Acid-Induced Molecular Folding and Unfolding of N-Methyl Aromatic Amide Bearing 2,6-Disubstituted Pyridines
Iwao Okamoto; Mayumi Nabeta; Yasuko Hayakawa; Nobuyoshi Morita; Tetsuya Takeya; Hyuma Masu; Isao Azumaya; Osamu Tamura; Journal of the American Chemical Society 129 (2007) 1892–1893; doi:10.1021/ja0682879

data_4109105
_publ_contact_author_address
;Showa Pharmaceutical University, 
3-3165 Higashi-Tamagawagakuen, Machida, Tokyo
194-8543, Japan
;
_publ_contact_author_email       iokamoto@ac.shoyaku.ac.jp
_publ_contact_author_fax         +81-42-721-1579
_publ_contact_author_name        'Iwao Okamoto'
_publ_contact_author_phone       +81-42-721-1579
_publ_section_title
;
 Acid-Induced Molecular Folding and Unfolding of N-Methyl Aromatic Amide
 Bearing 2,6-Disubstituted Pyridines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1892
_journal_page_last               1893
_journal_paper_doi               10.1021/ja0682879
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C33 H29 N9 O4'
_chemical_formula_weight         615.65
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   37.074(2)
_cell_length_b                   9.0221(5)
_cell_length_c                   9.3593(5)
_cell_measurement_reflns_used    1083
_cell_measurement_temperature    120
_cell_measurement_theta_max      20.87
_cell_measurement_theta_min      4.40
_cell_volume                     3130.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker ApexII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7600
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.90
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9991
_exptl_absorpt_correction_T_min  0.9911
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.8(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3379
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                2126
_reflns_number_total             3379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0682879si20061120_025750.cif
_cod_data_source_block           compound2(a0509121mas)
_cod_database_code               4109105