#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100950.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_1100950 _chemical_formula_sum 'C20 H22 Cu Dy N5 O13' _chemical_formula_weight 766.47 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' 'Dy' 'Dy' -0.1892 4.4098 '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 8.5870(3) _cell_length_b 13.7580(5) _cell_length_c 21.1665(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2500.61(15) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6084 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 2.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 3.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2996 _exptl_absorpt_correction_T_max 0.4915 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 295(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22294 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5739 _reflns_number_gt 5040 _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^)+(0.0220P)^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 0.00012(6) _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 -0.002(8) _refine_ls_number_reflns 5739 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0452 _refine_ls_wR_factor_gt 0.0441 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _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 Dy Dy 0.260295(13) 0.498402(11) 0.900252(6) 0.02929(4) Uani 1 1 d . . . Cu Cu -0.06242(4) 0.55644(3) 0.81672(2) 0.03509(10) Uani 1 1 d . . . O3 O 0.1650(2) 0.32448(14) 0.92353(11) 0.0340(5) Uani 1 1 d . . . O1 O 0.0447(2) 0.44342(15) 0.84483(10) 0.0332(5) Uani 1 1 d . . . O2 O 0.0933(3) 0.62358(15) 0.86313(11) 0.0378(6) Uani 1 1 d . . . O4 O 0.3207(2) 0.68166(15) 0.92990(11) 0.0373(5) Uani 1 1 d . . . O10 O 0.2860(3) 0.4929(2) 1.01416(11) 0.0491(6) Uani 1 1 d . . . O9 O 0.0570(3) 0.52516(18) 0.98102(12) 0.0533(7) Uani 1 1 d . . . O8 O 0.0946(4) 0.5044(2) 1.08132(13) 0.0717(8) Uani 1 1 d . . . O13 O 0.3617(3) 0.38942(17) 0.81756(13) 0.0457(6) Uani 1 1 d . . . O12 O 0.3187(3) 0.5357(2) 0.78733(12) 0.0492(7) Uani 1 1 d . . . O11 O 0.3992(4) 0.4292(3) 0.71906(14) 0.0763(10) Uani 1 1 d . . . O6 O 0.5358(3) 0.53629(17) 0.88649(13) 0.0488(6) Uani 1 1 d . . . O7 O 0.5010(3) 0.4078(2) 0.94144(14) 0.0606(8) Uani 1 1 d . . . O5 O 0.7347(3) 0.4597(3) 0.92359(15) 0.0816(9) Uani 1 1 d . . . N1 N -0.1992(3) 0.48620(19) 0.76176(13) 0.0366(6) Uani 1 1 d . . . N2 N -0.1733(3) 0.6703(2) 0.79153(14) 0.0368(7) Uani 1 1 d . . . N4 N 0.1433(3) 0.5077(2) 1.02757(15) 0.0456(7) Uani 1 1 d . . . N5 N 0.3607(3) 0.4499(3) 0.77360(17) 0.0468(8) Uani 1 1 d . . . N3 N 0.5953(3) 0.4677(2) 0.91775(15) 0.0447(8) Uani 