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_7715250
_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         'C127 H256 Al6 Si24, 2(C6 H14)'
_chemical_formula_sum            'C139 H284 Al6 Si24'
_chemical_formula_weight         2791.69
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2024-01-16 deposited with the CCDC.	2024-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                105.168(2)
_cell_angle_beta                 93.414(2)
_cell_angle_gamma                105.343(2)
_cell_formula_units_Z            2
_cell_length_a                   17.4659(5)
_cell_length_b                   21.6812(6)
_cell_length_c                   26.9593(8)
_cell_measurement_reflns_used    31746
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      27.3310
_cell_measurement_theta_min      3.6270
_cell_volume                     9410.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.94a 64-bit (release 20-10-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -85.00  -6.00   1.00   50.00    --  -17.70 -67.00-126.00   79
  2  \w    -44.00  53.00   1.00   50.00    --  -17.70  67.00   7.00   97
  3  \w    -49.00 -11.00   1.00   50.00    --   18.33 -67.00-126.00   38
  4  \w     -7.00  89.00   1.00   50.00    --   18.33  67.00   7.00   96
  5  \w    -88.00 -17.00   1.00   50.00    --  -17.70 148.00 105.31   71
  6  \w    -93.00 -44.00   1.00   50.00    --  -17.70 155.00 -12.68   49
  7  \w    -84.00   2.00   1.00   50.00    --  -17.70 -38.00  90.00   86
  8  \w    -45.00  41.00   1.00   50.00    --   18.33 -38.00  90.00   86
  9  \w    -39.00  50.00   1.00   50.00    --   18.33 -77.00 -90.00   89
 10  \w     -6.00  42.00   1.00   50.00    --   18.33  77.00 120.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0315292000
_diffrn_orient_matrix_UB_12      0.0182315000
_diffrn_orient_matrix_UB_13      -0.0105682000
_diffrn_orient_matrix_UB_21      -0.0003575000
_diffrn_orient_matrix_UB_22      0.0300525000
_diffrn_orient_matrix_UB_23      0.0183466000
_diffrn_orient_matrix_UB_31      0.0285264000
_diffrn_orient_matrix_UB_32      -0.0044177000
_diffrn_orient_matrix_UB_33      0.0175871000
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            158906
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.301
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.94a (Rigaku Oxford Diffraction, 2023)
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    0.985
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.944
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1947
_refine_ls_number_reflns         34364
_refine_ls_number_restraints     1907
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0755
_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^)+(0.0557P)^2^+22.8162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.1872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24611
_reflns_number_total             34364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00379a2.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 7715245--7715251.cif.'
_cod_database_code               7715250
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C127 H256 Al6 Si24'
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.944
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C128-C129 \\sim C140-C141
 with sigma of 0.02
 C129-C130 \\sim C141-C142
 with sigma of 0.02
 C130-C131 \\sim C142-C143
 with sigma of 0.02
 C131-C132 \\sim C143-C144
 with sigma of 0.02
 C132-C133 \\sim C144-C145
 with sigma of 0.02
 C128-C130 \\sim C140-C142
 with sigma of 0.04
 C129-C131 \\sim C141-C143
 with sigma of 0.04
 C130-C132 \\sim C142-C144
