Poly[bis­(2,2′-bipyridine-κ2N,N′)deca-μ-oxido-dioxidodicopper(II)tetra­vanadium(V)]

Zhang, X.; Xia, W.; Xu, X.; Yi, Z.; Yang, C.

doi:10.1107/S1600536807067979

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 2| February 2008| Pages m287-m288

doi:10.1107/S1600536807067979

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Poly[bis(2,2′-bipyridine-κ²N,N′)deca-μ-oxido-dioxidodicopper(II)tetravanadium(V)]

Xiao Zhang,^a,^b Wujiong Xia,^a,^b ^* Xianzhu Xu,^a,^b Zhihui Yi ^c and Chao Yang ^a,^b

^aResearch Academy of Science and Technology, Harbin Institute of Technology, Harbin, Heilongjiang 150080, People's Republic of China, ^bState Key Laboratory of Applied Organic Chemistry, Lanzhou, Gansu 730000, People's Republic of China, and ^cState Key Laboratory of Polymer Physics and Chemistry, Changchun Institute of Applied Chemistry, Graduate School of the Chinese Academy of Sciences, Chinese Academy of Sciences, Changchun 130022, People's Republic of China
^*Correspondence e-mail: xiawj@hit.edu.cn

(Received 23 November 2007; accepted 21 December 2007; online 4 January 2008)

The title compound, [Cu₂V₄O₁₂(C₁₀H₈N₂)₂]_n, shows a two-dimensional copper–vanadate layer composed of eight-membered rings, each containing four corner-sharing VO₄ tetrahedra; these are linked through six pentacoordinated Cu^II atoms with the 2,2′-bipyridine ligands attached and pointing above and below the plane of the layer. The Cu atom is coordinated by two N donors from the 2,2′-bipyridine ligand and three O atoms from three adjacent VO₄ units to form a distorted tetragonal pyramid. These layers are further connected by π–π interactions between interleaving bipyridine ligands of adjacent layers [centroid–centroid distances = 3.63 (1) and 3.68 (1) Å] into a three-dimensional supramolecular structure.

Related literature

For related literature, see: DeBord et al. (1996 ); Kucsera et al. (2002 ); Lu et al. (2002 ); Yi et al. (2007 ).

Experimental

Crystal data

[Cu₂V₄O₁₂(C₁₀H₈N₂)₂]
M_r = 417.60
Triclinic, $[P \overline 1]$
a = 8.1019 (4) Å
b = 8.3122 (5) Å
c = 10.3501 (4) Å
α = 72.332 (3)°
β = 84.562 (3)°
γ = 77.878 (3)°
V = 648.98 (6) Å³
Z = 2
Mo Kα radiation
μ = 3.06 mm⁻¹
T = 298 (2) K
0.33 × 0.31 × 0.25 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2002 ) T_min = 0.379, T_max = 0.469
4603 measured reflections
3114 independent reflections
2553 reflections with I > 2σ(I)
R_int = 0.055

Refinement

R[F² > 2σ(F²)] = 0.034
wR(F²) = 0.084
S = 0.99
3114 reflections
190 parameters
H-atom parameters constrained
Δρ_max = 0.53 e Å⁻³
Δρ_min = −0.75 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Cu1—O1	2.012 (2)
Cu1—O4ⁱ	2.054 (2)
Cu1—O6ⁱⁱ	2.061 (2)
Cu1—N1	2.084 (2)
Cu1—N2	2.117 (2)
V1—O2	1.615 (2)
V1—O1	1.667 (2)
V1—O5ⁱⁱⁱ	1.824 (2)
V1—O3	1.833 (2)
V2—O4	1.655 (2)
V2—O6	1.670 (2)
V2—O5	1.774 (2)
V2—O3	1.790 (2)

O1—Cu1—O4ⁱ	89.62 (9)
O1—Cu1—O6ⁱⁱ	94.53 (9)
O4ⁱ—Cu1—O6ⁱⁱ	121.32 (9)
O1—Cu1—N1	100.17 (9)
O4ⁱ—Cu1—N1	124.55 (9)
O6ⁱⁱ—Cu1—N1	112.18 (9)
O1—Cu1—N2	172.29 (9)
O4ⁱ—Cu1—N2	85.25 (9)
O6ⁱⁱ—Cu1—N2	93.05 (9)
N1—Cu1—N2	78.18 (10)
O2—V1—O1	108.65 (12)
O2—V1—O5ⁱⁱⁱ	109.43 (12)
O1—V1—O5ⁱⁱⁱ	111.53 (11)
O2—V1—O3	107.98 (12)
O1—V1—O3	110.08 (11)
O5ⁱⁱⁱ—V1—O3	109.09 (10)
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) x, y-1, z; (iii) -x+2, -y+1, -z+1.

