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Volume 69 
Part 9 
Pages m520-m521  
September 2013  

Received 17 July 2013
Accepted 12 August 2013
Online 23 August 2013

Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.005 Å
R = 0.038
wR = 0.097
Data-to-parameter ratio = 18.0
Details
Open access

Dichlorido[6,8,22,24,34,36-hexamethyl-33,35-diaza-3,11,19,27-tetraazoniapentacyclo[27.3.1.15,9.113,17.121,25]hexatriaconta-1(33),5,7,9(34),13,15,17(35),21,23,25(36),29,31-dodecaene-[kappa]6N3,N11,N19,N27,N33,N35]dipalladium(II) bis(perchlorate) N,N-dimethylformamide disolvate methanol disolvate

aDepartment of Frontier Materials, Graduate School of Engineering, Nagoya Institute of Technology, Gokiso-cho, Showa-ku, Nagoya 466-8555, Japan,bDepartment of Chemistry, Graduate School of Science, Osaka University, Machikaneyama-cho, Toyonaka, Osaka 560-0043, Japan, and cPRESTO, Japan Science and Technology Agency (JST), Japan
Correspondence e-mail: masuda.hideki@nitech.ac.jp

In the crystal structure of the title compound, [Pd2(C36H42N6)Cl2](ClO4)2·2C3H7NO·2CH3OH, the dinuclear PdII complex cation lies on an inversion center. Each PdII ion has a distorted square-planar coordination sphere, defined by three N atoms of the macrocyclic ligand and a chloride ion. The PdII complex cations and the methanol molecules are linked through N-H...O and O-H...O hydrogen bonds, forming a zigzag chain along [101]. An intramolecular N-H...Cl hydrogen bond is also observed.

Related literature

For palladium(II) complexes with 2,6-bis(aminomethyl)pyridine, see: Arnáiz et al. (2002[Arnáiz, A., Cuevas, J. V., Herbosa, G. G., Carbayo, A., Casares, J. A. & Puebla, E. G. (2002). J. Chem. Soc. Dalton Trans. pp. 2581-2586.]). For dipalladium(II) complexes having a PdII-Cl unit, see: Suess & Peters (2010[Suess, D. L. M. & Peters, J. C. (2010). Chem. Commun. 46, 6554-6556.]); Goforth et al. (2013[Goforth, S. K., Walroth, R. C. & White, L. M. E. (2013). Inorg. Chem. 52, 5692-5701.]). For palladium(II) complexes containing a macrocyclic ligand, see: Parker (1985[Parker, D. (1985). J. Chem. Soc. Chem. Commun. pp. 1129-1131.]); Parker et al. (1985[Parker, D., Lehn, J. M. & Rimmer, J. (1985). J. Chem. Soc. Dalton Trans. pp. 1517-1521.]). For a similar macrocyclic ligand, see: Allmendinger et al. (2003[Allmendinger, M., Zell, P., Amin, A., Thewalt, U., Klinga, M. & Rieger, B. (2003). Heterocycles, 60, 1065-1081.]). For a similar cryptand ligand, see: Higa et al. (2010[Higa, T., Fukui, M., Fukui, K., Naganuma, Y., Kajita, Y., Inomata, T., Ozawa, T., Funahashi, Y. & Masuda, H. (2010). J. Inclusion Phenom. Macrocycl. Chem. 66, 171-177.]).

[Scheme 1]

Experimental

Crystal data
  • [Pd2(C36H42N6)Cl2](ClO4)2·2C3H7NO·2CH4O

  • Mr = 1255.68

  • Monoclinic, P 21 /n

  • a = 10.917 (2) Å

  • b = 19.083 (4) Å

  • c = 12.705 (3) Å

  • [beta] = 104.201 (2)°

  • V = 2566.0 (8) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.98 mm-1

  • T = 173 K

  • 0.20 × 0.20 × 0.20 mm

Data collection
  • Rigaku Mercury70 diffractometer

  • Absorption correction: numerical (NUMABS; Rigaku, 1999[Rigaku (1999). NUMABS. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.751, Tmax = 0.823

  • 19797 measured reflections

  • 5826 independent reflections

  • 4980 reflections with F2 > 2[sigma](F2)

  • Rint = 0.029

Refinement
  • R[F2 > 2[sigma](F2)] = 0.038

  • wR(F2) = 0.097

  • S = 1.08

  • 5826 reflections

  • 324 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.80 e Å-3

  • [Delta][rho]min = -0.81 e Å-3

Table 1
Selected bond lengths (Å)

Pd1-Cl1 2.3084 (9)
Pd1-N1 2.062 (3)
Pd1-N2 1.942 (3)
Pd1-N3 2.087 (3)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
O6-H18...O6i 0.84 2.33 2.757 (5) 112
N1-H12...O6 0.78 (4) 2.21 (4) 2.930 (5) 153 (4)
N3-H13...Cl1ii 0.71 (4) 2.67 (5) 3.332 (4) 156 (4)
Symmetry codes: (i) -x+2, -y+1, -z+1; (ii) -x+1, -y+1, -z.

Data collection: CrystalClear (Rigaku, 2001[Rigaku (2001). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SIR92 (Altomare et al., 1993[Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343-350.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: CrystalStructure (Rigaku, 2001[Rigaku (2001). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.]); software used to prepare material for publication: CrystalStructure.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IS5294 ).


Acknowledgements

This work was partially supported by Grants-in-Aid (No. 22550060 to YF and No. 22350028 to HM) for Scientific Research from the Ministry of Education, Science, Sports and Culture, Japan.

References

Allmendinger, M., Zell, P., Amin, A., Thewalt, U., Klinga, M. & Rieger, B. (2003). Heterocycles, 60, 1065-1081.  [ChemPort]
Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343-350.  [CrossRef] [ISI] [details]
Arnáiz, A., Cuevas, J. V., Herbosa, G. G., Carbayo, A., Casares, J. A. & Puebla, E. G. (2002). J. Chem. Soc. Dalton Trans. pp. 2581-2586.
Goforth, S. K., Walroth, R. C. & White, L. M. E. (2013). Inorg. Chem. 52, 5692-5701.  [ISI] [CrossRef] [ChemPort] [PubMed]
Higa, T., Fukui, M., Fukui, K., Naganuma, Y., Kajita, Y., Inomata, T., Ozawa, T., Funahashi, Y. & Masuda, H. (2010). J. Inclusion Phenom. Macrocycl. Chem. 66, 171-177.  [CSD] [CrossRef] [ChemPort]
Parker, D. (1985). J. Chem. Soc. Chem. Commun. pp. 1129-1131.  [CrossRef] [ISI]
Parker, D., Lehn, J. M. & Rimmer, J. (1985). J. Chem. Soc. Dalton Trans. pp. 1517-1521.  [CrossRef]
Rigaku (1999). NUMABS. Rigaku Corporation, Tokyo, Japan.
Rigaku (2001). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]
Suess, D. L. M. & Peters, J. C. (2010). Chem. Commun. 46, 6554-6556.  [CSD] [CrossRef] [ChemPort]


Acta Cryst (2013). E69, m520-m521   [ doi:10.1107/S1600536813022666 ]

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