5,6-Dihydro-1,10-phenanthroline-1,10-diium μ-oxido-bis­[penta­fluoridotantalate(V)]

Meng, Z.-H.; Feng, Y.-Q.; Chen, X.-F.

doi:10.1107/S1600536812014742

Volume 68
Part 5
Page m561
May 2012

Received 8 March 2012
Accepted 4 April 2012
Online 13 April 2012

Key indicators
Single-crystal X-ray study
T = 296 K
Mean (C-C) = 0.010 Å
R = 0.028
wR = 0.072
Data-to-parameter ratio = 13.9
Details

5,6-Dihydro-1,10-phenanthroline-1,10-diium -oxido-bis[pentafluoridotantalate(V)]

Zhao-Hui Meng,^a ^* Yu-Quan Feng ^a and Xin-Feng Chen ^a

^aCollege of Chemistry and Pharmacy Engineering, Nanyang Normal University, Nanyang 473061, People's Republic of China
Correspondence e-mail: nysymzh@126.com

In the title compound, (C₁₂H₁₂N₂)[Ta₂F₁₀O], the doubly protonated 5,6-dihydro-1,10-phenantroline-1,10-diium cation is located on a twofold rotation axis, whereas the isolated [Ta₂OF₁₀]^2- dianion has -1 symmetry. In the so far unknown dianion, the symmetry-related Ta^V atoms are octahedrally coordinated by five F atoms and a bridging O atom, the latter being located on an inversion centre. The two pyridine rings in the cation make a dihedral angle of 22.8 (4)°. The cations and dianions are arranged in layers parallel to (100) and are connected through N-HF and C-HF hydrogen-bonding interactions into a three-dimensional structure.

Related literature

For structure-property relations of metal oxyfluorides, see: Hagerman & Poeppelmeier (1995); Halasyamani & Poeppelmeier (1998); Welk et al. (2002).

Experimental

Crystal data

(C₁₂H₁₂N₂)[Ta₂F₁₀O]
M_r = 752.14
Monoclinic, C 2/c
a = 13.536 (2) Å
b = 11.3031 (17) Å
c = 11.5316 (17) Å
= 90.093 (2)°
V = 1764.4 (5) Å³
Z = 4
Mo K radiation
= 12.50 mm^-1
T = 296 K
0.21 × 0.20 × 0.17 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008) T_min = 0.179, T_max = 0.225
4738 measured reflections
1725 independent reflections
1573 reflections with I > 2(I)
R_int = 0.029

Refinement

R[F² > 2(F²)] = 0.028
wR(F²) = 0.072
S = 1.05
1725 reflections
124 parameters
H-atom parameters constrained
_max = 1.96 e Å^-3
_min = -1.14 e Å^-3

Table 1
Selected bond lengths (Å)

Ta1-F4	1.877 (5)
Ta1-F5	1.886 (5)
Ta1-F1	1.886 (5)
Ta1-O1	1.8924 (3)
Ta1-F3	1.895 (4)
Ta1-F2	1.905 (4)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N1-H1AF4ⁱ	0.86	2.45	3.114 (10)	135
C4-H4AF1ⁱⁱ	0.93	2.26	3.066 (9)	145
C6-H6AF3ⁱⁱⁱ	0.97	2.28	3.219 (8)	163
C6-H6BF5^iv	0.97	2.45	3.268 (9)	142
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) $[x+{\script{1\over 2}}, y+{\script{1\over 2}}, z+1]$ ; (iii) -x+1, -y, -z+1; (iv) $[-x+{\script{3\over 2}}, -y+{\script{1\over 2}}, -z+1]$ .

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); 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 data and figures for this paper are available from the IUCr electronic archives (Reference: WM2602 ).

References

Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Hagerman, M. E. & Poeppelmeier, K. R. (1995). Chem. Mater. 7, 602-621.
Halasyamani, P. S. & Poeppelmeier, K. R. (1998). Chem. Mater. 10, 2753-2769.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Welk, M. E., Norquist, A. J., Arnold, F. P., Stern, C. L. & Poeppelmeier, K. R. (2002). Inorg. Chem. 41, 5119-5125.

metal-organic compounds