Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Hirano, Toshiyuki' 'Mai Kuroda' 'Naoko Takeda' 'Mitsunori Hayashi' 'Mukaida, Masao' 'Oi, Takao' 'Nagao, Hirotaka' _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Dr Hirotaka Nagao' _publ_contact_author_address ; Department of Chemistry, Faculty of Science and Technology, Sophia University, Kioi-cho 7-1, Chiyoda-ku, Tokyo 102-8554, Japan ; _publ_contact_author_email 'h-nagao@sophia.ac.jp' _publ_contact_author_fax '81-3-3238-3361' _publ_contact_author_phone '81-3-3238-3448' _publ_section_title ; Cis-Trans Isomerization of {RuNO}6-type Nitrosylruthenium Complexes Containing 2-Pyridinecarboxylate and Structural Characterization of m-H3O2 Bridged Dinuclear Nitrosylruthenium Complex ; data_[{Ru(NO)(pyca)2}2(H3O2)]PF6_2H2O _database_code_CSD 177496 #------------------------------------------------------------------------------ _chemical_formula_sum 'C24 H23 F6 N6 O14 P Ru2 ' _chemical_formula_weight 966.58 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _cell_length_a 11.7164(2) _cell_length_b 13.5928(2) _cell_length_c 21.0368(4) _cell_angle_alpha 90 _cell_angle_beta 99.750(1) _cell_angle_gamma 90 _cell_volume 3301.88(9) _cell_formula_units_Z 4 #------------------------------------------------------------------------------ _exptl_crystal_density_diffrn 1.944 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 12786 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.4 _diffrn_ambient_temperature 123.2 #------------------------------------------------------------------------------ _exptl_absorpt_coefficient_mu 1.074 _exptl_crystal_description 'chip' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_colour 'yellow' _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_T_max 0.936 _diffrn_radiation_monochromator 'graphite' _diffrn_reflns_number 28439 _reflns_number_total 7559 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0364 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_number_reflns 5535 _refine_ls_number_parameters 478 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max 0.0007 _refine_diff_density_max 0.58 _refine_diff_density_min -0.96 #------------------------------------------------------------------------------ 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 0.68883(2) -0.11694(2) 0.38917(1) 0.01284(6) Uani 1.00 d . . . Ru(2) Ru 0.81256(2) 0.08701(2) 0.61922(1) 0.01314(6) Uani 1.00 d . . . P P 1.01566(7) -0.01447(7) 0.84452(4) 0.0202(2) Uani 1.00 d . . . F(1) F 1.1454(2) -0.0539(3) 0.8566(1) 0.0642(9) Uani 1.00 d . . . F(2) F 1.0108(2) -0.0242(2) 0.76812(9) 0.0295(6) Uani 1.00 d . . . F(3) F 0.8878(2) 0.0250(3) 0.8326(2) 0.092(1) Uani 1.00 d . . . F(4) F 1.0229(2) -0.0046(2) 0.9210(1) 0.0363(6) Uani 1.00 d . . . F(5) F 1.0649(3) 0.0934(2) 0.8429(1) 0.0703(10) Uani 1.00 d . . . F(6) F 0.9703(3) -0.1233(2) 0.8465(1) 0.077(1) Uani 1.00 d . . . O(1) O 0.5403(2) -0.2073(2) 0.2814(1) 0.0323(7) Uani 1.00 d . . . O(2) O 