1,4-Thiazepines, 1,4-Benzothiazepin-5-ones, and 1,4-Benzothioxepin Orthoamides via Multicomponent Reactions of Isocyanides
Stefano Marcaccini; Daniel Miguel; Tomás Torroba; María García-Valverde; Journal of Organic Chemistry 68 (2003) 3315–3318; doi:10.1021/jo026614z

data_4022318
_publ_section_title
;
 1,4-Thiazepines, 1,4-Benzothiazepin-5-ones, and 1,4-Benzothioxepin
 Orthoamides via Multicomponent Reactions of Isocyanides
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_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3315
_journal_page_last               3318
_journal_paper_doi               10.1021/jo026614z
_journal_volume                  68
_journal_year                    2003
_chemical_formula_sum            'C21 H29 N O4 S'
_chemical_formula_weight         391.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 98.457(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4558(16)
_cell_length_b                   18.361(3)
_cell_length_c                   10.7947(17)
_cell_measurement_temperature    299(2)
_cell_volume                     2049.8(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      299(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12972
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.733796
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0143(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         2952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.5210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                2584
_reflns_number_total             2952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo026614zsi20030127_013654.cif
_cod_data_source_block           c7pasm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4022318