Controlled and sequential single-electron reduction of the uranyl dication.
Obey, Tom J. N.; Nichol, Gary S.; Love, Jason B.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16229–16240; doi:10.1039/d4dt02367f

data_7717376
_publ_section_title
;
 Controlled and sequential single-electron reduction of the uranyl
 dication.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16229
_journal_page_last               16240
_journal_paper_doi               10.1039/d4dt02367f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C72 H96 N12 O4 U2, 2(C7 H8)'
_chemical_formula_sum            'C86 H112 N12 O4 U2'
_chemical_formula_weight         1853.93
_chemical_name_common            '[UO2(HL)]2'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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             2023-11-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-11 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6782(2)
_cell_length_b                   16.9971(2)
_cell_length_c                   18.3318(2)
_cell_measurement_reflns_used    23869
_cell_measurement_temperature    120.0(7)
_cell_measurement_theta_max      29.3740
_cell_measurement_theta_min      3.7580
_cell_volume                     4570.79(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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_environment      N~2~
_diffrn_ambient_temperature      120.0(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.882
_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    -53.00  23.00   1.00   12.50    --  -15.82  97.00 130.00   76
  2  \w    -23.00  54.00   1.00   12.50    --   17.54 -97.00  22.00   77
  3  \w    -30.00   5.00   1.00   12.50    --  -15.82  77.00   0.00   35
  4  \w    -88.00 -43.00   1.00   12.50    --  -15.82-178.00-180.00   45
  5  \w     35.00  90.00   1.00   12.50    --   17.54-178.00 -60.00   55
  6  \w     -9.00  36.00   1.00   12.50    --   17.54  77.00 -60.00   45
  7  \w     39.00  88.00   1.00   12.50    --   17.54 178.00  90.00   49
  8  \w      1.00  83.00   1.00   12.50    --   17.54  57.00-180.00   82
  9  \w     -9.00  39.00   1.00   12.50    --   17.54  77.00  30.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0470492000
_diffrn_orient_matrix_UB_12      -0.0090694000
_diffrn_orient_matrix_UB_13      -0.0019336000
_diffrn_orient_matrix_UB_21      -0.0112580000
_diffrn_orient_matrix_UB_22      -0.0381108000
_diffrn_orient_matrix_UB_23      -0.0132210000
_diffrn_orient_matrix_UB_31      -0.0001690000
_diffrn_orient_matrix_UB_32      0.0143505000
_diffrn_orient_matrix_UB_33      -0.0363245000
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51279
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.383
_diffrn_reflns_theta_min         3.498
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.589
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         11102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+4.6936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9250
_reflns_number_total             11102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02367f2.cif
_cod_data_source_block           to355_refinalised
_cod_database_code               7717376
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C36H47UO2N6
_chemical_oxdiff_usercomment     'Slow precip toluene'
_shelx_estimated_absorpt_t_max   0.673
_shelx_estimated_absorpt_t_min   0.402
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C20(H20), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C2(H2A,H2B), C36(H36A,H36B), C34(H34A,H34B), C35(H35A,H35B),
 C10(H10A,H10B), C13(H13A,H13B), C25(H25A,H25B), C11(H11A,H11B), C32(H32A,H32B),
  C12(H12A,H12B), C21(H21A,H21B), C24(H24A,H24B), C33(H33A,H33B), C23(H23A,
 H23B), C22(H22A,H22B)
2.c Me refined with riding coordinates:
 C37(H37A,H37B,H37C)
2.d Aromatic/amide H refined with riding coordinates:
 N1(H1), C30(H30), C8(H8), C19(H19), C28(H28), C16(H16), C17(H17), C27(H27),
 C6(H6), C5(H5), C43(H43), C40(H40), C39(H39), C42(H42), C41(H41)
2.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12202
_shelx_fab_checksum              8338
_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 1.284
_oxdiff_exptl_absorpt_empirical_full_min 0.805