Liquid–liquid phase separation and crystallization of aspirin polymorphs from a water–acetonitrile mixed solvent medium through a swift cooling process
Muthusamy, Ramya; Karuppannan, Srinivasan; CrystEngComm 25 (2023) 6611–6621; doi:10.1039/D3CE00611E

data_7247819
_publ_section_title
;
 Liquid--liquid phase separation and crystallization of aspirin polymorphs
 from a water--acetonitrile mixed solvent medium through a swift cooling
 process
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              6611
_journal_page_last               6621
_journal_paper_doi               10.1039/D3CE00611E
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C9 H8 04'
_chemical_formula_sum            'C9 H8 O4'
_chemical_formula_weight         180.15
_chemical_name_common            'Acetylsalicylic acid'
_chemical_name_systematic        2-acetoxybenzoicacid
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2bnj5q
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-04-06 deposited with the CCDC.	2023-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.750(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.429(4)
_cell_length_b                   6.597(2)
_cell_length_c                   11.395(4)
_cell_measurement_reflns_used    6570
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.47
_cell_measurement_theta_min      3.57
_cell_volume                     854.8(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-III CMOS Photon Detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1422
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            45382
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.442
_diffrn_reflns_theta_min         3.570
_diffrn_source                   'Sealed Microfocus Tube'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'B.H.Blessings,Acta CrystalograA,1995,51,33'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             376
_exptl_crystal_recrystallization_method 'Solution-state crystallization method'
_exptl_crystal_size_max          0.463
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.030
_exptl_transmission_factor_max   0.9970
_exptl_transmission_factor_min   0.9500
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0494P)^2^+0.2533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1245
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1141
_reflns_number_total             1946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00611e2.cif
_cod_data_source_block           ASAMONOP_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/current/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 
;
_cod_original_cell_volume        854.9(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7247819
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              23689