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Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 68| Part 5| May 2012| Pages m616-m617

Dipotassium tetra­kis­(thio­cyanato-κS)palladate(II)–(2,2′-bi­pyrimidine-κ2N1,N1′)bis­­(thio­cyanato-κS)palladium(II) (1/2)

aSchool of Applied Chemical Engineering, The Research Institute of Catalysis, Chonnam National University, Gwangju 500-757, Republic of Korea
*Correspondence e-mail: hakwang@chonnam.ac.kr

(Received 3 April 2012; accepted 8 April 2012; online 18 April 2012)

The asymmetric unit of the title compound, K2[Pd(NCS)4]·2[Pd(NCS)2(C8H6N4)], contains two crystallographically independent half-mol­ecules of the anionic PdII complex, two K+ cations and two independent neutral PdII complexes; an inversion centre is located at the centroid of each anionic complex. In the anionic complexes, each PdII ion is four-coordinated in an almost regular square-planar environment by four S atoms from four SCN anions, and the PdS4 unit is exactly planar. In the neutral complexes, the PdII ion has a slightly distorted square-planar coordination environment defined by two pyrimidine N atoms derived from a chelating 2,2′-bipyrimidine ligand and two mutually cis S atoms from two SCN anions. Both 2,2′-bipyrimidine ligands are almost planar [dihedral angle between the rings = 3.98 (16) and 4.57 (17)°] and also chelate to a potassium ion from their other two N atoms. In the crystal, the K+ ions inter­act with various S and N atoms of the ligands, forming a three-dimensional polymeric network, in which the shortest K⋯K contacts between the KN7S polyhedra are 4.4389 (17) and 4.4966 (18) Å. Intra- and inter­molecular C—H⋯S and C—H⋯N hydrogen bonds are also observed.

Related literature

For the crystal structure of K2[Pd(SCN)4], see: Mawby & Pringle (1972[Mawby, A. & Pringle, G. E. (1972). J. Inorg. Nucl. Chem. 34, 2213-2217.]); Ha (2010[Ha, K. (2010). Z. Kristallogr. New Cryst. Struct. 225, 619-620.]).

[Scheme 1]

Experimental

Crystal data
  • K2[Pd(NCS)4]·2[Pd(NCS)2(C8H6N4)]

  • Mr = 1178.38

  • Monoclinic, P 21 /c

  • a = 15.9625 (7) Å

  • b = 10.9700 (5) Å

  • c = 21.6801 (9) Å

  • β = 94.104 (1)°

  • V = 3786.6 (3) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 2.12 mm−1

  • T = 200 K

  • 0.28 × 0.24 × 0.18 mm

Data collection
  • Bruker SMART 1000 CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2000[Bruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.854, Tmax = 1.000

  • 22881 measured reflections

  • 7371 independent reflections

  • 5722 reflections with I > 2σ(I)

  • Rint = 0.030

Refinement
  • R[F2 > 2σ(F2)] = 0.030

  • wR(F2) = 0.080

  • S = 1.08

  • 7371 reflections

  • 481 parameters

  • H-atom parameters constrained

  • Δρmax = 0.65 e Å−3

  • Δρmin = −0.59 e Å−3

Table 1
Selected bond lengths (Å)

Pd1—N1 2.074 (3)
Pd1—N4 2.070 (3)
Pd1—S1 2.2945 (11)
Pd1—S2 2.3077 (11)
Pd2—N7 2.059 (3)
Pd2—N10 2.069 (3)
Pd2—S3i 2.2958 (10)
Pd2—S4 2.2829 (11)
Pd3—S5 2.3388 (9)
Pd3—S6 2.3314 (9)
Pd4—S7 2.3157 (10)
Pd4—S8 2.3419 (10)
Symmetry code: (i) [-x, y-{\script{1\over 2}}, -z-{\script{1\over 2}}].

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
C1—H1⋯S1 0.95 2.77 3.334 (4) 119
C1—H1⋯N11ii 0.95 2.45 3.134 (5) 128
C6—H6⋯S7iii 0.95 2.76 3.457 (4) 131
C8—H8⋯S2 0.95 2.77 3.321 (4) 118
C11—H11⋯S3i 0.95 2.82 3.371 (4) 118
C11—H11⋯N6iv 0.95 2.63 3.315 (5) 130
C13—H13⋯N15v 0.95 2.61 3.376 (5) 138
C16—H16⋯S6ii 0.95 2.83 3.640 (4) 144
C18—H18⋯S4 0.95 2.71 3.276 (4) 119
Symmetry codes: (i) [-x, y-{\script{1\over 2}}, -z-{\script{1\over 2}}]; (ii) -x+1, -y+1, -z; (iii) x, y-1, z; (iv) -x, -y+1, -z; (v) -x, -y+2, -z.

Data collection: SMART (Bruker, 2000[Bruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2000[Bruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

The title compound, K2[Pd(SCN)4].2[Pd(SCN)2(bpym)] (bpym = 2,2'-bipyrimidine), was unexpected obtained from the reaction of Na2PdCl4 with KSCN and bpym. The asymmetric unit contains two crystallographically independent half-molecules of the anionic PdII complex [Pd(SCN)4]2-, two K+ cations and two independent neutral PdII complexes [Pd(SCN)2(bpym)]; an inversion centre is located at the centroid of each anionic complex (Fig. 1). The crystal structure of K2[Pd(SCN)4] has been investigated previously (Mawby & Pringle, 1972; Ha, 2010).

In the anionic complexes, each PdII ion is four-coordinated in an essentially square-planar environment by four S atoms from four SCN- anions, and the PdS4 unit is exactly planar. The two complexes are chemically identical, but slightly different in geometry. The Pd—S bond lengths are roughly equal [Pd—S: 2.3157 (10)–2.3419 (10) Å] (Table 1). The thiocyanato ligands are almost linear displaying S—C—N bond angles of 174.8 (4)°–178.1 (4)°, and the S atoms coordinate to the Pd atom with the nearly tetrahedral Pd—S—C bond angles of 106.57 (13)°–110.44 (13)°.

