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_4117197
_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           78
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      78
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_audit_creation_date             'Fri Feb 16 16:46:43 1996'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.366(1)
_cell_length_b                   10.3659
_cell_length_c                   17.133(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      21.8
_cell_measurement_theta_min      19.4
_cell_volume                     1841.0(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      0.02686
_diffrn_orient_matrix_UB_12      -0.06761
_diffrn_orient_matrix_UB_13      -0.03832
_diffrn_orient_matrix_UB_21      -0.07612
_diffrn_orient_matrix_UB_22      -0.05374
_diffrn_orient_matrix_UB_23      0.01515
_diffrn_orient_matrix_UB_31      -0.05283
_diffrn_orient_matrix_UB_32      0.04297
_diffrn_orient_matrix_UB_33      -0.04133
_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  6.67
_diffrn_reflns_av_sigmaI/netI    0.075
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3226
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.05
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        -3.03
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       prismatic
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_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
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_refine_ls_extinction_coef       1.74(2)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian iso.'
_refine_ls_goodness_of_fit_obs   2.754
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     232
_refine_ls_number_reflns         1062
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0516
_refine_ls_shift/esd_max         5.2180
_refine_ls_shift/esd_mean        0.3010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00009|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0706
_reflns_number_observed          1062
_reflns_number_total             1440
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ja961878m_2.cif
_cod_data_source_block           Kentax_Sakamoto_96-02-15_C
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00009|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) + 0.00009|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 43 '
_cod_original_formula_sum        'C21 H23 N S '
_cod_database_code               4117197