Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address 'M A Bennett' ; Research School of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; 'Matthew Byrnes' ; Research School of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; 'Anthony C Willis' ; Research School of Chemistry, The Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_author_name 'Martin Bennett' _publ_contact_author_address ; Research School of Chemistry Australian National University Canberra ACT 0200 AUSTRALIA ; _publ_contact_author_email BENNETT@RSC.ANU.EDU.AU _publ_section_title ; Bis(acetylacetonato)ruthenium(II) complexes containing alkynyldiphenylphosphines. Formation and redox behaviour of [Ru(acac)2(Ph2PC?CR)2] (R = H, Me, Ph) complexes and the binuclear complex cis-[{Ru(acac)2}2(m-Ph2PC?CPPh2)}2] ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ; ? ; _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_volume ? _journal_year ? _publ_contact_author_fax ' 61 2 6125 0750 ' _publ_contact_author_phone ' 61 2 6125 4109 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category 'FM ' _publ_requested_coeditor_name ? data_mat12a _database_code_depnum_ccdc_archive 'CCDC 631384' #------------------------------------------------------------------------------ _audit_creation_date 1998-07-01 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 10.247(1) _cell_length_b 11.045(3) _cell_length_c 11.720(3) _cell_angle_alpha 117.21(2) _cell_angle_beta 94.27(2) _cell_angle_gamma 107.61(1) _cell_volume 1088.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 193.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 52.5 _cell_measurement_theta_max 54.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 917.64 _chemical_formula_analytical ? _chemical_formula_sum 'C42 H44 Cl4 O4 P2 Ru ' _chemical_formula_moiety ' C40 H40 O4 P2 Ru , 2(C H2 Cl2)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 470.00 _exptl_absorpt_coefficient_mu 6.316 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.608 _exptl_absorpt_correction_T_min 0.457 _exptl_special_details ; The scan width was (1.42+0.30tan\q)\% with an \w scan speed of 32\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 193.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6R' _diffrn_measurement_method \w-2\q _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 ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3425 _reflns_number_total 3241 _reflns_number_gt 3026 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.03925 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.38 _diffrn_reflns_theta_max 60.00 _diffrn_measured_fraction_theta_max 1.0 _diffrn_reflns_theta_full 60 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05131 _diffrn_orient_matrix_UB_12 -0.06212 _diffrn_orient_matrix_UB_13 -0.05173 _diffrn_orient_matrix_UB_21 0.08914 _diffrn_orient_matrix_UB_22 0.06889 _diffrn_orient_matrix_UB_23 0.07172 _diffrn_orient_matrix_UB_31 -0.02473 _diffrn_orient_matrix_UB_32 -0.05918 _diffrn_orient_matrix_UB_33 0.04477 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 42 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 44 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 4 0.348 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 1 -0.105 3.296 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.5000 0.5000 0.5000 0.02243(8) 1.0 S Uani d ? Cl(1) 0.7934(1) -0.0435(1) 1.0126(1) 0.0799(4) 1.000 . Uani d ? Cl(2) 0.8442(1) 0.0677(1) 0.8326(1) 0.0752(3) 1.000 . Uani d ? P(1) 0.53361(7) 0.33612(8) 0.56138(7) 0.0264(2) 1.000 . Uani d ? O(1) 0.2874(2) 0.3702(2) 0.4280(2) 0.0295(5) 1.000 . Uani d ? O(2) 0.4792(2) 0.6279(2) 0.6868(2) 0.0295(5) 1.000 . Uani d ? C(1) 0.0454(4) 0.3016(5) 0.4217(4) 0.051(1) 1.000 . Uani d ? C(2) 0.1967(3) 0.4021(3) 0.4939(3) 0.0341(8) 1.000 . Uani d ? C(3) 0.2264(3) 0.5188(4) 0.6217(3) 0.0390(9) 1.000 . Uani d ? C(4) 0.3576(3) 0.6183(3) 0.7095(3) 0.0345(9) 1.000 . Uani d ? C(5) 0.3624(5) 0.7274(5) 0.8492(4) 0.055(1) 1.000 . Uani d ? C(6) 0.5188(3) 0.1659(3) 0.4285(3) 0.0355(9) 1.000 . Uani d ? C(7) 0.5103(3) 0.0568(4) 0.3328(3) 0.0390(9) 1.000 . Uani d ? C(8) 0.4990(5) -0.0778(5) 0.2150(4) 0.057(1) 1.000 . Uani d ? C(9) 0.4017(3) 0.2814(3) 0.6440(3) 0.0317(8) 1.000 . Uani d ? C(10) 0.2855(4) 0.1514(4) 0.5749(4) 0.047(1) 1.000 . Uani d ? C(11) 0.1823(4) 0.1164(6) 0.6392(5) 0.068(2) 1.000 . Uani d ? C(12) 0.1991(4) 0.2114(6) 0.7708(5) 0.067(2) 1.000 . Uani d ? C(13) 0.3118(4) 0.3410(5) 0.8388(4) 0.056(1) 1.000 . Uani d ? C(14) 0.4147(4) 0.3774(4) 0.7767(3) 0.043(1) 1.000 . Uani d ? C(15) 0.7021(3) 0.3958(3) 0.6742(3) 0.0319(8) 1.000 . Uani d ? C(16) 0.7601(4) 0.5390(4) 0.7781(3) 0.043(1) 1.000 . Uani d ? C(17) 0.8878(4) 0.5904(5) 0.8646(4) 0.061(1) 1.000 . Uani d ? C(18) 0.9609(4) 0.4991(6) 0.8469(5) 0.068(2) 1.000 . Uani d ? C(19) 0.9050(4) 0.3567(6) 0.7443(5) 0.067(2) 1.000 . Uani d ? C(20) 0.7754(4) 0.3024(4) 0.6563(4) 0.047(1) 1.000 . Uani d ? C(21) 0.7806(6) -0.0877(5) 0.8484(4) 0.067(1) 1.000 . Uani d ? H(1) -0.025(4) 0.318(4) 0.466(4) 0.061 1.000 . Uiso d ? H(2) 0.031(4) 0.206(4) 0.381(4) 0.061 1.000 . Uiso d ? H(3) 0.015(4) 0.301(4) 0.339(4) 0.061 1.000 . Uiso d ? H(4) 0.153(4) 0.528(4) 0.647(3) 0.046 1.000 . Uiso d ? H(5) 0.418(4) 0.817(5) 0.876(4) 0.065 1.000 . Uiso d ? H(6) 0.274(4) 0.732(4) 0.860(4) 0.065 1.000 . Uiso d ? H(7) 0.385(4) 0.699(4) 0.907(4) 0.065 1.000 . Uiso d ? H(8) 0.430(4) -0.166(5) 0.207(4) 0.069 1.000 . Uiso d ? H(9) 0.584(4) -0.088(5) 0.212(4) 0.069 1.000 . Uiso d ? H(10) 0.468(4) -0.082(4) 0.137(4) 0.069 1.000 . Uiso d ? H(11) 0.276(4) 0.083(4) 0.490(4) 0.057 1.000 . Uiso d ? H(12) 0.108(5) 0.026(5) 0.589(4) 0.082 1.000 . Uiso d ? H(13) 0.138(5) 0.193(5) 0.808(4) 0.080 1.000 . Uiso d ? H(14) 0.322(4) 0.406(4) 0.933(4) 0.067 1.000 . Uiso d ? H(15) 0.502(4) 0.475(4) 0.833(3) 0.051 1.000 . Uiso d ? H(16) 0.713(4) 0.596(4) 0.790(3) 0.052 1.000 . Uiso d ? H(17) 0.931(4) 0.684(5) 0.928(4) 0.072 1.000 . Uiso d ? H(18) 1.045(5) 0.532(5) 0.905(4) 0.082 1.000 . Uiso d ? H(19) 0.951(5) 0.292(5) 0.731(4) 0.081 1.000 . Uiso d ? H(20) 0.734(4) 0.209(4) 0.585(4) 0.057 1.000 . Uiso d ? H(21) 0.829(5) -0.125(5) 0.829(5) 0.079 1.000 . Uiso d ? H(22) 0.677(5) -0.134(5) 0.806(4) 0.079 1.000 . Uiso d ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0232(2) 0.0220(2) 0.0218(2) 0.0075(1) 0.0066(1) 0.0113(1) Cl(1) 0.0924(8) 0.0957(9) 0.0546(6) 0.0382(7) 0.0219(6) 0.0380(6) Cl(2) 0.0549(6) 0.0648(7) 0.0847(7) -0.0102(5) -0.0081(5) 0.0450(6) P(1) 0.0286(4) 0.0250(4) 0.0270(4) 0.0095(3) 0.0072(3) 0.0145(3) O(1) 0.026(1) 0.030(1) 0.031(1) 0.0078(8) 0.0068(8) 0.0168(9) O(2) 0.035(1) 0.030(1) 0.025(1) 0.0126(9) 0.0110(8) 0.0136(9) C(1) 0.029(2) 0.058(2) 0.058(2) 0.011(2) 0.011(2) 0.024(2) C(2) 0.030(2) 0.037(2) 0.042(2) 0.011(1) 0.009(1) 0.026(1) C(3) 0.033(2) 0.047(2) 0.047(2) 0.022(2) 0.021(1) 0.026(2) C(4) 0.046(2) 0.034(2) 0.034(2) 0.020(1) 0.017(1) 0.021(1) C(5) 0.064(3) 0.050(2) 0.040(2) 0.022(2) 0.027(2) 0.013(2) C(6) 0.043(2) 0.031(2) 0.036(2) 0.014(1) 0.009(1) 0.019(2) C(7) 0.051(2) 0.035(2) 0.035(2) 0.019(2) 0.010(1) 0.020(2) C(8) 0.084(3) 0.045(2) 0.040(2) 0.034(2) 0.013(2) 0.013(2) C(9) 0.029(2) 0.037(2) 0.041(2) 0.014(1) 0.009(1) 0.028(1) C(10) 0.038(2) 0.051(2) 0.054(2) 0.006(2) 0.006(2) 0.035(2) C(11) 0.033(2) 0.093(3) 0.096(4) 0.005(2) 0.010(2) 0.075(3) C(12) 0.047(2) 0.119(4) 0.090(4) 0.040(3) 0.037(2) 0.086(3) C(13) 0.056(2) 0.086(3) 0.063(2) 0.042(2) 0.033(2) 0.055(2) C(14) 0.049(2) 0.051(2) 0.046(2) 0.026(2) 0.020(2) 0.032(2) C(15) 0.030(2) 0.041(2) 0.034(2) 0.011(1) 0.010(1) 0.026(1) C(16) 0.041(2) 0.048(2) 0.037(2) 0.009(2) 0.003(1) 0.024(2) C(17) 0.046(2) 0.076(3) 0.044(2) -0.002(2) -0.005(2) 0.035(2) C(18) 0.031(2) 0.118(4) 0.067(3) 0.009(2) 0.003(2) 0.069(3) C(19) 0.046(2) 0.114(4) 0.088(3) 0.044(3) 0.026(2) 0.077(3) C(20) 0.040(2) 0.064(2) 0.060(2) 0.026(2) 0.018(2) 0.043(2) C(21) 0.083(3) 0.050(3) 0.051(2) 0.010(2) 0.014(2) 0.021(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3026 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_all 0.0355 _refine_ls_wR_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0349 _refine_ls_goodness_of_fit_all 1.591 _refine_ls_goodness_of_fit_ref 1.628 _refine_ls_shift/su_max 0.0440 _refine_ls_shift/su_mean 0.0020 _refine_diff_density_min -0.43 _refine_diff_density_max 0.49 #------------------------------------------------------------------------------ _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) P(1) 2.3330(7) . . yes Ru(1) P(1) 2.3330(7) . 2_666 yes Ru(1) O(1) 2.060(2) . . yes Ru(1) O(1) 2.060(2) . 2_666 yes Ru(1) O(2) 2.063(2) . . yes Ru(1) O(2) 2.063(2) . 2_666 yes Cl(1) C(21) 1.739(5) . . yes Cl(2) C(21) 1.742(5) . . yes P(1) C(6) 1.760(3) . . yes P(1) C(9) 1.835(3) . . yes P(1) C(15) 1.827(3) . . yes O(1) C(2) 1.281(3) . . yes O(2) C(4) 1.277(3) . . yes C(1) C(2) 1.502(4) . . yes C(1) H(1) 0.93(4) . . no C(1) H(2) 0.90(4) . . no C(1) H(3) 0.98(4) . . no C(2) C(3) 1.388(4) . . yes C(3) C(4) 1.393(4) . . yes C(3) H(4) 0.84(3) . . no C(4) C(5) 1.511(4) . . yes C(5) H(5) 0.87(4) . . no C(5) H(6) 0.94(4) . . no C(5) H(7) 0.91(4) . . no C(6) C(7) 1.185(4) . . yes C(7) C(8) 1.458(5) . . yes C(8) H(8) 0.97(4) . . no C(8) H(9) 0.92(4) . . no C(8) H(10) 0.93(4) . . no C(9) C(10) 1.376(4) . . yes C(9) C(14) 1.392(4) . . yes C(10) C(11) 1.404(5) . . yes C(10) H(11) 0.91(4) . . no C(11) C(12) 1.372(7) . . yes C(11) H(12) 0.93(4) . . no C(12) C(13) 1.356(6) . . yes C(12) H(13) 0.82(4) . . no C(13) C(14) 1.388(5) . . yes C(13) H(14) 0.98(4) . . no C(14) H(15) 1.04(3) . . no C(15) C(16) 1.378(4) . . yes C(15) C(20) 1.402(4) . . yes C(16) C(17) 1.375(5) . . yes C(16) H(16) 0.87(3) . . no C(17) C(18) 1.382(7) . . yes C(17) H(17) 0.89(4) . . no C(18) C(19) 1.368(7) . . yes C(18) H(18) 0.92(4) . . no C(19) C(20) 1.391(5) . . yes C(19) H(19) 0.93(4) . . no C(20) H(20) 0.92(4) . . no C(21) H(21) 0.72(4) . . no C(21) H(22) 1.00(4) . . 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 P(1) Ru(1) P(1) 180.00 . . 2_666 yes P(1) Ru(1) O(1) 88.73(6) . . . yes P(1) Ru(1) O(1) 91.27(6) . . 2_666 yes P(1) Ru(1) O(2) 90.22(6) . . . yes P(1) Ru(1) O(2) 89.78(6) . . 2_666 yes P(1) Ru(1) O(1) 91.27(6) 2_666 . . yes P(1) Ru(1) O(1) 88.73(6) 2_666 . 2_666 yes P(1) Ru(1) O(2) 89.78(6) 2_666 . . yes P(1) Ru(1) O(2) 90.22(6) 2_666 . 2_666 yes O(1) Ru(1) O(1) 180.0000(1) . . 2_666 yes O(1) Ru(1) O(2) 93.34(7) . . . yes O(1) Ru(1) O(2) 86.66(7) . . 2_666 yes O(1) Ru(1) O(2) 86.66(7) 2_666 . . yes O(1) Ru(1) O(2) 93.34(7) 2_666 . 2_666 yes O(2) Ru(1) O(2) 180.00 . . 2_666 yes Ru(1) P(1) C(6) 114.8(1) . . . yes Ru(1) P(1) C(9) 113.34(9) . . . yes Ru(1) P(1) C(15) 117.7(1) . . . yes C(6) P(1) C(9) 102.6(1) . . . yes C(6) P(1) C(15) 103.1(1) . . . yes C(9) P(1) C(15) 103.5(1) . . . yes Ru(1) O(1) C(2) 122.2(2) . . . yes Ru(1) O(2) C(4) 121.2(2) . . . yes C(2) C(1) H(1) 119(2) . . . no C(2) C(1) H(2) 114(3) . . . no C(2) C(1) H(3) 113(2) . . . no H(1) C(1) H(2) 110(3) . . . no H(1) C(1) H(3) 104(3) . . . no H(2) C(1) H(3) 95(3) . . . no O(1) C(2) C(1) 114.9(3) . . . yes O(1) C(2) C(3) 126.1(3) . . . yes C(1) C(2) C(3) 119.0(3) . . . yes C(2) C(3) C(4) 128.7(3) . . . yes C(2) C(3) H(4) 113(2) . . . no C(4) C(3) H(4) 118(2) . . . no O(2) C(4) C(3) 127.2(3) . . . yes O(2) C(4) C(5) 114.0(3) . . . yes C(3) C(4) C(5) 118.7(3) . . . yes C(4) C(5) H(5) 114(3) . . . no C(4) C(5) H(6) 113(2) . . . no C(4) C(5) H(7) 111(3) . . . no H(5) C(5) H(6) 105(4) . . . no H(5) C(5) H(7) 111(4) . . . no H(6) C(5) H(7) 103(3) . . . no P(1) C(6) C(7) 174.5(3) . . . yes C(6) C(7) C(8) 179.6(4) . . . yes C(7) C(8) H(8) 113(2) . . . no C(7) C(8) H(9) 112(3) . . . no C(7) C(8) H(10) 113(3) . . . no H(8) C(8) H(9) 109(4) . . . no H(8) C(8) H(10) 103(3) . . . no H(9) C(8) H(10) 105(4) . . . no P(1) C(9) C(10) 121.1(3) . . . yes P(1) C(9) C(14) 119.3(2) . . . yes C(10) C(9) C(14) 119.4(3) . . . yes C(9) C(10) C(11) 119.8(4) . . . yes C(9) C(10) H(11) 122(2) . . . no C(11) C(10) H(11) 118(2) . . . no C(10) C(11) C(12) 119.7(4) . . . yes C(10) C(11) H(12) 116(3) . . . no C(12) C(11) H(12) 124(3) . . . no C(11) C(12) C(13) 120.9(4) . . . yes C(11) C(12) H(13) 120(3) . . . no C(13) C(12) H(13) 119(3) . . . no C(12) C(13) C(14) 120.2(4) . . . yes C(12) C(13) H(14) 119(2) . . . no C(14) C(13) H(14) 120(2) . . . no C(9) C(14) C(13) 120.0(4) . . . yes C(9) C(14) H(15) 122(2) . . . no C(13) C(14) H(15) 118(2) . . . no P(1) C(15) C(16) 118.3(2) . . . yes P(1) C(15) C(20) 122.3(3) . . . yes C(16) C(15) C(20) 119.3(3) . . . yes C(15) C(16) C(17) 120.8(4) . . . yes C(15) C(16) H(16) 119(2) . . . no C(17) C(16) H(16) 120(2) . . . no C(16) C(17) C(18) 120.1(4) . . . yes C(16) C(17) H(17) 123(3) . . . no C(18) C(17) H(17) 117(3) . . . no C(17) C(18) C(19) 119.9(4) . . . yes C(17) C(18) H(18) 121(3) . . . no C(19) C(18) H(18) 119(3) . . . no C(18) C(19) C(20) 120.8(4) . . . yes C(18) C(19) H(19) 122(3) . . . no C(20) C(19) H(19) 117(3) . . . no C(15) C(20) C(19) 119.1(4) . . . yes C(15) C(20) H(20) 117(2) . . . no C(19) C(20) H(20) 124(2) . . . no Cl(1) C(21) Cl(2) 112.5(2) . . . yes Cl(1) C(21) H(21) 103(4) . . . no Cl(1) C(21) H(22) 105(2) . . . no Cl(2) C(21) H(21) 107(4) . . . no Cl(2) C(21) H(22) 106(3) . . . no H(21) C(21) H(22) 124(5) . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(2) C(7) 3.512(3) . 2_656 no Cl(2) C(8) 3.563(5) . 2_656 no O(1) C(21) 3.134(5) . 2_656 no O(2) C(21) 3.288(5) . 1_565 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru(1) P(1) C(9) C(10) . . . . 97.6(3) no Ru(1) P(1) C(9) C(14) . . . . -78.2(2) no Ru(1) P(1) C(15) C(16) . . . . 40.5(3) no Ru(1) P(1) C(15) C(20) . . . . -137.7(2) no Ru(1) P(1) C(9) C(10) . 2_666 2_666 2_666 -97.6(3) no Ru(1) P(1) C(9) C(14) . 2_666 2_666 2_666 78.2(2) no Ru(1) P(1) C(15) C(16) . 2_666 2_666 2_666 -40.5(3) no Ru(1) P(1) C(15) C(20) . 2_666 2_666 2_666 137.7(2) no Ru(1) O(1) C(2) C(1) . . . . 175.5(2) no Ru(1) O(1) C(2) C(3) . . . . -4.0(4) no Ru(1) O(1) C(2) C(1) . 2_666 2_666 2_666 -175.5(2) no Ru(1) O(1) C(2) C(3) . 2_666 2_666 2_666 4.0(4) no Ru(1) O(2) C(4) C(3) . . . . 5.4(4) no Ru(1) O(2) C(4) C(5) . . . . -176.0(2) no Ru(1) O(2) C(4) C(3) . 2_666 2_666 2_666 -5.4(4) no Ru(1) O(2) C(4) C(5) . 2_666 2_666 2_666 176.0(2) no P(1) Ru(1) O(1) C(2) . . . . 99.8(2) no P(1) Ru(1) O(1) C(2) . . 2_666 2_666 80.2(2) no P(1) Ru(1) O(2) C(4) . . . . -99.0(2) no P(1) Ru(1) O(2) C(4) . . 2_666 2_666 -81.0(2) no P(1) C(9) C(10) C(11) . . . . -176.5(3) no P(1) C(9) C(14) C(13) . . . . 176.7(3) no P(1) C(15) C(16) C(17) . . . . -178.9(3) no P(1) C(15) C(20) C(19) . . . . 178.4(3) no O(1) Ru(1) P(1) C(6) . . . . 72.4(1) no O(1) Ru(1) P(1) C(9) . . . . -45.0(1) no O(1) Ru(1) P(1) C(15) . . . . -166.0(1) no O(1) Ru(1) P(1) C(6) . . 2_666 2_666 107.6(1) no O(1) Ru(1) P(1) C(9) . . 2_666 2_666 -135.0(1) no O(1) Ru(1) P(1) C(15) . . 2_666 2_666 -14.0(1) no O(1) Ru(1) O(2) C(4) . . . . -10.2(2) no O(1) Ru(1) O(2) C(4) . . 2_666 2_666 -169.8(2) no O(1) C(2) C(3) C(4) . . . . -5.5(6) no O(2) Ru(1) P(1) C(6) . . . . 165.8(1) no O(2) Ru(1) P(1) C(9) . . . . 48.3(1) no O(2) Ru(1) P(1) C(15) . . . . -72.7(1) no O(2) Ru(1) P(1) C(6) . . 2_666 2_666 14.2(1) no O(2) Ru(1) P(1) C(9) . . 2_666 2_666 131.7(1) no O(2) Ru(1) P(1) C(15) . . 2_666 2_666 -107.3(1) no O(2) Ru(1) O(1) C(2) . . . . 9.7(2) no O(2) Ru(1) O(1) C(2) . . 2_666 2_666 170.3(2) no O(2) C(4) C(3) C(2) . . . . 4.7(6) no C(1) C(2) C(3) C(4) . . . . 175.0(3) no C(2) C(3) C(4) C(5) . . . . -173.9(4) no C(6) P(1) C(9) C(10) . . . . -26.8(3) no C(6) P(1) C(9) C(14) . . . . 157.4(2) no C(6) P(1) C(15) C(16) . . . . 167.9(3) no C(6) P(1) C(15) C(20) . . . . -10.3(3) no C(9) P(1) C(15) C(16) . . . . -85.5(3) no C(9) P(1) C(15) C(20) . . . . 96.4(3) no C(9) C(10) C(11) C(12) . . . . -0.7(6) no C(9) C(14) C(13) C(12) . . . . 0.5(5) no C(10) C(9) P(1) C(15) . . . . -133.8(3) no C(10) C(9) C(14) C(13) . . . . 0.8(5) no C(10) C(11) C(12) C(13) . . . . 