The First in Situ Observation of Intramolecular Rotation and Cyclization of Anilide by an X-ray Study: Partial Single-Crystal to Single-Crystal Photocyclization of N-Methyl-N-{(E)-methylmethacryloyl}anilide in Inclusion Crystals
Hiroyuki Hosomi; Shigeru Ohba; Koichi Tanaka; Fumio Toda; Journal of the American Chemical Society 122 (2000) 1818–1819; doi:10.1021/ja992437g

data_4115935
_publ_contact_author_address
;
Department of Chemistry
Faculty of Science of Technology
Keio University
Hiyoshi 3-14-1, kohoku-ku
Yokohama 223-8522
Japan
;
_publ_contact_author_email       ohba@chem.keio.ac.jp
_publ_contact_author_fax         '(81) 45 563 5967'
_publ_contact_author_name        'Dr Shigeru Ohba'
_publ_contact_author_phone       '(81) 45 563 1141 ext 3912'
_publ_section_title
;
 The First in Situ Observation of Intramolecular Rotation and Cyclization
 of Anilide by an X-ray Study: Partial Single-Crystal to Single-Crystal
 Photocyclization of N-Methyl-N-{(E)-methylmethacryloyl}anilide in
 Inclusion Crystals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1818
_journal_page_last               1819
_journal_paper_doi               10.1021/ja992437g
_journal_volume                  122
_journal_year                    2000
_chemical_formula_moiety         'C33 H32 O4, C12 H15 N1 O1'
_chemical_formula_sum            'C45 H47 N O5'
_chemical_formula_weight         681.87
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_cell_angle_alpha                116.84(2)
_cell_angle_beta                 93.15(2)
_cell_angle_gamma                83.69(2)
_cell_formula_units_Z            1
_cell_length_a                   10.224(2)
_cell_length_b                   10.476(3)
_cell_length_c                   10.024(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      14.4
_cell_measurement_theta_min      12.3
_cell_volume                     952.2(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1993)
;
_computing_data_reduction
;TEXSAN
(Molecular Structure Corporation, 1998)
;
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \q-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4624
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       plate-like
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.17
_refine_ls_goodness_of_fit_ref   1.70
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     492
_refine_ls_number_reflns         4369
_refine_ls_R_factor_gt           0.068
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.172
_reflns_number_gt                2316
_reflns_number_total             4369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja992437g_1.cif
_cod_data_source_block           (I')
_cod_original_sg_symbol_H-M      'P 1 '
_cod_original_formula_sum        'C45 H47 N O5 '
_cod_database_code               4115935