Bis(azido-κN)(di-2-pyridyl­amine-κ2N2,N2′)palladium(II)

Ha, K.

doi:10.1107/S1600536812013074

Volume 68
Part 4
Page m519
April 2012

Received 23 March 2012
Accepted 25 March 2012
Online 31 March 2012

Key indicators
Single-crystal X-ray study
T = 200 K
Mean (C-C) = 0.005 Å
R = 0.029
wR = 0.073
Data-to-parameter ratio = 12.8
Details

Bis(azido-N)(di-2-pyridylamine-²N²,N^2')palladium(II)

Kwang Ha ^a ^*

^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

In the title complex, [Pd(N₃)₂(C₁₀H₉N₃)], the Pd^II ion is in a slightly distorted square-planar coordination environment. The ligator atoms comprise the two pyridine N atoms of the chelating di-2-pyridylamine (dpa) ligand and two N atoms from two azide anions. The dpa ligand coordinates the Pd atom in a boat conformation, the dihedral angle between the pyridine rings being 24.4 (1)°. The pyridine rings are somewhat inclined to the least-squares plane of the PdN₄ unit, making dihedral angles of 29.02 (9) and 26.47 (9)°. The azide ligands are slightly bent, with N-N-N angles of 173.0 (4) and 174.2 (4)°. In the crystal, molecules are connected by N-HN and C-HN hydrogen bonds, forming chains along the c axis. When viewed down the b axis, successive chains are stacked in opposite directions. Intramolecular C-HN hydrogen bonds are also observed.

Related literature

For the crystal structures of the related Pd^II complexes [PdX₂(dpa)] (X = Cl or Br), see: Rauterkus et al. (2003); Yao et al. (2003).

Experimental

Crystal data

[Pd(N₃)₂(C₁₀H₉N₃)]
M_r = 361.66
Monoclinic, C 2/c
a = 17.5552 (15) Å
b = 6.9773 (6) Å
c = 19.6654 (17) Å
= 99.206 (2)°
V = 2377.7 (4) Å³
Z = 8
Mo K radiation
= 1.57 mm^-1
T = 200 K
0.20 × 0.14 × 0.09 mm

Data collection

Bruker SMART 1000 CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2000) T_min = 0.901, T_max = 1.000
7041 measured reflections
2322 independent reflections
1751 reflections with I > 2(I)
R_int = 0.029

Refinement

R[F² > 2(F²)] = 0.029
wR(F²) = 0.073
S = 1.06
2322 reflections
181 parameters
H-atom parameters constrained
_max = 0.71 e Å^-3
_min = -0.41 e Å^-3

Table 1
Selected bond lengths (Å)

Pd1-N4	2.001 (3)
Pd1-N7	2.018 (3)
Pd1-N1	2.040 (3)
Pd1-N3	2.046 (3)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N2-H2NN9ⁱ	0.92	2.31	3.208 (4)	165
C1-H1N4	0.95	2.35	2.816 (5)	110
C4-H4N6ⁱ	0.95	2.40	3.175 (5)	138
C10-H10N7	0.95	2.35	2.861 (5)	113
Symmetry code: (i) $[x, -y+1, z-{\script{1\over 2}}]$ .

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.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: FJ2539 ).

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

Bruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Rauterkus, M. J., Fakih, S., Mock, C., Puscasu, I. & Krebs, B. (2003). Inorg. Chim. Acta, 350, 355-365.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Spek, A. L. (2009). Acta Cryst. D65, 148-155.
Yao, W.-R., Liu, Z.-H. & Zhang, Q.-F. (2003). Acta Cryst. C59, m139-m140.