Poly-Lewis-acids based on bowl-shaped tribenzotriquinacene.
Tomaschautzky, Janek; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1112–1123; doi:10.1039/c6dt04350j

data_7041480
_publ_section_title
;
 Poly-Lewis-acids based on bowl-shaped tribenzotriquinacene.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1112
_journal_page_last               1123
_journal_paper_doi               10.1039/c6dt04350j
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C31 H40 Si3'
_chemical_formula_sum            'C31 H40 Si3'
_chemical_formula_weight         496.90
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-17
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   10.20063(12)
_cell_length_b                   10.20063(12)
_cell_length_c                   46.3518(6)
_cell_measurement_reflns_used    12139
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.6300
_cell_measurement_theta_min      5.0740
_cell_volume                     4176.87(9)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_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 0.9938
_diffrn_measurement_details
;
  1 omega  -49.00   30.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -60.0000 158

  2 omega   51.00   78.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   60.0000 54

  3 omega   13.00   60.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -90.0000 94

  4 omega   64.00  111.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000  120.0000 94

  5 omega   55.00  125.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488 -178.0000   90.0000 140

  6 omega   57.00  103.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000 -180.0000 92

  7 omega   73.00  114.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000  -30.0000 82

  8 omega   13.00   68.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  150.0000 110

  9 omega   25.00   65.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000 -150.0000 80

 10 omega   13.00   50.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   60.0000 74

 11 omega   18.00   54.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000  120.0000 72

 12 omega   18.00   56.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000    0.0000 76

 13 omega   86.00  113.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  -90.0000 54

 14 omega   84.00  113.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   71.0000 -148.0000 58

 15 omega    1.00   71.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  -99.0000 -180.0000 140

 16 omega   17.00   71.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   71.0000 -148.0000 108

 17 omega   79.00  106.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000 -150.0000 54

 18 omega   89.00  115.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  150.0000 52

 19 omega   23.00   59.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000  -30.0000 72

 20 omega   13.00  115.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000    0.0000 204

 21 omega   37.00  138.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843  -77.0000 -150.0000 202

 22 omega   78.00  103.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000    0.0000 50

 23 omega   78.00  103.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   74.0000  -93.6977 50

 24 omega   78.00  163.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000   90.0000 170

 25 omega   39.00  106.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843 -125.0000  120.0000 134

 26 omega   82.00  134.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   61.0000 -120.0000 104

 27 omega   82.00  143.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   61.0000 -180.0000 122

 28 omega   78.00  178.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000  -60.0000 200

 29 omega   82.00  112.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   61.0000   30.0000 60

 30 omega   79.00  105.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   71.0000 -148.0000 52

 31 omega   78.00  177.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000   35.5414 198

 32 omega   83.00  109.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   56.0000 -105.1524 52

 33 omega   78.00  103.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   75.0000  -38.9174 50

 34 omega   82.00  141.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   61.0000  -60.0000 118

 35 omega   80.00  163.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   66.0000   87.1822 166

 36 omega   38.00  122.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843 -125.0000   60.0000 168

 37 omega   78.00  105.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000   60.0000 54

 38 omega   78.00  103.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   77.0000  150.0000 50

 39 omega   79.00  102.50   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7843   70.0000  134.8234 47
;
_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      0.0541730000
_diffrn_orient_matrix_UB_12      0.1296943000
_diffrn_orient_matrix_UB_13      0.0221108000
_diffrn_orient_matrix_UB_21      -0.0988079000
_diffrn_orient_matrix_UB_22      0.0553739000
_diffrn_orient_matrix_UB_23      -0.0147683000
_diffrn_orient_matrix_UB_31      -0.1331041000
_diffrn_orient_matrix_UB_32      -0.1025502000
_diffrn_orient_matrix_UB_33      0.0199461000
_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  0.0234
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            16974
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.833
_diffrn_reflns_theta_min         5.097
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) 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    1.185
_exptl_crystal_description       plate
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.1512
_exptl_crystal_size_mid          0.1298
_exptl_crystal_size_min          0.0227
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         1914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0642P)^2^+5.8983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1854
_reflns_number_total             1914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04350j2.cif
_cod_data_source_block           compound8
_cod_depositor_comments
'Adding full bibliography for 7041472--7041483.cif.'
_cod_original_cell_volume        4176.87(11)
_cod_database_code               7041480
_chemical_oxdiff_formula         'C31 H40 Si3 '
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_refinement_description
;
;
_shelxl_version_number           2014-1