In Situ X-ray Observation of Pedal-like Conformational Change and Dimerization of trans-Cinnamamide in Cocrystals with Phthalic Acid
Shigeru Ohba; Hiroyuki Hosomi; Yoshikatsu Ito; Journal of the American Chemical Society 123 (2001) 6349–6352; doi:10.1021/ja0034287

data_4115596
_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) 45 566 1697'
_publ_contact_author_name        'Dr Shigeru Ohba'
_publ_contact_author_phone       '(81) 45 566 1704'
_publ_section_title
;
 In Situ X-ray Observation of Pedal-like Conformational Change and
 Dimerization of trans-Cinnamamide in Cocrystals with Phthalic Acid
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6349
_journal_page_last               6352
_journal_paper_doi               10.1021/ja0034287
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         'C8 H6 O4, (C9 H9 N1 O1)2'
_chemical_formula_sum            'C26 H24 N2 O6'
_chemical_formula_weight         460.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                90.82(2)
_cell_angle_beta                 105.72(2)
_cell_angle_gamma                75.51(2)
_cell_formula_units_Z            2
_cell_length_a                   9.562(3)
_cell_length_b                   17.401(4)
_cell_length_c                   7.523(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      14.5
_cell_volume                     1164.7(7)
_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, 1999)
;
_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  0.008
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5674
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5350
_refine_ls_R_factor_gt           0.041
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.1225P)^2^+0.0844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.181
_reflns_number_gt                3942
_reflns_number_total             5350
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0034287_2.cif
_cod_data_source_block           (I)
_cod_original_cell_volume        1164.7(6)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C26 H24 N2 O6 '
_cod_database_code               4115596