# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yagi, Masayuki' _publ_contact_author_email yagi@eng.niigata-u.ac.jp _publ_section_title ; Highly active and tunable catalysts for O2 evolution from water based on mononuclear ruthenium (II) monoaquo complexes ; loop_ _publ_author_name M.Yagi S.Tajima M.Komi H.Yamazaki data_[Ru(EtOtpy)(bpy)(H2O)](NO3)2-2.5(H2O) _database_code_depnum_ccdc_archive 'CCDC 794628' #TrackingRef '- RuEtOtpy_revised.cif' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_name_common '(Ru(EtOtpy)(bpy)(H2O))(NO3)2 - 2.5(H2O)' _chemical_formula_sum 'C27 H30 N7 O10.50 Ru ' _chemical_formula_moiety '(C27 H25 N5 O2 Ru 3+), (N O3 1-)2, 2.5(H2 O)' _chemical_formula_weight 721.64 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.0976(7) _cell_length_b 11.4129(7) _cell_length_c 13.8155(8) _cell_angle_alpha 91.808(5) _cell_angle_beta 102.944(5) _cell_angle_gamma 115.411(2) _cell_volume 1524.1(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 431 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour deep-red _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738.00 _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.910 _exptl_absorpt_correction_T_max 0.959 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 296.2 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 12187 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9268 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9268 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement was carried out using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). Three nitrate anions were found in an asymmetric unit: one of them has occupancy 1 and the others are located on different two sites with occupancy 0.5. Four oxygen atoms of H2O were found in an asymmetric unit: one of them has occupancy 1 and the others are located on different theee sites with occupancy 0.5. ; _reflns_number_total 6474 _reflns_number_gt 5787 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1370 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6474 _refine_ls_number_parameters 451 _refine_ls_goodness_of_fit_ref 1.258 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.07800(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0793 _refine_diff_density_max 1.20 _refine_diff_density_min -0.79 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.259 0.836 ;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) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 