####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_210607_FAK_JES_NiCeSalen _audit_block_doi 10.5517/ccdc.csd.cc2c6nv3 _database_code_depnum_ccdc_archive 'CCDC 2181155' loop_ _citation_id _citation_doi _citation_year 1 10.3390/ijms23158742 2022 loop_ _audit_author_name _audit_author_address 'Kirill Faust' ;Johannes Kepler University Linz Austria ; _audit_update_record ; 2022-06-22 deposited with the CCDC. 2024-08-04 downloaded from the CCDC. ; _chemical_name_systematic ? _chemical_name_common 210607_FAK_JES_NiCeSalen _chemical_formula_moiety ? _chemical_formula_sum 'C21 H24 Ce N5 Ni O15' _chemical_formula_iupac ? _chemical_formula_weight 785.28 _chemical_absolute_configuration ? _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.9758(3) _cell_length_b 16.2125(6) _cell_length_c 10.1002(4) _cell_angle_alpha 90 _cell_angle_beta 91.2440(10) _cell_angle_gamma 90 _cell_volume 1469.44(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 372 _cell_measurement_theta_min 2.3694 _cell_measurement_theta_max 16.5336 _cell_measurement_temperature 296.(2) _exptl_crystal_description rhomboid _exptl_crystal_colour 'clear light blue' _exptl_crystal_size_max 0.229 _exptl_crystal_size_mid 0.208 _exptl_crystal_size_min 0.189 _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 782 _exptl_absorpt_coefficient_mu 2.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.68 _exptl_special_details ; ; _diffrn_ambient_temperature 296.(2) _diffrn_source Mo _diffrn_source_type 'sealed tube' _diffrn_source_power 1.00 _diffrn_source_current 20.0 _diffrn_source_voltage 50 _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker D8 Quest Eco' _diffrn_measurement_device_type ? _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 30317 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_unetI/netI 0.0547 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _refine_special_details ; ; _reflns_number_total 5359 _reflns_number_gt 4495 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.926 _reflns_Friedel_fraction_max 0.997 _reflns_Friedel_fraction_full 0.998 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.0585 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_number_reflns 5359 _refine_ls_number_parameters 392 _refine_ls_number_restraints 1 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.387 _refine_diff_density_min -0.579 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 1911 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.023(8) 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' Ce Ce -0.2486 2.6331 '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' Ni Ni 0.3393 1.1124 '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' _computing_data_collection 'Bruker Instrument Service vV6.2.15' _computing_cell_refinement 'APEX3 v2019.11-0 (Bruker AXS)' _computing_data_reduction 'SAINT V8.40B (Bruker Nano, Inc., 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 994)' _computing_publication_material 'publCIF, Diamond 3.2k' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ce Ce1 0.75655(4) 0.54963(3) 0.19740(3) 0.03686(12) Uani d . . . 