Pertosylated pillar[5]arene: self-template assisted synthesis and supramolecular polymer formation.
Ruengsuk, Araya; Khamphaijun, Korawit; Pananusorn, Puttipong; Docker, Andrew; Tantirungrotechai, Jonggol; Sukwattanasinitt, Mongkol; Harding, David J.; Bunchuay, Thanthapatra; Chemical communications (Cambridge, England) 56 (2020) 8739–8742; doi:10.1039/d0cc04005c

data_7126782
_publ_section_title
;
 Pertosylated pillar[5]arene: self-template assisted synthesis and
 supramolecular polymer formation.
;
_journal_issue                   62
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8739
_journal_page_last               8742
_journal_paper_doi               10.1039/d0cc04005c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C125 H130 O40 S10'
_chemical_formula_sum            'C125 H130 O40 S10'
_chemical_formula_weight         2592.88
_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             2019-12-11
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2019.12.03 svn.r3bd4ad22 for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2020-06-08 deposited with the CCDC.	2020-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5402(2)
_cell_length_b                   22.7876(2)
_cell_length_c                   28.6846(2)
_cell_measurement_reflns_used    36102
_cell_measurement_temperature    199.97(13)
_cell_measurement_theta_max      68.3350
_cell_measurement_theta_min      2.8290
_cell_volume                     13943.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      199.97(13)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -107.00 -21.00   0.50    1.50    --  -40.91 152.00-121.00  172
  2  \w    -87.00  -3.00   0.50    1.50    --  -40.91 121.00  79.00  168
  3  \w     21.00 107.00   0.50    1.50    --   40.91-152.00-163.00  172
  4  \w      4.00  87.00   0.50    1.50    --   40.91-121.00  -3.00  166
  5  \w     60.00 157.00   0.50    6.00    --   96.59 152.00-121.00  194
  6  \w     33.00 109.00   0.50    6.00    --   96.59-121.00  -3.00  152
  7  \w     33.00 130.00   0.50    6.00    --   96.59-152.00-163.00  194
  8  \w     79.00 157.00   0.50    6.00    --   96.59 121.00  79.00  156
  9  \w   -104.00 -21.00   0.50    1.50    --  -40.91 -63.00  30.00  166
 10  \w     21.00 105.00   0.50    1.50    --   40.91  63.00 -60.00  168
 11  \w    -23.00  53.00   0.50    1.50    --   40.91 -37.00   0.00  152
 12  \w    -23.00  53.00   0.50    1.50    --   40.91 -37.00-180.00  152
 13  \w     19.00 114.00   0.50    1.50    --   40.91  12.00  30.00  190
 14  \w    -23.00  71.00   0.50    1.50    --   40.91 -91.00 120.00  188
 15  \w     34.00 110.00   0.50    6.00    --   96.59 -42.00 -30.00  152
 16  \w     84.00 157.00   0.50    6.00    --   96.59  96.00 -60.00  146
 17  \w     32.00 109.00   0.50    6.00    --   96.59-117.00  30.00  154
 18  \w     33.00 118.00   0.50    6.00    --   96.59 -68.00 -30.00  170
 19  \w     27.00 105.00   0.50    6.00    --   96.59 -96.00   0.00  156
 20  \w     88.00 157.00   0.50    6.00    --   96.59  25.00-150.00  138
 21  \w     32.00 109.00   0.50    6.00    --   96.59-117.00-180.00  154
 22  \w     83.00 157.00   0.50    6.00    --   96.59  77.00 120.00  148
 23  \w     78.00 152.00   0.50    6.00    --   96.59  59.00  60.00  148
 24  \w     81.00 133.00   0.50    6.00    --   96.59  50.00   0.00  104
 25  \w     45.00 122.00   0.50    6.00    --   96.59 -77.00 150.00  154
 26  \w     33.00 110.00   0.50    6.00    --   96.59 -17.00 -60.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            55553
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.451
_diffrn_reflns_theta_min         2.837
_exptl_absorpt_coefficient_mu    2.099
_exptl_absorpt_correction_T_max  0.641
_exptl_absorpt_correction_T_min  0.448
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             5440
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.466
_exptl_crystal_size_min          0.317
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         12743
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0744
_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^)+(0.1634P)^2^+12.9976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2371
_refine_ls_wR_factor_ref         0.2434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11267
_reflns_number_total             12743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04005c2.cif
_cod_data_source_block           tbmu-1-200k
_cod_depositor_comments
'Adding full bibliography for 7126782--7126783.cif.'
