(Acetyl-acetonato-κ(2)O,O')dichlorido-bis(methano-lato-κO)niobium(V).

In the title compound, [Nb(CH(3)O)(2)(C(5)H(7)O(2))Cl(2)], a slightly distorted octa-hedral coordination geometry is observed around the Nb(V) atom with Nb-O distances in the range of 1.8254 (16)-2.0892 (16) Å and Nb-Cl distances of 2.3997 (14) and 2.4023 (12) Å. The O-Nb-O angles vary between 81.36 (7) and 172.65 (7) °, while the trans Cl-Nb-Cl angle is 167.34 (2)°. There are no hydrogen bonds observed.

Related literature

For synthetic background, see: Herbst et al. (2010 ▶; 2011 ▶); Davies et al. (1999 ▶). For applications of acetyl­acetone-type ligands in industry, see: Steyn et al. (1992 ▶, 1997 ▶, 2008 ▶); Otto et al. (1998 ▶); Roodt & Steyn (2000 ▶); Brink et al. (2010 ▶); Viljoen et al. (2008 ▶, 2009 ▶, 2010 ▶). For related niobium complexes, see: Sokolov et al. (1999 ▶, 2005 ▶); Anti­nolo et al. (2000 ▶); Dahan et al. (1976 ▶).

Experimental

Crystal data

[Nb(CH3O)2(C5H7O2)Cl2]

M = 324.98

Monoclinic,

a = 7.7985 (2) Å

b = 11.6028 (3) Å

c = 14.6819 (2) Å

β = 111.279 (1)°

V = 1237.91 (5) Å3

Z = 4

Mo Kα radiation

μ = 1.39 mm−1

T = 100 K

0.38 × 0.13 × 0.08 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T min = 0.810, T max = 0.895

25521 measured reflections

2995 independent reflections

2873 reflections with I > 2σ(I)

R int = 0.024

Refinement

R[F 2 > 2σ(F 2)] = 0.026

wR(F 2) = 0.060

S = 1.04

2995 reflections

131 parameters

H-atom parameters constrained

Δρmax = 1.90 e Å−3

Δρmin = −1.14 e Å−3

Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT-Plus (Bruker, 2004 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SIR92 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg & Putz, 2004 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Click here for additional data file.

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812042638/bt6846sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812042638/bt6846Isup2.hkl

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

[Nb(CH3O)2(C5H7O2)Cl2]	F(000) = 648
Mr = 324.98	Dx = 1.744 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybc	Cell parameters from 9867 reflections
a = 7.7985 (2) Å	θ = 2.3–32.9°
b = 11.6028 (3) Å	µ = 1.39 mm−1
c = 14.6819 (2) Å	T = 100 K
β = 111.279 (1)°	Cubiod, yellow
V = 1237.91 (5) Å3	0.38 × 0.13 × 0.08 mm
Z = 4

Bruker APEXII CCD diffractometer	2873 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.024
φ and ω scans	θmax = 28°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −10→9
Tmin = 0.810, Tmax = 0.895	k = −14→15
25521 measured reflections	l = −19→19
2995 independent reflections

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)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.060	H-atom parameters constrained
S = 1.04	w = 1/[σ2(Fo2) + (0.0177P)2 + 2.6018P] where P = (Fo2 + 2Fc2)/3
2995 reflections	(Δ/σ)max = 0.001
131 parameters	Δρmax = 1.90 e Å−3
0 restraints	Δρmin = −1.14 e Å−3

Experimental. The intensity data was collected on a Bruker X8 ApexII 4 K Kappa CCD diffractometer using an exposure time of 60 s/frame. A total of 1033 frames were collected with a frame width of 0.5° covering up to θ = 28.32° with 99.8% completeness accomplished.

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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.

	x	y	z	Uiso*/Ueq
C1	0.5973 (4)	0.0556 (2)	0.41589 (19)	0.0291 (5)
H1A	0.5041	0.0091	0.3698	0.044*
H1B	0.5461	0.0949	0.4577	0.044*
H1C	0.697	0.0073	0.4547	0.044*
C2	0.6671 (3)	0.14217 (19)	0.36226 (16)	0.0209 (4)
C3	0.6842 (3)	0.25776 (19)	0.38971 (15)	0.0217 (4)
H3	0.6428	0.2801	0.439	0.026*
C4	0.7590 (3)	0.34165 (18)	0.34795 (15)	0.0189 (4)
C5	0.7749 (3)	0.4644 (2)	0.38144 (17)	0.0256 (5)
H5A	0.8962	0.4925	0.3915	0.038*
H5B	0.7531	0.4689	0.4416	0.038*
H5C	0.6856	0.5104	0.3326	0.038*
C6	1.0638 (4)	0.3334 (2)	0.1093 (2)	0.0351 (6)
H6A	1.0417	0.4104	0.1263	0.053*
H6B	1.0441	0.3302	0.0409	0.053*
H6C	1.1884	0.3119	0.1467	0.053*
C7	0.7155 (4)	−0.0737 (2)	0.12959 (19)	0.0315 (5)
H7A	0.6627	−0.0836	0.1788	0.047*
H7B	0.8087	−0.131	0.1379	0.047*
H7C	0.6213	−0.0817	0.0661	0.047*
O1	0.7114 (2)	0.10264 (14)	0.29243 (12)	0.0260 (3)
O2	0.8199 (2)	0.32042 (13)	0.27942 (12)	0.0236 (3)
O3	0.9420 (2)	0.25678 (14)	0.12973 (12)	0.0249 (3)
O4	0.7944 (2)	0.03654 (13)	0.13835 (12)	0.0235 (3)
Cl1	1.11377 (9)	0.13058 (6)	0.32569 (5)	0.03473 (14)
Cl2	0.51757 (8)	0.23365 (5)	0.10144 (4)	0.02774 (12)
Nb1	0.82643 (3)	0.178209 (17)	0.198700 (15)	0.02255 (7)

