Constructing a solid-state supramolecular polymer based on host-guest recognition between perethylated pillar[5]arene and tetrathiafulvalene.
Zhao, Xueru; Hua, Bin; Shao, Li; Chemical communications (Cambridge, England) 60 (2024) 1164–1167; doi:10.1039/d3cc03579d

data_7132558
_publ_section_title
;
 Constructing a solid-state supramolecular polymer based on host-guest
 recognition between perethylated pillar[5]arene and tetrathiafulvalene.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1164
_journal_page_last               1167
_journal_paper_doi               10.1039/d3cc03579d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C6 H4 S4, C55 H70 O10'
_chemical_formula_sum            'C61 H74 O10 S4'
_chemical_formula_weight         1095.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-12-12 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.516(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.590(4)
_cell_length_b                   20.575(3)
_cell_length_c                   13.578(2)
_cell_measurement_reflns_used    2971
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      20.04
_cell_measurement_theta_min      2.49
_cell_volume                     5979.7(17)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.10-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_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      193.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS PHOTON 100'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13551
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        21.260
_diffrn_reflns_theta_max         21.260
_diffrn_reflns_theta_min         1.949
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0844 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.8220.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         3319
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.2097
_refine_ls_R_factor_gt           0.1555
_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^)+(0.3000P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4375
_refine_ls_wR_factor_ref         0.5004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1873
_reflns_number_total             3319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03579d2.cif
_cod_data_source_block           a
_cod_depositor_comments          'Adding full bibliography for 7132558.cif.'
_cod_original_cell_volume        5979.9(17)
_cod_database_code               7132558
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.973
_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
2. Restrained distances
 C28-C27 = C28A-C27A
 1.5 with sigma of 0.01
 C34-C33 = C30-C29 = C32-C31
 1.35 with sigma of 0.02
 S3-C33 = S4-C34 = S4-C32 = S3-C32 = S1-C31 = S2-C31 = S2-C30 = S1-C29
 1.75 with sigma of 0.02
 C29-S2 = C34-C32 = S1-C30
 2.6 with sigma of 0.04
 O5-C27 \\sim O5-C27A
 with sigma of 0.02
3. Restrained planarity
 S1, S2, S3, S4, C29, C30, C31, C32, C33, C34
 with sigma of 0.1
 S1A, S2A, S3A, S4A, C29A, C30A, C31A, C32A, C33A, C34A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O5 \\sim C27 \\sim C27A \\sim C28 \\sim C28A: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
S1 \\sim S2 \\sim S3 \\sim S4 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim S1A \\sim S2A \\sim S3A \\sim S4A \\sim C29A \\sim C30A \\sim
C31A \\sim C32A \\sim C33A \\sim C34A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
: with sigma of 0.03 and sigma for terminal atoms of 0.06
5. Same fragment restrains
{S1A, S2A, S3A, S4A, C29A, C30A, C31A, C32A, C33A, C34A} sigma for 1-2: 0.01,
1-3: 0.02
as in
{S1, S2, S3, S4, C29, C30, C31, C32, C33, C34}
6. Others
 Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
 Fixed Sof: S1(0.25) S2(0.25) S3(0.25) S4(0.25) C29(0.25) H29(0.25) C30(0.25)
 H30(0.25) C31(0.25) C32(0.25) C33(0.25) H33(0.25) C34(0.25) H34(0.25)
 S1A(0.25) S2A(0.25) S3A(0.25) S4A(0.25) C29A(0.25) H29A(0.25) C30A(0.25)
 H30A(0.25) C31A(0.25) C32A(0.25) C33A(0.25) H33A(0.25) C34A(0.25) H34A(0.25)
 H1A(0.5) H1B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B), C19(H19A,H19B),
 C21(H21A,H21B), C23(H23A,H23B), C27(H27A,H27B), C27A(H27C,H27D)
7.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C30(H30), C33(H33), C34(H34), C29A(H29A), C30A(H30A), C33A(H33A),
 C34A(H34A), C3(H3), C6(H6), C14(H14), C17(H17), C25(H25)
7.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C28(H28A,H28B,H28C), C28A(H28D,H28E,H28F)
;
_shelx_res_checksum              13061
_shelx_hkl_checksum              1893
_olex2_submission_special_instructions 'No special instructions were received'