H 3 {[ Cu( en) 2 ] 5 [ ( VO) 12 O 6 B 18 O 42 ] }[ B( OH) 3 ] 2 16 H 2 O

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2004 62 4, 391 398 ACTA CHIMICA SINICA Vol 62, 2004 No 4, 391 398 H 3 {[ Cu( en) 2 ] 5 [ ( VO) 12 O 6 B 18 O 42 ] }[ B( OH) 3 ] 2 16 H 2 O a Ξ, a, b a, b a a a Ξ ( a 350002) ( b 350002) H 3 BO 3, NH 4 VO 3, Cu (CH 3 COO) 2 H 2 O H 3 {[ Cu (en) 2 ] 5 2 [ (VO) 12 O 6 B 18 O 42 ]}[B(OH) 3 ] 2 16H 2 O, X -, B 18 O 42 18 B ( 3 2O) V V 6 O 18, [ (VO) 12 O 6 B 18 O 42 ] 13-4 [ Cu(en) 2 ] 2 +, 01619 11817 nm,,, Hydrothermal Synthesis, Crystal Structure and Properties of Polyoxovanadium Borate H 3 { [ Cu( en) 2 ] 5 [ ( VO) 12 O 6 B 18 O 42 ] } [ B( OH) 3 ] 2 16 H 2 O LIN, Zhi2Hua a ZHANG, Han2Hui Ξ, a, b HUANG, Chang2Cang a, b SUN, Rui2Qing a CHEN, Yi2Ping a WU, Xiao2Yuan a ( a Department of Chemistry, Fuzhou University, Fuzhou 350002) ( b State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002) Abstract A novel polyoxovanadium borate H 3 {[ Cu (en) 2 ] 5 [ (VO) 12 O 6 B 18 O 42 ]} [ B (OH) 3 ] 2 16H 2 O has been synthesized from a mixture of H 3 BO 3, NH 4 VO 3, Cu ( CH 3 COO) 2 H 2 O and ethylenediamine under hydrothermal condition and characterized by crystal X2ray structure analysis, IR spectrum, Raman spectrum, UV2Vis DRIS spectrum, fluorescence spectrum, ESR and TGA In the structure of the compound, there is a ring of B 18 O 42 sandwiched between two vanadium2oxygen clusters V 6 O 18 by eighteen B ( 3 2O) V bonds, and the anion clusters [ (VO) 12 O 6 B 18 O 42 ] 13 - are connected through four [ Cu ( en) 2 ] 2 + by the static electronic interaction Thus, the complex was extended to an infinite two2dimensional network structure, with size of the hole amounting to 0 619 11817 nm Keywords hydrothermal synthesis, polyoxovanadium borate, crystal structure, cluster compound,,, [1], [2], Ξ E2mail : hhzhang @fzu edu cn Received April 8, 2003 ; revised and accepted October 13, 2003 (No E0110013) (No K02028)

392 Vol 62, 2004 B V O [3] 1997 (enh) 2 4 ml 016 ml, ph 812 (enh 2 ) 4 [ (VO) 12 B 17 O 38 (OH) 8 ] H 2 O, (enh 2 ) 5 [ (VO) 12 O 6 {B 3 O 6 2 (OH) } 6 ] H 2 O [4] 1999 [ Zn (en) 2 ] 6 [ (VO) 12 O 6 B 18 2 O 39 (OH) 3 ] 13H 2 O [2] [Ni2, B 80 % ( (en) 2 ] 6 [ (VO) 12 O 6 B 18 O 39 (OH) 3 ] 8H 2 O [5], %),C 7184 (7174), N 8198 (9103), H 3176 (3190) B 18 O 39 (OH) 3 9 B ( 3 2O) V 1 3 X V 6 O 18,6 [Ni (en) 2 ] Ni ( 3 2 0130 mm 0130 mm 0148 mm, Rigaku R2 O) B B 18 O 39 (OH) AXIS Parid Weissenberg IP (293 2) K, 3 [ Cu(en) 2 ] 2 + Mo K ( = 01071073 nm),, 3108 2 54196 11134 H 3 {[ Cu ( en) 2 ] 5 2, Lp, I > 2 ( I) 9422 [ (VO) 12 O 6 B 18 O 42 ]}[B (OH) 3 ] 2 16H 2 O, X Cu - V,, 1 a = 114634 (1) nm, b = 115121 (2) nm, c = 114677 (2) 1 1 nm, = 951379 (4), = 1151103 (5), = 1121988 (4), V = H 3 BO 3, NH 4 VO 3, Cu(CH 3 COO) 2 H 2 O 215728 ( 5) nm 3, Z = 1, M r = 3099155, D c = 21000 g/ cm 3, Vario EL III,Perkin2Elmer Spectrum 2000 FTIR F(000) = 1558, = 21169 mm - 1, R 1 = 010657, wr 2 =,Nicolet 910 FT2Raman,Perkin2Elmer Lambda 900, Edinburgh2Instrument F920, Perkin2Elmer TGA 7,Rigaku R2AXIS Parid Weissenberg IP J EOL J ES FEXG ESR 815, 20 ml, 140 4 d, 2554 e nm - 3-1424 e nm - 3 :, P21, 011964, S = 11005, ( / ) max = 01000, P [6 SHELXTL297,7] 2 1 2 2 1 NH 4 VO 3 (01234 g, 2 mmol), H 3 BO 3 (11236 g, 20 mmol) 1, Cu(CH 3 COO) 2 H 2 O (01600 g, 3 mmol), 2 1 ( 10 4 ) ( 10 5 nm 2 ) Table 1 Atomic coordination ( 10 4 ) and thermal parameters ( 10 5 nm 2 ) for the title compound Atom x y z U eq Atom x y z U eq Cu(1) - 2961(1) 3753(1) - 888(1) 32 (1) O(2) - 377(3) 3789 (2) 2239(3) 19 (1) Cu(2) 5000 0 5000 30 (1) O(3) - 867(3) 5372 (2) 2506(3) 25 (1) Cu(3) - 5000 5000 5000 34 (1) O(4) - 2458(3) 4359 (2) 2794(3) 23 (1) Cu(4) 0 10000 5000 39 (1) O(5) - 2049(3) 2925 (3) 2784(3) 24 (1) V(1) - 1730(1) 3921(1) 2081 (1) 20 (1) O(6) - 2489(4) 6078 (3) 2210(3) 34 (1) V(2) - 1654(1) 5775(1) 3082 (1) 21 (1) O(7) - 205(3) 6991 (3) 3989(3) 24 (1) V(3) - 341(1) 7346(1) 5214 (1) 19 (1) O(8) - 1759(3) 6044 (2) 4307(3) 23 (1) V(4) - 1994(1) 5497(1) 5386 (1) 19 (1) O(9) - 683(3) 8234 (3) 5167(3) 32 (1) V(5) - 2262(1) 3448(1) 5592 (1) 19 (1) O(10) 1366 (3) 8026 (2) 6163(3) 21 (1) V(6) - 2893(1) 3276(1) 3326 (1) 21 (1) O(11) - 540(3) 6725 (2) 6259(3) 24 (1) B (1) - 181(5) 7448(4) 1889 (5) 26 (1) O(12) - 2991(3) 5690 (3) 5412(3) 31 (1) B (2) 727 (5) 7556(4) 3770 (4) 21 (1) O(13) - 1469(3) 4846 (2) 6440(3) 23 (1) B (3) 2143 (4) 8219(4) 5698 (5) 21 (1) O(14) - 2721(3) 4096 (2) 4501(3) 22 (1) B (4) 3666 (5) 9375(4) 7491 (5) 30 (1) O(15) - 3356(3) 2836 (3) 5734(3) 26 (1) B (5) 1905 (4) 7992(4) 7285 (4) 21 (1) O(16) - 1032(3) 3204 (2) 6599(3) 20 (1) B (6) 183 (5) 7075(4) 7427 (5) 22 (1) O(17) - 2357(3) 2663 (3) 4401(3) 24 (1)

No 4 : H 3 {[ Cu(en) 2 ] 5 [ (VO) 12 O 6 B 18 O 42 ]} 393 Atom x y z U eq Atom x y z U eq B (7) - 1071(5) 6637(4) 8216 (5) 25 (1) O(18) - 4230(3) 2501 (3) 2534(3) 33 (1) B (8) - 681(5) 5315(4) 7593 (5) 21 (1) O(19) - 549(5) 7900 (3) 1126(4) 45 (1) B (9) - 88(5) 3985(4) 7665 (5) 22 (1) O(20) - 324(3) 6514 (3) 1568(3) 26 (1) B (10) 2903 (11) 115(10) - 95(9) 75 (3) O(21) 321 (3) 7984 (3) 2918(3) 26 (1) C(1) - 1233(6) 3188(6) - 401(6) 47 (2) O(22) 1671 (3) 8378 (2) 4698(3) 22 (1) C(2) - 2250(7) 2380(6) - 1385(6) 56 (2) O(23) 3246 (3) 9134 (3) 6436(3) 26 (1) C(3) - 4503(8) 4246(8) - 572(8) 69 (2) O(24) 4762 (4) 10155(4) 8116(4) 62 (2) C(4) - 3700(9) 5190(7) - 554(8) 69 (2) O(25) 3047 (3) 8884 (3) 7935(3) 25 (1) C(5) 3826 (5) 378 (5) 3084 (6) 41 (1) O(26) 1242 (3) 7965 (2) 7775(3) 21 (1) C(6) 7068 (5) 172 (5) 6627 (5) 38 (1) O(27) - 422(3) 7323 (3) 7919(3) 25 (1) C(7) - 4294(7) 6874(6) 6409 (6) 49 (2) O(28) - 1629(4) 6871 (3) 8680(4) 39 (1) C(8) - 4584(6) 6103(5) 6950 (6) 47 (2) O(29) - 1231(3) 5679 (3) 8073(3) 25 (1) C(9) 2122 (9) 10593(9) 6899 (9) 83 (3) O(30) - 431(3) 4604 (2) 8082(3) 21 (1) C(10) 1561 (11) 11131(9) 7148 (9) 92 (4) O(31) 3723 (7) - 82(7) - 150(5) 97 (3) N(1) - 1327(4) 4112(4) - 400(4) 37 (1) O(32) 1756 (7) - 432(7) - 791(7) 110 (3) N(2) - 3298(5) 2324(4) - 1428(5) 44 (1) O(33) 3301 (7) 959 (7) 743(6) 98 (3) N(3) - 4571(5) 3410(5) - 1219(5) 48 (1) OW1-3324(4) 3998 (3) - 2609(3) 37 (1) N(4) - 2612(5) 5194(4) - 339(5) 46 (1) OW2 5337 (4) - 1060(4) 3755(4) 47 (1) N(5) 4949 (4) 883 (4) 4058 (4) 33 (1) OW3-3639(5) 6412 (4) 3300(5) 57 (1) N(6) 6695 (4) 789 (3) 5990 (4) 32 (1) OW4-3314(6) 8019 (4) 4738(5) 67 (2) N(7) - 4916(4) 6369(4) 5259 (5) 37 (1) OW5-1513(7) 8479 (6) 6717(6) 80 (2) N(8) - 4408(5) 5286(4) 6581 (5) 43 (1) OW6 1792 (8) 1395 (5) 1215(7) 91 (2) N(9) 1644 (5) 10290(4) 5743 (6) 49 (2) OW7 58 (9) - 48(6) 1365(8) 112 (3) N(10) 324 (6) 10537(5) 6478 (5) 56 (2) OW8 0 5000 5000 119 (4) O(1) - 2650(3) 3461(3) 835 (3) 32 (1) OW9 3 5150 (14) 1799(12) - 154(11) 125 (8) U eq = (1/ 3) i j U ij a i 3 a j 3 a i a j ; 3 : The occupancy is 015 2 (nm) ( ) Table 2 Selected bond lengths (nm) and bond angles ( ) Cu(1) N(1) 0 1996(5) V(2) O(7) 0 1936(3) B (1) O(21) 0 1357(7) B (8) O(29) 0 1484(6) Cu(1) N(2) 0 2015(5) V(2) V(3) 0 30109(12) B (1) O(19) 0 1389(7) B (8) O(2) # 4 0 1506(6) Cu(1) N(3) 0 2020(5) V(3) O(9) 0 1604(4) B (2) O(22) 0 1433(6) B (9) O(30) 0 1422(6) Cu(1) N(4) 0 2027(6) V(3) O(11) 0 1937(4) B (2) O(21) 0 1468(6) B (9) O(20) # 4 0 1463(7) Cu(1) OW1 0 2449(4) V(3) O(7) 0 1940(3) B (2) O(7) 0 1485(6) B (9) O(3) # 4 0 1497(6) Cu(1) O(1) 0 2486(4) V(3) O(8) 0 1982(3) B (2) O(16) # 4 0 1517(6) B (9) O(16) 0 1515(7) Cu(2) N(6) 0 1998(5) V(3) O(10) 0 2002(3) B (3) O(22) 0 1423(7) B (10) O(32) 0 1359(14) Cu(2) N(5) 0 2009(5) V(3) V(4) 0 30168(10) B (3) O(23) 0 1478(6) B (10) O(31) 0 1375(14) Cu(2) OW2 0 2642(5) V(4) O(12) 0 1612(3) B (3) O(17) # 4 0 1491(6) B (10) O(33) 0 1414(14) Cu(3) N(7) 0 2015(5) V(4) O(11) 0 1943(3) B (3) O(10) 0 1511(6) C(1) N(1) 0 1456(9) Cu(3) N(8) 0 2033(6) V(4) O(8) 0 1948(3) B (4) O(23) 0 1349(8) C(1) C(2) 0 1490(10) Cu(3) O(12) 0 2464(4) V(4) O(13) 0 1954(4) B (4) O(25) 0 1364(7) C(2) N(2) 0 1476(10) Cu(4) N(9) 0 2008(6) V(4) O(14) 0 1963(3) B (4) O(24) 0 1370(7) C(3) C(4) 0 1441(15) Cu(4) N(10) 0 2022(7) V(4) V(5) 0 30283(11) B (5) O(26) 0 1424(6) C(3) N(3) 0 1452(11) Cu(4) O(9) 0 2536(4) V(5) O(15) 0 1620(3) B (5) O(25) 0 1472(6) C(4) N(4) 0 1482(11) V(1) O(1) 0 1607(4) V(5) O(13) 0 1932(3) B (5) O(5) # 4 0 1482(6) C(5) N(5) 0 1467(8) V(1) O(5) 0 1923(3) V(5) O(17) 0 1939(3) B (5) O(10) 0 1509(7) C(5) C(6) # 1 0 1508(8) V(1) O(3) 0 1927(3) V(5) O(14) 0 1967(3) B (6) O(26) 0 1430(6) C(6) N(6) 0 1473(8) V(1) O(2) 0 1986(3) V(5) O(16) 0 1981(3) B (6) O(11) 0 1481(7) C(6) C(5) # 1 0 1508(8)

