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_4134807
_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         'F6 P, 1(C68 H56 O8), C5 H9 N2'
_chemical_formula_sum            'C73 H65 F6 N2 O8 P'
_chemical_formula_weight         1243.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.989(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5277(3)
_cell_length_b                   25.8886(4)
_cell_length_c                   21.7575(5)
_cell_measurement_reflns_used    9228
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      73.4770
_cell_measurement_theta_min      2.6520
_cell_volume                     6351.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_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    -51.00  16.00   0.50    1.00    --  -47.20  84.00 -24.00  134
  2  \w    -40.00  22.00   0.50    1.00    --  -47.20  38.00  90.00  124
  3  \w    -68.00 -43.00   0.50    4.50    --  -99.00  61.00  90.00   50
  4  \w    -76.00 -46.00   0.50    4.50    --  -99.00  84.00 -24.00   60
  5  \w    -66.00 -26.00   0.50    4.50    --  -99.00  61.00 -30.00   80
  6  \w    -67.00 -26.00   0.50    4.50    --  -99.00  61.00-180.00   82
  7  \w   -117.00 -80.00   0.50    4.50    --  -99.00 -84.00-145.00   74
  8  \w   -108.00 -81.00   0.50    1.00    --  -47.20-125.00 -60.00   54
  9  \w   -105.00 -75.00   0.50    1.00    --  -47.20-125.00   0.00   60
 10  \w    -24.00  60.00   0.50    1.00    --   47.20 -84.00-145.00  168
 11  \w     32.00 129.00   0.50    4.50    --  103.25 -84.00-145.00  194
 12  \w     97.00 157.00   0.50    4.50    --  103.25  45.00-120.00  120
 13  \w    142.00 168.00   0.50    4.50    --  103.25  61.00-120.00   52
 14  \w    114.00 168.00   0.50    4.50    --  103.25  45.00 -60.00  108
 15  \w    127.00 152.00   0.50    4.50    --  103.25  84.00 -24.00   50
 16  \w     99.00 167.00   0.50    4.50    --  103.25  45.00 -90.00  136
 17  \w     98.00 128.00   0.50    4.50    --  103.25  61.00-120.00   60
 18  \w     99.00 136.00   0.50    4.50    --  103.25  45.00-180.00   74
 19  \w     95.00 127.00   0.50    4.50    --  103.25  61.00-180.00   64
 20  \w     43.00  70.00   0.50    4.50    --  103.25 -61.00-120.00   54
 21  \w     42.00  68.00   0.50    4.50    --  103.25 -94.00 -60.00   52
 22  \w     32.00  67.00   0.50    4.50    --  103.25 -61.00   0.00   70
 23  \w     35.00  60.00   0.50    4.50    --  103.25 -61.00  60.00   50
 24  \w     40.00  75.00   0.50    4.50    --  103.25 -61.00  90.00   70
 25  \w   -102.00 -75.00   0.50    1.00    --  -47.20-125.00-180.00   54
 26  \w   -168.00-128.00   0.50    4.50    --  -99.00 -84.00-145.00   80
;
_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      -0.1335985000
_diffrn_orient_matrix_UB_12      0.0043895000
_diffrn_orient_matrix_UB_13      -0.0008781000
_diffrn_orient_matrix_UB_21      -0.0216233000
_diffrn_orient_matrix_UB_22      -0.0521253000
_diffrn_orient_matrix_UB_23      -0.0346440000
_diffrn_orient_matrix_UB_31      0.0188062000
_diffrn_orient_matrix_UB_32      -0.0283956000
_diffrn_orient_matrix_UB_33      0.0635351000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46929
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.610
_diffrn_reflns_theta_min         2.688
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       cube
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
TITL tx1988_a.res in P2(1)/c
CELL   11.5277   25.8886   21.7575     90.00    101.99     90.00
SPGR P21/c
C101 0.369 0.038 0.445 !       1.91 eA-3
C102 0.983 1.000 0.445 !       1.82 eA-3
C103 0.379 0.095 0.471 !       1.67 eA-3
C104 0.932 0.966 0.510 !       1.43 eA-3
C105 0.930 0.994 0.400 !       1.30 eA-3
Q106 0.602 0.555 0.093 !       1.06 eA-3
Q107 0.568 0.538 0.110 !       1.01 eA-3
;
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1514
_refine_ls_number_reflns         12753
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0895
_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^)+(0.1084P)^2^+4.5125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2342
