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_1548147
_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_absolute_configuration ad
_chemical_formula_moiety         'C16 H20 F3 N4 Na O5'
_chemical_formula_sum            'C16 H20 F3 N4 Na O5'
_chemical_formula_weight         428.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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
_audit_creation_date             2017-05-31
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.52266(9)
_cell_length_b                   9.79219(10)
_cell_length_c                   21.7134(2)
_cell_measurement_reflns_used    58601
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      31.1570
_cell_measurement_theta_min      3.4770
_cell_volume                     2024.72(3)
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3347
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -76.00  -2.00   1.00   14.00    --  -16.38 128.00-176.00   74
  2  \w    -72.00   0.00   1.00   14.00    --  -16.38 122.00 107.00   72
  3  \w    -90.00  12.00   1.00   14.00    --  -16.38 -77.00-150.00  102
  4  \w    -83.00   5.00   1.00   14.00    --  -16.38 -38.00 -90.00   88
  5  \w    -89.00   5.00   1.00   14.00    --  -16.38 -38.00  90.00   94
  6  \w    -47.00  50.00   1.00   14.00    --  -16.38  62.00  73.00   97
  7  \w    -87.00   9.00   1.00   14.00    --  -16.38 -38.00   0.00   96
  8  \w    -76.00  -2.00   1.00   14.00    --  -16.38 128.00 -88.00   74
  9  \w    -47.00  58.00   1.00   14.00    --  -16.38  62.00  73.00  105
 10  \w    -90.00  13.00   1.00   14.00    --  -16.38 -57.00 -60.00  103
 11  \w    -95.00  17.00   1.00   14.00    --  -16.38 -77.00  60.00  112
 12  \w    -58.00  47.00   1.00   14.00    --   16.70 -62.00 115.00  105
 13  \w    -57.00  46.00   1.00   14.00    --   16.70 -57.00 -30.00  103
 14  \w     56.00 106.00   1.00   14.00    --   16.70 179.00 120.00   50
 15  \w    -87.00 -10.00   1.00   14.00    --  -16.38 146.00  52.00   77
 16  \w    -87.00 -10.00   1.00   14.00    --  -16.38 146.00 -22.00   77
 17  \w     -4.00  59.00   1.00   14.00    --   16.70 -99.00   0.00   63
 18  \w     56.00 106.00   1.00   14.00    --   16.70 179.00 -60.00   50
 19  \w    -10.00  93.00   1.00   14.00    --   16.70  38.00-150.00  103
 20  \w    -30.00  98.00   1.00   14.00    --   16.70  19.00 120.00  128
 21  \w    -76.00   1.00   1.00   14.00    --  -16.38 128.00 156.00   77
 22  \w    -78.00  -1.00   1.00   14.00    --  -16.38 132.00  31.00   77
 23  \w    -76.00   1.00   1.00   14.00    --  -16.38 128.00 -88.00   77
 24  \w    -73.00  65.00   1.00   14.00    --   16.70   0.00-180.00  138
;
_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      0.0488885000
_diffrn_orient_matrix_UB_12      0.0149378000
_diffrn_orient_matrix_UB_13      0.0237054000
_diffrn_orient_matrix_UB_21      -0.0179934000
_diffrn_orient_matrix_UB_22      0.0701780000
_diffrn_orient_matrix_UB_23      -0.0018676000
_diffrn_orient_matrix_UB_31      -0.0532525000
_diffrn_orient_matrix_UB_32      -0.0099691000
_diffrn_orient_matrix_UB_33      0.0223884000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0092
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            106149
_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         27.364
_diffrn_reflns_theta_min         3.500
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.964
_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    1.405
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.2901
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 1913 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.08(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.3740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0584
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4483
_reflns_number_total             4574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b09705_si_002.cif
_cod_data_source_block           2_natdi_c15c5
_cod_depositor_comments
'Adding full bibliography for 1548146--1548153.cif.'
_cod_database_code               1548147
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              86350