Tridentate Lewis-acids based on triphenylsilane.
Tomaschautzky, Janek; Neumann, Beate; Stammler, Hans-Georg; Mix, Andreas; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1645–1659; doi:10.1039/c6dt04293g

data_7041624
_publ_section_title
;
 Tridentate Lewis-acids based on triphenylsilane.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1645
_journal_page_last               1659
_journal_paper_doi               10.1039/c6dt04293g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C33 H39 F Si4'
_chemical_formula_sum            'C33 H39 F Si4'
_chemical_formula_weight         567.00
_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             2014-08-13
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2016-10-28 deposited with the CCDC.
2017-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                71.086(3)
_cell_angle_beta                 85.433(3)
_cell_angle_gamma                67.607(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7140(4)
_cell_length_b                   12.9359(4)
_cell_length_c                   13.8460(4)
_cell_measurement_reflns_used    12463
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      76.0850
_cell_measurement_theta_min      3.3530
_cell_volume                     1676.37(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9962
_diffrn_measured_fraction_theta_max 0.9962
_diffrn_measurement_details
;
  1 omega -114.00  -45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000  150.0000 69

  2 omega  -60.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000 -150.0000 90

  3 omega  -48.00   33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -30.0000 81

  4 omega -123.00  -96.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  178.0000   90.0000 27

  5 omega  -41.00   -5.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000  150.0000 36

  6 omega   67.00  105.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -180.0000 38

  7 omega   15.00   61.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -180.0000 46

  8 omega   17.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -120.0000 31

  9 omega   24.00   96.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000   90.0000 72

 10 omega   11.00   78.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  -99.0000   30.0000 67

 11 omega   24.00  108.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000  -60.0000 84

 12 omega   15.00   80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000    0.0000 65

 13 omega   13.00   39.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   90.0000 26

 14 omega   13.00   80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  120.0000 67

 15 omega   13.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -60.0000 56

 16 omega   57.00   99.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000 -180.0000 42

 17 omega   82.00  114.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -60.0000 32

 18 omega   85.00  117.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 32

 19 omega   85.00  162.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 77

 20 omega  120.00  148.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 28

 21 omega   86.00  113.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 27

 22 omega   50.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   30.0000 47

 23 omega   81.00  176.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 95

 24 omega   32.00  101.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 69

 25 omega   31.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 76

 26 omega   81.00  163.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 82

 27 omega   85.00  162.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 77

 28 omega   85.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 26

 29 omega   89.00  157.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   30.0000 68

 30 omega   41.00  120.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 79

 31 omega   81.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 33

 32 omega   82.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   72.0000   26.5219 26

 33 omega   85.00  143.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 58

 34 omega   81.00  168.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 87

 35 omega   85.00  162.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 77

 36 omega   81.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 26

 37 omega   85.00  171.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 86

 38 omega   32.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 62

 39 omega   39.00  102.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 63

 40 omega   86.00  113.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 27

 41 omega   81.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 27

 42 omega   82.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 25

 43 omega   85.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 26

 44 omega   42.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -180.0000 49

 45 omega   85.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 26

 46 omega   81.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 26

 47 omega   81.00  175.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 94

 48 omega   81.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 26

 49 omega   82.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 25

 50 omega   81.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 27

 51 omega   84.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   63.0000 -118.5001 27

 52 omega  127.00  152.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   67.0000  -27.3729 25

 53 omega   83.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   67.0000  -27.3729 26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0468550000
_diffrn_orient_matrix_UB_12      -0.1218081000
_diffrn_orient_matrix_UB_13      -0.0151321000
_diffrn_orient_matrix_UB_21      0.0056536000
_diffrn_orient_matrix_UB_22      0.0576725000
_diffrn_orient_matrix_UB_23      -0.1157687000
_diffrn_orient_matrix_UB_31      0.1483879000
_diffrn_orient_matrix_UB_32      -0.0174408000
_diffrn_orient_matrix_UB_33      0.0153857000
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27635
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.114
_diffrn_reflns_theta_min         3.378
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.834
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    1.123
_exptl_crystal_description       plate
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.1876
_exptl_crystal_size_mid          0.1129
_exptl_crystal_size_min          0.0232
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0455P)^2^+0.4612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5699
_reflns_number_total             6581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma15_11
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_database_code               7041624
_chemical_oxdiff_formula         'C20 H20 F20 Si'
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_shelx_res_checksum              18018
_shelxl_version_number           2014-3