#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100946.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_1100946 _chemical_formula_sum 'C20 H22 Ce Cu N5 O13' _chemical_formula_weight 744.09 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.697(6) _cell_length_b 13.905(6) _cell_length_c 21.176(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2561(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour Red _exptl_crystal_size_max 58 _exptl_crystal_size_mid 36 _exptl_crystal_size_min 20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.930 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 2.662 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2575 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2575 _reflns_number_gt 2059 _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^)+(0.0157P)^2^+5.4164P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_number_reflns 2575 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 Ce Ce 1.74099(6) 0.49939(5) 0.09408(2) 0.02818(13) Uani 1 1 d . . . Cu Cu 2.06776(15) 0.44371(9) 0.18283(7) 0.0344(3) Uani 1 1 d . . . N1 N 2.2012(9) 0.5131(7) 0.2389(4) 0.037(2) Uani 1 1 d . . . O1 O 1.9626(8) 0.5565(5) 0.1537(3) 0.0331(16) Uani 1 1 d . . . C15 C 1.7935(12) 0.2427(7) 0.0899(5) 0.033(2) Uani 1 1 d . . . O2 O 1.9163(9) 0.3747(5) 0.1366(4) 0.0383(18) Uani 1 1 d . . . C1 C 2.0225(12) 0.6451(7) 0.1550(5) 0.034(2) Uani 1 1 d . . . O4 O 1.6895(8) 0.3118(5) 0.0688(4) 0.0382(19) Uani 1 1 d . . . N2 N 2.1801(11) 0.3319(7) 0.2094(5) 0.035(2) Uani 1 1 d . . . C10 C 2.1522(14) 0.2458(8) 0.1921(6) 0.039(3) Uani 1 1 d . . . H10A H 2.2177 0.1980 0.2070 0.046 Uiso 1 1 calc R . . C9 C 2.3158(14) 0.3555(9) 0.2499(6) 0.043(3) Uani 1 1 d . . . H9B H 2.3351 0.3039 0.2797 0.051 Uiso 1 1 calc R . . H9A H 2.4068 0.3642 0.2241 0.051 Uiso 1 1 calc R . . C13 C 1.9008(15) 0.0821(7) 0.0977(6) 0.055(3) Uani 1 1 d . . . H13A H 1.8972 0.0171 0.0875 0.065 Uiso 1 1 calc R . . C6 C 2.1437(14) 0.6706(8) 0.1967(6) 0.035(3) Uani 1 1 d . . . C12 C 2.0153(15) 0.1166(7) 0.1337(6) 0.048(3) Uani 1 1 d . . . H12A H 2.0905 0.0743 0.1480 0.058 Uiso 1 1 calc R . . C11 C 2.0260(13) 0.2157(8) 0.1507(6) 0.037(3) Uani 1 1 d . . . C5 C 2.1996(15) 0.7678(8) 0.1941(6) 0.045(3) Uani 1 1 d . . . H5A H 2.2785 0.7869 0.2210 0.054 Uiso 1 1 calc R . . C7 C 2.2206(13) 0.6059(8) 0.2392(5) 0.041(3) Uani 1 1 