#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100956.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_1100956 _chemical_formula_sum 'C20 H22 Eu N5 Ni O13' _chemical_formula_weight 751.10 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Eu' 'Eu' -0.1578 3.6682 '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 8.617(4) _cell_length_b 21.215(3) _cell_length_c 13.754(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2514.5(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 52 _exptl_crystal_size_mid 34 _exptl_crystal_size_min 22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 3.298 _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 2534 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2534 _reflns_number_gt 2332 _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^)+(0.0399P)^2^+2.4203P] 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 -0.02(3) _refine_ls_number_reflns 2534 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 Eu Eu 0.00272(4) 0.152695(13) 0.24965(2) 0.02685(12) Uani 1 1 d . . . Ni Ni -0.31772(10) 0.06454(4) 0.19007(6) 0.02885(19) Uani 1 1 d . . . O1 O -0.2172(5) 0.0944(2) 0.3009(3) 0.0297(10) Uani 1 1 d . . . N1 N -0.4496(7) 0.0120(3) 0.2574(4) 0.0341(13) Uani 1 1 d . . . O2 O -0.1707(6) 0.1131(2) 0.1256(3) 0.0328(11) Uani 1 1 d . . . N2 N -0.4230(7) 0.0397(3) 0.0798(4) 0.0314(13) Uani 1 1 d . . . O12 O 0.0703(7) 0.0395(3) 0.2091(4) 0.0495(15) Uani 1 1 d . . . O13 O 0.1010(6) 0.0672(3) 0.3591(4) 0.0448(12) Uani 1 1 d . . . N5 N 0.1081(8) 0.0244(3) 0.2948(6) 0.0460(17) Uani 1 1 d . . . O10 O 0.0209(6) 0.2685(3) 0.2570(4) 0.0467(13) Uani 1 1 d . . . O3 O -0.0987(6) 0.1742(2) 0.4230(3) 0.0321(11) Uani 1 1 d . . . O4 O 0.0614(6) 0.1796(2) 0.0685(4) 0.0355(11) Uani 1 1 d . . . N4 N -0.1215(9) 0.2808(3) 0.2410(5) 0.0433(16) Uani 1 1 d . . . C11 C -0.2721(9) 0.0995(3) -0.0362(5) 0.0342(16) Uani 1 1 d . . . O8 O -0.1737(10) 0.3343(3) 0.2473(5) 0.0697(19) Uani 1 1 d . . . C15 C -0.0394(8) 0.1602(3) -0.0048(5) 0.0330(16) Uani 1 1 d . . . O9 O -0.2051(7) 0.2343(3) 0.2200(4) 0.0532(15) Uani 1 1 d . . . C2 C -0.2167(8) 0.1365(3) 0.4588(5) 0.0308(15) Uani 1 1 d . . . C19 C 0.1981(9) 0.2148(3) 0.0380(6) 0.0413(18) Uani 1 1 d . . . H19A H 0.2396 0.2377 0.0933 0.050 Uiso 1 1 calc R . . H19B H 0.1683 0.2454 -0.0110 0.050 Uiso 1 1 calc R . . C16 C -0.1642(8) 0.1226(3) 0.0301(4) 0.0279(14) Uani 1 1 d . . . C10 C -0.3966(8) 