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_4506150
_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             2007-12-22T14:32:02-00:00
_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                   8.8376(2)
_cell_length_b                   12.9393(3)
_cell_length_c                   14.6165(3)
_cell_measurement_reflns_used    9299
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1577
_cell_measurement_theta_min      2.683
_cell_volume                     1671.43(6)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.96
_diffrn_measurement_device_type
;
 Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       '\p and \w scans'
_diffrn_orient_matrix_UB_11      -0.0139823614
_diffrn_orient_matrix_UB_12      0.0519877999
_diffrn_orient_matrix_UB_13      -0.0126781554
_diffrn_orient_matrix_UB_21      0.0352295181
_diffrn_orient_matrix_UB_22      -0.0089070318
_diffrn_orient_matrix_UB_23      -0.0428305743
_diffrn_orient_matrix_UB_31      -0.0706428905
_diffrn_orient_matrix_UB_32      -0.0147906727
_diffrn_orient_matrix_UB_33      -0.0188052535
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25957
_diffrn_reflns_theta_full        31.5
_diffrn_reflns_theta_max         32.31
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.91762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         5599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0598
_reflns_number_gt                4115
_reflns_number_total             5599
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cg201592u_si_003.cif
_cod_data_source_block           dab2tf
_cod_database_code               4506150