Di-μ-methoxo-bis­{[diacetyl monooxime (4-methoxy­benzo­yl)hydrazonato-κ³O,N,N′]oxovanadium(V)}

In the title centrosymmetric dimeric complex, [V₂(C₁₂H₁₃N₃O₃)₂(CH₃O)₂O₂], each V^V atom is six-coordinated by one oxo O atom, two N atoms and one O atom of the tridentate hydrazone ligand and two O atoms of two methoxo groups, leading to a distorted octa­hedral environment. Two V^V atoms are bridged by methoxo groups, resulting in a dimer, with a V...V separation of 3.324 (3) Å.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C)= 0.003 Å
• R factor = 0.041
• wR factor = 0.117
• Data-to-parameter ratio = 17.5

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Computing details

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Di-µ-methoxo-bis{[diacetyl monoxime (4-methoxybenzoyl)hydrazonato-κ³O,N,N']oxovanadium(V)}

Crystal data

[V2(C12H13N3O3)2(CH3O)2O2]	F(000) = 712
Mr = 690.46	Dx = 1.482 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 13756 reflections
a = 7.3381 (15) Å	θ = 3.4–27.5°
b = 22.166 (4) Å	µ = 0.67 mm^−1
c = 9.6540 (19) Å	T = 295 K
β = 99.75 (3)°	Prism, black
V = 1547.6 (5) Å^3	0.35 × 0.23 × 0.18 mm
Z = 2

