# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Lehnert, Nicolai' _publ_contact_author_email lehnertn@umich.edu _publ_section_title ; Synthesis, Spectroscopic Analysis and Photolabilization of Water-Soluble Ruthenium(III)-Nitrosyl Complexes ; loop_ _publ_author_name A.Merkle N.Lehnert # Attachment '- [Ru(TPA)(NO2)2].cif' data_am2 _database_code_depnum_ccdc_archive 'CCDC 869443' #TrackingRef '- [Ru(TPA)(NO2)2].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 N6 O4 Ru, 2(C H4 O)' _chemical_formula_sum 'C20 H26 N6 O6 Ru' _chemical_formula_weight 547.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 19.347(7) _cell_length_b 14.704(5) _cell_length_c 16.562(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4712(3) _cell_formula_units_Z 8 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 9966 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 22.91 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8705 _exptl_absorpt_correction_T_max 0.9585 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2008/1) Bruker AXS area detector absorption and other corrections, University of Gottingen, Germany 2008. ; _exptl_special_details ; 2190 frames x 30 sec. @ 5.055 cm; 0.5 deg steps in omega Data collection at 225K due to destructive phase change at lower temperatures. ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 63152 _diffrn_reflns_av_R_equivalents 0.1070 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 23.99 _reflns_number_total 3651 _reflns_number_gt 2684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+14.8898P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3650 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1521 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ru1 Ru 0.56205(3) 0.22337(4) 0.30464(3) 0.0393(2) Uani 1 1 d . . . N1 N 0.6062(3) 0.3515(4) 0.2823(3) 0.0417(13) Uani 1 1 d . . . N2 N 0.5158(3) 0.3002(4) 0.3972(3) 0.0463(14) Uani 1 1 d . . . N3 N 0.6338(3) 0.1979(4) 0.3944(3) 0.0446(14) Uani 1 1 d . . . N4 N 0.5038(3) 0.1209(4) 0.3562(3) 0.0481(14) Uani 1 1 d . . . N5 N 0.6110(3) 0.1470(4) 0.2197(3) 0.0454(14) Uani 1 1 d . . . N6 N 0.4876(3) 0.2444(4) 0.2202(3) 0.0503(14) Uani 1 1 d . . . C1 C 0.6643(3) 0.3731(5) 0.2440(4) 0.0446(16) Uani 1 1 d . . . H1A H 0.6900 0.3258 0.2190 0.053 Uiso 1 1 calc R . . C2 C 0.6889(4) 0.4596(6) 0.2387(4) 0.058(2) Uani 1 1 d . . . H2A H 0.7313 0.4717 0.2119 0.070 Uiso 1 1 calc R . . C3 C 0.6511(4) 0.5299(5) 0.2729(5) 0.062(2) Uani 1 1 d . . . H3A H 0.6659 0.5912 0.2674 0.075 Uiso 1 1 calc R . . C4 C 0.5921(4) 0.5092(5) 0.3146(4) 0.0538(18) Uani 1 1 d . . . H4A H 0.5668 0.5559 0.3410 0.065 Uiso 1 1 calc R . . C5 C 0.5699(4) 0.4208(5) 0.3183(4) 0.0468(17) Uani 1 1 d . . . C6 C 0.5061(4) 0.3927(5) 0.3626(4) 0.0534(19) Uani 1 1 d . . . H6A H 0.4964 0.4366 0.4065 0.064 Uiso 1 1 calc R . . H6B H 0.4662 0.3926 0.3252 0.064 Uiso 1 1 calc R . . C7 C 0.5626(4) 0.3045(5) 0.4690(4) 0.0522(18) Uani 1 1 d . . . H7A H 0.5347 0.2962 0.5185 0.063 Uiso 1 1 calc R . . H7B H 0.5839 0.3657 0.4715 0.063 Uiso 1 1 calc R . . C8 C 0.6188(4) 0.2345(4) 0.4678(4) 0.0440(16) Uani 1 1 d . . . C9 C 0.6560(4) 0.2117(5) 0.5347(4) 0.0525(19) Uani 1 1 d . . . H9A H 0.6434 0.2361 0.5857 0.063 Uiso 1 1 calc R . . C10 C 0.7117(4) 0.1537(5) 0.5291(4) 0.0536(19) Uani 1 1 d . . . H10A H 0.7379 0.1382 0.5756 0.064 Uiso 1 1 calc R . . C11 C 0.7283(4) 0.1188(5) 0.4554(4) 0.0520(18) Uani 1 1 d . . . H11A H 0.7667 0.0790 0.4497 0.062 Uiso 1 1 calc R . . C12 C 0.6888(4) 0.1420(5) 0.3895(4) 0.0485(17) Uani 1 1 d . . . H12A H 0.7009 0.1176 0.3383 0.058 Uiso 1 1 calc R . . C13 C 0.4509(4) 0.2540(6) 0.4180(5) 0.062(2) Uani 1 1 d . . . H13A H 0.4139 0.2750 0.3812 0.074 Uiso 1 1 calc R . . H13B H 0.4375 0.2704 0.4738 0.074 Uiso 1 1 calc R . . C14 C 0.4574(4) 0.1545(5) 0.4118(4) 0.0528(18) Uani 1 1 d . . . C15 C 0.4183(4) 0.0940(6) 0.4579(5) 0.067(2) Uani 1 1 d . . . H15A H 0.3875 0.1169 0.4977 0.081 Uiso 1 1 calc R . . C16 C 0.4237(5) 0.0027(6) 0.4468(5) 0.073(3) Uani 1 1 d . . . H16A H 0.3955 -0.0377 0.4771 0.087 Uiso 1 1 calc R . . C17 C 0.4700(5) -0.0309(6) 0.3917(5) 0.065(2) Uani 1 1 d . . . H17A H 0.4749 -0.0946 0.3838 0.078 Uiso 1 1 calc R . . C18 C 0.5097(4) 0.0304(5) 0.3479(4) 0.0525(18) Uani 1 1 d . . . H18A H 0.5425 0.0073 0.3105 0.063 Uiso 1 1 calc R . . C20 C 0.3045(8) 0.3547(14) 0.1504(11) 0.209(10) Uani 1 1 d . . . H20A H 0.3354 0.4063 0.1606 0.314 Uiso 1 1 calc R . . H20B H 0.2888 0.3294 0.2019 0.314 Uiso 1 1 calc R . . H20C H 0.2645 0.3752 0.1190 0.314 Uiso 1 1 calc R . . O1 O 0.5815(3) 0.0822(4) 0.1857(3) 0.0665(15) Uani 1 1 d . . . O2 O 0.6724(3) 0.1627(4) 0.2003(3) 0.0526(12) Uani 1 1 d . . . O3 O 0.4245(3) 0.2430(5) 0.2376(4) 0.0817(18) Uani 1 1 d . . . O4 O 0.5012(3) 0.2566(4) 0.1492(3) 0.0706(16) Uani 1 1 d . . . O6 O 0.3415(5) 0.2853(9) 0.1055(5) 0.155(4) Uani 1 1 d . . . H6 H 0.3797 0.2752 0.1278 0.232 Uiso 1 1 calc R . . C19 C 0.6847(7) -0.0628(9) 0.0597(8) 0.127(5) Uani 1 1 d . . . H19A H 0.6745 -0.0893 0.1127 0.191 Uiso 1 1 calc R . . H19B H 0.7318 -0.0384 0.0597 0.191 Uiso 1 1 calc R . . H19C H 0.6806 -0.1099 0.0181 0.191 Uiso 1 1 calc R . . O5 O 0.6358(4) 0.0101(5) 0.0429(4) 0.095(2) Uani 1 1 d . . . H5 H 0.6213 0.0318 