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807067979/hy2113sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536807067979/hy2113Isup2.hkl

checkCIF report

Comment top

Considerable efforts have been devoted to the hydrothermal synthesis of solid-state inorganic–organic hybrid vanadate(V) species based on discrete clusters, infinite chain and layer structures, such as [Zn(phen)₃][V₂O₆].10H₂O and [Cu(bipy)V₂O₆] (Yi et al., 2007), [Cu(bipy)][V₂O₆] and [Cu(bipy)₂][V₂O₆] (DeBord et al., 1996), [Mn(phen)₂]₂[V₄O₁₂].0.5H₂O (Lu et al., 2002), and [Co(phen)₂]₂[V₄O₁₂].H₂O (Kucsera et al., 2002), because of their diverse topologies and fascinating physical properties. We report here the crystal structure of a new complex, {[Cu(bipy)]₂V₄O₁₂}_n (bipy = 2,2'-bipyridine).

The asymmetric unit of the title compound consists of one Cu^II atom, one bipy molecule and a half of V₄O₁₂ unit (Fig. 1). The V₄O₁₂ units are linked through six square-pyramidal Cu^II atoms to six adjacent V₄O₁₂ rings (Fig. 2). Two of VO₄ units in the V₄O₁₂ unit each connect with one square-pyramidal Cu unit, while the other two VO₄ units each exhibit corner-sharing interactions with two Cu units. Each Cu unit links three V₄O₁₂ units through corner-sharing interactions. In this way, a two-dimensional layer is formed (Fig. 2). The Cu^II atom is coordinated by two pyridine N atoms and three tetravanadate O atoms (Fig. 1 and Table 1). The relative orientation of the bipy ligand with respect to the copper–vanadate layer is depicted by a dihedral angel of 84.6 (6)°. Furthermore, these bipy ligands interact with each other through π–π interactions between adjacent layers with centroid–centroid distances of 3.63 (1) and 3.68 (1) Å.

Related literature top

For related literature, see: DeBord et al. (1996); Kucsera et al. (2002); Lu et al. (2002); Yi et al. (2007).

Experimental top

The title compound was prepared hydrothermally from a mixture of V₂O₅ (0.73 g, 4.0 mmol), 2,2'-bipyridine dihydrate (0.38 g, 2.0 mmol), CuCl₂.2H₂O (0.34 g, 2.0 mmol) and water (18 ml) (molar ratio 2:1:1:500), adjusting pH to ca 6.1 with 4 M KOH, in a 25 ml Teflon-lined stainless steel reactor heated to 443 K for 7 d. After cooling to room temperature, green crystals were collected.

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top

	Fig. 1. The asymmetric unit of the title compound, extended to show the V₄O₁₂ unit. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) 1 - x, 1 - y, 1 - z; (ii) x, y - 1, z; (iii) 2 - x, 1 - y, 1 - z.]
	Fig. 2. A view of the copper–vanadate layer with C and H atoms of the bipy ligands omitted for clarity.

poly[bis(2,2'-bipyridine-κ²N,N')deca-µ-oxido- dioxidodicopper(II)tetravanadium(V)], top

Crystal data top

[Cu₂V₄O₁₂(C₁₀H₈N₂)₂]	Z = 2
M_r = 417.60	F(000) = 410
Triclinic, P1	D_x = 2.137 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.1019 (4) Å	Cell parameters from 3811 reflections
b = 8.3122 (5) Å	θ = 2.1–28.3°
c = 10.3501 (4) Å	µ = 3.06 mm⁻¹
α = 72.332 (3)°	T = 298 K
β = 84.562 (3)°	Block, green
γ = 77.878 (3)°	0.33 × 0.31 × 0.25 mm
V = 648.98 (6) Å³

Data collection top

Bruker SMART APEX CCD diffractometer	3114 independent reflections
Radiation source: fine-focus sealed tube	2553 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.055
ϕ and ω scans	θ_max = 28.3°, θ_min = 2.1°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −10→9
T_min = 0.379, T_max = 0.469	k = −10→7
4603 measured reflections	l = −13→12

