Racemic 9,10-dimethoxy-3-methyl-6-phenyl-7,7a-dihydrobenzo[<i>b</i>]benzo[4,5]isothiazolo[2,3-<i>d</i>][1,4]diazepine 12,12-dioxide
Bassin, Jatinder P.; Shah, Virender P.; Martin, Lee; Horton, Peter N.; Acta Crystallographica Section E 67 (2011) o684–o685; doi:10.1107/S1600536811004983

data_2229484
_publ_section_title
;
 Racemic
 9,10-dimethoxy-3-methyl-6-phenyl-7,7a-dihydrobenzo[<i>b</i>]benzo[4,5]isothiazolo[2,3-<i>d</i>][1,4]diazepine
 12,12-dioxide
;
_journal_coeditor_code           RK2256
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o684
_journal_page_last               o685
_journal_paper_doi               10.1107/S1600536811004983
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C24 H22 N2 O4 S'
_chemical_formula_moiety         'C24 H22 N2 O4 S'
_chemical_formula_sum            'C24 H22 N2 O4 S'
_chemical_formula_weight         434.51
_chemical_melting_point          498
_chemical_name_systematic
;
9,10-dimethoxy-3-methyl-6-phenyl-7,7a-
dihydrobenzo[<i>b</i>]benzo[4,5]isothiazolo[2,3-<i>d</i>][1,4]diazepine
12,12-dioxide
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                109.852(2)
_cell_angle_beta                 90.743(2)
_cell_angle_gamma                92.775(2)
_cell_formula_units_Z            4
_cell_length_a                   11.9007(4)
_cell_length_b                   12.8521(4)
_cell_length_c                   14.6202(5)
_cell_measurement_reflns_used    25443
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2099.76(12)
_computing_cell_refinement       '<i>DENZO</i> (Otwinowski & Minor, 1997)'
_computing_data_collection       '<i>COLLECT</i> (Hooft, 1998)'
_computing_data_reduction
;
<i>DENZO</i> (Otwinowski & Minor, 1997), <i>COLLECT</i> (Hooft,
1998) and
<i>maXus</i> (Mackay <i>et al.</i>, 1999)
;
_computing_molecular_graphics    '<i>CAMERON</i> (Watkin, <i>et al.</i>, 1993)'
_computing_publication_material  '<i>WinGX</i> (Farrugia, 1999)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f- and \w'
_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  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31054
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  0.9814
_exptl_absorpt_correction_T_min  0.9115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SORTAV</i>; Blessing, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.456
_refine_ls_extinction_coef       0.0053(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     '<i>SHELXL97</i> (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         7393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0595P)^2^+0.1891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                5463
_reflns_number_total             7393
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2256.cif
_cod_data_source_block           I
_cod_database_code               2229484
_cod_database_fobs_code          2229484