0.0866 0.143 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0444(4) 0.0469(4) 0.0266(3) 0.0000(2) 0.0029(2) -0.0006(2) N1 0.054(4) 0.046(3) 0.026(3) 0.004(2) -0.005(2) 0.002(3) N2 0.050(3) 0.050(3) 0.039(3) -0.002(3) 0.009(3) 0.004(3) N3 0.058(4) 0.051(3) 0.025(3) 0.001(2) 0.005(3) -0.001(3) N4 0.055(4) 0.057(4) 0.032(3) 0.010(3) -0.001(3) -0.009(3) N5 0.053(4) 0.055(4) 0.028(3) 0.000(3) -0.001(3) 0.000(3) N6 0.050(4) 0.061(4) 0.040(3) 0.002(3) -0.002(3) -0.005(3) C1 0.047(4) 0.056(4) 0.030(3) 0.000(3) -0.003(3) -0.010(3) C2 0.052(5) 0.074(5) 0.049(4) 0.008(4) -0.003(4) -0.001(4) C3 0.073(6) 0.050(5) 0.064(5) 0.013(4) -0.014(4) -0.005(4) C4 0.063(5) 0.057(5) 0.041(4) 0.000(4) -0.007(4) 0.002(4) C5 0.056(4) 0.051(4) 0.034(4) -0.001(3) -0.001(3) 0.004(4) C6 0.064(5) 0.051(4) 0.044(4) -0.002(3) 0.004(3) 0.014(4) C7 0.071(5) 0.055(4) 0.031(4) -0.003(3) 0.005(3) 0.002(4) C8 0.059(4) 0.045(4) 0.028(3) -0.001(3) 0.007(3) -0.012(3) C9 0.076(5) 0.061(5) 0.020(3) -0.002(3) -0.003(3) -0.010(4) C10 0.063(5) 0.069(5) 0.029(4) 0.010(3) -0.011(3) -0.011(4) C11 0.049(4) 0.063(5) 0.044(4) 0.006(4) -0.005(3) -0.008(4) C12 0.048(4) 0.060(4) 0.038(4) 0.000(3) 0.002(3) 0.004(4) C13 0.059(5) 0.079(5) 0.047(4) 0.001(4) 0.017(4) 0.008(4) C14 0.049(4) 0.068(5) 0.042(4) 0.006(4) 0.003(3) -0.005(4) C15 0.063(5) 0.090(7) 0.048(5) 0.002(5) 0.005(4) -0.014(5) C16 0.082(6) 0.078(6) 0.059(5) 0.009(5) 0.001(4) -0.040(5) C17 0.091(6) 0.059(5) 0.045(4) 0.003(4) -0.010(4) -0.025(4) C18 0.067(5) 0.053(5) 0.038(4) -0.001(3) -0.010(3) -0.010(4) C20 0.148(14) 0.33(3) 0.152(15) 0.025(17) 0.021(12) 0.127(17) O1 0.079(4) 0.068(4) 0.052(3) -0.023(3) 0.012(3) -0.017(3) O2 0.051(3) 0.072(3) 0.034(3) 0.002(2) 0.007(2) 0.003(3) O3 0.050(4) 0.125(5) 0.071(4) 0.020(4) -0.007(3) 0.003(3) O4 0.066(4) 0.112(5) 0.034(3) 0.010(3) -0.006(3) -0.005(3) O6 0.111(7) 0.264(13) 0.089(6) 0.033(7) -0.017(5) 0.035(8) C19 0.154(12) 0.122(10) 0.106(9) 0.001(8) 0.028(9) -0.040(10) O5 0.130(6) 0.099(5) 0.056(4) 0.000(4) 0.033(4) 0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N6 2.031(6) . ? Ru1 N5 2.033(6) . ? Ru1 N4 2.067(5) . ? Ru1 N3 2.068(6) . ? Ru1 N1 2.101(6) . ? Ru1 N2 2.105(5) . ? N1 C1 1.329(8) . ? N1 C5 1.375(9) . ? N2 C13 1.468(9) . ? N2 C6 1.488(9) . ? N2 C7 1.496(9) . ? N3 C12 1.347(9) . ? N3 C8 1.361(8) . ? N4 C18 1.343(9) . ? N4 C14 1.377(9) . ? N5 O1 1.245(7) . ? N5 O2 1.252(7) . ? N6 O4 1.218(7) . ? N6 O3 1.255(8) . ? C1 C2 1.361(10) . ? C2 C3 1.387(11) . ? C3 C4 1.368(11) . ? C4 C5 1.371(10) . ? C5 C6 1.494(10) . ? C7 C8 1.498(10) . ? C8 C9 1.364(10) . ? C9 C10 1.376(10) . ? C10 C11 1.361(10) . ? C11 C12 1.376(10) . ? C13 C14 1.471(11) . ? C14 C15 1.396(11) . ? C15 C16 1.359(12) . ? C16 C17 1.371(12) . ? C17 C18 1.389(10) . ? C20 O6 1.450(18) . ? C19 O5 1.456(14) . ? 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_3 _geom_angle_publ_flag N6 Ru1 N5 86.4(2) . . ? N6 Ru1 N4 90.5(2) . . ? N5 Ru1 N4 97.9(2) . . ? N6 Ru1 N3 176.8(2) . . ? N5 Ru1 N3 94.8(2) . . ? N4 Ru1 N3 86.4(2) . . ? N6 Ru1 N1 91.8(2) . . ? N5 Ru1 N1 100.6(2) . . ? N4 Ru1 N1 161.5(2) . . ? N3 Ru1 N1 90.9(2) . . ? N6 Ru1 N2 96.8(2) . . ? N5 Ru1 N2 176.8(2) . . ? N4 Ru1 N2 81.9(2) . . ? N3 Ru1 N2 81.9(2) . . ? N1 Ru1 N2 79.6(2) . . ? C1 N1 C5 117.5(6) . . ? C1 N1 Ru1 130.0(5) . . ? C5 N1 Ru1 112.3(4) . . ? C13 N2 C6 114.0(6) . . ? C13 N2 C7 110.5(6) . . ? C6 N2 C7 110.1(6) . . ? C13 N2 Ru1 106.6(4) . . ? C6 N2 Ru1 105.3(4) . . ? C7 N2 Ru1 110.1(4) . . ? C12 N3 C8 117.6(6) . . ? C12 N3 Ru1 126.7(4) . . ? C8 N3 Ru1 115.3(5) . . ? C18 N4 C14 118.7(6) . . ? C18 N4 Ru1 129.3(5) . . ? C14 N4 Ru1 111.7(5) . . ? O1 N5 O2 117.3(6) . . ? O1 N5 Ru1 121.5(5) . . ? O2 N5 Ru1 121.2(5) . . ? O4 N6 O3 115.7(6) . . ? O4 N6 Ru1 122.2(5) . . ? O3 N6 Ru1 122.0(5) . . ? N1 C1 C2 123.4(7) . . ? C1 C2 C3 119.1(7) . . ? C4 C3 C2 118.7(7) . . ? C3 C4 C5 119.7(7) . . ? C4 C5 N1 121.5(7) . . ? C4 C5 C6 122.9(7) . . ? N1 C5 C6 115.5(6) . . ? N2 C6 C5 109.7(6) . . ? N2 C7 C8 113.6(5) . . ? N3 C8 C9 121.1(7) . . ? N3 C8 C7 116.0(6) . . ? C9 C8 C7 122.8(6) . . ? C8 C9 C10 120.7(6) . . ? C11 C10 C9 118.6(6) . . ? C10 C11 C12 119.2(7) . . ? N3 C12 C11 122.8(6) . . ? N2 C13 C14 111.8(6) . . ? N4 C14 C15 119.3(7) . . ? N4 C14 C13 117.3(6) . . ? C15 C14 C13 123.3(7) . . ? C16 C15 C14 120.9(8) . . ? C15 C16 C17 119.8(8) . . ? C16 C17 C18 118.4(8) . . ? N4 C18 C17 122.8(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O1 0.84 1.96 2.797(8) 176.5 . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.485 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.117 # Attachment '- [Ru(TPA)(ONO)(NO)](PF6)2.cif' data_am163 _database_code_depnum_ccdc_archive 'CCDC 869444' #TrackingRef '- [Ru(TPA)(ONO)(NO)](PF6)2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 N6 O3 Ru, 2(F6 P)' _chemical_formula_sum 'C18 H18 F12 N6 O3 P2 Ru' _chemical_formula_weight 757.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.3726(3) _cell_length_b 9.9439(2) _cell_length_c 17.3570(12) _cell_angle_alpha 90.00 _cell_angle_beta 114.313(8) _cell_angle_gamma 90.00 _cell_volume 2575.