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_4134804
_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      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.123(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2300(2)
_cell_length_b                   22.9910(6)
_cell_length_c                   11.9920(3)
_cell_measurement_reflns_used    14654
_cell_measurement_temperature    170.01(12)
_cell_measurement_theta_max      71.3000
_cell_measurement_theta_min      3.8310
_cell_volume                     3072.31(12)
_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      170.01(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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    -73.00  26.00   0.50    0.06    --  -46.95  85.00 111.00  198
  2  \w    -25.00  73.00   0.50    0.06    --   46.95 -85.00  -7.00  196
  3  \w   -168.00 -76.00   0.50    0.30    --  -99.00 -85.00  -7.00  184
  4  \w   -125.00 -26.00   0.50    0.30    --  -99.00  85.00 111.00  198
  5  \w     83.00 169.00   0.50    0.30    --  103.25  85.00 111.00  172
  6  \w     31.00 130.00   0.50    0.30    --  103.25 -85.00  -7.00  198
  7  \w   -118.00 -32.00   0.50    0.06    --  -46.95 -57.00  30.00  172
  8  \w   -119.00 -71.00   0.50    0.06    --  -46.95-125.00-180.00   96
  9  \w   -119.00 -71.00   0.50    0.06    --  -46.95-125.00  60.00   96
 10  \w    -26.00  60.00   0.50    0.06    --   46.95 -38.00   0.00  172
 11  \w     32.00 118.00   0.50    0.06    --   46.95  57.00 150.00  172
 12  \w    -27.00  60.00   0.50    0.06    --   46.95 -19.00  60.00  174
 13  \w   -117.00 -26.00   0.50    0.30    --  -99.00 125.00  90.00  182
 14  \w   -112.00 -24.00   0.50    0.30    --  -99.00  30.00   0.00  176
 15  \w   -115.00 -26.00   0.50    0.30    --  -99.00  61.00   0.00  178
 16  \w   -115.00 -26.00   0.50    0.30    --  -99.00  61.00 120.00  178
 17  \w   -168.00 -85.00   0.50    0.30    --  -99.00 -15.00 120.00  166
 18  \w   -117.00 -26.00   0.50    0.30    --  -99.00 125.00  30.00  182
 19  \w   -168.00 -85.00   0.50    0.30    --  -99.00 -15.00-150.00  166
 20  \w   -168.00 -86.00   0.50    0.30    --  -99.00 -30.00 -60.00  164
 21  \w   -113.00 -24.00   0.50    0.30    --  -99.00  15.00 120.00  178
 22  \w   -168.00 -85.00   0.50    0.30    --  -99.00 -15.00-120.00  166
 23  \w   -168.00 -76.00   0.50    0.30    --  -99.00 -77.00-150.00  184
 24  \w     87.00 169.00   0.50    0.30    --  103.25  61.00  60.00  164
 25  \w     91.00 169.00   0.50    0.30    --  103.25  45.00-180.00  156
 26  \w     31.00 109.00   0.50    0.30    --  103.25 -94.00 -90.00  156
 27  \w     91.00 169.00   0.50    0.30    --  103.25  45.00  90.00  156
 28  \w     31.00 109.00   0.50    0.30    --  103.25 -94.00 -30.00  156
 29  \w     90.00 169.00   0.50    0.30    --  103.25  15.00  60.00  158
 30  \w   -119.00 -24.00   0.50    0.06    --  -46.95 -77.00 -30.00  190
 31  \w     24.00  90.00   0.50    0.06    --   46.95  77.00  60.00  132
;
_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      -0.1150803000
_diffrn_orient_matrix_UB_12      0.0372273000
_diffrn_orient_matrix_UB_13      -0.0151960000
_diffrn_orient_matrix_UB_21      0.0653880000
_diffrn_orient_matrix_UB_22      0.0465476000
_diffrn_orient_matrix_UB_23      -0.0618487000
_diffrn_orient_matrix_UB_31      -0.0400115000
_diffrn_orient_matrix_UB_32      -0.0306639000
_diffrn_orient_matrix_UB_33      -0.1126354000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            57488
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.633
_diffrn_reflns_theta_min         3.715
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51332
_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            'light yellow'
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 4408 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.26(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         12214
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0815
_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^)+(0.1550P)^2^+1.4186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2363
_refine_ls_wR_factor_ref         0.2417
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.937
_reflns_number_gt                11027
_reflns_number_total             12214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00624_si_010.cif
_cod_data_source_block           tx1640_sq
_cod_database_code               4134804
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHO
_reflns_odcompleteness_completeness 99.98
_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
 H2-H15B
 2.1 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C34(H34A,H34B), C51(H51A,H51B), C68(H68A,H68B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C12(H12), C20(H20), C21(H21),
 C23(H23), C27(H27), C28(H28), C30(H30), C37(H37), C39(H39), C40(H40), C44(H44),
  C46(H46), C47(H47), C54(H54), C56(H56), C57(H57), C61(H61), C63(H63), C64(H64)
3.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              95505
_shelx_hkl_checksum              98868
_shelx_fab_checksum              29451
_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 2.098
_oxdiff_exptl_absorpt_empirical_full_min 0.520