Neptunium Thiophosphate Chemistry: Intermediate Behavior between Uranium and Plutonium
Geng Bang Jin; S. Skanthakumar; Richard G. Haire; L. Soderholm; James A. Ibers; Inorganic Chemistry 50 (2011) 9688–9695; doi:10.1021/ic201493w

data_4326412
_publ_contact_author_address
;
       Chemical Sciences and Engineering Division
       Argonne National Laboratory
       Argonne, IL 60439, USA

       Department of Chemistry
       Northwestern University
       2145 Sheridan Road
       Evanston, IL 60208-3113, 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
;
 Neptunium Thiophosphate Chemistry: Intermediate Behavior between Uranium
 and Plutonium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9688
_journal_page_last               9695
_journal_paper_doi               10.1021/ic201493w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'K11 Np7 P13 S52'
_chemical_formula_sum            'K11 Np7 P13 S52'
_chemical_formula_weight         4158.83
_chemical_name_common
'Undecapotassium Heptaneptunium Tridecakis(tetrathioPhosphate)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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            8
_cell_length_a                   31.937(3)
_cell_length_b                   31.937(3)
_cell_length_c                   17.2691(15)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.85
_cell_volume                     17614(3)
_computing_cell_refinement       'APEX2 v2.0-2 (Bruker, 2005)'
_computing_data_collection       'APEX2 v2.1-4 (Bruker, 2007)'
_computing_data_reduction        'SAINT version 7.23a (Bruker, 2005)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            112684
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    10.194
_exptl_absorpt_correction_T_max  0.51024
_exptl_absorpt_correction_T_min  0.34255
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'faces indexed'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.137
_exptl_crystal_description       prism
_exptl_crystal_F_000             15096
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.084
_refine_diff_density_max         3.575
_refine_diff_density_min         -1.350
_refine_diff_density_rms         0.248
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.528
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         10221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.528
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0376
_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 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0120P)^2^+0.0000sin\q/\l] 
 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                9955
_reflns_number_total             10221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201493w_si_001_4.cif
_cod_data_source_block           compound(3)
_cod_database_code               4326412