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 32688 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 68.20 _exptl_crystal_description blade _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.954 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 7.272 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.559 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'micro-focus rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn744+ CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.629 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39910 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 68.22 _reflns_number_total 4645 _reflns_number_gt 4482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r5' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r5' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+15.0335P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4645 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 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 Ru1 Ru 0.292383(18) 0.35843(3) 0.106350(18) 0.02238(7) Uani 1 1 d . . . P1 P 0.64514(6) 0.20354(10) 0.05809(6) 0.0238(2) Uani 1 1 d . . . P2 P 0.49955(6) 0.88951(10) 0.35253(6) 0.0238(2) Uani 1 1 d . . . F1 F 0.55988(16) 0.1369(3) -0.01531(16) 0.0380(7) Uani 1 1 d . . . F2 F 0.70115(14) 0.0677(2) 0.06453(15) 0.0317(6) Uani 1 1 d . . . F3 F 0.67854(16) 0.2614(3) -0.01026(14) 0.0359(6) Uani 1 1 d . . . F4 F 0.73109(15) 0.2672(3) 0.13235(14) 0.0332(6) Uani 1 1 d . . . F5 F 0.58914(17) 0.3368(3) 0.05172(18) 0.0404(6) Uani 1 1 d . . . F6 F 0.61386(15) 0.1434(3) 0.12793(15) 0.0354(6) Uani 1 1 d . . . F7 F 0.45479(17) 0.7489(3) 0.35395(16) 0.0383(6) Uani 1 1 d . . . F8 F 0.46364(18) 0.8820(3) 0.25189(15) 0.0389(7) Uani 1 1 d . . . F9 F 0.59023(16) 0.8152(3) 0.36225(17) 0.0431(7) Uani 1 1 d . . . F10 F 0.54640(16) 1.0319(3) 0.35220(15) 0.0359(6) Uani 1 1 d . . . F11 F 0.53821(17) 0.8998(3) 0.45376(15) 0.0389(6) Uani 1 1 d . . . F12 F 0.41143(16) 0.9663(3) 0.34447(19) 0.0464(7) Uani 1 1 d . . . N1 N 0.2365(2) 0.5138(3) 0.0989(2) 0.0281(8) Uani 1 1 d . . . N2 N 0.2998(3) 0.3791(5) 0.2812(3) 0.0501(11) Uani 1 1 d . . . N3 N 0.1851(2) 0.2288(3) 0.0449(2) 0.0263(7) Uani 1 1 d . . . N4 N 0.3686(3) 0.1788(4) 0.1168(3) 0.0340(11) Uani 1 1 d . . . N5 N 0.4227(2) 0.4277(3) 0.17132(19) 0.0235(7) Uani 1 1 d . . . N6 N 0.2965(2) 0.3658(3) -0.0124(2) 0.0242(7) Uani 1 1 d . . . O1 O 0.2056(2) 0.6168(3) 0.0943(2) 0.0368(8) Uani 1 1 d . . . O2 O 0.2941(2) 0.2974(3) 0.21859(18) 0.0373(7) Uani 1 1 d . . . O3 O 0.3008(2) 0.4953(4) 0.2672(2) 0.0544(10) Uani 1 1 d . . . C1 C 0.1010(3) 0.2639(5) -0.0033(2) 0.0289(9) Uani 1 1 d . . . H1A H 0.0835 0.3554 -0.0053 0.035 Uiso 1 1 calc R . . C2 C 0.0395(3) 0.1707(5) -0.0500(3) 0.0320(10) Uani 1 1 d . . . H2A H -0.0205 0.1978 -0.0831 0.038 Uiso 1 1 calc R . . C3 C 0.0632(3) 0.0380(4) -0.0497(3) 0.0299(9) Uani 1 1 d . . . H3A H 0.0209 -0.0264 -0.0836 0.036 Uiso 1 1 calc R . . C4 C 0.1511(3) 0.0003(4) 0.0016(3) 0.0327(9) Uani 1 1 d . . . H4A H 0.1692 -0.0910 0.0043 0.039 Uiso 1 1 calc R . . C5 C 0.2122(3) 0.0989(4) 0.0491(2) 0.0260(9) Uani 1 1 d . . . C6 C 0.3058(3) 0.0671(4) 0.1107(3) 0.0289(9) Uani 1 1 d . . . H6A H 0.3063 0.0504 0.1671 0.035 Uiso 1 1 calc R . . H6B H 0.3263 -0.0159 0.0926 0.035 Uiso 1 1 calc R . . C7 C 0.4510(3) 0.5570(4) 0.1789(3) 0.0285(9) Uani 1 1 d . . . H7A H 0.4092 0.6260 0.1509 0.034 Uiso 1 1 calc R . . C8 C 0.5400(3) 0.5905(5) 0.2268(3) 0.0306(10) Uani 1 1 d . . . H8A H 0.5591 0.6816 0.2319 0.037 Uiso 1 1 calc R . . C9 C 0.6001(3) 0.4895(5) 0.2669(3) 0.0326(10) Uani 1 1 d . . . H9A H 0.6612 0.5104 0.3003 0.039 Uiso 1 1 calc R . . C10 C 0.5712(3) 0.3581(5) 0.2583(3) 0.0323(10) Uani 1 1 d . . . H10A H 0.6123 0.2876 0.2852 0.039 Uiso 1 1 calc R . . C11 C 0.4830(3) 0.3300(4) 0.2107(2) 0.0264(9) Uani 1 1 d . . . C12 C 0.4460(3) 0.1889(4) 0.1989(3) 0.0289(9) Uani 1 1 d . . . H12A H 0.4929 0.1242 0.2011 0.035 Uiso 1 1 calc R . . H12B H 0.4275 0.1666 0.2449 0.035 Uiso 1 1 calc R . . C13 C 0.2473(3) 0.4486(4) -0.0756(3) 0.0281(9) Uani 1 1 d . . . H13A H 0.2174 0.5227 -0.0640 0.034 Uiso 1 1 calc R . . C14 C 0.2394(3) 0.4280(5) -0.1572(3) 0.0342(10) Uani 1 1 d . . . H14A H 0.2045 0.4877 -0.2012 0.041 Uiso 1 1 calc R . . C15 C 0.2833(3) 0.3183(5) -0.1747(3) 0.0345(10) Uani 1 1 d . . . H15A H 0.2780 0.3017 -0.2305 0.041 Uiso 1 1 calc R . . C16 C 0.3342(3) 0.2357(5) -0.1088(3) 0.0294(9) Uani 1 1 d . . . H16A H 0.3649 0.1611 -0.1186 0.035 Uiso 1 1 calc R . . C17 C 0.3406(2) 0.2617(4) -0.0273(2) 0.0205(8) Uani 1 1 d . . . C18 C 0.3998(2) 0.1821(4) 0.0469(2) 0.0251(9) Uani 1 1 d . . . H18A H 0.4610 0.2207 0.0689 0.030 Uiso 1 1 calc R . . H18B H 0.4033 0.0888 0.0285 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02579(13) 0.01932(15) 0.02679(14) -0.00039(11) 0.01561(10) 0.00101(11) P1 0.0233(4) 0.0225(5) 0.0266(4) -0.0004(4) 0.0114(4) 0.0000(4) P2 0.0251(4) 0.0231(5) 0.0246(4) 0.0025(4) 0.0116(4) -0.0001(4) F1 0.0287(12) 0.0328(14) 0.0413(14) -0.0087(11) 0.0033(10) 0.0018(10) F2 0.0270(10) 0.0299(13) 0.0381(12) 0.0027(10) 0.0134(9) 0.0080(10) F3 0.0395(12) 0.0462(15) 0.0244(11) 0.0093(10) 0.0157(9) 0.0017(11) F4 0.0354(11) 0.0351(13) 0.0276(11) -0.0009(10) 0.0115(9) -0.0108(10) F5 0.0427(13) 0.0237(12) 0.0580(15) -0.0030(11) 0.0240(11) 0.0050(11) F6 0.0354(11) 0.0394(14) 0.0397(12) 