Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_TWH301 _database_code_CSD 192811 #---------------------------------------------------------------------- #------- _audit_creation_date '1998-03-09' _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; #---------------------------------------------------------------------- #------- _journal_coden_Cambridge 186 loop_ _publ_author_name 'Janice Aldrich-Wright' 'Ronald F. Fenton' 'Ivan D. Greguric' 'T. Hambley' 'Peter A. Williams' _publ_contact_author_name 'Dr Janice Aldrich-Wright' _publ_contact_author_address ; College of Science, Technology & Environment University Of Western Sydney Locked Bag 1797 Penrith South DC NSW 1797 AUSTRALIA ; _publ_contact_author_email 'J.ALDRICH-WRIGHT@UWS.EDU.AU' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The stereospecific synthesis of L-a-{dipyrido[3,2-a:2'3'-c] (6,7,8,9-tetrahydro)phenazine[N,N¢-di(2-picolyl)-2,5-dimethyl-2S,5S-diaminoc yclohexane]ruthenium(II)} and related b isomers ; _publ_section_abstract ; The conglomerate???-?-[Ru(R*,R*-picchxnMe2)(dpqC)](ClO4)2.0.5H2O and ?-?-[Ru(S,S-picchxnMe2)(dpqC)](ClO4)2.0.5H2O (where picchxnMe2 = N,N?- dimethyl-1,2-di(2?-picolyl)-S,S-diaminocyclohexane and dpqC = dipyrido [3,2-a:2'3'-c](6,7,8,9-tetrahydro)phenazine) have been isolated. Single crystal X-ray structures have been determined, although it was discovered only after initial data had been collected that the ??-?- [Ru(R*,R*-picchxnMe2)(dpqC)](ClO4)2.0.5H2O species was in fact a conglomerate. ?-?-[Ru(S,S-picchxnMe2)(dpqC)](ClO4)2.0.5H2O crystallises in the orthorhombic space group C2221 with a = 15.127(2), b = 22.976(4), c = 25.561(7) Å, (alternatively a =15.187 (3), b = 23.003(6), c = 25. 685 (7) Å, for the separate determination of a crystal of the conglomerate), Z = 8, and the ?-??structure was refined to an R value of 0.059. This structure enables, for the first time, the correlation of the absolute configurations for Ru(II) complexes of the N4 tetradentate with their CD spectra. We also report the synthesis and properties of ?- [Ru(R*,R*-picchxnMe2)(dpqc)]2+ isomers.here a procedure to synthesise and isolate enantiomerically pure tetradentate metal complexes of the type ?- the ?-[Ru(R*,R*-picchxnMe2)(dpqC)]2+ isomers. ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. ; _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' #---------------------------------------------------------------------- #------- _cell_length_a 15.1270 _cell_length_b 22.9762 _cell_length_c 25.5610 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8884.0059 _cell_formula_units_Z 8 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #---------------------------------------------------------------------- #------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21 ' _symmetry_Int_Tables_number 20 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, -y, -z' ' -x, -y, 1/2+z' ' -x, +y, 1/2-z' ' 1/2+x, 1/2+y, z' ' 1/2+x, 1/2-y, -z' ' 1/2-x, 1/2-y, 1/2+z' ' 1/2-x, 1/2+y, 1/2-z' #---------------------------------------------------------------------- #------- _exptl_crystal_description 'prisms' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.275 _exptl_crystal_size_mid 0.325 _exptl_crystal_size_min 0.40 _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 918.78 _chemical_formula_analytical ? _chemical_formula_sum 'C38 H42 Cl2 N8 O8.5 Ru' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2696.00 _exptl_absorpt_coefficient_mu 0.72 _exptl_absorpt_correction_type ; \DF (DIFABS; Walker & Stuart, 1983) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.892 _exptl_special_details ; ? ; #---------------------------------------------------------------------- #------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 273.2 _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 'unknown' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 4279 _reflns_number_total 4279 _reflns_number_observed 3313 _reflns_observed_criterion >3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.05893 _diffrn_orient_matrix_UB_12 -0.00640 _diffrn_orient_matrix_UB_13 0.01679 _diffrn_orient_matrix_UB_21 0.02188 _diffrn_orient_matrix_UB_22 -0.01895 _diffrn_orient_matrix_UB_23 -0.03276 _diffrn_orient_matrix_UB_31 0.02047 _diffrn_orient_matrix_UB_32 0.03865 _diffrn_orient_matrix_UB_33 -0.01324 #---------------------------------------------------------------------- #------- 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 Ru 0 8 -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 224 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 