#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100958.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_1100958 _chemical_formula_sum 'C20 H22 Er N5 Ni O13' _chemical_formula_weight 766.40 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' 'Er' 'Er' -0.2586 4.9576 '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 8.601(4) _cell_length_b 13.710(4) _cell_length_c 21.252(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2506.0(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 50 _exptl_crystal_size_mid 32 _exptl_crystal_size_min 20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.031 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 4.156 _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 2515 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0329 _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 24.99 _reflns_number_total 2515 _reflns_number_gt 2266 _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^)+(0.0228P)^2^+3.8857P] 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 0.00064(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 -0.02(2) _refine_ls_number_reflns 2515 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 Er Er 0.75352(4) 0.50103(2) 0.100335(13) 0.02767(12) Uani 1 1 d . . . Ni Ni 0.43543(11) 0.44047(7) 0.18550(5) 0.0296(2) Uani 1 1 d . . . O1 O 0.5368(6) 0.5511(4) 0.1561(2) 0.0305(11) Uani 1 1 d . . . N1 N 0.3018(7) 0.5076(5) 0.2371(3) 0.0343(14) Uani 1 1 d . . . N2 N 0.3293(8) 0.3297(5) 0.2099(3) 0.0337(16) Uani 1 1 d . . . C16 C 0.5933(9) 0.2811(5) 0.1266(4) 0.0300(17) Uani 1 1 d . . . C10 C 0.3566(10) 0.2418(6) 0.1899(4) 0.040(2) Uani 1 1 d . . . H10A H 0.2875 0.1932 0.2020 0.048 Uiso 1 1 calc R . . O2 O 0.5838(7) 0.3771(3) 0.1375(3) 0.0349(13) Uani 1 1 d . . . C6 C 0.3503(9) 0.6694(5) 0.1955(4) 0.0318(18) Uani 1 1 d . . . C7 C 0.2762(9) 0.6005(6) 0.2376(4) 0.0348(18) Uani 1 1 d . . . H7A H 0.2057 0.6247 0.2669 0.042 Uiso 1 1 calc R . . O4 O 0.8165(7) 0.3214(4) 0.0708(3) 0.0368(13) Uani 1 1 d . . . C15 C 0.7182(9) 0.2477(5) 0.0901(4) 0.0324(18) Uani 1 1 d . . . O6 O 1.0280(7) 0.4674(4) 0.1108(3) 0.0444(15) Uani 1 1 d . . . N3 N 1.0823(9) 0.5397(5) 0.0802(3) 0.0406(17) Uani 1 1 d . . . C19 C 0.9546(10) 0.2927(6) 0.0349(4) 0.041(2) Uani 1 1 d . . . H19A H 0.9961 0.3494 0.0133 0.049 Uiso 1 1 calc R . . H19B H 0.9250 0.2452 0.0032 0.049 Uiso 1 1 calc R . . C11 C 0.4845(9) 0.2138(6) 0.1506(4) 0.0320(18) Uani 1 1 d . . . O3 