#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100938.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100938 _chemical_formula_moiety 'C27 H20 N7 O Ru.2(ClO4).(NO3).(H2O).0.5(C6H6) _chemical_formula_sum 'C30 H25 Cl2 N8 O13 Ru' _chemical_formula_weight 877.55 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.07(3) _cell_length_b 9.625(8) _cell_length_c 19.353(16) _cell_angle_alpha 90.00 _cell_angle_beta 111.644(13) _cell_angle_gamma 90.00 _cell_volume 6765(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used '1115' _cell_measurement_theta_min '2.22' _cell_measurement_theta_max '17.30' _exptl_crystal_description 'Needle' _exptl_crystal_colour 'Brown' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 0.702 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8654 _exptl_absorpt_correction_T_max 0.9578 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_ambient_temperature 293(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_device ' Bruker Smart APEX' _diffrn_measurement_method 'Omega Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22233 _diffrn_reflns_av_R_equivalents 0.1745 _diffrn_reflns_av_sigmaI/netI 0.1605 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 23.50 _reflns_number_total 5014 _reflns_number_gt 2526 _reflns_threshold_expression >2sigma(I) _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^)+(0.0786P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5014 _refine_ls_number_parameters 487 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.1679 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1846 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _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 Ru Ru 0.12471(2) 0.84864(9) 0.17243(4) 0.0412(3) Uani 1 1 d . . . O1 O 0.1400(2) 1.0578(9) 0.0822(4) 0.068(2) Uani 1 1 d . . . N1 N 0.1589(2) 0.9334(8) 0.2711(4) 0.041(2) Uani 1 1 d . . . N2 N 0.1241(2) 0.6962(8) 0.2504(4) 0.041(2) Uani 1 1 d . . . N3 N 0.1601(2) 0.7138(8) 0.1505(4) 0.044(2) Uani 1 1 d . . . N4 N 0.0893(2) 0.7377(9) 0.0904(4) 0.044(2) Uani 1 1 d . . . N5 N 0.0756(2) 0.9324(9) 0.1702(4) 0.044(2) Uani 1 1 d . . . N6 N 0.1322(2) 0.9777(11) 0.1165(4) 0.052(3) Uani 1 1 d . . . N7 N 0.1861(2) 0.9175(9) 0.3931(4) 0.054(3) Uani 1 1 d . . . H7 H 0.1933 0.8820 0.4369 0.065 Uiso 1 1 calc R . . C1 C 0.1941(3) 1.0491(12) 0.3749(6) 0.053(3) Uani 1 1 d . . . C2 C 0.2129(3) 1.1583(14) 