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) ; #------------------------------------------------------------------------------ # 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.05722(2) 0.31121(2) 0.22832(2) 0.03468(7) Uani 1.00 1 d . . . O(1) O -0.2595(3) -0.1415(3) 0.4311(2) 0.0598(7) Uani 1.00 1 d . . . O(1w) O -0.1159(3) 0.3536(3) 0.1912(2) 0.0584(8) Uani 1.00 1 d . . . O(2) O 0.7206(5) 0.5124(6) 0.1726(5) 0.158(3) Uani 1.00 1 d . . . O(2w) O 0.1187(5) -0.1617(5) 0.3179(3) 0.131(2) Uani 1.00 1 d . . . O(3) O 0.9209(4) 0.6099(4) 0.1646(5) 0.120(2) Uani 1.00 1 d . . . O(3w) O 0.406(1) -0.130(1) 0.3039(9) 0.143(5) Uani 0.50 2 d P . . O(4) O 0.7718(9) 0.6842(7) 0.1261(7) 0.225(4) Uani 1.00 1 d . . . O(4w) O 0.491(1) -0.042(1) 0.2100(9) 0.136(4) Uani 0.50 2 d P . . O(5) O 0.4259(7) -0.0628(7) 0.5382(6) 0.170(3) Uani 1.00 1 d . . . O(5w) O 0.6322(8) 0.1569(7) 0.1067(7) 0.088(2) Uani 0.50 2 d P . . O(6) O 0.387(1) -0.142(1) 0.3786(7) 0.131(4) Uani 0.50 2 d P . . O(7) O 0.4765(9) -0.0426(7) 0.1059(8) 0.113(2) Uani 0.50 2 d P . . O(8) O 0.6413(7) 0.1386(7) 0.1871(6) 0.081(2) Uani 0.50 2 d P . . O(9) O 0.586(1) 0.1122(9) 0.0289(8) 0.126(3) Uani 0.50 2 d P . . N(1) N -0.0531(3) 0.1641(2) 0.2918(2) 0.0379(6) Uani 1.00 1 d . . . N(2) N -0.0446(3) 0.1630(3) 0.1063(2) 0.0400(6) Uani 1.00 1 d . . . N(3) N 0.1099(3) 0.4044(3) 0.3738(2) 0.0402(6) Uani 1.00 1 d . . . N(4) N 0.1877(3) 0.4588(3) 0.1630(2) 0.0422(6) Uani 1.00 1 d . . . N(5) N 0.2242(3) 0.2759(3) 0.2565(2) 0.0407(6) Uani 1.00 1 d . . . N(6) N 0.8063(4) 0.6073(5) 0.1558(4) 0.087(1) Uani 1.00 1 d . . . N(7) N 0.459(1) -0.061(1) 0.451(1) 0.122(3) Uani 0.50 2 d P . . N(8) N 0.5684(8) 0.0720(8) 0.1094(7) 0.072(2) Uani 0.50 2 d P . . C(1) C -0.1326(3) 0.0450(3) 0.2362(2) 0.0413(7) Uani 1.00 1 d . . . C(2) C -0.2049(4) -0.0615(3) 0.2786(2) 0.0478(8) Uani 1.00 1 d . . . C(3) C -0.1938(4) -0.0436(3) 0.3813(3) 0.0491(8) Uani 1.00 1 d . . . C(4) C -0.1129(4) 0.0802(3) 0.4385(2) 0.0478(8) Uani 1.00 1 d . . . C(5) C -0.0430(3) 0.1835(3) 0.3916(2) 0.0404(7) Uani 1.00 1 d . . . C(6) C -0.1314(3) 0.0467(3) 0.1290(2) 0.0410(7) Uani 1.00 1 d . . . C(7) C -0.2146(4) -0.0600(4) 0.0554(3) 0.0534(9) Uani 1.00 1 d . . . C(8) C -0.2075(5) -0.0475(4) -0.0433(3) 0.065(1) Uani 1.00 1 d . . . C(9) C -0.1198(5) 0.0693(4) -0.0663(3) 0.062(1) Uani 1.00 1 d . . . C(10) C -0.0383(4) 0.1729(4) 0.0099(2) 0.0496(9) Uani 1.00 1 d . . . C(11) C 0.0504(3) 0.3227(3) 0.4377(2) 0.0415(7) Uani 1.00 1 d . . . C(12) C 0.0750(4) 0.3680(4) 0.5368(3) 0.0521(9) Uani 1.00 1 d . . . C(13) C 