Unusual Syntheses, Structures, and Electronic Properties of Compounds Containing Ternary, T3-Type Supertetrahedral M/Sn/S Anions [M5Sn(μ3-S)4(SnS4)4]10- (M = Zn, Co)
Christian Zimmermann; Christopher E. Anson; Florian Weigend; Rodolphe Clérac; Stefanie Dehnen; Inorganic Chemistry 44 (2005) 5686–5695; doi:10.1021/ic050466o

data_4309332
_publ_contact_author
;
 Dr. Stefanie Dehnen
 Institut fuer Anorganische Chemie der Universitaet
  Engesserstrasse, Gebaeude 30.45
  D-76128 Karlsruhe
  Deutschland
;
_publ_contact_author_email       dehnen@chemie.uni-karlsruhe.de
_publ_contact_author_fax         'Int + 721/608 7021'
_publ_contact_author_phone       'Int + 721/608 2850'
_publ_section_title
;
Unusual Syntheses, Structures, and Electronic Properties of Compounds
Containing Ternary, T3-Type Supertetrahedral M/Sn/S Anions
[M5Sn(\m3-S)4(SnS4)4]10- (M = Zn, Co)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5686
_journal_page_last               5695
_journal_paper_doi               10.1021/ic050466o
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'H68 Na10 O34 S20 Sn5 Zn5'
_chemical_formula_weight         2403.94
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.402(1)
_cell_angle_beta                 100.211(1)
_cell_angle_gamma                103.956(1)
_cell_formula_units_Z            2
_cell_length_a                   14.8457(10)
_cell_length_b                   14.8772(9)
_cell_length_c                   17.5101(11)
_cell_measurement_reflns_used    9320
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.31
_cell_volume                     3633.6(4)
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2000)'
_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2000)'
_computing_data_reduction        'SAINT+ 6.0 (Bruker AXS Inc., 2000)'
_computing_molecular_graphics    'XP: SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_publication_material  'XCIF: SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_structure_refinement  'XL: SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_structure_solution    'XS: SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18078
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    4.007
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS Inc., 2000)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.358
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.238
_refine_ls_extinction_coef       0.00091(9)
_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   1.003
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         15329
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0551
_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 w=1/[\s^2^(Fo^2^)+(0.1062P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1593
_reflns_number_gt                11168
_reflns_number_total             15329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050466osi20050329_113249.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
;
 Removing the '_pupl_author_name' data item since it was not found in the
 core CIF dictionary and the same information was already provided in the
 official bibliography data items. No information was lost by removing this
 data item. Changing data name '_publ_author_adress' to '_publ_author_address'
 and moving the data item to the '_publ_author' loop.

 Antanas Vaitkus,
 2017-03-07
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_cod_database_code               4309332