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_4135249
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-04
_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                   32.3016(10)
_cell_length_b                   34.0393(11)
_cell_length_c                   50.8944(14)
_cell_measurement_reflns_used    23740
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      67.6550
_cell_measurement_theta_min      3.0940
_cell_volume                     55960(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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  39.00   0.50    5.00    --   47.79 -49.00 169.00  126
  2  \w     22.00  63.00   0.50    5.00    --   47.79 -57.00  90.00   82
  3  \w     80.00 114.00   0.50   12.00    --  107.75 -49.00 169.00   68
  4  \w     68.00 117.00   0.50   12.00    --  107.75-125.00 120.00   98
  5  \w     78.00 117.00   0.50   12.00    --  107.75-125.00 150.00   78
  6  \w     49.00  75.00   0.50   12.00    --  107.75 -49.00 169.00   52
  7  \w     36.00 100.00   0.50   12.00    --  107.75 -94.00 150.00  128
  8  \w     44.00  70.00   0.50   12.00    --  107.75-125.00 150.00   52
  9  \w     36.00  95.00   0.50   12.00    --  107.75-125.00  90.00  118
 10  \w    104.00 133.00   0.50   12.00    --  107.75-148.00  15.57   58
 11  \w     82.00 109.00   0.50   12.00    --  107.75-109.00 -77.56   54
 12  \w     73.00  99.00   0.50   12.00    --  107.75 -61.00 -60.00   52
 13  \w     69.00 116.00   0.50   12.00    --  107.75 -30.00 -30.00   94
 14  \w    101.00 178.00   0.50   12.00    --  107.75  30.00 -60.00  154
 15  \w    142.00 176.00   0.50   12.00    --  107.75 125.00-180.00   68
 16  \w    127.00 178.00   0.50   12.00    --  107.75  45.00-180.00  102
 17  \w     99.00 177.00   0.50   12.00    --  107.75  49.00 -42.00  156
 18  \w    106.00 174.00   0.50   12.00    --  107.75  45.00-120.00  136
 19  \w     96.00 123.00   0.50   12.00    --  107.75  45.00-180.00   54
 20  \w     94.00 150.00   0.50   12.00    --  107.75 125.00-120.00  112
 21  \w     98.00 124.00   0.50   12.00    --  107.75 125.00-180.00   52
 22  \w     43.00 120.00   0.50    5.00    --   47.79  49.00 -42.00  154
 23  \w     94.00 160.00   0.50   12.00    --  107.75  61.00  60.00  132
 24  \w    137.00 176.00   0.50   12.00    --  107.75 125.00 150.00   78
 25  \w     99.00 144.00   0.50   12.00    --  107.75  77.00 150.00   90
 26  \w     94.00 122.00   0.50   12.00    --  107.75 125.00 150.00   56
 27  \w     92.00 178.00   0.50   12.00    --  107.75  61.00   0.00  172
 28  \w     76.00 101.00   0.50   12.00    --  107.75 -94.00-180.00   50
 29  \w     84.00 109.00   0.50   12.00    --  107.75 -94.00-150.00   50
 30  \w     78.00 116.00   0.50   12.00    --  107.75-125.00-180.00   76
;
_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      0.0279553000
_diffrn_orient_matrix_UB_12      -0.0346277000
_diffrn_orient_matrix_UB_13      -0.0080873000
_diffrn_orient_matrix_UB_21      -0.0356842000
_diffrn_orient_matrix_UB_22      -0.0175036000
_diffrn_orient_matrix_UB_23      -0.0163276000
_diffrn_orient_matrix_UB_31      0.0147455000
_diffrn_orient_matrix_UB_32      0.0233697000
_diffrn_orient_matrix_UB_33      -0.0241784000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            127633
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        64.998
_diffrn_reflns_theta_max         64.998
_diffrn_reflns_theta_min         2.076
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.339
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07060
_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    0.744
_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         0.082
_refine_diff_density_min         -0.082
_refine_diff_density_rms         0.016
_refine_ls_abs_structure_details
;
 Flack x determined using 6226 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.46(12)
_refine_ls_extinction_coef       0.000006(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         23393
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0812P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                15831
_reflns_number_total             23393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c08243_si_002.cif
_cod_data_source_block           4M-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               4135249
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.935
_reflns_odcompleteness_completeness 98.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C94, C95, C96, C97, C98, C99, H99
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C94 \\sim C95 \\sim C96 \\sim C97 \\sim C98 \\sim C99: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4.a Ternary CH refined with riding coordinates:
 C94(H94), C99(H99), C100(H100), C103(H103), C35(H35), C40(H40), C44(H44),
 C48(H48), C53(H53)
4.b Secondary CH2 refined with riding coordinates:
 C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C101(H10A,
 H10B), C102(H10C,H10D), C105(H10E,H10F), C106(H10G,H10H), C107(H10I,H10J),
 C108(H10K,H10L), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,
 H39B), C45(H45A,H45B), C46(H46A,H46B), C49(H49A,H49B), C50(H50A,H50B),
 C51(H51A,H51B), C52(H52A,H52B)
4.c Aromatic/amide H refined with riding coordinates:
 C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C67(H67), C68(H68),
 C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C77(H77), C78(H78), C79(H79),
  C81(H81), C82(H82), C84(H84), C85(H85), C86(H86), C88(H88), C89(H89),
 C91(H91), C92(H92), C93(H93), C6(H6), C1AA(H1AA), C9(H9), C10(H10), C12(H12),
 C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24),
  C25(H25), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34),
 C41(H41), C42(H42), C43(H43), C47(H47), C54(H54)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91640
_shelx_hkl_checksum              77757
_shelx_fab_checksum              2355
_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 9.184
_oxdiff_exptl_absorpt_empirical_full_min 0.506