Steric hindrance of phenanthroline diamides enables a hundredfold increase in Am(III) extraction efficiency.
Avagyan, Nane A.; Zonov, Roman V.; Lemport, Pavel S.; Evsiunina, Mariia V.; Matveev, Petr I.; Roznyatovsky, Vitaly A.; Averin, Alexei D.; Kalle, Paulina; Tafeenko, Victor A.; Soloveva, Svetlana A.; Nelyubina, Yulia V.; Petrov, Vladimir G.; Ustynyuk, Yuri A.; Nenajdenko, Valentine G.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5425–5437; doi:10.1039/d5dt00076a

data_7718114
_publ_section_title
;
 Steric hindrance of phenanthroline diamides enables a hundredfold
 increase in Am(III) extraction efficiency.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5425
_journal_page_last               5437
_journal_paper_doi               10.1039/d5dt00076a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C38 H42 N4 O2'
_chemical_formula_sum            'C38 H42 N4 O2'
_chemical_formula_weight         586.75
_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   geom
_audit_creation_date             2025-02-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-11 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                94.213(8)
_cell_angle_beta                 92.420(8)
_cell_angle_gamma                95.485(8)
_cell_formula_units_Z            4
_cell_length_a                   8.974(2)
_cell_length_b                   14.552(4)
_cell_length_c                   24.460(6)
_cell_measurement_reflns_used    2719
_cell_measurement_temperature    120
_cell_measurement_theta_max      22.574
_cell_measurement_theta_min      2.269
_cell_volume                     3167.1(14)
_computing_cell_refinement       'SAINT V8.30A (22 Oct 2012)'
_computing_data_reduction        'SAINT V8.30A (22 Oct 2012)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.00
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1858
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16184
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         0.836
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0819 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.8630.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       prism
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0071(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         16184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1698
_refine_ls_R_factor_gt           0.0940
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1343P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2439
_refine_ls_wR_factor_ref         0.2956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8515
_reflns_number_total             16184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00076a2.cif
_cod_data_source_block           l2
_cod_depositor_comments
'Adding full bibliography for 7718113--7718120.cif.'
_cod_original_cell_volume        3167.2(14)
_cod_database_code               7718114
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.810(3)
 0.190(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C31A(H31C,H31D), C37A(H37C,H37D), C18(H18A,H18B), C18A(H18C,H18D), C27A(H27C,
 H27D), C31(H31A,H31B), C24(H24A,H24B), C14(H14A,H14B), C27(H27A,H27B),
 C24A(H24C,H24D), C37(H37A,H37B), C14A(H14C,H14D)
3.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C35A(H35A), C21(H21), C34A(H34A), C20A(H20A), C20(H20), C35(H35),
 C33A(H33A), C5A(H5A), C21A(H21A), C22A(H22A), C4A(H4A), C11A(H11A), C34(H34),
 C8A(H8A), C33(H33), C10(H10), C10A(H10A), C5(H5), C11(H11), C7A(H7A), C4(H4),
 C7(H7), C8(H8)
3.c Idealised Me refined as rotating group:
 C32A(H32D,H32E,H32F), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C28(H28A,
 H28B,H28C), C25(H25A,H25B,H25C), C15A(H15D,H15E,H15F), C38A(H38D,H38E,H38F),
 C25A(H25D,H25E,H25F), C38(H38A,H38B,H38C), C32(H32A,H32B,H32C), C28A(H28D,H28E,
 H28F), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              30108
_shelx_hkl_checksum              99656
_olex2_submission_special_instructions 'No special instructions were received'