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

In the title compound, (C(12)H(12)N(2))[Ta(2)F(10)O], the doubly protonated 5,6-dihydro-1,10-phenantroline-1,10-diium cation is located on a twofold rotation axis, whereas the isolated [Ta(2)OF(10)](2-) dianion has -1 symmetry. In the so far unknown dianion, the symmetry-related Ta(V) atoms are octa-hedrally 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-H⋯F and C-H⋯F hydrogen-bonding inter-actions 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 = 752.14

Monoclinic,

a = 13.536 (2) Å

b = 11.3031 (17) Å

c = 11.5316 (17) Å

β = 90.093 (2)°

V = 1764.4 (5) Å3

Z = 4

Mo Kα radiation

μ = 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 > 2σ(I)

R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.028

wR(F 2) = 0.072

S = 1.05

1725 reflections

124 parameters

H-atom parameters constrained

Δρmax = 1.96 e Å−3

Δρmin = −1.14 e Å−3

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.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812014742/wm2602sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812014742/wm2602Isup2.hkl

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

(C12H12N2)[Ta2F10O]	F(000) = 1368
Mr = 752.14	Dx = 2.831 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 3156 reflections
a = 13.536 (2) Å	θ = 2.4–28.3°
b = 11.3031 (17) Å	µ = 12.50 mm−1
c = 11.5316 (17) Å	T = 296 K
β = 90.093 (2)°	Block, yellow
V = 1764.4 (5) Å3	0.21 × 0.20 × 0.17 mm
Z = 4

Bruker APEXII CCD diffractometer	1725 independent reflections
Radiation source: fine-focus sealed tube	1573 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.029
φ and ω scans	θmax = 26.0°, θmin = 2.9°
Absorption correction: multi-scan (SADABS; Bruker, 2008)	h = −13→16
Tmin = 0.179, Tmax = 0.225	k = −13→13
4738 measured reflections	l = −14→12

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.072	H-atom parameters constrained
S = 1.05	w = 1/[σ2(Fo2) + (0.0278P)2 + 20.5568P] where P = (Fo2 + 2Fc2)/3
1725 reflections	(Δ/σ)max < 0.001
124 parameters	Δρmax = 1.96 e Å−3
0 restraints	Δρmin = −1.14 e Å−3

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

	x	y	z	Uiso*/Ueq
Ta1	0.193168 (19)	0.18732 (2)	0.13666 (2)	0.03630 (12)
C2	0.9169 (6)	0.2166 (8)	0.9660 (7)	0.0499 (19)
H2A	0.9123	0.1448	1.0050	0.060*
C1	0.9649 (4)	0.2220 (5)	0.8646 (5)	0.0210 (10)
C5	0.9738 (5)	0.3254 (5)	0.8051 (5)	0.0332 (13)
N1	0.9318 (6)	0.4270 (7)	0.8502 (7)	0.069 (2)
H1A	0.9361	0.4931	0.8136	0.083*
C4	0.8832 (7)	0.4207 (9)	0.9546 (7)	0.062 (2)
H4A	0.8558	0.4890	0.9858	0.075*
C3	0.8742 (7)	0.3164 (9)	1.0135 (7)	0.060 (2)
H3A	0.8403	0.3127	1.0834	0.072*
F1	0.2944 (5)	0.0732 (6)	0.1479 (5)	0.093 (2)
F2	0.1355 (4)	0.1192 (5)	0.2716 (4)	0.0684 (14)
F3	0.1159 (4)	0.0811 (4)	0.0475 (4)	0.0692 (15)
F4	0.0908 (5)	0.2992 (5)	0.1343 (7)	0.0867 (19)
F5	0.2665 (4)	0.2877 (5)	0.2351 (5)	0.0720 (15)
O1	0.2500	0.2500	0.0000	0.082 (3)
C6	1.0104 (5)	0.1139 (6)	0.8134 (6)	0.0408 (15)
H6A	0.9827	0.0436	0.8490	0.049*
H6B	1.0811	0.1141	0.8270	0.049*

