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_1548374
_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_melting_point          ?
_chemical_name_common            (CCCA)-3
_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                   23.2072(6)
_cell_length_b                   23.2072(6)
_cell_length_c                   52.1786(11)
_cell_measurement_reflns_used    7656
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      63.0010
_cell_measurement_theta_min      4.0200
_cell_volume                     24337.1(10)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.3415
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cuat zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.844
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            16439
_diffrn_reflns_point_group_measured_fraction_full 0.501
_diffrn_reflns_point_group_measured_fraction_max 0.590
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         61.166
_diffrn_reflns_theta_min         3.809
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    0.721
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   'Not measured'
_exptl_transmission_factor_min   'Not measured'
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.7(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         9834
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0646
_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^)+(0.1379P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.186
_reflns_Friedel_fraction_full    0.157
_reflns_Friedel_fraction_max     0.185
_reflns_number_gt                7008
_reflns_number_total             9834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms12469-s6.cif
_cod_data_source_block           (CCCA)-3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'Not measured' was changed to '?' -
the value is undefined or not given.

'_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        24337.1(13)
_cod_database_code               1548374
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.887
_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
 C4-C022
 1.54 with sigma of 0.02
 C01V-C01E
 1.54 with sigma of 0.02
 C01Y-C01V
 1.54 with sigma of 0.02
 C19-C01Y
 1.54 with sigma of 0.02
 C19-C15
 1.54 with sigma of 0.02
 C9-C7
 1.54 with sigma of 0.02
 C6-C021
 1.54 with sigma of 0.02
 C7-C6
 1.54 with sigma of 0.02
 C27-C0
 1.54 with sigma of 0.02
 C27-C01W
 2.55 with sigma of 0.02
 C12-C01Z
 1.54 with sigma of 0.02
 C0AA-C026
 1.54 with sigma of 0.02
 C27-C0
 1.54 with sigma of 0.02
 C46-C12
 1.54 with sigma of 0.02
 C20A-C1AA
 1.54 with sigma of 0.02
 C4-C20
 1.54 with sigma of 0.02
 C1AB-C20
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C006, C00B, C00J, C00L, C01C, C01L
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C011, C01J
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C01F, C01M
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C01V, C01Y, C15, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C01T, C01W, C0, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C46, C12, C01Z, C01H
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C022, C4, C20, C20A, C1AA, C1AB
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C006 \\sim C00B \\sim C00J \\sim C00L \\sim C01C \\sim C01L: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C011 \\sim C01J: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C01F \\sim C01M: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C01S \\sim C020 \\sim C026 \\sim C0AA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C01V \\sim C01Y \\sim C15 \\sim C19: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C021 \\sim C6 \\sim C7 \\sim C9: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C01W \\sim C0 \\sim C27: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C46 \\sim C12 \\sim C01Z \\sim C01H: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C022 \\sim C4 \\sim C20 \\sim C20A \\sim C1AA \\sim C1AB: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C20) = Uanis(C20A)
Uanis(C1AA) = Uanis(C1AB)
5. Others
 Sof(H4BD)=Sof(H4BE)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C1AA)=Sof(H1AB)=
 Sof(H1AC)=Sof(H1AD)=1-FVAR(1)
 Sof(H4AB)=Sof(H4AC)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C1AB)=Sof(H1AE)=
 Sof(H1AF)=Sof(H1AG)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C005(H005), C00B(H00F), C00E(H00G), C00L(H00M)
6.b Secondary CH2 refined with riding coordinates:
 C006(H00A,H00B), C009(H00C,H00D), C00J(H00J,H00K), C00V(H00N,H00P), C00Y(H00Q,
 H00R), C014(H01A,H01B), C015(H01C,H01D), C016(H01E,H01F), C01B(H01G,H01H),
 C01C(H01I,H01J), C01H(H01L,H01M), C01I(H01N,H01O), C01L(H01P,H01Q), C01O(H01U,
 H01V), C01Q(H01X,H01Y), C01S(H01,HB), C01T(H0AA,HC), C01V(H2AA,HD), C01W(H3AA,
 HE), C01Y(H5AA,HF), C01Z(H6AA,HG), C020(H02A,H02B), C021(H02C,H02D), C022(H02E,
 H02F), C026(H02G,H02H), C4(H4AB,H4AC), C4(H4BD,H4BE), C6(H6A,H6B), C7(H7A,H7B),
  C20(H20A,H20B), C12(H12A,H12B), C0(H0A,H0B), C20A(H20C,H20D), C19(H19A,H19B)
6.c Me refined with riding coordinates:
 C01N(H01R,H01S,H01T), C01R(H01Z,H,HA), C9(H9A,H9B,H9C), C0AA(H0AB,H0AC,H0AD),
 C1AA(H1AB,H1AC,H1AD), C1AB(H1AE,H1AF,H1AG), C15(H15A,H15B,H15C), C27(H27A,H27B,
 H27C), C46(H46A,H46B,H46C)
6.d Aromatic/amide H refined with riding coordinates:
 C008(H008), C00A(H00E), C00F(H00H), C00I(H00I), C00K(H00L), C00O(H00O),
 C00S(H00S), C00W(H00W), C00X(H00X), C010(H010), C013(H013), C018(H018),
 C01G(H01K), C01P(H01W), C01U(H1AA), C01X(H4AA)
;
_shelx_res_checksum              3684
_shelx_hkl_checksum              33576
_olex2_submission_special_instructions 'No special instructions were received'