Crystal and Electronic Structure of a Mixed-Valent Np(IV)-Np(V) Compound: [BuMeIm]5[Np(NpO2)3(H2O)6Cl12]
Iraida Charushnikova; Emilie Bossé; Dominique Guillaumont; Philippe Moisy; Inorganic Chemistry 49 (2010) 2077–2082; doi:10.1021/ic901526e

data_4314945
_publ_section_title
;
 Crystal and Electronic Structure of a Mixed-Valent Np(IV)-Np(V) Compound:
 [BuMeIm]5[Np(NpO2)3(H2O)6Cl12]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2077
_journal_page_last               2082
_journal_paper_doi               10.1021/ic901526e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'Cl12 H12 Np4 O12, 5(C8 H15 N2)'
_chemical_formula_sum            'C40 H87 Cl12 N10 Np4 O12'
_chemical_formula_weight         2273.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.8718(12)
_cell_angle_beta                 70.2530(14)
_cell_angle_gamma                62.2690(12)
_cell_formula_units_Z            2
_cell_length_a                   14.5485(3)
_cell_length_b                   14.8947(3)
_cell_length_c                   20.7821(6)
_cell_measurement_reflns_used    55089
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3723.14(16)
_computing_cell_refinement       'HKL package (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL package (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f-  \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43779
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    6.018
_exptl_absorpt_correction_T_max  0.537
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.028
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2138
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.718
_refine_diff_density_min         -2.031
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         14601
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0907P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                9801
_reflns_number_total             14601
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic901526e_si_002.cif
_cod_data_source_block           pm2
_cod_original_cell_volume        3723.14(15)
_cod_database_code               4314945