In the two neutral complexes, each PdII ion has a slightly distorted square-planar coordination environment defined by two pyrimidine N atoms derived from a chelating bpym ligand and two mutually cis S atoms from two SCN- anions. The complexes are fairly different in geometry, because the coordination modes of the anions are significantly different. The two thiocyanato ligands are located on the same side of the PdS2N2 unit plane in the complex with Pd1, whereas in the other complex with Pd2, the ligands lie on the opposite sides of the PdS2N2 unit. But, the Pd—N and Pd—S bond lengths are nearly equivalent, respectively [Pd—N = 2.059 (3)–2.074 (3) Å; Pd—S = 2.2829 (11)–2.3077 (11) Å] (Table 1). The bpym ligands are slightly inclined to the least-squares plane of the PdS2N2 unit [maximum deviation = 0.090 (1) Å], making dihedral angles of 9.55 (9)° in the complex with Pd1 and 7.28 (7)° in the complex with Pd2.

In the crystal structure, the K+ ions interact with the various S and N atoms of the ligands with the distances of K···S = 3.6081 (13) Å and 3.6692 (13) Å, and K···N = 2.806 (3)–3.370 (5) Å, forming a three-dimensional polymeric network, and the short K···K contacts are present [4.4389 (17) Å and 4.4966 (18) Å]. Intra- and intramolecular C—H···S and C—H···N hydrogen bonds are also observed (Table 2).

Related literature top

For the crystal structure of K2[Pd(SCN)4], see: Mawby & Pringle (1972); Ha (2010).

Experimental top

To a solution of Na2PdCl4 (0.1478 g, 0.502 mmol) in MeOH (30 ml) were added KSCN (0.5358 g, 5.513 mmol) and 2,2'-bipyrimidine (0.0819 g, 0.518 mmol), and refluxed for 3 h. The formed precipitate was separated by filtration and washed with H2O and acetone, and dried at 50 °C, to give a pale red powder (0.1095 g). Red blocks were obtained by slow evaporation from a CH3CN solution.

