Truncated Face-Rotating Polyhedra Constructed from Pentagonal Pentaphenylpyrrole through Graph Theory.
Qu, Hang; Huang, Zheyu; Dong, Xue; Wang, Xinchang; Tang, Xiao; Li, Zhihao; Gao, Wenbin; Liu, Haoliang; Huang, Ruishan; Zhao, Zujin; Zhang, Hui; Yang, Liulin; Tian, Zhongqun; Cao, Xiaoyu; Journal of the American Chemical Society 142 (2020) 16223–16228; doi:10.1021/jacs.0c08243

data_4135250
_publ_section_title
;
 Truncated Face-Rotating Polyhedra Constructed from Pentagonal
 Pentaphenylpyrrole through Graph Theory.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16223
_journal_page_last               16228
_journal_paper_doi               10.1021/jacs.0c08243
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C39 H25 N O5'
_chemical_formula_sum            'C39 H25 N O5'
_chemical_formula_weight         587.60
_chemical_melting_point          ?
_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             2020-01-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.267(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5727(2)
_cell_length_b                   9.6630(2)
_cell_length_c                   38.7804(6)
_cell_measurement_reflns_used    12658
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.7890
_cell_measurement_theta_min      3.4190
_cell_volume                     3960.99(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.940
_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    -24.00  15.00   0.50    1.06    --   46.75 -37.00  90.00   78
  2  \w     19.00  52.00   0.50    1.06    --   46.75 -37.00  90.00   66
  3  \w     35.00  61.00   0.50    1.06    --   46.75-115.00 137.00   52
  4  \w     78.00 111.00   0.50    5.00    --  101.48-115.00 137.00   66
  5  \w     73.00 108.00   0.50    5.00    --  101.48 -57.00 120.00   70
  6  \w     47.00 106.00   0.50    5.00    --  101.48 -99.00  60.00  118
  7  \w     63.00  88.00   0.50    1.06    --   46.75-167.00  -7.00   50
  8  \w     61.00 144.00   0.50    5.00    --  101.48-167.00  -7.00  166
  9  \w     79.00 174.00   0.50    5.00    --  101.48  77.00 -60.00  190
 10  \w     99.00 162.00   0.50    5.00    --  101.48 115.00-133.00  126
 11  \w     97.00 122.00   0.50    5.00    --  101.48 167.00  12.00   50
 12  \w    -70.00 -44.00   0.50    5.00    --  -88.50 125.00-180.00   52
 13  \w    -80.00 -16.00   0.50    1.06    --  -46.75 115.00-133.00  128
 14  \w    -84.00 -59.00   0.50    1.06    --  -46.75 125.00-180.00   50
 15  \w   -157.00 -72.00   0.50    5.00    --  -88.50 -57.00-180.00  170
 16  \w   -118.00 -78.00   0.50    1.06    --  -46.75-125.00-180.00   80
 17  \w    -81.00 -56.00   0.50    1.06    --  -46.75-167.00  -7.00   50
 18  \w   -114.00 -49.00   0.50    1.06    --  -46.75 -57.00 120.00  130
 19  \w   -119.00 -94.00   0.50    5.00    --  -88.50-115.00 137.00   50
 20  \w   -122.00 -73.00   0.50    5.00    --  -88.50-125.00  30.00   98
 21  \w   -157.00-130.00   0.50    5.00    --  -88.50-125.00  30.00   54
 22  \w   -152.00 -71.00   0.50    5.00    --  -88.50-125.00 120.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0000927000
_diffrn_orient_matrix_UB_12      -0.1573321000
_diffrn_orient_matrix_UB_13      0.0064947000
_diffrn_orient_matrix_UB_21      -0.1418506000
_diffrn_orient_matrix_UB_22      -0.0061133000
_diffrn_orient_matrix_UB_23      -0.0098175000
_diffrn_orient_matrix_UB_31      0.0332363000
_diffrn_orient_matrix_UB_32      -0.0252900000
_diffrn_orient_matrix_UB_33      -0.0379572000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            27743
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.865
_diffrn_reflns_theta_min         4.183
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.985
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   'Not measured'
_exptl_transmission_factor_min   'Not measured'
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7528
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0854
_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^)+(0.0985P)^2^+5.7001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2274
_refine_ls_wR_factor_ref         0.2316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6850
_reflns_number_total             7528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c08243_si_004.cif
_cod_data_source_block           PPAP
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'Not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'Not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 4135248--4135250.cif.
;
_cod_database_code               4135250
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.902
_reflns_odcompleteness_completeness 99.40
_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
2. Restrained distances
 O6-C39
 1.2 with sigma of 0.02
 O1-C11 \\sim O6-C39
 with sigma of 0.02
3. Others
 Fixed Sof: O3(0.75) H25(0.75) H25A(0.25) O4(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C27(H27), C24(H24), C28(H28), C31(H31), C30(H30), C20(H20), C21(H21),
 C13(H13), C16(H16), C17(H17), C23(H23), C14(H14), C10(H10), C18(H18), C32(H32),
  C9(H9), C6(H6), C7(H7), C34(H34), C25(H25), C25(H25A), C38(H38), C11(H11),
 C35(H35), C37(H37), C39(H39)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45148
_shelx_hkl_checksum              87985
_shelx_fab_checksum              37885
_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 1.792
_oxdiff_exptl_absorpt_empirical_full_min 0.551