Literature DB >> 22346825

(2,3-Di-2-pyridyl-pyrazine-κN,N)bis-(thio-cyanato-κS)palladium(II).

Kwang Ha1.   

Abstract

The Pd(II) ion in the title complex, [Pd(NCS)(2)(C(14)H(10)N(4))], is four-coordinated in a distorted square-planar environment by the two pyridine N atoms of the chelating 2,3-di-2-pyridyl-pyrazine (dpp) ligand and two S atoms from two thio-cyanate anions. The pyridine rings are considerably inclined to the least-squares plane of the PdS(2)N(2) unit [maximum deviation = 0.027 (1) Å], making dihedral angles of 70.3 (2) and 69.2 (1)°. The pyrazine ring is almost perpendicular to the PdS(2)N(2) plane, with a dihedral angle of 86.3 (1)°. The thio-cyanate ligands are located on opposite sides of the PdS(2)N(2) unit plane and are almost linear [N-C-S angles = 177.8 (6) and 178.9 (6)°]. The complex mol-ecules are stacked in columns along the b axis and are connected by inter-molecular C-H⋯N hydrogen bonds, forming chains along the a axis.

Entities:  

Year:  2012        PMID： 22346825      PMCID： PMC3274878          DOI： 10.1107/S1600536812000980

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For related crystal structures of [PdX 2(dpp)] (X = Cl, Br or I), see: Ha (2011a ▶,b ▶,c ▶). For related Pt and Pd complexes, see: Granifo et al. (2000 ▶); Cai et al. (2009 ▶).

Experimental

Crystal data

[Pd(NCS)2(C14H10N4)] M = 456.82 Monoclinic, a = 15.8236 (11) Å b = 13.5901 (9) Å c = 7.9189 (6) Å β = 102.960 (1)° V = 1659.5 (2) Å3 Z = 4 Mo Kα radiation μ = 1.38 mm−1 T = 200 K 0.27 × 0.25 × 0.13 mm

Data collection

Bruker SMART 1000 CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.835, T max = 1.000 10174 measured reflections 3247 independent reflections 2248 reflections with I > 2σ(I) R int = 0.071

