Controlling mixed-valence states of pyridyldiimino-bis(<i>o</i>-phenolato) ligand radical in uranyl(VI) complexes.
Takeyama, Tomoyuki; Tsushima, Satoru; Takao, Koichiro; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16671–16684; doi:10.1039/d4dt01821d

data_7717089
_publ_section_title
;
 Controlling mixed-valence states of
 pyridyldiimino-bis(<i>o</i>-phenolato) ligand radical in uranyl(VI)
 complexes.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16671
_journal_page_last               16684
_journal_paper_doi               10.1039/d4dt01821d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C19 H13 N3 O4 U'
_chemical_formula_sum            'C19 H13 N3 O4 U'
_chemical_formula_weight         585.35
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-08-20 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9774(2)
_cell_length_b                   6.9774(2)
_cell_length_c                   34.432(2)
_cell_measurement_reflns_used    2979
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.5280
_cell_measurement_theta_min      2.9630
_cell_volume                     1676.29(12)
_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      113.0
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.968
_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     67.00 105.00   0.50   20.86    --   20.00  54.00  60.00   76
  2  \w    -73.00  12.00   0.50   20.86    --   20.00  54.00  30.00  170
  3  \w    -35.00  49.00   0.50   20.86    --   20.00  54.00 -90.00  168
  4  \w    -39.00 -13.00   0.50   20.86    --   20.00  54.00  60.00   52
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            6932
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.859
_diffrn_reflns_theta_min         2.366
_exptl_absorpt_coefficient_mu    9.716
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35160
_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    2.319
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.054
_refine_diff_density_max         5.011
_refine_diff_density_min         -3.869
_refine_diff_density_rms         0.264
_refine_ls_abs_structure_details
;
 Flack x determined using 651 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         2499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+21.0676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.559
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.910
_reflns_number_gt                2150
_reflns_number_total             2499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01821d2.cif
_cod_data_source_block           210528_uo2pdiop
_cod_depositor_comments
'Adding full bibliography for 7717089--7717091.cif.'
_cod_original_cell_volume        1676.29(14)
_cod_database_code               7717089
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C6) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C2)
Uanis(O2) = Uanis(N1) = Uanis(N2)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C3(H3), C4(H4), C10(H10), C9(H9), C5(H5)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              43317
_shelx_hkl_checksum              4189
_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
;