0.1607(4) 0.5009(4) 0.5723(3) 0.0592(10) Uani 1.00 1 d . . . C(14) C 0.2167(4) 0.5825(4) 0.5069(3) 0.0575(9) Uani 1.00 1 d . . . C(15) C 0.1908(4) 0.5322(3) 0.4094(3) 0.0470(8) Uani 1.00 1 d . . . C(16) C -0.3568(4) -0.2673(4) 0.3732(3) 0.0568(10) Uani 1.00 1 d . . . C(17) C -0.4232(5) -0.3552(4) 0.4436(3) 0.069(1) Uani 1.00 1 d . . . C(18) C 0.3112(3) 0.4589(3) 0.1677(2) 0.0447(8) Uani 1.00 1 d . . . C(19) C 0.4077(4) 0.5467(4) 0.1242(3) 0.062(1) Uani 1.00 1 d . . . C(20) C 0.3772(5) 0.6373(5) 0.0743(4) 0.074(1) Uani 1.00 1 d . . . C(21) C 0.2536(5) 0.6406(5) 0.0708(4) 0.068(1) Uani 1.00 1 d . . . C(22) C 0.1609(4) 0.5487(4) 0.1153(3) 0.0527(10) Uani 1.00 1 d . . . C(23) C 0.3320(3) 0.3561(3) 0.2217(2) 0.0446(8) Uani 1.00 1 d . . . C(24) C 0.4520(4) 0.3403(4) 0.2361(3) 0.058(1) Uani 1.00 1 d . . . C(25) C 0.4604(4) 0.2390(4) 0.2867(3) 0.063(1) Uani 1.00 1 d . . . C(26) C 0.3516(5) 0.1590(4) 0.3210(3) 0.061(1) Uani 1.00 1 d . . . C(27) C 0.2361(4) 0.1801(4) 0.3055(3) 0.0516(9) Uani 1.00 1 d . . . H(1) H -0.2616 -0.1457 0.2390 0.0576 Uiso 1.00 1 calc . . . H(2) H -0.1057 0.0927 0.5084 0.0568 Uiso 1.00 1 calc . . . H(3) H -0.2761 -0.1421 0.0724 0.0638 Uiso 1.00 1 calc . . . H(4) H -0.2662 -0.1202 -0.0951 0.0761 Uiso 1.00 1 calc . . . H(5) H -0.1126 0.0785 -0.1340 0.0728 Uiso 1.00 1 calc . . . H(6) H 0.0248 0.2547 -0.0056 0.0600 Uiso 1.00 1 calc . . . H(7) H 0.0317 0.3078 0.5805 0.0608 Uiso 1.00 1 calc . . . H(8) H 0.1802 0.5344 0.6410 0.0693 Uiso 1.00 1 calc . . . H(9) H 0.2742 0.6735 0.5307 0.0674 Uiso 1.00 1 calc . . . H(10) H 0.2321 0.5906 0.3644 0.0560 Uiso 1.00 1 calc . . . H(11) H -0.4265 -0.2588 0.3225 0.0692 Uiso 1.00 1 calc . . . H(12) H -0.3109 -0.3039 0.3407 0.0692 Uiso 1.00 1 calc . . . H(13) H -0.4698 -0.3187 0.4753 0.0818 Uiso 1.00 1 calc . . . H(14) H -0.4881 -0.4398 0.4082 0.0818 Uiso 1.00 1 calc . . . H(15) H -0.3539 -0.3635 0.4938 0.0818 Uiso 1.00 1 calc . . . H(16) H 0.4943 0.5447 0.1300 0.0743 Uiso 1.00 1 calc . . . H(17) H 0.4430 0.6986 0.0432 0.0887 Uiso 1.00 1 calc . . . H(18) H 0.2293 0.7028 0.0374 0.0809 Uiso 1.00 1 calc . . . H(19) H 0.0733 0.5497 0.1115 0.0635 Uiso 1.00 1 calc . . . H(20) H 0.5289 0.3986 0.2118 0.0691 Uiso 1.00 1 calc . . . H(21) H 0.5424 0.2252 0.2968 0.0749 Uiso 1.00 1 calc . . . H(22) H 0.3575 0.0897 0.3560 0.0730 Uiso 1.00 1 calc . . . H(23) H 0.1594 0.1240 0.3316 0.0628 Uiso 1.00 1 calc . . . H(24) H -0.1231 0.4239 0.1872 0.0627 Uiso 1.00 1 calc . . . H(25) H -0.2090 0.2835 0.1888 0.0627 Uiso 1.00 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru 0.0372(1) 0.0367(1) 0.0315(1) 0.01684(10) 0.01034(9) 0.00677(9) O(1) 0.069(2) 0.047(1) 0.045(1) 0.007(1) 0.018(1) 0.0139(10) O(1w) 0.046(1) 0.055(1) 0.079(2) 0.029(1) 0.011(1) 0.015(1) O(2) 0.094(3) 0.170(5) 0.229(7) 0.045(3) 0.092(4) 0.115(5) O(2w) 0.132(4) 0.113(3) 0.092(3) -0.003(3) 0.042(3) 0.007(3) O(3) 0.071(2) 0.091(3) 0.208(5) 0.035(2) 0.058(3) 0.005(3) O(3w) 0.17(1) 0.138(9) 0.131(8) 0.103(9) 0.004(8) -0.005(8) O(4) 0.271(8) 0.180(6) 0.38(1) 0.200(7) 0.143(8) 0.163(7) O(4w) 0.128(8) 0.126(8) 0.152(6) 0.039(7) 0.065(7) 0.024(7) O(5) 0.148(5) 0.199(8) 0.195(6) 0.089(6) 0.067(5) 0.101(6) O(5w) 0.065(4) 0.064(4) 0.103(3) 0.004(3) 0.013(4) 0.016(4) O(6) 0.139(9) 0.100(7) 0.143(7) 0.052(6) 0.016(7) 0.034(6) O(7) 0.091(5) 0.060(4) 0.148(6) 0.001(3) 0.020(5) 0.023(5) O(8) 0.067(4) 0.079(4) 0.103(3) 0.033(3) 0.032(3) 0.016(3) O(9) 0.144(9) 0.097(6) 0.098(3) 0.024(6) 0.019(5) 0.030(4) N(1) 0.043(1) 0.039(1) 0.0308(10) 0.018(1) 0.0095(9) 0.0051(8) N(2) 0.044(1) 0.044(1) 0.032(1) 0.020(1) 0.0105(9) 0.0049(9) N(3) 0.040(1) 0.042(1) 0.038(1) 0.017(1) 0.0097(9) 0.0050(9) N(4) 0.040(1) 0.045(1) 0.039(1) 0.016(1) 0.0113(10) 0.0052(10) N(5) 0.044(1) 0.045(1) 0.033(1) 0.021(1) 0.0081(9) 0.0014(10) N(6) 0.064(2) 0.100(2) 0.094(3) 0.025(2) 0.042(2) -0.017(2) N(7) 0.095(8) 0.071(6) 0.167(6) 0.035(6) -0.024(6) 0.031(6) N(8) 0.054(4) 0.062(3) 0.105(4) 0.028(3) 0.025(3) 0.025(3) C(1) 0.045(2) 0.041(1) 0.036(1) 0.017(1) 0.010(1) 0.004(1) C(2) 0.055(2) 0.039(1) 0.043(1) 0.016(1) 0.012(1) 0.005(1) C(3) 0.052(2) 0.044(2) 0.044(1) 0.014(1) 0.015(1) 0.015(1) C(4) 0.053(2) 0.049(2) 0.034(1) 0.016(1) 0.013(1) 0.009(1) C(5) 0.044(2) 0.044(1) 0.032(1) 0.018(1) 0.012(1) 0.004(1) C(6) 0.046(2) 0.040(1) 0.037(1) 0.019(1) 0.010(1) 0.006(1) C(7) 0.065(2) 0.047(2) 0.042(1) 0.020(2) 0.012(1) 0.001(1) C(8) 0.084(3) 0.065(2) 0.037(2) 0.029(2) 0.009(2) -0.003(2) C(9) 0.091(3) 0.069(2) 0.033(2) 0.043(2) 0.016(2) 0.008(1) C(10) 0.060(2) 0.063(2) 0.032(1) 0.032(2) 0.014(1) 0.015(1) C(11) 0.043(2) 0.046(1) 0.036(1) 0.020(1) 0.011(1) 0.005(1) C(12) 0.056(2) 0.059(2) 0.036(1) 0.022(2) 0.012(1) 0.001(1) C(13) 0.059(2) 0.065(2) 0.044(2) 0.022(2) 0.008(1) -0.009(1) C(14) 0.056(2) 0.050(2) 0.054(2) 0.018(2) 0.005(2) -0.005(1) C(15) 0.045(2) 0.040(1) 0.050(1) 0.016(1) 0.009(1) 0.001(1) C(16) 0.060(2) 0.046(2) 0.054(2) 0.014(2) 0.014(1) 0.012(1) C(17) 0.072(3) 0.055(2) 0.063(2) 0.007(2) 0.026(2) 0.013(2) C(18) 0.041(1) 0.047(2) 0.044(2) 0.018(1) 0.012(1) 0.004(1) C(19) 0.047(2) 0.067(2) 0.070(2) 0.016(2) 