#------------------------------------------------------------------------------
#$Date: 2019-11-23 09:39:04 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232747 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/45/7124574.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7124574
loop_
_publ_author_name
'Schaltin, Stijn'
'Brooks, Neil R.'
'Sniekers, Jeroen'
'Van Meervelt, Luc'
'Binnemans, Koen'
'Fransaer, Jan'
_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
;
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       'ω 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/[σ²(Fo²)+(0.0234P)²+0.6259P] where P=(Fo²+2Fc²)/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)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.5000 0.0000 0.5000 0.01556(5) Uani 1 d . . 2 S T P
N1 N 0.29891(16) -0.03005(16) 0.37872(10) 0.0188(3) Uani 1 d . . 1 . . .
C2 C 0.2891(2) -0.0646(2) 0.28557(12) 0.0202(3) Uani 1 d . . 1 . . .
H2 H 0.3768 -0.0789 0.2657 0.024 Uiso 1 calc . . 1 R . .
N3 N 0.13748(17) -0.07645(17) 0.22327(10) 0.0215(3) Uani 1 d . . 1 . . .
C4 C 0.0460(2) -0.0477(2) 0.27955(13) 0.0264(4) Uani 1 d . . 1 . . .
H4 H -0.0658 -0.0480 0.2559 0.032 Uiso 1 calc . . 1 R . .
C5 C 0.1466(2) -0.0189(2) 0.37559(13) 0.0263(4) Uani 1 d . . 1 . . .
H5 H 0.1170 0.0051 0.4314 0.032 Uiso 1 calc . . 1 R . .
C6 C 0.0789(2) -0.1168(3) 0.11467(13) 0.0306(4) Uani 1 d . . 1 . . .
H6A H 0.1818 -0.0823 0.0921 0.037 Uiso 1 calc . . 1 R . .
H6B H 0.0105 -0.0570 0.0861 0.037 Uiso 1 calc . . 1 R . .
C7 C -0.0309(3) -0.2945(3) 0.07804(17) 0.0534(6) Uani 1 d . . 1 . . .
H7A H -0.0668 -0.3173 0.0057 0.080 Uiso 1 calc . . 1 GR . .
H7B H -0.1344 -0.3285 0.0988 0.080 Uiso 1 calc . . 1 GR . .
H7C H 0.0369 -0.3540 0.1057 0.080 Uiso 1 calc . . 1 GR . .
N8 N 0.46561(17) 0.17493(17) 0.56975(10) 0.0188(3) Uani 1 d . . 1 . . .
C9 C 0.5567(2) 0.3323(2) 0.57879(11) 0.0183(3) Uani 1 d . . 1 . . .
H9 H 0.6465 0.3805 0.5510 0.022 Uiso 1 calc . . 1 R . .
N10 N 0.50410(18) 0.41428(17) 0.63292(10) 0.0207(3) Uani 1 d . . 1 . . .
C11 C 0.3729(2) 0.3029(2) 0.65964(15) 0.0315(4) Uani 1 d . . 1 . . .
H11 H 0.3105 0.3254 0.6982 0.038 Uiso 1 calc . . 1 R . .
C12 C 0.3493(2) 0.1555(2) 0.62065(15) 0.0305(4) Uani 1 d . . 1 . . .
H12 H 0.2666 0.0552 0.6271 0.037 Uiso 1 calc . . 1 R . .
C13 C 0.5773(3) 0.5904(2) 0.66100(14) 0.0276(4) Uani 1 d . . 1 . . .
H13A H 0.4836 0.6264 0.6375 0.033 Uiso 1 calc . . 1 R . .
H13B H 0.6656 0.6418 0.6286 0.033 Uiso 1 calc . . 1 R . .
C14 C 0.6611(3) 0.6442(2) 0.77217(15) 0.0378(5) Uani 1 d . . 1 . . .
H14A H 0.7116 0.7623 0.7886 0.057 Uiso 1 calc . . 1 GR . .
H14B H 0.7530 0.6076 0.7956 0.057 Uiso 1 calc . . 1 GR . .
H14C H 0.5727 0.5973 0.8042 0.057 Uiso 1 calc . . 1 GR . .
C15 C 0.5294(14) 1.2777(10) 0.9615(12) 0.048(3) Uani 0.50 d A -1 1 . . .
F16 F 0.4367(5) 1.3537(4) 0.9175(2) 0.0634(9) Uani 0.50 d A -1 1 . . .