1 1 d . . . C18 C 0.3519(4) 0.1907(3) 0.9410(2) 0.0545(11) Uani 1 1 d . . . H18A H 0.3954 0.1498 0.9733 0.082 Uiso 1 1 calc R . . H18B H 0.4337 0.2269 0.9210 0.082 Uiso 1 1 calc R . . H18C H 0.3002 0.1511 0.9101 0.082 Uiso 1 1 calc R . . C17 C 0.2361(4) 0.2602(2) 0.97036(15) 0.0412(8) Uani 1 1 d . . . H17A H 0.1550 0.2232 0.9913 0.049 Uiso 1 1 calc R . . H17B H 0.2885 0.2992 1.0021 0.049 Uiso 1 1 calc R . . C2 C 0.0454(4) 0.2872(2) 0.88667(16) 0.0307(7) Uani 1 1 d . . . C3 C -0.0146(4) 0.1936(2) 0.89059(19) 0.0397(8) Uani 1 1 d . . . H3A H 0.0258 0.1494 0.9195 0.048 Uiso 1 1 calc R . . C4 C -0.1368(4) 0.1665(3) 0.85032(19) 0.0492(10) Uani 1 1 d . . . H4A H -0.1764 0.1036 0.8523 0.059 Uiso 1 1 calc R . . C5 C -0.1982(4) 0.2308(2) 0.8084(2) 0.0444(9) Uani 1 1 d . . . H5A H -0.2774 0.2107 0.7814 0.053 Uiso 1 1 calc R . . C6 C -0.1438(4) 0.3277(2) 0.80505(17) 0.0355(8) Uani 1 1 d . . . C1 C -0.0176(3) 0.3549(2) 0.84401(15) 0.0288(7) Uani 1 1 d . . . C7 C -0.2209(3) 0.3949(2) 0.76259(16) 0.0370(7) Uani 1 1 d . . . H7A H -0.2916 0.3692 0.7338 0.044 Uiso 1 1 calc R . . C8 C -0.2760(4) 0.5526(3) 0.71713(16) 0.0437(8) Uani 1 1 d . . . H8A H -0.3717 0.5238 0.7016 0.052 Uiso 1 1 calc R . . H8B H -0.2083 0.5653 0.6814 0.052 Uiso 1 1 calc R . . C9 C -0.3113(4) 0.6473(3) 0.75228(19) 0.0438(9) Uani 1 1 d . . . H9A H -0.3310 0.6993 0.7224 0.053 Uiso 1 1 calc R . . H9B H -0.4027 0.6394 0.7788 0.053 Uiso 1 1 calc R . . C10 C -0.1432(4) 0.7570(2) 0.80943(18) 0.0371(8) Uani 1 1 d . . . H10A H -0.2085 0.8062 0.7951 0.044 Uiso 1 1 calc R . . C11 C -0.0141(4) 0.7848(2) 0.85063(17) 0.0355(8) Uani 1 1 d . . . C12 C -0.0012(4) 0.8841(2) 0.86727(18) 0.0445(9) Uani 1 1 d . . . H12A H -0.0752 0.9282 0.8529 0.053 Uiso 1 1 calc R . . C13 C 0.1184(4) 0.9156(2) 0.90406(19) 0.0487(9) Uani 1 1 d . . . H13A H 0.1243 0.9809 0.9152 0.058 Uiso 1 1 calc R . . C14 C 0.2323(4) 0.8512(2) 0.92534(17) 0.0423(8) Uani 1 1 d . . . H14A H 0.3152 0.8736 0.9495 0.051 Uiso 1 1 calc R . . C15 C 0.2210(4) 0.7543(2) 0.91034(15) 0.0327(7) Uani 1 1 d . . . C16 C 0.0953(4) 0.7190(2) 0.87351(16) 0.0315(8) Uani 1 1 d . . . C19 C 0.4566(4) 0.7122(3) 0.96567(17) 0.0433(9) Uani 1 1 d . . . H19A H 0.4986 0.6567 0.9883 0.052 Uiso 1 1 calc R . . H19B H 0.4255 0.7604 0.9966 0.052 Uiso 1 1 calc R . . C20 C 0.5809(5) 0.7542(3) 0.9242(2) 0.0571(11) Uani 1 1 d . . . H20A H 0.6684 0.7731 0.9496 0.086 Uiso 1 1 calc R . . H20B H 0.5407 0.8101 0.9025 0.086 Uiso 1 1 calc R . . H20C H 0.6133 0.7064 0.8939 0.086 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 Dy 0.02809(6) 0.02553(6) 0.03426(7) 0.00209(7) -0.00386(6) 0.00071(8) Cu 0.03439(19) 0.02681(18) 0.0441(2) 