0.7915(2) -0.0488(2) 0.4612(1) 0.0161(5) Uani 1.00 d . . . O(3) O 0.5594(2) -0.0449(2) 0.4223(1) 0.0156(5) Uani 1.00 d . . . O(4) O 0.4634(2) 0.0972(2) 0.4167(1) 0.0207(6) Uani 1.00 d . . . O(5) O 0.8322(2) -0.1837(2) 0.3662(1) 0.0196(6) Uani 1.00 d . . . O(6) O 0.9509(2) -0.3109(2) 0.3903(1) 0.0310(7) Uani 1.00 d . . . O(7) O 0.9696(2) 0.1831(2) 0.7216(1) 0.0274(6) Uani 1.00 d . . . O(8) O 0.7049(2) 0.0287(2) 0.5454(1) 0.0160(5) Uani 1.00 d . . . O(9) O 0.6793(2) 0.0922(2) 0.6704(1) 0.0189(6) Uani 1.00 d . . . O(10) O 0.5890(2) 0.0053(2) 0.7364(1) 0.0305(7) Uani 1.00 d . . . O(11) O 0.9345(2) 0.0736(2) 0.5616(1) 0.0153(5) Uani 1.00 d . . . O(12) O 1.0120(2) 0.1509(2) 0.4861(1) 0.0191(6) Uani 1.00 d . . . O(13) O 0.5446(3) -0.0071(3) 0.8631(2) 0.056(1) Uani 1.00 d . . . O(14) O 0.3444(4) 0.0995(4) 0.8287(2) 0.087(2) Uani 1.00 d . . . N(1) N 0.5979(2) -0.1715(2) 0.3249(1) 0.0176(6) Uani 1.00 d . . . N(2) N 0.6949(2) 0.0154(2) 0.3418(1) 0.0168(6) Uani 1.00 d . . . N(3) N 0.6991(2) -0.2369(2) 0.4496(1) 0.0171(6) Uani 1.00 d . . . N(4) N 0.9087(2) 0.1427(2) 0.6811(1) 0.0162(6) Uani 1.00 d . . . N(5) N 0.8236(2) -0.0525(2) 0.6575(1) 0.0170(6) Uani 1.00 d . . . N(6) N 0.7811(2) 0.2146(2) 0.5663(1) 0.0160(6) Uani 1.00 d . . . C(1) C 0.6209(2) 0.0827(3) 0.3587(1) 0.0174(7) Uani 1.00 d . . . C(2) C 0.6192(3) 0.1779(3) 0.3360(2) 0.0243(9) Uani 1.00 d . . . C(3) C 0.6953(3) 0.2040(3) 0.2949(2) 0.0297(10) Uani 1.00 d . . . C(4) C 0.7700(3) 0.1339(3) 0.2777(2) 0.0302(10) Uani 1.00 d . . . C(5) C 0.7686(3) 0.0394(3) 0.3022(2) 0.0245(9) Uani 1.00 d . . . C(6) C 0.5418(2) 0.0452(2) 0.4027(1) 0.0154(7) Uani 1.00 d . . . C(7) C 0.7936(3) -0.2935(3) 0.4480(2) 0.0219(8) Uani 1.00 d . . . C(8) C 0.8228(3) -0.3692(3) 0.4917(2) 0.0285(9) Uani 1.00 d . . . C(9) C 0.7523(3) -0.3866(3) 0.5373(2) 0.0323(10) Uani 1.00 d . . . C(10) C 0.6556(3) -0.3287(3) 0.5380(2) 0.0282(9) Uani 1.00 d . . . C(11) C 0.6308(3) -0.2530(3) 0.4932(2) 0.0218(8) Uani 1.00 d . . . C(12) C 0.8658(3) -0.2633(3) 0.3980(2) 0.0222(8) Uani 1.00 d . . . C(13) C 0.7429(3) -0.0718(3) 0.6941(2) 0.0204(8) Uani 1.00 d . . . C(14) C 0.7306(3) -0.1652(3) 0.7185(2) 0.0290(9) Uani 1.00 d . . . C(15) C 0.8019(3) -0.2394(3) 0.7035(2) 0.0329(10) Uani 1.00 d . . . C(16) C 0.8835(3) -0.2189(3) 0.6646(2) 0.0267(9) Uani 1.00 d . . . C(17) C 0.8941(3) -0.1241(3) 0.6425(2) 0.0205(8) Uani 1.00 d . . . C(18) C 0.6640(3) 0.0132(3) 0.7026(2) 0.0208(8) Uani 1.00 d . . . C(19) C 0.8459(2) 0.2217(2) 0.5193(1) 0.0169(7) Uani 1.00 d . . . C(20) C 0.8286(3) 0.2964(3) 0.4738(2) 0.0219(8) Uani 1.00 d . . . C(21) C 0.7429(3) 0.3654(3) 0.4775(2) 0.0234(8) Uani 1.00 d . . . C(22) C 0.6765(3) 0.3570(3) 0.5263(2) 0.0245(9) Uani 1.00 d . . . C(23) C 0.6977(3) 0.2812(3) 0.5701(2) 0.0209(8) Uani 1.00 d . . . C(24) C 0.9376(2) 0.1443(2) 0.5208(1) 0.0151(7) Uani 1.00 d . . . H(1) H 0.7554 -0.0323 0.4930 0.0211 Uiso 1.00 calc . . . H(2) H 0.8561 -0.0806 0.4738 0.0211 Uiso 1.00 calc . . . H(3) H 0.5591 0.2254 0.3492 