Role of Anions and Reaction Conditions in the Preparation of Uranium(VI), Neptunium(VI), and Plutonium(VI) Borates
Shuao Wang; Eric M. Villa; Juan Diwu; Evgeny V. Alekseev; Wulf Depmeier; Thomas E. Albrecht-Schmitt; Inorganic Chemistry 50 (2011) 2527–2533; doi:10.1021/ic102356d

data_4324669
_publ_section_title
;
 Role of Anions and Reaction Conditions in the Preparation of Uranium(VI),
 Neptunium(VI), and Plutonium(VI) Borates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2527
_journal_page_last               2533
_journal_paper_doi               10.1021/ic102356d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'PuO2[B8 O11 (OH)4]'
_chemical_formula_sum            'B8 O17 Pu'
_chemical_formula_weight         600.48
_chemical_name_common            'Plutonyl(VI) borate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.7440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4391(8)
_cell_length_b                   16.714(2)
_cell_length_c                   10.9648(13)
_cell_measurement_reflns_used    2750
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      2.44
_cell_volume                     1180.0(2)
_computing_cell_refinement       'smart saint'
_computing_data_collection       smart
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_source         'Imus microfocused'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6456
_diffrn_reflns_theta_full        28.63
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    5.697
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELTXPREP
_exptl_crystal_colour            peach/pink
_exptl_crystal_density_diffrn    3.380
_exptl_crystal_description       Tablet
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.294
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.00016(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         2750
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0205
_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^)+(0.0000P)^2^+9.6865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0473
_reflns_number_gt                2724
_reflns_number_total             2750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102356d_si_002_3.cif
_cod_data_source_block           Pu6BO
_cod_original_cell_volume        1180.0(3)
_cod_database_code               4324669