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_7706181
_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 N4 O4 U'
_chemical_formula_sum            'C33.94 H32 N4 O4 U'
_chemical_formula_weight         797.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           50
_space_group_name_Hall           '-P 2ab 2b'
_space_group_name_H-M_alt        'P b a n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-28
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6015(7)
_cell_length_b                   14.6038(8)
_cell_length_c                   13.9168(7)
_cell_measurement_reflns_used    9188
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      28.323
_cell_measurement_theta_min      3.151
_cell_volume                     2967.6(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      105.87
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            172988
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.342
_diffrn_reflns_theta_min         3.151
_exptl_absorpt_coefficient_mu    5.515
_exptl_absorpt_correction_T_max  0.6035
_exptl_absorpt_correction_T_min  0.2053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1568 before and 0.0596 after correction.
The Ratio of minimum to maximum transmission is 0.3402.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear reddish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_description       prism
_exptl_crystal_F_000             1551
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.55
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.00325(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+12.0209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2210
_reflns_number_total             3709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03405c2.cif
_cod_data_source_block           mo_tr_12_2908_0m
_cod_original_sg_symbol_H-M      'P b a n'
_cod_database_code               7706181
_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, All C(H,H,H,H) groups
2. Others
 Fixed Sof: H18A(0.5) H18B(0.5) H17C(0.4) H17D(0.4) H17A(0.6) H17B(0.6)
 N2A(0.4) H9A(0.5) H9B(0.5) H8A(0.55) H8B(0.55) H8BC(0.45) H8BD(0.45) N1(0.55)
 C7(0.55) H7(0.55) C16A(0.4) H16A(0.4) C2A(0.45) H2A(0.45) C3A(0.45) H3A(0.45)
 C4A(0.45) H4A(0.45) C5A(0.45) H5A(0.45) C6A(0.45) C4(0.55) H4(0.55) C5(0.55)
 H5(0.55) C6(0.55) C15A(0.4) C14A(0.4) H14A(0.4) C13A(0.4) H13A(0.4) C12A(0.4)
 H12A(0.4) C11A(0.4) H11A(0.4) C3(0.55) H3(0.55) O1(0.55) C2(0.55) H2(0.55)
 O2A(0.4) N2(0.6) C16(0.6) H16(0.6) C15(0.6) O2(0.6) C14(0.6) H14(0.6) C13(0.6)
 H13(0.6) C12(0.6) H12(0.6) C11(0.6) H11(0.6) N1A(0.45) C7A(0.45) H7A(0.45)
 O1A(0.45)
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C17(H17C,H17D), C17(H17A,H17B), C9(H9A,H9B), C8(H8A,H8B),
 C8(H8BC,H8BD)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C16A(H16A), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C4(H4), C5(H5),
 C14A(H14A), C13A(H13A), C12A(H12A), C11A(H11A), C3(H3), C2(H2), C16(H16),
 C14(H14), C13(H13), C12(H12), C11(H11), C7A(H7A)
3.c Fitted hexagon refined as free rotating group:
 C1(C2A,C3A,C4A,C5A,C6A), C10(C15A,C14A,C13A,C12A,C11A)
;
_olex2_submission_special_instructions 'No special instructions were received'