#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100953.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_1100953 _chemical_formula_sum 'C20 H22 Cu N5 O13 Yb' _chemical_formula_weight 777.01 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' 'Yb' 'Yb' -0.3850 5.5486 '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 8.576(3) _cell_length_b 13.705(3) _cell_length_c 21.114(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2481.6(12) _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 45 _exptl_crystal_size_mid 30 _exptl_crystal_size_min 15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 4.682 _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 2485 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0239 _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 1.77 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2485 _reflns_number_gt 2307 _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^)+(0.0811P)^2^+10.5328P] 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 0.00(3) _refine_ls_number_reflns 2485 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.1137 _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 Yb Yb 0.25866(5) 0.00072(3) 0.10166(2) 0.0283(2) Uani 1 1 d . . . Cu Cu -0.06187(18) -0.05762(10) 0.18298(8) 0.0346(4) Uani 1 1 d . . . O10 O 0.2911(12) 0.0075(8) -0.0087(5) 0.046(2) Uani 1 1 d . . . N4 N 0.1507(15) -0.0081(8) -0.0243(6) 0.045(3) Uani 1 1 d . . . O8 O 0.1059(16) -0.0054(8) -0.0786(5) 0.069(3) Uani 1 1 d . . . N1 N -0.2003(12) 0.0129(8) 0.2375(5) 0.034(2) Uani 1 1 d . . . O9 O 0.0596(12) -0.0235(8) 0.0210(5) 0.052(3) Uani 1 1 d . . . C7 C -0.2219(14) 0.1044(9) 0.2371(6) 0.034(3) Uani 1 1 d . . . H7A H -0.2917 0.1307 0.2661 0.041 Uiso 1 1 calc R . . C6 C -0.1423(16) 0.1709(9) 0.1932(6) 0.037(3) Uani 1 1 d . . . O1 O 0.0451(10) 0.0551(6) 0.1557(4) 0.0297(17) Uani 1 1 d . . . O4 O 0.3217(11) -0.1813(6) 0.0704(4) 0.037(2) Uani 1 1 d . . . C2 C 0.0484(15) 0.2115(8) 0.1142(6) 0.034(3) Uani 1 1 d . . . O2 O 0.0953(11) -0.1235(6) 0.1364(5) 0.043(2) Uani 1 1 d . . . O3 O 0.1693(10) 0.1746(6) 0.0773(4) 0.0310(18) Uani 1 1 d . . . C15 C 0.2230(15) -0.2539(8) 0.0908(6) 0.034(3) Uani 1 1 d . . . C16 C 0.0989(17) -0.2201(8) 0.1257(6) 0.034(3) Uani 1 1 d . . . C1 C -0.0148(14) 0.1434(8) 0.1564(6) 0.030(3) Uani 1 1 d . . . O13 O 0.3592(11) 0.1085(6) 0.1847(5) 0.045(2) Uani 1 1 d . . . O12 O 0.3157(13) -0.0380(7) 0.2117(5) 0.046(3) Uani 1 1 d . . . N5 