A binuclear vanadium oxyfluoride: di-μ-oxido-bis­[fluoridooxido(1,10-phenanthro­line)vanadium(V)]

DeBurgomaster, P.; Zubieta, J.

doi:10.1107/S1600536810037232

metal-organic compounds

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Volume 66| Part 10| October 2010| Page m1303

doi:10.1107/S1600536810037232

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A binuclear vanadium oxyfluoride: di-μ-oxido-bis[fluoridooxido(1,10-phenanthroline)vanadium(V)]

Paul DeBurgomaster ^a and Jon Zubieta ^a ^*

^aDepartment of Chemistry, Syracuse University, Syracuse, New York 13244, USA
^*Correspondence e-mail: jazubiet@syr.edu

(Received 13 September 2010; accepted 16 September 2010; online 25 September 2010)

The title compound, [V₂F₂O₄(C₁₂H₈N₂)₂], is a centrosymmetric binuclear vanadium(V) species with the metal ions in a distorted octahedral environment. The symmetry-equivalent V^V atoms exhibit coordination geometries defined by cis-terminal fluoride and oxide groups, unsymmetrically bridging oxide groups and the N-atom donors of the phenanthroline ligands. The crystal packing is stabilized by weak intermolecular C—H⋯O and C—H⋯F hydrogen bonds.

Related literature

For the properties and applications of oxyfluoridomolybdates and -vanadates, see: Adil et al. (2010 ); Burkholder & Zubieta (2004 ); DeBurgomaster & Zubieta (2010 ); Jones et al. (2010 ); Michailovski et al. (2006 , 2009 ). For examples of solid phase vanadium oxyfluorides in the presence of coligands, see: Ouellette et al. (2005 , 2006 , 2007 ); Ouellette & Zubieta (2007 ). For hydrothermal preparation of metal oxyfluorides, see: Gopalakrishnan (1995 ); Whittingham (1996 ); Zubieta (2003 ).

Experimental

Crystal data

[V₂F₂O₄(C₁₂H₈N₂)₂]
M_r = 564.29
Triclinic, $[P \overline 1]$
a = 7.8320 (9) Å
b = 8.4937 (10) Å
c = 9.2007 (11) Å
α = 113.741 (3)°
β = 102.834 (2)°
γ = 97.848 (2)°
V = 528.46 (11) Å³
Z = 1
Mo Kα radiation
μ = 0.95 mm⁻¹
T = 90 K
0.36 × 0.31 × 0.12 mm

Data collection

Bruker APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 1998 ) T_min = 0.626, T_max = 0.747
5297 measured reflections
2550 independent reflections
2502 reflections with I > 2σ(I)
R_int = 0.018

Refinement

R[F² > 2σ(F²)] = 0.034
wR(F²) = 0.084
S = 1.14
2550 reflections
163 parameters
H-atom parameters constrained
Δρ_max = 0.41 e Å⁻³
Δρ_min = −0.35 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C2—H2⋯F1ⁱ	0.95	2.49	3.393 (2)	160
C3—H3⋯O1ⁱⁱ	0.95	2.44	3.191 (2)	136
C6—H6⋯O1ⁱⁱ	0.95	2.46	3.200 (2)	135
C10—H10⋯O2ⁱⁱⁱ	0.95	2.39	3.282 (2)	157
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) x, y, z-1; (iii) x, y+1, z.

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalMaker (Palmer, 2006 ); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810037232/lh5133sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810037232/lh5133Isup2.hkl