Refinement

R[F 2 > 2σ(F 2)] = 0.046 wR(F 2) = 0.100 S = 1.00 3247 reflections 226 parameters H-atom parameters constrained Δρmax = 0.89 e Å−3 Δρmin = −0.66 e Å−3 Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶) and PLATON (Spek, 2009 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablock(s) global. DOI: 10.1107/S1600536812000980/bt5782sup1.cif Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Pd(NCS)2(C14H10N4)]F(000) = 904
Mr = 456.82Dx = 1.828 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2951 reflections
a = 15.8236 (11) Åθ = 2.6–25.6°
b = 13.5901 (9) ŵ = 1.38 mm−1
c = 7.9189 (6) ÅT = 200 K
β = 102.960 (1)°Plate, yellow
V = 1659.5 (2) Å30.27 × 0.25 × 0.13 mm
Z = 4
Bruker SMART 1000 CCD diffractometer3247 independent reflections
Radiation source: fine-focus sealed tube2248 reflections with I > 2σ(I)
graphiteRint = 0.071
φ and ω scansθmax = 26.0°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2000)h = −19→19
Tmin = 0.835, Tmax = 1.000k = −16→14
10174 measured reflectionsl = −9→9
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.100H-atom parameters constrained
S = 1.00w = 1/[σ2(Fo2) + (0.0351P)2] where P = (Fo2 + 2Fc2)/3
3247 reflections(Δ/σ)max < 0.001
226 parametersΔρmax = 0.89 e Å−3
0 restraintsΔρmin = −0.66 e Å−3
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.
xyzUiso*/Ueq
Pd10.19166 (3)0.47138 (3)0.53401 (6)0.02445 (15)
S10.11316 (10)0.43246 (12)0.2597 (2)0.0379 (4)
S20.23273 (12)0.30866 (11)0.5347 (2)0.0455 (5)
N10.3412 (3)0.7055 (3)0.3986 (6)0.0299 (12)
N20.4466 (3)0.5833 (3)0.6359 (6)0.0298 (11)
N30.1593 (3)0.6182 (3)0.5309 (5)0.0229 (10)
N40.2666 (3)0.4960 (3)0.7755 (6)0.0236 (11)
N5−0.0358 (3)0.5536 (4)0.2015 (7)0.0434 (14)
N60.3992 (4)0.3047 (4)0.7615 (8)0.0519 (16)
C10.3097 (3)0.6576 (4)0.5210 (7)0.0237 (13)
C20.3637 (3)0.5968 (4)0.6413 (7)0.0249 (13)
C30.4761 (4)0.6298 (4)0.5124 (8)0.0330 (15)
H30.53500.62150.50630.040*
C40.4231 (4)0.6892 (4)0.3940 (8)0.0317 (14)
H40.44590.71970.30580.038*
C50.2195 (3)0.6873 (4)0.5241 (7)0.0230 (13)
C60.1985 (4)0.7861 (4)0.5149 (8)0.0323 (14)
H60.24100.83380.50510.039*
C70.1161 (4)0.8153 (4)0.5200 (8)0.0328 (15)
H70.10130.88320.51380.039*
C80.0551 (4)0.7456 (4)0.5339 (8)0.0331 (14)
H8−0.00200.76450.53990.040*
C90.0785 (4)0.6479 (4)0.5391 (7)0.0256 (13)
H90.03650.59950.54870.031*
C100.3414 (3)0.5479 (3)0.7954 (7)0.0218 (12)
C110.3978 (4)0.5543 (4)0.9550 (7)0.0298 (14)
H110.44940.59210.96810.036*
C120.3797 (4)0.5061 (4)1.0957 (8)0.0308 (14)