0.0045(10) 0.0238(10) -0.0051(11) F7 0.0495(13) 0.0265(13) 0.0390(13) 0.0038(10) 0.0183(11) -0.0091(11) F8 0.0507(14) 0.0346(14) 0.0240(12) 0.0013(10) 0.0079(11) -0.0018(12) F9 0.0303(11) 0.0466(16) 0.0513(15) -0.0099(13) 0.0158(11) 0.0076(11) F10 0.0405(12) 0.0313(13) 0.0342(12) 0.0028(10) 0.0138(10) -0.0100(11) F11 0.0496(14) 0.0382(14) 0.0267(11) -0.0011(10) 0.0135(10) -0.0038(12) F12 0.0254(11) 0.0449(16) 0.0658(17) -0.0125(13) 0.0155(11) 0.0056(11) N1 0.0322(15) 0.0200(17) 0.0394(17) -0.0011(14) 0.0222(13) 0.0007(14) N2 0.052(2) 0.052(3) 0.054(2) -0.008(2) 0.0288(19) 0.004(2) N3 0.0347(15) 0.0208(17) 0.0357(16) 0.0005(13) 0.0268(13) -0.0031(13) N4 0.0384(19) 0.026(2) 0.041(2) 0.0051(17) 0.0200(16) 0.0077(17) N5 0.0247(14) 0.0282(17) 0.0196(14) 0.0014(13) 0.0112(12) -0.0026(13) N6 0.0179(13) 0.0228(17) 0.0316(16) -0.0006(13) 0.0098(12) -0.0045(12) O1 0.0370(14) 0.0267(16) 0.0500(17) -0.0021(13) 0.0212(13) 0.0029(13) O2 0.0458(15) 0.0402(18) 0.0344(14) -0.0048(13) 0.0251(12) -0.0009(14) O3 0.065(2) 0.060(2) 0.0483(18) -0.0082(17) 0.0337(16) -0.0007(19) C1 0.0312(17) 0.032(2) 0.0339(19) 0.0009(16) 0.0237(15) -0.0011(17) C2 0.0348(19) 0.035(2) 0.034(2) -0.0022(17) 0.0226(16) -0.0046(18) C3 0.0333(18) 0.033(2) 0.0326(19) -0.0059(17) 0.0226(15) -0.0127(17) C4 0.046(2) 0.024(2) 0.041(2) 0.0007(17) 0.0316(17) -0.0024(18) C5 0.0311(17) 0.027(2) 0.0267(17) 0.0000(15) 0.0193(14) 0.0006(16) C6 0.0360(19) 0.0184(19) 0.040(2) 0.0026(16) 0.0230(16) -0.0014(16) C7 0.0292(18) 0.028(2) 0.0307(19) 0.0007(16) 0.0148(15) 0.0026(17) C8 0.0331(19) 0.028(2) 0.034(2) -0.0073(17) 0.0173(16) -0.0048(17) C9 0.0285(18) 0.041(3) 0.0281(19) -0.0035(18) 0.0118(16) -0.0026(18) C10 0.0311(19) 0.037(2) 0.0265(19) 0.0012(17) 0.0102(16) 0.0067(18) C11 0.0306(18) 0.028(2) 0.0233(17) -0.0012(16) 0.0138(15) 0.0026(16) C12 0.0308(19) 0.027(2) 0.0294(19) 0.0048(16) 0.0124(16) 0.0053(17) C13 0.0273(18) 0.026(2) 0.0292(19) 0.0031(16) 0.0101(15) -0.0042(16) C14 0.037(2) 0.039(2) 0.0258(19) 0.0035(18) 0.0121(16) -0.0070(19) C15 0.039(2) 0.041(3) 0.0250(19) -0.0008(18) 0.0147(16) -0.0132(19) C16 0.0282(18) 0.033(2) 0.0300(19) -0.0056(17) 0.0154(15) -0.0068(17) C17 0.0196(15) 0.0199(18) 0.0247(17) -0.0006(14) 0.0118(13) -0.0050(14) C18 0.0274(17) 0.023(2) 0.0296(18) -0.0026(15) 0.0170(15) -0.0007(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 1.772(3) . ? Ru1 O2 2.030(3) . ? Ru1 N5 2.078(3) . ? Ru1 N3 2.083(3) . ? Ru1 N6 2.091(4) . ? Ru1 N4 2.143(4) . ? P1 F5 1.589(3) . ? P1 F1 1.596(2) . ? P1 F4 1.597(2) . ? P1 F3 1.604(3) . ? P1 F2 1.610(3) . ? P1 F6 1.613(3) . ? P2 F7 1.583(3) . ? P2 F12 1.587(3) . ? P2 F8 1.599(3) . ? P2 F9 1.604(3) . ? P2 F11 1.607(3) . ? P2 F10 1.612(3) . ? N1 O1 1.131(4) . ? N2 O3 1.182(6) . ? N2 O2 1.329(5) . ? N3 C1 1.332(5) . ? N3 C5 1.357(5) . ? N4 C12 1.470(5) . ? N4 C6 1.486(6) . ? N4 C18 1.498(6) . ? N5 C11 1.353(5) . ? N5 C7 1.355(5) . ? N6 C13 1.342(5) . ? N6 C17 1.346(5) . ? C1 C2 1.362(6) . ? C2 C3 1.375(6) . ? C3 C4 1.396(6) . ? C4 C5 1.401(6) . ? C5 C6 1.497(5) . ? C7 C8 1.389(5) . ? C8 C9 1.377(6) . ? C9 C10 1.377(7) . ? C10 C11 1.366(6) . ? C11 C12 1.507(6) . ? C13 C14 1.384(6) . ? C14 C15 1.407(7) . ? C15 C16 1.376(6) . ? C16 C17 1.399(6) . ? C17 C18 1.482(5) . ? 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_3 _geom_angle_publ_flag N1 Ru1 O2 97.67(15) . . ? N1 Ru1 N5 97.73(14) . . ? O2 Ru1 N5 88.45(12) . . ? N1 Ru1 N3 101.62(14) . . ? O2 Ru1 N3 88.95(13) . . ? N5 Ru1 N3 160.66(13) . . ? N1 Ru1 N6 97.03(15) . . ? O2 Ru1 N6 164.43(13) . . ? N5 Ru1 N6 94.62(12) . . ? N3 Ru1 N6 83.09(12) . . ? N1 Ru1 N4 175.82(16) . . ? O2 Ru1 N4 83.82(16) . . ? N5 Ru1 N4 78.38(14) . . ? N3 Ru1 N4 82.29(14) . . ? N6 Ru1 N4 81.87(15) . . ? F5 P1 F1 90.04(14) . . ? F5 P1 F4 90.97(14) . . ? F1 P1 F4 178.83(15) . . ? F5 P1 F3 90.68(15) . . ? F1 P1 F3 90.63(14) . . ? F4 P1 F3 89.95(13) . . ? F5 P1 F2 179.50(15) . . ? F1 P1 F2 89.61(13) . . ? F4 P1 F2 89.38(13) . . ? F3 P1 F2 89.68(14) . . ? F5 P1 F6 90.52(15) . . ? F1 P1 F6 90.11(14) . . ? F4 P1 F6 89.29(13) . . ? F3 P1 F6 178.58(14) . . ? F2 P1 F6 89.12(14) . . ? F7 P2 F12 90.93(15) . . ? F7 P2 F8 90.66(14) . . ? F12 P2 F8 90.81(16) . . ? F7 P2 F9 90.33(15) . . ? F12 P2 F9 178.44(16) . . ? F8 P2 F9 90.09(15) . . ? F7 P2 F11 90.89(14) . . ? F12 P2 F11 90.03(16) . . ? F8 P2 F11 178.23(16) . . ? F9 P2 F11 89.04(15) . . ? F7 P2 F10 179.17(15) . . ? F12 P2 F10 89.65(15) . . ? F8 P2 F10 89.92(14) . . ? F9 P2 F10 89.08(15) . . ? F11 P2 F10 88.52(14) . . ? O1 N1 Ru1 175.7(3) . . ? O3 N2 O2 115.6(4) . . ? C1 N3 C5 120.9(3) . . ? C1 N3 Ru1 126.5(3) . . ? C5 N3 Ru1 111.9(2) . . ? C12 N4 C6 114.5(4) . . ? C12 N4 C18 109.7(4) . . ? C6 N4 C18 114.5(4) . . ? C12 N4 Ru1 105.3(3) . . ? C6 N4 Ru1 104.8(3) . . ? C18 N4 Ru1 107.1(3) . . ? C11 N5 C7 118.9(3) . . ? C11 N5 Ru1 114.1(3) . . ? C7 N5 Ru1 126.9(3) . . ? C13 N6 C17 120.3(4) . . ? C13 N6 Ru1 125.0(3) . . ? C17 N6 Ru1 113.5(3) . . ? N2 O2 Ru1 124.8(3) . . ? N3 C1 C2 121.0(4) . . ? C1 C2 C3 120.8(4) . . ? C2 C3 C4 118.4(4) . . ? C3 C4 C5 119.1(4) . . ? N3 C5 C4 119.7(3) . . ? N3 C5 C6 117.1(3) . . ? C4 C5 C6 123.0(4) . . ? N4 C6 C5 111.5(3) . . ? N5 C7 C8 121.3(4) . . ? C9 C8 C7 118.8(4) . . ? C10 C9 C8 