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_7041776
_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 H12 Si'
_chemical_formula_sum            'C16 H12 Si'
_chemical_formula_weight         232.35
_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     iterative
_audit_creation_date             2014-05-05
_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                 101.1855(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.06686(12)
_cell_length_b                   7.54672(9)
_cell_length_c                   19.5187(2)
_cell_measurement_reflns_used    43071
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      32.5710
_cell_measurement_theta_min      2.8060
_cell_volume                     1310.20(3)
_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    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9766
_diffrn_measurement_details
;
  1 omega  -74.00  -27.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  130.0000  142.9169 47

  2 omega  -90.00  -38.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000 -143.5500 52

  3 omega  -71.00  -23.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  125.0000   14.0144 48

  4 omega  -51.00   43.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  -57.0000    0.0000 94

  5 omega  -51.00   43.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  -57.0000 -150.0000 94

  6 omega   35.00  101.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  178.0000   30.0000 66

  7 omega   -8.00   86.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922   57.0000  150.0000 94

  8 omega  -54.00   48.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  -77.0000  120.0000 102

  9 omega   -8.00   86.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922   57.0000  -90.0000 94

 10 omega  -13.00   89.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922   77.0000    0.0000 102

 11 omega  -71.00  -23.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  125.0000  -23.7215 48

 12 omega  -90.00  -38.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000   85.0506 52

 13 omega  -90.00  -38.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  153.0000  -75.8600 52

 14 omega  -75.00  -27.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  131.0000  175.8677 48

 15 omega  -94.00   17.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672  -19.0000  -60.0000 111

 16 omega   35.00  101.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  178.0000   90.0000 66

 17 omega   -8.00   86.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922   57.0000 -180.0000 94

 18 omega   -3.00   89.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922   37.0000   60.0000 92

 19 omega  -37.00   54.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672   37.0000  150.0000 91

 20 omega  -47.00   55.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7672   77.0000   60.0000 102

 21 omega  -68.00  103.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -180.0000 171

 22 omega  -68.00   51.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922    0.0000 -150.0000 119

 23 omega  -20.00   56.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       17.3922  -99.0000 -150.0000 76
;
_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      -0.0612491000
_diffrn_orient_matrix_UB_12      0.0128070000
_diffrn_orient_matrix_UB_13      0.0172186000
_diffrn_orient_matrix_UB_21      0.0286178000
_diffrn_orient_matrix_UB_22      -0.0674458000
_diffrn_orient_matrix_UB_23      0.0242758000
_diffrn_orient_matrix_UB_31      0.0422850000
_diffrn_orient_matrix_UB_32      0.0641863000
_diffrn_orient_matrix_UB_33      0.0220610000
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0094
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            73396
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.020
_diffrn_reflns_theta_min         4.182
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87179
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    1.178
_exptl_crystal_description       irregular
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.3211
_exptl_crystal_size_mid          0.2217
_exptl_crystal_size_min          0.1451
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0393P)^2^+0.6159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3646
_reflns_number_total             3827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04608h2.cif
_cod_data_source_block           horst21
_cod_depositor_comments
'Adding full bibliography for 7041769--7041777.cif.'
_cod_original_cell_volume        1310.19(3)
_cod_database_code               7041776
_chemical_oxdiff_formula         'C20 H20 Si2'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelx_res_checksum              18339
_shelxl_version_number           2014-3