Selective Extraction of Light Lanthanides(III) by N,N-Di(2-ethylhexyl)-diglycolamic Acid: A Comparative Study with N,N-Dimethyl-diglycolamic Acid as a Chelator in Aqueous Solutions
Ibrahim, Sherif M.; Zhang, Yan; Xue, Yun; Yang, Suliang; Ma, Fuqiu; Gao, Yang; Zhou, Yu; Tian, Guoxin; ACS Omega  (2019) –; doi:10.1021/acsomega.9b03241

data_4517156
_publ_section_title
;
 Selective Extraction of Light Lanthanides(III) by
 N,N-Di(2-ethylhexyl)-diglycolamic Acid: A Comparative Study with
 N,N-Dimethyl-diglycolamic Acid as a Chelator in Aqueous Solutions
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.9b03241
_journal_year                    2019
_chemical_formula_moiety         'C18 H30 N3 Nd O12'
_chemical_formula_sum            'C18 H30 N3 Nd O12'
_chemical_formula_weight         624.69
_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             2019-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                79.596(4)
_cell_angle_beta                 80.582(4)
_cell_angle_gamma                88.007(4)
_cell_formula_units_Z            2
_cell_length_a                   9.5238(4)
_cell_length_b                   12.2283(6)
_cell_length_c                   13.4495(6)
_cell_measurement_reflns_used    6834
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.6000
_cell_measurement_theta_min      4.1680
_cell_volume                     1519.79(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -45.00 -10.00   1.00    2.00    --  -11.20 -37.00-150.00   35
  2  \w    -19.00  30.00   1.00    2.00    --  -11.20 -99.00 -60.00   49
  3  \w    -12.00  86.00   1.00    2.00    --   12.45  37.00-120.00   98
  4  \w    -56.00  15.00   1.00    2.00    --   12.45 -37.00 -60.00   71
  5  \w    -52.00  41.00   1.00    2.00    --   12.45 -57.00  60.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0594610000
_diffrn_orient_matrix_UB_12      -0.0168335000
_diffrn_orient_matrix_UB_13      0.0383346000
_diffrn_orient_matrix_UB_21      0.0168835000
_diffrn_orient_matrix_UB_22      0.0405044000
_diffrn_orient_matrix_UB_23      0.0278024000
_diffrn_orient_matrix_UB_31      -0.0433459000
_diffrn_orient_matrix_UB_32      0.0394218000
_diffrn_orient_matrix_UB_33      -0.0266113000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13903
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.633
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         7173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0129P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6290
_reflns_number_total             7173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03241_si_003.cif
_cod_data_source_block           20190315b
_cod_database_code               4517156
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1Nd1
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.720
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C8(H8A,H8B), C9(H9A,H9B), C14(H14A,H14B), C15(H15A,
 H15B)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              20630
_shelx_hkl_checksum              3313
_shelx_fab_checksum              91664
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.856