catena-Poly[[triaqua­zinc(II)]-μ-1H-1,2,4-triazole-3,5-dicarboxyl­ato]

Sun, Y.-Y.; Zhang, Y.-W.; Zhang, G.; Cheng, L.

doi:10.1107/S1600536808023994

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 9| September 2008| Page m1113

doi:10.1107/S1600536808023994

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catena-Poly[[triaquazinc(II)]-μ-1H-1,2,4-triazole-3,5-dicarboxylato]

Yan-Yan Sun,^a Ya-Wen Zhang,^a Gong Zhang ^b and Lin Cheng ^a ^*

^aDepartment of Chemistry and Chemical Engineering, Southeast University, Nanjing, People's Republic of China, and ^bDepartment of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing, People's Republic of China
^*Correspondence e-mail: cep02chl@yahoo.com.cn

(Received 22 July 2008; accepted 29 July 2008; online 6 August 2008)

In the title compound, [Zn(C₄HN₃O₄)(H₂O)₃]_n, each Zn^II atom adopts a distorted octahedral coordination geometry, being surrounded by one chelating and one monodentate 1H-1,2,4-triazole-3,5-dicarboxylate ligand and three water molecules. Adjacent Zn^II cations are linked by a 1H-1,2,4-triazole-3,5-dicarboxylate ligand in a μ₂,κ³ fashion to form a chain running along the c axis. The crystal packing is stabilized by N—H⋯O, O—H⋯N and O—H⋯O hydrogen bonds.

Related literature

For related literature, see: Yang et al. (2004 ); Yin et al. (2001 ); Tian et al. (2003 ).

Experimental

Crystal data

[Zn(C₄HN₃O₄)(H₂O)₃]
M_r = 274.50
Monoclinic, P 2₁ /c
a = 10.7388 (11) Å
b = 6.6608 (7) Å
c = 13.7789 (10) Å
β = 120.384 (6)°
V = 850.22 (14) Å³
Z = 4
Mo Kα radiation
μ = 2.92 mm⁻¹
T = 293 (2) K
0.13 × 0.12 × 0.12 mm

Data collection

Bruker APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2000 ) T_min = 0.703, T_max = 0.721
4297 measured reflections
1652 independent reflections
1501 reflections with I > 2σ(I)
R_int = 0.026

Refinement

R[F² > 2σ(F²)] = 0.034
wR(F²) = 0.090
S = 1.06
1652 reflections
136 parameters
H-atom parameters constrained
Δρ_max = 0.53 e Å⁻³
Δρ_min = −0.31 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2A⋯O1ⁱ	0.81	1.95	2.723 (3)	161
O1W—H1WA⋯O2ⁱⁱ	0.85	1.85	2.697 (3)	176
O1W—H1WB⋯O3Wⁱⁱⁱ	0.85	2.16	2.946 (3)	154
O2W—H2WA⋯N1^iv	0.85	2.08	2.925 (4)	172
O2W—H2WB⋯O3^v	0.85	2.01	2.848 (3)	170
O3W—H3WA⋯O3	0.85	1.86	2.708 (3)	174
O3W—H3WB⋯O4^v	0.85	1.91	2.753 (3)	174
Symmetry codes: (i) $[x, -y-{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (ii) $[-x-1, y+{\script{1\over 2}}, -z-{\script{3\over 2}}]$ ; (iii) -x, -y, -z-1; (iv) -x-1, -y-1, -z-1; (v) $[-x, y-{\script{1\over 2}}, -z-{\script{1\over 2}}]$ .

Data collection: SMART (Bruker, 2000 ); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; 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: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808023994/bt2754sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808023994/bt2754Isup2.hkl

checkCIF report

Comment top

Synthesis and characterization of coordination polymers is of great interest due to the formation of fascinating structures with interesting applications (Yin et al. 2001; Yang et al. 2004). Among these coordination polymers, one-dimensional chain complexes as important precursors of molecular magnets have attracted wide interest of experimental and theoretical chemists (Tian et al. 2003). Herein, we report a new one-dimensional compound [Zn(Htda)(H₂O)₃)]n (H₃tda = 1H-1,2,4-triazole-3,5-dicarboxylic acid).

