H30K4M11M04O53SIW7, tetragonal, PAImnc (No. 128), a= 14.105(5)A,c = 12.476(7)Â, V = 2482.1 Â ,Z = 2, Rgt(F) = 0.064, WRKIIF) = 0.154, T= 293 K. Source of material K4H2[SiW7Mo4Mn(H20)039] · 1 3 H 2 0 was synthesized by the method in situ degradation. H4S1W8M04O40 · ( 2 0 2 5 ) H 2 0 ( 1 0 g), which was prepared according to the literature method [ 1 ], was dissolved in 100 ml of water at 353 Κ in the water-bath, Mn(N03)2 (0.62 g) was added to this solution on stirring. The pH of the mixture solution was adjusted to pH = 4.7 5.0 with aqueous solution of KAc-HAc ( K A C : H A C : H 2 0 = 15:3:30) . The crystals of title compound was formed in a refrigerator at 270 Κ 276 Κ. The components of the compound was determined by chemical analysis as follows. Manganese was estimated by DTPA methods (back-titration with standard zinc solution, in pH = 9.5 buffer in presence of Zn-agent). Molybdenum and tungsten in the compound was separated using literature methods [2], then Mo was weighed as M0O3 after precipitation with a-benzoinoxime and tungsten was weighed as WO3 after precipitation with cincholine. Potassium was weighed as KB(C 2 crf/obs). 1044 Nfparamhcnneu: 91 Program: SHELXTL [8] Unauthenticated Download Date | 2/16/16 5:16 AM 452 K4H2[SiW4Mo7Mn(H20)039] · 13H 20 Table 2. Atomic coordinates and displacement parameters (in A). Atom Site Occ. χ y ζ i/iso Si(l) 2a 0 0 0 0.012(2) 0(1) 16/ 1/2 0.012(2) 0.095(2) 0.075(2) 0.017(5) Table 3. Atomic coordinates and displacement parameters (in Â). Atom Site Occ. X y ζ l/ii U22 Ui3 Un Un Uzy W(l) 16/ 7/12 0.13823(7) 0.10921(8) 0.20000(8) 0.0275(6) 0.0348(6) 0.0262(6) -0.0143(4) -0.0045(4) -0.0029(4) Mo(l) 16i 4/12 0.13823 0.10921 0.20000 0.0275 0.0348 0.0262 -0.0143 -0.0045 -0.0029 Mn(l) 16/ 1/12 0.13823 0.10921 0.20000 0.0275 0.0348 0.0262 -0.0143 -0.0045 -0.0029 W(2) 8 A 7/12 0.24651(9) -0.0281(1) 0 0.0120(7) 0.0289(8) 0.0421(9) 0.0031(6) 0 0 Mo(2) 8 h 4/12 0.24651 -0.0281 0 0.0120 0.0289 0.0421 0.0031 0 0 Mn(2) 8 h 1/12 0.24651 -0.0281 0 0.0120 0.0289 0.0421 0.0031 0 0 K(l) 8 h 0.2967(5) 0.2447(5) 0 0.047(4) 0.053(4) 0.033(3) -0.028(4) 0 0 0(2) 16/ 0.235(2) 0.069(1) 0.105(2) 0.13(2) 0.028(8) 0.07(1) 0.001(9) 0.08(1) -0.006(8) CK3) 16/ 0.129(2) -0.016(1) 0.255(2) 0.14(2) 0.020(8) 0.11(2) -0.02(1) 0.10(2) -0.016(9) 0(4) 16/ 0.122(1) 0.212(2) 0.105(2) 0.020(7) 0.12(2) 0.08(1) 0.010(9) 0.009(8) 0.07(1) 0(5) 8Λ 0.365(2) -0.044(2) 0 0.03(1) 0.08(2) 0.09(2) 0.01(1) 0 0 0(6) 16/ 0.203(1) 0.158(1) 0.296(1) 0.06(1) 0.07(1) 0.031(8) -0.046(9) -0.005(7) -0.016(8) Ow(7) 8 h 0.319(3) 0.442(2) 0 0.14(3) 0.08(2) 0.11(3) 0.01(2) 0 0 Ow(8) 8 g 0.407(1) -JC+ 1/2 1/4 0.035(7) Ul i 0.16(3) 0.01(1) -0.03(1) U13 Ow(9) 4e 1/2 1/2 1/2 0.065(4) 0.07(3) Ul i 0.01(3) 0 0 0 Ow(lO) 8« 0.113(2) -χ + 1/2 1/4 0.14(2) Ul i 0.14(3) 0.06(3) -0.08(2) U13 Acknowledgment. We thank the state key basic program of China for the financial support (No. G2000048).