Literature DB >> 21579931

Poly[bis(2,2'-bipyridine-κN,N')heptadeca-μ-oxido-tetraoxidodicopper(II)divanadate(IV)hexavanadate(V)].

Hai-Hui Yu, Li Kong.   

Abstract

In the title complex, [Cu(2)V(8)O(21)(2,2'-bpy)(2)](n) (bpy = bipyridine, C(10)H(8)N(2)), the asymmetric unit contains four independent V atoms briged by 11 O atoms, one of which lies on an inversion center, and a [Cu(2,2'-bpy)](2+) unit. Three V atoms in the polyoxoanion exhibit distorted tetra-hedral coordination geometries while the fourth V atom adopts a trigonal-bipyramidal geometry. The Cu atom adopts a square-pyramidal geometry being coordinated by two nitro-gen donors of a 2,2'-bpy ligand, and three bridging O atoms which are linked with V atoms. The V(8) polyoxoanion is connected to [Cu(2,2'-bpy)](2+) cations, resulting in a two-dimensional layer structure extending parallel to (010). C-H⋯O hydrogen bonding consolidates the structure.

Entities:  

Year:  2009        PMID： 21579931      PMCID： PMC2980047          DOI： 10.1107/S1600536809052118

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For hybrid organic-inorganic vanadium oxides, see: Zapf et al. (1997 ▶); Liu et al. (2001 ▶, 2002 ▶); Yuan et al. (2002 ▶). For the organic substituents, see: Girginova et al. (2005 ▶); Paz & Klinowski (2003 ▶); Shi et al. (2005 ▶).

Experimental

Crystal data

[Cu2V8O21(C10H8N2)2] M = 591.48 Triclinic, a = 8.0721 (16) Å b = 9.764 (2) Å c = 11.607 (2) Å α = 85.58 (3)° β = 72.79 (3)° γ = 72.28 (3)° V = 832.4 (3) Å3 Z = 2 Mo Kα radiation μ = 3.48 mm−1 T = 293 K 0.20 × 0.18 × 0.16 mm

Data collection

Rigaku R-AXIS RAPID diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.504, T max = 0.573 7138 measured reflections 3261 independent reflections 2916 reflections with I > 2σ(I) R int = 0.018

