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_7041773
_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         '2(C18 H36 K N2 O6), C16 H18 F8 Si3'
_chemical_formula_sum            'C52 H90 F8 K2 N4 O12 Si3'
_chemical_formula_weight         1277.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-06
_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                101.0019(12)
_cell_angle_beta                 99.0164(12)
_cell_angle_gamma                106.2033(12)
_cell_formula_units_Z            2
_cell_length_a                   11.42848(16)
_cell_length_b                   14.5458(2)
_cell_length_c                   20.6353(3)
_cell_measurement_reflns_used    50130
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.7290
_cell_measurement_theta_min      3.2160
_cell_volume                     3152.29(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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 0.9994
_diffrn_measured_fraction_theta_max 0.9881
_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   -116.00 -11.00   1.00    2.73    --  -42.33 -77.00  60.00  105
  2  \w   -112.00 -16.00   1.00    2.73    --  -42.33 -57.00 -30.00   96
  3  \w   -115.00 -20.00   1.00    2.73    --  -42.33 -37.00 120.00   95
  4  \w    -69.00  28.00   1.00    2.73    --  -42.33  57.00 -60.00   97
  5  \w   -116.00 -11.00   1.00    2.73    --  -42.33 -77.00-120.00  105
  6  \w   -115.00 -20.00   1.00    2.73    --  -42.33 -37.00-150.00   95
  7  \w   -116.00 -11.00   1.00    2.73    --  -42.33 -77.00 -30.00  105
  8  \w   -115.00 -20.00   1.00    2.73    --  -42.33 -37.00   0.00   95
  9  \w    -69.00  28.00   1.00    2.73    --  -42.33  57.00 120.00   97
 10  \w   -129.00 -35.00   1.00    2.73    --  -42.33-178.00 -90.00   94
 11  \w   -116.00 -11.00   1.00    2.73    --  -42.33 -77.00 150.00  105
 12  \w     57.00 129.00   1.00    2.73    --   42.33 178.00 -60.00   72
 13  \w     39.00 121.00   1.00   12.50    --  111.00-125.00  90.00   82
 14  \w     81.00 178.00   1.00   12.50    --  111.00  70.00  77.56   97
 15  \w     81.00 178.00   1.00   12.50    --  111.00  73.00  11.59   97
 16  \w     81.00 178.00   1.00   12.50    --  111.00  72.00  79.66   97
 17  \w     80.00 178.00   1.00   12.50    --  111.00  75.00  85.72   98
 18  \w     80.00 107.00   1.00   12.50    --  111.00  76.00  50.44   27
 19  \w     32.00  73.00   1.00   12.50    --  111.00 -94.00-120.00   41
 20  \w     83.00 110.00   1.00   12.50    --  111.00  61.00 -30.00   27
 21  \w     80.00 106.00   1.00   12.50    --  111.00  77.00-150.00   26
 22  \w     41.00 138.00   1.00   12.50    --  111.00 -61.00 -60.00   97
 23  \w     80.00 112.00   1.00   12.50    --  111.00  77.00-180.00   32
 24  \w    117.00 164.00   1.00   12.50    --  111.00  77.00-180.00   47
 25  \w     80.00 176.00   1.00   12.50    --  111.00  77.00 150.00   96
 26  \w     80.00 151.00   1.00   12.50    --  111.00  77.00 -60.00   71
 27  \w     83.00 109.00   1.00   12.50    --  111.00  61.00-120.00   26
 28  \w     82.00 148.00   1.00   12.50    --  111.00  66.00-143.80   66
 29  \w     31.00 106.00   1.00   12.50    --  111.00 -94.00 120.00   75
 30  \w     31.00 109.00   1.00   12.50    --  111.00 -94.00 -60.00   78
 31  \w     82.00 178.00   1.00   12.50    --  111.00  69.00-112.96   96
 32  \w     85.00 177.00   1.00   12.50    --  111.00  52.00  85.36   92
 33  \w     81.00 173.00   1.00   12.50    --  111.00  77.00  30.00   92
 34  \w     83.00 109.00   1.00   12.50    --  111.00  61.00-180.00   26
 35  \w     39.00 121.00   1.00   12.50    --  111.00-125.00 120.00   82
 36  \w     84.00 176.00   1.00   12.50    --  111.00  61.00 120.00   92
 37  \w     80.00 107.00   1.00   12.50    --  111.00  77.00 120.00   27
 38  \w     30.00 103.00   1.00   12.50    --  111.00 -94.00-180.00   73
 39  \w     81.00 108.00   1.00   12.50    --  111.00  70.00 117.98   27
 40  \w     80.00 177.00   1.00   12.50    --  111.00  77.00 -30.00   97
 41  \w     83.00 149.00   1.00   12.50    --  111.00  61.00-150.00   66
 42  \w     80.00 107.00   1.00   12.50    --  111.00  77.00  90.00   27
 43  \w    121.00 178.00   1.00   12.50    --  111.00  77.00 -90.00   57
 44  \w     80.00 106.00   1.00   12.50    --  111.00  77.00   0.00   26
 45  \w     80.00 106.00   1.00   12.50    --  111.00  77.00 -90.00   26
 46  \w     65.00 121.00   1.00   12.50    --  111.00-125.00 -60.00   56
 47  \w     87.00 114.00   1.00   12.50    --  111.00  45.00 -60.00   27
 48  \w     83.00 109.00   1.00   12.50    --  111.00  61.00   0.00   26
 49  \w     84.00 109.00   1.00   12.50    --  111.00  61.00 -90.00   25
 50  \w     83.00 119.00   1.00   12.50    --  111.00  61.00 150.00   36
 51  \w    134.00 161.00   1.00   12.50    --  111.00  76.00  50.44   27
 52  \w     80.00 118.00   1.00   12.50    --  111.00  74.00  26.31   38
 53  \w     84.00 128.00   1.00   12.50    --  111.00  61.00 -60.00   44
 54  \w     86.00 136.00   1.00   12.50    --  111.00  55.00  14.32   50
;
_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      -0.0647625000
_diffrn_orient_matrix_UB_12      -0.1126516000
_diffrn_orient_matrix_UB_13      -0.0224001000
_diffrn_orient_matrix_UB_21      -0.1016111000
_diffrn_orient_matrix_UB_22      0.0111193000
_diffrn_orient_matrix_UB_23      0.0390739000
_diffrn_orient_matrix_UB_31      -0.0788370000
_diffrn_orient_matrix_UB_32      0.0119544000
_diffrn_orient_matrix_UB_33      -0.0637003000
_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  0.0252
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            68977
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.343
_diffrn_reflns_theta_min         3.265
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.587
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.346
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         12436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0434P)^2^+1.1217P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11890
_reflns_number_total             12436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04608h2.cif
_cod_data_source_block           horst59
_cod_depositor_comments
'Adding full bibliography for 7041769--7041777.cif.'
