Unexpected formation of a cyclic vinylene sulfate in the synthesis of ethynyl-substituted acenes
Brandon Djukic; Dmitrii Perepichka; Chem.Commun. 48 (2012) 6651–; doi:10.1039/c2cc32805d

data_7107921
_publ_section_title
;
 Unexpected formation of a cyclic vinylene sulfate in the synthesis of
 ethynyl-substituted acenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              6651
_journal_paper_doi               10.1039/c2cc32805d
_journal_volume                  48
_journal_year                    2012
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C44 H56 O4 S Si2'
_chemical_formula_sum            'C44 H56 O4 S Si2'
_chemical_formula_weight         737.13
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.192(2)
_cell_angle_beta                 79.705(2)
_cell_angle_gamma                76.941(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4790(4)
_cell_length_b                   15.5718(7)
_cell_length_c                   15.9893(7)
_cell_measurement_reflns_used    24380
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.60
_cell_measurement_theta_min      2.81
_cell_volume                     2022.67(16)
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Quazar MX'
_diffrn_radiation_source         'Incoatec I\muS Microsource '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_av_sigmaI/netI    0.0131
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            85141
_diffrn_reflns_theta_full        70.99
_diffrn_reflns_theta_max         70.99
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    1.594
_exptl_absorpt_correction_T_max  0.9382
_exptl_absorpt_correction_T_min  0.8256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         7572
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.6090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                7067
_reflns_number_total             7572
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cc32805d.txt
_cod_data_source_block           pere21
_cod_original_cell_volume        2022.66(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107921