Chiral separation and characterization of triazatruxene-based face-rotating polyhedra: the role of non-covalent facial interactions.
Zhang, Pei; Wang, Xinchang; Xuan, Wei; Peng, Pixian; Li, Zhihao; Lu, Ruqiang; Wu, Shuang; Tian, Zhongqun; Cao, Xiaoyu; Chemical communications (Cambridge, England) 54 (2018) 4685–4688; doi:10.1039/c8cc02049c

data_7125319
_publ_section_title
;
 Chiral separation and characterization of triazatruxene-based
 face-rotating polyhedra: the role of non-covalent facial interactions.
;
_journal_issue                   37
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4685
_journal_page_last               4688
_journal_paper_doi               10.1039/c8cc02049c
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C96 H108 N12'
_chemical_formula_sum            'C96 H108 N12'
_chemical_formula_weight         1429.94
_chemical_melting_point          ?
_chemical_name_common            S-CHDA-FRP-7
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-08 deposited with the CCDC.
2018-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   23.3854(7)
_cell_length_b                   23.3854(7)
_cell_length_c                   89.444(2)
_cell_measurement_reflns_used    10836
_cell_measurement_temperature    150
_cell_measurement_theta_max      57.9660
_cell_measurement_theta_min      3.2710
_cell_volume                     42362(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'SIR2011 (Burla et al., 2007)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  ZP622
_diffrn_measurement_method       'omega rotation'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       107
_diffrn_reflns_limit_l_min       -110
_diffrn_reflns_number            93184
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.972
_diffrn_reflns_theta_min         2.944
_diffrn_source                   synchrotron
_diffrn_source_type              'Bend magnet, Station 11.3.1, ALS, LBNL'
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13824
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   'not measured'
_exptl_transmission_factor_min   'not measured'
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 5841 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1476
_refine_ls_number_reflns         27811
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0891
_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^)+(0.1218P)^2^+5.4292P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2366
_refine_ls_wR_factor_ref         0.2613
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                19345
_reflns_number_total             27811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02049c2.cif
_cod_data_source_block           S-CHDA-FRP-7
_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 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        42361(3)
_cod_database_code               7125319
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H6CA-H62
 2.5 with sigma of 0.02
3. Rigid bond restraints
 C7, C3FA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C50, N1BA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N67, C97
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2CA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, C22, C99, C82
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N84, C2CA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C3FA \\sim C7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N1BA \\sim C50: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N67 \\sim C97: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N84 \\sim C2CA: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C22 \\sim C16 \\sim C99 \\sim C82: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C2CA \\sim N84: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C23) = Uanis(C23A)
Uanis(C17) = Uanis(C17A)
Uanis(C3FA) = Uanis(C3FB)
5. Others
 Sof(H49C)=Sof(H49D)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(H49A)=Sof(H49B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
 Sof(H98C)=Sof(H98D)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(2)
 Sof(H98A)=Sof(H98B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2)
 Sof(H7BC)=Sof(H7BD)=Sof(C3FB)=Sof(H3FD)=Sof(H3FE)=Sof(H3FF)=1-FVAR(3)
 Sof(H7AA)=Sof(H7AB)=Sof(C3FA)=Sof(H3FA)=Sof(H3FB)=Sof(H3FC)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C5CA(H5CA), C4EA(H4EA), C0DA(H0DA), C2CA(H2CA), C2DA(H2DA), C9DA(H9DA),
 C1FA(H1FA), C5(H5), C6(H6)
6.b Secondary CH2 refined with riding coordinates:
 C3BA(H3BA,H3BB), C42(H42A,H42B), C45(H45A,H45B), C49(H49A,H49B), C49(H49C,
 H49D), C52(H52A,H52B), C65(H65A,H65B), C75(H75A,H75B), C76(H76A,H76B),
 C82(H82A,H82B), C83(H83A,H83B), C88(H88A,H88B), C90(H90A,H90B), C91(H91A,H91B),
  C94(H94A,H94B), C98(H98A,H98B), C98(H98C,H98D), C99(H99A,H99B), C101(H10A,
 H10B), C102(H10C,H10D), C9CA(H9CA,H9CB), C6CA(H6CA,H6CB), C0FA(H0FA,H0FB),
 C3CA(H3CA,H3CB), C4CA(H4CA,H4CB), C1DA(H1DA,H1DB), C3DA(H3DA,H3DB), C6DA(H6DA,
 H6DB), C8DA(H8DA,H8DB), C0EA(H0EA,H0EB), C3EA(H3EA,H3EB), C2FA(H2FA,H2FB),
 C3(H3A,H3B), C4(H4A,H4B), C7(H7AA,H7AB), C7(H7BC,H7BD), C8(H8A,H8B), C9(H9A,
 H9B), C10(H10E,H10F), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,
 H15B), C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B)
6.c Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C2(H2A,H2B,H2C), C3FA(H3FA,H3FB,
 H3FC), C23A(H23D,H23E,H23F), C17A(H17D,H17E,H17F), C3FB(H3FD,H3FE,H3FF)
6.d Aromatic/amide H refined with riding coordinates:
 C0CA(H0CA), C8EA(H8EA), C3AA(H3AA), C4AA(H4AA), C2BA(H2BA), C4BA(H4BA),
 C6BA(H6BA), C26(H26), C30(H30), C31(H31), C35(H35), C37(H37), C41(H41),
 C44(H44), C47(H47), C51(H51), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63),
  C69(H69), C71(H71), C72(H72), C74(H74), C79(H79), C80(H80), C87(H87),
 C89(H89), C93(H93), C100(H100), C8CA(H8CA), C7CA(H7CA), C9EA(H9EA), C4DA(H4DA),
  C5DA(H5DA)
6.e Idealised Me refined as rotating group:
 C1BA(H1BA,H1BB,H1BC), C2EA(H2EA,H2EB,H2EC), C22(H22A,H22B,H22C), C25(H25A,
 H25B,H25C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              63440
_shelx_fab_checksum              66459
_olex2_submission_special_instructions 'No special instructions were received'