394 Vol 62, 2004 V(1) O(4) 0 2009(3) V(5) V(6) 0 30037(12) B (6) O(27) 0 1482(6) C(7) N(7) 0 1474(9) V(1) V(6) 0 29776(11) V(6) O(18) 0 1605(4) B (6) O(2) # 4 0 1522(6) C(7) C(8) 0 1497(10) V(1) V(2) 0 29792(11) V(6) O(4) 0 1884(3) B (7) O(27) 0 1354(6) C(8) N(8) 0 1458(9) V(2) O(6) 0 1601(4) V(6) O(14) 0 1888(3) B (7) O(29) 0 1355(6) C(9) N(9) 0 1474(13) V(2) O(8) 0 1889(4) V(6) O(5) 0 1926(3) B (7) O(28) 0 1381(7) C(9) C(10) 0 1481(14) V(2) O(4) 0 1893(3) V(6) O(17) 0 1937(4) B (8) O(30) 0 1426(6) C(10) N(10) 0 1451(14) V(2) O(3) 0 1920(3) B (1) O(20) 0 1349(7) B (8) O(13) 0 1475(7) N(1) Cu(1) N(2) 85 1 (2) O(8) V(4) O(13) 144 33 (15) C(4) C(3) N(3) 109 7 (7) N(1) Cu(1) N(3) 173 9 (2) O(12) V(4) O(14) 107 41 (18) C(4) C(3) Cu(1) 76 8 (5) N(2) Cu(1) N(3) 96 4 (2) O(11) V(4) O(14) 144 33 (15) N(3) C(3) Cu(1) 42 8 (3) N(1) Cu(1) N(4) 94 6 (2) O(8) V(4) O(14) 92 62 (14) C(3) C(4) N(4) 111 5 (7) N(2) Cu(1) N(4) 179 6 (3) O(13) V(4) O(14) 78 08 (14) C(3) C(4) Cu(1) 73 9 (5) N(3) Cu(1) N(4) 84 0 (3) V(3) V(4) V(5) 138 46 (3) N(4) C(4) Cu(1) 42 1 (3) N(1) Cu(1) OW1 93 29 (18) O(15) V(5) O(13) 108 72 (17) N(5) C(5) C(6) # 1 107 8 (5) N(2) Cu(1) OW1 91 2 (2) O(15) V(5) O(17) 111 26 (17) N(5) C(5) Cu(2) 41 5 (3) N(3) Cu(1) OW1 92 6 (2) O(13) V(5) O(17) 137 82 (15) C(6) # 1 C(5) Cu(2) 74 1 (4) N(4) Cu(1) OW1 88 9 (2) O(15) V(5) O(14) 107 95 (17) N(6) C(6) C(5) # 1 108 1 (5) N(1) Cu(1) O(1) 88 02 (17) O(13) V(5) O(14) 78 50 (14) N(6) C(6) Cu(2) 41 8 (2) N(2) Cu(1) O(1) 87 9 (2) O(17) V(5) O(14) 76 98 (14) C(5) # 1 C(6) Cu(2) 75 3 (4) N(3) Cu(1) O(1) 86 1 (2) O(15) V(5) O(16) 105 03 (17) N(7) C(7) C(8) 109 3 (6) N(4) Cu(1) O(1) 92 0 (2) O(13) V(5) O(16) 91 47 (14) N(7) C(7) Cu(3) 41 8 (3) OW1 Cu(1) O(1) 178 32 (14) O(17) V(5) O(16) 90 82 (14) C(8) C(7) Cu(3) 74 9 (4) N(6) Cu(2) N(6) # 1 180 0 O(14) V(5) O(16) 147 02 (14) N(8) C(8) C(7) 107 6 (6) N(6) Cu(2) N(5) # 1 84 50 (19) V(6) V(5) V(4) 74 79 (3) N(8) C(8) Cu(3) 42 3 (3) N(6) Cu(2) N(5) 95 5 (2) O(18) V(6) O(4) 108 45 (19) C(7) C(8) Cu(3) 74 8 (4) N(5) # 1 Cu(2) N(5) 180 000 (1) O(18) V(6) O(14) 109 46 (18) N(9) C(9) C(10) 108 2 (8) N(6) Cu(2) OW2 # 1 90 24 (18) O(4) V(6) O(14) 92 90 (15) N(9) C(9) Cu(4) 41 1 (3) N(6) # 1 Cu(2) OW2 # 1 89 76 (18) O(18) V(6) O(5) 107 06 (18) C(10) C(9) Cu(4) 72 8 (6) N(5) # 1 Cu(2) OW2 # 1 86 74 (18) O(4) V(6) O(5) 80 63 (14) N(10) C(10) C(9) 109 8 (8) N(5) Cu(2) OW2 # 1 93 26 (18) O(14) V(6) O(5) 143 