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_7125318
_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            R-CHDA-FRP-8
_chemical_name_systematic        R-CHDA-FRP-8
_space_group_crystal_system      hexagonal
_space_group_IT_number           178
_space_group_name_Hall           'P 61 2 (0 0 5)'
_space_group_name_H-M_alt        'P 61 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-06 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                   23.3698(13)
_cell_length_b                   23.3698(13)
_cell_length_c                   89.848(3)
_cell_measurement_reflns_used    12697
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.8800
_cell_measurement_theta_min      3.6710
_cell_volume                     42496(4)
_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      293(2)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -108
_diffrn_reflns_number            98322
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.235
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.006
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             13824
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   'not measured'
_exptl_transmission_factor_min   'not measured'
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 3557 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_coef       0.00006(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1484
_refine_ls_number_reflns         25951
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.1020
_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^)+(0.1834P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2755
_refine_ls_wR_factor_ref         0.3379
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                13693
_reflns_number_total             25951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02049c2.cif
_cod_data_source_block           R-CHDA-FRP-8
_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        42496(5)
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_database_code               7125318
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.875
_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
 C5-C17A
 1.54 with sigma of 0.02
 C7EB-C38
 1.54 with sigma of 0.02
 H1CA-H83B
 2.5 with sigma of 0.02
3. Rigid bond restraints
 N24, C4BA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8BA, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6BA, C99
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C83, N5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C68, C101, C2BA, C24, C24A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4BA, N24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N44, C1FA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C19 \\sim C8BA: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C6BA \\sim C99: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C83 \\sim N5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C24 \\sim C2BA \\sim C24A \\sim C101 \\sim C68: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
N24 \\sim C4BA: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N44 \\sim C1FA: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C7EA) = Uanis(C7EB)
Uanis(C4DA) = Uanis(C4DB)
Uanis(C24) = Uanis(C24A)
Uanis(C17) = Uanis(C17A)
Uanis(C5FA) = Uanis(C5FB)
Uanis(C45) = Uanis(C45A)
5. Others
 Sof(H38C)=Sof(H38D)=Sof(C7EB)=Sof(H7ED)=Sof(H7EE)=Sof(H7EF)=1-FVAR(1)
 Sof(H38A)=Sof(H38B)=Sof(C7EA)=Sof(H7EA)=Sof(H7EB)=Sof(H7EC)=FVAR(1)
 Sof(H56C)=Sof(H56D)=Sof(C4DB)=Sof(H4DD)=Sof(H4DE)=Sof(H4DF)=1-FVAR(2)
 Sof(H56A)=Sof(H56B)=Sof(C4DA)=Sof(H4DA)=Sof(H4DB)=Sof(H4DC)=FVAR(2)
 Sof(H2BC)=Sof(H2BD)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(3)
 Sof(H2BA)=Sof(H2BB)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(3)
 Sof(H5BC)=Sof(H5BD)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(4)
 Sof(H5AA)=Sof(H5AB)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(4)
 Sof(H2EC)=Sof(H2ED)=Sof(C5FB)=Sof(H5FD)=Sof(H5FE)=Sof(H5FF)=1-FVAR(5)
 Sof(H2EA)=Sof(H2EB)=Sof(C5FA)=Sof(H5FA)=Sof(H5FB)=Sof(H5FC)=FVAR(5)
 Sof(H49C)=Sof(H49D)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(6)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(H49A)=Sof(H49B)=FVAR(6)
6.a Ternary CH refined with riding coordinates:
 C21(H21), C0FA(H0FA), C4EA(H4EA), C13(H13), C8EA(H8EA), C20(H20), C6CA(H6CA),
 C0EA(H0EA), C4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C3CA(H3CA,H3CB), C56(H56A,H56B), C56(H56C,H56D), C60(H60A,H60B), C67(H67A,
 H67B), C68(H68A,H68B), C69(H69A,H69B), C78(H78A,H78B), C81(H81A,H81B),
 C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C87(H87A,H87B), C96(H96A,H96B),
  C101(H10A,H10B), C1(H1A,H1B), C3DA(H3DA,H3DB), C15(H15A,H15B), C18(H18A,H18B),
  C2EA(H2EA,H2EB), C2EA(H2EC,H2ED), C5CA(H5CA,H5CB), C2BA(H2BA,H2BB), C2BA(H2BC,
 H2BD), C9EA(H9EA,H9EB), C3FA(H3FA,H3FB), C7(H7A,H7B), C22(H22A,H22B), C23(H23A,
 H23B), C25(H25A,H25B), C27(H27A,H27B), C5DA(H5DA,H5DB), C35(H35A,H35B),
 C38(H38A,H38B), C38(H38C,H38D), C40(H40A,H40B), C42(H42A,H42B), C43(H43A,H43B),
  C44(H44A,H44B), C46(H46A,H46B), C49(H49A,H49B), C49(H49C,H49D), C50(H50A,
 H50B), C3(H3A,H3B), C5(H5AA,H5AB), C5(H5BC,H5BD), C7FA(H7FA,H7FB), C8(H8A,H8B),
  C9(H9A,H9B), C16(H16A,H16B), C4FA(H4FA,H4FB)
6.c Me refined with riding coordinates:
 C5AA(H5AC,H5AD,H5AE), C3EA(H3EA,H3EB,H3EC), C24(H24A,H24B,H24C), C9CA(H9CA,
 H9CB,H9CC), C4DA(H4DA,H4DB,H4DC), C45(H45A,H45B,H45C), C17(H17A,H17B,H17C),
 C7EA(H7EA,H7EB,H7EC), C5FA(H5FA,H5FB,H5FC), C7EB(H7ED,H7EE,H7EF), C4DB(H4DD,
 H4DE,H4DF), C24A(H24D,H24E,H24F), C17A(H17D,H17E,H17F), C5FB(H5FD,H5FE,H5FF),
 C45A(H45D,H45E,H45F)
6.d Aromatic/amide H refined with riding coordinates:
 C6DA(H6DA), C2AA(H2AA), C1AA(H1AA), C12(H12), C1DA(H1DA), C7DA(H7DA),
 C2CA(H2CA), C26(H26), C30(H30), C8DA(H8DA), C36(H36), C0CA(H0CA), C39(H39),
 C1CA(H1CA), C8CA(H8CA), C51(H51), C52(H52), C58(H58), C59(H59), C61(H61),
 C63(H63), C66(H66), C72(H72), C73(H73), C76(H76), C77(H77), C86(H86), C97(H97),
  C99(H99), C7AA(H7AA), C5EA(H5EA), C6BA(H6BA), C14(H14), C0DA(H0DA),
 C6EA(H6EA), C6FA(H6FA)
;
_shelx_res_checksum              772
_shelx_fab_checksum              93930
_olex2_submission_special_instructions 'No special instructions were received'