Literature DB >> 21583762

Poly[[diaqua-{N-[1-(3-pyrid-yl)ethyl-idene]-4H-1,2,4-triazol-4-amine}zinc(II)] bis-(perchlorate)].

Xiaodan Sun¹, Xianhua He, Wei Wang, Donghua Miao, Qiaozhen Sun.

Abstract

In the title compound, {[Zn(C(9)H(9)N(5))(2)(H(2)O)(2)](ClO(4))(2)}(n), the Zn(II) ion lies on an inversion center and is coordinated by two triazolyl N atoms and two pyridyl N atoms from four symmetry-related N-1-(3-pyrid-yl)ethyl-idene-4H-1,2,4-triazol-4-amine (L) ligands and two O atoms from coordinated water mol-ecules in a slightly distorted octa-hedral environment. Each L ligand bridges symmetry-related Zn(II) ions, forming a two-dimensional layer with a (4,4) grid. In the crystal structure, inter-molecular O-H⋯O hydrogen bonds connect perchlorate counter-anions to the layers.

Entities: CellLine Chemical Disease Species

Year: 2009 PMID： 21583762 PMCID： PMC2977576 DOI： 10.1107/S1600536809013130

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For the structures of triazole complexes, see: Wang et al. (2006 ▶, 2007 ▶); Drabent et al. (2003 ▶, 2004 ▶, 2008 ▶); Sun et al. (2009a ▶,b ▶); Yi et al. (2004 ▶). For general background information, see: Beckmann & Brooker (2003 ▶); Ding et al. (2007 ▶); Haasnoot (2000 ▶); Klingele & Brooker (2003 ▶); Zhai et al. (2006 ▶). For the (4,4) topology, see: Batten & Robson (1998 ▶).

Experimental

Crystal data

[Zn(C9H9N5)2(H2O)2](ClO4)2 M = 674.75 Monoclinic, a = 7.4929 (9) Å b = 10.0963 (12) Å c = 17.149 (2) Å β = 94.887 (2)° V = 1292.6 (3) Å3 Z = 2 Mo Kα radiation μ = 1.23 mm−1 T = 293 K 0.38 × 0.30 × 0.30 mm

Data collection

Bruker SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.647, T max = 0.697 6344 measured reflections 2266 independent reflections 1856 reflections with I > 2σ(I) R int = 0.053

Refinement

R[F 2 > 2σ(F 2)] = 0.044 wR(F 2) = 0.130 S = 1.05 2266 reflections 187 parameters H-atom parameters constrained Δρmax = 0.34 e Å−3 Δρmin = −0.35 e Å−3 Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL, DIAMOND (Brandenburg & Putz, 1999 ▶) and OLEX (Dolomanov et al., 2003 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809013130/lh2801sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809013130/lh2801Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Zn(C₉H₉N₅)₂(H₂O)₂](ClO₄)₂	F(000) = 688
M_r = 674.75	D_x = 1.734 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 2652 reflections
a = 7.4929 (9) Å	θ = 2.4–27.8°
b = 10.0963 (12) Å	µ = 1.23 mm⁻¹
c = 17.149 (2) Å	T = 293 K
β = 94.887 (2)°	Block, colourless
V = 1292.6 (3) Å³	0.38 × 0.30 × 0.30 mm
Z = 2

Bruker SMART CCD diffractometer	2266 independent reflections
Radiation source: fine-focus sealed tube	1856 reflections with I > 2σ(I)
graphite	R_int = 0.053
φ and ω scans	θ_max = 25.0°, θ_min = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −8→8
T_min = 0.647, T_max = 0.697	k = −11→11
6344 measured reflections	l = −20→18

