Tetra­kis(3,5-dimethyl-1H-pyrazole-κN 2)(nitrato-κ2 O,O′)cadmium(II) nitrate

Su-Qing Wang; Fang-Fang Jian

doi:10.1107/S160053680803626X

. 2008 Nov 13;64(Pt 12):m1532. doi: 10.1107/S160053680803626X

Tetrakis(3,5-dimethyl-1H-pyrazole-κN ²)(nitrato-κ² O,O′)cadmium(II) nitrate

Su-Qing Wang ^a, Fang-Fang Jian ^b,^*

PMCID: PMC2959841 PMID: 21581147

Abstract

The title compound, [Cd(NO₃)(C₅H₈N₂)₄]NO₃, was prepared by reaction of cadmium nitrate and 3,5-dimethylpyrazole in ethanol solution. The Cd atom adopts a distorted cis-CdO₂N₄ octahedral geometry involving four dimethylpyrazole molecules and one bidentate nitrate anion. The molecular structure and packing are stabilized by N—H⋯O and C—H⋯O inter- and intramolecular hydrogen-bonding interactions.

Related literature

For background on the coordination chemistry of Cd(II) in biological systems, see: Dressing et al. (1982 ▶). For related literature, see: Addison et al. (1984 ▶).

Experimental

Crystal data

[Cd(NO₃)(C₅H₈N₂)₄]NO₃
M _r = 620.97
Triclinic,
a = 9.1790 (18) Å
b = 11.353 (2) Å
c = 13.669 (3) Å
α = 94.79 (3)°
β = 105.61 (3)°
γ = 90.68 (3)°
V = 1366.2 (5) Å³
Z = 2
Mo Kα radiation
μ = 0.85 mm⁻¹
T = 293 (2) K
0.25 × 0.20 × 0.18 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: none
7482 measured reflections
5035 independent reflections
4677 reflections with I > 2σ(I)
R _int = 0.016

Refinement

R[F ² > 2σ(F ²)] = 0.046
wR(F ²) = 0.137
S = 1.06
5035 reflections
319 parameters
1 restraint
H-atom parameters constrained
Δρ_max = 1.66 e Å⁻³
Δρ_min = −0.87 e Å⁻³

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053680803626X/at2668sup1.cif

e-64-m1532-sup1.cif^{(22.2KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S160053680803626X/at2668Isup2.hkl

e-64-m1532-Isup2.hkl^{(246.6KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N3—H4A⋯O1ⁱ	0.86	2.13	2.943 (8)	157
N3—H4A⋯O3ⁱ	0.86	2.50	3.289 (16)	152
N4—H5A⋯O1ⁱ	0.86	1.92	2.771 (8)	171
N6—H7A⋯O6ⁱⁱ	0.86	2.33	3.131 (6)	156
N9—H10A⋯O4	0.86	2.50	3.106 (5)	128
C5—H5B⋯O4	0.96	2.59	3.530 (7)	166
C10—H10B⋯O5	0.96	2.29	3.157 (7)	150
C13—H13A⋯O1ⁱⁱⁱ	0.93	2.49	3.375 (8)	159

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

supplementary crystallographic information

Comment

It is also known that most of the Cd(II) in biological systems is not in the form of free Cd(II) ions, but is coordinated by the abundance of biological ligands (Dressing et al., 1982). Therefore the coordination chemistry of Cd(II) with ligands is of great interest. In this paper, we reported the synthesis and the crystal structure of tri(3,5-dimenthyl pyrazolyl)cadmium(II) nitrate (I).

In the molecule of (I) (Fig. 1), each Cd atoms is coordinated by four nitrogen atoms from four 3,5-dimethyl pyrazoles respectively and two oxygen atoms from nitrate anion. All the bond length and angle are in the normal range. Another nitrate anion exists in the crystal lattice.

The molecular structure and packing are stabilized by the N—H···O and C—H···O inter and intraintermolecular hydrogen-bonding intercations.

Experimental

Solid 3,5-dimethyl pyrazole 0.96 g (0.01 mol) and cadmium nitrate 0.77 g (0.0025 mol) were added in 50 ml anhydrous alcohol under stirring. The mixture was refluxed for 3.5 h. The colourless solution was filtered and the filtrate was left to stand undisturbed. Upon slow evaporation at room temperature, a colourless crystalline solid appeared three days later and was separated by filtration.