2.1(7) no C(11) C(10) C(9) C(14) . . . . -0.7(5) no C(11) C(12) C(13) C(14) . . . . -2.0(6) no C(14) C(9) P(1) C(15) . . . . 50.4(3) no C(15) C(16) C(17) C(18) . . . . 1.0(6) no C(15) C(20) C(19) C(18) . . . . -0.2(6) no C(16) C(15) C(20) C(19) . . . . 0.2(5) no C(16) C(17) C(18) C(19) . . . . -1.0(6) no C(17) C(16) C(15) C(20) . . . . -0.6(5) no C(17) C(18) C(19) C(20) . . . . 0.6(6) no #------------------------------------------------------------------------------ # start Validation Reply Form _vrf_PLAT027_mat12a ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 60.00 Deg. RESPONSE: ... Data can only be collected to 2theta 120 deg on a AFC6R diffractometer when the evacuated beam tunnel in used. ; # end Validation Reply Form #===END data_mat13 _database_code_depnum_ccdc_archive 'CCDC 631385' #------------------------------------------------------------------------------ _audit_creation_date 1998-07-01 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 9.7900(9) _cell_length_b 11.1192(8) _cell_length_c 11.1518(9) _cell_angle_alpha 104.946(6) _cell_angle_beta 93.248(7) _cell_angle_gamma 97.520(7) _cell_volume 1157.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 193.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 45.8 _cell_measurement_theta_max 53.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description rhomboid _exptl_crystal_colour green _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1062.60 _chemical_formula_analytical ? _chemical_formula_sum 'C42 H44 Cl4 F6 O4 P3 Ru ' _chemical_formula_moiety ' C40 H40 O4 P2 Ru +, P F6 - , 2(C H2 Cl2) ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 539.00 _exptl_absorpt_coefficient_mu 6.407 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.747 _exptl_absorpt_correction_T_min 0.518 _exptl_special_details ; The scan width was (1.30+0.30tan\q)\% with an \w scan speed of 32\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 193.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.62 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3678 _reflns_number_total 3443 _reflns_number_gt 2737 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.03076 _diffrn_reflns_av_sigmaI/netI 0.080 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 60.03 _diffrn_measured_fraction_theta_max 1.0 _diffrn_reflns_theta_full 60 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.03213 _diffrn_orient_matrix_UB_12 -0.01786 _diffrn_orient_matrix_UB_13 -0.09044 _diffrn_orient_matrix_UB_21 0.05452 _diffrn_orient_matrix_UB_22 0.08163 _diffrn_orient_matrix_UB_23 -0.00289 _diffrn_orient_matrix_UB_31 0.08189 _diffrn_orient_matrix_UB_32 -0.04341 _diffrn_orient_matrix_UB_33 -0.02244 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 42 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 44 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 4 0.348 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 6 0.069 0.053 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 3 0.283 0.434 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 1 -0.105 3.296 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.5000 0.5000 0.5000 0.0207(1) 1.0 S Uani d ? Cl(1) 0.6085(1) 1.0079(1) 0.6774(1) 0.0721(5) 1.000 . Uani d ? Cl(2) 0.8924(1) 1.0188(1) 0.6155(1) 0.0619(4) 1.000 . Uani d ? P(1) 0.5264(1) 0.49321(8) 0.71272(8) 0.0244(3) 1.000 . Uani d ? P(2) 1.0000 1.0000 1.0000 0.0404(5) 1.0 S Uani d ? F(1) 0.9643(3) 1.1074(2) 0.9376(2) 0.0568(9) 1.000 . Uani d ? F(2) 1.0318(3) 0.9183(2) 0.8671(2) 0.0609(9) 1.000 . Uani d ? F(3) 0.8422(3) 0.9346(3) 0.9713(3) 0.0634(9) 1.000 . Uani d ? O(1) 0.6859(3) 0.6087(2) 0.5248(2) 0.0258(7) 1.000 . Uani d ? O(2) 0.5902(3) 0.3450(2) 0.4522(2) 0.0263(7) 1.000 . Uani d ? C(1) 0.9070(5) 0.6757(4) 0.4733(5) 0.039(1) 1.000 . Uani d ? C(2) 0.7898(4) 0.5724(3) 0.4686(3) 0.0260(9) 1.000 . Uani d ? C(3) 0.8013(4) 0.4484(4) 0.4074(4) 0.030(1) 1.000 . Uani d ? C(4) 0.7075(4) 0.3415(4) 0.4071(4) 0.029(1) 1.000 . Uani d ? C(5) 0.7436(5) 0.2129(4) 0.3574(5) 0.041(1) 1.000 . Uani d ? C(6) 0.4848(4) 0.6254(4) 0.8207(4) 0.032(1) 1.000 . Uani d ? C(7) 0.4545(5) 0.7138(4) 0.8932(4) 0.045(1) 1.000 D Uani d ? C(8) 0.4158(7) 0.8210(5) 0.9824(5) 0.093(2) 1.000 D Uani d ? C(9) 0.7044(4) 0.4873(3) 0.7668(3) 0.0271(9) 1.000 . Uani d ? C(10) 0.7994(4) 0.5981(4) 0.8024(4) 0.033(1) 1.000 . Uani d ? C(11) 0.9350(5) 0.5957(4) 0.8392(4) 0.043(1) 1.000 . Uani d ? C(12) 0.9786(5) 0.4834(5) 0.8417(4) 0.044(1) 1.000 . Uani d ? C(13) 0.8867(5) 0.3732(5) 0.8057(5) 0.046(1) 1.000 . Uani d ? C(14) 0.7503(5) 0.3746(4) 0.7675(4) 0.038(1) 1.000 . Uani d ? C(15) 0.4205(4) 0.3599(3) 0.7439(3) 0.0264(9) 1.000 . Uani d ? C(16) 0.4100(4) 0.2428(4) 0.6570(4) 0.031(1) 1.000 . Uani d ? C(17) 0.3267(4) 0.1396(4) 0.6749(4) 0.035(1) 1.000 . Uani d ? C(18) 0.2550(5) 0.1519(4) 0.7782(4) 0.040(1) 1.000 . Uani d ? C(19) 0.2655(5) 0.2664(5) 0.8646(4) 0.045(1) 1.000 . Uani d ? C(20) 0.3465(4) 0.3711(4) 0.8491(4) 0.036(1) 1.000 . Uani d ? C(21) 0.7598(6) 0.9389(5) 0.6786(5) 0.053(1) 1.000 . Uani d ? H(1) 0.873(4) 0.729(4) 0.424(4) 0.047 1.000 . Uiso d ? H(2) 0.988(5) 0.639(4) 0.442(4) 0.047 1.000 . Uiso d ? H(3) 0.931(5) 0.720(4) 0.557(4) 0.047 1.000 . Uiso d ? H(4) 0.881(4) 0.432(4) 0.371(4) 0.037 1.000 . Uiso d ? H(5) 0.665(5) 0.154(4) 0.311(4) 0.050 1.000 . Uiso d ? H(6) 0.770(5) 0.190(4) 0.425(4) 0.050 1.000 . Uiso d ? H(7) 0.805(5) 0.208(4) 0.290(4) 0.050 1.000 . Uiso d ? H(8) 0.474(3) 0.840(3) 1.057(2) 0.110 1.000 D Uiso d ? H(9) 0.425(4) 0.891(1) 0.949(2) 0.110 1.000 D Uiso d ? H(10) 0.323(2) 0.802(2) 0.999(3) 0.110 1.000 D Uiso d ? H(11) 0.764(4) 0.671(4) 0.804(4) 0.040 1.000 . Uiso d ? H(12) 1.000(5) 0.672(4) 0.867(4) 0.051 1.000 . Uiso d ? H(13) 1.063(5) 0.482(4) 0.865(4) 0.054 1.000 . Uiso d ? H(14) 0.909(5) 0.291(4) 0.795(4) 0.055 1.000 . Uiso d ? H(15) 0.686(4) 0.298(4) 0.738(4) 0.046 1.000 . Uiso d ? H(16) 0.443(4) 0.234(4) 0.581(4) 0.036 1.000 . Uiso d ? H(17) 0.321(4) 0.060(4) 0.620(4) 0.041 1.000 . Uiso d ? H(18) 0.203(4) 0.088(4) 0.792(4) 0.047 1.000 . Uiso d ? H(19) 0.220(5) 0.273(4) 0.928(4) 0.055 1.000 . Uiso d ? H(20) 0.358(4) 0.445(4) 0.911(4) 0.043 1.000 . Uiso d ? H(21) 0.734(5) 0.860(5) 0.624(4) 0.062 1.000 . Uiso d ? H(22) 0.786(5) 0.946(4) 0.767(4) 0.062 1.000 . Uiso d ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0211(2) 0.0194(2) 0.0224(2) 0.0014(2) 0.0059(2) 0.0067(2) Cl(1) 0.0506(8) 0.0595(8) 0.098(1) 0.0152(7) 0.0111(8) 0.0013(8) Cl(2) 0.0534(8) 0.0687(9) 0.0562(8) -0.0056(6) 0.0064(6) 0.0109(6) P(1) 0.0276(6) 0.0235(5) 0.0225(5) 0.0024(4) 0.0060(4) 0.0066(4) P(2) 0.051(1) 0.0361(9) 0.0348(9) -0.0026(7) 0.0124(7) 0.0133(7) F(1) 0.080(2) 0.046(2) 0.053(2) 0.009(1) 0.013(1) 0.027(1) F(2) 0.088(2) 0.052(2) 0.042(1) 0.006(2) 0.025(1) 0.009(1) F(3) 0.052(2) 0.076(2) 0.061(2) -0.015(1) 0.008(1) 0.029(2) O(1) 0.024(1) 0.024(1) 0.029(1) 0.0003(9) 0.009(1) 0.007(1) O(2) 0.027(1) 0.022(1) 0.031(1) 0.005(1) 0.010(1) 0.008(1) C(1) 0.024(2) 0.033(2) 0.060(3) -0.002(2) 0.008(2) 0.017(2) C(2) 0.024(2) 0.028(2) 0.027(2) 0.001(1) 0.006(1) 0.010(1) C(3) 0.024(2) 0.032(2) 0.039(2) 0.009(1) 0.014(2) 0.013(2) C(4) 0.025(2) 0.031(2) 0.032(2) 0.008(1) 0.004(2) 0.007(2) C(5) 0.041(3) 0.033(2) 0.051(3) 0.012(2) 0.016(2) 0.008(2) C(6) 0.037(2) 0.029(2) 0.028(2) 0.003(2) 0.005(2) 0.007(1) C(7) 0.057(3) 0.040(2) 0.036(3) 0.013(2) 0.004(2) 0.004(2) C(8) 0.148(7) 0.060(4) 0.064(4) 0.049(4) 0.030(4) -0.019(3) C(9) 0.028(2) 0.032(2) 0.021(2) 0.002(1) 0.006(2) 0.006(2) C(10) 0.035(2) 0.029(2) 0.033(2) 0.002(2) 0.005(2) 0.006(2) C(11) 0.031(2) 0.047(2) 0.043(3) -0.004(2) 0.006(2) 0.002(2) C(12) 0.030(2) 0.057(2) 0.043(3) 0.012(2) 0.003(2) 0.008(2) C(13) 0.039(2) 0.046(2) 0.057(3) 0.015(2) 0.006(2) 0.015(2) C(14) 0.038(2) 0.033(2) 0.044(3) 0.004(2) 0.003(2) 0.013(2) C(15) 0.026(2) 0.029(2) 0.025(2) 0.000(1) 0.005(1) 0.012(1) C(16) 0.035(2) 0.030(2) 0.028(2) 0.004(2) 0.008(2) 0.010(1) C(17) 0.035(2) 0.029(2) 0.040(2) 0.000(2) 0.002(2) 0.012(2) C(18) 0.037(3) 0.044(2) 0.048(2) -0.002(2) 0.012(2) 0.029(2) C(19) 0.040(3) 0.056(2) 0.043(3) 0.001(2) 0.018(2) 0.021(2) C(20) 0.036(3) 0.045(2) 0.028(2) 0.006(2) 0.013(2) 0.009(2) C(21) 0.049(2) 0.055(3) 0.052(3) 0.008(2) 0.007(2) 0.011(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2737 _refine_ls_number_parameters 340 _refine_ls_number_restraints 9 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_all 0.0452 _refine_ls_wR_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0414 _refine_ls_goodness_of_fit_all 1.306 _refine_ls_goodness_of_fit_ref 1.362 _refine_ls_shift/su_max 0.0943 _refine_ls_shift/su_mean 0.0030 _refine_diff_density_min -0.46 _refine_diff_density_max 0.55 #------------------------------------------------------------------------------ _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) P(1) 2.393(1) . . yes Ru(1) P(1) 2.393(1) . 2_666 yes Ru(1) O(1) 2.011(3) . . yes Ru(1) O(1) 2.011(3) . 2_666 yes Ru(1) O(2) 2.003(3) . . yes Ru(1) O(2) 2.003(3) . 2_666 yes Cl(1) C(21) 1.756(6) . . yes Cl(2) C(21) 1.760(6) . . yes P(1) C(6) 1.753(5) . . yes P(1) C(9) 1.826(4) . . yes P(1) C(15) 1.816(4) . . yes P(2) F(1) 1.595(3) . . yes P(2) F(1) 1.595(3) . 2_777 yes P(2) F(2) 1.597(3) . . yes P(2) F(2) 1.597(3) . 2_777 yes P(2) F(3) 1.597(3) . . yes P(2) F(3) 1.597(3) . 2_777 yes O(1) C(2) 1.280(5) . . yes O(2) C(4) 1.281(5) . . yes C(1) C(2) 1.503(6) . . yes C(1) H(1) 0.98(5) . . no C(1) H(2) 0.98(5) . . no C(1) H(3) 0.93(5) . . no C(2) C(3) 1.394(6) . . yes C(3) C(4) 1.403(6) . . yes C(3) H(4) 0.92(5) . . no C(4) C(5) 1.490(6) . . yes C(5) H(5) 0.97(5) . . no C(5) H(6) 0.89(5) . . no C(5) H(7) 0.98(5) . . no C(6) C(7) 1.185(6) . . yes C(7) C(8) 1.451(7) . . yes C(8) H(8) 0.945(7) . . no C(8) H(9) 0.945(7) . . no C(8) H(10) 0.942(7) . . no C(9) C(10) 1.395(6) . . yes C(9) C(14) 1.388(6) . . yes C(10) C(11) 1.372(7) . . yes C(10) H(11) 0.92(5) . . no C(11) C(12) 1.378(8) . . yes C(11) H(12) 0.96(5) . . no C(12) C(13) 1.374(8) . . yes C(12) H(13) 0.86(5) . . no C(13) C(14) 1.381(7) . . yes C(13) H(14) 0.95(5) . . no C(14) H(15) 0.96(5) . . no C(15) C(16) 1.395(6) . . yes C(15) C(20) 1.400(6) . . yes C(16) C(17) 1.383(6) . . yes C(16) H(16) 0.91(5) . . no C(17) C(18) 1.369(7) . . yes C(17) H(17) 0.93(5) . . no C(18) C(19) 1.371(8) . . yes C(18) H(18) 0.87(5) . . no C(19) C(20) 1.376(7) . . yes C(19) H(19) 0.85(5) . . no C(20) H(20) 0.91(5) . . no C(21) H(21) 0.92(5) . . no C(21) H(22) 0.98(5) . . 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 P(1) Ru(1) P(1) 180.00 . . 2_666 yes P(1) Ru(1) O(1) 89.64(8) . . . yes P(1) Ru(1) O(1) 90.36(8) . . 2_666 yes P(1) Ru(1) O(2) 88.88(9) . . . yes P(1) Ru(1) O(2) 91.12(9) . . 2_666 yes P(1) Ru(1) O(1) 90.36(8) 2_666 . . yes P(1) Ru(1) O(1) 89.64(8) 2_666 . 2_666 yes P(1) Ru(1) O(2) 91.12(9) 2_666 . . yes P(1) Ru(1) O(2) 88.88(9) 2_666 . 2_666 yes O(1) Ru(1) O(1) 180.00 . . 2_666 yes O(1) Ru(1) O(2) 90.3(1) . . . yes O(1) Ru(1) O(2) 89.7(1) . . 2_666 yes O(1) Ru(1) O(2) 89.7(1) 2_666 . . yes O(1) Ru(1) O(2) 90.3(1) 2_666 . 2_666 yes O(2) Ru(1) O(2) 180.00 . . 2_666 yes Ru(1) P(1) C(6) 114.6(2) . . . yes Ru(1) P(1) C(9) 113.1(1) . . . yes Ru(1) P(1) C(15) 113.8(1) . . . yes C(6) P(1) C(9) 103.2(2) . . . yes C(6) P(1) C(15) 104.7(2) . . . yes C(9) P(1) C(15) 106.4(2) . . . yes F(1) P(2) F(1) 180.00 . . 2_777 yes F(1) P(2) F(2) 89.4(2) . . . yes F(1) P(2) F(2) 90.6(2) . . 2_777 yes F(1) P(2) F(3) 89.9(2) . . . yes F(1) P(2) F(3) 90.1(2) . . 2_777 yes F(1) P(2) F(2) 90.6(2) 2_777 . . yes F(1) P(2) F(2) 89.4(2) 2_777 . 2_777 yes F(1) P(2) F(3) 90.1(2) 2_777 . . yes F(1) P(2) F(3) 89.9(2) 2_777 . 2_777 yes F(2) P(2) F(2) 180.0000(1) . . 2_777 yes F(2) P(2) F(3) 89.5(2) . . . yes F(2) P(2) F(3) 90.5(2) . . 2_777 yes F(2) P(2) F(3) 90.5(2) 2_777 . . yes F(2) P(2) F(3) 89.5(2) 2_777 . 2_777 yes F(3) P(2) F(3) 180.00 . . 2_777 yes Ru(1) O(1) C(2) 122.9(3) . . . yes Ru(1) O(2) C(4) 124.2(3) . . . yes C(2) C(1) H(1) 107(3) . . . no C(2) C(1) H(2) 110(3) . . . no C(2) C(1) H(3) 108(3) . . . no H(1) C(1) H(2) 113(4) . . . no H(1) C(1) H(3) 112(4) . . . no H(2) C(1) H(3) 108(4) . . . no O(1) C(2) C(1) 114.8(4) . . . yes O(1) C(2) C(3) 125.5(4) . . . yes C(1) C(2) C(3) 119.6(4) . . . yes C(2) C(3) C(4) 125.8(4) . . . yes C(2) C(3) H(4) 119(3) . . . no C(4) C(3) H(4) 115(3) . . . no O(2) C(4) C(3) 124.3(4) . . . yes O(2) C(4) C(5) 115.2(4) . . . yes C(3) C(4) C(5) 120.4(4) . . . yes C(4) C(5) H(5) 112(3) . . . no C(4) C(5) H(6) 104(3) . . . no C(4) C(5) H(7) 113(3) . . . no H(5) C(5) H(6) 110(5) . . . no H(5) C(5) H(7) 99(4) . . . no H(6) C(5) H(7) 119(5) . . . no P(1) C(6) C(7) 178.9(5) . . . yes C(6) C(7) C(8) 179.3(6) . . . yes C(7) C(8) H(8) 109.5(9) . . . no C(7) C(8) H(9) 109.4(9) . . . no C(7) C(8) H(10) 109.6(9) . . . no H(8) C(8) H(9) 109(1) . . . no H(8) C(8) H(10) 109(1) . . . no H(9) C(8) H(10) 109(1) . . . no P(1) C(9) C(10) 119.4(4) . . . yes P(1) C(9) C(14) 121.9(4) . . . yes C(10) C(9) C(14) 118.6(4) . . . yes C(9) C(10) C(11) 120.6(5) . . . yes C(9) C(10) H(11) 116(3) . . . no C(11) C(10) H(11) 123(3) . . . no C(10) C(11) C(12) 120.2(5) . . . yes C(10) C(11) H(12) 121(3) . . . no C(12) C(11) H(12) 119(3) . . . no C(11) C(12) C(13) 120.0(5) . . . yes C(11) C(12) H(13) 120(4) . . . no C(13) C(12) H(13) 120(4) . . . no C(12) C(13) C(14) 120.3(5) . . . yes C(12) C(13) H(14) 126(3) . . . no C(14) C(13) H(14) 114(3) . . . no C(9) C(14) C(13) 120.4(5) . . . yes C(9) C(14) H(15) 119(3) . . . no C(13) C(14) H(15) 121(3) . . . no P(1) C(15) C(16) 118.1(3) . . . yes P(1) C(15) C(20) 122.6(4) . . . yes C(16) C(15) C(20) 119.3(4) . . . yes C(15) C(16) C(17) 120.0(4) . . . yes C(15) C(16) H(16) 122(3) . . . no C(17) C(16) H(16) 117(3) . . . no C(16) C(17) C(18) 120.1(5) . . . yes C(16) C(17) H(17) 122(3) . . . no C(18) C(17) H(17) 118(3) . . . no C(17) C(18) C(19) 120.2(5) . . . yes C(17) C(18) H(18) 122(3) . . . no C(19) C(18) H(18) 118(3) . . . no C(18) C(19) C(20) 121.1(5) . . . yes C(18) C(19) H(19) 119(4) . . . no C(20) C(19) H(19) 119(4) . . . no C(15) C(20) C(19) 119.2(5) . . . yes C(15) C(20) H(20) 121(3) . . . no C(19) C(20) H(20) 120(3) . . . no Cl(1) C(21) Cl(2) 110.9(3) . . . yes Cl(1) C(21) H(21) 103(4) . . . no Cl(1) C(21) H(22) 105(3) . . . no Cl(2) C(21) H(21) 107(4) . . . no Cl(2) C(21) H(22) 111(3) . . . no H(21) C(21) H(22) 119(5) . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(17) 3.291(5) . 1_565 no Cl(1) C(16) 3.498(5) . 1_565 no Cl(2) Cl(2) 3.396(3) . 2_776 no Cl(2) F(1) 3.474(4) . . no Cl(2) F(2) 3.545(4) . . no F(1) C(21) 3.381(7) . . no F(1) C(19) 3.483(6) . 1_665 no F(1) C(18) 3.487(6) . 1_665 no F(1) C(11) 3.563(6) . 2_777 no F(2) C(21) 3.366(7) . . no F(2) C(11) 3.516(6) . . no F(2) C(18) 3.548(6) . 1_665 no F(2) C(5) 3.580(6) . 2_766 no F(3) C(18) 3.328(6) . 2_667 no F(3) C(21) 3.332(7) . . no F(3) C(19) 3.341(6) . 2_667 no O(1) C(21) 3.586(7) . . no C(12) C(12) 3.45(1) . 2_767 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru(1) P(1) C(9) C(10) . . . . 80.1(4) no Ru(1) P(1) C(9) C(14) . . . . -96.6(4) no Ru(1) P(1) C(15) C(16) . . . . 41.6(4) no Ru(1) P(1) C(15) C(20) . . . . -136.5(4) no Ru(1) P(1) C(9) C(10) . 2_666 2_666 2_666 -80.1(4) no Ru(1) P(1) C(9) C(14) . 2_666 2_666 2_666 96.6(4) no Ru(1) P(1) C(15) C(16) . 2_666 2_666 2_666 -41.6(4) no Ru(1) P(1) C(15) C(20) . 2_666 2_666 2_666 136.5(4) no Ru(1) O(1) C(2) C(1) . . . . 165.2(3) no Ru(1) O(1) C(2) C(3) . . . . -15.7(6) no Ru(1) O(1) C(2) C(1) . 2_666 2_666 2_666 -165.2(3) no Ru(1) O(1) C(2) C(3) . 2_666 2_666 2_666 15.7(6) no Ru(1) O(2) C(4) C(3) . . . . 13.1(6) no Ru(1) O(2) C(4) C(5) . . . . -169.7(3) no Ru(1) O(2) C(4) C(3) . 2_666 2_666 2_666 -13.1(6) no Ru(1) O(2) C(4) C(5) . 2_666 2_666 2_666 169.7(3) no P(1) Ru(1) O(1) C(2) . . . . 114.7(3) no P(1) Ru(1) O(1) C(2) . . 2_666 2_666 65.3(3) no P(1) Ru(1) O(2) C(4) . . . . -114.4(3) no P(1) Ru(1) O(2) C(4) . . 