Characterization of a Mixed Salt of 1-Hydroxypyridin-2-one Pu(IV) Complexes1
Anne E. V. Gorden; Jide Xu; Géza Szigethy; Allen Oliver; David K. Shuh; Kenneth N. Raymond; Journal of the American Chemical Society 129 (2007) 6674–6675; doi:10.1021/ja070168l

data_4109451
_publ_section_title
;
 Characterization of a Mixed Salt of 1-Hydroxypyridin-2-one Pu(IV)
 Complexes1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6674
_journal_page_last               6675
_journal_paper_doi               10.1021/ja070168l
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         '[Pu(C5H4NO2)4][Pu(C5H4NO2)3(H2O)2.CClO4]'
_chemical_formula_sum            'C35 H32 Cl N7 O20 Pu2'
_chemical_formula_weight         1390.13
_chemical_name_common            'Plutonium(IV) 1,2-HOPO complex'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 91.779(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8065(14)
_cell_length_b                   20.935(3)
_cell_length_c                   11.1771(18)
_cell_measurement_reflns_used    6674
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.000
_cell_measurement_theta_min      2.738
_cell_volume                     2059.7(6)
_computing_cell_refinement       'Saint v.7.23'
_computing_data_collection       'Bruker APEX-II V.2.0.2'
_computing_data_reduction        'Saint v.7.23'
_computing_molecular_graphics    'ORTEP-3 v.1.08, POV-Ray v3.6.1c.icl8.win32'
_computing_publication_material  'ORTEP-3 v.1.08, POV-Ray v3.6.1c.icl8.win32'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      446(2)
_diffrn_detector_area_resol_mean 36.23
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Platinum 200'
_diffrn_measurement_method       \w/2\q-scans
_diffrn_radiation_monochromator  'chanel-ut Si-<111> crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14186
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         29.00
_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    3.372
_exptl_absorpt_correction_T_max  0.2834
_exptl_absorpt_correction_T_min  0.2834
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.241
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.784
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.481(16)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         7089
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0474P)^2^+0.7967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                6966
_reflns_number_total             7089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070168lsi20070413_011504.cif
_cod_data_source_block           pu12hopc
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4109451