Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email ktanaka@ims.ac.jp _publ_contact_author_name 'Koji Tanaka' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Institute for Molecular Science 38 Nishigonaka Myodaiji Okazaki Aichi 444-8585 JAPAN ; _publ_contact_author_fax ' +81-564-55-5245 ' _publ_contact_author_phone ' +81-564-55-7241 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; Acid-base equilibria of various oxidation states of aqua-ruthenium complexes with 1,10-phenanthroline-5,6-dione in aqueous media ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; loop_ _publ_author_name _publ_author_address T.Fujihara ; Institute for Molecular Science 38 Nishigonaka Myodaiji Okazaki Aichi 444-8585 JAPAN ; T.Wada ; Institute for Molecular Science 38 Nishigonaka Myodaiji Okazaki Aichi 444-8585 JAPAN ; K.Tanaka ; Institute for Molecular Science 38 Nishigonaka Myodaiji Okazaki Aichi 444-8585 JAPAN ; #------------------------------------------------------------------------------ data_[Ru(trpy)(PDA)(OH2)]_1.5(ClO4)_0.5(PF6)_3.5(H2O) _database_code_depnum_ccdc_archive 'CCDC 220055' _audit_creation_date 'Wed Dec 24 13:50:20 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C30 H32 Cl1.50 F3 N5 O13.50 P0.50 Ru ' _chemical_formula_moiety ? _chemical_formula_weight 905.34 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 33.010(3) _cell_length_b 8.4218(7) _cell_length_c 26.360(2) _cell_angle_alpha 90 _cell_angle_beta 90.451(4) _cell_angle_gamma 90 _cell_volume 7327(1) _cell_formula_units_Z 8 _cell_measurement_reflns_used 7142 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.2 #------------------------------------------------------------------------------ _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 29185 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.2580 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.2580 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 34 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8930 _reflns_number_gt 4272 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.1842 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4272 _refine_ls_number_parameters 456 _refine_ls_goodness_of_fit_ref 1.751 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.03500(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0128 _refine_diff_density_max 1.84 _refine_diff_density_min -1.66 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.00000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru Ru -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru(1) Ru 0.13721(2) 0.16799(8) 0.35226(2) 0.0204(1) Uani 1.00 d . . . Cl(1) Cl 0.19525(8) 0.4068(3) 0.08049(8) 0.0424(6) Uani 1.00 d . . . Cl(2) Cl 0.5338(3) 0.070(1) 0.5634(3) 0.095(2) Uiso 0.50 d P . . P(1) P 1.0000 0.3330(9) 0.7500 0.097(2) Uiso 1.00 d S . . F(1) F 1.0041(8) 0.209(3) 0.7073(8) 0.35(1) Uiso 1.00 d . . . F(2) F 1.0020(4) 0.456(2) 0.7898(4) 0.162(4) Uiso 1.00 d . . . F(3) F 1.0451(4) 0.298(2) 0.7505(5) 0.181(5) Uiso 1.00 d . . . O(1) O 0.0849(2) 0.2599(7) 0.3904(2) 0.033(1) Uani 1.00 d . . . O(2) O 0.1418(2) 0.0512(7) 0.1116(2) 0.037(2) Uani 1.00 d . . . O(3) O 0.2116(2) -0.1060(7) 0.1423(2) 0.038(2) Uani 1.00 d . . . O(4) O 0.1488(2) -0.2962(7) 0.2231(2) 0.051(2) Uani 1.00 d . . . O(5) O 0.2275(3) 0.368(1) 0.0481(3) 0.113(4) Uani 1.00 d . . . O(6) O 0.2005(3) 0.5614(8) 0.0991(3) 0.075(2) Uani 1.00 d . . . O(7) O 0.1948(2) 0.2989(8) 0.1231(2) 0.067(2) Uani 1.00 d . . . O(8) O 0.1590(2) 0.393(1) 0.0533(3) 0.086(3) Uani 