Azido-{2-[bis-(2-hy-droxy-eth-yl)amino]-ethano-lato-κN,O,O',O''}cobalt(II).

In the title complex, [Co(C(6)H(14)NO(3))(N(3))] or [Co(teaH(2))N(3)], the Co(II) atom resides in a trigonal-bipymidal O(3)N(2) environment formed by three O atoms and one N atom from a simply deprotonated tetra-dentate triethano-lamine ligand, and one N atom from an azide ligand. The O atoms define the equatorial plane whereas both N atoms are in axial positions. The mononuclear units are linked through O-H⋯O hydrogen-bonding inter-actions between the ethanol OH groups and the ethano-late O atom of a neighbouring complex into chains running parallel to [010].

Related literature

For general background to complexes including teaH3 ligands, see: Liu, Wang et al. (2008 ▶); Liu, Zhang et al. (2008 ▶). For CoII complexes with similar ligands, see: Malaestean et al. (2010 ▶).

Experimental

Crystal data

[Co(C6H14NO3)(N3)]

M = 249.14

Monoclinic,

a = 8.7752 (2) Å

b = 7.9373 (1) Å

c = 14.4097 (3) Å

β = 107.084 (1)°

V = 959.37 (3) Å3

Z = 4

Mo Kα radiation

μ = 1.78 mm−1

T = 293 K

0.20 × 0.20 × 0.10 mm

Data collection

Rigaku Saturn CCD diffractometer

Absorption correction: multi-scan (REQAB; Jacobson, 1998 ▶) T min = 0.708, T max = 0.823

4004 measured reflections

2179 independent reflections

1253 reflections with I > 2σ(I)

R int = 0.055

Refinement

R[F 2 > 2σ(F 2)] = 0.038

wR(F 2) = 0.089

S = 0.89

2179 reflections

135 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.55 e Å−3

Δρmin = −0.38 e Å−3

Data collection: CrystalClear (Rigaku/MSC, 2006 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810047100/wm2427sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810047100/wm2427Isup2.hkl

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

[Co(C6H14NO3)(N3)]	F(000) = 516
Mr = 249.14	Dx = 1.725 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2179 reflections
a = 8.7752 (2) Å	θ = 3.4–27.5°
b = 7.9373 (1) Å	µ = 1.78 mm−1
c = 14.4097 (3) Å	T = 293 K
β = 107.084 (1)°	Pillar, red
V = 959.37 (3) Å3	0.20 × 0.20 × 0.10 mm
Z = 4

Rigaku Saturn CCD diffractometer	2179 independent reflections
Radiation source: fine-focus sealed tube	1253 reflections with I > 2σ(I)
graphite	Rint = 0.055
Detector resolution: 0.76 pixels mm-1	θmax = 27.5°, θmin = 3.5°
ω scans	h = −11→11
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	k = −10→10
Tmin = 0.708, Tmax = 0.823	l = −18→18
4004 measured 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)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.089	H atoms treated by a mixture of independent and constrained refinement
S = 0.89	w = 1/[σ2(Fo2) + (0.0427P)2] where P = (Fo2 + 2Fc2)/3
2179 reflections	(Δ/σ)max = 0.001
135 parameters	Δρmax = 0.55 e Å−3
0 restraints	Δρmin = −0.38 e Å−3

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.

