#------------------------------------------------------------------------------ #$Date: 2008-02-25 19:08:55 +0200 (Mon, 25 Feb 2008) $ #$Revision: 178 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100943.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_1100943 _chemical_formula_sum 'C27 H19 Cl2 N5 O5 Ru' _chemical_formula_weight 665.44 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' 'O' 'O' 0.0106 0.0060 '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' '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 'Orthorhombic' _symmetry_space_group_name_H-M 'P c a b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 11.1910(11) _cell_length_b 14.1940(10) _cell_length_c 33.1510(10) _cell_angle_alpha 90.000(4) _cell_angle_beta 90.000(6) _cell_angle_gamma 90.000(7) _cell_volume 5265.9(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.2500 _cell_measurement_theta_max 11.4900 _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max '0.40 mm' _exptl_crystal_size_mid '0.25 mm' _exptl_crystal_size_min '0.25 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.991 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; psi-scan (North, Philips & Mathews, 1968) ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type ' MoK\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% <3% _diffrn_reflns_number 3762 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 24.93 _reflns_number_total 3762 _reflns_number_gt 3143 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+9.2470P] 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 3762 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.20425(3) 0.02081(2) 0.609164(10) 0.02978(12) Uani 1 d . . . Cl1 Cl 0.33954(12) 0.03038(9) 0.55306(4) 0.0520(3) Uani 1 d . . . Cl2 Cl 0.21929(11) 0.78348(9) 0.73381(4) 0.0489(3) Uani 1 d . . . N1 N 0.1571(3) -0.1203(2) 0.60040(10) 0.0323(8) Uani 1 d . . . N2 N 0.0817(3) -0.0012(2) 0.65447(10) 0.0328(8) Uani 1 d . . . N3 N 0.3481(3) 0.0038(2) 0.64719(11) 0.0345(8) Uani 1 d . . . N4 N 0.2374(3) 0.1514(2) 0.62216(11) 0.0345(8) Uani 1 d . . . N5 N 0.0732(3) 0.0873(3) 0.57515(10) 0.0371(9) Uani 1 d . . . O1 O 0.0309(3) -0.2359(2) 0.61805(9) 0.0440(8) Uani 1 d . . . O2 O 0.1360(5) 0.7365(4) 0.75821(14) 0.1091(17) Uani 1 d . . . O3 O 0.3385(4) 0.7590(3) 0.74464(13) 0.0885(14) Uani 1 d . . . O4 O 0.2059(4) 0.8825(3) 0.73881(15) 0.0937(15) Uani 1 d . . . O5 O 0.2014(3) 0.7599(3) 0.69238(11) 0.0678(10) Uani 1 d . . . C1 C 0.1111(4) -0.2727(3) 0.59005(14) 0.0425(11) Uani 1 d . . . C2 C 0.1142(6) -0.3627(4) 0.57473(18) 0.0609(16) Uani 1 d . . . C3 C 0.2062(7) -0.3801(4) 0.54820(18) 