1 . . C C1 0.1743(8) 0.4258(4) 0.5995(7) 0.0397(18) Uani d . . . 1 . . O O1 0.6398(5) 0.4371(3) 0.3155(4) 0.0332(11) Uani d . . . 1 . . N N1 0.4086(6) 0.3776(3) 0.4905(5) 0.0337(13) Uani d . . . 1 . . Ni Ni1 0.45994(9) 0.48702(5) 0.40769(8) 0.0304(2) Uani d . . . 1 . . N N3 0.8606(7) 0.6421(5) 0.4388(9) 0.0606(19) Uani d . . . 1 . . O O3 0.5314(5) 0.5880(3) 0.3056(4) 0.0338(11) Uani d . . . 1 . . C C3 0.0868(9) 0.4069(5) 0.7262(7) 0.059(2) Uani d . . . 1 . . H H3A -0.008854 0.433345 0.720607 0.089 Uiso calc U . R 1 . . H H3B 0.141399 0.427375 0.802106 0.089 Uiso calc U . R 1 . . H H3C 0.073554 0.348428 0.734473 0.089 Uiso calc U . R 1 . . N N2 0.2896(5) 0.5508(5) 0.4875(4) 0.0336(11) Uani d . . . 1 . . O O2 0.8392(5) 0.3980(3) 0.1447(5) 0.0489(13) Uani d . . . 1 . . C C2 0.0789(8) 0.4005(5) 0.4789(7) 0.052(2) Uani d . . . 1 . . H H2A 0.130948 0.413284 0.399494 0.078 Uiso calc U . R 1 . . H H2B -0.013819 0.429948 0.479359 0.078 Uiso calc U . R 1 . . H H2C 0.05973 0.342244 0.482288 0.078 Uiso calc U . R 1 . . N N4 1.0680(7) 0.5901(4) 0.1040(6) 0.0510(17) Uani d . . . 1 . . O O4 0.6196(5) 0.6828(3) 0.1148(5) 0.0452(12) Uani d . . . 1 . . C C4 0.3149(7) 0.3736(4) 0.6090(6) 0.0392(18) Uani d . . . 1 . . H H4A 0.373736 0.391557 0.685338 0.047 Uiso calc U . R 1 . . H H4AB 0.286713 0.316654 0.623706 0.047 Uiso calc U . R 1 . . N N5 0.5912(8) 0.5055(4) -0.0638(7) 0.0521(17) Uani d . . . 1 . . O O5 0.3260(5) 0.4562(3) 0.2335(4) 0.0402(12) Uani d . . . 1 . . C C5 0.4526(7) 0.3097(4) 0.4426(7) 0.0389(18) Uani d . . . 1 . . H H5 0.412961 0.262461 0.480284 0.047 Uiso calc U . R 1 . . O O6 0.5992(5) 0.5219(3) 0.5745(4) 0.0502(15) Uani d . . . 1 . . C C6 0.5579(7) 0.2959(4) 0.3356(6) 0.0319(16) Uani d . . . 1 . . O O8 0.8883(8) 0.6795(4) 0.5434(7) 0.095(2) Uani d . . . 1 . . C C8 0.7516(8) 0.3337(4) 0.1887(7) 0.0395(17) Uani d . . . 1 . . O O7 0.8447(5) 0.5640(3) 0.4406(4) 0.0457(13) Uani d . . . 1 . . C C7 0.6470(7) 0.3577(4) 0.2838(6) 0.0323(16) Uani d . . . 1 . . O O9 0.8470(7) 0.6781(3) 0.3289(7) 0.0692(18) Uani d . . . 1 . . C C9 0.7640(9) 0.2535(5) 0.1460(8) 0.051(2) Uani d . . . 1 . . H H9 0.833771 0.239495 0.08307 0.061 Uiso calc U . R 1 . . O O10 1.0446(5) 0.5409(4) 0.1997(4) 0.0463(12) Uani d . . . 1 . . C C10 0.6710(10) 0.1933(5) 0.1981(7) 0.055(2) Uani d . . . 1 . . H H10 0.676425 0.139045 0.168511 0.066 Uiso calc U . R 1 . . O O11 0.9582(6) 0.6282(4) 0.0579(6) 0.083(2) Uani d . . . 1 . . C C11 0.5717(9) 0.2147(4) 0.2930(7) 0.046(2) Uani d . . . 1 . . H H11 0.512108 0.174169 0.329865 0.055 Uiso calc U . R 1 . . O O12 1.1905(6) 0.5981(4) 0.0603(5) 0.0757(19) Uani d . . . 1 . . C C12 0.9616(10) 0.3752(6) 0.0624(9) 0.079(3) Uani d . . . 1 . . H H12A 0.923688 0.35087 -0.01808 0.118 Uiso calc U . R 1 . . H H12B 1.024083 0.336206 0.108679 0.118 Uiso calc U . R 1 . . H H12C 1.018701 0.423476 0.041908 0.118 Uiso calc U . R 1 . . O O13 0.7203(7) 0.5345(4) -0.0667(5) 0.0712(18) Uani d . . . 1 . . C C13 0.2080(8) 0.5174(4) 0.6025(7) 0.044(2) Uani d . . . 