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_1569505
_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 H34 N8 O6 S2, 5(C0.333 H0.333 Cl)'
_chemical_formula_sum            'C43.67 H35.67 Cl5 N8 O6 S2'
_chemical_formula_weight         1009.84
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-10
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   21.6918(2)
_cell_length_b                   21.6918(2)
_cell_length_c                   24.6601(2)
_cell_measurement_reflns_used    44576
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      77.7660
_cell_measurement_theta_min      2.9180
_cell_volume                     10048.86(15)
_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      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_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    -95.00 -14.00   0.50    0.23    --  -48.26 126.00  85.00  162
  2  \w   -107.00 -23.00   0.50    0.23    --  -48.26 145.00-106.00  168
  3  \w   -119.00 -60.50   0.50    0.23    --  -48.26-145.00-158.00  117
  4  \w   -119.00 -73.50   0.50    0.23    --  -48.26-126.00   9.00   91
  5  \w     66.00 121.00   0.50    0.23    --   48.26 145.00-106.00  110
  6  \w     19.00  95.00   0.50    0.23    --   48.26-126.00   9.00  152
  7  \w     30.00 107.00   0.50    0.23    --   48.26-145.00-158.00  154
  8  \w   -126.00 -32.00   0.50    0.91    -- -104.00 145.00-106.00  188
  9  \w   -112.00 -32.00   0.50    0.91    -- -104.00 126.00  85.00  160
 10  \w   -175.00 -73.50   0.50    0.91    -- -104.00-126.00   9.00  203
 11  \w     66.00 170.00   0.50    0.91    --  106.93 145.00-106.00  208
 12  \w     35.00 126.00   0.50    0.91    --  106.93-145.00-158.00  182
 13  \w     79.00 178.00   0.50    0.91    --  106.93 126.00  85.00  198
 14  \w     35.00 112.00   0.50    0.91    --  106.93-126.00   9.00  154
 15  \w    -24.00  26.00   0.50    0.23    --  -48.26  19.00 -60.00  100
 16  \w    -24.00  26.00   0.50    0.23    --  -48.26  19.00-120.00  100
 17  \w    -24.00  26.00   0.50    0.23    --  -48.26  19.00  60.00  100
 18  \w   -119.00 -74.00   0.50    0.23    --  -48.26-125.00 -30.00   90
 19  \w   -119.00 -27.00   0.50    0.23    --  -48.26 -77.00 -60.00  184
 20  \w   -119.00 -74.00   0.50    0.23    --  -48.26-125.00-120.00   90
 21  \w   -119.00 -74.00   0.50    0.23    --  -48.26-125.00  60.00   90
 22  \w    -64.00 -32.00   0.50    0.91    -- -104.00  57.00 120.00   64
 23  \w    -64.00 -32.00   0.50    0.91    -- -104.00  57.00 -90.00   64
 24  \w    -64.00 -32.00   0.50    0.91    -- -104.00  57.00 150.00   64
 25  \w   -175.00 -92.00   0.50    0.91    -- -104.00 -48.00 -30.32  166
 26  \w   -175.00 -87.00   0.50    0.91    -- -104.00 -66.00 -48.07  176
 27  \w   -108.00 -32.00   0.50    0.91    -- -104.00 111.00   2.42  152
 28  \w   -111.00 -32.00   0.50    0.91    -- -104.00 125.00  30.00  158
 29  \w    -64.00 -32.00   0.50    0.91    -- -104.00  57.00  60.00   64
 30  \w   -103.00 -32.00   0.50    0.91    -- -104.00  77.00 -60.00  142
 31  \w   -175.00 -92.00   0.50    0.91    -- -104.00 -53.00  18.45  166
 32  \w    -61.00 -32.00   0.50    0.91    -- -104.00  57.00-120.00   58
 33  \w   -139.00-113.00   0.50    0.91    -- -104.00-145.00-158.00   52
 34  \w   -169.00-117.00   0.50    0.91    -- -104.00 -49.00 -83.28  104
 35  \w    -63.00 -38.00   0.50    0.91    -- -104.00  57.00  30.00   50
 36  \w    -64.00 -32.00   0.50    0.91    -- -104.00  57.00  90.00   64
 37  \w   -175.00 -92.00   0.50    0.91    -- -104.00 -52.00  95.82  166
 38  \w     36.00  61.00   0.50    0.91    --  106.93 -57.00-180.00   50
 39  \w     36.00  65.00   0.50    0.91    --  106.93 -57.00 -30.00   58
 40  \w    121.00 171.00   0.50    0.91    --  106.93 125.00 -60.00  100
 41  \w     42.00  67.00   0.50    0.91    --  106.93 -57.00-120.00   50
 42  \w     38.00 105.00   0.50    0.91    --  106.93 -99.00  30.00  134
 43  \w     39.00  68.00   0.50    0.91    --  106.93 -57.00  60.00   58
 44  \w    132.00 158.00   0.50    0.91    --  106.93  38.00-150.00   52
 45  \w     55.00 106.00   0.50    0.91    --  106.93 -99.00-120.00  102
 46  \w     65.00 103.00   0.50    0.91    --  106.93 -99.00-180.00   76
 47  \w     51.00 100.00   0.50    0.91    --  106.93 -99.00-150.00   98
;
_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      -0.0553288667
_diffrn_orient_matrix_UB_12      -0.0400685333
_diffrn_orient_matrix_UB_13      0.0447941667
_diffrn_orient_matrix_UB_21      -0.0417239000
_diffrn_orient_matrix_UB_22      -0.0629819000
_diffrn_orient_matrix_UB_23      -0.0389671000
_diffrn_orient_matrix_UB_31      0.0438447333
_diffrn_orient_matrix_UB_32      -0.0339043333
_diffrn_orient_matrix_UB_33      0.0194423667
_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  0.0527
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            64749
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.622
_diffrn_reflns_theta_min         2.957
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70686
_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 red'
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       block
_exptl_crystal_F_000             4668
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.922
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 4312 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         9218
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0554
_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^)+(0.1287P)^2^+12.0225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1658
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                9059
_reflns_number_total             9218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           22a1_auto
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_original_cell_volume        10048.9(2)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               1569505
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O F N S'
_reflns_odcompleteness_completeness 100.00
_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.a Ternary CH refined with riding coordinates:
 C60(H60), C66(H66), C62(H62)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C18(H18A,H18B), C50(H50A,H50B), C28(H28A,H28B), C41(H41A,H41B),
 C14(H14A,H14B), C34(H34A,H34B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C55(H55), C16(H16), C23(H23), C22(H22), C53(H53), C40(H40), C39(H39),
 C11(H11), C54(H54), C10(H10), C5(H5), C58(H58), C52(H52), C56(H56), C36(H36),
 C57(H57), C37(H37), C51(H51)
;
_shelx_res_checksum              68005
_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 2.456
_oxdiff_exptl_absorpt_empirical_full_min 0.537