07 (16) N(10) C(10) Cu(4) 43 4 (4) N(6) Cu(2) OW2 89 76 (18) O(18) V(6) O(17) 106 12 (19) C(9) C(10) Cu(4) 77 0 (6) N(5) Cu(2) OW2 86 74 (18) O(4) V(6) O(17) 145 24 (16) C(1) N(1) Cu(1) 108 0 (4) OW2 # 1 Cu(2) OW2 180 0 O(14) V(6) O(17) 78 92 (14) C(2) N(2) Cu(1) 107 0 (4) N(7) # 2 Cu(3) N(7) 180 00 (5) O(5) V(6) O(17) 85 97 (15) C(3) N(3) Cu(1) 108 0 (5) N(7) # 2 Cu(3) N(8) # 2 83 9 (2) V(1) V(6) V(5) 138 73 (4) C(4) N(4) Cu(1) 108 5 (5) N(7) Cu(3) N(8) # 2 96 1 (2) O(20) B (1) O(21) 124 0 (5) C(5) N(5) Cu(2) 109 6 (4) N(7) # 2 Cu(3) N(8) 96 1 (2) O(20) B (1) O(19) 118 4 (5) C(6) N(6) Cu(2) 108 9 (3) N(8) # 2 Cu(3) N(8) 180 000 (2) O(21) B (1) O(19) 117 7 (5) C(7) N(7) Cu(3) 109 1 (4) N(7) # 2 Cu(3) O(12) 86 12 (17) O(22) B (2) O(21) 107 8 (4) C(8) N(8) Cu(3) 108 9 (4) N(7) Cu(3) O(12) 93 88 (17) O(22) B (2) O(7) 109 6 (4) C(9) N(9) Cu(4) 110 0 (5) N(8) # 2 Cu(3) O(12) 92 09 (19) O(21) B (2) O(7) 110 4 (4) C(10) N(10) Cu(4) 107 0 (6) N(8) Cu(3) O(12) 87 91 (19) O(22) B (2) O(16) # 4 113 7 (4) V(1) O(1) Cu(1) 142 1 (2) O(12) Cu(3) O(12) # 2 180 0 O(21) B (2) O(16) # 4 108 7 (4) B (8) # 4 O(2) B (6) # 4 114 6 (3) N(9) Cu(4) N(9) # 3 180 00 (19) O(7) B (2) O(16) # 4 106 7 (4) B (8) # 4 O(2) V(1) 121 0 (3) N(9) Cu(4) N(10) 84 2 (3) O(22) B (3) O(23) 108 3 (4) B (6) # 4 O(2) V(1) 121 2 (3) N(9) Cu(4) N(10) # 3 95 8 (3) O(22) B (3) O(17) # 4 110 4 (4) B (9) # 4 O(3) V(2) 129 0 (3) N(10) Cu(4) N(10) # 3 180 000 (2) O(23) B (3) O(17) # 4 108 9 (4) B (9) # 4 O(3) V(1) 129 2 (3) N(9) Cu(4) O(9) 91 74 (18) O(22) B (3) O(10) 112 5 (4) V(2) O(3) V(1) 101 51 (15) N(10) Cu(4) O(9) 88 9 (2) O(23) B (3) O(10) 108 4 (4) V(6) O(4) V(2) 147 5 (2) N(10) # 3 Cu(4) O(9) 91 1 (2) O(17) # 4 B (3) O(10) 108 2 (4) V(6) O(4) V(1) 99 76 (15)

No 4 : H 3 {[ Cu(en) 2 ] 5 [ (VO) 12 O 6 B 18 O 42 ]} 395 N(9) Cu(4) O(9) # 3 88 26 (18) O(23) B (4) O(25) 122 9 (5) V(2) O(4) V(1) 99 52 (15) O(9) Cu(4) O(9) # 3 180 000 (1) O(23) B (4) O(24) 116 6 (5) B (5) # 4 O(5) V(1) 128 3 (3) O(1) V(1) O(5) 110 75 (18) O(25) B (4) O(24) 120 5 (5) B (5) # 4 O(5) V(6) 129 1 (3) O(1) V(1) O(3) 111 17 (19) O(26) B (5) O(25) 108 3 (4) V(1) O(5) V(6) 101 34 (16) O(5) V(1) O(3) 135 86 (16) O(26) B (5) O(5) # 4 110 9 (4) B (2) O(7) V(2) 129 2 (3) O(1) V(1) O(2) 105 82 (18) O(25) B (5) O(5) # 4 108 7 (4) B (2) O(7) V(3) 128 7 (3) O(5) V(1) O(2) 90 35 (14) O(26) B (5) O(10) 113 6 (4) V(2) O(7) V(3) 101 92 (15) O(3) V(1) O(2) 91 13 (14) O(25) B (5) O(10) 109 7 (4) V(2) O(8) V(4) 144 89 (19) O(1) V(1) O(4) 106 71 (18) O(5) # 4 B (5) O(10) 105 7 (4) V(2) O(8) V(3) 102 10 (15) O(5) V(1) O(4) 77 62 (14) O(26) B (6) O(11) 110 8 (4) V(4) O(8) V(3) 100 30 (16) O(3) V(1) O(4) 77 81 (14) O(26) B (6) O(27) 107 9 (4) V(3) O(9) Cu(4) 140 2 (2) O(2) V(1) O(4) 