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_7717382
_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         'C92 H114 Cl2 N16 O4 Sm2 U2'
_chemical_formula_sum            'C92 H114 Cl2 N16 O4 Sm2 U2'
_chemical_formula_weight         2355.65
_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             2023-11-24
_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                 104.5910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.5417(2)
_cell_length_b                   17.1342(2)
_cell_length_c                   17.6710(2)
_cell_measurement_reflns_used    45983
_cell_measurement_temperature    120.1(3)
_cell_measurement_theta_max      29.3130
_cell_measurement_theta_min      3.6640
_cell_volume                     5139.95(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      120.1(3)
_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 0.918
_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  51.00   1.00   20.00    --  -15.66  60.00-143.00   84
  2  \w    -83.00   2.00   1.00   20.00    --  -15.66 -60.00  76.00   85
  3  \w      0.00  84.00   1.00   20.00    --   17.38  60.00-143.00   84
  4  \w    -50.00  35.00   1.00   20.00    --   17.38 -60.00  76.00   85
  5  \w    -88.00 -39.00   1.00   20.00    --  -15.66-178.00 -90.00   49
  6  \w    -52.00  36.00   1.00   20.00    --   17.38 -38.00 -60.00   88
  7  \w     -9.00  39.00   1.00   20.00    --   17.38  77.00 -60.00   48
  8  \w     -9.00  39.00   1.00   20.00    --   17.38  77.00-180.00   48
  9  \w     -9.00  39.00   1.00   20.00    --   17.38  77.00  60.00   48
 10  \w    -42.00  39.00   1.00   20.00    --  -15.66  77.00-120.00   81
 11  \w      1.00  85.00   1.00   20.00    --   17.38  57.00 -60.00   84
 12  \w    -20.00  55.00   1.00   20.00    --   17.38 -99.00  30.00   75
 13  \w    -20.00  55.00   1.00   20.00    --   17.38 -99.00-180.00   75
 14  \w     -9.00  39.00   1.00   20.00    --   17.38  77.00   0.00   48
 15  \w    -20.00  55.00   1.00   20.00    --   17.38 -99.00 -90.00   75
 16  \w    -52.00  36.00   1.00   20.00    --   17.38 -38.00 120.00   88
 17  \w      1.00  30.00   1.00   20.00    --   17.38  57.00  30.00   29
;
_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      0.0072686000
_diffrn_orient_matrix_UB_12      0.0180993000
_diffrn_orient_matrix_UB_13      0.0372064000
_diffrn_orient_matrix_UB_21      0.0022353000
_diffrn_orient_matrix_UB_22      0.0368782000
_diffrn_orient_matrix_UB_23      -0.0176048000
_diffrn_orient_matrix_UB_31      -0.0410802000
_diffrn_orient_matrix_UB_32      0.0052392000
_diffrn_orient_matrix_UB_33      -0.0049846000
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            133748
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.478
_diffrn_reflns_theta_min         3.366
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.371
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_correction_T_min  0.363
_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    1.522
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             2304
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pyridene, hexane'
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.044
_refine_diff_density_max         2.035
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         13125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0231P)^2^+7.0749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11074
_reflns_number_total             13125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02367f2.cif
_cod_data_source_block           to516_refinalised
_cod_database_code               7717382
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C72 H94 N12 U2 O4 Sm2 Cl2'
_chemical_oxdiff_usercomment     pyridine/hexane
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.393
_reflns_odcompleteness_completeness 99.74
_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
 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:
 C21(H21A,H21B), C2(H2A,H2B), C25(H25A,H25B), C14(H14A,H14B), C22(H22A,H22B),
 C32(H32A,H32B), C36(H36A,H36B), C10(H10A,H10B), C23(H23A,H23B), C34(H34A,H34B),
  C33(H33A,H33B), C35(H35A,H35B), C24(H24A,H24B), C11(H11A,H11B), C13(H13A,
 H13B), C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C30(H30), C17(H17), C16(H16), C42(H42), C27(H27), C28(H28), C6(H6),
 C37(H37), C5(H5), C8(H8), C41(H41), C46(H46), C43(H43), C40(H40), C39(H39),
 C44(H44), C45(H45), C38(H38)
2.d 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              4931
_shelx_fab_checksum              5130
_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 1.091
_oxdiff_exptl_absorpt_empirical_full_min 0.917