0.0211 Uiso 1.00 calc . . . H(4) H 0.6881 0.2758 0.2725 0.0211 Uiso 1.00 calc . . . H(5) H 0.8276 0.1456 0.2462 0.0211 Uiso 1.00 calc . . . H(6) H 0.8283 -0.0129 0.2939 0.0211 Uiso 1.00 calc . . . H(7) H 0.8962 -0.4013 0.4860 0.0211 Uiso 1.00 calc . . . H(8) H 0.7750 -0.4417 0.5663 0.0211 Uiso 1.00 calc . . . H(9) H 0.6060 -0.3358 0.5721 0.0211 Uiso 1.00 calc . . . H(10) H 0.5543 -0.2159 0.4936 0.0211 Uiso 1.00 calc . . . H(11) H 0.6355 -0.0116 0.5533 0.0211 Uiso 1.00 calc . . . H(12) H 0.6687 -0.1718 0.7474 0.0211 Uiso 1.00 calc . . . H(13) H 0.8023 -0.3046 0.7195 0.0211 Uiso 1.00 calc . . . H(14) H 0.9353 -0.2671 0.6526 0.0211 Uiso 1.00 calc . . . H(15) H 0.9415 -0.1066 0.6131 0.0211 Uiso 1.00 calc . . . H(16) H 0.8730 0.2925 0.4368 0.0211 Uiso 1.00 calc . . . H(17) H 0.7166 0.4162 0.4442 0.0211 Uiso 1.00 calc . . . H(18) H 0.6122 0.4041 0.5312 0.0211 Uiso 1.00 calc . . . H(19) H 0.6547 0.2651 0.6073 0.0211 Uiso 1.00 calc . . . H(20) H 0.4716 0.0431 0.8550 0.0211 Uiso 1.00 calc . . . H(21) H 0.5097 -0.0732 0.8737 0.0211 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) 0.0109(1) 0.0147(1) 0.0130(1) -0.00015(9) 0.00210(8) -0.00227(9) Ru(2) 0.0112(1) 0.0154(1) 0.0127(1) 0.00034(9) 0.00153(8) -0.00203(9) P 0.0200(4) 0.0199(4) 0.0214(4) -0.0036(3) 0.0050(3) -0.0034(3) F(1) 0.042(1) 0.117(3) 0.031(1) 0.038(2) -0.002(1) -0.004(2) F(2) 0.029(1) 0.039(1) 0.0187(10) -0.0028(10) 0.0001(8) -0.0015(9) F(3) 0.034(1) 0.172(4) 0.063(2) 0.045(2) -0.012(1) -0.066(2) F(4) 0.045(1) 0.042(1) 0.024(1) -0.013(1) 0.0130(9) -0.009(1) F(5) 0.134(3) 0.033(2) 0.033(1) -0.044(2) -0.017(2) 0.008(1) F(6) 0.145(3) 0.048(2) 0.047(2) -0.060(2) 0.040(2) -0.016(1) O(1) 0.031(1) 0.035(2) 0.026(1) -0.003(1) -0.007(1) -0.012(1) O(2) 0.0118(9) 0.019(1) 0.018(1) 0.0016(8) 0.0034(8) -0.0039(9) O(3) 0.0122(9) 0.018(1) 0.017(1) 0.0024(8) 0.0037(8) -0.0002(9) O(4) 0.015(1) 0.024(1) 0.024(1) 0.0051(9) 0.0058(9) -0.0009(10) O(5) 0.018(1) 0.020(1) 0.022(1) 0.0016(9) 0.0062(9) -0.0049(10) O(6) 0.024(1) 0.032(2) 0.037(1) 0.011(1) 0.003(1) -0.010(1) O(7) 0.030(1) 0.027(1) 0.022(1) -0.007(1) -0.0046(10) -0.003(1) O(8) 0.0119(9) 0.020(1) 0.017(1) -0.0003(9) 0.0035(8) -0.0020(9) O(9) 0.018(1) 0.022(1) 0.017(1) -0.0004(9) 0.0054(8) -0.0021(9) O(10) 0.025(1) 0.044(2) 0.026(1) -0.002(1) 0.0121(10) 0.004(1) O(11) 0.0115(9) 0.016(1) 0.019(1) 0.0003(8) 0.0029(8) -0.0021(9) O(12) 0.017(1) 0.023(1) 0.019(1) 0.0016(9) 0.0066(8) 0.0010(9) O(13) 0.065(2) 0.062(2) 0.041(2) -0.034(2) 0.011(2) 0.002(2) O(14) 0.094(3) 0.074(3) 0.100(4) 0.006(3) 0.038(3) -0.005(3) N(1) 0.015(1) 0.017(1) 0.020(1) 0.001(1) 0.0030(10) -0.002(1) N(2) 0.015(1) 0.020(1) 0.016(1) -0.001(1) 0.0044(10) -0.003(1) N(3) 0.018(1) 0.014(1) 0.018(1) -0.002(1) 0.0008(10) -0.002(1) N(4) 0.017(1) 0.016(1) 0.016(1) 0.000(1) 0.0022(10) -0.002(1) N(5) 0.017(1) 0.020(1) 0.012(1) 0.000(1) -0.0015(9) -0.001(1) N(6) 0.012(1) 0.017(1) 0.018(1) 0.0007(10) -0.0008(9) -0.004(1) C(1) 0.011(1) 0.023(2) 0.018(1) 0.001(1) 