Refinement top

H atoms were positioned geometrically and allowed to ride on their respective parent atoms: C—H = 0.95 Å with Uiso(H) = 1.2Ueq(C). The highest peak (0.65 e Å-3) and the deepest hole (-0.59 e Å-3) in the difference Fourier map are located 0.71 Å and 0.83 Å, respectively, from the Pd1 atom.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. A structure detail of the title compound, with displacement ellipsoids drawn at the 30% probability level for non-H atoms. Unlabelled atoms are generated by the application of the inversion centres.
Dipotassium tetrakis(thiocyanato-κS)palladate(II)– (2,2'-bipyrimidine-κ2N1,N1')bis(thiocyanato- κS)palladium(II) (1/2) top
Crystal data top
K2[Pd(NCS)4]·2[Pd(NCS)2(C8H6N4)]F(000) = 2288
Mr = 1178.38Dx = 2.067 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5010 reflections
a = 15.9625 (7) Åθ = 2.5–26.0°
b = 10.9700 (5) ŵ = 2.12 mm1
c = 21.6801 (9) ÅT = 200 K
β = 94.104 (1)°Block, red
V = 3786.6 (3) Å30.28 × 0.24 × 0.18 mm
Z = 4
Data collection top
Bruker SMART 1000 CCD
diffractometer
7371 independent reflections
Radiation source: fine-focus sealed tube5722 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
ϕ and ω scansθmax = 26.0°, θmin = 1.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1819
Tmin = 0.854, Tmax = 1.000k = 1213
22881 measured reflectionsl = 2526
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.080H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0336P)2 + 1.0988P]
where P = (Fo2 + 2Fc2)/3
7371 reflections(Δ/σ)max = 0.001
481 parametersΔρmax = 0.65 e Å3
0 restraintsΔρmin = 0.59 e Å3
Crystal data top
K2[Pd(NCS)4]·2[Pd(NCS)2(C8H6N4)]V = 3786.6 (3) Å3
Mr = 1178.38Z = 4
Monoclinic, P21/cMo Kα radiation
a = 15.9625 (7) ŵ = 2.12 mm1
b = 10.9700 (5) ÅT = 200 K
c = 21.6801 (9) Å0.28 × 0.24 × 0.18 mm
β = 94.104 (1)°
Data collection top
Bruker SMART 1000 CCD
diffractometer
7371 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
5722 reflections with I > 2σ(I)
Tmin = 0.854, Tmax = 1.000Rint = 0.030
22881 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.080H-atom parameters constrained
S = 1.08Δρmax = 0.65 e Å3
7371 reflectionsΔρmin = 0.59 e Å3
481 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pd10.482313 (18)0.51068 (2)0.188694 (12)0.03065 (9)
Pd20.014348 (18)0.00967 (2)0.182524 (12)0.02913 (8)
Pd30.50000.50000.00000.02538 (10)
Pd40.00001.00000.00000.02620 (10)
K10.42675 (5)0.96456 (8)0.08137 (4)0.0397 (2)
K20.09465 (6)0.52691 (8)0.07076 (4)0.0426 (2)
S10.59836 (7)0.62463 (10)0.21959 (5)0.0483 (3)
S20.39550 (7)0.62960 (10)0.24449 (5)0.0498 (3)
S30.13902 (6)0.40429 (9)0.28031 (5)0.0412 (2)
S40.05796 (7)0.17773 (10)0.21091 (5)0.0515 (3)
S50.41359 (6)0.64489 (9)0.04273 (5)0.0376 (2)
S60.61598 (6)0.62728 (9)0.01879 (5)0.0396 (2)
S70.11212 (6)1.12966 (9)0.02391 (5)0.0448 (3)
S80.09601 (6)0.84561 (9)0.01933 (5)0.0405 (2)
N10.55052 (17)0.3754 (2)0.14802 (12)0.0263 (6)
N20.53434 (18)0.1777 (3)0.10408 (12)0.0312 (7)
N30.36456 (18)0.1932 (3)0.11846 (13)0.0330 (7)
N40.38671 (18)0.3913 (3)0.16051 (12)0.0302 (7)
N50.5592 (2)0.8652 (3)0.18054 (17)0.0528 (9)
N60.3527 (2)0.8499 (4)0.18235 (19)0.0607 (11)
N70.06619 (17)0.1506 (3)0.15385 (12)0.0280 (6)
N80.02642 (18)0.3475 (3)0.11603 (13)0.0347 (7)
N90.13917 (19)0.2811 (3)0.12042 (14)0.0381 (8)
N100.09353 (18)0.0838 (3)0.15250 (13)0.0320 (7)
N110.17991 (19)0.5602 (3)0.17926 (16)0.0460 (9)
N120.0430 (3)0.3800 (4)0.1863 (2)0.0694 (12)
N130.2462 (2)0.5816 (3)0.00536 (17)0.0509 (9)
N140.5701 (2)0.8743 (3)0.02917 (15)0.0427 (8)
N150.0555 (2)1.3726 (3)0.03105 (16)0.0469 (9)
N160.2599 (2)0.9214 (3)0.02070 (17)0.0516 (9)
C10.6330 (2)0.3698 (4)0.14158 (16)0.0353 (9)
H10.66750.43680.15490.042*
C20.6693 (2)0.2698 (3)0.11627 (16)0.0355 (9)
H20.72800.26610.11180.043*
C30.6171 (2)0.1759 (4)0.09784 (16)0.0372 (9)
H30.64070.10620.07980.045*
C40.5048 (2)0.2778 (3)0.12903 (14)0.0268 (8)
C50.4131 (2)0.2861 (3)0.13633 (14)0.0272 (8)
C60.2825 (2)0.2081 (4)0.12340 (17)0.0402 (10)
H60.24580.14270.11170.048*
C70.2488 (2)0.3139 (4)0.14461 (18)0.0441 (10)
H70.18990.32430.14590.053*
