Z. Kristallogr. NCS 226 (2011) 161-162 / DOI 10.1524/ncrs.2011.0073
161
© by Oldenbourg Wissenschaftsverlag, München
Crystal structure of (1,3-bis(4-pyridyl)propane)-(1H-2-ethyl-4,5dicarboxylato-imidazole-N,O)cobalt(II), Co(C7H5O4N2)(C13H14N2) Hai-Xia Wu*,I, Hua WuII, Ying WangI and Jun-Long ZhanI I II
LuoYang Normal University, College of Chemistry and Chemical Engineering, Luoyang 471022, Henan, P. R. China LuoYang Normal University, Library, Luoyang 471022, Henan, P. R. China
Received March 11, 2011, accepted and available on-line April 19, 2011; CCDC no. 1267/3439
symmetry-related 1H-2-ethyl-4,5-imidazoledicarboxylate molecules forming a one-dimensional chain.
Table 1. Data collection and handling. Crystal: Wavelength: -: Diffractometer, scan mode: 2+max: N(hkl)measured, N(hkl)unique: N(param)refined: Programs:
Abstract C20H19CoN4O4, monoclinic, P21/m (no. 11), a = 8.171(1) Å, b = 12.812(2) Å, c = 9.698(1) Å, ) = 108.056(1)°, V = 965.2 Å3, Z = 2, Rgt(F) = 0.032, wRref(F2) = 0.092, T = 296 K. Source of material 1-hydrogen-2-ethyl-4,5-imidazole dicarboxylate acid (0.019 g, 0.1 mmol), Co(CH3CH2COO) ⋅ 4H2O (0.025 g, 0.1 mmol), and NaOH (0.004 g, 0.1 mmol) were added to water (10 ml) in a Teflon-lined stainless-steel reactor. The mixture was heated at 403 K for 4 d, and then slowly cooled down to room temperature. Pink block-shaped crystals of the title compound were obtained. Discussion The design and construction of metal-organic coodination polymers is of current interest in the field of supramocular chemistry and crystal engineering. The effective and facile approach for the synthesis of such complexes is still the appropriate choice. It is well known carboxylate ligands play an important role in coodination chemistry [1,2]. On the other hand, N-containing auxiliary ligands may tune the structures of the resultant metalorganic complexes [3-6]. The asymmetric unit of the title crystal structure consists of a 1Hhydrogen-2-ethyl-4,5-imidazoledicarboxylate, a Co(II) ion and a 1,3-di(4-pyridyl)-propane. Co ion is six-coordinated by two carboxlate oxygen atoms and two N atoms of two 1H-2-ethyl-4,5imidazoledicarboxylate and two N atoms of two 1,3-di(4pyridyl)propane, forming a distorted octahedron with (d(Co1—O1) = 2.167(2) Å, d(Co1—N1) = 2.166(2) Å, d(Co1—N2) = 2.128(2) Å. Furthermore, CoN4O2 octahedra are bridged by two symmetry-related bipyridyl molecules and two
pink block, size 0.07 × 0.19 × 0.41 mm Mo K* radiation (0.71073 Å) 9.24 cm−1 Bruker SMART CCD, "/% 51° 7074, 1881 140 SHELXS-97, SHELXL-97, SHELXTL [7]
Table 2. Atomic coordinates and displacement parameters (in Å2). Atom
Site Occ.
H(1) H(2) H(4) H(5) H(6A) H(6B) H(7A) H(7B) H(11A) H(11B) H(12A) H(12B) H(12C)
4f 4f 4f 4f 4f 4f 2e 2e 4f 4f 4f 4f 4f
0.50 0.50 0.50 0.50 0.50
_____________
* Correspondence author (e-mail:
[email protected])
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x 0.1000 −0.1363 0.1752 0.4044 −0.2495 −0.1299 −0.3698 −0.2522 0.7047 0.7047 0.9305 0.9866 0.9363
y 0.0072 0.0613 0.1509 0.0967 0.0947 0.1603 ¼ ¼ 0.3112 0.1888 0.3076 0.2567 0.1858
z 0.4106 0.2283 0.0053 0.1943 −0.0479 −0.1131 −0.0621 0.0997 0.3471 0.3471 0.5721 0.4467 0.5591
Uiso 0.050 0.056 0.058 0.050 0.081 0.081 0.077 0.077 0.046 0.046 0.090 0.090 0.090
162
Co(C7H5O4N2)(C13H14N2)
Table 3. Atomic coordinates and displacement parameters (in Å2). Atom
Site
Co(1) N(1) N(2) O(1) O(2) C(1) C(2) C(3) C(4) C(5) C(6) C(7) C(8) C(9) C(10) C(11) C(12)
2d 4f 4f 4f 4f 4f 4f 4f 4f 4f 4f 2e 4f 2e 4f 2e 2e
x ½ 0.2773(3) 0.5452(2) 0.3611(2) 0.2748(2) 0.1160(3) −0.0273(3) −0.0093(4) 0.1565(4) 0.2942(3) −0.1649(4) −0.2512(6) 0.4460(3) 0.6028(4) 0.3562(3) 0.7254(5) 0.9119(5)
y 0 0.0470(2) 0.1623(1) 0.0259(1) 0.1538(1) 0.0373(2) 0.0699(2) 0.1150(2) 0.1229(2) 0.0894(2) 0.1504(2) ¼ 0.1964(2) ¼ 0.1199(2) ¼ ¼
z ½ 0.3227(2) 0.5417(2) 0.6545(2) 0.7723(2) 0.3285(3) 0.2188(3) 0.0954(3) 0.0876(3) 0.2018(3) −0.0271(4) 0.0000(5) 0.6234(2) 0.4958(3) 0.6872(2) 0.4090(4) 0.5056(6)
U11
U22
U33
0.0361(3) 0.041(1) 0.033(1) 0.048(1) 0.062(1) 0.048(2) 0.041(1) 0.058(2) 0.072(2) 0.050(2) 0.077(2) 0.061(3) 0.032(1) 0.029(2) 0.037(1) 0.047(2) 0.043(2)
0.0165(2) 0.025(1) 0.0193(9) 0.0214(8) 0.0317(9) 0.035(1) 0.040(1) 0.028(1) 0.034(1) 0.031(1) 0.043(2) 0.055(3) 0.021(1) 0.022(2) 0.024(1) 0.028(2) 0.057(3)
0.0345(3) 0.038(1) 0.0332(9) 0.0448(9) 0.053(1) 0.045(1) 0.058(2) 0.046(2) 0.039(1) 0.045(1) 0.059(2) 0.061(3) 0.029(1) 0.032(2) 0.033(1) 0.051(2) 0.089(3)
U12 0.0007(2) −0.0001(8) 0.0001(7) −0.0021(7) −0.0015(8) 0.001(1) 0.003(1) 0.007(1) 0.003(1) −0.002(1) 0.013(2) 0 −0.0004(9) 0 0.0000(9) 0 0
U13 0.0154(2) 0.0124(9) 0.0147(8) 0.0238(8) 0.0407(9) 0.018(1) 0.012(1) 0.004(1) 0.016(1) 0.017(1) −0.013(2) −0.005(2) 0.0124(9) 0.013(1) 0.014(1) 0.031(2) 0.034(2)
U23 0.0005(2) 0.0006(8) −0.0008(7) 0.0025(7) 0.0017(8) 0.004(1) −0.004(1) −0.006(1) 0.006(1) 0.004(1) −0.010(1) 0 0.0001(9) 0 0.0031(9) 0 0
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