Molecular Design of Organic Superbases, Azacalix[3](2,6)pyridines: Catalysts for 1,2- and 1,4-Additions
Natsuko Uchida; Junpei Kuwabara; Ayako Taketoshi; Takaki Kanbara; Journal of Organic Chemistry 77 (2012) 10631–10637; doi:10.1021/jo3017428

data_4027752
_publ_contact_author_email       kanbara@ims.tsukuba.ac.jp
_publ_contact_author_fax         +81-29-853-4490
_publ_contact_author_name        'Takaki Kanbara'
_publ_contact_author_phone       +81-290853-5066
_publ_section_title
;
 Molecular Design of Organic Superbases, Azacalix[3](2,6)pyridines:
 Catalysts for 1,2- and 1,4-Additions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              10631
_journal_page_last               10637
_journal_paper_doi               10.1021/jo3017428
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C57 H69 Br Cl9 N9 O3'
_chemical_formula_sum            'C57 H69 Br Cl9 N9 O3'
_chemical_formula_weight         1327.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-22
_audit_creation_method           'by CrystalStructure 4.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.745(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.364(3)
_cell_length_b                   30.543(9)
_cell_length_c                   19.545(6)
_cell_measurement_reflns_used    3329
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.86
_cell_measurement_theta_min      2.23
_cell_volume                     6057(3)
_computing_cell_refinement       Unknown
_computing_data_collection       Unknown
_computing_data_reduction        Unknown
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Schneider, et al., 2002)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1305
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31777
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS V2008/1 (Bruker AXS)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       none
_exptl_crystal_F_000             2744.00
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.400
_refine_diff_density_min         -2.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     698
_refine_ls_number_reflns         13105
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.1979
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.5033
_reflns_number_gt                4405
_reflns_number_total             13105
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo3017428_si_002.cif
_cod_data_source_block           ucd701
_cod_database_code               4027752