Bis(2,2′-bipyridyl-κ2N,N′)dichlorido­rhodium(III) perchlorate

Dikhtiarenko, A.; Torre-Fernández, L.; García-Granda, S.; García, J.R.; Gimeno, J.

doi:10.1107/S1600536812018685

Volume 68
Part 6
Pages m713-m714
June 2012

Received 3 April 2012
Accepted 25 April 2012
Online 2 May 2012

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.005 Å
Disorder in solvent or counterion
R = 0.042
wR = 0.081
Data-to-parameter ratio = 23.5
Details

Bis(2,2'-bipyridyl-²N,N')dichloridorhodium(III) perchlorate

Alla Dikhtiarenko,^a Laura Torre-Fernández,^b Santiago García-Granda,^b ^* José R. García ^a and José Gimeno ^a

^aDepartamento Química Orgánica e Inorgánica, Universidad de Oviedo, 33006 Oviedo, Spain, and ^bDepartamento de Química Física y Analítica, Facultad de Química, Universidad de Oviedo-CINN, C/ Julián Clavería, 8, 33006 Oviedo, Asturias, Spain
Correspondence e-mail: sgg@uniovi.es

The asymmetric unit of the title compound, [RhCl₂(C₁₀H₈N₂)₂]ClO₄, consists of one unit of the cationic complex [RhCl₂(bipy)₂]⁺ and one uncoordinated perchlorate anion. The Rh^III atom is coordinated by four N atoms from two bipyridyl ligands and two Cl atoms, forming a distorted octahedral environment. The Cl ligands are cis. Two intramolecular C-HCl hydrogen bonds occur in the cationic complex . In the crystal, molecules are linked together by a hydrogen-bond network involving the H atoms of bipyridyl rings and perchlorate anions. An O atom of the perchlorate anion is disordered over two sites, with an occupancy-factor ratio of 0.78 (3):0.22 (3).

Related literature

For potential applications of noble metal complexes of pyridyl ligands in biochemistry, catalysis and anticancer activity, see: Chifotides et al. (2004); Mbaye et al. (2003); Karidi et al. (2005); Tan et al. (2005). For their photochemical and photophysical properties, see: Forster & Rund (2003); Arachchige et al. (2008) and for their electrochemical properties, see: Rasmussen et al. (1990). For related structures, see: Al-Noaimi & Haddad (2007); Andansen & Josephsen (1971); Choudhury et al. (2006); De Munno et al. (1993); Figgis et al. (1985); Fontaine (2001); Gao & Ng (2010); Kramer & Straehle (1986); Sofetis et al. (2006); Strenger et al. (2000). For similar structures with platinum group metals, see: Lahuerta et al. (1991); Kim et al. (2009); Helberg et al. (1996); Prajapati et al. (2008); Eggleston et al. (1985).

Experimental

Crystal data

[RhCl₂(C₁₀H₈N₂)₂]ClO₄
M_r = 585.63
Orthorhombic, P 2₁ 2₁ 2₁
a = 11.0344 (2) Å
b = 11.6796 (2) Å
c = 17.0884 (3) Å
V = 2202.33 (8) Å³
Z = 4
Mo K radiation
= 1.18 mm^-1
T = 293 K
0.19 × 0.16 × 0.12 mm

Data collection

Agilent Xcalibur Ruby Gemini diffractometer
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2011) T_min = 0.973, T_max = 1
12115 measured reflections
6922 independent reflections
5569 reflections with I > 2(I)
R_int = 0.026

Refinement

R[F² > 2(F²)] = 0.042
wR(F²) = 0.081
S = 1.02
6922 reflections
294 parameters
H-atom parameters constrained
_max = 0.75 e Å^-3
_min = -0.25 e Å^-3
Absolute structure: Flack (1983), 2630 Friedel pairs
Flack parameter: 0.47 (3)

Table 1
Selected geometric parameters (Å, °)

Rh1-N2	2.019 (2)
Rh1-N1	2.023 (2)
Rh1-N3	2.037 (2)
Rh1-N4	2.038 (3)
Rh1-Cl3	2.3291 (9)
Rh1-Cl2	2.3344 (9)

N1-Rh1-N3	174.22 (10)
Cl3-Rh1-Cl2	91.18 (4)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C1-H1Cl2	0.93	2.70	3.301 (4)	123
C11-H11Cl3	0.93	2.76	3.358 (4)	123
C3-H3O1ⁱ	0.93	2.29	3.192 (5)	164
C8-H8O1ⁱⁱ	0.93	2.56	3.142 (6)	121
C9-H9O1ⁱⁱ	0.93	2.58	3.154 (6)	120
C13-H13O4ⁱⁱⁱ	0.93	2.56	3.427 (6)	155
Symmetry codes: (i) $[-x+2, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (ii) $[x-{\script{1\over 2}}, -y-{\script{1\over 2}}, -z+1]$ ; (iii) $[-x+2, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: CrysAlis PRO (Agilent, 2011); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2006); software used to prepare material for publication: WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: LR2059 ).

Acknowledgements

This work was supported by the Spanish MICINN (projects MAT2006-01997, FC-08-IB08-036 and MAT2010-15094) and FEDER. AD also thanks MICINN for their pre-doctoral FPU grant (AP2008-03942).

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