checkCIF report

Comment top

Metal oxyfluorides exhibit a range of compositions and considerable structural versatility that give rise to useful physical properties and potential applications (Adil, et al., 2010; Burkholder & Zubieta, 2004; DeBurgomaster & Zubieta, 2010; Jones et al., 2010; Michailovski, et al., 2006,2009; Ouellette et al., 2005,2006,2007); Ouellette & Zubieta, 2007). Hydrothermal chemistry offers one approach to the preparation of novel metal oxyfluorides where the complexity of the synthetic domain allows incorporation of fluoride into metal oxide frameworks, providing unusual and often unprecedented structures (Gopalakrishnan, 1995; Whittingham, 1996; Zubieta, 2003) Furthermore, the metal-oxyfluoride core can be stabilized or modified by the introduction of appropriate coligands, such as organonitrogen donors of the pyridyl family. In the course of our investigations of the hydrothermal chemistry of metal oxides in the presence of fluoride anion, the title compound [V₂F₂O₄(phen)₂] was isolated. The compound crystallizes in the triclinic space group P1 with one binuclear molecule per unit cell, whose halves are related by a center of symmetry at the mid-point of the V···V vector. The V atoms exhibit distorted octahedral geometry with {VFO₃N₂} coordination (Fig. 1). The µ-bis-oxo bridging mode is characterized by a {V₂O₂} rhombus with alternating short-long V—O bond distances of 1.724 (1) Å and 2.316 (1) Å, respectively. The terminal oxo-groups lie in the plane of the {V₂O₂} rhombus and exhibit a pronounced trans-influence as shown by the elongated bridging oxo-group-vanadium distance, V1—O1. The coordination geometry at the vanadium sites also exhibits a fluoride ligand with V—F of 1.787 (1) Å with the V—F vector approximately normal to the {V₂O₂} rhombus. The V—F vectors of the binuclear unit adopt an anti-orientation with respect to the plane if the {V₂O₂} rhombus. The geometry is completed by the nitrogen donors of the phenanthroline ligand, which occupy positions trans to the short V—O bond of the rhombus and trans to the terminal fluoride ligand. The crystal packing is stabilized by weak intermolecular C—H···O and C—H···F hydrogen bonds which produces two-dimensional connectivity in the bc plane (Figure 2).

Related literature top

For the properties and applications of oxyfluoromolybdates and oxyfluorovanadates, see: Adil et al. (2010); Burkholder & Zubieta (2004); DeBurgomaster & Zubieta (2010); Jones et al. (2010); Michailovski et al. (2006,2009). For examples of solid phase vanadium oxyfluorides in the presence of coligands, see: Ouellette et al. (2005, 2006, 2007); Ouellette & Zubieta (2007). For hydrothermal preparation of metal oxyfluorides, see: Gopalakrishnan (1995); Whittingham (1996); Zubieta (2003).

Experimental top

A mixture of V₂O₅ (0.062 g, 0.34 mmol), 1,10-phenanthroline (0.367 g, 2.04 mmol), H₂O (5 ml, 277.5 mmol) and HF (0.200 ml, 5.80 mmol) in the mole ratio 1.00:6.03:1620:17.06 was stirred briefly before heating to 170 oC for 48 h (initial and final pH values of 2.5 and 2.0, respectively). Yellow rods suitable for X-ray diffraction were isolated in 65% yield. Anal. Calcd. for C₂₄H₂₀F₂N₄O₄V₂: C, 51.0; H, 2.84; N, 9.92; F, 6.73. Found: C, 50.7;H,3.01;N, 9.67; F, 6.55.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: CrystalMaker (Palmer, 2006); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. View of the molecular dimer of the title compound, with the atom-labeling scheme and the displacement ellipsoids drawn at the 50% probability level. Color scheme: vanadium, orange; oxygen, red; fluorine, green; nitrogen, light blue; carbon, black; hydrogen, pink.
	Fig. 2. A packing diagram illustrating the C-H···O and C-H···F contacts (illustrated as multiband cylinders). Color code as for Fig. 1.

di-µ-oxido-bis[fluoridooxido(1,10-phenanthroline)vanadium(V)] top

Crystal data top

[V₂F₂O₄(C₁₂H₈N₂)₂]	Z = 1
M_r = 564.29	F(000) = 284.0
Triclinic, P1	D_x = 1.773 Mg m⁻³ D_m = 1.77 (2) Mg m⁻³ D_m measured by flotation
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.8320 (9) Å	Cell parameters from 3266 reflections
b = 8.4937 (10) Å	θ = 2.4–28.3°
c = 9.2007 (11) Å	µ = 0.95 mm⁻¹
α = 113.741 (3)°	T = 90 K
β = 102.834 (2)°	Plate, yellow
γ = 97.848 (2)°	0.36 × 0.31 × 0.12 mm
V = 528.46 (11) Å³

