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_7041477
_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 F6 Si3, Cl3 Sb'
_chemical_formula_sum            'C34 H40 Cl3 F6 Sb Si3'
_chemical_formula_weight         875.03
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-20
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2016-11-02 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.165(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.27399(19)
_cell_length_b                   26.8362(6)
_cell_length_c                   14.2421(3)
_cell_measurement_reflns_used    57901
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.0400
_cell_measurement_theta_min      2.9310
_cell_volume                     3790.01(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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 0.9987
_diffrn_measured_fraction_theta_max 0.9968
_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    -72.00 -24.00   1.00   16.50    --  -17.08 126.00-131.72   48
  2  \w    -72.00 -24.00   1.00   16.50    --  -17.08 126.00 122.74   48
  3  \w    -75.00 -27.00   1.00   16.50    --  -17.08 131.00  37.75   48
  4  \w     -8.00  86.00   1.00   16.50    --   17.39  57.00 -60.00   94
  5  \w    -13.00  89.00   1.00   16.50    --   17.39  77.00 150.00  102
  6  \w    -51.00  43.00   1.00   16.50    --   17.39 -57.00   0.00   94
  7  \w     35.00 101.00   1.00   16.50    --   17.39 178.00-180.00   66
  8  \w     -8.00  86.00   1.00   16.50    --   17.39  57.00  60.00   94
  9  \w    -54.00  38.00   1.00   16.50    --   17.39 -37.00-120.00   92
 10  \w    -51.00  43.00   1.00   16.50    --   17.39 -57.00 150.00   94
 11  \w    -85.00   8.00   1.00   16.50    --  -17.08 -57.00-150.00   93
 12  \w    -91.00 -39.00   1.00   16.50    --  -17.08 154.00 149.93   52
 13  \w    -88.00  13.00   1.00   16.50    --  -17.08 -77.00 -60.00  101
 14  \w    -75.00 -27.00   1.00   16.50    --  -17.08 131.00 -13.33   48
 15  \w    -69.00 -20.00   1.00   16.50    --  -17.08 121.00 -91.07   49
 16  \w    -88.00   3.00   1.00   16.50    --  -17.08 -37.00-150.00   91
 17  \w    -76.00 -29.00   1.00   16.50    --  -17.08 133.00  65.82   47
 18  \w    -75.00 -27.00   1.00   16.50    --  -17.08 131.00 -45.22   48
 19  \w    -42.00  51.00   1.00   16.50    --  -17.08  57.00-120.00   93
 20  \w   -101.00 -55.00   1.00   16.50    --  -17.08 178.00 -30.00   46
 21  \w    -50.00  15.00   1.00   16.50    --  -17.08  85.00 -96.69   65
 22  \w    -51.00  43.00   1.00   16.50    --   17.39 -57.00  60.00   94
 23  \w    -20.00  56.00   1.00   16.50    --   17.39 -99.00  60.00   76
 24  \w    -68.00 103.00   1.00   16.50    --   17.39   0.00-180.00  171
 25  \w     35.00 101.00   1.00   16.50    --   17.39 178.00  90.00   66
;
_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      -0.0038738000
_diffrn_orient_matrix_UB_12      0.0262813000
_diffrn_orient_matrix_UB_13      -0.0053597000
_diffrn_orient_matrix_UB_21      0.0699687000
_diffrn_orient_matrix_UB_22      0.0009113000
_diffrn_orient_matrix_UB_23      0.0030241000
_diffrn_orient_matrix_UB_31      -0.0143088000
_diffrn_orient_matrix_UB_32      -0.0026959000
_diffrn_orient_matrix_UB_33      -0.0512289000
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            222083
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.079
_diffrn_reflns_theta_min         2.554
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         11143
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0395P)^2^+2.9446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9358
_reflns_number_total             11143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04350j2.cif
_cod_data_source_block           compound13
_cod_depositor_comments
'Adding full bibliography for 7041472--7041483.cif.'
_cod_original_cell_volume        3790.02(14)
_cod_database_code               7041477
_chemical_oxdiff_formula         'C34 H40 Cl3 F6 Sb1 Si3'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_date_sample_data_collection 2016-05-03
_olex2_date_sample_submission    1461189600
_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 1.520
_oxdiff_exptl_absorpt_empirical_full_min 0.539
_shelx_res_checksum              88308
_shelxl_version_number           2014-3