1.00 d . . . O(9) O 0.5390(8) 0.173(3) 0.6107(9) 0.148(9) Uiso 0.50 d P . . O(10) O 0.5641(10) -0.059(4) 0.559(1) 0.19(1) Uiso 0.50 d P . . O(11) O 0.5319(7) 0.217(3) 0.5262(8) 0.117(7) Uiso 0.50 d P . . O(12) O 0.4977(7) 0.009(3) 0.5702(7) 0.114(7) Uiso 0.50 d P . . O(16) O 0.9838(3) 0.116(1) 0.1223(4) 0.104(3) Uiso 1.00 d . . . O(17) O 0.9058(3) 0.285(1) 0.0079(3) 0.090(3) Uiso 1.00 d . . . O(18) O 0.0792(3) 0.006(1) 0.0417(3) 0.098(3) Uiso 1.00 d . . . O(19) O 0.0157(8) 0.191(3) 0.6141(10) 0.157(9) Uiso 0.50 d P . . N(1) N 0.1648(2) 0.3893(7) 0.3580(2) 0.022(1) Uani 1.00 d . . . N(2) N 0.1637(2) 0.1495(8) 0.4188(2) 0.026(2) Uani 1.00 d . . . N(3) N 0.1182(2) -0.0590(7) 0.3730(2) 0.024(1) Uani 1.00 d . . . N(4) N 0.1834(2) 0.0879(7) 0.3084(2) 0.018(1) Uani 1.00 d . . . N(5) N 0.1097(2) 0.1645(8) 0.2815(2) 0.022(1) Uani 1.00 d . . . C(1) C 0.1650(2) 0.5083(10) 0.3242(3) 0.027(2) Uani 1.00 d . . . C(2) C 0.1855(2) 0.6469(9) 0.3320(3) 0.029(2) Uani 1.00 d . . . C(3) C 0.2073(2) 0.669(1) 0.3757(3) 0.033(2) Uani 1.00 d . . . C(4) C 0.2077(3) 0.5480(9) 0.4112(3) 0.030(2) Uani 1.00 d . . . C(5) C 0.1861(2) 0.4117(9) 0.4012(3) 0.023(2) Uani 1.00 d . . . C(6) C 0.1842(3) 0.2740(9) 0.4369(3) 0.027(2) Uani 1.00 d . . . C(7) C 0.2008(3) 0.266(1) 0.4856(3) 0.036(2) Uani 1.00 d . . . C(8) C 0.1954(3) 0.128(1) 0.5139(3) 0.037(2) Uani 1.00 d . . . C(9) C 0.1734(3) 0.002(1) 0.4938(3) 0.035(2) Uani 1.00 d . . . C(10) C 0.1580(2) 0.0153(10) 0.4456(3) 0.027(2) Uani 1.00 d . . . C(11) C 0.1317(2) -0.1012(9) 0.4200(3) 0.023(2) Uani 1.00 d . . . C(12) C 0.1197(3) -0.244(1) 0.4421(3) 0.033(2) Uani 1.00 d . . . C(13) C 0.0948(3) -0.344(1) 0.4157(3) 0.037(2) Uani 1.00 d . . . C(14) C 0.0816(3) -0.301(1) 0.3684(3) 0.037(2) Uani 1.00 d . . . C(15) C 0.0933(2) -0.159(1) 0.3487(3) 0.032(2) Uani 1.00 d . . . C(16) C 0.2224(2) 0.0669(9) 0.3221(3) 0.021(2) Uani 1.00 d . . . C(17) C 0.2515(2) 0.006(1) 0.2890(3) 0.027(2) Uani 1.00 d . . . C(18) C 0.2402(2) -0.0385(9) 0.2409(3) 0.027(2) Uani 1.00 d . . . C(19) C 0.2005(2) -0.0141(9) 0.2252(3) 0.022(2) Uani 1.00 d . . . C(20) C 0.1732(2) 0.0510(9) 0.2600(2) 0.020(2) Uani 1.00 d . . . C(21) C 0.1319(2) 0.0888(9) 0.2450(2) 0.020(2) Uani 1.00 d . . . C(22) C 0.1168(2) 0.0512(10) 0.1974(3) 0.027(2) Uani 1.00 d . . . C(23) C 0.0778(3) 0.097(1) 0.1865(3) 0.035(2) Uani 1.00 d . . . C(24) C 0.0549(2) 0.176(1) 0.2224(3) 0.041(2) Uani 1.00 d . . . C(25) C 0.0720(3) 0.210(1) 0.2689(3) 0.034(2) Uani 1.00 d . . . C(26) C 0.1875(3) -0.0576(9) 0.1736(3) 0.027(2) Uani 1.00 d . . . C(27) C 0.1426(3) -0.037(1) 0.1586(3) 0.030(2) Uani 1.00 d . . . C(28) C 0.1251(3) -0.197(1) 0.1452(3) 0.037(2) Uani 1.00 d . . . C(29) C 0.1293(3) -0.327(1) 0.1854(3) 0.039(2) Uani 1.00 d . . . C(30) C 0.1083(4) -0.482(1) 0.1772(4) 0.062(3) Uani 1.00 d . . . H(1) H 0.1496 0.4946 0.2936 0.0360 Uiso 1.00 calc . . . H(2) H 0.1839 0.7309 0.3070 0.0331 Uiso 1.00 calc . . . H(3) H 0.2222 0.7671 0.3813 0.0375 Uiso 1.00 calc . . . H(4) H 0.2228 0.5590 0.4422 0.0372 Uiso 1.00 calc . . . H(5) H 0.2156 0.3566 0.4990 0.0400 Uiso 1.00 calc . . . H(6) H 0.2070 0.1218 0.5478 0.0450 Uiso 1.00 calc . . . H(7) H 0.1687 -0.0936 0.5134 0.0429 Uiso 1.00 calc . . . H(8) H 0.1297 -0.2715 0.4752 0.0359 Uiso 1.00 calc . . . H(9) H 0.0859 -0.4422 0.4314 0.0465 Uiso 1.00 calc . . . H(10) H 0.0643 -0.3714 0.3494 0.0426 Uiso 1.00 calc . . . H(11) H 0.0834 -0.1242 0.3155 0.0381 Uiso 1.00 calc . . . H(12) H 0.2302 0.0924 0.3564 0.0261 Uiso 1.00 calc . . . H(13) H 0.2797 -0.0041 0.2996 0.0318 Uiso 