119.7(4) . . ? C11 C10 C9 119.4(4) . . ? N5 C11 C10 121.9(4) . . ? N5 C11 C12 115.5(3) . . ? C10 C11 C12 122.6(4) . . ? N4 C12 C11 109.5(3) . . ? N6 C13 C14 121.1(4) . . ? C13 C14 C15 119.7(4) . . ? C16 C15 C14 118.1(4) . . ? C15 C16 C17 119.9(4) . . ? N6 C17 C16 120.9(3) . . ? N6 C17 C18 117.1(3) . . ? C16 C17 C18 122.0(4) . . ? C17 C18 N4 113.3(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 68.22 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.679 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.108 # Attachment '- [Ru(TPA)Cl2(NO)]ClO4.cif' data_am375 _database_code_depnum_ccdc_archive 'CCDC 869445' #TrackingRef '- [Ru(TPA)Cl2(NO)]ClO4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration ad _chemical_formula_moiety 'C18 H18 Cl2 N5 O Ru, C H2 Cl2, Cl O4' _chemical_formula_sum 'C19 H20 Cl5 N5 O5 Ru' _chemical_formula_weight 676.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.75460(10) _cell_length_b 13.7776(2) _cell_length_c 9.9353(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.935(8) _cell_angle_gamma 90.00 _cell_volume 1247.11(11) _cell_formula_units_Z 2 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 14168 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 67.80 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 10.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2083 _exptl_absorpt_correction_T_max 0.5744 _exptl_absorpt_process_details ; Jacobson, R. (1998) Private Communication ; _exptl_special_details ; 2231 images collected at 42.00 mm; 1.0 deg. oscialltions in omega 10 sec. (low-resolution), 20 sec. (high-resolution) exposures ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'micro-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn 944+ CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16404 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.77 _diffrn_reflns_theta_max 67.82 _reflns_number_total 3946 _reflns_number_gt 3898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 7.0r5 (Rigaku, (2010)' _computing_cell_refinement 'CrystalClear-SM Expert 7.0r5' _computing_data_reduction 'CrystalClear-SM Expert 7.0r5' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00047(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(5) _refine_ls_number_reflns 3946 _refine_ls_number_parameters 317 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0175 _refine_ls_R_factor_gt 0.0174 _refine_ls_wR_factor_ref 0.0406 _refine_ls_wR_factor_gt 0.0405 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ru1 Ru 0.962699(17) -0.112741(12) 0.849183(16) 0.01035(6) Uani 1 1 d . . . Cl1 Cl 0.87255(7) -0.21376(5) 0.99306(6) 0.01480(14) Uani 1 1 d . . . Cl2 Cl 1.13970(6) -0.23166(5) 0.85550(6) 0.01742(14) Uani 1 1 d . . . Cl3 Cl 0.27275(8) 0.82328(5) 0.43368(7) 0.02677(17) Uani 1 1 d . . . Cl4 Cl 0.46562(7) 0.75640(6) 0.71550(7) 0.03107(17) Uani 1 1 d . . . Cl5 Cl 0.21483(6) 0.46480(4) 0.62886(5) 0.01296(13) Uani 1 1 d . . . O1 O 0.7462(2) -0.20776(14) 0.60754(18) 0.0200(4) Uani 1 1 d . . . O2 O 0.28504(19) 0.48820(14) 0.52729(17) 0.0198(4) Uani 1 1 d . . . O3 O 0.1356(2) 0.54760(14) 0.64889(19) 0.0241(4) Uani 1 1 d . . . O4 O 0.32638(18) 0.43849(14) 0.76469(17) 0.0192(4) Uani 1 1 d . . . O5 O 0.11671(17) 0.38378(17) 0.57540(16) 0.0228(4) Uani 1 1 d . . . N1 N 0.8332(2) -0.16479(16) 0.6966(2) 0.0126(5) Uani 1 1 d . . . N2 N 1.0460(2) -0.01200(16) 0.7453(2) 0.0126(5) Uani 1 1 d . . . N3 N 0.8380(2) 0.00821(15) 0.87321(19) 0.0104(4) Uani 1 1 d . . . N4 N 1.1063(2) -0.04939(16) 1.0399(2) 0.0113(4) Uani 1 1 d . . . N5 N 0.5610(2) 0.14894(15) 0.7381(2) 0.0146(5) Uani 1 1 d . . . C1 C 1.1447(3) -0.0308(2) 0.6820(2) 0.0142(5) Uani 1 1 d . . . H1A H 1.1793 -0.0953 0.6826 0.017 Uiso 1 1 calc R . . C2 C 1.1962(3) 0.0411(2) 0.6167(2) 0.0158(6) Uani 1 1 d . . . H2B H 1.2660 0.0264 0.5731 0.019 Uiso 1 1 calc R . . C3 C 1.1457(3) 0.1354(2) 0.6148(2) 0.0161(6) Uani 1 1 d . . . H3B H 1.1798 0.1859 0.5697 0.019 Uiso 1 1 calc R . . C4 C 1.0446(3) 0.1546(2) 0.6800(2) 0.0150(6) Uani 1 1 d . . . H4B H 1.0090 0.2187 0.6808 0.018 Uiso 1 1 calc R . . C5 C 0.9959(3) 0.07978(19) 0.7439(2) 0.0118(5) Uani 1 1 d . . . C6 C 0.8842(3) 0.09777(19) 0.8122(3) 0.0138(5) Uani 1 1 d . . . H6A H 0.7960 0.1270 0.7394 0.017 Uiso 1 1 calc R . . H6B H 0.9245 0.1457 0.8908 0.017 Uiso 1 1 calc R . . C7 C 0.8773(3) 0.0202(2) 1.0332(2) 0.0113(5) Uani 1 1 d . . . H7A H 0.8431 0.0841 1.0543 0.014 Uiso 1 1 calc R . . H7B H 0.8296 -0.0311 1.0708 0.014 Uiso 1 1 calc R . . C8 C 1.0409(3) 0.01306(18) 1.1034(3) 0.0123(5) Uani 1 1 d . . . C9 C 1.1212(3) 0.0656(2) 1.2251(3) 0.0150(6) Uani 1 1 d . . . H9A H 1.0736 0.1086 1.2691 0.018 Uiso 1 1 calc R . . C10 C 1.2729(3) 0.0542(2) 1.2812(2) 0.0155(6) Uani 1 1 d . . . H10A H 1.3304 0.0898 1.3639 0.019 Uiso 1 1 calc R . . C11 C 1.3391(3) -0.0094(2) 1.2159(3) 0.0174(6) Uani 1 1 d . . . H11A H 1.4426 -0.0178 1.2532 0.021 Uiso 1 1 calc R . . C12 C 1.2538(3) -0.0606(2) 1.0961(3) 0.0149(5) Uani 1 1 d . . . H12A H 1.2996 -0.1048 1.0519 0.018 Uiso 1 1 calc R . . C13 C 0.6747(3) -0.0094(2) 0.8016(2) 0.0129(5) Uani 1 1 d . . . H13A H 0.6511 -0.0176 0.6967 0.015 Uiso 1 1 calc R . . H13B H 0.6492 -0.0707 0.8391 0.015 Uiso 1 1 calc R . . C14 C 0.5819(3) 0.07149(19) 