0.00394(18) -0.01088(19) 0.00153(15) O3 0.0383(12) 0.0254(11) 0.0384(14) 0.0069(10) -0.0059(10) 0.0012(9) O1 0.0309(11) 0.0242(10) 0.0445(13) 0.0062(10) -0.0077(10) -0.0009(9) O2 0.0386(13) 0.0222(10) 0.0528(16) 0.0005(10) -0.0124(11) 0.0021(9) O4 0.0346(12) 0.0302(12) 0.0470(15) -0.0007(10) -0.0069(10) -0.0020(9) O10 0.0486(12) 0.0539(15) 0.0447(14) 0.0001(13) -0.0065(10) 0.0056(15) O9 0.0444(13) 0.068(2) 0.0476(15) -0.0013(13) -0.0031(12) 0.0053(12) O8 0.103(2) 0.0682(18) 0.0438(16) 0.0009(17) 0.0208(15) 0.022(2) O13 0.0490(14) 0.0393(13) 0.0487(16) -0.0033(13) 0.0048(13) -0.0018(10) O12 0.0501(16) 0.0526(16) 0.0450(16) 0.0133(12) -0.0041(13) -0.0051(12) O11 0.081(2) 0.108(3) 0.0403(17) -0.0206(17) 0.0165(15) -0.0423(19) O6 0.0373(13) 0.0429(13) 0.0664(18) 0.0021(12) -0.0084(13) 0.0011(10) O7 0.0496(16) 0.074(2) 0.0588(19) 0.0246(16) -0.0017(14) 0.0167(14) O5 0.0332(14) 0.123(3) 0.089(2) -0.006(2) -0.0086(14) 0.0188(15) N1 0.0343(11) 0.0398(16) 0.0357(15) 0.0050(13) -0.0049(11) -0.0030(11) N2 0.0322(15) 0.0360(15) 0.0422(19) 0.0102(13) -0.0012(13) 0.0054(12) N4 0.0647(18) 0.0301(15) 0.0418(18) -0.0008(17) 0.0023(14) 0.0029(17) N5 0.0332(16) 0.057(2) 0.050(2) -0.0060(19) -0.0017(14) -0.0169(15) N3 0.0337(15) 0.058(2) 0.0426(18) -0.0089(14) -0.0028(14) 0.0087(13) C18 0.055(2) 0.036(2) 0.072(3) -0.0025(19) -0.018(2) 0.0106(16) C17 0.056(2) 0.0328(16) 0.0351(19) 0.0090(13) -0.0096(18) 0.0012(16) C2 0.0300(16) 0.0274(15) 0.035(2) -0.0014(13) 0.0041(15) 0.0019(12) C3 0.0385(17) 0.0277(16) 0.053(2) 0.0065(16) 0.0043(18) -0.0006(12) C4 0.050(2) 0.0263(17) 0.071(3) 0.0023(18) -0.0023(19) -0.0120(15) C5 0.0394(19) 0.0341(17) 0.060(3) -0.0054(17) -0.0063(19) -0.0102(14) C6 0.0351(18) 0.0328(17) 0.039(2) 0.0007(15) 0.0003(16) -0.0042(13) C1 0.0275(15) 0.0261(15) 0.0327(18) 0.0000(12) 0.0041(13) 0.0005(11) C7 0.0295(16) 0.0436(18) 0.0379(19) -0.0015(15) -0.0001(15) -0.0067(14) C8 0.0395(18) 0.0467(19) 0.045(2) 0.0138(16) -0.0101(16) -0.0037(16) C9 0.0351(17) 0.049(2) 0.048(2) 0.0131(17) -0.0103(17) 0.0044(14) C10 0.0366(19) 0.0346(18) 0.040(2) 0.0114(16) 0.0052(17) 0.0109(14) C11 0.0387(18) 0.0291(16) 0.039(2) 0.0072(14) 0.0072(15) 0.0055(13) C12 0.057(2) 0.0250(16) 0.051(2) 0.0031(15) 0.0041(18) 0.0114(15) C13 0.067(2) 0.0232(16) 0.056(3) -0.0047(16) 0.014(2) -0.0016(14) C14 0.051(2) 0.0319(16) 0.044(2) -0.0038(14) 0.0038(18) -0.0051(15) C15 0.0370(16) 0.0274(14) 0.0337(18) 0.0028(12) 0.0050(14) -0.0015(12) C16 0.0391(19) 0.0235(15) 0.0321(19) 0.0025(13) 0.0032(15) 0.0001(12) C19 0.0375(18) 0.0443(19) 0.048(2) -0.0055(16) -0.0097(17) -0.0061(15) C20 0.050(2) 0.049(2) 0.072(3) -0.008(2) 0.002(2) -0.0135(18)