Z. Kristallogr. NCS 2016; 231(1): 333–334
Open Access
Kwang Ha*
Crystal structure of trans-dibromidodi(pyridineκN)palladium(II), PdBr2(C5H5N)2
Table 1: Data collection and handling.
Br1
C5
C4
Crystal:
Pd1
C3
N1
C1
C2
DOI 10.1515/ncrs-2015-0204
Received September 3, 2015; accepted January 18, 2016; available
online February 8, 2016
Abstract
C10 H10 Br2 N2 Pd, triclinic, P1̄ (no. 2), a = 5.6549(3) Å, b =
7.0210(3) Å, c = 7.7723(4) Å, α = 80.031(3)°, β = 84.601(2)°,
γ = 89.222(2)°, V = 302.58(3) Å3 , Z = 1, Rgt (F) = 0.0309,
wRref (F 2 ) = 0.0841, T = 223(2) K.
CCDC no.: 1447960
The crystal structure is shown in the figure. Tables 1–3 contain
details of the measurement method and a list of the atoms
including atomic coordinates and displacement parameters.
Source of material
To an orange suspension of dibromido(1,5-cyclooctadiene)
palladium(II) (0.1802 g, 0.481 mmol) in acetone (30 mL) was
added pyridine (py; 0.2161 g, 2.732 mmol) and stirred for
3 h at room temperature. After evaporation of the solvent,
the residue was washed with ether, and dried at 50 °C, to
give a yellow powder (0.1862 g). Crystals suitable for X-ray
diffraction analysis were obtained by slow evaporation from
a CH3 CN solution.
Experimental details
Hydrogen atoms were positioned geometrically and allowed
to ride on their parent atoms with d(C—H) = 0.94 Å and
U iso (H) = 1.2U eq (C). The highest peak (0.99 e Å−3 ) and the
*Corresponding author: Kwang Ha, Chonnam National
University, School of Applied Chemical Engineering, Research
Institute of Catalysis, Gwangju 500–757, Republic of Korea,
e-mail: [email protected]
Wavelength:
µ:
Diffractometer, scan mode:
2θmax :
N(hkl)measured , N(hkl)unique :
N(param)refined :
Programs:
Yellow, block,
size 0.08×0.12×0.18 mm
Mo K α radiation (0.71073 Å)
81.04 cm−1
PHOTON 100 CMOS, φ and ω
scans
56.88°
11965, 1523
70
SHELX [6], WinGX [7], PLATON [8]
Table 2: Atomic coordinates and isotropic displacement parameters
(Å2 ).
Atom
Site
H(1)
H(2)
H(3)
H(4)
H(5)
2i
2i
2i
2i
2i
x
y
z
Uiso
0.9545
1.2373
1.1793
0.8388
0.5674
0.2839
0.1370
0.1223
0.2607
0.4102
0.5378
0.3704
0.0799
−0.0368
0.1381
0.033
0.037
0.042
0.044
0.037
deepest hole (−1.26 e Å−3 ) in the difference Fourier map
are located 0.87 Å and 0.87 Å from the atoms Br1 and Pd1,
respectively.
Discussion
The crystal structures of the related trans-dipyridine-Pd(II)
complexes [PdX2 (py)2 ] (X = Cl, I) have been determined previously [1–5]. The chlorido complex [PdCl2 (py)2 ] has three polymorphic forms: it crystallized in three space groups C2/c [1],
P1̄ [2] and P21 /n [3], whereas the iodido complex [PdI2 (py)2 ]
has two polymorphs with the space groups C2/m [4, 5] and
C2/c [5]. In the title complex [PdBr2 (py)2 ], the central Pd(II)
ion has a trans-Br2 N2 square-planar coordination defined by
two N atoms from two distinct pyridine ligands and two Br−
anions. The complex crystallizes in the triclinic space group
P1̄ and the asymmetric unit contains one half of the complex:
the Pd atom is located on an inversion center, and therefore
the PdBr2 N2 moiety is exactly planar and two pyridine rings
are parallel. The dihedral angle between the PdBr2 N2 unit
© 2016 Kwang Ha, published by De Gruyter.
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334 | Ha: PdBr2 (C5 H5 N)2
Table 3: Atomic coordinates and displacement parameters (Å2 ).
Atom
Site
Pd(1)
Br(1)
N(1)
C(1)
C(2)
C(3)
C(4)
C(5)
1h
2i
2i
2i
2i
2i
2i
2i
x
y
z
U11
U22
U33
U12
U13
U23
0.5
0.55852(7)
0.7368(5)
0.9324(7)
1.1009(7)
1.0669(8)
0.8657(8)
0.7042(8)
0.5
0.79493(5)
0.3628(4)
0.2805(6)
0.1914(6)
0.1831(6)
0.2652(6)
0.3541(6)
0.5
0.28409(5)
0.3527(4)
0.4200(5)
0.3212(6)
0.1491(6)
0.0799(6)
0.1852(6)
0.0214(2)
0.0374(3)
0.025(2)
0.026(2)
0.024(2)
0.037(2)
0.049(3)
0.035(2)
0.0239(2)
0.0290(2)
0.025(2)
0.030(2)
0.030(2)
0.030(2)
0.032(2)
0.029(2)
0.0196(2)
0.0283(3)
0.022(2)
0.027(2)
0.039(2)
0.036(2)
0.029(2)
0.029(2)
0.0052(2)
0.0061(2)
0.003(1)
0.003(2)
0.005(2)
0.003(2)
−0.003(2)
0.003(2)
0.0003(2)
0.0037(2)
0.002(1)
−0.002(2)
0.001(2)
0.009(2)
0.003(2)
−0.004(2)
−0.0022(2)
0.0023(2)
−0.003(1)
−0.006(2)
−0.008(2)
−0.011(2)
−0.009(2)
−0.002(2)
plane and the nearly planar pyridine ring (maximum deviation = 0.006(3) Å) is 57.8(1)°. The complexes are stacked in
columns along [010] with d(Pd· · · Pd) = 7.0210(3) Å (length of
b axis).
Acknowledgements: This work was supported by Priority
Research Centers Program through the National Research
Foundation of Korea (NRF) funded by the Ministry of Education, Science and Technology (2009–0094055). The author
thanks the KBSI, Seoul Center, for the X-ray data collection.
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