N 0.3589(15) 0.0467(10) 0.2252(6) 0.046(3) Uani 1 1 d . . . O6 O 0.5262(11) -0.0358(7) 0.1106(5) 0.045(2) Uani 1 1 d . . . C10 C -0.1398(16) -0.2582(9) 0.1911(6) 0.038(3) Uani 1 1 d . . . H10A H -0.2050 -0.3077 0.2055 0.045 Uiso 1 1 calc R . . C5 C -0.1951(16) 0.2682(9) 0.1905(7) 0.039(3) Uani 1 1 d . . . H5A H -0.2741 0.2879 0.2179 0.047 Uiso 1 1 calc R . . N2 N -0.1705(14) -0.1715(8) 0.2080(5) 0.037(3) Uani 1 1 d . . . N3 N 0.5932(13) 0.0321(9) 0.0832(6) 0.041(3) Uani 1 1 d . . . C14 C 0.2338(19) -0.3523(9) 0.0752(7) 0.047(4) Uani 1 1 d . . . H14A H 0.3169 -0.3743 0.0508 0.056 Uiso 1 1 calc R . . C17 C 0.2399(17) 0.2382(9) 0.0294(6) 0.041(3) Uani 1 1 d . . . H17A H 0.1585 0.2744 0.0078 0.049 Uiso 1 1 calc R . . H17B H 0.2934 0.1985 -0.0018 0.049 Uiso 1 1 calc R . . C13 C 0.123(2) -0.4167(9) 0.0955(7) 0.048(4) Uani 1 1 d . . . H13A H 0.1297 -0.4820 0.0839 0.058 Uiso 1 1 calc R . . C8 C -0.2756(16) -0.0540(11) 0.2822(6) 0.043(3) Uani 1 1 d . . . H8A H -0.3712 -0.0253 0.2982 0.052 Uiso 1 1 calc R . . H8B H -0.2069 -0.0667 0.3177 0.052 Uiso 1 1 calc R . . C19 C 0.4609(17) -0.2104(11) 0.0335(7) 0.048(4) Uani 1 1 d . . . H19A H 0.5021 -0.1539 0.0115 0.057 Uiso 1 1 calc R . . H19B H 0.4310 -0.2584 0.0020 0.057 Uiso 1 1 calc R . . O7 O 0.5027(16) 0.0971(9) 0.0607(6) 0.074(4) Uani 1 1 d . . . C12 C 0.0033(19) -0.3850(9) 0.1331(7) 0.047(4) Uani 1 1 d . . . H12A H -0.0709 -0.4293 0.1474 0.056 Uiso 1 1 calc R . . C3 C -0.0131(15) 0.3042(8) 0.1098(7) 0.039(3) Uani 1 1 d . . . H3A H 0.0267 0.3478 0.0802 0.047 Uiso 1 1 calc R . . C11 C -0.0089(16) -0.2853(9) 0.1505(6) 0.034(3) Uani 1 1 d . . . O5 O 0.7314(14) 0.0360(14) 0.0781(7) 0.089(5) Uani 1 1 d . . . O11 O 0.3965(15) 0.0680(11) 0.2817(5) 0.075(4) Uani 1 1 d . . . C9 C -0.3116(16) -0.1495(10) 0.2470(7) 0.044(3) Uani 1 1 d . . . H9A H -0.3315 -0.2018 0.2768 0.053 Uiso 1 1 calc R . . H9B H -0.4025 -0.1417 0.2201 0.053 Uiso 1 1 calc R . . C18 C 0.3555(17) 0.3098(10) 0.0588(8) 0.046(3) Uani 1 1 d . . . H18A H 0.3996 0.3500 0.0262 0.069 Uiso 1 1 calc R . . H18B H 0.4372 0.2741 0.0796 0.069 Uiso 1 1 calc R . . H18C H 0.3025 0.3501 0.0891 0.069 Uiso 1 1 calc R . . C20 C 0.586(2) -0.2527(12) 0.0753(8) 0.056(4) Uani 1 1 d . . . H20A H 0.6740 -0.2708 0.0500 0.084 Uiso 1 1 calc R . . H20B H 0.5458 -0.3094 0.0966 0.084 Uiso 1 1 calc R . . H20C H 0.6169 -0.2050 0.1061 0.084 Uiso 1 1 calc R . . C4 C -0.1353(18) 0.3332(9) 0.1499(8) 0.051(4) Uani 1 1 d . . . H4A H -0.1741 