Manipulating AIE ligands into layers of pillar-layered MOFs for enhanced emission.
Chang, Manman; Li, Nan; Guo, Lingxiao; Zhang, Yijia; Liu, Xiao-Ting; Lu, Chao; Chemical communications (Cambridge, England) 60 (2024) 8696–8699; doi:10.1039/d4cc01831a

data_7133350
_publ_section_title
;
 Manipulating AIE ligands into layers of pillar-layered MOFs for enhanced
 emission.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8696
_journal_page_last               8699
_journal_paper_doi               10.1039/d4cc01831a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C128 H64 Cd6 N8 O32, 2(C1.5 H3.5 N0.5 O0.5), 4(C2 H8 N)'
_chemical_formula_sum            'C139 H103 Cd6 N13 O33'
_chemical_formula_weight         3157.74
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2024-03-29 deposited with the CCDC.	2024-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                80.911(3)
_cell_angle_beta                 84.233(3)
_cell_angle_gamma                61.359(3)
_cell_formula_units_Z            1
_cell_length_a                   12.2239(8)
_cell_length_b                   12.3893(7)
_cell_length_c                   30.5039(16)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.442
_cell_measurement_theta_min      4.098
_cell_volume                     4001.9(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      173.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            48131
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.685
_diffrn_reflns_theta_min         4.098
_exptl_absorpt_coefficient_mu    6.843
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1464 before and 0.0947 after correction. The Ratio of minimum to maximum transmission is 0.5845. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         9.027
_refine_diff_density_min         -3.159
_refine_diff_density_rms         0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.442
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         15521
_refine_ls_number_restraints     2669
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.1527
_refine_ls_R_factor_gt           0.1316
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3561
_refine_ls_wR_factor_ref         0.3808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11393
_reflns_number_total             15521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01831a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7133350--7133354.cif.'
_cod_database_code               7133350
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.494
_shelx_estimated_absorpt_t_min   0.427
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N6-C68 = N6-C69
 1.45 with sigma of 0.01
 N7-C70 = N7-C71 = N7-C71A
 1.45 with sigma of 0.01
 O17-C67
 1.25 with sigma of 0.01
 N5-C65 = N5-C66 = N5-C67
 1.45 with sigma of 0.01
 C71A-C71 \\sim C71-C70
 with sigma of 0.02
 C67-O17 \\sim C66-O17A
 with sigma of 0.02
 C66-O17 \\sim C67-O17A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C69) = Uanis(C68)
4. Others
 Sof(H7BC)=Sof(H7BD)=Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=1-FVAR(1)
 Sof(H7AA)=Sof(H7AB)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=FVAR(1)
 Fixed Sof: C65(0.5) H65A(0.5) H65B(0.5) H65C(0.5) C66(0.5) H66A(0.25)
 H66B(0.25) H66C(0.25) H66(0.25) C67(0.5) H67A(0.25) H67B(0.25) H67C(0.25)
 H67(0.25) N5(0.5) O17(0.25) O17A(0.25)
5.a Riding coordinates:
 C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C67(H67), C71(H71A,H71B,H71C),
 C71A(H71D,H71E,H71F)
5.b Secondary CH2 refined with riding coordinates:
 N7(H7AA,H7AB), N7(H7BC,H7BD), N6(H6A,H6B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C14(H14), C15(H15),
 C19(H19), C20(H20), C22(H22), C23(H23), C27(H27), C28(H28), C30(H30), C31(H31),
  C35(H35), C36(H36), C38(H38), C39(H39), C43(H43), C44(H44), C46(H46),
 C47(H47), C51(H51), C52(H52), C54(H54), C55(H55), C59(H59), C60(H60), C62(H62),
  C63(H63), C66(H66)
5.d Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C70(H70A,H70B,H70C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C)
;
_shelx_res_checksum              78542
_shelx_hkl_checksum              36550
_shelx_fab_checksum              57562
_olex2_submission_special_instructions 'No special instructions were received'