0.0585(4) -0.0075(5) 0.0376(17) Uani 1 1 d . . . H10A H -0.4635 0.0444 -0.0559 0.045 Uiso 1 1 calc R . . C1 C -0.2789(8) 0.0940(3) 0.3904(5) 0.0291(15) Uani 1 1 d . . . O6 O 0.2853(6) 0.1412(3) 0.2166(4) 0.0455(14) Uani 1 1 d . . . N3 N 0.3366(7) 0.1720(3) 0.2871(5) 0.0441(16) Uani 1 1 d . . . O7 O 0.2350(7) 0.1958(3) 0.3440(5) 0.0591(17) Uani 1 1 d . . . O11 O 0.1478(8) -0.0292(3) 0.3155(6) 0.073(2) Uani 1 1 d . . . C7 C -0.4732(9) 0.0120(3) 0.3504(5) 0.0370(17) Uani 1 1 d . . . H7A H -0.5417 -0.0178 0.3753 0.044 Uiso 1 1 calc R . . C14 C -0.0280(10) 0.1753(4) -0.1025(5) 0.0394(18) Uani 1 1 d . . . H14A H 0.0543 0.1999 -0.1244 0.047 Uiso 1 1 calc R . . C13 C -0.1397(10) 0.1537(4) -0.1682(5) 0.045(2) Uani 1 1 d . . . H13A H -0.1325 0.1649 -0.2334 0.054 Uiso 1 1 calc R . . C6 C -0.4010(9) 0.0547(4) 0.4182(5) 0.0354(17) Uani 1 1 d . . . C3 C -0.2765(9) 0.1396(4) 0.5517(5) 0.0401(17) Uani 1 1 d . . . H3A H -0.2376 0.1688 0.5958 0.048 Uiso 1 1 calc R . . C9 C -0.5621(9) -0.0003(4) 0.1002(6) 0.0427(19) Uani 1 1 d . . . H9A H -0.5795 -0.0300 0.0476 0.051 Uiso 1 1 calc R . . H9B H -0.6540 0.0256 0.1078 0.051 Uiso 1 1 calc R . . C5 C -0.4553(9) 0.0568(4) 0.5150(5) 0.0413(19) Uani 1 1 d . . . H5A H -0.5326 0.0291 0.5350 0.050 Uiso 1 1 calc R . . C8 C -0.5255(9) -0.0345(3) 0.1928(6) 0.0409(17) Uani 1 1 d . . . H8A H -0.6198 -0.0504 0.2224 0.049 Uiso 1 1 calc R . . H8B H -0.4566 -0.0697 0.1802 0.049 Uiso 1 1 calc R . . C12 C -0.2599(10) 0.1161(4) -0.1376(5) 0.044(2) Uani 1 1 d . . . H12A H -0.3330 0.1015 -0.1820 0.053 Uiso 1 1 calc R . . C17 C -0.0285(9) 0.2208(3) 0.4880(5) 0.0389(17) Uani 1 1 d . . . H17A H -0.1098 0.2417 0.5246 0.047 Uiso 1 1 calc R . . H17B H 0.0244 0.2524 0.4494 0.047 Uiso 1 1 calc R . . C20 C 0.3216(11) 0.1725(4) -0.0026(6) 0.053(2) Uani 1 1 d . . . H20A H 0.4094 0.1974 -0.0219 0.079 Uiso 1 1 calc R . . H20B H 0.2815 0.1504 -0.0581 0.079 Uiso 1 1 calc R . . H20C H 0.3528 0.1427 0.0461 0.079 Uiso 1 1 calc R . . C4 C -0.3951(9) 0.0989(4) 0.5791(5) 0.045(2) Uani 1 1 d . . . H4A H -0.4338 0.1005 0.6422 0.054 Uiso 1 1 calc R . . C18 C 0.0850(11) 0.1916(4) 0.5577(6) 0.051(2) Uani 1 1 d . . . H18A H 0.1279 0.2238 0.5987 0.076 Uiso 1 1 calc R . . H18B H 0.1669 0.1716 0.5219 0.076 Uiso 1 1 calc R . . H18C H 0.0327 0.1609 0.5970 0.076 Uiso 1 1 calc R . . O5 O 0.4739(7) 0.1805(4) 0.3007(7) 0.079(2) 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 Eu 