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_4134806
_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 P1, C68 H56 O8, C7 H10 N'
_chemical_formula_sum            'C75 H66 F6 N O8 P'
_chemical_formula_weight         1254.25
_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             2020-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.098(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5052(2)
_cell_length_b                   26.1338(4)
_cell_length_c                   21.4462(4)
_cell_measurement_reflns_used    16299
_cell_measurement_temperature    169.99(13)
_cell_measurement_theta_max      74.4670
_cell_measurement_theta_min      2.7110
_cell_volume                     6225.74(19)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.947
_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    -15.00  10.00   0.50    8.00    --  -47.20  19.00 -90.00   50
  2  \w    -22.00  20.00   0.50    8.00    --  -47.20  19.00  60.00   84
  3  \w    -21.00  26.00   0.50    8.00    --  -47.20  98.00 163.00   94
  4  \w    -39.00  20.00   0.50    8.00    --  -47.20  38.00 150.00  118
  5  \w    -56.00 -30.00   0.50    7.00    --  -99.00  61.00 120.00   52
  6  \w    -67.00 -28.00   0.50    7.00    --  -99.00  61.00 150.00   78
  7  \w    -77.00 -35.00   0.50    8.00    --  -47.20  98.00 163.00   84
  8  \w    -56.00 -30.00   0.50    7.00    --  -99.00 125.00-120.00   52
  9  \w    -63.00 -30.00   0.50    7.00    --  -99.00  77.00 -60.00   66
 10  \w   -112.00 -83.00   0.50    7.00    --  -99.00 125.00-120.00   58
 11  \w   -126.00 -65.00   0.50    7.00    --  -99.00 144.00 -35.91  122
 12  \w   -124.00 -90.00   0.50    7.00    --  -99.00 142.00  43.83   68
 13  \w   -101.00 -26.00   0.50    7.00    --  -99.00 110.00 142.17  150
 14  \w    -90.00 -65.00   0.50    7.00    --  -99.00  98.00 163.00   50
 15  \w   -155.00-111.00   0.50    7.00    --  -99.00 -66.00 172.67   88
 16  \w   -103.00 -78.00   0.50    8.00    --  -47.20-125.00 120.00   50
 17  \w   -155.00-129.00   0.50    7.00    --  -99.00 -98.00  56.00   52
 18  \w   -166.00 -81.00   0.50    7.00    --  -99.00 -64.00 -69.49  170
 19  \w      6.00  31.00   0.50    8.00    --   47.20 -98.00  56.00   50
 20  \w     68.00  93.00   0.50    7.00    --  103.25 -98.00  56.00   50
 21  \w     49.00  75.00   0.50    7.00    --  103.25 -61.00 -30.00   52
 22  \w     39.00  66.00   0.50    7.00    --  103.25 -94.00 -30.00   54
 23  \w     31.00  98.00   0.50    7.00    --  103.25-125.00 -60.00  134
 24  \w     31.00  63.00   0.50    7.00    --  103.25-125.00  60.00   64
 25  \w     31.00  93.00   0.50    7.00    --  103.25-125.00  30.00  124
 26  \w     40.00  74.00   0.50    7.00    --  103.25 -61.00  60.00   68
 27  \w     90.00 139.00   0.50    7.00    --  103.25  15.00  90.00   98
 28  \w    144.00 169.00   0.50    7.00    --  103.25  15.00  90.00   50
 29  \w     92.00 145.00   0.50    7.00    --  103.25  98.00 163.00  106
 30  \w     19.00  91.00   0.50    8.00    --   47.20-125.00 -90.00  144
;
_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      -0.0809967000
_diffrn_orient_matrix_UB_12      0.0340967000
_diffrn_orient_matrix_UB_13      0.0295442000
_diffrn_orient_matrix_UB_21      -0.0074897000
_diffrn_orient_matrix_UB_22      0.0396114000
_diffrn_orient_matrix_UB_23      -0.0540992000
_diffrn_orient_matrix_UB_31      -0.1122566000
_diffrn_orient_matrix_UB_32      -0.0272988000
_diffrn_orient_matrix_UB_33      -0.0417128000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53058
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.679
_diffrn_reflns_theta_min         2.723
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78614
_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            'translucent yellow'
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       cube
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.631
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1584
_refine_ls_number_reflns         12254
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.648
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0796
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2258
_refine_ls_wR_factor_ref         0.2416
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7931
_reflns_number_total             12254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00624_si_007.cif
_cod_data_source_block           tx2075a
_cod_database_code               4134806
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONPF
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.930
_reflns_odcompleteness_completeness 98.69
_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,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P2-F9
 1.58 with sigma of 0.01
 P1A-F5A = P1A-F2A = P1A-F3A = P1A-F6A = P1A-F1A = P1A-F4A = P1-F4 = P1-F1 =
 P1-F5 = P1-F3 = P1-F6 = P1-F2
 1.58 with sigma of 0.01
 C11A-C10A = C12A-C11A = C4A-C3A = C5A-C4A = C5A-C10A = C3A-C12A
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
P1 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim P1A \\sim F1A
\\sim F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(F5) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim
Ueq, Uanis(F6) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F1A)
\\sim Ueq, Uanis(P1A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F2A) \\sim Ueq,
Uanis(F5A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4A) \\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(C3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=Sof(H6A)=
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(C9A)=Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=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(H36A)=Sof(C37A)=Sof(H37A)=
 Sof(C38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(C41A)=Sof(C42A)=Sof(C43A)=
 Sof(H43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=
 Sof(C48A)=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(C1)=
 Sof(C2)=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(P1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=0.5*(1-FVAR(3))
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=0.5*FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17C,H17D), C17(H17A,H17B), C34(H34C,H34D), C34(H34A,H34B), C51(H51C,
 H51D), C51(H51A,H51B), C68(H68A,H68B), C68(H68C,H68D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C4A(H4A), C6(H6), C6A(H6A), C7A(H7A), C10(H10), C11(H11),
 C11A(H11A), C13(H13), C13A(H13A), C14A(H14A), C20(H20), C20A(H20A), C21(H21),
 C21A(H21A), C23(H23), C23A(H23A), C27(H27), C27A(H27A), C28(H28), C28A(H28A),
 C30(H30), C30A(H30A), C36A(H36A), C37(H37), C37A(H37A), C38(H38), C39A(H39A),
 C40(H40), C43A(H43A), C44(H44), C44A(H44A), C45(H45), C46A(H46A), C47(H47),
 C54(H54), C54A(H54A), C55(H55), C55A(H55A), C57(H57), C57A(H57A), C61(H61),
 C61A(H61A), C62(H62), C62A(H62A), C64(H64), C64A(H64A), C69(H69), C70(H70),
 C72(H72), C73(H73)
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), C74(H74A,H74B,H74C), C75(H75A,H75B,
 H75C)
;
_shelx_res_checksum              50975
_shelx_hkl_checksum              26637
_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 1.453
_oxdiff_exptl_absorpt_empirical_full_min 0.711