Data collection top

Bruker APEX CCD diffractometer	2550 independent reflections
Radiation source: fine-focus sealed tube	2502 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.018
Detector resolution: 512 pixels mm^-1	θ_max = 28.1°, θ_min = 2.5°
ϕ and ω scans	h = −10→9
Absorption correction: multi-scan (SADABS; Bruker, 1998)	k = −11→11
T_min = 0.626, T_max = 0.747	l = −12→12
5297 measured reflections

Refinement top

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)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.084	H-atom parameters constrained
S = 1.14	w = 1/[σ²(F_o²) + (0.0297P)² + 0.608P] where P = (F_o² + 2F_c²)/3
2550 reflections	(Δ/σ)_max = 0.001
163 parameters	Δρ_max = 0.41 e Å⁻³
0 restraints	Δρ_min = −0.35 e Å⁻³

Crystal data top

[V₂F₂O₄(C₁₂H₈N₂)₂]	γ = 97.848 (2)°
M_r = 564.29	V = 528.46 (11) Å³
Triclinic, P1	Z = 1
a = 7.8320 (9) Å	Mo Kα radiation
b = 8.4937 (10) Å	µ = 0.95 mm⁻¹
c = 9.2007 (11) Å	T = 90 K
α = 113.741 (3)°	0.36 × 0.31 × 0.12 mm
β = 102.834 (2)°

Data collection top

Bruker APEX CCD diffractometer	2550 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 1998)	2502 reflections with I > 2σ(I)
T_min = 0.626, T_max = 0.747	R_int = 0.018
5297 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.034	0 restraints
wR(F²) = 0.084	H-atom parameters constrained
S = 1.14	Δρ_max = 0.41 e Å⁻³
2550 reflections	Δρ_min = −0.35 e Å⁻³
163 parameters