Data collection

Rigaku R-AXIS RAPID diffractometer	3546 independent reflections
Radiation source: fine-focus sealed tube	2751 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.026
Detector resolution: 10 pixels mm^-1	θmax = 27.5°, θmin = 3.4°
ω scans	h = −8→9
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −28→28
Tmin = 0.800, Tmax = 0.889	l = −12→12
15118 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.117	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0644P)^2 + 0.3702P] where P = (Fo^2 + 2Fc^2)/3
3546 reflections	(Δ/σ)max = 0.001
203 parameters	Δρmax = 0.32 e Å^−3
0 restraints	Δρmin = −0.27 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
V1	0.63964 (5)	0.550359 (16)	0.09092 (4)	0.04551 (14)
O1	0.8160 (3)	0.59138 (8)	0.08863 (18)	0.0623 (4)
O2	0.4594 (3)	0.60771 (7)	0.07521 (19)	0.0637 (5)
O3	0.7545 (2)	0.47963 (6)	0.18633 (14)	0.0468 (3)
O4	0.9999 (3)	0.25899 (7)	0.59293 (19)	0.0622 (5)
O5	0.61636 (19)	0.51089 (7)	−0.07867 (15)	0.0475 (4)
N1	0.4619 (3)	0.66342 (9)	0.1360 (3)	0.0648 (6)
N2	0.6360 (2)	0.56555 (8)	0.30606 (18)	0.0429 (4)
N3	0.6971 (2)	0.51818 (8)	0.39580 (18)	0.0433 (4)
C1	0.5154 (4)	0.72840 (12)	0.3312 (4)	0.0776 (8)
C2	0.5239 (3)	0.66641 (10)	0.2691 (3)	0.0561 (6)
C3	0.5915 (3)	0.61517 (10)	0.3618 (2)	0.0468 (5)
C4	0.6091 (4)	0.62195 (12)	0.5174 (3)	0.0603 (6)
C5	0.7578 (3)	0.47525 (9)	0.3210 (2)	0.0410 (4)
C6	0.8279 (3)	0.41908 (9)	0.3907 (2)	0.0406 (4)
C7	0.8779 (3)	0.41540 (10)	0.5367 (2)	0.0446 (5)
C8	0.9329 (3)	0.36174 (10)	0.6003 (2)	0.0487 (5)
C9	0.9422 (3)	0.31004 (10)	0.5194 (2)	0.0468 (5)
C10	0.8942 (3)	0.31274 (10)	0.3746 (2)	0.0516 (5)
C11	0.8382 (3)	0.36739 (10)	0.3115 (2)	0.0480 (5)
C12	1.0192 (5)	0.20489 (11)	0.5150 (3)	0.0712 (7)
C13	0.7616 (4)	0.50182 (15)	−0.1569 (3)	0.0730 (8)
H1A	0.4757	0.7569	0.2573	0.116*
H1B	0.6357	0.7395	0.3800	0.116*
H1C	0.4293	0.7283	0.3958	0.116*
H4A	0.5791	0.5844	0.5576	0.090*
H4B	0.5258	0.6527	0.5383	0.090*
H4C	0.7338	0.6331	0.5562	0.090*
H7	0.8738	0.4498	0.5912	0.053*
H8	0.9643	0.3597	0.6976	0.058*
H10	0.8995	0.2783	0.3203	0.062*
H11	0.8070	0.3694	0.2141	0.058*
H12A	0.8999	0.1922	0.4671	0.107*
H12B	1.0721	0.1737	0.5782	0.107*
H12C	1.0985	0.2126	0.4474	0.107*
H13A	0.8461	0.5352	−0.1418	0.109*
H13B	0.7109	0.4990	−0.2551	0.109*
H13C	0.8261	0.4652	−0.1266	0.109*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V1	0.0496 (2)	0.0497 (2)	0.0360 (2)	−0.00215 (16)	0.00352 (15)	−0.00439 (15)
O1	0.0730 (11)	0.0626 (10)	0.0519 (10)	−0.0182 (9)	0.0121 (8)	−0.0028 (8)
O2	0.0720 (11)	0.0586 (9)	0.0547 (10)	0.0142 (9)	−0.0062 (8)	−0.0060 (8)
O3	0.0525 (8)	0.0530 (8)	0.0340 (7)	0.0061 (7)	0.0050 (6)	−0.0046 (6)
O4	0.0790 (12)	0.0538 (9)	0.0553 (10)	0.0120 (8)	0.0154 (9)	0.0032 (8)
O5	0.0452 (8)	0.0648 (9)	0.0333 (7)	−0.0020 (7)	0.0084 (6)	−0.0062 (7)
N1	0.0681 (13)	0.0539 (11)	0.0698 (15)	0.0106 (10)	0.0040 (11)	−0.0029 (10)
N2	0.0372 (8)	0.0497 (9)	0.0411 (10)	−0.0016 (7)	0.0044 (7)	−0.0066 (7)
N3	0.0436 (9)	0.0494 (10)	0.0371 (9)	−0.0021 (8)	0.0071 (7)	−0.0049 (7)
C1	0.0739 (18)	0.0553 (14)	0.100 (2)	0.0082 (13)	0.0039 (16)	−0.0174 (15)
C2	0.0479 (12)	0.0505 (12)	0.0692 (16)	0.0034 (10)	0.0075 (11)	−0.0100 (11)
C3	0.0371 (10)	0.0528 (12)	0.0510 (12)	−0.0051 (9)	0.0083 (9)	−0.0120 (10)
C4	0.0578 (14)	0.0664 (15)	0.0588 (15)	−0.0018 (12)	0.0162 (11)	−0.0197 (12)
C5	0.0345 (9)	0.0501 (11)	0.0374 (10)	−0.0059 (9)	0.0036 (8)	−0.0060 (9)
C6	0.0352 (9)	0.0491 (11)	0.0373 (10)	−0.0026 (8)	0.0061 (8)	−0.0057 (8)
C7	0.0455 (11)	0.0509 (11)	0.0374 (11)	−0.0016 (9)	0.0076 (8)	−0.0091 (9)
C8	0.0516 (12)	0.0613 (13)	0.0330 (11)	−0.0011 (10)	0.0065 (9)	−0.0027 (9)
C9	0.0462 (11)	0.0499 (11)	0.0451 (12)	−0.0003 (9)	0.0104 (9)	−0.0011 (9)
C10	0.0615 (13)	0.0495 (12)	0.0438 (12)	0.0005 (10)	0.0090 (10)	−0.0114 (9)
C11	0.0543 (12)	0.0559 (12)	0.0331 (10)	−0.0007 (10)	0.0049 (9)	−0.0081 (9)
C12	0.088 (2)	0.0486 (13)	0.0784 (19)	0.0053 (14)	0.0173 (15)	−0.0015 (13)
C13	0.0576 (14)	0.107 (2)	0.0596 (16)	−0.0097 (15)	0.0252 (12)	−0.0185 (15)