48 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 16 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 264 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #---------------------------------------------------------------------- #------- 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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) -0.39316(6) -0.18779(4) -0.56816(4) 0.0435(2) 1.000 . Uani d ? Cl(1) -0.6883(4) 0.0000 -0.5000 0.133(3) 0.500 ST Uani d ? Cl(2) -0.7597(3) -0.1341(2) -0.7204(2) 0.104(2) 1.000 . Uani d ? Cl(3) -0.433(1) -0.1687(6) -0.1340(8) 0.190(7) 0.500 . Uani d ? O(1) -0.676(3) -0.030(2) -0.548(1) 0.32(2) 0.750 . Uani d ? O(2) -0.774(1) 0.0000 -0.5000 0.144(8) 0.500 ST Uani d ? O(3) -0.652(2) 0.052(1) -0.509(2) 0.31(2) 0.750 . Uani d ? O(4) -0.813(2) -0.1548(10) -0.6831(10) 0.103(7) 0.500 . Uiso d ? O(5) -0.768(2) -0.118(1) -0.669(1) 0.141(10) 0.500 . Uiso d ? O(6) -0.747(2) -0.063(1) -0.717(1) 0.14(1) 0.500 . Uiso d ? O(7) -0.790(2) -0.083(1) -0.746(1) 0.140(10) 0.500 . Uiso d ? O(8) -0.795(2) -0.144(1) -0.769(1) 0.119(8) 0.500 . Uiso d ? O(9) -0.6700(8) -0.1488(7) -0.7240(5) 0.151(6) 1.000 . Uani d ? O(10) -0.530(3) -0.194(2) -0.146(1) 0.21(2) 0.500 . Uiso d ? O(11) -0.383(2) -0.164(1) -0.091(1) 0.13(1) 0.500 . Uiso d ? O(12) -0.376(2) -0.199(1) -0.173(1) 0.12(1) 0.350 . Uiso d ? O(13) -0.456(3) -0.123(2) -0.157(2) 0.21(2) 0.350 . Uiso d ? O(14) -0.5000 -0.1762(6) -0.7500 0.094(5) 0.500 ST Uani d ? N(1) -0.2564(5) -0.1703(3) -0.5647(4) 0.044(2) 1.000 . Uani d ? N(2) -0.3889(6) -0.1226(4) -0.5109(4) 0.047(3) 1.000 . Uani d ? N(3) -0.0464(6) -0.0610(5) -0.4591(4) 0.059(3) 1.000 . Uani d ? N(4) -0.1864(7) -0.0118(4) -0.4043(4) 0.061(3) 1.000 . Uani d ? N(5) -0.3901(8) -0.2605(4) -0.6208(4) 0.053(3) 1.000 . Uani d ? N(6) -0.5338(5) -0.2008(3) -0.5767(4) 0.041(3) 1.000 . Uani d ? N(7) -0.3700(7) -0.2549(4) -0.5155(4) 0.051(3) 1.000 . Uani d ? N(8) -0.4219(6) -0.1235(4) -0.6224(4) 0.051(3) 1.000 . Uani d ? C(1) -0.1920(8) -0.1915(5) -0.5911(5) 0.058(4) 1.000 . Uani d ? C(2) -0.1031(8) -0.1791(5) -0.5823(4) 0.061(4) 1.000 . Uani d ? C(3) -0.0815(8) -0.1417(6) -0.5429(6) 0.070(5) 1.000 . Uani d ? C(4) -0.1474(7) -0.1163(5) -0.5134(5) 0.048(3) 1.000 . Uani d ? C(5) -0.2341(7) -0.1309(5) -0.5268(5) 0.047(3) 1.000 . Uani d ? C(6) -0.3079(7) -0.1038(5) -0.4978(4) 0.039(3) 1.000 . Uani d ? C(7) -0.2904(7) -0.0652(4) -0.4584(5) 0.051(3) 1.000 . Uani d ? C(8) -0.3635(7) -0.0387(5) -0.4331(6) 0.060(4) 1.000 . Uani d ? C(9) -0.4462(8) -0.0547(6) -0.4482(6) 0.075(5) 1.000 . Uani d ? C(10) -0.4543(7) -0.0959(6) -0.4858(5) 0.064(4) 1.000 . Uani d ? C(11) -0.1325(6) -0.0735(5) -0.4716(4) 0.041(3) 1.000 . Uani d ? C(12) -0.2010(7) -0.0498(4) -0.4445(5) 0.047(4) 1.000 . Uani d ? C(13) -0.0352(8) -0.0242(6) -0.4195(6) 0.064(4) 1.000 . Uani d ? C(14) -0.1029(9) -0.0010(5) -0.3927(5) 0.062(4) 1.000 . Uani d ? C(15) 0.0621(9) -0.0108(6) -0.4072(7) 0.091(6) 1.000 . Uani d ? C(16) -0.085(1) 0.0369(6) -0.3444(7) 0.084(5) 1.000 . Uani d ? C(17) 0.068(1) 0.0256(9) -0.3596(8) 0.130(8) 1.000 . Uani d ? C(18) 0.004(1) 0.045(1) -0.3331(10) 0.158(10) 1.000 . Uani d ? C(19) -0.4827(7) -0.2886(5) -0.6214(5) 0.049(3) 1.000 . Uani d ? C(20) -0.5499(8) -0.2392(5) -0.6212(6) 0.060(4) 1.000 . Uani d ? C(21) -0.6436(10) -0.2651(6) -0.6236(6) 0.081(5) 1.000 . Uani d ? C(22) -0.657(1) -0.3028(6) -0.6705(7) 0.095(6) 1.000 . Uani d ? C(23) -0.589(1) -0.3535(6) -0.6694(5) 0.084(5) 1.000 . Uani d ? C(24) -0.4933(9) -0.3280(5) -0.6700(6) 0.070(4) 1.000 . Uani d ? C(25) -0.3292(7) -0.3052(5) -0.5946(5) 0.053(4) 1.000 . Uani d ? C(26) -0.3402(8) -0.3040(5) -0.5356(5) 0.052(4) 1.000 . Uani d ? C(27) -0.3193(9) -0.3483(6) -0.5067(6) 0.070(5) 1.000 . Uani d ? C(28) -0.3268(9) -0.3454(7) -0.4512(6) 0.081(6) 1.000 . Uani d ? C(29) -0.3559(8) -0.2946(6) -0.4309(6) 0.063(4) 1.000 . Uani d ? C(30) -0.3780(8) -0.2530(5) -0.4640(5) 0.055(4) 1.000 . Uani d ? C(31) -0.3560(9) -0.2462(5) -0.6755(5) 0.063(4) 1.000 . Uani d ? C(32) -0.5733(8) -0.1428(6) -0.5903(5) 0.065(4) 1.000 . Uani d ? C(33) -0.5098(9) -0.1069(5) -0.6240(5) 0.057(4) 1.000 . Uani d ? C(34) -0.5349(10) -0.0576(5) -0.6538(6) 0.071(5) 1.000 . Uani d ? C(35) -0.474(1) -0.0262(5) -0.6818(6) 0.077(5) 1.000 . Uani d ? C(36) -0.390(1) -0.0472(5) -0.6815(5) 0.082(5) 1.000 . Uani d ? C(37) -0.3664(8) -0.0938(5) -0.6529(5) 0.058(4) 1.000 . Uani d ? C(38) -0.5753(9) -0.2225(6) -0.5294(6) 0.069(5) 1.000 . Uani d ? H(1) -0.2089 -0.2164 -0.6184 0.063 1.000 . Uiso c ? H(2) -0.0589 -0.1979 -0.6021 0.072 1.000 . Uiso c ? H(3) -0.0208 -0.1324 -0.5351 0.078 1.000 . Uiso c ? H(4) -0.3539 -0.0088 -0.4088 0.069 1.000 . Uiso c ? H(5) -0.4955 -0.0382 -0.4329 0.103 1.000 . Uiso c ? H(6) -0.5127 -0.1081 -0.4963 0.079 1.000 . Uiso c ? H(7) 0.0893 0.0090 -0.4357 0.103 1.000 . Uiso c ? H(8) 0.0921 -0.0475 -0.4027 0.103 1.000 . Uiso c ? H(9) -0.1144 0.0189 -0.3147 0.102 1.000 . Uiso c ? H(10) -0.1125 0.0742 -0.3495 0.102 1.000 . Uiso c ? H(11) 0.1055 0.0566 -0.3687 0.148 1.000 . Uiso c ? H(12) 0.1034 0.0002 -0.3354 0.148 1.000 . Uiso c ? H(13) 0.0117 0.0291 -0.2985 0.161 1.000 . Uiso c ? H(14) 0.0130 0.0852 -0.3322 0.161 1.000 . Uiso c ? H(15) -0.4896 -0.3110 -0.5912 0.061 1.000 . Uiso c ? H(16) -0.5428 -0.2169 -0.6522 0.078 1.000 . Uiso c ? H(17) -0.6880 -0.2343 -0.6251 0.100 1.000 . Uiso c ? H(18) -0.6564 -0.2879 -0.5934 0.100 1.000 . Uiso c ? H(19) -0.6496 -0.2801 -0.7017 0.106 1.000 . Uiso c ? H(20) -0.7161 -0.3186 -0.6711 0.106 1.000 . Uiso c ? H(21) -0.5986 -0.3769 -0.6995 0.109 1.000 . Uiso c ? H(22) -0.5978 -0.3747 -0.6388 0.109 1.000 . Uiso c ? H(23) -0.4511 -0.3581 -0.6700 0.082 1.000 . Uiso c ? H(24) -0.4842 -0.3050 -0.7019 0.082 1.000 . Uiso c ? H(25) -0.2690 -0.2968 -0.6024 0.063 1.000 . Uiso c ? H(26) -0.3430 -0.3434 -0.6067 0.063 1.000 . Uiso c ? H(27) -0.2987 -0.3856 -0.5217 0.081 1.000 . Uiso c ? H(28) -0.3086 -0.3782 -0.4292 0.103 1.000 . Uiso c ? H(29) -0.3606 -0.2905 -0.3948 0.080 1.000 . Uiso c ? H(30) -0.4035 -0.2183 -0.4489 0.068 1.000 . Uiso c ? H(31) -0.3541 -0.2802 -0.6962 0.080 1.000 . Uiso c ? H(32) -0.2994 -0.2290 -0.6733 0.080 1.000 . Uiso c ? H(33) -0.3962 -0.2189 -0.6912 0.080 1.000 . Uiso c ? H(34) -0.5855 -0.1238 -0.5570 0.083 1.000 . Uiso c ? H(35) -0.6296 -0.1493 -0.6068 0.083 1.000 . Uiso c ? H(36) -0.5972 -0.0456 -0.6533 0.080 1.000 . Uiso c ? H(37) -0.4923 0.0074 -0.7006 0.100 1.000 . Uiso c ? H(38) -0.3418 -0.0294 -0.7029 0.118 1.000 . Uiso c ? H(39) -0.3049 -0.1072 -0.6539 0.073 1.000 . Uiso c ? H(40) -0.6371 -0.2233 -0.5363 0.101 1.000 . Uiso c ? H(41) -0.5605 -0.1977 -0.5031 0.101 1.000 . Uiso c ? H(42) -0.5539 -0.2607 -0.5248 0.101 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) 0.0459(4) 0.0425(4) 0.0423(5) 0.0030(5) 0.0002(5) -0.0024(5) Cl(1) 0.047(3) 0.091(4) 0.26(1) 0.0000 0.0000 -0.074(6) Cl(2) 0.088(3) 0.150(4) 0.074(3) 0.024(3) 0.014(3) 0.015(3) Cl(3) 0.17(1) 0.12(1) 0.27(2) 0.073(10) 0.09(1) 0.04(1) O(1) 0.43(5) 0.28(4) 0.26(4) 0.01(4) 0.13(4) -0.12(3) O(2) 0.06(1) 0.12(1) 0.25(3) -0.0001 0.0001 0.06(2) O(3) 0.15(2) 0.19(2) 0.57(7) -0.15(2) 0.22(3) -0.21(3) O(9) 0.110(9) 0.23(2) 0.11(1) 0.03(1) 0.018(9) -0.02(1) O(14) 0.12(1) 0.066(9) 0.10(1) 0.0000 -0.036(10) 0.0001 N(1) 0.049(5) 0.041(4) 0.041(6) 0.006(4) 0.010(5) -0.015(5) N(2) 0.035(5) 0.054(5) 0.052(6) 0.010(5) -0.001(6) -0.005(5) N(3) 0.056(7) 0.057(6) 0.065(8) -0.012(5) 0.002(6) -0.003(6) N(4) 0.060(6) 0.048(6) 0.075(8) 0.001(5) -0.005(6) -0.013(6) N(5) 0.071(6) 0.043(5) 0.047(6) 0.007(6) -0.005(7) -0.009(4) N(6) 0.047(5) 0.039(5) 0.037(6) 0.000(4) -0.010(4) 0.007(4) N(7) 0.057(7) 0.053(6) 0.044(7) -0.001(5) 0.001(5) 0.008(5) N(8) 0.065(7) 0.047(5) 0.040(6) 0.018(5) 0.008(5) 0.004(5) C(1) 0.062(7) 0.047(6) 0.065(8) 0.014(7) 0.008(6) -0.004(7) C(2) 0.065(7) 0.063(7) 0.054(8) 0.014(8) 0.006(7) -0.013(6) C(3) 0.049(8) 0.063(8) 0.10(1) 0.005(6) 0.016(8) -0.012(8) C(4) 0.038(6) 0.048(6) 0.057(8) -0.002(5) 0.013(6) -0.001(6) C(5) 0.044(6) 0.051(6) 0.047(7) 0.003(5) 0.008(6) 0.003(6) C(6) 0.052(7) 0.043(6) 0.023(6) 0.008(5) 0.000(5) -0.003(5) C(7) 0.054(7) 0.033(5) 0.065(9) 0.000(5) 0.008(6) -0.004(6) C(8) 0.053(7) 0.057(6) 0.070(9) 0.004(5) 0.017(7) -0.040(8) C(9) 0.068(9) 0.077(9) 0.08(1) -0.001(7) 0.005(8) -0.042(9) C(10) 0.045(7) 0.081(9) 0.066(10) 0.013(7) 0.000(7) -0.020(8) C(11) 0.034(6) 0.051(6) 0.040(7) 0.001(5) 0.000(5) -0.001(5) C(12) 0.058(7) 0.037(6) 0.045(8) -0.002(5) -0.014(6) 0.005(5) C(13) 0.053(7) 0.062(8) 0.08(1) -0.013(6) -0.010(8) 0.005(8) C(14) 0.072(8) 0.050(6) 0.065(9) 0.005(8) -0.022(9) -0.011(6) C(15) 0.062(9) 0.079(10) 0.13(2) -0.015(8) -0.012(10) 0.00(1) C(16) 0.09(1) 0.067(9) 0.09(1) -0.009(8) 0.01(1) -0.018(9) C(17) 0.08(1) 0.16(2) 0.15(2) -0.02(1) -0.01(1) -0.08(2) C(18) 0.08(1) 0.22(2) 0.17(2) 0.02(2) -0.04(1) -0.14(2) C(19) 0.054(7) 0.049(6) 0.046(8) 0.001(5) -0.018(6) -0.003(6) C(20) 0.060(8) 0.047(7) 0.072(10) 0.000(6) -0.029(7) -0.002(7) C(21) 0.08(1) 0.083(10) 0.08(1) 0.006(8) -0.008(9) -0.004(9) C(22) 0.11(1) 0.065(9) 0.11(1) -0.031(9) -0.06(1) -0.013(9) C(23) 0.13(1) 0.061(8) 0.065(10) -0.019(9) -0.05(1) -0.005(7) C(24) 0.077(9) 0.062(8) 0.07(1) -0.008(7) -0.016(8) -0.025(7) C(25) 0.057(7) 