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_7718120
_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         'C42 H50 Eu N7 O11, C2 H3 N'
_chemical_formula_sum            'C44 H53 Eu N8 O11'
_chemical_formula_weight         1021.90
_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             2024-10-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-27 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.189(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5781(7)
_cell_length_b                   20.0588(13)
_cell_length_c                   17.1370(9)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.242
_cell_measurement_theta_min      2.357
_cell_volume                     4630.7(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX-II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50214
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.570
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.421
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1193 before and 0.0643 after correction.
The Ratio of minimum to maximum transmission is 0.7397.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         10635
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+7.2289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8643
_reflns_number_total             10635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00076a2.cif
_cod_data_source_block           2113eu
_cod_depositor_comments
'Adding full bibliography for 7718113--7718120.cif.'
_cod_database_code               7718120
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.580
_olex2_refinement_description
;
1. 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
2. Restrained distances
 N4-C41 = N4-C41A
 1.45 with sigma of 0.02
 C40-C38 = C40A-C38
 1.54 with sigma of 0.02
 C40-C38 \\sim C40A-C38
 with sigma of 0.02
 C42-C41 \\sim C41A-C42A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C42) = Uanis(C42A)
Uanis(C40A) = Uanis(C40)
4. Rigid body (RIGU) restrains
 C42, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41A, C42A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H38(0.75) H38A(0.25) C40(0.75) H40A(0.75) H40B(0.75) H40C(0.75)
 C40A(0.25) H40D(0.25) H40E(0.25) H40F(0.25) C41(0.5) H41A(0.5) H41B(0.5)
 C41A(0.5) H41C(0.5) H41D(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C42A(0.5)
 H42D(0.5) H42E(0.5) H42F(0.5)
6.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23), C35(H35), C38(H38), C38(H38A)
6.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C41(H41A,H41B), C41A(H41C,H41D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C16(H16), C17(H17), C18(H18),
 C31(H31), C32(H32), C33(H33)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C40A(H40D,H40E,H40F), C42(H42A,H42B,H42C),
 C42A(H42D,H42E,H42F), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              76020
_shelx_hkl_checksum              41330
_olex2_submission_special_instructions 'No special instructions were received'