Hexadentate poly-Lewis acids based on the bowl-shaped tribenzotriquinacene.
Franke, Maurice; Klingsiek, Maximilian J.; Buth, Julian; Lamm, Jan-Hendrik; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7751–7762; doi:10.1039/d4dt00379a

data_7715245
_publ_section_title
;
 Hexadentate poly-Lewis acids based on the bowl-shaped
 tribenzotriquinacene.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7751
_journal_page_last               7762
_journal_paper_doi               10.1039/d4dt00379a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C31 H34'
_chemical_formula_sum            'C31 H34'
_chemical_formula_weight         406.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-20
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-01-16 deposited with the CCDC.	2024-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                99.294(3)
_cell_angle_beta                 104.180(3)
_cell_angle_gamma                93.662(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0140(4)
_cell_length_b                   9.3643(3)
_cell_length_c                   14.7850(5)
_cell_measurement_reflns_used    5009
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.3050
_cell_measurement_theta_min      4.8300
_cell_volume                     1187.09(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.975
_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    -57.00 -10.00   1.00    5.50    --  -38.50 125.00-180.00   47
  2  \w    -56.00  32.00   1.00    5.50    --  -38.50  37.00  90.00   88
  3  \w   -114.00 -13.00   1.00    5.50    --  -38.50 -19.00 -90.00  101
  4  \w    -82.00 -17.00   1.00    5.50    --  -38.50 125.00 120.00   65
  5  \w     47.00  93.00   1.00    5.50    --   42.70-125.00  30.00   46
  6  \w     85.00 113.00   1.00   31.50    --  111.00-125.00   0.00   28
  7  \w    100.00 177.00   1.00   31.50    --  111.00  15.00  30.00   77
  8  \w     46.00  79.00   1.00   31.50    --  111.00 -61.00 120.00   33
  9  \w     41.00 113.00   1.00   31.50    --  111.00-125.00-120.00   72
 10  \w     55.00 137.00   1.00   31.50    --  111.00 -61.00-150.00   82
 11  \w    139.00 178.00   1.00   31.50    --  111.00  77.00-180.00   39
 12  \w     39.00 106.00   1.00   31.50    --  111.00 -94.00 120.00   67
 13  \w     85.00 178.00   1.00   31.50    --  111.00  61.00 -90.00   93
 14  \w    149.00 177.00   1.00   31.50    --  111.00  77.00 -60.00   28
 15  \w     31.00 107.00   1.00   31.50    --  111.00 -94.00   0.00   76
 16  \w     97.00 163.00   1.00   31.50    --  111.00 125.00-150.00   66
 17  \w     98.00 134.00   1.00   31.50    --  111.00 125.00   0.00   36
 18  \w     33.00  63.00   1.00   31.50    --  111.00 -94.00-120.00   30
 19  \w     74.00  99.00   1.00   31.50    --  111.00 -94.00-120.00   25
 20  \w    112.00 137.00   1.00   31.50    --  111.00 -61.00 120.00   25
 21  \w     95.00 169.00   1.00   31.50    --  111.00  30.00 -30.00   74
 22  \w     62.00 107.00   1.00   31.50    --  111.00 -94.00  60.00   45
 23  \w     38.00  76.00   1.00   31.50    --  111.00 -94.00  30.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1721229000
_diffrn_orient_matrix_UB_12      -0.0369919000
_diffrn_orient_matrix_UB_13      -0.0075814000
_diffrn_orient_matrix_UB_21      0.0207695000
_diffrn_orient_matrix_UB_22      0.0912957000
_diffrn_orient_matrix_UB_23      0.0996269000
_diffrn_orient_matrix_UB_31      -0.0372057000
_diffrn_orient_matrix_UB_32      0.1357013000
_diffrn_orient_matrix_UB_33      -0.0443608000
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9704
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.342
_diffrn_reflns_theta_min         3.136
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
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    1.137
_exptl_crystal_description       plate
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         4856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0550P)^2^+0.3012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4125
_reflns_number_total             4856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00379a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7715245--7715251.cif.'
_cod_database_code               7715245
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C31 H34'
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.945
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
;
_shelx_res_checksum              56330
_olex2_date_sample_data_collection 2021-07-19
_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 1.104
_oxdiff_exptl_absorpt_empirical_full_min 0.908