(Acetyl-acetonato-κO,O')chlorido-trimethano-latoniobium(V).

In the title compound, [Nb(CH(3)O)(3)(C(5)H(7)O(2))Cl], the Nb(V) atom is coordinated by two O atoms from the chelating acetyl-acetonate ligand, three O atoms from the methano-late groups and one chloride ligand. The octa-hedral environment around niobium is slightly distorted with Nb-O distances in the range 1.8603 (15)-2.1083 (15) Å and an Nb-Cl distance of 2.4693 (9) Å. The O-Nb-O angles vary between 80.74 (6) and 100.82 (7)°, while the trans Cl-Nb-O angle is 167.60 (5)°. There are no hydrogen bonds observed, only an inter-molecular C-H⋯O inter-action.

Related literature

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

Experimental

Crystal data

[Nb(CH3O)3(C5H7O2)Cl]

M = 320.57

Orthorhombic,

a = 12.296 (5) Å

b = 12.915 (4) Å

c = 15.470 (5) Å

V = 2456.7 (16) Å3

Z = 8

Mo Kα radiation

μ = 1.20 mm−1

T = 100 K

0.36 × 0.30 × 0.19 mm

Data collection

Bruker X8 APEXII 4K Kappa CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T min = 0.673, T max = 0.805

28601 measured reflections

3083 independent reflections

2757 reflections with I > 2σ(I)

R int = 0.030

Refinement

R[F 2 > 2σ(F 2)] = 0.023

wR(F 2) = 0.068

S = 1.16

3083 reflections

141 parameters

H-atom parameters constrained

Δρmax = 1.06 e Å−3

Δρmin = −0.87 e Å−3

Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT-Plus (Bruker, 2004 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg & Putz, 2005 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810021719/pv2289sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810021719/pv2289Isup2.hkl

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

[Nb(CH3O)3(C5H7O2)Cl]	F(000) = 1296
Mr = 320.57	Dx = 1.733 Mg m−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 9878 reflections
a = 12.296 (5) Å	θ = 2.6–28.4°
b = 12.915 (4) Å	µ = 1.20 mm−1
c = 15.470 (5) Å	T = 100 K
V = 2456.7 (16) Å3	Cuboid, pale-yellow
Z = 8	0.36 × 0.3 × 0.19 mm

Bruker X8 APEXII 4K Kappa CCD diffractometer	3083 independent reflections
Radiation source: fine-focus sealed tube	2757 reflections with I > 2σ(I)
graphite	Rint = 0.030
ω and φ scans	θmax = 28.4°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −12→16
Tmin = 0.673, Tmax = 0.805	k = −14→17
28601 measured reflections	l = −18→20

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)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.068	H-atom parameters constrained
S = 1.16	w = 1/[σ2(Fo2) + (0.0273P)2 + 3.5334P] where P = (Fo2 + 2Fc2)/3
3083 reflections	(Δ/σ)max = 0.001
141 parameters	Δρmax = 1.06 e Å−3
0 restraints	Δρmin = −0.87 e Å−3
0 constraints

Experimental. The intensity data were collected on a Bruker X8 ApexII 4 K Kappa CCD diffractometer using an exposure time of 60 s/frame. A total of 688 frames were collected with a frame width of 0.5° covering up to θ = 28.24° with 99.1% 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	0.00363 (19)	0.09540 (17)	0.76165 (14)	0.0195 (4)
H1A	−0.0385	0.1594	0.7676	0.029*
H1B	0.0228	0.0692	0.8191	0.029*
H1C	−0.04	0.0435	0.7311	0.029*
C2	0.3610 (2)	0.07674 (19)	0.54112 (15)	0.0217 (5)
H2A	0.3222	0.0834	0.4861	0.033*
H2B	0.3847	0.0049	0.5488	0.033*
H2C	0.4247	0.1224	0.5409	0.033*
C3	0.26952 (19)	0.38799 (16)	0.74055 (15)	0.0195 (4)
H3A	0.2855	0.43	0.6894	0.029*
H3B	0.3309	0.3915	0.7809	0.029*
H3C	0.2039	0.4145	0.7689	0.029*
C4	0.2957 (2)	0.37805 (19)	0.41139 (16)	0.0231 (5)
H4A	0.3083	0.44	0.4466	0.035*
H4B	0.2605	0.3978	0.357	0.035*
H4C	0.3654	0.3443	0.399	0.035*
C5	0.22378 (18)	0.30466 (16)	0.45973 (14)	0.0158 (4)
C6	0.14339 (18)	0.24919 (17)	0.41581 (14)	0.0174 (4)
H6	0.1304	0.2657	0.3569	0.021*
C7	0.08152 (17)	0.17147 (16)	0.45334 (13)	0.0148 (4)
O1	0.09963 (13)	0.11572 (11)	0.71426 (9)	0.0162 (3)
O2	0.29097 (12)	0.10497 (12)	0.60982 (10)	0.0161 (3)
O3	0.25251 (13)	0.28363 (11)	0.71528 (9)	0.0158 (3)
O4	0.24286 (13)	0.29502 (11)	0.54083 (10)	0.0155 (3)
O5	0.09160 (13)	0.14211 (11)	0.53257 (9)	0.0158 (3)
Cl1	0.02912 (4)	0.32547 (4)	0.64105 (3)	0.01788 (11)
Nb1	0.178955 (15)	0.198214 (14)	0.638103 (11)	0.01144 (7)
C8	−0.00329 (19)	0.11656 (18)	0.40125 (14)	0.0200 (4)
H8A	−0.0015	0.0424	0.4147	0.03*
H8B	0.0113	0.1268	0.3396	0.03*
H8C	−0.0752	0.1445	0.4154	0.03*

