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_7717377
_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         'C40 H56 N6 O3 U'
_chemical_formula_sum            'C40 H56 N6 O3 U'
_chemical_formula_weight         906.93
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2023-11-23
_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                81.684(4)
_cell_angle_beta                 84.377(4)
_cell_angle_gamma                75.615(5)
_cell_formula_units_Z            2
_cell_length_a                   11.5408(7)
_cell_length_b                   11.7266(6)
_cell_length_c                   15.0732(7)
_cell_measurement_reflns_used    11735
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      25.4270
_cell_measurement_theta_min      3.6040
_cell_volume                     1951.09(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_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    -42.00  14.00   1.00   30.00    --  -15.66 -84.00-146.00   56
  2  \w    -46.00  43.00   1.00   30.00    --  -15.66  84.00 -26.00   89
  3  \w    -43.00  48.00   1.00   30.00    --   17.38 -84.00-146.00   91
  4  \w    -88.00 -39.00   1.00   30.00    --  -15.66-178.00-150.00   49
  5  \w    -39.00  11.00   1.00   30.00    --  -15.66 -77.00 120.00   50
  6  \w    -85.00   3.00   1.00   30.00    --  -15.66 -38.00  30.00   88
  7  \w    -87.00  14.00   1.00   30.00    --  -15.66 -19.00 120.00  101
  8  \w     -9.00  39.00   1.00   30.00    --   17.38  77.00  30.00   48
  9  \w    -39.00  44.00   1.00   30.00    --   17.38 -77.00 120.00   83
 10  \w     -9.00  39.00   1.00   30.00    --   17.38  77.00 -30.00   48
 11  \w    -32.00  52.00   1.00   30.00    --  -15.66  57.00  90.00   84
 12  \w    -83.00   1.00   1.00   30.00    --  -15.66 -57.00 -30.00   84
 13  \w    -39.00  44.00   1.00   30.00    --   17.38 -77.00 -60.00   83
 14  \w     -9.00  39.00   1.00   30.00    --   17.38  77.00-180.00   48
 15  \w    -20.00  56.00   1.00   30.00    --   17.38 -99.00 150.00   76
 16  \w    -20.00   5.00   1.00   30.00    --   17.38 -99.00 -60.00   25
 17  \w    -20.00  56.00   1.00   30.00    --   17.38 -99.00  60.00   76
;
_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      0.0629418000
_diffrn_orient_matrix_UB_12      -0.0234360000
_diffrn_orient_matrix_UB_13      -0.0027774000
_diffrn_orient_matrix_UB_21      0.0038472000
_diffrn_orient_matrix_UB_22      0.0190550000
_diffrn_orient_matrix_UB_23      0.0419538000
_diffrn_orient_matrix_UB_31      -0.0081459000
_diffrn_orient_matrix_UB_32      -0.0552141000
_diffrn_orient_matrix_UB_33      0.0224358000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15591
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.768
_diffrn_reflns_theta_min         3.262
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Tetrahydrofuran'
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.244
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         15591
_refine_ls_number_restraints     460
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0558P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12658
_reflns_number_total             15591
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 6.9604\% 
around [0.56 0.82 0.11] (reciprocal) or [0.47 0.88 -0.05] (direct)
;
_cod_data_source_file            d4dt02367f2.cif
_cod_data_source_block           to257_2comp_221123_refinalized_twin1_hklf4
_cod_database_code               7717377
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C36H48N6O2U
_chemical_oxdiff_usercomment     '@ 120 K'
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.460
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4401(7)
 0.5599(7)
2. 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
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C31(H31), C20(H20), C9(H9)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C40(H40A,H40B), C32(H32A,H32B), C10(H10A,H10B), C21(H21A,H21B),
 C37(H37A,H37B), C25(H25A,H25B), C11(H11A,H11B), C36(H36A,H36B), C39(H39A,H39B),
  C33(H33A,H33B), C34(H34A,H34B), C14(H14A,H14B), C22(H22A,H22B), C23(H23A,
 H23B), C12(H12A,H12B), C35(H35A,H35B), C24(H24A,H24B), C38(H38A,H38B),
 C13(H13A,H13B)
4.c Aromatic/amide H refined with riding coordinates:
 C30(H30), N1(H1), C19(H19), C8(H8), C27(H27), C17(H17), C16(H16), C28(H28),
 C5(H5), C6(H6)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              6836
_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 2.425
_oxdiff_exptl_absorpt_empirical_full_min 0.743
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2