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_4134805
_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         '2(C H2 Cl2), C68 H56 O8'
_chemical_formula_sum            'C70 H60 Cl4 O8'
_chemical_formula_weight         1170.98
_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     dual
_audit_creation_date             2019-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3783(2)
_cell_length_b                   23.7901(2)
_cell_length_c                   10.94360(10)
_cell_measurement_reflns_used    13239
_cell_measurement_temperature    169.99(14)
_cell_measurement_theta_max      72.7670
_cell_measurement_theta_min      2.7170
_cell_volume                     5735.01(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(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.926
_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    -49.00 -23.00   0.50    0.52    --  -47.20 108.00 125.00   52
  2  \w     24.00  86.00   0.50    0.52    --   47.20-108.00  28.00  124
  3  \w   -148.00-123.00   0.50    2.08    --  -99.00-108.00  28.00   50
  4  \w    -92.00 -67.00   0.50    2.08    --  -99.00 108.00 125.00   50
  5  \w     87.00 163.00   0.50    2.08    --  103.25 108.00 125.00  152
  6  \w     65.00 108.00   0.50    2.08    --  103.25-108.00  28.00   86
  7  \w   -119.00 -80.00   0.50    0.52    --  -47.20-125.00 -90.00   78
  8  \w   -109.00 -82.00   0.50    0.52    --  -47.20-125.00  90.00   54
  9  \w   -110.00 -83.00   0.50    0.52    --  -47.20-125.00-120.00   54
 10  \w     26.00 120.00   0.50    0.52    --   47.20  77.00 120.00  188
 11  \w    -88.00 -37.00   0.50    2.08    --  -99.00  30.00 150.00  102
 12  \w   -165.00 -83.00   0.50    2.08    --  -99.00 -61.00 -60.00  164
 13  \w    -97.00 -26.00   0.50    2.08    --  -99.00  77.00-180.00  142
 14  \w   -161.00-133.00   0.50    2.08    --  -99.00 -77.00  60.00   56
 15  \w   -117.00 -77.00   0.50    2.08    --  -99.00 -77.00  60.00   80
 16  \w     31.00 106.00   0.50    2.08    --  103.25 -94.00-150.00  150
 17  \w     43.00 100.00   0.50    2.08    --  103.25 -94.00-180.00  114
 18  \w     31.00  42.00   0.50    2.08    --  103.25 -94.00  60.00   22
;
_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      -0.0166157000
_diffrn_orient_matrix_UB_12      0.0140998000
_diffrn_orient_matrix_UB_13      0.1272839000
_diffrn_orient_matrix_UB_21      -0.0120448000
_diffrn_orient_matrix_UB_22      0.0614950000
_diffrn_orient_matrix_UB_23      -0.0412026000
_diffrn_orient_matrix_UB_31      -0.0668714000
_diffrn_orient_matrix_UB_32      -0.0145407000
_diffrn_orient_matrix_UB_33      -0.0504902000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            34797
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.421
_diffrn_reflns_theta_min         2.734
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.352
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57957
_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    1.356
_exptl_crystal_description       needle
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         11002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0930
_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^)+(0.1664P)^2^+7.2994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2568
_refine_ls_wR_factor_ref         0.2723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9208
_reflns_number_total             11002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00624_si_005.cif
_cod_data_source_block           tx1582a
_cod_database_code               4134805
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOCl
_reflns_odcompleteness_completeness 98.25
_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:
 C69(H69A,H69B), C70(H70A,H70B), C17(H17A,H17B), C34(H34A,H34B), C51(H51A,
 H51B), C68(H68A,H68B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C12(H12), 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), C56(H56), C57(H57), C61(H61), C63(H63), 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              76565
_shelx_hkl_checksum              75090
_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 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.721