Multiple oxidation states of uranium stabilized by an O,N,O-ligand
Juarez, Gabriel J.; Mason, Harris E.; Mangel, Daniel N.; Tondreau, Aaron M.; Sessler, Jonathan L.; Chemical Science  (2025) –; doi:10.1039/D5SC04158A

data_1576300
_publ_section_title
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 Multiple oxidation states of uranium stabilized by an O,N,O-ligand
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC04158A
_journal_year                    2025
_chemical_formula_moiety         'C47 H36 N8 O4 U, 2.5[C4H8O]'
_chemical_formula_sum            'C57 H56 N8 O6.5 U'
_chemical_formula_weight         1195.12
_chemical_name_systematic        U(IV)ExPh
_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   mixed
_audit_creation_date             2025-04-22
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7221)
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_audit_update_record
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2025-04-22 deposited with the CCDC.	2025-11-12 downloaded from the CCDC.
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_cell_angle_alpha                67.8940(10)
_cell_angle_beta                 88.4530(10)
_cell_angle_gamma                88.5700(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9637(6)
_cell_length_b                   13.5417(7)
_cell_length_c                   15.7213(8)
_cell_measurement_reflns_used    9817
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      2.22
_cell_volume                     2358.6(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      101.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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  0.0358
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31410
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.224
_exptl_absorpt_coefficient_mu    3.507
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       plate
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.559
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         9602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+5.5779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8459
_reflns_number_total             9602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04158a2.cif
_cod_data_source_block           uexph_dmap_a
_cod_original_formula_sum        'C57 H56 N8 O6.50 U'
_cod_database_code               1576300
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.721
_shelx_estimated_absorpt_t_min   0.621
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C45(H45), C41(H41), C11(H11), C16(H16), C44(H44), C4(H4), C12(H12), C52(H52),
 C33(H33), C42(H42), C32(H32), C14(H14), C30(H30), C31(H31), C13(H13), C24(H24),
  C27(H27), C39(H39), C48(H48), C17(H17), C40(H40), C36(H36), C38(H38),
 C25(H25), C26(H26), C18(H18), C37(H37)
1.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C)
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_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48434
_shelx_fab_checksum              66571
_olex2_submission_special_instructions 'No special instructions were received'