trans-Aqua­bis(glyoximato-κ²N,N′)nitro­cobalt(III)

The molecule of the title compound, [Co(C₂H₃N₂O₂)₂(NO₂)(H₂O)], is located on a twofold crystallographic twofold rotation axis, with the metal in a pseudo-octa­hedral coordination, the bond between Co and the aqua ligand being the longest. In addition to the two intra­molecular hydrogen bonds between the equatorial bidentate glyoximate ligands, two pairs of inter­molecular hydrogen bonds to two adjacent mol­ecules are formed.

Key indicators

• Single-crystal X-ray study
• T = 130 K
• R factor = 0.038
• wR factor = 0.089
• Data-to-parameter ratio = 12.3

checkCIF/PLATON results

No syntax errors found


No errors found in this datablock

---

Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: PLATON (Spek, 2003).

trans-Aquabis(glyoximato-κ²N,N')nitrocobalt(III)

Crystal data

[Co(C2H3N2O2)2(NO2)(H2O)]	Dx = 2.093 Mg m^−3
Mr = 297.08	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pbcn	Cell parameters from 859 reflections
a = 8.4127 (18) Å	θ = 3.7–28.0°
b = 11.366 (2) Å	µ = 1.86 mm^−1
c = 9.859 (2) Å	T = 130 K
V = 942.7 (3) Å^3	Plate, brown
Z = 4	0.37 × 0.10 × 0.03 mm
F(000) = 600

Data collection

Bruker SMART CCD area-detector diffractometer	1168 independent reflections
Radiation source: fine-focus sealed tube	1067 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.076
ω scans	θmax = 28.3°, θmin = 3.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→11
Tmin = 0.55, Tmax = 0.94	k = −15→15
11831 measured reflections	l = −13→13

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)] = 0.038	Hydrogen site location: difference Fourier map
wR(F^2) = 0.089	All H-atom parameters refined
S = 1.08	w = 1/[σ^2(Fo^2) + (0.04P)^2 + P] where P = (Fo^2 + 2Fc^2)/3
1168 reflections	(Δ/σ)max = 0.001
95 parameters	Δρmax = 0.70 e Å^−3
0 restraints	Δρmin = −0.55 e Å^−3

Special details

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

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

	x	y	z	Uiso*/Ueq
Co1	0.0000	0.14091 (4)	0.2500	0.00958 (17)
O1	0.3129 (2)	0.12770 (16)	0.37417 (18)	0.0183 (4)
H11	0.249 (5)	0.134 (3)	0.432 (5)	0.058 (14)*
O2	−0.0738 (2)	0.14648 (14)	−0.03132 (16)	0.0137 (4)
O3	0.0000	−0.0303 (2)	0.2500	0.0179 (5)
H3	0.025 (5)	−0.071 (3)	0.183 (4)	0.050 (12)*
O4	0.1085 (3)	0.36182 (17)	0.1944 (3)	0.0379 (6)
N2	0.0416 (2)	0.13965 (15)	0.0600 (2)	0.0104 (4)
N3	0.2256 (3)	0.13403 (16)	0.2579 (2)	0.0135 (4)
N5	0.0000	0.3114 (3)	0.2500	0.0125 (5)
C1	0.2960 (3)	0.1245 (2)	0.1434 (3)	0.0145 (5)
C2	0.1904 (3)	0.12940 (19)	0.0276 (2)	0.0130 (5)
H1	0.397 (3)	0.116 (2)	0.131 (3)	0.011 (5)*
H2	0.229 (3)	0.125 (2)	−0.062 (3)	0.011 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0085 (2)	0.0106 (2)	0.0096 (2)	0.000	0.00034 (15)	0.000
O1	0.0114 (8)	0.0303 (10)	0.0132 (9)	0.0008 (7)	−0.0040 (7)	−0.0014 (7)
O2	0.0141 (8)	0.0173 (8)	0.0097 (8)	0.0014 (6)	−0.0017 (6)	0.0002 (6)
O3	0.0299 (14)	0.0110 (11)	0.0128 (12)	0.000	0.0070 (11)	0.000
O4	0.0366 (13)	0.0181 (10)	0.0589 (16)	−0.0066 (8)	0.0209 (11)	0.0012 (10)
N2	0.0108 (9)	0.0095 (8)	0.0108 (9)	−0.0003 (6)	−0.0004 (7)	0.0013 (7)
N3	0.0121 (10)	0.0149 (9)	0.0136 (10)	−0.0001 (7)	−0.0004 (7)	0.0010 (7)
N5	0.0105 (12)	0.0184 (13)	0.0087 (12)	0.000	−0.0015 (11)	0.000
C1	0.0105 (11)	0.0145 (11)	0.0186 (12)	−0.0005 (8)	0.0021 (9)	0.0012 (9)
C2	0.0152 (11)	0.0114 (10)	0.0123 (11)	−0.0014 (8)	0.0056 (9)	0.0012 (8)

Geometric parameters (Å, º)

Co1—N3^i	1.901 (2)	O3—H3	0.83 (4)
Co1—N3	1.901 (2)	O4—N5	1.209 (2)
Co1—N2^i	1.906 (2)	N2—C2	1.297 (3)
Co1—N2	1.906 (2)	N3—C1	1.280 (3)
Co1—N5	1.938 (3)	N5—O4^i	1.209 (2)
Co1—O3	1.946 (3)	C1—C2	1.447 (3)
O1—N3	1.363 (3)	C1—H1	0.86 (3)
O1—H11	0.79 (5)	C2—H2	0.94 (3)
O2—N2	1.326 (3)
N3^i—Co1—N3	175.28 (11)	Co1—O3—H3	124 (3)
N3^i—Co1—N2^i	81.78 (8)	C2—N2—O2	123.0 (2)
N3—Co1—N2^i	98.19 (8)	C2—N2—Co1	114.79 (16)
N3^i—Co1—N2	98.19 (8)	O2—N2—Co1	122.16 (15)
N3—Co1—N2	81.78 (8)	C1—N3—O1	119.2 (2)
N2^i—Co1—N2	179.13 (11)	C1—N3—Co1	115.41 (17)
N3^i—Co1—N5	92.36 (6)	O1—N3—Co1	125.08 (15)
N3—Co1—N5	92.36 (6)	O4^i—N5—O4	123.4 (3)
N2^i—Co1—N5	90.43 (5)	O4^i—N5—Co1	118.29 (16)
N2—Co1—N5	90.43 (5)	O4—N5—Co1	118.29 (16)
N3^i—Co1—O3	87.64 (6)	N3—C1—C2	114.1 (2)
N3—Co1—O3	87.64 (6)	N3—C1—H1	126.0 (19)
N2^i—Co1—O3	89.57 (5)	C2—C1—H1	119.9 (19)
N2—Co1—O3	89.57 (5)	N2—C2—C1	113.7 (2)
N5—Co1—O3	180.0	N2—C2—H2	124.4 (17)
N3—O1—H11	104 (3)	C1—C2—H2	121.8 (17)

Symmetry code: (i) −x, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H11···O2^i	0.79 (5)	1.78 (4)	2.548 (2)	167 (5)
O3—H3···O2^ii	0.83 (4)	1.77 (4)	2.603 (2)	175 (4)

Symmetry codes: (i) −x, y, −z+1/2; (ii) −x, −y, −z.