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_7240980
_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         'C8 H8 Cl N O3'
_chemical_formula_sum            'C8 H8 Cl N O3'
_chemical_formula_weight         201.60
_chemical_name_systematic        '4-amino-5-chloro-2-methoxybenzoic acid'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-15
_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                94.713(6)
_cell_angle_beta                 91.340(6)
_cell_angle_gamma                106.926(7)
_cell_formula_units_Z            4
_cell_length_a                   7.2780(6)
_cell_length_b                   7.5330(7)
_cell_length_c                   16.2004(11)
_cell_measurement_reflns_used    2223
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.0600
_cell_measurement_theta_min      3.9350
_cell_volume                     845.80(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1636
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.823
_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    -61.00  33.00   1.00    4.53    --   10.40 -57.00-120.00   94
  2  \w    -16.00  78.00   1.00    4.53    --   10.40  57.00  30.00   94
  3  \w    -74.00 -43.00   1.00    4.53    --   10.40 178.00   0.00   31
  4  \w    -23.00  45.00   1.00    4.53    --   10.40 -99.00 150.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0075528000
_diffrn_orient_matrix_UB_12      0.0920600000
_diffrn_orient_matrix_UB_13      0.0039107000
_diffrn_orient_matrix_UB_21      0.0987029000
_diffrn_orient_matrix_UB_22      0.0346767000
_diffrn_orient_matrix_UB_23      0.0129740000
_diffrn_orient_matrix_UB_31      0.0245775000
_diffrn_orient_matrix_UB_32      0.0096897000
_diffrn_orient_matrix_UB_33      -0.0418463000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7197
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.683
_diffrn_reflns_theta_min         3.612
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       plank
_exptl_crystal_F_000             416
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone'
_exptl_crystal_size_max          0.42044
_exptl_crystal_size_mid          0.14536
_exptl_crystal_size_min          0.06109
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0559
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2562
_reflns_number_total             3951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00970a2.cif
_cod_data_source_block           oacc35
_cod_database_code               7240980
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C8 O3 N1 Cl1 H8'
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.843
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Rotating group:
 N2(H2a), N1(H1a,H1b)
2.b Me refined with riding coordinates:
 C16(H16a,H16b,H16c), C17(H17a,H17b,H17c)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C10(H10), C1(H1), C4(H4)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6)
;
_shelx_res_checksum              1262
_olex2_date_sample_data_collection 2018-11-14
_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 1.117
_oxdiff_exptl_absorpt_empirical_full_min 0.893