Abstract
C10H10Br2N2Pd, triclinic, P1̅ (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(F2) = 0.0841, T = 223(2) K.
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.
Data collection and handling.
| Crystal: | Yellow, block, size 0.08×0.12×0.18 mm |
| Wavelength: | Mo Kα radiation (0.71073 Å) |
| μ: | 81.04 cm−1 |
| Diffractometer, scan mode: | PHOTON 100 CMOS, φ and ω scans |
| 2θmax: | 56.88° |
| N(hkl)measured, N(hkl)unique: | 11965, 1523 |
| N(param)refined: | 70 |
| Programs: | SHELX [6], WinGX [7], PLATON [8] |
Atomic coordinates and isotropic displacement parameters (Å2).
| Atom | Site | x | y | z | Uiso |
|---|---|---|---|---|---|
| H(1) | 2i | 0.9545 | 0.2839 | 0.5378 | 0.033 |
| H(2) | 2i | 1.2373 | 0.1370 | 0.3704 | 0.037 |
| H(3) | 2i | 1.1793 | 0.1223 | 0.0799 | 0.042 |
| H(4) | 2i | 0.8388 | 0.2607 | −0.0368 | 0.044 |
| H(5) | 2i | 0.5674 | 0.4102 | 0.1381 | 0.037 |
Atomic coordinates and displacement parameters (Å2).
| Atom | Site | x | y | z | U11 | U22 | U33 | U12 | U13 | U23 |
|---|---|---|---|---|---|---|---|---|---|---|
| Pd(1) | 1h | 0.5 | 0.5 | 0.5 | 0.0214(2) | 0.0239(2) | 0.0196(2) | 0.0052(2) | 0.0003(2) | −0.0022(2) |
| Br(1) | 2i | 0.55852(7) | 0.79493(5) | 0.28409(5) | 0.0374(3) | 0.0290(2) | 0.0283(3) | 0.0061(2) | 0.0037(2) | 0.0023(2) |
| N(1) | 2i | 0.7368(5) | 0.3628(4) | 0.3527(4) | 0.025(2) | 0.025(2) | 0.022(2) | 0.003(1) | 0.002(1) | −0.003(1) |
| C(1) | 2i | 0.9324(7) | 0.2805(6) | 0.4200(5) | 0.026(2) | 0.030(2) | 0.027(2) | 0.003(2) | −0.002(2) | −0.006(2) |
| C(2) | 2i | 1.1009(7) | 0.1914(6) | 0.3212(6) | 0.024(2) | 0.030(2) | 0.039(2) | 0.005(2) | 0.001(2) | −0.008(2) |
| C(3) | 2i | 1.0669(8) | 0.1831(6) | 0.1491(6) | 0.037(2) | 0.030(2) | 0.036(2) | 0.003(2) | 0.009(2) | −0.011(2) |
| C(4) | 2i | 0.8657(8) | 0.2652(6) | 0.0799(6) | 0.049(3) | 0.032(2) | 0.029(2) | −0.003(2) | 0.003(2) | −0.009(2) |
| C(5) | 2i | 0.7042(8) | 0.3541(6) | 0.1852(6) | 0.035(2) | 0.029(2) | 0.029(2) | 0.003(2) | −0.004(2) | −0.002(2) |
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 CH3CN solution.
Experimental details
Hydrogen atoms were positioned geometrically and allowed to ride on their parent atoms with d(C—H) = 0.94 Å and Uiso(H) = 1.2Ueq(C). The highest peak (0.99 e Å−3) and the 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], P1̅ [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-Br2N2 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 P1̅ and the asymmetric unit contains one half of the complex: the Pd atom is located on an inversion center, and therefore the PdBr2N2 moiety is exactly planar and two pyridine rings are parallel. The dihedral angle between the PdBr2N2 unit 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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©2016 Kwang Ha, published by De Gruyter.
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