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_7717379
_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         'C80 H110 N12 O6 U2 Y2'
_chemical_formula_sum            'C80 H110 N12 O6 U2 Y2'
_chemical_formula_weight         1989.67
_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             2023-11-24
_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                74.514(2)
_cell_angle_beta                 87.911(2)
_cell_angle_gamma                82.799(2)
_cell_formula_units_Z            2
_cell_length_a                   15.3299(4)
_cell_length_b                   16.2642(4)
_cell_length_c                   21.1749(4)
_cell_measurement_reflns_used    47441
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.7540
_cell_measurement_theta_min      4.2410
_cell_volume                     5047.7(2)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2792
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_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   -118.00 -16.00   1.00    5.00    --  -42.00 -27.00  -4.00  102
  2  \w     16.00 118.00   1.00    5.00    --   42.00  27.00 157.00  102
  3  \w    -34.00  68.00   1.00    5.00    --   42.00 -27.00  -4.00  102
  4  \w     35.00 137.00   1.00   20.00    --  111.00 -27.00  -4.00  102
  5  \w     85.00 178.00   1.00   20.00    --  111.00  27.00 157.00   93
  6  \w    -65.00  31.00   1.00    5.00    --  -42.00  38.00 -60.00   96
  7  \w    -68.00  34.00   1.00    5.00    --  -42.00  27.00 157.00  102
  8  \w   -126.00 -37.00   1.00    5.00    --  -42.00 178.00 120.00   89
  9  \w     10.00  42.00   1.00    5.00    --   42.00  80.00  64.74   32
 10  \w     10.00  42.00   1.00    5.00    --   42.00  80.00 -33.33   32
 11  \w      9.00  42.00   1.00    5.00    --   42.00  82.00  14.12   33
 12  \w     10.00  42.00   1.00    5.00    --   42.00  79.00 157.13   32
 13  \w     61.00 129.00   1.00    5.00    --   42.00 178.00 -90.00   68
 14  \w     10.00  42.00   1.00    5.00    --   42.00  78.00  35.18   32
 15  \w     37.00 108.00   1.00   20.00    --  111.00-107.00 101.80   71
 16  \w     41.00 131.00   1.00   20.00    --  111.00-152.00 -83.39   90
 17  \w     30.00 107.00   1.00   20.00    --  111.00 -94.00-150.00   77
 18  \w     99.00 177.00   1.00   20.00    --  111.00  45.00   0.00   78
 19  \w     61.00 107.00   1.00   20.00    --  111.00 -94.00   0.00   46
 20  \w    121.00 148.00   1.00   20.00    --  111.00 125.00  60.00   27
 21  \w     74.00 107.00   1.00   20.00    --  111.00 -94.00  30.00   33
 22  \w    124.00 174.00   1.00   20.00    --  111.00  15.00-120.00   50
 23  \w     44.00 127.00   1.00   20.00    --  111.00 -61.00-180.00   83
 24  \w     80.00 107.00   1.00   20.00    --  111.00 -94.00 120.00   27
 25  \w     76.00 107.00   1.00   20.00    --  111.00 -94.00-180.00   31
 26  \w    106.00 139.00   1.00   20.00    --  111.00  45.00 -60.00   33
 27  \w     43.00  68.00   1.00   20.00    --  111.00-125.00  60.00   25
 28  \w     99.00 126.00   1.00   20.00    --  111.00 -45.00  30.00   27
 29  \w     98.00 161.00   1.00   20.00    --  111.00 125.00 -90.00   63
 30  \w     42.00 112.00   1.00   20.00    --  111.00-125.00   0.00   70
 31  \w    122.00 165.00   1.00   20.00    --  111.00 125.00-180.00   43
 32  \w     92.00 119.00   1.00   20.00    --  111.00-134.00 -88.39   27
 33  \w     88.00 125.00   1.00   20.00    --  111.00  30.00 -90.00   37
 34  \w     89.00 114.00   1.00   20.00    --  111.00  15.00-120.00   25
 35  \w    104.00 177.00   1.00   20.00    --  111.00  77.00  60.00   73
 36  \w     38.00  65.00   1.00   20.00    --  111.00 -94.00 120.00   27
 37  \w    114.00 165.00   1.00   20.00    --  111.00  30.00-180.00   51
 38  \w     57.00  84.00   1.00   20.00    --  111.00 -77.00 -30.00   27
 39  \w     76.00 103.00   1.00   20.00    --  111.00 -71.00 -41.58   27
 40  \w     44.00 109.00   1.00   20.00    --  111.00-112.00   2.71   65
 41  \w     45.00  70.00   1.00   20.00    --  111.00-107.00-102.22   25
 42  \w     78.00 108.00   1.00   20.00    --  111.00-107.00-102.22   30
 43  \w     44.00  81.00   1.00   20.00    --  111.00 -45.00 -30.00   37
 44  \w    142.00 168.00   1.00   20.00    --  111.00 101.00   0.90   26
 45  \w     42.00  69.00   1.00   20.00    --  111.00 -94.00-180.00   27
 46  \w     82.00 108.00   1.00   20.00    --  111.00-105.00 -87.12   26
 47  \w     83.00 125.00   1.00   20.00    --  111.00  68.00  82.95   42
 48  \w     85.00 113.00   1.00   20.00    --  111.00  66.00 -96.45   28
 49  \w    133.00 177.00   1.00   20.00    --  111.00  66.00 -96.45   44
 50  \w    127.00 154.00   1.00   20.00    --  111.00  30.00 120.00   27
 51  \w     80.00 112.00   1.00   20.00    --  111.00-125.00  60.00   32
 52  \w     52.00  88.00   1.00   20.00    --  111.00 -94.00 -90.00   36
 53  \w     71.00 107.00   1.00   20.00    --  111.00 -94.00  90.00   36
 54  \w     69.00  96.00   1.00   20.00    --  111.00-125.00  90.00   27
 55  \w     94.00 146.00   1.00   20.00    --  111.00  56.00 -63.77   52
