Synthesis of bi- and tetradentate poly-Lewis acids by hydroalumination of poly-alkynyl-anthracene derivatives
Mitzel, Norbert Werner; Aders, Niklas; Lamm, Jan-Hendrik; Beckmann, Jean Louis; Neumann, Beate; Stammler, Georg; Dalton Transactions  (2022) –; doi:10.1039/D2DT02118H

data_7710926
_publ_section_title
;
 Synthesis of bi- and tetradentate poly-Lewis acids by hydroalumination of
 poly-alkynyl-anthracene derivatives
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02118H
_journal_year                    2022
_chemical_formula_moiety         'C100 H184 Al4 N4 Si16, 10(C6 H6)'
_chemical_formula_sum            'C160 H244 Al4 N4 Si16'
_chemical_formula_weight         2780.94
_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             2022-06-20
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-06-21 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                111.110(2)
_cell_angle_beta                 103.729(2)
_cell_angle_gamma                96.176(2)
_cell_formula_units_Z            2
_cell_length_a                   15.7845(3)
_cell_length_b                   22.9127(5)
_cell_length_c                   26.7425(5)
_cell_measurement_reflns_used    52975
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.6070
_cell_measurement_theta_min      1.6960
_cell_volume                     8563.8(3)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.910
_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    -13.00  99.00   1.00   72.00    --   26.19  19.00 -30.00  112
  2  \w    -46.00  44.00   1.00   72.00    --   26.19 -38.00 150.00   90
  3  \w     17.00  79.00   1.00   72.00    --   26.19-118.00 -53.00   62
  4  \w     -4.00  42.00   1.00   72.00    --   26.19  77.00 150.00   46
  5  \w     -4.00  42.00   1.00   72.00    --   26.19  77.00   0.00   46
  6  \w    -21.00  44.00   1.00   72.00    --   26.19 -57.00   0.00   65
  7  \w      5.00  80.00   1.00   72.00    --   26.19  57.00  60.00   75
  8  \w     -4.00  34.00   1.00   72.00    --   26.19  77.00 -60.00   38
  9  \w      9.00  81.00   1.00   72.00    --   26.19  57.00-150.00   72
 10  \w    -12.00  68.00   1.00   72.00    --   26.19 -99.00 120.00   80
 11  \w      3.00  32.00   1.00   72.00    --   26.19  77.00  90.00   29
 12  \w    -47.00  92.00   1.00   72.00    --   26.19   0.00-150.00  139
;
_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      -0.0212578000
_diffrn_orient_matrix_UB_12      -0.0183266000
_diffrn_orient_matrix_UB_13      -0.0290394000
_diffrn_orient_matrix_UB_21      -0.0044463000
_diffrn_orient_matrix_UB_22      -0.0282975000
_diffrn_orient_matrix_UB_23      0.0051359000
_diffrn_orient_matrix_UB_31      -0.0420699000
_diffrn_orient_matrix_UB_32      0.0041086000
_diffrn_orient_matrix_UB_33      0.0041544000
_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  0.0443
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            179787
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.321
_diffrn_reflns_theta_min         1.532
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.481
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1705
_refine_ls_number_reflns         55632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+10.3055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                40002
_reflns_number_total             55632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02118h2.cif
_cod_data_source_block           anti-9xPyz2
_cod_database_code               7710926
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C157H184Al4N4Si16
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.878
_diffrn_oxdiff_digest_frames
;
01d30368ded648226537352b48e682f6d7008582449
;
_diffrn_oxdiff_digest_hkl
;
01b84260c3529fc2e8f0b8d7b274bf59c0ff4e
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C17(H17), C24(H24), C33(H33), C40(H40), C49(H49), C56(H56),
 C63(H63), C70(H70), C79(H79), C86(H86)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C31(H31), C32(H32), C51(H51), C52(H52), C53(H53), C58(H58), C59(H59), C60(H60),
  C61(H61), C62(H62), C77(H77), C78(H78), C93(H93), C94(H94), C95(H95),
 C96(H96), C97(H97), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105), C106(H106), C107(H107), C108(H108),
 C109(H109), C110(H110), C111(H111), C112(H112), C113(H113), C114(H114),
 C115(H115), C116(H116), C117(H117), C118(H118), C119(H119), C120(H120),
 C121(H121), C122(H122), C123(H123), C124(H124), C125(H125), C126(H126),
 C127(H127), C128(H128), C129(H129), C130(H130), C131(H131), C132(H132),
 C133(H133), C134(H134), C135(H135), C136(H136), C137(H137), C138(H138),
 C139(H139), C140(H140), C141(H141), C142(H142), C143(H143), C144(H144),
 C145(H145), C146(H146), C147(H147), C148(H148), C149(H149), C150(H150),
 C151(H151), C152(H152), C153(H153), C154(H154), C155(H155), C156(H156),
 C157(H157), C158(H158), C159(H159), C160(H160)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C64(H64A,H64B,H64C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,
 H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C),
 C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C80(H80A,H80B,
 H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,
 H84B,H84C), C85(H85A,H85B,H85C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C),
 C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,
 H92C)
;
_shelx_res_checksum              3396
_olex2_date_sample_data_collection 2022-06-15
_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 1.386
_oxdiff_exptl_absorpt_empirical_full_min 0.696