H120.41900.50861.20560.037*
C130.3029 (4)0.4541 (4)1.0736 (8)0.0323 (14)
H130.28840.42061.16840.039*
C140.2480 (4)0.4517 (4)0.9131 (8)0.0292 (14)
H140.19470.41710.89920.035*
C150.0257 (4)0.5056 (4)0.2271 (8)0.0326 (14)
C160.3312 (5)0.3072 (4)0.6693 (9)0.0371 (16)
U11U22U33U12U13U23
Pd10.0243 (3)0.0191 (2)0.0282 (3)0.00066 (18)0.00218 (18)−0.00024 (19)
S10.0347 (10)0.0434 (10)0.0325 (10)−0.0005 (7)0.0006 (8)−0.0074 (7)
S20.0538 (12)0.0205 (8)0.0555 (12)0.0066 (7)−0.0018 (9)−0.0058 (7)
N10.029 (3)0.028 (3)0.034 (3)0.002 (2)0.009 (2)0.004 (2)
N20.026 (3)0.028 (3)0.036 (3)0.003 (2)0.008 (2)0.002 (2)
N30.027 (3)0.022 (2)0.020 (3)−0.0008 (19)0.005 (2)0.0022 (19)
N40.022 (3)0.022 (2)0.027 (3)0.0048 (18)0.006 (2)0.0001 (19)
N50.028 (3)0.052 (4)0.046 (4)0.001 (3)−0.002 (3)0.004 (3)
N60.039 (4)0.052 (4)0.065 (5)0.016 (3)0.013 (3)0.009 (3)
C10.021 (3)0.019 (3)0.029 (3)−0.004 (2)0.002 (3)−0.007 (2)
C20.025 (3)0.020 (3)0.027 (3)−0.002 (2)0.000 (3)−0.004 (2)
C30.029 (4)0.032 (3)0.042 (4)0.003 (3)0.014 (3)−0.004 (3)
C40.033 (4)0.024 (3)0.040 (4)−0.003 (3)0.011 (3)−0.002 (3)
C50.024 (3)0.025 (3)0.017 (3)0.001 (2)−0.001 (3)0.001 (2)
C60.033 (4)0.028 (3)0.032 (4)0.000 (3)0.000 (3)0.000 (3)
C70.043 (4)0.019 (3)0.037 (4)0.009 (3)0.010 (3)0.002 (3)
C80.026 (3)0.034 (3)0.037 (4)0.009 (3)0.003 (3)−0.001 (3)
C90.029 (3)0.028 (3)0.019 (3)−0.004 (2)0.004 (3)0.001 (2)
C100.016 (3)0.018 (3)0.029 (3)0.005 (2)0.001 (2)0.001 (2)
C110.027 (3)0.027 (3)0.034 (4)0.006 (2)0.004 (3)−0.002 (3)
C120.029 (4)0.026 (3)0.032 (4)0.011 (3)−0.004 (3)−0.001 (3)
C130.043 (4)0.025 (3)0.029 (4)0.014 (3)0.008 (3)0.008 (3)
C140.023 (3)0.029 (3)0.037 (4)0.003 (2)0.010 (3)0.002 (3)
C150.034 (4)0.041 (4)0.021 (3)−0.014 (3)0.002 (3)0.003 (3)
C160.047 (4)0.021 (3)0.049 (5)0.006 (3)0.022 (4)0.006 (3)
Pd1—N32.059 (4)C3—C41.372 (8)
Pd1—N42.039 (5)C3—H30.9500
Pd1—S12.3090 (17)C4—H40.9500
Pd1—S22.3045 (15)C5—C61.382 (7)
S1—C151.677 (7)C6—C71.371 (7)
S2—C161.679 (7)C6—H60.9500
N1—C41.324 (7)C7—C81.374 (8)
N1—C11.352 (7)C7—H70.9500
N2—C31.333 (7)C8—C91.377 (7)
N2—C21.336 (6)C8—H80.9500
N3—C51.347 (6)C9—H90.9500
N3—C91.356 (6)C10—C111.378 (7)
N4—C141.334 (7)C11—C121.377 (8)
N4—C101.356 (6)C11—H110.9500
N5—C151.151 (7)C12—C131.383 (8)
N6—C161.157 (8)C12—H120.9500
C1—C21.398 (7)C13—C141.369 (8)
C1—C51.488 (7)C13—H130.9500
C2—C101.499 (7)C14—H140.9500
N4—Pd1—N386.73 (16)C6—C5—C1118.9 (5)
N4—Pd1—S292.92 (12)C7—C6—C5120.0 (5)
N3—Pd1—S2177.82 (13)C7—C6—H6120.0
