Poly[aqua­(μ1,1-azido)(μ-3H-1,2,3-tri­azolo[4,5-b]pyridin-3-olato)cobalt(II)]

Zhao, J.-P.; Liu, F.-C.

doi:10.1107/S1600536810023809

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 7| July 2010| Page m847

doi:10.1107/S1600536810023809

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Poly[aqua(μ_1,1-azido)(μ-3H-1,2,3-triazolo[4,5-b]pyridin-3-olato)cobalt(II)]

Jiong-Peng Zhao ^a and Fu-Chen Liu ^a ^*

^aSchool of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin 300191, People's Republic of China
^*Correspondence e-mail: fuchenliutj@yahoo.com

(Received 30 May 2010; accepted 19 June 2010; online 26 June 2010)

In the title compound, [Co(C₅H₃N₄O)(N₃)(H₂O)]_n, the cobalt ion is coordinated by three N atoms of two organic ligands, two N atoms of two azide anions and one water molecule in a distorted octahedral geometry. The metal atoms are connected via the ligands into layers, which are further connected by O—H⋯N and O—H⋯O hydrogen bonding.

Related literature

For the coordination modes of azide anions, see: Zeng et al. (2009 ). For the preparation and chacterization of metal–azide complexes with different co-ligands, see: Wang et al. (2008 ).

Experimental

Crystal data

[Co(C₅H₃N₄O)(N₃)(H₂O)]
M_r = 254.09
Monoclinic, P 2₁ /c
a = 7.0891 (14) Å
b = 10.122 (2) Å
c = 12.685 (4) Å
β = 113.08 (2)°
V = 837.4 (4) Å³
Z = 4
Mo Kα radiation
μ = 2.04 mm⁻¹
T = 293 K
0.20 × 0.18 × 0.18 mm

Data collection

Rigaku SCXmini diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.462, T_max = 1
6902 measured reflections
1469 independent reflections
1352 reflections with I > 2σ(I)
R_int = 0.040

Refinement

R[F² > 2σ(F²)] = 0.044
wR(F²) = 0.112
S = 1.09
1469 reflections
144 parameters
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.50 e Å⁻³
Δρ_min = −0.43 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1WB⋯N7ⁱ	0.74 (7)	2.15 (7)	2.894 (6)	178 (7)
O1W—H1WA⋯O1ⁱⁱ	0.84 (8)	1.87 (8)	2.661 (5)	156 (8)
Symmetry codes: (i) $[-x, y+{\script{1\over 2}}, -z-{\script{3\over 2}}]$ ; (ii) -x, -y-1, -z-1.

Data collection: SCXmini Benchtop Crystallography System Software (Rigaku, 2006 ); cell refinement: PROCESS-AUTO (Rigaku, 1998 ); data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996 ) and PLATON (Spek, 2009 ); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810023809/nc2187sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536810023809/nc2187Isup2.hkl

checkCIF report

Comment top

Azide anion has drawn much attentions because they can coordinate to metal ions in diverse coordination modes (Zeng, et al., 2009). Therefore, several metal azide complexes with different co-ligand has been prepared and characterized (Wang, et al., 2008). As a part on a project of new metal azide coordination polymers the structure of the title compound was determined.

In the crystal structure of the title compound the Co ions are coordinated by two N atoms of two symmetry related azide anion, three N atoms of two symmetry related organic ligands and one water molecule within slightly distorted octahedra (Fig. 1). The Co ions are connected via two end-on bridging thiocyanato anions into chains, that are further be connected into layers by the organic ligands. These layers are located in the b-c-plane and are linked via N-H···O and N-H···N hydrogen bonding to adjacent water molecules and azide anions (Fig. 2).

Related literature top

For the coordination modes of azide anions, see: Zeng et al. (2009). For the preparation and chacterzation of metal–azide complexes with different co-ligands, see: Wang et al. (2008).

Experimental top

A mixture of Co(II)nitrate (1.5mmol), 3H-[1,2,3]triazolo[4,5-b]pyridin-3-ol(0.75 mmol), and sodium azide (2mmol), in 10 ml MeOH solvent was sealed in a Teflon-lined stainless-steel Parr bomb that was heated at 413 K for 48 h. Red crystals of the title complex were collected after the bomb was allowed to cool to room temperature. Yield 20% based on metal salt.

Computing details top

Data collection: SCXmini Benchtop Crystallography System Software (Rigaku, 2006); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: PROCESS-AUTO (Rigaku, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and PLATON (Spek, 2009); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The structure of the complex with labelling and displacement ellipsoids drawn at the 30% probability level. Symmetry codes: i = x,-y-1/2,z-1/2, ii = -x+1,-y-1,-z-1 and iii = x,-y-1/2,z+1/2
	Fig. 2. Crystal structure of the title compound with view along the c axis.