0.047(7) 0.055(8) 0.018(6) 0.003(6) -0.007(6) C(26) 0.058(7) 0.034(6) 0.065(9) -0.001(6) -0.008(6) 0.003(6) C(27) 0.060(8) 0.085(10) 0.06(1) 0.023(7) -0.006(8) -0.001(8) C(28) 0.067(9) 0.09(1) 0.09(1) -0.032(8) -0.038(9) 0.032(10) C(29) 0.053(7) 0.085(9) 0.051(8) -0.004(6) -0.012(7) 0.004(9) C(30) 0.045(7) 0.055(7) 0.064(9) -0.006(6) -0.007(7) -0.005(6) C(31) 0.079(9) 0.078(9) 0.032(7) 0.005(7) 0.014(6) -0.015(6) C(32) 0.052(8) 0.091(10) 0.053(9) -0.001(7) 0.002(7) -0.014(7) C(33) 0.066(8) 0.060(7) 0.045(8) 0.001(7) -0.008(7) -0.015(7) C(34) 0.09(1) 0.047(7) 0.07(1) 0.027(7) -0.035(9) -0.012(7) C(35) 0.11(1) 0.044(7) 0.08(1) 0.005(8) 0.01(1) 0.011(8) C(36) 0.15(1) 0.045(7) 0.055(9) -0.032(10) -0.01(1) 0.008(6) C(37) 0.065(8) 0.064(8) 0.045(8) -0.008(7) 0.005(6) -0.011(7) C(38) 0.070(9) 0.065(8) 0.07(1) -0.004(7) -0.008(8) -0.002(7) #---------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|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 3313 _refine_ls_number_parameters 520 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_obs 0.0600 _refine_ls_wR_factor_all 0.0586 _refine_ls_wR_factor_obs 0.0586 _refine_ls_goodness_of_fit_all 2.839 _refine_ls_goodness_of_fit_obs 2.839 _refine_ls_shift/esd_max 0.1616 _refine_ls_shift/esd_mean 0.0844 _refine_diff_density_min -0.72 _refine_diff_density_max 0.57 #---------------------------------------------------------------------- #------- _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) N(1) 2.110(8) . . yes Ru(1) N(2) 2.095(9) . . yes Ru(1) N(5) 2.147(8) . . yes Ru(1) N(6) 2.159(8) . . yes Ru(1) N(7) 2.076(10) . . yes Ru(1) N(8) 2.072(9) . . yes Cl(1) O(1) 1.42(3) . . yes Cl(1) O(1) 1.42(3) . 2_554 yes Cl(1) O(2) 1.30(2) . . yes Cl(1) O(3) 1.34(2) . . yes Cl(1) O(3) 1.34(2) . 2_554 yes Cl(2) O(4) 1.34(2) . . yes Cl(2) O(5) 1.37(3) . . yes Cl(2) O(6) 1.64(3) . . yes Cl(2) O(7) 1.42(3) . . yes Cl(2) O(8) 1.36(3) . . yes Cl(2) O(9) 1.40(1) . . yes Cl(3) O(10) 1.61(4) . . yes Cl(3) O(11) 1.34(3) . . yes Cl(3) O(12) 1.49(4) . . yes Cl(3) O(13) 1.27(5) . . yes O(1) O(3) 1.57(5) . 2_554 yes O(4) O(5) 1.15(3) . . yes O(6) O(7) 1.10(3) . . yes O(7) O(8) 1.50(3) . . yes N(1) C(1) 1.28(1) . . yes N(1) C(5) 1.37(1) . . yes N(2) C(6) 1.34(1) . . yes N(2) C(10) 1.33(1) . . yes N(3) C(11) 1.37(1) . . yes N(3) C(13) 1.33(2) . . yes N(4) C(12) 1.37(1) . . yes N(4) C(14) 1.32(1) . . yes N(5) C(19) 1.54(2) . . yes N(5) C(25) 1.53(1) . . yes N(5) C(31) 1.52(1) . . yes N(6) C(20) 1.46(1) . . yes N(6) C(32) 1.50(1) . . yes N(6) C(38) 1.45(1) . . yes N(7) C(26) 1.32(1) . . yes N(7) C(30) 1.32(1) . . yes N(8) C(33) 1.38(2) . . yes N(8) C(37) 1.33(1) . . yes C(1) C(2) 1.39(2) . . yes C(1) H(1) 0.94 . . no C(2) C(3) 1.36(2) . . yes C(2) H(2) 0.94 . . no C(3) C(4) 1.38(2) . . yes C(3) H(3) 0.96 . . no C(4) C(5) 1.40(1) . . yes C(4) C(11) 1.47(2) . . yes C(5) C(6) 1.48(1) . . yes C(6) C(7) 1.37(2) . . yes C(7) C(8) 1.42(1) . . yes C(7) C(12) 1.44(2) . . yes C(8) C(9) 1.36(2) . . yes C(8) H(4) 0.94 . . no C(9) C(10) 1.36(2) . . yes C(9) H(5) 0.92 . . no C(10) H(6) 0.96 . . no C(11) C(12) 1.36(1) . . yes C(13) C(14) 1.34(2) . . yes C(13) C(15) 1.54(2) . . yes C(14) C(16) 1.54(2) . . yes C(15) C(17) 1.48(2) . . yes C(15) H(7) 0.95 . . no C(15) H(8) 0.97 . . no C(16) C(18) 1.38(2) . . yes C(16) H(9) 0.97 . . no C(16) H(10) 0.96 . . no C(17) C(18) 1.26(2) . . yes C(17) H(11) 0.94 . . no C(17) H(12) 1.01 . . no C(18) H(13) 0.96 . . no C(18) H(14) 0.94 . . no C(19) C(20) 1.52(1) . . yes C(19) C(24) 1.55(2) . . yes C(19) H(15) 0.93 . . no C(20) C(21) 1.54(2) . . yes C(20) H(16) 0.95 . . no C(21) C(22) 1.49(2) . . yes C(21) H(17) 0.98 . . no C(21) H(18) 0.95 . . no C(22) C(23) 1.55(2) . . yes C(22) H(19) 0.96 . . no C(22) H(20) 0.97 . . no C(23) C(24) 1.56(2) . . yes C(23) H(21) 0.95 . . no C(23) H(22) 0.93 . . no C(24) H(23) 0.94 . . no C(24) H(24) 0.98 . . no C(25) C(26) 1.52(1) . . yes C(25) H(25) 0.95 . . no C(25) H(26) 0.95 . . no C(26) C(27) 1.30(2) . . yes C(27) C(28) 1.43(2) . . yes C(27) H(27) 0.99 . . no C(28) C(29) 1.35(2) . . yes C(28) H(28) 0.98 . . no C(29) C(30) 1.32(2) . . yes C(29) H(29) 0.93 . . no C(30) H(30) 0.96 . . no C(31) H(31) 0.94 . . no C(31) H(32) 0.94 . . no C(31) H(33) 0.96 . . no C(32) C(33) 1.53(2) . . yes C(32) H(34) 0.97 . . no C(32) H(35) 0.96 . . no C(33) C(34) 1.42(2) . . yes C(34) C(35) 1.37(2) . . yes C(34) H(36) 0.98 . . no C(35) C(36) 1.37(2) . . yes C(35) H(37) 0.95 . . no C(36) C(37) 1.34(2) . . yes C(36) H(38) 1.00 . . no C(37) H(39) 0.98 . . no C(38) H(40) 0.95 . . no C(38) H(41) 0.91 . . no C(38) H(42) 0.94 . . 