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_1548851
_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 H14 F3 Li N4 O3, C6 H2 F3 Li N4 O'
_chemical_formula_sum            'C18 H16 F6 Li2 N8 O4'
_chemical_formula_weight         536.27
_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'
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_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                102.766(4)
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_cell_length_c                   15.4277(8)
_cell_measurement_reflns_used    13651
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      31.4140
_cell_measurement_theta_min      4.0220
_cell_volume                     1252.86(11)
_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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0(1)
_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 0.998
_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    -94.00 -15.00   1.00   25.00    --  -17.09 154.00 -26.78   79
  2  \w    -90.00 -12.00   1.00   25.00    --  -17.09 149.00  85.81   78
  3  \w    -71.00   8.00   1.00   25.00    --  -17.09 119.00-110.01   79
  4  \w    -96.00  17.00   1.00   25.00    --  -17.09 -77.00 120.00  113
  5  \w    -93.00   9.00   1.00   25.00    --  -17.09 -38.00 -30.00  102
  6  \w    -47.00  57.00   1.00   25.00    --  -17.09  57.00   0.00  104
  7  \w    -91.00  12.00   1.00   25.00    --  -17.09 -57.00 -60.00  103
  8  \w    -93.00   9.00   1.00   25.00    --  -17.09 -38.00-150.00  102
  9  \w    -58.00  44.00   1.00   25.00    --   17.87 -38.00-120.00  102
 10  \w   -107.00 -34.00   1.00   25.00    --  -17.09-179.00  30.00   73
 11  \w    -96.00  17.00   1.00   25.00    --  -17.09 -77.00-150.00  113
 12  \w    -89.00 -11.00   1.00   25.00    --  -17.09 148.00 133.24   78
 13  \w    -17.00  43.00   1.00   25.00    --   17.87  84.00 160.00   60
;
_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      -0.0527159000
_diffrn_orient_matrix_UB_12      -0.0649155000
_diffrn_orient_matrix_UB_13      -0.0078480000
_diffrn_orient_matrix_UB_21      -0.0245582000
_diffrn_orient_matrix_UB_22      0.0231441000
_diffrn_orient_matrix_UB_23      0.0416418000
_diffrn_orient_matrix_UB_31      -0.0633221000
_diffrn_orient_matrix_UB_32      0.0255018000
_diffrn_orient_matrix_UB_33      -0.0228348000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33633
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.384
_diffrn_reflns_theta_min         3.242
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         5128
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0320P)^2^+0.4880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4469
_reflns_number_total             5128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b11145_si_001.cif
_cod_data_source_block           6a6b
_cod_original_cell_volume        1252.86(10)
_cod_database_code               1548851
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              49335