Bis[tris­(ethane-1,2-diamine)nickel(II)] octa­cyanidomolybdate(IV) penta­hydrate

Jun, Q.; Zhang, C.

doi:10.1107/S1600536809051964

Volume 66
Part 1
Pages m24-m25
January 2010

Received 25 November 2009
Accepted 3 December 2009
Online 9 December 2009

Key indicators
Single-crystal X-ray study
T = 153 K
Mean (C-C) = 0.003 Å
R = 0.028
wR = 0.059
Data-to-parameter ratio = 14.9
Details

Bis[tris(ethane-1,2-diamine)nickel(II)] octacyanidomolybdate(IV) pentahydrate

Qian Jun ^a and Chi Zhang ^a ^*

^aMolecular Materials Research Center, School of Chemical Engineering, Nanjing University of Science and Technology, 200 Xiaolingwei Road, Nanjing 210094, People's Republic of China
Correspondence e-mail: zhangchinjust@yahoo.com

In the title compound, [Ni(C₂H₈N₂)₃]₂[Mo(CN)₈]·5H₂O, the Ni^II ion is coordinated by six N atoms from three ethane-1,2-diamine ligands in a distorted octahedral geometry, while the Mo^IV atom is coordianted by eight cyanide ligands. The Ni-N bond distances range from 2.1061 (18) to 2.1425 (18) Å. The Mo-C and C-N distances in the [Mo(CN)₈] unit range from 2.154 (2) to 2.174 (2) Å and 1.149 (3) to 1.156 (3) Å, respectively. The complex ions and water molecules are linked by weak N-HN/O and O-HN/O hydrogen bonds into a three-demensional structure.

Related literature

For octacyanidometalates as molecular building units for transition metal complex assemblies, see: Przychodzen et al. (2006); Withers et al. (2005). For a related structure, see: Liu et al. (2008).

Experimental

Crystal data

[Ni(C₂H₈N₂)₃]₂[Mo(CN)₈]·5H₂O
M_r = 872.18
Monoclinic, P 2₁ /c
a = 13.384 (3) Å
b = 16.465 (3) Å
c = 21.094 (6) Å
= 124.45 (2)°
V = 3833.2 (18) Å³
Z = 4
Mo K radiation
= 1.35 mm^-1
T = 153 K
0.40 × 0.23 × 0.18 mm

Data collection

Rigaku Mercury CCD diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) T_min = 0.770, T_max = 1.000
36947 measured reflections
6993 independent reflections
6541 reflections with I > 2(I)
R_int = 0.030

Refinement

R[F² > 2(F²)] = 0.028
wR(F²) = 0.059
S = 1.16
6993 reflections
469 parameters
H atoms treated by a mixture of independent and constrained refinement
_max = 0.50 e Å^-3
_min = -0.47 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N13-H13BN8ⁱ	0.92	2.32	3.138 (3)	148
N11-H11AN5ⁱⁱ	0.92	2.26	3.149 (3)	163
N11-H11BN8ⁱ	0.92	2.51	3.285 (3)	142
N12-H12BO1ⁱⁱ	0.92	2.35	3.230 (3)	161
N14-H14AN5ⁱ	0.92	2.35	3.231 (3)	160
N14-H14BN4ⁱⁱ	0.92	2.40	3.178 (3)	143
N15-H15AN7ⁱⁱⁱ	0.92	2.38	3.189 (3)	146
N15-H15BN4^iv	0.92	2.34	3.223 (3)	162
N19-H19BN4^iv	0.92	2.40	3.226 (3)	149
N18-H18BN1ⁱⁱⁱ	0.92	2.48	3.364 (3)	161
N16-H16BN1ⁱⁱⁱ	0.83 (3)	2.34 (3)	3.141 (3)	162 (2)
N20-H20AO5^v	0.92	2.26	3.152 (3)	164
O3-H3BN8^vi	0.76 (3)	2.32 (3)	3.066 (3)	167 (3)
O4-H4AO2^vii	0.81 (3)	1.99 (3)	2.779 (3)	164 (3)
O4-H4BO2^viii	0.80 (3)	2.15 (3)	2.927 (3)	166 (3)
O5-H5AN6^ix	0.84 (3)	1.93 (3)	2.767 (3)	177 (3)
O5-H5BN7ⁱⁱ	0.77 (3)	2.04 (3)	2.795 (3)	170 (3)
N13-H13AN6	0.92	2.44	3.214 (3)	142
N12-H12AN1	0.92	2.23	3.135 (3)	166
N19-H19AN2	0.92	2.39	3.207 (3)	149
N17-H17AN2	0.92	2.42	3.183 (3)	141
N17-H17BN3	0.92	2.50	3.401 (3)	166
N16-H16AO1	0.84 (3)	2.35 (3)	3.183 (3)	173 (2)
N20-H20BO2	0.92	2.57	3.353 (3)	143
O2-H2AN3	0.76 (3)	2.04 (3)	2.788 (3)	169 (3)
O2-H2BO5	0.80 (3)	1.89 (3)	2.671 (2)	167 (3)
O1-H1AO3	0.73 (3)	2.05 (3)	2.767 (3)	166 (3)
O1-H1BN2	0.86 (3)	2.07 (3)	2.906 (3)	161 (3)
O3-H3AO4	0.81 (3)	2.01 (3)	2.788 (3)	161 (3)
Symmetry codes: (i) $[-x, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) $[x, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (iii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iv) $[x+1, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (v) -x+1, -y+1, -z+1; (vi) x+1, y, z; (vii) $[x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (viii) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ix) $[-x, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear; data reduction: CrystalClear; 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 data and figures for this paper are available from the IUCr electronic archives (Reference: PV2243 ).

Acknowledgements

This work was supported by the Graduate Innovation Foundation of Nanjing University of Science and Technology.

References

Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Liu, W.-Y., Zhou, H., Guo, J.-X. & Yuan, A.-H. (2008). Acta Cryst. E64, m1152-m1153.
Przychodzen, P., Korzenial, T., Podgajny, R. & Sieklucka, B. (2006). Coord. Chem. Rev. 250, 2234-2260.
Rigaku (2008). CrystalClear. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Withers, J. R., Ruschmann, C., Bojang, P., Parkin, S. & Holmes, S. M. (2005). Inorg. Chem. 44, 352-358.

metal-organic compounds