Synthesis and High Solid-State Fluorescence of Cyclic Silole Derivatives
Cai, Yuanjing; Samedov, Kerim; Dolinar, Brian S.; Song, Zhegang; Tang, Ben Zhong; Zhang, Chaocan; West, Robert; Organometallics 34 (2014) 78–; doi:10.1021/om500884b

data_4089692
_publ_section_title
;
 Synthesis and High Solid-State Fluorescence of Cyclic Silole Derivatives
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              78
_journal_paper_doi               10.1021/om500884b
_journal_volume                  34
_journal_year                    2014
_chemical_formula_moiety         'C62 H48 O3.91 Si3.91, 2(C7 H8), 0.09(O Si)'
_chemical_formula_sum            'C76 H64 O4 Si4'
_chemical_formula_weight         1153.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                102.992(19)
_cell_angle_beta                 101.607(18)
_cell_angle_gamma                103.183(13)
_cell_formula_units_Z            1
_cell_length_a                   10.722(4)
_cell_length_b                   11.006(4)
_cell_length_c                   13.920(6)
_cell_measurement_reflns_used    4472
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.39
_cell_volume                     1502.2(10)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31268
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.462
_diffrn_reflns_theta_min         1.558
_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  0.7457
_exptl_absorpt_correction_T_min  0.6573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0736 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.8815.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7546
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+0.6367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5234
_reflns_number_total             7546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500884b_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        1502.1(10)
_cod_database_code               4089692
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.970
_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
 Si2A-O2A \\sim Si2-O2
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(Si2A) = Uiso(O2A)
4. Others
 Sof(Si2A)=Sof(O2A)=1-FVAR(1)
 Sof(Si2)=Sof(O2)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C3S(H3S), C4S(H4S),
 C5S(H5S), C6S(H6S), C7S(H7S)
5.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              91385
_shelx_hkl_checksum              47013
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'