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_1569488
_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 H20 F4 O4'
_chemical_formula_sum            'C28 H20 F4 O4'
_chemical_formula_weight         496.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 90.3250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.69180(10)
_cell_length_b                   8.03030(10)
_cell_length_c                   23.5644(2)
_cell_measurement_reflns_used    10250
_cell_measurement_temperature    169.99(11)
_cell_measurement_theta_max      75.0490
_cell_measurement_theta_min      3.7300
_cell_volume                     2212.39(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.968
_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    -26.00  -1.00   0.50    0.05    --  -47.70  29.00  86.00   50
  2  \w    -64.00 -32.00   0.50    0.05    --  -99.00  61.00  60.00   64
  3  \w    -67.00 -32.00   0.50    0.05    --  -99.00  61.00  90.00   70
  4  \w    -65.00 -27.00   0.50    0.05    --  -99.00  61.00   0.00   76
  5  \w    -65.00 -27.00   0.50    0.05    --  -99.00  77.00 -90.00   76
  6  \w    -91.00 -64.00   0.50    0.05    --  -47.70 -29.00 -74.00   54
  7  \w     52.00 123.00   0.50    0.05    --   47.70  29.00  86.00  142
  8  \w     91.00 138.00   0.50    0.05    --  103.25  29.00  86.00   94
  9  \w     62.00 106.00   0.50    0.05    --  103.25 -77.00  30.00   88
 10  \w     71.00 108.00   0.50    0.05    --  103.25 -77.00  90.00   74
 11  \w     41.00  74.00   0.50    0.05    --  103.25 -61.00 120.00   66
 12  \w     33.00  58.00   0.50    0.05    --  103.25 -77.00  90.00   50
 13  \w     39.00  73.00   0.50    0.05    --  103.25 -61.00  90.00   68
 14  \w     39.00  75.00   0.50    0.05    --  103.25 -61.00 150.00   72
 15  \w     46.00  73.00   0.50    0.05    --  103.25 -61.00 -30.00   54
 16  \w     33.00  75.00   0.50    0.05    --  103.25 -61.00 -60.00   84
 17  \w     37.00  68.00   0.50    0.05    --  103.25 -61.00-180.00   62
 18  \w     31.00  56.00   0.50    0.05    --  103.25-125.00-180.00   50
 19  \w     80.00 105.00   0.50    0.05    --  103.25-125.00-180.00   50
 20  \w    127.00 168.00   0.50    0.05    --  103.25  30.00-180.00   82
 21  \w     98.00 124.00   0.50    0.05    --  103.25  30.00-180.00   52
 22  \w    -25.00  33.00   0.50    0.05    --   47.70 -29.00 -74.00  116
 23  \w    -27.00  27.00   0.50    0.05    --   47.70 -19.00 150.00  108
 24  \w   -119.00 -81.00   0.50    0.05    --  -47.70-125.00 120.00   76
 25  \w   -155.00 -90.00   0.50    0.05    --  -99.00 -29.00 -74.00  130
 26  \w    -99.00 -74.00   0.50    0.05    --  -99.00  77.00 -90.00   50
;
_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      -0.1107735000
_diffrn_orient_matrix_UB_12      0.0719023000
_diffrn_orient_matrix_UB_13      0.0252453000
_diffrn_orient_matrix_UB_21      -0.0536915000
_diffrn_orient_matrix_UB_22      0.0074898000
_diffrn_orient_matrix_UB_23      -0.0598080000
_diffrn_orient_matrix_UB_31      -0.0469968000
_diffrn_orient_matrix_UB_32      -0.1777084000
_diffrn_orient_matrix_UB_33      0.0077288000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14843
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.311
_diffrn_reflns_theta_min         3.752
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88904
_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    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0509P)^2^+0.6162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3951
_reflns_number_total             4415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           tx5286
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_database_code               1569488
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O F'
_reflns_odcompleteness_completeness 99.95
_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:
 C00V(H00A,H00B), C00W(H00E,H00F), C00Y(H00G,H00J), C010(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00H(H00H), C00I(H00I), C00M(H00M), C00O(H00O),
 C00P(H00P), C00R(H00R), C00S(H00S), C00U(H00U), C00X(H00X), C00Z(H00Z)
;
_shelx_res_checksum              90651
_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 1.379
_oxdiff_exptl_absorpt_empirical_full_min 0.777