.0(1) . . . . yes N Ru P(1) C(28) -38.0(1) . . . . yes N Ru P(2) C(35) -100.8(1) . . . . yes N Ru P(2) C(42) 19.6(1) . . . . yes N Ru P(2) C(49) 135.0(1) . . . . yes N Ru C(3) C(2) 2.2(2) . . . . yes N Ru C(3) C(4) 177.8(2) . . . . yes N Ru C(5) C(4) -6.0(3) . . . . yes N Ru C(5) C(6) 167.4(3) . . . . yes C(1) O(3) C(2) C(3) 179.6(3) . . . . yes C(2) C(3) Ru C(5) -175.6(3) . . . . yes C(2) C(3) C(4) C(5) 175.8(2) . . . . yes C(3) Ru P(1) C(14) 107.9(1) . . . . yes C(3) Ru P(1) C(21) -17.6(1) . . . . yes C(3) Ru P(1) C(28) -132.5(1) . . . . yes C(3) Ru P(2) C(35) -6.4(1) . . . . yes C(3) Ru P(2) C(42) 114.1(1) . . . . yes C(3) Ru P(2) C(49) -130.5(1) . . . . yes C(3) Ru C(5) C(4) -0.1(1) . . . . yes C(3) Ru C(5) C(6) 173.3(4) . . . . yes C(3) C(4) C(5) C(6) -175.9(2) . . . . yes C(4) C(3) Ru C(5) 0.1(2) . . . . yes C(4) C(5) C(6) C(7) -177.3(3) . . . . yes C(5) Ru P(1) C(14) 44.9(1) . . . . yes C(5) Ru P(1) C(21) -80.6(1) . . . . yes C(5) Ru P(1) C(28) 164.5(1) . . . . yes C(5) Ru P(2) C(35) 56.6(1) . . . . yes C(5) Ru P(2) C(42) 177.0(1) . . . . yes C(5) Ru P(2) C(49) -67.6(1) . . . . yes C(5) C(6) C(7) C(8) 23.7(5) . . . . yes C(5) C(6) C(7) C(12) -158.3(3) . . . . yes C(6) C(7) C(8) C(9) 177.5(3) . . . . yes C(6) C(7) C(12) C(11) -178.6(3) . . . . yes C(7) C(8) C(9) C(10) 0.0(5) . . . . yes C(7) C(12) C(11) C(10) 2.2(6) . . . . yes C(8) C(7) C(12) C(11) -0.5(5) . . . . yes C(8) C(9) C(10) C(11) 1.6(5) . . . . yes C(8) C(9) C(10) C(13) -178.0(3) . . . . yes C(9) C(8) C(7) C(12) -0.6(4) . . . . yes C(9) C(10) C(11) C(12) -2.7(6) . . . . yes C(12) C(11) C(10) C(13) 176.9(4) . . . . yes C(14) P(1) C(21) C(22) 8.9(3) . . . . yes C(14) P(1) C(21) C(26) -178.7(2) . . . . yes C(14) P(1) C(28) C(29) -68.9(3) . . . . yes C(14) P(1) C(28) C(33) 112.5(3) . . . . yes C(14) C(15) C(16) C(17) 0.5(5) . . . . yes C(14) C(19) C(18) C(17) -1.9(5) . . . . yes C(15) C(14) P(1) C(21) -135.8(2) . . . . yes C(15) C(14) P(1) C(28) -30.8(3) . . . . yes C(15) C(14) C(19) C(18) 0.8(4) . . . . yes C(15) C(16) C(17) C(18) -1.6(5) . . . . yes C(15) C(16) C(17) C(20) 177.4(3) . . . . yes C(16) C(15) C(14) C(19) -0.1(4) . . . . yes C(16) C(17) C(18) C(19) 2.3(5) . . . . yes C(19) C(14) P(1) C(21) 52.3(3) . . . . yes C(19) C(14) P(1) C(28) 157.4(2) . . . . yes C(19) C(18) C(17) C(20) -176.7(3) . . . . yes C(21) P(1) C(28) C(29) 41.6(3) . . . . yes C(21) P(1) C(28) C(33) -137.1(3) . . . . yes C(21) C(22) C(23) C(24) 0.2(6) . . . . yes C(21) C(26) C(25) C(24) 0.2(5) . . . . yes C(22) C(21) P(1) C(28) -99.7(3) . . . . yes C(22) C(21) C(26) C(25) 0.6(5) . . . . yes