Pharmaceutical cocrystals of the anti-tuberculosis drug pyrazinamide with dicarboxylic and tricarboxylic acids
Wang, Jian-Rong; Ye, Chanjuan; Zhu, Bingqing; Zhou, Chun; Mei, Xuefeng; CrystEngComm 17 (2015) 747–; doi:10.1039/C4CE02044H

data_7218809
_publ_section_title
;
 Pharmaceutical cocrystals of the anti-tuberculosis drug pyrazinamide with
 dicarboxylic and tricarboxylic acids
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              747
_journal_paper_doi               10.1039/C4CE02044H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C11 H13 N3 O8'
_chemical_formula_weight         315.24
_chemical_name_common            PZA-SEB
_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           SHELXL-97
_cell_angle_alpha                117.195(2)
_cell_angle_beta                 93.573(2)
_cell_angle_gamma                96.119(2)
_cell_formula_units_Z            2
_cell_length_a                   5.4495(2)
_cell_length_b                   11.7840(3)
_cell_length_c                   12.0250(4)
_cell_measurement_reflns_used    6169
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      54.87
_cell_measurement_theta_min      4.50
_cell_volume                     677.53(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9524
_diffrn_reflns_theta_full        24.72
_diffrn_reflns_theta_max         24.72
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.9749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             326
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.158
_refine_diff_density_min         -0.135
_refine_diff_density_rms         0.031
_refine_ls_extinction_coef       0.012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0361P)^2^+0.1545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                1764
_reflns_number_total             2307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02044h2.cif
_cod_data_source_block           F:\Paper\PZA\SEB\2013084.CIF
_cod_depositor_comments
'Adding full bibliography for 7218806--7218809.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7218809