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_4303822
_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 Cu Np S3'
_chemical_formula_sum            'Cu K Np S3'
_chemical_formula_weight         435.82
_chemical_name_common            'Potassium copper neptunium trisulfide'
_chemical_name_systematic        'Copper neptunium potassium 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
;
2009-06-23 # 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                   3.9616(8)
_cell_length_b                   13.862(3)
_cell_length_c                   10.234(2)
_cell_measurement_reflns_used    2710
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.53
_cell_measurement_theta_min      2.94
_cell_volume                     562.0(2)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5040
_diffrn_reflns_theta_full        33.88
_diffrn_reflns_theta_max         33.88
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    23.861
_exptl_absorpt_correction_T_max  0.9035
_exptl_absorpt_correction_T_min  0.2050
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed (SADABS; Sheldrick, 2006)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.006
_refine_diff_density_max         1.063
_refine_diff_density_min         -1.781
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       0.00209(15)
_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   1.020
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0157
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [1.00000]/
   [\s^2^(Fo^2^)+(0.0228Fo^2^)^2^]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0356
_refine_ls_wR_factor_ref         0.0368
_reflns_number_gt                589
_reflns_number_total             651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901229d_si_001_2.cif
_cod_data_source_block           KCu
_cod_original_cell_volume        562.01(19)
_cod_database_code               4303822