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_4334256
_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
'C68 H76 N17 O3 Pr, N5 O15 Pr, 1.63(C2 H6 O), 0.75(H2O)'
_chemical_formula_sum            'C71.25 H87.25 N22 O20.38 Pr2'
_chemical_formula_weight         1859.70
_chemical_name_systematic
'[Pr(CyMe4-BTPhen)2(NO3)][Pr(NO3)5].1.63EtOH.0.75H2O'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-04-30
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                107.225(5)
_cell_angle_beta                 99.422(5)
_cell_angle_gamma                97.083(5)
_cell_formula_units_Z            2
_cell_length_a                   13.716(5)
_cell_length_b                   15.221(5)
_cell_length_c                   20.359(5)
_cell_measurement_reflns_used    3434
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.910
_cell_measurement_theta_min      2.154
_cell_volume                     3938(2)
_computing_cell_refinement       'SMART v5.625 (Bruker, 2001)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_av_unetI/netI     0.2615
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25422
_diffrn_reflns_theta_full        25.47
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         1.53
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40.0
_diffrn_source_power             1.6
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.326834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0819 before and 0.0408 after correction.
The Ratio of minimum to maximum transmission is 0.3268.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       plate
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.381
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.677
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1093
_refine_ls_number_reflns         14178
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      0.681
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                6746
_reflns_number_total             14178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301599y_si_002_02.cif
_cod_data_source_block           complex2
_cod_database_code               4334256