Host-guest chemistry of tridentate Lewis acids based on tribenzotriquinacene.
Franke, Maurice; Ens, Tobin; Mix, Andreas; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11970–11980; doi:10.1039/d4dt01558d

data_7716494
_publ_section_title
;
 Host-guest chemistry of tridentate Lewis acids based on
 tribenzotriquinacene.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11970
_journal_page_last               11980
_journal_paper_doi               10.1039/d4dt01558d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C40 H49 F9 O9 S3 Si3'
_chemical_formula_sum            'C40 H49 F9 O9 S3 Si3'
_chemical_formula_weight         1025.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-11
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-04-02 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.786(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.6372(6)
_cell_length_b                   16.1597(5)
_cell_length_c                   34.9455(11)
_cell_measurement_reflns_used    13650
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1420
_cell_measurement_theta_min      2.8000
_cell_volume                     9955.0(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -110.00 -29.00   1.00   49.50    --  -38.50 -37.00  30.00   81
  2  \w    -72.00  39.00   1.00   49.50    --  -38.50  19.00-150.00  111
  3  \w    -51.00  30.00   1.00   49.50    --  -38.50  57.00 -90.00   81
  4  \w     43.00  97.00   1.00   49.50    --   42.70-125.00-180.00   54
  5  \w      7.00  77.00   1.00   49.50    --   42.70 -99.00 -30.00   70
  6  \w     43.00  80.00   1.00   77.50    --  111.00 -45.00 -60.00   37
  7  \w     76.00 113.00   1.00   77.50    --  111.00-125.00 -30.00   37
  8  \w     79.00 113.00   1.00   77.50    --  111.00-125.00 150.00   34
  9  \w     48.00 132.00   1.00   77.50    --  111.00 -45.00-150.00   84
 10  \w     47.00 129.00   1.00   77.50    --  111.00 -45.00  30.00   82
 11  \w    111.00 162.00   1.00   77.50    --  111.00  30.00-150.00   51
 12  \w     46.00  74.00   1.00   77.50    --  111.00-125.00  60.00   28
 13  \w     66.00 107.00   1.00   77.50    --  111.00 -94.00-180.00   41
 14  \w     42.00 133.00   1.00   77.50    --  111.00 -45.00 120.00   91
 15  \w     76.00 113.00   1.00   77.50    --  111.00-125.00 -90.00   37
 16  \w     88.00 131.00   1.00   77.50    --  111.00 -45.00 -60.00   43
 17  \w     31.00  62.00   1.00   77.50    --  111.00 -94.00  30.00   31
 18  \w     72.00 113.00   1.00   77.50    --  111.00-125.00-180.00   41
 19  \w     75.00 113.00   1.00   77.50    --  111.00-125.00   0.00   38
 20  \w     63.00 107.00   1.00   77.50    --  111.00 -94.00   0.00   44
 21  \w     63.00 107.00   1.00   77.50    --  111.00 -94.00  60.00   44
 22  \w     26.00 172.00   1.00   77.50    --  111.00   0.00-180.00  146
;
_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      0.0577010000
_diffrn_orient_matrix_UB_12      0.0595829000
_diffrn_orient_matrix_UB_13      -0.0174538000
_diffrn_orient_matrix_UB_21      0.0516312000
_diffrn_orient_matrix_UB_22      -0.0085847000
_diffrn_orient_matrix_UB_23      0.0361361000
_diffrn_orient_matrix_UB_31      0.0404173000
_diffrn_orient_matrix_UB_32      -0.0739290000
_diffrn_orient_matrix_UB_33      -0.0183455000
_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  0.0813
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            71522
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.013
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.786
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.649
_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    1.368
_exptl_crystal_description       needle
_exptl_crystal_F_000             4256
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.094
_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     1375
_refine_ls_number_reflns         18213
_refine_ls_number_restraints     1340
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0988
_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^)+(0.1080P)^2^+41.5780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2465
_refine_ls_wR_factor_ref         0.2682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12624
_reflns_number_total             18213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01558d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7716492--7716494.cif.'
