Study on the extraction behavior of Nd(iii) in nitric acid medium by novel asymmetric alkyl diglycolamide extractants with different structures
Yin, Jingjing; Peng, Xiujing; Zhang, Miaomiao; Liu, Yifan; Wang, Haoran; Zheng, Jixi; Sun, Guoxin; Cui, Yu; New Journal of Chemistry 49 (2025) 2973–2979; doi:10.1039/D4NJ04748F

data_7063620
_publ_section_title
;
 Study on the extraction behavior of Nd(iii) in nitric acid medium by
 novel asymmetric alkyl diglycolamide extractants with different
 structures
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2973
_journal_page_last               2979
_journal_paper_doi               10.1039/D4NJ04748F
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C66 H120 N6 Nd1 O9, 3(N O3)'
_chemical_formula_sum            'C66 H120 N9 Nd O18'
_chemical_formula_weight         1471.94
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2025-01-07 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   20.0940(7)
_cell_length_b                   20.0940(7)
_cell_length_c                   36.2908(12)
_cell_measurement_reflns_used    5329
_cell_measurement_temperature    169.15
_cell_measurement_theta_max      20.81
_cell_measurement_theta_min      2.54
_cell_volume                     12690.0(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      169.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            16243
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.798
_diffrn_reflns_theta_max         66.798
_diffrn_reflns_theta_min         5.499
_exptl_absorpt_coefficient_mu    5.193
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5709
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1014 before and 0.0681 after correction.
The Ratio of minimum to maximum transmission is 0.7661.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       block
_exptl_crystal_F_000             4698
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2479
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2421
_refine_ls_wR_factor_ref         0.2923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1567
_reflns_number_total             2479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04748f2.cif
_cod_data_source_block           3
_cod_depositor_comments          'Adding full bibliography for 7063620.cif.'
_cod_original_cell_volume        12689.9(10)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7063620
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.455
_shelx_estimated_absorpt_t_min   0.395
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6B-C1B = C6A-C5A = C6A-C1A = C6B-C5B = C5A-C4B = C4A-C3B = C5B-C4A = C4B-C3A
 = C3A-C2A = C3B-C2B = C2A-C1A = C2B-C1B
 1.54 with sigma of 0.01
 C8A-C7A = C9A-C8A = C9B-C8B
 1.54 with sigma of 0.01
 N1-C1B = N1-C1A
 1.46 with sigma of 0.01
 N1-C7A
 1.46 with sigma of 0.01
 C8B-C7A = C8A-C7A
 1.54 with sigma of 0.01
 C9A-C7A \\sim C9B-C7A
 with sigma of 0.01
 C6A-C4B \\sim C5A-C3A \\sim C5A-C1A \\sim C6A-C2A \\sim C3A-C1A \\sim C4B-C2A
 with sigma of 0.01
 C5B-C1B \\sim C3B-C1B \\sim C5B-C3B \\sim C4A-C2B \\sim C6B-C4A \\sim C6B-C2B
 with sigma of 0.01
 N1-C8A \\sim N1-C8B
 with sigma of 0.01
3. Rigid bond restraints
 C8B, C9B, C7A, C8A, C9A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C1B, C2B, C3B, C4B, C5B, C6B, C1A, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C8B \\sim C9B \\sim C7A \\sim C8A \\sim C9A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C1A \\sim C2A \\sim
C3A \\sim C4A \\sim C5A \\sim C6A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
5. Others
 Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(H9BA)=Sof(H8BC)=Sof(H9BB)=Sof(H7AC)=
 Sof(H7AD)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=FVAR(1)
 Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=
 Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=Sof(H6BA)=
 Sof(H6BB)=1-FVAR(2)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=
 Sof(H6AB)=FVAR(2)
6.a Riding coordinates:
 C9B(H9BA,H8BC,H9BB), C9A(H9AA,H9AB,H9AC)
6.b Ternary CH refined with riding coordinates:
 C1B(H1B), C1A(H1A)
6.c Secondary CH2 refined with riding coordinates:
 C2B(H2BA,H2BB), C3B(H3BA,H3BB), C4B(H4BA,H4BB), C5B(H5BA,H5BB), C6B(H6BA,
 H6BB), C8B(H8BA,H8BB), C11(H11A,H11B), C7A(H7AC,H7AD), C7A(H7AA,H7AB),
 C8A(H8AA,H8AB), C2A(H2AA,H2AB), C3A(H3AA,H3AB), C4A(H4AA,H4AB), C5A(H5AA,H5AB),
  C6A(H6AA,H6AB)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32027
_shelx_fab_checksum              64774
_olex2_submission_special_instructions 'No special instructions were received'