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_1548846
_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         'C24 H54 Li2 O15, 2(C6 F3 N4)'
_chemical_formula_sum            'C36 H54 F6 Li2 N8 O15'
_chemical_formula_weight         966.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-21
_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            4
_cell_length_a                   14.2835(3)
_cell_length_b                   17.9913(4)
_cell_length_c                   18.1462(4)
_cell_measurement_reflns_used    17340
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      25.8640
_cell_measurement_theta_min      3.4680
_cell_volume                     4663.19(18)
_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 0.996
_diffrn_measured_fraction_theta_max 0.997
_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    -97.00  10.00   1.00   35.00    --  -19.34 -77.00 150.00  107
  2  \w    -45.00  62.00   1.00   35.00    --  -19.34  19.00-180.00  107
  3  \w    -97.00 -17.00   1.00   35.00    --  -19.34 155.00-106.34   80
  4  \w    -84.00  10.00   1.00   35.00    --  -19.34 -57.00-120.00   94
  5  \w    -98.00   5.00   1.00   35.00    --  -19.34 -77.00  30.00  103
  6  \w    -56.00  36.00   1.00   35.00    --   20.12 -38.00-120.00   92
  7  \w    -59.00  54.00   1.00   35.00    --   20.12 -77.00  60.00  113
  8  \w     22.00  81.00   1.00   35.00    --   20.12-130.00-157.72   59
;
_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      -0.0453328000
_diffrn_orient_matrix_UB_12      0.0155076000
_diffrn_orient_matrix_UB_13      0.0042913000
_diffrn_orient_matrix_UB_21      -0.0088153000
_diffrn_orient_matrix_UB_22      -0.0054567000
_diffrn_orient_matrix_UB_23      -0.0380657000
_diffrn_orient_matrix_UB_31      -0.0182584000
_diffrn_orient_matrix_UB_32      -0.0358586000
_diffrn_orient_matrix_UB_33      0.0076544000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            76851
_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         26.313
_diffrn_reflns_theta_min         3.494
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.972
_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    1.377
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.257
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 3214 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         9466
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0310P)^2^+0.9710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8122
_reflns_number_total             9466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b11145_si_001.cif
_cod_data_source_block           4
_cod_database_code               1548846
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              26571