Diaqua­bis­(propane-1,3-diamine)­nickel(II) bis­(propane-1,3-diamine)­disulfato­nickelate(II)

Rusanova, J.A.

doi:10.1107/S1600536812009750

Volume 68
Part 4
Pages m400-m401
April 2012

Received 24 February 2012
Accepted 5 March 2012
Online 10 March 2012

Key indicators
Single-crystal X-ray study
T = 296 K
Mean (C-C) = 0.003 Å
R = 0.024
wR = 0.063
Data-to-parameter ratio = 15.6
Details

Diaquabis(propane-1,3-diamine)nickel(II) bis(propane-1,3-diamine)disulfatonickelate(II)

Julia A. Rusanova ^a ^*

^aNational Taras Shevchenko University, Department of Chemistry, Volodymyrska str. 64, 01033 Kyiv, Ukraine
Correspondence e-mail: rusanova_j@yahoo.com

The ionic Ni^II title complex, [Ni(C₃H₁₀N₂)₂(H₂O)₂][Ni(SO₄)₂(C₃H₁₀N₂)₂], is built up of [Ni(dipr)₂(H₂O)₂]²⁺ complex cations and [Ni(dipr)₂(SO₄)₂]^2- complex anions (dipr is propane-1,3-diamine). Both Ni^II atoms display a slightly distorted octahedral coordination and are located on inversion centers. There are several types of hydrogen-bonding interactions, which connect complex cations and anions into a two-dimensional network parallel to (010). Hydrogen bonds formed by the axially coordinated water molecule of the complex cation and one of the O atoms of the sulfate groups of the complex anion (first type) link them into chains along the c axis. These chains are linked to each other through hydrogen bonds formed by an O atom (second type) of the SO₄ groups and NH₂ groups of the ligand of the complex cations from neighboring chains, forming a two-dimensional hydrogen-bonded net perpendicular to the b axis. The third type of O atoms of the sulfate groups of the complex anion are also linked into chains by a combination of both previously described types of H-atom connections.

Related literature

For background to direct synthesis, see: Nesterov et al. (2004, 2006); Kovbasyuk et al. (1997, 1998); Vassilyeva et al. (1997). For the structures of related complexes, see: Clegg et al. (1992); Kim & Lee (2002); Fritsky et al. (2004); Nowicka et al. (2002); Stockner et al. (2007); Duesler & Raymond (1978); Jurnak & Raymond (1974); Solans et al. (1982).

Experimental

Crystal data

[Ni(C₃H₁₀N₂)₂(H₂O)₂][Ni(SO₄)₂(C₃H₁₀N₂)₂]
M_r = 642.1
Triclinic, $[P \overline 1]$
a = 6.7055 (1) Å
b = 8.9098 (2) Å
c = 11.9504 (4) Å
= 103.016 (2)°
= 103.795 (2)°
= 105.729 (1)°
V = 634.52 (3) Å³
Z = 1
Mo K radiation
= 1.71 mm^-1
T = 296 K
0.49 × 0.15 × 0.12 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: numerical (SADABS; Sheldrick, 2009) T_min = 0.488, T_max = 0.703
10425 measured reflections
3078 independent reflections
2728 reflections with I > 2(I)
R_int = 0.030

Refinement

R[F² > 2(F²)] = 0.024
wR(F²) = 0.063
S = 1.07
3078 reflections
197 parameters
H atoms treated by a mixture of independent and constrained refinement
_max = 0.41 e Å^-3
_min = -0.37 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O5-H9O1	0.82 (2)	1.96 (2)	2.7739 (16)	172 (2)
N2-H1O4	0.823 (19)	2.265 (19)	3.0528 (18)	160.4 (16)
N1-H4O2ⁱ	0.84 (2)	2.28 (2)	3.0621 (18)	154.9 (18)
O5-H10O2ⁱ	0.70 (2)	2.15 (3)	2.8476 (18)	179 (3)
N3-H5O3ⁱⁱ	0.86 (2)	2.06 (2)	2.8900 (17)	161.4 (17)
N2-H2O2ⁱⁱⁱ	0.923 (19)	2.145 (19)	3.0600 (17)	171.2 (15)
N4-H7O3^iv	0.91 (2)	2.03 (2)	2.9269 (18)	170 (2)
Symmetry codes: (i) x-1, y, z; (ii) -x+2, -y+2, -z+1; (iii) -x+2, -y+2, -z; (iv) -x+1, -y+2, -z+1.

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: publCIF (Westrip, 2010).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BR2192 ).

References

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Kim, C.-H. & Lee, S.-G. (2002). Acta Cryst. C58, m421-m423.
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metal-organic compounds