#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100939.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_1100939 _chemical_formula_sum 'C28 H22 Cl2 N6 O4 Ru' _chemical_formula_weight 678.49 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' 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 'Monoclinic' 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 14.3980(8) _cell_length_b 12.1620(9) _cell_length_c 15.4770(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.644(6) _cell_angle_gamma 90.00 _cell_volume 2707.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.5900 _cell_measurement_theta_max 12.4500 _exptl_crystal_description Square _exptl_crystal_colour Brown _exptl_crystal_size_max '0.30 mm' _exptl_crystal_size_mid '0.20 mm' _exptl_crystal_size_min '0.20 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.966 _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 4396 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.94 _reflns_number_total 4396 _reflns_number_gt 3960 _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^)+(0.0454P)^2^+3.9339P] 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 4396 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.081 _refine_ls_shift/su_mean 0.010 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 0.137754(19) 0.26465(2) 0.137761(18) 0.03327(11) Uani 1 d . . . Cl1 Cl 0.16385(7) 0.45547(8) 0.17676(6) 0.0449(2) Uani 1 d . . . Cl2 Cl 0.75961(8) 0.00094(11) 0.13424(8) 0.0642(3) Uani 1 d . . . N1 N 0.3816(2) 0.0852(3) 0.1201(2) 0.0469(8) Uani 1 d . . . N2 N 0.2777(2) 0.2158(3) 0.1449(2) 0.0384(7) Uani 1 d . . . N3 N 0.1281(2) 0.0981(3) 0.11455(19) 0.0384(7) Uani 1 d . . . N4 N 0.0924(2) 0.2298(2) 0.25946(19) 0.0379(7) Uani 1 d . . . N5 N 0.0065(2) 0.3006(2) 0.1212(2) 0.0361(7) Uani 1 d . . . N6 N 0.1335(2) 0.3100(3) 0.00955(19) 0.0389(7) Uani 1 d . . . C1 C 0.4228(4) -0.0212(5) 0.1009(4) 0.0693(15) Uani 1 d . . . C2 C 0.3658(3) 0.2636(3) 0.1493(2) 0.0433(9) Uani 1 d . . . C3 C 0.3937(3) 0.3706(4) 0.1668(3) 0.0559(11) Uani 1 d . . . C4 C 0.4882(4) 0.3912(5) 0.1683(4) 0.0691(14) Uani 1 d . . . C5 C 0.5527(3) 0.3086(5) 0.1542(3) 0.0693(14) Uani 1 d . . . C6 C 0.5262(3) 0.2042(5) 0.1360(3) 0.0614(13) Uani 1 d . . . C7 C 0.4305(3) 0.1815(4) 0.1340(3) 0.0475(10) Uani 1 d . . . C8 C 0.2904(3) 0.1099(3) 0.1277(2) 0.0393(8) Uani 1 d . . . C9 C 0.2090(3) 0.0397(3) 0.1186(2) 0.0417(9) Uani 1 d . . . C10 C 0.2079(4) -0.0739(4) 0.1170(3) 0.0553(11) Uani 1 d . . . C11 C 0.1251(4) -0.1289(4) 0.1107(3) 0.0647(14) Uani 1 d . . . C12 C 0.0438(3) -0.0706(4) 0.1048(3) 0.0562(11) Uani 