7/28/2019 1267-3643Crystal structure of catena-aqua(--chlorido)(2-carboxylato- 5-methylpyrazine-"2N,O)copper(II) monohydr

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Crystal structure ofcatena-aqua(m-chlorido)(2-carboxylato-5-methylpyrazine-k2N,O)copper(II) monohydrate,

CuCl(H2O)(C6H6N2O2)

H2O

Hai-Jun Qiao*, Zhi-Gang Tang and Min Yang

Science College, Gansu Agricultural University, Lanzhou 730070, Gansu, P. R. China

Received August 5, 2011, accepted and available on-line March 6, 2012; CCDC no. 1267/3643

Abstract

C6H9ClCuN2O4, triclinic, P1 (no. 2), a = 3.8512(6) ,b = 11.401(2) , c = 11.559(2) , a = 111.337(2),b = 96.290(2), g = 98.626(2), V= 459.9 3, Z= 2,Rgt(F) = 0.038, wRref(F

2) = 0.104, T= 296 K.

Source of material

The blue single crystals of the title compound were obtained fromthe mixture of copper chloride dihydrate (0.0487 g, 0.25 mmol),5-methylpyrazine-2-carboxylic acid (0.03311 g, 0.25 mmol), ten

drops of concentrated hydrochloric acid and distilled water(10 mL) after slow evaporation at room temperature (yield 74 %).IR data are available in the CIF file.

Experimental details

The hydrogen atoms of water molecule were found in the differ-ence Fourier maps and refined freely. The remaining hydrogenatoms were positioned geometrically and allowed to ride on theirparent atoms with d(CH) = 0.93 and Uiso(H)=1.2 Ueq(C) foraromatic and d(CH) = 0.96 , Uiso(H) = 1.5 Ueq(C) for methylcarbon.

Discussion

Due to rapid advances in the past several years, the field of supra-molecular chemistry has progressed to the point where specified

supramolecular structures can often be obtained via the assemblyof judiciously selected organic ligand and metal ions under con-trolled reaction conditions [1,2]. But the attainment of rationalcontrol over desired topologies and applications is still a greatchallenge [3,4]. 5-methylpyrazine-2-carboxylic acid (abbrevi-

ated for 2,5-mpac), which exhibits the coordination characteris-tics of both the pyrazine and the carboxylate group, has proven tobe extremely versatile for the construction of new frameworkmaterials due to their ability to engage in several different coordi-nation modes [5-14].The title coordination polymer exhibits a three-dimensionalsupramolecular framework. The title crystal structure displays aone-dimensional chain structure constructed from copper atomsbridged by Clanions. The Cu2+ is coordinated with one N atom,two Cl atoms, and two O atoms, in which the N atom and one Oatom are from a 2,5-mpac ligand, and another O atom from coor-dinated water molecule, with d(Cu1O3) = 1.929(3) ,d(Cu1O1) = 1.984(3) , d( C u 1 N 1 ) = 2 . 0 0 2 ,

d(Cu1Cl1) = 2.264(1) and d(Cu1Cl1A) = 2.272(1) ,giving rise to a distorted pentahedral environment. Additionally,each Cl atomactsas bridgingligand to form an infinite chain. Theadjacent chainsare further connectedto forma three-dimensionalsupramolecular structure through hydrogen bonding betweenfree water molecules, 2,5-mpac ligands and coordinated watermolecules.

Z. Kristallogr. NCS 227 (2012) 207-208 / DOI 10.1524/ncrs.2012.0094 207

by Oldenbourg Wissenschaftsverlag, Mnchen

Crystal: blue block, size 0.07 0.08 0.10 mmWavelength: Mo Ka radiation (0.71073 )m: 26.54 cm-1

Diffractometer, scan mode: Bruker Smart APEX-II CCD,j/w2qmax: 50.08N(hkl)measured, N(hkl)unique: 2310, 1604Criterion forIobs, N(hkl)gt: Iobs > 2 s(Iobs), 1429N(param)refined: 144Programs: SHELXS-97, SHELXL-97 [15]

Table 1. Data collection and handling.

