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_1553671
_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         'C39 H54 N4 O3'
_chemical_formula_sum            'C39 H54 N4 O3'
_chemical_formula_weight         626.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-09-18 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                82.005(2)
_cell_angle_beta                 79.707(2)
_cell_angle_gamma                86.311(2)
_cell_formula_units_Z            4
_cell_length_a                   12.9272(4)
_cell_length_b                   13.0256(4)
_cell_length_c                   23.4928(6)
_cell_measurement_reflns_used    6262
_cell_measurement_temperature    293
_cell_measurement_theta_max      72.1550
_cell_measurement_theta_min      4.7570
_cell_volume                     3851.2(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_temperature      293
_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 0.980
_diffrn_measurement_details
;
  1 omega   23.00   89.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421 -125.0000 -150.0000 66

  2 omega   17.00  105.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   38.0000  150.0000 88

  3 omega   19.00  103.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   57.0000 -120.0000 84

  4 omega   19.00  103.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   57.0000    0.0000 84

  5 omega   14.00  103.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   69.0000  -87.0000 89

  6 omega  -33.00   55.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421  -38.0000  150.0000 88

  7 omega    1.00   75.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421  -99.0000   60.0000 74

  8 omega    1.00   75.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421  -99.0000  -90.0000 74

  9 omega   19.00  103.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   57.0000  -60.0000 84

 10 omega    9.00  104.00   1.0000    1.5700
omega____ theta____ kappa____ phi______ frames
    -       36.0421   77.0000   30.0000 95

 11 omega   40.00   98.00   1.0000    6.2700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 58

 12 omega   40.00   98.00   1.0000    6.2700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58

 13 omega   39.00  109.00   1.0000    6.2700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   60.0000 70

 14 omega   38.00   91.00   1.0000    6.2700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

 15 omega   40.00   65.00   1.0000    6.2700
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -60.0000 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      0.0976428000
_diffrn_orient_matrix_UB_12      -0.0084262000
_diffrn_orient_matrix_UB_13      -0.0477345000
_diffrn_orient_matrix_UB_21      -0.0518189000
_diffrn_orient_matrix_UB_22      -0.0849889000
_diffrn_orient_matrix_UB_23      -0.0235242000
_diffrn_orient_matrix_UB_31      -0.0497850000
_diffrn_orient_matrix_UB_32      0.0834573000
_diffrn_orient_matrix_UB_33      -0.0410333000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42357
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.330
_diffrn_reflns_theta_min         4.755
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55727
_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    1.081
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         14910
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0752
_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^)+(0.1430P)^2^+0.6100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2199
_refine_ls_wR_factor_ref         0.2383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11557
_reflns_number_total             14910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qm00097a2.cif
_cod_data_source_block           zxg-zxh
_cod_depositor_comments
;

2022-03-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        3851.16(19)
_cod_original_formula_moiety     '2(C39 H54 N4 O3)'
_cod_original_formula_sum        'C78 H108 N8 O6'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1253.72
_cod_database_code               1553671
_reflns_odcompleteness_completeness 61.36
_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 C(H,H,H) groups, All O(H) groups
2. Rigid bond restraints
 N009, C00Q
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C00F, C00N
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C00Q(H00A,H00B), C00R(H00C,H00D), C00Z(H00E,H00G), C010(H01A,H01B), C014(H01M,
 H01N), C019(H01C,H01D), C01A(H01O,H01P), C01D(H01R,H01S), C01E(H01G,H01H),
 C01J(H01T,H01U), C01O(H01X,H01Y), C01U(H0AA,H)
3.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00K(H00K), C00M(H00M), C00O(H00O), C00S(H00S), C00V(H00V),
 C012(H012), C017(H017), C01B(H01E), C01C(H01F), C01F(H01I), C01G(H01J),
 C01H(H01K), C01K(H01W), C01L(H01L), C01Q(H01Q), C01R(H01Z), C01S(H01),
 C01V(H01V), C01W(H1AA), C01X(H2AA), C01Z(H3AA), C025(H025), C028(H028)
3.c Idealised Me refined as rotating group:
 C020(H02Z,HA,HB), C021(H02A,H02B,H02C), C022(H02D,H02E,H02F), C024(H02,HC,HD),
  C026(H4AA,HE,HF), C027(H5AA,HG,HH), C029(H02G,H02H,H02I), C02A(H6AA,HI,HJ),
 C02B(H7AA,HK,HL), C02C(H8AA,HM,HN), C02D(H02J,H02K,H02L), C02E(H9AA,HO,HP),
 C02F(H02M,H02N,H02O), C02G(H02P,H02Q,H02R), C02H(H02S,H02T,H02U), C02I(H02V,
 H02W,H02X), C02J(H0BA,HQ,HR), C02K(H02Y,HS,HT)
3.d Idealised tetrahedral OH refined as rotating group:
 O001(H001), O002(H002), O003(H003), O004(H004), O006(H006), O007(H007)
;
_shelx_res_checksum              91628
_shelx_hkl_checksum              70507
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-06-23
_olex2_submission_special_instructions 'No special instructions were received'