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 = 0.99	w = 1/[σ²(F_o²) + (0.0438P)²] where P = (F_o² + 2F_c²)/3
3114 reflections	(Δ/σ)_max = 0.001
190 parameters	Δρ_max = 0.53 e Å⁻³
0 restraints	Δρ_min = −0.75 e Å⁻³

Crystal data top

[Cu₂V₄O₁₂(C₁₀H₈N₂)₂]	γ = 77.878 (3)°
M_r = 417.60	V = 648.98 (6) Å³
Triclinic, P1	Z = 2
a = 8.1019 (4) Å	Mo Kα radiation
b = 8.3122 (5) Å	µ = 3.06 mm⁻¹
c = 10.3501 (4) Å	T = 298 K
α = 72.332 (3)°	0.33 × 0.31 × 0.25 mm
β = 84.562 (3)°

Data collection top

Bruker SMART APEX CCD diffractometer	3114 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2002)	2553 reflections with I > 2σ(I)
T_min = 0.379, T_max = 0.469	R_int = 0.055
4603 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.034	0 restraints
wR(F²) = 0.084	H-atom parameters constrained
S = 0.99	Δρ_max = 0.53 e Å⁻³
3114 reflections	Δρ_min = −0.75 e Å⁻³
190 parameters

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

	x	y	z	U_iso*/U_eq
Cu1	0.59216 (4)	0.14236 (4)	0.28662 (3)	0.01368 (10)
V1	0.87679 (6)	0.39002 (6)	0.34998 (5)	0.01604 (12)
V2	0.73879 (6)	0.72867 (6)	0.47736 (5)	0.01495 (12)
O1	0.7741 (3)	0.2421 (3)	0.3367 (2)	0.0249 (5)
O2	0.9198 (3)	0.5062 (3)	0.1993 (2)	0.0359 (6)
O3	0.7425 (3)	0.5317 (3)	0.4394 (2)	0.0259 (5)
O4	0.5705 (3)	0.7685 (3)	0.5748 (2)	0.0270 (5)
O5	0.9278 (3)	0.7084 (3)	0.5595 (2)	0.0285 (5)
O6	0.7286 (3)	0.8942 (3)	0.3363 (2)	0.0247 (5)
N1	0.5900 (3)	0.2590 (3)	0.0777 (2)	0.0191 (5)
N2	0.3794 (3)	0.0700 (3)	0.2320 (2)	0.0202 (5)
C1	0.7065 (4)	0.3461 (4)	0.0041 (3)	0.0242 (6)
H1	0.7903	0.3671	0.0489	0.029*
C2	0.7057 (4)	0.4056 (4)	−0.1364 (3)	0.0300 (7)
H2	0.7869	0.4667	−0.1848	0.036*
C3	0.5828 (4)	0.3731 (4)	−0.2037 (3)	0.0270 (7)
H3	0.5811	0.4107	−0.2980	0.032*
C4	0.4620 (4)	0.2835 (4)	−0.1289 (3)	0.0232 (6)
H4	0.3787	0.2594	−0.1722	0.028*
C5	0.4675 (4)	0.2303 (4)	0.0120 (3)	0.0192 (6)
C6	0.3397 (4)	0.1390 (4)	0.1003 (3)	0.0187 (6)
C7	0.1878 (4)	0.1270 (4)	0.0534 (3)	0.0288 (7)
H7	0.1610	0.1775	−0.0372	0.035*
C8	0.0781 (4)	0.0386 (4)	0.1448 (4)	0.0309 (7)
H8	−0.0237	0.0290	0.1160	0.037*
C9	0.1209 (4)	−0.0351 (4)	0.2786 (3)	0.0274 (7)
H9	0.0492	−0.0962	0.3409	0.033*
C10	0.2718 (4)	−0.0166 (4)	0.3187 (3)	0.0247 (6)
H10	0.3001	−0.0660	0.4091	0.030*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.01353 (17)	0.01631 (18)	0.01260 (17)	−0.00306 (12)	−0.00204 (12)	−0.00563 (13)
V1	0.0140 (2)	0.0172 (2)	0.0183 (2)	−0.00322 (18)	−0.00335 (18)	−0.00613 (19)
V2	0.0127 (2)	0.0155 (2)	0.0177 (2)	−0.00107 (17)	−0.00215 (18)	−0.00696 (18)
O1	0.0202 (11)	0.0282 (12)	0.0335 (12)	−0.0079 (9)	−0.0034 (9)	−0.0167 (10)
O2	0.0332 (14)	0.0428 (14)	0.0249 (12)	−0.0122 (11)	−0.0004 (10)	0.0031 (11)
O3	0.0243 (12)	0.0225 (11)	0.0346 (13)	−0.0036 (9)	0.0016 (10)	−0.0154 (10)
O4	0.0201 (11)	0.0366 (13)	0.0301 (12)	−0.0050 (9)	0.0047 (9)	−0.0201 (10)
O5	0.0228 (12)	0.0308 (12)	0.0346 (13)	−0.0013 (9)	−0.0112 (10)	−0.0128 (10)
O6	0.0245 (11)	0.0204 (11)	0.0266 (11)	−0.0018 (9)	−0.0051 (9)	−0.0034 (9)
N1	0.0195 (12)	0.0206 (12)	0.0179 (12)	−0.0040 (10)	−0.0029 (10)	−0.0059 (10)
N2	0.0225 (13)	0.0233 (13)	0.0178 (12)	−0.0065 (10)	−0.0011 (10)	−0.0088 (10)
C1	0.0211 (15)	0.0252 (16)	0.0269 (16)	−0.0057 (12)	−0.0012 (12)	−0.0077 (13)
C2	0.0264 (17)	0.0326 (18)	0.0299 (17)	−0.0117 (14)	0.0065 (14)	−0.0058 (14)
C3	0.0328 (18)	0.0269 (16)	0.0177 (15)	−0.0036 (13)	−0.0008 (13)	−0.0027 (12)
C4	0.0261 (16)	0.0256 (16)	0.0199 (15)	−0.0037 (12)	−0.0050 (12)	−0.0090 (12)
C5	0.0181 (14)	0.0190 (14)	0.0211 (14)	−0.0013 (11)	−0.0044 (11)	−0.0072 (11)
C6	0.0188 (14)	0.0207 (14)	0.0188 (14)	−0.0048 (11)	−0.0023 (11)	−0.0078 (11)
C7	0.0270 (17)	0.0350 (18)	0.0252 (16)	−0.0084 (14)	−0.0101 (13)	−0.0056 (14)
C8	0.0204 (16)	0.0381 (19)	0.0376 (19)	−0.0095 (14)	−0.0062 (14)	−0.0118 (15)
C9	0.0242 (16)	0.0299 (17)	0.0318 (18)	−0.0129 (13)	0.0058 (13)	−0.0110 (14)
C10	0.0263 (17)	0.0295 (17)	0.0192 (14)	−0.0094 (13)	0.0023 (12)	−0.0065 (12)

