Systematic comparison of the structure of homoleptic tetradentate N<sub>2</sub>O<sub>2</sub>-type Schiff base complexes of tetravalent f-elements (M(IV) = Ce, Th, U, Np, and Pu) in solid state and in solution.
Radoske, Thomas; Kloditz, Roger; Fichter, Sebastian; März, Juliane; Kaden, Peter; Patzschke, Michael; Schmidt, Moritz; Stumpf, Thorsten; Walter, Olaf; Ikeda-Ohno, Atsushi; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17559–17570; doi:10.1039/d0dt03405c

data_7706185
_publ_section_title
;
 Systematic comparison of the structure of homoleptic tetradentate
 N<sub>2</sub>O<sub>2</sub>-type Schiff base complexes of tetravalent
 f-elements (M(IV) = Ce, Th, U, Np, and Pu) in solid state and in
 solution.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17559
_journal_page_last               17570
_journal_paper_doi               10.1039/d0dt03405c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C34 H32 Ce N4 O4'
_chemical_formula_sum            'C34 H32 Ce N4 O4'
_chemical_formula_weight         700.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2019-12-09 deposited with the CCDC.	2020-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.480(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6108(14)
_cell_length_b                   13.4604(13)
_cell_length_c                   14.9187(15)
_cell_measurement_reflns_used    9192
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      3.12
_cell_volume                     2933.0(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            146349
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.450
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.598
_exptl_absorpt_correction_T_max  0.9676
_exptl_absorpt_correction_T_min  0.8368
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1496 before and 0.0643 after correction. The Ratio of minimum to maximum transmission is 0.8648. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.068
_refine_diff_density_max         9.155
_refine_diff_density_min         -2.875
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5168
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+45.1551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4219
_reflns_number_total             5168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03405c2.cif
_cod_data_source_block           mo_ce_2nd_polymorph_0m
_cod_database_code               7706185
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C8(H8A,H8B), C26(H26A,H26B), C10(H10A,H10B), C9(H9A,H9B),
 C27(H27A,H27B)
3.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C33(H33), C2(H2), C15(H15), C28(H28), C4(H4), C7(H7), C20(H20),
 C14(H14), C31(H31), C30(H30), C22(H22), C13(H13), C5(H5), C21(H21), C19(H19),
 C11(H11), C3(H3), C16(H16), C32(H32)
;
_olex2_submission_special_instructions 'No special instructions were received'