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_1548847
_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         'C26 H22 F9 Li3 N12 O5'
_chemical_formula_sum            'C26 H22 F9 Li3 N12 O5'
_chemical_formula_weight         774.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.7040(2)
_cell_length_b                   13.95120(10)
_cell_length_c                   26.6779(3)
_cell_measurement_reflns_used    13106
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      66.6930
_cell_measurement_theta_min      4.0020
_cell_volume                     7333.61(12)
_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_temperature      120.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3347
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     16.00 112.00   1.00    6.00    --   41.14  38.00 150.00   96
  2  \w     -1.00  66.00   1.00    6.00    --   41.14 -57.00 -60.00   67
  3  \w     17.00  43.00   1.00   12.00    --   93.50 -94.00 120.00   26
  4  \w     20.00  46.00   1.00   12.00    --   93.50 -61.00 -60.00   26
  5  \w     27.00  70.00   1.00   12.00    --   93.50 -45.00  60.00   43
  6  \w     28.00  56.00   1.00   12.00    --   93.50 -98.00  44.00   28
  7  \w     32.00  95.00   1.00   12.00    --   93.50-125.00-180.00   63
  8  \w     66.00  92.00   1.00   12.00    --   93.50-125.00 -90.00   26
  9  \w     81.00 124.00   1.00   12.00    --   93.50 -77.00   0.00   43
 10  \w     67.00  92.00   1.00   12.00    --   93.50  45.00   0.00   25
 11  \w    122.00 166.00   1.00   12.00    --   93.50  45.00   0.00   44
 12  \w     23.00 123.00   1.00   12.00    --   93.50 -61.00 -30.00  100
 13  \w     22.00  48.00   1.00   12.00    --   93.50 -45.00 -60.00   26
 14  \w     40.00  66.00   1.00   12.00    --   93.50 -45.00   0.00   26
 15  \w     21.00  65.00   1.00   12.00    --   93.50 -30.00 -60.00   44
 16  \w     62.00 140.00   1.00   12.00    --   93.50  77.00 -90.00   78
;
_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      -0.0105062000
_diffrn_orient_matrix_UB_12      -0.0040841000
_diffrn_orient_matrix_UB_13      0.0571577000
_diffrn_orient_matrix_UB_21      0.0729608000
_diffrn_orient_matrix_UB_22      0.0366744000
_diffrn_orient_matrix_UB_23      0.0080819000
_diffrn_orient_matrix_UB_31      -0.0261785000
_diffrn_orient_matrix_UB_32      0.1040562000
_diffrn_orient_matrix_UB_33      -0.0005585000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            34276
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.860
_diffrn_reflns_theta_max         66.860
_diffrn_reflns_theta_min         3.313
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.720
_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    1.403
_exptl_crystal_description       prism
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         6523
_refine_ls_number_restraints     249
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0750P)^2^+3.0480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5607
_reflns_number_total             6523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b11145_si_001.cif
_cod_data_source_block           5
_cod_database_code               1548847
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              76103