Donor-acceptor cyclopropanes with Lawesson's and Woollins' reagents: formation of bisthiophenes and unprecedented cage-like molecules
Johannes Kaschel; Christian D. Schmidt; Mark Mumby; Daniel Kratzert; Dietmar Stalke; Daniel B. Werz; Chem.Commun. 49 (2013) 4403–; doi:10.1039/c2cc37631h

data_7109239
_publ_section_title
;
 Donor-acceptor cyclopropanes with Lawesson's and Woollins' reagents:
 formation of bisthiophenes and unprecedented cage-like molecules
;
_journal_name_full               Chem.Commun.
_journal_page_first              4403
_journal_paper_doi               10.1039/c2cc37631h
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C10 H10 S2'
_chemical_formula_sum            'C10 H10 S2'
_chemical_formula_weight         194.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.301(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.955(2)
_cell_length_b                   7.649(3)
_cell_length_c                   20.480(7)
_cell_measurement_reflns_used    6971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.9195
_cell_measurement_theta_min      2.8430
_cell_volume                     928.9(6)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2010.7'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II ultra with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'Bruker TXS-Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18476
_diffrn_reflns_theta_full        26.95
_diffrn_reflns_theta_max         26.95
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+1.0157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                1750
_reflns_number_total             2006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37631h.txt
_cod_data_source_block           p21nb
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7109239