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_1569490
_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         'C32 H24 F4 O8'
_chemical_formula_sum            'C32 H24 F4 O8'
_chemical_formula_weight         612.51
_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             2023-03-27
_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                104.2800(10)
_cell_angle_beta                 105.1950(10)
_cell_angle_gamma                98.3680(10)
_cell_formula_units_Z            2
_cell_length_a                   10.04050(10)
_cell_length_b                   11.2749(2)
_cell_length_c                   12.9240(2)
_cell_measurement_reflns_used    20162
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      77.4520
_cell_measurement_theta_min      4.1160
_cell_volume                     1333.29(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.958
_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   -103.00 -32.00   0.50    0.05    -- -104.00  77.00  30.00  142
  2  \w    -64.00 -32.00   0.50    0.05    -- -104.00  57.00   0.00   64
  3  \w    -28.00  26.00   0.50    0.05    --  -48.14  24.00 -49.00  108
  4  \w    -41.00  24.00   0.50    0.05    --  -48.14  38.00  90.00  130
  5  \w    -24.00  26.00   0.50    0.05    --  -48.14  19.00 150.00  100
  6  \w     27.00  75.00   0.50    0.05    --   48.14  77.00  60.00   96
  7  \w     38.00 123.00   0.50    0.05    --   48.14  24.00 -49.00  170
  8  \w     38.00 120.00   0.50    0.05    --   48.14  38.00-180.00  164
  9  \w     35.00  68.00   0.50    0.05    --  106.93 -57.00-180.00   66
 10  \w     35.00 107.00   0.50    0.05    --  106.93 -77.00-180.00  144
 11  \w     35.00  68.00   0.50    0.05    --  106.93 -57.00-120.00   66
 12  \w    -23.00  70.00   0.50    0.05    --   48.14 -77.00 120.00  186
 13  \w    -25.00  32.00   0.50    0.05    --   48.14 -24.00 145.00  114
 14  \w     35.00 106.00   0.50    0.05    --  106.93 -99.00  60.00  142
 15  \w     35.00 106.00   0.50    0.05    --  106.93 -99.00 120.00  142
 16  \w     35.00 111.00   0.50    0.05    --  106.93-125.00 120.00  152
 17  \w     35.00 111.00   0.50    0.05    --  106.93-125.00  30.00  152
 18  \w     19.00  95.00   0.50    0.05    --   48.14-125.00   0.00  152
 19  \w     35.00 106.00   0.50    0.05    --  106.93 -99.00-180.00  142
 20  \w     97.00 178.00   0.50    0.05    --  106.93  24.00 -49.00  162
 21  \w     96.00 178.00   0.50    0.05    --  106.93  38.00-120.00  164
 22  \w     96.00 178.00   0.50    0.05    --  106.93  38.00-180.00  164
 23  \w   -120.00 -26.00   0.50    0.05    --  -48.14 -77.00-120.00  188
 24  \w   -120.00 -26.00   0.50    0.05    --  -48.14 -77.00 -30.00  188
 25  \w   -120.00 -26.00   0.50    0.05    --  -48.14 -77.00  60.00  188
 26  \w   -120.00 -26.00   0.50    0.05    --  -48.14 -77.00 150.00  188
 27  \w   -122.00 -38.00   0.50    0.05    --  -48.14 -24.00 145.00  168
 28  \w   -175.00 -83.00   0.50    0.05    -- -104.00 -76.00  35.55  184
 29  \w   -175.00 -93.00   0.50    0.05    -- -104.00 -38.00 120.00  164
 30  \w   -175.00 -94.00   0.50    0.05    -- -104.00 -24.00 145.00  162
 31  \w   -175.00 -91.00   0.50    0.05    -- -104.00 -53.00-115.46  168
 32  \w   -175.00 -92.00   0.50    0.05    -- -104.00 -49.00-106.48  166
 33  \w   -109.00 -32.00   0.50    0.05    -- -104.00 115.00-122.93  154
 34  \w   -111.00 -32.00   0.50    0.05    -- -104.00 125.00 -90.00  158
 35  \w   -111.00 -32.00   0.50    0.05    -- -104.00 125.00  30.00  158
 36  \w   -127.00 -32.00   0.50    0.05    -- -104.00 146.00  69.56  190
 37  \w   -127.00 -32.00   0.50    0.05    -- -104.00 146.00 134.45  190
;
_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      0.1591648000
_diffrn_orient_matrix_UB_12      0.0553733000
_diffrn_orient_matrix_UB_13      0.0273335000
_diffrn_orient_matrix_UB_21      -0.0261966000
_diffrn_orient_matrix_UB_22      0.1336785000
_diffrn_orient_matrix_UB_23      0.0306758000
_diffrn_orient_matrix_UB_31      0.0245787000
_diffrn_orient_matrix_UB_32      -0.0002333000
_diffrn_orient_matrix_UB_33      0.1227168000
_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  0.0227
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25157
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.791
_diffrn_reflns_theta_min         3.713
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59437
_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 colourless'
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0533P)^2^+0.5182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5189
_reflns_number_total             5461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           htc4_4f_2co2me_auto
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_database_code               1569490
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O F'
_reflns_odcompleteness_completeness 99.64
_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:
 C24(H24A,H24B), C3(H3A,H3B), C10(H10A,H10B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C27(H27), C22(H22), C8(H8), C19(H19), C21(H21), C7(H7), C6(H6),
 C5(H5), C20(H20)
2.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              96771
_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 2.821
_oxdiff_exptl_absorpt_empirical_full_min 0.478