Intermittent ultrasound-assisted anti-solvent crystallization for sucralose production with ultra-low aspect ratio and larger crystal size
Zhou, Dongyu; Li, Yongshang; Jie, Huimin; Lei, Jiayan; Chen, Zi'ang; Chen, Xiaoping; Cui, Can; Luo, Huadong; Chen, Jingjing; Li, Haohong; Zheng, Huidong; CrystEngComm 27 (2025) 3492–3501; doi:10.1039/D5CE00006H

data_7250294
_publ_section_title
;
 Intermittent ultrasound-assisted anti-solvent crystallization for
 sucralose production with ultra-low aspect ratio and larger crystal size
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              3492
_journal_page_last               3501
_journal_paper_doi               10.1039/D5CE00006H
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C12 H19 Cl3 O8'
_chemical_formula_sum            'C12 H19 Cl3 O8'
_chemical_formula_weight         397.62
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-12-26 deposited with the CCDC.	2025-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.041(4)
_cell_length_b                   7.3141(12)
_cell_length_c                   18.158(6)
_cell_measurement_reflns_used    679
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      17.99
_cell_measurement_theta_min      2.24
_cell_volume                     1599.2(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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_temperature      296.15
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1569
_diffrn_reflns_av_unetI/netI     0.1516
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9243
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.044
_diffrn_reflns_theta_max         25.044
_diffrn_reflns_theta_min         2.243
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6238
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0893 before and 0.0778 after correction.
The Ratio of minimum to maximum transmission is 0.8371.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       needle
_exptl_crystal_F_000             824
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 452 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.0572
_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          0.1279
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.707
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                1553
_reflns_number_total             2750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00006h2.cif
_cod_data_source_block           xinsuan
_cod_depositor_comments
'Adding full bibliography for 7250292--7250295.cif.'
_cod_original_cell_volume        1599.2(7)
_cod_database_code               7250294
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H17), C10(H15), C5(H8), C6(H10), C2(H4), C3(H5), C4(H7), C9(H13)
2.b Secondary CH2 refined with riding coordinates:
 C1(H3,H2), C7(H12,H11), C12(H18,H19)
2.c Idealised tetrahedral OH refined as rotating group:
 O7(H16), O8(H14), O1(H1), O4(H9), O3(H6)
;
_shelx_res_checksum              77546
_olex2_submission_special_instructions 'No special instructions were received'