	U11	U22	U33	U12	U13	U23
Ta1	0.03744 (18)	0.03940 (18)	0.03206 (18)	−0.00695 (11)	0.00427 (11)	−0.00056 (11)
C2	0.047 (4)	0.069 (5)	0.033 (4)	−0.008 (4)	0.001 (3)	0.012 (4)
C1	0.023 (3)	0.023 (2)	0.016 (2)	−0.001 (2)	0.004 (2)	0.002 (2)
C5	0.039 (3)	0.032 (3)	0.028 (3)	0.000 (3)	0.001 (3)	−0.004 (2)
N1	0.087 (5)	0.062 (5)	0.059 (4)	0.015 (4)	0.000 (4)	−0.007 (4)
C4	0.069 (6)	0.076 (6)	0.042 (4)	0.016 (5)	0.015 (4)	−0.022 (4)
C3	0.056 (5)	0.099 (7)	0.025 (4)	0.003 (4)	0.013 (3)	−0.012 (4)
F1	0.094 (4)	0.117 (5)	0.066 (3)	0.058 (4)	−0.006 (3)	−0.024 (3)
F2	0.097 (4)	0.066 (3)	0.042 (3)	−0.019 (3)	0.024 (3)	0.005 (2)
F3	0.095 (4)	0.065 (3)	0.048 (3)	−0.038 (3)	−0.010 (3)	0.002 (2)
F4	0.070 (4)	0.061 (3)	0.128 (6)	0.017 (3)	−0.009 (4)	0.007 (3)
F5	0.071 (3)	0.082 (4)	0.063 (3)	−0.031 (3)	0.001 (3)	−0.023 (3)
O1	0.106 (8)	0.095 (7)	0.045 (5)	−0.054 (6)	0.018 (5)	0.008 (5)
C6	0.043 (4)	0.031 (3)	0.048 (4)	0.002 (3)	0.005 (3)	0.004 (3)

Ta1—F4	1.877 (5)	C5—N1	1.384 (9)
Ta1—F5	1.886 (5)	C5—C5i	1.455 (13)
Ta1—F1	1.886 (5)	N1—C4	1.374 (11)
Ta1—O1	1.8924 (3)	N1—H1A	0.8600
Ta1—F3	1.895 (4)	C4—C3	1.366 (13)
Ta1—F2	1.905 (4)	C4—H4A	0.9300
C2—C1	1.340 (9)	C3—H3A	0.9300
C2—C3	1.381 (12)	O1—Ta1ii	1.8924 (3)
C2—H2A	0.9300	C6—C6i	1.488 (14)
C1—C5	1.361 (8)	C6—H6A	0.9700
C1—C6	1.490 (8)	C6—H6B	0.9700
F4—Ta1—F5	89.5 (3)	C5—C1—C6	117.8 (5)
F4—Ta1—F1	176.8 (3)	C1—C5—N1	119.1 (6)
F5—Ta1—F1	89.3 (3)	C1—C5—C5i	119.0 (4)
F4—Ta1—O1	92.1 (2)	N1—C5—C5i	122.0 (5)
F5—Ta1—O1	93.55 (17)	C4—N1—C5	118.9 (8)
F1—Ta1—O1	91.0 (2)	C4—N1—H1A	120.5
F4—Ta1—F3	90.7 (3)	C5—N1—H1A	120.5
F5—Ta1—F3	175.8 (2)	C3—C4—N1	121.6 (8)
F1—Ta1—F3	90.2 (3)	C3—C4—H4A	119.2
O1—Ta1—F3	90.60 (15)	N1—C4—H4A	119.2
F4—Ta1—F2	88.9 (3)	C4—C3—C2	118.1 (7)
F5—Ta1—F2	88.1 (2)	C4—C3—H3A	121.0
F1—Ta1—F2	88.1 (3)	C2—C3—H3A	121.0
O1—Ta1—F2	178.07 (15)	Ta1ii—O1—Ta1	180.00 (2)
F3—Ta1—F2	87.7 (2)	C1—C6—C6i	108.2 (5)
C1—C2—C3	120.8 (7)	C1—C6—H6A	110.1
C1—C2—H2A	119.6	C6i—C6—H6A	110.1
C3—C2—H2A	119.6	C1—C6—H6B	110.1
C2—C1—C5	121.5 (6)	C6i—C6—H6B	110.1
C2—C1—C6	120.7 (6)	H6A—C6—H6B	108.4
C3—C2—C1—C5	0.4 (11)	C5i—C5—N1—C4	179.8 (8)
C3—C2—C1—C6	−179.6 (7)	C5—N1—C4—C3	−1.0 (13)
C2—C1—C5—N1	−0.4 (10)	N1—C4—C3—C2	1.0 (14)
C6—C1—C5—N1	179.6 (6)	C1—C2—C3—C4	−0.7 (13)
C2—C1—C5—C5i	−179.6 (8)	C2—C1—C6—C6i	138.0 (7)
C6—C1—C5—C5i	0.4 (10)	C5—C1—C6—C6i	−42.0 (9)
C1—C5—N1—C4	0.7 (11)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···F4iii	0.86	2.45	3.114 (10)	135
C4—H4A···F1iv	0.93	2.26	3.066 (9)	145
C6—H6A···F3v	0.97	2.28	3.219 (8)	163
C6—H6B···F5vi	0.97	2.45	3.268 (9)	142

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—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯F4i	0.86	2.45	3.114 (10)	135
C4—H4A⋯F1ii	0.93	2.26	3.066 (9)	145
C6—H6A⋯F3iii	0.97	2.28	3.219 (8)	163
C6—H6B⋯F5iv	0.97	2.45	3.268 (9)	142

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