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_1548849
_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, H2 O'
_chemical_formula_sum            'C6 H8 F3 Li N4 O4'
_chemical_formula_weight         264.10
_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   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                 91.321(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0805(12)
_cell_length_b                   6.7141(6)
_cell_length_c                   18.9826(18)
_cell_measurement_reflns_used    1369
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      25.9930
_cell_measurement_theta_min      4.3760
_cell_volume                     1157.0(2)
_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      100.0(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 0.996
_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    -86.00   4.00   1.00   50.00    --  -19.34 -77.00   0.00   90
  2  \w    -91.00  14.00   1.00   50.00    --  -19.34 -77.00 120.00  105
  3  \w     68.00  94.00   1.00   50.00    --   20.12-179.00 -60.00   26
  4  \w    -49.00  34.00   1.00   50.00    --   20.12 -38.00 -30.00   83
  5  \w     84.00 109.00   1.00   50.00    --   20.12-179.00  30.00   25
  6  \w    -53.00  48.00   1.00   50.00    --   20.12 -57.00-120.00  101
;
_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      0.0009420000
_diffrn_orient_matrix_UB_12      -0.1056509000
_diffrn_orient_matrix_UB_13      -0.0000457000
_diffrn_orient_matrix_UB_21      0.0521670000
_diffrn_orient_matrix_UB_22      0.0007388000
_diffrn_orient_matrix_UB_23      0.0284007000
_diffrn_orient_matrix_UB_31      -0.0581439000
_diffrn_orient_matrix_UB_32      -0.0011411000
_diffrn_orient_matrix_UB_33      0.0242977000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3488
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.395
_diffrn_reflns_theta_min         3.718
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.959
_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    1.516
_exptl_crystal_description       needle
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3488
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0815P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2580
_reflns_number_total             3488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp7b11145_si_001.cif
_cod_data_source_block           1b
_cod_database_code               1548849
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.932
_shelx_res_checksum              67448
_twin_special_details
;
Component 2 rotated by 179.9782\% 
 around [-0.00 -0.00 1.00] (reciprocal) or [0.05 -0.00 1.00] (direct)
;