Crystal structure of dichloro(4'-(4-t-butylphenyl)- 2,2':6

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Crystal structure of dichloro(4'-(4-t-butylphenyl)-. 2,2':6' .... tahedral complex [(4'-(4-tbutylphenyl)-2,2':6',2''-terpyridine) RhIII(Br). (acetonyl)2]. Inorg. Chim. Acta.
Z. Kristallogr. NCS 227 (2012) 133-134 / DOI 10.1524/ncrs.2012.0061

133

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Crystal structure of dichloro(4'-(4-t-butylphenyl)2,2':6',2''-terpyridyl)copper(II), CuCl2(C25H23N3) Daocheng Xia*,I,V, Lifeng LiuII, Xiuying MaIII, Jingxia MaIV and Jihuan YaoI I

College of Chemistry, Yuncheng University, Yuncheng 044000, Shanxi, P. R. China Yong Ji Fourth Middle School, Yong Ji 132200, Jilin, P. R. China III Baisheng Elementary School, Jiaohe City 132500, Jilin, P. R. China IV Science of Education Research Institute, Jiaohe City 132500, Jilin, P. R. China V College of Chemistry and Chemical Engineering, Shanxi University, Taiyuan 030006, Shanxi, P. R. China

II

Received September 28, 2011, accepted and available on-line February 7, 2012; CCDC no. 1267/3696

interactions between C atoms of the L ligand and the Cl atoms, which interlink the discrete units into a 3D supramolecular framework. Table 1. Data collection and handling. Crystal: Wavelength: -: Diffractometer, scan mode: 2+max: N(hkl)measured, N(hkl)unique: Criterion for Iobs, N(hkl)gt: N(param)refined: Program:

Abstract C25H23Cl2CuN3, monoclinic, P121/c1 (no. 14), a = 7.8744(3) Å, b = 10.9456(5) Å, c = 25.939(1) Å, ) = 94.129(3)°, V = 2229.9 Å3, Z = 4, Rgt(F) = 0.053, wRref(F2) = 0.120, T = 293 K. Source of material 4'-(4-t-butylphenyl)-2,2':6',2''-terpyridyl (L) was prepared by the procedures described in [1]. A mixture of L (0.037 g, 0.1 mmol), CuCl2 (0.017 g, 0.1 mmol) and 8 mL water was placed in a Teflon reactor (15 mL) and heated at 120 °C for 3 days. After cooling to room temperature at a rate of 10 °C/h, green crystals of the title compound were obtained in 56 % yield. Experimental details All H atoms on C atoms were generated at idealized positions and refined as riding with d(C—H) = 0.93-0.96 Å, and Uiso(H) = 1.2 Ueq(C). Discussion The title compound displays a crystal structure with discrete units. The asymmetric part contains one Cu(II) ion, one L ligand and two Cl anions. Cu1 is five-coordinated in a trigonal biyramidal manner, defined by three nitrogen atoms from one L ligand and two Cl anions. The Cu—N bond distances are in the range of 1.948(3)-2.048(3) Å. The Cu—Cl bond lengths are 2.228(1) Å and 2.520(1) Å. The N–Cu–N bond angles range from 78.8(1) to 156.0(1)°, and the Cl–Cu–Cl bond angle is 105.29(4)°. In addition, there are intermolecular C–H,,,Cl hydrogen bond

green block, size 0.21 " 0.24 " 0.26 mm Mo K* radiation (0.71073 Å) 12.37 cm&1 Oxford Diffraction Gemini R Ultra, & 58.42° 10302, 5170 Iobs > 2 ((Iobs), 3640 280 SHELXL-97 [2]

Table 2. Atomic coordinates and displacement parameters (in Å2). Atom

Site

H(4) H(2) H(12) H(17) H(20) H(25A) H(25B) H(25C) H(18) H(9) H(7) H(14) H(1) H(15) H(3) H(13) H(21) H(24A) H(24B) H(24C) H(23A) H(23B) H(23C)

