Non-conjugated fluorescent molecular cages of salicylaldehyde-based tri-Schiff bases: AIE, enantiomers, mechanochromism, anion hosts/probes, and cell imaging properties
Zhang, Xiaohong; Shi, Jun; Shen, Guangyu; Gou, Fei; Cheng, Jinghui; Zhou, Xiangge; Xiang, Haifeng; Materials Chemistry Frontiers 1 (2017) 1041–; doi:10.1039/C7QM00097A

data_1553667
_publ_section_title
;
 Non-conjugated fluorescent molecular cages of salicylaldehyde-based
 tri-Schiff bases: AIE, enantiomers, mechanochromism, anion hosts/probes,
 and cell imaging properties
;
_journal_issue                   6
_journal_name_full               'Materials Chemistry Frontiers'
_journal_page_first              1041
_journal_paper_doi               10.1039/C7QM00097A
_journal_volume                  1
_journal_year                    2017
_chemical_formula_moiety         'C9 H8 Cl2 N1.33 O, C9 H7.78 Cl2 N1.33 O'
_chemical_formula_sum            'C18 H16 Cl4 N4 O2'
_chemical_formula_weight         462.15
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-18 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   14.7047(4)
_cell_length_b                   14.7047(4)
_cell_length_c                   23.9058(8)
_cell_measurement_reflns_used    5051
_cell_measurement_temperature    103(4)
_cell_measurement_theta_max      72.3940
_cell_measurement_theta_min      5.0740
_cell_volume                     4476.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      103(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -35.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -19.0000   60.0000 101

  2 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921   57.0000  -60.0000 84

  3 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921 -125.0000 -180.0000 67

  4 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921 -125.0000    0.0000 67

  5 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -57.0000    0.0000 84

  6 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -77.0000   90.0000 94

  7 omega   17.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921   38.0000 -120.0000 88

  8 omega   38.00  116.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 78

  9 omega   38.00   91.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

 10 omega   39.00  109.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  150.0000 70

 11 omega   38.00   91.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 53

 12 omega   40.00  135.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   60.0000 95

 13 omega   38.00   91.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

 14 omega   38.00   91.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 53

 15 omega   70.00  178.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 108

 16 omega   46.00  104.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 58

 17 omega   99.00  171.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 72

 18 omega   46.00  121.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -180.0000 75

 19 omega   38.00   68.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 30

 20 omega   45.00  115.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000    0.0000 70

 21 omega   91.00  116.00   1.0000    2.1900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000   45.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0798216000
_diffrn_orient_matrix_UB_12      0.0566787000
_diffrn_orient_matrix_UB_13      0.0473305000
_diffrn_orient_matrix_UB_21      -0.0349520000
_diffrn_orient_matrix_UB_22      0.0826967000
_diffrn_orient_matrix_UB_23      0.0033335000
_diffrn_orient_matrix_UB_31      -0.0838585000
_diffrn_orient_matrix_UB_32      -0.0677194000
_diffrn_orient_matrix_UB_33      0.0436214000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10167
_diffrn_reflns_point_group_measured_fraction_full 0.865
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        66.911
_diffrn_reflns_theta_max         66.911
_diffrn_reflns_theta_min         5.075
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 1189 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.360(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3102
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0700
_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^)+(0.1330P)^2^+20.4400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.1915
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_full    0.730
_reflns_Friedel_fraction_max     0.730
_reflns_number_gt                3063
_reflns_number_total             3102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qm00097a2.cif
_cod_data_source_block           zxg-zhx-3-100k
_cod_original_cell_volume        4476.6(3)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               1553667
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Others
 Sof(Cl)=1-FVAR(1)
 Sof(Cl04)=Sof(H00Q)=FVAR(1)
 Sof(Cl1)=1-FVAR(2)
 Sof(Cl02)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C00J(H00H,H00J), C00K(H00K,H00M), C00M(H00A,H00B), C00R(H00C,H00D)
3.b Aromatic/amide H refined with riding coordinates:
 C00A(H00E), C00C(H00F), C00E(H00G), C00I(H00I), C00L(H00L), C00Q(H00Q)
3.c Idealised tetrahedral OH refined as rotating group:
 O005(H005), O006(H006)
;
_shelx_res_checksum              68624
_shelx_hkl_checksum              24881
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-05-10
_olex2_submission_special_instructions 'No special instructions were received'