Homoleptic and heteroleptic N-alkylimidazole zinc(ii)-containing ionic liquids for high current density electrodeposition.
Steichen, Marc; Brooks, Neil R.; Van Meervelt, Luc; Fransaer, Jan; Binnemans, Koen; Dalton transactions (Cambridge, England : 2003) 43 (2014) 12329–12341; doi:10.1039/c4dt00182f

data_7031358
_publ_section_title
;
 Homoleptic and heteroleptic N-alkylimidazole zinc(ii)-containing ionic
 liquids for high current density electrodeposition.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12329
_journal_page_last               12341
_journal_paper_doi               10.1039/c4dt00182f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C25.5 H39 N12 Zn, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C29.5 H39 F12 N14 O8 S4 Zn'
_chemical_formula_weight         1139.36
_chemical_name_common
;
4.5(N-methylimidazole) 1.5(N-ethylimidazole) zinc(II)
bis(trifluoromethylsulfony)limide
;
_chemical_name_systematic
;
4.5(N-methylimidazole) 1.5(N-ethylimidazole) zinc(II)
bis(trifluoromethylsulfony)limide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-12-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.811(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.3667(2)
_cell_length_b                   11.5721(3)
_cell_length_c                   24.0909(4)
_cell_measurement_reflns_used    3706
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6960
_cell_measurement_theta_min      3.3890
_cell_volume                     2320.50(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0241151000
_diffrn_orient_matrix_UB_12      -0.0593854000
_diffrn_orient_matrix_UB_13      0.0012941000
_diffrn_orient_matrix_UB_21      0.0453692000
_diffrn_orient_matrix_UB_22      -0.0056575000
_diffrn_orient_matrix_UB_23      0.0264080000
_diffrn_orient_matrix_UB_31      -0.0679163000
_diffrn_orient_matrix_UB_32      0.0172464000
_diffrn_orient_matrix_UB_33      0.0131896000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10876
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67906
_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    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5326
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+3.0966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                4415
_reflns_number_total             5326
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00182f2.cif
_cod_data_source_block           nrb182
_cod_depositor_comments
'Adding full bibliography for 7031354--7031358.cif.'
_cod_original_cell_volume        2320.49(9)
_cod_original_formula_sum        'C29.50 H39 F12 N14 O8 S4 Zn'
_cod_database_code               7031358
_chemical_oxdiff_formula         'Zn C4 F12 S4 O8 N2 N12 C26 H50'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C6, C6'}
{C13, C13'}
{C20, C20'}
3. Restrained distances
 C6-C7 = C13-C14 = C20-C21
 1.5 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C6')
Uanis(C13) = Uanis(C13')
Uanis(C20) = Uanis(C20')
5. Others
 1*[Sof(C6)+Sof(H6A)+Sof(H6B)+Sof(C7)+Sof(H7A)+Sof(H7B)+Sof(H7C)+Sof(C6')+
 Sof(H6'A)+Sof(H6'B)+Sof(H6'C)]+1*[Sof(C13)+Sof(H13A)+Sof(H13B)+Sof(C14)+
 Sof(H14A)+Sof(H14B)+Sof(H14C)+Sof(C13')+Sof(H13C)+Sof(H13D)+Sof(H13E)]+1*
 [Sof(C20)+Sof(H20A)+Sof(H20B)+Sof(C21)+Sof(H21A)+Sof(H21B)+Sof(H21C)+Sof(C20')+
 Sof(H20C)+Sof(H20D)+Sof(H20E)]=0.75 with esd of 0.00001
 Sof(C6')=Sof(H6'A)=Sof(H6'B)=Sof(H6'C)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(1)
 Sof(C13')=Sof(H13C)=Sof(H13D)=Sof(H13E)=1-FVAR(2)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
 Sof(C20')=Sof(H20C)=Sof(H20D)=Sof(H20E)=1-FVAR(3)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B), C20(H20A,H20B)
6.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C9(H9), C11(H11), C12(H12), C16(H16), C18(H18),
 C19(H19)
6.d Idealised Me refined as rotating group:
 C6'(H6'A,H6'B,H6'C), C13'(H13C,H13D,H13E), C20'(H20C,H20D,H20E)
;