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_1569495
_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         'C42 H34 N8 O6 S2, C2 H4 Cl2'
_chemical_formula_sum            'C44 H38 Cl2 N8 O6 S2'
_chemical_formula_weight         909.84
_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
_audit_creation_date             2023-02-19
_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                 90.3860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.3087(3)
_cell_length_b                   11.0893(2)
_cell_length_c                   37.4232(5)
_cell_measurement_reflns_used    38401
_cell_measurement_temperature    105(4)
_cell_measurement_theta_max      66.9540
_cell_measurement_theta_min      4.0680
_cell_volume                     8842.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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    -19.00   6.00   0.50    0.79    --    0.70  30.00  12.00   50
  2  \w    -62.00 -25.00   0.50    0.79    --    0.70  30.00  12.00   74
  3  \w      5.00  30.00   0.50    2.50    --   90.00  30.00  12.00   50
  4  \w     -1.00  24.00   0.50    0.79    --   -0.70  30.00  12.00   50
  5  \w    -88.00  56.00   0.50    0.79    --    0.70  28.00 -90.00  288
  6  \w     62.00  89.00   0.50    0.79    --    0.70  28.00 -90.00   54
  7  \w    138.00 173.00   0.50    2.50    --   90.00  46.00-120.00   70
  8  \w     54.00  99.00   0.50    2.50    --   90.00  37.00-180.00   90
  9  \w      8.00  47.00   0.50    2.50    --   90.00  46.00 120.00   78
 10  \w     80.00 106.00   0.50    2.50    --   90.00  46.00-120.00   52
 11  \w    132.00 161.00   0.50    2.50    --   90.00  46.00 120.00   58
 12  \w    105.00 131.00   0.50    2.50    --   90.00  28.00 -90.00   52
 13  \w    144.00 170.00   0.50    2.50    --   90.00  28.00 -90.00   52
 14  \w      1.00  63.00   0.50    2.50    --   90.00  18.00 -30.00  124
 15  \w    154.00 179.00   0.50    2.50    --   90.00  37.00-180.00   50
 16  \w    116.00 179.00   0.50    2.50    --   90.00   0.00-150.00  126
 17  \w    131.00 157.00   0.50    2.50    --   90.00  28.00  30.00   52
 18  \w      4.00  30.00   0.50    2.50    --   90.00  18.00  60.00   52
 19  \w      1.00 107.00   0.50    2.50    --   90.00  54.00  98.59  212
 20  \w     77.00 103.00   0.50    2.50    --   90.00  18.00  60.00   52
 21  \w      2.00  80.00   0.50    2.50    --   90.00  37.00  90.00  156
 22  \w    111.00 136.00   0.50    2.50    --   90.00  37.00  90.00   50
 23  \w     22.00 169.00   0.50    2.50    --   90.00  46.00 150.00  294
 24  \w      6.00  89.00   0.50    2.50    --   90.00  46.00-150.00  166
 25  \w    151.00 177.00   0.50    2.50    --   90.00  46.00-150.00   52
 26  \w     73.00  99.00   0.50    2.50    --   90.00  46.00 120.00   52
 27  \w    114.00 179.00   0.50    2.50    --   90.00  18.00 -30.00  130
 28  \w      4.00  30.00   0.50    2.50    --   90.00  28.00 120.00   52
 29  \w    142.00 168.00   0.50    2.50    --   90.00  28.00 120.00   52
 30  \w     15.00  40.00   0.50    2.50    --   90.00  46.00-120.00   50
 31  \w      3.00 156.00   0.50    2.50    --   90.00  46.00   0.00  306
 32  \w    140.00 171.00   0.50    2.50    --   90.00  30.00  12.00   62
 33  \w      4.00  45.00   0.50    2.50    --   90.00  18.00 150.00   82
 34  \w      5.00  31.00   0.50    2.50    --   90.00  37.00 -60.00   52
 35  \w     36.00  61.00   0.50    2.50    --   90.00  37.00 -60.00   50
 36  \w     90.00 115.00   0.50    2.50    --   90.00  37.00 -60.00   50
 37  \w     27.00  52.00   0.50    2.50    --   90.00   9.00 -60.00   50
 38  \w    154.00 179.00   0.50    2.50    --   90.00  28.00-150.00   50
 39  \w    149.00 176.00   0.50    2.50    --   90.00  46.00-180.00   54
 40  \w      1.00  29.00   0.50    2.50    --   90.00  47.00 129.10   56
 41  \w     55.00 125.00   0.50    2.50    --   90.00  30.00  12.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0453178000
_diffrn_orient_matrix_UB_12      -0.0148784000
_diffrn_orient_matrix_UB_13      -0.0319757000
_diffrn_orient_matrix_UB_21      -0.0511270000
_diffrn_orient_matrix_UB_22      0.0689103000
_diffrn_orient_matrix_UB_23      0.0205826000
_diffrn_orient_matrix_UB_31      0.0236388000
_diffrn_orient_matrix_UB_32      0.1196221000
_diffrn_orient_matrix_UB_33      -0.0158324000
_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  0.1147
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            101790
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.490
_diffrn_reflns_theta_max         67.490
_diffrn_reflns_theta_min         4.095
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.679
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.78a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       plate
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         15613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0769
_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^)+(0.1095P)^2^+14.0924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2023
_refine_ls_wR_factor_ref         0.2115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13138
_reflns_number_total             15613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02417b2.cif
_cod_data_source_block           gsy1463dcehex-2_sq
_cod_depositor_comments
'Adding full bibliography for 1569486--1569506.cif.'
_cod_database_code               1569495
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N S'
_reflns_odcompleteness_completeness 98.90
_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:
 C01J(H01A,H01B), C01S(H01C,H01D), C01T(H01E,H01H), C01W(H01I,H01J), C01X(H01L,
 H01P), C02M(H02M,H02N), C02N(H02A,H02B), C02X(H02C,H02E), C02Y(H02F,H02I),
 C030(H03A,H03B), C032(H03C,H03D), C033(H03E,H03F), C034(H03G,H03H), C036(H03I,
 H03J), C03A(H03K,H03L), C03E(H03P,H03Q), C03F(H03V,H03W), C03G(H03X,H03Y),
 C03H(H03R,H03S), C03I(H03T,H03U)
2.b Aromatic/amide H refined with riding coordinates:
 C00X(H00X), C013(H013), C017(H017), C018(H018), C01F(H01F), C01G(H01G),
 C01K(H01K), C01M(H01M), C01N(H01N), C01O(H01O), C01Q(H01Q), C01R(H01R),
 C021(H021), C025(H025), C027(H027), C029(H029), C02D(H02D), C02F(H02L),
 C02G(H02G), C02H(H02H), C02J(H02J), C02K(H02K), C02O(H02O), C02Q(H02Q),
 C02R(H02R), C02T(H02T), C02U(H02U), C02V(H02V), C02Z(H02Z), C031(H031),
 C035(H035), C037(H037), C038(H038), C03B(H03M), C03C(H03N), C03D(H03O)
;
_shelx_res_checksum              49510
_shelx_fab_checksum              92191
_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 3.394
_oxdiff_exptl_absorpt_empirical_full_min 0.371