The first thiosilicate from solution: synthesis and crystal structure of (NH4)2[SiS3(NH3)]·2NH3
Meier, Martin; Korber, Nikolaus; Dalton Transactions  (2009) 1506–1508; doi:10.1039/b818856d

data_7000612
_publ_section_title
;
 The first thiosilicate from solution: synthesis and crystal structure
 of (NH4)2[SiS3(NH3)]&#x00B7;2NH3
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1506
_journal_page_last               1508
_journal_paper_doi               10.1039/b818856d
_journal_year                    2009
_chemical_formula_moiety         '2 (H4 N +) , (H3 N S3 Si 2-) , 2 (H3 N)'
_chemical_formula_sum            'H17 N5 S3 Si'
_chemical_formula_weight         211.46
_chemical_name_common
'Diammonium hydrogenamidotrithiosilicate-ammonia(2)'
_chemical_name_systematic
;
Diammonium hydrogenamidotrithiosilicate-ammonia(2)
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2008-11-12 # Formatted by publCIF
;
_cell_angle_alpha                97.32(3)
_cell_angle_beta                 91.37(3)
_cell_angle_gamma                94.13(3)
_cell_formula_units_Z            2
_cell_length_a                   6.3474(13)
_cell_length_b                   6.5730(13)
_cell_length_c                   13.055(3)
_cell_measurement_reflns_used    7378
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      3.13
_cell_volume                     538.5(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2004)'
_computing_data_collection       'IPDS (Stoe & Cie, 1998)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2005)'
_computing_molecular_graphics    'DIAMOND 2.1e (Crystal Impact, 2001)'
_computing_publication_material  'CIFTAB in SHELXL97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       Phi
_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  0.1341
_diffrn_reflns_av_sigmaI/netI    0.3194
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7378
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  0.8549
_exptl_absorpt_correction_T_min  0.7370
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.251
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1870
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.822
_refine_ls_R_factor_all          0.1684
_refine_ls_R_factor_gt           0.0998
_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^)+(0.0915P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2386
_refine_ls_wR_factor_ref         0.2556
_reflns_number_gt                691
_reflns_number_total             1870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b818856d.txt
_cod_data_source_block           abs
_cod_original_cell_volume        538.55(19)
_cod_database_code               7000612