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) = 0.130	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0859P)² + 0.0827P] where P = (F_o² + 2F_c²)/3
2266 reflections	(Δ/σ)_max < 0.001
187 parameters	Δρ_max = 0.34 e Å⁻³
0 restraints	Δρ_min = −0.35 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	U_iso*/U_eq
Zn1	0.5000	0.0000	0.0000	0.0318 (2)
N1	0.6739 (4)	0.0235 (3)	0.10252 (15)	0.0313 (6)
N2	0.8545 (4)	0.0414 (3)	0.09414 (16)	0.0388 (7)
N3	0.8080 (3)	0.0549 (3)	0.21762 (14)	0.0295 (6)
N4	0.8448 (4)	0.0976 (3)	0.29546 (14)	0.0339 (6)
N5	0.9165 (4)	0.2865 (3)	0.50082 (15)	0.0346 (6)
C1	0.6489 (4)	0.0320 (3)	0.17647 (18)	0.0311 (7)
H1B	0.5392	0.0237	0.1976	0.037*
C2	0.9296 (4)	0.0616 (4)	0.16374 (18)	0.0375 (8)
H2B	1.0511	0.0784	0.1753	0.045*
C3	0.7815 (4)	0.0301 (3)	0.34965 (19)	0.0305 (7)
C4	0.6845 (5)	−0.0988 (3)	0.3412 (2)	0.0433 (9)
H4B	0.6757	−0.1257	0.2873	0.065*
H4C	0.5665	−0.0889	0.3582	0.065*
H4D	0.7489	−0.1648	0.3726	0.065*
C5	0.8132 (4)	0.0933 (3)	0.42821 (17)	0.0289 (7)
C6	0.7662 (5)	0.0350 (4)	0.4965 (2)	0.0383 (8)
H6A	0.7139	−0.0486	0.4953	0.046*
C7	0.7979 (5)	0.1027 (4)	0.56667 (19)	0.0419 (9)
H7A	0.7705	0.0639	0.6134	0.050*
C8	0.8695 (5)	0.2266 (4)	0.56639 (19)	0.0388 (8)
H8A	0.8870	0.2721	0.6136	0.047*
C9	0.8878 (4)	0.2192 (3)	0.43411 (18)	0.0336 (8)
H9A	0.9199	0.2592	0.3885	0.040*
Cl1	0.65614 (11)	0.77575 (8)	0.69869 (5)	0.0395 (3)
O2	0.6939 (3)	0.9043 (3)	0.73148 (17)	0.0567 (7)
O1	0.5062 (4)	0.7213 (3)	0.7307 (2)	0.0798 (11)
O3	0.6227 (7)	0.7890 (4)	0.6170 (2)	0.1085 (14)
O4	0.8049 (5)	0.6906 (3)	0.7127 (3)	0.0937 (12)
O1W	0.7229 (3)	0.0328 (3)	−0.06446 (14)	0.0425 (6)
H1WA	0.8172	0.0228	−0.0338	0.051*
H1WB	0.7353	0.0972	−0.0954	0.051*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.0407 (4)	0.0362 (4)	0.0182 (3)	0.0009 (2)	0.0001 (2)	0.00160 (19)
N1	0.0336 (15)	0.0363 (16)	0.0236 (14)	0.0012 (12)	−0.0006 (11)	−0.0013 (11)
N2	0.0366 (16)	0.0505 (18)	0.0295 (16)	−0.0022 (14)	0.0039 (12)	−0.0054 (13)
N3	0.0340 (14)	0.0331 (15)	0.0205 (13)	−0.0001 (12)	−0.0014 (11)	−0.0046 (11)
N4	0.0432 (16)	0.0377 (16)	0.0202 (14)	−0.0052 (13)	−0.0014 (11)	−0.0075 (11)
N5	0.0452 (17)	0.0345 (16)	0.0235 (14)	−0.0029 (13)	−0.0003 (11)	−0.0017 (11)
C1	0.0358 (18)	0.0342 (18)	0.0231 (17)	0.0003 (14)	0.0018 (14)	−0.0037 (13)
C2	0.0329 (18)	0.049 (2)	0.0310 (19)	−0.0013 (16)	0.0051 (14)	−0.0044 (16)
C3	0.0302 (17)	0.0324 (18)	0.0281 (17)	0.0047 (14)	−0.0034 (14)	−0.0024 (14)
C4	0.060 (2)	0.035 (2)	0.0332 (19)	−0.0104 (17)	−0.0008 (16)	−0.0012 (15)
C5	0.0290 (16)	0.0318 (18)	0.0255 (16)	0.0025 (13)	0.0006 (12)	0.0020 (13)
C6	0.042 (2)	0.0398 (19)	0.0335 (19)	−0.0050 (16)	0.0045 (15)	0.0020 (15)
C7	0.051 (2)	0.048 (2)	0.0270 (18)	−0.0056 (17)	0.0055 (15)	0.0059 (15)
C8	0.050 (2)	0.044 (2)	0.0222 (17)	−0.0012 (16)	0.0023 (15)	−0.0005 (14)
C9	0.0439 (19)	0.0359 (19)	0.0212 (16)	−0.0003 (15)	0.0035 (13)	0.0014 (13)
Cl1	0.0451 (5)	0.0349 (5)	0.0397 (5)	0.0018 (4)	0.0111 (4)	−0.0036 (3)
O2	0.0545 (16)	0.0439 (16)	0.073 (2)	−0.0038 (13)	0.0105 (14)	−0.0182 (13)
O1	0.068 (2)	0.067 (2)	0.110 (3)	−0.0251 (17)	0.043 (2)	−0.0256 (18)
O3	0.196 (4)	0.089 (3)	0.041 (2)	0.001 (3)	0.010 (2)	−0.0046 (18)
O4	0.067 (2)	0.054 (2)	0.161 (4)	0.0276 (17)	0.012 (2)	0.011 (2)
O1W	0.0432 (14)	0.0514 (16)	0.0339 (14)	−0.0006 (12)	0.0092 (11)	0.0095 (11)

