Crown-ether enclosure generated by ionic liquid components—synthesis, crystal structure and Raman spectra of compounds of imidazolium based salts and 18-crown-6
Gjikaj, Mimoza; Brockner, Wolfgang; Namyslo, Jan; Adam, Arnold; CrystEngComm 10 (2008) 103–; doi:10.1039/b708724c

data_7201526
_publ_section_title
;
 Crown-ether enclosure generated by ionic liquid
 components---synthesis, crystal structure and Raman spectra of
 compounds of imidazolium based salts and 18-crown-6
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              103
_journal_paper_doi               10.1039/b708724c
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C12 H24 O6, (C6 H11 N2)2 (SO3 CH3)2'
_chemical_formula_sum            'C26 H52 N4 O12 S2'
_chemical_formula_weight         676.84
_chemical_name_common
'1-ethyl-3-methylimidazolium methanesulfanate (18-crown-6)'
_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                97.26(4)
_cell_angle_beta                 97.99(4)
_cell_angle_gamma                97.76(4)
_cell_formula_units_Z            1
_cell_length_a                   8.751(5)
_cell_length_b                   9.126(4)
_cell_length_c                   11.357(6)
_cell_measurement_reflns_used    11401
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.28
_cell_volume                     880.2(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'IPDS II (Stoe & Cie)'
_diffrn_measurement_method       '\w and \f scans'
_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  0.1755
_diffrn_reflns_av_sigmaI/netI    0.1189
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11401
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       cubic
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         3085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.4026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1638
_reflns_number_gt                1860
_reflns_number_total             3085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708724c.txt
_cod_data_source_block           3
_cod_original_cell_volume        880.1(7)
_cod_database_code               7201526