N4—Pd1—S1175.50 (12)C5—C6—H6120.0
N3—Pd1—S197.51 (13)C6—C7—C8119.4 (5)
S2—Pd1—S182.78 (6)C6—C7—H7120.3
C15—S1—Pd1105.1 (2)C8—C7—H7120.3
C16—S2—Pd1103.5 (2)C7—C8—C9118.6 (5)
C4—N1—C1117.4 (5)C7—C8—H8120.7
C3—N2—C2117.8 (5)C9—C8—H8120.7
C5—N3—C9118.5 (4)N3—C9—C8122.4 (5)
C5—N3—Pd1120.0 (4)N3—C9—H9118.8
C9—N3—Pd1121.5 (3)C8—C9—H9118.8
C14—N4—C10119.1 (5)N4—C10—C11120.6 (5)
C14—N4—Pd1120.2 (4)N4—C10—C2119.7 (5)
C10—N4—Pd1120.2 (4)C11—C10—C2119.8 (5)
N1—C1—C2120.4 (5)C12—C11—C10120.2 (5)
N1—C1—C5113.0 (5)C12—C11—H11119.9
C2—C1—C5126.2 (5)C10—C11—H11119.9
N2—C2—C1120.9 (5)C11—C12—C13118.5 (6)
N2—C2—C10112.2 (5)C11—C12—H12120.8
C1—C2—C10126.7 (5)C13—C12—H12120.8
N2—C3—C4121.3 (5)C14—C13—C12119.1 (5)
N2—C3—H3119.4C14—C13—H13120.4
C4—C3—H3119.4C12—C13—H13120.4
N1—C4—C3122.1 (5)N4—C14—C13122.4 (5)
N1—C4—H4118.9N4—C14—H14118.8
C3—C4—H4118.9C13—C14—H14118.8
N3—C5—C6121.0 (5)N5—C15—S1177.8 (6)
N3—C5—C1120.1 (5)N6—C16—S2178.9 (6)
N3—Pd1—S1—C15−32.7 (2)N1—C1—C5—N3133.2 (5)
S2—Pd1—S1—C15149.5 (2)C2—C1—C5—N3−54.5 (8)
N4—Pd1—S2—C16−26.8 (3)N1—C1—C5—C6−44.9 (7)
S1—Pd1—S2—C16151.9 (2)C2—C1—C5—C6127.3 (6)
N4—Pd1—N3—C568.5 (4)N3—C5—C6—C72.8 (8)
S1—Pd1—N3—C5−110.0 (4)C1—C5—C6—C7−179.1 (5)
N4—Pd1—N3—C9−110.1 (4)C5—C6—C7—C8−0.1 (9)
S1—Pd1—N3—C971.4 (4)C6—C7—C8—C9−1.2 (9)
N3—Pd1—N4—C14115.9 (4)C5—N3—C9—C82.6 (8)
S2—Pd1—N4—C14−66.3 (4)Pd1—N3—C9—C8−178.8 (4)
N3—Pd1—N4—C10−72.1 (4)C7—C8—C9—N30.0 (8)
S2—Pd1—N4—C10105.8 (4)C14—N4—C10—C110.4 (7)
C4—N1—C1—C22.5 (8)Pd1—N4—C10—C11−171.7 (4)
C4—N1—C1—C5175.3 (5)C14—N4—C10—C2179.1 (4)
C3—N2—C2—C10.0 (8)Pd1—N4—C10—C27.0 (6)
C3—N2—C2—C10−174.9 (5)N2—C2—C10—N4−135.8 (5)
N1—C1—C2—N2−1.2 (8)C1—C2—C10—N449.7 (7)
C5—C1—C2—N2−173.0 (5)N2—C2—C10—C1142.9 (6)
N1—C1—C2—C10172.9 (5)C1—C2—C10—C11−131.6 (6)
C5—C1—C2—C101.2 (9)N4—C10—C11—C121.5 (7)
C2—N2—C3—C4−0.3 (8)C2—C10—C11—C12−177.2 (5)
C1—N1—C4—C3−2.8 (8)C10—C11—C12—C13−1.9 (8)
N2—C3—C4—N11.7 (9)C11—C12—C13—C140.5 (8)
C9—N3—C5—C6−4.0 (8)C10—N4—C14—C13−1.9 (7)
Pd1—N3—C5—C6177.4 (4)Pd1—N4—C14—C13170.2 (4)
C9—N3—C5—C1177.9 (5)C12—C13—C14—N41.4 (8)
Pd1—N3—C5—C1−0.7 (7)
D—H···AD—HH···AD···AD—H···A
C12—H12···N2i0.952.543.306 (7)138
C14—H14···N5ii0.952.493.277 (8)140
Pd1—N32.059 (4)
Pd1—N42.039 (5)
Pd1—S12.3090 (17)
Pd1—S22.3045 (15)
N4—Pd1—N386.73 (16)
S2—Pd1—S182.78 (6)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C12—H12⋯N2i0.952.543.306 (7)138
C14—H14⋯N5ii0.952.493.277 (8)140

Symmetry codes: (i) ; (ii) .

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