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_1569506
_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         'C42 H30 F4 N8 O6 S2, 0.5(C4 H8 O2), C6 H4 S4'
_chemical_formula_sum            'C50 H38 F4 N8 O7 S6'
_chemical_formula_weight         1131.24
_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                73.686(2)
_cell_angle_beta                 88.364(2)
_cell_angle_gamma                89.8450(10)
_cell_formula_units_Z            4
_cell_length_a                   10.4191(2)
_cell_length_b                   18.3885(3)
_cell_length_c                   26.4258(6)
_cell_measurement_reflns_used    29314
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3320
_cell_measurement_theta_min      2.4470
_cell_volume                     4857.05(17)
_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 0.970
_diffrn_measured_fraction_theta_max 0.917
_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   -118.00 -37.00   0.50    0.92    --  -47.89 -43.00-161.00  162
  2  \w    -43.00  24.00   0.50    0.92    --  -47.89  43.00 -10.00  134
  3  \w     78.00 103.00   0.50    0.92    --   47.89  43.00 -10.00   50
  4  \w    -11.00  15.00   0.50    0.92    --   47.89 -43.00-161.00   52
  5  \w   -166.00-140.00   0.50    3.68    -- -104.00 -43.00-161.00   52
  6  \w     97.00 163.00   0.50    3.68    --  106.93  43.00 -10.00  132
  7  \w    -14.00  23.00   0.50    0.92    --  -47.89  19.00 150.00   74
  8  \w   -120.00 -95.00   0.50    0.92    --  -47.89-125.00 -30.00   50
  9  \w   -119.00 -82.00   0.50    0.92    --  -47.89-125.00 -90.00   74
 10  \w    -10.00  25.00   0.50    0.92    --  -47.89  19.00 120.00   70
 11  \w   -118.00 -93.00   0.50    3.68    -- -104.00 -19.00 -90.00   50
 12  \w   -163.00-133.00   0.50    3.68    -- -104.00 -99.00 120.00   60
 13  \w    -60.00 -32.00   0.50    3.68    -- -104.00  57.00  30.00   56
 14  \w    -59.00 -32.00   0.50    3.68    -- -104.00  57.00 120.00   54
 15  \w    -63.00 -37.00   0.50    3.68    -- -104.00  57.00  60.00   52
 16  \w   -107.00 -76.00   0.50    3.68    -- -104.00 125.00  90.00   62
 17  \w    -63.00 -37.00   0.50    3.68    -- -104.00  57.00-150.00   52
 18  \w    -67.00 -41.00   0.50    3.68    -- -104.00 125.00  90.00   52
 19  \w    -63.00 -32.00   0.50    3.68    -- -104.00  57.00   0.00   62
 20  \w   -127.00 -96.00   0.50    3.68    -- -104.00 -99.00 120.00   62
 21  \w   -162.00-137.00   0.50    3.68    -- -104.00 -19.00 -90.00   50
 22  \w    -64.00 -38.00   0.50    3.68    -- -104.00  57.00  90.00   52
 23  \w    -62.00 -34.00   0.50    3.68    -- -104.00  57.00 150.00   56
 24  \w     54.00 100.00   0.50    3.68    --  106.93 -77.00 -90.00   92
 25  \w     35.00 107.00   0.50    3.68    --  106.93 -77.00 150.00  144
 26  \w     70.00  95.00   0.50    3.68    --  106.93 -99.00 -30.00   50
 27  \w     43.00  68.00   0.50    3.68    --  106.93 -57.00 150.00   50
 28  \w     35.00  65.00   0.50    3.68    --  106.93 -57.00-180.00   60
 29  \w     93.00 178.00   0.50    3.68    --  106.93  57.00 -90.00  170
 30  \w     35.00  60.00   0.50    3.68    --  106.93 -57.00  60.00   50
 31  \w     35.00  63.00   0.50    3.68    --  106.93 -57.00-150.00   56
 32  \w     94.00 120.00   0.50    5.20    --  106.93  91.00 103.00   52
 33  \w    -62.00 -15.00   0.50    2.55    --  -48.26  57.00-150.00   94
 34  \w    -11.00  18.00   0.50    2.55    --  -48.26  19.00 -90.00   58
 35  \w    -18.00  81.00   0.50    2.55    --   48.26 -99.00  30.00  198
 36  \w     10.00  45.00   0.50    2.55    --   48.26 -38.00  30.00   70