4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e

_____________

* Correspondence author (e-mail: [email protected])

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x 0.9712 0.7059 0.3644 1.0922 0.9886 1.1259 1.2944 1.1569 1.2852 0.6196 0.9394 &0.0386 0.4789 0.0752 0.9575 0.1084 0.7974 1.3045 1.4440 1.4681 1.4840 1.3751 1.5120

y 0.3013 0.4394 &0.1421 0.1949 &0.0671 &0.0359 0.0110 0.1046 0.1767 &0.0343 0.1936 &0.1808 0.3198 &0.0334 0.4242 &0.2384 &0.0521 &0.1546 &0.0861 &0.1042 0.1365 0.2097 0.1158

z

Uiso

0.4604 0.5727 0.3076 0.3214 0.1851 0.1193 0.0973 0.1132 0.2603 0.3013 0.3816 0.3917 0.5439 0.4472 0.5328 0.3213 0.2465 0.1867 0.2219 0.1629 0.2127 0.1701 0.1541

0.047 0.065 0.047 0.047 0.063 0.095 0.095 0.095 0.048 0.042 0.039 0.057 0.060 0.049 0.061 0.054 0.060 0.093 0.093 0.093 0.112 0.112 0.112

134

CuCl2(C25H23N3)

Table 3. Atomic coordinates and displacement parameters (in Å2). Atom

Site

x

Cu(1) Cl(2) Cl(1) N(1) C(4) N(3) C(19) C(8) C(6) C(22) C(2) N(2) C(16) C(12) C(10) C(17) C(20) C(11) C(25) C(18) C(9) C(7) C(5) C(14) C(1) C(15) C(3) C(13) C(21) C(24) C(23)

4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e

0.39044(5) 0.2507(1) 0.2433(1) 0.5846(4) 0.8712(5) 0.2812(3) 1.1617(4) 0.7995(4) 0.7148(4) 1.2955(5) 0.7144(6) 0.5656(3) 0.9212(4) 0.3044(5) 0.5314(4) 1.0704(5) 1.0118(5) 0.3668(4) 1.2103(6) 1.1866(5) 0.6454(4) 0.8355(4) 0.7279(4) 0.0649(5) 0.5785(5) 0.1337(4) 0.8625(6) 0.1516(5) 0.8960(5) 1.3866(6) 1.4290(6)

y 0.14012(4) 0.31119(9) 0.1246(1) 0.2443(3) 0.3069(4) &0.0001(3) 0.0517(3) 0.0810(3) 0.1650(3) 0.0322(4) 0.3875(4) 0.1069(3) 0.0716(3) &0.1212(3) 0.0306(3) 0.1404(4) &0.0145(4) &0.0332(3) 0.0275(5) 0.1297(4) 0.0173(3) 0.1534(3) 0.2422(3) &0.1444(4) 0.3170(4) &0.0555(4) 0.3800(4) &0.1782(4) &0.0051(4) &0.0896(5) 0.1328(5)

z

U11

U22

U33

0.45412(2) 0.40167(4) 0.52406(4) 0.4854(1) 0.4773(2) 0.4113(1) 0.2157(1) 0.3332(1) 0.4130(1) 0.1760(2) 0.5446(2) 0.4066(1) 0.2921(1) 0.3359(2) 0.3669(1) 0.2943(2) 0.2129(2) 0.3702(1) 0.1214(2) 0.2572(2) 0.3293(2) 0.3768(1) 0.4600(1) 0.3857(2) 0.5267(2) 0.4187(2) 0.5203(2) 0.3439(2) 0.2499(2) 0.1880(2) 0.1785(2)

0.0304(2) 0.0395(5) 0.0493(6) 0.037(2) 0.038(2) 0.030(2) 0.037(2) 0.028(2) 0.027(2) 0.044(2) 0.069(3) 0.027(2) 0.029(2) 0.036(2) 0.028(2) 0.043(2) 0.051(2) 0.030(2) 0.074(3) 0.038(2) 0.035(2) 0.027(2) 0.030(2) 0.036(2) 0.054(3) 0.033(2) 0.060(3) 0.044(2) 0.036(2) 0.056(3) 0.077(3)

