Z. Kristallogr. NCS 2016; 231(2): 457–460 Open Access Qifan Chen, Fang Huang, Wenjing Quan, Yanhua Lu, Fang Zhang* and Fei Liu* The crystal structure of hexaqua(µ2-3-(3-(pyridin- 4-yl)-1,2,4-oxadiazol-5-yl)propanoato-1κ2O,O′; 2κO′)(3-(3-(pyridin-4-yl)-1,2,4-oxadiazol-5-yl) propanoato-κO)(3-(3-(pyridin-4-yl)-1,2,4-oxadia- zol-5-yl)propanoato-κ2O,O′)digadolinium(III) octahydrate, C60H76Gd2N18O32 DOI 10.1515/ncrs-2015-0136 Received December 30, 2015; accepted March 1, 2016; available online March 19, 2016 Abstract C60H76N18O32Gd2, monoclinic, P21/c (no. 14), a = 10.560(5) Å, b = 31.243(5) Å, c = 12.383(4) Å, β = 116.51(3)°, V = 3 2 3656(2) Å , Z = 2, Rgt(F) = 0.0470, wRref(F ) = 0.1013, T = 293(2) K. CCDC no.: 1456749 Table 1: Data collection and handling. Crystal: Black, strip, size 0.13×0.21×0.30 mm Wavelength: Mo Kα radiation (0.71069 Å) µ: 19.00 cm−1 Diractometer, scan mode: multiwire, φ and ω scans 2θmax: 50° N(hkl)measured, N(hkl)unique: 12131, 6453 Criterion for Iobs, N(hkl)gt: Iobs > 2 σ(Iobs), 5554 N(param) : 484 *Corresponding authors: Fang Zhang, The College of Chemical rened Programs: SHELX [8] Engineering, Eastern Liaoning University; No. 325, Wenhua Road, Yuanbao District, Dandong City, Liaoning Province, P. R. 118003, People’s Republic of China, e-mail: [email protected]; Fei Liu, and College of Chemical Engineering & Materials, Eastern Table 2: Fractional atomic coordinates and isotropic or equivalent Liaoning University, No. 325, Wenhua Road, Yuanbao District, isotropic displacement parameters (Å2). Dandong City, Liaoning Province, P. R. 118003, People’s Republic of China, e-mail: [email protected] Atom Site x y z Uiso Qifan Chen and Fang Huang: College of Chemical Engineering, Eastern Liaoning University, No. 325, Wenhua Road, Yuanbao H(2A) 4e −0.0726 −0.1288 −0.0580 0.043 District, Dandong City, Liaoning Province, P. R. 118003, People’s H(2B) 4e 0.0460 −0.0944 −0.0286 0.043 Republic of China H(3A) 4e −0.1596 −0.0839 −0.2588 0.052 Wenjing Quan: FengCheng Environmental Monitoring Station, H(3B) 4e 0.0034 −0.0890 −0.2158 0.052 Dandong City, Liaoning Province, P. R. 118100, People’s Republic H(7) 4e −0.1144 −0.2586 −0.1270 0.040 of China H(8) 4e −0.1369 −0.3315 −0.1183 0.045 Yanhua Lu: Liaoning Provincial Key Laboratory of Functional Textile H(9) 4e −0.1987 −0.2716 −0.4737 0.041 Materials, EasternLiaoning University, Dandong, Liaoning, China H(10) 4e −0.2140 −0.3436 −0.4541 0.044 © 2016 Qifan Chen et al., published by De Gruyter. This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License. 458 Ë Chen et al.: C60H76Gd2N18O32 Table 2 (continued) The crystal structure is shown in the gure. Tables 1–3 contain details of the measurement method and a list of the atoms Atom Site x y z U iso including atomic coordinates and displacement parameters. H(12A) 4e −0.6261 −0.1356 −0.0068 0.050 H(12B) 4e −0.4662 −0.1223 0.0434 0.050 Source of material H(13A) 4e −0.4526 −0.1097 0.2332 0.055 3-(3-Pyridin-4-yl-[1, 2, 4]oxadiazol-5-yl)-propionic acid (HL) is H(13B) 4e −0.6147 −0.1187 0.1846 0.055 H(17) 4e −0.4899 −0.2781 0.0336 0.052 easily available by a literature known synthesis [1]. A solution H(18) 4e −0.4786 −0.3493 −0.0024 