O 0.6588(6) 0.6722(4) 0.0762(2) 0.0333(12) Uani 1 1 d . . . C2 C 0.5383(9) 0.7091(5) 0.1148(4) 0.0320(18) Uani 1 1 d . . . C17 C 0.7282(10) 0.7374(6) 0.0295(4) 0.0393(19) Uani 1 1 d . . . H17A H 0.6459 0.7719 0.0076 0.047 Uiso 1 1 calc R . . H17B H 0.7841 0.6987 -0.0013 0.047 Uiso 1 1 calc R . . O5 O 1.2222(7) 0.5489(7) 0.0716(4) 0.078(2) Uani 1 1 d . . . C3 C 0.4766(10) 0.8028(5) 0.1107(5) 0.044(2) Uani 1 1 d . . . H3A H 0.5166 0.8468 0.0816 0.053 Uiso 1 1 calc R . . O7 O 0.9847(8) 0.5989(5) 0.0593(3) 0.0575(19) Uani 1 1 d . . . C1 C 0.4753(9) 0.6415(5) 0.1549(4) 0.0293(17) Uani 1 1 d . . . O10 O 0.7818(7) 0.5061(5) -0.0121(3) 0.0471(14) Uani 1 1 d . . . N4 N 0.6404(9) 0.4914(6) -0.0261(3) 0.0416(17) Uani 1 1 d . . . O8 O 0.5921(10) 0.4938(5) -0.0804(3) 0.067(2) Uani 1 1 d . . . O9 O 0.5518(8) 0.4723(4) 0.0201(3) 0.0528(16) Uani 1 1 d . . . C8 C 0.2249(10) 0.4429(6) 0.2837(4) 0.042(2) Uani 1 1 d . . . H8A H 0.1298 0.4725 0.2992 0.051 Uiso 1 1 calc R . . H8B H 0.2933 0.4305 0.3191 0.051 Uiso 1 1 calc R . . C14 C 0.7302(12) 0.1492(6) 0.0744(4) 0.043(2) Uani 1 1 d . . . H14A H 0.8129 0.1279 0.0498 0.052 Uiso 1 1 calc R . . C13 C 0.6198(12) 0.0827(6) 0.0951(4) 0.048(2) Uani 1 1 d . . . H13A H 0.6268 0.0175 0.0834 0.058 Uiso 1 1 calc R . . C5 C 0.2966(10) 0.7653(6) 0.1919(4) 0.043(2) Uani 1 1 d . . . H5A H 0.2179 0.7852 0.2190 0.051 Uiso 1 1 calc R . . C20 C 1.0774(11) 0.2500(7) 0.0760(5) 0.059(3) Uani 1 1 d . . . H20A H 1.1657 0.2322 0.0508 0.089 Uiso 1 1 calc R . . H20B H 1.0373 0.1932 0.0968 0.089 Uiso 1 1 calc R . . H20C H 1.1084 0.2973 0.1069 0.089 Uiso 1 1 calc R . . C12 C 0.4997(11) 0.1137(5) 0.1333(4) 0.043(2) Uani 1 1 d . . . H12A H 0.4274 0.0686 0.1479 0.051 Uiso 1 1 calc R . . C18 C 0.8383(12) 0.8109(6) 0.0579(5) 0.051(2) Uani 1 1 d . . . H18A H 0.8800 0.8516 0.0252 0.077 Uiso 1 1 calc R . . H18B H 0.9216 0.7774 0.0787 0.077 Uiso 1 1 calc R . . H18C H 0.7834 0.8506 0.0877 0.077 Uiso 1 1 calc R . . O12 O 0.8179(8) 0.4569(5) 0.2102(3) 0.0478(17) Uani 1 1 d . . . N5 N 0.8553(9) 0.5440(6) 0.2265(4) 0.0443(19) Uani 1 1 d . . . C4 C 0.3557(11) 0.8307(6) 0.1499(5) 0.048(2) Uani 1 1 d . . . H4A H 0.3153 0.8935 0.1476 0.057 Uiso 1 1 calc R . . C9 C 0.1895(10) 0.3485(6) 0.2484(4) 0.042(2) Uani 1 1 d . . . H9A H 0.1714 0.2954 0.2777 0.051 Uiso 1 1 calc R . . H9B H 0.0984 0.3561 0.2220 0.051 Uiso 1 1 calc R . . O13 O 0.8487(7) 0.6084(4) 0.1848(3) 0.0436(14) Uani 1 1 d . . . O11 O 0.8953(8) 0.5632(6) 