Electrodeposition of Lithium from Lithium-Containing Solvate Ionic Liquids
Vanhoutte, Gijs; Brooks, Neil R.; Schaltin, Stijn; Opperdoes, Bastiaan; Van Meervelt, Luc; Locquet, Jean-Pierre; Vereecken, Philippe M.; Fransaer, Jan; Binnemans, Koen; The Journal of Physical Chemistry C 118 (2014) 20152–; doi:10.1021/jp505479x

data_1517427
_publ_section_title
;
 Electrodeposition of Lithium from Lithium-Containing Solvate Ionic
 Liquids
;
_journal_issue                   35
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              20152
_journal_paper_doi               10.1021/jp505479x
_journal_volume                  118
_journal_year                    2014
_chemical_formula_moiety         'I, C12 H28 Li O6'
_chemical_formula_sum            'C12 H28 I Li O6'
_chemical_formula_weight         402.18
_chemical_melting_point          351
_chemical_name_common
;
bis(1,5-Dimethoxy-3-oxapentane)-lithium iodide  
;
_chemical_name_systematic
;
bis(1,5-Dimethoxy-3-oxapentane)-lithium iodide  
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-18
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1824(7)
_cell_length_b                   12.0243(8)
_cell_length_c                   14.6817(15)
_cell_measurement_reflns_used    2842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4490
_cell_measurement_theta_min      2.9640
_cell_volume                     1797.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_details
;
  1 omega  -44.00   52.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9951   77.0000 -120.0000 96

  2 omega    8.00   88.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701   57.0000   30.0000 80

  3 omega  -12.00   34.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701  -57.0000  -90.0000 46

  4 omega  -40.00   92.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8701    0.0000  -60.0000 132
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0380914000
_diffrn_orient_matrix_UB_12      -0.0455653000
_diffrn_orient_matrix_UB_13      -0.0154817000
_diffrn_orient_matrix_UB_21      -0.0456033000
_diffrn_orient_matrix_UB_22      -0.0093300000
_diffrn_orient_matrix_UB_23      -0.0357808000
_diffrn_orient_matrix_UB_31      0.0363067000
_diffrn_orient_matrix_UB_32      0.0362132000
_diffrn_orient_matrix_UB_33      -0.0286221000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11189
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.05
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2196
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0607
_reflns_number_gt                1486
_reflns_number_total             2196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp505479x_si_002.cif
_cod_data_source_block           nrb150
_cod_depositor_comments          'Adding full bibliography for 1517427.cif.'
_cod_database_code               1517427
_chemical_oxdiff_formula         'Li I C6 H12 O3'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C1')
Uanis(O2) = Uanis(O2')
Uanis(C3) = Uanis(C3')
Uanis(C4) = Uanis(C4')
Uanis(O5) = Uanis(O5')
Uanis(C6) = Uanis(C6')
Uanis(C7) = Uanis(C7')
Uanis(O8) = Uanis(O8')
Uanis(C9) = Uanis(C9')
3. Same fragment restrains
{C1, O2, C3, C4, O5, C6, C7, O8, C9}
as
{C1', O2', C3', C4', O5', C6', C7', O8', C9'}
4. Others
 Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(H1'C)=Sof(O2')=Sof(C3')=Sof(H3'A)=Sof(H3'B)=
 Sof(C4')=Sof(H4'A)=Sof(H4'B)=Sof(O5')=Sof(C6')=Sof(H6'A)=Sof(H6'B)=Sof(C7')=
 Sof(H7'A)=Sof(H7'B)=Sof(O8')=Sof(C9')=Sof(H9'A)=Sof(H9'B)=Sof(H9'C)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(O2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(O5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 Sof(O8)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C3'(H3'A,H3'B), C4'(H4'A,
 H4'B), C6'(H6'A,H6'B), C7'(H7'A,H7'B)
5.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C1'(H1'A,H1'B,H1'C), C9'(H9'A,H9'B,H9'C)
;