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_4089690
_publ_section_title
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 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         'C38 H32 O4 Si4'
_chemical_formula_sum            'C38 H32 O4 Si4'
_chemical_formula_weight         664.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.306(3)
_cell_length_b                   22.618(8)
_cell_length_c                   34.932(12)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      2.51
_cell_volume                     6563(4)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            168971
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.546
_diffrn_reflns_theta_min         1.166
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9267
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0717 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.9267.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         9176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0400P)^2^+4.9320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7792
_reflns_number_total             9176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500884b_si_002.cif
_cod_data_source_block           1b
_cod_original_cell_volume        6562(4)
_cod_database_code               4089690
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H27 of C27, H21 of C21, H24 of C24, H22 of C22, H17 of C17, H16 of C16, H18
  of C18, H23 of C23, H37 of C37, H36 of C36, H35 of C35, H34 of C34, H28 of
  C28, H29 of C29, H30 of C30, H33 of C33, H5 of C5, H15 of C15, H2 of C2, H10
  of C10, H3 of C3, H11 of C11, H8 of C8, H9 of C9, H14 of C14, H4 of C4
 At 1.5 times of:
  {H19A,H19B,H19C} of C19, {H38A,H38B,H38C} of C38
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24),
  C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C38(H38A,H38B,H38C)
;
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.963
_shelxl_version_number           2013-3