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_7719944
_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         'Br2.66 N1.34 O6.02 U, C28 H62 P2'
_chemical_formula_sum            'C28 H62 Br2.66 N1.34 O6.02 P2 U'
_chemical_formula_weight         1026.40
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-08-20
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-08-20 deposited with the CCDC.	2025-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.3210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1103(7)
_cell_length_b                   15.2774(6)
_cell_length_c                   16.2613(6)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.466
_cell_measurement_theta_min      2.520
_cell_volume                     3986.2(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_av_unetI/netI     0.0630
_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       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            79960
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.498
_diffrn_reflns_theta_min         1.841
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed X-ray tube'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    6.854
_exptl_absorpt_correction_T_max  0.4935
_exptl_absorpt_correction_T_min  0.2502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1319 before and 0.0712 after correction.
The Ratio of minimum to maximum transmission is 0.5070.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       block
_exptl_crystal_F_000             2011
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.982
_refine_diff_density_min         -2.282
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         10101
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0388
_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^)+11.0512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7989
_reflns_number_total             10101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02671g2.cif
_cod_data_source_block           auf3
_cod_database_code               7719944
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.250
_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. Restrained distances
 O7-N2 \\sim O8-N2 \\sim O6-N2
 with sigma of 0.02
 O9-N3 \\sim O10-N3 \\sim O11-N3
 with sigma of 0.02
3. Restrained planarity
 N3, O11, O9, O10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(Br2) = Uanis(N2)
Uanis(Br3) = Uanis(N3)
5. Rigid body (RIGU) restrains
 O7, N2, O8, O6
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 O9, N3, O10, O11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: Br2(0.86) Br3(0.8) O9(0.2) O11(0.2) O10(0.2) N3(0.2) O6(0.14)
 O7(0.14) O8(0.14) N2(0.14)
7.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C21(H21A,H21B), C18(H18A,H18B), C4(H4A,H4B), C1(H1A,H1B),
 C23(H23A,H23B), C9(H9A,H9B), C2(H2A,H2B), C13(H13A,H13B), C3(H3A,H3B),
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C22(H22A,H22B), C19(H19A,H19B),
  C11(H11A,H11B), C5(H5A,H5B), C14(H14A,H14B), C6(H6A,H6B), C7(H7A,H7B),
 C15(H15A,H15B), C10(H10A,H10B)
7.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C28(H28A,H28B,H28C), C20(H20A,H20B,H20C), C24(H24A,H24B,
 H24C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              17238
_olex2_submission_special_instructions 'No special instructions were received'