147 46 (15) O(11) B (6) O(27) 110 0 (4) B (5) O(10) B (3) 113 8 (4) V(6) V(1) V(2) 74 99 (3) O(26) B (6) O(2) # 4 111 8 (4) B (5) O(10) V(3) 121 6 (3) O(6) V(2) O(8) 107 01 (19) O(11) B (6) O(2) # 4 107 9 (4) B (3) O(10) V(3) 120 3 (3) O(6) V(2) O(4) 107 47 (19) O(27) B (6) O(2) # 4 108 3 (4) B (6) O(11) V(3) 130 7 (3) O(8) V(2) O(4) 92 38 (15) O(27) B (7) O(29) 122 9 (5) B (6) O(11) V(4) 127 2 (3) O(6) V(2) O(3) 107 99 (19) O(27) B (7) O(28) 121 8 (5) V(3) O(11) V(4) 102 09 (17) O(8) V(2) O(3) 144 78 (16) O(29) B (7) O(28) 115 3 (4) V(4) O(12) Cu(3) 148 8 (2) O(4) V(2) O(3) 80 82 (14) O(30) B (8) O(13) 111 4 (4) B (8) O(13) V(5) 129 4 (3) O(6) V(2) O(7) 107 80 (19) O(30) B (8) O(29) 107 3 (4) B (8) O(13) V(4) 128 2 (3) O(8) V(2) O(7) 78 99 (14) O(13) B (8) O(29) 109 4 (4) V(5) O(13) V(4) 102 39 (17) O(4) V(2) O(7) 144 68 (16) O(30) B (8) O(2) # 4 112 8 (4) V(6) O(14) V(4) 144 07 (19) O(3) V(2) O(7) 86 82 (14) O(13) B (8) O(2) # 4 107 3 (4) V(6) O(14) V(5) 102 34 (15) V(1) V(2) V(3) 139 01 (4) O(29) B (8) O(2) # 4 108 6 (4) V(4) O(14) V(5) 100 79 (16) O(9) V(3) O(11) 111 40 (19) O(30) B (9) O(20) # 4 108 5 (4) B (9) O(16) B (2) # 4 113 7 (4) O(9) V(3) O(7) 109 87 (19) O(30) B (9) O(3) # 4 109 6 (4) B (9) O(16) V(5) 121 4 (3) O(11) V(3) O(7) 136 61 (15) O(20) # 4 B (9) O(3) # 4 109 1 (4) B (2) # 4 O(16) V(5) 121 6 (3) O(9) V(3) O(8) 108 27 (18) O(30) B (9) O(16) 113 7 (4) B (3) # 4 O(17) V(6) 128 5 (3) O(11) V(3) O(8) 78 31 (15) O(20) # 4 B (9) O(16) 110 0 (4) B (3) # 4 O(17) V(5) 129 9 (3) O(7) V(3) O(8) 76 68 (14) O(3) # 4 B (9) O(16) 105 9 (4) V(6) O(17) V(5) 101 58 (15) O(9) V(3) O(10) 105 82 (18) O(32) B (10) O(31) 124 7 (10) B (1) O(20) B (9) # 4 120 9 (4) O(11) V(3) O(10) 90 00 (14) O(32) B (10) O(33) 118 6 (10) B (1) O(21) B (2) 120 9 (4) O(7) V(3) O(10) 91 29 (14) O(31) B (10) O(33) 116 7 (10) B (3) O(22) B (2) 121 0 (4) O(8) V(3) O(10) 145 91 (14) N(1) C(1) C(2) 107 5 (6) B (4) O(23) B (3) 121 1 (4) V(2) V(3) V(4) 74 74 (3) N(1) C(1) Cu(1) 42 5 (3) B (4) O(25) B (5) 121 2 (4) O(12) V(4) O(11) 108 25 (18) C(2) C(1) Cu(1) 75 1 (4) B (5) O(26) B (6) 119 7 (4) O(12) V(4) O(8) 105 38 (18) N(2) C(2) C(1) 108 5 (6) B (7) O(27) B (6) 121 8 (4) O(11) V(4) O(8) 78 98 (15) N(2) C(2) Cu(1) 43 0 (3) B (7) O(29) B (8) 121 7 (4) O(12) V(4) O(13) 110 27 (18) C(1) C(2) Cu(1) 74 2 (4) B (9) O(30) B (8) 120 8 (4) O(11) V(4) O(13) 88 74 (15) Symmetry codes : # 1 - x + 1, - y, - z + 1; # 2 - x - 1, - y + 1, - z + 1 ; # 3 - x, - y + 2, - z + 1 ; # 4 - x, - y + 1, - z + 1 {[ Cu ( en) 2 ] 5 [ ( VO) 12 O 6 B 18 2 [VO 5 ],6 V O 42 ]} 3 - [ H 2 O ] [ (VO) 12 O 6 B 18 O 42 ] 13 - [ H 2 O], ; (Figure 1),B 18 O 42 18 B ( 3 2O) V 60, V O t V 6 O 18 (, 6 3 2O 2 B V 6,V O t 011602 (4) 011620 (3) 1 V, 3 2O B 011506 (6) 011522 (6) nm, 3 2 nm, 6 3 2O 3 V, 3 2O V O V 011981 (3) 012002 (3) nm ; 12 3 2O 1 011884 (3) 012009 ( 3) nm O V O 76168 ( 14) B 2 V, 3 2O B 011475 (7) 011498 (6) 147102(14), V O V 99152 (15) 14715 (2) B 18 nm, 3 2O V 011920 (3) 011954 (4) nm) V 6 O 18 6 [ B 3 O 7 ] ( Figure 2 ( b) ), (Figure 2 (a) ),V [ VO 5 ],6 [ B 3 O 7 ],