_refine_ls_wR_factor_ref         0.2557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8612
_reflns_number_total             12753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00624_si_008.cif
_cod_data_source_block           tx1988_sq
_cod_database_code               4134807
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONPFCl
_reflns_odcompleteness_completeness 99.79
_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
 C31A-C30A = C31A-C18A = C31A-C22A = C22A-C21A = C23A-C22A = C19A-C18A = C20A-
 C19A = C21A-C20A = C30A-C29A = C29A-C24A = C24A-C23A = C29A-C28A = C28A-C27A =
 C27A-C26A = C26A-C25A = C25A-C24A
 1.39 with sigma of 0.01
 C4A-C3A = C4A-C13A = C3A-C2A = C2A-C1A = C1A-C14A = C14A-C13A = C5A-C4A = C6A-
 C5A = C6A-C11A = C12A-C11A = C13A-C12A
 1.39 with sigma of 0.01
 C17A-C14A = C34-C25 = C18A-C17A = C35-C34
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C40 \\sim C41 \\sim C42 \\sim C39 \\sim C38 \\sim C43 \\sim C37 \\sim C44:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C11A) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C23A) \\sim Ueq,
Uanis(C41A) \\sim Ueq, Uanis(C40A) \\sim Ueq, Uanis(C65A) \\sim Ueq,
Uanis(C56A) \\sim Ueq, Uanis(C57A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(C44) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C17A)=Sof(H17C)=Sof(H17D)=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(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(C34A)=Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(C36A)=Sof(C37A)=
 Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=
 Sof(C42A)=Sof(C43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=
 Sof(C47A)=Sof(H47A)=Sof(C48A)=Sof(C49A)=Sof(H49D)=Sof(H49E)=Sof(H49F)=
 Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=Sof(C51A)=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(C68A)=Sof(H68C)=Sof(H68D)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=Sof(C1)=
 Sof(C2)=Sof(C3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=
 Sof(C8)=Sof(C9)=Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(C13)=Sof(H13)=Sof(C14)=
 Sof(H14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(C19)=Sof(C20)=Sof(H20)=
 Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(C25)=Sof(C26)=
 Sof(C27)=Sof(H27)=Sof(C28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C35)=Sof(C36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(C39)=Sof(H39)=Sof(C40)=
 Sof(H40)=Sof(C41)=Sof(C42)=Sof(C43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(C46)=
 Sof(H46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=
 Sof(C53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=
 Sof(C58)=Sof(C59)=Sof(C60)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(C63)=Sof(H63)=
 Sof(C64)=Sof(H64)=Sof(C65)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C67)=
 Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C17A(H17C,H17D), C51(H51A,H51B), C68(H68A,H68B), C34(H34A,
 H34B), C34A(H34C,H34D), C51A(H51C,H51D), C68A(H68C,H68D)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C11(H11), C13(H13), C14(H14), C20(H20), C22(H22),
 C23(H23), C27(H27), C29(H29), 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), C2A(H2A), C3A(H3A), C5A(H5A), C9A(H9A), C10A(H10A), C12A(H12A),
 C20A(H20A), C21A(H21A), C23A(H23A), C27A(H27A), C28A(H28A), C30A(H30A),
 C37A(H37A), C38A(H38A), C40A(H40A), C44A(H44A), C45A(H45A), C47A(H47A),
 C54A(H54A), C55A(H55A), C57A(H57A), C61A(H61A), C62A(H62A), C64A(H64A),
 C69(H69), C70(H70), C71(H71)
5.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), C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F), C32A(H32D,H32E,H32F),
 C33A(H33D,H33E,H33F), C49A(H49D,H49E,H49F), C50A(H50D,H50E,H50F), C66A(H66D,
 H66E,H66F), C67A(H67D,H67E,H67F), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C)
;
_platon_squeeze_void_probe_radius 1.20
_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 1.727
_oxdiff_exptl_absorpt_empirical_full_min 0.697