 56  \w     84.00 124.00   1.00   20.00    --  111.00  61.00-180.00   40
 57  \w    129.00 155.00   1.00   20.00    --  111.00  61.00-180.00   26
 58  \w    100.00 129.00   1.00   20.00    --  111.00  70.00-112.42   29
 59  \w    138.00 166.00   1.00   20.00    --  111.00  70.00-112.42   28
 60  \w     77.00 108.00   1.00   20.00    --  111.00-125.00 120.00   31
 61  \w     65.00  92.00   1.00   20.00    --  111.00 -94.00 -60.00   27
 62  \w     41.00  87.00   1.00   20.00    --  111.00 -45.00   0.00   46
 63  \w    148.00 178.00   1.00   20.00    --  111.00 125.00-120.00   30
 64  \w    131.00 158.00   1.00   20.00    --  111.00 125.00 120.00   27
 65  \w    114.00 141.00   1.00   20.00    --  111.00  45.00-180.00   27
 66  \w     88.00 147.00   1.00   20.00    --  111.00  45.00  36.65   59
 67  \w    104.00 131.00   1.00   20.00    --  111.00 -77.00   0.00   27
 68  \w    101.00 128.00   1.00   20.00    --  111.00  30.00  90.00   27
 69  \w    107.00 134.00   1.00   20.00    --  111.00  30.00  30.00   27
 70  \w     95.00 132.00   1.00   20.00    --  111.00 -45.00   0.00   37
 71  \w     85.00 124.00   1.00   20.00    --  111.00  62.00-168.61   39
 72  \w    131.00 160.00   1.00   20.00    --  111.00  30.00 -90.00   29
 73  \w    105.00 176.00   1.00   20.00    --  111.00  77.00 120.00   71
 74  \w     71.00 116.00   1.00   20.00    --  111.00 -61.00  90.00   45
 75  \w    102.00 141.00   1.00   20.00    --  111.00 -77.00  60.00   39
 76  \w     81.00 108.00   1.00   20.00    --  111.00 -84.00 171.87   27
 77  \w     96.00 123.00   1.00   20.00    --  111.00 -86.00 123.27   27
 78  \w     37.00  69.00   1.00   20.00    --  111.00 -94.00  30.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0965039000
_diffrn_orient_matrix_UB_12      0.0371506000
_diffrn_orient_matrix_UB_13      0.0060286000
_diffrn_orient_matrix_UB_21      0.0305996000
_diffrn_orient_matrix_UB_22      0.0716021000
_diffrn_orient_matrix_UB_23      0.0258887000
_diffrn_orient_matrix_UB_31      0.0033144000
_diffrn_orient_matrix_UB_32      0.0574030000
_diffrn_orient_matrix_UB_33      -0.0706610000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            107929
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.932
_diffrn_reflns_theta_min         3.630
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.768
_exptl_absorpt_correction_T_max  0.5882
_exptl_absorpt_correction_T_min  0.1098
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1210 before and 0.0749 after correction.
The Ratio of minimum to maximum transmission is 0.1867.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       blade
_exptl_crystal_F_000             1968
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Tetrahydrofuran'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.057
_refine_diff_density_max         4.558
_refine_diff_density_min         -5.129
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         20831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0372P)^2^+69.4686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16990
_reflns_number_total             20831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02367f2.cif
_cod_data_source_block           jl23019_231123_sadabs
_cod_database_code               7717379
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C72H100N12O4Y2U2
_chemical_oxdiff_usercomment     '@ 120 K JHPC TO517-3'
_shelx_estimated_absorpt_t_max   0.579
_shelx_estimated_absorpt_t_min   0.113
_reflns_odcompleteness_completeness 97.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     76.86
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H3BC)=Sof(H3BD)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C80)=Sof(H80A)=Sof(H80B)=
 Sof(C79A)=Sof(H79C)=Sof(H79D)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C79)=Sof(H79A)=Sof(H79B)=
 Sof(C78)=Sof(H78A)=Sof(H78B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C20(H20), C27(H27), C28(H28), C31(H31), C45(H45), C56(H56), C63(H63),
 C64(H64), C67(H67), C81(H81)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C38(H38A,H38B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B), C50(H50A,H50B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
  C60(H60A,H60B), C61(H61A,H61B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,
 H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B),
 C75(H75A,H75B), C76(H76A,H76B), C82(H82A,H82B), C3(H3AA,H3AB), C3(H3BC,H3BD),
 C10(H10A,H10B), C77(H77A,H77B), C79(H79A,H79B), C78(H78A,H78B), C80(H80A,H80B),
  C79A(H79C,H79D)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C16(H16), C17(H17), C19(H19), C30(H30), C41(H41),
 C42(H42), C44(H44), C52(H52), C53(H53), C55(H55), C66(H66)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C37(H37A,H37B,H37C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              72529
_shelx_fab_checksum              32619
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.824
_oxdiff_exptl_absorpt_empirical_full_min 0.595