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_7715247
_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         'C61 H81 Si6, 2.5[C6H6], 1[C6H6]'
_chemical_formula_sum            'C82 H102 Si6'
_chemical_formula_weight         1256.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-23
_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                90
_cell_angle_beta                 99.9320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.3971(4)
_cell_length_b                   25.3293(3)
_cell_length_c                   24.4731(3)
_cell_measurement_reflns_used    71305
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0920
_cell_measurement_theta_min      3.4560
_cell_volume                     16728.6(4)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_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    -54.00  27.00   1.00    3.00    --  -38.50  32.00-110.00   81
  2  \w    -56.00  32.00   1.00    3.00    --  -38.50  37.00 -30.00   88
  3  \w    -59.00  33.00   1.00    3.00    --  -38.50  37.00 150.00   92
  4  \w    -56.00  14.00   1.00    3.00    --  -38.50  37.00  60.00   70
  5  \w    -86.00 -47.00   1.00    3.00    --  -38.50 125.00 -60.00   39
  6  \w     12.00  39.00   1.00    3.00    --   42.70  80.00-127.93   27
  7  \w     18.00  79.00   1.00    3.00    --   42.70  57.00 -60.00   61
  8  \w     12.00  37.00   1.00    3.00    --   42.70  80.00 117.21   25
  9  \w     12.00  41.00   1.00    3.00    --   42.70  82.00 176.37   29
 10  \w     25.00 109.00   1.00    3.00    --   42.70  32.00-110.00   84
 11  \w     46.00  97.00   1.00    3.00    --   42.70-125.00-180.00   51
 12  \w     12.00  40.00   1.00    3.00    --   42.70  78.00  56.01   28
 13  \w     20.00  51.00   1.00    3.00    --   42.70  57.00 150.00   31
 14  \w     11.00  38.00   1.00    3.00    --   42.70  82.00 -88.36   27
 15  \w     54.00 105.00   1.00    3.00    --   42.70  57.00 150.00   51
 16  \w     13.00  40.00   1.00    3.00    --   42.70  78.00  -5.75   27
 17  \w     20.00  89.00   1.00    3.00    --   42.70  57.00  90.00   69
 18  \w     18.00  96.00   1.00    3.00    --   42.70  57.00   0.00   78
 19  \w     86.00 158.00   1.00   12.50    --  111.00  58.00 104.79   72
 20  \w     82.00 171.00   1.00   12.50    --  111.00  71.00  10.56   89
 21  \w     86.00 167.00   1.00   12.50    --  111.00  57.00 115.81   81
 22  \w     84.00 176.00   1.00   12.50    --  111.00  63.00 -18.23   92
 23  \w     42.00  69.00   1.00   12.50    --  111.00-100.00 158.30   27
 24  \w     41.00 108.00   1.00   12.50    --  111.00-107.00  89.12   67
 25  \w     78.00 107.00   1.00   12.50    --  111.00-100.00 158.30   29
 26  \w     89.00 119.00   1.00   12.50    --  111.00  45.00  90.00   30
 27  \w     43.00 113.00   1.00   12.50    --  111.00-125.00 -30.00   70
 28  \w     31.00 107.00   1.00   12.50    --  111.00 -94.00 -30.00   76
 29  \w     89.00 116.00   1.00   12.50    --  111.00  45.00 -30.00   27
 30  \w     85.00 111.00   1.00   12.50    --  111.00  60.00 -36.52   26
 31  \w     87.00 176.00   1.00   12.50    --  111.00  54.00  50.67   89
 32  \w    121.00 148.00   1.00   12.50    --  111.00  57.00 -81.00   27
 33  \w    100.00 126.00   1.00   12.50    --  111.00-143.00 -66.53   26
 34  \w     83.00 177.00   1.00   12.50    --  111.00  68.00 -73.96   94
 35  \w     85.00 111.00   1.00   12.50    --  111.00  61.00  88.90   26
 36  \w     83.00 109.00   1.00   12.50    --  111.00  67.00   4.14   26
 37  \w     85.00 112.00   1.00   12.50    --  111.00  61.00 150.00   27
 38  \w     85.00 111.00   1.00   12.50    --  111.00  61.00  60.00   26
 39  \w    118.00 178.00   1.00   12.50    --  111.00  69.00 165.36   60
 40  \w     82.00 178.00   1.00   12.50    --  111.00  71.00-115.04   96
 41  \w    121.00 148.00   1.00   12.50    --  111.00  56.00-124.14   27
 42  \w     43.00 132.00   1.00   12.50    --  111.00 -61.00 150.00   89
 43  \w     85.00 112.00   1.00   12.50    --  111.00  61.00 -60.00   27
 44  \w    139.00 178.00   1.00   12.50    --  111.00  61.00 -60.00   39
 45  \w     90.00 116.00   1.00   12.50    --  111.00  45.00-150.00   26
 46  \w     32.00  85.00   1.00   12.50    --  111.00 -94.00  30.00   53
 47  \w     85.00 112.00   1.00   12.50    --  111.00  61.00  30.00   27
 48  \w     85.00 112.00   1.00   12.50    --  111.00  61.00 -30.00   27
 49  \w     89.00 136.00   1.00   12.50    --  111.00  45.00-180.00   47
 50  \w     89.00 115.00   1.00   12.50    --  111.00  45.00-120.00   26
 51  \w     86.00 176.00   1.00   12.50    --  111.00  61.00   0.00   90
 52  \w     85.00 111.00   1.00   12.50    --  111.00  60.00 144.07   26
 53  \w     83.00 110.00   1.00   12.50    --  111.00  69.00 165.36   27
