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_1548848
_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         'C6 H6 F3 Li N4 O3'
_chemical_formula_sum            'C6 H6 F3 Li N4 O3'
_chemical_formula_weight         246.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 91.590(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9332(4)
_cell_length_b                   9.3110(5)
_cell_length_c                   15.6864(8)
_cell_measurement_reflns_used    2952
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      66.9310
_cell_measurement_theta_min      5.5180
_cell_volume                     1012.25(10)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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 -34.00   1.00    2.00    --  -41.01 125.00 120.00   60
  2  \w    -34.00  67.00   1.00    2.00    --   41.01 -44.00  60.00  101
  3  \w     22.00  50.00   1.00    4.00    --   93.50 -45.00-150.00   28
  4  \w     20.00  76.00   1.00    4.00    --   93.50 -45.00  90.00   56
  5  \w    141.00 168.00   1.00    4.00    --   93.50 125.00-180.00   27
  6  \w     75.00 135.00   1.00    4.00    --   93.50  82.00 -44.00   60
  7  \w     23.00  48.00   1.00    4.00    --   93.50 -44.00  60.00   25
  8  \w     96.00 122.00   1.00    4.00    --   93.50  45.00-120.00   26
  9  \w     84.00 119.00   1.00    4.00    --   93.50 107.00-153.00   35
 10  \w     14.00  54.00   1.00    4.00    --   93.50 -15.00  90.00   40
 11  \w     77.00 110.00   1.00    4.00    --   93.50 -15.00  90.00   33
 12  \w     32.00  65.00   1.00    4.00    --   93.50 -77.00  30.00   33
 13  \w     84.00 127.00   1.00    4.00    --   93.50 -77.00  30.00   43
 14  \w    107.00 169.00   1.00    4.00    --   93.50  82.00 165.00   62
 15  \w     79.00 109.00   1.00    4.00    --   93.50 125.00 -30.00   30
 16  \w     51.00  77.00   1.00    4.00    --   93.50 -45.00  30.00   26
 17  \w    135.00 166.00   1.00    4.00    --   93.50  45.00-120.00   31
 18  \w    107.00 151.00   1.00    4.00    --   93.50  45.00-150.00   44
 19  \w     18.00  67.00   1.00    4.00    --   93.50 -77.00  60.00   49
 20  \w     22.00  77.00   1.00    4.00    --   93.50 -45.00 150.00   55
;
_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      -0.0493379000
_diffrn_orient_matrix_UB_12      0.0651490000
_diffrn_orient_matrix_UB_13      -0.0882841000
_diffrn_orient_matrix_UB_21      -0.1866941000
_diffrn_orient_matrix_UB_22      0.0639885000
_diffrn_orient_matrix_UB_23      0.0349423000
_diffrn_orient_matrix_UB_31      0.1099299000
_diffrn_orient_matrix_UB_32      0.1379470000
_diffrn_orient_matrix_UB_33      0.0254634000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3070
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.034
_diffrn_reflns_theta_max         67.034
_diffrn_reflns_theta_min         5.526
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.441
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.761
_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    1.615
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0535
_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^)+(0.1016P)^2^+0.5079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2770
_reflns_number_total             3070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b11145_si_001.cif
_cod_data_source_block           1a
_cod_database_code               1548848
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.715
_shelx_res_checksum              3554
_twin_special_details
;
Component 2 rotated by 179.9896\% 
 around [0.00 0.00 1.00] (reciprocal) or [0.06 -0.00 1.00] (direct)
;