0.2808(3) 0.068(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 Er 0.02794(18) 0.02314(18) 0.03192(18) 0.00227(14) 0.00302(13) 0.0001(2) Ni 0.0264(5) 0.0232(4) 0.0392(5) 0.0048(4) 0.0057(5) 0.0007(4) O1 0.027(3) 0.022(2) 0.042(3) 0.006(2) 0.006(2) 0.000(2) N1 0.029(3) 0.038(4) 0.036(3) 0.006(4) 0.000(3) -0.003(3) N2 0.029(3) 0.033(4) 0.039(4) 0.010(3) 0.006(3) -0.002(3) C16 0.030(4) 0.022(3) 0.038(4) -0.002(3) -0.004(4) 0.004(3) C10 0.041(5) 0.032(4) 0.047(5) 0.013(4) -0.005(5) -0.012(4) O2 0.035(3) 0.019(2) 0.051(3) -0.001(2) 0.004(3) 0.000(2) C6 0.030(4) 0.027(4) 0.039(5) 0.004(4) 0.000(4) 0.002(3) C7 0.031(4) 0.039(4) 0.035(4) 0.004(3) 0.002(4) 0.004(4) O4 0.036(3) 0.027(3) 0.048(3) 0.000(2) 0.009(3) 0.005(3) C15 0.032(4) 0.025(4) 0.041(4) 0.001(3) -0.003(4) 0.001(3) O6 0.039(3) 0.036(3) 0.058(4) 0.007(3) 0.007(3) 0.000(3) N3 0.036(4) 0.047(4) 0.039(4) -0.003(3) -0.001(4) -0.011(4) C19 0.038(5) 0.046(5) 0.039(5) -0.009(4) 0.007(4) 0.001(4) C11 0.034(4) 0.030(4) 0.032(4) 0.003(3) -0.004(4) -0.002(3) O3 0.039(3) 0.026(3) 0.035(3) 0.006(2) 0.004(3) 0.001(3) C2 0.028(4) 0.024(4) 0.044(5) -0.001(3) 0.000(4) 0.003(3) C17 0.047(5) 0.032(4) 0.039(4) 0.010(3) 0.003(4) 0.000(4) O5 0.034(4) 0.108(6) 0.091(6) 0.011(5) 0.005(4) -0.020(4) C3 0.039(5) 0.019(4) 0.075(6) 0.013(4) -0.002(5) -0.002(3) O7 0.043(4) 0.059(4) 0.070(5) 0.025(4) -0.004(3) -0.004(3) C1 0.030(4) 0.021(3) 0.038(4) -0.002(3) -0.007(4) 0.001(3) O10 0.049(4) 0.044(3) 0.048(3) 0.005(3) 0.007(3) -0.005(4) N4 0.060(5) 0.031(4) 0.034(4) -0.004(4) 0.000(3) -0.004(4) O8 0.103(6) 0.059(4) 0.039(3) -0.001(4) -0.016(4) -0.012(5) O9 0.046(3) 0.051(4) 0.062(4) 0.002(3) 0.004(3) -0.002(3) C8 0.033(4) 0.049(5) 0.045(4) 0.012(4) 0.014(4) 0.004(4) C14 0.051(6) 0.030(4) 0.049(5) -0.005(4) -0.005(5) 0.005(4) C13 0.069(6) 0.025(4) 0.050(5) -0.005(4) -0.013(5) 0.002(4) C5 0.039(5) 0.032(4) 0.057(5) -0.010(4) 0.006(5) 0.008(4) C20 0.038(5) 0.051(6) 0.088(8) -0.017(6) -0.006(6) 0.013(5) C12 0.053(5) 0.018(4) 0.056(5) 0.008(4) -0.002(5) -0.012(4) C18 0.052(6) 0.033(5) 0.068(6) -0.005(4) 0.010(5) -0.001(4) O12 0.050(4) 0.048(4) 0.046(4) 0.016(3) 0.002(3) 0.001(3) N5 0.035(4) 0.052(5) 0.047(5) -0.004(4) 0.001(4) 0.009(4) C4 0.041(5) 0.029(4) 0.073(7) -0.004(4) -0.001(5) 0.011(4) C9 0.034(4) 0.054(5) 0.040(5) 0.010(4) 0.007(4) -0.005(4) O13 0.043(3) 0.034(3) 0.053(4) 0.000(3) -0.003(3) 0.002(3) O11 0.069(5) 0.101(6) 0.035(3) -0.023(4) -0.016(3) 0.031(5)