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_7717384
_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         'C87 H109 N15 O4 U2 Zn2'
_chemical_formula_sum            'C87 H109 N15 O4 U2 Zn2'
_chemical_formula_weight         2035.69
_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             2023-09-04
_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                 100.975(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3634(6)
_cell_length_b                   18.9972(7)
_cell_length_c                   15.4266(6)
_cell_measurement_reflns_used    9385
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.499
_cell_measurement_theta_min      2.586
_cell_volume                     4132.4(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            196713
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.620
_diffrn_reflns_theta_min         2.144
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.540
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0886 before and 0.0493 after correction.
The Ratio of minimum to maximum transmission is 0.7390.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       slab
_exptl_crystal_F_000             2024
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pyridene, hexane'
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.047
_refine_diff_density_max         1.927
_refine_diff_density_min         -2.158
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         15026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+6.4586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12811
_reflns_number_total             15026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02367f2.cif
_cod_data_source_block           mo_jl23016_0m
_cod_database_code               7717384
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.427
_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. Others
 Fixed Sof: N2(0.5) C7(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C8(0.5) H8(0.5)
 C9(0.5) H9(0.5) N52(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5) C55(0.5) H55(0.5)
 CXF(0.5) HXF(0.5) C24(0.5) H24(0.5) C14(0.5) H14A(0.5) H14B(0.5) C13(0.5)
 H13A(0.5) H13B(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 C10(0.5) H10A(0.5) H10B(0.5) C19(0.5) H19(0.5) N3(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) C52(0.5) H52A(0.5) H52B(0.5) C20(0.5) H20A(0.5) H20B(0.5) C21(0.5)
 H21A(0.5) H21B(0.5) C18(0.5) H18(0.5) C22(0.5) H22A(0.5) H22B(0.5) C17(0.5)
 C16(0.5) H16(0.5) C15(0.5) H15(0.5)
3.a Ternary CH refined with riding coordinates:
 C41(H41), C30(H30), C24(H24), C19(H19)
3.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C35(H35A,H35B), C31(H31A,H31B), C2(H2A,H2B), C34(H34A,H34B),
 C42(H42A,H42B), C45(H45A,H45B), C32(H32A,H32B), C43(H43A,H43B), C44(H44A,H44B),
  C33(H33A,H33B), C14(H14A,H14B), C13(H13A,H13B), C11(H11A,H11B), C12(H12A,
 H12B), C10(H10A,H10B), C23(H23A,H23B), C52(H52A,H52B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B)
3.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C26(H26), C40(H40), C27(H27), C37(H37), C38(H38), C51(H51),
 C47(H47), C5(H5), C50(H50), C6(H6), C49(H49), C48(H48), C8(H8), C9(H9),
 C53(H53), C54(H54), C55(H55), CXF(HXF), C18(H18), C16(H16), C15(H15)
3.d Fitted hexagon refined as free rotating group:
 C9(N52,C53,C54,C55,CXF)
3.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              38409
_olex2_submission_special_instructions 'No special instructions were received'