0.026(2) 0.014(2) C(20) 0.060(2) 0.074(3) 0.088(3) 0.019(2) 0.037(2) 0.035(2) C(21) 0.064(2) 0.068(2) 0.073(3) 0.025(2) 0.026(2) 0.036(2) C(22) 0.054(2) 0.055(2) 0.056(2) 0.028(2) 0.018(2) 0.020(1) C(23) 0.042(1) 0.046(2) 0.041(2) 0.017(1) 0.007(1) -0.002(1) C(24) 0.039(2) 0.065(2) 0.066(2) 0.022(2) 0.009(2) -0.004(2) C(25) 0.057(2) 0.073(2) 0.062(2) 0.043(2) -0.004(1) -0.011(2) C(26) 0.069(2) 0.068(2) 0.057(2) 0.047(2) 0.003(2) 0.006(2) C(27) 0.061(2) 0.054(2) 0.045(2) 0.033(2) 0.008(1) 0.009(1) #------------------------------------------------------------------------------ _computing_data_collection 'RAPID-AUTO Ver. 1.06' _computing_cell_refinement 'RAPID-AUTO Ver. 1.06' _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 2.0' _computing_publication_material 'teXsan Ver. 2.0' _computing_molecular_graphics ? #------------------------------------------------------------------------------ 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 O(1w) 2.135(3) . . yes Ru N(1) 1.974(3) . . yes Ru N(2) 2.075(3) . . yes Ru N(3) 2.078(3) . . yes Ru N(4) 2.082(3) . . yes Ru N(5) 2.019(3) . . yes O(1) C(3) 1.352(4) . . yes O(1) C(16) 1.442(5) . . yes O(1w) H(24) 0.842 . . no O(1w) H(25) 0.991 . . no O(2) N(6) 1.166(7) . . yes O(3) N(6) 1.237(6) . . yes O(4) N(6) 1.152(7) . . yes O(5) N(7) 1.33(2) . . yes O(5) N(7) 1.42(1) . 2_656 yes O(6) N(7) 1.20(2) . . yes O(7) N(8) 1.26(1) . . yes O(8) N(8) 1.19(1) . . yes O(9) N(8) 1.24(1) . . yes N(1) C(1) 1.348(4) . . yes N(1) C(5) 1.360(4) . . yes N(2) C(6) 1.361(5) . . yes N(2) C(10) 1.355(4) . . yes N(3) C(11) 1.367(4) . . yes N(3) C(15) 1.344(4) . . yes N(4) C(18) 1.357(5) . . yes N(4) C(22) 1.339(5) . . yes N(5) C(23) 1.358(5) . . yes N(5) C(27) 1.342(5) . . yes N(7) N(7) 1.68(3) . 2_656 yes C(1) C(2) 1.372(5) . . yes C(1) C(6) 1.485(5) . . yes C(2) C(3) 1.397(5) . . yes C(2) H(1) 0.955 . . no C(3) C(4) 1.396(5) . . yes C(4) C(5) 1.378(5) . . yes C(4) H(2) 0.953 . . no C(5) C(11) 1.494(5) . . yes C(6) C(7) 1.381(5) . . yes C(7) C(8) 1.392(6) . . yes C(7) H(3) 0.967 . . no C(8) C(9) 1.370(7) . . yes C(8) H(4) 0.956 . . no C(9) C(10) 1.379(6) . . yes C(9) H(5) 0.961 . . no C(10) H(6) 0.962 . . no C(11) C(12) 1.373(5) . . yes C(12) C(13) 1.397(6) . . yes C(12) H(7) 0.969 . . no C(13) C(14) 1.371(7) . . yes C(13) H(8) 0.953 . . no C(14) C(15) 1.365(6) . . yes C(14) H(9) 0.954 . . no C(15) H(10) 0.965 . . no C(16) C(17) 1.497(6) . . yes C(16) H(11) 0.962 . . no C(16) H(12) 0.953 . . no C(17) H(13) 0.953 . . no C(17) H(14) 0.952 . . no