1 . . H H13A 0.114416 0.546959 0.608721 0.053 Uiso calc U . R 1 . . H H13B 0.266014 0.529215 0.682349 0.053 Uiso calc U . R 1 . . O O14 0.5159(7) 0.4928(4) -0.1614(5) 0.0736(17) Uani d . . . 1 . . C C14 0.2570(7) 0.6242(4) 0.4541(6) 0.0355(16) Uani d . . . 1 . . H H14 0.181062 0.648828 0.501279 0.043 Uiso calc U . R 1 . . O O15 0.5442(6) 0.4889(4) 0.0496(5) 0.0635(15) Uani d . . . 1 . . C C15 0.3228(7) 0.6749(4) 0.3519(7) 0.0383(18) Uani d . . . 1 . . C C17 0.3014(9) 0.8041(5) 0.2327(8) 0.055(2) Uani d . . . 1 . . H H17 0.253121 0.854072 0.217729 0.066 Uiso calc U . R 1 . . C C18 0.4244(8) 0.7832(4) 0.1597(8) 0.048(2) Uani d . . . 1 . . H H18 0.458 0.818685 0.094411 0.058 Uiso calc U . R 1 . . C C19 0.4968(8) 0.7100(4) 0.1839(7) 0.0369(17) Uani d . . . 1 . . C C20 0.4500(7) 0.6545(4) 0.2830(6) 0.0305(16) Uani d . . . 1 . . C C21 0.6751(9) 0.7378(5) 0.0132(8) 0.063(2) Uani d . . . 1 . . H H21A 0.761365 0.713756 -0.026005 0.094 Uiso calc U . R 1 . . H H21B 0.701503 0.789902 0.052355 0.094 Uiso calc U . R 1 . . H H21C 0.599065 0.746061 -0.05381 0.094 Uiso calc U . R 1 . . C C16 0.2510(8) 0.7512(5) 0.3263(8) 0.052(2) Uani d . . . 1 . . H H16 0.167741 0.765549 0.374531 0.062 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ce1 0.0299(2) 0.0372(2) 0.0438(2) -0.0008(2) 0.00735(15) 0.0093(2) C1 0.036(4) 0.045(4) 0.039(4) 0.003(3) 0.016(4) 0.006(3) O1 0.037(3) 0.025(2) 0.038(3) -0.001(2) 0.007(2) 0.001(2) N1 0.034(3) 0.034(3) 0.034(3) 0.004(3) 0.003(3) 0.006(3) Ni1 0.0312(5) 0.0284(5) 0.0318(5) 0.0008(4) 0.0057(4) 0.0027(4) N3 0.038(4) 0.049(5) 0.094(6) 0.001(3) 0.001(4) -0.026(5) O3 0.028(3) 0.031(2) 0.042(3) 0.006(2) 0.005(2) 0.008(2) C3 0.053(5) 0.065(5) 0.061(5) 0.001(4) 0.029(4) 0.013(4) N2 0.034(3) 0.032(3) 0.035(3) -0.001(4) 0.006(2) -0.002(4) O2 0.045(3) 0.047(3) 0.056(3) 0.003(3) 0.030(3) 0.000(2) C2 0.037(5) 0.054(5) 0.064(6) 0.000(4) 0.007(4) 0.013(4) N4 0.036(4) 0.062(4) 0.056(4) -0.005(3) 0.005(4) 0.014(3) O4 0.037(3) 0.046(3) 0.053(3) 0.004(2) 0.007(2) 0.022(2) C4 0.047(5) 0.041(4) 0.030(4) -0.005(4) 0.006(4) 0.008(3) N5 0.068(5) 0.049(4) 0.039(4) 0.006(4) 0.010(4) 0.003(3) O5 0.033(3) 0.048(3) 0.039(3) -0.004(2) 0.002(2) 0.005(2) C5 0.041(5) 0.033(4) 0.043(4) -0.004(3) 0.003(3) 0.014(3) O6 0.044(3) 0.073(4) 0.033(3) -0.010(2) -0.001(2) -0.002(2) C6 0.038(4) 0.030(4) 0.028(4) 0.004(3) 0.002(3) 0.003(3) O8 0.105(6) 0.083(5) 0.096(5) 0.007(4) -0.022(4) -0.038(4) C8 0.043(4) 0.035(4) 0.040(4) 0.009(4) 0.006(4) 0.002(4) O7 0.043(3) 0.042(4) 0.052(3) -0.003(3) 0.002(2) -0.005(3) C7 0.031(4) 0.036(4) 0.030(4) 0.001(3) 0.002(3) 0.001(3) O9 0.077(5) 0.036(3) 0.094(5) -0.005(3) -0.007(4) 0.009(3) C9 0.063(5) 0.049(5) 0.042(5) 0.012(4) 0.018(4) -0.001(4) O10 0.040(2) 0.051(3) 0.048(3) -0.002(3) 0.011(2) 0.021(3) C10 0.085(7) 0.031(4) 0.050(5) 0.012(4) 0.015(5) -0.002(4) O11 0.034(3) 0.106(5) 0.111(5) 0.009(4) 0.010(3) 0.062(4) C11 0.060(5) 0.034(4) 0.044(5) -0.004(4) 0.005(4) 0.001(4) O12 0.040(3) 0.113(5) 0.075(4) -0.012(3) 0.019(3) 0.041(4) C12 0.066(6) 0.086(7) 0.088(7) -0.017(5) 0.053(5) -0.027(6) O13 0.074(4) 0.079(5) 0.061(3) -0.014(4) 0.026(3) 0.007(3) C13 0.046(5) 0.047(5) 0.039(4) 0.003(3) 0.013(4) 0.000(3) O14 0.097(5) 