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_7041774
_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_absolute_configuration unk
_chemical_formula_moiety         'C28 H38 F7 K O6 Si3'
_chemical_formula_sum            'C28 H38 F7 K O6 Si3'
_chemical_formula_weight         726.95
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-03
_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                 100.137(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6707(3)
_cell_length_b                   14.7072(3)
_cell_length_c                   12.2271(3)
_cell_measurement_reflns_used    12901
_cell_measurement_temperature    99.93(16)
_cell_measurement_theta_max      71.8370
_cell_measurement_theta_min      3.6470
_cell_volume                     1711.90(8)
_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      99.93(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9988
_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   -119.00 -48.00   1.00    7.97    --  -38.50-178.00-180.00   71
  2  \w    -41.00 -13.00   1.00    7.97    --  -38.50 -57.00 -30.00   28
  3  \w   -106.00 -73.00   1.00    7.97    --  -38.50 -57.00 -30.00   33
  4  \w   -103.00 -70.00   1.00    7.97    --  -38.50 -57.00  60.00   33
  5  \w    -54.00  29.00   1.00    7.97    --  -38.50  57.00  30.00   83
  6  \w    -41.00 -13.00   1.00    7.97    --  -38.50 -57.00  60.00   28
  7  \w   -109.00 -53.00   1.00    7.97    --  -38.50-156.00 -11.00   56
  8  \w    -52.00  28.00   1.00    7.97    --  -38.50  57.00-150.00   80
  9  \w     13.00  78.00   1.00    7.97    --   42.95  77.00-180.00   65
 10  \w     91.00 126.00   1.00    7.97    --   42.95 178.00-180.00   35
 11  \w     76.00 104.00   1.00    7.97    --   42.95  77.00 -90.00   28
 12  \w     44.00  97.00   1.00    7.97    --   42.95  38.00  90.00   53
 13  \w     23.00 110.00   1.00    7.97    --   42.95  38.00 150.00   87
 14  \w     13.00  79.00   1.00    7.97    --   42.95  77.00 -60.00   66
 15  \w     14.00  49.00   1.00    7.97    --   42.95  77.00 -90.00   35
 16  \w     14.00  67.00   1.00    7.97    --   42.95  77.00  90.00   53
 17  \w     25.00 112.00   1.00    7.97    --   42.95  77.00-150.00   87
 18  \w     14.00  75.00   1.00    7.97    --   42.95  77.00   0.00   61
 19  \w     81.00 176.00   1.00   31.88    --  111.00  77.00-150.00   95
 20  \w     81.00 165.00   1.00   31.88    --  111.00  77.00  30.00   84
 21  \w    149.00 177.00   1.00   31.88    --  111.00  63.00 -77.39   28
 22  \w     85.00 117.00   1.00   31.88    --  111.00  61.00 -90.00   32
 23  \w     81.00 178.00   1.00   31.88    --  111.00  77.00 -30.00   97
 24  \w     85.00 112.00   1.00   31.88    --  111.00  61.00  60.00   27
 25  \w     83.00 110.00   1.00   31.88    --  111.00  77.00 150.00   27
 26  \w    125.00 178.00   1.00   31.88    --  111.00  61.00 -90.00   53
 27  \w    129.00 156.00   1.00   31.88    --  111.00  61.00 120.00   27
 28  \w     84.00 113.00   1.00   31.88    --  111.00  63.00 -77.39   29
 29  \w    123.00 178.00   1.00   31.88    --  111.00  77.00  78.56   55
 30  \w     85.00 123.00   1.00   31.88    --  111.00  61.00 120.00   38
 31  \w     81.00 108.00   1.00   31.88    --  111.00  77.00 -60.00   27
 32  \w     81.00 145.00   1.00   31.88    --  111.00  76.00  13.90   64
 33  \w     85.00 111.00   1.00   31.88    --  111.00  61.00   0.00   26
 34  \w     86.00 112.00   1.00   31.88    --  111.00  61.00-120.00   26
 35  \w     83.00 109.00   1.00   31.88    --  111.00  67.00 -34.72   26
 36  \w     84.00 111.00   1.00   31.88    --  111.00  69.00 177.27   27
 37  \w     85.00 111.00   1.00   31.88    --  111.00  61.00 150.00   26
 38  \w     32.00  92.00   1.00   31.88    --  111.00 -94.00-180.00   60
 39  \w     41.00 139.00   1.00   31.88    --  111.00 -77.00  30.00   98
 40  \w     81.00 108.00   1.00   31.88    --  111.00  77.00  90.00   27
 41  \w     81.00 137.00   1.00   31.88    --  111.00  77.00   0.00   56
 42  \w     81.00 108.00   1.00   31.88    --  111.00  77.00-180.00   27
 43  \w    119.00 178.00   1.00   31.88    --  111.00  77.00-120.00   59
 44  \w     82.00 177.00   1.00   31.88    --  111.00  77.00 120.00   95
 45  \w     86.00 178.00   1.00   31.88    --  111.00  61.00-180.00   92
 46  \w     86.00 113.00   1.00   31.88    --  111.00  61.00 -60.00   27
 47  \w    127.00 177.00   1.00   31.88    --  111.00  60.00 162.55   50
 48  \w     81.00 107.00   1.00   31.88    --  111.00  77.00-120.00   26
 49  \w     65.00 117.00   1.00   31.88    --  111.00-125.00   0.00   52
 50  \w     82.00 178.00   1.00   31.88    --  111.00  77.00  60.00   96
 51  \w     44.00 121.00   1.00   31.88    --  111.00-125.00 -90.00   77
 52  \w     85.00 113.00   1.00   31.88    --  111.00  61.00-150.00   28
 53  \w     43.00 109.00   1.00   31.88    --  111.00 -94.00   0.00   66
 54  \w     85.00 112.00   1.00   31.88    --  111.00  61.00  90.00   27
 55  \w     41.00  91.00   1.00   31.88    --  111.00 -77.00-120.00   50
 56  \w     86.00 118.00   1.00   31.88    --  111.00  60.00 162.55   32
 57  \w     83.00 110.00   1.00   31.88    --  111.00  68.00  59.35   27
 58  \w     81.00 108.00   1.00   31.88    --  111.00  77.00  78.56   27
 59  \w     86.00 154.00   1.00   31.88    --  111.00  59.00 -48.96   68
;
_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      0.0260221000
_diffrn_orient_matrix_UB_12      0.1032475000
_diffrn_orient_matrix_UB_13      0.0089980000
_diffrn_orient_matrix_UB_21      -0.0592922000
_diffrn_orient_matrix_UB_22      0.0104851000
_diffrn_orient_matrix_UB_23      -0.1247625000
_diffrn_orient_matrix_UB_31      -0.1481423000
_diffrn_orient_matrix_UB_32      0.0139635000
_diffrn_orient_matrix_UB_33      0.0269168000
_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  0.0528
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30331
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.991
_diffrn_reflns_theta_min         3.672
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.056
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.815
_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    1.410
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.498(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6734
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0667P)^2^+0.3461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6155
_reflns_number_total             6734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04608h2.cif
_cod_data_source_block           horst33
_cod_depositor_comments
'Adding full bibliography for 7041769--7041777.cif.'
_cod_original_cell_volume        1711.91(8)
_cod_database_code               7041774
_chemical_oxdiff_formula         'C22 H38 F7 K O6 Si3'
_reflns_odcompleteness_completeness 100.00
_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 1.798
_oxdiff_exptl_absorpt_empirical_full_min 0.603
_shelx_res_checksum              8700
_shelxl_version_number           2014-3