Synthesis, crystal structure, and solid-state NMR spectroscopy of a salt-inclusion stannosilicate: [Na3F][SnSi3O9].
Liao, Chen-Hui; Chang, Pai-Ching; Kao, Hsien-Ming; Lii, Kwang-Hwa; Inorganic chemistry 44 (2005) 9335–9339; doi:10.1021/ic0514086

data_4340410
_publ_section_title
;
 Synthesis, crystal structure, and solid-state NMR spectroscopy of a
 salt-inclusion stannosilicate: [Na3F][SnSi3O9].
;
_journal_issue                   25
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9335
_journal_page_last               9339
_journal_paper_doi               10.1021/ic0514086
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[Na3F][SnSi3O9]'
_chemical_formula_sum            'F Na3 O9 Si3 Sn'
_chemical_formula_weight         434.93
_chemical_name_systematic
; 
 ? 
;
_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_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                 111.576(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5393(11)
_cell_length_b                   13.9532(15)
_cell_length_c                   6.5171(7)
_cell_measurement_temperature    273(2)
_cell_volume                     891.23(16)
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega 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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3331
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    3.470
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS program'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0161
_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^)+(0.0200P)^2^+0.8926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0422
_reflns_number_gt                1115
_reflns_number_total             1148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0514086si20050817_114831.cif
_cod_data_source_block           ap29m
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4340410