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_7124574
_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         'C20 H32 N8 Pd, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C24 H32 F12 N10 O8 Pd S4'
_chemical_formula_weight         1051.24
_chemical_melting_point          349
_chemical_name_common
;
 tetrakis(N-ethylimidazole) palladium(II) bistriflimide
;
_chemical_name_systematic
;
 tetrakis(N-ethylimidazole) palladium(II) bis(trifluoromethyl)sulfonyl imide
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-06
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                92.776(5)
_cell_angle_beta                 106.337(5)
_cell_angle_gamma                113.370(6)
_cell_formula_units_Z            1
_cell_length_a                   8.8459(5)
_cell_length_b                   9.1693(6)
_cell_length_c                   14.3228(9)
_cell_measurement_reflns_used    5736
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0640
_cell_measurement_theta_min      3.4460
_cell_volume                     1006.34(13)
_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
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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 0.998
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0835511000
_diffrn_orient_matrix_UB_12      -0.0469677000
_diffrn_orient_matrix_UB_13      -0.0352484000
_diffrn_orient_matrix_UB_21      -0.0094602000
_diffrn_orient_matrix_UB_22      0.0715786000
_diffrn_orient_matrix_UB_23      -0.0097418000
_diffrn_orient_matrix_UB_31      0.0384443000
_diffrn_orient_matrix_UB_32      0.0037562000
_diffrn_orient_matrix_UB_33      -0.0376389000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8744
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72828
_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    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         4580
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0234P)^2^+0.6259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                4371
_reflns_number_total             4580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc04079a2.cif
_cod_data_source_block           nrb185
_cod_original_cell_volume        1006.34(11)
_cod_database_code               7124574
_chemical_oxdiff_formula         'Pd C4 F12 S4 O8 N2 N8 C20 H32'
_reflns_odcompleteness_completeness 99.85
_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. Restrained distances
 S34-C30 \\sim S38-C41 \\sim S19-C15 \\sim S23-C26
 with sigma of 0.01
3. Rigid bond restraints
 C30, F31, F32, F33, S34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
4. Others
 Fixed Sof: C15(0.5) F16(0.5) F17(0.5) F18(0.5) S19(0.5) O20(0.5) O21(0.5)
 N22(0.5) S23(0.5) O24(0.5) O25(0.5) C26(0.5) F27(0.5) F28(0.5) F29(0.5)
 C30(0.5) F31(0.5) F32(0.5) F33(0.5) S34(0.5) O35(0.5) O36(0.5) N37(0.5)
 S38(0.5) O39(0.5) O40(0.5) C41(0.5) F42(0.5) F43(0.5) F44(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C9(H9), C11(H11), C12(H12)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C)
;