396 Vol 62, 2004 1 [ (VO) 12 O 6 B 12 O 42 ] 13 - [ H 2 O] 012449 (4) 012486 (4) nm ; Cu (3) Cu (4) Figure 1 The structure of the title compound s anion cluster [ (VO) 12 2 O 6 B 18 O 42 ] 13 - [ H 2 O] [B 3 O 7 ],2 B, B, 4 O B B O 011422 (6) 011522 (6) nm,o B O 10517(4) 11317 (4) O B B O 011349 (7) 011389 (7) nm, O B O 11513 ( 4 ) 12410 ( 5 ) B O B 11317 ( 4 ) 12118 (4), B O V 12013 (3) 13017 (3), 01343 nm,cu, 2, 3 Cu (2), [ Cu (en) 2 ( H 2 O) 2 ] 2 + ;Cu (1) [V 6 O 18 ], Cu (1) O 2 [ V 6 O 18 ] Cu 2 +, Cu O, Cu (3) O (12) Cu (4) O(9) 012464 (4) 012536 (4) nm,, [ V 12 B 18 O 60 ] Cu ( 3) [ Cu(en) 2 ] 2 + a, b Cu (4) [ Cu (en) 2 ] 2 +, c (Figure 3), 11817 nm, 01619 nm, Cu (2) [ Cu ( en) 2 ( H 2 O) 2 ] 2 + [B (OH) 3 ] 3 Figure 3 The packing of the title compound with water moleculars, [B (OH) 3 ] and some [ Cu(en) 2 ] are omitted for clarity 2 V 6 O 18 (a) B 18 O 42 (b) Figure 2 Veiw of V 6 O 18 ring (a) and B 18 O 42 ring (b) [8,9] : V 4145, V V 7 5 4142 ;, V V 7 5, [B (OH) 3 ],B 3 O 360, B O [8 011359 (14) 011414 (14) nm,,9]

No 4 : H 3 {[ Cu(en) 2 ] 5 [ (VO) 12 O 6 B 18 O 42 ]} 397 B [ 2 ] [ Zn ( en) 2 ] 6 2 [ (VO) 12 O 6 B 18 O 39 (OH) 3 ] 13H 2 O, ph 8, ph = 812 815, [ Cu (en) 2 ] 2 + [ Zn (en) 2 ] 2 +, [ Zn ( en) 2 ] 2 + [ Cu(en) 2 ] 2 +,, 2 2 700 1000 cm - 1 V O, 950 cm - 1 V O t (O t ), 660 890 cm - 1 V O b,c V (O b,c ) 1042 cm - 1 1091 cm - 1 B O 4, B O 1356 cm - 1 1401 cm - 1, 1600 1650 cm - 1 Figure 4 The fluorescent spectra of the compound ( - NH) 3200 3500 cm - 1 O H, 2 3 400 1000 cm - 1 V O, 955 cm - 1 V O t,v O b,c V 866 cm - 1 746 cm - 1,, 372 cm - 1 Raman V O B O 2 4-230 nm 340 nm 2, (O t V) (O b,c 2 7 V), 570 nm, [ Cu(en) 2 ] Cu 2 + TGA (Figure 6), 29 d2d, 120 917 %, ( 9148 %) ; 120 500 2011 %, 2 5 310 nm, 415nm (Figure 4), O V 310 nm 415 nm, F ( t) = B 1 exp ( - t/ 1 ) + B 2 exp ( - t/ 2 ) ( B 1 = 53119, B 2 = 34128) 1 = 1178 ns 2 = 17181 ns, : en, [ Cu(en) 2 ] en 2 6 ESR 81956 GHz, (3300 250) Gauss, ( Figure 5),, g 119292 119185, Figure 6 The TGA diagram of the compound V 4 + Cu 2 +, V 4 + ESR 33 Gauss, - 5 ESR Figure 5 ESR of the compound en ( 19175 %), 500 800,, 6 TGA

