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_7710922
_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         'C46 H88 Al2 Si8'
_chemical_formula_sum            'C46 H88 Al2 Si8'
_chemical_formula_weight         919.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-09
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-04-01 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.3712(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.66217(18)
_cell_length_b                   15.35916(16)
_cell_length_c                   17.2597(2)
_cell_measurement_reflns_used    20173
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.3000
_cell_measurement_theta_min      3.9010
_cell_volume                     2966.23(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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      100.0(1)
_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 0.987
_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    -63.00  29.00   1.00    5.00    --  -38.50  57.00  90.00   92
  2  \w    -55.00  33.00   1.00    5.00    --  -38.50  38.00-180.00   88
  3  \w    -58.00  -6.00   1.00    5.00    --  -38.50 -19.00   0.00   52
  4  \w   -115.00 -87.00   1.00    5.00    --  -38.50 -19.00   0.00   28
  5  \w    -56.00 -17.00   1.00    5.00    --  -38.50  38.00  60.00   39
  6  \w    -16.00  11.00   1.00    5.00    --  -38.50  38.00  60.00   27
  7  \w     12.00  37.00   1.00    5.00    --   42.89  80.00  60.44   25
  8  \w     12.00  40.00   1.00    5.00    --   42.89  80.00-119.55   28
  9  \w     14.00 113.00   1.00    5.00    --   42.89  72.00  31.87   99
 10  \w    -19.00  73.00   1.00    5.00    --   42.89 -77.00 -90.00   92
 11  \w     38.00  77.00   1.00    5.00    --   42.89 -99.00-180.00   39
 12  \w     15.00  42.00   1.00    5.00    --   42.89  81.00 -61.59   27
 13  \w     22.00 110.00   1.00    5.00    --   42.89  38.00 150.00   88
 14  \w     13.00  40.00   1.00    5.00    --   42.89  82.00 101.56   27
 15  \w     12.00  42.00   1.00    5.00    --   42.89  80.00 154.68   30
 16  \w     19.00  95.00   1.00    5.00    --   42.89  57.00-150.00   76
 17  \w     33.00  74.00   1.00    5.00    --   42.89  57.00 -90.00   41
 18  \w     20.00  83.00   1.00    5.00    --   42.89  57.00 -30.00   63
 19  \w    115.00 167.00   1.00   12.50    --  111.00  67.00  41.71   52
 20  \w     83.00 112.00   1.00   12.50    --  111.00  67.00  41.71   29
 21  \w     84.00 177.00   1.00   12.50    --  111.00  65.00 139.83   93
 22  \w     85.00 112.00   1.00   12.50    --  111.00  62.00  97.97   27
 23  \w     85.00 178.00   1.00   12.50    --  111.00  61.00 -30.00   93
 24  \w     48.00 109.00   1.00   12.50    --  111.00-108.00 -83.20   61
 25  \w     31.00  82.00   1.00   12.50    --  111.00 -94.00   0.00   51
 26  \w     85.00 111.00   1.00   12.50    --  111.00  61.00-120.00   26
 27  \w    125.00 177.00   1.00   12.50    --  111.00  68.00-108.86   52
 28  \w     85.00 164.00   1.00   12.50    --  111.00  61.00 -60.00   79
 29  \w     36.00 105.00   1.00   12.50    --  111.00 -94.00 150.00   69
 30  \w     54.00 113.00   1.00   12.50    --  111.00-125.00   0.00   59
 31  \w     84.00 159.00   1.00   12.50    --  111.00  63.00  68.45   75
 32  \w     83.00 154.00   1.00   12.50    --  111.00  69.00 -46.14   71
 33  \w    127.00 176.00   1.00   12.50    --  111.00  69.00 160.90   49
 34  \w     83.00 109.00   1.00   12.50    --  111.00  69.00 160.90   26
 35  \w     83.00 109.00   1.00   12.50    --  111.00  68.00-108.86   26
 36  \w     83.00 109.00   1.00   12.50    --  111.00  68.00   7.97   26
 37  \w     86.00 111.00   1.00   12.50    --  111.00  61.00-150.00   25
 38  \w    123.00 150.00   1.00   12.50    --  111.00  61.00 120.00   27
 39  \w     83.00 110.00   1.00   12.50    --  111.00  68.00  77.74   27
 40  \w     88.00 142.00   1.00   12.50    --  111.00  48.00-144.54   54
 41  \w    147.00 174.00   1.00   12.50    --  111.00  61.00-150.00   27
 42  \w     85.00 121.00   1.00   12.50    --  111.00  61.00 -90.00   36
 43  \w     89.00 115.00   1.00   12.50    --  111.00  45.00-150.00   26
 44  \w     85.00 119.00   1.00   12.50    --  111.00  61.00 -72.60   34
 45  \w     85.00 111.00   1.00   12.50    --  111.00  61.00 120.00   26
 46  \w     85.00 113.00   1.00   12.50    --  111.00  61.00  30.00   28
 47  \w     89.00 116.00   1.00   12.50    --  111.00  45.00 150.00   27
 48  \w     42.00 132.00   1.00   12.50    --  111.00 -45.00 120.00   90
 49  \w     42.00  85.00   1.00   12.50    --  111.00-125.00 -30.00   43
 50  \w     85.00 114.00   1.00   12.50    --  111.00  61.00  60.00   29
 51  \w     88.00 116.00   1.00   12.50    --  111.00  48.00  -2.37   28
 52  \w     34.00 105.00   1.00   12.50    --  111.00 -94.00  90.00   71
 53  \w     85.00 112.00   1.00   12.50    --  111.00  61.00-180.00   27
 54  \w     86.00 178.00   1.00   12.50    --  111.00  63.00-133.77   92
;
_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      -0.0213784000
_diffrn_orient_matrix_UB_12      0.0674257000
_diffrn_orient_matrix_UB_13      0.0606400000
_diffrn_orient_matrix_UB_21      -0.0301702000
_diffrn_orient_matrix_UB_22      0.0693799000
_diffrn_orient_matrix_UB_23      -0.0671516000
_diffrn_orient_matrix_UB_31      -0.1325966000
_diffrn_orient_matrix_UB_32      -0.0264490000
_diffrn_orient_matrix_UB_33      -0.0216950000
_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  0.0889
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47794
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.473
_diffrn_reflns_theta_min         3.925
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.184
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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    1.030
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0671P)^2^+0.1079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5407
_reflns_number_total             6160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02118h2.cif
_cod_data_source_block           8
_cod_database_code               7710922
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C46H88Al2Si8
_shelx_estimated_absorpt_t_max   0.784
_shelx_estimated_absorpt_t_min   0.566
_diffrn_oxdiff_digest_frames
;
019e862db9bb3c7f38d79ef199d6a53eb9030247f2e
;
_diffrn_oxdiff_digest_hkl
;
010ba084dccac1a63508133daa16c5d310ae9e
;
_reflns_odcompleteness_completeness 99.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
;
_shelx_res_checksum              55379
_olex2_date_sample_data_collection 2020-06-29
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 5.548
_oxdiff_exptl_absorpt_empirical_full_min 0.404