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_4104715
_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            'Hg2.39 Na5 Sn9.61'
_chemical_formula_weight         1734.97
_chemical_name_common            'Sodium Mercury Stannide'
_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                   12.9583(8)
_cell_length_b                   10.9835(7)
_cell_length_c                   12.9596(7)
_cell_measurement_temperature    293(2)
_cell_volume                     1844.51(19)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.9 (release 17-07-2007 CrysAlis171 .NET)
(compiled Aug 17 2007,17:36:27)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.9 (release 17-07-2007 CrysAlis171 .NET)
(compiled Aug 17 2007,17:36:27)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.9 (release 17-07-2007 CrysAlis171 .NET)
(compiled Aug 17 2007,17:36:27)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.5467
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur CCD'
_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  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13440
_diffrn_reflns_theta_full        27.81
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    32.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.9 (release 17-07-2007 CrysAlis171 .NET)
(compiled Aug 17 2007,17:36:27)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Silvery
_exptl_crystal_density_diffrn    6.248
_exptl_crystal_description       Block
_exptl_crystal_F_000             2907
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.700
_refine_diff_density_min         -1.729
_refine_diff_density_rms         0.400
_refine_ls_extinction_coef       0.00109(5)
_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   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         2185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0329
_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 w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                1616
_reflns_number_total             2185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902664c_si_002.cif
_cod_data_source_block           Na5Hg2+xSn10-x
_cod_original_formula_sum        'Na5 Hg2.39 Sn9.61'
_cod_database_code               4104715