0.8257(2) 0.0121(5) Uani 1 1 d . . . C15 C 0.5227(3) 0.0648(2) 0.9342(2) 0.0145(6) Uani 1 1 d . . . H15A H 0.5375 0.0085 0.9927 0.017 Uiso 1 1 calc R . . C16 C 0.4415(3) 0.1426(2) 0.9546(3) 0.0181(6) Uani 1 1 d . . . H16A H 0.3988 0.1399 1.0267 0.022 Uiso 1 1 calc R . . C17 C 0.4238(3) 0.2239(2) 0.8686(3) 0.0170(6) Uani 1 1 d . . . H17A H 0.3712 0.2788 0.8823 0.020 Uiso 1 1 calc R . . C18 C 0.4843(3) 0.2239(2) 0.7619(3) 0.0166(6) Uani 1 1 d . . . H18A H 0.4710 0.2797 0.7024 0.020 Uiso 1 1 calc R . . C19 C 0.3146(3) 0.7276(2) 0.5588(3) 0.0277(7) Uani 1 1 d . . . H19A H 0.3373 0.6686 0.5139 0.033 Uiso 1 1 calc R . . H19B H 0.2281 0.7136 0.5854 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01177(9) 0.00937(10) 0.01102(9) 0.00068(8) 0.00541(7) 0.00047(9) Cl1 0.0165(3) 0.0129(3) 0.0173(3) 0.0043(3) 0.0088(2) 0.0009(3) Cl2 0.0188(3) 0.0127(3) 0.0245(3) 0.0016(3) 0.0123(3) 0.0042(3) Cl3 0.0394(4) 0.0195(4) 0.0226(3) 0.0047(3) 0.0125(3) 0.0033(3) Cl4 0.0258(3) 0.0397(5) 0.0225(3) -0.0018(3) 0.0023(3) -0.0032(3) Cl5 0.0128(3) 0.0141(3) 0.0113(2) 0.0007(2) 0.0034(2) 0.0011(2) O1 0.0259(10) 0.0177(11) 0.0157(9) -0.0037(8) 0.0066(8) -0.0054(9) O2 0.0255(10) 0.0208(11) 0.0167(9) -0.0018(8) 0.0119(8) -0.0031(8) O3 0.0251(10) 0.0214(11) 0.0282(10) 0.0021(9) 0.0124(9) 0.0110(9) O4 0.0147(8) 0.0243(11) 0.0139(8) 0.0026(8) -0.0005(7) 0.0030(8) O5 0.0220(9) 0.0241(10) 0.0216(8) -0.0027(10) 0.0070(7) -0.0119(10) N1 0.0175(11) 0.0097(11) 0.0133(10) 0.0023(9) 0.0090(9) 0.0025(9) N2 0.0123(10) 0.0153(13) 0.0104(9) -0.0020(9) 0.0043(8) -0.0027(9) N3 0.0110(10) 0.0115(12) 0.0082(9) 0.0011(8) 0.0028(8) 0.0000(8) N4 0.0112(10) 0.0114(12) 0.0122(9) 0.0047(9) 0.0052(8) 0.0008(9) N5 0.0124(11) 0.0119(13) 0.0176(10) 0.0019(9) 0.0032(9) 0.0014(9) C1 0.0118(12) 0.0193(16) 0.0118(11) -0.0018(11) 0.0046(10) 0.0003(11) C2 0.0145(13) 0.0249(17) 0.0077(11) -0.0018(11) 0.0038(10) -0.0041(12) C3 0.0169(13) 0.0198(16) 0.0095(11) 0.0015(11) 0.0023(10) -0.0073(12) C4 0.0157(14) 0.0133(15) 0.0115(11) 0.0004(11) -0.0009(10) -0.0036(11) C5 0.0120(12) 0.0138(15) 0.0065(11) 0.0001(10) -0.0004(10) -0.0020(11) C6 0.0143(13) 0.0077(14) 0.0186(12) 0.0032(10) 0.0049(10) 0.0018(11) C7 0.0131(12) 0.0121(15) 0.0088(11) -0.0014(10) 0.0041(10) 0.0005(11) C8 0.0165(13) 0.0082(14) 0.0134(11) 0.0023(10) 0.0068(10) 0.0009(10) C9 0.0173(13) 0.0137(15) 0.0153(12) 0.0009(10) 0.0075(11) -0.0021(11) C10 0.0163(13) 0.0172(15) 0.0099(11) 0.0020(11) 0.0011(11) -0.0053(11) C11 0.0123(13) 0.0209(15) 0.0184(12) 0.0082(12) 0.0050(10) 0.0019(11) C12 0.0129(12) 0.0170(15) 0.0160(12) 0.0060(11) 0.0068(10) 0.0023(11) C13 0.0100(12) 0.0157(14) 0.0114(11) -0.0007(10) 0.0019(10) -0.0008(10) C14 0.0075(12) 0.0141(15) 0.0107(11) -0.0010(10) -0.0016(10) -0.0015(10) C15 0.0143(13) 0.0156(15) 0.0123(12) 0.0019(10) 0.0029(10) 0.0000(11) C16 0.0142(13) 0.0256(18) 0.0147(12) -0.0011(12) 0.0053(10) -0.0002(12) C17 0.0129(12) 0.0162(16) 0.0192(13) -0.0045(11) 0.0024(11) 0.0003(11) C18 0.0137(13) 0.0131(15) 0.0194(13) 0.0023(11) 0.0015(11) -0.0008(11) C19 0.0354(17) 0.0203(17) 0.0206(14) 0.0037(12) 0.0017(13) -0.0052(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 1.743(2) . ? Ru1 N2 2.062(2) . ? Ru1 N4 2.102(2) . ? Ru1 N3 2.126(2) . ? Ru1 Cl2 2.3647(6) . ? Ru1 Cl1 2.3774(6) . ? Cl3 C19 1.756(3) . ? Cl4 C19 1.764(3) . ? Cl5 O3 1.4310(19) . ? Cl5 O5 1.443(2) . ? Cl5 O2 1.4441(18) . ? Cl5 O4 1.4447(17) . ? O1 N1 1.148(3) . ? N2 C1 1.350(3) . ? N2 C5 1.354(3) . ? N3 C7 1.505(3) . ? N3 C6 1.512(3) . ? N3 C13 1.514(3) . ? N4 C12 1.353(3) . ? N4 C8 1.355(3) . ? N5 C18 1.344(3) . ? N5 C14 1.346(3) . ? C1 C2 1.375(4) . ? C2 C3 1.387(4) . ? C3 C4 1.385(4) . ? C4 C5 1.381(3) . ? C5 C6 1.496(3) . ? C7 C8 1.499(4) . ? C8 C9 1.386(4) . ? C9 C10 1.391(4) . ? C10 C11 1.381(4) . ? C11 C12 1.378(4) . ? C13 C14 1.509(4) . ? C14 C15 1.396(3) . ? C15 C16 1.390(4) . ? C16 C17 1.382(4) . ? C17 C18 1.386(4) . ? 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_3 _geom_angle_publ_flag N1 Ru1 N2 97.72(8) . . ? N1 Ru1 N4 175.68(8) . . ? N2 Ru1 N4 85.21(7) . . ? N1 Ru1 N3 98.88(9) . . ? N2 Ru1 N3 82.66(8) . . ? N4 Ru1 N3 78.30(7) . . ? N1 Ru1 Cl2 91.91(7) . . ? N2 Ru1 Cl2 93.73(6) . . ? N4 Ru1 Cl2 91.06(6) . . ? N3 Ru1 Cl2 168.98(5) . . ? N1 Ru1 Cl1 88.47(7) . . ? N2 Ru1 Cl1 172.59(6) . . ? N4 Ru1 Cl1 88.39(5) . . ? N3 Ru1 Cl1 92.41(5) . . ? Cl2 Ru1 Cl1 90.10(2) . . ? O3 Cl5 O5 110.36(12) . . ? O3 Cl5 O2 109.49(11) . . ? O5 Cl5 O2 109.48(10) . . ? O3 Cl5 O4 109.51(11) . . ? O5 Cl5 O4 109.21(11) . . ? O2 Cl5 O4 108.77(10) . . ? O1 N1 Ru1 171.50(18) . . ? C1 N2 C5 119.3(2) . . ? C1 N2 Ru1 125.33(18) . . ? C5 N2 Ru1 115.36(15) . . ? C7 N3 C6 109.49(19) . . ? C7 N3 C13 110.01(18) . . ? C6 N3 C13 110.86(18) . . ? C7 N3 Ru1 105.35(14) . . ? C6 N3 Ru1 109.30(14) . . ? C13 N3 Ru1 111.67(15) . . ? C12 N4 C8 119.3(2) . . ? C12 N4 Ru1 126.33(17) . . ? C8 N4 Ru1 114.24(15) . . ? C18 N5 C14 117.4(2) . . ? N2 C1 C2 121.6(2) . . ? C1 C2 C3 119.6(2) . . ? C4 C3 C2 118.8(2) . . ? C5 C4 C3 119.5(2) . . ? N2 C5 C4 121.3(2) . . ? N2 C5 C6 118.0(2) . . ? C4 C5 C6 120.7(2) . . ? C5 C6 N3 114.6(2) . . ? C8 C7 N3 108.14(19) . . ? N4 C8 C9 121.6(2) . . ? N4 C8 C7 115.2(2) . . ? C9 C8 C7 123.2(2) . . ? C8 