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 N(1) Ru(1) N(2) 78.7(4) . . . yes N(1) Ru(1) N(5) 98.9(4) . . . yes N(1) Ru(1) N(6) 175.5(3) . . . yes N(1) Ru(1) N(7) 87.1(4) . . . yes N(1) Ru(1) N(8) 95.6(4) . . . yes N(2) Ru(1) N(5) 173.7(4) . . . yes N(2) Ru(1) N(6) 101.5(4) . . . yes N(2) Ru(1) N(7) 94.2(3) . . . yes N(2) Ru(1) N(8) 88.0(3) . . . yes N(5) Ru(1) N(6) 81.4(4) . . . yes N(5) Ru(1) N(7) 79.9(3) . . . yes N(5) Ru(1) N(8) 98.1(4) . . . yes N(6) Ru(1) N(7) 97.4(3) . . . yes N(6) Ru(1) N(8) 79.8(3) . . . yes N(7) Ru(1) N(8) 176.9(4) . . . yes O(1) Cl(1) O(1) 164(3) . . 2_554 yes O(1) Cl(1) O(2) 97(1) . . . yes O(1) Cl(1) O(3) 103(2) . . . yes O(1) Cl(1) O(3) 69(1) . . 2_554 yes O(1) Cl(1) O(2) 97(1) 2_554 . . yes O(1) Cl(1) O(3) 69(1) 2_554 . . yes O(1) Cl(1) O(3) 103(2) 2_554 . 2_554 yes O(2) Cl(1) O(3) 114(1) . . . yes O(2) Cl(1) O(3) 114(1) . . 2_554 yes O(3) Cl(1) O(3) 131(2) . . 2_554 yes O(4) Cl(2) O(5) 50(1) . . . yes O(4) Cl(2) O(6) 112(1) . . . yes O(4) Cl(2) O(7) 115(1) . . . yes O(4) Cl(2) O(8) 110(1) . . . yes O(4) Cl(2) O(9) 122(1) . . . yes O(5) Cl(2) O(6) 71(1) . . . yes O(5) Cl(2) O(7) 101(1) . . . yes O(5) Cl(2) O(8) 151(1) . . . yes O(5) Cl(2) O(9) 102(1) . . . yes O(6) Cl(2) O(7) 41(1) . . . yes O(6) Cl(2) O(8) 104(1) . . . yes O(6) Cl(2) O(9) 97(1) . . . yes O(7) Cl(2) O(8) 65(1) . . . yes O(7) Cl(2) O(9) 118(1) . . . yes O(8) Cl(2) O(9) 106(1) . . . yes O(10) Cl(3) O(11) 134(2) . . . yes O(10) Cl(3) O(12) 103(2) . . . yes O(10) Cl(3) O(13) 88(2) . . . yes O(11) Cl(3) O(12) 104(2) . . . yes O(11) Cl(3) O(13) 118(3) . . . yes O(12) Cl(3) O(13) 103(3) . . . yes Cl(1) O(1) O(3) 53(1) . . 2_554 yes Cl(1) O(3) O(1) 57(1) . . 2_554 yes Cl(2) O(4) O(5) 66(2) . . . yes Cl(2) O(5) O(4) 63(2) . . . yes Cl(2) O(6) O(7) 58(2) . . . yes Cl(2) O(7) O(6) 80(2) . . . yes Cl(2) O(7) O(8) 55(1) . . . yes O(6) O(7) O(8) 132(3) . . . yes Cl(2) O(8) O(7) 59(1) . . . yes Ru(1) N(1) C(1) 130.6(8) . . . yes Ru(1) N(1) C(5) 113.4(7) . . . yes C(1) N(1) C(5) 115.9(9) . . . yes Ru(1) N(2) C(6) 115.6(7) . . . yes Ru(1) N(2) C(10) 130.1(8) . . . yes C(6) N(2) C(10) 114.3(10) . . . yes C(11) N(3) C(13) 115(1) . . . yes C(12) N(4) C(14) 116(1) . . . yes Ru(1) N(5) C(19) 108.1(7) . . . yes Ru(1) N(5) C(25) 105.0(7) . . . yes Ru(1) N(5) C(31) 114.4(7) . . . yes C(19) N(5) C(25) 105.7(8) . . . yes C(19) N(5) C(31) 112.9(9) . . . yes C(25) N(5) C(31) 110(1) . . . yes Ru(1) N(6) C(20) 109.1(7) . . . yes Ru(1) N(6) C(32) 107.0(6) . . . yes Ru(1) N(6) C(38) 112.9(7) . . . yes C(20) N(6) C(32) 106.9(9) . . . yes C(20) N(6) C(38) 111.7(9) . . . yes C(32) N(6) C(38) 109.0(9) . . . yes Ru(1) N(7) C(26) 116.2(8) . . . yes Ru(1) N(7) C(30) 127.2(8) . . . yes C(26) N(7) C(30) 116(1) . . . yes Ru(1) N(8) C(33) 114.7(8) . . . yes Ru(1) N(8) C(37) 128.6(8) . . . yes C(33) N(8) C(37) 116(1) . . . yes N(1) C(1) C(2) 124(1) . . . yes N(1) C(1) H(1) 114.7 . . . no C(2) C(1) H(1) 120.5 . . . no C(1) C(2) C(3) 118(1) . . . yes C(1) C(2) H(2) 120.2 . . . no C(3) C(2) H(2) 121.1 . . . no C(2) C(3) C(4) 119(1) . . . yes C(2) C(3) H(3) 121.4 . . . no C(4) C(3) H(3) 118.8 . . . no C(3) C(4) C(5) 116(1) . . . yes C(3) C(4) C(11) 124(1) . . . yes C(5) C(4) C(11) 118.9(10) . . . yes N(1) C(5) C(4) 124.3(10) . . . yes N(1) C(5) C(6) 116.6(9) . . . yes C(4) C(5) C(6) 119(1) . . . yes N(2) C(6) C(5) 115.4(9) . . . yes N(2) C(6) C(7) 124(1) . . . yes C(5) C(6) C(7) 119(1) . . . yes C(6) C(7) C(8) 117(1) . . . yes C(6) C(7) C(12) 121(1) . . . yes C(8) C(7) C(12) 120(1) . . . yes C(7) C(8) C(9) 118(1) . . . yes C(7) C(8) H(4) 119.8 . . . no C(9) C(8) H(4) 121.8 . . . no C(8) C(9) C(10) 118(1) . . . yes C(8) C(9) H(5) 120.8 . . . no C(10) C(9) H(5) 121.0 . . . no N(2) C(10) C(9) 126(1) . . . yes N(2) C(10) H(6) 114.4 . . . no C(9) C(10) H(6) 118.9 . . . no N(3) C(11) C(4) 117.1(10) . . . yes N(3) C(11) C(12) 121(1) . . . yes C(4) C(11) C(12) 121.4(10) . . . yes N(4) C(12) C(7) 119(1) . . . yes N(4) C(12) C(11) 121(1) . . . yes C(7) C(12) C(11) 119(1) . . . yes N(3) C(13) C(14) 122(1) . . . yes N(3) C(13) C(15) 113(1) . . . yes C(14) C(13) C(15) 123(1) . . . yes N(4) C(14) C(13) 122(1) . . . yes N(4) C(14) C(16) 117(1) . . . yes C(13) C(14) C(16) 119(1) . . . yes C(13) C(15) C(17) 109(1) . . . yes C(13) C(15) H(7) 110.7 . . . no C(13) C(15) H(8) 107.4 . . . no C(17) C(15) H(7) 109.6 . . . no C(17) C(15) H(8) 111.6 . . . no H(7) C(15) H(8) 107.9 . . . no C(14) C(16) C(18) 114(1) . . . yes C(14) C(16) H(9) 107.7 . . . no C(14) C(16) H(10) 108.5 . . . no C(18) C(16) H(9) 109.8 . . . no C(18) C(16) H(10) 109.4 . . . no