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_7716492
_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         'C37 H49 Cl3 Si3'
_chemical_formula_sum            'C37 H49 Cl3 Si3'
_chemical_formula_weight         684.38
_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             2021-07-20
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-04-02 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.3410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9108(2)
_cell_length_b                   17.1765(2)
_cell_length_c                   17.5544(2)
_cell_measurement_reflns_used    19724
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.3550
_cell_measurement_theta_min      3.4960
_cell_volume                     3771.60(9)
_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 1.000
_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   -110.00 -18.00   1.00    1.21    --  -38.50 -37.00 120.00   92
  2  \w   -103.00 -22.00   1.00    1.21    --  -38.50 -37.00-150.00   81
  3  \w   -107.00 -13.00   1.00    1.21    --  -38.50 -57.00  30.00   94
  4  \w    -59.00  -6.00   1.00    1.21    --  -38.50 125.00 -90.00   53
  5  \w     49.00  81.00   1.00    1.21    --   42.70-121.00 -70.00   32
  6  \w     64.00 114.00   1.00    1.21    --   42.70-152.00 129.00   50
  7  \w     41.00  91.00   1.00    4.81    --  111.00-121.00 -70.00   50
  8  \w     42.00 113.00   1.00    4.81    --  111.00-125.00  60.00   71
  9  \w    103.00 152.00   1.00    4.81    --  111.00  77.00 -60.00   49
 10  \w     85.00 176.00   1.00    4.81    --  111.00  61.00 -90.00   91
 11  \w    119.00 150.00   1.00    4.81    --  111.00 125.00-150.00   31
 12  \w     87.00 113.00   1.00    4.81    --  111.00-125.00 -90.00   26
 13  \w     43.00 137.00   1.00    4.81    --  111.00 -61.00 120.00   94
 14  \w     42.00  67.00   1.00    4.81    --  111.00-125.00   0.00   25
 15  \w     90.00 166.00   1.00    4.81    --  111.00  61.00-180.00   76
 16  \w     96.00 177.00   1.00    4.81    --  111.00  30.00-120.00   81
 17  \w     84.00 109.00   1.00    4.81    --  111.00-108.00 124.71   25
 18  \w     39.00  75.00   1.00    4.81    --  111.00-108.00 124.71   36
 19  \w     98.00 136.00   1.00    4.81    --  111.00 125.00 120.00   38
 20  \w     74.00 107.00   1.00    4.81    --  111.00 -94.00-180.00   33
 21  \w     84.00 113.00   1.00    4.81    --  111.00-125.00   0.00   29
 22  \w     74.00 113.00   1.00    4.81    --  111.00-125.00 -30.00   39
 23  \w     41.00 118.00   1.00    4.81    --  111.00 -45.00-120.00   77
 24  \w     41.00  83.00   1.00    4.81    --  111.00-125.00  90.00   42
 25  \w     63.00 108.00   1.00    4.81    --  111.00-106.00  82.62   45
 26  \w     75.00 113.00   1.00    4.81    --  111.00-125.00  30.00   38
 27  \w     37.00 108.00   1.00    4.81    --  111.00-105.00 139.39   71
;
_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      0.0616551000
_diffrn_orient_matrix_UB_12      0.0777076000
_diffrn_orient_matrix_UB_13      0.0105858000
_diffrn_orient_matrix_UB_21      0.1045276000
_diffrn_orient_matrix_UB_22      -0.0438327000
_diffrn_orient_matrix_UB_23      0.0366428000
_diffrn_orient_matrix_UB_31      0.0208406000
_diffrn_orient_matrix_UB_32      -0.0095008000
_diffrn_orient_matrix_UB_33      -0.0821652000
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34291
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.525
_diffrn_reflns_theta_min         3.533
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.287
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.855
_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    1.205
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0742P)^2^+2.5581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7061
_reflns_number_total             7822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01558d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7716492--7716494.cif.'
_cod_database_code               7716492
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C37 H49 Cl3 Si3'
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.589
_reflns_odcompleteness_completeness 99.96
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl3B) = Uanis(C36A)
Uanis(Cl2B) = Uanis(Cl2A)
Uanis(C31B) = Uanis(C31A)
Uanis(C32A) = Uanis(C32B)
Uanis(Si2B) = Uanis(Si2A)
3. Others
 Sof(Cl3B)=Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(Cl3A)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Sof(H30C)=Sof(H30D)=Sof(C32B)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(Cl2B)=
 Sof(Si2B)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(2)
 Sof(Cl2A)=Sof(Si2A)=Sof(H30A)=Sof(H30B)=Sof(C31A)=Sof(H31A)=Sof(H31B)=
 Sof(H31C)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C30(H30C,H30D), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B)
4.c 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), C21(H21)
4.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C31A(H31A,H31B,H31C), C32B(H32A,
 H32B,H32C), C36A(H36A,H36B,H36C), C36B(H36D,H36E,H36F), C37(H37A,H37B,H37C),
 C31B(H31D,H31E,H31F), C32A(H32D,H32E,H32F)
;
_shelx_res_checksum              85503
_olex2_date_sample_data_collection 2021-07-20
_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 1.139
_oxdiff_exptl_absorpt_empirical_full_min 0.898