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_7706184
_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 Th'
_chemical_formula_sum            'C34 H32 N4 O4 Th'
_chemical_formula_weight         792.67
_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             2018-12-14
_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                   14.7012(7)
_cell_length_b                   14.7004(7)
_cell_length_c                   13.9369(7)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.77
_cell_volume                     3012.0(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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0077
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.990
_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            95957
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.337
_diffrn_reflns_theta_min         3.098
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.996
_exptl_absorpt_correction_T_max  0.6508
_exptl_absorpt_correction_T_min  0.5972
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0616 before and 0.0418 after correction.
The Ratio of minimum to maximum transmission is 0.9176.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.119
_refine_diff_density_max         3.226
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.0056(3)
_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   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3725
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0295
_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^)+21.9847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2566
_reflns_number_total             3725
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03405c2.cif
_cod_data_source_block           thsp2nabs
_cod_original_sg_symbol_H-M      'P b a n'
_cod_database_code               7706184
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.501(5) 0.499(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. 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
4. Others
 Sof(H8BC)=Sof(H8BD)=Sof(C6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=
 Sof(H3A)=Sof(C2A)=Sof(H2A)=Sof(N1A)=Sof(C7A)=Sof(H7A)=Sof(O1A)=1-FVAR(1)
 Sof(H8AA)=Sof(H8AB)=Sof(N1)=Sof(C7)=Sof(H7)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(O1)=FVAR(1)
 Sof(H17C)=Sof(H17D)=Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(C14A)=Sof(H14A)=
 Sof(C13A)=Sof(H13A)=Sof(C12A)=Sof(H12A)=Sof(C11A)=Sof(H11A)=Sof(N2A)=Sof(O2A)=
 1-FVAR(2)
 Sof(H17A)=Sof(H17B)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(N2)=Sof(C16)=Sof(H16)=Sof(O2)=FVAR(2)
 Fixed Sof: H9A(0.5) H9B(0.5) H18A(0.5) H18B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C18(H18A,H18B), C8(H8AA,H8AB), C8(H8BC,H8BD), C17(H17C,H17D),
 C17(H17A,H17B)
5.b Aromatic/amide H refined with riding coordinates:
 C16A(H16A), C14A(H14A), C13A(H13A), C12A(H12A), C11A(H11A), C11(H11),
 C12(H12), C13(H13), C14(H14), C7(H7), C5A(H5A), C4A(H4A), C3A(H3A), C2A(H2A),
 C2(H2), C3(H3), C4(H4), C5(H5), C7A(H7A), C16(H16)
5.c Fitted hexagon refined as free rotating group:
 C10(C15A,C14A,C13A,C12A,C11A), C1(C6A,C5A,C4A,C3A,C2A)
;
_olex2_submission_special_instructions 'No special instructions were received'