Two conformational polymorphs of 4-methylhippuric acid
Guillén, Marilia; Mora, Asiloé J.; Belandria, Lusbely M.; Seijas, Luis E.; Ramírez, Jeans W.; Burgos, José L.; Rincón, Luis; Delgado, Gerzon E.; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620013773

data_2108731
_publ_contact_author
;
Asiloe J. Mora
;
_publ_section_title
;
 Two conformational polymorphs of 4-methylhippuric acid
;
_journal_coeditor_code           AW5049SUP1
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620013773
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C10 H11 N O3'
_chemical_formula_moiety         'C10 H11 N O3'
_chemical_formula_sum            'C10 H11 N O3'
_chemical_formula_weight         193.20
_chemical_melting_point_gt       436
_chemical_melting_point_lt       438
_chemical_name_common            '4-Methylhippuric acid polymorph I'
_chemical_name_systematic        '2-[(4-Methylbenzoyl)amino]ethanoic acid'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-10-28 # Formatted by IUCr publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.1732(18)
_cell_length_b                   8.286(3)
_cell_length_c                   22.264(8)
_cell_measurement_reflns_used    770
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.107
_cell_measurement_theta_min      1.829
_cell_volume                     954.3(6)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_structure_refinement  'SHELXL2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean CCD
_diffrn_measured_fraction_theta_full 1.002
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 1.002
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6711
_diffrn_reflns_point_group_measured_fraction_full 1.001
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        19.107
_diffrn_reflns_theta_max         19.107
_diffrn_reflns_theta_min         1.829
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.117
_refine_diff_density_min         -0.105
_refine_diff_density_rms         0.025
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0599P)^2^+0.0172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.571
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                723
_reflns_number_total             770
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {1435ed5e-15b8-4ec0-a055-4741481d580f}
_cod_data_source_file            aw5049sup1.cif
_cod_data_source_block           4MHA-I
_cod_original_cell_volume        954.4(6)
_cod_database_code               2108731
_cod_database_fobs_code          2108731
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.960
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              8013
_shelx_hkl_checksum              5601