	U11	U22	U33	U12	U13	U23
C1	0.0207 (11)	0.0218 (10)	0.0160 (10)	−0.0056 (9)	0.0046 (8)	−0.0002 (8)
C2	0.0221 (11)	0.0254 (11)	0.0175 (10)	0.0029 (9)	0.0043 (9)	−0.0018 (8)
C3	0.0185 (11)	0.0155 (9)	0.0245 (11)	−0.0016 (8)	−0.0015 (9)	−0.0023 (8)
C4	0.0237 (12)	0.0247 (12)	0.0209 (11)	−0.0011 (9)	0.0053 (9)	0.0094 (9)
C5	0.0175 (10)	0.0160 (10)	0.0139 (10)	0.0040 (8)	0.0042 (8)	0.0037 (7)
C6	0.0192 (10)	0.0226 (10)	0.0105 (9)	0.0033 (9)	0.0009 (8)	0.0023 (8)
C7	0.0155 (10)	0.0178 (9)	0.0112 (9)	0.0054 (8)	−0.0003 (8)	−0.0029 (7)
O1	0.0187 (8)	0.0174 (7)	0.0125 (7)	−0.0016 (6)	0.0030 (6)	0.0022 (6)
O2	0.0161 (7)	0.0180 (7)	0.0140 (7)	0.0021 (6)	0.0020 (6)	0.0010 (6)
O3	0.0194 (8)	0.0148 (7)	0.0132 (7)	−0.0018 (6)	−0.0011 (6)	−0.0007 (5)
O4	0.0173 (7)	0.0170 (7)	0.0123 (7)	−0.0024 (6)	0.0009 (6)	0.0025 (5)
O5	0.0198 (8)	0.0165 (7)	0.0112 (7)	−0.0032 (6)	−0.0013 (6)	−0.0006 (5)
Cl1	0.0170 (2)	0.0169 (2)	0.0198 (3)	0.00236 (19)	0.00092 (19)	0.00026 (18)
Nb1	0.01376 (11)	0.01214 (10)	0.00841 (10)	−0.00081 (6)	0.00045 (6)	0.00115 (6)
C8	0.0199 (11)	0.0250 (11)	0.0150 (10)	0.0007 (9)	−0.0035 (8)	−0.0043 (8)

