(<i>R</i>)-2,3,4,5-Tetrahydro-2,2,4-trimethyl-1,5-benzothiazepine and <i>rac</i>-5-benzoyl-2,3,4,5-tetrahydro-2,2,4-trimethyl-1,5-benzothiazepine: chains built from N—H···S and C—H···π(arene) hydrogen bonds
Muthukumar, Manivannan; Thanikasalam, Kanagasabapathy; Mohamed, E. Mothi; Low, John N.; Glidewell, Christopher; Acta Crystallographica Section C 60 (2004) o346–o349; doi:10.1107/S0108270104006857

data_2014063
_publ_section_title
;
 (<i>R</i>)-2,3,4,5-Tetrahydro-2,2,4-trimethyl-1,5-benzothiazepine and
 <i>rac</i>-5-benzoyl-2,3,4,5-tetrahydro-2,2,4-trimethyl-1,5-benzothiazepine:
 chains built from N---H&#x00B7;&#x00B7;&#x00B7;S and
 C---H&#x00B7;&#x00B7;&#x00B7;\p(arene) hydrogen bonds
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o346
_journal_page_last               o349
_journal_paper_doi               10.1107/S0108270104006857
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C19 H21 N O S'
_chemical_formula_moiety         'C19 H21 N O S'
_chemical_formula_sum            'C19 H21 N O S'
_chemical_formula_weight         311.43
_chemical_name_systematic
;
rac-5-benzoyl-2,3,4,5-tetrahydro-2,2,4-trimethyl-1,5-benzothiazepine
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1757(2)
_cell_length_b                   12.5444(3)
_cell_length_c                   8.2147(2)
_cell_measurement_reflns_used    3762
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.00
_cell_volume                     1666.88(6)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'OSCAIL and SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'OSCAIL (McArdle, 2003) and SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19245
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.840
_refine_ls_abs_structure_details 'Flack (1983), 1719 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(9)
_refine_ls_extinction_coef       0.145(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3762
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.256
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+0.2569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                3605
_reflns_number_total             3762
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1712.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2014063
_cod_database_fobs_code          2014063