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_7717378
_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         'C41 H53 N7 O2 U'
_chemical_formula_sum            'C41 H53 N7 O2 U'
_chemical_formula_weight         913.93
_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                83.518(3)
_cell_angle_beta                 85.015(2)
_cell_angle_gamma                75.569(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3701(3)
_cell_length_b                   11.9785(5)
_cell_length_c                   14.9463(4)
_cell_measurement_reflns_used    14471
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      27.2660
_cell_measurement_theta_min      3.5150
_cell_volume                     1955.15(11)
_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  (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 0.998
_diffrn_measured_fraction_theta_max 0.994
_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    -33.00  54.00   1.00   30.00    --  -14.44  40.00  -3.00   87
  2  \w    -83.00   4.00   1.00   30.00    --  -14.44 -40.00-156.00   87
  3  \w    -53.00  34.00   1.00   30.00    --   16.16 -40.00-156.00   87
  4  \w    -11.00  39.00   1.00   30.00    --   16.16  77.00-120.00   50
  5  \w     -1.00  83.00   1.00   30.00    --   16.16  57.00  30.00   84
  6  \w    -53.00  35.00   1.00   30.00    --   16.16 -38.00  90.00   88
  7  \w    -20.00  54.00   1.00   30.00    --   16.16 -99.00-180.00   74
  8  \w    -11.00  39.00   1.00   30.00    --   16.16  77.00 120.00   50
  9  \w    -39.00  12.00   1.00   30.00    --  -14.44 -77.00 -90.00   51
 10  \w    -41.00   2.00   1.00   30.00    --  -14.44  77.00  30.00   43
 11  \w    -39.00  43.00   1.00   30.00    --   16.16 -77.00 -90.00   82
 12  \w    -20.00  54.00   1.00   30.00    --   16.16 -99.00  30.00   74
 13  \w    -11.00  39.00   1.00   30.00    --   16.16  77.00-180.00   50
;
_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      0.0173602000
_diffrn_orient_matrix_UB_12      -0.0613927000
_diffrn_orient_matrix_UB_13      0.0040008000
_diffrn_orient_matrix_UB_21      -0.0508367000
_diffrn_orient_matrix_UB_22      -0.0011044000
_diffrn_orient_matrix_UB_23      -0.0239377000
_diffrn_orient_matrix_UB_31      0.0357648000
_diffrn_orient_matrix_UB_32      0.0014246000
_diffrn_orient_matrix_UB_33      -0.0412397000
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_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            36204
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.404
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.195
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.631
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pyridene, hexane'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.970
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         7952
_refine_ls_number_restraints     516
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0469P)^2^+1.8730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6812
_reflns_number_total             7952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02367f2.cif
_cod_data_source_block           to500_twin1_hklf4_refinalised
_cod_database_code               7717378
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C41 H91 N7 U O2 '
_chemical_oxdiff_usercomment     pyr/hexane
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.356
_reflns_odcompleteness_completeness 99.42
_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 C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. 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
3. Others
 Sof(H23C)=Sof(H23D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C20A)=Sof(H20A)=
 Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C24A)=
 Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(C20)=Sof(H20)=Sof(H23A)=Sof(H23B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C21)=
 Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C31(H31), C9(H9), C20(H20), C20A(H20A)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C14(H14A,H14B), C32(H32A,H32B), C13(H13A,H13B), C33(H33A,H33B),
 C10(H10A,H10B), C12(H12A,H12B), C11(H11A,H11B), C23(H23A,H23B), C23(H23C,H23D),
  C34(H34A,H34B), C35(H35A,H35B), C25(H25A,H25B), C36(H36A,H36B), C21(H21A,
 H21B), C22(H22A,H22B), C24(H24A,H24B), C21A(H21C,H21D), C22A(H22C,H22D),
 C25A(H25C,H25D), C24A(H24C,H24D)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C41(H41), C19(H19), C28(H28), C30(H30), C27(H27), C40(H40), C8(H8),
 C38(H38), C37(H37), C17(H17), C16(H16), C39(H39), C5(H5), C6(H6)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              26470
_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 1.482
_oxdiff_exptl_absorpt_empirical_full_min 0.832