Identification of the Formal +2 Oxidation State of Plutonium: Synthesis and Characterization of {Pu(II)[C5H3(SiMe3)2]3}().
Windorff, Cory J.; Chen, Guo P.; Cross, Justin N.; Evans, William J.; Furche, Filipp; Gaunt, Andrew J.; Janicke, Michael T.; Kozimor, Stosh A.; Scott, Brian L.; Journal of the American Chemical Society 139 (2017) 3970–3973; doi:10.1021/jacs.7b00706

data_4125882
_publ_section_title
;
 Identification of the Formal +2 Oxidation State of Plutonium: Synthesis
 and Characterization of {Pu(II)[C5H3(SiMe3)2]3}().
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3970
_journal_page_last               3973
_journal_paper_doi               10.1021/jacs.7b00706
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C51 H99 K N2 O6 Pu Si6'
_chemical_formula_weight         1282.96
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                100.8106(7)
_cell_angle_beta                 104.3697(6)
_cell_angle_gamma                95.5916(7)
_cell_formula_units_Z            2
_cell_length_a                   12.2131(8)
_cell_length_b                   12.7370(8)
_cell_length_c                   22.2524(14)
_cell_measurement_reflns_used    38381
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.606
_cell_measurement_theta_min      1.647
_cell_volume                     3255.8(4)
_computing_cell_refinement       'smart saint'
_computing_data_collection       smart
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-2014 (Sheldrick, 2014)'
_computing_publication_material  'SHELXCIF-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '0.5 wide w/exposures'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38381
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.606
_diffrn_reflns_theta_min         1.647
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.228
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       cube
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   'not measured'
_exptl_transmission_factor_min   N/A
_refine_diff_density_max         2.143
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         15297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+0.7719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13926
_reflns_number_total             15297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00706_si_003.cif
_cod_data_source_block           apx2349
_cod_database_code               4125882
_shelx_shelxl_version_number     2014/7
_shelxl_version_number           2014-3
_shelx_res_checksum              91372
_shelx_hkl_checksum              91974