H(9) C(16) H(10) 106.3 . . . no C(15) C(17) C(18) 126(1) . . . yes C(15) C(17) H(11) 105.0 . . . no C(15) C(17) H(12) 102.1 . . . no C(18) C(17) H(11) 109.3 . . . no C(18) C(17) H(12) 106.4 . . . no H(11) C(17) H(12) 105.0 . . . no C(16) C(18) C(17) 125(1) . . . yes C(16) C(18) H(13) 105.1 . . . no C(16) C(18) H(14) 106.2 . . . no C(17) C(18) H(13) 105.7 . . . no C(17) C(18) H(14) 104.4 . . . no H(13) C(18) H(14) 109.4 . . . no N(5) C(19) C(20) 107.1(8) . . . yes N(5) C(19) C(24) 110(1) . . . yes N(5) C(19) H(15) 109.0 . . . no C(20) C(19) C(24) 111.7(10) . . . yes C(20) C(19) H(15) 109.6 . . . no C(24) C(19) H(15) 109.1 . . . no N(6) C(20) C(19) 110.0(9) . . . yes N(6) C(20) C(21) 114(1) . . . yes N(6) C(20) H(16) 107.8 . . . no C(19) C(20) C(21) 109.1(9) . . . yes C(19) C(20) H(16) 108.9 . . . no C(21) C(20) H(16) 106.2 . . . no C(20) C(21) C(22) 112(1) . . . yes C(20) C(21) H(17) 110.8 . . . no C(20) C(21) H(18) 111.5 . . . no C(22) C(21) H(17) 107.2 . . . no C(22) C(21) H(18) 107.8 . . . no H(17) C(21) H(18) 106.9 . . . no C(21) C(22) C(23) 109(1) . . . yes C(21) C(22) H(19) 109.7 . . . no C(21) C(22) H(20) 110.8 . . . no C(23) C(22) H(19) 110.4 . . . no C(23) C(22) H(20) 109.3 . . . no H(19) C(22) H(20) 107.3 . . . no C(22) C(23) C(24) 109(1) . . . yes C(22) C(23) H(21) 107.8 . . . no C(22) C(23) H(22) 108.2 . . . no C(24) C(23) H(21) 110.4 . . . no C(24) C(23) H(22) 109.9 . . . no H(21) C(23) H(22) 111.1 . . . no C(19) C(24) C(23) 107(1) . . . yes C(19) C(24) H(23) 111.2 . . . no C(19) C(24) H(24) 109.7 . . . no C(23) C(24) H(23) 110.6 . . . no C(23) C(24) H(24) 109.9 . . . no H(23) C(24) H(24) 107.4 . . . no N(5) C(25) C(26) 110.9(10) . . . yes N(5) C(25) H(25) 110.3 . . . no N(5) C(25) H(26) 110.1 . . . no C(26) C(25) H(25) 108.0 . . . no C(26) C(25) H(26) 108.4 . . . no H(25) C(25) H(26) 109.0 . . . no N(7) C(26) C(25) 116(1) . . . yes N(7) C(26) C(27) 122(1) . . . yes C(25) C(26) C(27) 121(1) . . . yes C(26) C(27) C(28) 120(1) . . . yes C(26) C(27) H(27) 122.5 . . . no C(28) C(27) H(27) 116.8 . . . no C(27) C(28) C(29) 116(1) . . . yes C(27) C(28) H(28) 120.9 . . . no C(29) C(28) H(28) 122.4 . . . no C(28) C(29) C(30) 117(1) . . . yes C(28) C(29) H(29) 119.6 . . . no C(30) C(29) H(29) 122.7 . . . no N(7) C(30) C(29) 126(1) . . . yes N(7) C(30) H(30) 117.5 . . . no C(29) C(30) H(30) 116.4 . . . no N(5) C(31) H(31) 110.3 . . . no N(5) C(31) H(32) 110.1 . . . no N(5) C(31) H(33) 108.1 . . . no H(31) C(31) H(32) 110.5 . . . no H(31) C(31) H(33) 108.9 . . . no H(32) C(31) H(33) 108.9 . . . no N(6) C(32) C(33) 111.0(10) . . . yes N(6) C(32) H(34) 105.8 . . . no N(6) C(32) H(35) 108.5 . . . no C(33) C(32) H(34) 111.7 . . . no C(33) C(32) H(35) 113.0 . . . no H(34) C(32) H(35) 106.5 . . . no N(8) C(33) C(32) 116(1) . . . yes N(8) C(33) C(34) 119(1) . . . yes C(32) C(33) C(34) 124(1) . . . yes C(33) C(34) C(35) 121(1) . . . yes C(33) C(34) H(36) 118.1 . . . no C(35) C(34) H(36) 120.2 . . . no C(34) C(35) C(36) 115(1) . . . yes C(34) C(35) H(37) 120.1 . . . no C(36) C(35) H(37) 124.0 . . . no C(35) C(36) C(37) 122(1) . . . yes C(35) C(36) H(38) 122.0 . . . no C(37) C(36) H(38) 116.0 . . . no N(8) C(37) C(36) 124(1) . . . yes N(8) C(37) H(39) 116.7 . . . no C(36) C(37) H(39) 119.1 . . . no N(6) C(38) H(40) 106.1 . . . no N(6) C(38) H(41) 107.2 . . . no N(6) C(38) H(42) 106.0 . . . no H(40) C(38) H(41) 113.0 . . . no H(40) C(38) H(42) 110.0 . . . no H(41) C(38) H(42) 113.9 . . . 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 O(1) C(32) 3.21(4) . . no O(1) C(34) 3.51(4) . . no O(2) C(15) 3.44(2) . 1_455 no O(2) C(15) 3.44(2) . 2_454 no O(2) C(27) 3.56(1) . 5_455 no O(2) C(27) 3.56(1) . 6_444 no O(3) C(10) 3.15(2) . 2_554 no O(3) C(9) 3.30(2) . 2_554 no O(3) O(11) 3.36(5) . 3_454 no O(3) C(27) 3.41(4) . 5_455 no O(3) C(32) 3.48(4) . 2_554 no O(4) C(29) 3.20(3) . 6_444 no O(4) C(28) 3.44(3) . 6_444 no O(5) C(28) 3.31(4) . 6_444 no O(5) C(17) 3.35(3) . 2_454 no O(5) C(29) 3.52(4) . 6_444 no O(6) C(36) 3.35(3) . 4_453 no O(6) C(17) 3.52(3) . 2_454 no O(6) C(34) 3.60(3) . . no O(7) C(16) 3.32(4) . 3_454 no O(7) C(36) 3.39(3) . 4_453 no O(7) C(37) 3.51(3) . 4_453 no O(8) C(37) 3.36(3) . 4_453 no O(8) C(31) 3.58(3) . 4_453 no O(9) O(14) 2.73(1) . . no O(9) C(31) 3.43(2) . 4_453 no O(9) C(34) 3.43(2) . . no O(9) C(37) 3.43(2) . 4_453 no O(9) C(36) 3.48(2) . 4_453 no O(10) C(30) 3.41(4) . 4_454 no O(10) C(29) 3.48(4) . 4_454 no O(11) C(25) 3.28(3) . 7_445 no O(11) C(38) 3.42(3) . 4_454 no O(11) C(1) 3.51(3) . 7_445 no O(11) C(10) 3.52(3) . 4_454 no O(12) C(1) 3.44(4) . 7_445 no O(13) C(9) 3.45(6) . 