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_1569492
_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         'C64 H44 F8 N8 O8 S4, 2(C7 H8)'
_chemical_formula_sum            'C78 H60 F8 N8 O8 S4'
_chemical_formula_weight         1517.58
_space_group_crystal_system      tetragonal
_space_group_IT_number           116
_space_group_name_Hall           'P -4 -2c'
_space_group_name_H-M_alt        'P -4 c 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-11-03
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7227(4)
_cell_length_b                   12.7227(4)
_cell_length_c                   23.8456(5)
_cell_measurement_reflns_used    3740
_cell_measurement_temperature    225(40)
_cell_measurement_theta_max      76.1830
_cell_measurement_theta_min      3.4840
_cell_volume                     3859.82(19)
_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      225(40)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.972
_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     51.00  77.00   0.50   14.54    --  106.93-130.00 -12.00   52
  2  \w     80.00 106.00   0.50   14.54    --  106.93-130.00 -12.00   52
  3  \w     79.00 170.00   0.50   14.54    --  106.93   3.00 -25.00  182
  4  \w   -115.00 -77.00   0.50    3.64    --  -48.26-130.00 -12.00   76
  5  \w    -25.00  28.00   0.50    3.64    --   48.26 -19.00 -30.00  106
  6  \w     61.00  87.00   0.50    3.64    --   48.26-130.00 -12.00   52
  7  \w    -23.00  21.00   0.50    3.64    --   48.26 -38.00  30.00   88
  8  \w     42.00  71.00   0.50   14.54    --  106.93 -99.00  60.00   58
  9  \w     75.00 104.00   0.50   14.54    --  106.93 -99.00  60.00   58
 10  \w     44.00 111.00   0.50   14.54    --  106.93-125.00 150.00  134
 11  \w     35.00  64.00   0.50   14.54    --  106.93 -57.00  60.00   58
 12  \w     39.00  68.00   0.50   14.54    --  106.93 -57.00  30.00   58
;
_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      0.1087389000
_diffrn_orient_matrix_UB_12      -0.0526246000
_diffrn_orient_matrix_UB_13      0.0042939000
_diffrn_orient_matrix_UB_21      0.0523912000
_diffrn_orient_matrix_UB_22      0.1090833000
_diffrn_orient_matrix_UB_23      0.0025646000
_diffrn_orient_matrix_UB_31      -0.0092438000
_diffrn_orient_matrix_UB_32      -0.0008026000
_diffrn_orient_matrix_UB_33      0.0644142000
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11709
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.312
_diffrn_reflns_theta_min         3.474
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.800
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59978
_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 red'
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       needle
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 878 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.050(13)
_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     241
_refine_ls_number_reflns         3719
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0608P)^2^+0.0877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.710
_reflns_Friedel_fraction_full    0.885
_reflns_Friedel_fraction_max     0.831
_reflns_number_gt                2598
_reflns_number_total             3719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           gsy1417-tolhex_auto_sq
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_original_cell_volume        3859.8(3)
_cod_database_code               1569492
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N S F'
_reflns_odcompleteness_completeness 99.04
_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. Restrained distances
 C15-C13
 1.38 with sigma of 0.01
 C8-C18
 1.38 with sigma of 0.01
 C13-C8
 1.38 with sigma of 0.01
3. Others
 Fixed Sof: H16A(0.5) H16B(0.5) H16C(0.5)
 Fixed X: H16A(0.42864) H16B(0.54318) H16C(0.528171)
 Fixed Y: H16A(-0.00867) H16B(-0.057471) H16C(0.06613)
 Fixed Z: H16A(0.439179) H16B(0.439179) H16C(0.439179)
4.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C12(H12A,H12B), C7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C2(H2), C5(H5), C3(H3), C4(H4), C13(H13), C8(H8), C18(H18)
;
_shelx_res_checksum              85038
_shelx_fab_checksum              94524
_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 1.465
_oxdiff_exptl_absorpt_empirical_full_min 0.284