0.4190(7) 0.079(4) Uani 1 1 d . . . H2 H 0.2235 1.1511 0.4705 0.095 Uiso 1 1 calc R . . C3 C 0.2151(4) 1.2779(14) 0.3824(7) 0.087(5) Uani 1 1 d . . . H3 H 0.2280 1.3529 0.4102 0.105 Uiso 1 1 calc R . . C4 C 0.1988(3) 1.2926(12) 0.3052(7) 0.076(4) Uani 1 1 d . . . H4 H 0.2011 1.3754 0.2825 0.091 Uiso 1 1 calc R . . C5 C 0.1791(3) 1.1813(11) 0.2626(6) 0.059(3) Uani 1 1 d . . . H5 H 0.1676 1.1896 0.2113 0.070 Uiso 1 1 calc R . . C6 C 0.1771(3) 1.0595(11) 0.2978(6) 0.047(3) Uani 1 1 d . . . C7 C 0.1652(2) 0.8564(11) 0.3306(5) 0.042(3) Uani 1 1 d . . . C8 C 0.1486(3) 0.7208(11) 0.3214(5) 0.042(3) Uani 1 1 d . . . C9 C 0.1555(3) 0.6242(12) 0.3766(6) 0.055(3) Uani 1 1 d . . . H9 H 0.1723 0.6424 0.4241 0.066 Uiso 1 1 calc R . . C10 C 0.1366(3) 0.4970(13) 0.3603(6) 0.067(4) Uani 1 1 d . . . H10 H 0.1404 0.4295 0.3968 0.080 Uiso 1 1 calc R . . C11 C 0.1126(3) 0.4755(12) 0.2894(6) 0.060(3) Uani 1 1 d . . . H11 H 0.0999 0.3918 0.2771 0.072 Uiso 1 1 calc R . . C12 C 0.1070(3) 0.5743(12) 0.2367(6) 0.063(3) Uani 1 1 d . . . H12 H 0.0905 0.5560 0.1888 0.076 Uiso 1 1 calc R . . C13 C 0.1969(3) 0.7019(11) 0.1841(6) 0.054(3) Uani 1 1 d . . . H13 H 0.2091 0.7648 0.2216 0.065 Uiso 1 1 calc R . . C14 C 0.2169(3) 0.6042(13) 0.1668(7) 0.075(4) Uani 1 1 d . . . H14 H 0.2422 0.6000 0.1922 0.090 Uiso 1 1 calc R . . C15 C 0.2000(4) 0.5119(13) 0.1119(8) 0.077(4) Uani 1 1 d . . . H15 H 0.2135 0.4446 0.0988 0.093 Uiso 1 1 calc R . . C16 C 0.1627(3) 0.5193(12) 0.0764(6) 0.062(3) Uani 1 1 d . . . H16 H 0.1507 0.4558 0.0390 0.075 Uiso 1 1 calc R . . C17 C 0.1429(3) 0.6195(11) 0.0953(5) 0.046(3) Uani 1 1 d . . . C18 C 0.1028(3) 0.6368(11) 0.0607(5) 0.043(3) Uani 1 1 d . . . C19 C 0.0780(3) 0.5629(12) 0.0021(6) 0.060(3) Uani 1 1 d . . . H19 H 0.0863 0.4933 -0.0212 0.072 Uiso 1 1 calc R . . C20 C 0.0416(3) 0.5923(13) -0.0211(6) 0.066(4) Uani 1 1 d . . . H20 H 0.0250 0.5422 -0.0602 0.080 Uiso 1 1 calc R . . C21 C 0.0290(3) 0.6954(12) 0.0125(6) 0.056(3) Uani 1 1 d . . . H21 H 0.0039 0.7142 -0.0037 0.067 Uiso 1 1 calc R . . C22 C 0.0528(3) 0.7695(12) 0.0691(5) 0.049(3) Uani 1 1 d . . . C23 C 0.0452(3) 0.8811(11) 0.1133(5) 0.049(3) Uani 1 1 d . . . C24 C 0.0119(3) 0.9361(12) 0.0992(6) 0.058(3) Uani 1 1 d . . . H24 H -0.0081 0.9013 0.0600 0.069 Uiso 1 1 calc R . . C25 C 0.0066(3) 1.0440(13) 0.1417(7) 0.070(4) Uani 1 1 d . . . H25 H -0.0167 1.0813 0.1323 0.084 Uiso 1 1 calc R . . C26 C 