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_7250295
_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_absolute_configuration ad
_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             2024-12-13
_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                   7.2691(14)
_cell_length_b                   11.947(2)
_cell_length_c                   17.987(3)
_cell_measurement_reflns_used    2038
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9430
_cell_measurement_theta_min      3.3190
_cell_volume                     1562.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.864
_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     20.00  79.00   0.50    3.50    --   -9.80  22.00  51.00  118
  2  \w    -22.00  79.00   0.50    3.50    --   -9.80  55.00-150.00  202
  3  \w    -10.00  15.00   0.50    3.50    --   -9.80  55.00-180.00   50
  4  \w    -99.00 -52.00   0.50    3.50    --   -9.80  55.00-150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0293768000
_diffrn_orient_matrix_UB_12      0.0460121000
_diffrn_orient_matrix_UB_13      0.0219976000
_diffrn_orient_matrix_UB_21      0.0229283000
_diffrn_orient_matrix_UB_22      -0.0301208000
_diffrn_orient_matrix_UB_23      0.0326664000
_diffrn_orient_matrix_UB_31      0.0901987000
_diffrn_orient_matrix_UB_32      0.0224947000
_diffrn_orient_matrix_UB_33      -0.0011439000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8712
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.484
_diffrn_reflns_theta_min         2.046
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       needle
_exptl_crystal_F_000             824
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 1032 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0400
_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          0.1040
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.644
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.744
_reflns_number_gt                2919
_reflns_number_total             3530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00006h2.cif
_cod_data_source_block           jisuan
_cod_depositor_comments
'Adding full bibliography for 7250292--7250295.cif.'
_cod_original_cell_volume        1562.0(5)
_cod_database_code               7250295
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.73
_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 C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H4), C6(H10), C11(H17), C4(H7), C3(H5), C10(H15), C5(H8), 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:
 O3(H6), O4(H9), O8(H14), O1(H1), O7(H16)
;
_shelx_res_checksum              27945
_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 2.270
_oxdiff_exptl_absorpt_empirical_full_min 0.668