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_1548373
_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            (CCCC)-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                   23.121(2)
_cell_length_b                   23.121(2)
_cell_length_c                   51.666(2)
_cell_measurement_reflns_used    2603
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      55.2440
_cell_measurement_theta_min      4.0510
_cell_volume                     23919(3)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -50.00  33.00   1.00    5.00    --  -41.44  38.00  30.00   83
  2  \w     -4.00  28.00   1.00    5.00    --  -41.44  38.00  60.00   32
  3  \w     28.00  81.00   1.00   75.00    --  102.29 -30.00-180.00   53
  4  \w     54.00  98.00   1.00   75.00    --  102.29 -45.00  90.00   44
  5  \w    107.00 170.00   1.00   75.00    --  102.29 125.00  90.00   63
  6  \w     59.00  95.00   1.00   75.00    --  102.29 -45.00-150.00   36
  7  \w     52.00  88.00   1.00   75.00    --  102.29 -30.00 120.00   36
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0381429000
_diffrn_orient_matrix_UB_12      -0.0737301000
_diffrn_orient_matrix_UB_13      0.0084483000
_diffrn_orient_matrix_UB_21      0.0613775000
_diffrn_orient_matrix_UB_22      -0.0065387000
_diffrn_orient_matrix_UB_23      -0.0068571000
_diffrn_orient_matrix_UB_31      0.0266403000
_diffrn_orient_matrix_UB_32      0.0209840000
_diffrn_orient_matrix_UB_33      0.0277502000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.1002
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16509
_diffrn_reflns_point_group_measured_fraction_full 0.547
_diffrn_reflns_point_group_measured_fraction_max 0.544
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.215
_diffrn_reflns_theta_min         3.824
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65570
_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_density_diffrn    0.733
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   'Not measured'
_exptl_transmission_factor_min   'Not measured'
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.7(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.811
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         10620
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0725
_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^)+(0.0701P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1850
_reflns_Friedel_coverage         0.104
_reflns_Friedel_fraction_full    0.104
_reflns_Friedel_fraction_max     0.102
_reflns_number_gt                4843
_reflns_number_total             10620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms12469-s5.cif
_cod_data_source_block           (CCCC)-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        23921(4)
_cod_database_code               1548373
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.912
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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
 C7BA-C5
 1.43 with sigma of 0.02
 C1BA-C7BA
 1.5 with sigma of 0.02
 C57-C30
 1.54 with sigma of 0.01
 C8AA-C57
 1.54 with sigma of 0.01
 C8AA-C0CA
 1.54 with sigma of 0.01
 C1CA-C0CA
 1.54 with sigma of 0.01
 C7BA-C14
 1.54 with sigma of 0.02
 C5CA-C1
 1.54 with sigma of 0.02
 C9BA-C4BA
 1.54 with sigma of 0.02
 C9BA-C6CA
 1.54 with sigma of 0.02
 C6CA-C4BA
 2.55 with sigma of 0.02
 C72-C4CA
 1.54 with sigma of 0.02
 C4CA-C46
 1.54 with sigma of 0.02
 C46-C72
 2.55 with sigma of 0.02
 C59-C30
 1.54 with sigma of 0.02
 C9CB-C2A
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C3BA, C5, C8CA, C8, C2BA, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1BA, C6BA, C7BA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C57, C8AA, C0CA, C1CA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C14, C9AA, C3, C7CA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C58, C71, C1, C5CA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C56, C4BA, C9BA, C6CA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C46, C4CA, C72, C59
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C54, C67, C69, C73
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2CA, C2, C6, C9CA, C6A, C2A, C9CB
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1CA \\sim C0CA \\sim C8AA \\sim C57: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C14 \\sim C3 \\sim C9AA \\sim C7CA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C5CA \\sim C1 \\sim C71 \\sim C58: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C6CA \\sim C9BA \\sim C4BA \\sim C56: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C46 \\sim C4CA \\sim C72 \\sim C59: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C54 \\sim C67 \\sim C69 \\sim C73: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C2CA \\sim C2 \\sim C6 \\sim C9CA \\sim C6A \\sim C2A \\sim C9CB: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C6) = Uanis(C6A)
Uanis(C2) = Uanis(C2A)
Uanis(C9CA) = Uanis(C9CB)
5. Others
 Sof(H2CC)=Sof(H2CD)=Sof(C6A)=Sof(H6AB)=Sof(H6AC)=Sof(C2A)=Sof(H2AB)=Sof(H2AC)=
 Sof(C9CB)=Sof(H9CD)=Sof(H9CE)=Sof(H9CF)=1-FVAR(1)
 Sof(H2CA)=Sof(H2CB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(C9CA)=Sof(H9CA)=Sof(H9CB)=Sof(H9CC)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C2AA(H2AA), C3CA(H3CA), C22(H22), C37(H37)
6.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C31(H31A,H31B), C33(H33A,H33B), C40(H40A,H40B), C42(H42A,
 H42B), C45(H45A,H45B), C50(H50A,H50B), C51(H51A,H51B), C54(H54A,H54B),
 C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
  C61(H61A,H61B), C62(H62A,H62B), C67(H67A,H67B), C69(H69A,H69B), C71(H71A,
 H71B), C8AA(H8AA,H8AB), C4BA(H4BA,H4BB), C72(H72A,H72B), C2CA(H2CA,H2CB),
 C2CA(H2CC,H2CD), C14(H14A,H14B), C9AA(H9AA,H9AB), C3(H3A,H3B), C1(H1A,H1B),
 C9BA(H9BA,H9BB), C0CA(H0CA,H0CB), C4CA(H4CA,H4CB), C2(H2A,H2B), C6(H6A,H6B),
 C6A(H6AB,H6AC), C2A(H2AB,H2AC)
6.c Me refined with riding coordinates:
 C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C1CA(H1CA,H1CB,H1CC), C5CA(H5CA,
 H5CB,H5CC), C6CA(H6CA,H6CB,H6CC), C46(H46A,H46B,H46C), C9CA(H9CA,H9CB,H9CC),
 C9CB(H9CD,H9CE,H9CF)
6.d Aromatic/amide H refined with riding coordinates:
 C6AA(H6AA), C5AA(H5AA), C5BA(H5BA), C15(H15), C18(H18), C19(H19), C20(H20),
 C24(H24), C27(H27), C39(H39), C44(H44), C48(H48), C53(H53), C3BA(H3BA), C8(H8),
  C2BA(H2BA)
6.e Fitted hexagon refined as free rotating group:
 C3BA(C5,C8CA,C8,C2BA,C4)
6.f Idealised Me refined as rotating group:
 C7CA(H7CA,H7CB,H7CC)
;
_shelx_res_checksum              28928
_shelx_hkl_checksum              70291
_olex2_date_sample_data_collection 2015-02-03
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.825
_oxdiff_exptl_absorpt_empirical_full_min 0.580