0.0369(3) 1.0927(13) 0.1977(7) 0.072(4) Uani 1 1 d . . . H26 H 0.0345 1.1658 0.2270 0.086 Uiso 1 1 calc R . . C27 C 0.0708(3) 1.0362(12) 0.2116(6) 0.055(3) Uani 1 1 d . . . H27 H 0.0910 1.0707 0.2507 0.066 Uiso 1 1 calc R . . Cl1 Cl 0.23176(9) 0.1366(4) 0.09661(18) 0.0746(10) Uani 1 1 d U . . O2 O 0.2004(2) 0.2002(8) 0.0419(4) 0.085(3) Uani 1 1 d U . . O3 O 0.2217(3) 0.0263(12) 0.1322(6) 0.138(4) Uani 1 1 d U . . O4 O 0.2542(3) 0.0922(11) 0.0574(7) 0.132(4) Uani 1 1 d U . . O5 O 0.2515(3) 0.2363(11) 0.1454(6) 0.150(4) Uani 1 1 d U . . Cl2 Cl 0.10266(8) 0.1164(3) 0.41833(15) 0.0599(8) Uani 1 1 d U . . O6 O 0.0828(3) 0.2141(8) 0.3621(4) 0.089(3) Uani 1 1 d U . . O7 O 0.0812(2) 0.0796(8) 0.4603(4) 0.067(2) Uani 1 1 d U . . O8 O 0.1102(2) -0.0030(9) 0.3825(5) 0.085(2) Uani 1 1 d U . . O9 O 0.1359(2) 0.1789(10) 0.4668(5) 0.094(3) Uani 1 1 d U . . N8 N 0.0732(3) 0.2906(10) 0.0988(5) 0.052(3) Uani 1 1 d . . . O10 O 0.0504(2) 0.3701(9) 0.1145(4) 0.081(3) Uani 1 1 d . . . O11 O 0.0603(2) 0.2091(10) 0.0485(5) 0.093(3) Uani 1 1 d . . . O12 O 0.1041(3) 0.2985(10) 0.1356(6) 0.122(4) Uani 1 1 d . . . C28 C 0.0173(5) 0.7346(19) 0.2768(10) 0.134(7) Uani 1 1 d . . . H28 H 0.0295 0.8181 0.2936 0.161 Uiso 1 1 calc R . . C29 C 0.0336(5) 0.613(2) 0.3054(10) 0.125(7) Uani 1 1 d . . . H29 H 0.0564 0.6127 0.3443 0.150 Uiso 1 1 calc R . . C30 C 0.0163(5) 0.490(2) 0.2762(9) 0.129(7) Uani 1 1 d . . . H30 H 0.0279 0.4065 0.2941 0.155 Uiso 1 1 calc R . . O13 O 0.1014(3) 0.7384(9) 0.4566(5) 0.107(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0369(5) 0.0400(5) 0.0353(5) -0.0032(5) -0.0001(3) -0.0024(5) O1 0.069(6) 0.079(7) 0.048(5) 0.014(5) 0.014(4) -0.011(5) N1 0.042(5) 0.034(5) 0.037(5) -0.002(4) 0.003(4) -0.007(4) N2 0.038(5) 0.040(6) 0.035(5) 0.002(4) 0.003(4) -0.006(4) N3 0.032(5) 0.047(6) 0.039(5) 0.000(4) -0.003(4) -0.003(4) N4 0.046(6) 0.044(6) 0.029(5) -0.011(4) -0.001(4) -0.007(5) N5 0.052(6) 0.040(6) 0.035(5) -0.004(4) 0.010(4) 0.002(4) N6 0.036(5) 0.085(8) 0.029(5) -0.005(5) 0.006(4) -0.008(5) N7 0.058(6) 0.048(6) 0.034(5) -0.003(4) -0.009(4) -0.013(5) C1 0.048(7) 0.046(8) 0.045(7) -0.002(6) -0.007(5) -0.011(6) C2 0.089(9) 0.061(9) 0.061(8) -0.010(8) -0.005(7) -0.023(8) C3 0.101(11) 0.049(9) 0.071(9) -0.015(8) -0.016(8) -0.011(8) C4 0.066(8) 0.042(8) 0.093(10) -0.001(7) -0.003(7) -0.021(7) C5 0.056(7) 0.036(8) 0.066(8) -0.003(6) 0.002(6) -0.008(6) C6 0.035(6) 