data_1100954 _chemical_formula_sum 'C20 H22 Ce N5 Ni O13' _chemical_formula_weight 739.26 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' 'Ce' 'Ce' -0.2486 2.6331 '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 8.6323(12) _cell_length_b 13.822(2) _cell_length_c 21.176(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2526.7(6) _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 60 _exptl_crystal_size_mid 35 _exptl_crystal_size_min 22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 2.602 _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 2546 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0260 _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 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2546 _reflns_number_gt 2372 _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^)+(0.0329P)^2^+1.6091P] 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 0.00047(13) _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 0.00(2) _refine_ls_number_reflns 2546 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _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 Ce Ce 0.75152(3) 0.00201(2) 0.093734(13) 0.02851(12) Uani 1 1 d . . . Ni Ni 0.42830(8) 0.06043(5) 0.18509(4) 0.03038(17) Uani 1 1 d . . . O6 O 1.0416(6) 0.0340(3) 0.1060(2) 0.0539(13) Uani 1 1 d . . . O7 O 0.9903(6) -0.0878(4) 0.0484(2) 0.0637(16) Uani 1 1 d . . . N3 N 1.0920(7) -0.0349(4) 0.0738(3) 0.0470(15) Uani 1 1 d . . . O10 O 0.7584(6) -0.0112(4) -0.0256(2) 0.0559(12) Uani 1 1 d . . . O1 O 0.5267(5) -0.0498(3) 0.15480(18) 0.0329(9) Uani 1 1 d . . . O2 O 0.5736(5) 0.1266(2) 0.13622(19) 0.0343(9) Uani 1 1 d . . . O12 O 0.8246(6) 0.0390(4) 0.2104(2) 0.0553(13) Uani 1 1 d . . . N4 N 0.6161(7) 0.0071(4) -0.0362(3) 0.0468(13) Uani 1 1 d . . . O8 O 0.5607(9) -0.0007(4) -0.0888(2) 0.0763(17) Uani 1 1 d . . . N5 N 0.8612(7) -0.0468(5) 0.2245(3) 0.0489(15) Uani 1 1 d . . . O13 O 0.8528(6) -0.1099(3) 0.1815(2) 0.0512(12) Uani 1 1 d . . . O9 O 0.5394(6) 0.0344(4) 0.0107(2) 0.0565(13) Uani 1 1 d . . . O3 O 0.6436(5) -0.1724(3) 0.07509(19) 0.0351(9) Uani 1 1 d . . . O4 O 0.8034(5) 0.1866(3) 0.0693(2) 0.0368(10) Uani 1 1 d . . . C6 C 0.3470(7) -0.1669(4) 0.1967(3) 0.0367(15) Uani 1 1 d . . . C10 C 0.3472(7) 0.2564(4) 0.1914(3) 0.0396(15) Uani 1 1 d . . . H10A H 0.2793 0.3039 0.2056 0.048 Uiso 1 1 calc R . . N2 N 0.3222(6) 0.1702(4) 0.2098(2) 0.0347(11) Uani 1 1 d . . . C16 C 0.5790(7) 0.2217(4) 0.1270(2) 