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_7041482
_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 H31 F9 Si3, Cl3 Sb'
_chemical_formula_sum            'C31 H31 Cl3 F9 Sb Si3'
_chemical_formula_weight         886.93
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-21
_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            2
_cell_length_a                   14.3167(4)
_cell_length_b                   14.3167(4)
_cell_length_c                   10.44916(16)
_cell_measurement_reflns_used    25281
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      71.7310
_cell_measurement_theta_min      3.5320
_cell_volume                     1854.80(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 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    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9988
_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    -64.00  30.00   1.00    3.50    --  -38.50  57.00  60.00   94
  2  \w    -64.00  30.00   1.00    3.50    --  -38.50  57.00-180.00   94
  3  \w    -64.00  30.00   1.00    3.50    --  -38.50  57.00 -60.00   94
  4  \w     13.00 115.00   1.00    3.50    --   43.45  77.00 -30.00  102
  5  \w     13.00 115.00   1.00    3.50    --   43.45  77.00  30.00  102
  6  \w     13.00 115.00   1.00    3.50    --   43.45  77.00-150.00  102
  7  \w     23.00 114.00   1.00    3.50    --   43.45  38.00 -60.00   91
  8  \w     13.00 115.00   1.00    3.50    --   43.45  77.00 -90.00  102
  9  \w     13.00 115.00   1.00    3.50    --   43.45  77.00 150.00  102
 10  \w     23.00  97.00   1.00    3.50    --   43.45-125.00 -90.00   74
 11  \w     23.00 114.00   1.00    3.50    --   43.45  38.00-180.00   91
 12  \w     23.00  97.00   1.00    3.50    --   43.45-125.00  90.00   74
 13  \w     13.00 115.00   1.00    3.50    --   43.45  77.00  90.00  102
 14  \w     23.00 114.00   1.00    3.50    --   43.45  38.00  60.00   91
 15  \w     31.00 109.00   1.00   33.00    --  111.00 -94.00 -60.00   78
 16  \w     85.00 178.00   1.00   33.00    --  111.00  61.00 150.00   93
 17  \w     40.00 141.00   1.00   33.00    --  111.00 -77.00  60.00  101
 18  \w     81.00 178.00   1.00   33.00    --  111.00  77.00-150.00   97
 19  \w     41.00 122.00   1.00   33.00    --  111.00-125.00-120.00   81
 20  \w     41.00 133.00   1.00   33.00    --  111.00 -45.00  60.00   92
 21  \w     81.00 178.00   1.00   33.00    --  111.00  77.00  90.00   97
 22  \w     85.00 178.00   1.00   33.00    --  111.00  61.00  60.00   93
 23  \w     31.00 109.00   1.00   33.00    --  111.00 -94.00-120.00   78
 24  \w     81.00 178.00   1.00   33.00    --  111.00  77.00  30.00   97
 25  \w     85.00 178.00   1.00   33.00    --  111.00  61.00 -90.00   93
 26  \w     82.00 178.00   1.00   33.00    --  111.00  72.00  76.59   96
 27  \w     81.00 178.00   1.00   33.00    --  111.00  77.00-120.00   97
 28  \w     31.00 109.00   1.00   33.00    --  111.00 -94.00  30.00   78
 29  \w     85.00 178.00   1.00   33.00    --  111.00  61.00  30.00   93
 30  \w     85.00 178.00   1.00   33.00    --  111.00  61.00 -60.00   93
 31  \w     85.00 178.00   1.00   33.00    --  111.00  61.00-150.00   93
 32  \w     85.00 178.00   1.00   33.00    --  111.00  61.00 120.00   93
 33  \w     81.00 178.00   1.00   33.00    --  111.00  77.00  60.00   97
 34  \w     81.00 178.00   1.00   33.00    --  111.00  77.00 -90.00   97
 35  \w     81.00 178.00   1.00   33.00    --  111.00  77.00-180.00   97
 36  \w     81.00 178.00   1.00   33.00    --  111.00  77.00 150.00   97
