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_7717388
_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         'C66 H77 Cl3 Li2 N12 O2 U Y, C5 H5 N'
_chemical_formula_sum            'C71 H82 Cl3 Li2 N13 O2 U Y'
_chemical_formula_weight         1596.66
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-12
_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                 106.506(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0604(3)
_cell_length_b                   17.0605(2)
_cell_length_c                   24.4496(4)
_cell_measurement_reflns_used    41820
_cell_measurement_temperature    120.2(8)
_cell_measurement_theta_max      28.4090
_cell_measurement_theta_min      3.5350
_cell_volume                     7622.9(2)
_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      120.2(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.904
_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    -35.00  55.00   1.00   60.00    --  -14.44  33.00  95.00   90
  2  \w    -53.00  37.00   1.00   60.00    --   16.16 -33.00 -62.00   90
  3  \w     -4.00  86.00   1.00   60.00    --   16.16  33.00  95.00   90
  4  \w    -39.00  12.00   1.00   60.00    --  -14.44 -77.00-180.00   51
  5  \w    -41.00  39.00   1.00   60.00    --  -14.44  77.00 -90.00   80
  6  \w    -39.00  12.00   1.00   60.00    --  -14.44 -77.00  60.00   51
  7  \w    -87.00 -39.00   1.00   60.00    --  -14.44-178.00 120.00   48
  8  \w    -11.00  39.00   1.00   60.00    --   16.16  77.00 -30.00   50
  9  \w     35.00  89.00   1.00   60.00    --   16.16-178.00-120.00   54
 10  \w    -11.00  39.00   1.00   60.00    --   16.16  77.00-180.00   50
 11  \w    -20.00  54.00   1.00   60.00    --   16.16 -99.00-180.00   74
 12  \w    -11.00  39.00   1.00   60.00    --   16.16  77.00-120.00   50
 13  \w    -20.00  54.00   1.00   60.00    --   16.16 -99.00  60.00   74
 14  \w     -1.00  83.00   1.00   60.00    --   16.16  57.00   0.00   84
;
_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      0.0295581000
_diffrn_orient_matrix_UB_12      0.0006810000
_diffrn_orient_matrix_UB_13      -0.0122524000
_diffrn_orient_matrix_UB_21      -0.0039983000
_diffrn_orient_matrix_UB_22      0.0411658000
_diffrn_orient_matrix_UB_23      -0.0036612000
_diffrn_orient_matrix_UB_31      0.0248521000
_diffrn_orient_matrix_UB_32      0.0058121000
_diffrn_orient_matrix_UB_33      0.0274104000
_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  0.0709
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            153359
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.868
_diffrn_reflns_theta_min         3.327
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.034
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_correction_T_min  0.203
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       plate
_exptl_crystal_F_000             3212
_exptl_crystal_preparation
'Vapour diffusion of hexane into pyridine solution'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pyridene, hexane'
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.382
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         18097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0254P)^2^+10.9349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13924
_reflns_number_total             18097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02367f2.cif
_cod_data_source_block           to505_refinalised
_cod_database_code               7717388
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H70 N6 U O2 Y Cl2 Li'
_chemical_oxdiff_usercomment     Pyr/hex
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.383
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C31(H31), C20(H20), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C14(H14A,H14B), C2(H2A,H2B), C25(H25A,H25B), C24(H24A,H24B),
 C36(H36A,H36B), C21(H21A,H21B), C23(H23A,H23B), C33(H33A,H33B), C10(H10A,H10B),
  C22(H22A,H22B), C13(H13A,H13B), C11(H11A,H11B), C35(H35A,H35B), C12(H12A,
 H12B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C19(H19), C52(H52), C27(H27), C17(H17), C28(H28), C16(H16),
 C41(H41), C37(H37), C6(H6), C8(H8), C42(H42), C71(H71), C57(H57), C38(H38),
 C5(H5), C59(H59), C56(H56), C61(H61), C39(H39), C64(H64), C51(H51), C53(H53),
 C62(H62), C46(H46), C66(H66), C47(H47), C50(H50), C40(H40), C60(H60), C63(H63),
  C58(H58), C67(H67), C54(H54), C49(H49), C70(H70), C55(H55), C65(H65),
 C48(H48), C68(H68), C69(H69), C43(H43), C45(H45), C44(H44)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 156 electrons were 
found in a volume of 910\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
1[C5H5N] per Formula Unit 
which account for 168 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1054
_shelx_fab_checksum              12009
_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 1.263
_oxdiff_exptl_absorpt_empirical_full_min 0.705