Photosensitized 2 + 2 Cycloaddition Reaction Using Homochirality Generated by Spontaneous Crystallization
Masami Sakamoto; Mamoru Kato; Yoko Aida; Kazuyuki Fujita; Takashi Mino; Tsutomu Fujita; Journal of the American Chemical Society 130 (2008) 1132–1133; doi:10.1021/ja077912m

data_4107356
_publ_contact_author_address
;
Department of Applied Chemistry and Biotechnology, Chiba University
;
_publ_contact_author_email       sakamotom@faculty.chiba-u.jp
_publ_contact_author_name        'Masami Sakamoto'
_publ_section_title
;
 Photosensitized 2 + 2 Cycloaddition Reaction Using Homochirality
 Generated by Spontaneous Crystallization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1132
_journal_page_last               1133
_journal_paper_doi               10.1021/ja077912m
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C16 H19 N O3'
_chemical_formula_weight         273.32
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   9.228(2)
_cell_length_b                   11.560(3)
_cell_length_c                   14.204(4)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.69
_cell_measurement_theta_min      28.13
_cell_volume                     1515.2(7)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_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      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0090
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1656
_diffrn_reflns_theta_full        70.02
_diffrn_reflns_theta_max         70.02
_diffrn_reflns_theta_min         4.93
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.8244
_exptl_absorpt_correction_T_min  0.8244
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       cube
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.9(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         1656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+0.0948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                1564
_reflns_number_total             1656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja077912m-file002.cif
_cod_data_source_block           coumarinamide_1a
_cod_original_cell_volume        1515.1(6)
_cod_database_code               4107356