0.089(4) 0.035(3) -0.003(4) -0.007(3) -0.006(3) C14 0.027(4) 0.035(4) 0.044(4) 0.002(3) 0.005(3) -0.006(3) O15 0.057(4) 0.102(4) 0.032(3) -0.013(3) 0.008(3) 0.009(3) C15 0.033(4) 0.032(4) 0.050(5) 0.001(3) 0.003(4) 0.001(4) C17 0.050(5) 0.037(4) 0.078(6) 0.015(4) 0.002(5) 0.014(4) C18 0.048(5) 0.041(4) 0.056(5) 0.000(4) -0.007(4) 0.011(4) C19 0.035(4) 0.035(4) 0.040(4) 0.000(3) -0.003(3) 0.003(3) C20 0.035(4) 0.024(4) 0.033(4) -0.002(3) -0.004(3) 0.005(3) C21 0.057(5) 0.069(5) 0.064(6) 0.002(4) 0.021(4) 0.037(5) C16 0.048(5) 0.036(4) 0.072(6) 0.009(4) 0.005(4) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ce1 O3 . 2.401(4) ? Ce1 O1 . 2.430(4) ? Ce1 O7 . 2.575(4) ? Ce1 O10 . 2.589(4) ? Ce1 O15 . 2.590(5) ? Ce1 O9 . 2.591(6) ? Ce1 O4 . 2.613(4) ? Ce1 O2 . 2.626(5) ? Ce1 O11 . 2.645(5) ? Ce1 O13 . 2.692(5) ? Ce1 N3 . 2.994(8) ? C1 C13 . 1.517(9) ? C1 C4 . 1.520(9) ? C1 C2 . 1.529(10) ? C1 C3 . 1.546(9) ? O1 C7 . 1.330(7) ? O1 Ni1 . 2.047(4) ? N1 C5 . 1.268(8) ? N1 C4 . 1.479(7) ? N1 Ni1 . 2.019(5) ? Ni1 N2 . 2.028(5) ? Ni1 O3 . 2.045(4) ? Ni1 O6 . 2.152(4) ? Ni1 O5 . 2.167(5) ? N3 O8 . 1.239(8) ? N3 O9 . 1.257(9) ? N3 O7 . 1.274(8) ? O3 C20 . 1.319(7) ? N2 C14 . 1.269(9) ? N2 C13 . 1.488(8) ? O2 C8 . 1.385(8) ? O2 C12 . 1.440(8) ? N4 O12 . 1.200(7) ? N4 O11 . 1.245(7) ? N4 O10 . 1.275(7) ? O4 C19 . 1.389(8) ? O4 C21 . 1.455(8) ? N5 O14 . 1.201(7) ? N5 O13 . 1.252(8) ? N5 O15 . 1.259(7) ? C5 C6 . 1.469(9) ? C6 C7 . 1.390(9) ? C6 C11 . 1.392(9) ? C8 C9 . 1.375(10) ? C8 C7 . 1.412(9) ? C9 C10 . 1.395(11) ? C10 C11 . 1.368(10) ? C14 C15 . 1.455(9) ? C15 C20 . 1.391(9) ? C15 C16 . 1.416(9) ? C17 C16 . 1.361(10) ? C17 C18 . 1.383(10) ? C18 C19 . 1.373(9) ? C19 C20 . 1.416(9) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 Ce1 O1 . . 66.07(13) ? O3 Ce1 O7 . . 77.68(14) ? O1 Ce1 O7 . . 74.13(15) ? O3 Ce1 O10 . . 149.39(15) ? O1 Ce1 O10 . . 113.32(16) ? O7 Ce1 O10 . . 73.15(14) ? O3 Ce1 O15 . . 75.19(16) ? O1 Ce1 O15 . . 71.20(16) ? O7 Ce1 O15 . . 142.32(15) ? O10 Ce1 O15 . . 134.97(17) ? O3 Ce1 O9 . . 79.40(17) ? O1 Ce1 O9 . . 119.04(17) ? O7 Ce1 O9 . . 49.58(18) ? O10 Ce1 O9 . . 74.78(18) ? O15 Ce1 O9 . . 145.04(19) ? O3 Ce1 O4 . . 62.38(14) ? O1 Ce1 O4 . . 124.92(15) ? O7 Ce1 O4 . . 111.25(16) ? O10 Ce1 O4 . . 120.72(16) ? O15 Ce1 O4 . . 78.16(18) ? O9 Ce1 O4 . . 68.87(18) ? O3 Ce1 O2 . . 125.41(14) ? O1 Ce1 O2 . . 61.55(14) ? O7 Ce1 O2 . . 101.30(16) ? O10 Ce1 O2 . . 70.36(17) ? O15 Ce1 O2 . . 74.63(18) ? O9 Ce1 O2 . . 140.31(18) ? O4 Ce1 O2 . . 147.37(16) ? O3 Ce1 O11 . . 135.27(18) ? O1 Ce1 O11 . . 158.56(17) ? O7 Ce1 O11 . . 105.36(18) ? O10 Ce1 O11 . . 48.43(16) ? O15 Ce1 O11 . . 112.30(18) ? O9 Ce1 O11 . . 71.1(2) ? O4 Ce1 O11 . . 75.77(17) ? O2 Ce1 O11 . . 98.24(18) ? O3 Ce1 O13 . . 112.96(16) ? O1 Ce1 O13 . . 111.97(17) ? O7 Ce1 O13 . . 169.04(16) ? O10 Ce1 O13 . . 95.91(16) ? O15 Ce1 O13 . . 47.35(17) ? O9 Ce1 O13 . . 127.7(2) ? O4 Ce1 O13 . . 73.32(18) ? O2 Ce1 O13 . . 75.06(18) ? O11 Ce1 O13 . . 65.5(2) ? O3 Ce1 N3 . . 75.54(16) ? O1 Ce1 N3 . . 96.11(19) ? O7 Ce1 N3 . . 25.02(19) ? O10 Ce1 N3 . . 74.12(16) ? O15 Ce1 N3 . . 