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_1576301
_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         'C60 H42 N9 O13 U3, C6 H15 N, C6 H16 N'
_chemical_formula_sum            'C72 H73 N11 O13 U3'
_chemical_formula_weight         2014.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-04-22
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7221)
;
_audit_update_record
;
2025-04-22 deposited with the CCDC.	2025-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4420(6)
_cell_length_b                   17.7005(6)
_cell_length_c                   26.7887(9)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.25
_cell_volume                     7793.5(5)
_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      100.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0894
_diffrn_reflns_av_unetI/netI     0.1026
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            64779
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.498
_diffrn_reflns_theta_min         1.907
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.283
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       plate
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.911
_refine_diff_density_min         -2.650
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         19664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0466P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12714
_reflns_number_total             19664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04158a2.cif
_cod_data_source_block           peetwooneoncee_a
_cod_database_code               1576301
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.366
_shelx_estimated_absorpt_t_min   0.303
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N00N(H00N)
2.b Secondary CH2 refined with riding coordinates:
 C010(H01B,H01E), C017(H01G,H01J), C01U(H01W,H01), C023(H02X,H02Y), C026(H02,
 HB), C02F(H02S,H02T)
2.c Aromatic/amide H refined with riding coordinates:
 N00K(H00K), C4(H4), N00U(H00U), N00X(H00X), C00Z(H00Z), C012(H012),
 C019(H019), C01A(H01A), C01C(H01C), C01D(H01D), C01F(H01F), C01H(H01H),
 C01I(H01I), C01K(H01K), C01M(H01M), C01P(H01P), C01Q(H01Q), C01S(H01S),
 C01T(H01T), C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020), C022(H022),
 C024(H024), C028(H028), C029(H029), C02A(H02A), C02B(H02B), C02D(H02D),
 C02E(H02E), C02G(H02G), C02H(H02H), C02I(H02I), C02J(H02J), C02L(H02L),
 C02M(H02M), C02N(H02N), C02O(H02O), C02P(H02P), C02Q(H02Q), C02R(H02R)
2.d Idealised Me refined as rotating group:
 C01E(H01R,H01U,H01V), C01G(H01L,H01N,H01O), C025(H02Z,H,HA), C027(H1,HC,HD),
 C02C(H02C,H02F,H02K), C02K(H02U,H02V,H02W)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78076
_shelx_fab_checksum              6955
_olex2_submission_special_instructions 'No special instructions were received'