Refinement

R[F 2 > 2σ(F 2)] = 0.024 wR(F 2) = 0.056 S = 1.06 3261 reflections 282 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.39 e Å−3 Δρmin = −0.37 e Å−3 Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Burnett & Johnson, 1996 ▶); software used to prepare material for publication: SHELXTL97. Crystal structure: contains datablocks I, New_Global_Publ_Block. DOI: 10.1107/S1600536809052118/pv2241sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809052118/pv2241Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cu2V8O21(C10H8N2)2]Z = 2
Mr = 591.48F(000) = 574
Triclinic, P1Dx = 2.360 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.0721 (16) ÅCell parameters from 3536 reflections
b = 9.764 (2) Åθ = 2.8–26.1°
c = 11.607 (2) ŵ = 3.48 mm−1
α = 85.58 (3)°T = 293 K
β = 72.79 (3)°Block, brown
γ = 72.28 (3)°0.20 × 0.18 × 0.16 mm
V = 832.4 (3) Å3
Rigaku R-AXIS RAPID diffractometer3261 independent reflections
Radiation source: fine-focus sealed tube2916 reflections with I > 2σ(I)
graphiteRint = 0.018
Detector resolution: 10 pixels mm-1θmax = 26.1°, θmin = 2.2°
ω scansh = −9→9
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)k = −12→12
Tmin = 0.504, Tmax = 0.573l = −14→14
7138 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.056H atoms treated by a mixture of independent and constrained refinement
S = 1.06w = 1/[σ2(Fo2) + (0.0235P)2 + 0.7292P] where P = (Fo2 + 2Fc2)/3
3261 reflections(Δ/σ)max = 0.001
282 parametersΔρmax = 0.39 e Å−3
0 restraintsΔρmin = −0.37 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.
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 > 2sigma(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.
xyzUiso*/Ueq
C10.2395 (4)0.5437 (3)0.9302 (3)0.0289 (7)
C20.2805 (5)0.4323 (3)1.0073 (3)0.0320 (7)
C30.4432 (5)0.3260 (3)0.9710 (3)0.0317 (7)
C40.5612 (4)0.3335 (3)0.8579 (3)0.0274 (6)
C50.5109 (4)0.4469 (3)0.7846 (2)0.0198 (6)
C60.6235 (4)0.4644 (3)0.6616 (2)0.0201 (6)
C70.7827 (4)0.3634 (3)0.6024 (3)0.0284 (7)
C80.8728 (4)0.3894 (3)0.4858 (3)0.0322 (7)
C90.8050 (4)0.5152 (3)0.4314 (3)0.0306 (7)
C100.6460 (4)0.6144 (3)0.4955 (3)0.0265 (6)
Cu10.31722 (4)0.71169 (3)0.70685 (3)0.01922 (9)
H10.128 (4)0.617 (3)0.952 (3)0.029 (8)*
H20.200 (4)0.430 (3)1.081 (3)0.029 (8)*
H30.472 (4)0.254 (4)1.021 (3)0.033 (9)*
H40.668 (4)0.267 (3)0.832 (3)0.029 (8)*
H50.823 (4)0.284 (4)0.644 (3)0.036 (9)*
H60.987 (4)0.315 (3)0.445 (3)0.029 (8)*
H70.865 (4)0.532 (3)0.356 (3)0.027 (8)*
H80.591 (4)0.703 (3)0.461 (3)0.026 (8)*
N10.3521 (3)0.5516 (2)0.8213 (2)0.0210 (5)
N20.5557 (3)0.5887 (2)0.6079 (2)0.0205 (5)
O10.4258 (3)0.8537 (2)0.79009 (18)0.0333 (5)
O20.3334 (3)1.0721 (2)0.41281 (17)0.0276 (4)
O30.3006 (3)0.8439 (2)0.57234 (18)0.0270 (4)
O40.0648 (3)0.8000 (2)0.79171 (18)0.0296 (5)