150.73(17) ? O9 Ce1 N3 . . 24.68(17) ? O4 Ce1 N3 . . 88.99(19) ? O2 Ce1 N3 . . 123.33(18) ? O11 Ce1 N3 . . 89.3(2) ? O13 Ce1 N3 . . 151.8(2) ? C13 C1 C4 . . 112.3(6) ? C13 C1 C2 . . 112.7(6) ? C4 C1 C2 . . 110.5(6) ? C13 C1 C3 . . 106.4(6) ? C4 C1 C3 . . 105.9(6) ? C2 C1 C3 . . 108.7(6) ? C7 O1 Ni1 . . 122.4(4) ? C7 O1 Ce1 . . 125.8(4) ? Ni1 O1 Ce1 . . 106.23(18) ? C5 N1 C4 . . 117.3(5) ? C5 N1 Ni1 . . 121.9(4) ? C4 N1 Ni1 . . 120.8(4) ? N1 Ni1 N2 . . 95.9(2) ? N1 Ni1 O3 . . 171.5(2) ? N2 Ni1 O3 . . 92.3(2) ? N1 Ni1 O1 . . 91.75(19) ? N2 Ni1 O1 . . 172.4(2) ? O3 Ni1 O1 . . 80.10(16) ? N1 Ni1 O6 . . 92.29(19) ? N2 Ni1 O6 . . 89.15(18) ? O3 Ni1 O6 . . 90.08(17) ? O1 Ni1 O6 . . 90.54(17) ? N1 Ni1 O5 . . 90.38(19) ? N2 Ni1 O5 . . 91.75(17) ? O3 Ni1 O5 . . 87.10(17) ? O1 Ni1 O5 . . 88.20(18) ? O6 Ni1 O5 . . 177.08(18) ? O8 N3 O9 . . 122.7(7) ? O8 N3 O7 . . 119.6(9) ? O9 N3 O7 . . 117.7(7) ? O8 N3 Ce1 . . 173.2(5) ? O9 N3 Ce1 . . 59.4(4) ? O7 N3 Ce1 . . 58.7(4) ? C20 O3 Ni1 . . 124.3(4) ? C20 O3 Ce1 . . 126.9(4) ? Ni1 O3 Ce1 . . 107.36(17) ? C14 N2 C13 . . 115.7(6) ? C14 N2 Ni1 . . 123.0(4) ? C13 N2 Ni1 . . 120.9(5) ? C8 O2 C12 . . 115.9(6) ? C8 O2 Ce1 . . 118.4(4) ? C12 O2 Ce1 . . 125.4(5) ? O12 N4 O11 . . 122.2(7) ? O12 N4 O10 . . 120.9(6) ? O11 N4 O10 . . 116.9(6) ? C19 O4 C21 . . 116.6(5) ? C19 O4 Ce1 . . 118.3(4) ? C21 O4 Ce1 . . 124.4(4) ? N1 C4 C1 . . 114.3(5) ? O14 N5 O13 . . 123.4(7) ? O14 N5 O15 . . 121.1(7) ? O13 N5 O15 . . 115.5(7) ? N1 C5 C6 . . 128.6(6) ? C7 C6 C11 . . 120.6(6) ? C7 C6 C5 . . 123.5(6) ? C11 C6 C5 . . 115.7(6) ? C9 C8 O2 . . 124.1(6) ? C9 C8 C7 . . 122.2(7) ? O2 C8 C7 . . 113.6(6) ? N3 O7 Ce1 . . 96.2(5) ? O1 C7 C6 . . 125.1(6) ? O1 C7 C8 . . 117.9(6) ? C6 C7 C8 . . 117.0(6) ? N3 O9 Ce1 . . 95.9(4) ? C8 C9 C10 . . 119.4(7) ? N4 O10 Ce1 . . 98.1(4) ? C11 C10 C9 . . 119.4(7) ? N4 O11 Ce1 . . 96.1(4) ? C10 C11 C6 . . 121.3(7) ? N5 O13 Ce1 . . 95.9(4) ? N2 C13 C1 . . 116.3(6) ? N2 C14 C15 . . 128.6(6) ? N5 O15 Ce1 . . 100.7(5) ? C20 C15 C16 . . 119.5(6) ? C20 C15 C14 . . 124.8(6) ? C16 C15 C14 . . 115.7(6) ? C16 C17 C18 . . 119.9(7) ? C19 C18 C17 . . 119.8(7) ? C18 C19 O4 . . 124.2(6) ? C18 C19 C20 . . 121.9(7) ? O4 C19 C20 . . 113.9(6) ? O3 C20 C15 . . 124.4(6) ? O3 C20 C19 . . 118.1(6) ? C15 C20 C19 . . 117.5(6) ? C17 C16 C15 . . 121.3(7) ? _shelx_res_file ; TITL 210607_FAK_JES_NiCeSalen_0m_a.res in P2(1) 210607_FAK_JES_NiCeSalen_0m_a.res created by SHELXL-2018/3 at 11:10:06 on 14-Jun-2021 REM Old TITL 210607_FAK_JES_NiCeSalen_0m in P2(1) REM SHELXT solution in P2(1): R1 0.086, Rweak 0.035, Alpha 0.009 REM 0.827 for 9 systematic absences, Orientation as input REM Flack x = 0.060 ( 0.008 ) from 1949 Parsons' quotients REM Formula found by SHELXT: C22 Ce N4 Ni O15 CELL 0.71073 8.9758 16.2125 10.1002 90.000 91.244 90.000 ZERR 2.000 0.0003 0.0006 0.0004 0.000 0.001 0.000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H CE N NI O UNIT 42 48 2 10 2 30 ACTA TEMP 23.000 SIZE 0.189 0.208 0.229 L.S. 10 BOND OMIT 1 0 1 OMIT 1 0 0 LIST 6 FMAP 2 PLAN 20 WGHT 0.024100 FVAR 0.35664 CE1 3 0.756548 0.549632 0.197399 11.00000 0.02985 0.03723 = 0.04379 0.00926 0.00735 -0.00082 C1 1 0.174305 0.425755 0.599520 11.00000 0.03558 0.04526 = 0.03885 0.00590 0.01614 0.00294 O1 6 0.639763 0.437137 0.315515 11.00000 0.03683 0.02534 = 0.03765 0.00094 0.00687 -0.00085 N1 4 0.408647 0.377604 0.490536 11.00000 0.03368 0.03360 = 0.03378 0.00566 0.00315 0.00368 NI1 5 0.459940 0.487020 0.407692 11.00000 0.03120 0.02841 = 0.03179 0.00271 0.00570 0.00081 N3 4 0.860583 0.642130 0.438796 11.00000 0.03825 0.04933 = 0.09407 -0.02568 0.00136 0.00147 O3 6 0.531358 0.587994 0.305605 11.00000 0.02837 0.03097 = 0.04214 0.00811 0.00546 0.00646 C3 1 0.086810 0.406943 0.726178 11.00000 0.05347 0.06459 = 0.06142 0.01260 0.02886 0.00094 AFIX 137 H3A 2 -0.008854 0.433345 0.720607 11.00000 -1.50000 H3B 2 0.141399 0.427375 0.802106 11.00000 -1.50000 H3C 2 0.073554 0.348428 0.734473 11.00000 -1.50000 AFIX 0 N2 4 0.289574 0.550803 0.487506 11.00000 0.03396 0.03187 = 0.03528 -0.00193 0.00595 -0.00114 O2 6 0.839236 0.398013 0.144679 11.00000 0.04517 0.04657 = 0.05609 -0.00044 0.03041 0.00295 C2 1 0.078911 0.400452 0.478941 11.00000 0.03706 0.05392 = 0.06441 0.01286 0.00651 -0.00035 AFIX 137 H2A 2 0.130948 0.413284 0.399494 11.00000 -1.50000 H2B 2 -0.013819 0.429948 0.479359 11.00000 -1.50000 H2C 2 0.059730 0.342244 0.482288 11.00000 -1.50000 AFIX 0 N4 4 1.068018 0.590133 0.104030 11.00000 0.03596 0.06164 = 0.05557 0.01430 0.00470 -0.00549 O4 6 0.619626 0.682850 0.114772 11.00000 0.03729 0.04611 = 0.05253 0.02234 0.00706 0.00429 C4 1 0.314874 0.373628 0.608969 11.00000 0.04686 0.04120 = 0.02981 0.00766 0.00630 -0.00478 AFIX 23 H4A 2 0.373736 0.391557 0.685338 11.00000 -1.20000 H4AB 2 0.286713 0.316654 0.623706 11.00000 -1.20000 AFIX 0 N5 4 0.591222 0.505490 -0.063846 11.00000 0.06835 0.04902 = 0.03931 0.00310 0.01049 0.00641 O5 6 0.326036 0.456234 0.233488 11.00000 0.03332 0.04837 = 0.03891 0.00450 0.00170 -0.00370 C5 1 0.452634 0.309741 0.442628 11.00000 0.04060 0.03349 = 0.04263 0.01443 0.00280 -0.00395 AFIX 43 H5 2 0.412961 0.262461 0.480284 11.00000 -1.20000 AFIX 0 O6 6 0.599222 0.521867 0.574509 11.00000 0.04427 0.07327 = 0.03306 -0.00245 -0.00061 -0.01016 C6 1 0.557929 0.295943 0.335555 11.00000 0.03789 0.02975 = 0.02801 0.00343 0.00211 0.00431 O8 6 0.888268 0.679536 0.543426 11.00000 0.10489 0.08294 = 0.09610 -0.03813 -0.02221 0.00684 C8 1 0.751648 0.333663 0.188710 11.00000 0.04306 0.03518 = 0.04044 0.00186 0.00562 0.00886 O7 6 0.844717 0.564039 0.440598 11.00000 0.04342 0.04156 = 0.05203 -0.00508 0.00240 -0.00282 C7 1 0.646998 0.357673 0.283780 11.00000 0.03114 0.03607 = 0.02961 0.00068 0.00193 0.00138 O9 6 0.847040 0.678076 0.328907 11.00000 0.07740 0.03578 = 0.09403 0.00882 -0.00749 -0.00536 C9 1 0.764026 0.253462 0.146034 11.00000 0.06321 0.04886 = 0.04174 -0.00081 0.01751 0.01245 AFIX 43 H9 2 0.833771 0.239495 0.083070 11.00000 -1.20000 AFIX 0 O10 6 1.044566 0.540884 0.199706 11.00000 0.03993 0.05115 = 0.04812 0.02106 0.01083 -0.00176 C10 1 0.671000 0.193267 0.198068 11.00000 0.08495 0.03106 = 0.05050 -0.00164 0.01521 0.01206 AFIX 43 H10 2 0.676425 0.139045 0.168511 11.00000 -1.20000 AFIX 0 O11 6 0.958184 