 37  \w     81.00 178.00   1.00   33.00    --  111.00  77.00   0.00   97
 38  \w     85.00 178.00   1.00   33.00    --  111.00  61.00   0.00   93
 39  \w     81.00 178.00   1.00   33.00    --  111.00  77.00 120.00   97
 40  \w     85.00 178.00   1.00   33.00    --  111.00  61.00-120.00   93
 41  \w     85.00 178.00   1.00   33.00    --  111.00  61.00-180.00   93
 42  \w     41.00 122.00   1.00   33.00    --  111.00-125.00  30.00   81
 43  \w     81.00 178.00   1.00   33.00    --  111.00  77.00 -30.00   97
 44  \w     85.00 178.00   1.00   33.00    --  111.00  61.00 -30.00   93
 45  \w     41.00 122.00   1.00   33.00    --  111.00-125.00 150.00   81
 46  \w     84.00 178.00   1.00   33.00    --  111.00  64.00 -48.37   94
 47  \w     82.00 178.00   1.00   33.00    --  111.00  72.00 120.40   96
 48  \w   -110.00  -8.00   1.00    3.50    --  -38.50 -77.00-180.00  102
 49  \w   -107.00 -13.00   1.00    3.50    --  -38.50 -57.00-180.00   94
 50  \w     23.00 114.00   1.00    3.50    --   43.45  38.00  90.00   91
 51  \w     18.00 112.00   1.00    3.50    --   43.45  57.00-120.00   94
 52  \w     21.00 117.00   1.00    3.50    --   43.45  28.00 -24.00   96
 53  \w    -42.00 129.00   1.00    3.50    --   43.45   0.00-180.00  171
 54  \w     18.00 112.00   1.00    3.50    --   43.45  57.00-150.00   94
 55  \w    -42.00 129.00   1.00    3.50    --   43.45   0.00-150.00  171
 56  \w    -42.00 129.00   1.00    3.50    --   43.45   0.00-120.00  171
 57  \w    -42.00 129.00   1.00    3.50    --   43.45   0.00 -90.00  171
 58  \w    -42.00 129.00   1.00    3.50    --   43.45   0.00 -60.00  171
 59  \w    -42.00 129.00   1.00    3.50    --   43.45   0.00 -30.00  171
 60  \w     23.00 114.00   1.00    3.50    --   43.45  38.00 -90.00   91
;
_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      0.0128807000
_diffrn_orient_matrix_UB_12      0.0700936000
_diffrn_orient_matrix_UB_13      0.1179166000
_diffrn_orient_matrix_UB_21      0.0436051000
_diffrn_orient_matrix_UB_22      -0.0615123000
_diffrn_orient_matrix_UB_23      0.0776425000
_diffrn_orient_matrix_UB_31      0.1156281000
_diffrn_orient_matrix_UB_32      0.0820560000
_diffrn_orient_matrix_UB_33      -0.0424581000
_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  0.0573
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            65175
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.239
_diffrn_reflns_theta_min         3.565
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.426
_exptl_absorpt_correction_T_max  0.440
_exptl_absorpt_correction_T_min  0.150
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.588
_exptl_crystal_description       fragment
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0683
_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^)+(0.1800P)^2^+0.1423P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1785
_reflns_number_total             2286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04350j2.cif
_cod_data_source_block           compound15
_cod_depositor_comments
'Adding full bibliography for 7041472--7041483.cif.'
_cod_original_cell_volume        1854.80(10)
_cod_database_code               7041482
_chemical_oxdiff_formula         'C31 H31 Cl3 F9 Sb Si3'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: F1A(0.5) F1B(0.5) F2A(0.5) F2B(0.5) F3A(0.5) F3B(0.5) Sb1(0.33333)
 Cl1(0.33333) Cl2(0.33333) Cl3(0.33333)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
;
_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 1.531
_oxdiff_exptl_absorpt_empirical_full_min 0.590
_shelxl_version_number           2013-2