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_1548852
_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, C4 H10 O2'
_chemical_formula_sum            'C16 H18 F6 Li2 N8 O6'
_chemical_formula_weight         546.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 91.5(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.653(14)
_cell_length_b                   18.007(5)
_cell_length_c                   16.68(4)
_cell_measurement_reflns_used    200
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      25.7390
_cell_measurement_theta_min      4.1650
_cell_volume                     2598(8)
_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      120.0(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    -77.00 -32.00   0.50   20.00    --  -14.25 133.00  -6.25   90
  2  \w    -77.00 -16.00   0.50   20.00    --  -14.25 133.00 170.07  122
  3  \w    -10.00  89.00   0.50   20.00    --   14.87  57.00-180.00  198
  4  \w     -2.00  91.00   0.50   20.00    --   14.87  38.00  90.00  186
  5  \w    -61.00  41.00   0.50   20.00    --   14.87 -38.00  30.00  204
  6  \w    -58.00  44.00   0.50   20.00    --   14.87 -57.00 -60.00  204
  7  \w    -55.00  48.00   0.50   20.00    --   14.87 -77.00-180.00  206
  8  \w    -17.00  79.00   0.50   20.00    --   14.87  77.00 -60.00  192
;
_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      -0.0210558000
_diffrn_orient_matrix_UB_12      0.0356516000
_diffrn_orient_matrix_UB_13      -0.0143692000
_diffrn_orient_matrix_UB_21      -0.0782928000
_diffrn_orient_matrix_UB_22      -0.0116357000
_diffrn_orient_matrix_UB_23      -0.0038197000
_diffrn_orient_matrix_UB_31      -0.0133857000
_diffrn_orient_matrix_UB_32      0.0117675000
_diffrn_orient_matrix_UB_33      0.0399048000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9822
_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         25.998
_diffrn_reflns_theta_min         3.266
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69630
_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    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.732
_exptl_crystal_size_mid          0.681
_exptl_crystal_size_min          0.297
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         9822
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      2.059
_refine_ls_R_factor_all          0.1380
_refine_ls_R_factor_gt           0.1287
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4384
_refine_ls_wR_factor_ref         0.4439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8031
_reflns_number_total             9822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b11145_si_001.cif
_cod_data_source_block           2xG1
_cod_original_cell_volume        2599(7)
_cod_database_code               1548852
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              81808
_twin_special_details
;
Component 2 rotated by -179.5576\% 
 around [-0.01 -0.00 1.00] (reciprocal) or [0.00 0.00 1.00] (direct)

;