F17 F 0.5771(8) 1.3160(6) 1.0567(4) 0.0708(14) Uani 0.50 d A -1 1 . . .
F18 F 0.6756(5) 1.3371(4) 0.9329(4) 0.0709(11) Uani 0.50 d A -1 1 . . .
S19 S 0.4106(5) 1.0603(6) 0.9151(3) 0.0221(5) Uani 0.50 d A -1 1 . . .
O20 O 0.2611(4) 1.0169(4) 0.9451(2) 0.0372(7) Uani 0.50 d A -1 1 . . .
O21 O 0.3880(4) 1.0476(4) 0.8116(2) 0.0369(6) Uani 0.50 d A -1 1 . . .
N22 N 0.5492(4) 0.9985(4) 0.9662(2) 0.0249(6) Uani 0.50 d A -1 1 . . .
S23 S 0.5563(6) 0.9224(6) 1.0639(3) 0.0247(6) Uani 0.50 d A -1 1 . . .
O24 O 0.4802(3) 0.9707(3) 1.12825(18) 0.0310(6) Uani 0.50 d A -1 1 . . .
O25 O 0.7263(4) 0.9310(5) 1.1045(3) 0.0489(9) Uani 0.50 d A -1 1 . . .
C26 C 0.4117(13) 0.7073(8) 1.0167(10) 0.041(2) Uani 0.50 d A -1 1 . . .
F27 F 0.2531(4) 0.6873(3) 0.9660(2) 0.0542(7) Uani 0.50 d A -1 1 . . .
F28 F 0.4061(7) 0.6271(4) 1.0884(3) 0.0704(12) Uani 0.50 d A -1 1 . . .
F29 F 0.4717(9) 0.6475(6) 0.9558(4) 0.0672(14) Uani 0.50 d A -1 1 . . .
C30 C -0.082(2) 0.420(2) 0.3090(9) 0.0208(17) Uani 0.50 d B -1 1 . U .
F31 F 0.0322(3) 0.5715(3) 0.31764(17) 0.0366(5) Uani 0.50 d B -1 1 . U .
F32 F -0.0570(4) 0.3229(3) 0.25379(17) 0.0397(6) Uani 0.50 d B -1 1 . U .
F33 F -0.2396(3) 0.4125(4) 0.27066(19) 0.0433(6) Uani 0.50 d B -1 1 . U .
S34 S -0.0584(12) 0.3587(11) 0.4299(8) 0.0228(10) Uani 0.50 d B -1 1 . U .
O35 O 0.0101(4) 0.2335(3) 0.4253(2) 0.0332(6) Uani 0.50 d B -1 1 . . .
O36 O -0.2284(3) 0.2904(3) 0.4466(2) 0.0293(6) Uani 0.50 d B -1 1 . . .
N37 N 0.0879(4) 0.5049(4) 0.5061(2) 0.0233(6) Uani 0.50 d B -1 1 . . .
S38 S 0.0563(13) 0.6462(12) 0.5609(7) 0.0210(9) Uani 0.50 d B -1 1 . . .
O39 O 0.1983(5) 0.7861(4) 0.5803(2) 0.0485(9) Uani 0.50 d B -1 1 . . .
O40 O -0.1194(4) 0.6231(3) 0.53240(19) 0.0315(6) Uani 0.50 d B -1 1 . . .
C41 C 0.093(3) 0.589(3) 0.6830(11) 0.032(3) Uani 0.50 d B -1 1 . . .
F42 F 0.1388(6) 0.4689(5) 0.6871(2) 0.0660(10) Uani 0.50 d B -1 1 . . .
F43 F -0.0485(3) 0.5437(4) 0.71287(18) 0.0429(6) Uani 0.50 d B -1 1 . . .
F44 F 0.2198(4) 0.7089(5) 0.7552(2) 0.0720(11) Uani 0.50 d B -1 1 . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Pd1 N1 179.999(1) 2_656 .
N8 Pd1 N1 90.54(5) 2_656 2_656
N8 Pd1 N1 89.46(5) 2_656 .
N8 Pd1 N1 90.54(5) . .
N8 Pd1 N1 89.46(5) . 2_656
N8 Pd1 N8 180.00(7) 2_656 .
C2 N1 Pd1 125.91(11) . .
C2 N1 C5 106.56(14) . .
C5 N1 Pd1 127.53(11) . .
N1 C2 N3 110.48(14) . .
C2 N3 C4 107.60(14) . .
C2 N3 C6 126.04(14) . .
C4 N3 C6 126.35(14) . .
