Cation-Cation Interactions in Neptunyl(V) Compounds: Hydrothermal Preparation and Structural Characterization of NpO2(IO3) and α- and β-AgNpO2(SeO3)
Thomas E. Albrecht-Schmitt; Philip M. Almond; Richard E. Sykora; Inorganic Chemistry 42 (2003) 3788–3795; doi:10.1021/ic034124z

data_4313775
_publ_contact_author
;
Prof. Thomas E. Albrecht-Schmitt 
179 Chemistry Building
Department of Chemistry
Auburn University, AL
36849
;
_publ_contact_author_email       ' albreth@auburn.edu '
_publ_contact_author_fax         ' 334 844 6959 '
_publ_contact_author_phone       ' 334 844 6948 '
_publ_section_title
;
 Cation-Cation Interactions in Neptunyl(V) Compounds: Hydrothermal
 Preparation and Structural Characterization of NpO2(IO3) and \a- and
 \b-AgNpO2(SeO3)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3788
_journal_page_last               3795
_journal_paper_doi               10.1021/ic034124z
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         NpO2(IO3)
_chemical_formula_sum            'I Np O5'
_chemical_formula_weight         443.90
_chemical_name_common            'neptunyl(V) iodate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   13.8163(19)
_cell_length_b                   5.8949(8)
_cell_length_c                   5.5852(8)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.95
_cell_volume                     454.89(11)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX'
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4363
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.95
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         na
_exptl_absorpt_coefficient_mu    29.539
_exptl_absorpt_correction_T_max  '0.700598 ratio of min/max'
_exptl_absorpt_correction_T_min  '0.700508 ratio of min/max'
_exptl_absorpt_correction_type   'analytical and multiscan(SADABS)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    6.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.016
_refine_diff_density_max         1.991
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.253
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       0.00000(10)
_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   1.000
_refine_ls_hydrogen_treatment    na
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1125
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          2.025
_refine_ls_shift/su_mean         0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0447
_reflns_number_gt                932
_reflns_number_total             1125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034124zsi20030417_113632_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'nm' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4313775