Influence of degraded 1,4-dioxane on the formylation of para-aminobenzoic acid: a pathway to the reactive crystallization of para-formamidobenzoic acid
Mathew, Ansu; Karuppannan, Srinivasan; CrystEngComm 27 (2025) 7071–7080; doi:10.1039/D5CE00628G

data_7250899
_publ_section_title
;
 Influence of degraded 1,4-dioxane on the formylation of para-aminobenzoic
 acid: a pathway to the reactive crystallization of para-formamidobenzoic
 acid
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              7071
_journal_page_last               7080
_journal_paper_doi               10.1039/D5CE00628G
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C8 H7 N O3'
_chemical_formula_sum            'C8 H7 N O3'
_chemical_formula_weight         165.15
_chemical_melting_point          523
_chemical_name_common            pFBA
_chemical_name_systematic        '4 Formamidobenzoic acid'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2fhlk3
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-03-16 deposited with the CCDC.	2025-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.148(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0401(7)
_cell_length_b                   3.8577(4)
_cell_length_c                   11.7923(10)
_cell_measurement_reflns_used    3126
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.93
_cell_measurement_theta_min      3.46
_cell_volume                     365.75(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL AND ENCIFER'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-III CMOS PHOTON DECTECTOR'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5477
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.533
_diffrn_source                   'SEALED MICRO FOCUS TUBE'
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'R.H.Blessing,Acta Crystallogr.A 1995,51,33'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       Needle-like
_exptl_crystal_F_000             172
_exptl_crystal_recrystallization_method 'Reactive Crystallization'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   0.9990
_exptl_transmission_factor_min   0.9660
_refine_diff_density_max         0.153
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
;
 Flack x determined using 607 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(5)
_refine_ls_extinction_coef       0.055(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1555
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0355P)^2^+0.0613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                1404
_reflns_number_total             1555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00628g2.cif
_cod_data_source_block           M1_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7250899.cif.
;
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7250899
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              78199