pH-Dependent Crystallization of 2-, 4-, 5-, and 6-Hydroxynicotinic Acids in Aqueous Media
Johnson, Aidan V.; Piedade, M. Fátima M.; Esteves, Catarina V.; Crystals 13 (2023) 1062–; doi:10.3390/cryst13071062

data_1569628
_publ_section_title
;
 pH-Dependent Crystallization of 2-, 4-, 5-, and 6-Hydroxynicotinic Acids
 in Aqueous Media
;
_journal_issue                   7
_journal_name_full               Crystals
_journal_page_first              1062
_journal_paper_doi               10.3390/cryst13071062
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C6  H5  Cl1  N1  O3'
_chemical_formula_sum            'C6 H6 Cl N O3'
_chemical_formula_weight         175.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 97.801(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.648(3)
_cell_length_b                   13.634(3)
_cell_length_c                   8.574(2)
_cell_measurement_reflns_used    4340
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      3.07
_cell_volume                     1464.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Mercury
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1262
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.928
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17885
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.491
_diffrn_reflns_theta_min         2.207
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5814
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.1619
_refine_ls_R_factor_gt           0.1045
_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^)+5.9795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1743
_reflns_number_total             2812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            new_4HNAPH02_ta.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1464.9(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1569628
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.833
_shelx_estimated_absorpt_t_max   0.911
_shelx_res_checksum              30113
_shelx_hkl_checksum              28541