Bis(2,2′:6′,2′′-terpyridine)­ruthenium(II) bis­(perchlorate) hemihydrate

Kozlowska, M.; Rodziewicz, P.; Brus, D.M.; Breczko, J.; Brzezinski, K.

doi:10.1107/S1600536812043917

Volume 68
Part 11
Pages m1414-m1415
November 2012

Received 16 October 2012
Accepted 23 October 2012
Online 27 October 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.005 Å
Disorder in solvent or counterion
R = 0.042
wR = 0.083
Data-to-parameter ratio = 14.0
Details

Bis(2,2':6',2''-terpyridine)ruthenium(II) bis(perchlorate) hemihydrate

Mariana Kozlowska,^a Pawel Rodziewicz,^a Diana Malgorzata Brus,^a Joanna Breczko ^a and Krzysztof Brzezinski ^a ^*

^aInstitute of Chemistry, University of Bialystok, Hurtowa 1, 15-399 Bialystok, Poland
Correspondence e-mail: k.brzezinski@uwb.edu.pl

The asymmetric unit of the title compound, [Ru(C₁₅H₁₁N₃)₂](ClO₄)₂·0.5H₂O, contains one ruthenium-terpiridine complex cation, two perchlorate anions and one half-molecule of water. Face-to-face and face-to-edge [pi] -stacking interactions between terpyridine units [centroid-centroid distances = 3.793 (2) and 3.801 (2) Å] stabilize the crystal lattice The partially occupied water molecule interacts with two perchlorate ions via O-HO hydrogen bonds. In the crystal lattice, the complex cations, perchlorate ion-water pairs and the second perchlorate anions are arranged into columns along b direction.

Related literature

For the preparation of terpyridine complexes with transition metals, see: Burstall & Nyholm (1952). For the structures of salts of complexes of ruthenium with terpyridine, see: Craig et al. (1998); Lashgari et al. (1999); Pyo et al. (1999); Tovee et al. (2009); Walstrom et al. (2009). For background to the properties and applications of terpiridine complexes, see: Anders & Schubert (2004); Constable (2007); Plonska et al. (2002); Winkler et al. (2003, 2006).

Experimental

Crystal data

[Ru(C₁₅H₁₁N₃)₂](ClO₄)₂·0.5H₂O
M_r = 775.51
Monoclinic, P 2₁ /n
a = 8.7676 (2) Å
b = 8.8221 (9) Å
c = 39.118 (4) Å
= 93.582 (5)°
V = 3019.8 (4) Å³
Z = 4
Mo K radiation
= 0.76 mm^-1
T = 100 K
0.15 × 0.12 × 0.03 mm

Data collection

Agilent SuperNova (Dual, Cu at zero, Atlas) diffractometer
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2011) T_min = 0.801, T_max = 1.000
16537 measured reflections
6158 independent reflections
5858 reflections with I > 2(I)
R_int = 0.027

Refinement

R[F² > 2(F²)] = 0.042
wR(F²) = 0.083
S = 1.27
6158 reflections
439 parameters
3 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 0.65 e Å^-3
_min = -1.17 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

Cg1 and Cg2 are the centoids of the N3A-C15A and N3B-C15B rings, respectively.

D-HA	D-H	HA	DA	D-HA
O5-H5AO2Aⁱ	0.85 (2)	1.98 (3)	2.790 (6)	159 (7)
O5-H5BO1A	0.85 (2)	2.03 (3)	2.824 (6)	157 (7)
C2B-H2BCg1ⁱⁱ	0.95	3.09 (1)	3.945 (4)	45 (1)
C14A-H14ACg2ⁱⁱⁱ	0.95	3.01 (1)	3.878 (4)	43 (1)
Symmetry codes: (i) -x+2, -y+1, -z; (ii) x-1, y, z; (iii) x, y+1, z.

Data collection: CrysAlis PRO (Agilent, 2011); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXD (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997) 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: BT6849 ).

Acknowledgements

This work was supported by the HOMING PLUS project of the Foundation for Polish Science (MK and PR) and the National Science Center, Poland (grant No. NN204396640). The X-ray diffractometer was funded by EFRD as part of the Operational Programme Development of Eastern Poland 2007-2013, project POPW.01.03.00-20-034/09-00.

References

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metal-organic compounds