Real-time fluorescence visualization of the evaporation crystallization process based on the AIEE mechanism
Gao, Lijie; Wang, Meng; Li, Shuyu; Chen, Kui; Zhou, Lina; Li, Xin; Wang, Na; Huang, Xin; Hao, Hongxun; Wang, Ting; CrystEngComm 25 (2023) 4064–4075; doi:10.1039/D3CE00232B

data_7246933
_publ_section_title
;
 Real-time fluorescence visualization of the evaporation crystallization
 process based on the AIEE mechanism
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              4064
_journal_page_last               4075
_journal_paper_doi               10.1039/D3CE00232B
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C10 H11 N O4'
_chemical_formula_sum            'C10 H11 N O4'
_chemical_formula_weight         209.20
_chemical_name_systematic        'Dimethyl 5-aminoisophthalate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-04 deposited with the CCDC.	2023-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.084(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5646(11)
_cell_length_b                   3.7993(5)
_cell_length_c                   13.5636(17)
_cell_measurement_reflns_used    2710
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      32.6000
_cell_measurement_theta_min      2.2910
_cell_volume                     473.59(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.933
_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   -115.00  65.00   2.00    2.00    --  -25.00  45.00   0.00   90
  2  \w   -115.00  45.00   2.00    2.00    --  -25.00  45.00  90.00   80
  3  \w   -115.00  25.00   2.00    2.00    --  -25.00  45.00 180.00   70
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku mm007 Saturn70'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2785
_diffrn_reflns_point_group_measured_fraction_full 0.559
_diffrn_reflns_point_group_measured_fraction_max 0.506
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.835
_diffrn_reflns_theta_min         2.331
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)'
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details
;
 Flack x determined using 348 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.9(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2785
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0637
_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^)+(0.1404P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1842
_reflns_Friedel_coverage         0.084
_reflns_Friedel_fraction_full    0.119
_reflns_Friedel_fraction_max     0.078
_reflns_number_gt                2361
_reflns_number_total             2785
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9695\% 
around [0.71 0.00 -0.71] (reciprocal) or [0.94 -0.00 -0.35] (direct)
;
_cod_data_source_file            d3ce00232b6.cif
_cod_data_source_block           r20220718a_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7246933--7246934.cif.'
_cod_database_code               7246933
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.973
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.588(3)
 0.412(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Rotating group:
 N1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              8875
_shelx_hkl_checksum              88501
_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
;