C(17) H(15) 0.954 . . no C(18) C(19) 1.386(6) . . yes C(18) C(23) 1.483(5) . . yes C(19) C(20) 1.377(7) . . yes C(19) H(16) 0.957 . . no C(20) C(21) 1.379(7) . . yes C(20) H(17) 0.964 . . no C(21) C(22) 1.391(6) . . yes C(21) H(18) 0.960 . . no C(22) H(19) 0.967 . . no C(23) C(24) 1.391(5) . . yes C(24) C(25) 1.395(7) . . yes C(24) H(20) 0.970 . . no C(25) C(26) 1.361(7) . . yes C(25) H(21) 0.970 . . no C(26) C(27) 1.375(6) . . yes C(26) H(22) 0.959 . . no C(27) H(23) 0.974 . . 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 O(1w) Ru N(1) 87.9(1) . . . yes O(1w) Ru N(2) 87.4(1) . . . yes O(1w) Ru N(3) 89.6(1) . . . yes O(1w) Ru N(4) 97.7(1) . . . yes O(1w) Ru N(5) 176.7(1) . . . yes N(1) Ru N(2) 79.3(1) . . . yes N(1) Ru N(3) 79.4(1) . . . yes N(1) Ru N(4) 174.3(1) . . . yes N(1) Ru N(5) 95.1(1) . . . yes N(2) Ru N(3) 158.6(1) . . . yes N(2) Ru N(4) 99.8(1) . . . yes N(2) Ru N(5) 91.7(1) . . . yes N(3) Ru N(4) 101.6(1) . . . yes N(3) Ru N(5) 92.5(1) . . . yes N(4) Ru N(5) 79.3(1) . . . yes C(3) O(1) C(16) 117.9(3) . . . yes Ru O(1w) H(24) 133.2 . . . no Ru O(1w) H(25) 119.0 . . . no H(24) O(1w) H(25) 106.9 . . . no Ru N(1) C(1) 119.2(2) . . . yes Ru N(1) C(5) 119.4(2) . . . yes C(1) N(1) C(5) 121.3(3) . . . yes Ru N(2) C(6) 113.5(2) . . . yes Ru N(2) C(10) 127.3(3) . . . yes C(6) N(2) C(10) 119.1(3) . . . yes Ru N(3) C(11) 113.7(2) . . . yes Ru N(3) C(15) 127.8(3) . . . yes C(11) N(3) C(15) 118.5(3) . . . yes Ru N(4) C(18) 114.9(2) . . . yes Ru N(4) C(22) 127.3(3) . . . yes C(18) N(4) C(22) 117.8(3) . . . yes Ru N(5) C(23) 116.4(2) . . . yes Ru N(5) C(27) 125.4(3) . . . yes C(23) N(5) C(27) 118.2(3) . . . yes O(2) N(6) O(3) 116.7(7) . . . yes O(2) N(6) O(4) 116.0(7) . . . yes O(3) N(6) O(4) 127.1(7) . . . yes O(5) N(7) O(5) 104(1) . . 2_656 yes O(5) N(7) O(6) 123(1) . . . yes O(5) N(7) O(6) 130(1) 2_656 . . yes O(7) N(8) O(8) 121(1) . . . yes O(7) N(8) O(9) 117(1) . . . yes O(8) N(8) O(9) 120(1) . . . yes N(1) C(1) C(2) 121.1(3) . . . yes N(1) C(1) C(6) 112.3(3) . . . yes C(2) C(1) C(6) 126.5(3) . . . yes C(1) C(2) C(3) 118.2(3) . . . yes C(1) C(2) H(1) 121.0 . . . no C(3) C(2) H(1) 120.8 . . . no O(1) C(3) C(2) 123.4(4) . . . yes O(1) C(3) C(4) 116.1(3) . . . yes C(2) C(3) C(4) 120.5(3) . . . yes C(3) C(4) C(5) 118.5(3) . . . yes C(3) C(4) H(2) 120.6 . . . no C(5) C(4) H(2) 120.9 . . . no N(1) C(5) C(4) 120.3(3) . . . yes N(1) C(5) C(11) 112.0(3) . . . yes C(4) C(5) C(11) 127.7(3) . . . yes N(2) C(6) C(1) 115.5(3) . . . yes N(2) C(6) C(7) 121.2(3) . . . yes C(1) C(6) C(7) 