0.628230 0.057851 11.00000 0.03404 0.10623 = 0.11050 0.06218 0.00952 0.00855 C11 1 0.571659 0.214712 0.293016 11.00000 0.06049 0.03361 = 0.04422 0.00125 0.00474 -0.00431 AFIX 43 H11 2 0.512108 0.174169 0.329865 11.00000 -1.20000 AFIX 0 O12 6 1.190477 0.598115 0.060342 11.00000 0.04001 0.11305 = 0.07487 0.04114 0.01915 -0.01175 C12 1 0.961620 0.375245 0.062448 11.00000 0.06578 0.08584 = 0.08755 -0.02721 0.05308 -0.01726 AFIX 137 H12A 2 0.923688 0.350870 -0.018080 11.00000 -1.50000 H12B 2 1.024083 0.336206 0.108679 11.00000 -1.50000 H12C 2 1.018701 0.423476 0.041908 11.00000 -1.50000 AFIX 0 O13 6 0.720345 0.534480 -0.066737 11.00000 0.07402 0.07920 = 0.06135 0.00687 0.02627 -0.01428 C13 1 0.207971 0.517414 0.602456 11.00000 0.04619 0.04742 = 0.03898 -0.00031 0.01290 0.00305 AFIX 23 H13A 2 0.114416 0.546959 0.608721 11.00000 -1.20000 H13B 2 0.266014 0.529215 0.682349 11.00000 -1.20000 AFIX 0 O14 6 0.515934 0.492820 -0.161447 11.00000 0.09676 0.08920 = 0.03457 -0.00626 -0.00739 -0.00272 C14 1 0.257014 0.624198 0.454149 11.00000 0.02735 0.03526 = 0.04407 -0.00569 0.00491 0.00176 AFIX 43 H14 2 0.181062 0.648828 0.501279 11.00000 -1.20000 AFIX 0 O15 6 0.544197 0.488914 0.049610 11.00000 0.05712 0.10167 = 0.03205 0.00894 0.00825 -0.01340 C15 1 0.322796 0.674912 0.351919 11.00000 0.03281 0.03189 = 0.05034 0.00095 0.00292 0.00089 C17 1 0.301354 0.804055 0.232662 11.00000 0.05030 0.03669 = 0.07800 0.01449 0.00193 0.01507 AFIX 43 H17 2 0.253121 0.854072 0.217729 11.00000 -1.20000 AFIX 0 C18 1 0.424418 0.783215 0.159690 11.00000 0.04751 0.04134 = 0.05561 0.01076 -0.00651 -0.00010 AFIX 43 H18 2 0.458000 0.818685 0.094411 11.00000 -1.20000 AFIX 0 C19 1 0.496832 0.709999 0.183940 11.00000 0.03539 0.03547 = 0.03967 0.00308 -0.00256 -0.00042 C20 1 0.450018 0.654478 0.282950 11.00000 0.03481 0.02373 = 0.03275 0.00458 -0.00408 -0.00182 C21 1 0.675109 0.737817 0.013188 11.00000 0.05741 0.06851 = 0.06357 0.03693 0.02078 0.00172 AFIX 137 H21A 2 0.761365 0.713756 -0.026005 11.00000 -1.50000 H21B 2 0.701503 0.789902 0.052355 11.00000 -1.50000 H21C 2 0.599065 0.746061 -0.053810 11.00000 -1.50000 AFIX 0 C16 1 0.250988 0.751244 0.326332 11.00000 0.04778 0.03646 = 0.07199 0.00625 0.00492 0.00852 AFIX 43 H16 2 0.167741 0.765549 0.374531 11.00000 -1.20000 AFIX 0 HKLF 4 REM 210607_FAK_JES_NiCeSalen_0m_a.res in P2(1) REM wR2 = 0.058481, GooF = S = 1.03337, Restrained GooF = 1.03326 for all data REM R1 = 0.031442 for 4495 Fo > 4sig(Fo) and 0.042926 for all 5359 data REM 392 parameters refined using 1 restraints END WGHT 0.0241 0.0000 REM Highest difference peak 0.387, deepest hole -0.579, 1-sigma level 0.120 Q1 1 0.6806 0.4653 0.2802 11.00000 0.05 0.39 Q2 1 0.6165 0.3954 0.2934 11.00000 0.05 0.38 Q3 1 0.8541 0.4763 0.1786 11.00000 0.05 0.38 Q4 1 0.6784 0.8793 0.0558 11.00000 0.05 0.38 Q5 1 0.5312 0.5891 0.3636 11.00000 0.05 0.37 Q6 1 0.3471 0.5018 -0.0466 11.00000 0.05 0.37 Q7 1 0.2477 0.4753 0.0586 11.00000 0.05 0.37 Q8 1 0.3881 0.9053 0.1849 11.00000 0.05 0.37 Q9 1 0.7326 0.3476 0.2563 11.00000 0.05 0.37 Q10 1 0.3696 0.3628 0.4441 11.00000 0.05 0.36 Q11 1 1.0799 0.4800 