High solid-state fluorescence in ring-shaped AEE-active tetraphenylsilole derivatives
Yuanjing Cai; Kerim Samedov; Haley Albright; Brian S. Dolinar; Ilia A. Guzei; Rongrong Hu; Chaocan Zhang; Ben Zhong Tang; Robert West; Chem.Commun. 50 (2014) 12714–; doi:10.1039/C4cc06203E

data_7115796
_publ_section_title
;
 High solid-state fluorescence in ring-shaped AEE-active tetraphenylsilole
 derivatives
;
_journal_name_full               Chem.Commun.
_journal_page_first              12714
_journal_paper_doi               10.1039/C4cc06203E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C52 H40 O3 Si3'
_chemical_formula_sum            'C52 H40 O3 Si3'
_chemical_formula_weight         797.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                104.62(5)
_cell_angle_beta                 103.75(4)
_cell_angle_gamma                103.50(4)
_cell_formula_units_Z            2
_cell_length_a                   10.688(4)
_cell_length_b                   14.471(8)
_cell_length_c                   17.002(6)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.90
_cell_measurement_theta_min      2.83
_cell_volume                     2348(2)
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT+ Ver. 7.68A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\ \w and 0.6\ \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40264
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         72.419
_diffrn_reflns_theta_min         2.830
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  0.9715
_exptl_absorpt_correction_T_min  0.8637
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0526 before and 0.0435 after correction.
The Ratio of minimum to maximum transmission is 0.8890.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         8905
_refine_ls_number_restraints     673
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0519P)^2^+0.8708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7335
_reflns_number_total             8905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc06203e2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2348.0(19)
_cod_database_code               7115796
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.772
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C4-C23 \\sim C4-C23A \\sim C4-C23B \\sim C4-C23C
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C23A \\sim C24A
\\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim C23B \\sim C24B \\sim C25B
\\sim C26B \\sim C27B \\sim C28B \\sim C23C \\sim C24C \\sim C25C \\sim C26C
\\sim C27C \\sim C28C: within 1.7A with sigma of 0.005 and sigma for terminal
atoms of 0.01
4. Others
 1*[Sof(C23)+Sof(C24)+Sof(H24)+Sof(C25)+Sof(H25)+Sof(C26)+Sof(H26)+Sof(C27)+
 Sof(H27)+Sof(C28)+Sof(H28)]+1*[Sof(C23A)+Sof(C24A)+Sof(H24A)+Sof(C25A)+
 Sof(H25A)+Sof(C26A)+Sof(H26A)+Sof(C27A)+Sof(H27A)+Sof(C28A)+Sof(H28A)]+1*
 [Sof(C23B)+Sof(C24B)+Sof(H24B)+Sof(C25B)+Sof(H25B)+Sof(C26B)+Sof(H26B)+
 Sof(C27B)+Sof(H27B)+Sof(C28B)+Sof(H28B)]+1*[Sof(C23C)+Sof(C24C)+Sof(H24C)+
 Sof(C25C)+Sof(H25C)+Sof(C26C)+Sof(H26C)+Sof(C27C)+Sof(H27C)+Sof(C28C)+
 Sof(H28C)]=1 with esd of 0
 Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=
 Sof(H27)=Sof(C28)=Sof(H28)=FVAR(1)
 Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=
 Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=FVAR(2)
 Sof(C23B)=Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(H26B)=
 Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28B)=FVAR(3)
 Sof(C23C)=Sof(C24C)=Sof(H24C)=Sof(C25C)=Sof(H25C)=Sof(C26C)=Sof(H26C)=
 Sof(C27C)=Sof(H27C)=Sof(C28C)=Sof(H28C)=FVAR(4)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C24A(H24A), C25A(H25A), C26A(H26A),
 C27A(H27A), C28A(H28A), C24B(H24B), C25B(H25B), C26B(H26B), C27B(H27B),
 C28B(H28B), C24C(H24C), C25C(H25C), C26C(H26C), C27C(H27C), C28C(H28C),
 C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38),
  C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C48(H48), C49(H49), C50(H50), C51(H51), C52(H52)
5.b Fitted hexagon refined as free rotating group:
 C23(C24,C25,C26,C27,C28), C23A(C24A,C25A,C26A,C27A,C28A), C23B(C24B,C25B,C26B,
 C27B,C28B), C23C(C24C,C25C,C26C,C27C,C28C)
;
_shelx_res_checksum              95347
_shelx_fab_checksum              23441