0.0280(11) Uani 1 1 d . . . C1 C 0.4680(7) -0.1389(4) 0.1563(3) 0.0335(14) Uani 1 1 d . . . O11 O 0.9018(7) -0.0688(5) 0.2779(2) 0.083(2) Uani 1 1 d . . . C11 C 0.4706(8) 0.2868(4) 0.1508(3) 0.0346(14) Uani 1 1 d . . . C15 C 0.7029(7) 0.2578(4) 0.0901(3) 0.0337(13) Uani 1 1 d . . . C19 C 0.9426(8) 0.2181(5) 0.0358(3) 0.0429(15) Uani 1 1 d . . . H19B H 0.9150 0.2679 0.0055 0.051 Uiso 1 1 calc R . . H19A H 0.9856 0.1639 0.0126 0.051 Uiso 1 1 calc R . . C2 C 0.5278(7) -0.2075(4) 0.1143(3) 0.0329(13) Uani 1 1 d . . . O5 O 1.2276(6) -0.0497(6) 0.0662(3) 0.089(2) Uani 1 1 d . . . N1 N 0.2994(6) -0.0072(4) 0.2385(2) 0.0340(11) Uani 1 1 d . . . C8 C 0.2238(7) 0.0571(5) 0.2851(3) 0.0431(14) Uani 1 1 d . . . H8B H 0.2931 0.0704 0.3201 0.052 Uiso 1 1 calc R . . H8A H 0.1302 0.0274 0.3015 0.052 Uiso 1 1 calc R . . C7 C 0.2761(7) -0.0983(5) 0.2398(3) 0.0391(15) Uani 1 1 d . . . H7A H 0.2091 -0.1223 0.2704 0.047 Uiso 1 1 calc R . . C13 C 0.6002(8) 0.4183(4) 0.0973(3) 0.0471(17) Uani 1 1 d . . . H13A H 0.6062 0.4836 0.0870 0.056 Uiso 1 1 calc R . . C14 C 0.7126(8) 0.3547(4) 0.0752(3) 0.0411(16) Uani 1 1 d . . . H14A H 0.7938 0.3775 0.0505 0.049 Uiso 1 1 calc R . . C17 C 0.7148(7) -0.2377(4) 0.0291(3) 0.0394(15) Uani 1 1 d . . . H17B H 0.7653 -0.1997 -0.0034 0.047 Uiso 1 1 calc R . . H17A H 0.6346 -0.2761 0.0091 0.047 Uiso 1 1 calc R . . C12 C 0.4810(9) 0.3857(4) 0.1342(3) 0.0453(17) Uani 1 1 d . . . H12A H 0.4061 0.4289 0.1484 0.054 Uiso 1 1 calc R . . C3 C 0.4698(7) -0.2999(4) 0.1125(3) 0.0416(15) Uani 1 1 d . . . H3A H 0.5089 -0.3442 0.0836 0.050 Uiso 1 1 calc R . . C5 C 0.2941(8) -0.2629(5) 0.1955(3) 0.0462(17) Uani 1 1 d . . . H5A H 0.2178 -0.2824 0.2238 0.055 Uiso 1 1 calc R . . C9 C 0.1861(8) 0.1480(5) 0.2502(3) 0.0444(16) Uani 1 1 d . . . H9B H 0.0943 0.1391 0.2245 0.053 Uiso 1 1 calc R . . H9A H 0.1673 0.2005 0.2796 0.053 Uiso 1 1 calc R . . C4 C 0.3529(9) -0.3275(5) 0.1537(3) 0.0513(18) Uani 1 1 d . . . H4A H 0.3148 -0.3904 0.1526 0.062 Uiso 1 1 calc R . . C20 C 1.0609(9) 0.2565(6) 0.0796(4) 0.0596(19) Uani 1 1 d . . . H20A H 1.1505 0.2764 0.0561 0.089 Uiso 1 1 calc R . . H20C H 1.0897 0.2071 0.1092 0.089 Uiso 1 1 calc R . . H20B H 1.0193 0.3110 0.1020 0.089 Uiso 1 1 calc R . . C18 C 0.8321(9) -0.3045(5) 0.0591(4) 0.055(2) Uani 1 1 d . . . H18A H 0.8758 -0.3459 0.0273 0.083 Uiso 1 1 calc R . . H18C H 0.7822 -0.3432 0.0908 0.083 Uiso 1 1 calc R . . H18B H 0.9129 -0.2668 0.0782 0.083 