1 d . . . C13 C 0.0483(3) 0.0424(3) 0.1066(3) 0.0472(10) Uani 1 d . . . C14 C 0.1407(3) 0.1872(4) 0.3277(3) 0.0497(10) Uani 1 d . . . C15 C 0.1009(4) 0.1669(4) 0.4055(3) 0.0643(13) Uani 1 d . . . C16 C 0.0078(4) 0.1920(5) 0.4147(3) 0.0671(14) Uani 1 d . . . C17 C -0.0425(4) 0.2343(4) 0.3449(3) 0.0557(11) Uani 1 d . . . C18 C 0.0000(3) 0.2515(3) 0.2673(3) 0.0417(9) Uani 1 d . . . C19 C -0.0495(3) 0.2936(3) 0.1888(3) 0.0413(9) Uani 1 d . . . C20 C -0.1418(3) 0.3237(4) 0.1783(3) 0.0543(11) Uani 1 d . . . C21 C -0.1749(3) 0.3626(4) 0.0990(4) 0.0608(13) Uani 1 d . . . C22 C -0.1169(3) 0.3715(3) 0.0312(3) 0.0498(10) Uani 1 d . . . C23 C -0.0251(3) 0.3392(3) 0.0434(2) 0.0395(8) Uani 1 d . . . C24 C 0.0472(3) 0.3439(3) -0.0206(2) 0.0379(8) Uani 1 d . . . C25 C 0.0321(3) 0.3800(3) -0.1047(3) 0.0496(10) Uani 1 d . . . C26 C 0.1051(4) 0.3835(4) -0.1590(3) 0.0594(12) Uani 1 d . . . C27 C 0.1920(4) 0.3495(4) -0.1292(3) 0.0651(13) Uani 1 d . . . C28 C 0.2031(3) 0.3125(4) -0.0454(3) 0.0545(11) Uani 1 d . . . O1 O 0.7408(6) 0.1074(6) 0.1143(8) 0.260(5) Uani 1 d . . . O2 O 0.8239(4) -0.0301(8) 0.0809(4) 0.190(4) Uani 1 d . . . O3 O 0.7932(6) -0.0124(10) 0.2163(4) 0.244(5) Uani 1 d . . . O4 O 0.6758(4) -0.0487(6) 0.1201(6) 0.197(4) Uani 1 d . . . H13 H -0.005(3) 0.082(3) 0.102(2) 0.041(11) Uiso 1 d . . . H22 H -0.138(3) 0.402(3) -0.022(3) 0.047(11) Uiso 1 d . . . H28 H 0.260(4) 0.291(5) -0.024(4) 0.085(18) Uiso 1 d . . . H25 H -0.026(3) 0.400(4) -0.127(3) 0.059(13) Uiso 1 d . . . H14 H 0.200(3) 0.169(4) 0.321(3) 0.049(12) Uiso 1 d . . . H9 H 0.353(3) 0.421(4) 0.174(3) 0.052(13) Uiso 1 d . . . H10 H 0.265(3) -0.108(4) 0.125(3) 0.059(13) Uiso 1 d . . . H26 H 0.099(3) 0.408(4) -0.213(3) 0.053(12) Uiso 1 d . . . H12 H -0.018(3) -0.104(4) 0.100(3) 0.067(14) Uiso 1 d . . . H20 H -0.177(3) 0.322(4) 0.220(3) 0.055(13) Uiso 1 d . . . H1 H 0.416(3) -0.077(5) 0.153(3) 0.079(16) Uiso 1 d . . . H6 H 0.572(4) 0.147(4) 0.128(3) 0.067(14) Uiso 1 d . . . H27 H 0.245(4) 0.352(5) -0.173(4) 0.10(2) Uiso 1 d . . . H4 H 0.505(3) 0.458(4) 0.182(3) 0.059(14) Uiso 1 d . . . H21 H -0.237(4) 0.382(4) 0.092(3) 0.078(16) Uiso 1 d . . . H15 H 0.141(4) 0.135(5) 0.450(4) 0.091(18) Uiso 1 d . . . H17 H -0.109(4) 0.258(4) 0.350(4) 0.078(16) Uiso 1 d . . . H5 H 0.621(4) 0.327(5) 0.155(4) 0.091(17) Uiso 1 d . . . H11 H 0.124(4) -0.203(6) 0.113(4) 0.10(2) Uiso 1 d . . . H16 H -0.020(4) 0.168(6) 0.473(4) 0.12(2) Uiso 1 d . . . H1B H 0.484(4) -0.005(4) 0.099(3) 0.060(14) Uiso 1 d . . . H1A H 0.395(4) -0.048(5) 0.040(4) 0.10(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 0.03010(16) 0.03443(17) 