The asymmetric unit of the title compound, [Zn(Htda)(H₂O)₃)]n (H₃tda = 1H-1,2,4-triazole-3,5-dicarboxylic acid), contains a Zn^II cation, a Htda anion and three coordinated water molecules. In the compound, the Zn^II ion displays a slightly distorted octahedral geometry, being surrounded by one chelating and one monodentate Htda ligands, and three H₂O molecules. Meanwhile, the adjacent Zn^II cations are linked by a µ³-Htda ligand to form a one-dimensional chain. The shortest intrachain Zn···Zn distance is 6.936 (4) Å. The chains are further stabilized by N—H···O and O—H···O hydrogen bonds.

Related literature top

For related literature, see: Yang et al. (2004); Yin et al. (2001); Tian et al. (2003).

Experimental top

A mixture of H₃tda (0.0157 g, 0.1 mmol), Zn(NO₃)₂.6H₂O (0.0297 g, 0.1 mmol), and water (10 ml) was stirred for 1 h at room temperature, and then filtered. The filtrate was allowed to evaporate slowly at room temperature. After 3 weeks, colorless block crystals were obtained in 30% yield (0.0082 g) based on Zn^II.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); 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: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. Local coordination environment of the title compound with 30% thermal ellipsoids. Symmetry code: a: x, -1/2 - y, -1/2 + z.
	Fig. 2. The one-dimensional chain of the title compound.

catena-Poly[[triaquazinc(II)]-µ-1H-1,2,4-triazole- 3,5-dicarboxylato] top

Crystal data top

[Zn(C₄HN₃O₄)(H₂O)₃]	F(000) = 552
M_r = 274.50	D_x = 2.144 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 805 reflections
a = 10.7388 (11) Å	θ = 2.5–28.0°
b = 6.6608 (7) Å	µ = 2.92 mm⁻¹
c = 13.7789 (10) Å	T = 293 K
β = 120.384 (6)°	Block, colourless
V = 850.22 (14) Å³	0.13 × 0.12 × 0.12 mm
Z = 4

Data collection top

Bruker APEX CCD diffractometer	1652 independent reflections
Radiation source: fine-focus sealed tube	1501 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.026
ϕ and ω scans	θ_max = 26.0°, θ_min = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 2000)	h = −12→13
T_min = 0.703, T_max = 0.721	k = −8→7
4297 measured reflections	l = −16→16

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)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.090	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0485P)² + 1.155P] where P = (F_o² + 2F_c²)/3
1652 reflections	(Δ/σ)_max < 0.001
136 parameters	Δρ_max = 0.53 e Å⁻³
0 restraints	Δρ_min = −0.31 e Å⁻³

Crystal data top

[Zn(C₄HN₃O₄)(H₂O)₃]	V = 850.22 (14) Å³
M_r = 274.50	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 10.7388 (11) Å	µ = 2.92 mm⁻¹
b = 6.6608 (7) Å	T = 293 K
c = 13.7789 (10) Å	0.13 × 0.12 × 0.12 mm
β = 120.384 (6)°

Data collection top

Bruker APEX CCD diffractometer	1652 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2000)	1501 reflections with I > 2σ(I)
T_min = 0.703, T_max = 0.721	R_int = 0.026
4297 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.034	0 restraints
wR(F²) = 0.090	H-atom parameters constrained
S = 1.06	Δρ_max = 0.53 e Å⁻³
1652 reflections	Δρ_min = −0.31 e Å⁻³
136 parameters

