Halide-free highly-pure imidazolium triflate ionic liquids: Preparation and use in palladium-catalysed allylic alkylation
Leclercq, Loïc; Suisse, Isabelle; Nowogrocki, Guy; Agbossou-Niedercorn, Francine; Green Chemistry 9 (2007) 1097–; doi:10.1039/b703096g

data_7202845
_publ_section_title
;
 Halide-free highly-pure imidazolium triflate ionic liquids:
 Preparation and use in palladium-catalysed allylic alkylation
;
_journal_issue                   10
_journal_name_full               'Green Chemistry'
_journal_page_first              1097
_journal_paper_doi               10.1039/b703096g
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C27 H51 F6 N3 O7 S2'
_chemical_formula_weight         707.83
_chemical_melting_point          95
_chemical_name_common
;
1-methyl-3-(tetrahydrofuran-3-ylmethyl)-1H-imidazol-3-ium
trifluoromethanesulfonate / tetrabuthylammonium
trifluoromethanesulfonate
;
_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                85.627(2)
_cell_angle_beta                 88.693(2)
_cell_angle_gamma                88.563(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5883(13)
_cell_length_b                   9.7729(13)
_cell_length_c                   19.198(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1792.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.820
_diffrn_measured_fraction_theta_max 0.820
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14089
_diffrn_reflns_theta_full        28.93
_diffrn_reflns_theta_max         28.93
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    0.223
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             752
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .25
_refine_diff_density_max         1.781
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+0.3212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1722
_reflns_number_gt                5727
_reflns_number_total             7772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b703096g.txt
_cod_data_source_block           ionicjjm
_cod_original_cell_volume        1792.7(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7202845