#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100949.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_1100949 _chemical_formula_sum 'C20 H22 Cu N5 O13 Tb' _chemical_formula_weight 762.89 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' 'Tb' 'Tb' -0.1723 4.1537 '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 8.611(3) _cell_length_b 13.814(5) _cell_length_c 21.244(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2527.1(14) _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 55 _exptl_crystal_size_mid 38 _exptl_crystal_size_min 22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1500 _exptl_absorpt_coefficient_mu 3.695 _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 2543 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0377 _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 1.92 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2543 _reflns_number_gt 2260 _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^)+(0.0234P)^2^+6.0316P] 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 SHELXL _refine_ls_extinction_coef 0.00057(9) _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 -0.01(3) _refine_ls_number_reflns 2543 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _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 Tb Tb 0.76036(4) 0.00144(3) 0.099217(17) 0.02796(13) Uani 1 1 d . . . Cu Cu 0.43712(13) -0.05640(8) 0.18330(6) 0.0346(3) Uani 1 1 d . . . O10 O 0.7837(8) 0.0080(6) -0.0155(3) 0.0488(17) Uani 1 1 d . . . N4 N 0.6419(10) -0.0074(7) -0.0285(4) 0.045(2) Uani 1 1 d . . . O12 O 0.8185(10) -0.0358(6) 0.2119(4) 0.050(2) Uani 1 1 d . . . O8 O 0.5937(11) -0.0039(7) -0.0813(4) 0.070(2) Uani 1 1 d . . . O1 O 0.5437(7) 0.0564(4) 0.1547(3) 0.0305(14) Uani 1 1 d . . . O9 O 0.5562(8) -0.0262(6) 0.0183(4) 0.055(2) Uani 1 1 d . . . N1 N 0.3012(9) 0.0136(6) 0.2382(4) 0.0366(18) Uani 1 1 d . . . O4 O 0.8190(7) -0.1820(4) 0.0702(3) 0.0375(16) Uani 1 1 d . . . O3 O 0.6635(7) 0.1759(4) 0.0759(3) 0.0317(14) Uani 1 1 d . . . O2 O 0.5933(8) -0.1233(4) 0.1367(3) 0.0387(17) Uani 1 1 d . . . C6 C 0.3563(11) 0.1719(7) 0.1949(5) 0.033(2) Uani 1 1 d . . . C2 C 0.5447(11) 0.2123(6) 0.1141(5) 0.034(2) Uani 1 1 d . . . N2 N 0.3258(10) -0.1698(6) 0.2087(4) 0.037(2) Uani 1 1 d . . . C18 C 0.8497(13) 0.3096(7) 0.0590(5) 0.048(3) Uani 1 1 d . . . H18A H 0.8940 0.3500 0.0269 0.072 Uiso 1 1 calc R . . H18B H 0.9308 0.2739 0.0796 0.072 Uiso 1 1 calc R . . H18C H 0.7968 0.3493 0.0893 0.072 Uiso 1 1 calc R . . C15 C 0.7181(12) -0.2541(6) 0.0903(4) 0.033(2) Uani 1 1 d . . . C10 C 0.3556(11) -0.2562(7) 0.1908(5) 0.036(2) Uani 1 1 d . . . H10A H 0.2896 -0.3049 0.2048 0.044 Uiso 1 1 calc R . . N3 N 1.0962(10) 0.0313(7) 0.0817(4) 0.045(2) Uani 1 1 d . . . O6 O 1.0362(8) -0.0370(5) 0.1119(4) 0.0491(18) Uani 1 1 d . . . C7 C 0.2793(11) 0.1058(7) 0.2374(5) 0.036(2) Uani 1 1 d . . . H7A H 0.2091 0.1316 0.2661 0.044 Uiso 1 1 calc R . . O13 O 0.8625(8) 0.1106(5) 0.1824(4) 0.0451(17) Uani 1 1 d . . . C11 C 0.4854(11) -0.2847(6) 0.1501(5) 0.034(2) Uani 1 1 d . . . C16 C 0.5952(11) -0.2191(6) 0.1261(5) 0.033(2) Uani 1 1 d . . . O7 O 0.9999(9) 0.0920(6) 0.0583(4) 0.060(2) Uani 1 1 d . . . O11 O 0.8993(10) 0.0718(7) 0.2803(4) 0.074(3) Uani 1 1 d . . . C1 C 0.4838(10) 0.1454(6) 0.1555(5) 0.031(2) Uani 1 1 d . . . C14 C 0.7296(13) -0.3518(7) 0.0751(5) 0.044(2) Uani 1 1 d . . . H14A H 0.8125 -0.3739 0.0510 0.053 Uiso 1 1 calc R . . C17 C 0.7359(12) 0.2400(6) 0.0296(4) 0.040(2) Uani 1 1 d . . . H17A H 0.6556 0.2765 0.0081 0.048 Uiso 1 1 calc R . . H17B H 0.7896 0.2011 -0.0016 0.048 Uiso 1 1 calc R . . C3 C 0.4841(11) 0.3060(6) 0.1094(5) 0.039(2) Uani 1 1 d . . . H3A H 0.5232 0.3492 0.0798 0.047 Uiso 1 1 calc R . . C19 C 0.9568(11) -0.2126(8) 0.0340(5) 0.042(2) Uani 1 1 d . . . H19A H 0.9990 -0.1573 0.0117 0.051 Uiso 1 1 calc R . . H19B H 0.9261 -0.2605 0.0029 0.051 Uiso 1 1 calc R . . C13 C 0.6155(13) -0.4170(7) 0.0962(5) 0.047(3) Uani 1 1 d . . . H13A H 0.6213 -0.4822 0.0856 0.056 Uiso 1 1 calc R . . C8 C 0.2233(12) -0.0526(7) 0.2832(4) 0.043(2) Uani 1 1 d . . . H8A H 0.1275 -0.0239 0.2983 0.051 Uiso 1 1 calc R . . H8B H 0.2902 -0.0650 0.3190 0.051 Uiso 1 1 calc R . . C9 C 0.1888(12) -0.1475(7) 0.2481(5) 0.043(2) Uani 1 1 d . . . H9A H 0.1703 -0.1994 0.2779 0.052 Uiso 1 1 calc R . . H9B H 0.0973 -0.1402 0.2219 0.052 Uiso 1 1 calc R . . C12 C 0.4984(14) -0.3839(7) 0.1317(5) 0.047(3) Uani 1 1 d . . . H12A H 0.4225 -0.4272 0.1449 0.056 Uiso 1 1 calc R . . C20 C 1.0810(14) -0.2552(9) 0.0762(6) 0.060(3) Uani 1 1 d . . . H20A H 1.1686 -0.2743 0.0511 0.090 Uiso 1 1 calc R . . H20B H 1.0401 -0.3107 0.0977 0.090 Uiso 1 1 calc R . . H20C H 1.1130 -0.2076 0.1064 0.090 Uiso 1 1 calc R . . N5 N 0.8603(10) 0.0494(8) 0.2259(5) 0.046(2) Uani 1 1 d . . . C4 C 0.3637(13) 0.3339(7) 0.1499(6) 0.050(3) Uani 1 1 d . . . H4A H 0.3257 0.3969 0.1484 0.060 Uiso 1 1 calc R . . C5 C 0.3018(12) 0.2691(7) 0.1915(5) 0.041(3) Uani 1 1 d . . . H5A H 0.2222 0.2889 0.2182 0.049 Uiso 1 1 calc R . . O5 O 1.2365(8) 0.0407(8) 0.0762(4) 0.080(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 Tb 0.02471(19) 0.0247(2) 0.0344(2) 0.0023(2) 0.00377(16) -0.0010(2) Cu 0.0297(6) 0.0256(5) 0.0487(6) 0.0034(5) 0.0100(6) -0.0018(5) O10 0.050(4) 0.053(4) 0.044(4) 0.000(4) 0.003(3) -0.010(5) N4 0.057(5) 0.033(4) 0.044(5) 0.000(5) -0.001(4) -0.006(5) O12 0.052(5) 0.051(5) 0.048(4) 0.016(4) 0.001(4) 0.003(4) O8 0.095(6) 0.061(5) 0.055(5) 0.000(5) -0.023(5) -0.013(6) O1 0.024(3) 0.023(3) 0.044(3) 0.006(3) 0.007(3) 0.004(3) O9 0.038(4) 0.065(5) 0.063(4) 0.000(4) 0.001(4) -0.008(4) N1 0.033(4) 0.036(4) 0.041(4) 0.002(4) 0.006(3) 0.001(4) O4 0.027(3) 0.029(3) 0.056(4) -0.001(3) 0.010(3) 0.001(3) O3 0.038(3) 0.025(3) 0.033(3) 0.002(3) 0.004(3) 0.000(3) O2 0.035(4) 0.021(3) 0.060(4) 0.006(3) 0.008(3) 0.001(3) C6 0.029(5) 0.034(5) 0.037(6) -0.007(4) -0.015(5) 0.005(4) C2 0.024(5) 0.024(4) 0.054(6) -0.003(4) -0.006(5) -0.003(4) N2 0.031(4) 0.037(4) 0.044(5) 0.010(4) 0.008(4) -0.007(4) C18 0.048(6) 0.038(6) 0.058(7) 0.001(5) 0.005(5) -0.013(5) C15 0.039(5) 0.028(4) 0.032(5) -0.002(4) -0.006(4) 0.007(4) C10 0.028(5) 0.029(5) 0.052(7) 0.012(5) -0.003(5) -0.008(4) N3 0.032(4) 0.055(6) 0.048(5) -0.011(4) 0.005(4) -0.006(4) O6 0.037(4) 0.042(4) 0.068(5) 0.009(4) 0.005(4) 0.001(3) C7 0.023(4) 0.044(5) 0.043(5) 0.001(5) 0.000(4) 0.005(4) O13 0.050(4) 0.036(4) 0.049(4) -0.001(4) -0.005(4) 0.002(3) C11 0.036(5) 0.024(4) 0.041(5) 0.006(4) -0.010(5) -0.010(4) C16 0.030(5) 0.024(4) 0.044(5) 0.006(4) -0.006(5) -0.003(4) O7 0.044(4) 0.064(5) 0.073(6) 0.023(5) -0.002(4) -0.013(4) O11 0.071(6) 0.108(7) 0.044(4) -0.023(5) -0.016(4) 0.043(6) C1 0.020(4) 0.023(4) 0.049(6) 0.003(4) -0.006(4) 0.002(4) C14 0.046(6) 0.029(5) 0.057(6) -0.005(4) -0.008(6) 0.005(5) C17 0.046(6) 0.030(4) 0.045(5) 0.008(4) 0.008(5) 0.003(5) C3 0.034(5) 0.020(4) 0.063(7) 0.008(5) -0.012(5) 0.000(4) C19 0.031(5) 0.043(5) 0.053(7) -0.004(5) 0.011(5) 0.009(5) C13 0.060(7) 0.032(5) 0.049(6) -0.001(5) -0.004(6) -0.005(5) C8 0.039(5) 0.043(5) 0.045(5) 0.009(5) 0.013(5) 0.000(5) C9 0.033(5) 0.046(6) 0.050(6) 0.013(5) -0.003(5) -0.004(5) C12 0.058(7) 0.026(5) 0.056(7) 0.008(5) -0.008(6) -0.015(5) C20 0.044(6) 0.054(7) 0.083(9) -0.013(7) 0.000(6) 0.008(6) N5 0.031(5) 0.059(6) 0.049(6) -0.008(5) 0.000(4) 0.021(5) C4 0.044(6) 0.025(5) 0.081(8) 0.007(5) -0.003(6) 0.009(5) C5 0.035(5) 0.037(5) 0.051(6) -0.009(5) 0.001(5) 0.013(4) O5 0.027(4) 0.123(8) 0.090(6) -0.004(6) 0.011(4) -0.024(5) _cod_database_code 1100949