Annular desmotropy of three pairs of seven-membered heterocycles confirmed by X-ray crystallography
Holczbauer, Tamás; Fábián, László; Csomós, Péter; Fodor, Lajos; Kálmán, Alajos; CrystEngComm 12 (2010) 1712–; doi:10.1039/b925635k

data_7212350
_publ_section_title
;
 Annular desmotropy of three pairs of seven-membered heterocycles
 confirmed by X-ray crystallography
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1712
_journal_paper_doi               10.1039/b925635k
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C20 H20 Cl N O4 S'
_chemical_formula_sum            'C20 H20 Cl N O4 S'
_chemical_formula_weight         405.88
_chemical_name_common
;
2-Ethoxycarbonyl-3-(4-chlorophenyl)-4,5-dihydro-7,8-dimethoxy-
1,4-benzothiazepine
;
_chemical_name_systematic
;
2-Ethoxycarbonyl-3-(4-chlorophenyl)-
4,5-dihydro-7,8-dimethoxy-1,4-benzothiazepine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 115.920(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2508(4)
_cell_length_b                   9.1719(3)
_cell_length_c                   14.8923(4)
_cell_measurement_reflns_used    7880
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      71.75
_cell_measurement_theta_min      6.60
_cell_volume                     1873.57(10)
_computing_cell_refinement       'CrystalClear v1.4.0 (Rigaku, 2008)'
_computing_data_collection       'CrystalClear v1.4.0 (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear v1.4.0 (Rigaku, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      98(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku R-axis RAPID'
_diffrn_measurement_method       '\w -scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12566
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         6.61
_exptl_absorpt_coefficient_mu    3.077
_exptl_absorpt_correction_T_max  0.8369
_exptl_absorpt_correction_T_min  0.4588
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear v1.4.0 (Rigaku, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+7.6759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.2473
_reflns_number_gt                1795
_reflns_number_total             3194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b925635k.txt
_cod_data_source_block           alap19
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7212350