Effects of coordinating heteroatoms on molecular structure, thermodynamic stability and redox behavior of uranyl(vi) complexes with pentadentate Schiff-base ligands
Takeyama, Tomoyuki; Takao, Koichiro; RSC Advances 12 (2022) 24260–24268; doi:10.1039/D2RA04639C

data_7245386
_publ_section_title
;
 Effects of coordinating heteroatoms on molecular structure, thermodynamic
 stability and redox behavior of uranyl(vi) complexes with pentadentate
 Schiff-base ligands
;
_journal_issue                   37
_journal_name_full               'RSC Advances'
_journal_page_first              24260
_journal_page_last               24268
_journal_paper_doi               10.1039/D2RA04639C
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C28 H39 N3 O6 U, C H2 Cl2'
_chemical_formula_sum            'C29 H41 Cl2 N3 O6 U'
_chemical_formula_weight         836.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-06 deposited with the CCDC.	2022-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.798(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9547(2)
_cell_length_b                   29.1269(5)
_cell_length_c                   11.6812(2)
_cell_measurement_reflns_used    16046
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.7740
_cell_measurement_theta_min      2.0130
_cell_volume                     3242.44(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      6.00  35.00   0.50   28.35    --   20.00  54.00  90.00   58
  2  \w     43.00  86.00   0.50   28.35    --   20.00  54.00  90.00   86
  3  \w    -74.00 109.00   0.50   28.35    --   20.00  54.00-150.00  366
  4  \w    -50.00 -15.00   0.50   28.35    --   20.00  54.00-120.00   70
  5  \w     48.00  73.00   0.50   28.35    --   20.00  54.00-120.00   50
  6  \w    -70.00   2.00   0.50   28.35    --   20.00  54.00  30.00  144
  7  \w     55.00  80.00   0.50   28.35    --   20.00  54.00  30.00   50
  8  \w     85.00 110.00   0.50   28.35    --   20.00  54.00  30.00   50
  9  \w    -29.00  -1.00   0.50   28.35    --   20.00  54.00 150.00   56
 10  \w     59.00  84.00   0.50   28.35    --   20.00  54.00 150.00   50
 11  \w    -71.00  28.00   0.50   28.35    --   20.00  54.00 -30.00  198
 12  \w    -27.00  -2.00   0.50   28.35    --   20.00  54.00  90.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0688281000
_diffrn_orient_matrix_UB_12      -0.0084996000
_diffrn_orient_matrix_UB_13      0.0260161000
_diffrn_orient_matrix_UB_21      0.0280633000
_diffrn_orient_matrix_UB_22      0.0193618000
_diffrn_orient_matrix_UB_23      -0.0219008000
_diffrn_orient_matrix_UB_31      0.0035711000
_diffrn_orient_matrix_UB_32      0.0120627000
_diffrn_orient_matrix_UB_33      0.0535920000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36149
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.960
_diffrn_reflns_theta_min         2.296
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.732
_refine_diff_density_min         -1.817
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         9910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+4.7176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7869
_reflns_number_total             9910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra04639c2.cif
_cod_data_source_block           211115_uo2meosaldien
_cod_database_code               7245386
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C29H34N3O6U1
_chemical_oxdiff_usercomment     211115_UO2MeOsaldien
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H9AA(0.6) H9AB(0.6) H9BC(0.4) H9BD(0.4) H11C(0.4) H11D(0.4)
 H11B(0.6) H11A(0.6) N3A(0.6) H3A(0.6) C10B(0.4) H10A(0.4) H10B(0.4) N3B(0.4)
 H3B(0.4) C10A(0.6) H10C(0.6) H10D(0.6)
3.a Ternary CH refined with riding coordinates:
 N3A(H3A), N3B(H3B)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9AA,H9AB), C9(H9BC,H9BD), C8(H8A,H8B), C11(H11C,H11D), C11(H11B,H11A),
 C10B(H10A,H10B), C29(H29A,H29B), C10A(H10C,H10D)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C3(H3), C14(H14), C12(H12), C16(H16)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C21(H21A,H21B,H21C), C28(H28A,
 H28B,H28C)
;
_shelx_res_checksum              35719
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.545
_oxdiff_exptl_absorpt_empirical_full_min 0.866