C9 C10 118.6(2) . . ? C11 C10 C9 119.6(2) . . ? C12 C11 C10 119.4(2) . . ? N4 C12 C11 121.5(2) . . ? C14 C13 N3 113.4(2) . . ? N5 C14 C15 122.9(2) . . ? N5 C14 C13 116.4(2) . . ? C15 C14 C13 120.8(2) . . ? C16 C15 C14 118.5(2) . . ? C17 C16 C15 119.1(2) . . ? C16 C17 C18 118.6(2) . . ? N5 C18 C17 123.5(2) . . ? Cl3 C19 Cl4 111.46(16) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 67.82 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.412 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.057 # Attachment '- [Ru(TPA)Cl2]ClO4.cif' data_ama _database_code_depnum_ccdc_archive 'CCDC 869446' #TrackingRef '- [Ru(TPA)Cl2]ClO4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 Cl2 N4 Ru, Cl O4, 0.5(C H4 O), 0.5(H2 O)' _chemical_formula_sum 'C18.50 H21 Cl3 N4 O5 Ru' _chemical_formula_weight 586.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4799(8) _cell_length_b 15.1542(12) _cell_length_c 14.4573(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.5790(10) _cell_angle_gamma 90.00 _cell_volume 2176.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 9479 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 29.35 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 1.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7071 _exptl_absorpt_correction_T_max 0.8955 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38. Sheldrick, G. SADABS (Version 2.10) Bruker/Siemens area detector absorption and other corrections, University of Gottingen, Germany 2003. ; _exptl_special_details ; 3730 frames x 15 sec. @ 5.055 cm; 0.5 deg. steps in omega & phi ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75588 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 29.65 _reflns_number_total 6147 _reflns_number_gt 5885 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART-APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+2.0366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6147 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 Ru1 Ru 0.294527(10) 0.185020(7) 0.695273(7) 0.01103(4) Uani 1 1 d . . . Cl1 Cl 0.51459(3) 0.19282(2) 0.68535(3) 0.01557(7) Uani 1 1 d . . . Cl2 Cl 0.20216(4) 0.23471(2) 0.53536(2) 0.01774(7) Uani 1 1 d . . . Cl3 Cl 0.79009(3) 0.09948(2) 0.00966(2) 0.01658(7) Uani 1 1 d . . . N1 N 0.29516(13) 0.05177(8) 0.66537(9) 0.0158(2) Uani 1 1 d . . . N2 N 0.35915(11) 0.13686(7) 0.83661(8) 0.0120(2) Uani 1 1 d . . . N3 N 0.10875(12) 0.18001(7) 0.71819(9) 0.0128(2) Uani 1 1 d . . . N4 N 0.32102(12) 0.30587(8) 0.76409(9) 0.0132(2) Uani 1 1 d . . . O1 O 0.68310(13) 0.09518(8) 0.05232(10) 0.0269(3) Uani 1 1 d . . . O2 O 0.76748(13) 0.03406(9) -0.06581(10) 0.0308(3) Uani 1 1 d . . . O3 O 0.78996(13) 0.18601(8) -0.03204(9) 0.0244(2) Uani 1 1 d . . . O4 O 0.91742(13) 0.08359(9) 0.08300(10) 0.0322(3) Uani 1 1 d . . . C1 C 0.23189(18) 0.01037(11) 0.58128(12) 0.0224(3) Uani 1 1 d . . . H1B H 0.1812 0.0440 0.5264 0.027 Uiso 1 1 calc R . . C2 C 0.2388(2) -0.08055(11) 0.57263(13) 0.0282(4) Uani 1 1 d . . . H2B H 0.1951 -0.1087 0.5121 0.034 Uiso 1 1 calc R . . C3 C 0.31004(19) -0.12966(11) 0.65305(13) 0.0262(3) Uani 1 1 d . . . H3B H 0.3145 -0.1921 0.6486 0.031 Uiso 1 1 calc R . . C4 C 0.37478(17) -0.08715(10) 0.74020(12) 0.0208(3) Uani 1 1 d . . . H4B H 0.4234 -0.1199 0.7964 0.025 Uiso 1 1 calc R . . C5 C 0.36740(15) 0.00400(9) 0.74414(11) 0.0162(3) Uani 1 1 d . . . C6 C 0.44126(14) 0.05633(9) 0.83377(10) 0.0151(2) Uani 1 1 d . . . H6A H 0.4536 0.0202 0.8931 0.018 Uiso 1 1 calc R . . H6B H 0.5311 0.0738 0.8313 0.018 Uiso 1 1 calc R . . C7 C 0.24133(14) 0.10869(9) 0.86747(10) 0.0141(2) Uani 1 1 d . . . H7A H 0.2338 0.0436 0.8638 0.017 Uiso 1 1 calc R . . H7B H 0.2578 0.1262 0.9363 0.017 Uiso 1 1 calc R . . C8 C 0.11171(14) 0.14810(9) 0.80599(10) 0.0132(2) Uani 1 1 d . . . C9 C -0.00205(14) 0.14587(10) 0.83522(10) 0.0161(3) Uani 1 1 d . . . H9A H 0.0028 0.1238 0.8978 0.019 Uiso 1 1 calc R . . C10 C -0.12277(15) 0.17634(10) 0.77177(11) 0.0180(3) Uani 1 1 d . . . H10A H -0.2024 0.1747 0.7897 0.022 Uiso 1 1 calc R . . C11 C -0.12565(15) 0.20935(11) 0.68148(11) 0.0193(3) Uani 1 1 d . . . H11A H -0.2075 0.2306 0.6369 0.023 Uiso 1 1 calc R . . C12 C -0.00850(14) 0.21108(10) 0.65692(11) 0.0170(3) Uani 1 1 d . . . H12A H -0.0106 0.2347 0.5956 0.020 Uiso 1 1 calc R . . C13 C 0.43928(14) 0.20941(9) 0.89941(10) 0.0149(2) Uani 1 1 d . . . H13A H 0.5343 0.2050 0.9013 0.018 Uiso 1 1 calc R . . H13B H 0.4366 0.2024 0.9669 0.018 Uiso 1 1 calc R . . C14 C 0.38480(14) 0.29901(9) 0.86115(10) 0.0139(2) Uani 1 1 d . . . C15 C 0.40706(16) 0.37259(10) 0.92146(11) 0.0182(3) Uani 1 1 d . . . H15A H 0.4490 0.3668 0.9899 0.022 Uiso 1 1 calc R . . C16 C 0.36701(17) 0.45474(10) 0.87999(12) 0.0211(3) Uani 1 1 d . . . H16A H 0.3832 0.5061 0.9197 0.025 Uiso 1 1 calc R . . C17 C 0.30335(17) 0.46133(10) 0.78042(12) 0.0210(3) Uani 1 1 d . . . H17A H 0.2763 0.5172 0.7510 0.025 Uiso 1 1 calc R . . C18 C 0.27966(15) 0.38531(9) 0.72425(11) 0.0168(3) Uani 1 1 d . . . H18A H 0.2333 0.3894 0.6562 0.020 Uiso 1 1 calc R . . O5 O -0.0102(3) 0.89387(18) 0.6678(2) 0.0308(5) Uani 0.50 1 d P A 1 H5 H -0.009(5) 0.885(3) 0.597(4) 0.034(12) Uiso 0.50 1 d P B 1 C19 C 0.0391(7) 0.9634(4) 0.7253(3) 0.0473(14) Uani 