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_4334262
_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
'C64 H76 Eu N17 O3, 2(N O3), 4(C2 H6 O), 2(O)'
_chemical_formula_sum            'C72 H104 Eu N19 O15'
_chemical_formula_weight         1627.70
_chemical_name_systematic        '[Eu(CyMe4-BTBP)2(NO3)](NO3)2.4EtOH.2H2O'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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            4
_cell_length_a                   16.4128(6)
_cell_length_b                   23.8916(6)
_cell_length_c                   19.7838(6)
_cell_measurement_reflns_used    15897
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.9736
_cell_measurement_theta_min      2.9416
_cell_volume                     7757.8(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_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 -117.00  -32.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6964  179.0000  150.0000 85

  2 omega   67.00  107.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0245   37.0000   30.0000 40

  3 omega  -68.00  -34.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0245 -179.0000  -60.0000 34

  4 omega   20.00   48.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0245   37.0000   30.0000 28

  5 omega  -18.00   94.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0245   37.0000   90.0000 112

  6 omega  -74.00   53.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0245  -77.0000  150.0000 127
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0375237000
_diffrn_orient_matrix_UB_12      0.0071692000
_diffrn_orient_matrix_UB_13      0.0155536000
_diffrn_orient_matrix_UB_21      0.0131238000
_diffrn_orient_matrix_UB_22      -0.0127902000
_diffrn_orient_matrix_UB_23      0.0304616000
_diffrn_orient_matrix_UB_31      0.0169526000
_diffrn_orient_matrix_UB_32      0.0258121000
_diffrn_orient_matrix_UB_33      0.0107564000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47979
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'Enhance (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.034
_refine_diff_density_min         -4.181
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.333
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         6854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.333
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.1158
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+230.2072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2577
_refine_ls_wR_factor_ref         0.2628
_reflns_number_gt                5726
_reflns_number_total             6854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301599y_si_002_08.cif
_cod_data_source_block           complex8
_cod_database_code               4334262
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97