Synthesis, Characterization, and Crystal Structures of Silylium Compounds of the Weakly Coordinating Dianion [B12Cl12]2-
Mathias Kessler; Carsten Knapp; Vanessa Sagawe; Harald Scherer; Rabiya Uzun; Inorganic Chemistry 49 (2010) 5223–5230; doi:10.1021/ic100337k

data_4315648
_publ_section_title
;
 Synthesis, Characterization, and Crystal Structures of Silylium Compounds
 of the Weakly Coordinating Dianion [B12Cl12]2-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5223
_journal_page_last               5230
_journal_paper_doi               10.1021/ic100337k
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C18 H42 O2 S Si2, C9 H21 B12 Cl12 Si'
_chemical_formula_sum            'C27 H63 B12 Cl12 O2 S Si3'
_chemical_formula_weight         1091.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 92.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.814(3)
_cell_length_b                   11.993(2)
_cell_length_c                   15.922(3)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.01
_cell_volume                     2635.6(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS Spider'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       RX
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33585
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
March 2001 T Higashi
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1126
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         8245
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0843P)^2^+0.9108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1609
_reflns_number_gt                6178
_reflns_number_total             8245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100337k_si_002_5.cif
_cod_data_source_block           ck013-3-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2635.5(9)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4315648