0.001(1) -0.001(1) C(2) 0.023(2) 0.020(2) 0.030(2) 0.004(1) 0.005(1) 0.003(1) C(3) 0.030(2) 0.024(2) 0.037(2) 0.001(1) 0.009(2) 0.010(2) C(4) 0.029(2) 0.031(2) 0.034(2) -0.001(2) 0.016(2) 0.009(2) C(5) 0.023(2) 0.030(2) 0.022(2) 0.001(1) 0.011(1) 0.000(1) C(6) 0.011(1) 0.019(2) 0.015(1) -0.001(1) 0.000(1) -0.003(1) C(7) 0.020(2) 0.017(2) 0.026(2) 0.000(1) -0.003(1) -0.006(1) C(8) 0.028(2) 0.016(2) 0.038(2) -0.001(1) -0.005(1) -0.003(2) C(9) 0.043(2) 0.014(2) 0.034(2) -0.004(2) -0.011(2) 0.005(2) C(10) 0.037(2) 0.022(2) 0.025(2) -0.011(2) 0.002(1) 0.004(1) C(11) 0.024(2) 0.019(2) 0.022(2) -0.006(1) 0.004(1) 0.001(1) C(12) 0.017(1) 0.025(2) 0.023(2) -0.001(1) -0.001(1) -0.008(1) C(13) 0.021(1) 0.024(2) 0.015(1) -0.004(1) 0.000(1) 0.002(1) C(14) 0.026(2) 0.031(2) 0.028(2) -0.004(2) 0.001(1) 0.010(2) C(15) 0.038(2) 0.024(2) 0.033(2) -0.002(2) -0.005(2) 0.009(2) C(16) 0.034(2) 0.022(2) 0.021(2) 0.008(1) -0.005(1) 0.001(1) C(17) 0.024(2) 0.020(2) 0.016(1) 0.001(1) -0.001(1) 0.000(1) C(18) 0.015(1) 0.029(2) 0.017(1) -0.002(1) 0.000(1) -0.001(1) C(19) 0.013(1) 0.019(2) 0.019(1) 0.000(1) 0.003(1) -0.003(1) C(20) 0.022(2) 0.027(2) 0.018(2) 0.004(1) 0.004(1) 0.001(1) C(21) 0.025(2) 0.019(2) 0.025(2) 0.007(1) 0.001(1) 0.005(1) C(22) 0.021(2) 0.021(2) 0.030(2) 0.007(1) 0.000(1) -0.001(1) C(23) 0.017(1) 0.022(2) 0.025(2) 0.003(1) 0.006(1) -0.003(1) C(24) 0.011(1) 0.016(2) 0.017(1) 0.000(1) -0.001(1) -0.004(1) #------------------------------------------------------------------------------ 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(2) 1.995(2) . . yes Ru(1) O(3) 2.026(2) . . yes Ru(1) O(5) 2.038(2) . . yes Ru(1) N(1) 1.739(3) . . yes Ru(1) N(2) 2.064(3) . . yes Ru(1) N(3) 2.058(3) . . yes Ru(2) O(8) 1.992(2) . . yes Ru(2) O(9) 2.042(2) . . yes Ru(2) O(11) 2.032(2) . . yes Ru(2) N(4) 1.744(3) . . yes Ru(2) N(5) 2.056(3) . . yes Ru(2) N(6) 2.060(3) . . yes P F(1) 1.591(3) . . no P F(2) 1.604(2) . . no P F(3) 1.570(3) . . no P F(4) 1.603(2) . . no P F(5) 1.579(3) . . no P F(6) 1.575(3) . . no O(1) N(1) 1.150(3) . . yes O(2) O(8) 2.427(3) . . yes O(3) C(6) 1.297(4) . . no O(4) C(6) 1.233(4) . . no O(5) C(12) 1.299(4) . . no O(6) C(12) 1.222(4) . . no O(7) N(4) 1.153(3) . . yes O(9) C(18) 1.298(4) . . no O(10) C(18) 1.225(4) . . no O(11) C(24) 1.293(4) . . no O(12) C(24) 1.232(4) . . no N(2) C(1) 1.349(4) . . no N(2) C(5) 1.337(4) . . no N(3) C(7) 1.354(4) . . no N(3) C(11) 1.333(4) . . no N(5) C(13) 1.343(4) . . no N(5) C(17) 1.347(4) . . no N(6) C(19) 1.348(4) . . no N(6) C(23) 1.344(4) . . no C(1) C(2) 1.378(5) . . no C(1) C(6) 1.506(4) . . no C(2) C(3) 1.388(5) . . no C(3) C(4) 1.383(5) . . no C(4) C(5) 1.385(5) . . no C(7) C(8) 1.383(5) . . no C(7) C(12) 1.512(5) . . no C(8) C(9) 1.388(6) . . no C(9) C(10) 1.381(6) . . no C(10) C(11) 1.393(5) . . no C(13) C(14) 1.385(5) . . no C(13) C(18) 1.510(5) . . no C(14) C(15) 1.380(6) . . no C(15) C(16) 1.388(6) . . no C(16) C(17) 1.383(5) . . no C(19) C(20) 1.386(5) . . no C(19) C(24) 1.500(4) . . no C(20) C(21) 1.385(5) . . no C(21) C(22) 1.394(5) . . no C(22) C(23) 1.378(5) . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(2) Ru(1) O(3) 84.52(8) . . . no O(2) Ru(1) O(5) 88.38(9) . . . no O(2) Ru(1) N(1) 177.6(1) . . . no O(2) Ru(1) N(2) 84.06(10) . . . no O(2) Ru(1) N(3) 86.21(10) . . . no O(3) Ru(1) O(5) 172.78(9) . . . no O(3) Ru(1) N(1) 94.5(1) . . . no O(3) Ru(1) N(2) 80.42(9) . . . no O(3) Ru(1) N(3) 98.00(10) . . . no O(5) Ru(1) N(1) 92.7(1) . . . no O(5) Ru(1) N(2) 100.14(10) . . . no O(5) Ru(1) N(3) 80.2(1) . . . no N(1) Ru(1) N(2) 93.6(1) . . . no N(1) Ru(1) N(3) 96.1(1) . . . no N(2) Ru(1) N(3) 170.2(1) . . . no O(8) Ru(2) O(9) 89.12(9) . . . no O(8) Ru(2) O(11) 85.18(8) . . . no O(8) Ru(2) N(4) 177.0(1) . . . no O(8) Ru(2) N(5) 85.85(9) . . . no O(8) Ru(2) N(6) 83.20(9) . . . no O(9) Ru(2) O(11) 174.21(8) . . . no O(9) Ru(2) N(4) 92.7(1) . . . no O(9) Ru(2) N(5) 80.15(10) . . . no O(9) Ru(2) N(6) 99.95(10) . . . no O(11) Ru(2) N(4) 93.1(1) . . . no O(11) Ru(2) N(5) 98.42(10) . . . no O(11) Ru(2) N(6) 80.37(10) . . . no N(4) Ru(2) N(5) 96.8(1) . . . no N(4) Ru(2) N(6) 94.1(1) . . . no N(5) Ru(2) N(6) 169.05(9) . . . no F(1) P F(2) 90.2(1) . . . no F(1) P F(3) 179.7(2) . . . no F(1) P F(4) 88.9(1) . . . no F(1) P F(5) 88.5(2) . . . no F(1) P F(6) 89.8(2) . . . no F(2) P F(3) 89.8(1) . . . no F(2) P F(4) 179.0(1) . . . no F(2) P F(5) 90.4(1) . . . no F(2) P F(6) 89.6(1) . . . no F(3) P F(4) 91.1(2) . . . no F(3) P F(5) 91.2(2) . . . no F(3) P F(6) 90.5(2) . . . no F(4) P F(5) 89.2(1) . . . no F(4) P F(6) 90.8(1) . . . no F(5) P F(6) 178.3(2) . . . no Ru(1) O(2) O(8) 118.9(1) . . . no Ru(1) O(3) C(6) 115.8(2) . . . no Ru(1) O(5) C(12) 116.0(2) . . . no Ru(2) O(8) O(2) 117.0(1) . . . no Ru(2) O(9) C(18) 115.6(2) . . . no Ru(2) O(11) C(24) 115.5(2) . . . no Ru(1) N(1) O(1) 178.0(3) . . . yes Ru(1) N(2) C(1) 112.8(2) . . . no Ru(1) N(2) C(5) 126.2(2) . . . no C(1) N(2) C(5) 120.7(3) . . . no Ru(1) N(3) C(7) 113.4(2) . . . no Ru(1) N(3) C(11) 125.2(2) . . . no C(7) N(3) C(11) 120.8(3) . . . no Ru(2) N(4) O(7) 177.1(3) . . . yes Ru(2) N(5) C(13) 113.6(2) . . . no Ru(2) N(5) C(17) 125.1(2) . . . no C(13) N(5) C(17) 120.8(3) . . . no Ru(2) N(6) C(19) 112.7(2) . . . no Ru(2) N(6) C(23) 126.8(2) . . . no C(19) N(6) C(23) 120.1(3) . . . no N(2) C(1) C(2) 121.1(3) . . . no N(2) C(1) C(6) 115.0(3) . . . no C(2) C(1) C(6) 123.9(3) . . . no C(1) C(2) C(3) 118.9(3) . . . no C(2) C(3) C(4) 119.3(3) . . . no C(3) C(4) C(5) 119.6(3) . . . no N(2) C(5) C(4) 120.4(3) . . . no O(3) C(6) O(4) 123.4(3) . . . no O(3) C(6) C(1) 115.7(3) . . . no O(4) C(6) C(1) 120.9(3) . . . no N(3) C(7) C(8) 121.1(3) . . . no N(3) C(7) C(12) 114.8(3) . . . no C(8) C(7) C(12) 124.0(3) . . . no C(7) C(8) C(9) 118.5(3) . . . no C(8) C(9) C(10) 119.7(3) . . . no C(9) C(10) C(11) 119.4(3) . . . no N(3) C(11) C(10) 120.5(3) . . . no O(5) C(12) O(6) 123.7(3) . . . no O(5) C(12) C(7) 115.4(3) . . . no O(6) C(12) C(7) 