Molecular Face-Rotating Cube with Emergent Chiral and Fluorescence Properties.
Qu, Hang; Wang, Yu; Li, Zhihao; Wang, Xinchang; Fang, Hongxun; Tian, Zhongqun; Cao, Xiaoyu; Journal of the American Chemical Society 139 (2017) 18142–18145; doi:10.1021/jacs.7b07657

data_4131626
_publ_section_title
;
 Molecular Face-Rotating Cube with Emergent Chiral and Fluorescence
 Properties.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18142
_journal_page_last               18145
_journal_paper_doi               10.1021/jacs.7b07657
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration
;
The absolute configuration of 2P4M-2 in crystal was assigned by comparing the (ZINDO/S)-predicted circular dichroism(CD) spectrum 
of crystal structures to the experimental CD spectrum, instead of anomalous dispersion effects in diffraction measurements on 
the crystal and the derived Flack x parameter. The cage crystal contains only light atoms (N, O, C, H) and has large void regions, 
therefore it&#x00A1;&#x00AF;s extremely difficult to determine the absolute configuration by the Flack x parameter with such large uncertainty. 
However,the (ZINDO/S)-predicted CD spectrum by using crystal structures highly matched the experimental one
(see Supplementary Method).Therefore, this evidence can be used to determine the absolute configuration of 2P4M-2.
;
_chemical_formula_moiety         'C228 H216 N32'
_chemical_formula_sum            'C228 H216 N32'
_chemical_formula_weight         3404.32
_chemical_melting_point          ?
_chemical_name_common            2P4M-2
_space_group_crystal_system      hexagonal
_space_group_IT_number           181
_space_group_name_Hall           'P 64 2 (0 0 2)'
_space_group_name_H-M_alt        'P 64 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-05-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   35.7068(6)
_cell_length_b                   35.7068(6)
_cell_length_c                   22.6261(4)
_cell_measurement_reflns_used    11773
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      67.0090
_cell_measurement_theta_min      3.7570
_cell_volume                     24982.9(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -50.00   36.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1498   38.0000   90.0000 86

  2 omega -119.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1498  -77.0000   60.0000 113

  3 omega   75.00  177.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745   45.0000  150.0000 102

  4 omega   94.00  170.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745  125.0000   90.0000 76

  5 omega   28.00   98.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745  -45.0000 -180.0000 70

  6 omega   72.00  178.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745   30.0000 -120.0000 106

  7 omega   18.00   49.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745  -94.0000   30.0000 31

  8 omega  -70.00  -27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1498  -57.0000  150.0000 43

  9 omega   75.00  120.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745   45.0000  -30.0000 45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0483933000
_diffrn_orient_matrix_UB_12      0.0143175000
_diffrn_orient_matrix_UB_13      -0.0045028000
_diffrn_orient_matrix_UB_21      -0.0006834000
_diffrn_orient_matrix_UB_22      0.0094145000
_diffrn_orient_matrix_UB_23      -0.0663226000
_diffrn_orient_matrix_UB_31      0.0118217000
_diffrn_orient_matrix_UB_32      0.0467523000
_diffrn_orient_matrix_UB_33      0.0147772000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            99433
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.116
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    0.679
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             5424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   'Not measured'
_exptl_transmission_factor_min   'Not measured'
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 3703 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.95(17)
_refine_ls_extinction_coef       0.00022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         15952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0548
_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^)+(0.1018P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1676
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                10550
_reflns_number_total             15952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            (2P4M)-2.cif
_cod_data_source_block           2P4M-2
_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        24982.9(10)
_cod_original_sg_symbol_Hall     'P 64 2c (0 0 -1)'
_cod_database_code               4131626
_shelx_shelxl_version_number     2014-7
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.940
_exptl_absorpt_special_details   'Not measured'
_reflns_odcompleteness_completeness 99.87
_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
2.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C55(H55A,H55B), C56(H56A,H56B), C31(H31A,H31B), C37(H37A,
 H37B), C53(H53A,H53B), C36(H36A,H36B), C52(H52A,H52B), C29(H29A,H29B),
 C32(H32A,H32B), C28(H28A,H28B), C57(H57A,H57B)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C51(H51), C49(H49), C40(H40), C7(H7), C19(H19), C14(H14), C44(H44),
 C50(H50), C4(H4), C35(H35), C17(H17), C47(H47), C20(H20), C22(H22), C41(H41),
 C43(H43), C25(H25), C23(H23), C46(H46), C13(H13), C26(H26), C10(H10), C16(H16),
  C8(H8), C54(H54), C33(H33), C11(H11), C5(H5), C27(H27)
;
_olex2_submission_original_sample_id (2P4M)-2
_olex2_submission_special_instructions 'No special instructions were received'