 37  \w    -57.00 -32.00   0.50    5.20    -- -104.00 125.00 120.00   50
 38  \w   -172.00-147.00   0.50    5.20    -- -104.00 -38.00  90.00   50
 39  \w   -105.00 -72.00   0.50    5.20    -- -104.00 125.00 120.00   66
 40  \w   -111.00 -32.00   0.50    5.20    -- -104.00 125.00   0.00  158
 41  \w   -129.00-103.00   0.50    5.20    -- -104.00 -38.00  90.00   52
 42  \w     76.00 106.00   0.50    5.20    --  106.93-125.00-120.00   60
 43  \w    105.00 168.00   0.50    5.20    --  106.93  38.00 -60.00  126
 44  \w     36.00  61.00   0.50    5.20    --  106.93 -57.00   0.00   50
 45  \w     66.00 110.00   0.50    5.20    --  106.93-125.00 120.00   88
 46  \w     58.00 108.00   0.50    5.20    --  106.93-107.00  13.30  100
 47  \w    101.00 124.00   0.50    5.20    --  106.93  57.00   0.00   46
;
_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      -0.0094758000
_diffrn_orient_matrix_UB_12      0.0492945000
_diffrn_orient_matrix_UB_13      0.0384249000
_diffrn_orient_matrix_UB_21      0.0759854000
_diffrn_orient_matrix_UB_22      -0.0598094000
_diffrn_orient_matrix_UB_23      0.0407197000
_diffrn_orient_matrix_UB_31      0.1265594000
_diffrn_orient_matrix_UB_32      0.0401654000
_diffrn_orient_matrix_UB_33      -0.0236280000
_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  0.0507
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            55744
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.993
_diffrn_reflns_theta_min         2.504
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.281
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86460
_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            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       plate
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.733
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1351
_refine_ls_number_reflns         19059
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.1140
_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^)+(0.1893P)^2^+21.9058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3014
_refine_ls_wR_factor_ref         0.3080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16432
_reflns_number_total             19059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           10b-ttf-thf-hex_auto
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_database_code               1569506
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N S F'
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.560
_reflns_odcompleteness_completeness 97.16
_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. Restrained distances
 O145-C147
 1.48 with sigma of 0.02
 C150-O148
 1.48 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C119(H11A,H11B), C34(H34A,H34B), C6(H6A,H6B), C56(H56A,H56B),
 C99(H99A,H99B), C106(H10A,H10B), C78(H78A,H78B), C13(H13A,H13B), C128(H12A,
 H12B), C40(H40A,H40B), C27(H27A,H27B), C92(H92A,H92B), C112(H11C,H11D),
 C85(H85A,H85B), C20(H20A,H20B), C146(H14A,H14B), C149(H14E,H14F), C147(H14C,
 H14D), C150(H15A,H15B)
3.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C3(H3), C102(H102), C42(H42), C118(H118), C75(H75), C25(H25),
 C45(H45), C46(H46), C80(H80), C22(H22), C83(H83), C114(H114), C97(H97),
 C117(H117), C8(H8), C43(H43), C24(H24), C115(H115), C11(H11), C23(H23), C9(H9),
  C82(H82), C10(H10), C94(H94), C95(H95), C81(H81), C96(H96), C5(H5), C14(H14),
 C32(H32), C35(H35), C37(H37), C38(H38), C50(H50), C48(H48)
;
_shelx_res_checksum              38058
_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 2.689
_oxdiff_exptl_absorpt_empirical_full_min 0.435