H(3) 2i 1.2366 0.9662 0.9103 0.036H(5) 2i 0.4421 0.6480 0.5917 0.034H(6A) 2i 0.4659 0.9392 0.5733 0.055H(6B) 2i 0.3616 0.7915 0.4900 0.055H(6C) 2i 0.7373 0.8705 0.4953 0.055

H(3A) 2i 0.401(7) 0.329(4) 0.821(5) 0.06(2)H(3B) 2i 0.76(1) 0.397(6) 0.914(4) 0.10(2)H(4A) 2i 0.07(2) 0.113(4) 0.749(8) 0.13(3)H(4B) 2i -0.141(9) 0.199(7) 0.729(8) 0.13(3)

Table 2. Atomic coordinates and displacement parameters (in 2).

Atom Site x y z U iso

_____________* Correspondence author (e-mail: qiaohj1999@126.com)

7/28/2019 1267-3643Crystal structure of catena-aqua(--chlorido)(2-carboxylato- 5-methylpyrazine-"2N,O)copper(II) monohydr

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208 CuCl(H2O)(C6H6N2O2) H2O

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Cu(1) 2i 0.6583(1) 0.52542(4) 0.78830(4) 0.0336(3) 0.0216(3) 0.0276(3) -0.0011(2) -0.0044(2) 0.0130(2)Cl(1) 2i 0.1484(2) 0.43690(8) 0.64377(8) 0.0297(5) 0.0273(5) 0.0301(5) -0.0001(3) -0.0026(4) 0.0107(4)O(3) 2i 0.6010(9) 0.3873(3) 0.8479(3) 0.052(2) 0.043(2) 0.056(2) -0.015(1) -0.018(2) 0.038(2)

N(1) 2i 0.7427(8) 0.6878(3) 0.7565(3) 0.029(2) 0.023(2) 0.024(2) 0.005(1) 0.003(1) 0.010(1)

C(3) 2i 1.074(1) 0.9018(4) 0.8443(4) 0.035(2) 0.022(2) 0.027(2) -0.002(2) 0.002(2) 0.008(2)N(2) 2i 0.9364(8) 0.9276(3) 0.7469(3) 0.037(2) 0.024(2) 0.033(2) 0.003(1) 0.002(1) 0.014(1)C(4) 2i 0.7038(9) 0.8324(4) 0.6528(4) 0.030(2) 0.031(2) 0.031(2) 0.008(2) 0.007(2) 0.017(2)C(5) 2i 0.605(1) 0.7124(4) 0.6577(3) 0.033(2) 0.027(2) 0.025(2) 0.002(2) 0.000(2) 0.011(2)C(2) 2i 0.9811(9) 0.7828(3) 0.8496(3) 0.024(2) 0.024(2) 0.025(2) 0.002(1) 0.002(1) 0.008(2)C(6) 2i 0.554(1) 0.8609(4) 0.5430(4) 0.042(2) 0.034(2) 0.037(2) 0.002(2) -0.001(2) 0.022(2)O(1) 2i 1.0314(7) 0.6292(2) 0.9388(2) 0.046(2) 0.023(1) 0.030(2) -0.004(1) -0.010(1) 0.014(1)O(4) 2i 0.074(1) 0.1824(3) 0.7331(3) 0.065(2) 0.032(2) 0.049(2) -0.002(2) -0.003(2) 0.022(2)C(1) 2i 1.1430(9) 0.7469(3) 0.9539(3) 0.032(2) 0.028(2) 0.027(2) 0.004(2) 0.002(2) 0.010(2)O(2) 2i 1.3661(8) 0.8261(3) 1.0410(3) 0.052(2) 0.034(2) 0.034(2) -0.010(1) -0.016(1) 0.016(1)

Table 3. Atomic coordinates and displacement parameters (in 2).

Atom Site x y z U 11 U22 U33 U12 U13 U23

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