Home Crystal structure of cyclo-[tetrachlorido-bis(μ2-p-xylylenediamine-κ2N:N′)dipalladium(II)] dimethyl sulfoxide solvate, C20H36Cl4N4O2Pd2S2
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Crystal structure of cyclo-[tetrachlorido-bis(μ2-p-xylylenediamine-κ2N:N′)dipalladium(II)] dimethyl sulfoxide solvate, C20H36Cl4N4O2Pd2S2

  • Kwang Ha ORCID logo EMAIL logo
Published/Copyright: January 29, 2020

Abstract

C20H36Cl4N4O2Pd2S2, tetragonal, I41cd (no. 110), a = 17.3126(19) Å, c = 19.725(2) Å, V = 5912.1(14) Å3, Z = 8, Rgt(F) = 0.0284, wRref(F2) = 0.0536, T = 223(2) K.

CCDC no.: 1976493

Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Yellow block
Size:0.13 × 0.10 × 0.05 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.74 mm−1
Diffractometer, scan mode:PHOTON 100 CMOS, φ and ω
θmax, completeness:28.3°, >99%
N(hkl)measured, N(hkl)unique, Rint:92873, 3644, 0.096
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3037
N(param)refined:156
Programs:Bruker [1], SHELX [2], ORTEP-3 [3], Platon [4]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
Pd10.14995(2)0.34518(2)0.22290(5)0.02295(8)
Cl10.24240(9)0.43944(9)0.23687(7)0.0438(4)
Cl20.06969(10)0.24040(9)0.21084(7)0.0502(5)
N10.1408(3)0.3376(3)0.3256(3)0.0272(14)
H1A0.16110.29210.33850.033*
H1B0.17030.37510.34390.033*
N20.1579(3)0.3496(3)0.1197(4)0.0282(15)
H2A0.20390.32960.10780.034*
H2B0.12130.31820.10260.034*
C10.0625(3)0.3438(3)0.3558(3)0.0321(14)
H1C0.06440.32570.40290.038*
H1D0.02720.30990.33090.038*
C20.0311(3)0.4246(3)0.3547(3)0.0252(12)
C30.0157(3)0.4628(3)0.4143(2)0.0334(12)
H30.02650.43840.45590.040*
C40.0148(3)0.4633(3)0.2940(2)0.0280(11)
H40.02420.43840.25250.034*
C50.1502(3)0.4254(3)0.0858(3)0.0328(13)
H5A0.15960.41870.03720.039*
H5B0.19000.46030.10350.039*
C60.0724(3)0.4623(3)0.0955(3)0.0268(12)
C70.0040(3)0.4204(3)0.0967(3)0.0313(11)
H70.00590.36620.09720.038*
C80.0672(3)0.5425(3)0.0971(3)0.0310(11)
H80.11270.57210.09850.037*
S10.25896(8)0.13619(7)0.31097(7)0.0367(3)
O10.2463(3)0.21404(17)0.3429(3)0.0403(8)
C90.3248(4)0.0893(4)0.3655(3)0.0575(18)
H9A0.36720.12390.37590.086*
H9B0.34460.04330.34340.086*
H9C0.29860.07480.40710.086*
C100.3231(5)0.1524(4)0.2421(3)0.077(2)
H10A0.29780.18430.20830.115*
H10B0.33750.10330.22200.115*
H10C0.36910.17860.25840.115*

Source of material

To a solution of Na2PdCl4 (0.2943 g; 1.000 mmol) in MeOH (30 mL) was added p-xylylenediamine (0.1402 g, 1.029 mmol) and stirred for 3 h at room temperature. The formed precipitate was separated by filtration, washed with H2O and acetone, and dried at 50 °C, to give a yellow powder (0.2875 g). Crystals suitable for X-ray diffraction analysis were obtained by slow evaporation from a dimethyl sulfoxide (DMSO) solution at 90 °C.

Experimental details

Hydrogen atoms were positioned geometrically and allowed to ride on their parent atoms with d(N—H) = 0.90 Å, d(C—H) = 0.98, 0.94 or 0.97 Å and Uiso(H) = 1.2Ueq(N,C) or 1.5Ueq(methyl C) with the help of the SHELXL program (AFIX 23, 43 or 137 options) [2]. The highest peak (0.43 e Å−3) and the deepest hole (−0.30 e Å−3) in the difference Fourier map are located 0.55 Å and 1.39 Å from the atoms C2 and C8, respectively.