0.0432(3) 0.0391(5) 0.0716(8) 0.046(2) 0.046(2) 0.035(2) 0.033(2) 0.032(2) 0.035(2) 0.050(3) 0.057(3) 0.036(2) 0.033(2) 0.038(2) 0.032(2) 0.039(2) 0.063(3) 0.032(2) 0.079(4) 0.040(2) 0.037(2) 0.035(2) 0.039(2) 0.043(2) 0.057(3) 0.043(2) 0.058(3) 0.035(2) 0.064(3) 0.076(4) 0.086(4)

0.0347(3) 0.0447(6) 0.0423(6) 0.029(2) 0.033(2) 0.039(2) 0.032(2) 0.034(2) 0.032(2) 0.033(2) 0.037(2) 0.032(2) 0.033(2) 0.045(2) 0.036(2) 0.038(2) 0.045(3) 0.035(2) 0.038(3) 0.042(2) 0.034(2) 0.037(2) 0.024(2) 0.065(3) 0.041(2) 0.049(3) 0.034(2) 0.056(3) 0.052(3) 0.056(3) 0.067(3)

Acknowledgments. This work was financially supported by the National Natural Young Science Foundation of China (grant no. 61006034), the Natural Science Foundation for Young Scientists of Shanxi Province (grant no. 2010021010-3), College Science Fund of Shanxi Province (grant no. 2010021), Foundation of Yuncheng University (grant no. 975175) and Higher Education Foundation of Shanxi Outstanding Young Academic Leaders.

References 1. de Pater, B. C.; Frühauf, H. W.; Goubitz, K.; Fraanje, J.; Budzelaar, P. H. M.; Gal, A. W.; Vrieze, K.: Crystal structure of the novel neutral octahedral complex [(4'-(4-tbutylphenyl)-2,2':6',2''-terpyridine) RhIII(Br) (acetonyl)2]. Inorg. Chim. Acta. 358 (2005) 431-436. 2. Sheldrick, G. M.: A short history of SHELX. Acta Crystallogr. A64 (2008) 112-122.

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U12 &0.0007(2) &0.0019(4) &0.0022(5) 0.001(2) &0.006(2) 0.002(1) &0.002(2) 0.002(2) 0.003(2) &0.008(2) &0.008(2) 0.001(1) &0.001(2) 0.001(2) 0.003(2) &0.004(2) &0.016(2) 0.004(2) &0.006(3) &0.010(2) &0.001(2) &0.001(2) 0.003(2) &0.009(2) &0.001(2) &0.003(2) &0.021(2) &0.005(2) &0.021(2) 0.004(3) &0.038(3)

U13 0.0108(2) 0.0017(4) 0.0210(4) 0.007(1) 0.005(2) 0.007(1) 0.011(2) 0.004(1) 0.005(1) 0.013(2) 0.010(2) 0.006(1) 0.007(1) 0.008(2) 0.004(1) 0.010(2) 0.013(2) 0.005(2) 0.014(2) 0.011(2) 0.006(2) 0.007(1) 0.003(1) 0.013(2) 0.017(2) 0.013(2) &0.001(2) 0.004(2) 0.012(2) 0.022(2) 0.044(3)

U23 &0.0024(2) &0.0012(5) 0.0045(6) &0.003(2) &0.001(2) 0.002(2) &0.003(2) 0.001(2) 0.002(2) &0.009(2) &0.016(2) &0.004(1) &0.004(2) &0.001(2) &0.002(2) &0.014(2) &0.024(2) 0.003(2) &0.003(3) &0.008(2) &0.007(2) &0.004(2) 0.002(2) 0.001(2) &0.014(2) 0.007(2) 0.004(2) &0.006(2) &0.021(2) &0.013(3) &0.021(3)