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Volume 68 
Part 12 
Pages m1557-m1558  
December 2012  

Received 3 November 2012
Accepted 22 November 2012
Online 30 November 2012

Key indicators
Single-crystal X-ray study
T = 180 K
Mean [sigma](C-C) = 0.003 Å
R = 0.027
wR = 0.071
Data-to-parameter ratio = 19.3
Details
Open access

Di-[mu]-azido-bis([mu]-1,4,7,10,13,16-hexaoxacyclooctadecane)bis(5,10,15,20-tetraphenylporphyrinato)dicadmiumdisodium

aLaboratoire de Physico-chimie des Matériaux, Université de Monastir, Faculté des Sciences de Monastir, Avenue de l'environnement, 5019 Monastir, Tunisia, and bLaboratoire de Chimie de Coordination CNRS UPR 8241, 205 Route de Norbone, 31077 Toulouse Cedex 04, France
Correspondence e-mail: hnasri1@gmail.com

The asymmetric unit of the title compound, [Cd2Na2(N3)2(C44H28N4)2(C12H24O6)2], consists of one half of the dimeric complex; the tetranuclear molecule lies about an inversion centre. The CdII atom is coordinated by the four pyrrole N atoms of the 5,10,15,20-tetraphenylporphyrinate ligand and one N atom of the axial azide ligand in a square-pyramidal geometry. The azide group is also linked to the NaI atom, which is surrounded by one 18-crown-6 molecule and additionally bonded to a second 18-crown-6 molecule trans to the azide group. The porphyrin core exhibits a major doming distortion (~40%) and the crystal structure is stabilized by weak C-H...[pi] interactions. The molecular structure features weak intramolecular hydrogen bonds: two O-H...O interactions within the 18-crown-6 molecule and one C-H(18-crown-6)...N(azido) contact.

Related literature

For the synthesis of [Cd(TPP)] (TPP = 5,10,15,20-tetraphenylporphyrinato), see: Rodesiler et al. (1985[Rodesiler, P. F., Griffith, E. A. H., Charles, N. G., Lebioda, L. & Amma, E. L. (1985). Inorg. Chem. 24, 4595-4600.]). For related structures, see: Byrn et al. (1991[Byrn, M. P., Curtis, C. J., Goldberg, I., Hsiou, Y., Khan, S. I., Sawin, P. A., Tendick, S. K. & Strouse, C. E. (1991). J. Am. Chem. Soc. 113, 6549-6557.]); Mansour et al. (2010[Mansour, A., Belkhiria, M. S., Daran, J.-C. & Nasri, H. (2010). Acta Cryst. E66, m509-m510.]); Liu et al. (2009[Liu, J.-J., He, X., Shao, M. & Li, M.-X. (2009). Inorg. Chem. Commun. 12, 972-974.]). For further details of geometric distortions in related compounds, see: Jentzen et al. (1997[Jentzen, W., Song, X. & Shelnutt, J. A. (1997). J. Phys. Chem. B, 101, 1684-1699.]).

[Scheme 1]

Experimental

Crystal data
  • [Cd2Na2(N3)2(C44H28N4)2(C12H24O6)2]

  • Mr = 2108.90

  • Monoclinic, P 21 /n

  • a = 11.4175 (3) Å

  • b = 19.5363 (4) Å

  • c = 22.6086 (6) Å

  • [beta] = 102.683 (2)°

  • V = 4919.9 (2) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 0.51 mm-1

  • T = 180 K

  • 0.48 × 0.42 × 0.28 mm

Data collection
  • Oxford Diffraction Xcalibur (Sapphire1) diffractometer

  • Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2009[Oxford Diffraction (2009). CrystAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]) Tmin = 0.791, Tmax = 0.870

  • 44385 measured reflections

  • 12338 independent reflections

  • 9493 reflections with I > 2[sigma](I)

  • Rint = 0.030

Refinement
  • R[F2 > 2[sigma](F2)] = 0.027

  • wR(F2) = 0.071

  • S = 1.02

  • 12338 reflections

  • 640 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.54 e Å-3

  • [Delta][rho]min = -0.39 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

Cg1, Cg2, Cg3 and Cg11 are the centroids of the N1/C11-C14, N2/C21-C24, N3/C31-C34 and C351-C356 rings, respectively.

D-H...A D-H H...A D...A D-H...A
C62-H62A...N6 0.99 2.51 3.303 (3) 137
C63-H63B...O3i 0.99 2.56 3.489 (2) 156
C65-H65B...O6i 0.99 2.47 3.257 (2) 136
C62-H62B...Cg1 0.99 2.90 3.555 (2) 124
C63-H63A...Cg11ii 0.99 2.75 3.662 (2) 154
C71-H71A...Cg3iii 0.99 2.88 3.535 (2) 124
C353-H353...Cg2iv 0.95 2.62 3.459 (2) 147
C454-H454...Cg11iii 0.95 2.82 3.697 (3) 153
Symmetry codes: (i) -x+1, -y+1, -z; (ii) x-1, y, z; (iii) [x-{\script{3\over 2}}, -y-{\script{1\over 2}}, z-{\script{3\over 2}}]; (iv) x+1, y, z.

Data collection: CrysAlis CCD (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrystAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]); cell refinement: CrysAlis RED (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrystAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]); data reduction: CrysAlis RED; program(s) used to solve structure: SIR2004 (Burla et al., 2005[Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381-388.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEPIII (Burnett & Johnson, 1996[Burnett, M. N. & Johnson, C. K. (1996). ORTEPII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.]) and ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: SHELXL97.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NG5303 ).


Acknowledgements

The authors gratefully acknowledge financial support from the Ministry of Higher Education and Scientific Research of Tunisia.

References

Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R. (2005). J. Appl. Cryst. 38, 381-388.  [ISI] [CrossRef] [ChemPort] [details]
Burnett, M. N. & Johnson, C. K. (1996). ORTEPII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.
Byrn, M. P., Curtis, C. J., Goldberg, I., Hsiou, Y., Khan, S. I., Sawin, P. A., Tendick, S. K. & Strouse, C. E. (1991). J. Am. Chem. Soc. 113, 6549-6557.  [CrossRef] [ChemPort] [ISI]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Jentzen, W., Song, X. & Shelnutt, J. A. (1997). J. Phys. Chem. B, 101, 1684-1699.  [CrossRef] [ChemPort]
Liu, J.-J., He, X., Shao, M. & Li, M.-X. (2009). Inorg. Chem. Commun. 12, 972-974.  [CrossRef] [ChemPort]
Mansour, A., Belkhiria, M. S., Daran, J.-C. & Nasri, H. (2010). Acta Cryst. E66, m509-m510.  [CSD] [CrossRef] [details]
Oxford Diffraction (2009). CrystAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.
Rodesiler, P. F., Griffith, E. A. H., Charles, N. G., Lebioda, L. & Amma, E. L. (1985). Inorg. Chem. 24, 4595-4600.  [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]


Acta Cryst (2012). E68, m1557-m1558   [ doi:10.1107/S1600536812048052 ]

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