Special details top

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
V1	0.32341 (4)	0.84898 (4)	0.86984 (4)	0.01413 (10)
F1	0.43262 (16)	0.67119 (15)	0.83110 (14)	0.0199 (2)
O1	0.39833 (17)	0.97396 (17)	1.08350 (15)	0.0130 (3)
O2	0.11464 (19)	0.74797 (18)	0.82733 (18)	0.0182 (3)
N1	0.3194 (2)	0.8039 (2)	0.61559 (19)	0.0128 (3)
N2	0.2439 (2)	1.0719 (2)	0.83968 (19)	0.0131 (3)
C1	0.3604 (2)	0.6671 (2)	0.5064 (2)	0.0152 (4)
H1	0.3896	0.5771	0.5364	0.018*
C2	0.3623 (3)	0.6503 (3)	0.3487 (2)	0.0168 (4)
H2	0.3938	0.5514	0.2746	0.020*
C3	0.3182 (2)	0.7782 (3)	0.3023 (2)	0.0161 (4)
H3	0.3184	0.7682	0.1957	0.019*
C4	0.2724 (2)	0.9249 (2)	0.4151 (2)	0.0143 (3)
C5	0.2775 (2)	0.9315 (2)	0.5709 (2)	0.0121 (3)
C6	0.2197 (2)	1.0641 (3)	0.3789 (2)	0.0169 (4)
H6	0.2146	1.0606	0.2735	0.020*
C7	0.1770 (2)	1.2007 (3)	0.4937 (2)	0.0167 (4)
H7	0.1410	1.2904	0.4666	0.020*
C8	0.1852 (2)	1.2119 (2)	0.6554 (2)	0.0144 (3)
C9	0.2355 (2)	1.0768 (2)	0.6925 (2)	0.0126 (3)
C10	0.1417 (2)	1.3488 (2)	0.7797 (2)	0.0168 (4)
H10	0.1096	1.4451	0.7621	0.020*
C11	0.1464 (3)	1.3406 (3)	0.9264 (2)	0.0180 (4)
H11	0.1145	1.4302	1.0103	0.022*
C12	0.1982 (3)	1.2007 (2)	0.9531 (2)	0.0159 (4)
H12	0.2008	1.1976	1.0556	0.019*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
V1	0.01424 (17)	0.01694 (17)	0.01513 (17)	0.00489 (12)	0.00478 (12)	0.01048 (13)
F1	0.0238 (6)	0.0184 (5)	0.0203 (6)	0.0093 (5)	0.0074 (5)	0.0096 (5)
O1	0.0156 (6)	0.0145 (6)	0.0113 (6)	0.0054 (5)	0.0052 (5)	0.0070 (5)
O2	0.0174 (7)	0.0177 (6)	0.0218 (7)	0.0049 (5)	0.0070 (5)	0.0103 (6)
N1	0.0115 (7)	0.0145 (7)	0.0125 (7)	0.0039 (6)	0.0032 (6)	0.0060 (6)
N2	0.0123 (7)	0.0144 (7)	0.0120 (7)	0.0044 (6)	0.0033 (6)	0.0054 (6)
C1	0.0142 (8)	0.0153 (8)	0.0155 (9)	0.0053 (7)	0.0042 (7)	0.0059 (7)
C2	0.0153 (9)	0.0181 (9)	0.0121 (8)	0.0032 (7)	0.0049 (7)	0.0021 (7)
C3	0.0136 (8)	0.0210 (9)	0.0115 (8)	0.0022 (7)	0.0043 (7)	0.0059 (7)
C4	0.0100 (8)	0.0177 (8)	0.0139 (8)	0.0009 (6)	0.0023 (6)	0.0075 (7)
C5	0.0097 (8)	0.0137 (8)	0.0129 (8)	0.0028 (6)	0.0028 (6)	0.0064 (7)
C6	0.0129 (8)	0.0230 (9)	0.0171 (9)	0.0011 (7)	0.0024 (7)	0.0134 (8)
C7	0.0136 (8)	0.0182 (9)	0.0213 (9)	0.0024 (7)	0.0030 (7)	0.0134 (8)
C8	0.0098 (8)	0.0151 (8)	0.0176 (9)	0.0018 (6)	0.0017 (7)	0.0083 (7)
C9	0.0099 (8)	0.0137 (8)	0.0136 (8)	0.0025 (6)	0.0026 (6)	0.0061 (7)
C10	0.0123 (8)	0.0131 (8)	0.0231 (10)	0.0035 (7)	0.0015 (7)	0.0081 (7)
C11	0.0162 (9)	0.0154 (9)	0.0174 (9)	0.0067 (7)	0.0023 (7)	0.0031 (7)
C12	0.0159 (9)	0.0168 (8)	0.0132 (8)	0.0061 (7)	0.0038 (7)	0.0046 (7)

Geometric parameters (Å, º) top

V1—O2	1.6203 (14)	C3—H3	0.9500
V1—O1	1.7241 (13)	C4—C5	1.404 (2)
V1—F1	1.7871 (12)	C4—C6	1.438 (3)
V1—N2	2.1724 (16)	C5—C9	1.430 (2)
V1—N1	2.2052 (16)	C6—C7	1.360 (3)
V1—O1ⁱ	2.3162 (13)	C6—H6	0.9500
N1—C1	1.330 (2)	C7—C8	1.438 (3)
N1—C5	1.358 (2)	C7—H7	0.9500
N2—C12	1.329 (2)	C8—C9	1.402 (2)
N2—C9	1.359 (2)	C8—C10	1.409 (3)
C1—C2	1.403 (3)	C10—C11	1.373 (3)
C1—H1	0.9500	C10—H10	0.9500
C2—C3	1.376 (3)	C11—C12	1.400 (3)
C2—H2	0.9500	C11—H11	0.9500
C3—C4	1.415 (3)	C12—H12	0.9500

