Crystal-to-Crystal Solid-State Photochemistry: Absolute Asymmetric β-Thiolactam Synthesis from an Achiral α,β-Unsaturated Thioamide
Masami Sakamoto; Masaki Takahashi; Kenji Kamiya; Kentaro Yamaguchi; Tsutomu Fujita; Shoji Watanabe; Journal of the American Chemical Society 118 (1996) 10664–10665; doi:10.1021/ja961878m

data_4117196
_publ_section_title
;
 Crystal-to-Crystal Solid-State Photochemistry: Absolute Asymmetric
 \b-Thiolactam Synthesis from an Achiral \a,\b-Unsaturated Thioamide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10664
_journal_page_last               10665
_journal_paper_doi               10.1021/ja961878m
_journal_volume                  118
_journal_year                    1996
_chemical_formula_moiety         'C21 H23 N S '
_chemical_formula_sum            'C21 H23 N S'
_chemical_formula_weight         321.48
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             'Mon Feb  5 10:06:52 1996'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 100.15(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.760(2)
_cell_length_b                   10.262(3)
_cell_length_c                   10.238(3)
_cell_measurement_reflns_used    17
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      23.3
_cell_measurement_theta_min      19.7
_cell_volume                     905.9(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.10162
_diffrn_orient_matrix_UB_12      -0.03973
_diffrn_orient_matrix_UB_13      0.00991
_diffrn_orient_matrix_UB_21      -0.02223
_diffrn_orient_matrix_UB_22      -0.01926
_diffrn_orient_matrix_UB_23      -0.09725
_diffrn_orient_matrix_UB_31      0.05127
_diffrn_orient_matrix_UB_32      -0.08687
_diffrn_orient_matrix_UB_33      0.01702
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  4.73
_diffrn_reflns_av_sigmaI/netI    0.063
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3080
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.06
_diffrn_reflns_theta_min         4.31
_diffrn_standards_decay_%        -0.66
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.555
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             344.00
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   4.123
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2367
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0627
_refine_ls_shift/esd_max         0.2740
_refine_ls_shift/esd_mean        0.0400
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0571
_reflns_number_observed          2367
_reflns_number_total             1436
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ja961878m_1.cif
_cod_data_source_block           Kentax_Sakamoto_DIBENCYH_9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00000|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C21 H23 N S '
_cod_database_code               4117196