Geometric parameters (Å, º)

V1—O1	1.5846 (17)	C3—C4	1.493 (3)
V1—O2	1.8224 (17)	C4—H4A	0.96
V1—O3	1.9374 (15)	C4—H4B	0.96
V1—O5	1.8386 (15)	C4—H4C	0.96
V1—O5^i	2.3046 (15)	C5—C6	1.466 (3)
V1—N2	2.1087 (18)	C6—C7	1.398 (3)
O2—N1	1.366 (3)	C6—C11	1.387 (3)
O3—C5	1.300 (2)	C7—C8	1.368 (3)
N1—C2	1.290 (3)	C7—H7	0.93
N2—N3	1.386 (2)	C8—C9	1.395 (3)
N2—C3	1.291 (3)	C8—H8	0.93
N3—C5	1.316 (2)	C9—C10	1.384 (3)
O4—C9	1.364 (3)	C10—C11	1.387 (3)
O4—C12	1.435 (3)	C10—H10	0.93
O5—V1^i	2.3046 (15)	C11—H11	0.93
O5—C13	1.421 (3)	C12—H12A	0.96
C1—C2	1.505 (3)	C12—H12B	0.96
C1—H1A	0.96	C12—H12C	0.96
C1—H1B	0.96	C13—H13A	0.96
C1—H1C	0.96	C13—H13B	0.96
C2—C3	1.479 (3)	C13—H13C	0.96
V1—O5—V1^i	106.14 (7)	C3—N2—N3	117.55 (18)
O1—V1—O2	100.45 (10)	C3—C2—C1	119.5 (2)
O1—V1—O3	100.40 (8)	C3—C4—H4A	109.5
O1—V1—O5	102.33 (8)	C3—C4—H4B	109.5
O1—V1—O5^i	176.15 (7)	C3—C4—H4C	109.5
O1—V1—N2	93.93 (8)	C5—O3—V1	117.95 (13)
O2—V1—O3	148.79 (8)	C5—N3—N2	107.95 (17)
O2—V1—O5	107.53 (8)	C6—C7—H7	119.7
O2—V1—O5^i	80.37 (7)	C6—C11—C10	121.3 (2)
O2—V1—N2	80.82 (8)	C6—C11—H11	119.3
O3—V1—O5^i	80.38 (6)	C7—C6—C5	121.60 (18)
O3—V1—N2	74.81 (7)	C7—C8—C9	120.1 (2)
O5—V1—O3	90.32 (7)	C7—C8—H8	119.9
O5—V1—O5^i	73.86 (7)	C8—C7—C6	120.69 (19)
O5—V1—N2	159.77 (7)	C8—C7—H7	119.7
N2—V1—O5^i	89.91 (6)	C9—O4—C12	118.0 (2)
O3—C5—N3	122.94 (19)	C9—C8—H8	119.9
O3—C5—C6	117.89 (18)	C9—C10—C11	119.2 (2)
O4—C9—C8	115.5 (2)	C9—C10—H10	120.4
O4—C9—C10	124.4 (2)	C10—C9—C8	120.1 (2)
O4—C12—H12A	109.5	C10—C11—H11	119.3
O4—C12—H12B	109.5	C11—C6—C7	118.6 (2)
O4—C12—H12C	109.5	C11—C6—C5	119.76 (19)
O5—C13—H13A	109.5	C11—C10—H10	120.4
O5—C13—H13B	109.5	C13—O5—V1	125.14 (15)
O5—C13—H13C	109.5	C13—O5—V1^i	124.59 (15)
N1—O2—V1	129.65 (16)	H1A—C1—H1B	109.5
N1—C2—C1	114.3 (2)	H1A—C1—H1C	109.5
N1—C2—C3	126.1 (2)	H1B—C1—H1C	109.5
N2—C3—C2	119.0 (2)	H4A—C4—H4B	109.5
