Structural Studies on the Basic Ionic Liquid 1-Ethyl-1,4-diazabicyclo[2.2.2]octanium Bis(trifluoromethylsulfonyl)imide and Its Bromide Precursor
Lauw, Yansen; Rüther, Thomas; Horne, Michael D.; Wallwork, Kia S.; Skelton, Brian W.; Madsen, Ian C.; Rodopoulos, Theo; Crystal Growth & Design 12 (2012) 2803–; doi:10.1021/cg201592u

data_4506152
_publ_section_title
;
 Structural Studies on the Basic Ionic Liquid
 1-Ethyl-1,4-diazabicyclo[2.2.2]octanium Bis(trifluoromethylsulfonyl)imide
 and Its Bromide Precursor
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2803
_journal_paper_doi               10.1021/cg201592u
_journal_volume                  12
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 H17 N2, C2 F6 N O4 S2'
_chemical_formula_sum            'C10 H17 F6 N3 O4 S2'
_chemical_formula_weight         421.39
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-05-26T10:15:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9626(2)
_cell_length_b                   13.0484(3)
_cell_length_c                   14.9163(3)
_cell_measurement_reflns_used    14490
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      33.9929
_cell_measurement_theta_min      2.6452
_cell_volume                     1744.43(7)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0242166376
_diffrn_orient_matrix_UB_12      0.0511313106
_diffrn_orient_matrix_UB_13      -0.0073912453
_diffrn_orient_matrix_UB_21      -0.0086852048
_diffrn_orient_matrix_UB_22      -0.0107306188
_diffrn_orient_matrix_UB_23      -0.0463401627
_diffrn_orient_matrix_UB_31      -0.0749263886
_diffrn_orient_matrix_UB_32      -0.0152935767
_diffrn_orient_matrix_UB_33      0.0078052046
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46958
_diffrn_reflns_theta_full        33.5
_diffrn_reflns_theta_max         34.06
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
        (compiled Feb 27 2009,15:38:38)
   Gaussian numeric absorption correction using a multifaceted crystal
                      model based on expressions derived by R.C. Clark & J.S.
      (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.2
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         6898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0698P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                4364
_reflns_number_total             6898
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg201592u_si_005.cif
_cod_data_source_block           dab295
_cod_original_sg_symbol_Hall     P_2ac_2ab
_cod_database_code               4506152