0.0868 11.00000 0.05 0.36 Q12 1 0.5268 0.4995 0.3452 11.00000 0.05 0.36 Q13 1 0.9113 0.5538 0.2033 11.00000 0.05 0.35 Q14 1 0.4481 0.4135 0.4060 11.00000 0.05 0.35 Q15 1 0.6002 0.4584 -0.1669 11.00000 0.05 0.35 Q16 1 1.0554 0.5408 0.1319 11.00000 0.05 0.35 Q17 1 0.6273 0.4270 0.3568 11.00000 0.05 0.35 Q18 1 0.7402 0.5049 0.7146 11.00000 0.05 0.34 Q19 1 0.8886 0.3999 0.1237 11.00000 0.05 0.34 Q20 1 0.1465 0.4340 0.5442 11.00000 0.05 0.34 ; _shelx_res_checksum 84860 _shelx_hkl_file ; -1 0 0 0.30 0.40 1 0 0 0.50 0.90 1 0 0 0.20 0.80 -1 0 0 0.60 1.00 2 0 0 394.36 24.00 2 0 0 361.46 24.00 2 0 0 371.46 24.50 2 0 0 388.26 23.70 2 0 0 384.46 24.10 -2 0 0 396.66 24.20 -2 0 0 386.46 24.00 2 0 0 372.16 24.00 2 0 0 352.76 24.10 -2 0 0 377.36 23.70 -2 0 0 370.86 24.10 -2 0 0 350.76 24.30 3 0 0 278.67 18.10 3 0 0 295.27 19.10 -3 0 0 279.47 18.10 -3 0 0 267.97 18.80 3 0 0 273.87 18.90 3 0 0 313.47 18.80 3 0 0 305.07 18.90 3 0 0 300.37 19.60 -3 0 0 287.27 19.50 -3 0 0 281.57 19.00 -3 0 0 259.47 18.60 4 0 0 998.20 57.59 -4 0 0 888.21 57.69 -4 0 0 908.91 57.39 -4 0 0 803.12 58.09 -4 0 0 916.41 56.69 -4 0 0 922.81 57.79 4 0 0 907.91 57.59 4 0 0 885.21 57.39 4 0 0 884.11 57.29 4 0 0 917.91 56.69 4 0 0 867.21 57.79 4 0 0 914.91 58.39 -5 0 0 -0.50 6.10 -5 0 0 2.10 2.30 5 0 0 1.80 3.70 5 0 0 -2.00 4.00 5 0 0 2.60 5.80 5 0 0 4.20 2.20 -5 0 0 0.40 5.00 -5 0 0 12.00 4.90 -5 0 0 3.70 6.60 5 0 0 -0.40 5.00 5 0 0 4.70 4.60 5 0 0 3.40 4.80 -6 0 0 293.37 22.80 6 0 0 349.27 24.50 6 0 0 340.87 24.70 -6 0 0 296.87 22.30 -6 0 0 345.57 23.90 -6 0 0 323.77 21.00 -6 0 0 331.87 21.00 6 0 0 312.47 22.90 6 0 0 364.06 23.40 6 0 0 315.57 22.80 6 0 0 323.77 24.70 7 0 0 9.20 10.30 7 0 0 4.60 7.40 7 0 0 -1.40 9.70 -7 0 0 -4.20 8.80 -7 0 0 10.20 6.70 -7 0 0 8.80 8.10 -8 0 0 32.30 11.80 -8 0 0 30.80 8.90 -8 0 0 32.60 11.60 8 0 0 55.89 11.30 8 0 0 53.59 10.60 9 0 0 32.20 12.40 -9 0 0 32.00 11.20 9 0 0 12.00 13.50 -9 0 0 19.50 16.60 -10 0 0 247.98 27.40 10 0 0 240.98 24.90 2 -1 0 156.88 12.00 2 -1 0 161.78 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66.19 6.00 -4 -1 0 71.09 6.90 4 -1 0 72.89 5.80 4 -1 0 55.19 5.90 4 1 0 53.09 4.90 4 1 0 59.69 6.70 4 1 0 63.49 6.40 -4 1 0 52.29 6.10 4 1 0 58.89 6.20 -4 1 0 53.99 6.00 -4 1 0 53.29 7.60 4 1 0 61.29 6.60 4 1 0 56.69 5.70 4 1 0 80.39 7.40 -4 1 0 53.09 6.80 -5 -1 0 78.99 9.70 5 -1 0 77.69 8.10 5 -1 0 86.49 9.10 -5 -1 0 69.39 5.80 -5 -1 0 82.49 8.30 -5 -1 0 66.49 9.20 5 -1 0 89.29 8.90 5 -1 0 70.29 7.90 5 1 0 51.39 7.70 5 1 0 45.70 7.20 5 1 0 59.19 6.90 -5 1 0 53.39 6.70 -5 1 0 67.69 7.80 -5 1 0 47.00 7.80 5 1 0 47.50 8.80 5 1 0 56.39 8.80 5 1 0 56.09 7.90 5 1 0 54.29 5.50 6 -1 0 145.29 12.00 6 -1 0 149.59 12.00 -6 -1 0 126.89 9.90 6 -1 0 126.69 13.40 -6 -1 0 156.68 12.90 -6 -1 0 139.29 11.20 6 -1 0 121.59 11.70 6 -1 0 131.59 14.80 6 -1 0 124.29 16.30 -6 -1 0 130.39 12.50 6 1 0 147.39 14.10 -6 1 0 137.39 12.80 6 1 0 107.89 12.30 6 1 0 109.99 11.20 6 1 0 123.49 14.20 6 1 0 127.69 11.80 6 1 0 108.69 9.60 -6 1 0 143.09 14.10 -6 1 0 120.19 11.00 6 1 0 134.29 12.40 -6 1 0 139.09 14.00 7 -1 0 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