Synthesis and Characterization of Na5M2+xSn10-x (x~ 0.5, M = Zn, Hg) - A Doped Tetrahedral Framework Structure
Siméon Ponou; Sung-Jin Kim; Thomas F. Fässler; Journal of the American Chemical Society 131 (2009) 10246–10252; doi:10.1021/ja902664c

data_4104716
_publ_contact_author             'Thomas F. Faessler'
_publ_contact_author_email       thomas.faessler@lrz.tum.de
_publ_contact_author_fax         '++49-89 28913186'
_publ_contact_author_phone       '++49-89 28913131'
_publ_section_title
;
 Synthesis and Characterization of Na5M2+xSn10-x (x~ 0.5, M = Zn, Hg) - A
 Doped Tetrahedral Framework Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10246
_journal_page_last               10252
_journal_paper_doi               10.1021/ja902664c
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'Na5 Sn9.72 Zn2.28'
_chemical_formula_weight         1417.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   12.7717(7)
_cell_length_b                   10.8042(7)
_cell_length_c                   12.7774(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1763.13(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24268
_diffrn_reflns_theta_full        27.81
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    16.636
_exptl_crystal_density_diffrn    5.341
_exptl_crystal_F_000             2438
_refine_diff_density_max         1.630
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.293
_refine_ls_extinction_coef       0.00058(3)
_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   1.219
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         2083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0353
_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 w=1/[\s^2^(Fo^2^)+(0.0051P)^2^+56.7008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                1593
_reflns_number_total             2083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902664c_si_003.cif
_cod_data_source_block           Na5Zn2+xSn10-x
_cod_database_code               4104716