1.00 calc . . . H(14) H 0.2596 -0.0856 0.2179 0.0321 Uiso 1.00 calc . . . H(15) H 0.0674 0.0743 0.1538 0.0407 Uiso 1.00 calc . . . H(16) H 0.0276 0.2119 0.2150 0.0474 Uiso 1.00 calc . . . H(17) H 0.0563 0.2685 0.2936 0.0381 Uiso 1.00 calc . . . H(18) H 0.0972 -0.1843 0.1375 0.0436 Uiso 1.00 calc . . . H(19) H 0.1388 -0.2348 0.1148 0.0436 Uiso 1.00 calc . . . H(20) H 0.0889 -0.5028 0.2042 0.0815 Uiso 1.00 calc . . . H(21) H 0.0942 -0.4841 0.1459 0.0815 Uiso 1.00 calc . . . H(22) H 0.1275 -0.5681 0.1773 0.0815 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.0232(3) 0.0204(3) 0.0175(3) 0.0015(4) 0.0016(2) -0.0012(3) Cl(1) 0.051(1) 0.038(1) 0.039(1) -0.003(1) -0.0065(10) -0.0019(10) O(1) 0.033(3) 0.033(3) 0.032(3) 0.016(3) 0.014(2) -0.003(3) O(2) 0.053(4) 0.043(4) 0.014(2) 0.000(3) -0.002(3) 0.000(2) O(3) 0.036(3) 0.049(4) 0.028(3) 0.002(3) 0.011(2) -0.012(3) O(4) 0.079(5) 0.040(4) 0.034(3) -0.018(4) -0.011(3) 0.007(3) O(5) 0.101(7) 0.16(1) 0.077(6) 0.080(7) 0.060(5) 0.030(6) O(6) 0.131(7) 0.036(3) 0.059(4) -0.001(5) -0.044(5) 0.001(3) O(7) 0.096(6) 0.060(5) 0.047(4) -0.033(5) -0.009(4) 0.021(3) O(8) 0.066(5) 0.132(8) 0.061(5) -0.022(6) -0.042(4) -0.002(5) N(1) 0.019(3) 0.020(2) 0.025(3) 0.007(2) 0.003(2) -0.006(2) N(2) 0.038(4) 0.026(3) 0.013(2) 0.001(3) 0.001(2) -0.005(2) N(3) 0.032(4) 0.017(2) 0.022(3) 0.000(3) 0.005(2) -0.003(2) N(4) 0.022(3) 0.012(3) 0.021(2) 0.001(3) 0.000(2) 0.003(2) N(5) 0.021(3) 0.025(3) 0.019(2) 0.000(3) 0.003(2) -0.001(3) C(1) 0.027(4) 0.025(4) 0.028(4) 0.003(3) 0.007(3) 0.000(3) C(2) 0.032(5) 0.019(4) 0.034(4) 0.006(3) 0.008(3) 0.010(4) C(3) 0.031(4) 0.027(4) 0.040(4) -0.002(5) 0.002(3) 0.005(3) C(4) 0.033(5) 0.024(4) 0.033(4) 0.003(3) 0.004(4) -0.009(3) C(5) 0.023(4) 0.024(3) 0.024(3) 0.008(3) 0.001(3) -0.005(3) C(6) 0.033(5) 0.021(3) 0.029(3) 0.002(3) 0.003(3) -0.004(3) C(7) 0.037(5) 0.040(4) 0.030(4) -0.010(5) -0.004(3) -0.005(3) C(8) 0.035(5) 0.051(5) 0.025(4) -0.007(4) -0.002(4) 0.005(3) C(9) 0.044(5) 0.040(5) 0.022(3) 0.001(4) 0.000(3) 0.007(4) C(10) 0.031(5) 0.028(4) 0.022(3) 0.001(3) 0.002(3) 0.002(3) C(11) 0.019(4) 0.023(3) 0.028(3) 0.008(3) 0.004(3) 0.004(3) C(12) 0.040(5) 0.027(4) 0.030(4) -0.001(4) 0.008(4) 0.011(3) C(13) 0.042(5) 0.018(4) 0.051(4) -0.007(4) 0.013(3) 0.006(4) C(14) 0.029(5) 0.033(5) 0.050(4) -0.012(4) 0.006(4) -0.003(4) C(15) 0.026(4) 0.030(4) 0.040(4) -0.006(4) -0.005(3) -0.005(4) C(16) 0.024(3) 0.018(4) 0.021(3) 0.001(3) -0.006(3) 0.005(3) C(17) 0.015(4) 0.032(4) 0.035(3) -0.003(4) -0.001(3) 0.003(3) C(18) 0.026(4) 0.024(4) 0.031(3) 0.007(4) 0.009(3) 0.000(3) C(19) 0.028(3) 0.022(4) 0.017(3) 0.002(3) 0.005(2) 0.005(3) C(20) 0.020(3) 0.020(4) 0.018(3) -0.006(3) 0.001(2) 0.005(3) C(21) 0.021(3) 0.021(4) 0.017(3) 0.001(3) 0.000(2) 0.004(3) C(22) 0.029(4) 0.036(5) 0.018(3) -0.004(4) 0.000(3) 0.000(3) C(23) 0.034(4) 0.043(5) 0.028(4) 0.005(4) -0.011(3) -0.001(4) C(24) 0.022(4) 0.062(6) 0.040(4) 0.006(5) -0.006(3) -0.010(5) C(25) 0.026(4) 0.042(6) 0.034(4) 0.010(4) 0.000(3) -0.001(4) C(26) 0.035(4) 0.027(4) 0.019(3) -0.004(4) 0.003(2) -0.002(3) C(27) 0.036(4) 0.036(4) 0.017(3) -0.005(4) 0.003(3) 0.003(3) C(28) 0.044(5) 0.042(4) 0.024(4) -0.009(4) -0.003(4) -0.016(3) C(29) 0.037(5) 0.038(4) 0.042(4) 0.000(5) 0.004(3) -0.003(4) C(30) 0.072(8) 0.056(6) 0.058(6) -0.046(6) -0.011(6) 0.003(6) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) O(1) 2.136(7) . . yes Ru(1) N(1) 2.081(8) . . yes Ru(1) N(2) 1.972(7) . . yes Ru(1) N(3) 2.083(8) . . yes Ru(1) N(4) 2.023(8) . . yes Ru(1) N(5) 2.081(7) . . yes Cl(1) O(5) 1.400(10) . . yes Cl(1) O(6) 1.403(9) . . yes Cl(1) O(7) 1.446(9) . . yes Cl(1) O(8) 1.403(9) . . yes Cl(2) O(9) 1.53(3) . . yes Cl(2) O(10) 1.48(4) . . yes Cl(2) O(11) 1.58(3) . . yes Cl(2) O(12) 1.31(3) . . yes P(1) F(1) 1.54(3) . . yes P(1) F(1) 1.54(3) . 