Geometric parameters (Å, º) top

Cu1—O1	2.012 (2)	N2—C6	1.350 (4)
Cu1—O4ⁱ	2.054 (2)	C1—C2	1.387 (4)
Cu1—O6ⁱⁱ	2.061 (2)	C1—H1	0.9300
Cu1—N1	2.084 (2)	C2—C3	1.381 (5)
Cu1—N2	2.117 (2)	C2—H2	0.9300
V1—O2	1.615 (2)	C3—C4	1.388 (5)
V1—O1	1.667 (2)	C3—H3	0.9300
V1—O5ⁱⁱⁱ	1.824 (2)	C4—C5	1.392 (4)
V1—O3	1.833 (2)	C4—H4	0.9300
V2—O4	1.655 (2)	C5—C6	1.488 (4)
V2—O6	1.670 (2)	C6—C7	1.397 (4)
V2—O5	1.774 (2)	C7—C8	1.384 (5)
V2—O3	1.790 (2)	C7—H7	0.9300
O4—Cu1ⁱ	2.054 (2)	C8—C9	1.379 (5)
O5—V1ⁱⁱⁱ	1.824 (2)	C8—H8	0.9300
O6—Cu1^iv	2.061 (2)	C9—C10	1.379 (4)
N1—C1	1.346 (4)	C9—H9	0.9300
N1—C5	1.352 (4)	C10—H10	0.9300
N2—C10	1.344 (4)