120.9(3) . . . no N(5) C(13) C(14) 121.2(3) . . . no N(5) C(13) C(18) 115.1(3) . . . no C(14) C(13) C(18) 123.6(3) . . . no C(13) C(14) C(15) 118.7(3) . . . no C(14) C(15) C(16) 119.5(3) . . . no C(15) C(16) C(17) 119.6(3) . . . no N(5) C(17) C(16) 120.1(3) . . . no O(9) C(18) O(10) 123.5(3) . . . no O(9) C(18) C(13) 115.4(3) . . . no O(10) C(18) C(13) 121.0(3) . . . no N(6) C(19) C(20) 121.6(3) . . . no N(6) C(19) C(24) 115.1(3) . . . no C(20) C(19) C(24) 123.3(3) . . . no C(19) C(20) C(21) 118.6(3) . . . no C(20) C(21) C(22) 119.1(3) . . . no C(21) C(22) C(23) 119.6(3) . . . no N(6) C(23) C(22) 120.9(3) . . . no O(11) C(24) O(12) 123.3(3) . . . no O(11) C(24) C(19) 115.8(3) . . . no O(12) C(24) C(19) 120.9(3) . . . no #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_[Ru(NO)(OCH3)(pyca)2]CH3OH _database_code_CSD 177497 #------------------------------------------------------------------------------ _chemical_formula_sum 'C14 H15 N3 O7 Ru ' _chemical_formula_weight 438.36 #------------------------------------------------------------------------------ _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 8.120(1) _cell_length_b 15.082(3) _cell_length_c 7.009(1) _cell_angle_alpha 91.963(7) _cell_angle_beta 103.913(6) _cell_angle_gamma 97.687(10) _cell_volume 823.8(2) _cell_formula_units_Z 2 #------------------------------------------------------------------------------ _exptl_crystal_density_diffrn 1.767 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 5677 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 173.2 #------------------------------------------------------------------------------ _exptl_absorpt_coefficient_mu 0.995 _exptl_crystal_description 'block' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.170 _exptl_crystal_colour 'orange' _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 0.844 _diffrn_radiation_monochromator 'graphite' _diffrn_reflns_number 6734 _reflns_number_total 3510 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0729 _refine_ls_goodness_of_fit_ref 1.444 _refine_ls_number_reflns 3374 _refine_ls_number_parameters 226 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00250|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max 0.0014 _refine_diff_density_max 0.46 _refine_diff_density_min -1.39 #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.29685(2) 0.27003(1) 0.94876(3) 0.0160(1) Uani 1.00 d . . . O(1) O 0.2284(4) 0.3401(2) 0.5621(3) 0.0388(7) Uani 1.00 d . . . O(2) O 0.3344(3) 0.2174(2) 1.2053(4) 0.0236(6) Uani 1.00 d . . . O(3) O 0.5237(3) 0.3504(2) 1.0651(4) 0.0195(5) Uani 1.00 d . . . O(4) O 0.6322(3) 0.4826(2) 1.2276(4) 0.0277(6) Uani 1.00 d . . . O(5) O 0.0721(3) 0.1848(2) 0.8591(4) 0.0213(6) Uani 1.00 d . . . O(6) O -0.0378(3) 0.0470(2) 0.7246(4) 0.0346(7) Uani 1.00 d . . . O(7) O 0.5943(4) 0.2805(2) 1.5153(4) 0.0510(8) Uani 1.00 d . . . N(1) N 0.2640(4) 0.3161(2) 0.7176(5) 0.0237(7) Uani 1.00 d . . . N(2) N 0.2084(4) 0.3718(2) 1.0851(4) 