Assembled molecular face-rotating polyhedra to transfer chirality from two to three dimensions
Xinchang Wang; Yu Wang; Huayan Yang; Hongxun Fang; Ruixue Chen; Yibin Sun; Nanfeng Zheng; Kai Tan; Xin Lu; Zhongqun Tian; Xiaoyu Cao; Nature Communications 7 (2016) 12469–; doi:10.1038/ncomms12469

data_1548371
_publ_section_title
;
 Assembled molecular face-rotating polyhedra to transfer chirality from
 two to three dimensions
;
_journal_name_full               'Nature Communications'
_journal_page_first              12469
_journal_paper_doi               10.1038/ncomms12469
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C252 H324 N12'
_chemical_formula_sum            'C252 H324 N12'
_chemical_formula_weight         3521.21
_chemical_name_common            (AAAA)-2
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.3017(3)
_cell_length_b                   23.3017(3)
_cell_length_c                   51.4329(7)
_cell_measurement_reflns_used    8934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.6990
_cell_measurement_theta_min      4.0620
_cell_volume                     24185.0(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.963
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            20428
_diffrn_reflns_point_group_measured_fraction_full 0.718
_diffrn_reflns_point_group_measured_fraction_max 0.684
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.790
_diffrn_reflns_theta_min         3.794
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    0.725
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   'Not measured'
_exptl_transmission_factor_min   'Not measured'
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.2(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         14879
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0960
_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^)+(0.1688P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2428
_refine_ls_wR_factor_ref         0.2551
_reflns_Friedel_coverage         0.420
_reflns_Friedel_fraction_full    0.444
_reflns_Friedel_fraction_max     0.404
_reflns_number_gt                10504
_reflns_number_total             14879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms12469-s3.cif
_cod_data_source_block           (AAAA)-2
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        24184.9(7)
_cod_database_code               1548371
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.861
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9AA-C61
 1.54 with sigma of 0.02
 C74-C1AA
 1.54 with sigma of 0.02
 C67-C0BA
 1.54 with sigma of 0.02
 C67-C56
 1.54 with sigma of 0.02
 C3AA-C0BA
 1.54 with sigma of 0.02
 C2AA-C69
 2.55 with sigma of 0.02
 C72-C2AA
 1.54 with sigma of 0.02
 C2AA-C1BA
 1.54 with sigma of 0.02
 C8AA-C80
 1.54 with sigma of 0.02
 C7-C1AA
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C49, C7AA, C5, C0AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C27, C32, C62, C68
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C69, C72, C2AA, C1BA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C56, C67, C0BA, C3AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C61, C80, C9AA, C8AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C60, C74, C1AA, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C66, C70, C71, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C64, C65, C76, C81
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C49 \\sim C7AA \\sim C5 \\sim C0AA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C27 \\sim C32 \\sim C62 \\sim C68: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C69 \\sim C72 \\sim C2AA \\sim C1BA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C56 \\sim C67 \\sim C0BA \\sim C3AA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C61 \\sim C80 \\sim C9AA \\sim C8AA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C60 \\sim C74 \\sim C1AA \\sim C7: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C66 \\sim C70 \\sim C71 \\sim C1: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C64 \\sim C65 \\sim C76 \\sim C81: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
5.a Ternary CH refined with riding coordinates:
 C8(H8), C17(H17), C35(H35), C39(H39)
5.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C30(H30A,H30B), C32(H32A,H32B), C37(H37A,H37B), C42(H42A,
 H42B), C43(H43A,H43B), C46(H46A,H46B), C49(H49A,H49B), C56(H56A,H56B),
 C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
  C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,
 H67B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B),
 C74(H74A,H74B), C76(H76A,H76B), C80(H80A,H80B), C7AA(H7AA,H7AB), C9AA(H9AA,
 H9AB), C0BA(H0BA,H0BB), C5(H5A,H5B), C1AA(H1AA,H1AB), C2AA(H2AA,H2AB)
5.c Me refined with riding coordinates:
 C68(H68A,H68B,H68C), C1(H1A,H1B,H1C), C0AA(H0AA,H0AB,H0AC), C7(H7A,H7B,H7C),
 C8AA(H8AA,H8AB,H8AC), C1BA(H1BA,H1BB,H1BC), C81(H81A,H81B,H81C)
5.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C18(H18), C19(H19), C20(H20), C22(H22), C25(H25), C28(H28),
 C29(H29), C34(H34), C36(H36), C41(H41), C45(H45), C48(H48), C51(H51), C54(H54),
  C55(H55)
5.e Idealised Me refined as rotating group:
 C3AA(H3AA,H3AB,H3AC)
;
_shelx_res_checksum              96997
_shelx_hkl_checksum              32697
_olex2_submission_special_instructions 'No special instructions were received'