Nucleation control and separation of ethyl maltol polymorphs under different growth conditions through solution crystallization process in selected solvent environments
Thirumalaisamy, Anitha; Karuppannan, Srinivasan; CrystEngComm 26 (2024) 1902–1911; doi:10.1039/D3CE01154B

data_7248281
_publ_section_title
;
 Nucleation control and separation of ethyl maltol polymorphs under
 different growth conditions through solution crystallization process in
 selected solvent environments
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1902
_journal_page_last               1911
_journal_paper_doi               10.1039/D3CE01154B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C7 H8 O3'
_chemical_formula_sum            'C7 H8 O3'
_chemical_formula_weight         140.13
_chemical_name_common            'ETHYL MALTOL'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2bk3np
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-03-23 deposited with the CCDC.	2024-02-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   20.9615(11)
_cell_length_b                   20.9615(11)
_cell_length_c                   7.8858(5)
_cell_measurement_reflns_used    9651
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.82
_cell_volume                     3000.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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 0.996
_diffrn_measurement_device_type  'Bruker APEX-III  Photon Cmos Detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0056
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            57071
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.334
_diffrn_reflns_theta_min         2.816
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.9780
_exptl_absorpt_correction_T_min  0.9680
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1332
_exptl_crystal_recrystallization_method 'Solution Growth Method'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.030
_refine_ls_extinction_coef       0.0174(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0426P)^2^+1.9829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1389
_reflns_number_total             1496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01154b2.cif
_cod_data_source_block           Id1176r_a
_cod_depositor_comments
'Adding full bibliography for 7248281--7248283.cif.'
_cod_original_cell_volume        3000.7(4)
_cod_database_code               7248281
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              863