0.0187(6) Uani 1.00 d . . . N(3) N 0.3863(3) 0.1586(2) 0.8520(4) 0.0181(6) Uani 1.00 d . . . C(1) C 0.2051(5) 0.1616(2) 1.2676(5) 0.0352(9) Uani 1.00 d . . . C(2) C 0.3336(4) 0.4361(2) 1.1785(4) 0.0196(7) Uani 1.00 d . . . C(3) C 0.3010(4) 0.5070(2) 1.2859(4) 0.0235(7) Uani 1.00 d . . . C(4) C 0.1349(4) 0.5094(2) 1.2991(5) 0.0268(8) Uani 1.00 d . . . C(5) C 0.0063(4) 0.4425(2) 1.2043(5) 0.0282(8) Uani 1.00 d . . . C(6) C 0.0466(4) 0.3740(2) 1.0964(5) 0.0238(7) Uani 1.00 d . . . C(7) C 0.5127(4) 0.4245(2) 1.1580(5) 0.0217(7) Uani 1.00 d . . . C(8) C 0.2627(4) 0.0879(2) 0.7898(5) 0.0222(7) Uani 1.00 d . . . C(9) C 0.2982(4) 0.0057(2) 0.7285(4) 0.0252(7) Uani 1.00 d . . . C(10) C 0.4671(4) -0.0031(2) 0.7327(5) 0.0299(8) Uani 1.00 d . . . C(11) C 0.5957(4) 0.0697(2) 0.7959(5) 0.0296(8) Uani 1.00 d . . . C(12) C 0.5499(4) 0.1506(2) 0.8536(5) 0.0220(7) Uani 1.00 d . . . C(13) C 0.0838(4) 0.1053(2) 0.7886(5) 0.0237(7) Uani 1.00 d . . . C(14) C 0.7436(5) 0.2542(3) 1.4783(7) 0.051(1) Uani 1.00 d . . . H(1) H 0.2424 0.1477 1.4079 0.0256 Uiso 1.00 calc . . . H(2) H 0.0767 0.1759 1.2871 0.0256 Uiso 1.00 calc . . . H(3) H 0.1803 0.1082 1.1995 0.0256 Uiso 1.00 calc . . . H(4) H 0.4042 0.5532 1.3683 0.0256 Uiso 1.00 calc . . . H(5) H 0.1200 0.5591 1.4006 0.0256 Uiso 1.00 calc . . . H(6) H -0.1171 0.4412 1.2091 0.0256 Uiso 1.00 calc . . . H(7) H -0.0347 0.3228 1.0323 0.0256 Uiso 1.00 calc . . . H(8) H 0.2008 -0.0456 0.6702 0.0256 Uiso 1.00 calc . . . H(9) H 0.4879 -0.0667 0.6706 0.0256 Uiso 1.00 calc . . . H(10) H 0.7211 0.0647 0.7940 0.0256 Uiso 1.00 calc . . . H(11) H 0.6416 0.2046 0.9079 0.0256 Uiso 1.00 calc . . . H(12) H 0.8441 0.2708 1.6203 0.0256 Uiso 1.00 calc . . . H(13) H 0.7248 0.1827 1.4662 0.0256 Uiso 1.00 calc . . . H(14) H 0.7648 0.2685 1.3653 0.0256 Uiso 1.00 calc . . . H(15) H 0.5042 0.2561 1.4012 0.0256 Uiso 1.00 calc . . . #------------------------------------------------------------------------------ loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru 0.0148(2) 0.0167(2) 0.0168(2) 0.0025(1) 0.0044(1) 0.0019(1) O(1) 0.061(2) 0.032(1) 0.019(1) 0.003(1) 0.003(1) 0.0077(9) O(2) 0.024(1) 0.031(1) 0.016(1) 0.0044(9) 0.0043(9) 0.0058(9) O(3) 0.016(1) 0.021(1) 0.022(1) 0.0009(8) 0.0074(9) -0.0023(8) O(4) 0.022(1) 0.025(1) 0.033(1) -0.0021(9) 0.0057(10) -0.0078(10) O(5) 0.015(1) 0.021(1) 0.028(1) 0.0015(8) 0.0060(9) -0.0004(9) O(6) 0.021(1) 0.032(1) 0.049(2) -0.0046(9) 0.011(1) -0.013(1) O(7) 0.058(2) 0.050(2) 0.034(1) -0.002(1) -0.004(1) 0.000(1) N(1) 0.025(1) 0.019(1) 0.025(1) 0.001(1) 0.002(1) 0.000(1) N(2) 0.020(1) 0.018(1) 0.021(1) 0.0052(9) 0.011(1) 0.0030(9) N(3) 0.017(1) 0.018(1) 0.020(1) 0.0032(9) 0.0057(10) 0.0009(9) C(1) 0.045(2) 0.033(2) 0.027(2) -0.006(1) 0.015(2) 0.005(1) C(2) 0.019(1) 0.024(1) 0.017(1) 0.004(1) 0.006(1) 0.004(1) C(3) 0.028(1) 0.024(1) 0.020(1) 0.005(1) 0.008(1) 0.002(1) C(4) 0.034(2) 0.030(2) 0.025(1) 0.015(1) 0.017(1) 0.007(1) C(5) 0.023(1) 0.041(2) 0.027(2) 0.015(1) 0.012(1) 