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_4517157
_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 La N3 O12'
_chemical_formula_sum            'C18 H30 La N3 O12'
_chemical_formula_weight         619.36
_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             2019-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                79.729(6)
_cell_angle_beta                 80.339(5)
_cell_angle_gamma                87.876(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4804(5)
_cell_length_b                   12.3468(10)
_cell_length_c                   13.5959(10)
_cell_measurement_reflns_used    4593
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      27.1160
_cell_measurement_theta_min      4.0130
_cell_volume                     1543.68(19)
_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      150.01(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 0.825
_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    -61.00 -33.00   1.00    2.00    --  -11.36 115.00  98.00   28
  2  \w     -4.00  29.00   1.00    2.00    --  -11.36 -99.00 -30.00   33
  3  \w     18.00  50.00   1.00    2.00    --   12.61 -99.00   0.00   32
  4  \w     45.00 100.00   1.00    2.00    --   12.61 178.00-180.00   55
  5  \w     -4.00  87.00   1.00    2.00    --   12.61  37.00 -30.00   91
  6  \w    -67.00  37.00   1.00    2.00    --   12.61 -19.00 150.00  104
;
_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      0.0110466000
_diffrn_orient_matrix_UB_12      -0.0404927000
_diffrn_orient_matrix_UB_13      -0.0315986000
_diffrn_orient_matrix_UB_21      0.0220163000
_diffrn_orient_matrix_UB_22      0.0414840000
_diffrn_orient_matrix_UB_23      -0.0426148000
_diffrn_orient_matrix_UB_31      0.0717876000
_diffrn_orient_matrix_UB_32      -0.0069460000
_diffrn_orient_matrix_UB_33      0.0086160000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.825
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13654
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.778
_diffrn_reflns_theta_min         3.450
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66534
_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    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.408
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         7271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0152P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5930
_reflns_number_total             7271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03241_si_002.cif
_cod_data_source_block           20190403e
_cod_database_code               4517157
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1La1
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.762
_reflns_odcompleteness_completeness 99.73
_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              94191
_shelx_hkl_checksum              23827
_shelx_fab_checksum              63304
_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 1.386
_oxdiff_exptl_absorpt_empirical_full_min 0.623