_cod_original_cell_volume        3152.30(8)
_cod_database_code               7041773
_chemical_oxdiff_formula         'C52 H54 F8 K2 N4 O12 Si3'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_date_sample_data_collection 2016-09-05
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{C35A, C35B}
{C38A, C43B}
{C42A, C37B}
{C44A, C39B}
{C46A, C46B}
3. Uiso/Uaniso restraints and constraints
Uanis(C35A) = Uanis(C35B)
Uanis(C38A) = Uanis(C43B)
Uanis(C42A) = Uanis(C37B)
Uanis(C44A) = Uanis(C39B)
Uanis(C46A) = Uanis(C46B)
Uanis(F6B) = Uanis(F8A)
Uanis(F6A) = Uanis(F7B)
Uanis(F7A) = Uanis(F5B)
Uanis(F5A) = Uanis(F8B)
Uiso(C1A) = Uiso(C1B)
4. Others
 Sof(F5B)=Sof(F6B)=Sof(F7B)=Sof(F8B)=1-FVAR(1)
 Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=FVAR(1)
 Sof(C1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=
 Sof(H5B)=Sof(C6B)=Sof(H6B)=1-FVAR(2)
 Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(H6A)=FVAR(2)
 Sof(O7B)=Sof(O8B)=Sof(O9B)=Sof(O10B)=Sof(N3B)=Sof(N4B)=Sof(C35B)=Sof(H35C)=
 Sof(H35D)=Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(C37B)=Sof(H37C)=Sof(H37D)=
 Sof(C38B)=Sof(H38C)=Sof(H38D)=Sof(C39B)=Sof(H39C)=Sof(H39D)=Sof(C40B)=
 Sof(H40C)=Sof(H40D)=Sof(C41B)=Sof(H41C)=Sof(H41D)=Sof(C42B)=Sof(H42C)=
 Sof(H42D)=Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(C44B)=Sof(H44C)=Sof(H44D)=
 Sof(C45B)=Sof(H45C)=Sof(H45D)=Sof(C46B)=Sof(H46C)=Sof(H46D)=Sof(C47B)=
 Sof(H47C)=Sof(H47D)=Sof(C48B)=Sof(H48C)=Sof(H48D)=Sof(C49B)=Sof(H49C)=
 Sof(H49D)=Sof(C50B)=Sof(H50C)=Sof(H50D)=Sof(C51B)=Sof(H51C)=Sof(H51D)=
 Sof(C52B)=Sof(H52C)=Sof(H52D)=1-FVAR(3)
 Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=Sof(N3A)=Sof(N4A)=Sof(C35A)=Sof(H35A)=
 Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(C37A)=Sof(H37A)=Sof(H37B)=
 Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(C40A)=
 Sof(H40A)=Sof(H40B)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(C42A)=Sof(H42A)=
 Sof(H42B)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(C44A)=Sof(H44A)=Sof(H44B)=
 Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(C47A)=
 Sof(H47A)=Sof(H47B)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(C49A)=Sof(H49A)=
 Sof(H49B)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(C51A)=Sof(H51A)=Sof(H51B)=
 Sof(C52A)=Sof(H52A)=Sof(H52B)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
  C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35A(H35A,H35B),
 C36A(H36A,H36B), C37A(H37A,H37B), C38A(H38A,H38B), C39A(H39A,H39B), C40A(H40A,
 H40B), C41A(H41A,H41B), C42A(H42A,H42B), C43A(H43A,H43B), C44A(H44A,H44B),
 C45A(H45A,H45B), C46A(H46A,H46B), C47A(H47A,H47B), C48A(H48A,H48B), C49A(H49A,
 H49B), C50A(H50A,H50B), C51A(H51A,H51B), C52A(H52A,H52B), C35B(H35C,H35D),
 C36B(H36C,H36D), C37B(H37C,H37D), C38B(H38C,H38D), C39B(H39C,H39D), C40B(H40C,
 H40D), C41B(H41C,H41D), C42B(H42C,H42D), C43B(H43C,H43D), C44B(H44C,H44D),
 C45B(H45C,H45D), C46B(H46C,H46D), C47B(H47C,H47D), C48B(H48C,H48D), C49B(H49C,
 H49D), C50B(H50C,H50D), C51B(H51C,H51D), C52B(H52C,H52D)
5.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C2B(H2B), C3B(H3B),
 C4B(H4B), C5B(H5B), C6B(H6B), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12)
;
_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 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.859
_shelx_res_checksum              23416
_shelxl_version_number           2013-2