C80.3038 (2)0.4030 (4)0.16362 (17)0.0398 (9)
H80.28250.47640.17970.048*
C90.5728 (2)0.7657 (4)0.19553 (18)0.0411 (10)
C100.3729 (2)0.7573 (4)0.20423 (18)0.0405 (10)
C110.1472 (2)0.1804 (3)0.15213 (16)0.0329 (8)
H110.18940.12260.16470.039*
C120.1702 (2)0.2942 (3)0.13225 (16)0.0370 (9)
H120.22770.31570.13070.044*
C130.1075 (2)0.3756 (3)0.11476 (17)0.0378 (9)
H130.12250.45460.10130.045*
C140.0094 (2)0.2372 (3)0.13530 (15)0.0293 (8)
C150.0802 (2)0.2000 (3)0.13587 (15)0.0309 (8)
C160.2179 (2)0.2413 (4)0.12183 (19)0.0487 (11)
H160.26240.29730.11260.058*
C170.2379 (3)0.1234 (4)0.1360 (2)0.0517 (11)
H170.29460.09690.13520.062*
C180.1730 (2)0.0461 (4)0.15129 (19)0.0445 (10)
H180.18460.03630.16130.053*
C190.1617 (2)0.4984 (3)0.22118 (18)0.0342 (9)
C200.0035 (3)0.2959 (4)0.19531 (18)0.0452 (10)
C210.3143 (2)0.6055 (3)0.02093 (17)0.0379 (9)
C220.5851 (2)0.7726 (4)0.02536 (16)0.0328 (8)
C230.0761 (2)1.2729 (4)0.02831 (17)0.0362 (9)
C240.1932 (2)0.8932 (3)0.00439 (17)0.0373 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.03478 (17)0.02747 (16)0.02909 (15)0.00023 (12)0.00199 (12)0.00338 (12)
Pd20.03272 (16)0.02533 (16)0.02903 (15)0.00017 (12)0.00016 (12)0.00167 (12)
Pd30.0290 (2)0.0225 (2)0.02406 (19)0.00083 (15)0.00188 (15)0.00014 (15)
Pd40.0283 (2)0.0216 (2)0.0280 (2)0.00027 (15)0.00313 (16)0.00051 (16)
K10.0359 (5)0.0320 (5)0.0517 (5)0.0038 (4)0.0055 (4)0.0031 (4)
K20.0389 (5)0.0381 (5)0.0512 (5)0.0072 (4)0.0072 (4)0.0074 (4)
S10.0455 (6)0.0389 (6)0.0580 (7)0.0035 (5)0.0140 (5)0.0123 (5)
S20.0631 (7)0.0439 (6)0.0430 (6)0.0079 (5)0.0090 (5)0.0079 (5)
S30.0449 (6)0.0334 (6)0.0442 (6)0.0121 (4)0.0041 (5)0.0023 (5)
S40.0507 (7)0.0383 (6)0.0668 (7)0.0042 (5)0.0134 (6)0.0161 (6)
S50.0363 (5)0.0318 (5)0.0449 (5)0.0030 (4)0.0035 (4)0.0079 (4)
S60.0338 (5)0.0279 (5)0.0558 (6)0.0010 (4)0.0051 (5)0.0041 (5)
S70.0336 (6)0.0276 (5)0.0713 (7)0.0023 (4)0.0106 (5)0.0040 (5)
S80.0338 (5)0.0302 (5)0.0568 (6)0.0030 (4)0.0014 (5)0.0082 (5)
N10.0283 (16)0.0246 (16)0.0259 (14)0.0013 (12)0.0002 (12)0.0035 (12)
N20.0306 (17)0.0335 (18)0.0294 (15)0.0005 (13)0.0008 (13)0.0028 (14)
N30.0296 (17)0.0369 (18)0.0322 (16)0.0059 (14)0.0009 (13)0.0015 (14)
N40.0325 (17)0.0305 (17)0.0273 (15)0.0023 (13)0.0005 (13)0.0041 (13)
N50.050 (2)0.047 (2)0.061 (2)0.0081 (19)0.0080 (18)0.003 (2)
N60.035 (2)0.054 (3)0.092 (3)0.0003 (18)0.0020 (19)0.028 (2)
N70.0288 (16)0.0247 (16)0.0302 (15)0.0014 (12)0.0001 (13)0.0008 (13)
N80.0339 (18)0.0308 (18)0.0386 (17)0.0005 (14)0.0028 (14)0.0057 (14)
N90.0316 (18)0.0382 (19)0.0435 (18)0.0095 (15)0.0049 (14)0.0035 (15)
N100.0316 (17)0.0307 (18)0.0333 (16)0.0012 (13)0.0003 (13)0.0021 (14)
N110.0307 (19)0.051 (2)0.055 (2)0.0003 (16)0.0048 (16)0.0065 (19)
N120.079 (3)0.041 (2)0.092 (3)0.017 (2)0.035 (2)0.011 (2)
N130.036 (2)0.046 (2)0.072 (2)0.0018 (17)0.0105 (18)0.0076 (19)
N140.046 (2)0.034 (2)0.0476 (19)0.0019 (16)0.0009 (16)0.0057 (16)
N150.049 (2)0.030 (2)0.061 (2)0.0015 (16)0.0027 (17)0.0088 (17)
N160.032 (2)0.045 (2)0.078 (3)0.0001 (16)0.0049 (18)0.001 (2)
C10.031 (2)0.040 (2)0.034 (2)0.0060 (17)0.0021 (16)0.0059 (17)
C20.030 (2)0.042 (2)0.034 (2)0.0014 (17)0.0050 (16)0.0010 (18)
C30.033 (2)0.042 (2)0.037 (2)0.0028 (18)0.0042 (17)0.0032 (18)
C40.0296 (19)0.030 (2)0.0202 (17)0.0024 (15)0.0009 (14)0.0026 (15)
C50.0303 (19)0.030 (2)0.0211 (17)0.0024 (16)0.0013 (14)0.0025 (15)
C60.031 (2)0.047 (3)0.042 (2)0.0082 (18)0.0003 (17)0.0030 (19)
C70.021 (2)0.053 (3)0.058 (3)0.0011 (18)0.0021 (18)0.006 (2)
C80.030 (2)0.042 (2)0.048 (2)0.0082 (18)0.0075 (18)0.005 (2)
C90.034 (2)0.050 (3)0.040 (2)0.0090 (19)0.0030 (17)0.014 (2)
C100.035 (2)0.046 (3)0.040 (2)0.0071 (19)0.0047 (18)0.013 (2)
C110.031 (2)0.031 (2)0.037 (2)0.0038 (16)0.0000 (16)0.0005 (17)
C120.035 (2)0.036 (2)0.039 (2)0.0056 (17)0.0010 (17)0.0055 (18)
C130.043 (2)0.027 (2)0.043 (2)0.0051 (17)0.0013 (18)0.0066 (18)
C140.031 (2)0.028 (2)0.0278 (18)0.0038 (16)0.0001 (15)0.0011 (16)
C150.033 (2)0.031 (2)0.0280 (19)0.0020 (16)0.0033 (15)0.0037 (16)
C160.032 (2)0.058 (3)0.055 (3)0.012 (2)0.0032 (19)0.008 (2)
C170.029 (2)0.054 (3)0.071 (3)0.002 (2)0.000 (2)0.009 (2)