2_666 2_666 -65.6(3) no P(1) C(9) C(10) C(11) . . . . -177.7(4) no P(1) C(9) C(14) C(13) . . . . 178.2(4) no P(1) C(15) C(16) C(17) . . . . -177.8(4) no P(1) C(15) C(20) C(19) . . . . 178.3(4) no O(1) Ru(1) P(1) C(6) . . . . 81.5(2) no O(1) Ru(1) P(1) C(9) . . . . -36.5(2) no O(1) Ru(1) P(1) C(15) . . . . -158.0(2) no O(1) Ru(1) P(1) C(6) . . 2_666 2_666 98.5(2) no O(1) Ru(1) P(1) C(9) . . 2_666 2_666 -143.5(2) no O(1) Ru(1) P(1) C(15) . . 2_666 2_666 -22.0(2) no O(1) Ru(1) O(2) C(4) . . . . -24.8(3) no O(1) Ru(1) O(2) C(4) . . 2_666 2_666 -155.2(3) no O(1) C(2) C(3) C(4) . . . . -6.5(8) no O(2) Ru(1) P(1) C(6) . . . . 171.8(2) no O(2) Ru(1) P(1) C(9) . . . . 53.9(2) no O(2) Ru(1) P(1) C(15) . . . . -67.7(2) no O(2) Ru(1) P(1) C(6) . . 2_666 2_666 8.2(2) no O(2) Ru(1) P(1) C(9) . . 2_666 2_666 126.1(2) no O(2) Ru(1) P(1) C(15) . . 2_666 2_666 -112.3(2) no O(2) Ru(1) O(1) C(2) . . . . 25.8(3) no O(2) Ru(1) O(1) C(2) . . 2_666 2_666 154.2(3) no O(2) C(4) C(3) C(2) . . . . 8.1(8) no C(1) C(2) C(3) C(4) . . . . 172.6(5) no C(2) C(3) C(4) C(5) . . . . -169.1(5) no C(6) P(1) C(9) C(10) . . . . -44.3(4) no C(6) P(1) C(9) C(14) . . . . 139.0(4) no C(6) P(1) C(15) C(16) . . . . 167.6(4) no C(6) P(1) C(15) C(20) . . . . -10.5(4) no C(9) P(1) C(15) C(16) . . . . -83.6(4) no C(9) P(1) C(15) C(20) . . . . 98.4(4) no C(9) C(10) C(11) C(12) . . . . -0.2(8) no C(9) C(14) C(13) C(12) . . . . -0.9(9) no C(10) C(9) P(1) C(15) . . . . -154.3(4) no C(10) C(9) C(14) C(13) . . . . 1.5(8) no C(10) C(11) C(12) C(13) . . . . 0.9(9) no C(11) C(10) C(9) C(14) . . . . -0.9(7) no C(11) C(12) C(13) C(14) . . . . -0.3(9) no C(14) C(9) P(1) C(15) . . . . 29.1(4) no C(15) C(16) C(17) C(18) . . . . -0.4(8) no C(15) C(20) C(19) C(18) . . . . -0.7(8) no C(16) C(15) C(20) C(19) . . . . 0.2(7) no C(16) C(17) C(18) C(19) . . . . -0.1(8) no C(17) C(16) C(15) C(20) . . . . 0.3(7) no C(17) C(18) C(19) C(20) . . . . 0.7(9) no #------------------------------------------------------------------------------ # start Validation Reply Form #_vrf_PLAT027_mat13 #; #PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 60.00 Deg. #RESPONSE: ... #Data can only be collected to 2theta 120 deg on a AFC6R diffractometer #when the evacuated beam tunnel in used. #; # end Validation Reply Form #===END data_mat14 _database_code_depnum_ccdc_archive 'CCDC 631386' #------------------------------------------------------------------------------ _audit_creation_date 1998-10-20 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 16.317(4) _cell_length_b 16.469(6) _cell_length_c 18.975(4) _cell_angle_alpha 65.46(2) _cell_angle_beta 66.17(2) _cell_angle_gamma 60.76(2) _cell_volume 3915(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.7 _cell_measurement_theta_max 20.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description hexprism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1580.48 _chemical_formula_analytical ? _chemical_formula_sum 'C81 H82 Cl2 O8 P4 Ru2 ' _chemical_formula_moiety ' 2(C40 H40 O4 P2 Ru) , C H2 Cl2' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1628.00 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.918 _exptl_absorpt_correction_T_min 0.882 _exptl_special_details ; The scan width was (1.10+0.34tan\q)\% with an \w scan speed of 8\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -11.82 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 18715 _reflns_number_total 18081 _reflns_number_gt 9045 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.03038 _diffrn_reflns_av_sigmaI/netI 0.120 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.55 _diffrn_measured_fraction_theta_max 1.0 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06942 _diffrn_orient_matrix_UB_12 0.01060 _diffrn_orient_matrix_UB_13 0.01150 _diffrn_orient_matrix_UB_21 0.00212 _diffrn_orient_matrix_UB_22 0.03185 _diffrn_orient_matrix_UB_23 -0.05815 _diffrn_orient_matrix_UB_31 0.02115 _diffrn_orient_matrix_UB_32 -0.06407 _diffrn_orient_matrix_UB_33 -0.00854 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 162 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 164 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 4 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru 0 4 -1.420 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.65745(3) 0.13728(3) 0.12973(2) 0.0406(1) 1.000 . Uani d ? Ru(2) 0.94000(3) 0.32890(3) 0.29568(2) 0.0459(1) 1.000 . Uani d ? Cl(1) 0.7176(2) 0.3714(2) -0.1942(2) 0.174(1) 1.000 . Uani d ? Cl(21) 0.6038(3) 0.2786(3) -0.1824(2) 0.192(2) 0.864(4) . Uani d ? Cl(22) 0.726(2) 0.236(2) -0.242(1) 0.191 0.136 . Uiso d ? P(1) 0.70703(9) -0.0170(1) 0.13123(8) 0.0445(4) 1.000 . Uani d ? P(2) 0.54249(9) 0.1260(1) 0.24701(7) 0.0439(4) 1.000 . Uani d ? P(3) 0.8176(1) 0.3318(1) 0.40838(8) 0.0583(5) 1.000 . Uani d ? P(4) 0.90888(9) 0.4875(1) 0.26286(8) 0.0491(4) 1.000 . Uani d ? O(1) 0.5563(2) 0.1832(3) 0.0683(2) 0.054(1) 1.000 . Uani d ? O(2) 0.6253(2) 0.2798(2) 0.1213(2) 0.056(1) 1.000 . Uani d ? O(3) 0.7598(2) 0.1044(2) 0.1849(2) 0.050(1) 1.000 . Uani d ? O(4) 0.7535(2) 0.1614(2) 0.0166(2) 0.051(1) 1.000 . Uani d ? O(5) 0.8505(2) 0.3542(2) 0.2313(2) 0.053(1) 1.000 . Uani d ? O(6) 1.0565(2) 0.3178(2) 0.1933(2) 0.053(1) 1.000 . Uani d ? O(7) 1.0380(2) 0.2921(3) 0.3575(2) 0.059(1) 1.000 . Uani d ? O(8) 0.9796(3) 0.1814(3) 0.3113(2) 0.061(1) 1.000 . Uani d ? C(1) 0.4144(4) 0.2831(5) 0.0242(4) 0.095(2) 1.000 . Uani d ? C(2) 0.4909(4) 0.2692(5) 0.0584(3) 0.061(2) 1.000 . Uani d ? C(3) 0.4845(4) 0.3462(4) 0.0761(3) 0.067(2) 1.000 . Uani d ? C(4) 0.5509(4) 0.3493(4) 0.1029(3) 0.061(2) 1.000 . Uani d ? C(5) 0.5327(5) 0.4443(4) 0.1110(4) 0.091(2) 1.000 . Uani d ? C(6) 0.9075(4) 0.0719(5) 0.2026(4) 0.086(2) 1.000 . Uani d ? C(7) 0.8469(4) 0.0966(4) 0.1485(3) 0.056(2) 1.000 . Uani d ? C(8) 0.8883(3) 0.1085(4) 0.0672(3) 0.063(2) 1.000 . Uani d ? C(9) 0.8429(4) 0.1389(4) 0.0076(3) 0.054(2) 1.000 . Uani d ? C(10) 0.9033(4) 0.1474(4) -0.0782(3) 0.074(2) 1.000 . Uani d ? C(11) 0.7949(4) -0.1035(4) 0.1855(3) 0.051(2) 1.000 . Uani d ? C(12) 0.8541(4) -0.1567(4) 0.2222(3) 0.055(2) 1.000 . Uani d ? C(13) 0.9280(4) -0.2207(5) 0.2669(3) 0.083(2) 1.000 . Uani d ? C(14) 0.7669(3) -0.0444(4) 0.0340(3) 0.048(2) 1.000 . Uani d ? C(15) 0.7296(4) 0.0196(4) -0.0314(3) 0.062(2) 1.000 . Uani d ? C(16) 0.7709(5) -0.0048(5) -0.1037(3) 0.079(2) 1.000 . Uani d ? C(17) 0.8490(5) -0.0897(6) -0.1118(4) 0.080(3) 1.000 . Uani d ? C(18) 0.8854(4) -0.1511(5) -0.0476(4) 0.079(2) 1.000 . Uani d ? C(19) 0.8455(4) -0.1295(4) 0.0247(4) 0.066(2) 1.000 . Uani d ? C(20) 0.6154(3) -0.0694(4) 0.1716(3) 0.050(2) 1.000 . Uani d ? C(21) 0.5503(4) -0.0393(4) 0.1278(3) 0.068(2) 1.000 . Uani d ? C(22) 0.4776(4) -0.0750(5) 0.1590(5) 0.087(3) 1.000 . Uani d ? C(23) 0.4693(5) -0.1388(6) 0.2337(5) 0.094(3) 1.000 . Uani d ? C(24) 0.5322(5) -0.1681(5) 0.2772(4) 0.082(2) 1.000 . Uani d ? C(25) 0.6055(4) -0.1341(4) 0.2459(3) 0.061(2) 1.000 . Uani d ? C(26) 0.4362(3) 0.1264(4) 0.2422(3) 0.053(2) 1.000 . Uani d ? C(27) 0.3658(4) 0.1301(4) 0.2349(3) 0.062(2) 1.000 . Uani d ? C(28) 0.2792(4) 0.1344(5) 0.2244(4) 0.092(3) 1.000 . Uani d ? C(29) 0.4903(4) 0.2286(4) 0.2892(3) 0.051(2) 1.000 . Uani d ? C(30) 0.5517(4) 0.2455(4) 0.3101(4) 0.071(2) 1.000 . Uani d ? C(31) 0.5155(6) 0.3210(5) 0.3424(4) 0.095(3) 1.000 . Uani d ? C(32) 0.4205(7) 0.3825(5) 0.3509(4) 0.098(3) 1.000 . Uani d ? C(33) 0.3600(5) 0.3680(5) 0.3295(4) 0.086(2) 1.000 . Uani d ? C(34) 0.3938(4) 0.2914(4) 0.2986(3) 0.065(2) 1.000 . Uani d ? C(35) 0.5712(3) 0.0248(3) 0.3359(3) 0.045(1) 1.000 . Uani d ? C(36) 0.6614(4) -0.0097(4) 0.3499(3) 0.056(2) 1.000 . Uani d ? C(37) 0.6833(4) -0.0820(4) 0.4183(3) 0.062(2) 1.000 . Uani d ? C(38) 0.6168(4) -0.1206(4) 0.4723(3) 0.062(2) 1.000 . Uani d ? C(39) 0.5287(4) -0.0888(4) 0.4584(3) 0.066(2) 1.000 . Uani d ? C(40) 0.5057(4) -0.0164(4) 0.3905(3) 0.056(2) 1.000 . Uani d ? C(41) 0.7911(4) 0.3979(5) 0.1225(3) 0.082(2) 1.000 . Uani d ? C(42) 0.8714(4) 0.3761(4) 0.1555(3) 0.053(2) 1.000 . Uani d ? C(43) 0.9590(4) 0.3804(4) 0.1035(3) 0.060(2) 1.000 . Uani d ? C(44) 1.0445(4) 0.3511(4) 0.1232(3) 0.055(2) 1.000 . Uani d ? C(45) 1.1337(4) 0.3575(4) 0.0565(3) 0.075(2) 1.000 . Uani d ? C(46) 1.1415(5) 0.1999(5) 0.4425(4) 0.103(3) 1.000 . Uani d ? C(47) 1.0784(4) 0.2070(5) 0.3979(3) 0.065(2) 1.000 . Uani d ? C(48) 1.0724(4) 0.1235(4) 0.4036(3) 0.073(2) 1.000 . Uani d ? C(49) 1.0273(4) 0.1140(4) 0.3599(3) 0.064(2) 1.000 . Uani d ? C(50) 1.0390(5) 0.0142(5) 0.3682(4) 0.098(3) 1.000 . Uani d ? C(54) 0.7761(3) 0.2321(4) 0.4464(3) 0.059(2) 1.000 . Uani d ? C(55) 0.7755(4) 0.1965(5) 0.3932(4) 0.078(2) 1.000 . Uani d ? C(56) 0.7434(5) 0.1217(5) 0.4203(4) 0.090(3) 1.000 . Uani d ? C(57) 0.7121(5) 0.0841(5) 0.4992(5) 0.097(3) 1.000 . Uani d ? C(58) 0.7099(5) 0.1191(5) 0.5534(4) 0.101(3) 1.000 . Uani d ? C(59) 0.7429(5) 0.1923(5) 0.5279(4) 0.087(2) 1.000 . Uani d ? C(60) 0.7008(4) 0.4368(4) 0.4067(3) 0.061(2) 1.000 . Uani d ? C(61) 0.6559(4) 0.4598(5) 0.3493(4) 0.079(2) 1.000 . Uani d ? C(62) 0.5679(5) 0.5383(6) 0.3453(5) 0.101(3) 1.000 . Uani d ? C(63) 0.5243(5) 0.5930(6) 0.3983(6) 0.109(3) 1.000 . Uani d ? C(64) 0.5681(6) 0.5710(6) 0.4544(6) 0.108(3) 1.000 . Uani d ? C(65) 0.6556(5) 0.4933(5) 0.4599(4) 0.088(3) 1.000 . Uani d ? C(66) 0.8196(4) 0.5669(4) 0.2084(3) 0.053(2) 1.000 . Uani d ? C(67) 0.7577(4) 0.6175(4) 0.1745(3) 0.062(2) 1.000 . Uani d ? C(68) 0.6815(4) 0.6807(5) 0.1328(4) 0.098(2) 1.000 . Uani d ? C(69) 1.0127(4) 0.5221(4) 0.1972(3) 0.053(2) 1.000 . Uani d ? C(70) 1.1033(4) 0.4646(4) 0.2132(3) 0.067(2) 1.000 . Uani d ? C(71) 1.1819(4) 0.4901(5) 0.1664(4) 0.084(2) 1.000 . Uani d ? C(72) 1.1709(5) 0.5722(5) 0.1034(4) 0.081(2) 1.000 . Uani d ? C(73) 1.0825(5) 0.6288(5) 0.0869(3) 0.076(2) 1.000 . Uani d ? C(74) 1.0037(4) 0.6040(4) 0.1333(3) 0.062(2) 1.000 . Uani d ? C(75) 0.8678(4) 0.5473(4) 0.3408(3) 0.052(2) 1.000 . Uani d ? C(76) 0.9202(5) 0.5081(5) 0.3965(4) 0.096(3) 1.000 . Uani d ? C(77) 0.8888(6) 0.5506(6) 0.4574(5) 0.116(3) 1.000 . Uani d ? C(78) 0.8062(5) 0.6304(6) 0.4625(4) 0.088(3) 1.000 . Uani d ? C(79) 0.7525(5) 0.6689(5) 0.4094(4) 0.081(2) 1.000 . Uani d ? C(80) 0.7835(4) 0.6279(4) 0.3481(3) 0.064(2) 1.000 . Uani d ? C(81) 0.6562(6) 0.2981(6) -0.1378(5) 0.102(3) 0.864 P Uani d ? C(511) 0.847(1) 0.304(1) 0.4980(9) 0.061(4) 0.51(2) PPPPP Uiso d ? C(512) 0.837(1) 0.342(1) 0.4902(9) 0.065(4) 0.492 P Uiso d ? C(521) 0.876(1) 0.286(2) 0.5526(9) 0.082(5) 0.508 P Uiso d ? C(522) 0.860(1) 0.340(2) 0.544(1) 0.092(6) 0.492 P Uiso d ? C(531) 0.910(1) 0.268(2) 0.624(1) 0.109(7) 0.508 P Uiso d ? C(532) 0.890(1) 0.338(2) 0.612(1) 0.119(8) 0.492 P Uiso d ? H(1) 0.4281 0.4037 0.0693 0.080 1.000 . Uiso c ? H(2) 0.9561 0.0942 0.0501 0.076 1.000 . Uiso c ? H(3) 0.6765 0.0794 -0.0271 0.074 1.000 . Uiso c ? H(4) 0.7445 0.0383 -0.1483 0.094 1.000 . Uiso c ? H(5) 0.8770 -0.1052 -0.1615 0.096 1.000 . Uiso c ? H(6) 0.9394 -0.2101 -0.0526 0.094 1.000 . Uiso c ? H(7) 0.8723 -0.1737 0.0689 0.079 1.000 . Uiso c ? H(8) 0.5554 0.0057 0.0764 0.081 1.000 . Uiso c ? H(9) 0.4337 -0.0551 0.1286 0.104 1.000 . Uiso c ? H(10) 0.4192 -0.1627 0.2552 0.112 1.000 . Uiso c ? H(11) 0.5257 -0.2119 0.3292 0.099 1.000 . Uiso c ? H(12) 0.6500 -0.1559 0.2764 0.073 1.000 . Uiso c ? H(13) 0.6187 0.2049 0.3021 0.086 1.000 . Uiso c ? H(14) 0.5573 0.3302 0.3590 0.114 1.000 . Uiso c ? H(15) 0.3968 0.4356 0.3717 0.118 1.000 . Uiso c ? H(16) 0.2937 0.4108 0.3358 0.104 1.000 . Uiso c ? H(17) 0.3507 0.2819 0.2837 0.078 1.000 . Uiso c ? H(18) 0.7081 0.0165 0.3123 0.067 1.000 . Uiso c ? H(19) 0.7448 -0.1050 0.4279 0.074 1.000 . Uiso c ? H(20) 0.6318 -0.1696 0.5197 0.074 1.000 . Uiso c ? H(21) 0.4832 -0.1168 0.4957 0.079 1.000 . Uiso c ? H(22) 0.4443 0.0053 0.3812 0.067 1.000 . Uiso c ? H(23) 0.9608 0.4063 0.0481 0.072 1.000 . Uiso c ? H(24) 1.1020 0.0664 0.4411 0.088 1.000 . Uiso c ? H(25) 0.7971 0.2230 0.3374 0.093 1.000 . Uiso c ? H(26) 0.7437 0.0971 0.3828 0.108 1.000 . Uiso c ? H(27) 0.6913 0.0325 0.5171 0.117 1.000 . Uiso c ? H(28) 0.6857 0.0934 0.6089 0.121 1.000 . Uiso c ? H(29) 0.7430 0.2155 0.5661 0.104 1.000 . Uiso c ? H(30) 0.6851 0.4221 0.3125 0.094 1.000 . Uiso c ? H(31) 0.5376 0.5543 0.3052 0.121 1.000 . Uiso c ? H(32) 0.4636 0.6459 0.3955 0.130 1.000 . Uiso c ? H(33) 0.5385 0.6095 0.4906 0.130 1.000 . Uiso c ? H(34) 0.6849 0.4783 0.5003 0.106 1.000 . Uiso c ? H(35) 1.1112 0.4075 0.2565 0.081 1.000 . Uiso c ? H(36) 1.2436 0.4509 0.1779 0.101 1.000 . Uiso c ? H(37) 1.2250 0.5896 0.0712 0.097 1.000 . Uiso c ? H(38) 1.0752 0.6856 0.0433 0.091 1.000 . Uiso c ? H(39) 0.9424 0.6437 0.1212 0.075 1.000 . Uiso c ? H(40) 0.9781 0.4516 0.3933 0.115 1.000 . Uiso c ? H(41) 0.9256 0.5235 0.4955 0.139 1.000 . Uiso c ? H(42) 0.7857 0.6597 0.5038 0.106 1.000 . Uiso c ? H(43) 0.6936 0.7241 0.4142 0.097 1.000 . Uiso c ? H(44) 0.7460 0.6558 0.3104 0.076 1.000 . Uiso c ? H(45) 0.7009 0.2372 -0.1151 0.122 0.860 . Uiso d ? H(46) 0.6073 0.3258 -0.0962 0.122 0.860 . Uiso d ? H(47) 0.4274 0.3149 -0.0314 0.114 1.000 . Uiso c ? H(48) 0.3523 0.3212 0.0507 0.114 1.000 . Uiso c ? H(49) 0.4154 0.2218 0.0319 0.114 1.000 . Uiso c ? H(50) 0.4763 0.4930 0.0936 0.110 1.000 . Uiso c ? H(51) 0.5232 0.4382 0.1655 0.110 1.000 . Uiso c ? H(52) 0.5869 0.4616 0.0791 0.110 1.000 . Uiso c ? H(53) 0.8909 0.0274 0.2518 0.103 1.000 . Uiso c ? H(54) 0.9743 0.0436 0.1774 0.103 1.000 . Uiso c ? H(55) 0.8954 0.1291 0.2128 0.103 1.000 . Uiso c ? H(56) 0.8815 0.2131 -0.1088 0.089 1.000 . Uiso c ? H(57) 0.9696 0.1255 -0.0796 0.089 1.000 . Uiso c ? H(58) 0.8969 0.1090 -0.1001 0.089 1.000 . Uiso c ? H(59) 0.7302 0.4259 0.1568 0.099 1.000 . Uiso c ? H(60) 0.7957 0.3397 0.1193 0.099 1.000 . Uiso c ? H(61) 0.7966 0.4418 0.0706 0.099 1.000 . Uiso c ? H(62) 1.1545 0.3991 0.0614 0.090 1.000 . Uiso c ? H(63) 1.1185 0.3824 0.0063 0.090 1.000 . Uiso c ? H(64) 1.1840 0.2948 0.0598 0.090 1.000 . Uiso c ? H(65) 1.1168 0.2591 0.4550 0.124 1.000 . Uiso c ? H(66) 1.2061 0.1872 0.4099 0.124 1.000 . Uiso c ? H(67) 1.1410 0.1489 0.4906 0.124 1.000 . Uiso c ? H(68) 1.0668 0.0023 0.3170 0.118 1.000 . Uiso c ? H(69) 0.9773 0.0096 0.3903 0.118 1.000 . Uiso c ? H(70) 1.0803 -0.0323 0.4026 0.118 1.000 . Uiso c ? H(71) 0.9825 -0.2027 0.2421 0.100 1.000 . Uiso c ? H(72) 0.9021 -0.2157 0.3203 0.100 1.000 . Uiso c ? H(73) 0.9477 -0.2855 0.2673 0.100 1.000 . Uiso c ? H(74) 0.2284 0.1959 0.2267 0.111 1.000 . Uiso c ? H(75) 0.2590 0.0853 0.2658 0.111 1.000 . Uiso c ? H(76) 0.2941 0.1248 0.1739 0.111 1.000 . Uiso c ? H(80) 0.6200 0.6899 0.1705 0.117 1.000 . Uiso c ? H(81) 0.6871 0.6522 0.0958 0.117 1.000 . Uiso c ? H(82) 0.6874 0.7414 0.1049 0.117 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0344(2) 0.0471(3) 0.0388(2) -0.0163(2) -0.0105(2) -0.0086(2) Ru(2) 0.0396(2) 0.0557(3) 0.0425(2) -0.0162(2) -0.0131(2) -0.0136(2) Cl(1) 0.196(3) 0.155(2) 0.175(3) -0.098(2) -0.046(2) -0.012(2) Cl(21) 0.212(4) 0.222(4) 0.224(4) -0.098(3) -0.120(3) -0.054(3) P(1) 0.0384(7) 0.0492(8) 0.0457(8) -0.0166(6) -0.0114(6) -0.0122(6) P(2) 0.0375(7) 0.0531(8) 0.0405(7) -0.0175(6) -0.0101(6) -0.0119(6) P(3) 0.0491(8) 0.081(1) 0.0449(8) -0.0269(8) -0.0112(7) -0.0153(8) P(4) 0.0408(7) 0.0574(9) 0.0499(8) -0.0138(7) -0.0145(6) -0.0187(7) O(1) 0.044(2) 0.071(3) 0.047(2) -0.022(2) -0.017(2) -0.010(2) O(2) 0.051(2) 0.049(2) 0.062(2) -0.017(2) -0.014(2) -0.011(2) O(3) 0.043(2) 0.059(2) 0.051(2) -0.024(2) -0.016(2) -0.008(2) O(4) 0.045(2) 0.061(2) 0.042(2) -0.025(2) -0.008(2) -0.007(2) O(5) 0.051(2) 0.069(2) 0.049(2) -0.024(2) -0.019(2) -0.017(2) O(6) 0.040(2) 0.060(2) 0.051(2) -0.013(2) -0.010(2) -0.016(2) O(7) 0.050(2) 0.072(3) 0.058(2) -0.021(2) -0.023(2) -0.014(2) O(8) 0.065(2) 0.056(2) 0.062(2) -0.023(2) -0.023(2) -0.009(2) C(1) 0.068(4) 0.120(6) 0.086(5) -0.026(4) -0.046(4) -0.005(4) C(2) 0.043(3) 0.077(4) 0.041(3) -0.018(3) -0.016(2) 0.002(3) C(3) 0.054(3) 0.054(4) 0.058(4) -0.004(3) -0.018(3) -0.002(3) C(4) 0.067(4) 0.049(4) 0.046(3) -0.020(3) -0.006(3) -0.005(3) C(5) 0.109(6) 