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_7041629
_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         'C42 H30 F16 Si4'
_chemical_formula_sum            'C42 H30 F16 Si4'
_chemical_formula_weight         951.02
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-29
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   20.81418(9)
_cell_length_b                   20.81418(9)
_cell_length_c                   32.64138(14)
_cell_measurement_reflns_used    114950
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.1990
_cell_measurement_theta_min      2.7410
_cell_volume                     12246.66(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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 0.9998
_diffrn_measured_fraction_theta_max 0.9985
_diffrn_measurement_details
;
  1 omega  -50.00   33.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -180.0000 83

  2 omega   13.00  115.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  150.0000 102

  3 omega   23.00  114.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000  -90.0000 91

  4 omega   18.00  112.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000   60.0000 94

  5 omega   18.00  112.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  -30.0000 94

  6 omega   57.00  127.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  150.0000 70

  7 omega   13.00  115.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   90.0000 102

  8 omega   13.00  115.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -90.0000 102

  9 omega   13.00  115.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000    0.0000 102

 10 omega   13.00  115.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000 -150.0000 102

 11 omega   57.00  127.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000  -30.0000 70

 12 omega   57.00  127.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000   60.0000 70

 13 omega   41.00   99.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -120.0000 58

 14 omega   41.00  122.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 81

 15 omega   41.00  122.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 81

 16 omega   31.00  109.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 78

 17 omega   41.00  122.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 81

 18 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 93

 19 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 97

 20 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 93

 21 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 97

 22 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 97

 23 omega   86.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   57.0000  -73.6819 92

 24 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 97

 25 omega   43.00  137.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  150.0000 94

 26 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 97

 27 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 93

 28 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 93

 29 omega   31.00  109.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 78

 30 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 97

 31 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 97

 32 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 93

 33 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 97

 34 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 93

 35 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 93

 36 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 93

 37 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 97

 38 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -30.0000 93

 39 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 97

 40 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 93

 41 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 93

 42 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 97

 43 omega   85.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 93

 44 omega   81.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 97

 45 omega   83.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   69.0000   89.3485 95

 46 omega   84.00  178.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   65.0000 -175.5919 94

 47 omega -110.00  -18.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000 -180.0000 92

 48 omega -116.00   -5.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000   30.0000 111

 49 omega   13.00  115.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  120.0000 102

 50 omega   18.00  112.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  -90.0000 94

 51 omega   13.00  115.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -30.0000 102

 52 omega  -42.00  129.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000 -180.0000 171

 53 omega  -42.00  129.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000 -120.0000 171

 54 omega  -42.00  129.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000 -150.0000 171

 55 omega  -42.00  129.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000  -90.0000 171

 56 omega  -42.00  129.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000  -60.0000 171

 57 omega  -42.00  129.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000  -30.0000 171

 58 omega  -42.00   62.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000    0.0000 104

 59 omega   18.00  112.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -120.0000 94
;
_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      0.0663065000
_diffrn_orient_matrix_UB_12      -0.0129674000
_diffrn_orient_matrix_UB_13      -0.0046194000
_diffrn_orient_matrix_UB_21      -0.0090641000
_diffrn_orient_matrix_UB_22      -0.0027648000
_diffrn_orient_matrix_UB_23      -0.0469230000
_diffrn_orient_matrix_UB_31      0.0531140000
_diffrn_orient_matrix_UB_32      0.0844321000
_diffrn_orient_matrix_UB_33      -0.0022693000
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0070
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            147651
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.892
_diffrn_reflns_theta_min         2.800
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.317
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.547
_exptl_crystal_description       fragment
_exptl_crystal_F_000             5784
_exptl_crystal_size_max          0.2066
_exptl_crystal_size_mid          0.1432
_exptl_crystal_size_min          0.1398
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0637P)^2^+20.1703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5318
_reflns_number_total             5344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04293g2.cif
_cod_data_source_block           toma25_9
_cod_depositor_comments
'Adding full bibliography for 7041624--7041640.cif.'
_cod_original_cell_volume        12246.66(12)
_cod_database_code               7041629
_chemical_oxdiff_formula         'C42 H30 F16 Si4'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelx_res_checksum              39928
_shelxl_version_number           2014-3