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_1548372
_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            (CAAA)-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                   23.1134(9)
_cell_length_b                   23.1134(9)
_cell_length_c                   52.322(3)
_cell_measurement_reflns_used    7819
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      61.9260
_cell_measurement_theta_min      4.0150
_cell_volume                     24207.1(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      100.01(10)
_diffrn_detector_area_resol_mean 10.3415
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega  -43.00   30.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7424   38.0000  -30.0000 146

  2 omega  -25.00   24.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7424   38.0000 -180.0000 98

  3 omega  -49.00   32.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7424   38.0000   90.0000 162

  4 omega   64.00  166.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981   30.0000  -60.0000 204

  5 omega  106.00  158.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981  125.0000   90.0000 104

  6 omega  108.00  155.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981  125.0000 -120.0000 94

  7 omega   36.00   79.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981  -61.0000 -120.0000 86

  8 omega   71.00  166.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981   45.0000   30.0000 190

  9 omega   96.00  121.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981  -61.0000 -120.0000 50

 10 omega   94.00  121.50   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.7981  125.0000 -150.0000 55
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            29315
_diffrn_reflns_point_group_measured_fraction_full 0.753
_diffrn_reflns_point_group_measured_fraction_max 0.789
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.661
_diffrn_reflns_theta_min         3.825
_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  0.88191
_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)
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       block
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_exptl_transmission_factor_max   'Not measured'
_exptl_transmission_factor_min   'Not measured'
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 3565 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.8(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         14704
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0696
_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^)+(0.1535P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1906
_refine_ls_wR_factor_ref         0.2059
_reflns_Friedel_coverage         0.620
_reflns_Friedel_fraction_full    0.577
_reflns_Friedel_fraction_max     0.604
_reflns_number_gt                10078
_reflns_number_total             14704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms12469-s4.cif
_cod_data_source_block           (CAAA)-2
_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        24207(2)
_cod_database_code               1548372
_shelx_estimated_absorpt_t_max   0.886
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2AA-C22
 1.54 with sigma of 0.02
 C2AA-C23
 2.55 with sigma of 0.02
 C23-C22
 1.54 with sigma of 0.02
 C31-C6AA
 1.54 with sigma of 0.02
 C1AA-C31
 2.55 with sigma of 0.02
 C2AB-C22
 1.54 with sigma of 0.02
 C26-C13
 1.54 with sigma of 0.02
 C26-C14
 2.55 with sigma of 0.02
 C7-C25
 1.54 with sigma of 0.02
 C7-C0AA
 1.54 with sigma of 0.02
 H64A-H2A
 2 with sigma of 0.02
 H64A-H7AB
 1.9 with sigma of 0.02
 C61-C27
 1.54 with sigma of 0.02
 C27-C16
 1.54 with sigma of 0.02
 C61-C16
 2.55 with sigma of 0.02
 C11-C27
 2.55 with sigma of 0.02
 C16-C11
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C6, C22, C23, C2AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6AA, C5AA, C1AA, C31
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C12, C13, C14, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C24, C0AA, C7, C25
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C63, C64, C1, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C65, C7AA, C62
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11, C16, C27, C61
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C6 \\sim C22 \\sim C23 \\sim C2AA: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C6AA \\sim C5AA \\sim C1AA \\sim C31: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C12 \\sim C13 \\sim C14 \\sim C26: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C24 \\sim C0AA \\sim C7 \\sim C25: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C64 \\sim C1 \\sim C3 \\sim C63: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C7AA \\sim C2 \\sim C65 \\sim C62: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C11 \\sim C16 \\sim C27 \\sim C61: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C31) = Uanis(C31A)
Uanis(C2AA) = Uanis(C2AB)
5. Others
 Sof(H6AC)=Sof(H6AD)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(H6AA)=Sof(H6AB)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(H22C)=Sof(H22D)=Sof(C2AB)=Sof(H2AD)=Sof(H2AE)=Sof(H2AF)=1-FVAR(2)
 Sof(H22A)=Sof(H22B)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C005(H005), C009(H009), C00E(H00F), C00K(H00K)
6.b Secondary CH2 refined with riding coordinates:
 C006(H00A,H00B), C008(H00C,H00D), C00G(H00H,H00I), C00O(H00N,H00O), C00S(H00P,
 H00Q), C010(H01A,H01B), C01A(H01C,H01D), C01I(H01E,H01F), C6AA(H6AA,H6AB),
 C6AA(H6AC,H6AD), C5AA(H5AA,H5AB), C4(H4A,H4B), C6(H6A,H6B), C1AA(H1AA,H1AB),
 C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C16(H16A,H16B), C22(H22A,H22B), C22(H22C,H22D), C23(H23A,H23B), C24(H24A,H24B),
  C0AA(H0AA,H0AB), C7(H7A,H7B), C27(H27A,H27B), C4AA(H4AA,H4AB), C63(H63A,H63B),
  C62(H62A,H62B), C64(H64A,H64B), C65(H65A,H65B), C1(H1A,H1B), C2(H2A,H2B)
6.c Me refined with riding coordinates:
 C25(H25A,H25B,H25C), C2AA(H2AA,H2AB,H2AC), C26(H26A,H26B,H26C), C31(H31A,H31B,
 H31C), C3AA(H3AA,H3AB,H3AC), C31A(H31D,H31E,H31F), C2AB(H2AD,H2AE,H2AF),
 C61(H61A,H61B,H61C), C3(H3A,H3B,H3C), C7AA(H7AA,H7AB,H7AC)
6.d Aromatic/amide H refined with riding coordinates:
 C007(H007), C00B(H00E), C00F(H00G), C00H(H00J), C00L(H00L), C00M(H00M),
 C00T(H00T), C00V(H00V), C00Y(H00Y), C012(H012), C017(H017), C01J(H01J),
 C01P(H01P), C01X(H01X), C01B(H01G), C01V(H01V)
;
_shelx_res_checksum              20652
_shelx_hkl_checksum              30630
_olex2_submission_special_instructions 'No special instructions were received'