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_4089693
_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         'C96 H68 O6 Si4, 0.41(H2 O)'
_chemical_formula_sum            'C96 H68.83 O6.41 Si4'
_chemical_formula_weight         1437.26
_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   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                109.8140(9)
_cell_angle_beta                 107.0677(9)
_cell_angle_gamma                90.9332(10)
_cell_formula_units_Z            1
_cell_length_a                   10.7401(2)
_cell_length_b                   12.3839(2)
_cell_length_c                   15.3414(2)
_cell_measurement_temperature    100(2)
_cell_volume                     1819.86(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31204
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.152
_diffrn_reflns_theta_min         3.229
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_preparation       '0.094 x 0.0095 x 0.0062'
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.0095
_exptl_crystal_size_min          0.0062
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         6867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0892P)^2^+0.1923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5423
_reflns_number_total             6867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500884b_si_002.cif
_cod_data_source_block           S1
_cod_database_code               4089693
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H4A of O4
 At 1.201 times of:
  H4B of O4
2. Others
 Sof(O4)=Sof(H4A)=Sof(H4B)=FVAR(1)
3.a Free rotating group:
 O4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C8(H8), C33(H33), C24(H24), C20(H20), C2(H2), C5(H5), C10(H10),
 C23(H23), C14(H14), C28(H28), C35(H35), C15(H15), C47(H47), C21(H21), C30(H30),
  C22(H22), C27(H27), C39(H39), C42(H42), C41(H41), C3(H3A), C4(H4), C40(H40),
 C16(H16), C18(H18), C29(H29), C17(H17), C45(H45), C48(H48), C46(H46), C38(H38),
  C44(H44)
;
_shelx_res_checksum              11961
_shelx_hkl_checksum              22586
_olex2_submission_special_instructions 'No special instructions were received'