Poly[aqua(µ_1,1-azido)(µ-3H-1,2,3-triazolo[4,5- b]pyridin-3-olato)cobalt(II)] top

Crystal data top

[Co(C₅H₃N₄O)(N₃)(H₂O)]	F(000) = 508
M_r = 254.09	D_x = 2.015 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 7.0891 (14) Å	Cell parameters from 7903 reflections
b = 10.122 (2) Å	θ = 3.1–27.7°
c = 12.685 (4) Å	µ = 2.04 mm⁻¹
β = 113.08 (2)°	T = 293 K
V = 837.4 (4) Å³	Block, red
Z = 4	0.2 × 0.18 × 0.18 mm

Data collection top

Rigaku SCXmini diffractometer	1469 independent reflections
Radiation source: fine-focus sealed tube	1352 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.040
ω scans	θ_max = 25.0°, θ_min = 3.1°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −8→8
T_min = 0.462, T_max = 1	k = −12→12
6902 measured reflections	l = −15→15

Refinement top

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)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.112	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ²(F_o²) + (0.0466P)² + 3.7642P] where P = (F_o² + 2F_c²)/3
1469 reflections	(Δ/σ)_max < 0.001
144 parameters	Δρ_max = 1.50 e Å⁻³
0 restraints	Δρ_min = −0.43 e Å⁻³

Crystal data top

[Co(C₅H₃N₄O)(N₃)(H₂O)]	V = 837.4 (4) Å³
M_r = 254.09	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 7.0891 (14) Å	µ = 2.04 mm⁻¹
b = 10.122 (2) Å	T = 293 K
c = 12.685 (4) Å	0.2 × 0.18 × 0.18 mm
β = 113.08 (2)°

Data collection top

Rigaku SCXmini diffractometer	1469 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	1352 reflections with I > 2σ(I)
T_min = 0.462, T_max = 1	R_int = 0.040
6902 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.044	0 restraints
wR(F²) = 0.112	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	Δρ_max = 1.50 e Å⁻³
1469 reflections	Δρ_min = −0.43 e Å⁻³
144 parameters

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 (Å²) top

	x	y	z	U_iso*/U_eq
Co1	0.30993 (8)	−0.38921 (6)	−0.53843 (5)	0.0158 (2)
O1	0.2961 (5)	−0.4313 (3)	−0.3763 (3)	0.0234 (7)
N1	0.3036 (6)	−0.1727 (4)	−0.1987 (3)	0.0212 (8)
N2	0.3051 (6)	−0.3027 (4)	−0.2197 (3)	0.0204 (8)
N3	0.2971 (5)	−0.3160 (4)	−0.3251 (3)	0.0179 (8)
N4	0.2849 (6)	−0.1814 (4)	−0.4803 (3)	0.0211 (8)
N5	0.3650 (6)	−0.5988 (4)	−0.5436 (3)	0.0213 (8)
N6	0.2624 (6)	−0.6837 (4)	−0.6055 (3)	0.0230 (9)
N7	0.1639 (8)	−0.7656 (5)	−0.6637 (4)	0.0420 (12)
C1	0.2719 (7)	−0.0579 (5)	−0.5091 (4)	0.0261 (11)
H1A	0.2669	−0.0371	−0.5816	0.031*
C2	0.2650 (9)	0.0474 (5)	−0.4373 (4)	0.0317 (11)
H2A	0.2529	0.1337	−0.4644	0.038*
C3	0.2756 (8)	0.0249 (5)	−0.3296 (4)	0.0261 (10)
H3A	0.2724	0.0936	−0.2817	0.031*
C4	0.2914 (7)	−0.1065 (5)	−0.2948 (4)	0.0225 (10)
C5	0.2908 (6)	−0.1985 (4)	−0.3742 (3)	0.0172 (9)
O1W	−0.0066 (6)	−0.3972 (5)	−0.6162 (4)	0.0402 (10)
H1WB	−0.045 (10)	−0.364 (7)	−0.673 (6)	0.05 (2)*
H1WA	−0.078 (12)	−0.466 (8)	−0.626 (7)	0.07 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0175 (3)	0.0180 (3)	0.0126 (3)	−0.0012 (2)	0.0067 (2)	0.0002 (2)
O1	0.0313 (18)	0.0192 (16)	0.0224 (16)	−0.0006 (14)	0.0135 (14)	−0.0048 (13)
N1	0.0208 (19)	0.027 (2)	0.0158 (18)	0.0013 (16)	0.0071 (15)	0.0004 (16)
N2	0.029 (2)	0.0180 (19)	0.0177 (18)	0.0012 (16)	0.0130 (16)	0.0002 (15)
N3	0.0213 (19)	0.0178 (19)	0.0165 (18)	−0.0005 (15)	0.0094 (15)	−0.0018 (15)
N4	0.0217 (19)	0.029 (2)	0.0139 (18)	0.0027 (16)	0.0087 (15)	0.0016 (16)
N5	0.0205 (19)	0.019 (2)	0.023 (2)	−0.0030 (16)	0.0070 (16)	−0.0041 (16)
N6	0.026 (2)	0.023 (2)	0.0179 (19)	−0.0030 (18)	0.0063 (17)	0.0031 (18)
N7	0.050 (3)	0.035 (3)	0.031 (2)	−0.018 (2)	0.004 (2)	−0.006 (2)
C1	0.032 (3)	0.033 (3)	0.020 (2)	−0.006 (2)	0.017 (2)	−0.004 (2)
C2	0.049 (3)	0.023 (3)	0.026 (3)	−0.001 (2)	0.017 (2)	0.004 (2)
C3	0.037 (3)	0.022 (2)	0.022 (2)	0.000 (2)	0.014 (2)	−0.0031 (19)
C4	0.022 (2)	0.027 (3)	0.019 (2)	0.0011 (19)	0.0094 (18)	0.0003 (19)
C5	0.018 (2)	0.020 (2)	0.014 (2)	−0.0006 (17)	0.0074 (17)	−0.0007 (17)
O1W	0.0229 (19)	0.051 (3)	0.037 (2)	−0.0086 (18)	0.0013 (17)	0.021 (2)

