(IUCr) Three-dimensional hydrogen-bonded supramolecular assembly in tetrakis(1,3,5-triaza-7-phosphaadamantane)copper(I) chloride hexahydrate

Volume 64
Part 5
Pages m603-m604
May 2008

Received 22 March 2008
Accepted 26 March 2008
Online 2 April 2008

Key indicators
Single-crystal X-ray study
T = 150 K
Mean (N-C) = 0.003 Å
R = 0.034
wR = 0.093
Data-to-parameter ratio = 16.0
Details

Three-dimensional hydrogen-bonded supramolecular assembly in tetrakis(1,3,5-triaza-7-phosphaadamantane)copper(I) chloride hexahydrate

Alexander M. Kirillov,^a Piotr Smolenski,^a M. Fátima C. Guedes da Silva,^a,^b ^* Maximilian N. Kopylovich ^a and Armando J. L. Pombeiro ^a

^aCentro de Química Estrutural, Complexo Interdisciplinar, Instituto Superior Técnico, TU Lisbon, Av. Rovisco Pais, 1049-001 Lisbon, Portugal, and ^bUniversidade Lusófona de Humanidades e Tecnologias, ULHT Lisbon, Av. do Campo Grande 376, 1749-024 Lisbon, Portugal
Correspondence e-mail: fatima.guedes@ist.utl.pt

The structure of the title compound, [Cu(PTA)₄]Cl·6H₂O (PTA is 1,3,5-triaza-7-phosphaadamantane, C₆H₁₂N₃P), is composed of discrete monomeric [Cu(PTA)₄]⁺ cations, chloride anions and uncoordinated water molecules. The Cu^I atom exhibits tetrahedral coordination geometry, involving four symmetry-equivalent P-bound PTA ligands. The structure is extended to a regular three-dimensional supramolecular framework via numerous equivalent O-HN hydrogen bonds between all solvent water molecules (six per cation) and all PTA N atoms, thus simultaneously bridging each [Cu(PTA)₄]⁺ cation with 12 neighbouring units in multiple directions. The study also shows that PTA can be a convenient ligand in crystal engineering for the construction of supramolecular architectures.

Related literature

For general background, see: Kirillov et al. (2007, 2008); Karabach et al. (2006); Di Nicola et al. (2007). For a comprehensive review of PTA chemistry, see: Phillips et al. (2004). For PTA-derived polymeric networks, see: Lidrissi et al. (2005); Frost et al. (2006); Mohr et al. (2006). For related compounds, see: Forward et al. (1996); Darensbourg et al. (1997, 1999).

Experimental

Crystal data

[Cu(C₆H₁₂N₃P)₄]Cl·6H₂O
M_r = 835.71
Cubic, $[F d \overline 3m ]$
a = 19.795 (4) Å
V = 7757 (3) Å³
Z = 8
Mo K radiation
= 0.85 mm^-1
T = 150 (2) K
0.20 × 0.17 × 0.12 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) T_min = 0.848, T_max = 0.905
3022 measured reflections
447 independent reflections
361 reflections with I > 2(I)
R_int = 0.049

Refinement

R[F² > 2(F²)] = 0.034
wR(F²) = 0.092
S = 1.08
447 reflections
28 parameters
H-atom parameters constrained
_max = 0.75 e Å^-3
_min = -0.32 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O10-H10N1	0.81	2.04	2.843 (3)	174

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996), PLATON (Spek, 2003) and Mercury (Macrae et al., 2006); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: DN2329 ).

Acknowledgements

This work has been supported by the FCT, Portugal, and its POCI 2010 programme (FEDER funded).

References

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metal-organic compounds