1-Allyl-4-hydroxy-2,2-dioxo-<i>N</i>-(4-methoxyphenyl)-1<i>H</i>-2λ^6^,1-benzothiazine-3-carboxamide: polymorphic transition due to grinding with the loss of the biological activity
Shishkina, Svitlana V.; Shaposhnyk, Anna M.; Baumer, Vyacheslav N.; Voloshchuk, Natali I.; Bondarenko, Pavlo S.; Ukrainets, Igor V.; Acta Crystallographica Section B 78 (2022) –; doi:10.1107/S2052520621013093

data_2108927
_publ_section_title
;
 1-Allyl-4-hydroxy-2,2-dioxo-<i>N</i>-(4-methoxyphenyl)-1<i>H</i>-2\l^6^,1-benzothiazine-3-carboxamide:
 polymorphic transition due to grinding with the loss of the biological
 activity
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520621013093
_journal_volume                  78
_journal_year                    2022
_chemical_formula_moiety         'C19 H18 N2 O5 S'
_chemical_formula_sum            'C19 H18 N2 O5 S'
_chemical_formula_weight         386.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                87.896(4)
_cell_angle_beta                 76.578(4)
_cell_angle_gamma                87.155(4)
_cell_formula_units_Z            2
_cell_length_a                   7.2868(4)
_cell_length_b                   10.6462(5)
_cell_length_c                   11.5637(6)
_cell_measurement_reflns_used    3561
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.029
_cell_measurement_theta_min      3.0191
_cell_volume                     871.20(8)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7062
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.025
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       stick
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0570
_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^)+(0.1296P)^2^+0.2789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.1802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2732
_reflns_number_total             3069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xk5087sup1.cif
_cod_data_source_block           1t
_cod_database_code               2108927
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.937
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              47703
_shelx_hkl_checksum              46382
_cod_database_fobs_code 2108927