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_7240988
_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_absolute_configuration rm
_chemical_formula_moiety         'C8 H9 N O2'
_chemical_formula_sum            'C8 H9 N O2'
_chemical_formula_weight         151.16
_chemical_name_systematic        '4-amino-2-methylbenzoic 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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.74940(14)
_cell_length_b                   8.12614(16)
_cell_length_c                   22.7285(4)
_cell_measurement_reflns_used    5388
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.5250
_cell_measurement_theta_min      6.0180
_cell_volume                     1431.28(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14d (Rigaku OD, 2018)'
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.971
_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    -54.00  30.00   1.00    1.00    --  -45.00  56.00  89.00   84
  2  \w    -46.00  -5.00   1.00    1.00    --  -45.00 -76.00 177.00   41
  3  \w   -129.00 -51.00   1.00    1.00    --  -45.00 -76.00 177.00   78
  4  \w   -151.00-123.00   1.00    1.00    -- -110.00 -56.00 -53.00   28
  5  \w   -195.00-157.00   1.00    1.00    -- -110.00 -56.00 -53.00   38
  6  \w   -149.00-123.00   1.00    1.00    -- -110.00 -76.00 177.00   26
  7  \w     30.00  55.00   1.00    1.00    --    5.00  57.00-180.00   25
  8  \w   -113.00 -78.00   1.00    1.00    -- -110.00 -57.00-120.00   35
  9  \w   -199.00 -99.00   1.00    1.00    -- -110.00 -38.00-150.00  100
 10  \w   -198.00 -69.00   1.00    1.00    -- -110.00 -38.00-120.00  129
 11  \w   -101.00 -57.00   1.00    1.00    -- -110.00  56.00  89.00   44
 12  \w   -132.00 -25.00   1.00    1.00    -- -110.00  76.00 -56.00  107
;
_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      -0.1296739000
_diffrn_orient_matrix_UB_12      0.0784076000
_diffrn_orient_matrix_UB_13      0.0430198000
_diffrn_orient_matrix_UB_21      0.1308660000
_diffrn_orient_matrix_UB_22      0.1373054000
_diffrn_orient_matrix_UB_23      0.0138704000
_diffrn_orient_matrix_UB_31      -0.0746999000
_diffrn_orient_matrix_UB_32      0.1047294000
_diffrn_orient_matrix_UB_33      -0.0504729000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6832
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.829
_diffrn_reflns_theta_min         6.033
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14d (Rigaku Oxford Diffraction, 2018)
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    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone'
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.159
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
;
 Flack x determined using 1138 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         2901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0418P)^2^+0.2167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                2813
_reflns_number_total             2901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00970a2.cif
_cod_data_source_block           s5326r
_cod_database_code               7240988
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.842
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
;
_shelx_res_checksum              40429
_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 1.179
_oxdiff_exptl_absorpt_empirical_full_min 0.826