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_4134811
_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'
_chemical_formula_sum            'C68 H56 O8'
_chemical_formula_weight         1001.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7975(10)
_cell_length_b                   11.8330(12)
_cell_length_c                   43.114(4)
_cell_measurement_reflns_used    2978
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      54.6810
_cell_measurement_theta_min      3.7180
_cell_volume                     6018.7(10)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.920
_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    -23.00  29.00   0.50    5.00    --  -46.95  19.00 -90.00  104
  2  \w    -23.00  29.00   0.50    5.00    --  -46.95  19.00  60.00  104
  3  \w    -26.00  28.00   0.50    5.00    --  -46.95  23.00 176.00  108
  4  \w     32.00  98.00   0.50    5.00    --   46.95  57.00 -90.00  132
  5  \w     92.00 169.00   0.50    9.00    --  103.25 101.00 -23.00  154
  6  \w     78.00 169.00   0.50    9.00    --  103.25 128.00-129.00  182
  7  \w     31.00  75.00   0.50    9.00    --  103.25 -61.00 150.00   88
  8  \w     31.00 106.00   0.50    9.00    --  103.25 -94.00-180.00  150
  9  \w   -102.00 -26.00   0.50    9.00    --  -99.00  77.00  90.00  152
 10  \w   -168.00 -84.00   0.50    9.00    --  -99.00 -94.00-180.00  168
 11  \w   -119.00 -72.00   0.50    5.00    --  -46.95-128.00 156.00   94
;
_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      -0.0026176000
_diffrn_orient_matrix_UB_12      -0.0307702000
_diffrn_orient_matrix_UB_13      0.0346858000
_diffrn_orient_matrix_UB_21      0.0383473000
_diffrn_orient_matrix_UB_22      0.1206249000
_diffrn_orient_matrix_UB_23      0.0082275000
_diffrn_orient_matrix_UB_31      -0.1248373000
_diffrn_orient_matrix_UB_32      0.0384686000
_diffrn_orient_matrix_UB_33      0.0018146000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1494
_diffrn_reflns_av_unetI/netI     0.1552
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            27702
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.414
_diffrn_reflns_theta_min         3.874
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04462
_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    1.105
_exptl_crystal_description       needle
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 1264 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.0(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         10923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.2096
_refine_ls_R_factor_gt           0.1407
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3333
_refine_ls_wR_factor_ref         0.3811
_reflns_Friedel_coverage         0.717
_reflns_Friedel_fraction_full    0.898
_reflns_Friedel_fraction_max     0.826
_reflns_number_gt                4958
_reflns_number_total             10923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00624_si_011.cif
_cod_data_source_block           tx2025a_sq
_cod_original_cell_volume        6018.8(10)
_cod_database_code               4134811
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOCl
_reflns_odcompleteness_completeness 96.88
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C13(H13), C15(H15), C21(H21), C22(H22),
 C25(H25), C28(H28), C31(H31), C32(H32), C37(H37), C39(H39), C42(H42), C43(H43),
  C46(H46), C48(H48), C54(H54), C56(H56), C59(H59), C60(H60), C64(H64), C66(H66)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C67(H67A,
 H67B,H67C)
;
_shelx_res_checksum              8588
_shelx_hkl_checksum              69587
_shelx_fab_checksum              95937
_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 15.769
_oxdiff_exptl_absorpt_empirical_full_min 0.202