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_7041775
_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 H18 F6 Si3'
_chemical_formula_sum            'C16 H18 F6 Si3'
_chemical_formula_weight         408.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-12-08
_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                 109.1776(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.58517(10)
_cell_length_b                   15.67457(13)
_cell_length_c                   13.23279(17)
_cell_measurement_reflns_used    38458
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.9650
_cell_measurement_theta_min      4.4910
_cell_volume                     1877.81(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 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      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 0.9214
_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   -110.00 -18.00   1.00    3.00    --  -38.50 -38.00-150.00   92
  2  \w    -64.00  30.00   1.00    3.00    --  -38.50  57.00 -30.00   94
  3  \w    -59.00  33.00   1.00    3.00    --  -38.50  38.00 -90.00   92
  4  \w   -116.00  -5.00   1.00    3.00    --  -38.50 -19.00-120.00  111
  5  \w     18.00 112.00   1.00    3.00    --   43.20  57.00  90.00   94
  6  \w      1.00  82.00   1.00    3.00    --   43.20 -99.00  30.00   81
  7  \w     13.00 115.00   1.00    3.00    --   43.20  77.00  90.00  102
  8  \w     57.00 127.00   1.00    3.00    --   43.20 178.00-120.00   70
  9  \w     13.00 115.00   1.00    3.00    --   43.20  77.00   0.00  102
 10  \w     13.00 115.00   1.00    3.00    --   43.20  77.00-180.00  102
 11  \w      9.00  35.00   1.00    3.00    --   43.20  86.00 -54.88   26
 12  \w     18.00 112.00   1.00    3.00    --   43.20  57.00 -30.00   94
 13  \w     13.00 115.00   1.00    3.00    --   43.20  77.00 -90.00  102
 14  \w     81.00 178.00   1.00    6.00    --  111.00  77.00  30.00   97
 15  \w     85.00 178.00   1.00    6.00    --  111.00  61.00  30.00   93
 16  \w     81.00 178.00   1.00    6.00    --  111.00  77.00  60.00   97
 17  \w     31.00 109.00   1.00    6.00    --  111.00 -94.00 -90.00   78
 18  \w     81.00 178.00   1.00    6.00    --  111.00  77.00-180.00   97
 19  \w     31.00 109.00   1.00    6.00    --  111.00 -94.00-180.00   78
 20  \w     82.00 178.00   1.00    6.00    --  111.00  74.00 -18.91   96
 21  \w     85.00 178.00   1.00    6.00    --  111.00  61.00-150.00   93
 22  \w     85.00 178.00   1.00    6.00    --  111.00  61.00  90.00   93
 23  \w     85.00 178.00   1.00    6.00    --  111.00  61.00-120.00   93
 24  \w     85.00 178.00   1.00    6.00    --  111.00  61.00 150.00   93
 25  \w     85.00 178.00   1.00    6.00    --  111.00  61.00 -30.00   93
 26  \w     85.00 178.00   1.00    6.00    --  111.00  61.00-180.00   93
 27  \w     85.00 178.00   1.00    6.00    --  111.00  61.00 -90.00   93
 28  \w     85.00 178.00   1.00    6.00    --  111.00  61.00 120.00   93
 29  \w     81.00 178.00   1.00    6.00    --  111.00  77.00 150.00   97
 30  \w     31.00 109.00   1.00    6.00    --  111.00 -94.00 -30.00   78
 31  \w     81.00 178.00   1.00    6.00    --  111.00  77.00  90.00   97
 32  \w     81.00 178.00   1.00    6.00    --  111.00  77.00-150.00   97
 33  \w     81.00 178.00   1.00    6.00    --  111.00  77.00-121.54   97
 34  \w     81.00 178.00   1.00    6.00    --  111.00  77.00   0.00   97
 35  \w     81.00 178.00   1.00    6.00    --  111.00  77.00 -90.00   97
 36  \w     81.00 178.00   1.00    6.00    --  111.00  77.00 -30.00   97
 37  \w     85.00 178.00   1.00    6.00    --  111.00  61.00 -60.00   93
 38  \w     81.00 178.00   1.00    6.00    --  111.00  77.00 -60.00   97
 39  \w     81.00 178.00   1.00    6.00    --  111.00  77.00 120.00   97
 40  \w     85.00 178.00   1.00    6.00    --  111.00  61.00  60.00   93
 41  \w     40.00 141.00   1.00    6.00    --  111.00 -77.00   0.00  101
 42  \w     83.00 178.00   1.00    6.00    --  111.00  69.00   0.32   95
 43  \w     41.00 122.00   1.00    6.00    --  111.00-125.00-180.00   81
 44  \w   -110.00 -18.00   1.00    3.00    --  -38.50 -38.00  60.00   92
 45  \w     23.00 114.00   1.00    3.00    --   43.20  38.00 120.00   91
 46  \w     13.00 106.00   1.00    3.00    --   43.20  77.00-150.00   93
 47  \w     23.00 114.00   1.00    3.00    --   43.20  38.00-120.00   91
 48  \w     18.00 112.00   1.00    3.00    --   43.20  57.00 -60.00   94
 49  \w     18.00 112.00   1.00    3.00    --   43.20  57.00 150.00   94
 50  \w    -28.00  64.00   1.00    3.00    --   43.20 -38.00  60.00   92
 51  \w     18.00 112.00   1.00    3.00    --   43.20  57.00 -90.00   94
;
_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      0.1294613000
_diffrn_orient_matrix_UB_12      -0.0122469000
_diffrn_orient_matrix_UB_13      0.1049588000
_diffrn_orient_matrix_UB_21      0.0535633000
_diffrn_orient_matrix_UB_22      0.0912928000
_diffrn_orient_matrix_UB_23      -0.0099014000
_diffrn_orient_matrix_UB_31      -0.0965348000
_diffrn_orient_matrix_UB_32      0.0342754000
_diffrn_orient_matrix_UB_33      0.0638868000
_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  0.0189
_diffrn_reflns_av_unetI/netI     0.0064
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53527
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.991
_diffrn_reflns_theta_min         4.525
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.843
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 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    1.445
_exptl_crystal_description       fragment
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0314P)^2^+1.5148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3621
_reflns_number_total             3697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04608h2.cif
_cod_data_source_block           horst42
_cod_depositor_comments
'Adding full bibliography for 7041769--7041777.cif.'
_cod_database_code               7041775
_chemical_oxdiff_formula         'C16 H18 F6 Si3'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_date_sample_data_collection 2015-12-07
_olex2_submission_special_instructions 'No special instructions were received'
_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 1.302
_oxdiff_exptl_absorpt_empirical_full_min 0.771
_shelx_res_checksum              82512
_shelxl_version_number           2014-3