Crystal structure of a 2:1 co-crystal of meloxicam with acetylendicarboxylic acid
Tantardini, Christian; Arkhipov, Sergey G.; Cherkashina, Ksenya A.; Kil'met'ev, Alexander S.; Boldyreva, Elena V.; Acta Crystallographica Section E 72 (2016) 1856–1859; doi:10.1107/S2056989016018909

data_2241961
_publ_section_title
;
 Crystal structure of a 2:1 co-crystal of meloxicam with
 acetylendicarboxylic acid
;
_journal_coeditor_code           LH5829
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1856
_journal_page_last               1859
_journal_paper_doi               10.1107/S2056989016018909
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '2C14 H13 N3 O4 S2, C4 H2 O4'
_chemical_formula_moiety         '2C14 H13 N3 O4 S2, C4 H2 O4'
_chemical_formula_sum            'C32 H28 N6 O12 S4'
_chemical_formula_weight         816.84
_chemical_name_common            'Meloxicam acetylenedicarboxylic acid'
_chemical_name_systematic
'4-Hydroxy-2-methyl-<i>N</i>-(5-methyl-1,3-thiazol-2-yl)-2<i>H</i>-1,2-benzothiazine-3-carboxamide--2-butynedioic acid (2/1)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                75.839(3)
_cell_angle_beta                 79.196(3)
_cell_angle_gamma                70.100(3)
_cell_formula_units_Z            1
_cell_length_a                   7.3861(3)
_cell_length_b                   8.5629(3)
_cell_length_c                   15.1619(6)
_cell_measurement_reflns_used    4820
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.0330
_cell_measurement_theta_min      2.5810
_cell_volume                     868.55(6)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009) and
Mercury (Macrae <i>et al.</i>,  2008
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Agilent Xcalibur (Ruby, Gemini ultra)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.580
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       prism
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0463P)^2^+0.2383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                2940
_reflns_number_total             3564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5829sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C14 H13 N3 O4 S2, 0.5(C4 H2 O4)'
_cod_original_formula_iupac      'C14 H13 N3 O4 S2, 0.5C4 H2 O4'
_cod_original_formula_sum        'C16 H14 N3 O6 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     408.42
_cod_database_code               2241961
_cod_database_fobs_code          2241961
_shelx_hkl_checksum              76763
_shelx_res_checksum              80268