O1—Cu1—O4ⁱ	89.62 (9)	C6—N2—Cu1	114.9 (2)
O1—Cu1—O6ⁱⁱ	94.53 (9)	N1—C1—C2	122.1 (3)
O4ⁱ—Cu1—O6ⁱⁱ	121.32 (9)	N1—C1—H1	118.9
O1—Cu1—N1	100.17 (9)	C2—C1—H1	118.9
O4ⁱ—Cu1—N1	124.55 (9)	C3—C2—C1	119.2 (3)
O6ⁱⁱ—Cu1—N1	112.18 (9)	C3—C2—H2	120.4
O1—Cu1—N2	172.29 (9)	C1—C2—H2	120.4
O4ⁱ—Cu1—N2	85.25 (9)	C2—C3—C4	119.1 (3)
O6ⁱⁱ—Cu1—N2	93.05 (9)	C2—C3—H3	120.4
N1—Cu1—N2	78.18 (10)	C4—C3—H3	120.4
O2—V1—O1	108.65 (12)	C3—C4—C5	118.9 (3)
O2—V1—O5ⁱⁱⁱ	109.43 (12)	C3—C4—H4	120.6
O1—V1—O5ⁱⁱⁱ	111.53 (11)	C5—C4—H4	120.6
O2—V1—O3	107.98 (12)	N1—C5—C4	121.9 (3)
O1—V1—O3	110.08 (11)	N1—C5—C6	115.6 (3)
O5ⁱⁱⁱ—V1—O3	109.09 (10)	C4—C5—C6	122.5 (3)
O4—V2—O6	107.88 (11)	N2—C6—C7	121.6 (3)
O4—V2—O5	111.20 (11)	N2—C6—C5	114.8 (2)
O6—V2—O5	108.55 (11)	C7—C6—C5	123.6 (3)
O4—V2—O3	109.63 (11)	C8—C7—C6	118.6 (3)
O6—V2—O3	111.29 (11)	C8—C7—H7	120.7
O5—V2—O3	108.30 (10)	C6—C7—H7	120.7
V1—O1—Cu1	159.01 (14)	C9—C8—C7	119.6 (3)
V2—O3—V1	139.64 (14)	C9—C8—H8	120.2
V2—O4—Cu1ⁱ	162.64 (14)	C7—C8—H8	120.2
V2—O5—V1ⁱⁱⁱ	160.20 (14)	C8—C9—C10	118.9 (3)
V2—O6—Cu1^iv	133.16 (13)	C8—C9—H9	120.6
C1—N1—C5	118.7 (3)	C10—C9—H9	120.6
C1—N1—Cu1	125.5 (2)	N2—C10—C9	122.5 (3)
C5—N1—Cu1	115.6 (2)	N2—C10—H10	118.7
C10—N2—C6	118.8 (3)	C9—C10—H10	118.7
C10—N2—Cu1	125.7 (2)

O2—V1—O1—Cu1	−60.3 (4)	N1—Cu1—N2—C10	−175.0 (3)
O5ⁱⁱⁱ—V1—O1—Cu1	179.0 (4)	O4ⁱ—Cu1—N2—C6	122.4 (2)
O3—V1—O1—Cu1	57.8 (4)	O6ⁱⁱ—Cu1—N2—C6	−116.4 (2)
O4ⁱ—Cu1—O1—V1	−68.8 (4)	N1—Cu1—N2—C6	−4.4 (2)
O6ⁱⁱ—Cu1—O1—V1	169.8 (4)	C5—N1—C1—C2	−0.6 (5)
N1—Cu1—O1—V1	56.3 (4)	Cu1—N1—C1—C2	173.5 (2)
O4—V2—O3—V1	−176.89 (19)	N1—C1—C2—C3	−0.8 (5)
O6—V2—O3—V1	63.8 (2)	C1—C2—C3—C4	0.8 (5)
O5—V2—O3—V1	−55.4 (2)	C2—C3—C4—C5	0.5 (5)
O2—V1—O3—V2	−51.5 (2)	C1—N1—C5—C4	2.0 (4)
O1—V1—O3—V2	−169.94 (19)	Cu1—N1—C5—C4	−172.6 (2)
O5ⁱⁱⁱ—V1—O3—V2	67.4 (2)	C1—N1—C5—C6	−177.8 (3)
O6—V2—O4—Cu1ⁱ	−84.8 (5)	Cu1—N1—C5—C6	7.5 (3)
O5—V2—O4—Cu1ⁱ	34.1 (5)	C3—C4—C5—N1	−2.0 (4)
O3—V2—O4—Cu1ⁱ	153.8 (4)	C3—C4—C5—C6	177.9 (3)
O4—V2—O5—V1ⁱⁱⁱ	104.6 (4)	C10—N2—C6—C7	2.1 (4)
O6—V2—O5—V1ⁱⁱⁱ	−136.9 (4)	Cu1—N2—C6—C7	−169.2 (2)
O3—V2—O5—V1ⁱⁱⁱ	−15.9 (5)	C10—N2—C6—C5	−179.3 (3)
O4—V2—O6—Cu1^iv	17.23 (19)	Cu1—N2—C6—C5	9.5 (3)
O5—V2—O6—Cu1^iv	−103.38 (17)	N1—C5—C6—N2	−11.3 (4)
O3—V2—O6—Cu1^iv	137.53 (15)	C4—C5—C6—N2	168.8 (3)
O1—Cu1—N1—C1	11.4 (3)	N1—C5—C6—C7	167.3 (3)
O4ⁱ—Cu1—N1—C1	108.1 (2)	C4—C5—C6—C7	−12.5 (5)
O6ⁱⁱ—Cu1—N1—C1	−87.8 (3)	N2—C6—C7—C8	−1.5 (5)
N2—Cu1—N1—C1	−176.2 (3)	C5—C6—C7—C8	180.0 (3)
O1—Cu1—N1—C5	−174.30 (19)	C6—C7—C8—C9	0.0 (5)
O4ⁱ—Cu1—N1—C5	−77.7 (2)	C7—C8—C9—C10	0.9 (5)
O6ⁱⁱ—Cu1—N1—C5	86.5 (2)	C6—N2—C10—C9	−1.2 (5)
N2—Cu1—N1—C5	−1.97 (19)	Cu1—N2—C10—C9	169.1 (2)
O4ⁱ—Cu1—N2—C10	−48.2 (3)	C8—C9—C10—N2	−0.3 (5)
O6ⁱⁱ—Cu1—N2—C10	73.0 (3)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y−1, z; (iii) −x+2, −y+1, −z+1; (iv) x, y+1, z.