C5 C4 N3 106.62(15) . .
C4 C5 N1 108.74(15) . .
N3 C6 C7 111.58(17) . .
C9 N8 Pd1 125.94(11) . .
C9 N8 C12 106.63(14) . .
C12 N8 Pd1 127.38(12) . .
N8 C9 N10 110.38(14) . .
C9 N10 C11 107.49(14) . .
C9 N10 C13 126.27(14) . .
C11 N10 C13 126.22(14) . .
C12 C11 N10 106.93(15) . .
C11 C12 N8 108.57(16) . .
N10 C13 C14 111.29(14) . .
F16 C15 F18 103.9(11) . .
F16 C15 S19 110.4(6) . .
F17 C15 F16 110.8(10) . .
F17 C15 F18 108.6(8) . .
F17 C15 S19 113.6(10) . .
F18 C15 S19 109.1(9) . .
O20 S19 C15 103.3(6) . .
O20 S19 O21 118.6(3) . .
O20 S19 N22 117.8(3) . .
O21 S19 C15 103.2(7) . .
O21 S19 N22 109.2(4) . .
N22 S19 C15 101.8(4) . .
S19 N22 S23 124.8(4) . .
N22 S23 C26 103.3(5) . .
O24 S23 N22 115.8(4) . .
O24 S23 C26 103.9(6) . .
O25 S23 N22 107.6(4) . .
O25 S23 O24 118.8(3) . .
O25 S23 C26 105.6(5) . .
F27 C26 S23 110.7(5) . .
F27 C26 F29 107.8(9) . .
F28 C26 S23 110.8(8) . .
F28 C26 F27 109.7(10) . .
F28 C26 F29 108.3(7) . .
F29 C26 S23 109.4(9) . .
F31 C30 S34 110.8(9) . .
F32 C30 F31 110.7(13) . .
F32 C30 F33 110.6(11) . .
F32 C30 S34 107.4(11) . .
F33 C30 F31 107.9(13) . .
F33 C30 S34 109.5(12) . .
O35 S34 C30 104.6(9) . .
O35 S34 N37 106.6(6) . .
O36 S34 C30 110.6(9) . .
O36 S34 O35 111.2(6) . .
O36 S34 N37 116.5(7) . .
N37 S34 C30 106.6(8) . .
S34 N37 S38 123.8(7) . .
N37 S38 C41 96.7(9) . .
O39 S38 N37 108.7(7) . .
O39 S38 O40 127.3(8) . .
O39 S38 C41 100.0(9) . .
O40 S38 N37 114.5(6) . .
O40 S38 C41 103.4(8) . .
F42 C41 S38 112.8(13) . .
F42 C41 F43 106.6(13) . .
F42 C41 F44 105.6(12) . .
F43 C41 S38 113.1(11) . .
F44 C41 S38 113.5(12) . .
F44 C41 F43 104.6(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.0208(13) 2_656
Pd1 N1 2.0209(13) .
Pd1 N8 2.0165(13) 2_656
Pd1 N8 2.0165(13) .
N1 C2 1.327(2) .
N1 C5 1.380(2) .
C2 N3 1.344(2) .
N3 C4 1.375(2) .
N3 C6 1.471(2) .
C4 C5 1.358(2) .
C6 C7 1.500(3) .
N8 C9 1.322(2) .
N8 C12 1.383(2) .
C9 N10 1.344(2) .
N10 C11 1.373(2) .
N10 C13 1.466(2) .
C11 C12 1.349(3) .
C13 C14 1.516(3) .
C15 F16 1.327(11) .
C15 F17 1.294(18) .
C15 F18 1.377(17) .
C15 S19 1.826(6) .
S19 O20 1.418(6) .
S19 O21 1.431(5) .
S19 N22 1.564(5) .
N22 S23 1.589(6) .
S23 O24 1.431(6) .
S23 O25 1.420(5) .
S23 C26 1.835(6) .
C26 F27 1.319(10) .
C26 F28 1.293(14) .
C26 F29 1.337(16) .
C30 F31 1.33(2) .
C30 F32 1.29(2) .
C30 F33 1.319(17) .
C30 S34 1.829(6) .
S34 O35 1.502(11) .
S34 O36 1.476(10) .
S34 N37 1.534(9) .
N37 S38 1.638(11) .
S38 O39 1.338(10) .
S38 O40 1.415(11) .
S38 C41 1.829(6) .
C41 F42 1.31(2) .
C41 F43 1.35(2) .
C41 F44 1.34(2) .
