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_7715248
_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 H82 Sn6, 4(C7 H8)'
_chemical_formula_sum            'C89 H114 Sn6'
_chemical_formula_weight         1895.94
_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             2022-05-04
_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                 97.566(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.3182(9)
_cell_length_b                   25.1639(5)
_cell_length_c                   25.1299(7)
_cell_measurement_reflns_used    26364
_cell_measurement_temperature    99.99(14)
_cell_measurement_theta_max      28.8630
_cell_measurement_theta_min      1.7600
_cell_volume                     17751.6(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (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      99.99(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -53.00 -25.00   1.00   44.00    --  -23.50  77.00 -90.00   28
  2  \w    -46.00  -6.00   1.00   44.00    --  -23.50 -57.00  90.00   40
  3  \w     -2.00  38.00   1.00   44.00    --   26.03  77.00 -30.00   40
  4  \w    -47.00  66.00   1.00   44.00    --   26.03 -19.00 -90.00  113
  5  \w     46.00  72.00   1.00   44.00    --   26.03 178.00-120.00   26
  6  \w     -1.00  33.00   1.00   44.00    --   26.03  77.00  30.00   34
  7  \w     -4.00  41.00   1.00   44.00    --   26.03  77.00 150.00   45
  8  \w      6.00  94.00   1.00   44.00    --   26.03  57.00  90.00   88
  9  \w     -2.00  34.00   1.00   44.00    --   26.03  77.00-150.00   36
 10  \w    -38.00  46.00   1.00   44.00    --   26.03 -57.00-150.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0242710000
_diffrn_orient_matrix_UB_12      -0.0072040000
_diffrn_orient_matrix_UB_13      -0.0066961000
_diffrn_orient_matrix_UB_21      -0.0018010000
_diffrn_orient_matrix_UB_22      -0.0043616000
_diffrn_orient_matrix_UB_23      0.0275485000
_diffrn_orient_matrix_UB_31      -0.0068007000
_diffrn_orient_matrix_UB_32      0.0268992000
_diffrn_orient_matrix_UB_33      0.0026700000
_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  0.0848
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            158656
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (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    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             7584
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.053
_refine_diff_density_max         2.245
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1753
_refine_ls_number_reflns         33709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0594P)^2^+107.8411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23036
_reflns_number_total             33709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00379a2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7715245--7715251.cif.'
_cod_database_code               7715248
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C89H114Sn6
_diffrn_oxdiff_digest_frames
;
018dd6cb9001ac729049c53fe3474b44bb00538dabb
;
_diffrn_oxdiff_digest_hkl
;
01aefe58a477ab4fbee0382395a888b96b5a9d
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_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.a Ternary CH refined with riding coordinates:
 C1(H1), C62(H62)
2.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B), C29(H29A,
 H29B), C30(H30A,H30B), C84(H84A,H84B), C85(H85A,H85B), C87(H87A,H87B),
 C88(H88A,H88B), C90(H90A,H90B), C91(H91A,H91B)
2.c Me refined with riding coordinates:
 C171(H17A,H17B,H17C), C157(H15A,H15B,H15C), C150(H15D,H15E,H15F), C129(H12J,
 H12K,H12L), C164(H16A,H16B,H16C), C136(H13A,H13B,H13C), C143(H14A,H14B,H14C),
 C178(H17D,H17E,H17F)
2.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C11(H11), C14(H14), C18(H18), C21(H21), C65(H65), C68(H68),
 C72(H72), C75(H75), C79(H79), C82(H82), C165(H165), C166(H166), C167(H167),
 C168(H168), C169(H169), C151(H151), C152(H152), C153(H153), C154(H154),
 C155(H155), C144(H144), C145(H145), C146(H146), C147(H147), C148(H148),
 C123(H123), C124(H124), C125(H125), C126(H126), C127(H127), C158(H158),
 C159(H159), C160(H160), C161(H161), C162(H162), C130(H130), C131(H131),
 C132(H132), C133(H133), C134(H134), C137(H137), C138(H138), C139(H139),
 C140(H140), C141(H141), C172(H172), C173(H173), C174(H174), C175(H175),
 C176(H176)
2.e 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), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C59(H59A,
 H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C86(H86A,H86B,H86C),
 C89(H89A,H89B,H89C), C92(H92A,H92B,H92C), C95(H95A,H95B,H95C), C96(H96A,H96B,
 H96C), C97(H97A,H97B,H97C), C100(H10A,H10B,H10C), C101(H10D,H10E,H10F),
 C102(H10G,H10H,H10I), C105(H10J,H10K,H10L), C106(H10M,H10N,H10O), C107(H10P,
 H10Q,H10R), C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I),
 C115(H11J,H11K,H11L), C116(H11M,H11N,H11O), C117(H11P,H11Q,H11R), C120(H12A,
 H12B,H12C), C121(H12D,H12E,H12F), C122(H12G,H12H,H12I)
;
_shelx_res_checksum              79854
_olex2_date_sample_data_collection 2022-05-03
_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 1.487
_oxdiff_exptl_absorpt_empirical_full_min 0.757