 with sigma of 0.04
 C131-C133 \\sim C143-C145
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C128 \\sim C129 \\sim C130 \\sim C131 \\sim C132 \\sim C133 \\sim C140 \\sim
C141 \\sim C142 \\sim C143 \\sim C144 \\sim C145: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.002 within 2A
4. Rigid body (RIGU) restrains
 Si1A, Si1B, C35A, C35B, C36A, C36B, C37A, C153
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Si3A, Si3B, Si4A, Si4B, C42A, C42B, C43A, C43B, C44A, C44B, C45A, C45B, C46A,
 C46B, C47A, C47B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Si2B, C38A, C38B, C39A, C40A, C40B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C23, C24A, C24B, C25A, C25B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Si8A, Si8B, C61A, C61B, C62A, C62B, C63A, C63B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Si7A, Si7B, C58A, C58B, C59A, C59B, C60A, C60B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Si2A, C38A, C39B, C40A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Si2B, C38B, C39A, C40B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Si9B, C67B, C68B, C69B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Si9A, C67A, C68A, C69A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C128, C129, C130, C131, C132, C133, C140, C141, C142, C143, C144, C145
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Si1B)=Sof(Si2B)=Sof(Si3B)=Sof(Si4B)=Sof(Si7B)=Sof(Si8B)=Sof(Si9B)=
 Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25D)=
 Sof(H25E)=Sof(H25F)=Sof(H34A)=Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=
 Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C38B)=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=Sof(C39B)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40B)=Sof(H40D)=
 Sof(H40E)=Sof(H40F)=Sof(H41A)=Sof(C42B)=Sof(H42D)=Sof(H42E)=Sof(H42F)=
 Sof(C43B)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C44B)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C45B)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C46B)=Sof(H46D)=
 Sof(H46E)=Sof(H46F)=Sof(C47B)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(H57A)=
 Sof(C58B)=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C59B)=Sof(H59D)=Sof(H59E)=
 Sof(H59F)=Sof(C60B)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C61B)=Sof(H61D)=
 Sof(H61E)=Sof(H61F)=Sof(C62B)=Sof(H62D)=Sof(H62E)=Sof(H62F)=Sof(C63B)=
 Sof(H63D)=Sof(H63E)=Sof(H63F)=Sof(H66A)=Sof(C67B)=Sof(H67D)=Sof(H67E)=
 Sof(H67F)=Sof(C68B)=Sof(H68D)=Sof(H68E)=Sof(H68F)=Sof(C69B)=Sof(H69D)=
 Sof(H69E)=Sof(H69F)=Sof(C153)=Sof(H15A)=Sof(H15B)=Sof(H15C)=1-FVAR(1)
 Sof(Si1A)=Sof(Si2A)=Sof(Si3A)=Sof(Si4A)=Sof(Si7A)=Sof(Si8A)=Sof(Si9A)=
 Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=Sof(H34)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36A)=
 Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=
 Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39A)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(H41)=Sof(C42A)=Sof(H42A)=
 Sof(H42B)=Sof(H42C)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44A)=
 Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47A)=Sof(H47A)=Sof(H47B)=
 Sof(H47C)=Sof(H57)=Sof(C58A)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59A)=Sof(H59A)=
 Sof(H59B)=Sof(H59C)=Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C61A)=
 Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C62A)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C63A)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(H66)=Sof(C67A)=Sof(H67A)=Sof(H67B)=
 Sof(H67C)=Sof(C68A)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C69A)=Sof(H69A)=
