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_4109106
_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 H31 Cl2 N9 O12'
_chemical_formula_weight         816.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 115.715(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.40(2)
_cell_length_b                   9.105(8)
_cell_length_c                   16.398(15)
_cell_measurement_reflns_used    4744
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.40
_cell_volume                     3551(5)
_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      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_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  0.0969
_diffrn_reflns_av_sigmaI/netI    0.0857
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16897
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.27
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.9743
_exptl_absorpt_correction_T_min  0.9496
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0083(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3851
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1766
_refine_ls_R_factor_gt           0.1345
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1228P)^2^+44.3123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3470
_refine_ls_wR_factor_ref         0.3668
_reflns_number_gt                2251
_reflns_number_total             3851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0682879si20061120_025807.cif
_cod_data_source_block           compound2H(a0511082mas)
_cod_original_cell_volume        3552(6)
_cod_database_code               4109106