Mixed-Valent Neptunium(IV/V) Compound with Cation-Cation-Bound Six-Membered Neptunyl Rings
Geng Bang Jin; Inorganic Chemistry 52 (2013) 12317–12319; doi:10.1021/ic4021492

data_4336651
_publ_contact_author_address
;
       Chemical Sciences and Engineering Division
       Argonne National Laboratory
       Argonne, IL 60439, USA
;
_publ_contact_author_email       gjin@anl.gov
_publ_contact_author_fax         '+1 630 252 4225'
_publ_contact_author_name        'Geng Bang Jin'
_publ_contact_author_phone       '+1 630 252 3658'
_publ_section_title
;
 Mixed-Valent Neptunium(IV/V) Compound with Cation-Cation-Bound
 Six-Membered Neptunyl Rings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12317
_journal_page_last               12319
_journal_paper_doi               10.1021/ic4021492
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'Na0.8(1) Np (Np O2)6 (O H)1.8(1) Cl9 (H2 O)7.2'
_chemical_formula_sum            'Cl9 H16.2 Na0.8 Np7 O21'
_chemical_formula_weight         2348.77
_chemical_name_common
'Sodium neptunium(IV) neptunyl(V) hydroxide chrolide hydrate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.9879(4)
_cell_length_b                   10.9879(4)
_cell_length_c                   14.3934(6)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.57
_cell_volume                     1504.95(10)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CrystalMaker for Windows ver. 2.0.6 (2008)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '0.3 wide w/ exposures'
_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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0081
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21429
_diffrn_reflns_theta_full        30.43
_diffrn_reflns_theta_max         30.43
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    24.823
_exptl_absorpt_correction_T_max  0.327
_exptl_absorpt_correction_T_min  0.232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    5.183
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1994
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.045
_refine_diff_density_max         17.950
_refine_diff_density_min         -3.084
_refine_diff_density_rms         0.654
_refine_ls_extinction_coef       0.00048(12)
_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   1.063
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         1544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+123.7396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                1440
_reflns_number_total             1544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4021492_si_001.cif
_cod_data_source_block           p63m
_cod_original_formula_sum        'Cl9 H16.20 Na0.80 Np7 O21'
_cod_database_code               4336651