0.056(4) 0.090(5) -0.023(4) -0.023(4) -0.014(4) C(6) 0.063(4) 0.142(6) 0.075(4) -0.054(4) -0.022(3) -0.026(4) C(7) 0.043(3) 0.066(4) 0.060(3) -0.027(3) -0.016(3) -0.008(3) C(8) 0.037(3) 0.082(4) 0.062(4) -0.027(3) -0.006(3) -0.013(3) C(9) 0.052(3) 0.052(3) 0.051(3) -0.026(3) -0.001(3) -0.011(3) C(10) 0.056(4) 0.095(5) 0.060(4) -0.034(3) 0.001(3) -0.019(3) C(11) 0.047(3) 0.050(3) 0.053(3) -0.016(3) -0.013(3) -0.012(3) C(12) 0.046(3) 0.060(4) 0.050(3) -0.021(3) -0.010(3) -0.008(3) C(13) 0.063(4) 0.098(5) 0.067(4) -0.031(4) -0.030(3) 0.011(4) C(14) 0.043(3) 0.055(3) 0.053(3) -0.021(3) -0.010(2) -0.021(3) C(15) 0.056(3) 0.076(4) 0.059(4) -0.023(3) -0.013(3) -0.028(3) C(16) 0.080(5) 0.119(6) 0.059(4) -0.054(4) -0.014(3) -0.029(4) C(17) 0.067(4) 0.126(6) 0.074(5) -0.050(4) 0.009(4) -0.061(5) C(18) 0.064(4) 0.086(5) 0.096(5) -0.021(4) -0.011(4) -0.053(4) C(19) 0.053(3) 0.071(4) 0.077(4) -0.021(3) -0.013(3) -0.031(3) C(20) 0.044(3) 0.055(3) 0.056(3) -0.022(3) -0.004(2) -0.021(3) C(21) 0.057(4) 0.076(4) 0.077(4) -0.031(3) -0.018(3) -0.020(3) C(22) 0.062(4) 0.106(6) 0.121(6) -0.036(4) -0.022(4) -0.051(5) C(23) 0.076(5) 0.110(6) 0.115(6) -0.061(5) 0.022(4) -0.062(5) C(24) 0.093(5) 0.083(5) 0.082(5) -0.056(4) -0.002(4) -0.025(4) C(25) 0.064(4) 0.060(4) 0.063(4) -0.030(3) -0.008(3) -0.021(3) C(26) 0.041(3) 0.067(4) 0.045(3) -0.021(3) -0.005(2) -0.015(3) C(27) 0.045(3) 0.080(4) 0.056(3) -0.028(3) -0.009(3) -0.015(3) C(28) 0.054(4) 0.127(6) 0.105(5) -0.039(4) -0.025(4) -0.029(5) C(29) 0.057(3) 0.051(3) 0.032(3) -0.016(3) -0.009(2) -0.008(2) C(30) 0.069(4) 0.071(4) 0.082(4) -0.014(3) -0.029(3) -0.035(3) C(31) 0.130(7) 0.087(5) 0.097(5) -0.039(5) -0.044(5) -0.039(4) C(32) 0.127(7) 0.072(5) 0.079(5) -0.014(5) -0.018(5) -0.043(4) C(33) 0.080(5) 0.065(5) 0.072(5) -0.005(4) -0.004(4) -0.024(4) C(34) 0.060(4) 0.054(4) 0.058(4) -0.011(3) -0.006(3) -0.015(3) C(35) 0.049(3) 0.045(3) 0.041(3) -0.017(2) -0.009(2) -0.015(2) C(36) 0.058(3) 0.062(4) 0.050(3) -0.025(3) -0.018(3) -0.011(3) C(37) 0.068(4) 0.064(4) 0.052(3) -0.017(3) -0.027(3) -0.012(3) C(38) 0.083(4) 0.047(3) 0.038(3) -0.011(3) -0.019(3) -0.011(2) C(39) 0.071(4) 0.064(4) 0.050(3) -0.029(3) -0.001(3) -0.013(3) C(40) 0.053(3) 0.061(4) 0.051(3) -0.023(3) -0.012(3) -0.012(3) C(41) 0.071(4) 0.122(6) 0.066(4) -0.029(4) -0.029(3) -0.034(4) C(42) 0.050(3) 0.058(3) 0.057(3) -0.011(3) -0.020(3) -0.026(3) C(43) 0.055(3) 0.074(4) 0.044(3) -0.015(3) -0.014(3) -0.019(3) C(44) 0.053(3) 0.051(3) 0.056(3) -0.016(3) -0.005(3) -0.024(3) C(45) 0.062(4) 0.092(5) 0.057(4) -0.030(3) 0.000(3) -0.023(3) C(46) 0.107(6) 0.105(6) 0.113(6) -0.022(5) -0.079(5) -0.016(4) C(47) 0.054(3) 0.076(4) 0.058(4) -0.017(3) -0.026(3) -0.011(3) C(48) 0.072(4) 0.068(4) 0.064(4) -0.022(3) -0.030(3) 0.002(3) C(49) 0.058(4) 0.058(4) 0.061(4) -0.024(3) -0.012(3) -0.004(3) C(50) 0.116(6) 0.072(5) 0.106(6) -0.041(4) -0.051(5) 0.003(4) C(54) 0.041(3) 0.062(4) 0.055(3) -0.014(3) -0.013(3) -0.004(3) C(55) 0.081(4) 0.090(5) 0.068(4) -0.054(4) -0.028(3) 0.008(4) C(56) 0.076(5) 0.096(5) 0.107(6) -0.050(4) -0.034(4) -0.004(4) C(57) 0.055(4) 0.074(5) 0.116(7) -0.025(4) -0.006(4) 0.002(5) C(58) 0.097(6) 0.077(5) 0.067(5) -0.033(4) 0.012(4) 0.004(4) C(59) 0.078(4) 0.072(5) 0.065(4) -0.016(4) -0.004(3) -0.007(4) C(60) 0.050(3) 0.066(4) 0.058(4) -0.030(3) 0.003(3) -0.014(3) C(61) 0.056(4) 0.088(5) 0.081(5) -0.023(4) -0.013(3) -0.022(4) C(62) 0.046(4) 0.097(6) 0.110(6) -0.020(4) -0.011(4) -0.002(5) C(63) 0.056(5) 0.070(5) 0.138(8) -0.021(4) 0.012(5) -0.013(5) C(64) 0.081(6) 0.070(5) 0.149(8) -0.034(5) 0.021(5) -0.051(6) C(65) 0.083(5) 0.089(5) 0.099(5) -0.048(4) 0.004(4) -0.038(4) C(66) 0.048(3) 0.056(3) 0.053(3) -0.014(3) -0.013(3) -0.021(3) C(67) 0.052(3) 0.069(4) 0.060(4) -0.005(3) -0.018(3) -0.031(3) C(68) 0.066(4) 0.123(6) 0.083(5) 0.005(4) -0.041(4) -0.037(4) C(69) 0.048(3) 0.062(4) 0.053(3) -0.019(3) -0.010(3) -0.025(3) C(70) 0.057(4) 0.072(4) 0.074(4) -0.029(3) -0.022(3) -0.011(3) C(71) 0.054(4) 0.107(6) 0.101(5) -0.039(4) -0.021(4) -0.025(4) C(72) 0.073(4) 0.114(6) 0.077(5) -0.062(4) -0.005(4) -0.026(4) C(73) 0.089(5) 0.084(5) 0.062(4) -0.052(4) -0.013(4) -0.009(3) C(74) 0.069(4) 0.064(4) 0.055(3) -0.026(3) -0.019(3) -0.013(3) C(75) 0.053(3) 0.064(4) 0.049(3) -0.024(3) -0.011(3) -0.023(3) C(76) 0.084(5) 0.119(6) 0.093(5) -0.004(4) -0.042(4) -0.059(5) C(77) 0.107(6) 0.163(8) 0.106(6) -0.022(6) -0.051(5) -0.076(6) C(78) 0.097(6) 0.109(6) 0.076(5) -0.046(5) -0.005(4) -0.049(4) C(79) 0.089(5) 0.082(5) 0.079(5) -0.030(4) -0.013(4) -0.039(4) C(80) 0.069(4) 0.061(4) 0.061(4) -0.019(3) -0.012(3) -0.028(3) C(81) 0.130(7) 0.102(7) 0.095(6) -0.072(6) -0.044(6) 0.003(5) #------------------------------------------------------------------------------ _refine_special_details ; Refinement with anisotropic displacement factors for all non-hydrogen atoms revealed severe anisotropy for atoms Cl(2) and C(53). Examination of a contour plot of the electron density at the dichloromethane molecule suggested that atom Cl(2) should be split over two sites, Cl(21) of occupancy p and Cl(22) of occupancy (1-p). In concert with this, C(81) would have occupancy p also. This corresponds to disordering of the dichloromethane molecule over two orientations: the major one being Cl(1)-C(81)-Cl(21) and the minor one Cl(1)-C-Cl(22). Sites Cl(21) and C(81) were refined with anisotropic displacement factors while Cl(22) was assigned an isotropic B equal to B$_{eq}$ of Cl(21). The C atom corresponding to orientation Cl(1)-C-Cl(22) was not located. The anisotropy of C(53), and to a lesser extent C(52) and C(51), suggested disorder of this unit too. Each atom was split over two sites and the relative occupancy of the two orientations was refined. Hydrogen atoms were included at geometrically determined positions based on peaks observed in inner-data difference electron density maps; hydrogen atoms for C(531) and C(532) were not included. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _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 9045 _refine_ls_number_parameters 876 _refine_ls_number_restraints 0 _refine_ls_number_constraints 7 _refine_ls_R_factor_all 0.1292 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_all 0.0547 _refine_ls_wR_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.0439 _refine_ls_goodness_of_fit_all 1.323 _refine_ls_goodness_of_fit_ref 1.538 _refine_ls_shift/su_max 0.0270 _refine_ls_shift/su_mean 0.0040 _refine_diff_density_min -0.54 _refine_diff_density_max 0.70 #------------------------------------------------------------------------------ _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) P(1) 2.249(1) . . yes Ru(1) P(2) 2.265(1) . . yes Ru(1) O(1) 2.063(3) . . yes Ru(1) O(2) 2.088(3) . . yes Ru(1) O(3) 2.059(3) . . yes Ru(1) O(4) 2.098(3) . . yes Ru(2) P(3) 2.259(1) . . yes Ru(2) P(4) 2.254(2) . . yes Ru(2) O(5) 2.056(3) . . yes Ru(2) O(6) 2.095(3) . . yes Ru(2) O(7) 2.069(3) . . yes Ru(2) O(8) 2.104(4) . . yes Cl(1) C(81) 1.687(8) . . yes Cl(21) Cl(22) 1.79(3) . . yes Cl(21) C(81) 1.621(8) . . yes P(1) C(11) 1.768(5) . . yes P(1) C(14) 1.834(5) . . yes P(1) C(20) 1.831(5) . . yes P(2) C(26) 1.770(5) . . yes P(2) C(29) 1.840(5) . . yes P(2) C(35) 1.840(5) . . yes P(3) C(54) 1.840(6) . . yes P(3) C(60) 1.846(6) . . yes P(3) C(511) 1.77(1) . . yes P(3) C(512) 1.79(2) . . yes P(4) C(66) 1.770(5) . . yes P(4) C(69) 1.842(5) . . yes P(4) C(75) 1.835(5) . . yes O(1) C(2) 1.282(6) . . yes O(2) C(4) 1.249(6) . . yes O(3) C(7) 1.271(5) . . yes O(4) C(9) 1.271(5) . . yes O(5) C(42) 1.267(5) . . yes O(6) C(44) 1.268(6) . . yes O(7) C(47) 1.265(6) . . yes O(8) C(49) 1.254(6) . . yes C(1) C(2) 1.511(7) . . yes C(1) H(47) 0.95 . . no C(1) H(48) 0.95 . . no C(1) H(49) 0.95 . . no C(2) C(3) 1.390(8) . . yes C(3) C(4) 1.398(8) . . yes C(3) H(1) 0.95 . . no C(4) C(5) 1.507(8) . . yes C(5) H(50) 0.95 . . no C(5) H(51) 0.95 . . no C(5) H(52) 0.95 . . no C(6) C(7) 1.510(7) . . yes C(6) H(53) 0.95 . . no C(6) H(54) 0.95 . . no C(6) H(55) 0.95 . . no C(7) C(8) 1.382(7) . . yes C(8) C(9) 1.387(7) . . yes C(8) H(2) 0.95 . . no C(9) C(10) 1.514(7) . . yes C(10) H(56) 0.95 . . no C(10) H(57) 0.95 . . no C(10) H(58) 0.95 . . no C(11) C(12) 1.183(6) . . yes C(12) C(13) 1.458(7) . . yes C(13) H(71) 0.95 . . no C(13) H(72) 0.95 . . no C(13) H(73) 0.95 . . no C(14) C(15) 1.386(7) . . yes C(14) C(19) 1.381(7) . . yes C(15) C(16) 1.394(7) . . yes C(15) H(3) 0.95 . . no C(16) C(17) 1.372(8) . . yes C(16) H(4) 0.95 . . no C(17) C(18) 1.354(8) . . yes C(17) H(5) 0.95 . . no C(18) C(19) 1.375(7) . . yes C(18) H(6) 0.95 . . no C(19) H(7) 0.95 . . no C(20) C(21) 1.387(7) . . yes C(20) C(25) 1.373(7) . . yes C(21) C(22) 1.387(8) . . yes C(21) H(8) 0.95 . . no C(22) C(23) 1.372(9) . . yes C(22) H(9) 0.95 . . no C(23) C(24) 1.355(9) . . yes C(23) H(10) 0.95 . . no C(24) C(25) 1.379(7) . . yes C(24) H(11) 0.95 . . no C(25) H(12) 0.95 . . no C(26) C(27) 1.180(6) . . yes C(27) C(28) 1.470(7) . . yes C(28) H(74) 0.95 . . no C(28) H(75) 0.95 . . no C(28) H(76) 0.95 . . no C(29) C(30) 1.386(7) . . yes C(29) C(34) 1.385(7) . . yes C(30) C(31) 1.376(8) . . yes C(30) H(13) 0.95 . . no C(31) C(32) 1.362(9) . . yes C(31) H(14) 0.95 . . no C(32) C(33) 1.354(9) . . yes C(32) H(15) 0.95 . . no C(33) C(34) 1.383(8) . . yes C(33) H(16) 0.95 . . no C(34) H(17) 0.95 . . no C(35) C(36) 1.391(6) . . yes C(35) C(40) 1.379(6) . . yes C(36) C(37) 1.381(7) . . yes C(36) H(18) 0.95 . . no C(37) C(38) 1.365(7) . . yes C(37) H(19) 0.95 . . no C(38) C(39) 1.366(7) . . yes C(38) H(20) 0.95 . . no C(39) C(40) 1.379(7) . . yes C(39) H(21) 0.95 . . no C(40) H(22) 0.95 . . no C(41) C(42) 1.501(7) . . yes C(41) H(59) 0.95 . . no C(41) H(60) 0.95 . . no C(41) H(61) 0.95 . . no C(42) C(43) 1.388(7) . . yes C(43) C(44) 1.390(7) . . yes C(43) H(23) 0.95 . . no C(44) C(45) 1.510(7) . . yes C(45) H(62) 0.95 . . no C(45) H(63) 0.95 . . no C(45) H(64) 0.95 . . no C(46) C(47) 1.515(7) . . yes C(46) H(65) 0.95 . . no C(46) H(66) 0.95 . . no C(46) H(67) 0.95 . . no C(47) C(48) 1.383(8) . . yes C(48) C(49) 1.402(8) . . yes C(48) H(24) 0.95 . . no C(49) C(50) 1.504(8) . . yes C(50) H(68) 0.95 . . no C(50) H(69) 0.95 . . no C(50) H(70) 0.95 . . no C(54) C(55) 1.365(8) . . yes C(54) C(59) 1.394(7) . . yes C(55) C(56) 1.395(8) . . yes C(55) H(25) 0.95 . . no C(56) C(57) 1.344(9) . . yes C(56) H(26) 0.95 . . no C(57) C(58) 1.35(1) . . yes C(57) H(27) 0.95 . . no C(58) C(59) 1.385(9) . . yes C(58) H(28) 0.95 . . no C(59) H(29) 0.95 . . no C(60) C(61) 1.377(8) . . yes C(60) C(65) 1.391(8) . . yes C(61) C(62) 1.390(8) . . yes C(61) H(30) 0.95 . . no C(62) C(63) 1.37(1) . . yes C(62) H(31) 0.95 . . no C(63) C(64) 1.35(1) . . yes C(63) H(32) 0.95 . . no C(64) C(65) 1.383(9) . . yes C(64) H(33) 0.95 . . no C(65) H(34) 0.95 . . no C(66) C(67) 1.177(6) . . yes C(67) C(68) 1.450(7) . . yes C(68) H(80) 0.95 . . no C(68) H(81) 0.95 . . no C(68) H(82) 0.95 . . no C(69) C(70) 1.388(7) . . yes C(69) C(74) 1.379(7) . . yes C(70) C(71) 1.381(7) . . yes C(70) H(35) 0.95 . . no C(71) C(72) 1.372(8) . . yes C(71) H(36) 0.95 . . no C(72) C(73) 1.362(8) . . yes C(72) H(37) 0.95 . . no C(73) C(74) 1.377(7) . . yes C(73) H(38) 0.95 . . no C(74) H(39) 0.95 . . no C(75) C(76) 1.374(7) . . yes C(75) C(80) 1.375(7) . . yes C(76) C(77) 1.390(8) . . yes C(76) H(40) 0.95 . . no C(77) C(78) 1.351(9) . . yes C(77) H(41) 0.95 . . no C(78) C(79) 1.351(8) . . yes C(78) H(42) 0.95 . . no C(79) C(80) 1.382(7) . . yes C(79) H(43) 0.95 . . no C(80) H(44) 0.95 . . no C(81) H(45) 0.95 . . no C(81) H(46) 0.95 . . no C(511) C(521) 1.18(2) . . yes C(512) C(522) 1.20(2) . . yes C(521) C(531) 1.53(2) . . yes C(522) C(532) 1.53(2) . . 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 P(1) Ru(1) P(2) 94.20(5) . . . yes P(1) Ru(1) O(1) 91.3(1) . . . yes P(1) Ru(1) O(2) 174.3(1) . . . yes P(1) Ru(1) O(3) 93.5(1) . . . yes P(1) Ru(1) O(4) 90.1(1) . . . yes P(2) Ru(1) O(1) 89.91(9) . . . yes P(2) Ru(1) O(2) 91.0(1) . . . yes P(2) Ru(1) O(3) 92.82(9) . . . yes P(2) Ru(1) O(4) 174.2(1) . . . yes O(1) Ru(1) O(2) 91.2(1) . . . yes O(1) Ru(1) O(3) 174.3(1) . . . yes O(1) Ru(1) O(4) 86.0(1) . . . yes O(2) Ru(1) O(3) 83.8(1) . . . yes O(2) Ru(1) O(4) 85.0(1) . . . yes O(3) Ru(1) O(4) 90.9(1) . . . yes P(3) Ru(2) P(4) 94.30(5) . . . yes P(3) Ru(2) O(5) 90.6(1) . . . yes P(3) Ru(2) O(6) 176.8(1) . . . yes P(3) Ru(2) O(7) 92.0(1) . . . yes P(3) Ru(2) O(8) 92.6(1) . . . yes P(4) Ru(2) O(5) 92.4(1) . . . yes P(4) Ru(2) O(6) 88.8(1) . . . yes P(4) Ru(2) O(7) 91.8(1) . . . yes P(4) Ru(2) O(8) 172.8(1) . . . yes O(5) Ru(2) O(6) 90.0(1) . . . yes O(5) Ru(2) O(7) 174.9(1) . . . yes O(5) Ru(2) O(8) 85.5(1) . . . yes O(6) Ru(2) O(7) 87.2(1) . . . yes O(6) Ru(2) O(8) 84.3(1) . . . yes O(7) Ru(2) O(8) 89.9(1) . . . yes Cl(22) Cl(21) C(81) 81.2(8) . . . yes Ru(1) P(1) C(11) 115.6(2) . . . yes Ru(1) P(1) C(14) 116.5(2) . . . yes Ru(1) P(1) C(20) 118.0(2) . . . yes C(11) P(1) C(14) 100.9(2) . . . yes C(11) P(1) C(20) 102.3(2) . . . yes C(14) P(1) C(20) 100.8(2) . . . yes Ru(1) P(2) C(26) 115.4(2) . . . yes Ru(1) P(2) C(29) 114.4(2) . . . yes Ru(1) P(2) C(35) 121.0(2) . . . yes C(26) P(2) C(29) 100.8(2) . . . yes C(26) P(2) C(35) 102.3(2) . . . yes C(29) P(2) C(35) 100.0(2) . . . yes Ru(2) P(3) C(54) 115.5(2) . . . yes Ru(2) P(3) C(60) 118.7(2) . . . yes Ru(2) P(3) C(511) 116.6(4) . . . yes Ru(2) P(3) C(512) 115.4(5) . . . yes C(54) P(3) C(60) 100.6(2) . . . yes C(54) P(3) C(511) 93.5(6) . . . yes C(54) P(3) C(512) 108.1(6) . . . yes C(60) P(3) C(511) 108.1(6) . . . yes C(60) P(3) C(512) 95.9(6) . . . yes Ru(2) P(4) C(66) 115.8(2) . . . yes Ru(2) P(4) C(69) 115.0(2) . . . yes Ru(2) P(4) C(75) 120.6(2) . . . yes C(66) P(4) C(69) 101.6(2) . . . yes C(66) P(4) C(75) 100.7(2) . . . yes C(69) P(4) C(75) 100.2(2) . . . yes Ru(1) O(1) C(2) 122.0(4) . . . yes Ru(1) O(2) C(4) 123.3(4) . . . yes Ru(1) O(3) C(7) 124.2(3) . . . yes Ru(1) O(4) C(9) 122.5(3) . . . yes Ru(2) O(5) C(42) 124.3(3) . . . yes Ru(2) O(6) C(44) 122.5(3) . . . yes Ru(2) O(7) C(47) 123.5(4) . . . yes Ru(2) O(8) C(49) 123.8(4) . . . yes C(2) C(1) H(47) 109.5 . . . no C(2) C(1) H(48) 109.5 . . . no C(2) C(1) H(49) 109.5 . . . no H(47) C(1) H(48) 109.5 . . . no H(47) C(1) H(49) 109.5 . . . no H(48) C(1) H(49) 109.5 . . . no O(1) C(2) C(1) 113.5(6) . . . yes O(1) C(2) C(3) 127.0(5) . . . yes C(1) C(2) C(3) 119.5(6) . . . yes C(2) C(3) C(4) 127.8(5) . . . yes C(2) C(3) H(1) 116.1 . . . no C(4) C(3) H(1) 116.1 . . . no O(2) C(4) C(3) 126.0(5) . . . yes O(2) C(4) C(5) 115.8(6) . . . yes C(3) C(4) C(5) 118.2(6) . . . yes C(4) C(5) H(50) 109.5 . . . no C(4) C(5) H(51) 109.5 . . . no C(4) C(5) H(52) 109.5 . . . no H(50) C(5) H(51) 109.5 . . . no H(50) C(5) H(52) 109.5 . . . no H(51) C(5) H(52) 109.5 . . . no C(7) C(6) H(53) 109.5 . . . no C(7) C(6) H(54) 109.5 . . . no C(7) C(6) H(55) 109.5 . . . no H(53) C(6) H(54) 109.5 . . . no H(53) C(6) H(55) 109.5 . . . no H(54) C(6) H(55) 109.5 . . . no O(3) C(7) C(6) 113.9(5) . . . yes O(3) C(7) C(8) 126.6(5) . . . yes C(6) C(7) C(8) 119.5(5) . . . yes C(7) C(8) C(9) 127.8(5) . . . yes C(7) C(8) H(2) 116.1 . . . no C(9) C(8) H(2) 116.1 . . . no O(4) C(9) C(8) 126.9(5) . . . yes O(4) C(9) C(10) 114.5(5) . . . yes C(8) C(9) C(10) 118.5(5) . . . yes C(9) C(10) H(56) 109.5 . . . no C(9) C(10) H(57) 109.5 . . . no C(9) C(10) H(58) 109.5 . . . no H(56) C(10) H(57) 109.5 . . . no H(56) C(10) H(58) 109.5 . . . no H(57) C(10) H(58) 109.5 . . . no P(1) C(11) C(12) 175.8(5) . . . yes C(11) C(12) C(13) 178.8(6) . . . yes C(12) C(13) H(71) 109.5 . . . no C(12) C(13) H(72) 109.5 . . . no C(12) C(13) H(73) 109.5 . . . no H(71) C(13) H(72) 109.5 . . . no H(71) C(13) H(73) 109.5 . . . no H(72) C(13) H(73) 109.5 . . . no P(1) C(14) C(15) 119.3(4) . . . yes P(1) C(14) C(19) 121.9(4) . . . yes C(15) C(14) C(19) 118.6(5) . . . yes C(14) C(15) C(16) 119.2(5) . . . yes C(14) C(15) H(3) 120.4 . . . no C(16) C(15) H(3) 120.4 . . . no C(15) C(16) C(17) 121.4(6) . . . yes C(15) C(16) H(4) 119.3 . . . no C(17) C(16) H(4) 119.3 . . . no C(16) C(17) C(18) 118.9(6) . . . yes C(16) C(17) H(5) 120.6 . . . no C(18) C(17) H(5) 120.6 . . . no C(17) C(18) C(19) 121.1(6) . . . yes C(17) C(18) H(6) 119.5 . . . no C(19) C(18) H(6) 119.5 . . . no C(14) C(19) C(18) 120.9(6) . . . yes C(14) C(19) H(7) 119.6 . . . no C(18) C(19) H(7) 119.6 . . . no P(1) C(20) C(21) 119.2(4) . . . yes P(1) C(20) C(25) 122.2(4) . . . yes C(21) C(20) C(25) 118.4(5) . . . yes C(20) C(21) C(22) 120.1(6) . . . yes C(20) C(21) H(8) 120.0 . . . no C(22) C(21) H(8) 120.0 . . . no C(21) C(22) C(23) 119.9(6) . . . yes C(21) C(22) H(9) 120.1 . . . no C(23) C(22) H(9) 120.1 . . . no C(22) C(23) C(24) 120.5(6) . . . yes C(22) C(23) H(10) 119.8 . . . no C(24) C(23) H(10) 119.8 . . . no C(23) C(24) C(25) 119.8(6) . . . yes C(23) C(24) H(11) 120.1 . . . no C(25) C(24) H(11) 120.1 . . . no C(20) C(25) C(24) 121.3(6) . . . yes C(20) C(25) H(12) 119.4 . . . no C(24) C(25) H(12) 119.4 . . . no P(2) C(26) C(27) 176.4(5) . . . yes C(26) C(27) C(28) 178.9(6) . . . yes C(27) C(28) H(74) 109.5 . . . no C(27) C(28) H(75) 109.5 . . . no C(27) C(28) H(76) 109.5 . . . no H(74) C(28) H(75) 109.5 . . . no H(74) C(28) H(76) 109.5 . . . no H(75) C(28) H(76) 109.5 . . . no P(2) C(29) C(30) 118.1(4) . . . yes P(2) C(29) C(34) 123.4(4) . . . yes C(30) C(29) C(34) 118.5(5) . . . yes C(29) C(30) C(31) 120.0(6) . . . yes C(29) C(30) H(13) 120.0 . . . no C(31) C(30) H(13) 120.0 . . . no C(30) C(31) C(32) 120.8(7) . . . yes C(30) C(31) H(14) 119.6 . . . no C(32) C(31) H(14) 119.6 . . . no C(31) C(32) C(33) 119.8(7) . . . yes C(31) C(32) H(15) 120.1 . . . no C(33) C(32) H(15) 120.1 . . . no C(32) C(33) C(34) 120.6(6) . . . yes C(32) C(33) H(16) 119.7 . . . no C(34) C(33) H(16) 119.7 . . . no C(29) C(34) C(33) 120.2(6) . . . yes C(29) C(34) H(17) 119.9 . . . no C(33) C(34) H(17) 119.9 . . . no P(2) C(35) C(36) 118.6(4) . . . yes P(2) C(35) C(40) 122.6(4) . . . yes C(36) C(35) C(40) 118.7(5) . . . yes C(35) C(36) C(37) 120.2(5) . . . yes C(35) C(36) H(18) 119.9 . . . no C(37) C(36) H(18) 119.9 . . . no C(36) C(37) C(38) 120.2(5) . . . yes C(36) C(37) H(19) 119.9 . . . no C(38) C(37) H(19) 119.9 . . . no C(37) C(38) C(39) 120.2(5) . . . yes C(37) C(38) H(20) 119.9 . . . no C(39) C(38) H(20) 119.9 . . . no C(38) C(39) C(40) 120.2(5) . . . yes C(38) C(39) H(21) 119.9 . . . no C(40) C(39) H(21) 119.9 . . . no C(35) C(40) C(39) 120.5(5) . . . yes C(35) C(40) H(22) 119.7 . . . no C(39) C(40) H(22) 119.7 . . . no C(42) C(41) H(59) 109.5 . . . no C(42) C(41) H(60) 109.5 . . . no C(42) C(41) H(61) 109.5 . . . no H(59) C(41) H(60) 109.5 . . . no H(59) C(41) H(61) 109.5 . . . no H(60) C(41) H(61) 109.5 . . . no O(5) C(42) C(41) 114.2(5) . . . yes O(5) C(42) C(43) 126.2(5) . . . yes C(41) C(42) C(43) 119.6(5) . . . yes C(42) C(43) C(44) 127.4(5) . . . yes C(42) C(43) H(23) 116.3 . . . no C(44) C(43) H(23) 116.3 . . . no O(6) C(44) C(43) 126.3(5) . . . yes O(6) C(44) C(45) 115.0(5) . . . yes C(43) C(44) C(45) 118.7(5) . . . yes C(44) C(45) H(62) 109.5 . . . no C(44) C(45) H(63) 109.5 . . . no C(44) C(45) H(64) 109.5 . . . no H(62) C(45) H(63) 109.5 . . . no H(62) C(45) H(64) 109.5 . . . no H(63) C(45) H(64) 109.5 . . . no C(47) C(46) H(65) 109.5 . . . no C(47) C(46) H(66) 109.5 . . . no C(47) C(46) H(67) 109.5 . . . no H(65) C(46) H(66) 109.5 . . . no H(65) C(46) H(67) 109.5 . . . no H(66) C(46) H(67) 109.5 . . . no O(7) C(47) C(46) 113.4(6) . . . yes O(7) C(47) C(48) 127.7(5) . . . yes C(46) C(47) C(48) 118.9(6) . . . yes C(47) C(48) C(49) 127.0(5) . . . yes C(47) C(48) H(24) 116.5 . . . no C(49) C(48) H(24) 116.5 . . . no O(8) C(49) C(48) 126.0(6) . . . yes O(8) C(49) C(50) 115.5(6) . . . yes C(48) C(49) C(50) 118.5(5) . . . yes C(49) C(50) H(68) 109.5 . . . no C(49) C(50) H(69) 109.5 . . . no C(49) C(50) H(70) 109.5 . . . no H(68) C(50) H(69) 109.5 . . . no H(68) C(50) H(70) 109.5 . . . no H(69) C(50) H(70) 109.5 . . . no P(3) C(54) C(55) 119.3(4) . . . yes P(3) C(54) C(59) 122.4(5) . . . yes C(55) C(54) C(59) 118.3(6) . . . yes C(54) C(55) C(56) 120.5(6) . . . yes C(54) C(55) H(25) 119.7 . . . no C(56) C(55) H(25) 119.7 . . . no C(55) C(56) C(57) 120.2(7) . . . yes C(55) C(56) H(26) 119.9 . . . no C(57) C(56) H(26) 119.9 . . . no C(56) C(57) C(58) 120.7(7) . . . yes C(56) C(57) H(27) 119.6 . . . no C(58) C(57) H(27) 119.6 . . . no C(57) C(58) C(59) 120.1(7) . . . yes C(57) C(58) H(28) 120.0 . . . no C(59) C(58) H(28) 120.0 . . . no C(54) C(59) C(58) 120.2(7) . . . yes C(54) C(59) H(29) 119.9 . . . no C(58) C(59) H(29) 119.9 . . . no P(3) C(60) C(61) 117.5(5) . . . yes P(3) C(60) C(65) 124.1(5) . . . yes C(61) C(60) C(65) 118.4(6) . . . yes C(60) C(61) C(62) 119.9(7) . . . yes C(60) C(61) H(30) 120.0 . . . no C(62) C(61) H(30) 120.0 . . . no C(61) C(62) C(63) 120.9(8) . . . yes C(61) C(62) H(31) 119.5 . . . no C(63) C(62) H(31) 119.5 . . . no C(62) C(63) C(64) 119.4(8) . . . yes C(62) C(63) H(32) 120.3 . . . no C(64) C(63) H(32) 120.3 . . . no C(63) C(64) C(65) 120.9(8) . . . yes C(63) C(64) H(33) 119.5 . . . no C(65) C(64) H(33) 119.5 . . . no C(60) C(65) C(64) 120.4(7) . . . yes C(60) C(65) H(34) 119.8 . . . no C(64) C(65) H(34) 119.8 . . . no P(4) C(66) C(67) 177.2(5) . . . yes C(66) C(67) C(68) 179.4(7) . . . yes C(67) C(68) H(80) 109.5 . . . no C(67) C(68) H(81) 109.5 . . . no C(67) C(68) H(82) 109.5 . . . no H(80) C(68) H(81) 109.5 . . . no H(80) C(68) H(82) 109.5 . . . no H(81) C(68) H(82) 109.5 . . . no P(4) C(69) C(70) 119.0(4) . . . yes P(4) C(69) C(74) 122.4(4) . . . yes C(70) C(69) C(74) 118.6(5) . . . yes C(69) C(70) C(71) 120.4(5) . . . yes C(69) C(70) H(35) 119.8 . . . no C(71) C(70) H(35) 119.8 . . . no C(70) C(71) C(72) 119.9(6) . . . yes C(70) C(71) H(36) 120.0 . . . no C(72) C(71) H(36) 120.0 . . . no C(71) C(72) C(73) 120.2(6) . . . yes C(71) C(72) H(37) 119.9 . . . no C(73) C(72) H(37) 119.9 . . . no C(72) C(73) C(74) 120.2(6) . . . yes C(72) C(73) H(38) 119.9 . . . no C(74) C(73) H(38) 119.9 . . . no C(69) C(74) C(73) 120.7(5) . . . yes C(69) C(74) H(39) 119.6 . . . no C(73) C(74) H(39) 119.6 . . . no P(4) C(75) C(76) 119.3(4) . . . yes P(4) C(75) C(80) 122.3(4) . . . yes C(76) C(75) C(80) 118.2(5) . . . yes C(75) C(76) C(77) 120.2(6) . . . yes C(75) C(76) H(40) 119.9 . . . no C(77) C(76) H(40) 119.9 . . . no C(76) C(77) C(78) 120.2(7) . . . yes C(76) C(77) H(41) 119.9 . . . no C(78) C(77) H(41) 119.9 . . . no C(77) C(78) C(79) 120.5(6) . . . yes C(77) C(78) H(42) 119.8 . . . no C(79) C(78) H(42) 119.8 . . . no C(78) C(79) C(80) 119.9(6) . . . yes C(78) C(79) H(43) 120.1 . . . no C(80) C(79) H(43) 120.1 . . . no C(75) C(80) C(79) 121.0(6) . . . yes C(75) C(80) H(44) 119.5 . . . no C(79) C(80) H(44) 119.5 . . . no Cl(1) C(81) Cl(21) 117.2(5) . . . yes Cl(1) C(81) H(45) 107.5 . . . no Cl(1) C(81) H(46) 107.5 . . . no Cl(21) C(81) H(45) 107.5 . . . no Cl(21) C(81) H(46) 107.5 . . . no H(45) C(81) H(46) 109.5 . . . no P(3) C(511) C(521) 173(1) . . . yes P(3) C(512) C(522) 173(2) . . . 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(1) C(72) 3.559(7) . 2_765 no Cl(22) C(531) 3.16(3) . 1_554 no Cl(22) C(532) 3.49(3) . 1_554 no O(4) C(81) 3.311(8) . . no O(6) C(28) 3.493(7) . 1_655 no C(38) C(40) 3.482(7) . 2_656 no C(38) C(79) 3.486(8) . 1_545 no C(38) C(39) 3.535(7) . 2_656 no C(39) C(39) 3.45(1) . 2_656 no C(63) C(64) 3.418(9) . 2_666 no C(63) C(65) 3.519(9) . 2_666 no C(64) C(64) 3.47(1) . 2_666 no Cl(1) Cl(22) 2.66(2) . . no Cl(1) Cl(21) 2.824(4) . . no Cl(21) Cl(22) 1.79(3) . . no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru(1) P(1) C(14) C(15) . . . . -42.0(5) no Ru(1) P(1) C(14) C(19) . . . . 141.3(4) no Ru(1) P(1) C(20) C(21) . . . . 71.9(5) no Ru(1) P(1) C(20) C(25) . . . . -104.6(4) no Ru(1) P(2) C(29) C(30) . . . . -62.2(5) no Ru(1) P(2) C(29) C(34) . . . . 115.7(4) no Ru(1) P(2) C(35) C(36) . . . . 37.6(5) no Ru(1) P(2) C(35) C(40) . . . . -144.4(4) no Ru(1) O(1) C(2) C(1) . . . . -170.4(3) no Ru(1) O(1) C(2) C(3) . . . . 9.0(7) no Ru(1) O(2) C(4) C(3) . . . . -8.0(8) no Ru(1) O(2) C(4) C(5) . . . . 171.7(3) no Ru(1) O(3) C(7) C(6) . . . . -179.9(4) no Ru(1) O(3) C(7) C(8) . . . . 0.3(8) no Ru(1) O(4) C(9) C(8) . . . . -9.2(8) no Ru(1) O(4) C(9) C(10) . . . . 170.9(3) no Ru(2) P(3) C(54) C(55) . . . . -35.4(5) no Ru(2) P(3) C(54) C(59) . . . . 146.0(4) no Ru(2) P(3) C(60) C(61) . . . . 55.7(5) no Ru(2) P(3) C(60) C(65) . . . . -124.7(5) no Ru(2) P(4) C(69) C(70) . . . . -43.7(5) no Ru(2) P(4) C(69) C(74) . . . . 137.3(4) no Ru(2) P(4) C(75) C(76) . . . . 52.3(6) no Ru(2) P(4) C(75) C(80) . . . . -124.5(4) no Ru(2) O(5) C(42) C(41) . . . . -175.8(4) no Ru(2) O(5) C(42) C(43) . . . . 4.7(8) no Ru(2) O(6) C(44) C(43) . . . . -14.0(7) no Ru(2) O(6) C(44) C(45) . . . . 166.5(3) no Ru(2) O(7) C(47) C(46) . . . . -175.7(4) no Ru(2) O(7) C(47) C(48) . . . . 5.7(8) no Ru(2) O(8) C(49) C(48) . . . . -8.7(8) no Ru(2) O(8) C(49) C(50) . . . . 173.8(4) no Cl(1) C(81) Cl(21) Cl(22) . . . . 58.0(9) no P(1) Ru(1) P(2) C(26) . . . . -75.4(2) no P(1) Ru(1) P(2) C(29) . . . . 168.3(2) no P(1) Ru(1) P(2) C(35) . . . . 48.7(2) no P(1) Ru(1) O(1) C(2) . . . . 169.6(4) no P(1) Ru(1) O(3) C(7) . . . . 83.6(4) no P(1) Ru(1) O(4) C(9) . . . . -82.9(4) no P(1) C(14) C(15) C(16) . . . . -175.4(4) no P(1) C(14) C(19) C(18) . . . . 176.0(4) no P(1) C(20) C(21) C(22) . . . . -177.1(5) no P(1) C(20) C(25) C(24) . . . . 175.9(5) no P(2) Ru(1) P(1) C(11) . . . . -85.5(2) no P(2) Ru(1) P(1) C(14) . . . . 156.2(2) no P(2) Ru(1) P(1) C(20) . . . . 35.9(2) no P(2) Ru(1) O(1) C(2) . . . . 75.4(4) no P(2) Ru(1) O(2) C(4) . . . . -74.5(4) no P(2) Ru(1) O(3) C(7) . . . . 178.0(4) no P(2) C(29) C(30) C(31) . . . . -179.5(5) no P(2) C(29) C(34) C(33) . . . . -178.9(4) no P(2) C(35) C(36) C(37) . . . . 176.4(4) no P(2) C(35) C(40) C(39) . . . . -176.6(4) no P(3) Ru(2) P(4) C(66) . . . . -85.2(2) no P(3) Ru(2) P(4) C(69) . . . . 156.7(2) no P(3) Ru(2) P(4) C(75) . . . . 36.5(2) no P(3) Ru(2) O(5) C(42) . . . . 168.7(4) no P(3) Ru(2) O(7) C(47) . . . . 79.9(4) no P(3) Ru(2) O(8) C(49) . . . . -77.8(4) no P(3) C(54) C(55) C(56) . . . . -179.3(5) no P(3) C(54) C(59) C(58) . . . . 178.2(5) no P(3) C(60) C(61) C(62) . . . . -179.9(5) no P(3) C(60) C(65) C(64) . . . . 179.8(5) no P(4) Ru(2) P(3) C(54) . . . . 159.3(2) no P(4) Ru(2) P(3) C(60) . . . . 39.7(2) no P(4) Ru(2) P(3) C(511) . . . . -92.4(7) no P(4) Ru(2) P(3) C(512) . . . . -73.3(7) no P(4) Ru(2) O(5) C(42) . . . . 74.4(4) no P(4) Ru(2) O(6) C(44) . . . . -73.7(4) no P(4) Ru(2) O(7) C(47) . . . . 174.3(4) no P(4) C(69) C(70) C(71) . . . . -178.2(5) no P(4) C(69) C(74) C(73) . . . . 178.2(4) no P(4) C(75) C(76) C(77) . . . . -178.1(6) no P(4) C(75) C(80) C(79) . . . . 177.4(5) no O(1) Ru(1) P(1) C(11) . . . . -175.5(2) no O(1) Ru(1) P(1) C(14) . . . . 66.2(2) no O(1) Ru(1) P(1) C(20) . . . . -54.1(2) no O(1) Ru(1) P(2) C(26) . . . . 15.9(2) no O(1) Ru(1) P(2) C(29) . . . . -100.4(2) no O(1) Ru(1) P(2) C(35) . . . . 140.0(2) no O(1) Ru(1) O(2) C(4) . . . . 15.4(4) no O(1) Ru(1) O(4) C(9) . . . . -174.2(4) no O(1) C(2) C(3) C(4) . . . . 5(1) no O(2) Ru(1) P(2) C(26) . . . . 107.1(2) no O(2) Ru(1) P(2) C(29) . . . . -9.2(2) no O(2) Ru(1) P(2) C(35) . . . . -128.8(2) no O(2) Ru(1) O(1) C(2) . . . . -15.6(4) no O(2) Ru(1) O(3) C(7) . . . . -91.3(4) no O(2) Ru(1) O(4) C(9) . . . . 94.3(4) no O(2) C(4) C(3) C(2) . . . . -6(1) no O(3) Ru(1) P(1) C(11) . . . . 7.6(2) no O(3) Ru(1) P(1) C(14) . . . . -110.7(2) no O(3) Ru(1) P(1) C(20) . . . . 129.0(2) no O(3) Ru(1) P(2) C(26) . . . . -169.1(2) no O(3) Ru(1) P(2) C(29) . . . . 74.6(2) no O(3) Ru(1) P(2) C(35) . . . . -45.0(2) no O(3) Ru(1) O(2) C(4) . . . . -167.2(4) no O(3) Ru(1) O(4) C(9) . . . . 10.6(4) no O(3) C(7) C(8) C(9) . . . . 6(1) no O(4) Ru(1) P(1) C(11) . . . . 98.4(2) no O(4) Ru(1) P(1) C(14) . . . . -19.9(2) no O(4) Ru(1) P(1) C(20) . . . . -140.1(2) no O(4) Ru(1) O(1) C(2) . . . . -100.5(4) no O(4) Ru(1) O(2) C(4) . . . . 101.4(4) no O(4) Ru(1) O(3) C(7) . . . . -6.5(4) no O(4) C(9) C(8) C(7) . . . . 0(1) no O(5) Ru(2) P(3) C(54) . . . . 66.8(2) no O(5) Ru(2) P(3) C(60) . . . . -52.7(2) no O(5) Ru(2) P(3) C(511) . . . . 175.1(7) no O(5) Ru(2) P(3) C(512) . . . . -165.7(7) no O(5) Ru(2) P(4) C(66) . . . . 5.5(2) no O(5) Ru(2) P(4) C(69) . . . . -112.6(2) no O(5) Ru(2) P(4) C(75) . . . . 127.2(2) no O(5) Ru(2) O(6) C(44) . . . . 18.7(4) no O(5) Ru(2) O(8) C(49) . . . . -168.1(4) no O(5) C(42) C(43) C(44) . . . . 8(1) no O(6) Ru(2) P(4) C(66) . . . . 95.5(2) no O(6) Ru(2) P(4) C(69) . . . . -22.7(2) no O(6) Ru(2) P(4) C(75) . . . . -142.8(2) no O(6) Ru(2) O(5) C(42) . . . . -14.4(4) no O(6) Ru(2) O(7) C(47) . . . . -97.0(4) no O(6) Ru(2) O(8) C(49) . . . . 101.4(4) no O(6) C(44) C(43) C(42) . . . . -3(1) no O(7) Ru(2) P(3) C(54) . . . . -108.8(2) no O(7) Ru(2) P(3) C(60) . . . . 131.7(2) no O(7) Ru(2) P(3) C(511) . . . . -0.5(7) no O(7) Ru(2) P(3) C(512) . . . . 18.7(7) no O(7) Ru(2) P(4) C(66) . . . . -177.4(2) no O(7) Ru(2) P(4) C(69) . . . . 64.5(2) no O(7) Ru(2) P(4) C(75) . . . . -55.7(2) no O(7) Ru(2) O(6) C(44) . . . . -165.5(4) no O(7) Ru(2) O(8) C(49) . . . . 14.3(4) no O(7) C(47) C(48) C(49) . . . . 6(1) no O(8) Ru(2) P(3) C(54) . . . . -18.7(2) no O(8) Ru(2) P(3) C(60) . . . . -138.3(2) no O(8) Ru(2) P(3) C(511) . . . . 89.6(7) no O(8) Ru(2) P(3) C(512) . . . . 108.7(7) no O(8) Ru(2) O(5) C(42) . . . . -98.7(4) no O(8) Ru(2) O(6) C(44) . . . . 104.3(4) no O(8) Ru(2) O(7) C(47) . . . . -12.7(4) no O(8) C(49) C(48) C(47) . . . . -5(1) no C(1) C(2) C(3) C(4) . . . . -175.4(5) no C(2) C(3) C(4) C(5) . . . . 174.5(5) no C(6) C(7) C(8) C(9) . . . . -174.1(6) no C(7) C(8) C(9) C(10) . . . . 179.6(6) no C(11) P(1) C(14) C(15) . . . . -168.0(4) no C(11) P(1) C(14) C(19) . . . . 15.3(5) no C(11) P(1) C(20) C(21) . . . . -160.0(4) no C(11) P(1) C(20) C(25) . . . . 23.5(5) no C(14) P(1) C(20) C(21) . . . . -56.1(5) no C(14) P(1) C(20) C(25) . . . . 127.4(4) no C(14) C(15) C(16) C(17) . . . . -1.5(9) no C(14) C(19) C(18) C(17) . . . . 0(1) no C(15) C(14) P(1) C(20) . . . . 87.1(4) no C(15) C(14) C(19) C(18) . . . . -0.8(8) no C(15) C(16) C(17) C(18) . . . . 1(1) no C(16) C(15) C(14) C(19) . . . . 1.5(8) no C(16) C(17) C(18) C(19) . . . . 0(1) no C(19) C(14) P(1) C(20) . . . . -89.6(5) no C(20) C(21) C(22) C(23) . . . . 1(1) no C(20) C(25) C(24) C(23) . . . . 1(1) no C(21) C(20) C(25) C(24) . . . . -0.7(8) no C(21) C(22) C(23) C(24) . . . . -1(1) no C(22) C(21) C(20) C(25) . . . . -0.5(9) no C(22) C(23) C(24) C(25) . . . . -1(1) no C(26) P(2) C(29) C(30) . . . . 173.3(4) no C(26) P(2) C(29) C(34) . . . . -8.9(5) no C(26) P(2) C(35) C(36) . . . . 167.7(4) no C(26) P(2) C(35) C(40) . . . . -14.3(5) no C(29) P(2) C(35) C(36) . . . . -88.8(4) no C(29) P(2) C(35) C(40) . . . . 89.2(5) no C(29) C(30) C(31) C(32) . . . . -3(1) no C(29) C(34) C(33) C(32) . . . . 0(1) no C(30) C(29) P(2) C(35) . . . . 68.6(5) no C(30) C(29) C(34) C(33) . . . . -1.1(8) no C(30) C(31) C(32) C(33) . . . . 2(1) no C(31) C(30) C(29) C(34) . . . . 2.6(9) no C(31) C(32) C(33) C(34) . . . . 0(1) no C(34) C(29) P(2) C(35) . . . . -113.6(4) no C(35) C(36) C(37) C(38) . . . . 0.5(8) no C(35) C(40) C(39) C(38) . . . . 0.0(9) no C(36) C(35) C(40) C(39) . . . . 1.4(8) no C(36) C(37) C(38) C(39) . . . . 1.0(9) no C(37) C(36) C(35) C(40) . . . . -1.7(8) no C(37) C(38) C(39) C(40) . . . . -1.2(9) no C(41) C(42) C(43) C(44) . . . . -171.2(6) no C(42) C(43) C(44) C(45) . . . . 176.9(5) no C(46) C(47) C(48) C(49) . . . . -172.2(6) no C(47) C(48) C(49) C(50) . . . . 172.9(6) no C(54) P(3) C(60) C(61) . . . . -71.4(5) no C(54) P(3) C(60) C(65) . . . . 108.2(5) no C(54) C(55) C(56) C(57) . . . . 0(1) no C(54) C(59) C(58) C(57) . . . . 2(1) no C(55) C(54) P(3) C(60) . . . . 93.7(5) no C(55) C(54) P(3) C(511) . . . . -157.1(7) no C(55) C(54) P(3) C(512) . . . . -166.4(7) no C(55) C(54) C(59) C(58) . . . . -0.4(9) no C(55) C(56) C(57) C(58) . . . . 