Synthesis and Electronic Factors in Thermal Cyclodimerization of Functionalized Aromatic Trifluorovinyl Ethers
Bryan K. Spraul; S. Suresh; Jianyong Jin; Dennis W. Smith; Journal of the American Chemical Society 128 (2006) 7055–7064; doi:10.1021/ja0600227

data_4110602
_publ_section_title
;
 Synthesis and Electronic Factors in Thermal Cyclodimerization of
 Functionalized Aromatic Trifluorovinyl Ethers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7055
_journal_page_last               7064
_journal_paper_doi               10.1021/ja0600227
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C20 H14 F6 O6'
_chemical_formula_weight         464.31
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8010(14)
_cell_length_b                   25.729(5)
_cell_length_c                   11.498(2)
_cell_measurement_temperature    153(2)
_cell_volume                     2012.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24701
_diffrn_reflns_theta_full        26.19
_diffrn_reflns_theta_max         26.19
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.9854
_exptl_absorpt_correction_T_min  0.9011
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0855
_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^)+(0.0945P)^2^+2.6083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2189
_reflns_number_gt                1915
_reflns_number_total             2055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0600227si20060109_045642.cif
_cod_data_source_block           diester
_cod_database_code               4110602