Selective electrochemical capture and release of uranyl from aqueous alkali, lanthanide, and actinide mixtures using redox-switchable carboranes
Keener, Megan; Mattejat, Maxwell; Zheng, Shao-Liang; Wu, Guang; Hayton, Trevor W.; Ménard, Gabriel; Chemical Science  (2022) –; doi:10.1039/D1SC07070C

data_1566417
_publ_section_title
;
 Selective electrochemical capture and release of uranyl from aqueous
 alkali, lanthanide, and actinide mixtures using redox-switchable
 carboranes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC07070C
_journal_year                    2022
_chemical_formula_moiety
'3(C20 Co), C78 H90 B30 Nd O6 P6, 4(C4 H6 N2)'
_chemical_formula_sum            'C154 H129 B30 Co3 N8 Nd O6 P6'
_chemical_formula_weight         3018.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-10-12
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2021-11-24 deposited with the CCDC.	2022-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.004(6)
_cell_length_b                   23.285(7)
_cell_length_c                   36.829(12)
_cell_measurement_reflns_used    3122
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      22.59
_cell_measurement_theta_min      2.33
_cell_volume                     16297(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1029
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            124957
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.106
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6709
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0761 before and 0.0677 after correction.
The Ratio of minimum to maximum transmission is 0.9001.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             6152
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.719
_refine_diff_density_min         -2.282
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         13905
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.0939
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1278P)^2^+193.5547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2423
_refine_ls_wR_factor_ref         0.2750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9769
_reflns_number_total             13905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc07070c2.cif
_cod_data_source_block           ndcp_0m
_cod_database_code               1566417
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.839
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C81 \\sim N2-C83 \\sim N3-C85 \\sim N4-C87
 with sigma of 0.01
 C81-C82 \\sim C83-C84 \\sim C85-C86 \\sim C87-C88
 with sigma of 0.01
 N1-C82 \\sim N2-C84 \\sim N3-C86 \\sim N4-C88
 with sigma of 0.01
 C77-C73 \\sim C77-C71 \\sim C78-C72 \\sim C78-C74 \\sim C75-C71 \\sim C75-C74
 with sigma of 0.01
 C60-C61 \\sim C61-C62 \\sim C62-C63 \\sim C63-C64 \\sim C64-C60
 with sigma of 0.01
 C60-C61 \\sim C70-C71 \\sim C71-C72 \\sim C72-C73 \\sim C73-C74 \\sim C74-C70
 with sigma of 0.01
 C60-C62 \\sim C61-C63 \\sim C62-C64 \\sim C63-C60 \\sim C64-C61
 with sigma of 0.01
 C60-C62 \\sim C70-C72 \\sim C71-C73 \\sim C72-C74 \\sim C73-C70 \\sim C74-C71
 with sigma of 0.01
 C65-C60 \\sim C66-C61 \\sim C67-C62 \\sim C68-C63 \\sim C69-C64
 with sigma of 0.01
 C65-C66 \\sim C77-C78 \\sim C78-C79 \\sim C79-C75
 with sigma of 0.01
 C65-C66 \\sim C66-C67 \\sim C67-C68 \\sim C68-C69 \\sim C69-C65
 with sigma of 0.01
 C65-C60 \\sim C75-C70 \\sim C77-C72 \\sim C78-C73 \\sim C79-C74
 with sigma of 0.01
 Co2-C75 \\sim Co2-C77 \\sim Co2-C78 \\sim Co2-C79 \\sim Co2-C65
 with sigma of 0.01
3. Restrained planarity
 C60, C61, C62, C63, C64, C65, C66, C67, C68, C69
 with sigma of 0.1
 C70, C71, C72, C73, C74, C75, C77, C78, C79
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(N2) = Uanis(N3) = Uanis(N4)
Uanis(C81) = Uanis(C83) = Uanis(C85) = Uanis(C87)
Uanis(C82) = Uanis(C84) = Uanis(C86) = Uanis(C88)
Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48) = Uanis(C49)
Uiso(C60) = Uiso(C61) = Uiso(C62) = Uiso(C63) = Uiso(C64) = Uiso(C70) =
Uiso(C71) = Uiso(C72) = Uiso(C73) = Uiso(C74)
Uiso(C65) = Uiso(C66) = Uiso(C67) = Uiso(C68) = Uiso(C69) = Uiso(C75) =
Uiso(C77) = Uiso(C78) = Uiso(C79)
5. Others
 Fixed Sof: C60(0.5) C61(0.5) C62(0.5) C63(0.5) C64(0.5) C65(0.5) C67(0.5)
 C68(0.5) C69(0.5) C70(0.5) C71(0.5) C72(0.5) C73(0.5) C74(0.5) C75(0.5)
 C78(0.5) C79(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4A), C5(H5A), C6(H6A), C7(H7A), C9(H9A), C10(H10A), C11(H11A),
 C12(H12A), C13(H13A), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31),
  C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
6.b Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C88(H88A,H88B,
 H88C)
6.c Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8), B9(H9),
 B10(H10), B11(H11), B12(H12), B13(H13), B14(H14), B15(H15)
;
_shelx_res_checksum              19797
_shelx_hkl_checksum              73645
_olex2_submission_special_instructions 'No special instructions were received'