0.057 of ammonia (0.5 M ) was added dropwise to a methanol H(19) 4e −0.4531 −0.3088 0.3593 0.047 (15 mL) solution of HL (3 mmol), resulting in a clear solution. H(20) 4e −0.4447 −0.3795 0.3142 0.053 A methanol (15 mL) solution of zinc acetate (1.5 mmol) was e − H(22A) 4 0.3375 0.0607 0.3615 0.048 added and allowed to stir for 3 h, resulting in a suspension. H(22B) 4e −0.2300 0.0324 0.4668 0.048 A methanol (15 mL) solution of gadolinium chloride (1 mmol) H(23A) 4e −0.1874 0.1011 0.5337 0.052 H(23B) 4e −0.0582 0.0872 0.5121 0.052 was added into the resulting suspension and allowed to stir H(27) 4e −0.2322 0.2422 0.1277 0.057 for 8 h. The suspension was ltered and diethyl ether was H(28) 4e −0.2117 0.3149 0.1238 0.064 allowed to diuse slowly into the solution of the ltrate. Black H(29) 4e −0.1320 0.3246 0.4586 0.065 crystals were obtained in about 3 weeks. H(30) 4e −0.1409 0.2518 0.4769 0.054 e − H(302) 4 0.0246 0.0109 0.2255 0.040 Experimental details H(301) 4e 0.0233 0.0021 0.1412 0.040 H(101) 4e −0.1481 −0.0823 0.2479 0.045 H atoms bound to C atoms were placed in calculated positions H(102) 4e −0.2337 −0.0542 0.2702 0.045 with C—H = 0.93 or 0.96 Å and Uiso(H) = 1.2 or 1.5 Ueq(C). H H(501) 4e −0.5208 −0.0172 −0.2244 0.047 atom of the hydroxy group were located in the dierence − − − H(502) 4e 0.3846 0.0287 0.1979 0.047 Fourier map and were rened with restraint as O—H = 0.82 Å, H(789) 4e −0.1991 −0.0839 0.4438 0.069 and H atoms of water molecule were initially found in the H(876) 4e −0.1226 −0.0491 0.5075 0.069 H(567) 4e −0.3817 −0.0319 −0.4036 0.070 dierence Fourier map and were rened with restraint as H(456) 4e −0.3510 −0.0520 −0.4878 0.070 O—H = 0.83 Å. H(992) 4e −0.3998 0.0426 −0.2905 0.075 H(991) 4e −0.3757 0.0391 −0.3903 0.075 Discussion e − H(999) 4 0.1118 0.1046 0.7813 0.078 Lanthanide-based carboxylate complexes have been found to H(998) 4e −0.094 0.0624 0.7600 0.078 exhibit anticancer and, unusual coordination characteristics, Table 3: Fractional coordinates and atomic displacement parameters (Å2). Atom Site x y z U11 U22 U33 U12 U13 U23 C(1) 4e −0.1408(5) −0.0686(2) −0.0531(4) 0.032(3) 0.026(3) 0.020(2) −0.001(2) 0.007(2) −0.003(2) C(2) 4e −0.0531(6) −0.1006(2) −0.0795(5) 0.045(3) 0.029(3) 0.038(3) 0.004(3) 0.023(3) 0.000(3) C(3) 4e −0.0779(7) −0.1015(2) −0.2108(5) 0.068(4) 0.030(3) 0.047(3) 0.000(3) 0.038(3) −0.006(3) C(4) 4e −0.1016(5) −0.1453(2) −0.2629(4) 0.032(3) 0.031(3) 0.031(3) 0.002(2) 0.016(2) 0.000(3) C(5) 4e −0.1338(5) −0.2099(2) −0.3102(4) 0.022(2) 0.029(3) 0.030(3) −0.002(2) 0.011(2) −0.004(2) C(6) 4e −0.1509(5) −0.2567(2) −0.3011(4) 0.025(2) 0.028(3) 0.031(3) 0.000(2) 0.012(2) −0.004(2) C(7) 4e −0.1345(5) −0.2753(2) −0.1949(5) 0.033(3) 0.038(3) 0.028(3) −0.002(3) 0.012(2) −0.010(3) C(8) 4e −0.1485(6) −0.3193(2) −0.1906(5) 0.041(3) 0.034(3) 0.033(3) −0.005(3) 0.013(2) 0.003(3) C(9) 4e −0.1838(5) −0.2831(2) −0.3997(5) 0.044(3) 0.032(3) 0.026(3) −0.002(3) 0.016(2) −0.002(3) C(10) 4e −0.1942(6) −0.3262(2) −0.3875(5) 0.046(3) 0.031(3) 0.034(3) −0.006(3) 0.019(3) −0.011(3) C(11) 4e −0.5969(5) −0.0703(2) 0.0213(4) 0.028(3) 0.022(3) 0.034(3) −0.002(2) 0.012(2) 0.003(2) C(12) 4e −0.5530(6) −0.1171(2) 0.0502(5) 