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_4131627
_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 4P2M-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 4P2M-2.
;
_chemical_formula_moiety         'C228 H216 N32'
_chemical_formula_sum            'C228 H216 N32'
_chemical_formula_weight         3404.32
_chemical_melting_point          ?
_chemical_name_common            4P2M-2
_space_group_crystal_system      hexagonal
_space_group_IT_number           180
_space_group_name_Hall           'P 62 2 (0 0 4)'
_space_group_name_H-M_alt        'P 62 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                   35.6733(20)
_cell_length_b                   35.6733(20)
_cell_length_c                   22.6222(16)
_cell_measurement_reflns_used    3014
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      57.8280
_cell_measurement_theta_min      3.7600
_cell_volume                     24932(3)
_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    'ShelXD (Sheldrick, 2008)'
_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 0.999
_diffrn_measurement_details
;
  1 omega -104.00  -21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3288  -57.0000  -60.0000 83

  2 omega  -94.00  -10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.3288  125.0000   90.0000 84

  3 omega   27.00  110.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       89.3368  -77.0000   30.0000 83

  4 omega   97.00  150.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       89.3368  125.0000  120.0000 53

  5 omega   94.00  163.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       89.3368  125.0000  -30.0000 69

  6 omega  101.00  163.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       89.3368  125.0000  -60.0000 62

  7 omega   57.00  113.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       89.3368   77.0000 -150.0000 56
;
_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      -0.0413808000
_diffrn_orient_matrix_UB_12      -0.0379542000
_diffrn_orient_matrix_UB_13      0.0264598000
_diffrn_orient_matrix_UB_21      -0.0056522000
_diffrn_orient_matrix_UB_22      0.0318618000
_diffrn_orient_matrix_UB_23      0.0399018000
_diffrn_orient_matrix_UB_31      -0.0272230000
_diffrn_orient_matrix_UB_32      0.0054442000
_diffrn_orient_matrix_UB_33      -0.0484640000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1669
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73412
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        61.168
_diffrn_reflns_theta_max         61.168
_diffrn_reflns_theta_min         3.465
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33819
_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    0.680
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             5424
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   'Not measured'
_exptl_transmission_factor_min   'Not measured'
_refine_diff_density_max         0.132
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details
;
 Flack x determined using 1695 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.9(3)
_refine_ls_extinction_coef       0.00022(3)
_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   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         12788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0519P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1731
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5972
_reflns_number_total             12788
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            (4P2M)-2.cif
_cod_data_source_block           4P2M-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_sg_symbol_Hall     'P 62 2c (0 0 1)'
_cod_database_code               4131627
_shelx_shelxl_version_number     2014-7
_chemical_oxdiff_formula         C228H216N32
_shelx_estimated_absorpt_t_max   1.00000
_shelx_estimated_absorpt_t_min   0.33819
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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:
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C47(H47A,
 H47B), C48(H48A,H48B), C49(H49A,H49B), C51(H51A,H51B), C53(H53A,H53B),
 C54(H54A,H54B), C56(H56A,H56B), C57(H57A,H57B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26),
  C29(H29), C30(H30), C32(H32), C33(H33), C35(H35), C36(H36), C38(H38),
 C39(H39), C40(H40), C41(H41), C46(H46), C50(H50), C52(H52), C55(H55)
;
_olex2_submission_special_instructions 'No special instructions were received'