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_7041472
_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         'C34 H40 Cl6 Si3'
_chemical_formula_sum            'C34 H40 Cl6 Si3'
_chemical_formula_weight         745.63
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-20
_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                 103.751(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7815(4)
_cell_length_b                   17.1132(5)
_cell_length_c                   17.4795(6)
_cell_measurement_reflns_used    4807
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      72.9450
_cell_measurement_theta_min      3.5590
_cell_volume                     3713.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.30a (Agilent, 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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_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    -92.00 -23.00   1.00   17.50    --  -38.50 -38.00 150.00   69
  2  \w    -97.00 -47.00   1.00   17.50    --  -38.50-178.00-180.00   50
  3  \w   -122.00 -43.00   1.00   17.50    --  -38.50-178.00 -90.00   79
  4  \w      6.00  66.00   1.00   17.50    --   43.20 -99.00 150.00   60
  5  \w     40.00  75.00   1.00   70.00    --  109.03-125.00 120.00   35
  6  \w     39.00 122.00   1.00   70.00    --  109.03-125.00-120.00   83
  7  \w     79.00 127.00   1.00   70.00    --  109.03  77.00 -60.00   48
  8  \w    102.00 156.00   1.00   70.00    --  109.03  30.00   0.00   54
  9  \w     50.00 120.00   1.00   70.00    --  109.03-125.00  90.00   70
 10  \w     53.00 126.00   1.00   70.00    --  109.03 -15.00 -60.00   73
 11  \w     57.00 116.00   1.00   70.00    --  109.03 -77.00-150.00   59
;
_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      0.1042652000
_diffrn_orient_matrix_UB_12      0.0048557000
_diffrn_orient_matrix_UB_13      -0.0294126000
_diffrn_orient_matrix_UB_21      -0.0431361000
_diffrn_orient_matrix_UB_22      0.0735126000
_diffrn_orient_matrix_UB_23      -0.0480743000
_diffrn_orient_matrix_UB_31      0.0515640000
_diffrn_orient_matrix_UB_32      0.0517159000
_diffrn_orient_matrix_UB_33      0.0711470000
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15261
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.313
_diffrn_reflns_theta_min         3.560
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.324
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.30a (Agilent, 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    1.334
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.383
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7396
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1217P)^2^+3.9325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1860
_refine_ls_wR_factor_ref         0.2055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5606
_reflns_number_total             7396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04350j2.cif
_cod_data_source_block           compound12
_cod_depositor_comments
'Adding full bibliography for 7041472--7041483.cif.'
_cod_database_code               7041472
_chemical_oxdiff_formula         'c6 h6 Cl f si'
_chemical_oxdiff_usercomment     'C40 H34 Si3'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_exptl_crystal_mounting_method mounted
_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 1.129
_oxdiff_exptl_absorpt_empirical_full_min 0.885
_shelx_res_checksum              8960
_shelxl_version_number           2014-3