Tetraphenylethene-based tetracationic dicyclophanes: synthesis, mechanochromic luminescence, and photochemical reactions.
Nian, Hao; Li, Aisen; Li, Yawen; Cheng, Lin; Wang, Ling; Xu, Weiqing; Cao, Liping; Chemical communications (Cambridge, England) 56 (2020) 3195–3198; doi:10.1039/d0cc00860e

data_7125977
_publ_section_title
;
 Tetraphenylethene-based tetracationic dicyclophanes: synthesis,
 mechanochromic luminescence, and photochemical reactions.
;
_journal_issue                   21
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3195
_journal_page_last               3198
_journal_paper_doi               10.1039/d0cc00860e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C54 H44 N8, 7.5(C H4 O), 4(Cl)'
_chemical_formula_sum            'C61.5 H74 Cl4 N8 O7.5'
_chemical_formula_weight         1187.08
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-08 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                78.553(5)
_cell_angle_beta                 73.274(4)
_cell_angle_gamma                75.000(5)
_cell_formula_units_Z            2
_cell_length_a                   11.8059(14)
_cell_length_b                   14.764(2)
_cell_length_c                   19.268(2)
_cell_measurement_reflns_used    9439
_cell_measurement_temperature    114(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.96
_cell_volume                     3078.7(6)
_computing_cell_refinement       'SAINT V8.38A (bruker, 2016)'
_computing_data_collection       'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (bruker, 2016)'
_computing_molecular_graphics    'Xshell v.6.3.1 (Bruker AXS Inc., 2016)'
_computing_publication_material  'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      114(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49040
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.056
_diffrn_reflns_theta_max         25.056
_diffrn_reflns_theta_min         2.228
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.6307
_exptl_absorpt_correction_T_min  0.5720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for 
absorption correction. The 
Ratio of minimum to maximum transmission is 
0.9069. The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       block
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0043(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         10847
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0725
_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^)+(0.0983P)^2^+2.6213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1814
_refine_ls_wR_factor_ref         0.2024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7281
_reflns_number_total             10847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00860e2.cif
_cod_data_source_block           1_a
_cod_depositor_comments
'Adding full bibliography for 7125976--7125977.cif.'
_cod_original_cell_volume        3078.7(7)
_cod_original_formula_sum        'C61.50 H74 Cl4 N8 O7.50'
_cod_database_code               7125977
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.970
_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. Restrained distances
 O3-C56
 1.406 with sigma of 0.005
 O3X-C56X
 1.406 with sigma of 0.005
 O1-C54 = O1X-C54X
 1.406 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O3 \\sim C56: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O3 \\sim C56 \\sim O3X \\sim C56X: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O1 \\sim C54 \\sim O1X \\sim C54X: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O3, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C56, O3X, C56X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C54, O1X, C54X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O3X)=Sof(H3X)=Sof(C56X)=Sof(H56D)=Sof(H56E)=Sof(H56F)=Sof(O1X)=Sof(H1X)=
 Sof(C54X)=Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(1)
 Sof(O1)=Sof(H1)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(O3)=Sof(H3A)=
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B), C38(H38A,H38B), C45(H45A,H45B)
6.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C23(H23),
  C24(H24), C26(H26), C27(H27), C30(H30), C31(H31), C33(H33), C34(H34),
 C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C43(H43), C44(H44), C46(H46),
  C47(H47), C48(H48), C50(H50), C51(H51), C53(H53)
6.c Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C59(H59A,H59B,H59C), C021(H02A,H02B,H02C), C56X(H56D,H56E,H56F),
 C54X(H54D,H54E,H54F)
6.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3A), O6(H6A), O5(H5), O4(H4A), O3X(H3X), O1X(H1X)
;
_shelx_res_checksum              13817
_shelx_fab_checksum              61138
_olex2_submission_special_instructions 'No special instructions were received'