 54  \w    126.00 162.00   1.00   12.50    --  111.00  45.00  90.00   36
 55  \w     43.00 118.00   1.00   12.50    --  111.00 -61.00  60.00   75
 56  \w     85.00 122.00   1.00   12.50    --  111.00  61.00-120.00   37
 57  \w    119.00 175.00   1.00   12.50    --  111.00  61.00-150.00   56
 58  \w     83.00 109.00   1.00   12.50    --  111.00  70.00  73.18   26
 59  \w     84.00 111.00   1.00   12.50    --  111.00  63.00  46.69   27
 60  \w     85.00 112.00   1.00   12.50    --  111.00  61.00-150.00   27
 61  \w     86.00 113.00   1.00   12.50    --  111.00  57.00 -92.78   27
 62  \w     85.00 112.00   1.00   12.50    --  111.00  61.00-180.00   27
 63  \w     82.00 108.00   1.00   12.50    --  111.00  71.00 -86.44   26
 64  \w     84.00 178.00   1.00   12.50    --  111.00  63.00 123.38   94
 65  \w     86.00 114.00   1.00   12.50    --  111.00  56.00-124.14   28
 66  \w     86.00 113.00   1.00   12.50    --  111.00  57.00 -81.00   27
 67  \w     84.00 111.00   1.00   12.50    --  111.00  63.00 -10.63   27
;
_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      -0.0230766000
_diffrn_orient_matrix_UB_12      -0.0380470000
_diffrn_orient_matrix_UB_13      -0.0465130000
_diffrn_orient_matrix_UB_21      0.0038764000
_diffrn_orient_matrix_UB_22      -0.0454617000
_diffrn_orient_matrix_UB_23      0.0422866000
_diffrn_orient_matrix_UB_31      -0.0520942000
_diffrn_orient_matrix_UB_32      0.0134565000
_diffrn_orient_matrix_UB_33      0.0116117000
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            166256
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.718
_diffrn_reflns_theta_min         2.392
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.208
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.644
_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    0.998
_exptl_crystal_description       block
_exptl_crystal_F_000             5424
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         17424
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0979
_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^)+(0.1613P)^2^+39.5396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2880
_refine_ls_wR_factor_ref         0.2938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15581
_reflns_number_total             17424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00379a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7715245--7715251.cif.'
_cod_database_code               7715247
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C61 H82 Si6'
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.760
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 Si2, C37, C38, C39A, C39B, C40A, C40B, C41A, C41B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 Si6A, Si6B, C58, C59A, C59B, C60A, C60B, C61A, C61B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 Si5, C53, C54A, C54B, C55A, C55B, C56A, C56B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
3. Others
 Sof(C39B)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40B)=Sof(H40A)=Sof(H40B)=
 Sof(H40C)=Sof(C41B)=Sof(H41A)=Sof(H41B)=Sof(H41C)=1-FVAR(1)
 Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=
 Sof(H40F)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=FVAR(1)
 Sof(C54B)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C55B)=Sof(H55A)=Sof(H55B)=
 Sof(H55C)=Sof(C56B)=Sof(H56A)=Sof(H56B)=Sof(H56C)=1-FVAR(2)
 Sof(C54A)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C55A)=Sof(H55D)=Sof(H55E)=
 Sof(H55F)=Sof(C56A)=Sof(H56D)=Sof(H56E)=Sof(H56F)=FVAR(2)
 Sof(Si6B)=Sof(C59B)=Sof(H59D)=Sof(H59E)=Sof(H59F)=Sof(C60B)=Sof(H60A)=
 Sof(H60B)=Sof(H60C)=Sof(C61B)=Sof(H61A)=Sof(H61B)=Sof(H61C)=1-FVAR(3)
 Sof(Si6A)=Sof(C59A)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60A)=Sof(H60D)=
 Sof(H60E)=Sof(H60F)=Sof(C61A)=Sof(H61D)=Sof(H61E)=Sof(H61F)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,
 H29B), C30(H30A,H30B)
4.b Me refined with riding coordinates:
 C39A(H39D,H39E,H39F), C39B(H39A,H39B,H39C), C40A(H40D,H40E,H40F), C40B(H40A,
 H40B,H40C), C41A(H41D,H41E,H41F), C41B(H41A,H41B,H41C), C54A(H54D,H54E,H54F),
 C54B(H54A,H54B,H54C), C55A(H55D,H55E,H55F), C55B(H55A,H55B,H55C), C56A(H56D,
 H56E,H56F), C56B(H56A,H56B,H56C), C59A(H59A,H59B,H59C), C59B(H59D,H59E,H59F),
 C60A(H60D,H60E,H60F), C60B(H60A,H60B,H60C), C61A(H61D,H61E,H61F), C61B(H61A,
 H61B,H61C)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C11(H11), C14(H14), C18(H18), C21(H21)
4.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C51(H51A,H51B,H51C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80516
_shelx_fab_checksum              10053
_olex2_date_sample_data_collection 2021-09-15
_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 1.151
_oxdiff_exptl_absorpt_empirical_full_min 0.884