Synthesis and Characterization of Eight Compounds of the MU8Q17 Family: ScU8S17, CoU8S17, NiU8S17, TiU8Se17, VU8Se17, CrU8Se17, CoU8Se17, and NiU8Se17.
Ward, Matthew D.; Mesbah, Adel; Minasian, Stefan G.; Shuh, David K.; Tyliszczak, Tolek; Lee, Minseong; Choi, Eun Sang; Lebègue, Sébastien; Ibers, James A.; Inorganic chemistry 53 (2014) 6920–6927; doi:10.1021/ic500721d

data_4339959
_publ_section_title
;
 Synthesis and Characterization of Eight Compounds of the MU8Q17 Family:
 ScU8S17, CoU8S17, NiU8S17, TiU8Se17, VU8Se17, CrU8Se17, CoU8Se17, and
 NiU8Se17.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6920
_journal_page_last               6927
_journal_paper_doi               10.1021/ic500721d
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'Ni S17 U8'
_chemical_formula_sum            'Ni S17 U8'
_chemical_formula_weight         2507.97
_chemical_name_systematic
; 
Nickel(II) octauranium(IV) heptadecasulfide  
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-08-14 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.5376(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2685(6)
_cell_length_b                   8.3504(3)
_cell_length_c                   10.3797(5)
_cell_measurement_reflns_used    8971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.89
_cell_volume                     1126.80(9)
_computing_cell_refinement       'APEX2 (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'Crystalmaker (Palmer, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008c)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008c)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX2 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    0.0245
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17882
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    59.640
_exptl_absorpt_correction_T_max  0.432
_exptl_absorpt_correction_T_min  0.140
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008b)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    7.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.043
_refine_diff_density_max         3.360
_refine_diff_density_min         -3.603
_refine_diff_density_rms         0.559
_refine_ls_extinction_coef       0.00061(8)
_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   1.191
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0298
_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+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0568P)^2^+0.0000sin\q/\l] 
 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                1682
_reflns_number_total             1786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500721d_si_001.cif
_cod_data_source_block           NiU8S17
_cod_depositor_comments
'Adding full bibliography for 4339953--4339960.cif.'
_cod_original_cell_volume        1126.80(8)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4339959