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_4131625
_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 6P-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?/>!?/>/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 6P-1.
;
_chemical_formula_moiety         'C228 H216 N32'
_chemical_formula_sum            'C228 H216 N32'
_chemical_formula_weight         3404.32
_chemical_melting_point          ?
_chemical_name_common            6P-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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-07-21
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   29.0242(9)
_cell_length_b                   29.0242(9)
_cell_length_c                   30.6505(11)
_cell_measurement_reflns_used    6643
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      65.9970
_cell_measurement_theta_min      3.7440
_cell_volume                     22360.9(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      223.00(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 0.986
_diffrn_measurement_details
;
  1 omega   24.00   89.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      101.9495  -30.0000  150.0000 65

  2 omega -110.00  -11.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0248  -57.0000  -30.0000 99

  3 omega -114.00  -13.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0248  -77.0000   90.0000 101

  4 omega -127.00  -37.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0248  178.0000   90.0000 90

  5 omega   75.00  171.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      101.9495   30.0000  -30.0000 96

  6 omega   31.00  108.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      101.9495  -94.0000 -180.0000 77

  7 omega   24.00   67.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      101.9495  -30.0000   60.0000 43

  8 omega   72.00  172.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      101.9495   30.0000   60.0000 100

  9 omega   35.00  107.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      101.9495 -125.0000   90.0000 72

 10 omega   32.00  132.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      101.9495  -61.0000 -120.0000 100

 11 omega   28.00  115.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      101.9495  -56.0000   45.0000 87

 12 omega  -18.00    9.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2748   38.0000  -30.0000 27

 13 omega   -2.00   24.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2748   38.0000   30.0000 26

 14 omega   58.00  121.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2748  178.0000    0.0000 63

 15 omega   56.00  105.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745  -94.0000  -90.0000 49

 16 omega  146.00  172.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745  125.0000  120.0000 26

 17 omega   68.00   96.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745  -77.0000   90.0000 28

 18 omega  112.00  138.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745  125.0000  120.0000 26

 19 omega   44.00   75.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745  -45.0000 -180.0000 31

 20 omega   85.00  111.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745  -15.0000   30.0000 26

 21 omega   36.00   71.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      102.5745  -15.0000   30.0000 35
;
_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      0.0022134000
_diffrn_orient_matrix_UB_12      -0.0145426000
_diffrn_orient_matrix_UB_13      -0.0480274000
_diffrn_orient_matrix_UB_21      0.0480206000
_diffrn_orient_matrix_UB_22      0.0558835000
_diffrn_orient_matrix_UB_23      -0.0078322000
_diffrn_orient_matrix_UB_31      0.0379874000
_diffrn_orient_matrix_UB_32      -0.0204398000
_diffrn_orient_matrix_UB_33      0.0127053000
_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     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            53848
_diffrn_reflns_point_group_measured_fraction_full 0.890
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.174
_diffrn_reflns_theta_min         5.295
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.351
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72572
_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_density_diffrn    0.758
_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         0.247
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   2.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         16778
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0820P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1796
_reflns_Friedel_coverage         0.766
_reflns_Friedel_fraction_full    0.781
_reflns_Friedel_fraction_max     0.755
_reflns_number_gt                8507
_reflns_number_total             16778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            (6P)-1.cif
_cod_data_source_block           6P-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        22360.9(16)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4131625
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C228H216N32
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.933
_reflns_odcompleteness_completeness 99.98
_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. Restrained distances
 C13-C02I
 1.34 with sigma of 0.01
 C4-C1
 1.34 with sigma of 0.005
 C004-C4
 1.54 with sigma of 0.01
 C011_$1-C13_$2
 1.54 with sigma of 0.01
 C017-C1
 1.54 with sigma of 0.01
3. Rigid bond restraints
 C017, C1, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 C13, C02I, C00W, C00V
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C017 \\sim C1 \\sim C4: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.08
C00V \\sim C13 \\sim C02I \\sim C00W: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.08
5.a Secondary CH2 refined with riding coordinates:
 C01G(H01B,H01C), C01K(H01D,H01E), C01L(H01F,H01G), C01Q(H01H,H01J), C01T(H01K,
 H01L), C021(H02A,H02B), C028(H02C,H02D), C02A(H02E,H02F), C02D(H02G,H02I),
 C02E(H02J,H02K), C02J(H02N,H02O), C02M(H02P,H02Q), C02N(H02R,H02S), C02Q(H02T,
 H02U), C02W(H02V,H02W), C02X(H02X,H02Y)
5.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C01P(H01P), C01A(H01A), C01N(H01N), C00F(H00F), C00H(H00H),
 C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00Q(H00Q), C00R(H00R),
 C00S(H00S), C00T(H00T), C00X(H00X), C009(H009), C010(H010), C023(H023),
 C012(H012), C013(H013), C015(H015), C00O(H00O), C00I(H00I), C025(H025),
 C02H(H02H), C01I(H01I), C01Y(H01Y), C019(H019), C005(H005), C018(H018),
 C01R(H01R), C01U(H01U), C01V(H01V), C01W(H01W), C01Z(H01Z), C022(H022),
 C024(H024), C029(H029), C02F(H02L), C02G(H02M)
5.c Fitted hexagon refined as free rotating group:
 C00D(C017,C01P,C01A,C01H,C01N), C00X(C00V,C009,C010,C01M,C023), C01B(C00O,
 C00I,C00W,C025,C02H), C01J(C01Y,C019,C007,C005,C018)
;
_olex2_date_sample_data_collection 2016-07-16
_olex2_submission_special_instructions 'No special instructions were received'