Geometric parameters (Å, º) top

Co1—O1W	2.069 (4)	N4—C5	1.341 (5)
Co1—N1ⁱ	2.111 (4)	N5—N6	1.198 (5)
Co1—N5ⁱⁱ	2.128 (4)	N5—Co1ⁱⁱ	2.128 (4)
Co1—O1	2.140 (3)	N6—N7	1.147 (6)
Co1—N5	2.163 (4)	C1—C2	1.416 (7)
Co1—N4	2.259 (4)	C1—H1A	0.9300
O1—N3	1.334 (5)	C2—C3	1.357 (7)
N1—N2	1.343 (5)	C2—H2A	0.9300
N1—C4	1.365 (6)	C3—C4	1.392 (7)
N1—Co1ⁱⁱⁱ	2.111 (4)	C3—H3A	0.9300
N2—N3	1.323 (5)	C4—C5	1.371 (6)
N3—C5	1.335 (6)	O1W—H1WB	0.74 (7)
N4—C1	1.295 (6)	O1W—H1WA	0.84 (8)

O1W—Co1—N1ⁱ	86.72 (16)	C1—N4—Co1	144.3 (3)
O1W—Co1—N5ⁱⁱ	174.45 (17)	C5—N4—Co1	103.4 (3)
N1ⁱ—Co1—N5ⁱⁱ	95.61 (15)	N6—N5—Co1ⁱⁱ	122.8 (3)
O1W—Co1—O1	90.03 (15)	N6—N5—Co1	130.7 (3)
N1ⁱ—Co1—O1	173.20 (13)	Co1ⁱⁱ—N5—Co1	102.40 (15)
N5ⁱⁱ—Co1—O1	88.16 (14)	N7—N6—N5	179.2 (5)
O1W—Co1—N5	97.02 (17)	N4—C1—C2	124.2 (4)
N1ⁱ—Co1—N5	101.43 (15)	N4—C1—H1A	117.9
N5ⁱⁱ—Co1—N5	77.60 (15)	C2—C1—H1A	117.9
O1—Co1—N5	84.88 (13)	C3—C2—C1	121.3 (5)
O1W—Co1—N4	89.00 (17)	C3—C2—H2A	119.4
N1ⁱ—Co1—N4	93.61 (14)	C1—C2—H2A	119.4
N5ⁱⁱ—Co1—N4	95.87 (14)	C2—C3—C4	116.4 (4)
O1—Co1—N4	80.35 (12)	C2—C3—H3A	121.8
N5—Co1—N4	164.06 (14)	C4—C3—H3A	121.8
N3—O1—Co1	107.4 (2)	N1—C4—C5	107.7 (4)
N2—N1—C4	107.9 (4)	N1—C4—C3	136.2 (4)
N2—N1—Co1ⁱⁱⁱ	118.9 (3)	C5—C4—C3	116.1 (4)
C4—N1—Co1ⁱⁱⁱ	133.2 (3)	N3—C5—N4	124.4 (4)
N3—N2—N1	107.4 (3)	N3—C5—C4	105.8 (4)
N2—N3—O1	124.8 (3)	N4—C5—C4	129.8 (4)
N2—N3—C5	111.2 (3)	Co1—O1W—H1WB	111 (5)
O1—N3—C5	124.0 (3)	Co1—O1W—H1WA	125 (5)
C1—N4—C5	112.2 (4)	H1WB—O1W—H1WA	105 (7)

