Pagoda[4]arene and <i>i</i>-Pagoda[4]arene.
Han, Xiao-Ni; Han, Ying; Chen, Chuan-Feng; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00624

data_4134809
_publ_section_title
;
 Pagoda[4]arene and <i>i</i>-Pagoda[4]arene.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00624
_journal_year                    2020
_chemical_formula_moiety         'C68 H56 O8'
_chemical_formula_sum            'C68 H56 O8'
_chemical_formula_weight         1001.12
_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             2019-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                86.3060(10)
_cell_angle_beta                 82.7190(10)
_cell_angle_gamma                75.013(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2952(2)
_cell_length_b                   16.2834(3)
_cell_length_c                   16.3725(2)
_cell_measurement_reflns_used    8531
_cell_measurement_temperature    169.99(16)
_cell_measurement_theta_max      73.6760
_cell_measurement_theta_min      2.7220
_cell_volume                     2883.84(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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      169.99(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.956
_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    -25.00  59.00   0.50    3.59    --   47.20 -19.00   0.00  168
  2  \w     31.00  64.00   0.50   15.00    --  103.25 -91.00  -1.00   66
  3  \w     54.00  80.00   0.50   15.00    --  103.25 -94.00  60.00   52
  4  \w     87.00 133.00   0.50   15.00    --  103.25 -91.00  -1.00   92
  5  \w    112.00 166.00   0.50   15.00    --  103.25  15.00 -90.00  108
  6  \w     97.00 162.00   0.50   15.00    --  103.25 125.00  60.00  130
  7  \w     93.00 120.00   0.50   15.00    --  103.25  91.00 112.00   54
  8  \w    133.00 160.00   0.50   15.00    --  103.25  30.00 150.00   54
  9  \w     92.00 118.00   0.50   15.00    --  103.25  30.00 150.00   52
 10  \w     91.00 143.00   0.50   15.00    --  103.25  15.00  60.00  104
 11  \w     77.00 152.00   0.50   15.00    --  103.25 125.00 -60.00  150
 12  \w     93.00 168.00   0.50   15.00    --  103.25  30.00-120.00  150
 13  \w     54.00 117.00   0.50   15.00    --  103.25-125.00 -60.00  126
 14  \w     36.00 116.00   0.50   15.00    --  103.25-125.00 -30.00  160
 15  \w     32.00 106.00   0.50   15.00    --  103.25 -94.00-180.00  148
 16  \w     31.00  95.00   0.50   15.00    --  103.25 -94.00-150.00  128
 17  \w     18.00  79.00   0.50    3.59    --   47.20-125.00-150.00  122
 18  \w    -23.00  33.00   0.50    3.59    --   47.20 -91.00  -1.00  112
 19  \w     31.00 110.00   0.50   15.00    --  103.25 -77.00  60.00  158
 20  \w    -26.00  60.00   0.50    3.59    --   47.20 -38.00 -90.00  172
 21  \w    -72.00  14.00   0.50    3.59    --  -47.20  91.00 112.00  172
 22  \w    -73.00 -47.00   0.50   15.00    --  -99.00  91.00 112.00   52
 23  \w   -115.00 -26.00   0.50   15.00    --  -99.00  61.00 120.00  178
 24  \w    -53.00 -26.00   0.50   15.00    --  -99.00  30.00 -30.00   54
 25  \w   -116.00 -78.00   0.50   15.00    --  -99.00 125.00   0.00   76
 26  \w   -112.00 -61.00   0.50   15.00    --  -99.00  30.00 -30.00  102
 27  \w   -167.00 -77.00   0.50   15.00    --  -99.00 -91.00  -1.00  180
 28  \w    -99.00 -72.00   0.50    3.59    --  -47.20-125.00  30.00   54
 29  \w   -111.00 -76.00   0.50    3.59    --  -47.20-125.00-120.00   70
 30  \w   -168.00 -93.00   0.50   15.00    --  -99.00-125.00-120.00  150
;
_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      0.0798009000
_diffrn_orient_matrix_UB_12      0.0375899000
_diffrn_orient_matrix_UB_13      0.0493403000
_diffrn_orient_matrix_UB_21      -0.0147320000
_diffrn_orient_matrix_UB_22      -0.0639950000
_diffrn_orient_matrix_UB_23      0.0716763000
_diffrn_orient_matrix_UB_31      0.1166778000
_diffrn_orient_matrix_UB_32      -0.0639885000
_diffrn_orient_matrix_UB_33      -0.0378974000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36076
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.686
_diffrn_reflns_theta_min         2.722
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         11466
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0818
_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^)+(0.1712P)^2^+0.1611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7044
_reflns_number_total             11466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00624_si_003.cif
_cod_data_source_block           tx1330_sq
_cod_database_code               4134809
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOCl
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.865
_reflns_odcompleteness_completeness 99.96
_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. Rigid bond restraints
 O5, C45
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C43, C48
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
3. Uiso/Uaniso restraints and constraints
C37: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
4.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C34(H34A,H34B), C51(H51A,H51B), C68(H68A,H68B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C10(H10), C11(H11), C13(H13), C20(H20), C21(H21),
 C23(H23), C27(H27), C28(H28), C30(H30), C37(H37), C39(H39), C40(H40), C42(H42),
  C46(H46), C47(H47), C54(H54), C55(H55), C57(H57), C61(H61), C62(H62), C64(H64)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C)
;
_shelx_res_checksum              41575
_shelx_hkl_checksum              55047
_shelx_fab_checksum              75254
_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 2.536
_oxdiff_exptl_absorpt_empirical_full_min 0.600