398 Vol 62, 2004 References 1 M ller, A ; Peters, F ; Pope, M T Chem Rev 1998, 98, 239 2 Zhang, L2R ; Shi, Z ; Yang, G2Y ; Chen, X2M ; Feng, S 2H J Solid State Chem 1999, 148, 450 3 Sevov, S C Angew Chem, Int Ed Engl 1996, 35, 2630 4 Rijssenbeek, J T ; Rose, D J ; Haushalter, R C ; Zubieta, J Angew Chem, Int Ed Engl 1997, 36, 1008 5 Lin, Z2H ; Zhang, H2H ; Huang, C2C ; Sun, R2Q ; Yang, Q 2Y ; Wu, X2Y Chin J Struct Chem 2003, 22 (6), in press (,,,,,,, 2004, 23 (1), ) 6 Sheldrick, G M SHELXS297, Program for Crystal Structure Solution, University of Gottingen, Germany, 1997 7 Sheldrick, G M SHELXS297, Program for Crystal Structure Refinement, University of Gottingen, Germany, 1997 8 Brown, I D ; Altermatt, D Acta Crystallogr 1985, B41, 244 9 Brown, I D ; Wu, K K Acta Crystallogr 1976, B32, 1950 (A0304089 ZHAO, X J ; LU, Z S )

No 4 Graphical Abstract Study on Thermochemistry and Thermal De2 composition Kinetics of Ternary Solid2State Complex of Gadolinium Chloride with L2Tyro2 sine and Glycine ZHANG, Zhong2Hai ; KU, Zong2Jun ; XIA, Fei ; LIU, Yi ; LI, Hui2Rong ; HU, Yan2Jun ; ZHAO, Shun2Sheng ; QU, Song2Sheng Acta Chimica Sinica 2004, 62 (4), 386 Hydrothermal Synthesis, Crystal Structure and Properties of Polyoxovanadium Borate H 3 {[ Cu( en) 2 ] 5 [ ( VO) 12 O 6 B 18 O 42 ] } [ B( OH) 3 ] 2 16 H 2 O Using a solution2reaction isoperibol calorimeter, the molar enthalpy of reaction for the follow2 ing reaction, GdCl 3 6H 2 O (s) + Tyr (s) + 3Gly ( s) = Gd ( Tyr) ( Gly) 3 Cl 3 3H 2 O ( s) + 3H 2 O (l), was determined to be (9 451 0 468) kj mol - 1 at 298 15 K The standard molar enthalpy of formation of Gd( Tyr) ( Gly) 3 Cl 3 3H 2 O ( s) at 298 15 K was derived as - (4269 7 2 3) kj mol - 1 The kinetics of thermal decomposition of the complex was studied by TG, DTG and DTA LIN, Zhi2Hua ; ZHANG, Han2Hui ; HUANG, Chang2Cang ; SUN, Rui2Qing ; CHEN, Yi2Ping ; WU, Xiao2Yuan Acta Chimica Sinica 2004, 62 (4), 391 In the structure of the compound, there is a ring of B 18 O 42 sandwiched between two vanadi2 um2oxygen clusters V 6 O 18 by eighteen B ( 3 2O) V bonds, and the anion clusters [ (VO) 12 O 6 B 18 O 42 ] 13 - are connected through four [ Cu(en) 2 ] 2 + by the static electronic in2 teraction Thus, the complex was extended to an infinite two2dimensional network structure, with size of the hole amounting to 0 619 1 817 nm Synthesis of 2Cyclodextrin2o2vanillin Benzoylhydrazone and Its Application TANG, Bo ; ZHANG, Li2Li ; ZHANG, Jie ; WANG, Xu ; CHEN, Zhen2Zhen ; WANG, Hong2Jian ; WU, Chang2Ju Acta Chimica Sinica 2004, 62 (4), 399 A novel host molecular probe of 2cyclodextrin2o2vanillin benzoylhydrazone ( 2CDP2OVBH) was synthesized, and the fluorescent excitation ( a) and emission spectra ( b) were deter2 mined It was indicated that the complex of 2CDP2OVBH2Al 3 + was superior to those of OVBH2Al 3 + and 2CDP + OVBH + Al 3 + in the spectrofluorimetric determination of alumini2 um

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