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_1569498
_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_absolute_configuration ad
_chemical_formula_moiety         'C36 H36 O8'
_chemical_formula_sum            'C36 H36 O8'
_chemical_formula_weight         596.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-07
_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            4
_cell_length_a                   10.6803(7)
_cell_length_b                   12.0458(8)
_cell_length_c                   23.3062(19)
_cell_measurement_reflns_used    20515
_cell_measurement_temperature    112(8)
_cell_measurement_theta_max      77.3460
_cell_measurement_theta_min      3.8260
_cell_volume                     2998.4(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      112(8)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_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     35.00  68.00   0.50    0.08    --  106.93 -57.00-180.00   66
  2  \w     35.00 105.00   0.50    0.08    --  106.93 -97.00 -58.00  140
  3  \w     35.00 107.00   0.50    0.08    --  106.93 -77.00 -30.00  144
  4  \w    -24.00  26.00   0.50    0.05    --  -48.14  19.00   0.00  100
  5  \w    -24.00  26.00   0.50    0.05    --  -48.14  19.00  60.00  100
  6  \w     35.00  68.00   0.50    0.08    --  106.93 -57.00  60.00   66
  7  \w     35.00  68.00   0.50    0.08    --  106.93 -57.00  30.00   66
  8  \w     35.00  68.00   0.50    0.08    --  106.93 -57.00 150.00   66
  9  \w     96.00 178.00   0.50    0.08    --  106.93  19.00 120.00  164
 10  \w     96.00 178.00   0.50    0.08    --  106.93  38.00   0.00  164
 11  \w     95.00 178.00   0.50    0.08    --  106.93  47.00 -51.00  166
 12  \w     27.00 120.00   0.50    0.05    --   48.14  77.00-180.00  186
 13  \w     37.00 120.00   0.50    0.05    --   48.14  47.00 -51.00  166
 14  \w     34.00  98.00   0.50    0.05    --   48.14  57.00   0.00  128
 15  \w     34.00 120.00   0.50    0.05    --   48.14  57.00  60.00  172
 16  \w    -64.00 -32.00   0.50    0.08    -- -104.00  57.00  90.00   64
 17  \w    -64.00 -32.00   0.50    0.08    -- -104.00  57.00  60.00   64
 18  \w    -64.00 -32.00   0.50    0.08    -- -104.00  57.00   0.00   64
 19  \w    -64.00 -32.00   0.50    0.08    -- -104.00  57.00 -30.00   64
 20  \w   -175.00 -90.00   0.50    0.08    -- -104.00 -57.00 -90.00  170
 21  \w   -120.00 -73.00   0.50    0.05    --  -48.14-125.00 -90.00   94
 22  \w   -129.00 -32.00   0.50    0.08    -- -104.00  84.00 156.00  194
;
_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      -0.1349768000
_diffrn_orient_matrix_UB_12      -0.0424666000
_diffrn_orient_matrix_UB_13      0.0073840000
_diffrn_orient_matrix_UB_21      0.0099357000
_diffrn_orient_matrix_UB_22      -0.0620612000
_diffrn_orient_matrix_UB_23      -0.0575602000
_diffrn_orient_matrix_UB_31      0.0495304000
_diffrn_orient_matrix_UB_32      -0.1036301000
_diffrn_orient_matrix_UB_33      0.0315467000
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25654
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.000
_diffrn_reflns_theta_min         4.131
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56712
_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_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 2565 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_coef       0.0036(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         6203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0381P)^2^+0.9130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                6085
_reflns_number_total             6203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           5d-a-dcm-hex-3_auto
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_database_code               1569498
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O'
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C27(H27), C33(H33)
1.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C7(H7A,H7B), C18(H18A,H18B), C14(H14A,H14B)
1.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C5(H5), C44(H44), C23(H23), C43(H43), C16(H16), C37(H37), C40(H40),
 C11(H11), C41(H41), C10(H10), C42(H42), C39(H39), C38(H38)
1.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C34(H34A,H34B,H34C), C29(H29A,H29B,H29C), C35(H35A,H35B,
 H35C)
;
_shelx_res_checksum              70807
_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 1.724
_oxdiff_exptl_absorpt_empirical_full_min 0.802