Straightforward Reductive Routes to Air-Stable Uranium(III) and Neptunium(III) Materials.
Cross, Justin N.; Villa, Eric M.; Darling, Victoria R.; Polinski, Matthew J.; Lin, Jian; Tan, Xiaoyan; Kikugawa, Naoki; Shatruk, Michael; Baumbach, Ryan; Albrecht-Schmitt, Thomas E; Inorganic chemistry 53 (2014) 7455–7466; doi:10.1021/ic500771t

data_4340115
_publ_section_title
;
 Straightforward Reductive Routes to Air-Stable Uranium(III) and
 Neptunium(III) Materials.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7455
_journal_page_last               7466
_journal_paper_doi               10.1021/ic500771t
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         KNp(SO4)2(H2O)
_chemical_formula_sum            'K Np O9 S2'
_chemical_formula_weight         484.22
_chemical_melting_point          ?
_chemical_name_common            'Potassium Neptunium(III) sulfate hydrate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   7.1963(14)
_cell_length_b                   7.1963(14)
_cell_length_c                   13.386(4)
_cell_measurement_reflns_used    6753
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      3.27
_cell_volume                     600.3(2)
_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, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_source         'Imus microfocused'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6753
_diffrn_reflns_theta_full        27.19
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    14.045
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.7
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SHELTXPREP
_exptl_crystal_colour            purple-blue
_exptl_crystal_density_diffrn    4.018
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.30(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         895
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+4.9251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0793
_reflns_number_gt                624
_reflns_number_total             895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500771t_si_002.cif
_cod_data_source_block           save
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'N/A' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4340109--4340117.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_original_sg_symbol_H-M      P3(1)2(1)
_cod_database_code               4340115