O50.00001.00000.50000.0330 (7)
O60.0361 (3)1.3383 (2)0.81792 (17)0.0274 (5)
O7−0.3076 (3)0.9544 (2)0.82587 (18)0.0308 (5)
O80.3910 (2)1.1332 (2)0.75539 (17)0.0262 (4)
O90.1379 (3)1.1176 (2)0.65337 (16)0.0244 (4)
O10−0.0633 (3)1.0792 (2)0.87494 (17)0.0247 (4)
O11−0.1608 (3)0.8630 (2)1.02173 (17)0.0284 (5)
V10.54061 (6)0.96749 (5)0.74290 (4)0.01637 (11)
V20.12848 (6)1.16967 (5)0.81859 (4)0.01575 (10)
V3−0.11097 (6)0.92167 (5)0.87896 (4)0.01417 (10)
V40.19437 (6)1.00633 (5)0.53774 (4)0.01430 (10)
U11U22U33U12U13U23
C10.0296 (16)0.0257 (16)0.0275 (16)−0.0045 (14)−0.0062 (13)0.0000 (13)
C20.0417 (19)0.0330 (17)0.0197 (16)−0.0140 (15)−0.0046 (14)0.0047 (13)
C30.0436 (19)0.0250 (16)0.0297 (17)−0.0111 (14)−0.0167 (15)0.0108 (13)
C40.0263 (16)0.0228 (15)0.0316 (17)−0.0029 (13)−0.0113 (13)0.0033 (12)
C50.0228 (14)0.0174 (13)0.0222 (14)−0.0052 (11)−0.0113 (11)−0.0006 (11)
C60.0199 (14)0.0171 (13)0.0243 (14)−0.0036 (11)−0.0095 (11)−0.0003 (11)
C70.0241 (15)0.0252 (16)0.0335 (17)−0.0007 (13)−0.0115 (13)0.0008 (13)
C80.0220 (15)0.0311 (17)0.0360 (18)−0.0008 (13)−0.0030 (14)−0.0057 (14)
C90.0281 (16)0.0340 (17)0.0266 (17)−0.0104 (14)−0.0017 (13)−0.0011 (13)
C100.0281 (16)0.0274 (16)0.0238 (15)−0.0085 (13)−0.0079 (13)0.0045 (12)
Cu10.01834 (17)0.01617 (17)0.02058 (18)−0.00094 (13)−0.00635 (13)0.00129 (13)
N10.0232 (12)0.0174 (11)0.0210 (12)−0.0046 (9)−0.0061 (10)0.0021 (9)
N20.0209 (12)0.0172 (11)0.0233 (12)−0.0040 (9)−0.0080 (10)0.0016 (9)
O10.0460 (13)0.0461 (13)0.0204 (10)−0.0322 (11)−0.0096 (10)0.0041 (9)
O20.0322 (11)0.0334 (11)0.0166 (10)−0.0143 (9)−0.0020 (8)0.0021 (8)
O30.0280 (11)0.0242 (10)0.0260 (11)−0.0007 (9)−0.0119 (9)0.0042 (8)
O40.0204 (10)0.0293 (11)0.0314 (12)0.0006 (9)−0.0038 (9)−0.0022 (9)
O50.0244 (15)0.0468 (19)0.0342 (17)−0.0099 (14)−0.0179 (13)−0.0021 (14)
O60.0340 (11)0.0217 (10)0.0213 (10)−0.0047 (9)−0.0038 (9)0.0000 (8)
O70.0211 (10)0.0457 (13)0.0304 (12)−0.0080 (9)−0.0159 (9)−0.0024 (10)
O80.0198 (10)0.0335 (11)0.0233 (10)−0.0052 (9)−0.0064 (8)0.0014 (9)
O90.0282 (11)0.0295 (11)0.0163 (10)−0.0069 (9)−0.0084 (8)−0.0033 (8)
O100.0246 (10)0.0259 (10)0.0267 (11)−0.0124 (9)−0.0075 (8)0.0029 (8)
O110.0348 (12)0.0411 (12)0.0181 (10)−0.0201 (10)−0.0132 (9)0.0078 (9)
V10.0148 (2)0.0247 (2)0.0129 (2)−0.00865 (19)−0.00619 (17)0.00187 (17)
V20.0192 (2)0.0173 (2)0.0117 (2)−0.00599 (18)−0.00523 (17)0.00065 (17)
V30.0121 (2)0.0199 (2)0.0120 (2)−0.00499 (17)−0.00582 (16)0.00196 (17)
V40.0136 (2)0.0184 (2)0.0109 (2)−0.00274 (17)−0.00571 (17)0.00037 (16)
C1—N11.333 (4)Cu1—N21.991 (2)
C1—C21.378 (4)Cu1—O12.252 (2)
C1—H10.94 (3)O1—V11.621 (2)
C2—C31.375 (5)O2—V41.763 (2)
C2—H20.91 (3)O2—V1i1.797 (2)
C3—C41.387 (4)O3—V41.6398 (19)
C3—H30.90 (3)O4—V31.661 (2)
C4—C51.379 (4)O5—V4ii1.7684 (6)
C4—H40.89 (3)O5—V41.7684 (6)
