Identification of the Formal +2 Oxidation State of Neptunium: Synthesis and Structural Characterization of {Np<sup>II</sup>[C<sub>5</sub>H<sub>3</sub>(SiMe<sub>3</sub>)<sub>2</sub>]<sub>3</sub>}<sup>1</sup>.
Su, Jing; Windorff, Cory J.; Batista, Enrique R.; Evans, William J.; Gaunt, Andrew J.; Janicke, Michael T.; Kozimor, Stosh A.; Scott, Brian L.; Woen, David H.; Yang, Ping; Journal of the American Chemical Society 140 (2018) 7425–7428; doi:10.1021/jacs.8b03907

data_4132429
_publ_section_title
;
 Identification of the Formal +2 Oxidation State of Neptunium: Synthesis
 and Structural Characterization of
 {Np<sup>II</sup>[C<sub>5</sub>H<sub>3</sub>(SiMe<sub>3</sub>)<sub>2</sub>]<sub>3</sub>}<sup>1</sup>.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7425
_journal_page_last               7428
_journal_paper_doi               10.1021/jacs.8b03907
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C51 H99 K N2 Np O6 Si6'
_chemical_formula_weight         1280.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                100.8858(13)
_cell_angle_beta                 104.3945(14)
_cell_angle_gamma                95.5327(14)
_cell_formula_units_Z            2
_cell_length_a                   12.1932(9)
_cell_length_b                   12.7204(9)
_cell_length_c                   22.2152(16)
_cell_measurement_reflns_used    9564
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      32.71
_cell_measurement_theta_min      2.37
_cell_volume                     3240.0(4)
_computing_cell_refinement       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_collection       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT, v. 8.34A (Bruker AXS, 2013)'
_computing_molecular_graphics    'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_publication_material  'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Quest with CMOS detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Bruker Triumph curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39454
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         2.213
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.821
_exptl_absorpt_correction_T_max  0.306
_exptl_absorpt_correction_T_min  0.217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2014/3 (Bruker AXS, 2013)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             1326
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.724
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.259
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         12247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0220P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11081
_reflns_number_total             12247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b03907_si_002.cif
_cod_data_source_block           dq0627
_cod_database_code               4132429
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.649
_shelx_estimated_absorpt_t_max   0.839
_shelx_res_checksum              35736
_shelx_hkl_checksum              12675