Zn1—O1W	2.106 (2)	C3—C5	1.491 (4)
Zn1—O1Wⁱ	2.106 (2)	C4—H4B	0.9600
Zn1—N1ⁱ	2.111 (3)	C4—H4C	0.9600
Zn1—N1	2.111 (3)	C4—H4D	0.9600
Zn1—N5ⁱⁱ	2.245 (3)	C5—C6	1.382 (4)
Zn1—N5ⁱⁱⁱ	2.245 (3)	C5—C9	1.389 (5)
N1—C1	1.301 (4)	C6—C7	1.387 (5)
N1—N2	1.385 (4)	C6—H6A	0.9300
N2—C2	1.292 (4)	C7—C8	1.362 (5)
N3—C1	1.352 (4)	C7—H7A	0.9300
N3—C2	1.354 (4)	C8—H8A	0.9300
N3—N4	1.408 (3)	C9—H9A	0.9300
N4—C3	1.276 (4)	Cl1—O1	1.404 (3)
N5—C9	1.332 (4)	Cl1—O3	1.409 (4)
N5—C8	1.349 (4)	Cl1—O4	1.412 (3)
N5—Zn1^iv	2.245 (3)	Cl1—O2	1.433 (3)
C1—H1B	0.9300	O1W—H1WA	0.8500
C2—H2B	0.9300	O1W—H1WB	0.8500
C3—C4	1.491 (5)

O1W—Zn1—O1Wⁱ	180	N4—C3—C5	112.9 (3)
O1W—Zn1—N1ⁱ	92.38 (10)	C4—C3—C5	120.0 (3)
O1Wⁱ—Zn1—N1ⁱ	87.62 (10)	C3—C4—H4B	109.5
O1W—Zn1—N1	87.62 (10)	C3—C4—H4C	109.5
O1Wⁱ—Zn1—N1	92.38 (10)	H4B—C4—H4C	109.5
N1ⁱ—Zn1—N1	180	C3—C4—H4D	109.5
O1W—Zn1—N5ⁱⁱ	94.97 (10)	H4B—C4—H4D	109.5
O1Wⁱ—Zn1—N5ⁱⁱ	85.03 (10)	H4C—C4—H4D	109.5
N1ⁱ—Zn1—N5ⁱⁱ	87.73 (10)	C6—C5—C9	117.2 (3)
N1—Zn1—N5ⁱⁱ	92.27 (10)	C6—C5—C3	123.4 (3)
O1W—Zn1—N5ⁱⁱⁱ	85.03 (10)	C9—C5—C3	119.3 (3)
O1Wⁱ—Zn1—N5ⁱⁱⁱ	94.97 (10)	C5—C6—C7	119.2 (3)
N1ⁱ—Zn1—N5ⁱⁱⁱ	92.27 (10)	C5—C6—H6A	120.4
N1—Zn1—N5ⁱⁱⁱ	87.73 (10)	C7—C6—H6A	120.4
N5ⁱⁱ—Zn1—N5ⁱⁱⁱ	180	C8—C7—C6	119.2 (3)
C1—N1—N2	108.4 (3)	C8—C7—H7A	120.4
C1—N1—Zn1	133.6 (2)	C6—C7—H7A	120.4
N2—N1—Zn1	117.9 (2)	N5—C8—C7	123.0 (3)
C2—N2—N1	106.1 (3)	N5—C8—H8A	118.5
C1—N3—C2	105.5 (3)	C7—C8—H8A	118.5
C1—N3—N4	129.8 (3)	N5—C9—C5	124.3 (3)
C2—N3—N4	122.9 (3)	N5—C9—H9A	117.8
C3—N4—N3	118.2 (3)	C5—C9—H9A	117.8
C9—N5—C8	116.9 (3)	O1—Cl1—O3	110.2 (3)
C9—N5—Zn1^iv	120.6 (2)	O1—Cl1—O4	110.0 (2)
C8—N5—Zn1^iv	121.9 (2)	O3—Cl1—O4	107.3 (3)
N1—C1—N3	109.0 (3)	O1—Cl1—O2	109.83 (17)
N1—C1—H1B	125.5	O3—Cl1—O2	108.5 (2)
N3—C1—H1B	125.5	O4—Cl1—O2	111.0 (2)
N2—C2—N3	110.9 (3)	Zn1—O1W—H1WA	108.1
N2—C2—H2B	124.5	Zn1—O1W—H1WB	125.6
N3—C2—H2B	124.5	H1WA—O1W—H1WB	110.4
N4—C3—C4	127.1 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···N2	0.85	2.20	2.814 (4)	130
O1W—H1WB···O4ⁱⁱⁱ	0.85	2.22	2.993 (5)	151
O1W—H1WB···O3ⁱⁱⁱ	0.85	2.26	3.003 (5)	147

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1WA⋯N2	0.85	2.20	2.814 (4)	130
O1W—H1WB⋯O4ⁱ	0.85	2.22	2.993 (5)	151
O1W—H1WB⋯O3ⁱ	0.85	2.26	3.003 (5)	147

Symmetry code: (i) .

7 in total

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5. Bis{4-[(4H-1,2,4-triazol-4-yl)iminomethyl]pyridinium} diaquapentanitratocerate(III).

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7. Novel triazole-bridged cadmium coordination polymers varying from zero- to three-dimensionality.

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7 in total