C180.030 (2)0.044 (2)0.059 (3)0.0055 (18)0.0024 (19)0.002 (2)
C190.0235 (19)0.035 (2)0.044 (2)0.0031 (16)0.0012 (17)0.0090 (19)
C200.059 (3)0.039 (3)0.039 (2)0.017 (2)0.013 (2)0.001 (2)
C210.037 (2)0.034 (2)0.044 (2)0.0084 (18)0.0138 (19)0.0008 (19)
C220.034 (2)0.036 (2)0.0283 (19)0.0049 (17)0.0007 (16)0.0011 (17)
C230.038 (2)0.032 (2)0.037 (2)0.0063 (17)0.0045 (17)0.0057 (18)
C240.040 (2)0.031 (2)0.042 (2)0.0073 (18)0.0102 (18)0.0034 (18)
Geometric parameters (Å, º) top
Pd1—N12.074 (3)N3—C51.321 (4)
Pd1—N42.070 (3)N3—C61.331 (4)
Pd1—S12.2945 (11)N3—K1vi2.835 (3)
Pd1—S22.3077 (11)N4—C81.336 (4)
Pd2—N72.059 (3)N4—C51.348 (4)
Pd2—N102.069 (3)N5—C91.155 (5)
Pd2—S3i2.2958 (10)N6—C101.158 (5)
Pd2—S42.2829 (11)N7—C111.337 (4)
Pd3—S5ii2.3388 (9)N7—C141.354 (4)
Pd3—S52.3388 (9)N8—C141.315 (4)
Pd3—S6ii2.3314 (9)N8—C131.333 (4)
Pd3—S62.3314 (9)N9—C151.321 (4)
Pd4—S7iii2.3157 (10)N9—C161.333 (5)
Pd4—S72.3157 (10)N10—C181.333 (5)
Pd4—S8iii2.3419 (10)N10—C151.346 (4)
Pd4—S82.3419 (10)N11—C191.154 (5)
K1—N142.806 (3)N12—C201.142 (5)
K1—N3iv2.835 (3)N12—K2vi3.370 (5)
K1—N62.853 (4)N13—C211.146 (5)
K1—N2iv2.922 (3)N14—C221.145 (5)
K1—N162.923 (4)N14—K1v2.981 (3)
K1—N14v2.981 (3)N15—C231.144 (5)
K1—N53.103 (4)N15—K2iii2.827 (4)
K1—S53.6081 (13)N15—K2iv2.886 (4)
K1—K1v4.4389 (17)N16—C241.141 (5)
K2—N112.824 (4)C1—C21.373 (5)
K2—N15iii2.827 (4)C1—H10.9500
K2—N82.881 (3)C2—C31.366 (5)
K2—N15vi2.886 (4)C2—H20.9500
K2—N132.892 (4)C3—H30.9500
K2—N93.008 (3)C4—C51.486 (5)
K2—N12iv3.370 (5)C6—C71.373 (5)
K2—S83.6692 (13)C6—H60.9500
K2—K2vii4.4966 (18)C7—C81.358 (5)
S1—C91.674 (5)C7—H70.9500
S2—C101.676 (5)C8—H80.9500
S3—C191.666 (4)C11—C121.379 (5)
S3—Pd2viii2.2958 (10)C11—H110.9500
S4—C201.675 (5)C12—C131.375 (5)
S5—C211.677 (4)C12—H120.9500
S6—C221.678 (4)C13—H130.9500
S7—C231.679 (4)C14—C151.487 (5)
S8—C241.683 (4)C16—C171.372 (6)
N1—C11.336 (4)C16—H160.9500
N1—C41.344 (4)C17—C181.361 (6)
N2—C41.325 (4)C17—H170.9500
N2—C31.338 (4)C18—H180.9500
N2—K1vi2.922 (3)
N4—Pd1—N179.65 (11)C10—S2—Pd1108.31 (14)
N4—Pd1—S1173.55 (8)C19—S3—Pd2viii98.67 (13)
N1—Pd1—S194.39 (8)C20—S4—Pd2104.84 (14)
N4—Pd1—S293.13 (8)C21—S5—Pd3106.57 (13)
N1—Pd1—S2168.65 (8)C21—S5—K1110.74 (13)
S1—Pd1—S292.38 (4)Pd3—S5—K1136.58 (4)
N7—Pd2—N1079.94 (11)C22—S6—Pd3110.44 (13)
N7—Pd2—S4173.34 (8)C23—S7—Pd4108.97 (13)
N10—Pd2—S493.40 (9)C24—S8—Pd4108.78 (13)
N7—Pd2—S3i95.74 (8)C24—S8—K2111.96 (13)
N10—Pd2—S3i174.43 (8)Pd4—S8—K2138.91 (4)
S4—Pd2—S3i90.90 (4)C1—N1—C4116.7 (3)
S6ii—Pd3—S6180.00 (5)C1—N1—Pd1128.9 (2)
S6ii—Pd3—S5ii90.42 (3)C4—N1—Pd1114.2 (2)
S6—Pd3—S5ii89.58 (3)C4—N2—C3115.8 (3)
S6ii—Pd3—S589.58 (3)C4—N2—K1vi120.7 (2)
S6—Pd3—S590.42 (3)C3—N2—K1vi123.0 (2)
S5ii—Pd3—S5180.00 (6)C5—N3—C6116.2 (3)
S7iii—Pd4—S7180.00 (6)C5—N3—K1vi123.7 (2)
S7iii—Pd4—S8iii88.80 (3)C6—N3—K1vi119.8 (2)
S7—Pd4—S8iii91.20 (3)C8—N4—C5116.1 (3)
S7iii—Pd4—S891.20 (3)C8—N4—Pd1129.5 (3)
S7—Pd4—S888.80 (4)C5—N4—Pd1114.3 (2)
S8iii—Pd4—S8180.00 (5)C9—N5—K1129.2 (3)
N14—K1—N3iv137.64 (9)C10—N6—K1125.6 (3)
N14—K1—N6123.28 (11)C11—N7—C14116.7 (3)
N3iv—K1—N689.98 (10)C11—N7—Pd2128.9 (2)
N14—K1—N2iv82.17 (9)C14—N7—Pd2114.4 (2)
N3iv—K1—N2iv57.16 (8)C14—N8—C13116.3 (3)
N6—K1—N2iv119.60 (10)C14—N8—K2126.0 (2)
N14—K1—N16120.30 (10)C13—N8—K2117.6 (2)
N3iv—K1—N1686.83 (9)C15—N9—C16115.5 (3)
N6—K1—N1681.96 (10)C15—N9—K2120.8 (2)
N2iv—K1—N16135.31 (10)C16—N9—K2123.3 (3)
N14—K1—N14v79.86 (10)C18—N10—C15117.2 (3)
N3iv—K1—N14v74.32 (9)C18—N10—Pd2128.5 (3)
N6—K1—N14v155.48 (10)C15—N10—Pd2114.2 (2)
N2iv—K1—N14v67.52 (8)C19—N11—K2118.1 (3)
N16—K1—N14v78.53 (10)C20—N12—K2vi91.9 (3)
N14—K1—N567.69 (10)C21—N13—K2162.4 (3)
N3iv—K1—N5110.45 (9)C22—N14—K1123.6 (3)
N6—K1—N567.21 (10)C22—N14—K1v120.3 (3)
N2iv—K1—N578.54 (9)K1—N14—K1v100.14 (10)
N16—K1—N5143.95 (10)C23—N15—K2iii129.9 (3)
N14v—K1—N5135.69 (9)C23—N15—K2iv116.2 (3)
N14—K1—S566.36 (7)K2iii—N15—K2iv103.82 (11)
N3iv—K1—S5155.51 (7)C24—N16—K1169.6 (3)
N6—K1—S574.30 (9)N1—C1—C2121.7 (3)
N2iv—K1—S5147.20 (7)N1—C1—H1119.2
N16—K1—S572.67 (7)C2—C1—H1119.2
N14v—K1—S5113.18 (7)C3—C2—C1117.0 (3)
N5—K1—S581.08 (7)C3—C2—H2121.5