4_454 no O(14) C(31) 3.31(1) . . no O(14) C(31) 3.31(1) . 4_453 no O(14) C(33) 3.60(1) . . no O(14) C(33) 3.60(1) . 4_453 no N(3) N(3) 3.50(2) . 2_554 no C(8) C(36) 3.55(2) . 2_554 no C(35) C(35) 3.57(3) . 4_453 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) N(1) C(1) C(2) . . . . -175.2(9) no Ru(1) N(1) C(5) C(4) . . . . 173.7(9) no Ru(1) N(1) C(5) C(6) . . . . -4(1) no Ru(1) N(2) C(6) C(5) . . . . 1(1) no Ru(1) N(2) C(6) C(7) . . . . -174.3(9) no Ru(1) N(2) C(10) C(9) . . . . 178(1) no Ru(1) N(5) C(19) C(20) . . . . 40(1) no Ru(1) N(5) C(19) C(24) . . . . 162.5(7) no Ru(1) N(5) C(25) C(26) . . . . 35(1) no Ru(1) N(6) C(20) C(19) . . . . 41(1) no Ru(1) N(6) C(20) C(21) . . . . 164.8(9) no Ru(1) N(6) C(32) C(33) . . . . 34(1) no Ru(1) N(7) C(26) C(25) . . . . -1(1) no Ru(1) N(7) C(26) C(27) . . . . 176(1) no Ru(1) N(7) C(30) C(29) . . . . -174.0(9) no Ru(1) N(8) C(33) C(32) . . . . -6(1) no Ru(1) N(8) C(33) C(34) . . . . 170.7(9) no Ru(1) N(8) C(37) C(36) . . . . -170.1(9) no Cl(2) O(6) O(7) O(8) . . . . -20(3) no Cl(2) O(8) O(7) O(6) . . . . 24(4) no O(1) Cl(1) O(1) O(3) . . 2_554 . 66(1) no O(1) O(3) Cl(1) O(2) . 2_554 . . 89(2) no O(1) O(3) Cl(1) O(3) . 2_554 . . -90(2) no O(2) Cl(1) O(1) O(3) . . . 2_554 -113(1) no O(2) Cl(1) O(1) O(3) . . 2_554 . -113(1) no O(4) Cl(2) O(6) O(7) . . . . -103(2) no O(4) Cl(2) O(7) O(6) . . . . 95(2) no O(4) Cl(2) O(7) O(8) . . . . -102(1) no O(4) Cl(2) O(8) O(7) . . . . 109(1) no O(4) O(5) Cl(2) O(6) . . . . 143(2) no O(4) O(5) Cl(2) O(7) . . . . 114(2) no O(4) O(5) Cl(2) O(8) . . . . 56(4) no O(4) O(5) Cl(2) O(9) . . . . -122(1) no O(5) Cl(2) O(6) O(7) . . . . -133(2) no O(5) Cl(2) O(7) O(6) . . . . 44(2) no O(5) Cl(2) O(7) O(8) . . . . -153(1) no O(5) Cl(2) O(8) O(7) . . . . 66(3) no O(5) O(4) Cl(2) O(6) . . . . -37(2) no O(5) O(4) Cl(2) O(7) . . . . -83(2) no O(5) O(4) Cl(2) O(8) . . . . -154(2) no O(5) O(4) Cl(2) O(9) . . . . 78(2) no O(6) Cl(2) O(7) O(8) . . . . 161(3) no O(6) Cl(2) O(8) O(7) . . . . -12(2) no O(6) O(7) Cl(2) O(8) . . . . -161(3) no O(6) O(7) Cl(2) O(9) . . . . -66(2) no O(7) O(6) Cl(2) O(8) . . . . 16(2) no O(7) O(6) Cl(2) O(9) . . . . 126(2) no O(7) O(8) Cl(2) O(9) . . . . -114(1) no O(8) O(7) Cl(2) O(9) . . . . 95(1) no N(1) Ru(1) N(2) C(6) . . . . -2.9(8) no N(1) Ru(1) N(2) C(10) . . . . 175(1) no N(1) Ru(1) N(5) C(19) . . . . 169.5(7) no N(1) Ru(1) N(5) C(25) . . . . 57.0(8) no N(1) Ru(1) N(5) C(31) . . . . -63.7(9) no N(1) Ru(1) N(6) C(20) . . . . 79(4) no N(1) Ru(1) N(6) C(32) . . . . -36(4) no N(1) Ru(1) N(6) C(38) . . . . -156(4) no N(1) Ru(1) N(7) C(26) . . . . -81.5(9) no N(1) Ru(1) N(7) C(30) . . . . 95(1) no N(1) Ru(1) N(8) C(33) . . . . -160.1(8) no N(1) Ru(1) N(8) C(37) . . . . 15(1) no N(1) C(1) C(2) C(3) . . . . 0(2) no N(1) C(5) C(4) C(3) . . . . 3(1) no N(1) C(5) C(4) C(11) . . . . -179.5(10) no N(1) C(5) C(6) N(2) . . . . 2(1) no N(1) C(5) C(6) C(7) . . . . 178.2(10) no N(2) Ru(1) N(1) C(1) . . . . -177(1) no N(2) Ru(1) N(1) C(5) . . . . 4.1(7) no N(2) Ru(1) N(5) C(19) . . . . 102(4) no N(2) Ru(1) N(5) C(25) . . . . -9(4) no N(2) Ru(1) N(5) C(31) . . . . -130(3) no N(2) Ru(1) N(6) C(20) . . . . 171.7(7) no N(2) Ru(1) N(6) C(32) . . . . 56.3(8) no N(2) Ru(1) N(6) C(38) . . . . -63.6(8) no N(2) Ru(1) N(7) C(26) . . . . -159.9(9) no N(2) Ru(1) N(7) C(30) . . . . 16(1) no N(2) Ru(1) N(8) C(33) . . . . -81.7(8) no N(2) Ru(1) N(8) C(37) . . . . 93(1) no N(2) C(6) C(5) C(4) . . . . -176(1) no N(2) C(6) C(7) C(8) . . . . -6(1) no N(2) C(6) C(7) C(12) . . . . 175(1) no N(2) C(10) C(9) C(8) . . . . -1(2) no N(3) C(11) C(4) C(3) . . . . -4(1) no N(3) C(11) C(4) C(5) . . . . 179(1) no N(3) C(11) C(12) N(4) . . . . 1(1) no N(3) C(11) C(12) C(7) . . . . -178(1) no N(3) C(13) C(14) N(4) . . . . -1(2) no N(3) C(13) C(14) C(16) . . . . 174(1) no N(3) C(13) C(15) C(17) . . . . -174(1) no N(4) C(12) C(7) C(6) . . . . -178(1) no N(4) C(12) C(7) C(8) . . . . 3(1) no N(4) C(12) C(11) C(4) . . . . 177(1) no N(4) C(14) C(13) C(15) . . . . 178(1) no N(4) C(14) C(16) C(18) . . . . 177(1) no N(5) Ru(1) N(1) C(1) . . . . 7(1) no N(5) Ru(1) N(1) C(5) . . . . -170.0(7) no N(5) Ru(1) N(2) C(6) . . . . 64(4) no N(5) Ru(1) N(2) C(10) . . . . -116(4) no N(5) Ru(1) N(6) C(20) . . . . -14.0(7) no N(5) Ru(1) N(6) C(32) . . . . -129.3(7) no N(5) Ru(1) N(6) C(38) . . . . 110.7(8) no N(5) Ru(1) N(7) C(26) . . . . 18.1(8) no N(5) Ru(1) N(7) C(30) . . . . -165(1) no N(5) Ru(1) N(8) C(33) . . . . 100.1(8) no N(5) Ru(1) N(8) C(37) . . . . -84(1) no N(5) C(19) C(20) N(6) . . . . -55(1) no N(5) C(19) C(20) C(21) . . . . 