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2004 62 22, 2259 2264 ACTA CHIMICA SINICA Vol 62, 2004 No 22, 2259 2264 4,52 292 Cu( II), Zn( II) Ξ Ξ ( 710069) 4,52 292 (dafo) Cu( II), Zn( II) [ Cu(dafo) 2 (H 2 O) 2 ] (NO 3 ) 2 [ Zn(dafo) 2 (H 2 O) 2 ] (NO 3 ) 2, X, Cu ( II), Zn( II),,,, Cu( II),Zn( II),, Gaussian298w DFT2B3LYP/ LANL2DZ 4,52 292,Cu( II),Zn( II),, Synthesis, Crystal Structure, Thermal Analysis and Theoretical Computation of Cu( II) and Zn( II) Complexes with 4,52Diazafluorene292one ZHANG, Rong2Lan HU, Juan ZHAO, Jian2She Ξ HE, Shui2Yang LIU, Jian2Ning SHI, Qi2Zhen ( Shaanxi Key Laboratory of Physico2Inorganic Chemistry, Department of Chemistry, Northwest University, Xi an 710069) Abstract Two novel complexes [ Cu (dafo) 2 ( H 2 O) 2 ] (NO 3 ) 2 and [ Zn (dafo) 2 ( H 2 O) 2 ] (NO 3 ) 2 were synthesized Their structures were determined by single crystal X2ray diffraction analysis The crystal structure data indicate that the Cu( II) and Zn ( II) ions are coordinated with the four nitrogen atoms from the two ligands (dafo) and two oxygen atoms from the two water molecules, respectively The two ligands (dafo), Cu( II) and Zn ( II) ions are in the same plane, the two water molecules are vertical to the plane, the Cu( II) ion is at the center of the malformed octahedron, and Zn ( II) ion is at the center of the normal octahedron The constitutes of the two complexes were proved by elemental analysis, IR spectra and thermal analysis On the basis of the experimentation, the two complexes were computed by DFT2B3L YP/ LANL2DZ in Gaussian298w Keywords 4, 52diazafluorene292one, copper ( II) complex, zinc ( II) complex, crystal structure, theoretical computation [7], 4,52 292 (dafo), dafo [1] ; [8 11],, dafo,, dafo [2 6] 1984 Henderson [12 14] 4,52 292 ( II) Ξ E2mail : jszhao @nwu edu cn Received March 1, 2004 ; revised June 10, 2004 ; accepted July 24, 2004 (No 20371039) (973 ) (No 2003CB214606) (No 03JS006) (No 04J K143)

2260 Vol 62, 2004 (II) [ Cu ( dafo) 2 ( H 2 O) 2 ] (NO 3 ) 2 ( I) [ Zn ( dafo) 2 2 (H 2 O) 2 ] (NO 3 ) 2 ( II) X, Bruker Smart21000CCD,, Mo K ( = 01071073 nm) 22 Gaussian298w DFT2B3LYP/ LANL2DZ 2989, 1953 [ I > 2 ( I) ] II, 1 e/ nm 1 1 3 :, P21 a = 016989 (4) nm, b = 018281 (5) nm, c = 110231 (5) nm, = 941934 (5), Vario EL III CHNOS, = 911366 (7), = 991820 (7), V = 015809 (5) nm 3, Z = 1, Bruker Smart21000CCD Rigaku F(000) = 300, M AFC7R, Bruker r = 589178, D c = 11686 g/ cm 3, (Mo K ) = EQUINO 55, NETZSCH 11130 mm - 1, R 1 = 010521, wr 2 = 011096 STA449C, AR dafo [7 ] 1 2 I 01363 g (1199 mmol) 4,52 292 30 ml, 01384 g (1154 mmol), 1 h 20 ml, 40 min,, 3 4 II,10 d m1p 271 273 Anal calcd for C 22 H 16 CuN 6 O 10 : C 45105, H 2173, N 14133 ; found C 45114, H 2143, N 14130 1 3 II 013632 g ( 01002 mol) dafo 30 ml,, O(3) Cu N (3), O (3) Cu N (4), O (3) Cu 012975 g (01001 mol) Zn(NO 3 ) 2 3 ml 95 %,01148 g (01001 mol) 3 ml 95 %, ; (2) dafo ; (3) Cu O (3) Cu O(4), 60, dafo O(5) O(9) 011784 nm, 1 h, 011828 nm,, 1 h,7 d X m1p 264 266 3, II I Anal calcd for C 22 H 16 ZnN 6 O 10 : C 44176, H 2171, N 14124 ; found C 44160, H 2172, N 13178 1 4 I, 0120 mm 0120 mm 0130 mm N(1A) Zn ( 1) N ( 2A, N ( 1) Zn ( 1) N ( 2A), N ( 2) Rigaku AFC7R, Mo K ( Zn(1) N ( 2A) Zn ( 1) N ( 1A), Zn ( 1) N ( 1), = 01071069 nm) 22 2892 Zn(1), Zn ( 1) N ( 2A) : ( 1) N ( 1),, 2357 [ I > 2 ( I) ] I, Zn(1), N(1A), N(2A), Fourier,Zn(1) ; (2) dafo,, Zn ( 1) dafo, DIRDIF92 PATTY F 2, O(5) Zn(1) O (5A) = 18010, Zn (1) O (5) Fourier 500-830 e/ nm 3 Zn(1) O(5A), Zn (1) dafo :, P1 ( # 1) a = 017987 (2) nm, b = 110543 (1) nm, c = 0170403 (5) nm, = 911557 (8), = 961711 (10), = 94145 (1), V = 015866 (1) nm 3, Z = 1, F(000) = 299100, M r = 587195, D c = 11664 g/ cm 3, (Mo K ) = 11003 mm - 1, R = 01035, wr = 01046 II, 0130 mm 0120 mm 0115 mm Fourier, SHELX297 F 2, Fourier 379-544 2 2 1 I II 1 2, 10 ml 3 2 mol L - 1, 1 2 I 1, I [ Cu(dafo) 2 ] 2 + H 2 O NO3 -, [ N (1), N (2), N (3), N (4), O(3), O (4) ] O (3) Cu, O (3) Cu O(4) : (1), [ Zn ( dafo) 2 ] 2 + H 2 O NO3 -,Zn ( 1), N ( 1A) Zn(1), N(1A) Zn(1), Zn(1), [ N (1), N (2), N (1A), N(2A), O(5), O (5A) ] O (3) O (3A) 011894 nm 011989 nm, 4,

No 22 :4,52 292 Cu( II), Zn( II) 2261 1 I (nm) ( ) Table 1 Parts of the bond length (nm) and bond angle ( ) data of complex I Cu 0 1999(4) 0 2011 N(3) Cu N(4) 79 5 (2) 80 10 Cu 0 2619(5) 0 2640 O(3) Cu O(4) 179 2 179 95 Cu N(3) 0 1987(6) 0 2011 O(3) Cu 90 5 88 40 Cu N(4) 0 2587(5) 0 2640 O(3) Cu 89 6 98 10 Cu O(3) 0 1988(4) 0 2062 O(3) Cu N(3) 89 9 88 41 Cu O(4) 0 1966(5) 0 2069 O(3) Cu N(4) 89 7 98 00 Cu 79 5 (1) 80 10 O(4) Cu 90 4 91 61 Cu N(3) 178 4 (2) 179 98 O(4) Cu 90 7 81 9 Cu N(4) 102 0 (2) 100 4 O(4) Cu N(3) 89 3 91 57 Cu N(3) 98 9 (2) 100 3 O(4) Cu