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_4334258
_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_absolute_configuration ad
_chemical_formula_moiety         'C68 H78 N16 O Tb, 3(N O3), 9(H2O)'
_chemical_formula_sum            'C68 H96 N19 O19 Tb'
_chemical_formula_weight         1642.56
_chemical_name_systematic        '[Tb(CyMe4-BTPhen)2(H2O)](NO3)3.9H2O'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-04-26
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.3486(7)
_cell_length_b                   38.0261(9)
_cell_length_c                   14.8414(3)
_cell_measurement_reflns_used    26649
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3116
_cell_measurement_theta_min      2.8693
_cell_volume                     17691.9(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics
;
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)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -60.00   51.00   1.0000   19.4400
omega____ theta____ kappa____ phi______ frames
    -      -21.0746   77.0000  -30.0000 111

  2 omega  -61.00   50.00   1.0000   19.4400
omega____ theta____ kappa____ phi______ frames
    -      -21.0746   77.0000   90.0000 111

  3 omega  -61.00   51.00   1.0000   19.4400
omega____ theta____ kappa____ phi______ frames
    -      -21.0746   77.0000 -150.0000 112

  4 omega  -10.00  102.00   1.0000   19.4400
omega____ theta____ kappa____ phi______ frames
    -       22.4808   77.0000  -30.0000 112

  5 omega   -6.00  105.00   1.0000   19.4400
omega____ theta____ kappa____ phi______ frames
    -       22.4808   77.0000   90.0000 111

  6 omega   -6.00  104.00   1.0000   19.4400
omega____ theta____ kappa____ phi______ frames
    -       22.4808   77.0000 -150.0000 110
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0468912000
_diffrn_orient_matrix_UB_12      0.0040400000
_diffrn_orient_matrix_UB_13      -0.0013565000
_diffrn_orient_matrix_UB_21      -0.0074370000
_diffrn_orient_matrix_UB_22      -0.0216210000
_diffrn_orient_matrix_UB_23      -0.0046760000
_diffrn_orient_matrix_UB_31      -0.0054628000
_diffrn_orient_matrix_UB_32      -0.0053175000
_diffrn_orient_matrix_UB_33      0.0180086000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49820
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'Enhance (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       plate
_exptl_crystal_F_000             6832
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.439
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         9044
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0986P)^2^+12.1124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1423
_reflns_number_gt                7867
_reflns_number_total             9044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301599y_si_002_04.cif
_cod_data_source_block           complex4
_cod_database_code               4334258
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32