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_7041777
_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 H14 F8 Si3, 2(C18 H36 K N2 O6)'
_chemical_formula_sum            'C52 H86 F8 K2 N4 O12 Si3'
_chemical_formula_weight         1273.71
_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             2016-09-30
_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                102.4812(10)
_cell_angle_beta                 98.9460(9)
_cell_angle_gamma                105.1347(11)
_cell_formula_units_Z            2
_cell_length_a                   11.25235(13)
_cell_length_b                   14.6618(2)
_cell_length_c                   20.6823(2)
_cell_measurement_reflns_used    72648
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      30.0410
_cell_measurement_theta_min      1.9220
_cell_volume                     3133.61(7)
_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(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9986
_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      6.00  95.00   1.00   25.00    --   25.97  57.00 150.00   89
  2  \w      6.00  95.00   1.00   25.00    --   25.97  57.00 -30.00   89
  3  \w    -43.00  47.00   1.00   25.00    --   25.97 -57.00   0.00   90
  4  \w      6.00  95.00   1.00   25.00    --   25.97  57.00  60.00   89
  5  \w      6.00  95.00   1.00   25.00    --   25.97  57.00-120.00   89
  6  \w    -43.00  47.00   1.00   25.00    --   25.97 -57.00  90.00   90
  7  \w    -44.00  56.00   1.00   25.00    --   25.97 -77.00 -60.00  100
  8  \w    -43.00  47.00   1.00   25.00    --   25.97 -57.00-180.00   90
  9  \w    -20.00  68.00   1.00   25.00    --   25.97 -99.00  30.00   88
 10  \w    -20.00  68.00   1.00   25.00    --   25.97 -99.00-150.00   88
 11  \w    -36.00  -7.00   1.00   25.00    --   25.97 133.00 -99.46   29
 12  \w    -45.00  45.00   1.00   25.00    --  -23.50  57.00   0.00   90
 13  \w    -92.00  -2.00   1.00   25.00    --  -23.50 -57.00 -90.00   90
 14  \w    -94.00   7.00   1.00   25.00    --  -23.50 -77.00  90.00  101
 15  \w    -46.00  51.00   1.00   25.00    --   25.97 -38.00-120.00   97
 16  \w     -4.00  96.00   1.00   25.00    --   25.97  77.00-180.00  100
 17  \w      0.00  98.00   1.00   25.00    --   25.97  38.00-120.00   98
 18  \w      6.00  95.00   1.00   25.00    --   25.97  57.00   0.00   89
 19  \w    -20.00  68.00   1.00   25.00    --   25.97 -99.00-120.00   88
 20  \w      7.00  88.00   1.00   25.00    --   25.97-133.00-167.82   81
 21  \w    -47.00  99.00   1.00   25.00    --   25.97   0.00-150.00  146
 22  \w    -47.00  99.00   1.00   25.00    --   25.97   0.00-120.00  146
 23  \w    -47.00  99.00   1.00   25.00    --   25.97   0.00 -90.00  146
 24  \w    -47.00  65.00   1.00   25.00    --   25.97   0.00 -60.00  112
 25  \w    -47.00  99.00   1.00   25.00    --   25.97   0.00-180.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0128709000
_diffrn_orient_matrix_UB_12      0.0452128000
_diffrn_orient_matrix_UB_13      0.0017514000
_diffrn_orient_matrix_UB_21      -0.0638118000
_diffrn_orient_matrix_UB_22      -0.0257607000
_diffrn_orient_matrix_UB_23      -0.0168128000
_diffrn_orient_matrix_UB_31      -0.0159265000
_diffrn_orient_matrix_UB_32      -0.0002287000
_diffrn_orient_matrix_UB_33      0.0318393000
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            183781
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         1.572
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.975
_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    1.350
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.187
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         18403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0318P)^2^+2.0536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16083
_reflns_number_total             18403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04608h2.cif
_cod_data_source_block           horst63
_cod_depositor_comments
'Adding full bibliography for 7041769--7041777.cif.'
_cod_original_cell_volume        3133.60(7)
_cod_database_code               7041777
_chemical_oxdiff_formula         'C52 H86 F8 K2 N4 O12 Si3'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_date_sample_data_collection 2016-09-28
_olex2_date_sample_submission    1474495200
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{C46A, C46B}
3. Uiso/Uaniso restraints and constraints
Uanis(F6B) = Uanis(F8A)
Uanis(F6A) = Uanis(F7B)
Uanis(F7A) = Uanis(F5B)
Uanis(F5A) = Uanis(F8B)
Uanis(C1A) = Uanis(C1B)
Uanis(C35B) = Uanis(C35A)
Uanis(C43A) = Uanis(C38B)
Uanis(C44B) = Uanis(C39A)
Uanis(C46A) = Uanis(C46B)
Uanis(C35A) = Uanis(C35B)
4. Others
 Sof(F5B)=Sof(F6B)=Sof(F7B)=Sof(F8B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=1-
 FVAR(1)
 Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=
 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(C40A)=Sof(H40A)=Sof(H40B)=Sof(C39A)=
 Sof(H39A)=Sof(H39B)=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:
 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), C40A(H40A,H40B),
 C39A(H39A,H39B), 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),
 C13(H13), C14(H14), C15A(H15A), C16A(H16A), C15B(H15B), C16B(H16B)
;
_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 1.298
_oxdiff_exptl_absorpt_empirical_full_min 0.788
_shelxl_version_number           2013-3