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Crystal Structure of Bis(5,17-dihydroxy-3,7,15,19,25,26-hexa-azatricyclo(19.3.1.19,13)hexacosa-1(25),2,7,9(26),10,12,14,19,21,23-decaene-μ1,2-perchlorato barium) diperchlorate: a Schiff-Base Macrocyclic Complex Derived from 2,6-Diformylpyridine and 1,3-Diaminopropan-2-ol

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Abstract

The title complex, [Ba(L1)(μ1,2-ClO4)]2(ClO4)2 (where L1 = 5,17-dihydroxy-3,7,15,19,25,26-hexa-azatricyclo(19.3.1.19,13)hexacosa-1(25),2,7,9(26),10,12,14,19,21,23-decaene), was synthesised by a Schiff base condensation of 2,6-diformylpyridine with 1,3-diaminopropan-2-ol in dry methanol using barium(II) as template ion. The complex was characterised by IR, 1H NMR, mass spectrometry, elemental analysis and X-ray crystallography. The structure was solved in the triclinic space group P\( {\bar{\text{1}}} \) with a = 8.4587(9), b = 8.7360(9), c = 17.7722(19) Å, α = 79.786(2), β = 88.780(2), γ = 83.048(2)°, V = 1283.0(2) Å3, Z = 1 and R1 = 0.0433. The macrocycle is folded and the complex dimerises via perchlorate anions which bridge the barium ions, and this interaction is supported by hydrogen bonding between neighbouring alcohol groups. The dimers are further linked into chains via intermolecular O–H···OClO3 hydrogen bonds.

Graphical Abstract

An 11-coordinate Ba(II) macrocyclic dimer linked by bridging perchlorate anions and hydrogen bonds.

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References

  1. Fenton DE (1986) Pure Appl Chem 58:1437

    Article  CAS  Google Scholar 

  2. Nelson SM (1980) Pure Appl Chem 52:2461

    Article  CAS  Google Scholar 

  3. Adams H, Bailey NA, Fenton, DE, Good RJ, Moody R, Rodriguez de Barbarin CO (1987) J Chem Soc Dalton Trans 207

  4. Brooker S, McKee V, Shepard WB, Pannell LK (1987) J Chem Soc Dalton Trans 2555

  5. Tsubomura T, Ito M, Fujita T (2002) Bull Chem Soc Jpn 75:2392

    Article  Google Scholar 

  6. Harding C, McDowell D, Nelson J, Raghunathan S, Stevenson C, Drew MGB, Yates PC (1990) J Chem Soc Dalton Trans 2521

  7. Dennett R, James L, McKee V (2007) Acta Cryst E63:m1720

    CAS  Google Scholar 

  8. Papadopolous EP, Jarrar A, Issadorides CH (1966) J Org Chem 31:615

    Article  Google Scholar 

  9. Sheldrick GM (2008) Acta Cryst A64:112

    CAS  Google Scholar 

Download references

Acknowledgments

We are grateful to the Turkish Government for the award of a postgraduate scholarship (to MK), to the University of Canterbury for an Erskine Fellowship (to VMcK), and to the EPSRC Mass Spectrometry Service, Swansea for FAB (LSIMS).

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Authors and Affiliations

  1. Department of Chemistry, Loughborough University, LE11 3TU, Loughborough, Leicestershire, UK

    Leanne James, Muhammet Kose & Vickie McKee

  2. Chemistry Department, University of Canterbury, Private Bag 4800, Christchurch, 8140, New Zealand

    Ted Metcalfe

Authors
  1. Leanne James
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  2. Muhammet Kose
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  3. Ted Metcalfe
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  4. Vickie McKee
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Correspondence to Vickie McKee.

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James, L., Kose, M., Metcalfe, T. et al. Crystal Structure of Bis(5,17-dihydroxy-3,7,15,19,25,26-hexa-azatricyclo(19.3.1.19,13)hexacosa-1(25),2,7,9(26),10,12,14,19,21,23-decaene-μ1,2-perchlorato barium) diperchlorate: a Schiff-Base Macrocyclic Complex Derived from 2,6-Diformylpyridine and 1,3-Diaminopropan-2-ol. J Chem Crystallogr 41, 577–581 (2011). https://doi.org/10.1007/s10870-010-9925-1

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