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_7041769
_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 F6 Si3'
_chemical_formula_sum            'C16 H14 F6 Si3'
_chemical_formula_weight         404.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-24
_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                 98.414(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.69282(16)
_cell_length_b                   12.4642(2)
_cell_length_c                   22.3387(4)
_cell_measurement_reflns_used    11668
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.7870
_cell_measurement_theta_min      3.9470
_cell_volume                     1843.45(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -103.00  -47.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000 -164.0000   35.0000 56

  2 omega  -46.00   32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   90.0000 78

  3 omega  -56.00   27.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000  -30.0000 83

  4 omega   15.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   90.0000 80

  5 omega   90.00  124.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  150.0000 34

  6 omega   81.00  106.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000   90.0000 25

  7 omega   60.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -30.0000 48

  8 omega   26.00   76.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000   90.0000 50

  9 omega   90.00  115.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   30.0000 25

 10 omega   55.00  124.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988 -178.0000  -60.0000 69

 11 omega   13.00   56.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -30.0000 43

 12 omega   13.00   45.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -180.0000 32

 13 omega   13.00   62.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   30.0000 49

 14 omega   13.00   67.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -120.0000 54

 15 omega   24.00  100.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -90.0000 76

 16 omega   23.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000 -150.0000 85

 17 omega   81.00  151.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 70

 18 omega   35.00  108.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 73

 19 omega   84.00  156.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   64.0000  -50.6529 72

 20 omega   82.00  154.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 72

 21 omega   85.00  112.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 27

 22 omega   85.00  120.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 35

 23 omega  129.00  156.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   55.0000 -100.4956 27

 24 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 26

 25 omega   32.00   92.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 60

 26 omega   41.00   92.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 51

 27 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 97

 28 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 97

 29 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   59.0000   37.2582 26

 30 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 26

 31 omega   81.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 26

 32 omega  113.00  156.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 43

 33 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 26

 34 omega   85.00  125.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 40

 35 omega   81.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 97

 36 omega   86.00  115.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   55.0000 -100.4956 29

 37 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 26

 38 omega   82.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 25

 39 omega   32.00   67.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -90.0000 35

 40 omega   85.00  110.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 25

 41 omega   81.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 26

 42 omega  147.00  173.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 26

 43 omega   34.00  108.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  120.0000 74

 44 omega   32.00   86.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 54

 45 omega   86.00  113.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 27

 46 omega   81.00  107.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 26

 47 omega   41.00  122.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 81

 48 omega   89.00  156.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  -60.0000 67

 49 omega  120.00  147.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -150.0000 27

 50 omega   89.00  115.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000 -150.0000 26

 51 omega   84.00  110.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   66.0000 -121.8190 26

 52 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   59.0000    4.6718 26

 53 omega   83.00  150.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   67.0000   43.6366 67

 54 omega   89.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   52.0000   77.3205 88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0969290000
_diffrn_orient_matrix_UB_12      0.0839769000
_diffrn_orient_matrix_UB_13      0.0459820000
_diffrn_orient_matrix_UB_21      -0.0805930000
_diffrn_orient_matrix_UB_22      -0.0613358000
_diffrn_orient_matrix_UB_23      0.0513453000
_diffrn_orient_matrix_UB_31      0.1955008000
_diffrn_orient_matrix_UB_32      -0.0668364000
_diffrn_orient_matrix_UB_33      0.0106033000
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28241
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.123
_diffrn_reflns_theta_min         4.001
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.896
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    1.458
_exptl_crystal_description       needle
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.2053
_exptl_crystal_size_mid          0.0697
_exptl_crystal_size_min          0.0311
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3633
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0533P)^2^+1.1727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3184
_reflns_number_total             3633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04608h2.cif
_cod_data_source_block           horst20
_cod_depositor_comments
'Adding full bibliography for 7041769--7041777.cif.'
_cod_original_cell_volume        1843.44(7)
_cod_database_code               7041769
_chemical_oxdiff_formula         'C16 H14 F6 Si3'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_date_sample_data_collection 2014-04-29
_olex2_date_sample_submission    1395615600
_olex2_exptl_crystal_mounting_method mounted
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              10751
_shelx_shelxl_version_number     2014/7