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_7041770
_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         'C28 H42 F7 K O6 Si3'
_chemical_formula_sum            'C28 H42 F7 K O6 Si3'
_chemical_formula_weight         730.98
_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             2016-01-13
_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                 99.8129(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.62226(18)
_cell_length_b                   14.66422(19)
_cell_length_c                   12.5895(2)
_cell_measurement_reflns_used    19340
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1470
_cell_measurement_theta_min      3.5410
_cell_volume                     1750.43(5)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_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 0.9865
_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    -52.00  29.00   1.00    4.00    --  -38.50  57.00 -30.00   81
  2  \w    -45.00 -16.00   1.00    4.00    --  -38.50 -57.00-180.00   29
  3  \w     24.00  91.00   1.00    4.00    --   43.45-125.00 -60.00   67
  4  \w     44.00 139.00   1.00   16.00    --  111.00 -77.00 -30.00   95
  5  \w    116.00 141.00   1.00   16.00    --  111.00 -77.00   0.00   25
  6  \w     94.00 122.00   1.00   16.00    --  111.00-125.00 120.00   28
  7  \w     52.00 137.00   1.00   16.00    --  111.00 -61.00 150.00   85
  8  \w     89.00 117.00   1.00   16.00    --  111.00  45.00 120.00   28
  9  \w    116.00 176.00   1.00   16.00    --  111.00  72.00 159.40   60
 10  \w    116.00 173.00   1.00   16.00    --  111.00  77.00  90.00   57
 11  \w    135.00 175.00   1.00   16.00    --  111.00  55.00   9.65   40
 12  \w    146.00 173.00   1.00   16.00    --  111.00  59.00 -44.28   27
 13  \w    120.00 178.00   1.00   16.00    --  111.00  77.00 -90.00   58
 14  \w    139.00 176.00   1.00   16.00    --  111.00  77.00-180.00   37
 15  \w    114.00 176.00   1.00   16.00    --  111.00  77.00 -60.00   62
 16  \w    117.00 176.00   1.00   16.00    --  111.00  64.00 -14.47   59
 17  \w    110.00 173.00   1.00   16.00    --  111.00  77.00-120.00   63
 18  \w     88.00 114.00   1.00   16.00    --  111.00  54.00-105.06   26
 19  \w     86.00 119.00   1.00   16.00    --  111.00  56.00 -68.14   33
 20  \w     85.00 112.00   1.00   16.00    --  111.00  68.00   1.81   27
 21  \w     85.00 117.00   1.00   16.00    --  111.00  59.00 -44.28   32
 22  \w     82.00 107.00   1.00   16.00    --  111.00  77.00   0.00   25
 23  \w     85.00 112.00   1.00   16.00    --  111.00  61.00  30.00   27
 24  \w     85.00 114.00   1.00   16.00    --  111.00  61.00  60.00   29
 25  \w     87.00 133.00   1.00   16.00    --  111.00  55.00   9.65   46
 26  \w     86.00 115.00   1.00   16.00    --  111.00  55.00 -53.00   29
 27  \w     85.00 112.00   1.00   16.00    --  111.00  61.00-120.00   27
 28  \w     86.00 175.00   1.00   16.00    --  111.00  61.00-150.00   89
 29  \w     85.00 117.00   1.00   16.00    --  111.00  61.00-180.00   32
 30  \w     81.00 108.00   1.00   16.00    --  111.00  77.00-120.00   27
 31  \w     86.00 113.00   1.00   16.00    --  111.00  61.00 -90.00   27
 32  \w     85.00 111.00   1.00   16.00    --  111.00  61.00 -30.00   26
 33  \w     83.00 110.00   1.00   16.00    --  111.00  77.00 -60.00   27
 34  \w     84.00 110.00   1.00   16.00    --  111.00  64.00 -14.47   26
 35  \w     81.00 167.00   1.00   16.00    --  111.00  77.00  30.00   86
 36  \w    117.00 178.00   1.00   16.00    --  111.00  77.00 120.00   61
 37  \w     81.00 177.00   1.00   16.00    --  111.00  77.00  60.00   96
 38  \w     85.00 111.00   1.00   16.00    --  111.00  61.00  90.00   26
 39  \w     85.00 112.00   1.00   16.00    --  111.00  61.00 120.00   27
