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_1548152
_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         'C26 H20 F9 N12 Na3 O4'
_chemical_formula_sum            'C26 H20 F9 N12 Na3 O4'
_chemical_formula_weight         804.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                90
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_cell_angle_gamma                90
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_cell_length_a                   37.2006(3)
_cell_length_b                   12.80126(12)
_cell_length_c                   7.46127(7)
_cell_measurement_reflns_used    71242
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.5200
_cell_measurement_theta_min      3.5570
_cell_volume                     3553.17(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3347
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -93.00 -15.00   0.50   38.00    --  -19.49 150.00-149.00  156
  2  \w    -45.00 -15.00   0.50   38.00    --  -19.49 154.00  30.00   60
  3  \w    -97.00 -47.00   0.50   38.00    --  -19.49 154.00  30.00  100
  4  \w    -96.00   7.00   0.50   38.00    --  -19.49 -77.00-120.00  206
  5  \w    -98.00   6.00   0.50   38.00    --  -19.49 -77.00 120.00  208
  6  \w    -45.00  54.00   0.50   38.00    --  -19.49  38.00  30.00  198
  7  \w    -50.00  54.00   0.50   38.00    --  -19.49  77.00-150.00  208
  8  \w    -98.00   6.00   0.50   38.00    --  -19.49 -77.00   0.00  208
  9  \w    -49.00  45.00   0.50   38.00    --   19.96 -38.00  90.00  188
 10  \w    -98.00  14.00   0.50   38.00    --  -19.49 -77.00 -60.00  224
 11  \w    -46.00  56.00   0.50   38.00    --  -19.49  38.00 150.00  204
 12  \w    -95.00   7.00   0.50   38.00    --  -19.49 -38.00  60.00  204
 13  \w    -66.00  17.00   0.50   38.00    --  -19.49 108.00  -1.00  166
 14  \w     -6.00  96.00   0.50   38.00    --   19.96  38.00-120.00  204
 15  \w     56.00 110.00   0.50   38.00    --   19.96 179.00 -30.00  108
 16  \w     -6.00  96.00   0.50   38.00    --   19.96  38.00  60.00  204
 17  \w    -97.00 -15.00   0.50   38.00    --  -19.49 154.00 -82.00  164
 18  \w    -82.00  -2.00   0.50   38.00    --  -19.49 133.00 159.00  160
 19  \w    -82.00  -3.00   0.50   38.00    --  -19.49 134.00  45.00  158
 20  \w    -98.00  14.00   0.50   38.00    --  -19.49 -77.00-150.00  224
 21  \w    -98.00  14.00   0.50   38.00    --  -19.49 -77.00  60.00  224
 22  \w      4.00  67.00   0.50   38.00    --   19.96-108.00  81.00  126
 23  \w     56.00 110.00   0.50   38.00    --   19.96 179.00  30.00  108
 24  \w    -82.00  -2.00   0.50   38.00    --  -19.49 133.00 137.00  160
 25  \w    -56.00   1.00   0.50   38.00    --   19.96 -38.00 -30.00  114
;
_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      -0.0119483000
_diffrn_orient_matrix_UB_12      0.0366657000
_diffrn_orient_matrix_UB_13      0.0391549000
_diffrn_orient_matrix_UB_21      0.0141996000
_diffrn_orient_matrix_UB_22      0.0367836000
_diffrn_orient_matrix_UB_23      0.0063766000
_diffrn_orient_matrix_UB_31      -0.0043685000
_diffrn_orient_matrix_UB_32      0.0193274000
_diffrn_orient_matrix_UB_33      -0.0863846000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            169271
_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         26.657
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.944
_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    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.214
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         7491
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0430P)^2^+2.5220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7407
_reflns_number_total             7491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b09705_si_002.cif
_cod_data_source_block           7_natdi_g1
_cod_depositor_comments
'Adding full bibliography for 1548146--1548153.cif.'
_cod_original_cell_volume        3553.16(5)
_cod_database_code               1548152
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              92013