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_1569489
_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         'C28 H16 F8 O4'
_chemical_formula_sum            'C28 H16 F8 O4'
_chemical_formula_weight         568.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-08 deposited with the CCDC.	2023-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2008(2)
_cell_length_b                   8.13200(10)
_cell_length_c                   33.0797(3)
_cell_measurement_reflns_used    10360
_cell_measurement_temperature    169.99(11)
_cell_measurement_theta_max      74.8220
_cell_measurement_theta_min      2.6460
_cell_volume                     4626.00(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(11)
_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 0.949
_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      5.00  50.00   0.50    0.30    --   47.70 -43.00  92.00   90
  2  \w     36.00  69.00   0.50    1.21    --  103.25 -61.00  30.00   66
  3  \w     32.00  66.00   0.50    1.21    --  103.25 -61.00  90.00   68
  4  \w     33.00  58.00   0.50    1.21    --  103.25 -61.00   0.00   50
  5  \w     38.00 102.00   0.50    0.30    --   47.70  43.00-116.00  128
  6  \w     96.00 169.00   0.50    1.21    --  103.25  43.00-116.00  146
  7  \w     92.00 169.00   0.50    1.21    --  103.25  45.00 -30.00  154
  8  \w     41.00  75.00   0.50    1.21    --  103.25 -61.00-180.00   68
  9  \w     33.00 100.00   0.50    1.21    --  103.25 -77.00-180.00  134
 10  \w    -44.00  19.00   0.50    0.30    --  -47.70  43.00-116.00  126
 11  \w    -23.00  28.00   0.50    0.30    --  -47.70  19.00  30.00  102
 12  \w    -67.00 -41.00   0.50    1.21    --  -99.00  61.00  60.00   52
 13  \w    -59.00 -33.00   0.50    1.21    --  -99.00  61.00  90.00   52
 14  \w    -68.00 -39.00   0.50    1.21    --  -99.00  61.00  30.00   58
 15  \w    -60.00 -27.00   0.50    1.21    --  -99.00 125.00   0.00   66
 16  \w   -111.00 -68.00   0.50    1.21    --  -99.00 125.00   0.00   86
 17  \w    -67.00 -42.00   0.50    1.21    --  -99.00  61.00-180.00   50
 18  \w   -107.00 -82.00   0.50    1.21    --  -99.00 -61.00   0.00   50
 19  \w   -120.00 -34.00   0.50    0.30    --  -47.70 -43.00  92.00  172
 20  \w   -129.00 -98.00   0.50    1.21    --  -99.00 -43.00  92.00   62
 21  \w   -168.00-116.00   0.50    1.21    --  -99.00 -61.00   0.00  104
 22  \w   -101.00 -76.00   0.50    1.21    --  -99.00 -77.00-180.00   50
 23  \w   -168.00-110.00   0.50    1.21    --  -99.00 -77.00-180.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0337010000
_diffrn_orient_matrix_UB_12      -0.1008736000
_diffrn_orient_matrix_UB_13      -0.0349315000
_diffrn_orient_matrix_UB_21      0.0823391000
_diffrn_orient_matrix_UB_22      0.0212684000
_diffrn_orient_matrix_UB_23      0.0185122000
_diffrn_orient_matrix_UB_31      -0.0103630000
_diffrn_orient_matrix_UB_32      -0.1589007000
_diffrn_orient_matrix_UB_33      0.0246666000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            16169
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.377
_diffrn_reflns_theta_min         2.672
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.336
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0491P)^2^+4.7532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4186
_reflns_number_total             4549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           tx5287
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_database_code               1569489
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O F'
_reflns_odcompleteness_completeness 99.73
_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 Secondary CH2 refined with riding coordinates:
 C00W(H00A,H00B), C010(H01A,H01B), C011(H01C,H01D), C014(H01E,H01F)
2.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00L(H00L), C00Q(H00Q), C00R(H00R), C00T(H00T), C00V(H00V),
 C00X(H00X), C012(H012)
;
_shelx_res_checksum              73349
_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 1.323
_oxdiff_exptl_absorpt_empirical_full_min 0.745