0.03493(17) 0.00055(12) -0.00239(11) 0.00441(12) Cl1 0.0439(5) 0.0380(5) 0.0520(6) -0.0010(4) -0.0070(4) 0.0032(4) Cl2 0.0531(6) 0.0683(8) 0.0728(8) -0.0064(6) 0.0190(6) 0.0017(6) N1 0.0430(19) 0.050(2) 0.0483(19) 0.0103(16) 0.0060(15) 0.0178(16) N2 0.0343(16) 0.0401(18) 0.0404(17) 0.0041(14) -0.0014(13) 0.0042(13) N3 0.0405(18) 0.0389(17) 0.0355(17) -0.0027(13) -0.0020(13) 0.0033(13) N4 0.0441(17) 0.0343(16) 0.0351(16) -0.0009(13) -0.0009(13) -0.0019(13) N5 0.0324(15) 0.0334(16) 0.0423(17) -0.0026(13) -0.0018(13) 0.0010(12) N6 0.0384(17) 0.0396(17) 0.0386(17) -0.0013(14) 0.0011(14) 0.0079(14) C1 0.065(3) 0.063(3) 0.082(4) 0.009(3) 0.024(3) 0.033(3) C2 0.034(2) 0.056(2) 0.040(2) 0.0121(18) -0.0020(16) 0.0017(17) C3 0.043(2) 0.057(3) 0.067(3) 0.007(2) -0.003(2) -0.003(2) C4 0.049(3) 0.080(4) 0.077(4) 0.009(3) -0.003(2) -0.019(3) C5 0.037(2) 0.104(4) 0.067(3) 0.021(3) 0.003(2) -0.003(3) C6 0.036(2) 0.091(4) 0.058(3) 0.027(3) 0.007(2) 0.010(2) C7 0.040(2) 0.062(3) 0.041(2) 0.0176(19) 0.0030(17) 0.012(2) C8 0.040(2) 0.040(2) 0.038(2) 0.0059(16) -0.0004(16) 0.0097(16) C9 0.048(2) 0.041(2) 0.036(2) -0.0009(16) -0.0027(16) 0.0090(17) C10 0.061(3) 0.043(2) 0.062(3) -0.003(2) -0.008(2) 0.012(2) C11 0.082(4) 0.037(3) 0.074(3) -0.006(2) -0.013(3) -0.003(2) C12 0.057(3) 0.047(3) 0.064(3) -0.007(2) -0.008(2) -0.010(2) C13 0.047(2) 0.042(2) 0.051(2) -0.0066(19) -0.0100(19) 0.0008(19) C14 0.057(3) 0.047(2) 0.044(2) 0.0030(19) -0.005(2) -0.003(2) C15 0.079(4) 0.068(3) 0.045(3) 0.013(2) -0.009(2) -0.007(3) C16 0.084(4) 0.071(3) 0.048(3) 0.002(2) 0.012(3) -0.017(3) C17 0.060(3) 0.055(3) 0.054(3) -0.001(2) 0.011(2) -0.013(2) C18 0.042(2) 0.036(2) 0.047(2) -0.0051(16) 0.0037(17) -0.0073(16) C19 0.037(2) 0.037(2) 0.051(2) -0.0037(17) 0.0040(17) -0.0048(16) C20 0.035(2) 0.058(3) 0.071(3) -0.002(2) 0.012(2) 0.0003(19) C21 0.030(2) 0.064(3) 0.089(4) 0.001(3) 0.000(2) 0.005(2) C22 0.038(2) 0.046(2) 0.064(3) 0.001(2) -0.014(2) 0.0032(18) C23 0.040(2) 0.0309(19) 0.046(2) -0.0040(16) -0.0107(17) 0.0005(15) C24 0.038(2) 0.0338(19) 0.041(2) -0.0027(16) -0.0053(16) 0.0041(15) C25 0.059(3) 0.041(2) 0.047(2) -0.0003(18) -0.017(2) 0.004(2) C26 0.079(3) 0.065(3) 0.034(2) 0.003(2) 0.000(2) 0.012(3) C27 0.071(3) 0.075(3) 0.051(3) 0.008(2) 0.016(2) 0.022(3) C28 0.053(3) 0.065(3) 0.046(2) 0.006(2) 0.005(2) 0.017(2) O1 0.166(7) 0.098(5) 0.518(18) 0.002(8) 0.025(9) 0.011(5) O2 0.114(4) 0.363(11) 0.094(4) -0.025(5) 0.029(3) 0.089(6) O3 0.193(7) 0.457(16) 0.080(4) 0.004(6) -0.005(4) -0.008(9) O4 0.090(4) 0.186(7) 0.311(10) 0.096(6) -0.043(5) -0.050(4) _cod_database_code 1100939