_cod_database_code               7126782
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.556
_shelx_estimated_absorpt_t_min   0.361
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19-C20 \\sim C19-C20A
 with sigma of 0.02
 C23A-C27A \\sim C23B-C27B
 with sigma of 0.04
 C20-O2A \\sim C20A-O2B
 with sigma of 0.02
 S1A-O2A \\sim S1B-O2B
 with sigma of 0.02
 S1A-O3A \\sim S1B-O3B
 with sigma of 0.02
 O3A-C21A \\sim O3B-C21B
 with sigma of 0.04
 S1A-O4A \\sim S1B-O4B
 with sigma of 0.02
 C21A-C25A \\sim C21B-C25B
 with sigma of 0.04
 S1A-C21A \\sim S1B-C21B
 with sigma of 0.02
 O2A-O4A \\sim O2B-O4B
 with sigma of 0.04
 C21A-C26A \\sim C21B-C26B
 with sigma of 0.02
 C22A-C24A \\sim C22B-C24B
 with sigma of 0.04
 C22A-C23A \\sim C22B-C23B
 with sigma of 0.02
 C23A-C24A \\sim C23B-C24B
 with sigma of 0.02
 C21A-C22A \\sim C21B-C22B
 with sigma of 0.02
 C24A-C25A \\sim C24B-C25B
 with sigma of 0.02
 O2A-C21A \\sim O2B-C21B
 with sigma of 0.04
 O3A-O4A \\sim O3B-O4B
 with sigma of 0.04
 C25A-C26A \\sim C25B-C26B
 with sigma of 0.02
 O4A-C21A \\sim O4B-C21B
 with sigma of 0.04
 C21A-C23A \\sim C21B-C23B
 with sigma of 0.04
 C22A-C26A \\sim C22B-C26B
 with sigma of 0.04
 C19-O2A \\sim C19-O2B
 with sigma of 0.04
 C20-S1A \\sim C20A-S1B
 with sigma of 0.04
 C23A-C25A \\sim C23B-C25B
 with sigma of 0.04
 C24A-C26A \\sim C24B-C26B
 with sigma of 0.04
 S1A-C22A \\sim S1B-C22B
 with sigma of 0.04
 S1A-C26A \\sim S1B-C26B
 with sigma of 0.04
 C25A-C27A \\sim C25B-C27B
 with sigma of 0.04
 C24A-C27A \\sim C24B-C27B
 with sigma of 0.02
 O2A-O3A \\sim O2B-O3B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C20) = Uanis(C20A)
4. Rigid body (RIGU) restrains
 C21A, C26A, C25A, C24A, C23A, C22A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C19, C20, S1A, O2A, O3A, O4A, C21A, C22A, C23A, C24A, C25A, C26A, C27A, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C20A, S1B, O2B, O3B, O4B, C21B, C22B, C23B, C24B, C25B, C26B, C27B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H19A)=Sof(H19B)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(S1B)=Sof(O2B)=Sof(O3B)=
 Sof(O4B)=Sof(C21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(C25B)=
 Sof(H25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(H19C)=Sof(H19D)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(S1A)=Sof(O2A)=Sof(O3A)=
 Sof(O4A)=Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(C25A)=
 Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
 Fixed Sof: H1A(0.5) H1B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C19(H19C,H19D), C19(H19A,H19B),
 C20(H20A,H20B), C28(H28A,H28B), C29(H29A,H29B), C36(H36A,H36B), C37(H37A,H37B),
  C45(H45A,H45B), C46(H46A,H46B), C54(H54A,H54B), C55(H55A,H55B), C20A(H20C,
 H20D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C13(H13), C17(H17), C31(H31), C32(H32), C34(H34),
 C35(H35), C39(H39), C40(H40), C42(H42), C43(H43), C48(H48), C49(H49), C51(H51),
  C52(H52), C57(H57), C58(H58), C60(H60), C61(H61), C22A(H22A), C23A(H23A),
 C25A(H25A), C26A(H26A), C22B(H22B), C23B(H23B), C25B(H25B), C26B(H26B)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C44(H44A,H44B,H44C), C53(H53A,H53B,H53C), C62(H62A,H62B,
 H62C), C27A(H27A,H27B,H27C), C27B(H27D,H27E,H27F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82576
_shelx_hkl_checksum              30228
_shelx_fab_checksum              5427
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;