Quaternary Neptunium Compounds: Syntheses and Characterization of KCuNpS3, RbCuNpS3, CsCuNpS3, KAgNpS3, and CsAgNpS3
Daniel M. Wells; Geng Bang Jin; S. Skanthakumar; Richard G. Haire; L. Soderholm; James A. Ibers; Inorganic Chemistry 48 (2009) 11513–11517; doi:10.1021/ic901229d

data_4303825
_publ_contact_author_address
;
Department of Chemistry
Northwestern University
Evanston, IL 60208-3113
;
_publ_contact_author_email       ibers@chem.northwestern.edu
_publ_contact_author_fax         '1 847 491 3976'
_publ_contact_author_name        'James A. Ibers'
_publ_contact_author_phone       '1 847 491 5449'
_publ_section_title
;
Quaternary Neptunium Compounds: Syntheses and Characterization of KCuNpS3,
RbCuNpS3, CsCuNpS3, KAgNpS3, and CsAgNpS3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11513
_journal_page_last               11517
_journal_paper_doi               10.1021/ic901229d
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'K Ag Np S3'
_chemical_formula_sum            'Ag K Np S3'
_chemical_formula_weight         480.15
_chemical_name_common            'potassium silver neptunium trisulfide'
_chemical_name_systematic        'neptunium potassium silver trisulfide'
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2009-04-05 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.0575(17)
_cell_length_b                   13.989(6)
_cell_length_c                   10.422(4)
_cell_measurement_reflns_used    237
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.34
_cell_measurement_theta_min      3.91
_cell_volume                     591.6(4)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2006)'
_computing_molecular_graphics    'CrystalMaker for Windows v2.0.6 (2008)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            835
_diffrn_reflns_theta_full        33.89
_diffrn_reflns_theta_max         33.89
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    22.386
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7776
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'numerical (TWINABS; Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.391
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.043
_refine_diff_density_max         2.004
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.418
_refine_ls_extinction_coef       0.00029(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   1.032
_refine_ls_matrix_type           full
_refine_ls_number_parameters     26
_refine_ls_number_reflns         896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0292
_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
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+(0.0229Fo^2^)^2^]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0537
_reflns_number_gt                717
_reflns_number_total             896
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901229d_si_001_5.cif
_cod_data_source_block           KAg
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4303825