1(1) no C(56) C(55) C(54) C(59) . . . . -0.7(9) no C(56) C(57) C(58) C(59) . . . . -2(1) no C(59) C(54) P(3) C(60) . . . . -84.9(5) no C(59) C(54) P(3) C(511) . . . . 24.3(7) no C(59) C(54) P(3) C(512) . . . . 15.0(7) no C(60) C(61) C(62) C(63) . . . . -1(1) no C(60) C(65) C(64) C(63) . . . . 1(1) no C(61) C(60) P(3) C(511) . . . . -168.6(7) no C(61) C(60) P(3) C(512) . . . . 178.9(7) no C(61) C(60) C(65) C(64) . . . . -0.6(9) no C(61) C(62) C(63) C(64) . . . . 1(1) no C(62) C(61) C(60) C(65) . . . . 0.5(9) no C(62) C(63) C(64) C(65) . . . . -1(1) no C(65) C(60) P(3) C(511) . . . . 11.0(8) no C(65) C(60) P(3) C(512) . . . . -1.5(7) no C(66) P(4) C(69) C(70) . . . . -169.5(4) no C(66) P(4) C(69) C(74) . . . . 11.5(5) no C(66) P(4) C(75) C(76) . . . . -178.9(5) no C(66) P(4) C(75) C(80) . . . . 4.2(5) no C(69) P(4) C(75) C(76) . . . . -74.9(5) no C(69) P(4) C(75) C(80) . . . . 108.2(5) no C(69) C(70) C(71) C(72) . . . . -1(1) no C(69) C(74) C(73) C(72) . . . . 0(1) no C(70) C(69) P(4) C(75) . . . . 87.2(5) no C(70) C(69) C(74) C(73) . . . . -0.7(8) no C(70) C(71) C(72) C(73) . . . . 0(1) no C(71) C(70) C(69) C(74) . . . . 0.8(9) no C(71) C(72) C(73) C(74) . . . . 0(1) no C(74) C(69) P(4) C(75) . . . . -91.8(5) no C(75) C(76) C(77) C(78) . . . . 0(1) no C(75) C(80) C(79) C(78) . . . . 1(1) no C(76) C(75) C(80) C(79) . . . . 0.5(9) no C(76) C(77) C(78) C(79) . . . . 1(1) no C(77) C(76) C(75) C(80) . . . . -1(1) no C(77) C(78) C(79) C(80) . . . . -2(1) no data_benmat17cu _database_code_depnum_ccdc_archive 'CCDC 631387' _audit_creation_date 06-09-18 _audit_creation_method CRYSTALS_ver_12.18 _audit_update_record ; 2000-04 acw tries to model solvent area with sensible fragments - but gets nowhere. 2000-04-13 acw puts together a cif for mjb's thesis with solvent area as unidentified atoms. 2006-09-19 acw tidies up structure using CRYSTALS ; _oxford_structure_analysis_title mat17cu _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.096(4) _cell_length_b 22.508(4) _cell_length_c 27.778(3) _cell_angle_alpha 90 _cell_angle_beta 102.41(2) _cell_angle_gamma 90 _cell_volume 7386(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.2955 0.4335 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru 0.0552 3.2960 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C72 H68 Cl2 O8 P4 Ru2 # Dc = 1.31 Fooo = 3032.00 Mu = 51.96 M = 1458.27 # Found Formula = C75.50 H76 Cl1 O8 P4 Ru2 # Dc = 1.32 FOOO = 3032.00 Mu = 48.76 M = 1472.92 _chemical_formula_sum 'C75.5 H76 Cl O8 P4 Ru2' _chemical_formula_moiety 'C72 H68 O8 P4 Ru2, 0.5(C H2 Cl2), 0.5(C6 H14)' _chemical_compound_source local _chemical_formula_weight 1472.92 _cell_measurement_temperature 193.2 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 53.9 _cell_measurement_theta_max 54.8 _exptl_crystal_description cuboid _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_meas 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 4.876 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.555 _exptl_absorpt_correction_T_min 0.392 _exptl_special_details ; The scan width was (1.10+0.30tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Data can only be collected to 2theta 120 deg on a AFC6R diffractometer when the evacuated beam tunnel in used. ; _diffrn_measurement_device_type 'Rigaku AFC6R' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method \w-2\q _diffrn_measurement_device_details ; Rigaku AFC6R diffractometer with extended arm and evacuated collimator and beam tunnel. Data cannot be collected beyond \y 60 deg in this configuration. ; # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Watkin et al 2003)' _computing_publication_material 'CRYSTALS (Watkin et al 2003)' _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -6.46 _diffrn_ambient_temperature 193.2 _diffrn_reflns_number 11280 _reflns_number_total 10940 _diffrn_reflns_av_R_equivalents 0.02294 _diffrn_reflns_av_sigmaI/netI 0.060 # Number of reflections with Friedels Law is 10940 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10951 _diffrn_reflns_theta_min 2.551 _diffrn_reflns_theta_max 59.954 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 59.954 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 31 _oxford_diffrn_Wilson_B_factor 1.95 _oxford_diffrn_Wilson_scale 3.28 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.61 _refine_diff_density_max 1.07 _refine_ls_number_reflns 8826 _refine_ls_number_restraints 54 _refine_ls_number_parameters 856 #_refine_ls_R_factor_ref 0.0394 _refine_ls_wR_factor_ref 0.0444 _refine_ls_goodness_of_fit_ref 1.1497 #_reflns_number_all 10879 _refine_ls_R_factor_all 0.0521 _refine_ls_wR_factor_all 0.0523 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 8826 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_gt 0.0444 _refine_ls_shift/su_max 0.019 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Carruthers & Watkin, 1979, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 4.09 -0.747 3.22 ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [Ru~2~(C~26~H~20~P~2~)~2~(C~5~H~7~O~2~)~4~].0.5CH~2~Cl~2~.0.5C~6~H~14~ is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one [Ru~2~(C~26~H~20~P~2~)~2~(C~5~H~7~O~2~)~4~] molecule and a region containing solvate molecules. Of the solvates, there appears to be a molecule of dichloromethane with occupancy about 0.5 and a series of peaks which are consistent with a molecule of n-hexane, again with an occupancy of about 0.5. Close contacts with adjacent solvate molecules indicate that their occupancies must, indeed, be =<0.5 and so these sites have all been assigned occupancies of 0.5. Restraints were imposed upon distances, angles and displacement parameters for the solvate molecules. The largest features in the final difference electron density map are close to the Ru atoms or within the disordered solvate region of the cell. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; Hydrogen atoms were included at idealized positions and ride on the atom to which they are attached. ; _publ_section_exptl_prep ; The compound was prepared by MJB and recrystallized from dichloromethane/hexane. The sample ID is mat17. ; #**************************************************************************** # Insert your own references if required - in alphabetical order _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Carruthers, J.R. & Watkin, D.J. (1979), Acta Cryst. A35, 698-699. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Johnson, C.K. (1976) ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ru1 Ru 0.20808(2) 0.409770(11) 0.920313(9) 0.0259 1.0000 Uani . . . . . . Ru2 Ru 0.16245(2) 0.335860(11) 0.664783(9) 0.0273 1.0000 Uani . . . . . . Cl1 Cl 0.1415(6) 0.3763(3) 0.4447(2) 0.1658 0.5000 Uani D U . . . . Cl2 Cl 0.3560(7) 0.3286(4) 0.4867(2) 0.1993 0.5000 Uani D U . . . . P1 P 0.29911(7) 0.33074(4) 0.89636(3) 0.0264 1.0000 Uani . . . . . . P2 P 0.06322(7) 0.40109(4) 0.85440(3) 0.0265 1.0000 Uani . . . . . . P3 P 0.22447(7) 0.27155(4) 0.72770(3) 0.0281 1.0000 Uani . . . . . . P4 P 0.21136(7) 0.41791(4) 0.71143(3) 0.0279 1.0000 Uani . . . . . . O1 O 0.2850(2) 0.46743(10) 0.88051(8) 0.0306 1.0000 Uani . . . . . . O2 O 0.1296(2) 0.47941(11) 0.94975(9) 0.0365 1.0000 Uani . . . . . . O3 O 0.1366(2) 0.35657(11) 0.96617(9) 0.0343 1.0000 Uani . . . . . . O4 O 0.3374(2) 0.43361(11) 0.98006(9) 0.0352 1.0000 Uani . . . . . . O5 O 0.0011(2) 0.33591(11) 0.67840(9) 0.0337 1.0000 Uani . . . . . . O6 O 0.1085(2) 0.38583(11) 0.60070(9) 0.0391 1.0000 Uani . . . . . . O7 O 0.3180(2) 0.33405(11) 0.64610(10) 0.0396 1.0000 Uani . . . . . . O8 O 0.1076(2) 0.26631(11) 0.61523(9) 0.0376 1.0000 Uani . . . . . . C1 C 0.3200(4) 0.55541(18) 0.84159(15) 0.0431 1.0000 Uani . . . . . . C2 C 0.2645(3) 0.52298(16) 0.87721(13) 0.0343 1.0000 Uani . . . . . . C3 C 0.1948(4) 0.55422(17) 0.90269(16) 0.0428 1.0000 Uani . . . . . . C4 C 0.1363(3) 0.53337(17) 0.93689(14) 0.0390 1.0000 Uani . . . . . . C5 C 0.0721(4) 0.5764(2) 0.96241(19) 0.0573 1.0000 Uani . . . . . . C6 C 0.1170(4) 0.3013(2) 1.03509(17) 0.0526 1.0000 Uani . . . . . . C7 C 0.1804(4) 0.34676(17) 1.01128(14) 0.0393 1.0000 Uani . . . . . . C8 C 0.2779(4) 0.37237(18) 1.03909(14) 0.0439 1.0000 Uani . . . . . . C9 C 0.3473(3) 0.41466(17) 1.02360(13) 0.0375 1.0000 Uani . . . . . . C10 C 0.4433(4) 0.4413(2) 1.06044(15) 0.0520 1.0000 Uani . . . . . . C11 C 0.2675(3) 0.30828(15) 0.83337(13) 0.0286 1.0000 Uani . . . . . . C12 C 0.2481(3) 0.29432(15) 0.79074(14) 0.0308 1.0000 Uani . . . . . . C13 C 0.2764(3) 0.25994(15) 0.92579(13) 0.0335 1.0000 Uani . . . . . . C14 C 0.3398(4) 0.24869(18) 0.97303(15) 0.0472 1.0000 Uani . . . . . . C15 C 0.3189(5) 0.1987(2) 0.99803(18) 0.0607 1.0000 Uani . . . . . . C16 C 0.2346(5) 0.1602(2) 0.9773(2) 0.0654 1.0000 Uani . . . . . . C17 C 0.1713(4) 0.17094(19) 0.9305(2) 0.0586 1.0000 Uani . . . . . . C18 C 0.1917(3) 0.22090(17) 0.90439(16) 0.0410 1.0000 Uani . . . . . . C19 C 0.4547(3) 0.33299(16) 0.90611(13) 0.0326 1.0000 Uani . . . . . . C20 C 0.5153(3) 0.38034(18) 0.93134(14) 0.0378 1.0000 Uani . . . . . . C21 C 0.6323(4) 0.3806(2) 0.93965(16) 0.0490 1.0000 Uani . . . . . . C22 C 0.6881(4) 0.3356(2) 0.92233(19) 0.0598 1.0000 Uani . . . . . . C23 C 0.6277(4) 0.2892(2) 0.8956(2) 0.0660 1.0000 Uani . . . . . . C24 C 0.5128(4) 0.2877(2) 0.88851(18) 0.0519 1.0000 Uani . . . . . . C25 C 0.1048(3) 0.41624(15) 0.79810(13) 0.0288 1.0000 Uani . . . . . . C26 C 0.1476(3) 0.42237(15) 0.76344(13) 0.0293 1.0000 Uani . . . . . . C27 C -0.0134(3) 0.33104(15) 0.84124(14) 0.0318 1.0000 Uani . . . . . . C28 C -0.0414(3) 0.30057(17) 0.88056(16) 0.0406 1.0000 Uani . . . . . . C29 C -0.1008(3) 0.24750(19) 0.87271(18) 0.0504 1.0000 Uani . . . . . . C30 C -0.1316(4) 0.22428(19) 0.8256(2) 0.0542 1.0000 Uani . . . . . . C31 C -0.1033(4) 0.2538(2) 0.78662(19) 0.0550 1.0000 Uani . . . . . . C32 C -0.0445(3) 0.30671(19) 0.79404(15) 0.0430 1.0000 Uani . . . . . . C33 C -0.0521(3) 0.45446(15) 0.85269(13) 0.0309 1.0000 Uani . . . . . . C34 C -0.1020(3) 0.45670(18) 0.89332(15) 0.0415 1.0000 Uani . . . . . . C35 C -0.1849(4) 0.49737(19) 0.89551(17) 0.0493 1.0000 Uani . . . . . . C36 C -0.2215(4) 0.53640(19) 0.85651(19) 0.0521 1.0000 Uani . . . . . . C37 C -0.1735(4) 0.53421(19) 0.81617(18) 0.0507 1.0000 Uani . . . . . . C38 C -0.0881(3) 0.49314(17) 0.81370(15) 0.0379 1.0000 Uani . . . . . . C39 C -0.1918(4) 0.3550(3) 0.6684(2) 0.0786 1.0000 Uani . . . . . . C40 C -0.0832(3) 0.36243(18) 0.65145(15) 0.0434 1.0000 Uani . . . . . . C41 C -0.0807(4) 0.39568(19) 0.60959(16) 0.0489 1.0000 Uani . . . . . . C42 C 0.0088(4) 0.40547(17) 0.58662(15) 0.0456 1.0000 Uani . . . . . . C43 C -0.0116(5) 0.4416(2) 0.53983(18) 0.0680 1.0000 Uani . . . . . . C44 C 0.4706(5) 0.3038(3) 0.6132(2) 0.0740 1.0000 Uani . . . . . . C45 C 0.3485(4) 0.2978(2) 0.61689(16) 0.0486 1.0000 Uani . . . . . . C46 C 0.2809(4) 0.2538(2) 0.58953(17) 0.0532 1.0000 Uani . . . . . . C47 C 0.1672(4) 0.24170(18) 0.58883(14) 0.0425 1.0000 Uani . . . . . . C48 C 0.1094(5) 0.1941(2) 0.55452(18) 0.0595 1.0000 Uani . . . . . . C49 C 0.1361(3) 0.20588(15) 0.73139(13) 0.0313 1.0000 Uani . . . . . . C50 C 0.0364(3) 0.19685(17) 0.69674(14) 0.0384 1.0000 Uani . . . . . . C51 C -0.0292(4) 0.14655(18) 0.70032(16) 0.0462 1.0000 Uani . . . . . . C52 C 0.0038(4) 0.10612(19) 0.73811(18) 0.0503 1.0000 Uani . . . . . . C53 C 0.1023(4) 0.11551(18) 0.77238(17) 0.0516 1.0000 Uani . . . . . . C54 C 0.1689(4) 0.16515(17) 0.76964(15) 0.0421 1.0000 Uani . . . . . . C55 C 0.3651(3) 0.23935(16) 0.72889(13) 0.0344 1.0000 Uani . . . . . . C56 C 0.3758(4) 0.18689(18) 0.70339(16) 0.0455 1.0000 Uani . . . . . . C57 C 0.4813(4) 0.1647(2) 0.7025(2) 0.0593 1.0000 Uani . . . . . . C58 C 0.5769(4) 0.1938(2) 0.7265(2) 0.0646 1.0000 Uani . . . . . . C59 C 0.5673(4) 0.2465(2) 0.7515(2) 0.0619 1.0000 Uani . . . . . . C60 C 0.4629(3) 0.26891(19) 0.75255(16) 0.0454 1.0000 Uani . . . . . . C61 C 0.1709(3) 0.49000(16) 0.68139(14) 0.0367 1.0000 Uani . . . . . . C62 C 0.2039(4) 0.50199(19) 0.63704(15) 0.0492 1.0000 Uani . . . . . . C63 C 0.1758(5) 0.5554(2) 0.61316(17) 0.0644 1.0000 Uani . . . . . . C64 C 0.1146(5) 0.5971(2) 0.63260(19) 0.0662 1.0000 Uani . . . . . . C65 C 0.0816(5) 0.5854(2) 0.6760(2) 0.0648 1.0000 Uani . . . . . . C66 C 0.1095(4) 0.53189(18) 0.70041(16) 0.0454 1.0000 Uani . . . . . . C67 C 0.3618(3) 0.42737(16) 0.73878(13) 0.0339 1.0000 Uani . . . . . . C68 C 0.4380(3) 0.4301(2) 0.70728(16) 0.0470 1.0000 Uani . . . . . . C69 C 0.5528(4) 0.4318(2) 0.72675(18) 0.0552 1.0000 Uani . . . . . . C70 C 0.5950(4) 0.4303(2) 0.77711(18) 0.0520 1.0000 Uani . . . . . . C71 C 0.5211(3) 0.42866(19) 0.80760(16) 0.0462 1.0000 Uani . . . . . . C72 C 0.4049(3) 0.42718(16) 0.78961(14) 0.0359 1.0000 Uani . . . . . . C101 C 0.7595(13) 0.5456(6) 0.6718(5) 0.0969 0.5000 Uani D U . . . . C102 C 0.6419(16) 0.5550(8) 0.6407(7) 0.1527 0.5000 Uani D U . . . . C103 C 0.6044(18) 0.5039(7) 0.6057(6) 0.1499 0.5000 Uani D U . . . . C104 C 0.4827(18) 0.5157(9) 0.5832(8) 0.1685 0.5000 Uani D U . . . . C105 C 0.4390(18) 0.4641(10) 0.5474(9) 0.1817 0.5000 Uani D U . . . . C106 C 0.3119(15) 0.4584(9) 0.5221(6) 0.1258 0.5000 Uani D U . . . . C110 C 0.2156(15) 0.3389(12) 0.4905(7) 0.1745 0.5000 Uani D U . . . . H11 H 0.3664 0.52692 0.82664 0.0511 1.0000 Uiso R . . . . . H12 H 0.3699 0.58742 0.85939 0.0511 1.0000 Uiso R . . . . . H13 H 0.2606 0.57352 0.81500 0.0511 1.0000 Uiso R . . . . . H31 H 0.1862 0.59762 0.89510 0.0506 1.0000 Uiso R . . . . . H51 H 0.0814 0.6176 0.95045 0.0691 1.0000 Uiso R . . . . . H52 H 0.1024 0.5745 0.99882 0.0691 1.0000 Uiso R . . . . . H53 H -0.0100 0.5656 0.95486 0.0691 1.0000 Uiso R . . . . . H61 H 0.1561 0.2959 1.07038 0.0656 1.0000 Uiso R . . . . . H62 H 0.0378 0.3154 1.03330 0.0656 1.0000 Uiso R . . . . . H63 H 0.1152 0.2625 1.01732 0.0656 1.0000 Uiso R . . . . . H81 H 0.3010 0.35903 1.07415 0.0517 1.0000 Uiso R . . . . . H101 H 0.4449 0.4239 1.09372 0.0597 1.0000 Uiso R . . . . . H102 H 0.4327 0.4853 1.06165 0.0597 1.0000 Uiso R . . . . . H103 H 0.5163 0.4325 1.05055 0.0597 1.0000 Uiso R . . . . . H141 H 0.4006 0.27704 0.98874 0.0561 1.0000 Uiso R . . . . . H151 H 0.3657 0.1905 1.03165 0.0737 1.0000 Uiso R . . . . . H161 H 0.2189 0.1243 0.9960 0.0829 1.0000 Uiso R . . . . . H171 H 0.1102 0.14251 0.9153 0.0735 1.0000 Uiso R . . . . . H181 H 0.1457 0.22853 0.87050 0.0504 1.0000 Uiso R . . . . . H201 H 0.4745 0.41398 0.94338 0.0449 1.0000 Uiso R . . . . . H211 H 0.6760 0.4140 0.95848 0.0581 1.0000 Uiso R . . . . . H221 H 0.7727 0.3358 0.92881 0.0711 1.0000 Uiso R . . . . . H231 H 0.6687 0.2571 0.8816 0.0793 1.0000 Uiso R . . . . . H241 H 0.4699 0.2535 0.87043 0.0619 1.0000 Uiso R . . . . . H281 H -0.0186 0.31706 0.91468 0.0489 1.0000 Uiso R . . . . . H291 H -0.1213 0.22602 0.90107 0.0616 1.0000 Uiso R . . . . . H301 H -0.1744 0.18601 0.8198 0.0654 1.0000 Uiso R . . . . . H311 H -0.1255 0.2368 0.75265 0.0668 1.0000 Uiso R . . . . . H321 H -0.0239 0.32771 0.76547 0.0520 1.0000 Uiso R . . . . . H341 H -0.0771 0.42830 0.92122 0.0512 1.0000 Uiso R . . . . . H351 H -0.2191 0.49904 0.92519 0.0614 1.0000 Uiso R . . . . . H361 H -0.2825 0.56590 0.85794 0.0629 1.0000 Uiso R . . . . . H371 H -0.1999 0.56228 0.78815 0.0591 1.0000 Uiso R . . . . . H381 H -0.0535 0.49173 0.78412 0.0459 1.0000 Uiso R . . . . . H391 H -0.2536 0.3769 0.6456 0.0935 1.0000 Uiso R . . . . . H392 H -0.1828 0.3714 0.7025 0.0935 1.0000 Uiso R . . . . . H393 H -0.2115 0.3119 0.6684 0.0935 1.0000 Uiso R . . . . . H411 H -0.1537 0.41531 0.59378 0.0558 1.0000 Uiso R . . . . . H431 H -0.0922 0.4552 0.53159 0.0764 1.0000 Uiso R . . . . . H432 H 0.0396 0.4770 0.54459 0.0764 1.0000 Uiso R . . . . . H433 H 0.0042 0.4166 0.51230 0.0764 1.0000 Uiso R . . . . . H441 H 0.5068 0.3370 0.6349 0.0926 1.0000 Uiso R . . . . . H442 H 0.5116 0.2659 0.6240 0.0926 1.0000 