O2—V1—O1	104.98 (7)	C2—C3—H3	120.4
O2—V1—F1	102.29 (6)	C4—C3—H3	120.4
O1—V1—F1	104.75 (6)	C5—C4—C3	116.98 (17)
O2—V1—N2	91.64 (6)	C5—C4—C6	118.79 (17)
O1—V1—N2	90.52 (6)	C3—C4—C6	124.22 (17)
F1—V1—N2	155.64 (6)	N1—C5—C4	123.54 (17)
O2—V1—N1	98.29 (6)	N1—C5—C9	116.19 (16)
O1—V1—N1	152.31 (6)	C4—C5—C9	120.27 (16)
F1—V1—N1	84.36 (6)	C7—C6—C4	120.81 (17)
N2—V1—N1	73.81 (6)	C7—C6—H6	119.6
O2—V1—O1ⁱ	170.39 (6)	C4—C6—H6	119.6
O1—V1—O1ⁱ	76.95 (6)	C6—C7—C8	121.25 (17)
F1—V1—O1ⁱ	86.10 (5)	C6—C7—H7	119.4
N2—V1—O1ⁱ	78.88 (5)	C8—C7—H7	119.4
N1—V1—O1ⁱ	77.68 (5)	C9—C8—C10	117.11 (17)
V1—O1—V1ⁱ	103.05 (6)	C9—C8—C7	118.67 (17)
C1—N1—C5	118.04 (16)	C10—C8—C7	124.21 (17)
C1—N1—V1	125.58 (12)	N2—C9—C8	123.62 (17)
C5—N1—V1	116.33 (12)	N2—C9—C5	116.17 (16)
C12—N2—C9	117.95 (16)	C8—C9—C5	120.20 (17)
C12—N2—V1	124.57 (13)	C11—C10—C8	118.87 (17)
C9—N2—V1	117.45 (12)	C11—C10—H10	120.6
N1—C1—C2	122.64 (17)	C8—C10—H10	120.6
N1—C1—H1	118.7	C10—C11—C12	120.26 (18)
C2—C1—H1	118.7	C10—C11—H11	119.9
C3—C2—C1	119.50 (17)	C12—C11—H11	119.9
C3—C2—H2	120.2	N2—C12—C11	122.16 (18)
C1—C2—H2	120.2	N2—C12—H12	118.9
C2—C3—C4	119.27 (17)	C11—C12—H12	118.9

