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_4134808
_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, 1.5(C6 H14)'
_chemical_formula_sum            'C77 H77 O8'
_chemical_formula_weight         1130.38
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.2060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8713(2)
_cell_length_b                   21.3316(3)
_cell_length_c                   24.2532(4)
_cell_measurement_reflns_used    9318
_cell_measurement_temperature    169.98(16)
_cell_measurement_theta_max      72.1840
_cell_measurement_theta_min      2.7730
_cell_volume                     6044.55(17)
_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      169.98(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.935
_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     13.00  39.00   0.50    2.34    --   47.20 -92.00 134.00   52
  2  \w     31.00 107.00   0.50   11.50    --  103.25 -92.00 134.00  152
  3  \w     33.00 115.00   0.50   11.50    --  103.25-125.00 120.00  164
  4  \w     66.00  94.00   0.50    2.34    --   47.20  38.00   0.00   56
  5  \w     85.00 128.00   0.50   11.50    --  103.25  92.00-112.00   86
  6  \w     92.00 128.00   0.50   11.50    --  103.25  45.00 -90.00   72
  7  \w    139.00 164.00   0.50   11.50    --  103.25  45.00 -90.00   50
  8  \w     99.00 137.00   0.50   11.50    --  103.25  45.00-150.00   76
  9  \w     91.00 169.00   0.50   11.50    --  103.25  45.00  30.00  156
 10  \w     38.00 108.00   0.50   11.50    --  103.25 -94.00-120.00  140
 11  \w    -77.00  25.00   0.50    2.34    --  -47.20  92.00-112.00  204
 12  \w    -79.00 -53.00   0.50   11.50    --  -99.00  92.00-112.00   52
 13  \w   -155.00 -86.00   0.50   11.50    --  -99.00 -45.00-150.00  138
 14  \w   -163.00 -82.00   0.50   11.50    --  -99.00 -61.00-180.00  162
 15  \w   -149.00-115.50   0.50   11.50    --  -99.00 -92.00 134.00   67
;
_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      0.0295418000
_diffrn_orient_matrix_UB_12      0.0651762000
_diffrn_orient_matrix_UB_13      0.0258701000
_diffrn_orient_matrix_UB_21      0.0790459000
_diffrn_orient_matrix_UB_22      0.0122749000
_diffrn_orient_matrix_UB_23      -0.0428348000
_diffrn_orient_matrix_UB_31      -0.1012973000
_diffrn_orient_matrix_UB_32      0.0286033000
_diffrn_orient_matrix_UB_33      -0.0407639000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            36134
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.514
_diffrn_reflns_theta_min         2.778
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45893
_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    1.242
_exptl_crystal_description       needle
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1491
_refine_ls_number_reflns         11722
_refine_ls_number_restraints     265
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0637
_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^)+(0.1219P)^2^+0.6383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.2054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7767
_reflns_number_total             11722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00624_si_002.cif
_cod_data_source_block           tx1497
_cod_database_code               4134808
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHO
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.802
_reflns_odcompleteness_completeness 96.71
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C23A-C24A = C24A-C29A = C30A-C29A = C31A-C30A = C23A-C22A = C25A-C24A = C28A-
 C29A
 1.39 with sigma of 0.01
 C13A-C14A = C4A-C13A = C4A-C3A = C5A-C4A = C12A-C13A = C11A-C12A = C5A-C6A
 1.39 with sigma of 0.01
 C48A-C47A = C39A-C48A = C39A-C38A = C40A-C39A = C40A-C41A = C35A-C40A = C38A-
 C37A
 1.39 with sigma of 0.01
 C65A-C52A = C53A-C52A = C65A-C56A = C56A-C57A = C64A-C65A = C56A-C55A
 1.39 with sigma of 0.01
 C70-C69 = C71-C70 = C72-C71 = C73-C72 = C74-C73 = C74A-C73A = C73A-C72A =
 C72A-C71A = C71A-C70A = C70A-C69A
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C69A \\sim C70A
\\sim C71A \\sim C72A \\sim C73A \\sim C74A: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C69A) \\sim Ueq,
Uanis(C70A) \\sim Ueq, Uanis(C71A) \\sim Ueq, Uanis(C72A) \\sim Ueq,
Uanis(C73A) \\sim Ueq, Uanis(C74A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=
 Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(C7A)=Sof(C8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=
 Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(C14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(H17C)=Sof(H17D)=
 Sof(C18A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(C25A)=Sof(C26A)=Sof(C27A)=Sof(H27A)=
 Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(C32A)=
 Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=
 Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(C36A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=
 Sof(H38A)=Sof(C39A)=Sof(C40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(C43A)=
 Sof(H43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(C46A)=Sof(C47A)=Sof(C48A)=
 Sof(H48A)=Sof(C49A)=Sof(H49D)=Sof(H49E)=Sof(H49F)=Sof(C50A)=Sof(H50D)=
 Sof(H50E)=Sof(H50F)=Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(C53A)=Sof(C54A)=
 Sof(H54A)=Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(C57A)=Sof(H57A)=Sof(C58A)=
 Sof(C59A)=Sof(C60A)=Sof(C61A)=Sof(H61A)=Sof(C62A)=Sof(H62A)=Sof(C63A)=
 Sof(C64A)=Sof(H64A)=Sof(C65A)=Sof(C66A)=Sof(H66D)=Sof(H66E)=Sof(H66F)=
 Sof(C67A)=Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(H68C)=Sof(H68D)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=Sof(C2)=
 Sof(C2EA)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=
 Sof(C8)=Sof(C9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(C13)=Sof(H13)=
 Sof(C14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=
 Sof(H21)=Sof(C22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(C25)=Sof(C26)=Sof(C27)=
 Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(C32)=
 Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(H34A)=
 Sof(H34B)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(C42)=Sof(C43)=Sof(C44)=Sof(H44)=Sof(C45)=
 Sof(H45)=Sof(C46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(C49)=Sof(H49A)=Sof(H49B)=
 Sof(H49C)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(H51A)=Sof(H51B)=Sof(C52)=
 Sof(C53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(C57)=Sof(H57)=
 Sof(C58)=Sof(C59)=Sof(C60)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=
 Sof(C64)=Sof(H64)=Sof(C65)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C67)=
 Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(H68A)=Sof(H68B)=FVAR(1)
 Sof(C69A)=Sof(H69D)=Sof(H69E)=Sof(H69F)=Sof(C70A)=Sof(H70C)=Sof(H70D)=
 Sof(C71A)=Sof(H71C)=Sof(H71D)=Sof(C72A)=Sof(H72C)=Sof(H72D)=Sof(C73A)=
 Sof(H73C)=Sof(H73D)=Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(2)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=
 Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=Sof(H73A)=Sof(H73B)=
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C17(H17C,H17D), C34(H34A,H34B), C34(H34C,H34D), C51(H51A,
 H51B), C51(H51C,H51D), C68(H68A,H68B), C68(H68C,H68D), C70(H70A,H70B),
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C76(H76A,H76B), C77(H77A,H77B),
  C70A(H70C,H70D), C71A(H71C,H71D), C72A(H72C,H72D), C73A(H73C,H73D)
5.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3(H3), C3A(H3A), C4(H4), C5A(H5A), C6(H6), C9A(H9A), C10(H10),
 C10A(H10A), C11(H11), C12A(H12A), C13(H13), C20(H20), C20A(H20A), C21(H21),
 C21A(H21A), C23(H23), C23A(H23A), C27(H27), C27A(H27A), C28(H28), C28A(H28A),
 C30(H30), C30A(H30A), C37(H37), C37A(H37A), C38(H38), C38A(H38A), C40(H40),
 C41A(H41A), C43A(H43A), C44(H44), C44A(H44A), C45(H45), C47(H47), C48A(H48A),
 C54(H54), C54A(H54A), C55(H55), C55A(H55A), C57(H57), C57A(H57A), C61(H61),
 C61A(H61A), C62(H62), C62A(H62A), C64(H64), C64A(H64A)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F), C16(H16A,H16B,H16C), C16A(H16D,
 H16E,H16F), C32(H32A,H32B,H32C), C32A(H32D,H32E,H32F), C33(H33A,H33B,H33C),
 C33A(H33D,H33E,H33F), C49(H49A,H49B,H49C), C49A(H49D,H49E,H49F), C50(H50A,H50B,
 H50C), C50A(H50D,H50E,H50F), C66(H66A,H66B,H66C), C66A(H66D,H66E,H66F),
 C67(H67A,H67B,H67C), C67A(H67D,H67E,H67F), C69(H69A,H69B,H69C), C74(H74A,H74B,
 H74C), C75(H75A,H75B,H75C), C69A(H69D,H69E,H69F), C74A(H74D,H74E,H74F)
;
_shelx_res_checksum              69453
_shelx_hkl_checksum              56316
_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 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.500