Experimental details

Crystal data
Chemical formula	[Cu₂V₄O₁₂(C₁₀H₈N₂)₂]
M_r	417.60
Crystal system, space group	Triclinic, P1
Temperature (K)	298
a, b, c (Å)	8.1019 (4), 8.3122 (5), 10.3501 (4)
α, β, γ (°)	72.332 (3), 84.562 (3), 77.878 (3)
V (Å³)	648.98 (6)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	3.06
Crystal size (mm)	0.33 × 0.31 × 0.25

Data collection
Diffractometer	Bruker SMART APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2002)
T_min, T_max	0.379, 0.469
No. of measured, independent and observed [I > 2σ(I)] reflections	4603, 3114, 2553
R_int	0.055
(sin θ/λ)_max (Å⁻¹)	0.666

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.034, 0.084, 0.99
No. of reflections	3114
No. of parameters	190
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.53, −0.75

Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 1999).

Selected geometric parameters (Å, º) top

Cu1—O1	2.012 (2)	V1—O5ⁱⁱⁱ	1.824 (2)
Cu1—O4ⁱ	2.054 (2)	V1—O3	1.833 (2)
Cu1—O6ⁱⁱ	2.061 (2)	V2—O4	1.655 (2)
Cu1—N1	2.084 (2)	V2—O6	1.670 (2)
Cu1—N2	2.117 (2)	V2—O5	1.774 (2)
V1—O2	1.615 (2)	V2—O3	1.790 (2)
V1—O1	1.667 (2)

O1—Cu1—O4ⁱ	89.62 (9)	O6ⁱⁱ—Cu1—N2	93.05 (9)
O1—Cu1—O6ⁱⁱ	94.53 (9)	N1—Cu1—N2	78.18 (10)
O4ⁱ—Cu1—O6ⁱⁱ	121.32 (9)	O2—V1—O1	108.65 (12)
O1—Cu1—N1	100.17 (9)	O2—V1—O5ⁱⁱⁱ	109.43 (12)
O4ⁱ—Cu1—N1	124.55 (9)	O1—V1—O5ⁱⁱⁱ	111.53 (11)
O6ⁱⁱ—Cu1—N1	112.18 (9)	O2—V1—O3	107.98 (12)
O1—Cu1—N2	172.29 (9)	O1—V1—O3	110.08 (11)
O4ⁱ—Cu1—N2	85.25 (9)	O5ⁱⁱⁱ—V1—O3	109.09 (10)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y−1, z; (iii) −x+2, −y+1, −z+1.

Acknowledgements

This work was supported by the New Century Talent Program of the Chinese Ministry of Education and the Postdoctoral Foundation of Heilongjiang Province.

References

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