fac-Tris(pyridine-2-carboxyl-ato-κN,O)cobalt(III).

In the title compound, [Co(C(6)H(4)NO(2))(3)], the Co(III) ion lies on a threefold rotation axis and is in a distorted octa-hedral environment defined by three N and three O donor atoms from three fac-disposed pyridine-2-carboxyl-ate ligands. The ligands are coordinated in a chelate fashion, forming three five-membered rings. In the crystal, translationally related complex molecules are organized into columns along [001] via C-H⋯O hydrogen bonds.

Related literature

For the use of hydroxamate ligands in the synthesis of polynuclear compounds, see: Dobosz et al. (1999 ▶); Fritsky et al. (1998 ▶); Sachse et al. (2008 ▶). For hydrolytic destruction of hydroxamate ligands upon complex formation, see: Świątek-Kozłowska et al. (2000 ▶). For related structures, see: Fritsky et al. (2001 ▶); Fu & Wang (2005 ▶); Kovbasyuk et al. (2004 ▶); Krämer & Fritsky (2000 ▶); Mokhir et al. (2002 ▶); Moroz et al. (2010 ▶); Pelizzi & Pelizzi (1981 ▶); Sliva et al. (1997 ▶); Wörl, Fritsky et al. (2005 ▶); Wörl, Pritzkow et al. (2005 ▶). For the synthesis of pyridine-2-hydroxamic acid, see: Hynes (1970 ▶).

Experimental

Crystal data

[Co(C6H4NO2)3]

M = 425.24

Hexagonal,

a = 12.8617 (12) Å

c = 6.2122 (9) Å

V = 890.0 (2) Å3

Z = 2

Mo Kα radiation

μ = 1.01 mm−1

T = 120 K

0.23 × 0.08 × 0.03 mm

Data collection

Nonius KappaCCD diffractometer

Absorption correction: multi-scan (DENZO/SCALEPACK; Otwinowski & Minor, 1997 ▶) T min = 0.800, T max = 0.970

5635 measured reflections

978 independent reflections

893 reflections with I > 2σ(I)

R int = 0.043

Refinement

R[F 2 > 2σ(F 2)] = 0.068

wR(F 2) = 0.197

S = 1.16

978 reflections

86 parameters

1 restraint

H-atom parameters constrained

Δρmax = 1.05 e Å−3

Δρmin = −0.59 e Å−3

Absolute structure: Flack (1983 ▶), 400 Friedel pairs

Flack parameter: −0.02 (7)

Data collection: COLLECT (Nonius, 1998 ▶); cell refinement: DENZO/SCALEPACK (Otwinowski & Minor, 1997 ▶); data reduction: DENZO/SCALEPACK; program(s) used to solve structure: SIR2004 (Burla et al., 2005 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811043303/hy2479sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811043303/hy2479Isup2.hkl

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

[Co(C6H4NO2)3]	Dx = 1.587 Mg m−3
Mr = 425.24	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6	Cell parameters from 713 reflections
Hall symbol: P 6	θ = 3.2–24.5°
a = 12.8617 (12) Å	µ = 1.01 mm−1
c = 6.2122 (9) Å	T = 120 K
V = 890.0 (2) Å3	Block, pink
Z = 2	0.23 × 0.08 × 0.03 mm
F(000) = 432

Nonius KappaCCD diffractometer	978 independent reflections
Radiation source: fine-focus sealed tube	893 reflections with I > 2σ(I)
horizontally mounted graphite crystal	Rint = 0.043
Detector resolution: 9 pixels mm-1	θmax = 25.0°, θmin = 3.2°
φ and ω scans with κ offset	h = −15→15
Absorption correction: multi-scan (DENZO/SCALEPACK; Otwinowski & Minor, 1997)	k = −15→15
Tmin = 0.800, Tmax = 0.970	l = −7→7
5635 measured reflections

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.068	H-atom parameters constrained
wR(F2) = 0.197	w = 1/[σ2(Fo2) + (0.1316P)2 + 0.9442P] where P = (Fo2 + 2Fc2)/3
S = 1.16	(Δ/σ)max < 0.001
978 reflections	Δρmax = 1.05 e Å−3
86 parameters	Δρmin = −0.59 e Å−3
1 restraint	Absolute structure: Flack (1983), 400 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: −0.02 (7)

Experimental. The final structural refinement was performed by using the twin law -1 -1 0 0 1 0 0 0 -1 with the final BASF parameter refining to 0.80178.

	x	y	z	Uiso*/Ueq
Co1	0.3333	0.6667	0.3408 (2)	0.0379 (5)
O1	0.4550 (7)	0.7860 (7)	0.5147 (11)	0.0514 (18)
O2	0.6490 (9)	0.8907 (8)	0.5627 (16)	0.083 (3)
N1	0.4619 (6)	0.6785 (6)	0.1705 (12)	0.0332 (15)
C1	0.4622 (10)	0.6303 (9)	−0.0009 (17)	0.051 (2)
H1	0.3875	0.5756	−0.0656	0.061*
C2	0.5687 (9)	0.6533 (9)	−0.1037 (17)	0.050 (2)
H2	0.5659	0.6145	−0.2355	0.061*
C3	0.6747 (10)	0.7308 (9)	−0.0138 (18)	0.052 (2)
H3	0.7483	0.7480	−0.0795	0.062*
C4	0.6729 (9)	0.7796 (9)	0.159 (2)	0.052 (3)
H4	0.7469	0.8358	0.2241	0.062*
C5	0.5690 (8)	0.7548 (9)	0.2577 (18)	0.048 (2)
C6	0.5660 (11)	0.8159 (9)	0.4512 (18)	0.057 (3)