Comment

The crystal structures of the related p-xylylenediamine-bridged complexes [M(μ3-SO4)(μ2-pxd)]n (M = Zn, Cd; pxd = p-xylylenediamine) [5] and [Zn23-S)22-pxd)]n [6] have been determined previously by X-ray powder diffraction techniques. Furthermore there is a single crystal structure determination of a Cd(II) complex [7].

The title complex has a cyclic dinuclear structure, in which two trans-chlorido-Pd(II) units [PdCl2] are linked by two pxd ligands. In the crystal, the benzene rings are positioned exactly perpendicular to each other. The complex is disposed about a twofold rotation axis running in the [001] direction passing through the centroid of one benzene ring, and bisecting the other benzene ring; the asymmetric unit contains one half of the compound (see the figure, the asymmetric unit is labelled). In the complex, each Pd(II) ion is four-coordinated in a slightly distorted square-planar environment by two Cl ligands and two mutually trans-positioned N atoms derived from two bridging bidentate pxd ligands. The Pd—Cl and Pd—N bond lengths are almost equal with d(Pd—Cl) = 2.2974(15) and 2.3023(14) Å, and d(Pd—N) = 2.037(7) and 2.042(7) Å), respectively. In the crystal structure, the complexes and solvent DMSO molecules are linked by N—H⋯O, N—H⋯Cl, C—H⋯Cl and C—H⋯O hydrogen bonds with distances of 2.834(6)–3.558(7) Å between the donor and acceptor atoms, forming a three-dimensional network [4].

Funding source: Ministry of Education

Award Identifier / Grant number: 2018R1D1A1B07050550

Funding statement: This research was supported by Basic Science Research Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Education (grant number: 2018R1D1A1B07050550). The author thanks the KBSI, Seoul Center, for the X-ray data collection.

References

1. Bruker. APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, WI, USA (2016).Search in Google Scholar

2. Sheldrick, G. M.: Crystal structure refinement with SHELXL. Acta Crystallogr. C71 (2015) 3–8.10.1107/S2053229614024218Search in Google Scholar PubMed PubMed Central

3. Farrugia, L. J.: ORTEP-3 for Windows − a version of ORTEP-III with a graphical user interface (GUI). J. Appl. Crystallogr. 30 (1997) 565.10.1107/S0021889897003117Search in Google Scholar

4. Spek, A. L.: Single-crystal structure validation with the program PLATON. J. Appl. Crystallogr. 36 (2003) 7–13.10.1107/S0021889802022112Search in Google Scholar

5. Luberda-Durnaś, K.; Mucha, D.; Sanz-Camacho, P.; Łasocha, W.: Synthesis and Characterization of Pillared Metal Sulfates (Diamine)MeSO4, (Me = Zn, Cd). Z. Anorg. Allg. Chem. 639 (2013) 2195–2201.10.1002/zaac.201300171Search in Google Scholar

6. Luberda-Durnaś, K.; González Guillén, A.; Łasocha, W.: Synthesis optimisation and characterisation of the organic-inorganic layered materials ZnS(m-xylylenediamine)1/2 and ZnS(m-xylylenediamine)1/2. J. Solid State Chem. 238 (2016) 162–169.10.1016/j.jssc.2016.03.022Search in Google Scholar

7. Yuge, H.; Noda, Y.; Iwamoto, T.: Variations in catenation behavior in aromatic guest clathrates containing rigid host entities p-xylylenediamine (p-xda) and tetracyanonickelate(II) linking octahedral cadmium(II) in [Cd(p-xda)nNi(CN)4] host (n = 1, 1.5, or 2) and the related complex [Cd(C6H5NH2)2(p-xda)Ni(CN)4]. Inorg. Chem. 35 (1996) 1842–1848.10.1021/ic950382nSearch in Google Scholar

Received: 2019-11-27
Accepted: 2020-01-10
Published Online: 2020-01-29
Published in Print: 2020-04-28

©2020 Kwang Ha, published by De Gruyter.

This work is licensed under the Creative Commons Attribution 4.0 Public License.

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  79. Crystal structure of 3-(1-benzyl-2-ethyl-4-nitro-1H-imidazol-5-ylthio)-propanoic acid, C15H17N3O4S
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