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_4134810
_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, C6 H8 N2'
_chemical_formula_sum            'C74 H64 N2 O8'
_chemical_formula_weight         1109.27
_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                 100.874(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1031(2)
_cell_length_b                   21.4125(4)
_cell_length_c                   25.1008(4)
_cell_measurement_reflns_used    14548
_cell_measurement_temperature    169.99(13)
_cell_measurement_theta_max      71.4810
_cell_measurement_theta_min      2.7350
_cell_volume                     6388.26(19)
_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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.946
_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     54.00 117.00   0.50    0.67    --   46.95  38.00 -60.00  126
  2  \w    100.00 126.00   0.50    2.60    --  103.25 111.00 -62.00   52
  3  \w     87.00 169.00   0.50    2.60    --  103.25  61.00   0.00  164
  4  \w     92.00 162.00   0.50    2.60    --  103.25  45.00  30.00  140
  5  \w     31.00 111.00   0.50    2.60    --  103.25-111.00-156.00  160
  6  \w     32.00  89.00   0.50    2.60    --  103.25 -94.00 -30.00  114
  7  \w     16.00  55.00   0.50    0.67    --   46.95-111.00-156.00   78
  8  \w     33.00 112.00   0.50    2.60    --  103.25 -45.00-180.00  158
  9  \w     39.00 115.00   0.50    2.60    --  103.25 -30.00-180.00  152
 10  \w    -83.00 -33.00   0.50    0.67    --  -46.95 111.00 -62.00  100
 11  \w    -58.00 -31.00   0.50    2.60    --  -99.00 125.00  30.00   54
 12  \w   -111.00 -84.00   0.50    2.60    --  -99.00 111.00 -62.00   54
 13  \w   -116.00 -91.00   0.50    2.60    --  -99.00 125.00  30.00   50
 14  \w   -166.00-136.00   0.50    2.60    --  -99.00 -45.00 120.00   60
 15  \w   -106.00 -79.00   0.50    0.67    --  -46.95-125.00  60.00   54
 16  \w   -118.00 -71.00   0.50    0.67    --  -46.95-125.00 -30.00   94
 17  \w   -119.00 -94.00   0.50    0.67    --  -46.95-125.00-120.00   50
 18  \w   -136.00 -80.00   0.50    2.60    --  -99.00-111.00-156.00  112
 19  \w   -166.00-139.00   0.50    2.60    --  -99.00-111.00-156.00   54
 20  \w   -118.00 -24.00   0.50    0.67    --  -46.95 -77.00 150.00  188
;
_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      -0.0842927000
_diffrn_orient_matrix_UB_12      -0.0231724000
_diffrn_orient_matrix_UB_13      0.0345436000
_diffrn_orient_matrix_UB_21      0.0073552000
_diffrn_orient_matrix_UB_22      -0.0664473000
_diffrn_orient_matrix_UB_23      -0.0225928000
_diffrn_orient_matrix_UB_31      0.0981769000
_diffrn_orient_matrix_UB_32      -0.0149320000
_diffrn_orient_matrix_UB_33      0.0469474000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44396
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.693
_diffrn_reflns_theta_min         2.733
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58436
_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    1.153
_exptl_crystal_description       needle
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.663
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         12565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.663
_refine_ls_R_factor_all          0.1555
_refine_ls_R_factor_gt           0.1396
_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          0.3588
_refine_ls_wR_factor_ref         0.3680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9825
_reflns_number_total             12565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00624_si_006.cif
_cod_data_source_block           tx1579_sq
_cod_database_code               4134810
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHON
_reflns_odcompleteness_completeness 99.80
_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), C70(H70A,
 H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B)
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), C39(H39), C40(H40), C44(H44),
  C46(H46), 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              31071
_shelx_hkl_checksum              86377
_shelx_fab_checksum              23953
_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 2.081
_oxdiff_exptl_absorpt_empirical_full_min 0.666