Molecular and crystal structure of 5,9-dimethyl-5<i>H</i>-pyrano[3,2-<i>c</i>:5,6-<i>c</i>']bis[2,1-benzothiazin]-7(9<i>H</i>)-one 6,6,8,8-tetroxide dimethylformamide monosolvate
Rybalka, Andrii; Shishkina, Svitlana; Ukrainets, Igor; Sidorenko, Lyudmila; Sim, Galina; Acta Crystallographica Section E 75 (2019) 1076–1078; doi:10.1107/S2056989019008788

data_2242997
_publ_section_title
;
 Molecular and crystal structure of
 5,9-dimethyl-5<i>H</i>-pyrano[3,2-<i>c</i>:5,6-<i>c</i>']bis[2,1-benzothiazin]-7(9<i>H</i>)-one
 6,6,8,8-tetroxide dimethylformamide monosolvate
;
_journal_coeditor_code           WM5508
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1076
_journal_page_last               1078
_journal_paper_doi               10.1107/S2056989019008788
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C19 H14 N2 O6 S2, C3 H7 N O'
_chemical_formula_moiety         'C19 H14 N2 O6 S2, C3 H7 N O'
_chemical_formula_sum            'C22 H21 N3 O7 S2'
_chemical_formula_weight         503.54
_chemical_name_systematic
'5,9-Dimethyl-5<i>H</i>-pyrano[3,2-<i>c</i>:5,6-<i>c</i>']bis[2,1-benzothiazin]-7(9<i>H</i>)-one 6,6,8,8-tetroxide dimethylformamide monosolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90.498(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2678(2)
_cell_length_b                   26.5667(7)
_cell_length_c                   11.3590(3)
_cell_measurement_reflns_used    8803
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.0720
_cell_measurement_theta_min      3.3310
_cell_volume                     2193.13(10)
_computing_cell_refinement
;
CrysAlis RED (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis CCD (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis RED (Agilent, 2012)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Agilent Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         3.195
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis RED</i>; Agilent, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         6370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0560P)^2^+0.5564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                5409
_reflns_number_total             6370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5508sup1.cif
_cod_data_source_block           I
_cod_database_code               2242997
_cod_database_fobs_code          2242997
_shelx_estimated_absorpt_t_min   0.943
_shelx_estimated_absorpt_t_max   0.949
_shelx_hkl_checksum              11098
_shelx_res_checksum              93123