Crystallization of para-aminobenzoic acid forms from specific solvents
Hussain, Mohammed Noorul; Van Meervelt, Luc; Van Gerven, Tom; CrystEngComm 26 (2024) 1647–1656; doi:10.1039/D3CE01055D

data_7248136
_publ_section_title
;
 Crystallization of para-aminobenzoic acid forms from specific solvents
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1647
_journal_page_last               1656
_journal_paper_doi               10.1039/D3CE01055D
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C3 H7 N O, C7 H7 N O2'
_chemical_formula_sum            'C10 H14 N2 O3'
_chemical_formula_weight         210.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-07-05 deposited with the CCDC.	2024-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.772(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1603(7)
_cell_length_b                   11.1181(8)
_cell_length_c                   11.9004(9)
_cell_measurement_reflns_used    4010
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9130
_cell_measurement_theta_min      2.9860
_cell_volume                     1133.22(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9631
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  25.00   1.00    5.00    --  -17.15 -99.00  90.00   45
  2  \w    -50.00  40.00   1.00    5.00    --   18.87 -57.00 -60.00   90
  3  \w    -50.00  40.00   1.00    5.00    --   18.87 -57.00-180.00   90
  4  \w    -51.00  49.00   1.00    5.00    --   18.87 -77.00  60.00  100
  5  \w    -87.00  13.00   1.00    5.00    --  -17.15 -77.00 -60.00  100
  6  \w    -20.00  10.00   1.00    5.00    --  -17.15 -99.00 150.00   30
  7  \w     -3.00  88.00   1.00    5.00    --   18.87  57.00  90.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0344677000
_diffrn_orient_matrix_UB_12      0.0391649000
_diffrn_orient_matrix_UB_13      -0.0305712000
_diffrn_orient_matrix_UB_21      -0.0201627000
_diffrn_orient_matrix_UB_22      0.0501505000
_diffrn_orient_matrix_UB_23      0.0283550000
_diffrn_orient_matrix_UB_31      0.0725418000
_diffrn_orient_matrix_UB_32      -0.0047044000
_diffrn_orient_matrix_UB_33      0.0482187000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            11747
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         2.433
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0717P)^2^+0.2611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1676
_reflns_number_total             2308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01055d2.cif
_cod_data_source_block           cit1001
_cod_depositor_comments          'Adding full bibliography for 7248136.cif.'
_cod_database_code               7248136
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C7 H6 N1 O2'
_chemical_oxdiff_usercomment     'PABA - DMF'
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.955
_diffrn_oxdiff_ac4_digest_frames
;
01fd32562cb657f2b4fc8b0e6c31a7d0400002732d2
;
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2A), C3(H3), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              22348
_olex2_submission_original_sample_id 'PABA + DMF'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.569
_oxdiff_exptl_absorpt_empirical_full_min 0.651