d . . . H7A H 2.2882 0.6319 0.2687 0.049 Uiso 1 1 calc R . . C16 C 1.9138(13) 0.2795(7) 0.1270(5) 0.033(3) Uani 1 1 d . . . O10 O 1.7326(9) 0.5145(6) -0.0258(3) 0.051(2) Uani 1 1 d . . . O8 O 1.9289(12) 0.5029(7) -0.0886(4) 0.070(2) Uani 1 1 d . . . N4 N 1.8730(11) 0.4945(9) -0.0370(4) 0.046(2) Uani 1 1 d . . . O13 O 1.6338(10) 0.6135(6) 0.1794(4) 0.048(2) Uani 1 1 d . . . O12 O 1.6759(11) 0.4688(6) 0.2129(4) 0.052(3) Uani 1 1 d . . . O3 O 1.8467(8) 0.6762(5) 0.0745(3) 0.0345(18) Uani 1 1 d . . . O9 O 1.9528(9) 0.4687(6) 0.0103(4) 0.053(2) Uani 1 1 d . . . O7 O 1.4930(10) 0.5831(7) 0.0487(5) 0.067(3) Uani 1 1 d . . . O5 O 1.2581(10) 0.5403(9) 0.0726(5) 0.090(4) Uani 1 1 d . . . N5 N 1.6347(12) 0.5553(9) 0.2241(6) 0.055(3) Uani 1 1 d . . . C19 C 1.5519(13) 0.2799(8) 0.0355(5) 0.042(3) Uani 1 1 d . . . H19B H 1.5804 0.2315 0.0047 0.051 Uiso 1 1 calc R . . H19A H 1.5079 0.3339 0.0129 0.051 Uiso 1 1 calc R . . O6 O 1.4521(10) 0.4626(6) 0.1113(4) 0.054(2) Uani 1 1 d . . . O11 O 1.5946(12) 0.5752(8) 0.2779(4) 0.083(4) Uani 1 1 d . . . C14 C 1.7847(14) 0.1462(8) 0.0754(5) 0.040(3) Uani 1 1 d . . . H14A H 1.7035 0.1230 0.0513 0.048 Uiso 1 1 calc R . . C8 C 2.2780(13) 0.4464(8) 0.2842(5) 0.044(3) Uani 1 1 d . . . H8B H 2.2102 0.4328 0.3194 0.052 Uiso 1 1 calc R . . H8A H 2.3712 0.4756 0.3005 0.052 Uiso 1 1 calc R . . C17 C 1.7734(15) 0.7405(7) 0.0284(5) 0.047(3) Uani 1 1 d . . . H17B H 1.7231 0.7022 -0.0039 0.056 Uiso 1 1 calc R . . H17A H 1.8518 0.7791 0.0079 0.056 Uiso 1 1 calc R . . N3 N 1.3963(12) 0.5274(8) 0.0767(5) 0.050(3) Uani 1 1 d . . . C20 C 1.4345(15) 0.2394(10) 0.0783(7) 0.061(4) Uani 1 1 d . . . H20A H 1.3466 0.2196 0.0542 0.092 Uiso 1 1 calc R . . H20C H 1.4041 0.2874 0.1084 0.092 Uiso 1 1 calc R . . H20B H 1.4766 0.1850 0.1002 0.092 Uiso 1 1 calc R . . C4 C 2.1388(15) 0.8319(8) 0.1529(6) 0.052(3) Uani 1 1 d . . . H4A H 2.1757 0.8946 0.1518 0.063 Uiso 1 1 calc R . . C2 C 1.9643(12) 0.7134(7) 0.1135(5) 0.030(3) Uani 1 1 d . . . C3 C 2.0206(13) 0.8041(8) 0.1120(6) 0.042(3) Uani 1 1 d . . . H3A H 1.9804 0.8484 0.0835 0.051 Uiso 1 1 calc R . . C18 C 1.6574(16) 0.8057(8) 0.0585(6) 0.056(4) Uani 1 1 d . . . H18A H 1.6125 0.8464 0.0269 0.084 Uiso 1 1 calc R . . H18C H 1.7071 0.8447 0.0899 0.084 Uiso 1 1 calc R . . H18B H 1.5784 0.7678 0.0781 0.084 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 Ce 0.0272(2) 