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_7710920
_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         'C52 H104 Al2 Si10'
_chemical_formula_sum            'C52 H104 Al2 Si10'
_chemical_formula_weight         1064.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-13
_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                 98.7252(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.90519(19)
_cell_length_b                   10.80972(12)
_cell_length_c                   35.6601(5)
_cell_measurement_reflns_used    18886
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.1100
_cell_measurement_theta_min      4.2570
_cell_volume                     6822.14(14)
_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 1.000
_diffrn_measured_fraction_theta_max 0.984
_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    -48.00  -8.00   1.00    2.00    --  -38.50 125.00 -90.00   40
  2  \w    -84.00 -13.00   1.00    2.00    --  -38.50 -57.00 150.00   71
  3  \w    -62.00 -11.00   1.00    2.00    --  -38.50  57.00 -60.00   51
  4  \w     31.00  88.00   1.00    2.00    --   42.70-125.00  90.00   57
  5  \w     72.00 112.00   1.00    8.00    --  111.00-125.00-180.00   40
  6  \w     49.00 103.00   1.00    8.00    --  111.00 -94.00  60.00   54
  7  \w    106.00 165.00   1.00    8.00    --  111.00  61.00 150.00   59
  8  \w    106.00 169.00   1.00    8.00    --  111.00  77.00-180.00   63
  9  \w     91.00 178.00   1.00    8.00    --  111.00  30.00  90.00   87
 10  \w     45.00  99.00   1.00    8.00    --  111.00-125.00  60.00   54
 11  \w     43.00  83.00   1.00    8.00    --  111.00 -94.00-150.00   40
 12  \w     52.00 133.00   1.00    8.00    --  111.00 -45.00  30.00   81
 13  \w     38.00 104.00   1.00    8.00    --  111.00 -30.00-150.00   66
 14  \w    -85.00 -58.00   1.00    2.00    --  -38.50 125.00 -30.00   27
 15  \w    -41.00  -6.00   1.00    2.00    --  -38.50 125.00 -30.00   35
 16  \w    -93.00 -18.00   1.00    2.00    --  -38.50 -38.00  60.00   75
 17  \w    -69.00  23.00   1.00    2.00    --  -38.50  77.00-150.00   92
 18  \w    -36.00  33.00   1.00    2.00    --  -38.50  38.00 120.00   69
 19  \w     11.00  38.00   1.00    2.00    --   42.70  82.00 155.71   27
 20  \w     19.00  63.00   1.00    2.00    --   42.70  57.00-150.00   44
 21  \w     39.00  95.00   1.00    2.00    --   42.70  38.00 -60.00   56
 22  \w     12.00  41.00   1.00    2.00    --   42.70  79.00-116.02   29
 23  \w     24.00  55.00   1.00    2.00    --   42.70  38.00-180.00   31
 24  \w     15.00  93.00   1.00    2.00    --   42.70  70.00  39.09   78
 25  \w     12.00  37.00   1.00    2.00    --   42.70  79.00  80.67   25
 26  \w     13.00  38.00   1.00    2.00    --   42.70  77.00 122.49   25
 27  \w     11.00  36.00   1.00    2.00    --   42.70  82.00   7.05   25
 28  \w     25.00 110.00   1.00    2.00    --   42.70  57.00 -30.00   85
 29  \w     11.00  41.00   1.00    2.00    --   42.70  81.00 -72.91   30
 30  \w     65.00  92.00   1.00    2.00    --   42.70  38.00-180.00   27
 31  \w     69.00 108.00   1.00    2.00    --   42.70  57.00-150.00   39
 32  \w     89.00 156.00   1.00    8.00    --  111.00  45.00  60.00   67
 33  \w    146.00 174.00   1.00    8.00    --  111.00  71.00-163.02   28
 34  \w     83.00 159.00   1.00    8.00    --  111.00  69.00 -88.48   76
 35  \w     82.00 109.00   1.00    8.00    --  111.00  71.00-163.02   27
 36  \w     34.00  68.00   1.00    8.00    --  111.00 -94.00   0.00   34
 37  \w    119.00 144.00   1.00    8.00    --  111.00  61.00 -30.00   25
;
_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      -0.0050622000
_diffrn_orient_matrix_UB_12      0.0196797000
_diffrn_orient_matrix_UB_13      0.0423472000
_diffrn_orient_matrix_UB_21      -0.0281172000
_diffrn_orient_matrix_UB_22      0.1331934000
_diffrn_orient_matrix_UB_23      -0.0085975000
_diffrn_orient_matrix_UB_31      -0.0821691000
_diffrn_orient_matrix_UB_32      -0.0468050000
_diffrn_orient_matrix_UB_33      -0.0066895000
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            34270
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.520
_diffrn_reflns_theta_min         2.507
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.280
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.545
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_description       plate
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0454P)^2^+5.3838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6278
_reflns_number_total             7067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02118h2.cif
_cod_data_source_block           7
_cod_original_cell_volume        6822.13(14)
_cod_database_code               7710920
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C52H104Al2Si10
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.509
_diffrn_oxdiff_digest_frames
;
01f586d5eca4eef9fc87b774e949422ed601915de33
;
_diffrn_oxdiff_digest_hkl
;
0113146467252f3d164cb0b2dca8c9b9880ccb
;
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
;
_shelx_res_checksum              83377
_olex2_date_sample_data_collection 2020-08-13
_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 1.203
_oxdiff_exptl_absorpt_empirical_full_min 0.849