N2—C3—C4	121.4 (2)	H4A—C4—H4C	109.5
N3—N2—V1	115.97 (12)	H4B—C4—H4C	109.5
N3—C5—C6	119.15 (18)	H12A—C12—H12B	109.5
C2—N1—O2	116.8 (2)	H12A—C12—H12C	109.5
C2—C1—H1A	109.5	H12B—C12—H12C	109.5
C2—C1—H1B	109.5	H13A—C13—H13B	109.5
C2—C1—H1C	109.5	H13A—C13—H13C	109.5
C2—C3—C4	119.7 (2)	H13B—C13—H13C	109.5
C3—N2—V1	126.39 (16)
V1—O2—N1—C2	−47.6 (3)	O5^i—V1—O5—C13	−157.9 (2)
V1—N2—N3—C5	4.81 (19)	O5—V1—N2—N3	38.5 (3)
V1—N2—C3—C2	4.3 (3)	O5^i—V1—N2—N3	74.60 (13)
V1—N2—C3—C4	−174.93 (15)	O5—V1—N2—C3	−145.14 (19)
V1—O3—C5—N3	−4.3 (2)	O5^i—V1—N2—C3	−109.04 (17)
V1—O3—C5—C6	174.02 (13)	N1—C2—C3—N2	17.8 (4)
O1—V1—O2—N1	−40.0 (2)	N1—C2—C3—C4	−163.0 (2)
O1—V1—O3—C5	96.31 (15)	N2—V1—O2—N1	52.4 (2)
O1—V1—O5—V1^i	−179.39 (8)	N2—V1—O3—C5	5.02 (14)
O1—V1—O5—C13	22.7 (2)	N2—V1—O5—V1^i	37.8 (2)
O1—V1—N2—N3	−105.17 (14)	N2—V1—O5—C13	−120.0 (3)
O1—V1—N2—C3	71.19 (18)	N2—N3—C5—O3	−0.6 (3)
O2—V1—O3—C5	−34.9 (2)	N2—N3—C5—C6	−178.94 (16)
O2—V1—O5—V1^i	−74.10 (9)	N3—N2—C3—C2	−179.37 (17)
O2—V1—O5—C13	128.0 (2)	N3—N2—C3—C4	1.4 (3)
O2—V1—N2—N3	154.86 (14)	N3—C5—C6—C7	−17.2 (3)
O2—V1—N2—C3	−28.78 (17)	N3—C5—C6—C11	160.11 (19)
O2—N1—C2—C3	−0.3 (4)	C1—C2—C3—N2	−165.3 (2)
O2—N1—C2—C1	−177.4 (2)	C1—C2—C3—C4	14.0 (3)
O3—V1—O2—N1	91.2 (2)	C3—N2—N3—C5	−171.88 (18)
O3—V1—O5—V1^i	79.89 (7)	C5—C6—C7—C8	176.22 (19)
O3—V1—O5—C13	−78.0 (2)	C5—C6—C11—C10	−176.4 (2)
O3—V1—N2—N3	−5.46 (12)	C6—C7—C8—C9	0.9 (3)
O3—V1—N2—C3	170.90 (18)	C7—C8—C9—O4	179.5 (2)
O3—C5—C6—C7	164.43 (18)	C7—C8—C9—C10	−0.5 (3)
O3—C5—C6—C11	−18.3 (3)	C7—C6—C11—C10	0.9 (3)
O4—C9—C10—C11	−179.7 (2)	C8—C9—C10—C11	0.3 (3)
O5—V1—O2—N1	−146.6 (2)	C9—C10—C11—C6	−0.6 (3)
O5^i—V1—O2—N1	143.9 (2)	C11—C6—C7—C8	−1.1 (3)
O5—V1—O3—C5	−161.09 (14)	C12—O4—C9—C10	2.5 (3)
O5^i—V1—O3—C5	−87.52 (14)	C12—O4—C9—C8	−177.6 (2)
O5^i—V1—O5—V1^i	0.0

Symmetry code: (i) −x+1, −y+1, −z.