0.036(7) 0.051(7) -0.009(6) -0.006(5) -0.009(5) C7 0.033(6) 0.044(7) 0.040(6) -0.008(6) 0.002(5) -0.011(6) C8 0.048(7) 0.032(7) 0.037(6) -0.003(5) 0.007(5) 0.001(5) C9 0.054(7) 0.060(9) 0.042(6) -0.010(6) 0.008(5) 0.000(7) C10 0.077(9) 0.056(9) 0.056(8) 0.001(7) 0.011(7) -0.002(7) C11 0.075(9) 0.043(8) 0.055(7) -0.007(6) 0.015(7) -0.021(6) C12 0.074(9) 0.050(8) 0.054(7) -0.004(7) 0.010(6) -0.033(7) C13 0.058(8) 0.037(7) 0.059(7) -0.008(6) 0.011(6) 0.002(6) C14 0.057(8) 0.073(10) 0.079(9) -0.008(8) 0.006(7) 0.027(7) C15 0.069(10) 0.054(9) 0.101(10) -0.021(8) 0.022(8) 0.012(7) C16 0.064(9) 0.059(9) 0.052(7) -0.017(6) 0.007(6) -0.001(7) C17 0.054(7) 0.039(8) 0.044(6) -0.007(5) 0.016(6) 0.007(6) C18 0.058(7) 0.033(7) 0.033(5) -0.011(5) 0.011(5) -0.008(6) C19 0.077(10) 0.049(8) 0.050(7) -0.011(6) 0.020(7) -0.007(7) C20 0.053(9) 0.066(9) 0.054(7) -0.006(7) -0.010(6) -0.014(7) C21 0.041(7) 0.066(9) 0.049(7) -0.009(6) 0.003(6) -0.007(6) C22 0.045(7) 0.053(8) 0.036(6) -0.006(6) 0.000(5) -0.010(6) C23 0.037(7) 0.052(8) 0.041(6) 0.007(6) -0.004(5) 0.002(6) C24 0.035(7) 0.064(9) 0.064(8) -0.007(7) 0.006(6) -0.004(6) C25 0.056(8) 0.072(10) 0.079(9) -0.003(8) 0.021(7) 0.012(7) C26 0.052(8) 0.079(10) 0.078(9) -0.011(7) 0.017(7) 0.003(7) C27 0.044(7) 0.058(8) 0.053(7) -0.007(6) 0.005(6) -0.009(6) Cl1 0.073(2) 0.061(2) 0.068(2) 0.0003(19) 0.0007(17) 0.013(2) O2 0.082(5) 0.067(6) 0.072(5) -0.003(4) -0.012(4) 0.013(4) O3 0.119(8) 0.136(8) 0.136(8) 0.067(7) 0.022(6) 0.006(6) O4 0.131(8) 0.112(8) 0.167(9) 0.027(6) 0.070(7) 0.046(6) O5 0.139(8) 0.116(7) 0.105(7) -0.022(6) -0.060(6) -0.004(6) Cl2 0.0633(19) 0.059(2) 0.0507(17) 0.0015(15) 0.0137(15) -0.0005(16) O6 0.126(7) 0.063(5) 0.061(5) 0.016(4) 0.013(4) 0.014(5) O7 0.063(5) 0.080(6) 0.059(5) -0.002(4) 0.022(4) -0.004(4) O8 0.103(7) 0.077(6) 0.078(5) 0.000(4) 0.037(5) 0.018(5) O9 0.055(5) 0.116(7) 0.093(6) -0.014(5) 0.007(4) -0.020(5) N8 0.035(6) 0.037(6) 0.061(6) -0.007(5) -0.010(5) -0.001(5) O10 0.068(6) 0.067(7) 0.084(6) -0.010(5) 0.002(5) -0.003(5) O11 0.077(6) 0.097(8) 0.090(7) -0.047(6) 0.013(5) -0.010(5) O12 0.064(7) 0.120(9) 0.130(8) -0.059(7) -0.026(6) 0.025(6) C28 0.16(2) 0.093(13) 0.13(2) -0.013(12) 0.033(14) -0.013(13) C29 0.102(14) 0.16(2) 0.096(13) -0.007(14) 0.013(10) 0.006(14) C30 0.15(2) 0.112(14) 0.107(17) 0.014(12) 0.025(12) 0.028(13) O13 0.134(8) 0.069(7) 0.115(7) -0.003(6) 0.043(7) -0.004(6)