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_7240979
_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_sum            'C10 H9 F4 N O3'
_chemical_formula_weight         267.18
_chemical_name_systematic
'4-amino-2,3,5,6-tetrafluorobenzoic acid acetone solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-03-18
_audit_creation_method           'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.754(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5218(10)
_cell_length_b                   17.636(2)
_cell_length_c                   10.0639(14)
_cell_measurement_reflns_used    1261
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      27.9050
_cell_measurement_theta_min      4.0420
_cell_volume                     1102.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.894
_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    -40.00  55.00   1.00    4.36    --  -17.77  37.00  90.00   95
  2  \w      0.00  36.00   1.00    4.36    --   18.86  77.00 -60.00   36
  3  \w    -87.00  12.00   1.00    4.36    --  -17.77 -77.00-180.00   99
  4  \w    -83.00   8.00   1.00    4.36    --  -17.77 -37.00 -90.00   91
  5  \w     32.00  60.00   1.00    4.36    --   18.86 -99.00  90.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0507241000
_diffrn_orient_matrix_UB_12      0.0113941000
_diffrn_orient_matrix_UB_13      0.0498604000
_diffrn_orient_matrix_UB_21      0.0914564000
_diffrn_orient_matrix_UB_22      0.0221637000
_diffrn_orient_matrix_UB_23      0.0346000000
_diffrn_orient_matrix_UB_31      -0.0458732000
_diffrn_orient_matrix_UB_32      0.0315694000
_diffrn_orient_matrix_UB_33      -0.0423483000
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3925
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.150
_diffrn_reflns_theta_min         3.320
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light white'
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone/Water'
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1014P)^2^+1.0432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.2030
_reflns_number_gt                978
_reflns_number_total             1363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00970a2.cif
_cod_data_source_block           s4436na
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               7240979
_oxdiff_exptl_absorpt_empirical_full_min 0.763
_oxdiff_exptl_absorpt_empirical_full_max 1.311
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              30088