Synthesis of Cage-Shaped Aluminum Aryloxides: Efficient Lewis Acid Catalyst for Stereoselective Glycosylation Driven by Flexible Shift of Four- to Five-Coordination.
Tanaka, Daiki; Kadonaga, Yuichiro; Manabe, Yoshiyuki; Fukase, Koichi; Sasaya, Shota; Maruyama, Hikaru; Nishimura, Sota; Yanagihara, Mayu; Konishi, Akihito; Yasuda, Makoto; Journal of the American Chemical Society 141 (2019) 17466–17471; doi:10.1021/jacs.9b08875

data_4133707
_publ_section_title
;
 Synthesis of Cage-Shaped Aluminum Aryloxides: Efficient Lewis Acid
 Catalyst for Stereoselective Glycosylation Driven by Flexible Shift of
 Four- to Five-Coordination.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17466
_journal_page_last               17471
_journal_paper_doi               10.1021/jacs.9b08875
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C24 H17 Al Br3 N O3 Si'
_chemical_formula_sum            'C24 H17 Al Br3 N O3 Si'
_chemical_formula_weight         662.18
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 122.5250(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.71975(18)
_cell_length_b                   31.8436(6)
_cell_length_c                   9.22858(17)
_cell_measurement_reflns_used    40222
_cell_measurement_temperature    123
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      4.17
_cell_volume                     2408.36(8)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2.1'
_computing_publication_material  'CrystalStructure 4.2.1 (Rigaku, 2016)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            43350
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         5.398
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.287
_exptl_absorpt_correction_T_max  0.483
_exptl_absorpt_correction_T_min  0.369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1296.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.571
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4149
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    3.2016    1.2653    2.3733
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0377
_reflns_number_gt                4149
_reflns_number_total             4387
_reflns_threshold_expression     F>2.0\s(F)
_cod_data_source_file            1aAl_py.cif
_cod_data_source_block           SN160618
_cod_original_cell_volume        2408.35(8)
_cod_database_code               4133707