N14—K1—K1v41.39 (7)C1—C2—H2121.5
N3iv—K1—K1v106.59 (7)N2—C3—C2123.0 (4)
N6—K1—K1v163.30 (9)N2—C3—H3118.5
N2iv—K1—K1v69.94 (6)C2—C3—H3118.5
N16—K1—K1v100.68 (8)N2—C4—N1125.7 (3)
N14v—K1—K1v38.47 (7)N2—C4—C5118.4 (3)
N5—K1—K1v103.93 (7)N1—C4—C5115.8 (3)
S5—K1—K1v90.63 (3)N3—C5—N4125.5 (3)
N11—K2—N15iii132.28 (10)N3—C5—C4118.9 (3)
N11—K2—N898.97 (9)N4—C5—C4115.6 (3)
N15iii—K2—N878.92 (9)N3—C6—C7122.8 (4)
N11—K2—N15vi148.93 (10)N3—C6—H6118.6
N15iii—K2—N15vi76.18 (11)C7—C6—H6118.6
N8—K2—N15vi71.51 (9)C8—C7—C6116.7 (4)
N11—K2—N1390.88 (10)C8—C7—H7121.6
N15iii—K2—N13115.96 (10)C6—C7—H7121.6
N8—K2—N13148.14 (10)N4—C8—C7122.5 (4)
N15vi—K2—N1384.46 (10)N4—C8—H8118.8
N11—K2—N971.18 (9)C7—C8—H8118.8
N15iii—K2—N9133.30 (9)N5—C9—S1176.3 (4)
N8—K2—N955.62 (8)N6—C10—S2172.0 (4)
N15vi—K2—N979.48 (9)N7—C11—C12120.6 (3)
N13—K2—N9100.43 (9)N7—C11—H11119.7
N11—K2—N12iv70.69 (9)C12—C11—H11119.7
N15iii—K2—N12iv65.57 (10)C13—C12—C11118.0 (3)
N8—K2—N12iv64.42 (10)C13—C12—H12121.0
N15vi—K2—N12iv125.51 (10)C11—C12—H12121.0
N13—K2—N12iv146.66 (11)N8—C13—C12122.2 (3)
N9—K2—N12iv99.44 (9)N8—C13—H13118.9
N11—K2—C1916.81 (8)C12—C13—H13118.9
N15iii—K2—C19129.62 (9)N8—C14—N7126.1 (3)
N8—K2—C1982.22 (9)N8—C14—C15118.4 (3)
N15vi—K2—C19138.92 (9)N7—C14—C15115.4 (3)
N13—K2—C19104.47 (9)N9—C15—N10125.6 (3)
N9—K2—C1959.54 (8)N9—C15—C14118.8 (3)
N12iv—K2—C1964.12 (9)N10—C15—C14115.6 (3)
N11—K2—S897.90 (8)N9—C16—C17123.2 (4)
N15iii—K2—S861.49 (7)N9—C16—H16118.4
N8—K2—S8138.05 (7)C17—C16—H16118.4
N15vi—K2—S8108.87 (7)C18—C17—C16117.2 (4)
N13—K2—S869.04 (7)C18—C17—H17121.4
N9—K2—S8165.17 (7)C16—C17—H17121.4
N12iv—K2—S885.78 (7)N10—C18—C17121.2 (4)
C19—K2—S8111.77 (7)N10—C18—H18119.4
N11—K2—K2vii166.57 (8)C17—C18—H18119.4
N15iii—K2—K2vii38.55 (7)N11—C19—S3177.2 (4)
N8—K2—K2vii71.07 (6)N11—C19—K245.1 (2)
N15vi—K2—K2vii37.63 (7)S3—C19—K2134.80 (17)
N13—K2—K2vii102.31 (8)N12—C20—S4176.7 (4)
N9—K2—K2vii108.30 (7)N13—C21—S5178.1 (4)
N12iv—K2—K2vii96.47 (7)N14—C22—S6174.8 (4)
C19—K2—K2vii152.22 (7)N15—C23—S7176.6 (4)
S8—K2—K2vii84.69 (3)N16—C24—S8177.7 (4)
C9—S1—Pd1103.83 (14)
N1—Pd1—S1—C9130.92 (16)S4—Pd2—N10—C15173.9 (2)
S2—Pd1—S1—C958.20 (15)N15iii—K2—N11—C1988.3 (3)
N4—Pd1—S2—C10104.11 (16)N8—K2—N11—C195.2 (3)
N1—Pd1—S2—C10154.2 (4)N15vi—K2—N11—C1963.7 (4)
S1—Pd1—S2—C1079.23 (14)N13—K2—N11—C19144.4 (3)
N10—Pd2—S4—C20145.08 (17)N9—K2—N11—C1943.7 (3)
S3i—Pd2—S4—C2038.46 (16)N12iv—K2—N11—C1964.0 (3)
S6ii—Pd3—S5—C2115.44 (14)S8—K2—N11—C19146.6 (3)
S6—Pd3—S5—C21164.56 (14)K2vii—K2—N11—C1946.4 (6)
S6ii—Pd3—S5—K1163.85 (6)N11—K2—N13—C211.9 (10)
S6—Pd3—S5—K116.15 (6)N15iii—K2—N13—C21141.0 (10)
N14—K1—S5—C21147.04 (16)N8—K2—N13—C21106.8 (10)
N3iv—K1—S5—C2122.9 (2)N15vi—K2—N13—C21147.3 (10)
N6—K1—S5—C2174.78 (16)N9—K2—N13—C2169.1 (10)
N2iv—K1—S5—C21164.47 (17)N12iv—K2—N13—C2156.5 (11)
N16—K1—S5—C2111.52 (16)C19—K2—N13—C218.1 (11)
N14v—K1—S5—C2180.41 (16)S8—K2—N13—C21100.0 (10)
N5—K1—S5—C21143.48 (16)K2vii—K2—N13—C21179.3 (10)
K1v—K1—S5—C21112.52 (14)N3iv—K1—N14—C22170.0 (3)
N14—K1—S5—Pd30.49 (9)N6—K1—N14—C2234.0 (4)
N3iv—K1—S5—Pd3170.47 (15)N2iv—K1—N14—C22154.4 (3)
N6—K1—S5—Pd3137.68 (9)N16—K1—N14—C2267.0 (4)
N2iv—K1—S5—Pd316.93 (14)N14v—K1—N14—C22137.2 (4)
N16—K1—S5—Pd3136.02 (9)N5—K1—N14—C2273.6 (3)
N14v—K1—S5—Pd367.13 (9)S5—K1—N14—C2216.2 (3)
N5—K1—S5—Pd368.98 (9)K1v—K1—N14—C22137.2 (4)
K1v—K1—S5—Pd335.02 (6)N3iv—K1—N14—K1v52.87 (16)
S5ii—Pd3—S6—C22157.74 (14)N6—K1—N14—K1v171.15 (11)
S5—Pd3—S6—C2222.26 (14)N2iv—K1—N14—K1v68.44 (9)
S8—Pd4—S7—C23168.18 (15)N16—K1—N14—K1v70.22 (13)
S7iii—Pd4—S8—C24170.46 (14)N14v—K1—N14—K1v0.0
S7—Pd4—S8—C249.54 (14)N5—K1—N14—K1v149.21 (12)
S7iii—Pd4—S8—K21.77 (7)S5—K1—N14—K1v120.99 (9)
S7—Pd4—S8—K2178.23 (7)N14—K1—N16—C24110.1 (18)
N11—K2—S8—C2469.23 (16)N3iv—K1—N16—C24104.3 (18)
N15iii—K2—S8—C24156.54 (17)N6—K1—N16—C2413.9 (18)
N8—K2—S8—C24177.82 (17)N2iv—K1—N16—C24138.4 (17)
N15vi—K2—S8—C2494.77 (16)N5—K1—N16—C2416.9 (19)
N13—K2—S8—C2418.67 (16)S5—K1—N16—C2462.1 (18)
N9—K2—S8—C2427.7 (3)K1v—K1—N16—C24149.4 (18)
N12iv—K2—S8—C24139.05 (16)C4—N1—C1—C20.6 (5)
C19—K2—S8—C2479.09 (16)Pd1—N1—C1—C2176.4 (2)
