Synthesis of Strained Pyridine-Containing Cyclyne via Reductive Aromatization
Koji Miki; Michiyasu Fujita; Yuki Inoue; Yoshinori Senda; Toshiyuki Kowada; Kouichi Ohe; Journal of Organic Chemistry 75 (2010) 3537–3540; doi:10.1021/jo1006202

data_4025438
_publ_contact_author_email       kojimiki@scl.kyoto-u.ac.jp
_publ_contact_author_fax         +81-75-383-2499
_publ_contact_author_name        'KOJI MIKI'
_publ_contact_author_phone       +81-75-383-2497
_publ_section_title
;
 Synthesis of Strained Pyridine-Containing Cyclyne via Reductive
 Aromatization
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3537
_journal_page_last               3540
_journal_paper_doi               10.1021/jo1006202
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C38 H54 N2 O6 '
_chemical_formula_sum            'C38 H54 N2 O6'
_chemical_formula_weight         634.85
_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'
_audit_creation_date             2009-07-08
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 103.023(13)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   9.590(9)
_cell_length_b                   10.948(9)
_cell_length_c                   15.807(14)
_cell_measurement_reflns_used    4443
_cell_measurement_temperature    143.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     1617(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12501
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             688.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     276
_refine_ls_number_reflns         1723
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.0007Fo^2^ + 1.0000\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                1705
_reflns_number_total             3631
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo1006202_si_003.cif
_cod_data_source_block           '__inoue007'
_cod_original_formula_sum        'C38 H54 N2 O6 '
_cod_database_code               4025438