Crystal structure of 4-[(2-hydroxy-3-methoxybenzyl)amino]benzoic acid hemihydrate
Kamaal, Saima; Faizi, Md. Serajul Haque; Ali, Arif; Ahmad, Musheer; Gupta, Mayank; Dege, Necmi; Iskenderov, Turganbay; Acta Crystallographica Section E 75 (2019) 159–162; doi:10.1107/S2056989018018455

data_2242814
_publ_section_title
;
 Crystal structure of 4-[(2-hydroxy-3-methoxybenzyl)amino]benzoic acid
 hemihydrate
;
_journal_coeditor_code           LD2147
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              159
_journal_page_last               162
_journal_paper_doi               10.1107/S2056989018018455
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C15 H15 N O4, 0.5H2 O'
_chemical_formula_moiety         'C15 H15 N O4, 0.5(H2 O)'
_chemical_formula_sum            'C15 H16 N O4.5'
_chemical_formula_weight         282.28
_chemical_name_systematic
;
4-[(2-Hydroxy-3-methoxybenzyl)amino]benzoic acid hemihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 98.292(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.742(3)
_cell_length_b                   5.5002(6)
_cell_length_c                   19.387(2)
_cell_measurement_reflns_used    6409
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.50
_cell_volume                     2610.7(5)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16146
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.880
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       prism
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2570
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0366P)^2^+3.8398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1073
_reflns_number_gt                2138
_reflns_number_total             2570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ld2147sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-09-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2610.8(5)
_cod_original_formula_moiety     '2(C15 H15 N O4), H2 O'
_cod_original_formula_iupac      '2C15 H15 N O4, H2 O'
_cod_original_formula_sum        'C30 H32 N2 O9'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     564.57
_cod_database_code               2242814
_cod_database_fobs_code          2242814
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.979
_shelx_hkl_checksum              21988
_shelx_res_checksum              49012