0.0689(18) Uani 1 d . . . C4 C 0.2897(6) -0.3120(4) 0.53774(16) 0.0580(15) Uani 1 d . . . C5 C 0.2833(5) -0.2212(4) 0.55262(15) 0.0456(12) Uani 1 d . . . C6 C 0.1901(4) -0.2024(3) 0.57940(12) 0.0354(10) Uani 1 d . . . C7 C 0.0676(4) -0.1453(3) 0.62321(13) 0.0353(10) Uani 1 d . . . C8 C 0.0194(4) -0.0838(3) 0.65303(13) 0.0335(10) Uani 1 d . . . C9 C -0.0708(5) -0.1055(3) 0.67987(16) 0.0463(12) Uani 1 d . . . C10 C -0.0997(5) -0.0412(4) 0.70957(15) 0.0487(13) Uani 1 d . . . C11 C -0.0363(5) 0.0413(3) 0.71170(15) 0.0445(12) Uani 1 d . . . C12 C 0.0524(5) 0.0583(3) 0.68431(14) 0.0392(11) Uani 1 d . . . C13 C 0.4033(4) -0.0763(4) 0.65777(15) 0.0415(11) Uani 1 d . . . C14 C 0.5039(5) -0.0777(4) 0.68121(16) 0.0516(13) Uani 1 d . . . C15 C 0.5488(5) 0.0052(4) 0.69585(16) 0.0549(14) Uani 1 d . . . C16 C 0.4928(5) 0.0885(4) 0.68620(15) 0.0487(13) Uani 1 d . . . C17 C 0.3921(4) 0.0869(3) 0.66154(12) 0.0372(10) Uani 1 d . . . C18 C 0.3283(4) 0.1712(3) 0.64763(13) 0.0373(10) Uani 1 d . . . C19 C 0.3522(5) 0.2635(4) 0.65785(16) 0.0486(13) Uani 1 d . . . C20 C 0.2849(6) 0.3347(4) 0.64127(17) 0.0610(15) Uani 1 d . . . C21 C 0.1933(5) 0.3140(3) 0.61481(17) 0.0543(14) Uani 1 d . . . C22 C 0.1697(4) 0.2204(3) 0.60513(13) 0.0386(10) Uani 1 d . . . C23 C 0.0761(4) 0.1830(3) 0.57867(13) 0.0404(11) Uani 1 d . . . C24 C -0.0047(5) 0.2396(4) 0.55808(17) 0.0557(14) Uani 1 d . . . C25 C -0.0892(6) 0.1997(5) 0.53408(19) 0.0669(17) Uani 1 d . . . C26 C -0.0926(5) 0.1038(5) 0.53026(17) 0.0606(16) Uani 1 d . . . C27 C -0.0105(4) 0.0496(4) 0.55140(15) 0.0468(12) Uani 1 d . . . H27 H -0.016(4) -0.019(3) 0.5521(13) 0.045(13) Uiso 1 d . . . H9 H -0.105(4) -0.160(3) 0.6763(13) 0.039(13) Uiso 1 d . . . H13 H 0.370(4) -0.125(3) 0.6481(12) 0.025(11) Uiso 1 d . . . H12 H 0.095(4) 0.103(3) 0.6875(14) 0.041(14) Uiso 1 d . . . H11 H -0.056(4) 0.079(3) 0.7314(13) 0.034(12) Uiso 1 d . . . H10 H -0.163(4) -0.055(3) 0.7269(13) 0.035(11) Uiso 1 d . . . H5 H 0.332(4) -0.179(3) 0.5448(12) 0.026(12) Uiso 1 d . . . H15 H 0.622(5) 0.012(3) 0.7136(16) 0.068(16) Uiso 1 d . . . H26 H -0.144(5) 0.076(4) 0.5158(15) 0.053(16) Uiso 1 d . . . H20 H 0.305(4) 0.398(4) 0.6481(15) 0.064(16) Uiso 1 d . . . H14 H 0.529(5) -0.134(4) 0.6879(15) 0.055(16) Uiso 1 d . . . H4 H 0.353(4) -0.326(3) 0.5184(14) 0.057(15) Uiso 1 d . . . H21 H 0.154(5) 0.358(4) 0.6021(16) 0.070(19) Uiso 1 d . . . H19 H 0.405(4) 0.273(3) 0.6733(14) 0.045(15) Uiso 1 d . . . H3 H 0.199(6) -0.443(5) 0.534(2) 0.12(2) Uiso 1 d . . . H2 H 0.065(5) -0.407(4) 0.5825(16) 0.063(17) Uiso 1 d . . . H16 H 0.516(5) 0.140(4) 0.6956(16) 0.062(17) Uiso 1 d . . . H24 H 0.004(5) 