Fluoride complexation by bidentate silicon Lewis acids.
Horstmann, Jan; Niemann, Mark; Berthold, Katarína; Mix, Andreas; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1898–1913; doi:10.1039/c6dt04608h

data_7041771
_publ_section_title
;
 Fluoride complexation by bidentate silicon Lewis acids.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1898
_journal_page_last               1913
_journal_paper_doi               10.1039/c6dt04608h
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C16 H14 Cl6 Si3'
_chemical_formula_sum            'C16 H14 Cl6 Si3'
_chemical_formula_weight         503.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-25
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2016-12-01 deposited with the CCDC.
2017-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.810(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2081(9)
_cell_length_b                   11.5831(8)
_cell_length_c                   11.3044(7)
_cell_measurement_reflns_used    5023
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      66.4180
_cell_measurement_theta_min      4.5980
_cell_volume                     2253.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9932
_diffrn_measured_fraction_theta_max 0.9944
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -115.00  -8.00   1.00   20.00    --  -38.50 -19.00 -30.00  107
  2  \w    -53.00  33.00   1.00   20.00    --  -38.50  38.00 150.00   86
  3  \w     69.00 119.00   1.00   20.00    --   43.20 178.00 -90.00   50
  4  \w     71.00 124.00   1.00   20.00    --   43.20 178.00 120.00   53
  5  \w    -22.00  52.00   1.00   20.00    --   43.20 -57.00-120.00   74
  6  \w     96.00 146.00   1.00   74.00    --  111.00 125.00 -90.00   50
  7  \w     46.00  98.00   1.00   74.00    --  111.00 -61.00-150.00   52
  8  \w     98.00 178.00   1.00   74.00    --  111.00  30.00  90.00   80
  9  \w    131.00 159.00   1.00   74.00    --  111.00  77.00  30.00   28
 10  \w     82.00 123.00   1.00   74.00    --  111.00  77.00  30.00   41
 11  \w     40.00 133.00   1.00   74.00    --  111.00 -77.00 -60.00   93
 12  \w     53.00 108.00   1.00   74.00    --  111.00-125.00 120.00   55
 13  \w    122.00 167.00   1.00   74.00    --  111.00  61.00 -30.00   45
 14  \w     37.00  82.00   1.00   74.00    --  111.00 -94.00-150.00   45
 15  \w     43.00 117.00   1.00   74.00    --  111.00-125.00 -30.00   74
 16  \w     86.00 117.00   1.00   74.00    --  111.00  61.00 -30.00   31
 17  \w    113.00 176.00   1.00   74.00    --  111.00 125.00-120.00   63
 18  \w     87.00 178.00   1.00   74.00    --  111.00  61.00   0.00   91
 19  \w     69.00 116.00   1.00   74.00    --  111.00-125.00  60.00   47
 20  \w     45.00 122.00   1.00   74.00    --  111.00-125.00-150.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0209701000
_diffrn_orient_matrix_UB_12      -0.1286040000
_diffrn_orient_matrix_UB_13      -0.0147302000
_diffrn_orient_matrix_UB_21      0.0329033000
_diffrn_orient_matrix_UB_22      -0.0252150000
_diffrn_orient_matrix_UB_23      0.1248089000
_diffrn_orient_matrix_UB_31      -0.0805500000
_diffrn_orient_matrix_UB_32      0.0234031000
_diffrn_orient_matrix_UB_33      0.0525404000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7654
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.972
_diffrn_reflns_theta_min         4.602
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.486
_exptl_absorpt_correction_T_max  0.664
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.30a (Agilent, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1016.0
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0551P)^2^+14.1992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1865
_reflns_number_total             2008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04608h2.cif
_cod_data_source_block           horst39
_cod_depositor_comments
'Adding full bibliography for 7041769--7041777.cif.'
_cod_database_code               7041771
_chemical_oxdiff_formula         'C16 H14 Cl6 Si4'
_chemical_oxdiff_usercomment     ' '
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.794
_oxdiff_exptl_absorpt_empirical_full_min 0.587
_shelx_res_checksum              48448
_shelxl_version_number           2014-3