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_7245385
_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 O6 S U, C H2 Cl2'
_chemical_formula_sum            'C29 H40 Cl2 N2 O6 S U'
_chemical_formula_weight         853.62
_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             2022-05-22
_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                 98.602(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3889(14)
_cell_length_b                   18.8968(9)
_cell_length_c                   10.3557(6)
_cell_measurement_reflns_used    6606
_cell_measurement_temperature    113
_cell_measurement_theta_max      28.8330
_cell_measurement_theta_min      1.7350
_cell_volume                     3171.1(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      113
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.952
_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    -73.00 -20.50   0.50   90.00    --   20.00  54.00 -30.00  105
  2  \w      4.00 106.50   0.50   90.00    --   20.00  54.00 -30.00  205
  3  \w    -69.00  -0.50   0.50   90.00    --   20.00  54.00-150.00  137
  4  \w     17.00  70.50   0.50   90.00    --   20.00  54.00-150.00  107
  5  \w    -36.00   3.50   0.50   90.00    --   20.00  54.00-180.00   79
  6  \w     34.00  67.50   0.50   90.00    --   20.00  54.00-180.00   67
  7  \w    -71.00 -40.50   0.50   90.00    --   20.00  54.00  30.00   61
  8  \w    -74.00  48.50   0.50   90.00    --   20.00  54.00 -90.00  245
  9  \w    -67.00  77.50   0.50   90.00    --   20.00  54.00  -8.79  289
;
_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      -0.0342679000
_diffrn_orient_matrix_UB_12      0.0233618000
_diffrn_orient_matrix_UB_13      -0.0061311000
_diffrn_orient_matrix_UB_21      0.0272471000
_diffrn_orient_matrix_UB_22      0.0293672000
_diffrn_orient_matrix_UB_23      0.0087938000
_diffrn_orient_matrix_UB_31      -0.0000539000
_diffrn_orient_matrix_UB_32      0.0017107000
_diffrn_orient_matrix_UB_33      -0.0683707000
_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  0.1055
_diffrn_reflns_av_unetI/netI     0.1154
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35851
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.890
_diffrn_reflns_theta_min         2.262
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21185
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.661
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.053
_refine_diff_density_max         4.306
_refine_diff_density_min         -4.642
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         9534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0940P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5994
_reflns_number_total             9534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra04639c2.cif
_cod_data_source_block           210120_uo2meosalidien_s
_cod_database_code               7245385
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C29H34N3O6S1U1
_chemical_oxdiff_usercomment     210120_UO2MeOsalidien_S
_reflns_odcompleteness_completeness 98.95
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) =
Uanis(C18)
Uanis(Cl1A) = Uanis(Cl1B) = Uanis(Cl2A) = Uanis(Cl2B)
Uanis(O1) = Uanis(O2)
3. Others
 Fixed Sof: Cl2B(0.8) Cl1A(0.8) H29A(0.8) H29B(0.8) H29C(0.2) H29D(0.2)
 Cl1B(0.2) Cl2A(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B), C8(H8A,H8B), C9(H9A,H9B), C29(H29A,H29B),
 C29(H29C,H29D)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C16(H16), C7(H7), C3(H3), C12(H12), C14(H14)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C20(H20A,H20B,H20C), C25(H25A,H25B,
 H25C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C)
;
_shelx_res_checksum              18414
_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 2.756
_oxdiff_exptl_absorpt_empirical_full_min 0.441