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
Zn1	−0.21910 (4)	−0.31001 (6)	−0.54678 (3)	0.01968 (16)
C1	−0.5300 (4)	−0.3318 (5)	−0.6300 (2)	0.0150 (6)
C2	−0.4615 (3)	−0.2580 (5)	−0.5104 (2)	0.0138 (6)
C3	−0.2985 (3)	−0.1691 (5)	−0.3493 (3)	0.0158 (6)
C4	−0.1588 (4)	−0.1138 (5)	−0.2453 (3)	0.0188 (7)
N1	−0.5320 (3)	−0.2264 (4)	−0.4566 (2)	0.0164 (6)
N2	−0.4261 (3)	−0.1687 (4)	−0.3544 (2)	0.0166 (6)
H2A	−0.4471	−0.1452	−0.3071	0.020*
N3	−0.3183 (3)	−0.2244 (4)	−0.4487 (2)	0.0155 (5)
O1	−0.4393 (2)	−0.3607 (4)	−0.66272 (18)	0.0200 (5)
O2	−0.6604 (3)	−0.3595 (4)	−0.68401 (19)	0.0258 (6)
O3	−0.0468 (3)	−0.1174 (5)	−0.2503 (2)	0.0327 (6)
O4	−0.1676 (2)	−0.0634 (4)	−0.16134 (18)	0.0227 (5)
O1W	−0.2327 (3)	−0.0209 (4)	−0.60933 (19)	0.0305 (6)
H1WA	−0.2626	0.0338	−0.6731	0.037*
H1WB	−0.1556	0.0484	−0.5776	0.037*
O2W	−0.1842 (2)	−0.6059 (4)	−0.47695 (19)	0.0231 (5)
H2WA	−0.2630	−0.6585	−0.4892	0.028*
H2WB	−0.1227	−0.6151	−0.4072	0.028*
O3W	−0.0099 (2)	−0.2331 (4)	−0.42261 (18)	0.0199 (5)
H3WA	−0.0169	−0.1900	−0.3675	0.024*
H3WB	0.0497	−0.3301	−0.3975	0.024*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.0174 (2)	0.0265 (2)	0.0153 (2)	−0.00014 (16)	0.00829 (18)	0.00025 (15)
C1	0.0181 (16)	0.0154 (15)	0.0108 (15)	−0.0001 (12)	0.0069 (13)	0.0002 (12)
C2	0.0149 (16)	0.0154 (14)	0.0108 (14)	0.0004 (12)	0.0062 (13)	0.0004 (12)
C3	0.0148 (16)	0.0180 (15)	0.0142 (15)	−0.0001 (12)	0.0070 (13)	0.0000 (12)
C4	0.0200 (17)	0.0205 (16)	0.0114 (15)	−0.0017 (14)	0.0047 (14)	−0.0023 (12)
N1	0.0147 (14)	0.0214 (14)	0.0127 (13)	−0.0021 (11)	0.0066 (11)	−0.0020 (10)
N2	0.0192 (14)	0.0234 (14)	0.0097 (13)	0.0000 (11)	0.0090 (12)	−0.0015 (10)
N3	0.0149 (14)	0.0185 (13)	0.0117 (13)	−0.0020 (11)	0.0058 (11)	−0.0016 (10)
O1	0.0192 (12)	0.0314 (13)	0.0105 (11)	−0.0023 (10)	0.0083 (10)	−0.0029 (9)
O2	0.0139 (12)	0.0414 (15)	0.0172 (12)	−0.0040 (11)	0.0042 (10)	−0.0087 (11)
O3	0.0151 (13)	0.0615 (18)	0.0201 (13)	−0.0055 (12)	0.0079 (11)	−0.0142 (12)
O4	0.0230 (13)	0.0337 (13)	0.0122 (11)	−0.0086 (11)	0.0095 (10)	−0.0049 (10)
O1W	0.0323 (15)	0.0272 (13)	0.0200 (12)	−0.0081 (11)	0.0045 (11)	0.0055 (10)
O2W	0.0187 (12)	0.0288 (13)	0.0187 (12)	−0.0025 (10)	0.0072 (10)	0.0037 (10)
O3W	0.0187 (12)	0.0252 (12)	0.0170 (11)	0.0015 (10)	0.0098 (10)	−0.0006 (10)

Geometric parameters (Å, º) top

Zn1—O1W	2.085 (2)	C3—C4	1.505 (5)
Zn1—O3W	2.085 (2)	C4—O3	1.241 (4)
Zn1—O4ⁱ	2.096 (2)	C4—O4	1.252 (4)
Zn1—O1	2.106 (2)	N1—N2	1.342 (4)
Zn1—O2W	2.141 (2)	N2—H2A	0.8053
Zn1—N3	2.177 (3)	O4—Zn1ⁱⁱ	2.096 (2)
C1—O2	1.223 (4)	O1W—H1WA	0.8499
C1—O1	1.278 (4)	O1W—H1WB	0.8500
C1—C2	1.508 (4)	O2W—H2WA	0.8500
C2—N1	1.316 (4)	O2W—H2WB	0.8500
C2—N3	1.348 (4)	O3W—H3WA	0.8500
C3—N3	1.328 (4)	O3W—H3WB	0.8500
C3—N2	1.336 (4)

