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_7710915
_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         'C16 H8 F6 O6 S2'
_chemical_formula_sum            'C16 H8 F6 O6 S2'
_chemical_formula_weight         474.361
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-03
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-04-01 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                69.951(2)
_cell_angle_beta                 73.313(2)
_cell_angle_gamma                76.994(2)
_cell_formula_units_Z            1
_cell_length_a                   5.8009(2)
_cell_length_b                   8.5919(2)
_cell_length_c                   9.7054(2)
_cell_measurement_reflns_used    24062
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      36.5080
_cell_measurement_theta_min      2.2840
_cell_volume                     430.94(2)
_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 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9942
_diffrn_measured_fraction_theta_max 0.9600
_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    -35.00 107.00   1.00   10.00    --   35.84   0.00-150.00  142
  2  \w    -35.00 107.00   1.00   10.00    --   35.84   0.00  30.00  142
  3  \w    -15.00  76.00   1.00   10.00    --   35.84 -99.00  30.00   91
  4  \w     14.00 106.00   1.00   10.00    --   35.84  38.00-120.00   92
  5  \w     14.00 106.00   1.00   10.00    --   35.84  38.00  30.00   92
  6  \w      0.00  29.00   1.00   10.00    --   35.84  90.00 -68.83   29
  7  \w      3.00  32.00   1.00   10.00    --   35.84  85.00  91.82   29
  8  \w    -15.00  76.00   1.00   10.00    --   35.84 -99.00-150.00   91
  9  \w      2.00  31.00   1.00   10.00    --   35.84  86.00 156.62   29
 10  \w      5.00  42.00   1.00   10.00    --   35.84  81.00-173.16   37
 11  \w    -33.00  64.00   1.00   10.00    --   35.84 -77.00 -90.00   97
 12  \w    -33.00  64.00   1.00   10.00    --   35.84 -77.00  90.00   97
 13  \w      6.00  42.00   1.00   10.00    --   35.84  79.00  29.87   36
 14  \w     10.00 104.00   1.00   10.00    --   35.84  71.00 -88.62   94
 15  \w      5.00 108.00   1.00   10.00    --   35.84  24.00 132.47  103
 16  \w      1.00  30.00   1.00   10.00    --   35.84  88.00 -17.63   29
 17  \w     54.00 105.00   1.00   10.00    --   35.84 160.00 140.00   51
 18  \w     10.00  36.00   1.00   10.00    --   35.84  72.00 -96.69   26
 19  \w     39.00 110.00   1.00   10.00    --   35.84 178.00 -60.00   71
 20  \w     10.00  36.00   1.00   10.00    --   35.84  72.00  70.23   26
 21  \w     17.00 104.00   1.00   10.00    --   35.84  57.00   0.00   87
 22  \w     17.00 104.00   1.00   10.00    --   35.84  57.00 -90.00   87
 23  \w     17.00 104.00   1.00   10.00    --   35.84  57.00 120.00   87
 24  \w    -35.00 107.00   1.00   10.00    --   35.84   0.00-180.00  142
 25  \w    -35.00 107.00   1.00   10.00    --   35.84   0.00-150.00  142
 26  \w    -35.00 107.00   1.00   10.00    --   35.84   0.00-120.00  142
 27  \w    -35.00 107.00   1.00   10.00    --   35.84   0.00 -90.00  142
 28  \w    -35.00 107.00   1.00   10.00    --   35.84   0.00 -60.00  142
 29  \w      3.00  32.00   1.00   10.00    --   35.84  85.00 117.91   29
 30  \w    -35.00 107.00   1.00   10.00    --   35.84   0.00   0.00  142
 31  \w    -35.00  88.00   1.00   10.00    --   35.84   0.00  30.00  123
 32  \w    -35.00 107.00   1.00   10.00    --   35.84   0.00 -30.00  142
;
_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      -0.0023557000
_diffrn_orient_matrix_UB_12      -0.0496145000
_diffrn_orient_matrix_UB_13      -0.0447145000
_diffrn_orient_matrix_UB_21      -0.0157419000
_diffrn_orient_matrix_UB_22      -0.0701953000
_diffrn_orient_matrix_UB_23      0.0652869000
_diffrn_orient_matrix_UB_31      -0.1279460000
_diffrn_orient_matrix_UB_32      0.0221360000
_diffrn_orient_matrix_UB_33      0.0112695000
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.9942
_diffrn_reflns_Laue_measured_fraction_max 0.9600
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40075
_diffrn_reflns_point_group_measured_fraction_full 0.9942
_diffrn_reflns_point_group_measured_fraction_max 0.9600
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         36.92
_diffrn_reflns_theta_min         2.55
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.501
_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    1.828
_exptl_crystal_description       block
_exptl_crystal_F_000             238.364
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.4423
_refine_diff_density_min         -0.3936
_refine_diff_density_rms         0.0531
_refine_ls_d_res_high            0.5916
_refine_ls_d_res_low             7.9909
_refine_ls_goodness_of_fit_ref   1.1747
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1747
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+0.0247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0539
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              14
_reflns_limit_k_min              -13
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3936
_reflns_number_total             4198
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt02118h2.cif
_cod_data_source_block           A
_cod_database_code               7710915
_chemical_oxdiff_formula         C16H8F6O6S2
_olex2_refinement_description
;
;
_olex2_date_sample_data_collection 2021-11-01
_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 1.242
_oxdiff_exptl_absorpt_empirical_full_min 0.866