K2vii—K2—S8—C24124.04 (14)N1—C1—C2—C30.0 (5)
N11—K2—S8—Pd4118.71 (9)C4—N2—C3—C20.6 (5)
N15iii—K2—S8—Pd415.52 (10)K1vi—N2—C3—C2170.9 (3)
N8—K2—S8—Pd45.76 (13)C1—C2—C3—N20.7 (5)
N15vi—K2—S8—Pd477.29 (10)C3—N2—C4—N10.1 (5)
N13—K2—S8—Pd4153.39 (10)K1vi—N2—C4—N1171.9 (2)
N9—K2—S8—Pd4160.2 (2)C3—N2—C4—C5179.1 (3)
N12iv—K2—S8—Pd448.89 (9)K1vi—N2—C4—C59.1 (4)
C19—K2—S8—Pd4108.84 (9)C1—N1—C4—N20.7 (5)
K2vii—K2—S8—Pd448.03 (7)Pd1—N1—C4—N2177.1 (3)
N4—Pd1—N1—C1179.1 (3)C1—N1—C4—C5179.7 (3)
S1—Pd1—N1—C13.3 (3)Pd1—N1—C4—C53.9 (4)
S2—Pd1—N1—C1129.7 (4)C6—N3—C5—N42.2 (5)
N4—Pd1—N1—C45.0 (2)K1vi—N3—C5—N4172.4 (2)
S1—Pd1—N1—C4172.5 (2)C6—N3—C5—C4176.9 (3)
S2—Pd1—N1—C446.1 (5)K1vi—N3—C5—C48.5 (4)
N1—Pd1—N4—C8175.6 (3)C8—N4—C5—N33.3 (5)
S2—Pd1—N4—C813.3 (3)Pd1—N4—C5—N3175.9 (3)
N1—Pd1—N4—C55.4 (2)C8—N4—C5—C4175.9 (3)
S2—Pd1—N4—C5165.8 (2)Pd1—N4—C5—C45.0 (3)
N14—K1—N5—C980.2 (4)N2—C4—C5—N30.8 (5)
N3iv—K1—N5—C9145.5 (4)N1—C4—C5—N3179.9 (3)
N6—K1—N5—C964.5 (4)N2—C4—C5—N4178.4 (3)
N2iv—K1—N5—C9166.3 (4)N1—C4—C5—N40.7 (4)
N16—K1—N5—C931.1 (5)C5—N3—C6—C71.2 (5)
N14v—K1—N5—C9126.3 (4)K1vi—N3—C6—C7176.0 (3)
S5—K1—N5—C912.2 (4)N3—C6—C7—C83.1 (6)
K1v—K1—N5—C9100.6 (4)C5—N4—C8—C71.0 (5)
N14—K1—N6—C106.0 (4)Pd1—N4—C8—C7178.0 (3)
N3iv—K1—N6—C10158.1 (4)C6—C7—C8—N41.9 (6)
N2iv—K1—N6—C10106.7 (4)C14—N7—C11—C120.0 (5)
N16—K1—N6—C10115.1 (4)Pd2—N7—C11—C12178.9 (3)
N14v—K1—N6—C10152.6 (3)N7—C11—C12—C130.4 (5)
N5—K1—N6—C1045.8 (4)C14—N8—C13—C120.3 (5)
S5—K1—N6—C1041.0 (4)K2—N8—C13—C12176.5 (3)
K1v—K1—N6—C1014.7 (6)C11—C12—C13—N80.6 (6)
N10—Pd2—N7—C11176.4 (3)C13—N8—C14—N70.1 (5)
S3i—Pd2—N7—C117.2 (3)K2—N8—C14—N7176.7 (2)
N10—Pd2—N7—C144.7 (2)C13—N8—C14—C15178.3 (3)
S3i—Pd2—N7—C14171.7 (2)K2—N8—C14—C151.7 (4)
N11—K2—N8—C1463.2 (3)C11—N7—C14—N80.3 (5)
N15iii—K2—N8—C14165.3 (3)Pd2—N7—C14—N8178.8 (3)
N15vi—K2—N8—C1486.3 (3)C11—N7—C14—C15178.2 (3)
N13—K2—N8—C1443.3 (4)Pd2—N7—C14—C152.8 (4)
N9—K2—N8—C143.4 (3)C16—N9—C15—N100.1 (5)
N12iv—K2—N8—C14126.6 (3)K2—N9—C15—N10172.9 (2)
C19—K2—N8—C1461.7 (3)C16—N9—C15—C14179.8 (3)
S8—K2—N8—C14175.7 (2)K2—N9—C15—C147.1 (4)
K2vii—K2—N8—C14126.1 (3)C18—N10—C15—N92.4 (5)
N11—K2—N8—C13120.3 (3)Pd2—N10—C15—N9173.7 (3)
N15iii—K2—N8—C1311.2 (3)C18—N10—C15—C14177.6 (3)
N15vi—K2—N8—C1390.2 (3)Pd2—N10—C15—C146.4 (4)
N13—K2—N8—C13133.2 (3)N8—C14—C15—N93.8 (5)
N9—K2—N8—C13180.0 (3)N7—C14—C15—N9177.7 (3)
N12iv—K2—N8—C1356.8 (3)N8—C14—C15—N10176.1 (3)
C19—K2—N8—C13121.8 (3)N7—C14—C15—N102.4 (4)
S8—K2—N8—C137.7 (3)C15—N9—C16—C172.3 (6)
K2vii—K2—N8—C1350.4 (2)K2—N9—C16—C17170.3 (3)
N11—K2—N9—C15121.0 (3)N9—C16—C17—C182.3 (7)
N15iii—K2—N9—C1510.0 (3)C15—N10—C18—C172.3 (6)
N8—K2—N9—C155.3 (2)Pd2—N10—C18—C17173.1 (3)
N15vi—K2—N9—C1569.4 (3)C16—C17—C18—N100.1 (6)
N13—K2—N9—C15151.7 (3)Pd2viii—S3—C19—K279.2 (2)
N12iv—K2—N9—C1555.2 (3)N15iii—K2—C19—N11106.2 (3)
C19—K2—N9—C15107.6 (3)N8—K2—C19—N11174.8 (3)
S8—K2—N9—C15164.9 (2)N15vi—K2—C19—N11135.2 (3)
K2vii—K2—N9—C1544.9 (3)N13—K2—C19—N1136.9 (3)
N11—K2—N9—C1666.8 (3)N9—K2—C19—N11130.7 (3)
N15iii—K2—N9—C16162.2 (3)N12iv—K2—C19—N11109.5 (3)
N8—K2—N9—C16177.5 (3)S8—K2—C19—N1135.9 (3)
N15vi—K2—N9—C16102.8 (3)K2vii—K2—C19—N11158.9 (3)
N13—K2—N9—C1620.5 (3)N11—K2—C19—S3176.0 (5)
N12iv—K2—N9—C16132.6 (3)N15iii—K2—C19—S377.8 (3)
C19—K2—N9—C1680.2 (3)N8—K2—C19—S39.2 (2)
S8—K2—N9—C1622.9 (5)N15vi—K2—C19—S340.8 (3)
K2vii—K2—N9—C16127.3 (3)N13—K2—C19—S3139.1 (2)
N7—Pd2—N10—C18178.4 (3)N9—K2—C19—S345.3 (2)
S4—Pd2—N10—C181.6 (3)N12iv—K2—C19—S374.5 (2)
N7—Pd2—N10—C156.1 (2)S8—K2—C19—S3148.1 (2)
Symmetry codes: (i) x, y1/2, z1/2; (ii) x+1, y+1, z; (iii) x, y+2, z; (iv) x, y+1, z; (v) x+1, y+2, z; (vi) x, y1, z; (vii) x, y+1, z; (viii) x, y+1/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1···S10.952.773.334 (4)119
C1—H1···N11ii0.952.453.134 (5)128
C6—H6···S7vi0.952.763.457 (4)131
C8—H8···S20.952.773.321 (4)118
C11—H11···S3i0.952.823.371 (4)118
C11—H11···N6vii0.952.633.315 (5)130
C13—H13···N15iii0.952.613.376 (5)138
C16—H16···S6ii0.952.833.640 (4)144
C18—H18···S40.952.713.276 (4)119
Symmetry codes: (i) x, y1/2, z1/2; (ii) x+1, y+1, z; (iii) x, y+2, z; (vi) x, y1, z; (vii) x, y+1, z.

