Snapshots of the Hydrolysis of Lithium 4,5-Dicyanoimidazolate–Glyme Solvates. Impact of Water Molecules on Aggregation Processes in Lithium-Ion Battery Electrolytes
Dranka, Maciej; Jankowski, Piotr; Żukowska, Grażyna Z.; The Journal of Physical Chemistry C  (2018) –; doi:10.1021/acs.jpcc.7b11145

data_1548850
_publ_section_title
;
 Snapshots of the Hydrolysis of Lithium 4,5-Dicyanoimidazolate--Glyme
 Solvates. Impact of Water Molecules on Aggregation Processes in
 Lithium-Ion Battery Electrolytes
;
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_paper_doi               10.1021/acs.jpcc.7b11145
_journal_year                    2018
_chemical_formula_moiety         'C12 H8 F6 Li2 N8 O4, 2(H2 O)'
_chemical_formula_sum            'C12 H12 F6 Li2 N8 O6'
_chemical_formula_weight         492.18
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                112.610(6)
_cell_angle_beta                 109.205(6)
_cell_angle_gamma                93.780(5)
_cell_formula_units_Z            1
_cell_length_a                   7.3838(5)
_cell_length_b                   8.5505(5)
_cell_length_c                   9.9562(6)
_cell_measurement_reflns_used    3162
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      67.0440
_cell_measurement_theta_min      5.2200
_cell_volume                     534.47(7)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_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     13.00 109.00   1.00    1.50    --   41.01  77.00-120.00   96
  2  \w     36.00 116.00   1.00    1.50    --   41.01  37.00   0.00   80
  3  \w     -1.00  87.00   1.00    1.50    --   41.01-125.00 150.00   88
  4  \w   -121.00 -60.00   1.00    1.50    --  -90.00 125.00   0.00   61
  5  \w   -117.00 -92.00   1.00    1.50    --  -90.00 125.00 -60.00   25
  6  \w     16.00  70.00   1.00    1.50    --   93.50 -86.00-148.00   54
  7  \w     89.00 128.00   1.00    1.50    --   93.50 -88.00  85.00   39
  8  \w     22.00  48.00   1.00    1.50    --   93.50 -86.00 -29.00   26
  9  \w     55.00  94.00   1.00    1.50    --   93.50  22.00  18.00   39
 10  \w     57.00 116.00   1.00    1.50    --   93.50  24.00 166.00   59
 11  \w     98.00 136.00   1.00    1.50    --   93.50  22.00  18.00   38
 12  \w     50.00 123.00   1.00    1.50    --   93.50 -60.00-123.00   73
 13  \w     50.00  87.00   1.00    1.50    --   93.50 -54.00 -42.00   37
 14  \w    107.00 133.00   1.00    1.50    --   93.50  15.00 120.00   26
 15  \w     26.00  51.00   1.00    1.50    --   93.50 -88.00  85.00   25
 16  \w    113.00 171.00   1.00    1.50    --   93.50  77.00-120.00   58
 17  \w     65.00  90.00   1.00    1.50    --   93.50  77.00-120.00   25
 18  \w     81.00 106.00   1.00    1.50    --   93.50 -92.00  32.00   25
 19  \w     16.00  61.00   1.00    1.50    --   93.50 -31.00-141.00   45
 20  \w     20.00  70.00   1.00    1.50    --   93.50 -45.00 120.00   50
 21  \w     78.00 103.00   1.00    1.50    --   93.50  77.00  90.00   25
 22  \w     88.00 137.00   1.00    1.50    --   93.50  45.00  60.00   49
 23  \w     87.00 113.00   1.00    1.50    --   93.50  31.00 -38.00   26
 24  \w    141.00 170.00   1.00    1.50    --   93.50  31.00 -38.00   29
 25  \w     45.00  72.00   1.00    1.50    --   93.50 -45.00-120.00   27
 26  \w     68.00 110.00   1.00    1.50    --   93.50 -77.00  30.00   42
 27  \w     91.00 167.00   1.00    1.50    --   93.50  77.00   0.00   76
 28  \w     40.00  65.00   1.00    1.50    --   93.50  15.00 120.00   25
 29  \w     95.00 121.00   1.00    1.50    --   93.50 -86.00-148.00   26
 30  \w     73.00  98.00   1.00    1.50    --   93.50 -86.00 -29.00   25
 31  \w     96.00 122.00   1.00    1.50    --   93.50 -90.00 145.00   26
 32  \w     73.00  98.00   1.00    1.50    --   93.50 -77.00 -90.00   25
 33  \w     50.00  76.00   1.00    1.50    --   93.50 -15.00 120.00   26
 34  \w     38.00  78.00   1.00    1.50    --   93.50 -90.00 145.00   40
;
_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      -0.2155928000
_diffrn_orient_matrix_UB_12      0.0157133000
_diffrn_orient_matrix_UB_13      -0.0348103000
_diffrn_orient_matrix_UB_21      -0.0315108000
_diffrn_orient_matrix_UB_22      -0.1334900000
_diffrn_orient_matrix_UB_23      0.0635028000
_diffrn_orient_matrix_UB_31      0.0619592000
_diffrn_orient_matrix_UB_32      0.1482434000
_diffrn_orient_matrix_UB_33      0.1665204000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.966
_diffrn_reflns_theta_max         66.966
_diffrn_reflns_theta_min         5.214
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.762
_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    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             248
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.187
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0132(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         1896
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0590P)^2^+0.3970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1750
_reflns_number_total             1896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b11145_si_001.cif
_cod_data_source_block           2x2H2O
_cod_original_cell_volume        534.47(6)
_cod_database_code               1548850
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.784
_shelx_estimated_absorpt_t_min   0.641
_shelx_res_checksum              16710