Reactivity of Chalcogenostannate Compounds: Syntheses, Crystal Structures, and Electronic Properties of Novel Compounds Containing Discrete Ternary Anions [MII4(μ4-Se)(SnSe4)4]10- (MII = Zn, Mn)
Stefanie Dehnen; Michael K. Brandmayer; Journal of the American Chemical Society 125 (2003) 6618–6619; doi:10.1021/ja029601b

data_4113785
_publ_contact_author_email       dehnen@achibm6.chemie.uni-karlsruhe.de
_publ_contact_author_fax         'Int + 721/608 7021'
_publ_contact_author_phone       'Int + 721/608 2850'
_publ_section_title
;
 Reactivity of Chalcogenostannate Compounds: Syntheses, Crystal
 Structures, and Electronic Properties of Novel Compounds Containing
 Discrete Ternary Anions [MII4(\m4-Se)(SnSe4)4]10- (MII = Zn, Mn)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6618
_journal_page_last               6619
_journal_paper_doi               10.1021/ja029601b
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C0.5 H34 K10 Mn4 O16.5 Se17 Sn4'
_chemical_formula_weight         2732.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_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            4
_cell_length_a                   15.515(2)
_cell_length_b                   15.515(2)
_cell_length_c                   25.440(5)
_cell_measurement_temperature    203(2)
_cell_volume                     6123.8(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.1264
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            52243
_diffrn_reflns_theta_full        22.58
_diffrn_reflns_theta_max         22.58
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    6.976
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.004
_exptl_crystal_description       'truncated octahedron'
_exptl_crystal_F_000             5030
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.8
_refine_diff_density_max         0.102
_refine_diff_density_min         -0.134
_refine_diff_density_rms         0.023
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         8108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          1.016
_refine_ls_shift/su_mean         0.033
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+0.0605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1617
_reflns_number_gt                6257
_reflns_number_total             8108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029601bsi20021205_074523_2.cif
_cod_data_source_block           K10Mn4Sn4Se17-compound_3
_cod_original_cell_volume        6123.5(17)
_cod_original_formula_sum        'C0.50 H34 K10 Mn4 O16.50 Se17 Sn4'
_cod_database_code               4113785