Bis(2,2′-bipyridyl-κ2 N,N′)chloridonickel(II) nitrate trihydrate

Mehdi Boutebdja; Adel Beghidja; Chahrazed Beghidja; Zouaoui Setifi; Hocine Merazig

doi:10.1107/S1600536814009064

. 2014 Apr 26;70(Pt 5):m190–m191. doi: 10.1107/S1600536814009064

Bis(2,2′-bipyridyl-κ² N,N′)chloridonickel(II) nitrate trihydrate

Mehdi Boutebdja ^a, Adel Beghidja ^a,^*, Chahrazed Beghidja ^a, Zouaoui Setifi ^b,^*, Hocine Merazig ^a

PMCID: PMC4011205 PMID: 24860319

Abstract

In the title hydrated salt, [NiCl(C₁₀H₈N₂)₂](NO₃)·3H₂O, the Ni²⁺ ion is coordinated by two 2,2′-bipyridyl (2,2′-bpy) ligands and a chloride ion in a trigonal–bipyramidal geometry. The chloride ion occupies an equatorial site and the dihedral angle between the 2,2′-bpy ring systems is 72.02 (6)°. In the crystal, the components are linked by C—H⋯O and O—H⋯O hydrogen bonds and aromatic π–π stacking interactions [shortest centroid–centroid separation = 3.635 (2) Å], generating a three-dimensional network.

Related literature

For the isotypic copper complex, see: Harrison et al. (1981 ▶); Liu et al. (2004 ▶). For related structures, see: Martens et al. (1996 ▶); Gao & Li (2009 ▶)

Experimental

Crystal data

[NiCl(C₁₀H₈N₂)₂](NO₃)·3H₂O
M _r = 522.57
Monoclinic,
a = 8.2341 (2) Å
b = 21.1920 (5) Å
c = 13.1284 (4) Å
β = 99.722 (1)°
V = 2257.97 (10) Å³
Z = 4
Mo Kα radiation
μ = 1.03 mm⁻¹
T = 296 K
0.15 × 0.13 × 0.10 mm

Data collection

Bruker APEXII CCD diffractometer
21125 measured reflections
5177 independent reflections
3811 reflections with I > 2σ(I)
R _int = 0.034

Refinement

R[F ² > 2σ(F ²)] = 0.044
wR(F ²) = 0.127
S = 1.01
5177 reflections
298 parameters
9 restraints
H-atom parameters constrained
Δρ_max = 0.47 e Å⁻³
Δρ_min = −0.47 e Å⁻³

Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ATOMS (Dowty, 1995 ▶); software used to prepare material for publication: WinGX publication routines (Farrugia, 2012 ▶).

Supplementary Material

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536814009064/hb7220sup1.cif

e-70-0m190-sup1.cif^{(33KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814009064/hb7220Isup2.hkl

e-70-0m190-Isup2.hkl^{(283.9KB, hkl)}

CCDC reference: 998760

Additional supporting information: crystallographic information; 3D view; checkCIF report

Table 1. Selected bond lengths (Å).

Ni1—Cl1	2.3035 (9)
Ni1—N1	1.989 (2)
Ni1—N2	2.088 (2)
Ni1—N3	2.107 (2)
Ni1—N4	1.983 (2)

Open in a new tab

Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1W⋯O3W ⁱ	0.81	2.29	2.876 (6)	129
O1W—H2W⋯O2ⁱⁱ	0.83	2.18	2.934 (7)	151
O2W—H3W⋯O2ⁱⁱ	0.84	1.90	2.723 (7)	166
O2W—H4W⋯Cl1ⁱ	0.83	2.47	3.245 (4)	155
O3W—H5W⋯O2W ⁱⁱⁱ	0.85	1.88	2.699 (6)	161
O3W—H6W⋯O1^iv	0.83	2.03	2.839 (7)	165
C14—H14⋯O2W	0.93	2.56	3.424 (5)	155
C18—H18⋯O1W	0.93	2.39	3.257 (6)	156

Open in a new tab

Symmetry codes: (i) Inline graphic ; (ii) ; (iii) ; (iv) .

Acknowledgments

The authors thank the MESRS (Algeria) for financial support. MB thanks the DG–RSDT and ANDRU (Direction Générale de la Recherche Scientifique et du Dévelopement Technologique et l’Agence Nationale pour le Développement de la Recherche Universitaire, Algeria) through the PNR project.

supplementary crystallographic information

1. Comment

The molecular structure of the title complex is shown in (Fig.1), The title compound is isostructural with the copper analogue (Harrison et al., 1981; Liu et al., 2004), crystalize in the monoclinic space group P2₁/n. The Ni(II) atom is five-coordinate and displays a distorted trigonal-bipyramidal coordination geometry with four N atoms from the two chelating 2,2'-bipyridine molecules and one chloride ion. The basal plane defined by the atoms (N1 N3 Cl1). The apical positions are occupied by the N2 and N4 atoms [N2—Ni1—N4 = 175.09 (10)°]. The Ni—N bond lenghts (table 1) are in normal range [Ni1—N1 = 2.086 (3), Ni1—N2 = 1.984 (3), Ni1—N3 = 2.108 (3), Ni1—N4 = 1.983 (3), Ni1—Cl1 = 2.3032 (10)]. In the crystal structure, the components are linked by weak C—H···O and medium O—H···O hydrogen bonds. Water molecules are further hydrogen-bond-interacting with the nitrate anion to complete a two-dimensional water-nitrate framework parallel to (101)which can be described by the graph set R97(24) (Fig. 2). Thus, the discrete [Ni(bpy)₂Cl]⁺ was linked to each other through pi-pi stacking to form two-dimensional supramolecular coordinated polymer parallel to the ac plane with centroid–centroiddistances of Cg(1)—Cg(2) = 3.660 (2) Å, Cg(2)—Cg(2i) = 3.635 (2) Å and Cg(3)—Cg(4) = 3.693 (2) Å. (Cg(1) is the centroid of N4—C20 2,2'-bpy ring, Cg(2) is the centroid of N3—C15 2,2'-bpy ring, Cg(3) is the centroid of N2—C10 2,2'-bpy ring, Cg(4) is the centroid of N1—C5 2,2'-bpy ring) (Fig.3). These layers are connected to each other via a weak O—H···Cl and C—H···O hydrogen bond to form a three-dimensional network(Fig.4).

2. Experimental

Compound (1) was obtained from the reaction of MSA 'mercaptosuccinic acid' (0.15 g, 1 mmol) in pyridine and an ethanolic solution of Ni(NO3)2.6H2O (0.290 g, 1 mmole) After several minutes of stirring an ethanol solution containing 2,2'-Bipyridine hydrochloride (0.114 g, 0.5 mmol) was add. The solution was kept for several weeks at room temperature. Green crystals suitable for X-ray analysis were obtained (yield: 0.1 g, 10% on the basis of Ni(NO3)2.6H2O).