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_2020118
_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          '2C16 H36 N +, 2Cl -, Cl12 Si6, 2C6 H6'
_chemical_formula_moiety         '2(C16 H36 N +), 2(Cl -), Cl12 Si6, 2(C6 H6)'
_chemical_formula_sum            'C44 H84 Cl14 N2 Si6'
_chemical_formula_weight         1305.97
_chemical_name_systematic
;
Bis(tetrabutylammonium) dichloride dodecachlorohexasilane benzene disolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4687(4)
_cell_length_b                   18.5439(5)
_cell_length_c                   22.8784(7)
_cell_measurement_reflns_used    57758
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.7
_cell_measurement_theta_min      1.8
_cell_volume                     6562.7(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.0769
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            80026
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.209
_diffrn_reflns_theta_min         1.932
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.652
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+6.5182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                5439
_reflns_number_total             6554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3599sup1.cif
_cod_data_source_block           III
_cod_database_code               2020118
_cod_database_fobs_code          2020118
_shelx_estimated_absorpt_t_min   0.868
_shelx_estimated_absorpt_t_max   0.899
_shelx_hkl_checksum              7485
_shelx_res_checksum              61461
_shelxl_version_number           2014/6