C5—N11.348 (3)O6—V21.588 (2)
C5—C61.477 (4)O7—V1iii1.7405 (19)
C6—N21.357 (3)O7—V31.8003 (19)
C6—C71.381 (4)O8—V11.686 (2)
C7—C81.379 (4)O8—V21.953 (2)
C7—H50.91 (3)O9—V41.6586 (19)
C8—C91.372 (4)O9—V21.9957 (19)
C8—H60.99 (3)O10—V31.6894 (19)
C9—C101.389 (4)O10—V21.936 (2)
C9—H70.89 (3)O11—V31.6840 (19)
C10—N21.340 (4)O11—V2iv1.9363 (19)
C10—H80.96 (3)V1—O7v1.7405 (19)
Cu1—O41.934 (2)V1—O2i1.797 (2)
Cu1—O31.957 (2)V2—O11iv1.9363 (19)
Cu1—N11.980 (2)
N1—C1—C2122.2 (3)C5—N1—Cu1114.58 (18)
N1—C1—H1116.7 (19)C10—N2—C6119.3 (2)
C2—C1—H1121.0 (19)C10—N2—Cu1126.54 (19)
C3—C2—C1118.9 (3)C6—N2—Cu1114.11 (18)
C3—C2—H2121 (2)V1—O1—Cu1136.75 (11)
C1—C2—H2120 (2)V4—O2—V1i142.02 (12)
C2—C3—C4119.2 (3)V4—O3—Cu1143.18 (12)
C2—C3—H3119 (2)V3—O4—Cu1156.12 (13)
C4—C3—H3121 (2)V4ii—O5—V4180.0
C5—C4—C3118.9 (3)V1iii—O7—V3166.30 (13)
C5—C4—H4120 (2)V1—O8—V2123.33 (11)
C3—C4—H4121 (2)V4—O9—V2154.58 (12)
N1—C5—C4121.5 (3)V3—O10—V2143.70 (12)
N1—C5—C6114.8 (2)V3—O11—V2iv153.85 (12)
C4—C5—C6123.7 (3)O1—V1—O8107.63 (11)
N2—C6—C7121.4 (3)O1—V1—O7v110.71 (11)
N2—C6—C5114.4 (2)O8—V1—O7v111.38 (10)
C7—C6—C5124.2 (3)O1—V1—O2i108.79 (10)
C8—C7—C6119.0 (3)O8—V1—O2i109.54 (10)
C8—C7—H5124 (2)O7v—V1—O2i108.75 (10)
C6—C7—H5117 (2)O6—V2—O11iv103.25 (10)
C9—C8—C7119.8 (3)O6—V2—O10107.76 (10)
C9—C8—H6122.7 (18)O11iv—V2—O1086.50 (9)
C7—C8—H6117.5 (18)O6—V2—O8107.90 (10)
C8—C9—C10119.0 (3)O11iv—V2—O887.79 (9)
C8—C9—H7119 (2)O10—V2—O8144.26 (9)
C10—C9—H7122 (2)O6—V2—O999.91 (10)
N2—C10—C9121.5 (3)O11iv—V2—O9156.82 (9)
N2—C10—H8116.0 (18)O10—V2—O985.62 (9)
C9—C10—H8122.4 (18)O8—V2—O985.96 (9)
O4—Cu1—O391.37 (9)O4—V3—O11110.09 (11)
O4—Cu1—N194.77 (10)O4—V3—O10110.01 (10)
O3—Cu1—N1170.15 (9)O11—V3—O10110.08 (10)
O4—Cu1—N2167.12 (9)O4—V3—O7110.49 (10)
O3—Cu1—N290.36 (9)O11—V3—O7108.55 (10)
N1—Cu1—N281.96 (10)O10—V3—O7107.58 (10)
O4—Cu1—O195.62 (9)O3—V4—O9109.67 (10)
O3—Cu1—O190.80 (8)O3—V4—O2111.30 (10)
N1—Cu1—O196.24 (9)O9—V4—O2107.76 (10)
N2—Cu1—O197.12 (9)O3—V4—O5108.67 (8)
C1—N1—C5119.1 (2)O9—V4—O5111.12 (7)
C1—N1—Cu1126.2 (2)O2—V4—O5108.34 (7)
D—H···AD—HH···AD···AD—H···A
C1—H1···O40.94 (3)2.53 (3)3.068 (4)117 (2)
C2—H2···O6iv0.91 (3)2.57 (3)3.132 (4)121 (2)
C4—H4···O10vi0.89 (3)2.53 (3)3.330 (4)150 (3)
C7—H5···O9vi0.91 (3)2.59 (3)3.306 (4)136 (3)
C9—H7···O6i0.89 (3)2.36 (3)3.216 (4)160 (3)
C10—H8···O30.96 (3)2.36 (3)2.937 (4)118 (2)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C1—H1⋯O40.94 (3)2.53 (3)3.068 (4)117 (2)
C2—H2⋯O6i0.91 (3)2.57 (3)3.132 (4)121 (2)
C4—H4⋯O10ii0.89 (3)2.53 (3)3.330 (4)150 (3)
C7—H5⋯O9ii0.91 (3)2.59 (3)3.306 (4)136 (3)
C9—H7⋯O6iii0.89 (3)2.36 (3)3.216 (4)160 (3)
C10—H8⋯O30.96 (3)2.36 (3)2.937 (4)118 (2)

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

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