0.051(3) 0.033(3) 0.039(3) 0.003(3) 0.018(3) 0.001(3) C(13) 4e −0.5305(7) −0.1269(2) 0.1769(5) 0.061(4) 0.032(3) 0.046(3) 0.001(3) 0.026(3) 0.001(3) C(14) 4e −0.4995(6) −0.1731(2) 0.2110(5) 0.040(3) 0.033(3) 0.042(3) 0.004(3) 0.020(3) 0.002(3) C(15) 4e −0.4762(5) −0.2392(2) 0.2287(5) 0.029(3) 0.033(3) 0.037(3) 0.006(3) 0.015(2) 0.012(3) C(16) 4e −0.4725(5) −0.2852(2) 0.2008(5) 0.025(3) 0.038(3) 0.035(3) −0.001(3) 0.010(2) 0.008(3) C(17) 4e −0.4801(6) −0.2981(2) 0.0924(5) 0.050(4) 0.044(4) 0.036(3) 0.001(3) 0.018(3) 0.010(3) C(18) 4e −0.4731(7) −0.3411(2) 0.0717(5) 0.059(4) 0.047(4) 0.039(3) −0.001(3) 0.025(3) −0.003(3) C(19) 4e −0.4586(6) −0.3165(2) 0.2847(5) 0.046(3) 0.036(3) 0.034(3) 0.004(3) 0.017(3) 0.004(3) C(20) 4e −0.4530(6) −0.3590(2) 0.2571(5) 0.047(3) 0.041(4) 0.044(3) 0.003(3) 0.019(3) 0.013(3) Chen et al.: C60H76Gd2N18O32 Ë 459 Table 3 (continued) Atom Site x y z U11 U22 U33 U12 U13 U23 C(21) 4e −0.1855(5) 0.0342(2) 0.3213(4) 0.032(3) 0.027(3) 0.028(3) 0.001(2) 0.012(2) 0.000(2) C(22) 4e −0.2381(6) 0.0537(2) 0.4071(5) 0.059(4) 0.036(3) 0.034(3) −0.006(3) 0.030(3) −0.006(3) C(23) 4e −0.1585(7) 0.0937(2) 0.4719(5) 0.060(4) 0.040(4) 0.028(3) 0.003(3) 0.018(3) −0.009(3) C(24) 4e −0.1798(5) 0.1314(2) 0.3940(4) 0.035(3) 0.042(4) 0.026(3) −0.006(3) 0.013(2) −0.006(3) C(25) 4e −0.1917(5) 0.1913(2) 0.3156(5) 0.023(3) 0.042(3) 0.032(3) −0.002(3) 0.011(2) 0.000(3) C(26) 4e −0.1873(5) 0.2381(2) 0.3042(5) 0.026(3) 0.042(4) 0.037(3) 0.000(3) 0.012(2) 0.001(3) C(27) 4e −0.2098(6) 0.2581(2) 0.1973(5) 0.044(3) 0.055(4) 0.043(3) 0.009(3) 0.020(3) 0.011(3) C(28) 4e −0.1983(7) 0.3020(2) 0.1958(6) 0.049(4) 0.055(5) 0.054(4) 0.009(4) 0.021(3) 0.024(4) C(29) 4e −0.1506(7) 0.3077(2) 0.3913(6) 0.051(4) 0.038(4) 0.064(4) −0.009(3) 0.017(3) −0.012(4) C(30) 4e −0.1570(6) 0.2638(2) 0.4032(5) 0.042(3) 0.044(4) 0.044(3) −0.001(3) 0.016(3) 0.000(3) Gd(1) 4e −0.28684(2) −0.016319(8) 0.04809(2) 0.0268(2) 0.0236(2) 0.0223(1) −0.0006(1) 0.0096(1) −0.0012(1) N(1) 4e −0.1774(5) −0.3449(2) −0.2840(4) 0.047(3) 0.031(3) 0.037(3) −0.003(2) 0.019(2) −0.002(2) N(2) 4e −0.1411(5) −0.1924(2) −0.4073(4) 0.052(3) 0.025(3) 0.035(2) −0.007(2) 0.020(2) −0.008(2) N(3) 4e −0.1085(5) −0.1818(1) −0.2162(4) 0.045(3) 0.025(3) 0.034(2) 0.001(2) 0.021(2) −0.003(2) N(4) 4e −0.4589(5) −0.3721(2) 0.1517(5) 0.054(3) 0.039(3) 0.053(3) 0.003(3) 0.023(3) −0.001(3) N(5) 4e −0.4449(6) −0.2269(2) 0.3375(4) 0.067(3) 0.034(3) 0.044(3) 0.005(3) 0.027(3) 0.006(3) N(6) 4e −0.5111(5) −0.2066(2) 0.1449(4) 0.042(3) 0.040(3) 0.038(3) 0.000(2) 0.015(2) 0.011(2) N(7) 4e −0.1691(5) 0.3272(2) 0.2909(6) 0.046(3) 0.042(3) 0.079(4) 0.003(3) 0.022(3) 0.013(3) N(8) 4e −0.1705(5) 0.1716(2) 0.4220(4) 0.039(3) 0.035(3) 0.027(2) −0.003(2) 0.012(2) −0.008(2) N(9) 4e −0.2149(5) 0.1657(2) 0.2264(4) 0.055(3) 0.039(3) 0.032(2) −0.007(3) 0.017(2) −0.004(2) O(1) 4e −0.1420(4) −0.0299(1) −0.0809(3) 0.037(2) 0.017(2) 0.036(2) −0.001(2) 0.019(2) 0.000(2) O(2) 4e −0.2097(4) −0.0819(1) 0.0018(3) 0.053(2) 0.026(2) 0.038(2) 0.003(2) 0.029(2) 0.003(2) O(3) 4e −0.0379(4) −0.0040(1) 0.1646(3) 0.034(2) 0.040(2) 0.029(2) −0.007(2) 0.017(2) −0.009(2) O(4) 4e −0.2207(4) −0.0667(1) 0.2151(3) 0.055(2) 0.030(2) 0.029(2) 0.011(2)