2_756 yes P(1) F(2) 1.48(2) . . yes P(1) F(2) 1.48(2) . 2_756 yes P(1) F(3) 1.52(2) . . yes P(1) F(3) 1.52(2) . 2_756 yes O(2) C(27) 1.44(1) . . yes O(3) C(26) 1.21(1) . . yes O(4) C(29) 1.21(1) . . yes N(1) C(1) 1.34(1) . . yes N(1) C(5) 1.36(1) . . yes N(2) C(6) 1.34(1) . . yes N(2) C(10) 1.35(1) . . yes N(3) C(11) 1.37(1) . . yes N(3) C(15) 1.34(1) . . yes N(4) C(16) 1.35(1) . . yes N(4) C(20) 1.36(1) . . yes N(5) C(21) 1.36(1) . . yes N(5) C(25) 1.35(1) . . yes C(1) C(2) 1.37(1) . . yes C(2) C(3) 1.38(1) . . yes C(3) C(4) 1.39(1) . . yes C(4) C(5) 1.38(1) . . yes C(5) C(6) 1.50(1) . . yes C(6) C(7) 1.40(1) . . yes C(7) C(8) 1.39(2) . . yes C(8) C(9) 1.39(2) . . yes C(9) C(10) 1.38(1) . . yes C(10) C(11) 1.48(1) . . yes C(11) C(12) 1.39(1) . . yes C(12) C(13) 1.37(2) . . yes C(13) C(14) 1.37(2) . . yes C(14) C(15) 1.36(2) . . yes C(16) C(17) 1.39(1) . . yes C(17) C(18) 1.38(1) . . yes C(18) C(19) 1.39(1) . . yes C(19) C(20) 1.39(1) . . yes C(19) C(26) 1.47(1) . . yes C(20) C(21) 1.46(1) . . yes C(21) C(22) 1.39(1) . . yes C(22) C(23) 1.38(1) . . yes C(22) C(27) 1.52(1) . . yes C(23) C(24) 1.38(2) . . yes C(24) C(25) 1.38(1) . . yes C(26) C(27) 1.55(1) . . yes C(27) C(28) 1.51(2) . . yes C(28) C(29) 1.53(2) . . yes C(29) C(30) 1.49(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 O(1) Ru(1) N(1) 89.7(3) . . . yes O(1) Ru(1) N(2) 88.5(3) . . . yes O(1) Ru(1) N(3) 88.2(3) . . . yes O(1) Ru(1) N(4) 173.2(3) . . . yes O(1) Ru(1) N(5) 94.0(3) . . . yes N(1) Ru(1) N(2) 79.0(3) . . . yes N(1) Ru(1) N(3) 159.0(3) . . . yes N(1) Ru(1) N(4) 90.6(3) . . . yes N(1) Ru(1) N(5) 105.8(3) . . . yes N(2) Ru(1) N(3) 80.1(3) . . . yes N(2) Ru(1) N(4) 98.3(3) . . . yes N(2) Ru(1) N(5) 174.6(3) . . . yes N(3) Ru(1) N(4) 93.9(3) . . . yes N(3) Ru(1) N(5) 95.2(3) . . . yes N(4) Ru(1) N(5) 79.3(3) . . . yes O(5) Cl(1) O(6) 109.6(9) . . . yes O(5) Cl(1) O(7) 109.3(7) . . . yes O(5) Cl(1) O(8) 108.4(7) . . . yes O(6) Cl(1) O(7) 108.2(6) . . . yes O(6) Cl(1) O(8) 111.5(7) . . . yes O(7) Cl(1) O(8) 109.8(7) . . . yes O(9) Cl(2) O(10) 113(2) . . . yes O(9) Cl(2) O(11) 93(1) . . . yes O(9) Cl(2) O(12) 102(1) . . . yes O(10) Cl(2) O(11) 124(2) . . . yes O(10) Cl(2) O(12) 109(2) . . . yes O(11) Cl(2) O(12) 110(1) . . . yes F(1) P(1) F(1) 94(2) . . 2_756 yes F(1) P(1) F(2) 172(1) . . . yes F(1) P(1) F(2) 87(1) . . 2_756 yes F(1) P(1) F(3) 78(1) . . . yes F(1) P(1) F(3) 86(1) . . 2_756 yes F(1) P(1) F(2) 87(1) 2_756 . . yes F(1) P(1) F(2) 172(1) 2_756 . 2_756 yes F(1) P(1) F(3) 86(1) 2_756 . . yes F(1) P(1) F(3) 78(1) 2_756 . 2_756 yes F(2) P(1) F(2) 91(1) . . 2_756 yes F(2) P(1) F(3) 94.6(9) . . . yes F(2) P(1) F(3) 101.0(9) . . 2_756 yes F(2) P(1) F(3) 101.0(9) 2_756 . . yes F(2) P(1) F(3) 94.6(9) 2_756 . 2_756 yes F(3) P(1) F(3) 157(1) . . 