Facile, Rapid, and High-Yield Synthesis of Pillar[5]arene from Commercially Available Reagents and Its X-ray Crystal Structure
Tomoki Ogoshi; Takamichi Aoki; Keisuke Kitajima; Shuhei Fujinami; Tada-aki Yamagishi; Yoshiaki Nakamoto; Journal of Organic Chemistry 76 (2011) 328–331; doi:10.1021/jo1020823

data_4025972
_publ_contact_author_address
;
    Graduate School of Natural Science and Technology,
Kanazawa University, Kakuma-machi, Kanazawa 920-1192,Japan
;
_publ_contact_author_email       ' ogoshi@t.kanazawa-u.ac.jp '
_publ_contact_author_fax         ' +81-76-234-4800 '
_publ_contact_author_name        ' Tomoki Ogoshi'
_publ_contact_author_phone       ' +81-76-234-4775 '
_publ_section_title
;
 Facile, Rapid, and High-Yield Synthesis of Pillar[5]arene from
 Commercially Available Reagents and Its X-ray Crystal Structure
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              328
_journal_page_last               331
_journal_paper_doi               10.1021/jo1020823
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C47 H54 O14'
_chemical_formula_weight         842.94
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                103.988(6)
_cell_angle_beta                 93.374(5)
_cell_angle_gamma                92.078(6)
_cell_formula_units_Z            2
_cell_length_a                   9.858(2)
_cell_length_b                   12.708(3)
_cell_length_c                   17.854(3)
_cell_measurement_reflns_used    9055
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2163.6(8)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      123.2
_diffrn_detector_area_resol_mean 14.46
_diffrn_measured_fraction_theta_full 0.9721
_diffrn_measured_fraction_theta_max 0.9721
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ?w
_diffrn_radiation_type           'Mo K?a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9661
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       Prism
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.65
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.704
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     530
_refine_ls_number_reflns         9096
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[?s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                5585
_reflns_number_total             9661
_reflns_threshold_expression     F^2^>2.0?s(F^2^)
_cod_data_source_file            jo1020823_si_002.cif
_cod_data_source_block           '_ogosi31'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C47 H54 O14 '
_cod_database_code               4025972