Coordination Abilities of 4,5-Dicyano-2-(trifluoromethyl)imidazolate Anion toward Sodium Cation: Structural and Spectroscopic Studies of Solid and Liquid Glyme-Solvated Electrolyte Systems
Dranka, Maciej; Żukowska, Grażyna Z.; Jankowski, Piotr; Plewa-Marczewska, Anna; Trzeciak, Tomasz; Zachara, Janusz; The Journal of Physical Chemistry C 121 (2017) 26713–; doi:10.1021/acs.jpcc.7b09705

data_1548150
_publ_section_title
;
 Coordination Abilities of 4,5-Dicyano-2-(trifluoromethyl)imidazolate
 Anion toward Sodium Cation: Structural and Spectroscopic Studies of Solid
 and Liquid Glyme-Solvated Electrolyte Systems
;
_journal_issue                   48
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              26713
_journal_paper_doi               10.1021/acs.jpcc.7b09705
_journal_volume                  121
_journal_year                    2017
_chemical_formula_moiety         'C28 H36 F6 N8 Na2 O8'
_chemical_formula_sum            'C28 H36 F6 N8 Na2 O8'
_chemical_formula_weight         772.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2017-06-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                82.713(2)
_cell_angle_beta                 67.371(2)
_cell_angle_gamma                74.624(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3885(2)
_cell_length_b                   10.2919(3)
_cell_length_c                   10.7572(3)
_cell_measurement_reflns_used    24971
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      32.6070
_cell_measurement_theta_min      3.5060
_cell_volume                     924.70(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3347
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -97.00 -19.00   1.00   12.00    --  -19.65 155.00 -57.00   78
  2  \w    -79.00   1.00   1.00   12.00    --  -19.65 128.00  56.00   80
  3  \w    -98.00   5.00   1.00   12.00    --  -19.65 -77.00 -60.00  103
  4  \w    -96.00   4.00   1.00   12.00    --  -19.65 -77.00-180.00  100
  5  \w    -39.00  50.00   1.00   12.00    --  -19.65  38.00-150.00   89
  6  \w    -53.00  54.00   1.00   12.00    --  -19.65  77.00 -90.00  107
  7  \w    -93.00   4.00   1.00   12.00    --  -19.65 -77.00  60.00   97
  8  \w    -48.00  23.00   1.00   12.00    --   19.96 -38.00  30.00   71
  9  \w    -53.00  59.00   1.00   12.00    --  -19.65  77.00 150.00  112
 10  \w    -96.00   7.00   1.00   12.00    --  -19.65 -38.00 150.00  103
 11  \w   -109.00 -32.00   1.00   12.00    --  -19.65 179.00-180.00   77
 12  \w     56.00 110.00   1.00   12.00    --   19.96 179.00 -30.00   54
 13  \w     56.00 110.00   1.00   12.00    --   19.96 179.00 -90.00   54
 14  \w     -6.00  96.00   1.00   12.00    --   19.96  38.00 120.00  102
 15  \w    -89.00  -9.00   1.00   12.00    --  -19.65 144.00-149.00   80
 16  \w    -46.00  56.00   1.00   12.00    --  -19.65  38.00 120.00  102
 17  \w    -98.00  14.00   1.00   12.00    --  -19.65 -77.00  60.00  112
 18  \w     22.00  81.00   1.00   12.00    --   19.96-131.00-109.00   59
 19  \w    -10.00  94.00   1.00   12.00    --   19.96  59.00 -65.00  104
 20  \w    -56.00  46.00   1.00   12.00    --   19.96 -38.00 -60.00  102
 21  \w    -79.00   1.00   1.00   12.00    --  -19.65 128.00  56.00   80
 22  \w   -109.00  70.00   1.00   12.00    --  -19.65   0.00-180.00  179
 23  \w     56.00 110.00   1.00   12.00    --   19.96 179.00-180.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0159468000
_diffrn_orient_matrix_UB_12      -0.0613787000
_diffrn_orient_matrix_UB_13      0.0359062000
_diffrn_orient_matrix_UB_21      0.0322102000
_diffrn_orient_matrix_UB_22      0.0313284000
_diffrn_orient_matrix_UB_23      0.0346350000
_diffrn_orient_matrix_UB_31      -0.0761843000
_diffrn_orient_matrix_UB_32      0.0190802000
_diffrn_orient_matrix_UB_33      0.0511694000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            47735
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.860
_diffrn_reflns_theta_min         3.524
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       irregular
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.274
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.3400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4020
_reflns_number_total             4400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b09705_si_002.cif
_cod_data_source_block           5_natd_g3
_cod_depositor_comments
'Adding full bibliography for 1548146--1548153.cif.'
_cod_original_cell_volume        924.71(4)
_cod_database_code               1548150
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              31964