2_756 yes Ru(1) N(1) C(1) 128.4(7) . . . yes Ru(1) N(1) C(5) 114.5(6) . . . yes C(1) N(1) C(5) 117.1(9) . . . yes Ru(1) N(2) C(6) 119.0(7) . . . yes Ru(1) N(2) C(10) 118.1(7) . . . yes C(6) N(2) C(10) 122.7(8) . . . yes Ru(1) N(3) C(11) 112.2(6) . . . yes Ru(1) N(3) C(15) 129.3(7) . . . yes C(11) N(3) C(15) 118.3(9) . . . yes Ru(1) N(4) C(16) 127.3(6) . . . yes Ru(1) N(4) C(20) 114.9(6) . . . yes C(16) N(4) C(20) 117.8(8) . . . yes Ru(1) N(5) C(21) 113.8(6) . . . yes Ru(1) N(5) C(25) 128.8(7) . . . yes C(21) N(5) C(25) 116.9(8) . . . yes N(1) C(1) C(2) 122.6(9) . . . yes C(1) C(2) C(3) 120.4(10) . . . yes C(2) C(3) C(4) 118(1) . . . yes C(3) C(4) C(5) 118.4(10) . . . yes N(1) C(5) C(4) 123.3(9) . . . yes N(1) C(5) C(6) 113.7(9) . . . yes C(4) C(5) C(6) 122.9(9) . . . yes N(2) C(6) C(5) 113.6(9) . . . yes N(2) C(6) C(7) 119.6(10) . . . yes C(5) C(6) C(7) 126.8(10) . . . yes C(6) C(7) C(8) 118(1) . . . yes C(7) C(8) C(9) 119.7(10) . . . yes C(8) C(9) C(10) 119(1) . . . yes N(2) C(10) C(9) 120.1(10) . . . yes N(2) C(10) C(11) 113.5(8) . . . yes C(9) C(10) C(11) 126.1(10) . . . yes N(3) C(11) C(10) 115.9(9) . . . yes N(3) C(11) C(12) 120.8(9) . . . yes C(10) C(11) C(12) 123.3(9) . . . yes C(11) C(12) C(13) 119.1(10) . . . yes C(12) C(13) C(14) 119(1) . . . yes C(13) C(14) C(15) 119(1) . . . yes N(3) C(15) C(14) 122.8(10) . . . yes N(4) C(16) C(17) 122.3(8) . . . yes C(16) C(17) C(18) 119.2(9) . . . yes C(17) C(18) C(19) 119.8(9) . . . yes C(18) C(19) C(20) 117.9(9) . . . yes C(18) C(19) C(26) 121.1(9) . . . yes C(20) C(19) C(26) 121.0(9) . . . yes N(4) C(20) C(19) 123.0(9) . . . yes N(4) C(20) C(21) 116.4(8) . . . yes C(19) C(20) C(21) 120.6(8) . . . yes N(5) C(21) C(20) 114.2(8) . . . yes N(5) C(21) C(22) 123.3(9) . . . yes C(20) C(21) C(22) 122.5(9) . . . yes C(21) C(22) C(23) 117.8(10) . . . yes C(21) C(22) C(27) 121.0(9) . . . yes C(23) C(22) C(27) 121.2(9) . . . yes C(22) C(23) C(24) 120.2(9) . . . yes C(23) C(24) C(25) 118.9(10) . . . yes N(5) C(25) C(24) 122.9(10) . . . yes O(3) C(26) C(19) 121.2(10) . . . yes O(3) C(26) C(27) 119.2(9) . . . yes C(19) C(26) C(27) 119.5(9) . . . yes O(2) C(27) C(22) 108.3(9) . . . yes O(2) C(27) C(26) 107.5(8) . . . yes O(2) C(27) C(28) 104.5(8) . . . yes C(22) C(27) C(26) 114.6(8) . . . yes C(22) C(27) C(28) 112.4(9) . . . yes C(26) C(27) C(28) 109.0(9) . . . yes C(27) C(28) C(29) 116.1(8) . . . yes O(4) C(29) C(28) 117(1) . . . yes O(4) C(29) C(30) 123(1) . . . yes C(28) C(29) C(30) 118(1) . . . yes #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_[Ru(trpy)(PD)(OH2)](ClO4)2_H2O _database_code_depnum_ccdc_archive 'CCDC 220056' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C27 H21 Cl2 N5 O12 Ru ' _chemical_formula_moiety ? _chemical_formula_weight 779.47 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 8.1295(8) _cell_length_b 17.782(2) _cell_length_c 10.410(1) _cell_angle_alpha 90 _cell_angle_beta 94.916(5) _cell_angle_gamma 90 _cell_volume 1499.4(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4953 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.2 #------------------------------------------------------------------------------ _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.030 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 11826 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9935 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9935 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3540 _reflns_number_gt 2995 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1926 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 2995 _refine_ls_number_parameters 420 _refine_ls_goodness_of_fit_ref 1.662 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.09500(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0286 _refine_diff_density_max 0.89 _refine_diff_density_min -0.85 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack -0.3(1) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru Ru -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru(1) Ru 0.26184(7) 0.2866(1) 0.72550(5) 0.0209(1) Uani 1.00 d . . . Cl(1) Cl 0.4394(6) 0.1148(4) 0.2699(8) 0.122(2) Uani 1.00 d . . . Cl(2) Cl -0.0248(7) 0.4665(3) 0.3150(7) 0.101(2) Uani 1.00 d . . . O(1) O 0.1307(8) 0.2434(4) 0.8776(6) 0.030(2) Uani 1.00 d . . . O(2) O 0.258(1) 0.3172(5) 0.1060(7) 0.050(2) Uani 1.00 d . . . O(3) O -0.0131(9) 0.2300(5) 0.1288(6) 0.038(2) Uani 1.00 d . . . O(4) O 0.558(1) 0.145(1) 0.193(2) 0.132(7) Uani 1.00 d . . . O(5) O 0.479(4) 0.047(1) 0.315(2) 0.22(1) Uani 1.00 d . . . O(6) O 0.471(2) 0.160(1) 0.395(2) 0.143(7) Uani 1.00 d . . . O(7) O 0.288(1) 0.1360(10) 0.234(2) 0.120(6) Uani 1.00 d . . . O(8) O 0.129(1) 0.4845(7) 0.377(1) 0.082(4) Uani 1.00 d . . . O(9) O -0.066(2) 0.3918(9) 0.316(3) 0.171(8) Uani 1.00 d . . . O(10) O -0.148(2) 0.5068(7) 0.364(2) 0.153(7) Uani 1.00 d . . . O(11) O -0.026(3) 0.499(2) 0.165(2) 0.194(9) Uani 1.00 d . . . O(12) O 0.221(2) 0.1019(10) 0.943(2) 0.110(5) Uiso 1.00 d . . . N(1) N 0.4311(9) 0.2012(5) 0.7486(8) 0.028(2) Uani 1.00 d . . . N(2) N 0.429(1) 0.3346(5) 0.8484(7) 0.030(2) Uani 1.00 d . . . N(3) N 0.152(1) 0.3903(5) 0.7518(8) 0.033(2) Uani 1.00 d . . . N(4) N 0.3580(10) 0.3228(5) 0.5645(7) 0.027(2) Uani 1.00 d . . . N(5) N 0.0934(9) 0.2411(5) 0.5853(7) 0.027(2) Uani 1.00 d . . . C(1) C 0.429(1) 0.1341(6) 0.694(1) 0.036(2) Uani 1.00 d . . . C(2) C 0.555(2) 0.0779(8) 0.719(1) 0.047(3) Uani 1.00 d . . . C(3) C 0.684(2) 0.0975(8) 0.811(1) 0.054(3) Uani 1.00 d . . . C(4) C 0.691(1) 0.1682(8) 0.869(1) 0.044(3) Uani 1.00 d . . . C(5) C 0.564(1) 0.2170(7) 0.8363(10) 0.036(2) Uani 1.00 d . . . C(6) C 0.562(1) 0.2939(9) 0.8902(8) 0.038(2) Uani 1.00 d . . . C(7) C 0.685(2) 0.3290(9) 0.974(1) 0.058(3) Uani 1.00 d . . . C(8) C 0.657(2) 0.4024(9) 1.010(2) 0.070(4) Uani 1.00 d . . . C(9) C 0.522(2) 0.4409(8) 0.970(1) 0.056(3) Uani 1.00 d . . . C(10) C 0.400(2) 0.4043(6) 0.888(1) 0.045(2) Uani 1.00 d . . . C(11) C 0.244(2) 0.4364(6) 0.833(1) 0.045(3) Uani 1.00 d . . . C(12) C 0.186(2) 0.5077(7) 0.861(1) 0.055(3) Uani 1.00 d . . . C(13) C 0.026(2) 0.528(1) 0.801(2) 0.075(5) Uani 1.00 d . . . C(14) C -0.068(2) 0.4854(8) 0.720(2) 0.077(5) Uani 1.00 d . . . C(15) C -0.002(2) 0.4101(7) 0.694(1) 0.052(3) Uani 1.00 d . . . C(16) C 0.496(1) 0.3639(6) 0.5560(9) 0.032(2) Uani 1.00 d . . . C(17) C 0.560(2) 0.3834(7) 0.442(1) 0.045(3) Uani 1.00 d . . . C(18) C 0.475(1) 0.3632(6) 0.327(1) 0.040(3) Uani 1.00 d . . . C(19) C 0.322(1) 0.3220(6) 0.3319(9) 0.031(2) Uani 1.00 d . . . C(20) C 0.272(1) 0.3011(5) 0.4502(8) 0.024(2) Uani 1.00 d . . . C(21) C 0.126(1) 0.2585(5) 0.4637(8) 0.024(2) Uani 1.00 d . . . C(22) C 0.025(1) 0.2337(5) 0.3577(8) 0.026(2) Uani 1.00 d . . . C(23) C -0.121(1) 0.1933(7) 0.379(1) 0.038(3) Uani 1.00 d . . . C(24) C -0.148(1) 0.1748(9) 0.502(1) 0.055(3) Uani 1.00 d . . . C(25) C -0.043(1) 0.2004(7) 0.6052(10) 0.040(3) Uani 1.00 d . . . C(26) C 0.224(1) 0.298(1) 0.2129(9) 0.045(3) Uani 1.00 d . . . C(27) C 0.065(1) 0.2509(6) 0.2270(9) 0.031(2) Uani 1.00 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) 0.0245(3) 0.0254(3) 0.0125(3) -0.0043(4) -0.0002(2) -0.0002(4) Cl(1) 0.060(3) 0.112(4) 0.192(7) 0.009(3) 0.002(3) -0.051(4) Cl(2) 0.079(3) 0.078(3) 0.145(5) -0.011(2) 0.008(3) -0.012(3) O(1) 0.034(3) 0.042(4) 0.013(3) -0.012(3) 0.006(2) 0.002(3) O(2) 0.085(6) 0.053(4) 0.014(3) -0.033(4) 0.008(3) -0.001(3) O(3) 0.044(4) 0.051(4) 0.017(3) -0.008(3) -0.004(3) -0.008(3) O(4) 0.038(6) 0.19(2) 0.16(1) -0.003(7) -0.022(6) -0.05(1) O(5) 