	U11	U22	U33	U12	U13	U23
C1	0.0387 (13)	0.0244 (11)	0.0336 (12)	0.0020 (10)	0.0241 (11)	0.0074 (9)
C2	0.0234 (10)	0.0220 (10)	0.0208 (10)	0.0033 (8)	0.0122 (8)	0.0047 (8)
C3	0.0271 (11)	0.0233 (10)	0.0194 (10)	0.0032 (8)	0.0142 (9)	0.0006 (8)
C4	0.0204 (10)	0.0202 (10)	0.0166 (9)	0.0022 (8)	0.0074 (8)	−0.0015 (7)
C5	0.0325 (12)	0.0212 (10)	0.0277 (11)	−0.0021 (9)	0.0162 (10)	−0.0065 (9)
C6	0.0348 (13)	0.0404 (14)	0.0344 (13)	−0.0160 (11)	0.0177 (11)	−0.0021 (11)
C7	0.0391 (14)	0.0204 (11)	0.0358 (13)	−0.0076 (10)	0.0145 (11)	−0.0050 (10)
O1	0.0399 (9)	0.0187 (7)	0.0296 (8)	−0.0034 (7)	0.0247 (8)	−0.0019 (6)
O2	0.0349 (9)	0.0186 (7)	0.0246 (8)	−0.0050 (6)	0.0194 (7)	−0.0042 (6)
O3	0.0307 (8)	0.0245 (8)	0.0274 (8)	−0.0071 (7)	0.0199 (7)	−0.0046 (6)
O4	0.0291 (8)	0.0184 (7)	0.0279 (8)	−0.0037 (6)	0.0161 (7)	−0.0059 (6)
Cl1	0.0379 (3)	0.0295 (3)	0.0374 (3)	−0.0022 (2)	0.0144 (3)	−0.0032 (2)
Cl2	0.0297 (3)	0.0293 (3)	0.0283 (3)	−0.0040 (2)	0.0154 (2)	−0.0029 (2)
Nb1	0.03316 (12)	0.01790 (10)	0.02524 (11)	−0.00586 (8)	0.02096 (9)	−0.00534 (7)

C1—C2	1.495 (3)	C6—H6A	0.96
C1—H1A	0.96	C6—H6B	0.96
C1—H1B	0.96	C6—H6C	0.96
C1—H1C	0.96	C7—O4	1.405 (3)
C2—O1	1.280 (3)	C7—H7A	0.96
C2—C3	1.393 (3)	C7—H7B	0.96
C3—C4	1.387 (3)	C7—H7C	0.96
C3—H3	0.93	O1—Nb1	2.0892 (16)
C4—O2	1.283 (3)	O2—Nb1	2.0429 (16)
C4—C5	1.497 (3)	O3—Nb1	1.8254 (16)
C5—H5A	0.96	O4—Nb1	1.8410 (17)
C5—H5B	0.96	Cl1—Nb1	2.4023 (12)
C5—H5C	0.96	Cl2—Nb1	2.3997 (14)
C6—O3	1.411 (3)
C2—C1—H1A	109.5	H6B—C6—H6C	109.5
C2—C1—H1B	109.5	O4—C7—H7A	109.5
H1A—C1—H1B	109.5	O4—C7—H7B	109.5
C2—C1—H1C	109.5	H7A—C7—H7B	109.5
H1A—C1—H1C	109.5	O4—C7—H7C	109.5
H1B—C1—H1C	109.5	H7A—C7—H7C	109.5
O1—C2—C3	123.49 (19)	H7B—C7—H7C	109.5
O1—C2—C1	115.9 (2)	C2—O1—Nb1	133.05 (15)
C3—C2—C1	120.6 (2)	C4—O2—Nb1	134.78 (14)
C4—C3—C2	124.00 (19)	C6—O3—Nb1	159.91 (16)
C4—C3—H3	118	C7—O4—Nb1	146.66 (15)
C2—C3—H3	118	O3—Nb1—O4	100.77 (7)
O2—C4—C3	123.2 (2)	O3—Nb1—O2	92.28 (7)
O2—C4—C5	115.49 (19)	O4—Nb1—O2	166.62 (7)
C3—C4—C5	121.35 (19)	O3—Nb1—O1	172.65 (7)
C4—C5—H5A	109.5	O4—Nb1—O1	85.79 (7)
C4—C5—H5B	109.5	O2—Nb1—O1	81.36 (7)
H5A—C5—H5B	109.5	O3—Nb1—Cl2	97.31 (7)
C4—C5—H5C	109.5	O4—Nb1—Cl2	91.23 (6)
H5A—C5—H5C	109.5	O2—Nb1—Cl2	84.13 (5)
H5B—C5—H5C	109.5	O1—Nb1—Cl2	85.76 (6)
O3—C6—H6A	109.5	O3—Nb1—Cl1	92.06 (7)
O3—C6—H6B	109.5	O4—Nb1—Cl1	95.37 (6)
H6A—C6—H6B	109.5	O2—Nb1—Cl1	87.03 (5)
O3—C6—H6C	109.5	O1—Nb1—Cl1	83.97 (7)
H6A—C6—H6C	109.5	Cl2—Nb1—Cl1	167.34 (2)