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_7245384
_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 H38 N2 O7 U, C5 H5 N'
_chemical_formula_sum            'C33 H43 N3 O7 U'
_chemical_formula_weight         831.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-06-06 deposited with the CCDC.	2022-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                75.1030(10)
_cell_angle_beta                 80.7980(10)
_cell_angle_gamma                71.7900(10)
_cell_formula_units_Z            2
_cell_length_a                   10.19370(10)
_cell_length_b                   13.0886(2)
_cell_length_c                   13.2854(2)
_cell_measurement_reflns_used    18600
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.5830
_cell_measurement_theta_min      2.0450
_cell_volume                     1621.06(4)
_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 0.994
_diffrn_measured_fraction_theta_max 0.947
_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    -72.00  76.00   0.50   15.26    --   20.00  54.00  30.00  296
  2  \w    -74.00  38.00   0.50   15.26    --   20.00  54.00 150.00  224
  3  \w     47.00  90.00   0.50   15.26    --   20.00  54.00 150.00   86
  4  \w    -70.00  10.00   0.50   15.26    --   20.00  54.00-150.00  160
  5  \w     38.00  63.00   0.50   15.26    --   20.00  54.00-150.00   50
  6  \w    -71.00  71.00   0.50   15.26    --   20.00  54.00  90.00  284
  7  \w    -74.00  32.00   0.50   15.26    --   20.00  54.00   0.00  212
  8  \w     69.00  94.00   0.50   15.26    --   20.00  54.00   0.00   50
  9  \w    -55.00 -28.00   0.50   15.26    --   20.00  54.00-106.60   54
 10  \w     63.00  88.00   0.50   15.26    --   20.00  54.00-106.60   50
 11  \w    -73.00 -39.00   0.50   15.26    --   20.00  54.00 -30.00   68
 12  \w     21.00  46.00   0.50   15.26    --   20.00  54.00 -30.00   50
 13  \w    -66.00 -40.00   0.50   15.26    --   20.00  54.00  60.00   52
 14  \w     17.00  42.00   0.50   15.26    --   20.00  54.00  60.00   50
 15  \w     55.00  81.00   0.50   15.26    --   20.00  54.00  60.00   52
 16  \w    -31.00  -6.00   0.50   15.26    --   20.00  54.00 -60.00   50
 17  \w      3.00  28.00   0.50   15.26    --   20.00  54.00 -60.00   50
 18  \w     85.00 110.00   0.50   15.26    --   20.00  54.00 -60.00   50
 19  \w    -69.00 -44.00   0.50   15.26    --   20.00  54.00-180.00   50
 20  \w    -66.00  54.00   0.50   15.26    --   20.00  54.00 -90.00  240
;
_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      0.0064964000
_diffrn_orient_matrix_UB_12      -0.0503124000
_diffrn_orient_matrix_UB_13      0.0377489000
_diffrn_orient_matrix_UB_21      -0.0697564000
_diffrn_orient_matrix_UB_22      0.0033689000
_diffrn_orient_matrix_UB_23      -0.0043409000
_diffrn_orient_matrix_UB_31      0.0223198000
_diffrn_orient_matrix_UB_32      -0.0296452000
_diffrn_orient_matrix_UB_33      -0.0403911000
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32663
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.896
_diffrn_reflns_theta_min         2.043
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.057
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80705
_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    1.704
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.993
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         9686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0347P)^2^+1.7594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8730
_reflns_number_total             9686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra04639c2.cif
_cod_data_source_block           210519_uo2meosaldien_o
_cod_database_code               7245384
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C29H34N3O4U1
_chemical_oxdiff_usercomment     210519_UO2MeOsaldien_O
_reflns_odcompleteness_completeness 98.92
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C32) = Uanis(C31) = Uanis(C30) = Uanis(C29) = Uanis(N3)
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C7(H7), C12(H12), C16(H16), C3(H3), C5(H5), C32(H32), C33(H33),
 C31(H31), C30(H30), C29(H29)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C23(H23A,
 H23B,H23C)
;
_shelx_res_checksum              52339
_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 1.260
_oxdiff_exptl_absorpt_empirical_full_min 0.847