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_1569487
_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 H28 O8'
_chemical_formula_sum            'C32 H28 O8'
_chemical_formula_weight         540.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-04
_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                72.256(2)
_cell_angle_beta                 77.897(2)
_cell_angle_gamma                64.159(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6793(3)
_cell_length_b                   11.6277(2)
_cell_length_c                   12.1410(3)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    169.98(11)
_cell_measurement_theta_max      75.1190
_cell_measurement_theta_min      3.8230
_cell_volume                     1287.12(6)
_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      169.98(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 0.953
_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    -21.00  27.00   0.50    0.05    --  -47.45  19.00 -30.00   96
  2  \w    -38.00  26.00   0.50    0.05    --  -47.45  38.00-120.00  128
  3  \w    -15.00  25.00   0.50    0.05    --  -47.45  19.00-150.00   80
  4  \w    -38.00  22.00   0.50    0.05    --  -47.45  38.00-180.00  120
  5  \w     79.00 112.00   0.50    0.05    --   47.45 138.00   9.00   66
  6  \w     96.00 121.00   0.50    0.05    --  103.25 138.00   9.00   50
  7  \w     91.00 158.00   0.50    0.05    --  103.25  77.00  90.00  134
  8  \w     95.00 169.00   0.50    0.05    --  103.25  45.00  60.00  148
  9  \w     81.00 166.00   0.50    0.05    --  103.25  77.00 -90.00  170
 10  \w    108.00 167.00   0.50    0.05    --  103.25  45.00-180.00  118
 11  \w     86.00 126.00   0.50    0.05    --  103.25 131.00-165.00   80
 12  \w     42.00  67.00   0.50    0.05    --  103.25 -61.00-180.00   50
 13  \w     34.00  85.00   0.50    0.05    --  103.25 -94.00-180.00  102
 14  \w     57.00 109.00   0.50    0.05    --  103.25-125.00-180.00  104
 15  \w     40.00  65.00   0.50    0.05    --   47.45-138.00 -51.00   50
 16  \w     56.00 113.00   0.50    0.05    --  103.25-138.00 -51.00  114
 17  \w     72.00 106.00   0.50    0.05    --  103.25-125.00  60.00   68
 18  \w     69.00 101.00   0.50    0.05    --  103.25-131.00 123.00   64
 19  \w     68.00 106.00   0.50    0.05    --  103.25 -94.00 150.00   76
 20  \w     58.00  84.00   0.50    0.05    --   47.45-131.00 123.00   52
 21  \w     31.00  91.00   0.50    0.05    --  103.25 -77.00  90.00  120
 22  \w     37.00 111.00   0.50    0.05    --  103.25-125.00 -30.00  148
 23  \w     33.00 109.00   0.50    0.05    --  103.25 -77.00 -60.00  152
 24  \w     31.00  59.00   0.50    0.05    --  103.25 -94.00 150.00   56
 25  \w    -23.00  17.00   0.50    0.05    --  -47.45  19.00 120.00   80
 26  \w    -60.00 -27.00   0.50    0.05    --  -99.00  61.00  60.00   66
 27  \w   -101.00 -55.00   0.50    0.05    --  -47.45 138.00   9.00   92
 28  \w   -121.00 -72.00   0.50    0.05    --  -99.00 138.00   9.00   98
 29  \w    -66.00 -28.00   0.50    0.05    --  -99.00  61.00-120.00   76
 30  \w    -64.00 -35.00   0.50    0.05    --  -99.00  61.00-150.00   58
 31  \w    -78.00 -52.00   0.50    0.05    --  -47.45 131.00-165.00   52
 32  \w    -95.00 -70.00   0.50    0.05    --  -99.00 131.00-165.00   50
 33  \w   -125.00 -60.00   0.50    0.05    --  -99.00 143.00-177.55  130
 34  \w   -125.00 -91.00   0.50    0.05    --  -99.00 -30.00-120.00   68
 35  \w   -106.00 -79.00   0.50    0.05    --  -47.45-125.00-180.00   54
 36  \w   -108.00 -82.00   0.50    0.05    --  -99.00-125.00-120.00   52
 37  \w   -119.00 -69.00   0.50    0.05    --  -47.45-138.00 -51.00  100
 38  \w   -137.00 -80.00   0.50    0.05    --  -99.00 -77.00   0.00  114
 39  \w   -119.00 -94.00   0.50    0.05    --  -47.45-131.00 123.00   50
 40  \w   -119.00 -87.00   0.50    0.05    --  -99.00-131.00 123.00   64
 41  \w   -167.00-104.00   0.50    0.05    --  -99.00 -30.00   0.00  126
 42  \w   -159.00-134.00   0.50    0.05    --  -99.00 -30.00-120.00   50
 43  \w   -166.00-132.00   0.50    0.05    --  -99.00-125.00-120.00   68
 44  \w   -136.00-109.00   0.50    0.05    --  -99.00-138.00 -51.00   54
;
_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      0.0315995000
_diffrn_orient_matrix_UB_12      -0.0213985000
_diffrn_orient_matrix_UB_13      0.1245351000
_diffrn_orient_matrix_UB_21      0.1118776000
_diffrn_orient_matrix_UB_22      0.0570782000
_diffrn_orient_matrix_UB_23      -0.0486835000
_diffrn_orient_matrix_UB_31      -0.1112837000
_diffrn_orient_matrix_UB_32      0.1389569000
_diffrn_orient_matrix_UB_33      0.0037561000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16920
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.332
_diffrn_reflns_theta_min         3.838
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87821
_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    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0711P)^2^+0.6296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4600
_reflns_number_total             5085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           tx5203
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_database_code               1569487
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O'
_reflns_odcompleteness_completeness 99.91
_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:
 C00W(H00A,H00B), C00Y(H00C,H00E), C00Z(H00H,H00I), C014(H01G,H01H)
2.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00F(H00F), C00G(H00G), C00K(H00K), C00M(H00M), C00P(H00P),
 C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00X(H00X),
 C011(H011), C013(H013)
2.c Idealised Me refined as rotating group:
 C010(H01A,H01B,H01C), C012(H01D,H01E,H01F)
;
_shelx_res_checksum              95975
_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 1.160
_oxdiff_exptl_absorpt_empirical_full_min 0.859