_cod_database_code               7716494
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40H49F9O9S3Si3
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.425
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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. Uiso/Uaniso restraints and constraints
C40A \\sim H78C \\sim O9A \\sim C34A \\sim H77A \\sim F17A \\sim O15A \\sim S5A
\\sim C78A \\sim F4A \\sim O6A \\sim F5A \\sim O18A \\sim F6A \\sim O14A \\sim
F18A \\sim H78A \\sim F9A \\sim H79B \\sim F14A \\sim O17A \\sim F16A \\sim
O16A \\sim S3A \\sim O7A \\sim S6A \\sim O5A \\sim Si6A \\sim O8A \\sim F7A
\\sim O13A \\sim F8A \\sim H78B \\sim S2A \\sim H79A \\sim F13A \\sim C79A
\\sim F15A \\sim H79C \\sim O4A \\sim C74A \\sim C80A \\sim H77B: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C40B \\sim O5B \\sim O4B \\sim C34B \\sim H78D \\sim S3B \\sim F17B \\sim S2B
\\sim H78F \\sim O18B \\sim F7B \\sim O16B \\sim O17B \\sim F5B \\sim F16B
\\sim F4B \\sim H79D \\sim F14B \\sim H77D \\sim F18B \\sim Si6B \\sim F6B
\\sim F9B \\sim O15B \\sim S5B \\sim O9B \\sim F13B \\sim O6B \\sim O13B \\sim
F8B \\sim S6B \\sim O7B \\sim H79F \\sim O14B \\sim C78B \\sim F15B \\sim H77C
\\sim C80B \\sim H78E \\sim O8B \\sim C79B \\sim C74B \\sim H79E: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40A) \\sim Ueq, Uanis(O9A) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(F17A)
\\sim Ueq, Uanis(O15A) \\sim Ueq, Uanis(S5A) \\sim Ueq, Uanis(C78A) \\sim Ueq,
Uanis(F4A) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(O18A)
\\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(O14A) \\sim Ueq, Uanis(F18A) \\sim Ueq,
Uanis(F9A) \\sim Ueq, Uanis(F14A) \\sim Ueq, Uanis(O17A) \\sim Ueq, Uanis(F16A)
\\sim Ueq, Uanis(O16A) \\sim Ueq, Uanis(S3A) \\sim Ueq, Uanis(O7A) \\sim Ueq,
Uanis(S6A) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(Si6A) \\sim Ueq, Uanis(O8A)
\\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(O13A) \\sim Ueq, Uanis(F8A) \\sim Ueq,
Uanis(S2A) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(C79A) \\sim Ueq, Uanis(F15A)
\\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(C74A) \\sim Ueq, Uanis(C80A) \\sim Ueq,
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40B) \\sim Ueq, Uanis(O5B) \\sim Ueq, Uanis(O4B) \\sim Ueq, Uanis(C34B)
\\sim Ueq, Uanis(S3B) \\sim Ueq, Uanis(F17B) \\sim Ueq, Uanis(S2B) \\sim Ueq,
Uanis(O18B) \\sim Ueq, Uanis(F7B) \\sim Ueq, Uanis(O16B) \\sim Ueq, Uanis(O17B)
\\sim Ueq, Uanis(F5B) \\sim Ueq, Uanis(F16B) \\sim Ueq, Uanis(F4B) \\sim Ueq,
Uanis(F14B) \\sim Ueq, Uanis(F18B) \\sim Ueq, Uanis(Si6B) \\sim Ueq, Uanis(F6B)
\\sim Ueq, Uanis(F9B) \\sim Ueq, Uanis(O15B) \\sim Ueq, Uanis(S5B) \\sim Ueq,
Uanis(O9B) \\sim Ueq, Uanis(F13B) \\sim Ueq, Uanis(O6B) \\sim Ueq, Uanis(O13B)
