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_1569500
_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, 2(C3 H6 O)'
_chemical_formula_sum            'C48 H42 F4 N8 O8 S2'
_chemical_formula_weight         999.01
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-24
_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                76.4380(10)
_cell_angle_beta                 89.655(2)
_cell_angle_gamma                73.552(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5906(2)
_cell_length_b                   15.6459(3)
_cell_length_c                   16.7187(2)
_cell_measurement_reflns_used    17059
_cell_measurement_temperature    137(50)
_cell_measurement_theta_max      66.4330
_cell_measurement_theta_min      3.4770
_cell_volume                     2334.04(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_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      137(50)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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    -45.00 132.00   0.50    2.00    --   43.50  28.00-150.00  354
  2  \w    -45.00 132.00   0.50    2.00    --   43.50  55.00  90.00  354
  3  \w    -45.00 132.00   0.50    2.00    --   43.50   9.00-180.00  354
  4  \w      4.00  33.00   0.50    4.00    --   90.00  54.00-171.53   58
  5  \w    138.00 178.00   0.50    4.00    --   90.00  54.00-171.53   80
  6  \w      5.00 178.00   0.50    4.00    --   90.00  55.00 -32.59  346
  7  \w    105.00 151.00   0.50    4.00    --   90.00  53.00 -54.15   92
  8  \w     98.00 179.00   0.50    4.00    --   90.00  55.00 115.99  162
  9  \w    121.00 172.00   0.50    4.00    --   90.00  37.00  90.00  102
 10  \w    121.00 147.00   0.50    4.00    --   90.00  51.00-165.73   52
 11  \w    148.00 176.00   0.50    4.00    --   90.00  54.00 158.29   56
 12  \w     13.00  39.00   0.50    4.00    --   90.00  54.00-110.43   52
 13  \w     98.00 131.00   0.50    4.00    --   90.00  54.00  36.83   66
 14  \w     71.00 178.00   0.50    4.00    --   90.00  37.00 150.00  214
 15  \w      9.00  64.00   0.50    4.00    --   90.00  37.00 150.00  110
 16  \w     17.00  61.00   0.50    4.00    --   90.00  55.00 115.99   88
 17  \w     46.00  71.00   0.50    4.00    --   90.00  52.00   9.51   50
 18  \w     89.00 177.00   0.50    4.00    --   90.00  52.00   9.51  176
 19  \w     22.00  49.00   0.50    4.00    --   90.00  37.00  90.00   54
 20  \w     70.00  96.00   0.50    4.00    --   90.00  37.00  90.00   52
 21  \w    129.00 155.00   0.50    4.00    --   90.00  28.00   0.00   52
 22  \w     37.00  83.00   0.50    4.00    --   90.00  51.00-165.73   92
 23  \w    116.00 142.00   0.50    4.00    --   90.00  54.00-110.43   52
 24  \w     14.00  50.00   0.50    4.00    --   90.00  54.00 158.29   72
 25  \w    137.00 163.00   0.50    4.00    --   90.00  53.00 -86.66   52
 26  \w     63.00  89.00   0.50    4.00    --   90.00  54.00-110.43   52
 27  \w     28.00  76.00   0.50    4.00    --   90.00  53.00 -86.66   96
 28  \w     35.00  70.00   0.50    4.00    --   90.00  54.00  36.83   70
 29  \w     35.00  70.00   0.50    4.00    --   90.00  50.00-159.05   70
 30  \w     85.00 110.00   0.50    4.00    --   90.00  50.00-159.05   50
 31  \w      8.00  46.00   0.50    4.00    --   90.00  55.00-119.24   76
 32  \w     78.00 179.00   0.50    4.00    --   90.00  55.00-119.24  202
 33  \w      9.00  52.00   0.50    4.00    --   90.00  37.00  60.00   86
 34  \w     87.00 154.00   0.50    4.00    --   90.00  37.00  60.00  134
 35  \w      1.00 102.00   0.50    4.00    --   90.00   9.00 -90.00  202
 36  \w      2.00  28.00   0.50    4.00    --   90.00   9.00   0.00   52
 37  \w    119.00 179.00   0.50    4.00    --   90.00   9.00   0.00  120
 38  \w     12.00  48.00   0.50    4.00    --   90.00  46.00 150.00   72
 39  \w     75.00 101.00   0.50    4.00    --   90.00  46.00 150.00   52
 40  \w    134.00 164.00   0.50    4.00    --   90.00  46.00 150.00   60
 41  \w      2.00 100.00   0.50    4.00    --   90.00  41.00-137.74  196
 42  \w      7.00  33.00   0.50    4.00    --   90.00  28.00   0.00   52
 43  \w     77.00 103.00   0.50    4.00    --   90.00  28.00   0.00   52
 44  \w    153.00 179.00   0.50    4.00    --   90.00  55.00  51.21   52
 45  \w    119.00 145.00   0.50    4.00    --   90.00  37.00 120.00   52
 46  \w     95.00 135.00   0.50    4.00    --   90.00  55.00  51.21   80
 47  \w    139.00 179.00   0.50    4.00    --   90.00  54.00  36.83   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0065175000
_diffrn_orient_matrix_UB_12      0.1015839000
_diffrn_orient_matrix_UB_13      -0.0105782000
_diffrn_orient_matrix_UB_21      0.0056475000
_diffrn_orient_matrix_UB_22      0.0119531000
_diffrn_orient_matrix_UB_23      -0.0939758000
_diffrn_orient_matrix_UB_31      -0.1676168000
_diffrn_orient_matrix_UB_32      0.0271643000
_diffrn_orient_matrix_UB_33      -0.0089136000
_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  0.1085
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37781
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        66.686
_diffrn_reflns_theta_max         66.686
_diffrn_reflns_theta_min         3.554
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.722
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.78a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         8027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1265P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6671
_reflns_number_total             8027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           gsy1357-2
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_database_code               1569500
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O S F'
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.425
_reflns_odcompleteness_completeness 96.32
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00T(H00A,H00B), C00X(H00C,H00D), C00Z(H00E,H00F), C01E(H01B,H01C), C01G(H01D,
 H01E), C01H(H01F,H01G), C01K(H01H,H01J), C01P(H01K,H01P)
2.b Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C00V(H00V), C00Y(H00Y), C011(H011), C015(H015), C01A(H01A),
 C01I(H01I), C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O), C01Q(H01Q),
 C01S(H01S), C01V(H01V)
2.c Idealised Me refined as rotating group:
 C01U(H01Z,H,HA), C01W(H01,HB,HC), C01X(H01R,H01T,H01U), C01Y(H01W,H01X,H01Y)
;
_shelx_res_checksum              18081
_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 6.452
_oxdiff_exptl_absorpt_empirical_full_min 0.261