Directed Synthesis of Crystalline Plutonium(III) and (IV) Oxalates: Accessing Redox-Controlled Separations in Acidic Solutions
Wolfgang Runde; Lia F. Brodnax; George Goff; Amanda C. Bean; Brian L. Scott; Inorganic Chemistry 48 (2009) 5967–5972; doi:10.1021/ic900344u

data_4302493
_publ_section_title
;
Directed Synthesis of Crystalline Plutonium(III) and (IV) Oxalates:
Accessing Redox-Controlled Separations in Acidic Solutions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5967
_journal_page_last               5972
_journal_paper_doi               10.1021/ic900344u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C3 K0 O10.5 Pu'
_chemical_formula_weight         446.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.477(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.246(3)
_cell_length_b                   9.610(3)
_cell_length_c                   10.315(3)
_cell_measurement_temperature    141(2)
_cell_volume                     1014.6(5)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.10 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker SMART 1k CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6228
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.535
_exptl_absorpt_correction_T_max  0.7359
_exptl_absorpt_correction_T_min  0.4212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    2.920
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.751
_refine_diff_density_min         -2.503
_refine_diff_density_rms         0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.308
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1710
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.306
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                1560
_reflns_number_total             1710
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900344u_si_001_1.cif
_cod_data_source_block           ccd687a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C3 K0 O10.50 Pu'
_cod_database_code               4302493