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_7041772
_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         'C20 H26 Cl2 Si3'
_chemical_formula_sum            'C20 H26 Cl2 Si3'
_chemical_formula_weight         421.58
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-03
_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                 90.416(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3643(4)
_cell_length_b                   11.5112(3)
_cell_length_c                   11.4420(3)
_cell_measurement_reflns_used    21088
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.0440
_cell_measurement_theta_min      2.3350
_cell_volume                     2287.01(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.9484
_diffrn_measurement_details
;
  1 omega  -38.00   76.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.0781   57.0000  -60.0000 114

  2 omega   -3.00  111.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706   57.0000  -30.0000 114

  3 omega  -46.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706  -38.0000  -30.0000 117

  4 omega  -46.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706  -38.0000   90.0000 117

  5 omega  -39.00   -7.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706  133.0000  125.0746 32

  6 omega   -3.00  111.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706   57.0000  -90.0000 114

  7 omega   -8.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706   77.0000    0.0000 128

  8 omega   -8.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706   77.0000   60.0000 128

  9 omega  -20.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706  -99.0000   90.0000 110

 10 omega   -3.00  111.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706   57.0000 -150.0000 114

 11 omega   -3.00  111.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706   57.0000  150.0000 114

 12 omega -105.00   -2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -35.4269  125.0000  -60.0000 103

 13 omega  -73.00   41.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -35.4269   57.0000  -60.0000 114

 14 omega  -94.00  -35.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.0781 -178.0000   30.0000 59

 15 omega  -56.00  126.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706    0.0000 -150.0000 182

 16 omega    2.00  105.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706 -125.0000   60.0000 103

 17 omega  -56.00  126.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706    0.0000 -180.0000 182

 18 omega  -32.00    1.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706  122.0000 -157.9822 33

 19 omega  -56.00  126.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706    0.0000 -120.0000 182

 20 omega  -56.00  126.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706    0.0000  -90.0000 182

 21 omega  -56.00  126.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706    0.0000  -60.0000 182

 22 omega  -56.00  126.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706    0.0000  -30.0000 182

 23 omega  -56.00  126.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706    0.0000    0.0000 182

 24 omega  -73.00   41.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -35.4269   57.0000 -120.0000 114

 25 omega  -38.00   76.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.0781   57.0000 -150.0000 114

 26 omega  -56.00   60.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706    0.0000   60.0000 116

 27 omega  -56.00  126.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       35.2706    0.0000   30.0000 182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0299965000
_diffrn_orient_matrix_UB_12      0.0376300000
_diffrn_orient_matrix_UB_13      0.0188070000
_diffrn_orient_matrix_UB_21      0.0246025000
_diffrn_orient_matrix_UB_22      -0.0485155000
_diffrn_orient_matrix_UB_23      0.0082545000
_diffrn_orient_matrix_UB_31      0.0127969000
_diffrn_orient_matrix_UB_32      0.0052611000
_diffrn_orient_matrix_UB_33      -0.0584822000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            44651
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.388
_diffrn_reflns_theta_min         2.123
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.224
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.4331
_exptl_crystal_size_mid          0.1662
_exptl_crystal_size_min          0.1244
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0411P)^2^+2.1850P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2003
_reflns_number_total             2333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04608h2.cif
_cod_data_source_block           horst28
_cod_depositor_comments
'Adding full bibliography for 7041769--7041777.cif.'
_cod_original_cell_volume        2287.02(10)
_cod_database_code               7041772
_chemical_oxdiff_formula         'C20 H33 Si3 Cl2'
_diffrn_oxdiff_twin_integration_method simultaneous
_shelx_res_checksum              1662
_shelxl_version_number           2013-2