0.34(3) 0.18(2) 0.15(2) 0.23(2) 0.07(2) 0.04(1) O(6) 0.15(2) 0.09(1) 0.18(1) 0.01(1) -0.07(1) -0.014(10) O(7) 0.051(4) 0.10(1) 0.21(2) 0.004(6) 0.040(8) 0.08(1) O(8) 0.068(5) 0.077(8) 0.103(10) 0.000(5) 0.024(5) 0.006(7) O(9) 0.07(1) 0.072(5) 0.37(4) 0.009(7) 0.02(1) 0.06(1) O(10) 0.058(7) 0.056(7) 0.35(3) 0.016(6) 0.07(1) 0.03(1) O(11) 0.17(2) 0.33(3) 0.093(7) -0.19(2) 0.053(9) -0.084(9) N(1) 0.024(3) 0.032(3) 0.028(4) -0.002(2) 0.005(3) 0.008(3) N(2) 0.037(4) 0.039(4) 0.015(3) -0.020(3) 0.003(2) -0.003(3) N(3) 0.041(4) 0.028(3) 0.032(4) 0.004(3) 0.020(3) 0.006(3) N(4) 0.030(4) 0.036(4) 0.014(2) -0.006(3) 0.000(2) 0.006(3) N(5) 0.025(3) 0.046(5) 0.012(3) -0.006(3) 0.002(2) -0.006(3) C(1) 0.045(5) 0.035(4) 0.031(5) -0.004(4) 0.011(4) 0.000(4) C(2) 0.047(6) 0.051(7) 0.046(6) 0.014(4) 0.024(4) 0.002(5) C(3) 0.046(6) 0.066(6) 0.051(7) 0.019(6) 0.011(5) 0.018(5) C(4) 0.025(4) 0.066(6) 0.043(6) 0.004(4) 0.006(4) 0.019(5) C(5) 0.026(4) 0.057(5) 0.025(5) -0.003(3) 0.007(3) 0.010(4) C(6) 0.035(4) 0.063(5) 0.015(3) -0.011(4) -0.004(3) -0.001(5) C(7) 0.056(7) 0.081(7) 0.034(6) -0.041(6) -0.019(5) -0.002(6) C(8) 0.071(8) 0.078(8) 0.059(9) -0.052(6) -0.012(7) -0.011(7) C(9) 0.077(7) 0.063(7) 0.029(6) -0.044(5) 0.009(5) -0.015(5) C(10) 0.075(6) 0.036(4) 0.025(5) -0.033(4) 0.016(4) -0.010(4) C(11) 0.080(6) 0.024(4) 0.034(5) -0.017(4) 0.026(4) -0.006(4) C(12) 0.084(8) 0.029(4) 0.055(8) -0.005(5) 0.029(6) -0.003(5) C(13) 0.083(9) 0.067(9) 0.08(1) 0.024(8) 0.031(7) -0.013(8) C(14) 0.074(10) 0.039(6) 0.12(1) 0.009(6) 0.035(9) -0.011(7) C(15) 0.046(5) 0.040(5) 0.071(9) 0.016(5) 0.004(5) 0.018(6) C(16) 0.041(5) 0.032(5) 0.024(4) -0.020(4) 0.001(4) 0.005(4) C(17) 0.058(7) 0.052(6) 0.026(4) -0.026(5) 0.012(4) 0.003(5) C(18) 0.052(6) 0.042(6) 0.028(4) -0.014(4) 0.010(4) 0.004(4) C(19) 0.044(5) 0.032(4) 0.017(3) 0.001(4) 0.006(3) 0.002(3) C(20) 0.027(3) 0.028(6) 0.016(3) 0.005(3) -0.001(2) 0.000(3) C(21) 0.028(4) 0.029(4) 0.014(3) 0.002(3) 0.003(3) -0.002(3) C(22) 0.029(4) 0.032(4) 0.017(3) -0.006(3) 0.001(3) 0.005(3) C(23) 0.026(5) 0.056(7) 0.034(4) -0.019(4) 0.006(4) -0.005(5) C(24) 0.032(5) 0.11(1) 0.025(4) -0.026(6) 0.001(4) -0.020(6) C(25) 0.032(5) 0.067(7) 0.019(4) -0.025(4) -0.004(3) 0.007(4) C(26) 0.057(5) 0.06(1) 0.016(3) -0.030(7) 0.009(3) 0.000(4) C(27) 0.039(5) 0.037(5) 0.015(3) 0.007(3) -0.004(3) 0.002(3) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) O(1) 2.126(7) . . yes Ru(1) N(1) 2.049(8) . . yes Ru(1) N(2) 1.976(8) . . yes Ru(1) N(3) 2.078(9) . . yes Ru(1) N(4) 2.015(8) . . yes Ru(1) N(5) 2.078(7) . . yes Cl(1) O(4) 1.42(2) . . yes Cl(1) O(5) 1.32(2) . . yes Cl(1) O(6) 1.54(2) . . yes Cl(1) O(7) 1.31(1) . . yes Cl(2) O(8) 1.39(1) . . yes Cl(2) O(9) 1.37(2) . . yes Cl(2) O(10) 1.36(2) . . yes Cl(2) O(11) 1.66(2) . . yes O(2) C(26) 1.22(1) . . yes O(3) C(27) 1.21(1) . . yes N(1) C(1) 1.32(1) . . yes N(1) C(5) 1.38(1) . . yes N(2) C(6) 1.34(1) . . yes N(2) C(10) 1.33(1) . . yes N(3) C(11) 1.36(1) . . yes N(3) C(15) 1.38(2) . . yes N(4) C(16) 1.35(1) . . yes N(4) C(20) 1.38(1) . . yes N(5) C(21) 1.35(1) . . yes N(5) C(25) 1.35(1) . . yes C(1) C(2) 1.44(2) . . yes C(2) C(3) 1.41(2) . . yes C(3) C(4) 1.39(2) . . yes C(4) C(5) 1.37(2) . . yes C(5) C(6) 1.48(2) . . yes C(6) C(7) 1.42(2) . . yes C(7) C(8) 1.38(2) . . yes C(8) C(9) 1.33(2) . . yes C(9) C(10) 1.41(2) . . yes C(10) C(11) 1.46(2) . . yes C(11) C(12) 1.39(2) . . yes C(12) C(13) 1.44(2) . . yes C(13) C(14) 1.32(3) . . yes C(14) C(15) 1.48(2) . . yes C(16) C(17) 1.38(2) . . yes C(17) C(18) 