	x	y	z	Uiso*/Ueq
Co1	0.49520 (5)	0.87496 (5)	0.81512 (3)	0.02597 (16)
C1	0.2117 (4)	0.6897 (4)	0.8302 (3)	0.0438 (10)
H1A	0.1899	0.6223	0.7716	0.053*
H1B	0.1173	0.6886	0.8522	0.053*
C2	0.3480 (4)	0.6158 (5)	0.9063 (3)	0.0405 (9)
H2A	0.3523	0.6638	0.9690	0.049*
H2B	0.3329	0.4951	0.9096	0.049*
C3	0.2225 (5)	0.9829 (4)	0.8818 (3)	0.0424 (10)
H3A	0.2555	0.9297	0.9451	0.051*
H3B	0.1099	1.0092	0.8665	0.051*
C4	0.3151 (4)	1.1428 (4)	0.8848 (3)	0.0362 (9)
H4A	0.2619	1.2139	0.8301	0.043*
H4B	0.3217	1.2040	0.9441	0.043*
C5	0.1604 (4)	0.9162 (5)	0.7086 (3)	0.0423 (10)
H5A	0.1562	1.0382	0.7049	0.051*
H5B	0.0518	0.8745	0.6925	0.051*
C6	0.2386 (4)	0.8496 (5)	0.6363 (2)	0.0361 (9)
H6A	0.2138	0.7309	0.6249	0.043*
H6B	0.1970	0.9086	0.5751	0.043*
N1	0.2476 (3)	0.8648 (3)	0.80846 (19)	0.0254 (6)
N2	0.7314 (3)	0.8811 (4)	0.8330 (2)	0.0405 (7)
N3	0.8273 (4)	0.8233 (4)	0.9028 (2)	0.0388 (8)
N4	0.9226 (5)	0.7663 (5)	0.9675 (3)	0.0703 (12)
O1	0.4947 (3)	0.6485 (3)	0.88538 (18)	0.0332 (6)
O2	0.4718 (3)	1.1008 (3)	0.88087 (18)	0.0344 (6)
O3	0.4087 (2)	0.8714 (3)	0.67098 (14)	0.0269 (5)
H1OA	0.508 (6)	1.183 (7)	0.863 (4)	0.11 (2)*
H2OA	0.525 (4)	0.569 (4)	0.870 (3)	0.035 (12)*

	U11	U22	U33	U12	U13	U23
Co1	0.0262 (2)	0.0243 (2)	0.0272 (2)	−0.0003 (2)	0.00739 (18)	0.0007 (2)
C1	0.040 (2)	0.0305 (19)	0.064 (3)	−0.0069 (17)	0.021 (2)	0.0004 (18)
C2	0.050 (2)	0.0339 (19)	0.046 (2)	0.002 (2)	0.0274 (19)	0.0055 (19)
C3	0.044 (2)	0.034 (2)	0.059 (2)	−0.0046 (18)	0.030 (2)	−0.0111 (19)
C4	0.042 (2)	0.0266 (19)	0.048 (2)	−0.0025 (18)	0.0257 (18)	−0.0068 (17)
C5	0.029 (2)	0.054 (3)	0.043 (2)	0.0035 (18)	0.0095 (17)	−0.0026 (18)
C6	0.0263 (19)	0.045 (2)	0.0335 (19)	−0.0002 (17)	0.0027 (16)	−0.0022 (17)
N1	0.0282 (14)	0.0220 (13)	0.0280 (14)	−0.0013 (13)	0.0114 (12)	−0.0021 (12)
N2	0.0264 (16)	0.0488 (18)	0.0465 (19)	0.0014 (16)	0.0112 (15)	0.0126 (17)
N3	0.0272 (18)	0.047 (2)	0.045 (2)	−0.0005 (15)	0.0145 (16)	−0.0082 (16)
N4	0.046 (2)	0.107 (3)	0.050 (2)	0.024 (2)	0.001 (2)	0.008 (2)
O1	0.0377 (15)	0.0227 (15)	0.0420 (15)	0.0045 (12)	0.0163 (12)	0.0026 (12)
O2	0.0372 (15)	0.0274 (14)	0.0411 (14)	−0.0091 (12)	0.0152 (11)	−0.0053 (12)
O3	0.0265 (12)	0.0302 (12)	0.0252 (11)	0.0039 (12)	0.0093 (9)	0.0022 (11)