C1—O1	1.414 (3)	C5—O4	1.282 (3)
C1—H1A	0.98	C5—C6	1.397 (3)
C1—H1B	0.98	C6—C7	1.387 (3)
C1—H1C	0.98	C6—H6	0.95
C2—O2	1.416 (3)	C7—O5	1.289 (3)
C2—H2A	0.98	C7—C8	1.497 (3)
C2—H2B	0.98	O1—Nb1	1.8640 (15)
C2—H2C	0.98	O2—Nb1	1.8811 (16)
C3—O3	1.419 (2)	O3—Nb1	1.8603 (15)
C3—H3A	0.98	O4—Nb1	2.1083 (15)
C3—H3B	0.98	O5—Nb1	2.0842 (15)
C3—H3C	0.98	Cl1—Nb1	2.4693 (9)
C4—C5	1.497 (3)	C8—H8A	0.98
C4—H4A	0.98	C8—H8B	0.98
C4—H4B	0.98	C8—H8C	0.98
C4—H4C	0.98
O1—C1—H1A	109.5	O5—C7—C6	123.9 (2)
O1—C1—H1B	109.5	O5—C7—C8	116.1 (2)
H1A—C1—H1B	109.5	C6—C7—C8	120.0 (2)
O1—C1—H1C	109.5	C1—O1—Nb1	150.52 (14)
H1A—C1—H1C	109.5	C2—O2—Nb1	141.71 (14)
H1B—C1—H1C	109.5	C3—O3—Nb1	144.27 (14)
O2—C2—H2A	109.5	C5—O4—Nb1	133.45 (14)
O2—C2—H2B	109.5	C7—O5—Nb1	133.79 (14)
H2A—C2—H2B	109.5	O3—Nb1—O1	100.82 (7)
O2—C2—H2C	109.5	O3—Nb1—O2	99.96 (7)
H2A—C2—H2C	109.5	O1—Nb1—O2	99.45 (7)
H2B—C2—H2C	109.5	O3—Nb1—O5	163.63 (6)
O3—C3—H3A	109.5	O1—Nb1—O5	91.53 (7)
O3—C3—H3B	109.5	O2—Nb1—O5	88.43 (7)
H3A—C3—H3B	109.5	O3—Nb1—O4	85.71 (7)
O3—C3—H3C	109.5	O1—Nb1—O4	170.09 (6)
H3A—C3—H3C	109.5	O2—Nb1—O4	86.60 (7)
H3B—C3—H3C	109.5	O5—Nb1—O4	80.74 (6)
C5—C4—H4A	109.5	O3—Nb1—Cl1	87.49 (6)
C5—C4—H4B	109.5	O1—Nb1—Cl1	88.76 (5)
H4A—C4—H4B	109.5	O2—Nb1—Cl1	167.60 (5)
C5—C4—H4C	109.5	O5—Nb1—Cl1	82.03 (5)
H4A—C4—H4C	109.5	O4—Nb1—Cl1	84.06 (5)
H4B—C4—H4C	109.5	C7—C8—H8A	109.5
O4—C5—C6	123.7 (2)	C7—C8—H8B	109.5
O4—C5—C4	116.2 (2)	H8A—C8—H8B	109.5
C6—C5—C4	120.0 (2)	C7—C8—H8C	109.5
C7—C6—C5	123.8 (2)	H8A—C8—H8C	109.5
C7—C6—H6	118.1	H8B—C8—H8C	109.5
C5—C6—H6	118.1
O4—C5—C6—C7	−5.6 (3)	C1—O1—Nb1—Cl1	5.1 (3)
C4—C5—C6—C7	172.5 (2)	C2—O2—Nb1—O3	−109.4 (2)
C5—C6—C7—O5	0.0 (3)	C2—O2—Nb1—O1	147.7 (2)
C5—C6—C7—C8	179.7 (2)	C2—O2—Nb1—O5	56.4 (2)
C6—C5—O4—Nb1	3.5 (3)	C2—O2—Nb1—O4	−24.4 (2)
C4—C5—O4—Nb1	−174.66 (15)	C2—O2—Nb1—Cl1	16.8 (4)
C6—C7—O5—Nb1	8.1 (3)	C7—O5—Nb1—O3	26.9 (3)
C8—C7—O5—Nb1	−171.59 (14)	C7—O5—Nb1—O1	166.10 (19)
C3—O3—Nb1—O1	−120.8 (2)	C7—O5—Nb1—O2	−94.49 (19)
C3—O3—Nb1—O2	137.5 (2)	C7—O5—Nb1—O4	−7.67 (19)
C3—O3—Nb1—O5	17.5 (4)	C7—O5—Nb1—Cl1	77.56 (19)
C3—O3—Nb1—O4	51.7 (2)	C5—O4—Nb1—O3	−169.00 (19)
C3—O3—Nb1—Cl1	−32.5 (2)	C5—O4—Nb1—O2	90.7 (2)
C1—O1—Nb1—O3	92.3 (3)	C5—O4—Nb1—O5	1.77 (19)
C1—O1—Nb1—O2	−165.5 (3)	C5—O4—Nb1—Cl1	−81.08 (19)
C1—O1—Nb1—O5	−76.9 (3)

D—H···A	D—H	H···A	D···A	D—H···A
C8—H8C···O4i	0.98	2.46	3.442 (3)	176

O1—Nb1	1.8640 (15)
O2—Nb1	1.8811 (16)
O3—Nb1	1.8603 (15)
O4—Nb1	2.1083 (15)
O5—Nb1	2.0842 (15)
Cl1—Nb1	2.4693 (9)

O3—Nb1—O1	100.82 (7)
O3—Nb1—O2	99.96 (7)
O1—Nb1—O2	99.45 (7)
O3—Nb1—O5	163.63 (6)
O1—Nb1—O5	91.53 (7)
O2—Nb1—O5	88.43 (7)
O3—Nb1—O4	85.71 (7)
O2—Nb1—Cl1	167.60 (5)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C8—H8C⋯O4i	0.98	2.46	3.442 (3)	176

Symmetry code: (i) .