\\sim Ueq, Uanis(F8B) \\sim Ueq, Uanis(S6B) \\sim Ueq, Uanis(O7B) \\sim Ueq,
Uanis(O14B) \\sim Ueq, Uanis(C78B) \\sim Ueq, Uanis(F15B) \\sim Ueq,
Uanis(C80B) \\sim Ueq, Uanis(O8B) \\sim Ueq, Uanis(C79B) \\sim Ueq, Uanis(C74B)
\\sim Ueq, : with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7A) = Uanis(O7B)
Uanis(C34A) = Uanis(C34B)
Uanis(O16A) = Uanis(O16B)
Uanis(O4A) = Uanis(O4B)
Uanis(C79A) = Uanis(C79B)
Uanis(C78A) = Uanis(C78B)
3. Rigid body (RIGU) restrains
 C40B, O5B, O4B, C34B, H78D, S3B, F17B, S2B, H78F, O18B, F7B, O16B, O17B, F5B,
 F16B, F4B, H79D, F14B, H77D, F18B, Si6B, F6B, F9B, O15B, S5B, O9B, F13B, O6B,
 O13B, F8B, S6B, O7B, H79F, O14B, C78B, F15B, H77C, C80B, H78E, O8B, C79B, C74B,
  H79E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C40A, H78C, O9A, C34A, H77A, F17A, O15A, S5A, C78A, F4A, O6A, F5A, O18A, F6A,
 O14A, F18A, H78A, F9A, H79B, F14A, O17A, F16A, O16A, S3A, O7A, S6A, O5A, Si6A,
 O8A, F7A, O13A, F8A, H78B, S2A, H79A, F13A, C79A, F15A, H79C, O4A, C74A, C80A,
 H77B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(S2B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(C34B)=
 Sof(S3B)=Sof(F7B)=Sof(F8B)=Sof(F9B)=Sof(O7B)=Sof(O8B)=Sof(O9B)=Sof(C40B)=
 Sof(S5B)=Sof(F13B)=Sof(F14B)=Sof(F15B)=Sof(O13B)=Sof(O14B)=Sof(O15B)=Sof(C74B)=
 Sof(S6B)=Sof(F16B)=Sof(F17B)=Sof(F18B)=Sof(O16B)=Sof(O17B)=Sof(O18B)=Sof(C80B)=
 Sof(Si6B)=Sof(H77C)=Sof(H77D)=Sof(C78B)=Sof(H78D)=Sof(H78E)=Sof(H78F)=
 Sof(C79B)=Sof(H79D)=Sof(H79E)=Sof(H79F)=1-FVAR(1)
 Sof(S2A)=Sof(S3A)=Sof(S5A)=Sof(S6A)=Sof(Si6A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=
 Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=Sof(F17A)=
 Sof(F18A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(O13A)=
 Sof(O14A)=Sof(O15A)=Sof(O16A)=Sof(O17A)=Sof(O18A)=Sof(C34A)=Sof(C40A)=
 Sof(C74A)=Sof(H77A)=Sof(H77B)=Sof(C78A)=Sof(H78A)=Sof(H78B)=Sof(H78C)=
 Sof(C79A)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(C80A)=FVAR(1)
5.a Free rotating group:
 S2B(F4B,F5B,F6B,O4B,O5B,O6B,C34B), S3B(F7B,F8B,F9B,O7B,O8B,O9B,C40B),
 S5B(F13B,F14B,F15B,O13B,O14B,O15B,C74B), S6B(F16B,F17B,F18B,O16B,O17B,O18B,
 C80B)
5.b Ternary CH refined with riding coordinates:
 C1(H1), C41(H41)
5.c Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C77(H77C,H77D)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C18(H18), C19(H19), C20(H20), C34(H34), C44(H44), C45(H45), C46(H46), C47(H47),
  C51(H51), C52(H52), C53(H53), C54(H54), C58(H58), C59(H59), C60(H60), C61(H61)
5.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C78A(H78A,H78B,H78C),
 C78B(H78D,H78E,H78F), C79A(H79A,H79B,H79C), C79B(H79D,H79E,H79F)
;
_shelx_res_checksum              32156
_olex2_date_sample_data_collection 2021-11-04
_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 1.913
_oxdiff_exptl_absorpt_empirical_full_min 0.672