Thermal 8π electrocyclic reaction of heteroarene tetramers: new efficient access to π-extended cyclooctatetraenes
Mouri, Kazuhiro; Saito, Shohei; Hisaki, Ichiro; Yamaguchi, Shigehiro; Chemical Science 4 (2013) 4465–; doi:10.1039/c3sc52232f

data_1514636
_publ_section_title
;
 Thermal 8\p electrocyclic reaction of heteroarene tetramers: new
 efficient access to \p-extended cyclooctatetraenes
;
_journal_issue                   12
_journal_name_full               'Chemical Science'
_journal_page_first              4465
_journal_paper_doi               10.1039/c3sc52232f
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C36 H20 N4 S4'
_chemical_formula_sum            'C36 H20 N4 S4'
_chemical_formula_weight         636.80
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.44
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.21460(10)
_cell_length_b                   8.72490(10)
_cell_length_c                   26.3340(2)
_cell_measurement_temperature    123(2)
_cell_volume                     3003.32(5)
_computing_cell_refinement       HKL2000
_computing_data_collection       HKL2000
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD Q315'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Si (111) double crystal monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80000
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18205
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.9827
_exptl_absorpt_correction_T_min  0.9332
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.170
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         4257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+30.1207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2169
_refine_ls_wR_factor_ref         0.2177
_reflns_number_gt                4087
_reflns_number_total             4257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52232f.txt
_cod_data_source_block           shelxl
_cod_original_cell_volume        3003.30(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1514636