A tetraphenylethene-based Pd<sub>2</sub>L<sub>4</sub> metallacage with aggregation-induced emission and stimuli-responsive behavior.
Li, Chenyang; Zhang, Beilin; Dong, Yunhong; Li, Yawen; Wang, Pinpin; Yu, Yang; Cheng, Lin; Cao, Liping; Dalton transactions (Cambridge, England : 2003) 49 (2020) 8051–8055; doi:10.1039/d0dt00469c

data_7704518
_publ_section_title
;
 A tetraphenylethene-based Pd<sub>2</sub>L<sub>4</sub> metallacage with
 aggregation-induced emission and stimuli-responsive behavior.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8051
_journal_page_last               8055
_journal_paper_doi               10.1039/d0dt00469c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C160 H104 N8 Pd2, 42(C3 H7 N O), 4(N O3)'
_chemical_formula_sum            'C286 H398 N54 O54 Pd2'
_chemical_formula_weight         5669.36
_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             2019-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-02 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                97.6580(10)
_cell_angle_beta                 95.1000(10)
_cell_angle_gamma                110.3330(10)
_cell_formula_units_Z            1
_cell_length_a                   15.7174(6)
_cell_length_b                   18.1192(6)
_cell_length_c                   18.6203(7)
_cell_measurement_reflns_used    9776
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.07
_cell_measurement_theta_min      2.81
_cell_volume                     4875.6(3)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            128455
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.358
_diffrn_reflns_theta_min         1.861
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  0.7028
_exptl_absorpt_correction_T_min  0.6119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for 
absorption correction. wR2(int) was 0.0742 
before and 0.0642 after correction. The 
Ratio of minimum to maximum transmission is 
0.8707. The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         17799
_refine_ls_number_restraints     938
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+2.3780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15713
_reflns_number_total             17799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00469c2.cif
_cod_data_source_block           1_b
_cod_depositor_comments
'Adding full bibliography for 7704518--7704519.cif.'
_cod_database_code               7704518
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.964
_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
 O5X-N6X
 1.234 with sigma of 0.02
 O6X-N6X = O4X-N6X
 1.245 with sigma of 0.02
 O5-N6
 1.234 with sigma of 0.02
 O4-N6 = O6-N6
 1.245 with sigma of 0.02
 O1-N5
 1.234 with sigma of 0.02
 O3-N5 = O2-N5
 1.245 with sigma of 0.02
 O2-N5 = O3-N5
 1.245 with sigma of 0.02
 O1X-N5X
 1.234 with sigma of 0.02
 O2X-N5X = O3X-N5X
 1.245 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N6 \\sim O4 \\sim O5 \\sim O6 \\sim N6X \\sim O4X \\sim O5X \\sim O6X: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N5 \\sim O1 \\sim O2 \\sim O3 \\sim N5X \\sim O1X \\sim O2X \\sim O3X: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N6, O4, O5, O6, N6X, O4X, O5X, O6X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, O1, O2, O3, N5X, O1X, O2X, O3X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C66, N3, N4, C39, C40, C41, C45, C38, H39, C36, H40, H41, C42, C44, H45, C37,
 H38, C35, C43, C46, H44, H37, C34, H43, C47, C31, C48, C30, C32, C49, C53, C29,
  H30, H32, C33, H49, C50, C52, H53, C28, H29, H33, H50, C51, H52, C27, C54,
 C11, C26, C55, C73, C10, C12, C19, C25, C56, C62, C68, C72, C9, H10, H12, C13,
 C14, C18, C20, C24, C57, C61, C63, C67, H68, C69, C71, H72, C8, H9, H13, H14,
 C15, C17, H18, H20, C21, C23, H24, H57, C58, C60, H61, H63, C64, H67, H69, C70,
  H71, C7, H15, C16, H17, H21, C22, H23, H58, C59, H60, H64, C65, H66, C74, C6,
 H16, H22, H59, H65, C75, C4, C76, C3, C5, C77, C80, C2, H3, N1, H5, H77, C78,
 N2, H80, C1, H2, H78, C79, H1, H79
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N6X)=Sof(O4X)=Sof(O5X)=Sof(O6X)=1-FVAR(1)
 Sof(N6)=Sof(O4)=Sof(O5)=Sof(O6)=FVAR(1)
 Sof(N5X)=Sof(O1X)=Sof(O2X)=Sof(O3X)=1-FVAR(2)
 Sof(N5)=Sof(O1)=Sof(O2)=Sof(O3)=FVAR(2)
6.a Free rotating group:
 N6X(O4X,O5X,O6X), N5X(O1X,O2X,O3X)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C29(H29), C30(H30), C32(H32), C33(H33), C37(H37),
 C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C49(H49),
  C50(H50), C52(H52), C53(H53), C57(H57), C58(H58), C59(H59), C60(H60),
 C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69),
  C71(H71), C72(H72), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81)
6.c Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C)
;
_shelx_res_checksum              80250
_shelx_fab_checksum              84942
_olex2_submission_special_instructions 'No special instructions were received'