Crystallization and disorder of the polytypic α1and α2polymorphs of piroxicam
Upadhyay, Pratik P.; Bond, Andrew D.; CrystEngComm 17 (2015) 5266–; doi:10.1039/C5CE00050E

data_7219754
_publ_section_title
;
 Crystallization and disorder of the polytypic \a1and \a2polymorphs of
 piroxicam
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5266
_journal_paper_doi               10.1039/C5CE00050E
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H13 N3 O4 S'
_chemical_formula_sum            'C15 H13 N3 O4 S'
_chemical_formula_weight         331.34
_chemical_name_common            'Piroxicam: Form Alpha1'
_chemical_name_systematic        Piroxicam
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2b'
_space_group_name_H-M_alt        'P b c 21'
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-02-23 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3964(14)
_cell_length_b                   11.7965(10)
_cell_length_c                   6.9851(5)
_cell_measurement_reflns_used    2039
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      50.03
_cell_measurement_theta_min      2.54
_cell_volume                     1433.5(2)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.485
_diffrn_measured_fraction_theta_max 0.831
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.485
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3586
_diffrn_reflns_point_group_measured_fraction_full 0.364
_diffrn_reflns_point_group_measured_fraction_max 0.635
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         50.437
_diffrn_reflns_theta_min         7.639
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    2.250
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       needle
_exptl_crystal_F_000             688
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
Flack x determined using 190 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.11(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         949
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+2.1533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1213
_reflns_Friedel_coverage         0.373
_reflns_Friedel_fraction_full    0.219
_reflns_Friedel_fraction_max     0.389
_reflns_number_gt                743
_reflns_number_total             949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00050e4.cif
_cod_data_source_block           alpha1
_cod_depositor_comments
'Adding full bibliography for 7219754--7219755.cif.'
_cod_database_code               7219754
_shelx_estimated_absorpt_t_min   0.806
_shelx_estimated_absorpt_t_max   0.936
_shelxl_version_number           2013-4
_shelx_res_checksum              98619