#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100951.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_1100951 _chemical_formula_sum 'C20 H22 Cu Ho N5 O13' _chemical_formula_weight 768.90 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' 'Ho' 'Ho' -0.2175 4.6783 '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 8.583(3) _cell_length_b 13.749(3) _cell_length_c 21.191(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2500.8(10) _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 48 _exptl_crystal_size_mid 28 _exptl_crystal_size_min 12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 4.070 _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 2518 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0648 _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 25.00 _reflns_number_total 2518 _reflns_number_gt 1899 _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^)+(0.0571P)^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 SHELXL _refine_ls_extinction_coef 0.00021(14) _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 0.02(4) _refine_ls_number_reflns 2518 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.1003 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _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 Ho Ho 0.25990(6) 0.49805(6) 0.10040(3) 0.0310(2) Uani 1 1 d . . . Cu Cu -0.0624(2) 0.55616(13) 0.18325(9) 0.0377(5) Uani 1 1 d . . . N1 N -0.2004(14) 0.4870(10) 0.2380(6) 0.043(3) Uani 1 1 d . . . N2 N -0.1735(16) 0.6681(10) 0.2095(7) 0.043(4) Uani 1 1 d . . . O2 O 0.0930(13) 0.6239(6) 0.1362(5) 0.041(3) Uani 1 1 d . . . O10 O 0.2866(11) 0.4948(11) -0.0128(5) 0.052(3) Uani 1 1 d . . . N4 N 0.1442(16) 0.5042(13) -0.0255(6) 0.052(3) Uani 1 1 d . . . O8 O 0.1029(16) 0.5068(11) -0.0808(5) 0.073(4) Uani 1 1 d . . . O9 O 0.0591(14) 0.5242(9) 0.0206(6) 0.065(4) Uani 1 1 d . . . O4 O 0.3190(11) 0.6810(7) 0.0703(5) 0.037(2) Uani 1 1 d . . . O12 O 0.3176(16) 0.5375(10) 0.2113(6) 0.056(4) Uani 1 1 d . . . C15 C 0.2179(17) 0.7545(10) 0.0897(7) 0.037(3) Uani 1 1 d . . . O13 O 0.3604(11) 0.3904(8) 0.1841(5) 0.046(3) Uani 1 1 d . . . O11 O 0.3990(16) 0.4294(12) 0.2803(5) 0.082(5) Uani 1 1 d . . . C16 C 0.0949(18) 0.7193(10) 0.1263(7) 0.032(4) Uani 1 1 d . . . O6 O 0.5344(13) 0.5376(8) 0.1119(6) 0.055(3) Uani 1 1 d . . . C10 C -0.143(2) 0.7574(12) 0.1900(10) 0.051(5) Uani 1 1 d . . . H10A H -0.2091 0.8064 0.2038 0.061 Uiso 1 1 calc R . . C14 C 0.233(2) 0.8502(10) 0.0744(7) 0.044(4) Uani 1 1 d . . . H14A H 0.3162 0.8720 0.0503 0.053 Uiso 1 1 calc R . . C11 C -0.0168(17) 0.7859(10) 0.1498(7) 0.034(3) Uani 1 1 d . . . N3 N 0.5952(15) 0.4670(11) 0.0825(7) 0.050(4) Uani 1 1 d . . . C12 C -0.0003(19) 0.8827(10) 0.1324(8) 0.044(4) Uani 1 1 d . . . H12A H -0.0742 0.9273 0.1463 0.053 Uiso 1 1 calc R . . C19 C 0.4544(17) 0.7100(11) 0.0331(7) 0.043(4) Uani 1 1 d . . . H19B H 0.4233 0.7584 0.0022 0.051 Uiso 1 1 calc R . . H19A H 0.4946 0.6540 0.0105 0.051 Uiso 1 1 calc R . . O7 O 0.5023(14) 0.4052(9) 0.0598(6) 0.062(4) Uani 1 1 d . . . C13 C 0.1179(19) 0.9151(11) 0.0962(8) 0.051(4) Uani 1 1 d . . . H13A H 0.1236 0.9806 0.0855 0.061 Uiso 1 1 calc R . . O1 O 0.0472(11) 0.4433(7) 0.1545(4) 0.032(2) Uani 1 1 d . . . O3 O 0.1658(11) 0.3248(7) 0.0772(4) 0.035(2) Uani 1 1 d . . . C7 C -0.2217(17) 0.3951(11) 0.2370(7) 0.036(3) Uani 1 1 d . . . H7A H -0.2931 0.3692 0.2654 0.044 Uiso 1 1 calc R . . O5 O 0.7330(13) 0.4614(13) 0.0761(7) 0.088(5) Uani 1 1 d . . . C1 C -0.0126(15) 0.3544(9) 0.1550(7) 0.030(3) Uani 1 1 d . . . C9 C -0.3111(18) 0.6460(12) 0.2486(8) 0.044(4) Uani 1 1 d . . . H9A H -0.4030 0.6397 0.2223 0.053 Uiso 1 1 calc R . . H9B H -0.3288 0.6977 0.2789 0.053 Uiso 1 1 calc R . . C17 C 0.240(2) 0.2604(11) 0.0314(7) 0.050(4) Uani 1 1 d . . . H17B H 0.2979 0.2995 0.0013 0.059 Uiso 1 1 calc R . . H17A H 0.1599 0.2257 0.0083 0.059 Uiso 1 1 calc R . . C8 C -0.2785(18) 0.5531(11) 0.2816(7) 0.045(4) Uani 1 1 d . . . H8B H -0.2126 0.5650 0.3180 0.054 Uiso 1 1 calc R . . H8A H -0.3752 0.5243 0.2962 0.054 Uiso 1 1 calc R . . C20 C 0.580(2) 0.7512(12) 0.0744(9) 0.059(5) Uani 1 1 d . . . H20A H 0.6672 0.7697 0.0489 0.089 Uiso 1 1 calc R . . H20C H 0.6117 0.7031 0.1045 0.089 Uiso 1 1 calc R . . H20B H 0.5404 0.8073 0.0962 0.089 Uiso 1 1 calc R . . C2 C 0.0434(19) 0.2879(11) 0.1140(8) 0.041(4) Uani 1 1 d . . . C6 C -0.1438(19) 0.3289(11) 0.1953(8) 0.035(4) Uani 1 1 d . . . N5 N 0.3584(17) 0.4522(14) 0.2269(7) 0.051(4) Uani 1 1 d . . . C3 C -0.0142(19) 0.1919(11) 0.1084(9) 0.050(4) Uani 1 1 d . . . H3A H 0.0269 0.1481 0.0794 0.060 Uiso 1 1 calc R . . C5 C -0.194(2) 0.2306(11) 0.1915(9) 0.047(4) Uani 1 1 d . . . H5A H -0.2705 0.2091 0.2195 0.056 Uiso 1 1 calc R . . C4 C -0.136(2) 0.1668(12) 0.1486(9) 0.057(5) Uani 1 1 d . . . H4A H -0.1781 0.1046 0.1460 0.068 Uiso 1 1 calc R . . C18 C 0.3472(19) 0.1888(11) 0.0601(9) 0.052(5) Uani 1 1 d . . . H18A H 0.3920 0.1489 0.0277 0.078 Uiso 1 1 calc R . . H18C H 0.2905 0.1486 0.0892 0.078 Uiso 1 1 calc R . . H18B