1.38(2) . . yes C(18) C(19) 1.45(2) . . yes C(19) C(20) 1.38(1) . . yes C(19) C(26) 1.47(1) . . yes C(20) C(21) 1.43(1) . . yes C(21) C(22) 1.39(1) . . yes C(22) C(23) 1.42(1) . . yes C(22) C(27) 1.46(1) . . yes C(23) C(24) 1.36(2) . . yes C(24) C(25) 1.39(2) . . yes C(26) C(27) 1.57(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 O(1) Ru(1) N(1) 91.1(3) . . . yes O(1) Ru(1) N(2) 91.9(3) . . . yes O(1) Ru(1) N(3) 88.4(3) . . . yes O(1) Ru(1) N(4) 171.8(3) . . . yes O(1) Ru(1) N(5) 92.3(3) . . . yes N(1) Ru(1) N(2) 80.0(3) . . . yes N(1) Ru(1) N(3) 159.2(3) . . . yes N(1) Ru(1) N(4) 91.7(3) . . . yes N(1) Ru(1) N(5) 100.9(3) . . . yes N(2) Ru(1) N(3) 79.2(4) . . . yes N(2) Ru(1) N(4) 96.2(3) . . . yes N(2) Ru(1) N(5) 175.7(3) . . . yes N(3) Ru(1) N(4) 91.7(4) . . . yes N(3) Ru(1) N(5) 99.9(3) . . . yes N(4) Ru(1) N(5) 79.6(3) . . . yes O(4) Cl(1) O(5) 113(1) . . . yes O(4) Cl(1) O(6) 102(1) . . . yes O(4) Cl(1) O(7) 113(1) . . . yes O(5) Cl(1) O(6) 99(1) . . . yes O(5) Cl(1) O(7) 123(2) . . . yes O(6) Cl(1) O(7) 100(1) . . . yes O(8) Cl(2) O(9) 115(1) . . . yes O(8) Cl(2) O(10) 111(1) . . . yes O(8) Cl(2) O(11) 106(1) . . . yes O(9) Cl(2) O(10) 108(1) . . . yes O(9) Cl(2) O(11) 111(2) . . . yes O(10) Cl(2) O(11) 103(1) . . . yes Ru(1) N(1) C(1) 129.4(7) . . . yes Ru(1) N(1) C(5) 114.0(7) . . . yes C(1) N(1) C(5) 116.6(9) . . . yes Ru(1) N(2) C(6) 117.8(8) . . . yes Ru(1) N(2) C(10) 118.2(7) . . . yes C(6) N(2) C(10) 123.9(10) . . . yes Ru(1) N(3) C(11) 113.2(7) . . . yes Ru(1) N(3) C(15) 123.5(7) . . . yes C(11) N(3) C(15) 123.2(10) . . . yes Ru(1) N(4) C(16) 127.7(6) . . . yes Ru(1) N(4) C(20) 115.2(6) . . . yes C(16) N(4) C(20) 117.1(8) . . . yes Ru(1) N(5) C(21) 113.6(6) . . . yes Ru(1) N(5) C(25) 126.8(6) . . . yes C(21) N(5) C(25) 119.6(8) . . . yes N(1) C(1) C(2) 124.6(10) . . . yes C(1) C(2) C(3) 115(1) . . . yes C(2) C(3) C(4) 121(1) . . . yes C(3) C(4) C(5) 117.6(10) . . . yes N(1) C(5) C(4) 124(1) . . . yes N(1) C(5) C(6) 113.8(9) . . . yes C(4) C(5) C(6) 121.7(9) . . . yes N(2) C(6) C(5) 114.2(8) . . . yes N(2) C(6) C(7) 118(1) . . . yes C(5) C(6) C(7) 127(1) . . . yes C(6) C(7) C(8) 117(1) . . . yes C(7) C(8) C(9) 123(1) . . . yes C(8) C(9) C(10) 118(1) . . . yes N(2) C(10) C(9) 118(1) . . . yes N(2) C(10) C(11) 114.5(10) . . . yes C(9) C(10) C(11) 126(1) . . . yes N(3) C(11) C(10) 114.9(9) . . . yes N(3) C(11) C(12) 119(1) . . . yes C(10) C(11) C(12) 125(1) . . . yes C(11) C(12) C(13) 116(1) . . . yes C(12) C(13) C(14) 125(1) . . . yes C(13) C(14) C(15) 116(2) . . . yes N(3) C(15) C(14) 118(1) . . . yes N(4) C(16) C(17) 124.7(9) . . . yes C(16) C(17) C(18) 118(1) . . . yes C(17) C(18) C(19) 118.1(10) . . . yes C(18) C(19) C(20) 119.0(8) . . . yes C(18) C(19) C(26) 121.0(9) . . . yes C(20) C(19) C(26) 119.9(9) . . . yes N(4) C(20) C(19) 122.1(8) . . . yes N(4) C(20) C(21) 115.2(7) . . . yes C(19) C(20) C(21) 122.6(8) . . . yes N(5) C(21) C(20) 116.3(7) . . . yes N(5) C(21) C(22) 121.7(8) . . . yes C(20) C(21) C(22) 121.9(8) . . . yes C(21) C(22) C(23) 118.6(9) . . . yes C(21) C(22) C(27) 120.0(8) . . . yes C(23) C(22) C(27) 120.4(8) . . . yes C(22) C(23) C(24) 118.5(10) . . . yes C(23) C(24) C(25) 120(1) . . . yes N(5) C(25) C(24) 120.9(10) . . . yes O(2) C(26) C(19) 123(1) . . . yes O(2) C(26) C(27) 119.1(9) . . . yes C(19) C(26) C(27) 117.7(9) . . . yes O(3) C(27) C(22) 125.6(9) . . . yes O(3) C(27) C(26) 117.5(8) . . . yes C(22) C(27) C(26) 116.8(8) . . . yes #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #==END