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_7124575
_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         'C18 H28 N8 Pd, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C22 H28 F12 N10 O8 Pd S4'
_chemical_formula_weight         1023.18
_chemical_melting_point          318
_chemical_name_common
;
 bis(N-methylimidazole) bis(N-ethylimidazole) palladium(II) bistriflimide
;
_chemical_name_systematic
;
  bis(N-methylimidazole) bis(N-ethylimidazole) 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     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                90.00
_cell_angle_beta                 90.056(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.2427(8)
_cell_length_b                   11.3109(5)
_cell_length_c                   15.6582(9)
_cell_measurement_reflns_used    4147
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.394
_cell_measurement_theta_min      3.263
_cell_volume                     1814.07(19)
_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 0.863
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0272066000
_diffrn_orient_matrix_UB_12      0.0420496000
_diffrn_orient_matrix_UB_13      -0.0284745000
_diffrn_orient_matrix_UB_21      0.0356803000
_diffrn_orient_matrix_UB_22      0.0254068000
_diffrn_orient_matrix_UB_23      0.0343211000
_diffrn_orient_matrix_UB_31      0.0526977000
_diffrn_orient_matrix_UB_32      -0.0389144000
_diffrn_orient_matrix_UB_33      -0.0083387000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9615
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72861
_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    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4200
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0376P)^2^+3.3950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                3503
_reflns_number_total             4200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc04079a2.cif
_cod_data_source_block           kb2019
_cod_original_cell_volume        1814.07(18)
_cod_database_code               7124575
_chemical_oxdiff_formula         'Pd C18 N4 H28 C4 F12 N2 S4 O8'
_reflns_odcompleteness_completeness 99.74
_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'}
3. Restrained distances
 C6'-C7'
 1.5 with sigma of 0.01
 C13'-C14'
 1.5 with sigma of 0.01
4. Rigid bond restraints
 C6, C6', C7', C13, C13', C14'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C6 \\sim C6' \\sim C7' \\sim C13 \\sim C13' \\sim C14': within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(C6) = Uanis(C6')
Uanis(C13) = Uanis(C13')
6. Others
 Fixed Sof: C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C6'(0.5) H6'A(0.5) H6'B(0.5)
 C7'(0.5) H7'A(0.5) H7'B(0.5) H7'C(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
 C13'(0.5) H13D(0.5) H13E(0.5) C14'(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C6'(H6'A,H6'B), C13'(H13D,H13E)
7.b Me refined with riding coordinates:
 C7'(H7'A,H7'B,H7'C), C14'(H14A,H14B,H14C)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C9(H9), C11(H11), C12(H12)
7.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C13(H13A,H13B,H13C)
;