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_4134802
_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 O9'
_chemical_formula_weight         1017.12
_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                 97.330(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1897(2)
_cell_length_b                   22.9476(4)
_cell_length_c                   11.9706(2)
_cell_measurement_reflns_used    17297
_cell_measurement_temperature    169.99(13)
_cell_measurement_theta_max      72.1900
_cell_measurement_theta_min      3.7060
_cell_volume                     3048.65(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(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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    -76.00  26.00   0.50    0.22    --  -46.70  92.00-131.00  204
  2  \w    -25.00  76.00   0.50    0.22    --   46.70 -92.00 115.00  202
  3  \w   -168.00 -77.00   0.50    0.90    --  -99.00 -92.00 115.00  182
  4  \w   -108.00 -26.00   0.50    0.90    --  -99.00  92.00-131.00  164
  5  \w     84.00 169.00   0.50    0.90    --  103.25  92.00-131.00  170
  6  \w     31.00 108.00   0.50    0.90    --  103.25 -92.00 115.00  154
  7  \w   -118.00 -71.00   0.50    0.22    --  -46.70-125.00-150.00   94
  8  \w   -118.00 -71.00   0.50    0.22    --  -46.70-125.00  90.00   94
  9  \w   -118.00 -71.00   0.50    0.22    --  -46.70-125.00-180.00   94
 10  \w     35.00 120.00   0.50    0.22    --   46.70  38.00  30.00  170
 11  \w    -26.00  59.00   0.50    0.22    --   46.70 -38.00 150.00  170
 12  \w     16.00  94.00   0.50    0.22    --   46.70-125.00 120.00  156
 13  \w     24.00 119.00   0.50    0.22    --   46.70  77.00 -90.00  190
 14  \w   -112.00 -27.00   0.50    0.90    --  -99.00  45.00 120.00  170
 15  \w   -115.00 -26.00   0.50    0.90    --  -99.00  61.00-120.00  178
 16  \w   -117.00 -26.00   0.50    0.90    --  -99.00 125.00  60.00  182
 17  \w   -168.00 -86.00   0.50    0.90    --  -99.00 -30.00  30.00  164
 18  \w     31.00 126.00   0.50    0.90    --  103.25 -77.00 120.00  190
 19  \w     28.00 117.00   0.50    0.90    --  103.25 -15.00  90.00  178
 20  \w     91.00 169.00   0.50    0.90    --  103.25  30.00-150.00  156
 21  \w     31.00 117.00   0.50    0.90    --  103.25-125.00 -30.00  172
 22  \w     31.00 126.00   0.50    0.90    --  103.25 -77.00 -30.00  190
 23  \w     91.00 169.00   0.50    0.90    --  103.25  30.00   0.00  156
 24  \w     87.00 169.00   0.50    0.90    --  103.25  61.00 -90.00  164
 25  \w     31.00 109.00   0.50    0.90    --  103.25 -94.00 -60.00  156
 26  \w     31.00 109.00   0.50    0.90    --  103.25 -94.00  30.00  156
 27  \w     91.00 169.00   0.50    0.90    --  103.25  45.00 150.00  156
 28  \w     91.00 169.00   0.50    0.90    --  103.25  30.00 -30.00  156
 29  \w     24.00 119.00   0.50    0.22    --   46.70  77.00-150.00  190
 30  \w     32.00 119.00   0.50    0.22    --   46.70  57.00  90.00  174
 31  \w     24.00 119.00   0.50    0.22    --   46.70  77.00   0.00  190
 32  \w     24.00  77.00   0.50    0.22    --   46.70  77.00 150.00  106
 33  \w     24.00 119.00   0.50    0.22    --   46.70  77.00 120.00  190
;
_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      -0.0134669000
_diffrn_orient_matrix_UB_12      -0.0609520000
_diffrn_orient_matrix_UB_13      0.0506976000
_diffrn_orient_matrix_UB_21      -0.1374048000
_diffrn_orient_matrix_UB_22      0.0088896000
_diffrn_orient_matrix_UB_23      -0.0088033000
_diffrn_orient_matrix_UB_31      -0.0147335000
_diffrn_orient_matrix_UB_32      -0.0267349000
_diffrn_orient_matrix_UB_33      -0.1190321000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            56240
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.518
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80823
_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    1.108
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 4410 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.87(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         12167
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1593P)^2^+1.2889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2279
_refine_ls_wR_factor_ref         0.2382
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                10849
_reflns_number_total             12167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00624_si_009.cif
_cod_data_source_block           tx1638_sq
_cod_database_code               4134802
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHO
_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.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C34(H34A,H34B), C51(H51A,H51B), C68(H68A,H68B)
2.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), C38(H38), C40(H40), C44(H44),
  C45(H45), C47(H47), C54(H54), C55(H55), C57(H57), C61(H61), C62(H62), C64(H64)
2.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              47185
_shelx_hkl_checksum              54152
_shelx_fab_checksum              26697
_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 1.283
_oxdiff_exptl_absorpt_empirical_full_min 0.574