 Sof(H69B)=Sof(H69C)=FVAR(1)
 Sof(C140)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C141)=Sof(H14D)=Sof(H14E)=
 Sof(C142)=Sof(H14F)=Sof(H14G)=Sof(C143)=Sof(H14H)=Sof(H14I)=Sof(C144)=
 Sof(H14J)=Sof(H14K)=Sof(C145)=Sof(H14L)=Sof(H14M)=Sof(H14N)=1-FVAR(2)
 Sof(C128)=Sof(H12V)=Sof(H12W)=Sof(H12X)=Sof(C129)=Sof(H12Y)=Sof(HB)=Sof(C130)=
 Sof(H13A)=Sof(H13B)=Sof(C131)=Sof(H13C)=Sof(H13D)=Sof(C132)=Sof(H13E)=
 Sof(H13F)=Sof(C133)=Sof(H13G)=Sof(H13H)=Sof(H13I)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C34(H34), C34(H34A), C41(H41), C41(H41A), C50(H50), C57(H57),
 C57(H57A), C66(H66), C66(H66A), C73(H73), C82(H82), C89(H89), C98(H98),
 C105(H105), C114(H114), C121(H121)
6.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C23(H23C,H23D), C24A(H24A,H24B), C24B(H24C,H24D), C26(H26A,
 H26B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C129(H12Y,HB),
 C130(H13A,H13B), C131(H13C,H13D), C132(H13E,H13F), C135(H13M,H13N), C136(H13O,
 H13P), C137(H13Q,H13R), C138(H13S,H13T), C141(H14D,H14E), C142(H14F,H14G),
 C143(H14H,H14I), C144(H14J,H14K)
6.c Me refined with riding coordinates:
 C128(H12V,H12W,H12X), C133(H13G,H13H,H13I), C140(H14A,H14B,H14C), C145(H14L,
 H14M,H14N)
6.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C11(H11), C14(H14), C18(H18), C21(H21)
6.e Idealised Me refined as rotating group:
 C25A(H25A,H25B,H25C), C25B(H25D,H25E,H25F), C28(H28A,H28B,H28C), C31(H31A,
 H31B,H31C), C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F), C36A(H36A,H36B,H36C),
 C36B(H36D,H36E,H36F), C37A(H37A,H37B,H37C), C38A(H38A,H38B,H38C), C38B(H38D,
 H38E,H38F), C39A(H39A,H39B,H39C), C39B(H39D,H39E,H39F), C40A(H40A,H40B,H40C),
 C40B(H40D,H40E,H40F), C42A(H42A,H42B,H42C), C42B(H42D,H42E,H42F), C43A(H43A,
 H43B,H43C), C43B(H43D,H43E,H43F), C44A(H44A,H44B,H44C), C44B(H44D,H44E,H44F),
 C45A(H45A,H45B,H45C), C45B(H45D,H45E,H45F), C46A(H46A,H46B,H46C), C46B(H46D,
 H46E,H46F), C47A(H47A,H47B,H47C), C47B(H47D,H47E,H47F), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C58A(H58A,H58B,H58C), C58B(H58D,H58E,H58F),
 C59A(H59A,H59B,H59C), C59B(H59D,H59E,H59F), C60A(H60A,H60B,H60C), C60B(H60D,
 H60E,H60F), C61A(H61A,H61B,H61C), C61B(H61D,H61E,H61F), C62A(H62A,H62B,H62C),
 C62B(H62D,H62E,H62F), C63A(H63A,H63B,H63C), C63B(H63D,H63E,H63F), C67A(H67A,
 H67B,H67C), C67B(H67D,H67E,H67F), C68A(H68A,H68B,H68C), C68B(H68D,H68E,H68F),
 C69A(H69A,H69B,H69C), C69B(H69D,H69E,H69F), C70(H70A,H70B,H70C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,
 H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C),
 C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,
 H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C90(H90A,H90B,H90C), C91(H91A,
 H91B,H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C),
 C95(H95A,H95B,H95C), C99(H99A,H99B,H99C), C100(H10A,H10B,H10C), C101(H10D,H10E,
 H10F), C102(H10G,H10H,H10I), C103(H10J,H10K,H10L), C104(H10M,H10N,H10O),
 C106(H10P,H10Q,H10R), C107(H10S,H10T,H10U), C108(H10V,H10W,H10X), C109(H10Y,H,
 HA), C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C115(H11G,H11H,H11I),
 C116(H11J,H11K,H11L), C117(H11M,H11N,H11O), C118(H11P,H11Q,H11R), C119(H11S,
 H11T,H11U), C120(H12A,H12B,H12C), C122(H12D,H12E,H12F), C123(H12G,H12H,H12I),
 C124(H12J,H12K,H12L), C125(H12M,H12N,H12O), C126(H12P,H12Q,H12R), C127(H12S,
 H12T,H12U), C153(H15A,H15B,H15C), C134(H13J,H13K,H13L), C139(H13U,H13V,H13W)
;
_shelx_res_checksum              17630
_olex2_date_sample_data_collection 2023-11-22
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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 1.170
_oxdiff_exptl_absorpt_empirical_full_min 0.890