Tetrahomo corona[4]arene-based spirophanes: synthesis, structure, and properties.
Guo, Shen-Yi; Zhang, Zhuo-Ang; Tong, Shuo; Guo, Qing-Hui; Hua, Ruimao; Wang, Mei-Xiang; Chemical science 14 (2023) 8393–8400; doi:10.1039/d3sc02417b

data_1569502
_publ_section_title
;
 Tetrahomo corona[4]arene-based spirophanes: synthesis, structure, and
 properties.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              8393
_journal_page_last               8400
_journal_paper_doi               10.1039/d3sc02417b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         '2(C6 H4 S4), C42 H30 F4 N8 O6 S2, C H Cl3'
_chemical_formula_sum            'C55 H39 Cl3 F4 N8 O6 S10'
_chemical_formula_weight         1410.89
_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             2023-03-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-05-08 deposited with the CCDC.	2023-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                86.0189(9)
_cell_angle_beta                 82.6961(8)
_cell_angle_gamma                88.0689(9)
_cell_formula_units_Z            4
_cell_length_a                   10.46661(10)
_cell_length_b                   23.8858(3)
_cell_length_c                   24.0457(2)
_cell_measurement_reflns_used    53882
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.0230
_cell_measurement_theta_min      1.8550
_cell_volume                     5946.46(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.952
_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   -119.00 -58.00   0.50    0.70    --  -48.26-149.00  54.00  122
  2  \w    -94.00 -13.00   0.50    0.70    --  -48.26 124.00 -62.00  162
  3  \w   -108.00 -26.00   0.50    0.70    --  -48.26 149.00 101.00  164
  4  \w     17.00  94.00   0.50    0.70    --   48.26-124.00-141.00  154
  5  \w     62.00 121.00   0.50    0.70    --   48.26 149.00 101.00  118
  6  \w     31.00 109.00   0.50    0.70    --   48.26-149.00  54.00  156
  7  \w   -128.00 -32.00   0.50    3.00    -- -104.00 149.00 101.00  192
  8  \w   -175.00 -75.00   0.50    3.00    -- -104.00-124.00-141.00  200
  9  \w   -166.00 -58.00   0.50    3.00    -- -104.00-149.00  54.00  216
 10  \w   -111.00 -32.00   0.50    3.00    -- -104.00 124.00 -62.00  158
 11  \w     35.00 128.00   0.50    3.00    --  106.93-149.00  54.00  186
 12  \w     79.00 178.00   0.50    3.00    --  106.93 124.00 -62.00  198
 13  \w     35.00 111.00   0.50    3.00    --  106.93-124.00-141.00  152
 14  \w    -24.00  26.00   0.50    0.70    --  -48.26  19.00-120.00  100
 15  \w    -41.00  24.00   0.50    0.70    --  -48.26  38.00 120.00  130
 16  \w   -119.00 -74.00   0.50    0.70    --  -48.26-125.00   0.00   90
 17  \w    -24.00  26.00   0.50    0.70    --  -48.26  19.00  30.00  100
 18  \w    -25.00  28.00   0.50    0.70    --   48.26 -19.00  30.00  106
 19  \w     27.00 121.00   0.50    0.70    --   48.26  77.00 150.00  188
 20  \w   -103.00 -32.00   0.50    3.00    -- -104.00  77.00 -60.00  142
 21  \w   -175.00 -93.00   0.50    3.00    -- -104.00 -38.00-120.00  164
 22  \w   -175.00 -89.00   0.50    3.00    -- -104.00 -60.00 -42.78  172
 23  \w    -64.00 -32.00   0.50    3.00    -- -104.00  57.00  90.00   64
 24  \w   -103.00 -32.00   0.50    3.00    -- -104.00  77.00 150.00  142
 25  \w    -64.00 -32.00   0.50    3.00    -- -104.00  57.00 -60.00   64
 26  \w   -124.00 -32.00   0.50    3.00    -- -104.00 142.00-118.54  184
 27  \w   -175.00 -93.00   0.50    3.00    -- -104.00 -19.00  90.00  164
 28  \w   -175.00 -92.00   0.50    3.00    -- -104.00 -48.00-136.32  166
 29  \w     77.00 104.00   0.50    3.00    --  106.93-125.00  90.00   54
