Can solvated intermediates inform us about nucleation pathways? The case of β-pABA
Cruz-Cabeza, A. J.; Taylor, E.; Sugden, I. J.; Bowskill, D. H.; Wright, S. E.; Abdullahi, H.; Tulegenov, D.; Sadiq, G.; Davey, R. J.; CrystEngComm  (2020) –; doi:10.1039/D0CE00970A

data_7240985
_publ_section_title
;
 Can solvated intermediates inform us about nucleation pathways? The case
 of \b-pABA
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00970A
_journal_year                    2020
_chemical_formula_moiety         'C7 H3 F4 N O2'
_chemical_formula_sum            'C7 H3 F4 N O2'
_chemical_formula_weight         209.10
_chemical_name_systematic        '4-amino-2,3,5,6-tetrafluorobenzoic acid'
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.566(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.1957(2)
_cell_length_b                   14.9867(6)
_cell_length_c                   11.5145(5)
_cell_measurement_reflns_used    4187
_cell_measurement_temperature    100.12(10)
_cell_measurement_theta_max      26.3070
_cell_measurement_theta_min      2.2390
_cell_volume                     717.72(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.12(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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    -81.00 -33.00   1.00    1.00    --    5.00 -12.00 -24.00   48
  2  \w    -28.00  -2.00   1.00    1.00    --    5.00 -12.00 -24.00   26
  3  \w      3.00  47.00   1.00    1.00    --    5.00 -12.00 -24.00   44
  4  \w    -26.00  94.00   1.00    1.00    --    5.00  57.00-180.00  120
  5  \w    -36.00  84.00   1.00    1.00    --   -5.70  57.00 -90.00  120
  6  \w      8.00  33.00   1.00    1.00    --   -5.70  76.00-150.00   25
  7  \w    -45.00 -13.00   1.00    1.00    --   -5.70  76.00-150.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0696133000
_diffrn_orient_matrix_UB_12      -0.0033135000
_diffrn_orient_matrix_UB_13      -0.0594206000
_diffrn_orient_matrix_UB_21      -0.1533078000
_diffrn_orient_matrix_UB_22      -0.0066865000
_diffrn_orient_matrix_UB_23      0.0181735000
_diffrn_orient_matrix_UB_31      -0.0268095000
_diffrn_orient_matrix_UB_32      0.0467350000
_diffrn_orient_matrix_UB_33      -0.0016010000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8394
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.345
_diffrn_reflns_theta_min         2.243
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_description       block
_exptl_crystal_F_000             416
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.483
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.1770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1306
_reflns_number_total             1458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00970a2.cif
_cod_data_source_block           s4880r
_cod_original_cell_volume        717.73(6)
_cod_database_code               7240985
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C6 H6 F6 O6'
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.880
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
;
_shelx_res_checksum              12961
_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 3.980
_oxdiff_exptl_absorpt_empirical_full_min 0.499