The Fixed Propeller-Like Conformation of Tetraphenylethylene that Reveals Aggregation-Induced Emission Effect, Chiral Recognition, and Enhanced Chiroptical Property.
Xiong, Jia-Bin; Feng, Hai-Tao; Sun, Jian-Ping; Xie, Wen-Zhao; Yang, Dong; Liu, Minghua; Zheng, Yan-Song; Journal of the American Chemical Society 138 (2016) 11469–11472; doi:10.1021/jacs.6b07087

data_4130814
_publ_section_title
;
 The Fixed Propeller-Like Conformation of Tetraphenylethylene that Reveals
 Aggregation-Induced Emission Effect, Chiral Recognition, and Enhanced
 Chiroptical Property.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11469
_journal_page_last               11472
_journal_paper_doi               10.1021/jacs.6b07087
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C H2 Cl2), C58 H44 O8'
_chemical_formula_sum            'C60 H48 Cl4 O8'
_chemical_formula_weight         1038.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-07-31
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206)
;
_audit_update_record
;
2016-08-02 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 103.704(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.7130(16)
_cell_length_b                   11.1639(12)
_cell_length_c                   16.1379(19)
_cell_measurement_reflns_used    3220
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.632
_cell_measurement_theta_min      2.240
_cell_volume                     2575.3(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13163
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.598
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 2540 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         8718
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0452P)^2^+0.8127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.917
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                7006
_reflns_number_total             8718
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {ee0768b6-70a8-4664-9930-86d3ad004332}
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_cod_data_source_file            ja6b07087_si_005.cif
_cod_data_source_block           a
_cod_database_code               4130814
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.945
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C50(H50A,H50B), C59(H59A,H59B), C8(H8A,H8B), C36(H36A,H36B),
 C15(H15A,H15B), C22(H22A,H22B), C29(H29A,H29B), C43(H43A,H43B), C60(H60A,H60B)
3.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C48(H48), C10(H10), C45(H45), C11(H11), C41(H41), C13(H13), C5(H5),
 C6(H6), C3(H3), C39(H39), C34(H34), C33(H33), C27(H27), C31(H31), C24(H24),
 C38(H38), C26(H26), C32(H32), C19(H19), C55(H55), C47(H47), C17(H17), C53(H53),
  C18(H18), C54(H54), C4(H4), C46(H46)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'