Uiso R . . . . . H443 H 0.4745 0.3124 0.5783 0.0926 1.0000 Uiso R . . . . . H461 H 0.3180 0.2282 0.56816 0.0652 1.0000 Uiso R . . . . . H481 H 0.0290 0.1902 0.55782 0.0686 1.0000 Uiso R . . . . . H482 H 0.1496 0.1555 0.56310 0.0686 1.0000 Uiso R . . . . . H483 H 0.1112 0.2050 0.51980 0.0686 1.0000 Uiso R . . . . . H501 H 0.0117 0.22606 0.66941 0.0457 1.0000 Uiso R . . . . . H511 H -0.1009 0.13976 0.67524 0.0552 1.0000 Uiso R . . . . . H521 H -0.0437 0.07032 0.74047 0.0613 1.0000 Uiso R . . . . . H531 H 0.1264 0.08623 0.79969 0.0621 1.0000 Uiso R . . . . . H541 H 0.2401 0.17166 0.79501 0.0503 1.0000 Uiso R . . . . . H561 H 0.3065 0.16539 0.68576 0.0541 1.0000 Uiso R . . . . . H571 H 0.4884 0.1271 0.6841 0.0709 1.0000 Uiso R . . . . . H581 H 0.6534 0.1773 0.7261 0.0770 1.0000 Uiso R . . . . . H591 H 0.6369 0.2679 0.7688 0.0731 1.0000 Uiso R . . . . . H601 H 0.4566 0.30690 0.77044 0.0537 1.0000 Uiso R . . . . . H621 H 0.2481 0.47176 0.62262 0.0577 1.0000 Uiso R . . . . . H631 H 0.1999 0.5639 0.58160 0.0745 1.0000 Uiso R . . . . . H641 H 0.0943 0.6358 0.61524 0.0743 1.0000 Uiso R . . . . . H651 H 0.0372 0.6157 0.6902 0.0748 1.0000 Uiso R . . . . . H661 H 0.0848 0.52377 0.73189 0.0540 1.0000 Uiso R . . . . . H681 H 0.4090 0.4307 0.67074 0.0576 1.0000 Uiso R . . . . . H691 H 0.6066 0.4342 0.70404 0.0690 1.0000 Uiso R . . . . . H701 H 0.6785 0.4305 0.79084 0.0617 1.0000 Uiso R . . . . . H711 H 0.5513 0.42848 0.84406 0.0538 1.0000 Uiso R . . . . . H721 H 0.3524 0.42599 0.81289 0.0434 1.0000 Uiso R . . . . . H1011 H 0.7808 0.5803 0.6944 0.1210 0.5000 Uiso R . . . . . H1012 H 0.7607 0.5085 0.6918 0.1210 0.5000 Uiso R . . . . . H1013 H 0.8147 0.5417 0.6499 0.1210 0.5000 Uiso R . . . . . H1021 H 0.5876 0.5591 0.6630 0.1876 0.5000 Uiso R . . . . . H1022 H 0.6415 0.5923 0.6211 0.1876 0.5000 Uiso R . . . . . H1031 H 0.6126 0.4653 0.6240 0.1846 0.5000 Uiso R . . . . . H1032 H 0.6501 0.5026 0.5797 0.1846 0.5000 Uiso R . . . . . H1041 H 0.4379 0.5177 0.6095 0.2111 0.5000 Uiso R . . . . . H1042 H 0.4753 0.5541 0.5647 0.2111 0.5000 Uiso R . . . . . H1051 H 0.4597 0.4265 0.5665 0.2231 0.5000 Uiso R . . . . . H1052 H 0.4815 0.4665 0.5203 0.2231 0.5000 Uiso R . . . . . H1061 H 0.3005 0.4224 0.5005 0.1640 0.5000 Uiso R . . . . . H1062 H 0.2658 0.4546 0.5478 0.1640 0.5000 Uiso R . . . . . H1063 H 0.2876 0.4946 0.5017 0.1640 0.5000 Uiso R . . . . . H1101 H 0.2141 0.3605 0.5218 0.2153 0.5000 Uiso R . . . . . H1102 H 0.1799 0.2990 0.4912 0.2153 0.5000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02846(15) 0.02270(14) 0.02679(15) 0.00105(10) 0.00661(10) 0.00253(10) Ru2 0.02964(15) 0.02534(15) 0.02660(15) -0.00144(10) 0.00510(10) -0.00167(10) Cl1 0.197(6) 0.177(5) 0.120(4) 0.029(4) 0.025(4) 0.038(4) Cl2 0.226(7) 0.266(8) 0.115(4) 0.012(4) 0.057(4) 0.067(6) P1 0.0253(4) 0.0239(4) 0.0297(4) 0.0003(3) 0.0051(3) 0.0020(3) P2 0.0258(4) 0.0256(4) 0.0292(4) 0.0024(3) 0.0085(3) 0.0031(3) P3 0.0278(4) 0.0243(4) 0.0309(4) -0.0030(3) 0.0031(3) -0.0006(3) P4 0.0301(4) 0.0254(4) 0.0289(4) 0.0000(3) 0.0079(4) -0.0037(3) O1 0.0338(13) 0.0251(13) 0.0329(13) 0.0030(10) 0.0068(10) 0.0006(10) O2 0.0426(14) 0.0322(14) 0.0364(13) -0.0038(11) 0.0125(11) 0.0083(11) O3 0.0389(14) 0.0315(13) 0.0350(14) 0.0053(10) 0.0132(11) 0.0031(11) O4 0.0382(14) 0.0356(13) 0.0302(13) -0.0040(11) 0.0036(11) 0.0025(11) O5 0.0276(13) 0.0356(14) 0.0368(13) 0.0002(11) 0.0044(11) 0.0000(10) O6 0.0536(17) 0.0331(13) 0.0284(13) 0.0014(11) 0.0040(12) -0.0036(12) O7 0.0356(14) 0.0429(15) 0.0444(15) -0.0072(12) 0.0178(12) -0.0022(11) O8 0.0448(15) 0.0323(13) 0.0325(13) -0.0045(11) 0.0013(11) -0.0017(11) C1 0.052(2) 0.032(2) 0.043(2) 0.0058(17) 0.0068(19) -0.0042(18) C2 0.040(2) 0.029(2) 0.0317(19) 0.0006(15) 0.0015(16) -0.0042(16) C3 0.050(2) 0.0230(18) 0.054(2) -0.0006(17) 0.0068(19) 0.0016(17) C4 0.041(2) 0.030(2) 0.043(2) -0.0082(17) 0.0017(17) 0.0064(16) C5 0.068(3) 0.038(2) 0.067(3) -0.012(2) 0.016(2) 0.017(2) C6 0.069(3) 0.043(2) 0.052(3) 0.011(2) 0.027(2) 0.009(2) C7 0.053(2) 0.034(2) 0.037(2) 0.0034(16) 0.0210(19) 0.0139(18) C8 0.060(3) 0.042(2) 0.0274(19) 0.0007(17) 0.0040(18) 0.0071(19) C9 0.042(2) 0.038(2) 0.030(2) -0.0059(16) 0.0034(16) 0.0144(17) C10 0.057(3) 0.053(3) 0.039(2) -0.0092(19) -0.0047(19) 0.010(2) C11 0.0278(18) 0.0244(17) 0.034(2) -0.0006(15) 0.0066(15) 0.0037(14) C12 0.0279(18) 0.0234(17) 0.040(2) 0.0023(15) 0.0047(15) 0.0037(14) C13 0.039(2) 0.0259(18) 0.038(2) 0.0026(15) 0.0126(16) 0.0076(15) C14 0.060(3) 0.039(2) 0.041(2) 0.0066(18) 0.0078(19) 0.0124(19) C15 0.088(4) 0.044(3) 0.053(3) 0.017(2) 0.020(3) 0.023(3) C16 0.087(4) 0.033(2) 0.087(4) 0.021(2) 0.043(3) 0.015(2) C17 0.061(3) 0.032(2) 0.092(4) 0.003(2) 0.035(3) 0.000(2) C18 0.035(2) 0.034(2) 0.057(2) 0.0033(18) 0.0166(18) 0.0015(16) C19 0.0240(17) 0.036(2) 0.0362(19) 0.0032(15) 0.0035(15) 0.0029(15) C20 0.036(2) 0.043(2) 0.0340(19) 0.0045(16) 0.0050(16) -0.0032(17) C21 0.040(2) 0.060(3) 0.046(2) 0.004(2) 0.0054(18) -0.011(2) C22 0.028(2) 0.081(4) 0.069(3) 0.003(3) 0.007(2) 0.003(2) C23 0.038(2) 0.073(3) 0.088(4) -0.017(3) 0.014(2) 0.015(2) C24 0.034(2) 0.052(3) 0.069(3) -0.010(2) 0.009(2) 0.0061(19) C25 0.0241(17) 0.0266(17) 0.035(2) 0.0010(14) 0.0047(15) -0.0001(14) C26 0.0300(18) 0.0250(17) 0.0328(19) 0.0026(14) 0.0066(16) -0.0001(14) C27 0.0232(17) 0.0296(18) 0.044(2) 0.0005(16) 0.0096(15) 0.0030(14) C28 0.033(2) 0.036(2) 0.053(2) 0.0077(18) 0.0103(17) 0.0001(16) C29 0.036(2) 0.045(2) 0.074(3) 0.011(2) 0.018(2) -0.0063(18) C30 0.035(2) 0.038(2) 0.091(4) -0.005(2) 0.016(2) -0.0060(18) C31 0.047(2) 0.052(3) 0.068(3) -0.021(2) 0.016(2) -0.016(2) C32 0.038(2) 0.045(2) 0.046(2) -0.0074(19) 0.0110(18) -0.0060(18) C33 0.0243(17) 0.0243(17) 0.042(2) -0.0012(15) 0.0033(15) 0.0025(14) C34 0.039(2) 0.041(2) 0.048(2) 0.0061(18) 0.0171(18) 0.0102(17) C35 0.048(2) 0.047(2) 0.059(3) -0.002(2) 0.024(2) 0.011(2) C36 0.040(2) 0.040(2) 0.077(3) 0.000(2) 0.015(2) 0.0160(18) C37 0.044(2) 0.038(2) 0.066(3) 0.006(2) 0.002(2) 0.0086(18) C38 0.036(2) 0.0329(19) 0.045(2) 0.0056(17) 0.0110(17) 0.0036(16) C39 0.044(3) 0.101(4) 0.089(4) 0.021(3) 0.010(3) 0.017(3) C40 0.033(2) 0.044(2) 0.051(2) -0.0070(19) 0.0025(18) 0.0024(17) C41 0.050(3) 0.044(2) 0.046(2) 0.0066(19) -0.005(2) 0.0097(19) C42 0.061(3) 0.031(2) 0.039(2) 0.0012(17) -0.002(2) -0.0037(19) C43 0.084(4) 0.059(3) 0.048(3) 0.021(2) -0.015(2) -0.010(3) C44 0.059(3) 0.089(4) 0.084(4) -0.030(3) 0.038(3) -0.001(3) C45 0.046(2) 0.057(3) 0.046(2) -0.008(2) 0.0185(19) 0.000(2) C46 0.060(3) 0.054(3) 0.049(2) -0.016(2) 0.019(2) 0.004(2) C47 0.055(3) 0.036(2) 0.033(2) -0.0029(17) 0.0023(18) 0.0056(18) C48 0.073(3) 0.046(3) 0.053(3) -0.016(2) -0.002(2) 0.004(2) C49 0.0332(19) 0.0233(17) 0.038(2) -0.0036(15) 0.0089(15) -0.0004(14) C50 0.041(2) 0.0309(19) 0.042(2) 0.0020(16) 0.0069(17) -0.0024(16) C51 0.048(2) 0.039(2) 0.051(2) -0.0071(19) 0.0092(19) -0.0137(19) C52 0.054(3) 0.032(2) 0.068(3) -0.002(2) 0.018(2) -0.0101(19) C53 0.068(3) 0.028(2) 0.059(3) 0.0130(19) 0.015(2) -0.0011(19) C54 0.048(2) 0.031(2) 0.047(2) 0.0023(17) 0.0091(18) 0.0018(17) C55 0.037(2) 0.0330(19) 0.0317(18) -0.0036(15) 0.0029(15) 0.0060(16) C56 0.041(2) 0.040(2) 0.054(2) -0.0137(19) 0.0078(19) 0.0035(18) C57 0.055(3) 0.049(3) 0.073(3) -0.017(2) 0.012(2) 0.013(2) C58 0.038(2) 0.065(3) 0.089(4) -0.012(3) 0.011(2) 0.018(2) C59 0.035(2) 0.069(3) 0.079(3) -0.015(3) 0.006(2) 0.002(2) C60 0.031(2) 0.044(2) 0.059(3) -0.013(2) 0.0053(18) 0.0011(17) C61 0.043(2) 0.0307(19) 0.0341(19) 0.0039(16) 0.0040(16) -0.0089(16) C62 0.067(3) 0.038(2) 0.039(2) 0.0031(18) 0.004(2) -0.016(2) C63 0.097(4) 0.049(3) 0.041(2) 0.013(2) -0.001(2) -0.030(3) C64 0.091(4) 0.035(2) 0.060(3) 0.015(2) -0.012(3) -0.011(2) C65 0.067(3) 0.033(2) 0.086(4) 0.009(2) 0.000(3) 0.003(2) C66 0.051(2) 0.036(2) 0.048(2) 0.0018(18) 0.0080(19) -0.0004(18) C67 0.0359(19) 0.0276(18) 0.038(2) -0.0041(15) 0.0079(16) -0.0084(15) C68 0.040(2) 0.061(3) 0.043(2) -0.012(2) 0.0158(18) -0.016(2) C69 0.043(2) 0.066(3) 0.064(3) -0.015(2) 0.027(2) -0.016(2) C70 0.035(2) 0.055(3) 0.065(3) -0.005(2) 0.007(2) -0.0105(19) C71 0.040(2) 0.050(2) 0.045(2) 0.0041(19) -0.0005(18) -0.0090(19) C72 0.038(2) 0.036(2) 0.035(2) -0.0017(16) 0.0094(16) -0.0081(16) C101 0.118(10) 0.082(8) 0.102(9) 0.019(7) 0.049(8) -0.018(8) C102 0.224(14) 0.107(10) 0.139(12) 0.020(9) 0.063(11) -0.017(11) C103 0.260(16) 0.111(10) 0.091(10) 0.033(8) 0.065(11) -0.006(12) C104 0.246(16) 0.119(11) 0.162(13) 0.027(10) 0.090(13) 0.018(13) C105 0.229(15) 0.162(13) 0.165(14) 0.006(11) 0.067(13) 0.018(14) C106 0.156(13) 0.151(13) 0.103(10) -0.001(9) 0.100(10) -0.006(11) C110 0.193(12) 0.212(13) 0.134(11) 0.037(10) 0.072(10) 0.069(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5753(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . P1 . 2.2659(10) yes Ru1 . P2 . 2.2543(10) yes Ru1 . O1 . 2.053(2) yes Ru1 . O2 . 2.088(2) yes Ru1 . O3 . 2.068(2) yes Ru1 . O4 . 2.092(2) yes Ru2 . P3 . 2.2690(10) yes Ru2 . P4 . 2.2605(10) yes Ru2 . O5 . 2.066(3) yes Ru2 . O6 . 2.088(2) yes Ru2 . O7 . 2.056(3) yes Ru2 . O8 . 2.096(2) yes Cl1 . C110 . 1.625(14) yes Cl2 . C110 . 1.740(15) yes P1 . C11 . 1.782(4) yes P1 . C13 . 1.838(4) yes P1 . C19 . 1.843(4) yes P2 . C25 . 1.776(4) yes P2 . C27 . 1.826(4) yes P2 . C33 . 1.834(3) yes P3 . C12 . 1.788(4) yes P3 . C49 . 1.840(4) yes P3 . C55 . 1.843(4) yes P4 . C26 . 1.781(4) yes P4 . C61 . 1.842(4) yes P4 . C67 . 1.828(4) yes O1 . C2 . 1.274(4) yes O2 . C4 . 1.274(5) yes O3 . C7 . 1.270(5) yes O4 . C9 . 1.264(5) yes O5 . C40 . 1.276(5) yes O6 . C42 . 1.265(5) yes O7 . C45 . 1.260(5) yes O8 . C47 . 1.261(5) yes C1 . C2 . 1.499(5) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C1 . H13 . 1.000 no C2 . C3 . 1.401(6) yes C3 . C4 . 1.383(6) yes C3 . H31 . 1.000 no C4 . C5 . 1.510(6) yes C5 . H51 . 1.000 no C5 . H52 . 1.000 no C5 . H53 . 1.000 no C6 . C7 . 1.513(6) yes C6 . H61 . 1.000 no C6 . H62 . 1.000 no C6 . H63 . 1.000 no C7 . C8 . 1.389(6) yes C8 . C9 . 1.397(6) yes C8 . H81 . 1.000 no C9 . C10 . 1.498(6) yes C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.199(5) yes C13 . C14 . 1.394(6) yes C13 . C18 . 1.383(6) yes C14 . C15 . 1.373(6) yes C14 . H141 . 1.000 no C15 . C16 . 1.368(8) yes C15 . H151 . 1.000 no C16 . C17 . 1.381(8) yes C16 . H161 . 1.000 no C17 . C18 . 1.389(6) yes C17 . H171 . 1.000 no C18 . H181 . 1.000 no C19 . C20 . 1.394(5) yes C19 . C24 . 1.386(6) yes C20 . C21 . 1.384(6) yes C20 . H201 . 1.000 no C21 . C22 . 1.362(7) yes C21 . H211 . 1.000 no C22 . C23 . 1.394(7) yes C22 . H221 . 1.000 no C23 . C24 . 1.362(6) yes C23 . H231 . 1.000 no C24 . H241 . 1.000 no C25 . C26 . 1.195(5) yes C27 . C28 . 1.392(5) yes C27 . C32 . 1.396(6) yes C28 . C29 . 1.387(6) yes C28 . H281 . 1.000 no C29 . C30 . 1.385(7) yes C29 . H291 . 1.000 no C30 . C31 . 1.374(7) yes C30 . H301 . 1.000 no C31 . C32 . 1.380(6) yes C31 . H311 . 1.000 no C32 . H321 . 1.000 no C33 . C34 . 1.390(5) yes C33 . C38 . 1.385(5) yes C34 . C35 . 1.368(6) yes C34 . H341 . 1.000 no C35 . C36 . 1.391(7) yes C35 . H351 . 1.000 no C36 . C37 . 1.369(7) yes C36 . H361 . 1.000 no C37 . C38 . 1.399(6) yes C37 . H371 . 1.000 no C38 . H381 . 1.000 no C39 . C40 . 1.497(7) yes C39 . H391 . 1.000 no C39 . H392 . 1.000 no C39 . H393 . 1.000 no C40 . C41 . 1.389(6) yes C41 . C42 . 1.387(7) yes C41 . H411 . 1.000 no C42 . C43 . 1.508(6) yes C43 . H431 . 1.000 no C43 . H432 . 1.000 no C43 . H433 . 1.000 no C44 . C45 . 1.509(7) yes C44 . H441 . 1.000 no C44 . H442 . 1.000 no C44 . H443 . 1.000 no C45 . C46 . 1.400(6) yes C46 . C47 . 1.399(6) yes C46 . H461 . 1.000 no C47 . C48 . 1.502(6) yes C48 . H481 . 1.000 no C48 . H482 . 1.000 no C48 . H483 . 1.000 no C49 . C50 . 1.386(5) yes C49 . C54 . 1.395(5) yes C50 . C51 . 1.399(6) yes C50 . H501 . 1.000 no C51 . C52 . 1.382(6) yes C51 . H511 . 1.000 no C52 . C53 . 1.372(7) yes C52 . H521 . 1.000 no C53 . C54 . 1.389(6) yes C53 . H531 . 1.000 no C54 . H541 . 1.000 no C55 . C56 . 1.397(5) yes C55 . C60 . 1.393(5) yes C56 . C57 . 1.377(6) yes C56 . H561 . 1.000 no C57 . C58 . 1.371(7) yes C57 . H571 . 1.000 no C58 . C59 . 1.391(7) yes C58 . H581 . 1.000 no C59 . C60 . 1.366(6) yes C59 . H591 . 1.000 no C60 . H601 . 1.000 no C61 . C62 . 1.401(6) yes C61 . C66 . 1.374(6) yes C62 . C63 . 1.381(7) yes C62 . H621 . 1.000 no C63 . C64 . 1.375(8) yes C63 . H631 . 1.000 no C64 . C65 . 1.376(8) yes C64 . H641 . 1.000 no C65 . C66 . 1.387(6) yes C65 . H651 . 1.000 no C66 . H661 . 1.000 no C67 . C68 . 1.401(5) yes C67 . C72 . 1.396(5) yes C68 . C69 . 1.379(6) yes C68 . H681 . 1.000 no C69 . C70 . 1.383(7) yes C69 . H691 . 1.000 no C70 . C71 . 1.358(6) yes C70 . H701 . 1.000 no C71 . C72 . 1.387(6) yes C71 . H711 . 1.000 no C72 . H721 . 1.000 no C101 . C102 . 1.512(16) yes C101 . H1011 . 1.000 no C101 . H1012 . 1.000 no C101 . H1013 . 1.000 no C102 . C103 . 1.513(16) yes C102 . H1021 . 1.000 no C102 . H1022 . 1.000 no C103 . C104 . 1.495(17) yes C103 . H1031 . 1.000 no C103 . H1032 . 1.000 no C104 . C105 . 1.545(17) yes C104 . H1041 . 1.000 no C104 . H1042 . 1.000 no C105 . C106 . 1.552(16) yes C105 . H1051 . 1.000 no C105 . H1052 . 1.000 no C106 . H1061 . 1.000 no C106 . H1062 . 1.000 no C106 . H1063 . 1.000 no C110 . H1101 . 1.000 no C110 . H1102 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 . Ru1 . P2 . 92.03(4) yes P1 . Ru1 . O1 . 91.90(7) yes P2 . Ru1 . O1 . 88.88(7) yes P1 . Ru1 . O2 . 174.14(7) yes P2 . Ru1 . O2 . 92.50(8) yes O1 . Ru1 . O2 . 91.90(10) yes P1 . Ru1 . O3 . 91.15(7) yes P2 . Ru1 . O3 . 95.47(8) yes O1 . Ru1 . O3 . 174.60(9) yes O2 . Ru1 . O3 . 84.72(10) yes P1 . Ru1 . O4 . 96.11(7) yes P2 . Ru1 . O4 . 170.09(7) yes O1 . Ru1 . O4 . 85.23(10) yes O2 . Ru1 . O4 . 79.76(10) yes O3 . Ru1 . O4 . 90.01(10) yes P3 . Ru2 . P4 . 94.43(4) yes P3 . Ru2 . O5 . 91.62(8) yes P4 . Ru2 . O5 . 92.05(8) yes P3 . Ru2 . O6 . 172.40(7) yes P4 . Ru2 . O6 . 92.52(7) yes O5 . Ru2 . O6 . 91.22(11) yes P3 . Ru2 . O7 . 90.73(8) yes P4 . Ru2 . O7 . 91.15(8) yes O5 . Ru2 . O7 . 175.87(10) yes O6 . Ru2 . O7 . 86.03(11) yes P3 . Ru2 . O8 . 92.01(7) yes P4 . Ru2 . O8 . 173.48(7) yes O5 . Ru2 . O8 . 86.69(10) yes O6 . Ru2 . O8 . 81.12(10) yes O7 . Ru2 . O8 . 89.84(11) yes Ru1 . P1 . C11 . 119.70(11) yes Ru1 . P1 . C13 . 114.92(12) yes C11 . P1 . C13 . 99.76(16) yes Ru1 . P1 . C19 . 118.71(12) yes C11 . P1 . C19 . 98.59(16) yes C13 . P1 . C19 . 101.78(16) yes Ru1 . P2 . C25 . 112.38(12) yes Ru1 . P2 . C27 . 120.67(12) yes C25 . P2 . C27 . 102.55(16) yes Ru1 . P2 . C33 . 114.75(12) yes C25 . P2 . C33 . 102.09(16) yes C27 . P2 . C33 . 102.10(15) yes Ru2 . P3 . C12 . 121.90(11) yes Ru2 . P3 . C49 . 117.10(12) yes C12 . P3 . C49 . 98.52(16) yes Ru2 . P3 . C55 . 114.58(12) yes C12 . P3 . C55 . 98.18(16) yes C49 . P3 . C55 . 103.19(17) yes Ru2 . P4 . C26 . 113.92(12) yes Ru2 . P4 . C61 . 116.65(12) yes C26 . P4 . C61 . 101.45(17) yes Ru2 . P4 . C67 . 116.61(12) yes C26 . P4 . C67 . 102.86(17) yes C61 . P4 . C67 . 103.28(17) yes Ru1 . O1 . C2 . 123.8(2) yes Ru1 . O2 . C4 . 123.0(2) yes Ru1 . O3 . C7 . 124.6(2) yes Ru1 . O4 . C9 . 125.0(3) yes Ru2 . O5 . C40 . 124.1(2) yes Ru2 . O6 . C42 . 123.7(3) yes Ru2 . O7 . C45 . 125.9(3) yes Ru2 . O8 . C47 . 124.7(3) yes C2 . C1 . H11 . 109.5 no C2 . C1 . H12 . 109.5 no H11 . C1 . H12 . 109.5 no C2 . C1 . H13 . 109.5 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no C1 . C2 . O1 . 114.7(3) yes C1 . C2 . C3 . 119.5(3) yes O1 . C2 . C3 . 125.8(3) yes C2 . C3 . C4 . 129.0(4) yes C2 . C3 . H31 . 115.5 no C4 . C3 . H31 . 115.5 no C3 . C4 . O2 . 126.1(3) yes C3 . C4 . C5 . 119.7(4) yes O2 . C4 . C5 . 114.2(4) yes C4 . C5 . H51 . 109.5 no C4 . C5 . H52 . 109.5 no H51 . C5 . H52 . 109.5 no C4 . C5 . H53 . 109.5 no H51 . C5 . H53 . 109.5 no H52 . C5 . H53 . 109.5 no C7 . C6 . H61 . 109.5 no C7 . C6 . H62 . 109.5 no H61 . C6 . H62 . 109.5 no C7 . C6 . H63 . 109.5 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no C6 . C7 . O3 . 113.9(4) yes C6 . C7 . C8 . 