Synthesis, Structure, and Infrared Spectroscopy of the First Np5+ Neptunyl Silicates, Li6(NpO2)4(H2Si2O7)(HSiO4)2(H2O)4 and K3(NpO2)3(Si2O7)
T. Z. Forbes; P. C. Burns; Inorganic Chemistry 47 (2008) 705–712; doi:10.1021/ic701335j

data_4304043
_publ_contact_author_address
;University of Notre Dame
Dept. of Civil Engineering and Geosciences
156 Fitzpatrick Hall
Notre Dame, IN 46556
;
_publ_contact_author_email       pburns@nd.edu
_publ_contact_author_name        'Peter Burns'
_publ_contact_author_phone       574-631-7216
_publ_section_title
;
Synthesis, Structure, and Infrared Spectroscopy of the First Np5+ Neptunyl
Silicates, Li6(NpO2)4(H2Si2O7)(HSiO4)2(H2O)4 and K3(NpO2)3(Si2O7)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              705
_journal_page_last               712
_journal_paper_doi               10.1021/ic701335j
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'Np4 O23 Si4, 4(O), 4(Li)'
_chemical_formula_sum            'Li4 Np4 O27 Si4'
_chemical_formula_weight         1520.27
_chemical_name_common            'Lithium neptunyl silicate tetrahydrate'
_chemical_name_systematic        'Lithium neptunyl silicate tetrahydrate'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   none
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.189(6)
_cell_length_b                   7.917(3)
_cell_length_c                   10.708(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1118.1(8)
_computing_cell_refinement       'APEX II Software'
_computing_data_collection       'APEX II Software'
_computing_data_reduction        'APEX II Software'
_computing_molecular_graphics    'CrystalMaker v 1.3.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker XRD w/ APEX II CCD Detector'
_diffrn_measurement_method       /w
_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  0.1238
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10516
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    18.769
_exptl_absorpt_correction_T_max  0.391
_exptl_absorpt_correction_T_min  0.057
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'modeled as an 001 plate using XPREP'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.659
_refine_diff_density_min         -2.164
_refine_diff_density_rms         0.438
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0668P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                725
_reflns_number_total             1065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701335j-file004.cif
_cod_data_source_block           pcd
_cod_database_code               4304043