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_4135248
_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_absolute_configuration
;
The absolute configuration in crystal was assigned by reference to an unchanging chiral centre
 in the assembly procedure, i.e., the chiral carbon atoms of the reagent
 (R, R)-CHDA or (S, S)-CHDA, instead of anomalous dispersion effects in diffraction
 measurements on the crystal and the derived Flack x parameter. 
;
_chemical_formula_moiety         'C216 H200 N24'
_chemical_formula_sum            'C216 H200 N24'
_chemical_formula_weight         3131.99
_chemical_melting_point          ?
_space_group_crystal_system      orthorhombic
_space_group_IT_number           22
_space_group_name_Hall           'F 2 2'
_space_group_name_H-M_alt        'F 2 2 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.3336(10)
_cell_length_b                   33.9663(8)
_cell_length_c                   51.4808(15)
_cell_measurement_reflns_used    10674
_cell_measurement_temperature    209(100)
_cell_measurement_theta_max      67.8350
_cell_measurement_theta_min      2.8600
_cell_volume                     56539(3)
_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      209(100)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_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     36.00  94.00   1.00   18.00    --  107.75 -36.00 -32.00   58
  2  \w     -7.00  18.00   1.00   10.00    --   47.73 -36.00 -32.00   25
  3  \w     81.00 108.00   1.00   18.00    --  107.75 -94.00 -30.00   27
  4  \w     84.00 117.00   1.00   18.00    --  107.75-125.00 -60.00   33
  5  \w     71.00 109.00   1.00   18.00    --  107.75 -94.00-150.00   38
  6  \w     49.00  74.00   1.00   18.00    --  107.75 -94.00 -30.00   25
  7  \w     35.00  91.00   1.00   18.00    --  107.75 -94.00 -90.00   56
  8  \w     36.00 123.00   1.00   18.00    --  107.75 -61.00-120.00   87
  9  \w     97.00 175.00   1.00   18.00    --  107.75  45.00  30.00   78
 10  \w    130.00 156.00   1.00   18.00    --  107.75  77.00   0.00   26
 11  \w    106.00 137.00   1.00   18.00    --  107.75  36.00 124.00   31
 12  \w     83.00 117.00   1.00   18.00    --  107.75 -30.00  90.00   34
 13  \w     96.00 121.00   1.00   10.00    --   47.73  36.00 124.00   25
 14  \w     86.00 111.00   1.00   18.00    --  107.75  77.00   0.00   25
 15  \w     37.00  76.00   1.00   18.00    --  107.75 -30.00  90.00   39
 16  \w     33.00  98.00   1.00   18.00    --  107.75 -15.00  90.00   65
 17  \w     41.00 100.00   1.00   18.00    --  107.75 -94.00  60.00   59
 18  \w     71.00  98.00   1.00   18.00    --  107.75-125.00 150.00   27
 19  \w     32.00  90.00   1.00   10.00    --   47.73-125.00  30.00   58
 20  \w     39.00  65.00   1.00   18.00    --  107.75-125.00 150.00   26
 21  \w    -50.00 -19.00   1.00   10.00    --  -47.73  36.00 124.00   31
 22  \w     35.00  72.00   1.00   10.00    --   47.73 -99.00-180.00   37
 23  \w     -6.00  19.00   1.00   10.00    --  -47.73  36.00 124.00   25
 24  \w    -53.00 -25.00   1.00   18.00    --  -86.25  36.00 124.00   28
 25  \w   -111.00 -37.00   1.00   10.00    --  -47.73 -36.00 -32.00   74
 26  \w   -113.00 -72.00   1.00   10.00    --  -47.73-125.00 120.00   41
 27  \w   -132.00-106.00   1.00   18.00    --  -86.25 -36.00 -32.00   26
;
_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      0.0363909000
_diffrn_orient_matrix_UB_12      0.0260425000
_diffrn_orient_matrix_UB_13      -0.0088248000
_diffrn_orient_matrix_UB_21      -0.0307409000
_diffrn_orient_matrix_UB_22      0.0314834000
_diffrn_orient_matrix_UB_23      -0.0095517000
_diffrn_orient_matrix_UB_31      0.0010235000
_diffrn_orient_matrix_UB_32      0.0197052000
_diffrn_orient_matrix_UB_33      0.0269419000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            110029
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.954
_diffrn_reflns_theta_min         2.733
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00514
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.736
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             13312
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   'Not measured'
_exptl_transmission_factor_min   'Not measured'
_refine_diff_density_max         0.076
_refine_diff_density_min         -0.093
_refine_diff_density_rms         0.015
_refine_ls_abs_structure_details
;
 Flack x determined using 4608 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.31(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         28775
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0726P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                12552
_reflns_number_total             28775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c08243_si_003.cif
_cod_data_source_block           4P-1
_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               4135248
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHN
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     59.94
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C8-C11
 1.54 with sigma of 0.001
 N02V-C11
 1.32 with sigma of 0.001
 C12-N02V
 1.4 with sigma of 0.001
 C12-C12_$1
 1.54 with sigma of 0.001
 C14_$2-C14_$3
 1.54 with sigma of 0.001
 H13A_$1-H14B
 2.5 with sigma of 0.02
3. Rigid bond restraints
 C11, N02V, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C11 \\sim N02V \\sim C12: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C48(H48), C49(H49), C71(H71), C88(H88), C89(H89), C106(H106), C101(H101),
 C34(H34), C12(H12), C29(H29)
5.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C72(H72A,H72B), C52(H52A,H52B), C51(H51A,H51B), C50(H50A,
 H50B), C105(H10A,H10B), C102(H10C,H10D), C73(H73A,H73B), C93(H93A,H93B),
 C104(H10E,H10F), C14(H14A,H14B), C103(H10G,H10H), C92(H92A,H92B), C90(H90A,
 H90B), C91(H91A,H91B), C13(H13A,H13B), C30(H30A,H30B), C33(H33A,H33B),
 C31(H31A,H31B), C32(H32A,H32B)
5.c Aromatic/amide H refined with riding coordinates:
 C62(H62), C60(H60), C98(H98), C63(H63), C47(H47), C78(H78), C99(H99),
 C86(H86), C59(H59), C100(H100), C2AA(H2AA), C76(H76), C96(H96), C28(H28),
 C85(H85), C75(H75), C23(H23), C80(H80), C39(H39), C95(H95), C68(H68), C40(H40),
  C24(H24), C26(H26), C46(H46), C69(H69), C41(H41), C87(H87), C16(H16),
 C79(H79), C107(H107), C27(H27), C20(H20), C83(H83), C70(H70), C44(H44),
 C36(H36), C43(H43), C37(H37), C17(H17), C82(H82), C65(H65), C21(H21), C19(H19),
  C66(H66), C7(H7), C6(H6), C10(H10), C9(H9), C11(H11)
5.d Fitted hexagon refined as free rotating group:
 C8(C7,C6,C5,C10,C9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36040
_shelx_hkl_checksum              40278
_shelx_fab_checksum              28141
_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 88.792
_oxdiff_exptl_absorpt_empirical_full_min 0.489