Morpholine-Derived Hydrophilic 1,10-phenanthroline-2,9-dicarboxamide for Americium–Lanthanide Separation in Phosphine Oxide Extraction Systems
Evsiunina, Mariia V.; Domnikov, Kirill S.; Matveev, Petr I.; Kalle, Paulina; Matazova, Ekaterina; Gerasimov, Mikhail A.; Lemport, Pavel S.; Sonin, Igor; Petrov, Vladimir G.; Kostikova, Galina V.; Ustynyuk, Yuri; Nenajdenko, Valentine; Dalton Transactions  (2025) –; doi:10.1039/D5DT02131F

data_7719890
_publ_section_title
;
 Morpholine-Derived Hydrophilic 1,10-phenanthroline-2,9-dicarboxamide for
 Americium--Lanthanide Separation in Phosphine Oxide Extraction Systems
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT02131F
_journal_year                    2025
_chemical_formula_moiety         'C26 H40 Er N7 O10, 2(H2 O), 4(N O3)'
_chemical_formula_sum            'C26 H44 Er N11 O24'
_chemical_formula_weight         1061.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-11
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-08-18 deposited with the CCDC.	2025-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.742(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.3427(15)
_cell_length_b                   7.2948(4)
_cell_length_c                   36.3733(17)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.524
_cell_measurement_theta_min      2.600
_cell_volume                     7782.1(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0558
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            30311
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.562
_diffrn_reflns_theta_min         2.241
_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    2.264
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1406 before and 0.0544 after correction.
The Ratio of minimum to maximum transmission is 0.8230.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_description       needle
_exptl_crystal_F_000             4296
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.485
_refine_diff_density_min         -1.471
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         7262
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0114P)^2^+86.6431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6364
_reflns_number_total             7262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02131f2.cif
_cod_data_source_block           kd9
_cod_database_code               7719890
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.472
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Er1-H5A \\sim Er1-H5B
 with sigma of 0.02
 Er1-H4A \\sim Er1-H4B
 with sigma of 0.02
3.a Riding coordinates:
 O11(H11A,H11B)
3.b Free rotating group:
 O4(H4A,H4B), O5(H5A,H5B), O9(H9A,H9B)
3.c Rotating group:
 O3(H3A,H3B)
3.d Ternary CH refined with riding coordinates:
 N5(H5), N6(H6)
3.e Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
3.f Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C3(H3C), C4(H4C), C9(H9), C10(H10), C13(H13), C14(H14)
;
_shelx_res_checksum              53106
_olex2_submission_special_instructions 'No special instructions were received'