Dynamic covalent bond and metal coordination bond-cross-linked silicone elastomers with excellent mechanical and aggregation-induced emission properties
Wang, Ning; Feng, Hui-Wei; Hao, Xinhui; Cao, Yang; Xu, Xing-Dong; Feng, Shengyu; Polymer Chemistry 14 (2023) 1396–1403; doi:10.1039/D3PY00140G

data_1568546
_publ_section_title
;
 Dynamic covalent bond and metal coordination bond-cross-linked silicone
 elastomers with excellent mechanical and aggregation-induced emission
 properties
;
_journal_issue                   12
_journal_name_full               'Polymer Chemistry'
_journal_page_first              1396
_journal_page_last               1403
_journal_paper_doi               10.1039/D3PY00140G
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C66 H64 N4 O4'
_chemical_formula_sum            'C66 H64 N4 O4'
_chemical_formula_weight         977.21
_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
_audit_creation_date             2022-04-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-07-25 deposited with the CCDC.	2023-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                83.662(5)
_cell_angle_beta                 76.429(5)
_cell_angle_gamma                87.119(5)
_cell_formula_units_Z            2
_cell_length_a                   9.3439(11)
_cell_length_b                   17.753(2)
_cell_length_c                   18.6225(18)
_cell_measurement_reflns_used    7484
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      62.77
_cell_measurement_theta_min      2.51
_cell_volume                     2983.6(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35198
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        66.810
_diffrn_reflns_theta_max         66.810
_diffrn_reflns_theta_min         2.505
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.3182
_exptl_absorpt_correction_T_min  0.2023
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1059 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.6358.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.127
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0013(7)
_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   1.337
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         10432
_refine_ls_number_restraints     406
_refine_ls_restrained_S_all      1.409
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_gt           0.1073
_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          0.3326
_refine_ls_wR_factor_ref         0.3772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6095
_reflns_number_total             10432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py00140g2.cif
_cod_data_source_block           cu_220422c_0m_a
_cod_depositor_comments
'Adding full bibliography for 1568545--1568546.cif.'
_cod_original_cell_volume        2983.5(6)
_cod_database_code               1568546
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.969
_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, All O(H) groups
2. Restrained distances
 C1-C2 = C2-C3 = C3A-C2A = C2A-C1A
 1.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O1 \\sim O1A \\sim N3 \\sim C1 \\sim C1A \\sim C2 \\sim C2A \\sim C3 \\sim C3A
\\sim C4 \\sim C4A \\sim C5 \\sim C5A \\sim C6 \\sim C6A \\sim C7 \\sim C7A
\\sim C8 \\sim C8A \\sim C9 \\sim C9A \\sim C10 \\sim C10A \\sim C13 \\sim C24
\\sim C38 \\sim C52 \\sim C60 \\sim C66: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 1.7A
N2 \\sim C20 \\sim C32 \\sim C49 \\sim C55: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 1.7A
O3 \\sim C63 \\sim C44 \\sim C65 \\sim N4 \\sim C30 \\sim C51 \\sim C53: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
4. Others
 Fixed Sof: O1(0.5) H1(0.5) O1A(0.5) H1A(0.5) C1(0.5) H1B(0.5) H1C(0.5)
 H1D(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C2(0.5) H2A(0.5) C2A(0.5)
 H2AA(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5)
 H3AC(0.5) C4(0.5) H4A(0.5) C4A(0.5) H4AA(0.5) C7(0.5) H7(0.5) C8(0.5) C9(0.5)
 H9(0.5) C10(0.5) C5(0.5) C6(0.5) H6(0.5) C7A(0.5) H7A(0.5) C8A(0.5) C9A(0.5)
 H9A(0.5) C10A(0.5) H10A(0.5) C5A(0.5) C6A(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2A), C2A(H2AA), C20(H20), C30(H30), C41(H41)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4A), C4A(H4AA), C7(H7), C9(H9), C6(H6), C7A(H7A), C9A(H9A), C10A(H10A),
 C11(H11), C14(H14), C16(H16), C18(H18), C24(H24), C25(H25), C27(H27), C33(H33),
  C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43),
 C45(H45), C46(H46), C49(H49), C50(H50), C52(H52), C54(H54), C56(H56), C57(H57),
  C59(H59), C60(H60), C61(H61), C64(H64), C65(H65)
5.c Fitted hexagon refined as free rotating group:
 C7(C8,C9,C10,C5,C6), C7A(C8A,C9A,C10A,C5A,C6A)
5.d Tetrahedral OH refined with riding coordinates:
 O1(H1), O1A(H1A)
5.e Idealised Me refined as rotating group:
 C1(H1B,H1C,H1D), C1A(H1AA,H1AB,H1AC), C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC),
 C12(H12A,H12B,H12C), C32(H32A,H32B,H32C), C47(H47A,H47B,H47C), C51(H51A,H51B,
 H51C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C)
5.f Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3), O4(H4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19535
_shelx_fab_checksum              5964
_olex2_submission_special_instructions 'No special instructions were received'