123.3(3) . . . yes C(6) C(7) C(8) 118.8(4) . . . yes C(6) C(7) H(3) 120.4 . . . no C(8) C(7) H(3) 120.8 . . . no C(7) C(8) C(9) 120.1(4) . . . yes C(7) C(8) H(4) 119.5 . . . no C(9) C(8) H(4) 120.3 . . . no C(8) C(9) C(10) 118.9(4) . . . yes C(8) C(9) H(5) 120.8 . . . no C(10) C(9) H(5) 120.2 . . . no N(2) C(10) C(9) 121.8(4) . . . yes N(2) C(10) H(6) 118.8 . . . no C(9) C(10) H(6) 119.3 . . . no N(3) C(11) C(5) 115.4(3) . . . yes N(3) C(11) C(12) 121.4(4) . . . yes C(5) C(11) C(12) 123.2(3) . . . yes C(11) C(12) C(13) 119.0(4) . . . yes C(11) C(12) H(7) 119.7 . . . no C(13) C(12) H(7) 121.3 . . . no C(12) C(13) C(14) 119.0(4) . . . yes C(12) C(13) H(8) 120.6 . . . no C(14) C(13) H(8) 120.4 . . . no C(13) C(14) C(15) 119.6(4) . . . yes C(13) C(14) H(9) 119.2 . . . no C(15) C(14) H(9) 121.1 . . . no N(3) C(15) C(14) 122.4(4) . . . yes N(3) C(15) H(10) 118.9 . . . no C(14) C(15) H(10) 118.7 . . . no O(1) C(16) C(17) 107.8(3) . . . yes O(1) C(16) H(11) 110.6 . . . no O(1) C(16) H(12) 110.5 . . . no C(17) C(16) H(11) 109.6 . . . no C(17) C(16) H(12) 110.2 . . . no H(11) C(16) H(12) 108.2 . . . no C(16) C(17) H(13) 109.9 . . . no C(16) C(17) H(14) 110.5 . . . no C(16) C(17) H(15) 109.5 . . . no H(13) C(17) H(14) 109.0 . . . no H(13) C(17) H(15) 108.9 . . . no H(14) C(17) H(15) 109.0 . . . no N(4) C(18) C(19) 122.4(4) . . . yes N(4) C(18) C(23) 114.2(3) . . . yes C(19) C(18) C(23) 123.4(4) . . . yes C(18) C(19) C(20) 118.8(4) . . . yes C(18) C(19) H(16) 120.0 . . . no C(20) C(19) H(16) 121.2 . . . no C(19) C(20) C(21) 119.6(4) . . . yes C(19) C(20) H(17) 119.8 . . . no C(21) C(20) H(17) 120.6 . . . no C(20) C(21) C(22) 118.6(4) . . . yes C(20) C(21) H(18) 121.9 . . . no C(22) C(21) H(18) 119.5 . . . no N(4) C(22) C(21) 122.8(4) . . . yes N(4) C(22) H(19) 118.6 . . . no C(21) C(22) H(19) 118.6 . . . no N(5) C(23) C(18) 115.2(3) . . . yes N(5) C(23) C(24) 121.4(4) . . . yes C(18) C(23) C(24) 123.4(4) . . . yes C(23) C(24) C(25) 118.9(4) . . . yes C(23) C(24) H(20) 120.9 . . . no C(25) C(24) H(20) 120.3 . . . no C(24) C(25) C(26) 119.3(4) . . . yes C(24) C(25) H(21) 120.4 . . . no C(26) C(25) H(21) 120.3 . . . no C(25) C(26) C(27) 119.3(4) . . . yes C(25) C(26) H(22) 119.3 . . . no C(27) C(26) H(22) 121.4 . . . no N(5) C(27) C(26) 123.0(4) . . . yes N(5) C(27) H(23) 117.9 . . . no C(26) C(27) H(23) 119.1 . . . no #------------------------------------------------------------------------------ # END of CIF #------------------------------------------------------------------------------