0.302(4) 0.5614(18) 0.09(2) Uiso 1 d . . . H25 H -0.141(6) 0.230(4) 0.5199(17) 0.08(2) Uiso 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 0.03124(19) 0.02602(18) 0.03206(19) 0.00011(15) -0.00159(15) -0.00257(15) Cl1 0.0583(7) 0.0507(7) 0.0471(7) 0.0055(6) 0.0158(6) -0.0029(6) Cl2 0.0435(7) 0.0478(7) 0.0554(7) -0.0088(5) -0.0022(6) 0.0027(6) N1 0.0328(19) 0.0315(19) 0.0327(19) -0.0021(15) -0.0029(15) -0.0014(16) N2 0.0344(19) 0.0298(19) 0.0342(18) 0.0011(14) -0.0035(15) 0.0017(15) N3 0.0307(18) 0.035(2) 0.038(2) -0.0004(15) -0.0011(16) -0.0030(15) N4 0.039(2) 0.0271(18) 0.0370(19) -0.0005(15) 0.0029(16) -0.0046(16) N5 0.040(2) 0.039(2) 0.0324(19) 0.0010(16) -0.0031(17) 0.0007(17) O1 0.0492(19) 0.0303(17) 0.0524(19) -0.0035(14) 0.0029(16) -0.0096(15) O2 0.114(4) 0.114(4) 0.100(4) 0.012(3) 0.032(3) -0.042(3) O3 0.069(3) 0.105(3) 0.092(3) -0.039(3) -0.031(2) 0.033(3) O4 0.106(4) 0.052(2) 0.123(4) -0.029(2) 0.009(3) 0.014(2) O5 0.070(3) 0.072(3) 0.062(2) -0.010(2) -0.014(2) 0.000(2) C1 0.049(3) 0.034(2) 0.044(3) -0.006(2) -0.008(2) 0.002(2) C2 0.088(5) 0.030(3) 0.065(4) -0.007(3) 0.002(3) -0.006(3) C3 0.102(5) 0.044(3) 0.060(3) -0.019(3) -0.010(4) 0.014(4) C4 0.072(4) 0.056(3) 0.046(3) -0.009(3) 0.001(3) 0.024(3) C5 0.046(3) 0.049(3) 0.041(3) -0.003(2) -0.001(2) 0.006(3) C6 0.039(3) 0.034(2) 0.033(2) -0.0052(18) -0.008(2) 0.003(2) C7 0.039(3) 0.025(2) 0.042(2) 0.0013(18) -0.003(2) -0.0060(19) C8 0.032(2) 0.033(2) 0.036(2) -0.0011(19) -0.0018(19) -0.0011(19) C9 0.045(3) 0.035(3) 0.059(3) 0.004(2) 0.008(2) -0.004(2) C10 0.047(3) 0.055(3) 0.044(3) 0.009(2) 0.017(2) 0.009(3) C11 0.056(3) 0.042(3) 0.035(3) 0.004(2) 0.008(2) 0.013(2) C12 0.048(3) 0.030(2) 0.039(3) -0.004(2) -0.005(2) 0.004(2) C13 0.041(3) 0.038(3) 0.046(3) 0.001(2) -0.007(2) 0.006(2) C14 0.047(3) 0.055(3) 0.053(3) 0.005(3) -0.009(2) 0.012(3) C15 0.043(3) 0.070(4) 0.051(3) 0.005(3) -0.013(2) -0.002(3) C16 0.045(3) 0.059(4) 0.042(3) -0.008(3) -0.007(2) -0.014(3) C17 0.039(3) 0.040(3) 0.032(2) -0.0039(19) 0.002(2) -0.005(2) C18 0.041(3) 0.036(2) 0.034(2) -0.0023(19) 0.002(2) -0.011(2) C19 0.049(3) 0.044(3) 0.053(3) -0.007(2) -0.012(3) -0.012(3) C20 0.080(4) 0.039(3) 0.065(3) -0.011(3) 0.001(3) -0.019(3) C21 0.069(4) 0.029(2) 0.065(4) 0.003(2) 0.006(3) 0.003(3) C22 0.042(3) 0.032(2) 0.042(3) 0.001(2) 0.006(2) 0.002(2) C23 0.043(3) 0.039(2) 0.039(2) 0.006(2) 0.004(2) 0.004(2) C24 0.060(3) 0.050(4) 0.056(3) 0.006(3) -0.003(3) 0.015(3) C25 0.062(4) 0.073(4) 0.066(4) 0.013(3) -0.012(3) 0.023(3) C26 0.047(3) 0.079(4) 0.056(3) 0.005(3) -0.018(3) -0.002(3) C27 0.046(3) 0.050(3) 0.045(3) 0.003(2) -0.007(2) -0.002(2)