119.1(4) yes O3 . C7 . C8 . 126.9(4) yes C7 . C8 . C9 . 127.3(4) yes C7 . C8 . H81 . 116.3 no C9 . C8 . H81 . 116.3 no C8 . C9 . O4 . 125.8(4) yes C8 . C9 . C10 . 119.4(4) yes O4 . C9 . C10 . 114.7(4) yes C9 . C10 . H101 . 109.5 no C9 . C10 . H102 . 109.5 no H101 . C10 . H102 . 109.5 no C9 . C10 . H103 . 109.5 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no P1 . C11 . C12 . 178.2(3) yes P3 . C12 . C11 . 177.6(3) yes P1 . C13 . C14 . 118.1(3) yes P1 . C13 . C18 . 121.8(3) yes C14 . C13 . C18 . 119.8(4) yes C13 . C14 . C15 . 120.1(4) yes C13 . C14 . H141 . 120.0 no C15 . C14 . H141 . 120.0 no C14 . C15 . C16 . 120.5(5) yes C14 . C15 . H151 . 119.7 no C16 . C15 . H151 . 119.7 no C15 . C16 . C17 . 119.8(4) yes C15 . C16 . H161 . 120.1 no C17 . C16 . H161 . 120.1 no C16 . C17 . C18 . 120.6(5) yes C16 . C17 . H171 . 119.7 no C18 . C17 . H171 . 119.7 no C17 . C18 . C13 . 119.2(4) yes C17 . C18 . H181 . 120.4 no C13 . C18 . H181 . 120.4 no P1 . C19 . C20 . 120.3(3) yes P1 . C19 . C24 . 120.4(3) yes C20 . C19 . C24 . 119.2(3) yes C19 . C20 . C21 . 119.7(4) yes C19 . C20 . H201 . 120.2 no C21 . C20 . H201 . 120.2 no C20 . C21 . C22 . 120.4(4) yes C20 . C21 . H211 . 119.8 no C22 . C21 . H211 . 119.8 no C21 . C22 . C23 . 120.1(4) yes C21 . C22 . H221 . 119.9 no C23 . C22 . H221 . 119.9 no C22 . C23 . C24 . 119.9(4) yes C22 . C23 . H231 . 120.1 no C24 . C23 . H231 . 120.1 no C19 . C24 . C23 . 120.6(4) yes C19 . C24 . H241 . 119.7 no C23 . C24 . H241 . 119.7 no P2 . C25 . C26 . 170.3(3) yes P4 . C26 . C25 . 170.1(3) yes P2 . C27 . C28 . 117.9(3) yes P2 . C27 . C32 . 123.3(3) yes C28 . C27 . C32 . 118.8(3) yes C27 . C28 . C29 . 120.4(4) yes C27 . C28 . H281 . 119.8 no C29 . C28 . H281 . 119.8 no C28 . C29 . C30 . 119.9(4) yes C28 . C29 . H291 . 120.0 no C30 . C29 . H291 . 120.0 no C29 . C30 . C31 . 120.0(4) yes C29 . C30 . H301 . 120.0 no C31 . C30 . H301 . 120.0 no C30 . C31 . C32 . 120.5(4) yes C30 . C31 . H311 . 119.7 no C32 . C31 . H311 . 119.7 no C27 . C32 . C31 . 120.3(4) yes C27 . C32 . H321 . 119.8 no C31 . C32 . H321 . 119.8 no P2 . C33 . C34 . 117.6(3) yes P2 . C33 . C38 . 122.8(3) yes C34 . C33 . C38 . 119.6(3) yes C33 . C34 . C35 . 120.7(4) yes C33 . C34 . H341 . 119.7 no C35 . C34 . H341 . 119.7 no C34 . C35 . C36 . 120.1(4) yes C34 . C35 . H351 . 120.0 no C36 . C35 . H351 . 119.9 no C35 . C36 . C37 . 119.6(4) yes C35 . C36 . H361 . 120.2 no C37 . C36 . H361 . 120.2 no C36 . C37 . C38 . 120.8(4) yes C36 . C37 . H371 . 119.6 no C38 . C37 . H371 . 119.6 no C37 . C38 . C33 . 119.2(4) yes C37 . C38 . H381 . 120.4 no C33 . C38 . H381 . 120.4 no C40 . C39 . H391 . 109.5 no C40 . C39 . H392 . 109.5 no H391 . C39 . H392 . 109.5 no C40 . C39 . H393 . 109.5 no H391 . C39 . H393 . 109.5 no H392 . C39 . H393 . 109.5 no C39 . C40 . O5 . 114.1(4) yes C39 . C40 . C41 . 120.1(4) yes O5 . C40 . C41 . 125.8(4) yes C40 . C41 . C42 . 129.1(4) yes C40 . C41 . H411 . 115.5 no C42 . C41 . H411 . 115.5 no C41 . C42 . O6 . 126.1(4) yes C41 . C42 . C43 . 118.9(4) yes O6 . C42 . C43 . 115.1(4) yes C42 . C43 . H431 . 109.5 no C42 . C43 . H432 . 109.5 no H431 . C43 . H432 . 109.5 no C42 . C43 . H433 . 109.5 no H431 . C43 . H433 . 109.5 no H432 . C43 . H433 . 109.5 no C45 . C44 . H441 . 109.5 no C45 . C44 . H442 . 109.5 no H441 . C44 . H442 . 109.5 no C45 . C44 . H443 . 109.5 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no C44 . C45 . O7 . 114.4(4) yes C44 . C45 . C46 . 119.5(4) yes O7 . C45 . C46 . 126.1(4) yes C45 . C46 . C47 . 127.1(4) yes C45 . C46 . H461 . 116.5 no C47 . C46 . H461 . 116.5 no C46 . C47 . O8 . 126.1(4) yes C46 . C47 . C48 . 118.0(4) yes O8 . C47 . C48 . 115.9(4) yes C47 . C48 . H481 . 109.5 no C47 . C48 . H482 . 109.5 no H481 . C48 . H482 . 109.5 no C47 . C48 . H483 . 109.5 no H481 . C48 . H483 . 109.5 no H482 . C48 . H483 . 109.5 no P3 . C49 . C50 . 120.5(3) yes P3 . C49 . C54 . 119.8(3) yes C50 . C49 . C54 . 119.7(3) yes C49 . C50 . C51 . 119.4(4) yes C49 . C50 . H501 . 120.3 no C51 . C50 . H501 . 120.3 no C50 . C51 . C52 . 120.7(4) yes C50 . C51 . H511 . 119.6 no C52 . C51 . H511 . 119.6 no C51 . C52 . C53 . 119.4(4) yes C51 . C52 . H521 . 120.3 no C53 . C52 . H521 . 120.3 no C52 . C53 . C54 . 120.9(4) yes C52 . C53 . H531 . 119.6 no C54 . C53 . H531 . 119.6 no C49 . C54 . C53 . 119.8(4) yes C49 . C54 . H541 . 120.1 no C53 . C54 . H541 . 120.1 no P3 . C55 . C56 . 120.6(3) yes P3 . C55 . C60 . 120.5(3) yes C56 . C55 . C60 . 118.8(4) yes C55 . C56 . C57 . 120.2(4) yes C55 . C56 . H561 . 119.9 no C57 . C56 . H561 . 119.9 no C56 . C57 . C58 . 120.4(4) yes C56 . C57 . H571 . 119.8 no C58 . C57 . H571 . 119.8 no C57 . C58 . C59 . 119.9(4) yes C57 . C58 . H581 . 120.1 no C59 . C58 . H581 . 120.0 no C58 . C59 . C60 . 120.2(4) yes C58 . C59 . H591 . 119.9 no C60 . C59 . H591 . 119.9 no C55 . C60 . C59 . 120.6(4) yes C55 . C60 . H601 . 119.7 no C59 . C60 . H601 . 119.7 no P4 . C61 . C62 . 118.0(3) yes P4 . C61 . C66 . 122.9(3) yes C62 . C61 . C66 . 119.1(4) yes C61 . C62 . C63 . 120.2(5) yes C61 . C62 . H621 . 119.9 no C63 . C62 . H621 . 119.9 no C62 . C63 . C64 . 120.3(5) yes C62 . C63 . H631 . 119.9 no C64 . C63 . H631 . 119.9 no C63 . C64 . C65 . 119.7(4) yes C63 . C64 . H641 . 120.2 no C65 . C64 . H641 . 120.2 no C64 . C65 . C66 . 120.6(5) yes C64 . C65 . H651 . 119.7 no C66 . C65 . H651 . 119.7 no C65 . C66 . C61 . 120.2(4) yes C65 . C66 . H661 . 119.9 no C61 . C66 . H661 . 119.9 no P4 . C67 . C68 . 118.3(3) yes P4 . C67 . C72 . 122.8(3) yes C68 . C67 . C72 . 118.6(3) yes C67 . C68 . C69 . 119.9(4) yes C67 . C68 . H681 . 120.1 no C69 . C68 . H681 . 120.1 no C68 . C69 . C70 . 121.2(4) yes C68 . C69 . H691 . 119.4 no C70 . C69 . H691 . 119.4 no C69 . C70 . C71 . 118.8(4) yes C69 . C70 . H701 . 120.6 no C71 . C70 . H701 . 120.6 no C70 . C71 . C72 . 121.9(4) yes C70 . C71 . H711 . 119.1 no C72 . C71 . H711 . 119.1 no C67 . C72 . C71 . 119.6(4) yes C67 . C72 . H721 . 120.2 no C71 . C72 . H721 . 120.2 no C102 . C101 . H1011 . 109.5 no C102 . C101 . H1012 . 109.5 no H1011 . C101 . H1012 . 109.5 no C102 . C101 . H1013 . 109.4 no H1011 . C101 . H1013 . 109.5 no H1012 . C101 . H1013 . 109.5 no C101 . C102 . C103 . 112.1(13) yes C101 . C102 . H1021 . 108.7 no C103 . C102 . H1021 . 108.8 no C101 . C102 . H1022 . 108.8 no C103 . C102 . H1022 . 108.8 no H1021 . C102 . H1022 . 109.5 no C102 . C103 . C104 . 105.5(12) yes C102 . C103 . H1031 . 110.4 no C104 . C103 . H1031 . 110.4 no C102 . C103 . H1032 . 110.5 no C104 . C103 . H1032 . 110.5 no H1031 . C103 . H1032 . 109.5 no C103 . C104 . C105 . 107.8(12) yes C103 . C104 . H1041 . 110.0 no C105 . C104 . H1041 . 109.8 no C103 . C104 . H1042 . 109.9 no C105 . C104 . H1042 . 109.9 no H1041 . C104 . H1042 . 109.5 no C104 . C105 . C106 . 121.4(14) yes C104 . C105 . H1051 . 106.4 no C106 . C105 . H1051 . 106.4 no C104 . C105 . H1052 . 106.4 no C106 . C105 . H1052 . 106.4 no H1051 . C105 . H1052 . 109.5 no C105 . C106 . H1061 . 109.5 no C105 . C106 . H1062 . 109.5 no H1061 . C106 . H1062 . 109.5 no C105 . C106 . H1063 . 109.4 no H1061 . C106 . H1063 . 109.5 no H1062 . C106 . H1063 . 109.5 no Cl2 . C110 . Cl1 . 113.8(9) yes Cl2 . C110 . H1101 . 108.6 no Cl1 . C110 . H1101 . 108.6 no Cl2 . C110 . H1102 . 108.2 no Cl1 . C110 . H1102 . 108.2 no H1101 . C110 . H1102 . 109.5 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl1 C106 3.22(2) . . no Cl1 C64 3.421(8) . 2_566 no Cl2 C106 3.16(2) . . no Cl2 C105 3.52(2) . . no Cl2 C44 3.534(8) . . no Cl2 C46 3.596(9) . . no C1 C10 3.501(6) . 2_667 no C1 C52 3.574(7) . 3_556 no C5 C6 3.589(7) . 2_567 no C17 C63 3.552(7) . 3_546 no C43 C43 3.49(1) . 2_566 no C46 C110 3.31(2) . . no C54 C65 3.557(7) . 3_546 no C106 C110 2.99(3) . . no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru1 P1 C13 C14 . . . . -80.7(3) no Ru1 P1 C13 C18 . . . . 93.0(3) no Ru1 P1 C19 C20 . . . . 5.1(4) no Ru1 P1 C19 C24 . . . . -174.9(3) no Ru1 P2 C27 C28 . . . . 43.1(3) no Ru1 P2 C27 C32 . . . . -136.6(3) no Ru1 P2 C33 C34 . . . . -55.2(3) no Ru1 P2 C33 C38 . . . . 122.7(3) no Ru1 O1 C2 C1 . . . . -173.2(2) no Ru1 O1 C2 C3 . . . . 5.4(5) no Ru1 O2 C4 C3 . . . . -0.2(5) no Ru1 O2 C4 C5 . . . . 179.4(2) no Ru1 O3 C7 C6 . . . . -174.0(3) no Ru1 O3 C7 C8 . . . . 5.0(6) no Ru1 O4 C9 C8 . . . . 3.6(6) no Ru1 O4 C9 C10 . . . . -176.4(3) no Ru2 P3 C49 C50 . . . . 0.2(4) no Ru2 P3 C49 C54 . . . . -179.1(3) no Ru2 P3 C55 C56 . . . . -89.1(3) no Ru2 P3 C55 C60 . . . . 86.7(3) no Ru2 P4 C61 C62 . . . . -53.5(3) no Ru2 P4 C61 C66 . . . . 126.0(3) no Ru2 P4 C67 C68 . . . . 58.7(3) no Ru2 P4 C67 C72 . . . . -116.0(3) no Ru2 O5 C40 C39 . . . . 178.9(3) no Ru2 O5 C40 C41 . . . . -0.8(6) no Ru2 O6 C42 C41 . . . . -2.5(5) no Ru2 O6 C42 C43 . . . . 178.8(3) no Ru2 O7 C45 C44 . . . . -175.3(3) no Ru2 O7 C45 C46 . . . . 3.6(6) no Ru2 O8 C47 C46 . . . . 3.6(6) no Ru2 O8 C47 C48 . . . . -177.9(3) no P1 Ru1 P2 C25 . . . . -66.5(1) no P1 Ru1 P2 C27 . . . . 54.7(2) no P1 Ru1 P2 C33 . . . . 177.5(1) no P1 Ru1 O1 C2 . . . . 177.3(2) no P1 Ru1 O3 C7 . . . . 91.1(3) no P1 Ru1 O4 C9 . . . . -90.2(3) no P1 C13 C14 C15 . . . . 174.5(4) no P1 C13 C18 C17 . . . . -173.7(3) no P1 C19 C20 C21 . . . . 178.1(3) no P1 C19 C24 C23 . . . . 180.0(4) no P2 Ru1 P1 C11 . . . . 22.0(1) no P2 Ru1 P1 C13 . . . . -96.8(1) no P2 Ru1 P1 C19 . . . . 142.5(1) no P2 Ru1 O1 C2 . . . . 85.3(2) no P2 Ru1 O2 C4 . . . . -84.3(2) no P2 Ru1 O3 C7 . . . . -176.8(3) no P2 C27 C28 C29 . . . . 179.2(3) no P2 C27 C32 C31 . . . . -179.4(3) no P2 C33 C34 C35 . . . . 176.9(3) no P2 C33 C38 C37 . . . . -177.3(3) no P3 Ru2 P4 C26 . . . . -57.4(1) no P3 Ru2 P4 C61 . . . . -175.2(1) no P3 Ru2 P4 C67 . . . . 62.2(1) no P3 Ru2 O5 C40 . . . . -174.7(3) no P3 Ru2 O7 C45 . . . . 88.7(3) no P3 Ru2 O8 C47 . . . . -90.8(3) no P3 C49 C50 C51 . . . . 179.9(3) no P3 C49 C54 C53 . . . . -179.9(4) no P3 C55 C56 C57 . . . . 176.8(4) no P3 C55 C60 C59 . . . . -176.9(4) no P4 Ru2 P3 C12 . . . . 18.3(2) no P4 Ru2 P3 C49 . . . . 139.3(1) no P4 Ru2 P3 C55 . . . . -99.7(1) no P4 Ru2 O5 C40 . . . . 90.8(3) no P4 Ru2 O6 C42 . . . . -88.8(3) no P4 Ru2 O7 C45 . . . . -176.9(3) no P4 C61 C62 C63 . . . . -179.9(3) no P4 C61 C66 C65 . . . . -180.0(3) no P4 C67 C68 C69 . . . . -174.1(3) no P4 C67 C72 C71 . . . . 173.6(3) no O1 Ru1 P1 C11 . . . . -67.0(2) no O1 Ru1 P1 C13 . . . . 174.3(1) no O1 Ru1 P1 C19 . . . . 53.6(1) no O1 Ru1 P2 C25 . . . . 25.4(1) no O1 Ru1 P2 C27 . . . . 146.5(2) no O1 Ru1 P2 C33 . . . . -90.7(2) no O1 Ru1 O2 C4 . . . . 4.7(2) no O1 Ru1 O4 C9 . . . . 178.4(3) no O1 C2 C3 C4 . . . . 1.6(6) no O2 Ru1 P2 C25 . . . . 117.2(1) no O2 Ru1 P2 C27 . . . . -121.6(2) no O2 Ru1 P2 C33 . . . . 1.2(2) no O2 Ru1 O1 C2 . . . . -7.1(2) no O2 Ru1 O3 C7 . . . . -84.7(3) no O2 Ru1 O4 C9 . . . . 85.6(3) no O2 C4 C3 C2 . . . . -4.6(7) no O3 Ru1 P1 C11 . . . . 117.5(2) no O3 Ru1 P1 C13 . . . . -1.3(1) no O3 Ru1 P1 C19 . . . . -122.0(1) no O3 Ru1 P2 C25 . . . . -157.8(1) no O3 Ru1 P2 C27 . . . . -36.7(2) no O3 Ru1 P2 C33 . . . . 86.1(2) no O3 Ru1 O2 C4 . . . . -179.5(2) no O3 Ru1 O4 C9 . . . . 1.0(3) no O3 C7 C8 C9 . . . . 0.9(8) no O4 Ru1 P1 C11 . . . . -152.4(2) no O4 Ru1 P1 C13 . . . . 88.9(1) no O4 Ru1 P1 C19 . . . . -31.8(2) no O4 Ru1 O1 C2 . . . . -86.7(2) no O4 Ru1 O2 C4 . . . . 89.5(2) no O4 Ru1 O3 C7 . . . . -5.0(3) no O4 C9 C8 C7 . . . . -5.7(7) no O5 Ru2 P3 C12 . . . . -73.9(2) no O5 Ru2 P3 C49 . . . . 47.1(2) no O5 Ru2 P3 C55 . . . . 168.2(1) no O5 Ru2 P4 C26 . . . . 34.4(1) no O5 Ru2 P4 C61 . . . . -83.4(2) no O5 Ru2 P4 C67 . . . . 154.0(2) no O5 Ru2 O6 C42 . . . . 3.3(3) no O5 Ru2 O8 C47 . . . . 177.6(3) no O5 C40 C41 C42 . . . . 3.2(7) no O6 Ru2 P4 C26 . . . . 125.7(1) no O6 Ru2 P4 C61 . . . . 7.9(2) no O6 Ru2 P4 C67 . . . . -114.7(2) no O6 Ru2 O5 C40 . . . . -1.7(3) no O6 Ru2 O7 C45 . . . . -84.4(3) no O6 Ru2 O8 C47 . . . . 85.9(3) no O6 C42 C41 C40 . . . . -1.2(7) no O7 Ru2 P3 C12 . . . . 109.5(2) no O7 Ru2 P3 C49 . . . . -129.5(2) no O7 Ru2 P3 C55 . . . . -8.5(1) no O7 Ru2 P4 C26 . . . . -148.2(1) no O7 Ru2 P4 C61 . . . . 94.0(2) no O7 Ru2 P4 C67 . . . . -28.6(2) no O7 Ru2 O6 C42 . . . . -179.7(3) no O7 Ru2 O8 C47 . . . . -0.1(3) no O7 C45 C46 C47 . . . . 0.5(8) no O8 Ru2 P3 C12 . . . . -160.6(2) no O8 Ru2 P3 C49 . . . . -39.6(2) no O8 Ru2 P3 C55 . . . . 81.4(1) no O8 Ru2 O5 C40 . . . . -82.8(3) no O8 Ru2 O6 C42 . . . . 89.8(3) no O8 Ru2 O7 C45 . . . . -3.3(3) no O8 C47 C46 C45 . . . . -4.6(7) no C1 C2 C3 C4 . . . . -179.8(4) no C2 C3 C4 C5 . . . . 175.8(4) no C6 C7 C8 C9 . . . . 179.8(4) no C7 C8 C9 C10 . . . . 174.3(4) no C11 P1 C13 C14 . . . . 149.9(3) no C11 P1 C13 C18 . . . . -36.4(4) no C11 P1 C19 C20 . . . . 136.0(3) no C11 P1 C19 C24 . . . . -44.0(4) no C12 P3 C49 C50 . . . . 132.8(3) no C12 P3 C49 C54 . . . . -46.5(4) no C12 P3 C55 C56 . . . . 140.1(3) no C12 P3 C55 C60 . . . . -44.1(4) no C13 P1 C19 C20 . . . . -122.1(3) no C13 P1 C19 C24 . . . . 57.9(4) no C13 C14 C15 C16 . . . . -1.2(8) no C13 C18 C17 C16 . . . . 0.0(7) no C14 C13 P1 C19 . . . . 48.9(4) no C14 C13 C18 C17 . . . . -0.0(6) no C14 C15 C16 C17 . . . . 1.3(9) no C15 C14 C13 C18 . . . . 0.6(7) no C15 C16 C17 C18 . . . . -0.6(8) no C18 C13 P1 C19 . . . . -137.3(3) no C19 C20 C21 C22 . . . . 1.5(7) no C19 C24 C23 C22 . . . . 2.3(8) no C20 C19 C24 C23 . . . . -0.1(7) no C20 C21 C22 C23 . . . . 0.7(7) no C21 C20 C19 C24 . . . . -1.8(6) no C21 C22 C23 C24 . . . . -2.6(8) no C25 P2 C27 C28 . . . . 169.0(3) no C25 P2 C27 C32 . . . . -10.8(3) no C25 P2 C33 C34 . . . . -177.1(3) no C25 P2 C33 C38 . . . . 0.9(3) no C26 P4 C61 C62 . . . . -177.9(3) no C26 P4 C61 C66 . . . . 1.6(4) no C26 P4 C67 C68 . . . . -175.9(3) no C26 P4 C67 C72 . . . . 9.4(3) no C27 P2 C33 C34 . . . . 77.1(3) no C27 P2 C33 C38 . . . . -104.9(3) no C27 C28 C29 C30 . . . . 0.6(6) no C27 C32 C31 C30 . . . . -0.3(6) no C28 C27 P2 C33 . . . . -85.6(3) no C28 C27 C32 C31 . . . . 0.9(6) no C28 C29 C30 C31 . . . . 0.0(6) no C29 C28 C27 C32 . . . . -1.1(5) no C29 C30 C31 C32 . . . . -0.2(7) no C32 C27 P2 C33 . . . . 94.7(3) no C33 C34 C35 C36 . . . . 1.1(6) no C33 C38 C37 C36 . . . . -0.1(6) no C34 C33 C38 C37 . . . . 0.6(5) no C34 C35 C36 C37 . . . . -0.5(6) no C35 C34 C33 C38 . . . . -1.1(5) no C35 C36 C37 C38 . . . . 0.0(7) no C39 C40 C41 C42 . . . . -176.5(5) no C40 C41 C42 C43 . . . . 177.4(4) no C44 C45 C46 C47 . . . . 179.4(4) no C45 C46 C47 C48 . . . . 176.9(4) no C49 P3 C55 C56 . . . . 39.3(4) no C49 P3 C55 C60 . . . . -144.9(3) no C49 C50 C51 C52 . . . . 0.5(7) no C49 C54 C53 C52 . . . . -0.5(7) no C50 C49 P3 C55 . . . . -126.7(3) no C50 C49 C54 C53 . . . . 0.8(6) no C50 C51 C52 C53 . . . . -0.2(7) no C51 C50 C49 C54 . . . . -0.8(6) no C51 C52 C53 C54 . . . . 0.2(8) no C54 C49 P3 C55 . . . . 54.1(4) no C55 C56 C57 C58 . . . . -0.1(7) no C55 C60 C59 C58 . . . . 0.2(7) no C56 C55 C60 C59 . . . . -1.0(6) no C56 C57 C58 C59 . . . . -0.7(8) no C57 C56 C55 C60 . . . . 1.0(6) no C57 C58 C59 C60 . . . . 0.6(8) no C61 P4 C67 C68 . . . . -70.6(3) no C61 P4 C67 C72 . . . . 114.7(3) no C61 C62 C63 C64 . . . . -0.4(7) no C61 C66 C65 C64 . . . . 0.2(7) no C62 C61 P4 C67 . . . . 75.8(3) no C62 C61 C66 C65 . . . . -0.5(6) no C62 C63 C64 C65 . . . . 0.1(8) no C63 C62 C61 C66 . . . . 0.6(6) no C63 C64 C65 C66 . . . . 0.0(8) no C66 C61 P4 C67 . . . . -104.7(3) no C67 C68 C69 C70 . . . . 0.6(7) no C67 C72 C71 C70 . . . . -0.0(6) no C68 C67 C72 C71 . . . . -1.1(6) no C68 C69 C70 C71 . . . . -1.7(7) no C69 C68 C67 C72 . . . . 0.8(6) no C69 C70 C71 C72 . . . . 1.4(7) no C101 C102 C103 C104 . . . . 172(2) no C102 C103 C104 C105 . . . . -179(2) no C103 C104 C105 C106 . . . . 173(2) no #------------------------------------------------------------------------------ # start Validation Reply Form _vrf_PLAT027_benmat17cu ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 59.95 Deg. RESPONSE: ... Data can only be collected to 2theta 120 deg on a AFC6R diffractometer when the evacuated beam tunnel in used. ; # end Validation Reply Form #===END