0.0235(2) 0.0339(2) 0.0023(3) -0.0037(3) 0.0012(4) Cu 0.0329(7) 0.0253(6) 0.0450(7) 0.0043(6) -0.0096(7) 0.0006(6) N1 0.029(4) 0.045(6) 0.037(4) 0.005(5) -0.009(3) -0.002(5) O1 0.032(4) 0.021(3) 0.045(4) 0.002(4) -0.011(4) -0.004(3) C15 0.037(6) 0.025(5) 0.036(6) 0.000(5) -0.002(5) 0.001(4) O2 0.034(4) 0.027(3) 0.054(5) -0.005(3) -0.009(4) -0.001(4) C1 0.033(6) 0.020(5) 0.048(6) 0.004(5) 0.004(6) -0.001(4) O4 0.034(4) 0.031(4) 0.049(5) 0.001(3) -0.013(4) -0.002(3) N2 0.023(5) 0.044(6) 0.038(6) 0.015(5) -0.003(4) 0.009(4) C10 0.037(7) 0.032(6) 0.047(8) 0.011(5) -0.001(6) 0.010(5) C9 0.038(6) 0.051(7) 0.038(6) 0.011(6) -0.011(6) 0.006(6) C13 0.069(9) 0.026(6) 0.069(8) 0.004(6) 0.002(8) 0.008(6) C6 0.030(6) 0.028(5) 0.048(8) -0.007(5) -0.006(6) -0.009(5) C12 0.064(8) 0.022(5) 0.059(8) 0.004(5) 0.011(7) 0.007(6) C11 0.035(6) 0.035(6) 0.040(6) 0.009(5) 0.007(6) -0.001(5) C5 0.047(8) 0.033(6) 0.054(8) -0.003(6) -0.008(6) -0.015(5) C7 0.034(6) 0.046(6) 0.044(6) -0.003(6) -0.002(6) -0.005(6) C16 0.033(6) 0.030(5) 0.037(6) 0.001(5) 0.007(6) 0.005(5) O10 0.053(5) 0.056(6) 0.045(4) 0.003(4) 0.000(4) 0.011(5) O8 0.093(6) 0.064(5) 0.053(5) 0.001(6) 0.019(5) 0.017(8) N4 0.063(6) 0.037(5) 0.037(5) -0.002(6) 0.010(5) 0.001(7) O13 0.054(5) 0.046(5) 0.042(5) -0.001(4) 0.005(4) -0.001(4) O12 0.052(5) 0.056(6) 0.048(5) 0.012(4) -0.003(4) -0.004(4) O3 0.038(4) 0.021(3) 0.045(5) 0.003(3) -0.007(4) 0.008(3) O9 0.042(4) 0.064(6) 0.054(5) -0.002(4) -0.001(4) 0.011(4) O7 0.045(5) 0.087(7) 0.070(6) 0.036(6) -0.002(5) 0.020(5) O5 0.030(4) 0.129(10) 0.110(8) 0.003(7) -0.005(6) 0.029(6) N5 0.044(6) 0.065(8) 0.055(7) -0.020(7) 0.005(6) -0.020(7) C19 0.035(6) 0.047(6) 0.045(7) -0.005(6) -0.013(6) -0.008(6) O6 0.046(5) 0.045(4) 0.073(6) 0.008(4) -0.002(5) -0.006(4) O11 0.082(7) 0.114(9) 0.052(5) -0.035(6) 0.021(6) -0.044(7) C14 0.045(7) 0.034(6) 0.040(6) -0.005(5) 0.002(5) -0.001(5) C8 0.041(7) 0.046(6) 0.044(6) 0.008(6) -0.008(6) -0.003(6) C17 0.066(8) 0.026(5) 0.049(6) 0.016(5) -0.012(7) -0.002(6) N3 0.040(6) 0.059(7) 0.051(6) -0.006(5) -0.008(5) 0.013(5) C20 0.041(7) 0.060(8) 0.082(10) -0.010(8) 0.003(8) -0.016(7) C4 0.058(8) 0.026(5) 0.073(9) 0.009(6) -0.001(7) -0.012(6) C2 0.030(6) 0.023(5) 0.038(6) -0.001(4) 0.016(5) 0.002(5) C3 0.038(6) 0.031(6) 0.058(8) 0.006(6) 0.001(6) 0.002(5) C18 0.061(8) 0.034(6) 0.072(9) -0.005(7) -0.021(8) 0.007(6)