Diphosphonium salts as effective extractants for the separation of uranium(VI) from nitric acid media
Fominykh, Anna; Gerasimov, Mikhail A.; Poliakova, Tatiana R.; Novichkov, Daniil; Kalle, Paulina; Averin, Alexey A.; Krot, Anna; Borisova, Nataliya E.; Matveev, Petr I.; Dalton Transactions  (2025) –; doi:10.1039/D5DT02671G

data_7719945
_publ_section_title
;
 Diphosphonium salts as effective extractants for the separation of
 uranium(VI) from nitric acid media
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT02671G
_journal_year                    2025
_chemical_formula_moiety         'N4 O14 U, C26 H58 P2'
_chemical_formula_sum            'C26 H58 N4 O14 P2 U'
_chemical_formula_weight         950.73
_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             2025-10-23
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-10-27 deposited with the CCDC.	2025-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.168(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5385(11)
_cell_length_b                   14.5329(10)
_cell_length_c                   20.9539(15)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.473
_cell_measurement_theta_min      2.342
_cell_volume                     3817.4(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART Photon II'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0984
_diffrn_reflns_av_unetI/netI     0.0929
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49200
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.581
_diffrn_reflns_theta_min         1.705
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed X-ray tube'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.400
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1402 before and 0.0912 after correction.
The Ratio of minimum to maximum transmission is 0.4079.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.929
_refine_diff_density_min         -1.824
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         11617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0204P)^2^+4.9722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8515
_reflns_number_total             11617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02671g2.cif
_cod_data_source_block           af882
_cod_database_code               7719945
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.473
_shelx_estimated_absorpt_t_min   0.325
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B),
  C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C18(H18A,H18B,
 H18C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              96238
_olex2_submission_special_instructions 'No special instructions were received'