Resolved structures of two picolinamide polymorphs. Investigation of the dimorphic system behaviour under conditions relevant to co-crystal synthesis
Évora, António O. L.; Castro, Ricardo A. E.; Maria, Teresa M. R.; Rosado, Mário T. S.; Silva, M. Ramos; Canotilho, João; Eusébio, M. Ermelinda S.; CrystEngComm 14 (2012) 8649–; doi:10.1039/c2ce26244d

data_7214680
_publ_section_title
;
 Resolved structures of two picolinamide polymorphs. Investigation of the
 dimorphic system behaviour under conditions relevant to co-crystal
 synthesis
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              8649
_journal_paper_doi               10.1039/c2ce26244d
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C6 H6 N2 O'
_chemical_formula_weight         122.13
_chemical_name_systematic
;
Picolinamide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.087(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   5.3463(2)
_cell_length_b                   11.3075(5)
_cell_length_c                   19.9400(10)
_cell_measurement_reflns_used    1595
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.34
_cell_measurement_theta_min      2.74
_cell_volume                     1193.45(9)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0509
_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       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13087
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.79
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.140
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0615P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1285
_reflns_number_gt                1192
_reflns_number_total             2287
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2ce26244d.txt
_cod_data_source_block           pico
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7214680