0.02788(19) 0.03011(19) 0.02256(19) -0.00240(13) -0.0001(2) -0.00272(12) Ni 0.0273(4) 0.0356(4) 0.0237(4) -0.0055(4) 0.0006(4) -0.0051(4) O1 0.031(2) 0.038(2) 0.020(2) -0.0043(19) 0.002(2) -0.005(2) N1 0.032(3) 0.034(3) 0.036(3) -0.006(3) -0.001(3) -0.002(2) O2 0.036(3) 0.045(3) 0.017(2) -0.0008(19) 0.003(2) -0.007(2) N2 0.026(3) 0.034(3) 0.034(3) -0.010(3) -0.003(3) 0.000(3) O12 0.052(3) 0.051(3) 0.046(3) -0.015(3) -0.004(3) 0.000(3) O13 0.048(3) 0.047(3) 0.040(3) 0.000(3) 0.005(2) 0.002(3) N5 0.032(3) 0.049(4) 0.057(4) 0.004(4) 0.009(3) -0.001(3) O10 0.049(3) 0.042(3) 0.049(3) 0.000(2) -0.002(4) -0.006(2) O3 0.039(3) 0.035(3) 0.022(2) -0.006(2) 0.002(2) -0.004(2) O4 0.034(3) 0.043(3) 0.030(2) 0.001(2) 0.005(2) -0.008(2) N4 0.067(4) 0.036(3) 0.027(3) 0.004(3) 0.002(3) -0.003(3) C11 0.036(4) 0.041(4) 0.026(3) -0.006(3) -0.001(3) 0.010(3) O8 0.107(5) 0.039(3) 0.063(4) -0.005(3) -0.016(5) 0.018(4) C15 0.036(4) 0.038(4) 0.025(3) -0.006(3) 0.001(3) 0.006(3) O9 0.051(3) 0.050(3) 0.059(3) 0.003(3) -0.004(3) 0.000(3) C2 0.027(3) 0.037(4) 0.029(3) 0.002(3) -0.004(3) 0.007(3) C19 0.038(4) 0.046(4) 0.040(4) 0.005(3) 0.006(4) -0.012(4) C16 0.030(3) 0.028(3) 0.026(3) 0.000(3) -0.001(3) 0.006(3) C10 0.037(4) 0.048(5) 0.027(3) -0.013(3) -0.006(3) 0.000(4) C1 0.030(4) 0.036(3) 0.022(3) 0.002(3) 0.002(3) 0.005(3) O6 0.036(3) 0.060(3) 0.041(3) -0.007(3) -0.002(2) -0.005(3) N3 0.030(3) 0.043(4) 0.059(4) 0.002(3) -0.011(3) -0.002(3) O7 0.041(3) 0.067(4) 0.069(4) -0.029(3) -0.011(3) -0.002(3) O11 0.076(5) 0.044(3) 0.100(5) 0.029(4) 0.041(4) 0.022(3) C7 0.035(4) 0.033(4) 0.043(4) -0.007(3) 0.008(3) 0.000(3) C14 0.048(5) 0.041(4) 0.029(4) 0.006(3) 0.000(3) -0.003(4) C13 0.052(5) 0.059(5) 0.025(4) 0.001(3) 0.006(3) 0.008(4) C6 0.032(4) 0.042(5) 0.032(3) -0.003(3) 0.003(3) 0.001(4) C3 0.038(4) 0.057(5) 0.025(3) -0.003(3) -0.002(3) 0.005(4) C9 0.035(4) 0.047(5) 0.045(4) -0.010(4) -0.007(3) -0.009(4) C5 0.041(4) 0.054(5) 0.029(3) 0.007(3) 0.010(3) -0.006(4) C8 0.036(4) 0.043(4) 0.044(4) -0.012(4) 0.004(4) -0.010(3) C12 0.054(5) 0.053(5) 0.025(3) -0.009(3) -0.015(3) 0.016(4) C17 0.054(5) 0.031(3) 0.032(3) -0.006(3) -0.001(4) -0.007(4) C20 0.049(5) 0.065(5) 0.044(4) 0.011(4) 0.007(4) 0.000(5) C4 0.043(4) 0.068(5) 0.024(4) -0.003(4) 0.013(3) -0.002(4) C18 0.055(5) 0.070(6) 0.028(4) 0.001(4) -0.002(4) -0.015(5) O5 0.032(3) 0.099(6) 0.108(6) -0.025(5) -0.014(4) -0.004(3) _cod_database_code 1100956