A structural study of Si~6~-ring-containing [Si~6~Cl~14~]^2{-^} chlorosilicates
Tillmann, Jan; Lerner, Hans-Wolfram; Bolte, Michael; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615016484

data_2020117
_publ_section_title
;
 A structural study of Si~6~-ring-containing [Si~6~Cl~14~]^2{-^}
 chlorosilicates
;
_journal_coeditor_code           SK3599
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615016484
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C16 H36 N +, C13 H30 N +, 2Cl -, Cl12 Si6'
_chemical_formula_moiety         'C16 H36 N +, C13 H30 N +, 2(Cl -), Cl12 Si6'
_chemical_formula_sum            'C29 H66 Cl14 N2 Si6'
_chemical_formula_weight         1107.67
_chemical_name_systematic
;
Tetrabutylammonium tributylmethylammonium dichloride dodecachlorohexasilane
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                89.672(6)
_cell_angle_beta                 88.689(6)
_cell_angle_gamma                89.854(6)
_cell_formula_units_Z            2
_cell_length_a                   11.1071(9)
_cell_length_b                   14.3992(12)
_cell_length_c                   16.7434(12)
_cell_measurement_reflns_used    23095
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      3.1
_cell_volume                     2677.1(4)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2001)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2001)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2001)
;
_computing_molecular_graphics
;
XP in SHELXTL-Plus (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015), PLATON (Spek, 2009)
and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32914
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.712
_diffrn_reflns_theta_min         3.322
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.370
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         10052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                6918
_reflns_number_total             10052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3599sup1.cif
_cod_data_source_block           II
_cod_database_code               2020117
_cod_database_fobs_code          2020117
_shelx_estimated_absorpt_t_min   0.879
_shelx_estimated_absorpt_t_max   0.966
_shelx_hkl_checksum              7451
_shelx_res_checksum              8570
_shelxl_version_number           2014/6