178(1) no N(5) C(19) C(24) C(23) . . . . -178.2(9) no N(5) C(25) C(26) N(7) . . . . -24(1) no N(5) C(25) C(26) C(27) . . . . 157(1) no N(6) Ru(1) N(1) C(1) . . . . -84(4) no N(6) Ru(1) N(1) C(5) . . . . 97(4) no N(6) Ru(1) N(2) C(6) . . . . -178.3(8) no N(6) Ru(1) N(2) C(10) . . . . 0(1) no N(6) Ru(1) N(5) C(19) . . . . -15.1(7) no N(6) Ru(1) N(5) C(25) . . . . -127.6(8) no N(6) Ru(1) N(5) C(31) . . . . 111.7(9) no N(6) Ru(1) N(7) C(26) . . . . 97.9(9) no N(6) Ru(1) N(7) C(30) . . . . -85(1) no N(6) Ru(1) N(8) C(33) . . . . 20.4(8) no N(6) Ru(1) N(8) C(37) . . . . -164(1) no N(6) C(20) C(19) C(24) . . . . -176(1) no N(6) C(20) C(21) C(22) . . . . 178(1) no N(6) C(32) C(33) N(8) . . . . -19(1) no N(6) C(32) C(33) C(34) . . . . 163(1) no N(7) Ru(1) N(1) C(1) . . . . 87(1) no N(7) Ru(1) N(1) C(5) . . . . -90.8(8) no N(7) Ru(1) N(2) C(6) . . . . 83.2(8) no N(7) Ru(1) N(2) C(10) . . . . -98(1) no N(7) Ru(1) N(5) C(19) . . . . 84.1(7) no N(7) Ru(1) N(5) C(25) . . . . -28.4(7) no N(7) Ru(1) N(5) C(31) . . . . -149.1(10) no N(7) Ru(1) N(6) C(20) . . . . -92.5(7) no N(7) Ru(1) N(6) C(32) . . . . 152.1(7) no N(7) Ru(1) N(6) C(38) . . . . 32.2(8) no N(7) Ru(1) N(8) C(33) . . . . 51(7) no N(7) Ru(1) N(8) C(37) . . . . -133(7) no N(7) C(26) C(27) C(28) . . . . 0(2) no N(7) C(30) C(29) C(28) . . . . -3(2) no N(8) Ru(1) N(1) C(1) . . . . -91(1) no N(8) Ru(1) N(1) C(5) . . . . 90.9(8) no N(8) Ru(1) N(2) C(6) . . . . -99.1(8) no N(8) Ru(1) N(2) C(10) . . . . 79(1) no N(8) Ru(1) N(5) C(19) . . . . -93.5(7) no N(8) Ru(1) N(5) C(25) . . . . 154.0(7) no N(8) Ru(1) N(5) C(31) . . . . 33.3(9) no N(8) Ru(1) N(6) C(20) . . . . 85.9(7) no N(8) Ru(1) N(6) C(32) . . . . -29.5(7) no N(8) Ru(1) N(6) C(38) . . . . -149.4(8) no N(8) Ru(1) N(7) C(26) . . . . 67(7) no N(8) Ru(1) N(7) C(30) . . . . -115(7) no N(8) C(33) C(34) C(35) . . . . 0(1) no N(8) C(37) C(36) C(35) . . . . 0(2) no C(1) N(1) C(5) C(4) . . . . -4(1) no C(1) N(1) C(5) C(6) . . . . 176(1) no C(1) C(2) C(3) C(4) . . . . -1(1) no C(2) C(1) N(1) C(5) . . . . 2(1) no C(2) C(3) C(4) C(5) . . . . 0(1) no C(2) C(3) C(4) C(11) . . . . -177(1) no C(3) C(4) C(5) C(6) . . . . -178(1) no C(3) C(4) C(11) C(12) . . . . 179(1) no C(4) C(5) C(6) C(7) . . . . 0(1) no C(4) C(11) N(3) C(13) . . . . -176(1) no C(4) C(11) C(12) C(7) . . . . -2(1) no C(5) C(4) C(11) C(12) . . . . 2(1) no C(5) C(6) N(2) C(10) . . . . -177(1) no C(5) C(6) C(7) C(8) . . . . 177(1) no C(5) C(6) C(7) C(12) . . . . 0(1) no C(6) N(2) C(10) C(9) . . . . -2(2) no C(6) C(5) C(4) C(11) . . . . -1(1) no C(6) C(7) C(8) C(9) . . . . 2(2) no C(6) C(7) C(12) C(11) . . . . 0(1) no C(7) C(6) N(2) C(10) . . . . 6(1) no C(7) C(8) C(9) C(10) . . . . 1(2) no C(7) C(12) N(4) C(14) . . . . 178(1) no C(8) C(7) C(12) C(11) . . . . -176(1) no C(9) C(8) C(7) C(12) . . . . 179(1) no C(11) N(3) C(13) C(14) . . . . 0(1) no C(11) N(3) C(13) C(15) . . . . -179(1) no C(11) C(12) N(4) C(14) . . . . -1(1) no C(12) N(4) C(14) C(13) . . . . 1(1) no C(12) N(4) C(14) C(16) . . . . -174(1) no C(12) C(11) N(3) C(13) . . . . 0(1) no C(13) C(14) C(16) C(18) . . . . 1(2) no C(13) C(15) C(17) C(18) . . . . -1(3) no C(14) C(13) C(15) C(17) . . . . 5(2) no C(14) C(16) C(18) C(17) . . . . 2(3) no C(15) C(13) C(14) C(16) . . . . -5(2) no C(15) C(17) C(18) C(16) . . . . -1(4) no C(19) N(5) C(25) C(26) . . . . -78(1) no C(19) C(20) N(6) C(32) . . . . 156.9(9) no C(19) C(20) N(6) C(38) . . . . -83(1) no C(19) C(20) C(21) C(22) . . . . -57(1) no C(19) C(24) C(23) C(22) . . . . 59(1) no C(20) N(6) C(32) C(33) . . . . -82(1) no C(20) C(19) N(5) C(25) . . . . 152.8(10) no C(20) C(19) N(5) C(31) . . . . -86(1) no C(20) C(19) C(24) C(23) . . . . -59(1) no C(20) C(21) C(22) C(23) . . . . 59(1) no C(21) C(20) N(6) C(32) . . . . -79(1) no C(21) C(20) N(6) C(38) . . . . 39(1) no C(21) C(20) C(19) C(24) . . . . 57(1) no C(21) C(22) C(23) C(24) . . . . -60(1) no C(24) C(19) N(5) C(25) . . . . -85(1) no C(24) C(19) N(5) C(31) . . . . 34(1) no C(25) C(26) N(7) C(30) . . . . -178(1) no C(25) C(26) C(27) C(28) . . . . 177(1) no C(26) N(7) C(30) C(29) . . . . 2(1) no C(26) C(25) N(5) C(31) . . . . 159.3(10) no C(26) C(27) C(28) C(29) . . . . 0(2) no C(27) C(26) N(7) C(30) . . . . 0(1) no C(27) C(28) C(29) C(30) . . . . 2(1) no C(32) C(33) N(8) C(37) . . . . 177(1) no C(32) C(33) C(34) C(35) . . . . 177(1) no C(33) N(8) C(37) C(36) . . . . 4(1) no C(33) C(32) N(6) C(38) . . . . 156.4(10) no C(33) C(34) C(35) C(36) . . . . 3(2) no C(34) C(33) N(8) C(37) . . . . -5(1) no C(34) C(35) C(36) C(37) . . . . -3(2) no #----------------------------------------------------------------------