O1W—Co1—O1—N3	−93.8 (3)	N5ⁱⁱ—Co1—N5—Co1ⁱⁱ	0.0
N1ⁱ—Co1—O1—N3	−32.4 (12)	O1—Co1—N5—Co1ⁱⁱ	−89.23 (15)
N5ⁱⁱ—Co1—O1—N3	91.4 (3)	N4—Co1—N5—Co1ⁱⁱ	−67.1 (5)
N5—Co1—O1—N3	169.1 (3)	Co1ⁱⁱ—N5—N6—N7	91 (38)
N4—Co1—O1—N3	−4.9 (2)	Co1—N5—N6—N7	−116 (38)
C4—N1—N2—N3	0.9 (5)	C5—N4—C1—C2	0.0 (7)
Co1ⁱⁱⁱ—N1—N2—N3	179.0 (3)	Co1—N4—C1—C2	−177.8 (4)
N1—N2—N3—O1	179.9 (4)	N4—C1—C2—C3	1.3 (8)
N1—N2—N3—C5	0.1 (5)	C1—C2—C3—C4	−0.6 (8)
Co1—O1—N3—N2	−174.8 (3)	N2—N1—C4—C5	−1.5 (5)
Co1—O1—N3—C5	4.9 (5)	Co1ⁱⁱⁱ—N1—C4—C5	−179.3 (3)
O1W—Co1—N4—C1	−87.4 (6)	N2—N1—C4—C3	176.7 (5)
N1ⁱ—Co1—N4—C1	−0.8 (6)	Co1ⁱⁱⁱ—N1—C4—C3	−1.1 (8)
N5ⁱⁱ—Co1—N4—C1	95.3 (6)	C2—C3—C4—N1	−179.2 (5)
O1—Co1—N4—C1	−177.6 (6)	C2—C3—C4—C5	−1.1 (7)
N5—Co1—N4—C1	160.0 (5)	N2—N3—C5—N4	179.1 (4)
O1W—Co1—N4—C5	94.7 (3)	O1—N3—C5—N4	−0.7 (6)
N1ⁱ—Co1—N4—C5	−178.7 (3)	N2—N3—C5—C4	−1.1 (5)
N5ⁱⁱ—Co1—N4—C5	−82.7 (3)	O1—N3—C5—C4	179.1 (4)
O1—Co1—N4—C5	4.5 (3)	C1—N4—C5—N3	177.6 (4)
N5—Co1—N4—C5	−17.9 (6)	Co1—N4—C5—N3	−3.7 (5)
O1W—Co1—N5—N6	24.1 (4)	C1—N4—C5—C4	−2.2 (7)
N1ⁱ—Co1—N5—N6	−64.0 (4)	Co1—N4—C5—C4	176.5 (4)
N5ⁱⁱ—Co1—N5—N6	−157.3 (5)	N1—C4—C5—N3	1.6 (5)
O1—Co1—N5—N6	113.5 (4)	C3—C4—C5—N3	−177.0 (4)
N4—Co1—N5—N6	135.6 (5)	N1—C4—C5—N4	−178.6 (4)
O1W—Co1—N5—Co1ⁱⁱ	−178.63 (17)	C3—C4—C5—N4	2.8 (7)
N1ⁱ—Co1—N5—Co1ⁱⁱ	93.31 (16)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WB···N7^iv	0.74 (7)	2.15 (7)	2.894 (6)	178 (7)
O1W—H1WA···O1^v	0.84 (8)	1.87 (8)	2.661 (5)	156 (8)

Symmetry codes: (iv) −x, y+1/2, −z−3/2; (v) −x, −y−1, −z−1.

Experimental details

Crystal data
Chemical formula	[Co(C₅H₃N₄O)(N₃)(H₂O)]
M_r	254.09
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	7.0891 (14), 10.122 (2), 12.685 (4)
β (°)	113.08 (2)
V (Å³)	837.4 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.04
Crystal size (mm)	0.2 × 0.18 × 0.18

Data collection
Diffractometer	Rigaku SCXmini diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.462, 1
No. of measured, independent and observed [I > 2σ(I)] reflections	6902, 1469, 1352
R_int	0.040
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.112, 1.09
No. of reflections	1469
No. of parameters	144
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.50, −0.43

Computer programs: SCXmini Benchtop Crystallography System Software (Rigaku, 2006), PROCESS-AUTO (Rigaku, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEPIII (Burnett & Johnson, 1996) and PLATON (Spek, 2009), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WB···N7ⁱ	0.74 (7)	2.15 (7)	2.894 (6)	178 (7)
O1W—H1WA···O1ⁱⁱ	0.84 (8)	1.87 (8)	2.661 (5)	156 (8)

Symmetry codes: (i) −x, y+1/2, −z−3/2; (ii) −x, −y−1, −z−1.

Acknowledgements

The authors acknowledge financial support from Tianjin Municipal Education Commission (grant No. 20060503).

References

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