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_2020119
_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          '2C25 H22 P +, 2Cl -, Cl12 Si6'
_chemical_formula_moiety         '2(C25 H22 P +), 2(Cl -), Cl12 Si6'
_chemical_formula_sum            'C50 H44 Cl14 P2 Si6'
_chemical_formula_weight         1371.64
_chemical_name_systematic
;
Bis(benzyltriphenylphosphonium) 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                61.618(10)
_cell_angle_beta                 72.804(11)
_cell_angle_gamma                71.605(11)
_cell_formula_units_Z            1
_cell_length_a                   11.0097(17)
_cell_length_b                   12.7082(18)
_cell_length_c                   13.0269(18)
_cell_measurement_reflns_used    10444
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      3.25
_cell_volume                     1498.3(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 0.993
_diffrn_measured_fraction_theta_max 0.982
_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  0.0708
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12339
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.180
_diffrn_reflns_theta_min         3.292
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.351
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5906
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0711
_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^)+(0.0697P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1650
_reflns_number_gt                3338
_reflns_number_total             5906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3599sup1.cif
_cod_data_source_block           IV
_cod_database_code               2020119
_cod_database_fobs_code          2020119
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.920
_shelx_hkl_checksum              81054
_shelx_res_checksum              65128
_shelxl_version_number           2014/6