O1W—Zn1—O3W	86.17 (10)	N2—C3—C4	123.4 (3)
O1W—Zn1—O4ⁱ	92.88 (10)	O3—C4—O4	125.8 (3)
O3W—Zn1—O4ⁱ	97.55 (9)	O3—C4—C3	118.0 (3)
O1W—Zn1—O1	91.02 (10)	O4—C4—C3	116.2 (3)
O3W—Zn1—O1	172.75 (9)	C2—N1—N2	102.3 (3)
O4ⁱ—Zn1—O1	89.25 (9)	C3—N2—N1	110.9 (3)
O1W—Zn1—O2W	174.71 (10)	C3—N2—H2A	131.1
O3W—Zn1—O2W	89.22 (9)	N1—N2—H2A	118.0
O4ⁱ—Zn1—O2W	85.14 (9)	C3—N3—C2	103.4 (3)
O1—Zn1—O2W	93.86 (9)	C3—N3—Zn1	147.1 (2)
O1W—Zn1—N3	93.49 (10)	C2—N3—Zn1	109.04 (19)
O3W—Zn1—N3	95.09 (9)	C1—O1—Zn1	118.15 (19)
O4ⁱ—Zn1—N3	166.20 (10)	C4—O4—Zn1ⁱⁱ	139.4 (2)
O1—Zn1—N3	78.40 (9)	Zn1—O1W—H1WA	137.2
O2W—Zn1—N3	89.51 (9)	Zn1—O1W—H1WB	116.3
O2—C1—O1	127.2 (3)	H1WA—O1W—H1WB	93.4
O2—C1—C2	119.3 (3)	Zn1—O2W—H2WA	111.1
O1—C1—C2	113.4 (3)	Zn1—O2W—H2WB	115.7
N1—C2—N3	114.6 (3)	H2WA—O2W—H2WB	108.8
N1—C2—C1	124.5 (3)	Zn1—O3W—H3WA	105.7
N3—C2—C1	120.9 (3)	Zn1—O3W—H3WB	115.1
N3—C3—N2	108.8 (3)	H3WA—O3W—H3WB	106.3
N3—C3—C4	127.8 (3)

Symmetry codes: (i) x, −y−1/2, z−1/2; (ii) 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
N2—H2A···O1ⁱⁱ	0.81	1.95	2.723 (3)	161
O1W—H1WA···O2ⁱⁱⁱ	0.85	1.85	2.697 (3)	176
O1W—H1WB···O3W^iv	0.85	2.16	2.946 (3)	154
O2W—H2WA···N1^v	0.85	2.08	2.925 (4)	172
O2W—H2WB···O3^vi	0.85	2.01	2.848 (3)	170
O3W—H3WA···O3	0.85	1.86	2.708 (3)	174
O3W—H3WB···O4^vi	0.85	1.91	2.753 (3)	174

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

Experimental details

Crystal data
Chemical formula	[Zn(C₄HN₃O₄)(H₂O)₃]
M_r	274.50
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	10.7388 (11), 6.6608 (7), 13.7789 (10)
β (°)	120.384 (6)
V (Å³)	850.22 (14)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.92
Crystal size (mm)	0.13 × 0.12 × 0.12

Data collection
Diffractometer	Bruker APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2000)
T_min, T_max	0.703, 0.721
No. of measured, independent and observed [I > 2σ(I)] reflections	4297, 1652, 1501
R_int	0.026
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.034, 0.090, 1.06
No. of reflections	1652
No. of parameters	136
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.53, −0.31

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2A···O1ⁱ	0.81	1.95	2.723 (3)	160.9
O1W—H1WA···O2ⁱⁱ	0.85	1.85	2.697 (3)	175.8
O1W—H1WB···O3Wⁱⁱⁱ	0.85	2.16	2.946 (3)	153.6
O2W—H2WA···N1^iv	0.85	2.08	2.925 (4)	171.7
O2W—H2WB···O3^v	0.85	2.01	2.848 (3)	170.1
O3W—H3WA···O3	0.85	1.86	2.708 (3)	173.9
O3W—H3WB···O4^v	0.85	1.91	2.753 (3)	173.5

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

Acknowledgements

The authors thank the Program for Young Excellent Talents in Southeast University for financial support.

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