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_1569491
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-03
_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                 94.927(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4892(2)
_cell_length_b                   7.62230(10)
_cell_length_c                   34.5522(6)
_cell_measurement_reflns_used    8260
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.2150
_cell_measurement_theta_min      2.5380
_cell_volume                     2752.30(8)
_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      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.959
_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    -23.00  29.00   0.50    0.06    --   47.20 -29.00  61.00  104
  2  \w     33.00  70.00   0.50    0.22    --  103.25 -61.00   0.00   74
  3  \w     48.00 102.00   0.50    0.22    --  103.25 -94.00 -30.00  108
  4  \w     83.00 108.00   0.50    0.22    --  103.25-125.00  60.00   50
  5  \w     47.00  73.00   0.50    0.22    --  103.25 -61.00  90.00   52
  6  \w     34.00  69.00   0.50    0.22    --  103.25 -61.00 120.00   70
  7  \w     40.00  75.00   0.50    0.22    --  103.25 -61.00  60.00   70
  8  \w     40.00  67.00   0.50    0.22    --  103.25-125.00  60.00   54
  9  \w     32.00  73.00   0.50    0.22    --  103.25 -61.00 150.00   82
 10  \w     92.00 159.00   0.50    0.22    --  103.25  15.00 120.00  134
 11  \w     45.00 122.00   0.50    0.06    --   47.20  29.00-136.00  154
 12  \w     91.00 169.00   0.50    0.22    --  103.25  29.00-136.00  156
 13  \w     32.00  57.00   0.50    0.22    --  103.25 -61.00-120.00   50
 14  \w    -92.00 -66.00   0.50    0.06    --  -47.20 -29.00  61.00   52
 15  \w    -22.00  26.00   0.50    0.06    --  -47.20  19.00   0.00   96
 16  \w    -22.00   5.00   0.50    0.06    --  -47.20  19.00 -30.00   54
 17  \w    -31.00  26.00   0.50    0.06    --  -47.20  29.00-136.00  114
 18  \w    -55.00 -26.00   0.50    0.22    --  -99.00  61.00 -60.00   58
 19  \w    -56.00 -26.00   0.50    0.22    --  -99.00  61.00 -30.00   60
 20  \w    -64.00 -33.00   0.50    0.22    --  -99.00  61.00   0.00   62
 21  \w    -63.00 -26.00   0.50    0.22    --  -99.00  61.00  60.00   74
 22  \w    -66.00 -40.00   0.50    0.22    --  -99.00  61.00 120.00   52
 23  \w    -67.00 -26.00   0.50    0.22    --  -99.00  61.00  30.00   82
 24  \w    -97.00 -39.00   0.50    0.22    --  -99.00  77.00-150.00  116
 25  \w   -166.00-141.00   0.50    0.22    --  -99.00 -29.00  61.00   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      -0.1377657000
_diffrn_orient_matrix_UB_12      -0.0598343000
_diffrn_orient_matrix_UB_13      0.0052416000
_diffrn_orient_matrix_UB_21      -0.0397424000
_diffrn_orient_matrix_UB_22      0.0452971000
_diffrn_orient_matrix_UB_23      -0.0427957000
_diffrn_orient_matrix_UB_31      0.0343264000
_diffrn_orient_matrix_UB_32      -0.1876494000
_diffrn_orient_matrix_UB_33      -0.0119817000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            18855
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.420
_diffrn_reflns_theta_min         2.567
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.063
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78324
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0489P)^2^+1.1493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4711
_reflns_number_total             5468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           tx5086
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_database_code               1569491
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H F O'
_reflns_odcompleteness_completeness 99.98
_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:
 C00V(H00A,H00B), C00Y(H00C,H00D), C00Z(H00E,H00F), C013(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00K(H00K), C00P(H00P), C00Q(H00Q), C010(H010), C011(H011),
 C012(H012), C014(H014), C015(H015), C016(H016)
2.c Idealised Me refined as rotating group:
 C017(H01C,H01D,H01E), C018(H01F,H01G,H01H)
;
_shelx_res_checksum              12402
_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 1.473
_oxdiff_exptl_absorpt_empirical_full_min 0.592