0.010(1) C(6) 0.019(1) 0.024(1) 0.028(2) 0.006(1) 0.005(1) 0.003(1) C(7) 0.016(1) 0.026(1) 0.023(2) 0.003(1) 0.004(1) 0.005(1) C(8) 0.020(1) 0.023(1) 0.022(1) 0.003(1) 0.002(1) 0.001(1) C(9) 0.031(2) 0.026(2) 0.020(1) 0.005(1) 0.008(1) -0.001(1) C(10) 0.031(2) 0.033(2) 0.030(2) 0.010(1) 0.013(1) 0.002(1) C(11) 0.028(2) 0.034(2) 0.030(2) 0.010(1) 0.011(1) 0.000(1) C(12) 0.016(1) 0.029(2) 0.023(1) 0.003(1) 0.010(1) 0.000(1) C(13) 0.018(1) 0.028(2) 0.024(2) 0.000(1) 0.007(1) 0.002(1) C(14) 0.039(2) 0.049(2) 0.056(3) 0.004(2) -0.004(2) 0.011(2) #------------------------------------------------------------------------------ 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(2) 1.964(2) . . yes Ru O(3) 2.035(2) . . yes Ru O(5) 2.036(2) . . yes Ru N(1) 1.760(3) . . yes Ru N(2) 2.076(3) . . yes Ru N(3) 2.073(3) . . yes O(1) N(1) 1.143(4) . . yes O(2) C(1) 1.417(4) . . no O(3) C(7) 1.297(4) . . no O(4) C(7) 1.209(4) . . no O(5) C(13) 1.304(4) . . no O(6) C(13) 1.216(4) . . no O(7) C(14) 1.403(6) . . no N(2) C(2) 1.332(4) . . no N(2) C(6) 1.340(4) . . no N(3) C(8) 1.344(4) . . no N(3) C(12) 1.347(4) . . no C(2) C(3) 1.377(4) . . no C(2) C(7) 1.528(4) . . no C(3) C(4) 1.379(4) . . no C(4) C(5) 1.375(5) . . no C(5) C(6) 1.378(5) . . no C(8) C(9) 1.387(4) . . no C(8) C(13) 1.508(4) . . no C(9) C(10) 1.390(4) . . no C(10) C(11) 1.389(5) . . no C(11) C(12) 1.397(4) . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(2) Ru O(3) 85.7(1) . . . no O(2) Ru O(5) 88.7(1) . . . no O(2) Ru N(1) 179.29(9) . . . no O(2) Ru N(2) 85.6(1) . . . no O(2) Ru N(3) 85.7(1) . . . no O(3) Ru O(5) 174.34(8) . . . no O(3) Ru N(1) 94.5(1) . . . no O(3) Ru N(2) 80.58(10) . . . no O(3) Ru N(3) 99.88(10) . . . no O(5) Ru N(1) 91.2(1) . . . no O(5) Ru N(2) 98.5(1) . . . no O(5) Ru N(3) 80.2(1) . . . no N(1) Ru N(2) 95.1(1) . . . no N(1) Ru N(3) 93.5(1) . . . no N(2) Ru N(3) 171.3(1) . . . no Ru O(2) C(1) 123.6(2) . . . no Ru O(3) C(7) 115.4(2) . . . no Ru O(5) C(13) 115.7(2) . . . no Ru N(1) O(1) 173.3(3) . . . yes Ru N(2) C(2) 113.0(2) . . . no Ru N(2) C(6) 126.5(2) . . . no C(2) N(2) C(6) 120.3(3) . . . no Ru N(3) C(8) 113.2(2) . . . no Ru N(3) C(12) 127.1(2) . . . no C(8) N(3) C(12) 119.7(3) . . . no N(2) C(2) C(3) 121.5(3) . . . no N(2) C(2) C(7) 115.1(3) . . . no C(3) C(2) C(7) 123.3(3) . . . no C(2) C(3) C(4) 118.4(3) . . . no C(3) C(4) C(5) 119.9(3) . . . no C(4) C(5) C(6) 118.9(3) . . . no N(2) C(6) C(5) 120.9(3) . . . no O(3) C(7) O(4) 124.8(3) . . . no O(3) C(7) C(2) 115.7(3) . . . no O(4) C(7) C(2) 119.5(3) . . . no N(3) C(8) C(9) 121.9(3) . . . no N(3) C(8) C(13) 115.1(3) . . . no C(9) C(8) C(13) 123.0(3) . . . no C(8) C(9) C(10) 118.5(3) . . . no C(9) C(10) C(11) 120.0(3) . . . no C(10) C(11) C(12) 118.3(3) . . . no N(3) C(12) C(11) 121.7(3) . . . no O(5) C(13) O(6) 124.3(3) . . . no O(5) C(13) C(8) 115.7(3) . . . no O(6) C(13) C(8) 120.0(3) . . . no #------------------------------------------------------------------------------ #===END