 40  \w     84.00 113.00   1.00   16.00    --  111.00  67.00 151.65   29
 41  \w     85.00 112.00   1.00   16.00    --  111.00  61.00 150.00   27
 42  \w     81.00 107.00   1.00   16.00    --  111.00  77.00  90.00   26
 43  \w     81.00 107.00   1.00   16.00    --  111.00  77.00 120.00   26
 44  \w     82.00 112.00   1.00   16.00    --  111.00  72.00 159.40   30
 45  \w     16.00  80.00   1.00    4.00    --   43.45  77.00 120.00   64
 46  \w     13.00  81.00   1.00    4.00    --   43.45  77.00  60.00   68
 47  \w     15.00 110.00   1.00    4.00    --   43.45  77.00 -30.00   95
 48  \w     82.00 109.00   1.00    4.00    --   43.45  77.00-120.00   27
 49  \w     71.00 115.00   1.00    4.00    --   43.45  77.00-150.00   44
 50  \w     81.00 108.00   1.00   16.00    --  111.00  77.00-180.00   27
 51  \w     81.00 107.00   1.00   16.00    --  111.00  77.00-150.00   26
 52  \w     81.00 108.00   1.00   16.00    --  111.00  77.00 -90.00   27
 53  \w     25.00  89.00   1.00    4.00    --   43.45  38.00-150.00   64
 54  \w     21.00  69.00   1.00    4.00    --   43.45  77.00-120.00   48
 55  \w     18.00  61.00   1.00    4.00    --   43.45  57.00 -60.00   43
 56  \w     13.00  60.00   1.00    4.00    --   43.45  77.00-150.00   47
 57  \w     44.00  84.00   1.00   16.00    --  111.00 -77.00   0.00   40
 58  \w     68.00 122.00   1.00   16.00    --  111.00-125.00 -30.00   54
 59  \w     51.00  78.00   1.00   16.00    --  111.00-125.00 120.00   27
 60  \w     50.00 108.00   1.00   16.00    --  111.00 -94.00 150.00   58
 61  \w      1.00  67.00   1.00    4.00    --   43.45 -99.00  90.00   66
 62  \w    -64.00  29.00   1.00    4.00    --  -38.50  57.00 150.00   93
 63  \w   -107.00 -78.00   1.00    4.00    --  -38.50 -57.00-180.00   29
 64  \w   -116.00 -12.00   1.00    4.00    --  -38.50 -19.00   0.00  104
;
_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      -0.0181333000
_diffrn_orient_matrix_UB_12      -0.0399834000
_diffrn_orient_matrix_UB_13      0.1100086000
_diffrn_orient_matrix_UB_21      -0.0776872000
_diffrn_orient_matrix_UB_22      -0.0828828000
_diffrn_orient_matrix_UB_23      -0.0573678000
_diffrn_orient_matrix_UB_31      0.1414610000
_diffrn_orient_matrix_UB_32      -0.0506412000
_diffrn_orient_matrix_UB_33      0.0068515000
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_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            31114
_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         72.000
_diffrn_reflns_theta_min         3.563
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.990
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.619
_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    1.387
_exptl_crystal_description       fragment
_exptl_crystal_F_000             764.0
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 3071 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(7)
_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     443
_refine_ls_number_reflns         6885
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0914P)^2^+0.3797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6665
_reflns_number_total             6885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04608h2.cif
_cod_data_source_block           horst43
_cod_depositor_comments
'Adding full bibliography for 7041769--7041777.cif.'
_cod_database_code               7041770
_chemical_oxdiff_formula         'C33 H33 F6 Si3 K1 O1 '
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_date_sample_data_collection 2016-01-05
_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 1.372
_oxdiff_exptl_absorpt_empirical_full_min 0.608
_shelx_res_checksum              88729
_shelxl_version_number           2014-3