Dramatic Emission Enhancement of Aggregation-Induced Emission Luminogens by Dynamic Metal Coordination Bonds and Anti-Heavy-Atom Effect
Cai, Xuting; Xiong, Zuping; Zhan, Jiale; Ping, Xinni; Zhu, Yuqing; Zuo, Jiaqi; Feng, Hui; Qian, Zhaosheng; Chemical Communications  (2022) –; doi:10.1039/D2CC03809A

data_7130624
_publ_section_title
;
 Dramatic Emission Enhancement of Aggregation-Induced Emission Luminogens
 by Dynamic Metal Coordination Bonds and Anti-Heavy-Atom Effect
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03809A
_journal_year                    2022
_chemical_formula_moiety         'C56 H48 N4 O8 Zn2, 5(C2 H3 N)'
_chemical_formula_sum            'C66 H63 N9 O8 Zn2'
_chemical_formula_weight         1240.99
_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     dual
_audit_creation_date             2022-08-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-11 deposited with the CCDC.	2022-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                86.984(8)
_cell_angle_beta                 85.155(8)
_cell_angle_gamma                89.371(8)
_cell_formula_units_Z            1
_cell_length_a                   8.1837(18)
_cell_length_b                   13.428(3)
_cell_length_c                   15.086(4)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.92
_cell_volume                     1649.6(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker SMART APEX II diffractrometer'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.00
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48270
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.707
_diffrn_reflns_theta_min         2.741
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6532
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0922 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.8760.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       block
_exptl_crystal_F_000             646
_exptl_crystal_recrystallization_method
'The crystals were growth by means of evaporation of a mixture of n-hexane and toluene at RT.'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         8402
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+0.2688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6433
_reflns_number_total             8402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03809a2.cif
_cod_data_source_block           zn-96
_cod_original_cell_volume        1649.5(7)
_cod_database_code               7130624
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.885
_exptl_crystal_mounting_method
'The title complex was mounted in a sealed capillary.'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34-C33 = C34A-C33A
 1.43 with sigma of 0.01
 C32-C31 = C32A-C31A
 1.43 with sigma of 0.01
 N5-C33 = N5A-C33A
 1.1 with sigma of 0.01
 N5A-C34A = N5-C34
 2.53 with sigma of 0.02
 C34-C33 \\sim C34A-C33A
 with sigma of 0.02
 N5A-C33A \\sim N5-C33
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N5 \\sim C33 \\sim C34 \\sim N5A \\sim C33A \\sim C34A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C32A \\sim N4A \\sim C31A \\sim C32 \\sim N4 \\sim C31: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 N5A, C33A, C34A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4A, C31A, C32A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C33, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N5A)=Sof(C33A)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=0.5*(1-FVAR(2))
 Sof(N5)=Sof(C33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=0.5*FVAR(2)
 Sof(N4A)=Sof(C31A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(2)
 Sof(N4)=Sof(C31)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(2)
6.a Me refined with riding coordinates:
 C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F), C32A(H32D,H32E,H32F)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              34473
_shelx_hkl_checksum              98836
_olex2_submission_special_instructions 'No special instructions were received'