O2—V1—O1—V1ⁱ	−170.30 (6)	C1—N1—C5—C4	1.1 (3)
F1—V1—O1—V1ⁱ	82.35 (6)	V1—N1—C5—C4	178.74 (13)
N2—V1—O1—V1ⁱ	−78.46 (6)	C1—N1—C5—C9	−179.58 (16)
N1—V1—O1—V1ⁱ	−24.09 (15)	V1—N1—C5—C9	−1.9 (2)
O1ⁱ—V1—O1—V1ⁱ	0.0	C3—C4—C5—N1	−1.6 (3)
O2—V1—N1—C1	−91.43 (15)	C6—C4—C5—N1	177.65 (16)
O1—V1—N1—C1	121.45 (17)	C3—C4—C5—C9	179.14 (16)
F1—V1—N1—C1	10.21 (15)	C6—C4—C5—C9	−1.7 (3)
N2—V1—N1—C1	179.27 (16)	C5—C4—C6—C7	0.6 (3)
O1ⁱ—V1—N1—C1	97.44 (15)	C3—C4—C6—C7	179.75 (17)
O2—V1—N1—C5	91.11 (13)	C4—C6—C7—C8	0.8 (3)
O1—V1—N1—C5	−56.00 (19)	C6—C7—C8—C9	−1.1 (3)
F1—V1—N1—C5	−167.25 (13)	C6—C7—C8—C10	−179.54 (18)
N2—V1—N1—C5	1.81 (12)	C12—N2—C9—C8	1.4 (3)
O1ⁱ—V1—N1—C5	−80.02 (12)	V1—N2—C9—C8	179.58 (13)
O2—V1—N2—C12	78.41 (16)	C12—N2—C9—C5	−177.17 (16)
O1—V1—N2—C12	−26.60 (15)	V1—N2—C9—C5	1.0 (2)
F1—V1—N2—C12	−156.19 (15)	C10—C8—C9—N2	0.1 (3)
N1—V1—N2—C12	176.56 (16)	C7—C8—C9—N2	−178.51 (16)
O1ⁱ—V1—N2—C12	−103.19 (15)	C10—C8—C9—C5	178.59 (16)
O2—V1—N2—C9	−99.64 (13)	C7—C8—C9—C5	0.0 (3)
O1—V1—N2—C9	155.36 (13)	N1—C5—C9—N2	0.6 (2)
F1—V1—N2—C9	25.8 (2)	C4—C5—C9—N2	179.98 (16)
N1—V1—N2—C9	−1.48 (12)	N1—C5—C9—C8	−178.00 (16)
O1ⁱ—V1—N2—C9	78.77 (13)	C4—C5—C9—C8	1.4 (3)
C5—N1—C1—C2	0.1 (3)	C9—C8—C10—C11	−1.6 (3)
V1—N1—C1—C2	−177.28 (13)	C7—C8—C10—C11	176.93 (17)
N1—C1—C2—C3	−0.8 (3)	C8—C10—C11—C12	1.6 (3)
C1—C2—C3—C4	0.3 (3)	C9—N2—C12—C11	−1.4 (3)
C2—C3—C4—C5	0.8 (3)	V1—N2—C12—C11	−179.42 (14)
C2—C3—C4—C6	−178.35 (17)	C10—C11—C12—N2	−0.1 (3)

Symmetry code: (i) −x+1, −y+2, −z+2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2···F1ⁱⁱ	0.95	2.49	3.393 (2)	160
C3—H3···O1ⁱⁱⁱ	0.95	2.44	3.191 (2)	136
C6—H6···O1ⁱⁱⁱ	0.95	2.46	3.200 (2)	135
C10—H10···O2^iv	0.95	2.39	3.282 (2)	157

Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x, y, z−1; (iv) x, y+1, z.

Experimental details

Crystal data
Chemical formula	[V₂F₂O₄(C₁₂H₈N₂)₂]
M_r	564.29
Crystal system, space group	Triclinic, P1
Temperature (K)	90
a, b, c (Å)	7.8320 (9), 8.4937 (10), 9.2007 (11)
α, β, γ (°)	113.741 (3), 102.834 (2), 97.848 (2)
V (Å³)	528.46 (11)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	0.95
Crystal size (mm)	0.36 × 0.31 × 0.12

Data collection
Diffractometer	Bruker APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 1998)
T_min, T_max	0.626, 0.747
No. of measured, independent and observed [I > 2σ(I)] reflections	5297, 2550, 2502
R_int	0.018
(sin θ/λ)_max (Å⁻¹)	0.662

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.034, 0.084, 1.14
No. of reflections	2550
No. of parameters	163
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.41, −0.35

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), CrystalMaker (Palmer, 2006), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C2—H2···F1ⁱ	0.95	2.49	3.393 (2)	160.0
C3—H3···O1ⁱⁱ	0.95	2.44	3.191 (2)	135.9
C6—H6···O1ⁱⁱ	0.95	2.46	3.200 (2)	134.9
C10—H10···O2ⁱⁱⁱ	0.95	2.39	3.282 (2)	156.9

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y, z−1; (iii) x, y+1, z.

Acknowledgements

This work was supported by a grant from the National Science Foundation, CHE-0907787.

References

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Volume 66| Part 10| October 2010| Page m1303

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

A binuclear vanadium oxyfluoride: di-μ-oxido-bis­­[fluoridooxido(1,10-phenanthro­line)vanadium(V)]

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

A binuclear vanadium oxyfluoride: di-μ-oxido-bis[fluoridooxido(1,10-phenanthroline)vanadium(V)]