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_4131624
_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 6M-1 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 6M-1.
;
_chemical_formula_moiety         'C228 H216 N32'
_chemical_formula_sum            'C228 H216 N32'
_chemical_formula_weight         3404.32
_chemical_melting_point          ?
_chemical_name_common            6M-1
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-05-09
_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                   28.1211(9)
_cell_length_b                   28.1211(9)
_cell_length_c                   30.4311(13)
_cell_measurement_reflns_used    5805
_cell_measurement_temperature    223.01(10)
_cell_measurement_theta_max      64.5070
_cell_measurement_theta_min      3.8840
_cell_volume                     20840.7(13)
_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      223.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega -117.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1498  -77.0000  -90.0000 102

  2 omega  -67.00   29.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1498   57.0000   30.0000 96

  3 omega  -32.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1498  -57.0000  120.0000 102

  4 omega   24.00  102.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4116  -94.0000   90.0000 78

  5 omega   35.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4116  -45.0000  120.0000 42

  6 omega   94.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4116  125.0000   60.0000 84

  7 omega   78.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4116   30.0000 -120.0000 100

  8 omega   57.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4116  -94.0000 -180.0000 51

  9 omega   32.00   60.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4116  -30.0000   60.0000 28

 10 omega   31.00   63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4116  -30.0000  -90.0000 32

 11 omega   45.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4116  -45.0000 -180.0000 53

 12 omega   32.00   80.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4116  -30.0000  -30.0000 48

 13 omega   38.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4116  -94.0000    0.0000 71

 14 omega   83.00  169.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4116   45.0000  150.0000 86
;
_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      -0.0374131000
_diffrn_orient_matrix_UB_12      -0.0009225000
_diffrn_orient_matrix_UB_13      -0.0373355000
_diffrn_orient_matrix_UB_21      0.0488986000
_diffrn_orient_matrix_UB_22      0.0511658000
_diffrn_orient_matrix_UB_23      -0.0205003000
_diffrn_orient_matrix_UB_31      0.0144698000
_diffrn_orient_matrix_UB_32      -0.0371586000
_diffrn_orient_matrix_UB_33      -0.0273877000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            35455
_diffrn_reflns_point_group_measured_fraction_full 0.788
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_theta_full        65.038
_diffrn_reflns_theta_max         65.037
_diffrn_reflns_theta_min         3.425
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84219
_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    0.814
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       cube
_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         0.270
_refine_diff_density_min         -0.135
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details
;
 Flack x determined using 1938 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   2.4(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         12455
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0934P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1762
_reflns_Friedel_coverage         0.577
_reflns_Friedel_fraction_full    0.576
_reflns_Friedel_fraction_max     0.576
_reflns_number_gt                7802
_reflns_number_total             12455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            (6M)-1.cif
_cod_data_source_block           6M-1
_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        20840.7(16)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4131624
_shelx_shelxl_version_number     2014-7
_chemical_oxdiff_formula         C228H216N32
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.928
_reflns_odcompleteness_completeness 95.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C38-C39
 1.34 with sigma of 0.001
 C1-C2
 1.34 with sigma of 0.001
 C38-C52
 1.54 with sigma of 0.001
 C1-C15
 1.54 with sigma of 0.001
 C39_$1-C40_$1
 1.54 with sigma of 0.001
 C2-C3
 1.54 with sigma of 0.001
 C37-N9
 1.47 with sigma of 0.001
3. Rigid bond restraints
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C36(H36A,
 H36B), C37(H37A,H37B), C68(H68A,H68B), C70(H70A,H70B), C71(H71A,H71B),
 C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B),
  C77(H77A,H77B), C78(H78A,H78B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C41(H41), C42(H42), C44(H44),
 C45(H45), C47(H47), C48(H48), C50(H50), C51(H51), C53(H53), C54(H54), C56(H56),
  C57(H57), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C69(H69)
;
_olex2_submission_original_sample_id (6M)-1
_olex2_submission_special_instructions 'No special instructions were received'