0.3965 0.1482 0.061 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 Yb 0.0277(3) 0.0262(3) 0.0311(3) 0.0015(2) 0.00382(17) 0.0002(3) Cu 0.0320(8) 0.0224(6) 0.0494(8) 0.0043(7) 0.0111(7) -0.0007(6) O10 0.050(5) 0.036(5) 0.051(5) 0.006(5) 0.002(5) 0.003(5) N4 0.061(7) 0.022(5) 0.052(7) -0.017(6) -0.003(6) 0.001(6) O8 0.103(10) 0.061(7) 0.043(6) -0.006(5) -0.023(6) -0.010(8) N1 0.026(4) 0.037(6) 0.040(5) 0.006(5) -0.001(4) -0.003(5) O9 0.048(5) 0.063(6) 0.045(5) 0.001(5) 0.007(5) -0.001(5) C7 0.023(5) 0.037(6) 0.041(7) 0.004(5) 0.001(5) 0.001(5) C6 0.042(8) 0.028(6) 0.040(7) -0.001(5) -0.014(7) -0.002(6) O1 0.030(4) 0.023(4) 0.036(4) 0.005(3) 0.003(4) 0.001(4) O4 0.032(5) 0.031(4) 0.048(5) -0.004(4) 0.010(4) 0.004(4) C2 0.031(6) 0.023(5) 0.047(7) -0.001(5) -0.001(6) -0.006(5) O2 0.037(5) 0.015(4) 0.079(7) -0.002(4) 0.018(5) 0.002(4) O3 0.035(5) 0.024(4) 0.033(4) 0.004(3) 0.010(4) -0.004(4) C15 0.033(6) 0.021(5) 0.047(7) 0.001(5) -0.014(6) -0.001(5) C16 0.043(8) 0.013(5) 0.048(7) 0.000(5) -0.010(6) 0.004(5) C1 0.023(6) 0.020(5) 0.045(7) -0.002(5) 0.002(5) -0.003(5) O13 0.046(5) 0.035(5) 0.054(6) 0.000(5) 0.006(5) 0.003(4) O12 0.041(6) 0.048(6) 0.050(5) 0.012(4) -0.001(5) -0.001(5) N5 0.042(7) 0.050(7) 0.045(7) -0.004(6) -0.010(6) 0.012(6) O6 0.037(5) 0.044(5) 0.053(6) 0.004(4) 0.000(5) -0.001(4) C10 0.039(8) 0.030(6) 0.045(7) 0.014(6) -0.014(6) -0.010(6) C5 0.030(7) 0.037(6) 0.051(8) -0.008(6) -0.001(7) 0.009(6) N2 0.035(6) 0.034(5) 0.041(6) 0.013(5) 0.008(5) -0.008(5) N3 0.027(6) 0.058(7) 0.038(6) 0.001(5) 0.003(5) -0.010(5) C14 0.054(9) 0.023(6) 0.063(9) -0.009(6) -0.010(8) 0.007(6) C17 0.054(8) 0.030(6) 0.038(6) 0.009(5) 0.013(7) -0.007(6) C13 0.069(10) 0.021(6) 0.055(9) -0.004(6) -0.006(8) -0.001(6) C8 0.036(7) 0.052(8) 0.042(7) 0.006(6) 0.013(6) 0.006(7) C19 0.044(8) 0.042(7) 0.058(9) -0.002(6) 0.015(7) 0.013(7) O7 0.074(8) 0.055(6) 0.093(9) 0.027(6) -0.007(8) -0.005(6) C12 0.060(9) 0.024(6) 0.056(8) 0.005(6) -0.009(8) -0.010(7) C3 0.037(7) 0.019(5) 0.061(8) 0.007(5) 0.008(7) 0.001(5) C11 0.037(7) 0.034(6) 0.031(6) 0.005(5) -0.001(6) -0.003(6) O5 0.041(7) 0.153(14) 0.072(8) -0.005(9) 0.005(6) -0.024(8) O11 0.077(8) 0.109(10) 0.039(5) -0.027(6) -0.016(6) 0.046(8) C9 0.032(7) 0.046(8) 0.053(8) 0.015(7) 0.007(7) -0.006(6) C18 0.037(7) 0.033(7) 0.069(10) 0.002(6) 0.012(7) -0.004(6) C20 0.047(9) 0.051(9) 0.071(10) -0.005(8) -0.009(8) 0.021(8) C4 0.044(8) 0.021(6) 0.087(12) 0.006(6) -0.004(8) 0.004(6)