Lanthanide Speciation in Potential SANEX and GANEX Actinide/Lanthanide Separations Using Tetra-N-Donor Extractants
Daniel M. Whittaker; Tamara L. Griffiths; Madeleine Helliwell; Adam N. Swinburne; Louise S. Natrajan; Frank W. Lewis; Laurence M. Harwood; Stephen A. Parry; Clint A. Sharrad; Inorganic Chemistry 52 (2013) 3429–3444; doi:10.1021/ic301599y

data_4334261
_publ_contact_author_address
;
Centre for Radiochemistry Research
School of Chemistry
University of Manchester
Oxford Road
Manchester
M13 9PL
;
_publ_contact_author_email       daniel.whittaker@postgrad.manchester.ac.uk
_publ_contact_author_name        'Daniel Whittaker'
_publ_contact_author_phone       +441612751405
_publ_section_title
;
 Lanthanide Speciation in Potential SANEX and GANEX Actinide/Lanthanide
 Separations Using Tetra-N-Donor Extractants
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3429
_journal_page_last               3444
_journal_paper_doi               10.1021/ic301599y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'2(C64 H74 N17 O3 Pr), N6 O18 Pr, 6(C2 H3 N), N O3'
_chemical_formula_sum            'C140 H166 N47 O27 Pr3'
_chemical_formula_weight         3361.93
_chemical_name_systematic        '[Pr(CyMe4-BTBP)2(NO3)]2[Pr(NO3)6](NO3).6CH3CN'
_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
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_cell_length_c                   17.7385(14)
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CrysAlisPro, Oxford Diffraction Ltd.,
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;
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
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;
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CrysAlisPro, Oxford Diffraction Ltd.,
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;
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;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.

L. J. Farrugia, ORTEP-3 for Windows - a version of ORTEP-III 
with a Graphical User Interface (GUI). J. Appl. Crystallogr. (1997). 30, 565.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
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_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details
;
  1 omega  -50.00   32.40   0.8000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0746   77.0000  -90.0000 103

  2 omega  -14.00   39.60   0.8000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4808   77.0000  120.0000 67

  3 omega    1.00  120.20   0.8000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4808   77.0000 -150.0000 149

  4 omega   -3.00   90.60   0.8000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4808   77.0000    0.0000 117
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0212965000
_diffrn_orient_matrix_UB_12      0.0062670000
_diffrn_orient_matrix_UB_13      -0.0279699000
_diffrn_orient_matrix_UB_21      -0.0391456000
_diffrn_orient_matrix_UB_22      0.0020280000
_diffrn_orient_matrix_UB_23      -0.0294058000
_diffrn_orient_matrix_UB_31      -0.0020930000
_diffrn_orient_matrix_UB_32      0.0243566000
_diffrn_orient_matrix_UB_33      0.0096420000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.2168
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17453
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'Enhance (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87506
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
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    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.358
_refine_diff_density_min         -1.652
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         17454
_refine_ls_number_restraints     1087
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1010P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.2209
_reflns_number_gt                9137
_reflns_number_total             17454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301599y_si_002_07.cif
_cod_data_source_block           complex7
_cod_original_cell_volume        7935.4(13)
_cod_database_code               4334261