Helical Sulfono-γ-AApeptides with Aggregation-Induced Emission and Circularly Polarized Luminescence.
Shi, Yan; Yin, Guangqiang; Yan, Zhiping; Sang, Peng; Wang, Minghui; Brzozowski, Robert; Eswara, Prahathees; Wojtas, Lukasz; Zheng, Youxuan; Li, Xiaopeng; Cai, Jianfeng; Journal of the American Chemical Society 141 (2019) 12697–12706; doi:10.1021/jacs.9b05329

data_4127729
_publ_section_title
;
 Helical Sulfono-\g-AApeptides with Aggregation-Induced Emission and
 Circularly Polarized Luminescence.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12697
_journal_page_last               12706
_journal_paper_doi               10.1021/jacs.9b05329
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C243 H241 N23 O30 S7'
_chemical_formula_sum            'C243 H241 N23 O30 S7'
_chemical_formula_weight         4187.99
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_symmetry_space_group_name_Hall  'P 65 2 (0 0 1)'
_symmetry_space_group_name_H-M   'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.2882(14)
_cell_length_b                   17.2882(14)
_cell_length_c                   95.075(8)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.18
_cell_measurement_theta_min      2.32
_cell_volume                     24609(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0263
_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       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            44063
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        30.916
_diffrn_reflns_theta_max         30.916
_diffrn_reflns_theta_min         2.789
_diffrn_source                   'INCOATEC Imus micro-focus source'
_exptl_absorpt_coefficient_mu    0.852
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.848
_exptl_crystal_description       block
_exptl_crystal_F_000             6636
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.139
_refine_diff_density_min         -0.116
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
;
 Flack x determined using 526 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.087(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         2557
_refine_ls_number_restraints     1458
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0697
_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^)+(0.1688P)^2^+8.4749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1992
_refine_ls_wR_factor_ref         0.2171
_reflns_Friedel_coverage         0.546
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1947
_reflns_number_total             2557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05329_si_002.cif
_cod_data_source_block           ys_f_13
_cod_original_cell_volume        24609(4)
_cod_database_code               4127729
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.830
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C_3) \\sim Ueq: with sigma of 0.025 and sigma for terminal atoms of 0.05
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: HAAA(0.875) HAAB(0.875) HABC(0.125) HABD(0.125) HABE(0.125)
 NT(0.875) S1(0.875) O3(0.875) O2(0.875) C4(0.875) C9(0.875) H9(0.875)
 C8(0.875) H8(0.875) C7(0.875) C6(0.875) H6(0.875) C5(0.875) H5(0.875)
 CB(0.875) HBA(0.875) HBB(0.875) CG(0.875) HG(0.875) CD(0.875) HDA(0.875)
 HDB(0.875) HDC(0.875) HA(0.875) HBC(0.125) HBD(0.125) C10(0.875) C11(0.875)
 C12(0.875) C13(0.875) H13(0.875) C14(0.875) H14(0.875) C15(0.875) H15(0.875)
 C16(0.875) H16(0.875) C17(0.875) H17(0.875) C18(0.875) C19(0.875) H19(0.875)
 C20(0.875) H20(0.875) C21(0.875) H21(0.875) C22(0.875) H22(0.875) C23(0.875)
 H23(0.875) C24(0.875) C25(0.875) H25(0.875) C26(0.875) H26(0.875) C27(0.875)
 H27(0.875) C28(0.875) H28(0.875) C29(0.875) H29(0.875) HAAA(0.875) HAAB(0.875)
 HABC(0.125) HABD(0.125) HABE(0.125) NT(0.875) S1(0.875) O3(0.875) O2(0.875)
 C4(0.875) C9(0.875) H9(0.875) C8(0.875) H8(0.875) C7(0.875) C6(0.875)
 H6(0.875) C5(0.875) H5(0.875) CB(0.875) HBA(0.875) HBB(0.875) CG(0.875)
 HG(0.875) CD(0.875) HDA(0.875) HDB(0.875) HDC(0.875) HA(0.875) HBC(0.125)
 HBD(0.125) C10(0.875) C11(0.875) C12(0.875) C13(0.875) H13(0.875) C14(0.875)
 H14(0.875) C15(0.875) H15(0.875) C16(0.875) H16(0.875) C17(0.875) H17(0.875)
 C18(0.875) C19(0.875) H19(0.875) C20(0.875) H20(0.875) C21(0.875) H21(0.875)
 C22(0.875) H22(0.875) C23(0.875) H23(0.875) C24(0.875) C29(0.875) H29(0.875)
 C28(0.875) H28(0.875) C27(0.875) H27(0.875) C26(0.875) H26(0.875) C25(0.875)
 H25(0.875)
5.a Ternary CH refined with riding coordinates:
 CA(HA), CG(HG), CA(HA), CG(HG)
5.b Secondary CH2 refined with riding coordinates:
 CA(HAAA,HAAB), CB(HBA,HBB), CA(HAAA,HAAB), CB(HBA,HBB)
5.c Me refined with riding coordinates:
 CB(HBA,HBB,HBC), CA(HABC,HABD,HABE), CD(HDA,HDB,HDC), CB(HBA,HBB,HBC),
 CA(HABC,HABD,HABE), CD(HDA,HDB,HDC)
5.d Aromatic/amide H refined with riding coordinates:
 N(H), C9(H9), C8(H8), C6(H6), C5(H5), N(HA), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), N(H), C9(H9), C8(H8), C6(H6), C5(H5),
 N(HA), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C29(H29), C28(H28), C27(H27), C26(H26), C25(H25)
5.e X=CH2 refined with riding coordinates:
 N(HBC,HBD), N(HBC,HBD)
;
_shelx_res_checksum              26902
_shelx_hkl_checksum              67316
_shelx_fab_checksum              94391
_olex2_submission_special_instructions 'No special instructions were received'