0.50 1 d P A 1 H19A H 0.0721 0.9442 0.7936 0.071 Uiso 0.50 1 calc PR A 1 H19B H -0.0322 1.0074 0.7173 0.071 Uiso 0.50 1 calc PR A 1 H19C H 0.1133 0.9895 0.7072 0.071 Uiso 0.50 1 calc PR A 1 O5A O -0.0243(6) 0.9829(3) 0.6636(6) 0.0599(17) Uani 0.50 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01459(6) 0.00946(6) 0.01043(6) 0.00048(3) 0.00596(4) 0.00031(3) Cl1 0.01651(14) 0.01525(14) 0.01745(15) -0.00029(11) 0.00894(12) -0.00032(11) Cl2 0.02241(16) 0.01995(15) 0.01200(14) 0.00333(11) 0.00709(12) 0.00185(12) Cl3 0.01820(15) 0.01634(15) 0.01574(14) -0.00175(11) 0.00619(12) -0.00019(11) N1 0.0220(6) 0.0118(5) 0.0167(5) -0.0013(4) 0.0106(5) -0.0010(4) N2 0.0146(5) 0.0099(5) 0.0125(5) 0.0009(4) 0.0059(4) 0.0013(4) N3 0.0149(5) 0.0117(5) 0.0128(5) -0.0002(4) 0.0059(4) -0.0007(4) N4 0.0169(5) 0.0104(5) 0.0142(5) 0.0008(4) 0.0078(4) 0.0006(4) O1 0.0346(6) 0.0221(6) 0.0336(6) 0.0076(5) 0.0242(5) 0.0049(5) O2 0.0303(6) 0.0315(7) 0.0296(6) -0.0173(5) 0.0080(5) -0.0008(5) O3 0.0280(6) 0.0234(6) 0.0230(6) 0.0066(4) 0.0099(5) -0.0030(4) O4 0.0271(6) 0.0294(6) 0.0303(6) -0.0010(5) -0.0049(5) 0.0048(5) C1 0.0337(8) 0.0179(7) 0.0179(7) -0.0032(5) 0.0114(6) -0.0032(6) C2 0.0452(10) 0.0186(7) 0.0243(8) -0.0080(6) 0.0161(7) -0.0059(7) C3 0.0411(9) 0.0130(6) 0.0308(8) -0.0048(6) 0.0206(7) -0.0018(6) C4 0.0290(7) 0.0126(6) 0.0262(7) 0.0009(5) 0.0167(6) 0.0027(5) C5 0.0209(6) 0.0126(6) 0.0189(6) 0.0001(5) 0.0118(5) 0.0014(5) C6 0.0176(6) 0.0111(6) 0.0182(6) 0.0014(5) 0.0078(5) 0.0037(5) C7 0.0159(6) 0.0137(6) 0.0145(6) 0.0031(5) 0.0075(5) 0.0015(5) C8 0.0160(6) 0.0108(6) 0.0134(6) -0.0004(4) 0.0057(5) -0.0002(4) C9 0.0183(6) 0.0166(6) 0.0152(6) 0.0002(5) 0.0079(5) -0.0009(5) C10 0.0161(6) 0.0203(7) 0.0190(7) -0.0007(5) 0.0078(5) -0.0008(5) C11 0.0151(6) 0.0236(7) 0.0184(7) 0.0029(6) 0.0040(5) 0.0008(5) C12 0.0167(6) 0.0186(6) 0.0153(6) 0.0026(5) 0.0044(5) -0.0001(5) C13 0.0189(6) 0.0121(6) 0.0130(6) 0.0003(5) 0.0040(5) -0.0003(5) C14 0.0172(6) 0.0122(6) 0.0141(6) 0.0007(5) 0.0074(5) -0.0002(5) C15 0.0253(7) 0.0156(6) 0.0154(6) -0.0019(5) 0.0091(5) -0.0021(5) C16 0.0317(8) 0.0130(6) 0.0221(7) -0.0034(5) 0.0136(6) -0.0009(6) C17 0.0317(8) 0.0115(6) 0.0232(7) 0.0013(5) 0.0134(6) 0.0021(5) C18 0.0237(7) 0.0122(6) 0.0164(6) 0.0025(5) 0.0090(5) 0.0022(5) O5 0.0255(12) 0.0285(13) 0.0412(15) -0.0036(11) 0.0143(11) -0.0040(10) C19 0.070(4) 0.046(3) 0.0233(18) -0.0073(18) 0.010(2) -0.031(3) O5A 0.061(3) 0.029(2) 0.114(5) -0.027(3) 0.061(4) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N4 2.0604(12) . ? Ru1 N1 2.0655(12) . ? Ru1 N2 2.0700(11) . ? Ru1 N3 2.0778(12) . ? Ru1 Cl2 2.3287(4) . ? Ru1 Cl1 2.3588(4) . ? Cl3 O4 1.4357(13) . ? Cl3 O2 1.4370(12) . ? Cl3 O1 1.4430(12) . ? Cl3 O3 1.4431(12) . ? N1 C1 1.341(2) . ? N1 C5 1.3581(19) . ? N2 C13 1.5008(18) . ? N2 C6 1.5012(17) . ? N2 C7 1.5024(17) . ? N3 C8 1.3493(17) . ? N3 C12 1.3501(18) . ? N4 C18 1.3452(17) . ? N4 C14 1.3523(18) . ? C1 C2 1.387(2) . ? C2 C3 1.382(3) . ? C3 C4 1.385(2) . ? C4 C5 1.386(2) . ? C5 C6 1.506(2) . ? C7 C8 1.4909(19) . ? C8 C9 1.3864(19) . ? C9 C10 1.384(2) . ? C10 C11 1.389(2) . ? C11 C12 1.383(2) . ? C13 C14 1.5082(19) . ? C14 C15 1.3886(19) . ? C15 C16 1.388(2) . ? C16 C17 1.384(2) . ? C17 C18 1.386(2) . ? O5 C19 1.340(5) . ? 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_3 _geom_angle_publ_flag N4 Ru1 N1 163.98(5) . . ? N4 Ru1 N2 83.42(5) . . ? N1 Ru1 N2 80.79(5) . . ? N4 Ru1 N3 86.82(5) . . ? N1 Ru1 N3 93.63(5) . . ? N2 Ru1 N3 81.85(5) . . ? N4 Ru1 Cl2 98.13(3) . . ? N1 Ru1 Cl2 97.84(4) . . ? N2 Ru1 Cl2 174.75(3) . . ? N3 Ru1 Cl2 93.20(3) . . ? N4 Ru1 Cl1 90.05(3) . . ? N1 Ru1 Cl1 88.16(4) . . ? N2 Ru1 Cl1 93.38(3) . . ? N3 Ru1 Cl1 174.56(3) . . ? Cl2 Ru1 Cl1 91.643(13) . . ? O4 Cl3 O2 109.55(8) . . ? O4 Cl3 O1 110.05(8) . . ? O2 Cl3 O1 109.31(8) . . ? O4 Cl3 O3 109.74(8) . . ? O2 Cl3 O3 109.37(8) . . ? O1 Cl3 O3 108.79(7) . . ? C1 N1 C5 119.56(13) . . ? C1 N1 Ru1 127.85(11) . . ? C5 N1 Ru1 112.56(10) . . ? C13 N2 C6 113.38(11) . . ? C13 N2 C7 112.51(11) . . ? C6 N2 C7 108.04(10) . . ? C13 N2 Ru1 106.43(8) . . ? C6 N2 Ru1 105.65(8) . . ? C7 N2 Ru1 110.61(8) . . ? C8 N3 C12 119.05(12) . . ? C8 N3 Ru1 114.91(9) . . ? C12 N3 Ru1 125.86(10) . . ? C18 N4 C14 119.89(12) . . ? C18 N4 Ru1 127.82(10) . . ? C14 N4 Ru1 112.25(9) . . ? N1 C1 C2 121.43(16) . . ? C3 C2 C1 119.26(16) . . ? C2 C3 C4 119.44(15) . . ? C3 C4 C5 118.92(15) . . ? N1 C5 C4 121.36(14) . . ? N1 C5 C6 115.92(12) . . ? C4 C5 C6 122.70(14) . . ? N2 C6 C5 108.04(11) . . ? C8 C7 N2 112.83(11) . . ? N3 C8 C9 122.09(13) . . ? N3 C8 C7 116.61(12) . . ? C9 C8 C7 121.14(12) . . ? C10 C9 C8 118.88(13) . . ? C9 C10 C11 118.98(14) . . ? C12 C11 C10 119.53(14) . . ? N3 C12 C11 121.46(13) . . ? N2 C13 C14 111.36(11) . . ? N4 C14 C15 121.23(13) . . ? N4 C14 C13 117.00(12) . . ? C15 C14 C13 121.62(13) . . ? C16 C15 C14 118.81(14) . . ? C17 C16 C15 119.57(14) . . ? C16 C17 C18 119.11(14) . . ? N4 C18 C17 121.33(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 Cl2 1.03(5) 2.94(5) 3.565(3) 120(3) 3_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.65 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.590 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.077