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 Ce 0.02983(18) 0.02389(17) 0.03181(18) -0.00291(12) 0.00295(12) 0.00054(18) Ni 0.0290(3) 0.0258(3) 0.0364(3) -0.0049(3) 0.0044(3) -0.0002(3) O6 0.046(3) 0.046(3) 0.070(3) -0.010(2) 0.001(3) -0.001(2) O7 0.041(3) 0.083(4) 0.067(3) -0.040(3) 0.002(3) 0.009(3) N3 0.035(3) 0.063(4) 0.043(3) 0.002(3) 0.002(3) 0.004(3) O10 0.064(3) 0.061(3) 0.042(2) -0.003(2) 0.006(2) 0.011(4) O1 0.032(2) 0.0231(19) 0.043(2) -0.0032(17) 0.0092(18) -0.0034(17) O2 0.037(2) 0.0219(17) 0.044(2) 0.0004(17) 0.011(2) -0.0012(19) O12 0.060(3) 0.054(3) 0.051(3) -0.016(2) 0.002(3) -0.002(3) N4 0.064(4) 0.032(3) 0.045(3) 0.008(3) -0.004(3) -0.002(3) O8 0.117(5) 0.068(3) 0.045(3) 0.001(3) -0.030(3) 0.005(4) N5 0.040(3) 0.065(4) 0.042(3) 0.006(3) 0.001(3) -0.016(3) O13 0.061(3) 0.044(3) 0.049(3) 0.005(2) -0.007(3) -0.002(2) O9 0.052(3) 0.073(3) 0.045(3) 0.002(2) 0.001(2) 0.010(3) O3 0.041(2) 0.0263(19) 0.038(2) -0.0069(18) 0.003(2) -0.0020(19) O4 0.036(2) 0.030(2) 0.044(2) 0.0019(18) 0.0104(19) -0.0036(19) C6 0.034(3) 0.027(3) 0.049(4) 0.000(3) 0.003(3) -0.002(3) C10 0.039(3) 0.029(3) 0.052(4) -0.012(3) -0.004(3) 0.007(3) N2 0.030(3) 0.042(3) 0.032(3) -0.009(2) 0.001(2) 0.000(2) C16 0.033(3) 0.023(2) 0.028(3) -0.001(2) -0.001(3) -0.004(2) C1 0.037(3) 0.021(3) 0.042(3) -0.001(2) -0.009(3) -0.003(2) O11 0.090(4) 0.113(5) 0.045(3) 0.030(3) -0.027(3) -0.051(4) C11 0.039(3) 0.030(3) 0.035(3) -0.003(3) -0.004(3) 0.002(3) C15 0.039(3) 0.023(3) 0.039(3) -0.002(2) -0.006(3) 0.003(2) C19 0.036(3) 0.043(3) 0.050(4) 0.006(3) 0.013(3) -0.004(3) C2 0.033(3) 0.025(3) 0.040(3) 0.001(2) -0.003(3) 0.002(2) O5 0.029(3) 0.132(6) 0.108(5) -0.026(5) 0.003(3) 0.014(4) N1 0.032(2) 0.037(3) 0.033(2) -0.003(2) 0.0046(19) 0.000(2) C8 0.041(3) 0.044(3) 0.044(3) -0.011(3) 0.011(3) -0.001(3) C7 0.036(4) 0.044(3) 0.037(3) 0.000(3) 0.004(3) -0.008(3) C13 0.060(4) 0.026(3) 0.056(4) 0.002(3) -0.008(4) -0.001(3) C14 0.048(4) 0.027(3) 0.049(3) 0.002(3) -0.001(3) -0.006(3) C17 0.051(4) 0.028(3) 0.039(3) -0.010(2) 0.011(3) -0.001(3) C12 0.056(4) 0.023(3) 0.057(4) -0.008(3) -0.009(4) 0.010(3) C3 0.039(3) 0.031(3) 0.054(4) -0.008(3) 0.000(3) 0.003(3) C5 0.043(4) 0.039(3) 0.056(4) 0.005(3) 0.008(3) -0.014(3) C9 0.035(3) 0.047(4) 0.052(4) -0.011(3) 0.012(3) 0.001(3) C4 0.054(4) 0.029(3) 0.071(5) -0.001(3) 0.003(4) -0.012(3) C20 0.050(4) 0.052(4) 0.077(5) 0.010(4) -0.004(4) -0.008(4) C18 0.059(5) 0.031(3) 0.077(5) 0.003(3) 0.017(4) 0.009(3)