	U11	U22	U33	U12	U13	U23
Co1	0.0513 (7)	0.0513 (7)	0.0111 (8)	0.0256 (3)	0.000	0.000
O1	0.067 (4)	0.066 (4)	0.018 (4)	0.031 (4)	−0.007 (3)	−0.008 (3)
O2	0.105 (7)	0.067 (5)	0.054 (6)	0.027 (4)	−0.036 (5)	0.004 (4)
N1	0.045 (4)	0.047 (4)	0.014 (3)	0.028 (3)	−0.001 (3)	0.007 (3)
C1	0.065 (5)	0.056 (5)	0.034 (5)	0.031 (4)	0.006 (4)	0.008 (4)
C2	0.061 (5)	0.058 (5)	0.041 (6)	0.036 (5)	0.010 (4)	0.006 (4)
C3	0.060 (6)	0.059 (6)	0.046 (6)	0.038 (5)	0.014 (5)	0.016 (5)
C4	0.042 (5)	0.067 (6)	0.055 (7)	0.033 (4)	0.012 (5)	0.023 (6)
C5	0.048 (5)	0.057 (5)	0.042 (6)	0.029 (4)	−0.005 (4)	0.021 (5)
C6	0.071 (7)	0.052 (6)	0.036 (6)	0.021 (5)	−0.027 (6)	0.010 (5)

Co1—O1i	1.889 (7)	C1—C2	1.402 (14)
Co1—O1	1.889 (7)	C1—H1	0.9500
Co1—O1ii	1.889 (7)	C2—C3	1.344 (16)
Co1—N1i	1.904 (7)	C2—H2	0.9500
Co1—N1ii	1.904 (7)	C3—C4	1.251 (15)
Co1—N1	1.904 (7)	C3—H3	0.9500
O1—C6	1.339 (15)	C4—C5	1.354 (14)
O2—C6	1.232 (14)	C4—H4	0.9500
N1—C1	1.233 (14)	C5—C6	1.447 (15)
N1—C5	1.343 (12)
O1i—Co1—O1	90.6 (3)	N1—C1—C2	122.4 (10)
O1i—Co1—O1ii	90.6 (3)	N1—C1—H1	118.8
O1—Co1—O1ii	90.6 (3)	C2—C1—H1	118.8
O1i—Co1—N1i	85.4 (3)	C3—C2—C1	119.3 (10)
O1—Co1—N1i	92.1 (2)	C3—C2—H2	120.4
O1ii—Co1—N1i	175.1 (3)	C1—C2—H2	120.4
O1i—Co1—N1ii	92.1 (2)	C4—C3—C2	117.6 (10)
O1—Co1—N1ii	175.1 (3)	C4—C3—H3	121.2
O1ii—Co1—N1ii	85.4 (3)	C2—C3—H3	121.2
N1i—Co1—N1ii	92.1 (3)	C3—C4—C5	122.2 (11)
O1i—Co1—N1	175.1 (3)	C3—C4—H4	118.9
O1—Co1—N1	85.4 (3)	C5—C4—H4	118.9
O1ii—Co1—N1	92.1 (2)	N1—C5—C4	121.4 (11)
N1i—Co1—N1	92.1 (3)	N1—C5—C6	115.8 (10)
N1ii—Co1—N1	92.1 (3)	C4—C5—C6	122.5 (11)
C6—O1—Co1	113.3 (7)	O2—C6—O1	116.2 (13)
C1—N1—C5	117.1 (9)	O2—C6—C5	130.0 (13)
C1—N1—Co1	131.3 (7)	O1—C6—C5	113.8 (10)
C5—N1—Co1	111.5 (7)
O1i—Co1—O1—C6	179.0 (6)	C1—C2—C3—C4	−0.2 (14)
O1ii—Co1—O1—C6	88.4 (8)	C2—C3—C4—C5	1.2 (15)
N1—Co1—O1—C6	−3.7 (7)	C1—N1—C5—C4	1.3 (13)
O1—Co1—N1—C1	−175.4 (8)	Co1—N1—C5—C4	−177.9 (7)
O1ii—Co1—N1—C1	94.2 (9)	C1—N1—C5—C6	176.1 (7)
N1i—Co1—N1—C1	−83.4 (7)	Co1—N1—C5—C6	−3.1 (8)
N1ii—Co1—N1—C1	8.8 (8)	C3—C4—C5—N1	−1.8 (14)
O1—Co1—N1—C5	3.7 (6)	C3—C4—C5—C6	−176.3 (8)
O1ii—Co1—N1—C5	−86.7 (6)	Co1—O1—C6—O2	−177.8 (7)
N1i—Co1—N1—C5	95.7 (7)	Co1—O1—C6—C5	2.9 (9)
N1ii—Co1—N1—C5	−172.1 (6)	N1—C5—C6—O2	−179.0 (10)
C5—N1—C1—C2	−0.3 (13)	C4—C5—C6—O2	−4.2 (13)
Co1—N1—C1—C2	178.7 (6)	N1—C5—C6—O1	0.2 (9)
N1—C1—C2—C3	−0.2 (14)	C4—C5—C6—O1	174.9 (9)

D—H···A	D—H	H···A	D···A	D—H···A
C3—H3···O2iii	0.95	2.60	3.212 (14)	123

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C3—H3⋯O2i	0.95	2.60	3.212 (14)	123

Symmetry code: (i) .