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_7717386
_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         'C47 H70 K N8 Na O2 Si2 U, 1.5(C6 H14)'
_chemical_formula_sum            'C56 H91 K N8 Na O2 Si2 U'
_chemical_formula_weight         1264.66
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-12-11
_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                 92.423(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.8382(18)
_cell_length_b                   15.5671(10)
_cell_length_c                   28.998(3)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      2.48
_cell_measurement_theta_min      26.08
_cell_volume                     12104.3(17)
_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)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21269
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.702
_diffrn_reflns_theta_min         2.043
_exptl_absorpt_coefficient_mu    2.843
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 595361 reflections, Rint = 0.0925
 (208722 with I > 3sig(I), Rint = 0.0572)
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             5192
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pyridene, hexane'
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.035
_exptl_transmission_factor_max   0.431466
_exptl_transmission_factor_min   0.334954
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         21269
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0518
_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^)+129.8202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16103
_reflns_number_total             21269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02367f2.cif
_cod_data_source_block           tom_jl22023_i2oa
_cod_original_cell_volume        12104.4(17)
_cod_database_code               7717386
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.431
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5741(6)
 0.4259(6)
2. 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
3. Restrained distances
 C53-C52 = C52-C51 = C51-C50 = C50-C49 = C49-C48
 1.52 with sigma of 0.02
 C54-C55 = C55-C56 = C56-C57 = C57-C58 = C58-C59
 1.52 with sigma of 0.02
 C60-C61 = C61-C62 = C62-C63 = C63-C64 = C64-C65
 1.52 with sigma of 0.02
 C53-C51 = C50-C48
 2.53 with sigma of 0.04
 C52-C50 = C51-C49
 2.54 with sigma of 0.04
 C54-C56 = C57-C59
 2.53 with sigma of 0.04
 C55-C57 = C56-C58
 2.54 with sigma of 0.04
 C60-C62 = C63-C65
 2.53 with sigma of 0.04
 C61-C63 = C62-C64
 2.54 with sigma of 0.04
 C53-C52 \\sim C52-C51 \\sim C51-C50 \\sim C50-C49 \\sim C49-C48
 with sigma of 0.02
 C53-C51 \\sim C51-C49 \\sim C52-C50 \\sim C50-C48
 with sigma of 0.04
 C54-C56 \\sim C56-C58 \\sim C55-C57 \\sim C57-C59
 with sigma of 0.04
 C54-C55 \\sim C55-C56 \\sim C56-C57 \\sim C57-C58 \\sim C58-C59
 with sigma of 0.02
 C60-C61 \\sim C61-C62 \\sim C62-C63 \\sim C63-C64 \\sim C64-C65
 with sigma of 0.02
 C60-C62 \\sim C62-C64 \\sim C61-C63 \\sim C63-C65
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C53 \\sim C52 \\sim C51 \\sim C50 \\sim C49 \\sim C48: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C53, C52, C51, C50, C49, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C54, C55, C56, C57, C58, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C60, C61, C62, C63, C64, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C52(0.5) H52A(0.5)
 H52B(0.5) C51(0.5) H51A(0.5) H51B(0.5) C50(0.5) H50A(0.5) H50B(0.5) C49(0.5)
 H49A(0.5) H49B(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C54(0.5) H54A(0.5)
 H54B(0.5) H54C(0.5) C55(0.5) H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5)
 C57(0.5) H57A(0.5) H57B(0.5) C58(0.5) H58A(0.5) H58B(0.5) C59(0.5) H59A(0.5)
 H59B(0.5) H59C(0.5) C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C61(0.5) H61A(0.5)
 H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) C64(0.5)
 H64A(0.5) H64B(0.5) C65(0.5) H65A(0.5) H65B(0.5) H65C(0.5)
7.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C16(H16), C31(H31), C9(H9)
7.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C2(H2A,H2B), C21(H21A,H21B), C25(H25A,H25B), C11(H11A,H11B),
 C32(H32A,H32B), C13(H13A,H13B), C23(H23A,H23B), C35(H35A,H35B), C36(H36A,H36B),
  C33(H33A,H33B), C12(H12A,H12B), C14(H14A,H14B), C34(H34A,H34B), C22(H22A,
 H22B), C24(H24A,H24B), C52(H52A,H52B), C51(H51A,H51B), C50(H50A,H50B),
 C49(H49A,H49B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B),
  C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B)
7.c Me refined with riding coordinates:
 C53(H53A,H53B,H53C), C48(H48A,H48B,H48C)
7.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C19(H19), C8(H8), C6(H6), C27(H27), C28(H28), C30(H30), C44(H44),
 C47(H47), C43(H43)
7.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C42(H42A,H42B,
 H42C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C40(H40A,H40B,H40C), C54(H54A,
 H54B,H54C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              33153
_olex2_submission_special_instructions 'No special instructions were received'