 30  \w    140.00 166.00   0.50    3.00    --  106.93  77.00   0.00   52
 31  \w     35.00 107.00   0.50    3.00    --  106.93-125.00-120.00  144
 32  \w     36.00  82.00   0.50    3.00    --  106.93 -99.00-120.00   92
 33  \w     85.00 138.00   0.50    3.00    --  106.93  77.00   0.00  106
 34  \w     82.00 107.00   0.50    3.00    --  106.93 -77.00  60.00   50
 35  \w     44.00  74.00   0.50    3.00    --  106.93 -77.00  60.00   60
 36  \w     99.00 157.00   0.50    3.00    --  106.93  38.00  90.00  116
 37  \w     35.00 106.00   0.50    3.00    --  106.93 -99.00  60.00  142
 38  \w    126.00 177.00   0.50    3.00    --  106.93  38.00-150.00  102
 39  \w     37.00  90.00   0.50    3.00    --  106.93-125.00  60.00  106
 40  \w     36.00  68.00   0.50    3.00    --  106.93 -57.00 -90.00   64
 41  \w     96.00 178.00   0.50    3.00    --  106.93  38.00 120.00  164
 42  \w     36.00  66.00   0.50    3.00    --  106.93 -57.00-120.00   60
 43  \w     90.00 115.00   0.50    3.00    --  106.93 149.00 101.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0165718000
_diffrn_orient_matrix_UB_12      -0.0138078000
_diffrn_orient_matrix_UB_13      -0.0602712000
_diffrn_orient_matrix_UB_21      0.0195130000
_diffrn_orient_matrix_UB_22      -0.0629686000
_diffrn_orient_matrix_UB_23      0.0161696000
_diffrn_orient_matrix_UB_31      -0.1462148000
_diffrn_orient_matrix_UB_32      -0.0051896000
_diffrn_orient_matrix_UB_33      0.0172145000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            112360
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.552
_diffrn_reflns_theta_min         1.855
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       needle
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1586
_refine_ls_number_reflns         24377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0869
_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^)+(0.0436P)^2^+54.8842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2143
_refine_ls_wR_factor_ref         0.2175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21064
_reflns_number_total             24377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           gsy-10b-ttf-chcl3-hex--25oc_auto
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_database_code               1569502
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N F S'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Sof(Cl4A)=Sof(Cl3A)=Sof(Cl5A)=Sof(C2A)=Sof(H2A)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(Cl5)=Sof(C2)=Sof(H2)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C166(H166), C2(H2), C2A(H2A)
3.b Secondary CH2 refined with riding coordinates:
 C124(H12a,H12b), C67(H67a,H67b), C76(H76a,H76b), C94(H94a,H94b), C60(H60a,
 H60b), C131(H13a,H13b), C140(H14a,H14b), C120(H12c,H12d), C47(H47a,H47b),
 C54(H54a,H54b), C40(H40a,H40b), C88(H88a,H88b), C87(H87a,H87b), C93(H93a,H93b),
  C26(H26a,H26b), C33(H33a,H33b)
3.c Aromatic/amide H refined with riding coordinates:
 C65(H65), C129(H129), C66(H66), C126(H126), C19(H19), C14(H14), C3(H3),
 C130(H130), C50(H50), C13(H13), C4(H4), C127(H127), C62(H62), C114(H114),
 C8(H8), C153(H153), C23(H23), C63(H63), C99(H99), C148(H148), C9(H9),
 C108(H108), C147(H147), C42(H42), C18(H18), C152(H152), C31(H31), C112(H112),
 C45(H45), C28(H28), C107(H107), C30(H30), C162(H162), C163(H163), C43(H43),
 C44(H44), C157(H157), C106(H106), C109(H109), C110(H110), C111(H111),
 C158(H158), C29(H29), C105(H105)
;
_shelx_res_checksum              95731
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.217
_oxdiff_exptl_absorpt_empirical_full_min 0.324