Homogeneous liquid-liquid extraction of neodymium(iii) by choline hexafluoroacetylacetonate in the ionic liquid choline bis(trifluoromethylsulfonyl)imide.
Onghena, Bieke; Jacobs, Jeroen; Van Meervelt, Luc; Binnemans, Koen; Dalton transactions (Cambridge, England : 2003) 43 (2014) 11566–11578; doi:10.1039/c4dt01340a

data_7031302
_publ_section_title
;
 Homogeneous liquid-liquid extraction of neodymium(iii) by choline
 hexafluoroacetylacetonate in the ionic liquid choline
 bis(trifluoromethylsulfonyl)imide.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11566
_journal_page_last               11578
_journal_paper_doi               10.1039/c4dt01340a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C25 H17 F24 N Nd O9, 0.39(O)'
_chemical_formula_sum            'C25 H17 F24 N Nd O9.4'
_chemical_formula_weight         1081.96
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.0479(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.03826(19)
_cell_length_b                   18.5663(5)
_cell_length_c                   17.8663(3)
_cell_measurement_reflns_used    9754
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.0540
_cell_measurement_theta_min      3.1690
_cell_volume                     3659.17(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0607538000
_diffrn_orient_matrix_UB_12      0.0101722000
_diffrn_orient_matrix_UB_13      -0.0062640000
_diffrn_orient_matrix_UB_21      0.0050111000
_diffrn_orient_matrix_UB_22      -0.0286403000
_diffrn_orient_matrix_UB_23      -0.0259689000
_diffrn_orient_matrix_UB_31      -0.0204615000
_diffrn_orient_matrix_UB_32      0.0231244000
_diffrn_orient_matrix_UB_33      -0.0294190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26960
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.87
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.592
_exptl_absorpt_correction_T_max  1.226
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2101
_exptl_crystal_size_max          0.2698
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1627
_refine_diff_density_max         1.751
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         7466
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+19.8090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1290
_reflns_number_gt                6147
_reflns_number_total             7466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01340a1.cif
_cod_data_source_block           kbtest
_cod_depositor_comments          'Adding full bibliography for 7031302.cif.'
_cod_original_cell_volume        3659.18(13)
_cod_original_formula_sum        'C25 H17 F24 N Nd O9.40'
_cod_database_code               7031302
_chemical_oxdiff_formula         'C26 F24 N Nd O9 '
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 N41-C41 = N41-C42 = N41-C43
 1.5 with sigma of 0.001
 N51-C51 = N51-C52 = N51-C53
 1.5 with sigma of 0.001
 N41-C44 = N51-C54
 1.521 with sigma of 0.001
 C44-C45 = C54-C55
 1.505 with sigma of 0.001
 C45-O41 = C55-O51
 1.413 with sigma of 0.001
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C11, C12, C13, C14, C15, C21, C22, C23, C24, C25, C31,
 C32, C33, C34, C35, C41, C42, C43, C44, C45, C51, C52, C53, C54, C55, F1, F2,
 F3, F4, F5, F6, F11, F12, F13, F14, F15, F16, F21, F22, F23, F24, F25, F26,
 F31, F32, F33, F34, F35, F46
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
4. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq,
Uanis(F16) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F23)
\\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F25) \\sim Ueq, Uanis(F26) \\sim Ueq,
Uanis(F31) \\sim Ueq, Uanis(F32) \\sim Ueq, Uanis(F33) \\sim Ueq, Uanis(F34)
\\sim Ueq, Uanis(F35) \\sim Ueq, Uanis(F46) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
5. Others
 Sof(N51)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 Sof(H52C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(O51)=Sof(O52)=1-FVAR(1)
 Sof(N41)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(O41)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B), C54(H54A,H54B), C55(H55A,H55B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C23(H23), C33(H33)
6.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;