AEE-active cyclic tetraphenylsilole derivatives with σim 100% solid-state fluorescence quantum efficiency.
Cai, Yuanjing; Samedov, Kerim; Dolinar, Brian S.; Albright, Haley; Song, Zhegang; Zhang, Chaocan; Tang, Ben Zhong; West, Robert; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12970–12975; doi:10.1039/c5dt01846c

data_7035453
_publ_section_title
;
 AEE-active cyclic tetraphenylsilole derivatives with \sim 100%
 solid-state fluorescence quantum efficiency.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12970
_journal_page_last               12975
_journal_paper_doi               10.1039/c5dt01846c
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C70 H56 O4 Si4'
_chemical_formula_sum            'C70 H56 O4 Si4'
_chemical_formula_weight         1073.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_update_record
;
2014-06-25 deposited with the CCDC.
2015-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.033(8)
_cell_length_b                   19.851(11)
_cell_length_c                   22.521(11)
_cell_measurement_reflns_used    5471
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      20.63
_cell_measurement_theta_min      2.39
_cell_volume                     5827(6)
_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 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1018
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58165
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.768
_diffrn_reflns_theta_min         1.367
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8402
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0915 before and 0.0765 after correction.
The Ratio of minimum to maximum transmission is 0.8402.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 3088 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.20(8)
_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     846
_refine_ls_number_reflns         11070
_refine_ls_number_restraints     508
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+3.6021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1345
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                8415
_reflns_number_total             11070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01846c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7035452--7035454.cif.'
_cod_database_code               7035453
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C17 \\sim C3-C17A
 with sigma of 0.01
 Si4-C69A \\sim Si4-C64
 with sigma of 0.01
 C58A-C39 \\sim C58-C39
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C17A \\sim C18A
\\sim C19A \\sim C20A \\sim C21A \\sim C22A: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C58A \\sim C59A
\\sim C60A \\sim C61A \\sim C62A \\sim C63A: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C64A \\sim C65A
\\sim C66A \\sim C67A \\sim C68A \\sim C69A: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Same fragment restrains
{C17A, C18A, C19A, C20A, C21A, C22A}
as
{C17, C18, C19, C20, C21, C22}
{C58A, C59A, C60A, C61A, C62A, C63A}
as
{C58, C59, C60, C61, C62, C63}
{C64, C65, C66, C67, C68, C69}
as
{C64, C65, C66, C67, C68, C69}
5. Others
 Sof(C17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=
 Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=1-FVAR(1)
 Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=
 Sof(H21)=Sof(C22)=Sof(H22)=FVAR(1)
 Sof(C58A)=Sof(C59A)=Sof(H59A)=Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(H61A)=
 Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(H63A)=1-FVAR(2)
 Sof(C58)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=Sof(C61)=Sof(H61)=Sof(C62)=
 Sof(H62)=Sof(C63)=Sof(H63)=FVAR(2)
 Sof(C64A)=Sof(H64A)=Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(H66A)=Sof(C67A)=
 Sof(H67A)=Sof(C68A)=Sof(H68A)=Sof(C69A)=1-FVAR(3)
 Sof(C64)=Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=Sof(C67)=Sof(H67)=Sof(C68)=
 Sof(H68)=Sof(C69)=Sof(H69)=FVAR(3)
6.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),
 C18A(H18A), C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48),
  C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55), C56(H56),
 C57(H57), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C59A(H59A),
 C60A(H60A), C61A(H61A), C62A(H62A), C63A(H63A), C65(H65), C66(H66), C67(H67),
 C68(H68), C69(H69), C64A(H64A), C65A(H65A), C66A(H66A), C67A(H67A), C68A(H68A)
6.b Fitted hexagon refined as free rotating group:
 C64(C65,C66,C67,C68,C69), C64A(C65A,C66A,C67A,C68A,C69A)
6.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C70(H70A,H70B,H70C)
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_shelx_res_checksum              76929