Non-aqueous neptunium and plutonium redox behaviour in THF - access to a rare Np(iii) synthetic precursor.
Pattenaude, Scott A.; Anderson, Nickolas H.; Bart, Suzanne C.; Gaunt, Andrew J.; Scott, Brian L.; Chemical communications (Cambridge, England) 54 (2018) 6113–6116; doi:10.1039/c8cc02611d

data_7121609
_publ_section_title
;
 Non-aqueous neptunium and plutonium redox behaviour in THF - access to a
 rare Np(iii) synthetic precursor.
;
_journal_issue                   48
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6113
_journal_page_last               6116
_journal_paper_doi               10.1039/c8cc02611d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C12 H24 Cl3.5 O3 Pu'
_chemical_formula_weight         579.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-03-27 deposited with the CCDC.
2018-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.374(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.264(3)
_cell_length_b                   11.172(3)
_cell_length_c                   13.938(4)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.50
_cell_volume                     1849.9(9)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20230
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.615
_diffrn_reflns_theta_min         1.714
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.070
_exptl_absorpt_correction_T_max  0.253
_exptl_absorpt_correction_T_min  0.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_description       block
_exptl_crystal_F_000             1094
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.270
_refine_diff_density_max         1.571
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.742
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.742
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0073P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4006
_reflns_number_total             4435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02611d2.cif
_cod_data_source_block           apx2586
_cod_depositor_comments
'Adding full bibliography for 7121609--7121611.cif.'
_cod_original_cell_volume        1850.0(8)
_cod_original_formula_sum        'C12 H24 Cl3.50 O3 Pu'
_cod_database_code               7121609
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.338
_shelx_estimated_absorpt_t_max   0.406
_shelx_res_checksum              88645