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_4134803
_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         '1.7(C0.59 H1.18 Cl1.18), C68 H56 O8'
_chemical_formula_sum            'C69 H58 Cl2 O8'
_chemical_formula_weight         1086.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.056(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7416(5)
_cell_length_b                   18.3691(6)
_cell_length_c                   18.8001(6)
_cell_measurement_reflns_used    4255
_cell_measurement_temperature    170.00(15)
_cell_measurement_theta_max      74.5570
_cell_measurement_theta_min      3.3690
_cell_volume                     5382.6(3)
_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      170.00(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.948
_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     39.00 120.00   0.50   20.00    --   47.20  39.00 -38.00  162
  2  \w     90.00 164.00   0.50   45.00    --  103.25  39.00 -38.00  148
  3  \w    100.00 169.00   0.50   45.00    --  103.25  15.00 120.00  138
  4  \w     32.00 115.00   0.50   45.00    --  103.25 -39.00 166.00  166
  5  \w     -6.00  22.00   0.50   20.00    --   47.20 -39.00 166.00   56
  6  \w    -85.00 -35.00   0.50   20.00    --  -47.20 -39.00 166.00  100
  7  \w     27.00  69.00   0.50   20.00    --   47.20-125.00-180.00   84
  8  \w     90.00 116.00   0.50   45.00    --  103.25-125.00-180.00   52
  9  \w    -59.00  11.00   0.50   20.00    --  -47.20  39.00 -38.00  140
 10  \w    -55.00 -28.00   0.50   45.00    --  -99.00  77.00-180.00   54
 11  \w    -85.00 -60.00   0.50   45.00    --  -99.00  39.00 -38.00   50
 12  \w   -114.00 -38.00   0.50   45.00    --  -99.00  61.00-180.00  152
 13  \w   -119.00 -61.00   0.50   45.00    --  -99.00  77.00-180.00  116
 14  \w   -161.00 -86.00   0.50   45.00    --  -99.00 -45.00  30.00  150
 15  \w   -120.00 -93.00   0.50   20.00    --  -47.20-125.00 -60.00   54
 16  \w   -110.00 -25.00   0.50   45.00    --  -99.00  15.00 150.00  170
 17  \w    -59.00 -29.00   0.50   45.00    --  -99.00  45.00 150.00   60
 18  \w    -96.00 -67.00   0.50   45.00    --  -99.00  45.00 150.00   58
 19  \w   -116.00 -91.00   0.50   20.00    --  -47.20 -39.00 166.00   50
 20  \w   -151.00-126.00   0.50   45.00    --  -99.00 -39.00 166.00   50
;
_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      -0.0797869000
_diffrn_orient_matrix_UB_12      -0.0183202000
_diffrn_orient_matrix_UB_13      0.0355552000
_diffrn_orient_matrix_UB_21      -0.0414581000
_diffrn_orient_matrix_UB_22      -0.0369622000
_diffrn_orient_matrix_UB_23      -0.0698635000
_diffrn_orient_matrix_UB_31      0.0410168000
_diffrn_orient_matrix_UB_32      -0.0730513000
_diffrn_orient_matrix_UB_33      0.0264978000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19285
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.422
_diffrn_reflns_theta_min         3.380
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37257
_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            'fluorescent light yellow'
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5291
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0853
_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^)+(0.1725P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2261
_refine_ls_wR_factor_ref         0.2763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2929
_reflns_number_total             5291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00624_si_004.cif
_cod_data_source_block           tx1510
_cod_original_cell_volume        5382.5(3)
_cod_database_code               4134803
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHO
_reflns_odcompleteness_completeness 99.70
_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. Uiso/Uaniso restraints and constraints
Cl1 \\sim C36 \\sim Cl1A \\sim C36A: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(Cl1A) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(C36)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Cl1A)=1-FVAR(1)
 Sof(C36A)=Sof(H36C)=Sof(H36D)=0.5*(1-FVAR(2))
 Sof(C36)=Sof(H36A)=Sof(H36B)=0.5*FVAR(2)
 Sof(Cl1)=FVAR(1)
 Fixed Sof: H15A(0.5) H15B(0.5) H31A(0.5) H31B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C36A(H36C,H36D), C15(H15A,H15B), C16(H16A,H16B), C31(H31A,H31B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C12(H12), C19(H19), C20(H20),
 C22(H22), C26(H26), C27(H27), C29(H29)
4.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C)
;
_shelx_res_checksum              62021
_shelx_hkl_checksum              95356
_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 4.172
_oxdiff_exptl_absorpt_empirical_full_min 0.273