C(22) C(23) C(24) C(25) 0.6(6) . . . . yes C(22) C(23) C(24) C(27) 179.6(4) . . . . yes C(23) C(22) C(21) C(26) -0.8(5) . . . . yes C(23) C(24) C(25) C(26) -0.8(5) . . . . yes C(26) C(21) P(1) C(28) 72.7(2) . . . . yes C(26) C(25) C(24) C(27) -179.9(3) . . . . yes C(28) C(29) C(30) C(31) 0.3(6) . . . . yes C(28) C(33) C(32) C(31) 1.4(5) . . . . yes C(29) C(28) C(33) C(32) -2.0(5) . . . . yes C(29) C(30) C(31) C(32) -0.8(6) . . . . yes C(29) C(30) C(31) C(34) 179.5(4) . . . . yes C(30) C(29) C(28) C(33) 1.1(5) . . . . yes C(30) C(31) C(32) C(33) 0.0(5) . . . . yes C(33) C(32) C(31) C(34) 179.6(3) . . . . yes C(35) P(2) C(42) C(43) -12.8(3) . . . . yes C(35) P(2) C(42) C(47) 172.7(2) . . . . yes C(35) P(2) C(49) C(50) 64.0(3) . . . . yes C(35) P(2) C(49) C(54) -120.4(3) . . . . yes C(35) C(36) C(37) C(38) 0.2(5) . . . . yes C(35) C(40) C(39) C(38) 1.0(5) . . . . yes C(36) C(35) P(2) C(42) 135.1(2) . . . . yes C(36) C(35) P(2) C(49) 30.1(3) . . . . yes C(36) C(35) C(40) C(39) -2.7(4) . . . . yes C(36) C(37) C(38) C(39) -1.9(5) . . . . yes C(36) C(37) C(38) C(41) 177.2(3) . . . . yes C(37) C(36) C(35) C(40) 2.2(4) . . . . yes C(37) C(38) C(39) C(40) 1.3(5) . . . . yes C(40) C(35) P(2) C(42) -51.1(3) . . . . yes C(40) C(35) P(2) C(49) -156.1(2) . . . . yes C(40) C(39) C(38) C(41) -177.8(3) . . . . yes C(42) P(2) C(49) C(50) -46.1(3) . . . . yes C(42) P(2) C(49) C(54) 129.6(3) . . . . yes C(42) C(43) C(44) C(45) 0.4(6) . . . . yes C(42) C(47) C(46) C(45) 0.9(5) . . . . yes C(43) C(42) P(2) C(49) 94.7(3) . . . . yes C(43) C(42) C(47) C(46) 0.5(5) . . . . yes C(43) C(44) C(45) C(46) 1.0(6) . . . . yes C(43) C(44) C(45) C(48) -178.2(4) . . . . yes C(44) C(43) C(42) C(47) -1.1(5) . . . . yes C(44) C(45) C(46) C(47) -1.6(5) . . . . yes C(47) C(42) P(2) C(49) -79.8(2) . . . . yes C(47) C(46) C(45) C(48) 177.5(3) . . . . yes C(49) C(50) C(51) C(52) -0.6(5) . . . . yes C(49) C(54) C(53) C(52) 1.6(5) . . . . yes C(50) C(49) C(54) C(53) 1.0(5) . . . . yes C(50) C(51) C(52) C(53) 3.1(5) . . . . yes C(50) C(51) C(52) C(55) -175.7(3) . . . . yes C(51) C(50) C(49) C(54) -1.5(5) . . . . yes C(51) C(52) C(53) C(54) -3.6(5) . . . . yes C(54) C(53) C(52) C(55) 175.1(3) . . . . yes C(54) C(53) C(52) C(55) 175.1(3) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(1) 3.524(4) . 2_555 ? O(1) C(11) 3.585(4) . 1_455 ? O(2) C(25) 3.348(4) . 2_555 ? C(1) C(12) 3.585(5) . 2_655 ? C(34) C(51) 3.492(5) . 2_556 ? C(34) C(52) 3.521(5) . 2_556 ? C(41) C(52) 3.500(5) . 2_665 ? C(55) C(55) 3.401(6) . 2_666 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------