Preparation, Properties, and Crystal Structures of Organometallic Ionic Liquids Comprising 1-Ferrocenyl-3-alkylimidazolium-Based Salts of Bis(trifluoromethanesulfonyl)amide and Hexafluorophosphate
Yuji Miura; Fumiko Shimizu; Tomoyuki Mochida; Inorganic Chemistry 49 (2010) 10032–10040; doi:10.1021/ic1013363

data_4316938
_publ_section_title
;
 Preparation, Properties, and Crystal Structures of Organometallic Ionic
 Liquids Comprising 1-Ferrocenyl-3-alkylimidazolium-Based Salts of
 Bis(trifluoromethanesulfonyl)amide and Hexafluorophosphate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10032
_journal_page_last               10040
_journal_paper_doi               10.1021/ic1013363
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C13 H14 Fe N3, I'
_chemical_formula_sum            'C13 H14 Fe I N3'
_chemical_formula_weight         395.02
_chemical_name_systematic
;
 Ferrocenylmethyltriazole iodide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 98.553(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.163(4)
_cell_length_b                   13.981(5)
_cell_length_c                   9.696(3)
_cell_measurement_reflns_used    2485
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.50
_cell_volume                     1362.4(8)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15227
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    3.358
_exptl_absorpt_correction_T_max  0.8239
_exptl_absorpt_correction_T_min  0.1887
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.257
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         5587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                4674
_reflns_number_total             5587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1013363_si_002_2.cif
_cod_data_source_block           9-I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4316938