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_7717090
_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         'C27 H29 N3 O4 U, 0.075[CH2Cl2]'
_chemical_formula_sum            'C27.07 H29.15 Cl0.15 N3 O4 U'
_chemical_formula_weight         703.87
_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
_audit_creation_date             2024-08-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-20 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.710(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1328(7)
_cell_length_b                   17.9440(8)
_cell_length_c                   10.8539(4)
_cell_measurement_reflns_used    6801
_cell_measurement_temperature    93
_cell_measurement_theta_max      28.7080
_cell_measurement_theta_min      2.7170
_cell_volume                     2591.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93.00
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.796
_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      0.00  54.00   0.50    7.63    --    3.93  37.00 -90.00  108
  2  \w    -18.00  37.00   0.50    7.63    --    3.93 -99.00 150.00  110
  3  \w     -5.00  77.00   0.50    7.63    --    3.93  37.00 150.00  164
  4  \w     -5.00  24.00   0.50    7.63    --   -6.20 -99.00 120.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18264
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.781
_diffrn_reflns_theta_min         2.738
_exptl_absorpt_coefficient_mu    6.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.106a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       plate
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.015
_refine_diff_density_max         5.093
_refine_diff_density_min         -2.760
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         6455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0618P)^2^+13.9697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4942
_reflns_number_total             6455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01821d2.cif
_cod_data_source_block           tbuhpdiop_mo_3
_cod_depositor_comments
'Adding full bibliography for 7717089--7717091.cif.'
_cod_database_code               7717090
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.165
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(C19) = Uanis(C18) = Uanis(C17) = Uanis(C16) = Uanis(C15)
Uanis(C25) = Uanis(C26) = Uanis(C24) = Uanis(C27)
Uanis(O3) = Uanis(O1) = Uanis(O4) = Uanis(N3) = Uanis(N2) = Uanis(N1) =
Uanis(O2)
Uanis(C13) = Uanis(C12) = Uanis(C8) = Uanis(C7)
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C11(H11), C10(H10), C15(H15), C9(H9), C3(H3), C5(H5),
 C4(H4), C2(H2), C17(H17)
3.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C27(H27A,H27B,
 H27C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              91608
_shelx_hkl_checksum              36354
_shelx_fab_checksum              63199
_platon_squeeze_void_probe_radius 1.20
_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
;