N(4) 89 9 81 9 Cu N(4) 178 3 (2) 163 8 2 II (nm) ( ) Table 2 The selected bond lengths (nm) and bond angles ( ) of complex II Zn(1) O(5) 0 2066(4) 0 2141 O(5A) Zn(1) N(1A) 90 68 (13) 90 02 Zn(1) O(5A) 0 2066(4) 0 2141 O(5) Zn(1) 90 68 (13) 89 99 Zn(1) N(1A) 0 2202(3) 0 2282 O(5A) Zn(1) 89 32 (13) 90 01 Zn(1) 0 2202(3) 0 2282 N(1A) Zn(1) 180 0 180 00 Zn(1) 0 2278(3) 0 2282 O(5) Zn(1) 89 69 (13) 90 01 Zn(1) N(2A) 0 2278(3) 0 2282 O(5A) Zn(1) 90 31 (13) 89 99 N(1A) Zn(1) 99 02 (12) 98 39 O(5) Zn(1) O(5A) 180 0 180 00 Zn(1) 80 98 (12) 81 61 Zn(1) N(2A) 99 02 (12) 98 38 O(5) Zn(1) N(2A) 90 31 (13) 90 01 O(5) Zn(1) N(1A) 89 32 (13) 89 98 O(5A) Zn(1) N(2A) 89 69 (13) 89 99 Zn(1) N(2A) 180 0 180 00 N(1A) Zn(1) N(2A) 80 98 (12) 81 61 II [ Zn(dafo) 2 ( H 2 O) 2 ] 2 + H 2 O H NO3 - O ; NO3 - O [ Zn (dafo) 2 ( H 2 O) 2 ] 2 + H 2 O 2 2 H II KBr, 400 4000 cm - 1 [16,, dafo I II,17] dafo I II : dafo, I II, C = O 1715 cm - 1, = C - H 907, 755 cm - 1, 1553 1397 cm - 1 ;, I, C = O 1731, = C - H 916 754 cm - 1, - 1567 1384 cm - 1 ; II, C = O,Zn 2 + d 10,d ; Cu 2 + 1724, = C - H 915 760 cm - 1, d 9,, 1385 cm - 1, I, I dafo I II Cu 2 + d (t 2g ) 6 2 2 (d ) 1 2 x - y (d ) 2[15] z ;, I,, II ; I C = O

2262 Vol 62, 2004 1 I Figure 1 Crystal structure of complex I 4 II Figure 4 Cell packing of complex II 2 3 N 2, 10 / min, (DSC) ( TG ) : 0 700, I : 50 196, 28171 %, H 2 O NO3 - ( 27121 %) ; 206 334, 32164 %, dafo ( 31100 %), DSC,, 251 28102 %, I TG, 690,, 700 I : 2 I Figure 2 Cell packing of complex I [ Cu(dafo) 2 ( H 2 O) ] (NO 3 ) 2 - H 2 O, 2NO 3 50 196 Cu(dafo) 2 - dafo 206 334 Cu(dafo) - dafo > 334 CuO 3 II Figure 3 Crystal structure of complex II 0 600, II, : 18119, 140, 205 6107 %, ( 6110 %) ; 25213 29212, 210, 368 61179 %, dafo ( 61172 %) ; 23146 %, ZnO, ZnO ZnO 140 205, (100 120 ) II, dafo Cu ( II), Zn( II), N dafo, ; I = C - H dafo II,

No 22 :4,52 292 Cu( II), Zn( II) 2263 II : 756, 1609 1340 cm - 1 ; II - 2H 2 O [ Zn(dafo) 2 ( H 2 O) ] (NO 3 ) 2 140 205 [ Zn(dafo) 2 ] (NO 3 ) 2-2dafo 210 368 Zn(NO 3) 2 > 368 :1724, 915, 760, 1566 1385 cm - 1, :1724, 910, 739, 1612 1341 cm - 1 Mulliken, 3,,, I II Pauling [18], I H 2 O NO3 -, II H 2 O : II I ; I dafo, II, II dafo I II I ( II I, ) I ( a1u ) : 2 4 HOMO, - 014794 ; LUMO, - 013271 ; E (L - H) 3, 011522 ; Gaussian298w DFT2B3LYP II (a1u ) : HOMO, - 014788 ;, LANL2DZ LUMO, - 013255 ; E(L - H) 3, 011533 1 2 LUMO - HOMO :,, ; II I, 1 % 2 %, II I 3 E(L - H) I : 1731, 916, 754,, EHOMO - ELUMO 1567 1384 cm - 1, 1723, 913, 3 ( %) Table 3 Atomic net charge populations ( %) Mulliken layout analysis I Cu 0 6261 O(3) - 0 7111 O(4) - 0 7147-0 2711-0 0871 N(3) - 0 2709 N(4) - 0 0870 II Zn(1) 1 0593 O(5) - 0 7557 O(5A) - 0 7557-0 2231-0 2232 N(1A) - 0 2231 N(2A) - 0 2232 Natural population analysis I Cu 1 0531 O(3) - 0 4868 O(4) - 0 4885-0 2553-0 2890 N(3) - 0 2592 N(4) - 0 2867 II Zn(1) 1 7186 O(5) - 1 0473 O(5A) - 1 0474-0 6398-0 6399 N(1A) - 0 6398 N(2A) - 0 63985 3 Ohba, M ; Maruono, N ; Okawa, H ; Enokl, T ; Latour, J Gaussian298w References 1 Sammes, P G ; Yahoglu, G J Chem Soc Rev 1994, 327 2 Kinosshita, M Jpn J Appl Phys 1994, 33, 5718 M J Am Chem Soc 1994, 116, 11566 4 Ohba, M ; Fukita, N ; Okawa, H J Chem Soc, Dalton Trans 1997, 1773 5 Ohba, M ; Okawa, H ; Ito, T ; Ohto, A J Chem Soc, Chem Commun 1995, 1545 6 Ohba, M ; Okawa, H ; Fukita, N ; Hashimoto, Y J Am Chem Soc 1997, 119, 1011 7 Henderson, L J Jr ; Fronzek, F R ; Cherry, W R J

2264 Vol 62, 2004 Am Chem Soc 1984, 106, 5876 8 Pyle, M ; Rahman, R ; Meshoyrer, J P ; Kumar, C V ; Turro, N J ; Barton, J K J Am Chem Soc 1989, 111, 3051 9 Wang, Y X ; Rillema, D P Tetrahedron 1997, 53, 12377 10 Cheng, Y X ; Xu, R J ; Xu, Y Z Chin J Inorg Chem 1998, 14, 181 (in Chinese) (,,,, 1998, 14, 181 ) 11 Wang, Y ; Perez, W ; Zheng, G Y ; Rillema, D P ; Huber, C L Inorg Chem 1998, 37, 2227 12 Hu, J MS Thesis, Northwest University, Xi an, 2001, p 6 (in Chinese) (,,,, 2001, p 6 ) 13 Gu, A P ; Zhang, R L ; Zhang, G ; Zhao, J S ; He, S Y ; Dou, J M ; Wang, D Q Chin J Chem 2002, 20, 1616 14 Zhang, R L ; Zhao, J S ; Gu, A P ; He, S Y Acta Chim Sinica 2003, 61, 262 (in Chinese) (,,,,, 2003, 61, 262 ) 15 Shen, P W Inorganic Chemistry, Chemical Industry Press, Beijing, 2002, p 94 (in Chinese) (,,,, 2002, p 94 ) 16 Nakamoto, K Infrared and Raman Spectra of Inorganic and Coordination Compounds, 3rd ed, John Wiley & Sons, New York, 1978, p 214 17 Chang, J H ; Dong, Q G The Theory and Analysis of Spectra, Science Press, Beijing, 2001 (in Chinese) (,,,,, 2001 ) 18 Tang, Z X Intermediate Inorganic Chemistry, High Education Press Beijing, 2003, p 405 (in Chinese) (,,,, 2003, p 405 ) (A0403018 ZAO, X J ; DONG, H Z )

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