Electrodeposition of thick palladium coatings from a palladium(II)-containing ionic liquid.
Schaltin, Stijn; Brooks, Neil R.; Sniekers, Jeroen; Van Meervelt, Luc; Binnemans, Koen; Fransaer, Jan; Chemical communications (Cambridge, England) 50 (2014) 10248–10250; doi:10.1039/c4cc04079a

data_7124573
_publ_section_title
;
 Electrodeposition of thick palladium coatings from a
 palladium(II)-containing ionic liquid.
;
_journal_issue                   71
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10248
_journal_page_last               10250
_journal_paper_doi               10.1039/c4cc04079a
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C16 H24 N8 Pd, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C20 H24 F12 N10 O8 Pd S4'
_chemical_formula_weight         995.13
_chemical_melting_point          378
_chemical_name_common
;
 tetrakis(N-methylimidazole) palladium(II) bistriflimide
;
_chemical_name_systematic
;
 tetrakis(N-methylimidazole) palladium(II) bis(trifluoromethyl)sulfonyl imide
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-05
_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                 99.330(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1556(2)
_cell_length_b                   10.8229(2)
_cell_length_c                   17.9774(3)
_cell_measurement_reflns_used    5107
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.860
_cell_measurement_theta_min      2.946
_cell_volume                     1757.82(6)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9631
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0647870000
_diffrn_orient_matrix_UB_12      0.0204441000
_diffrn_orient_matrix_UB_13      0.0132745000
_diffrn_orient_matrix_UB_21      0.0099454000
_diffrn_orient_matrix_UB_22      -0.0466243000
_diffrn_orient_matrix_UB_23      0.0280654000
_diffrn_orient_matrix_UB_31      0.0432768000
_diffrn_orient_matrix_UB_32      0.0412522000
_diffrn_orient_matrix_UB_33      0.0251799000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8254
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.10
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86769
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0233P)^2^+1.1985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                3632
_reflns_number_total             4114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc04079a2.cif
_cod_data_source_block           nrb143
_cod_database_code               7124573
_chemical_oxdiff_formula         'Pd C3 H3 N2 C H4 C2 F6 S2 O4 N'
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C13')
Uanis(F14) = Uanis(F14')
Uanis(F15) = Uanis(F15')
Uanis(F16) = Uanis(F16')
Uanis(S17) = Uanis(S17')
Uanis(O18) = Uanis(O18')
Uanis(O19) = Uanis(O19')
Uanis(N20) = Uanis(N20')
Uanis(S21) = Uanis(S21')
Uanis(O22) = Uanis(O22')
Uanis(O23) = Uanis(O23')
Uanis(C24) = Uanis(C24')
Uanis(F25) = Uanis(F25')
Uanis(F26) = Uanis(F26')
Uanis(F27) = Uanis(F27')
3. Same fragment restrains
{C13, F14, F15, F16, S17, O18, O19, N20, S21, O22, O23, C24, F25, F26, F27}
as
{C13', F14', F15', F16', S17', O18', O19', N20', S21', O22', O23', C24', F25',
F26', F27'}
4. Others
 Sof(C13')=Sof(F14')=Sof(F15')=Sof(F16')=Sof(S17')=Sof(O18')=Sof(O19')=
 Sof(N20')=Sof(S21')=Sof(O22')=Sof(O23')=Sof(C24')=Sof(F25')=Sof(F26')=
 Sof(F27')=1-FVAR(1)
 Sof(C13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(S17)=Sof(O18)=Sof(O19)=Sof(N20)=
 Sof(S21)=Sof(O22)=Sof(O23)=Sof(C24)=Sof(F25)=Sof(F26)=Sof(F27)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C)
;