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77953958472
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Preparation of, Er(Hbmdc)(bmdc)(H2O)3]·3H2O}n (1, a mixture of ErCl3·6H2O (8.0 mg, 0.02 mmol, H2bmdc (6.8 mg, 0.03 mmol, methanol (2 mL, and H2O (15 mL) was adjusted to pH, 5 with acetic acid and then placed in a sealed Teflon-lined stainless steel vessel, heated at 160 °C for 3 d. Then the reaction system was cooled at room temperature over 2 d in 40.3% yield. Anal. Calcd. for C18H21N4O14Er: C 31.49, H 3.12, N 8.21. IR data (KBr, cm-1, 3447 vs, 2929 w, 1631 s-1565 m, 1530 m-1475 m, 1430 s, 1366 s-1272 m, 1239 m, 1152 w-1036 w-887 m-807 m-690 m-647 m-618 m. Crystal data for compound 1: fw, 684.65, Monoclinic, P21/c, a, 11.1514(9) Å, b, 8.9392(7) Å, c, 23.0780 (2) Å, α, 90 °, β, 94.8790(1) °, γ, 90 °, V, 2292.2(3) Å3, Z, 4, D
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2 = 0.0229/ 0.0569 (I > 2σ) and 0.0270/ 0.0609 (all data); GOF = 1.073.
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77953958352
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Preparation of [Er2(Hbmdc)2(bmdc)2(H2O)8]·8H2O (2, The first procedure was the same with 1 as followed to prepare 2. The resulting solution was filtered to remove any insoluble matter and then set aside to evaporate at the room temperature. Pink X-ray quality crystals were obtained from the solution over 3 weeks in 37.5% yield. Anal. Calcd. for C36H50N8O32Er2 (1441.36, C 29.89, H 3.55, N 7.81. IR data (KBr, cm-1, 3424 vs, 2927 w, 2855 w, 1626 m, 1418 s, 1122 s, 1030 w, 658 m, 615 m. Crystal data for compound 2: fw, 1441.36, Triclinic, P-1, a, 7.4471(2) Å, b, 12.358(3) Å, c, 13.845(3) Å, α, 71.91(3) °, β, 82.65(3) °, γ, 79.04(3) °, V, 1185.9(5) Å3, Z, 1, DCalcd, 2.018 g cm-3; R1/wR2, 1.021/0.0634 I > 2
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2bmdc at room temperature and setting aside for weeks, we were failed to obtain well shaped single crystals but some tiny needles.
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Wang H., Wang Y.Y., Yang G.P., Wang C.J., Wen G.L., Shi Q.Z., and Batten S.R. Cryst. Eng. Commun. 10 (2008) 1583
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Huang Y.Q., Zhao X.Q., Shi W., Liu W.Y., Chen Z.L., Cheng P., Liao D.Z., and Yan S.P. Cryst. Growth Des. 8 (2008) 3652
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Yan, S.P.8
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