Co1—O3	1.991 (2)	C3—H3B	0.9700
Co1—N2	2.013 (3)	C4—O2	1.433 (4)
Co1—O1	2.064 (2)	C4—H4A	0.9700
Co1—O2	2.065 (2)	C4—H4B	0.9700
Co1—N1	2.148 (3)	C5—N1	1.475 (4)
C1—N1	1.478 (4)	C5—C6	1.502 (5)
C1—C2	1.486 (5)	C5—H5A	0.9700
C1—H1A	0.9700	C5—H5B	0.9700
C1—H1B	0.9700	C6—O3	1.439 (4)
C2—O1	1.430 (4)	C6—H6A	0.9700
C2—H2A	0.9700	C6—H6B	0.9700
C2—H2B	0.9700	N2—N3	1.197 (4)
C3—N1	1.476 (4)	N3—N4	1.147 (4)
C3—C4	1.501 (5)	O1—H2OA	0.74 (3)
C3—H3A	0.9700	O2—H1OA	0.81 (5)
O3—Co1—N2	101.32 (11)	O2—C4—H4B	110.0
O3—Co1—O1	116.37 (10)	C3—C4—H4B	110.0
N2—Co1—O1	96.24 (12)	H4A—C4—H4B	108.3
O3—Co1—O2	115.60 (10)	N1—C5—C6	111.6 (3)
N2—Co1—O2	99.08 (12)	N1—C5—H5A	109.3
O1—Co1—O2	121.07 (10)	C6—C5—H5A	109.3
O3—Co1—N1	83.24 (9)	N1—C5—H5B	109.3
N2—Co1—N1	175.37 (11)	C6—C5—H5B	109.3
O1—Co1—N1	80.87 (10)	H5A—C5—H5B	108.0
O2—Co1—N1	79.50 (10)	O3—C6—C5	110.8 (3)
N1—C1—C2	110.6 (3)	O3—C6—H6A	109.5
N1—C1—H1A	109.5	C5—C6—H6A	109.5
C2—C1—H1A	109.5	O3—C6—H6B	109.5
N1—C1—H1B	109.5	C5—C6—H6B	109.5
C2—C1—H1B	109.5	H6A—C6—H6B	108.1
H1A—C1—H1B	108.1	C5—N1—C3	112.2 (3)
O1—C2—C1	110.6 (3)	C5—N1—C1	112.6 (3)
O1—C2—H2A	109.5	C3—N1—C1	111.0 (3)
C1—C2—H2A	109.5	C5—N1—Co1	105.15 (19)
O1—C2—H2B	109.5	C3—N1—Co1	107.8 (2)
C1—C2—H2B	109.5	C1—N1—Co1	107.6 (2)
H2A—C2—H2B	108.1	N3—N2—Co1	122.8 (2)
N1—C3—C4	111.4 (3)	N4—N3—N2	177.5 (4)
N1—C3—H3A	109.4	C2—O1—Co1	113.2 (2)
C4—C3—H3A	109.4	C2—O1—H2OA	109 (3)
N1—C3—H3B	109.4	Co1—O1—H2OA	123 (3)
C4—C3—H3B	109.4	C4—O2—Co1	116.5 (2)
H3A—C3—H3B	108.0	C4—O2—H1OA	107 (4)
O2—C4—C3	108.7 (3)	Co1—O2—H1OA	117 (4)
O2—C4—H4A	110.0	C6—O3—Co1	113.77 (18)
C3—C4—H4A	110.0

D—H···A	D—H	H···A	D···A	D—H···A
O2—H1OA···O3i	0.80 (6)	1.80 (6)	2.595 (3)	176.90
O1—H2OA···O3ii	0.74 (3)	1.83 (3)	2.573 (3)	177.70

Table 1

Selected bond lengths (Å)

Co1—O3	1.991 (2)
Co1—N2	2.013 (3)
Co1—O1	2.064 (2)
Co1—O2	2.065 (2)
Co1—N1	2.148 (3)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H1OA⋯O3i	0.80 (6)	1.80 (6)	2.595 (3)	176.90
O1—H2OA⋯O3ii	0.74 (3)	1.83 (3)	2.573 (3)	177.70

Symmetry codes: (i) ; (ii) .