Experimental details

Crystal data
Chemical formulaK2[Pd(NCS)4]·2[Pd(NCS)2(C8H6N4)]
Mr1178.38
Crystal system, space groupMonoclinic, P21/c
Temperature (K)200
a, b, c (Å)15.9625 (7), 10.9700 (5), 21.6801 (9)
β (°) 94.104 (1)
V3)3786.6 (3)
Z4
Radiation typeMo Kα
µ (mm1)2.12
Crystal size (mm)0.28 × 0.24 × 0.18
Data collection
DiffractometerBruker SMART 1000 CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2000)
Tmin, Tmax0.854, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
22881, 7371, 5722
Rint0.030
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.080, 1.08
No. of reflections7371
No. of parameters481
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.65, 0.59

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997).

Selected bond lengths (Å) top
Pd1—N12.074 (3)Pd2—S3i2.2958 (10)
Pd1—N42.070 (3)Pd2—S42.2829 (11)
Pd1—S12.2945 (11)Pd3—S52.3388 (9)
Pd1—S22.3077 (11)Pd3—S62.3314 (9)
Pd2—N72.059 (3)Pd4—S72.3157 (10)
Pd2—N102.069 (3)Pd4—S82.3419 (10)
Symmetry code: (i) x, y1/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1···S10.952.773.334 (4)119
C1—H1···N11ii0.952.453.134 (5)128
C6—H6···S7iii0.952.763.457 (4)131
C8—H8···S20.952.773.321 (4)118
C11—H11···S3i0.952.823.371 (4)118
C11—H11···N6iv0.952.633.315 (5)130
C13—H13···N15v0.952.613.376 (5)138
C16—H16···S6ii0.952.833.640 (4)144
C18—H18···S40.952.713.276 (4)119
Symmetry codes: (i) x, y1/2, z1/2; (ii) x+1, y+1, z; (iii) x, y1, z; (iv) x, y+1, z; (v) x, y+2, z.
 

Acknowledgements

This work was supported by the Priority Research Centers Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Education, Science and Technology (2011–0030747).

References

First citationBruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationFarrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  CrossRef IUCr Journals Google Scholar
First citationHa, K. (2010). Z. Kristallogr. New Cryst. Struct. 225, 619–620.  CAS Google Scholar
First citationMawby, A. & Pringle, G. E. (1972). J. Inorg. Nucl. Chem. 34, 2213–2217.  CrossRef CAS Web of Science Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar

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Volume 68| Part 5| May 2012| Pages m616-m617
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