H 0.4286 0.2224 0.0822 0.078 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 Ho 0.0272(3) 0.0269(3) 0.0387(3) -0.0030(4) 0.0035(3) 0.0005(4) Cu 0.0327(9) 0.0281(8) 0.0523(11) -0.0037(9) 0.0098(9) 0.0029(8) N1 0.035(6) 0.051(8) 0.042(7) -0.013(7) 0.007(5) -0.003(7) N2 0.033(7) 0.041(7) 0.055(10) -0.019(7) 0.003(7) 0.007(6) O2 0.043(6) 0.013(4) 0.066(8) 0.002(5) 0.018(6) 0.004(5) O10 0.048(6) 0.049(6) 0.060(6) -0.003(7) 0.012(5) 0.006(8) N4 0.070(9) 0.039(7) 0.046(8) 0.003(10) 0.004(7) -0.004(11) O8 0.099(9) 0.073(8) 0.048(6) 0.002(8) -0.010(7) 0.023(10) O9 0.046(6) 0.083(11) 0.065(7) 0.006(7) 0.007(6) 0.003(7) O4 0.035(5) 0.030(5) 0.047(6) 0.001(5) 0.003(5) 0.002(5) O12 0.051(8) 0.052(7) 0.063(9) -0.004(7) 0.004(7) 0.003(6) C15 0.033(8) 0.030(7) 0.047(9) -0.005(6) -0.003(7) 0.001(6) O13 0.039(6) 0.055(7) 0.045(7) 0.002(6) -0.008(5) 0.002(5) O11 0.080(9) 0.125(13) 0.040(7) 0.019(8) -0.016(7) -0.054(10) C16 0.030(9) 0.028(7) 0.040(8) -0.002(7) -0.003(7) 0.004(7) O6 0.039(6) 0.045(6) 0.079(8) -0.007(6) 0.008(7) 0.008(5) C10 0.050(11) 0.031(8) 0.072(14) -0.012(9) -0.013(10) 0.021(8) C14 0.053(10) 0.029(7) 0.051(9) 0.003(6) -0.006(9) -0.008(8) C11 0.037(8) 0.026(7) 0.040(8) -0.011(7) -0.002(8) 0.012(7) N3 0.030(7) 0.058(9) 0.061(9) 0.019(7) 0.005(7) 0.010(7) C12 0.045(9) 0.025(7) 0.063(11) -0.007(7) -0.005(8) 0.005(7) C19 0.039(8) 0.038(8) 0.051(10) -0.001(7) 0.012(8) -0.004(7) O7 0.052(7) 0.066(8) 0.069(8) -0.022(7) -0.008(7) 0.015(7) C13 0.056(10) 0.034(8) 0.064(11) 0.007(8) -0.001(9) 0.009(8) O1 0.027(5) 0.027(5) 0.043(5) -0.007(5) 0.012(5) 0.000(5) O3 0.038(6) 0.034(5) 0.033(5) -0.011(5) 0.003(5) -0.001(5) C7 0.031(8) 0.042(8) 0.037(8) -0.001(7) 0.000(7) -0.008(7) O5 0.035(6) 0.129(13) 0.101(10) 0.021(9) 0.006(7) 0.018(8) C1 0.020(7) 0.023(6) 0.046(8) -0.005(6) -0.005(6) 0.004(6) C9 0.035(8) 0.053(10) 0.045(10) -0.015(8) 0.006(8) 0.003(8) C17 0.067(11) 0.039(8) 0.043(9) 0.000(7) 0.005(10) 0.016(10) C8 0.038(9) 0.042(8) 0.055(9) -0.009(8) 0.015(8) -0.001(8) C20 0.049(10) 0.045(10) 0.084(13) 0.005(9) -0.006(10) -0.037(9) C2 0.032(9) 0.038(8) 0.054(11) 0.003(8) -0.011(9) 0.001(7) C6 0.036(9) 0.040(8) 0.029(8) -0.004(7) 0.003(7) -0.002(7) N5 0.033(8) 0.079(11) 0.041(9) -0.006(9) 0.013(7) -0.020(8) C3 0.044(9) 0.036(9) 0.069(12) -0.001(9) -0.006(10) -0.002(7) C5 0.055(11) 0.033(8) 0.052(11) 0.015(8) 0.004(9) -0.004(8) C4 0.050(10) 0.029(8) 0.091(14) -0.010(9) 0.002(10) -0.005(8) C18 0.052(10) 0.031(8) 0.072(12) 0.008(8) 0.028(9) 0.001(8)