4, Cu( II), Zn( II)
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- Αλθαία Αντωνόπουλος
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1 , ACTA CHIMICA SINICA Vol 62, 2004 No 22, , Cu( II), Zn( II) Ξ Ξ ( ) 4, (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 ) 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, (dafo), dafo [1] ; [8 11],, dafo,, dafo [2 6] 1984 Henderson [12 14] 4, ( II) Ξ E2mail : edu cn Received March 1, 2004 ; revised June 10, 2004 ; accepted July 24, 2004 (No ) (973 ) (No 2003CB214606) (No 03JS006) (No 04J K143)
2 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 ( = nm) 22 Gaussian298w DFT2B3LYP/ LANL2DZ 2989, 1953 [ I > 2 ( I) ] II, 1 e/ nm :, P21 a = (4) nm, b = (5) nm, c = (5) nm, = (5), Vario EL III CHNOS, = (7), = (7), V = (5) nm 3, Z = 1, Bruker Smart21000CCD Rigaku F(000) = 300, M AFC7R, Bruker r = , D c = g/ cm 3, (Mo K ) = EQUINO 55, NETZSCH mm - 1, R 1 = , wr 2 = STA449C, AR dafo [7 ] 1 2 I g (1199 mmol) 4, ml, g (1154 mmol), 1 h 20 ml, 40 min,, 3 4 II,10 d m1p Anal calcd for C 22 H 16 CuN 6 O 10 : C 45105, H 2173, N ; found C 45114, H 2143, N II g ( mol) dafo 30 ml,, O(3) Cu N (3), O (3) Cu N (4), O (3) Cu 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) nm, 1 h, nm,, 1 h,7 d X m1p , II I Anal calcd for C 22 H 16 ZnN 6 O 10 : C 44176, H 2171, N ; found C 44160, H 2172, N 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), = nm) 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 e/ nm 3 Zn(1) O(5A), Zn (1) dafo :, P1 ( # 1) a = (2) nm, b = (1) nm, c = (5) nm, = (8), = (10), = (1), V = (1) nm 3, Z = 1, F(000) = , M r = , D c = g/ cm 3, (Mo K ) = mm - 1, R = 01035, wr = II, 0130 mm 0120 mm 0115 mm Fourier, SHELX297 F 2, Fourier 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) nm nm, 4,
3 No 22 :4, Cu( II), Zn( II) I (nm) ( ) Table 1 Parts of the bond length (nm) and bond angle ( ) data of complex I Cu (4) N(3) Cu N(4) 79 5 (2) Cu (5) O(3) Cu O(4) Cu N(3) (6) O(3) Cu Cu N(4) (5) O(3) Cu Cu O(3) (4) O(3) Cu N(3) Cu O(4) (5) O(3) Cu N(4) Cu 79 5 (1) O(4) Cu Cu N(3) (2) O(4) Cu Cu N(4) (2) O(4) Cu N(3) Cu N(3) 98 9 (2) O(4) Cu N(4) Cu N(4) (2) II (nm) ( ) Table 2 The selected bond lengths (nm) and bond angles ( ) of complex II Zn(1) O(5) (4) O(5A) Zn(1) N(1A) (13) Zn(1) O(5A) (4) O(5) Zn(1) (13) Zn(1) N(1A) (3) O(5A) Zn(1) (13) Zn(1) (3) N(1A) Zn(1) Zn(1) (3) O(5) Zn(1) (13) Zn(1) N(2A) (3) O(5A) Zn(1) (13) N(1A) Zn(1) (12) O(5) Zn(1) O(5A) Zn(1) (12) Zn(1) N(2A) (12) O(5) Zn(1) N(2A) (13) O(5) Zn(1) N(1A) (13) O(5A) Zn(1) N(2A) (13) Zn(1) N(2A) N(1A) Zn(1) N(2A) (12) 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, cm - 1 [16,, dafo I II,17] dafo I II : dafo, I II, C = O 1715 cm - 1, = C - H 907, 755 cm - 1, cm - 1 ;, I, C = O 1731, = C - H cm - 1, cm - 1 ; II, C = O,Zn 2 + d 10,d ; Cu , = C - H cm - 1, d 9,, 1385 cm - 1, I, I dafo I II Cu 2 + d (t 2g ) (d ) 1 2 x - y (d ) 2[15] z ;, I,, II ; I C = O
4 2262 Vol 62, 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 : , %, H 2 O NO3 - ( %) ; , %, dafo ( %), DSC,, %, 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 Cu(dafo) 2 - dafo Cu(dafo) - dafo > 334 CuO 3 II Figure 3 Crystal structure of complex II 0 600, II, : 18119, 140, %, ( 6110 %) ; , 210, %, dafo ( %) ; %, ZnO, ZnO ZnO , ( ) II, dafo Cu ( II), Zn( II), N dafo, ; I = C - H dafo II,
5 No 22 :4, Cu( II), Zn( II) 2263 II : 756, cm - 1 ; II - 2H 2 O [ Zn(dafo) 2 ( H 2 O) ] (NO 3 ) [ Zn(dafo) 2 ] (NO 3 ) 2-2dafo Zn(NO 3) 2 > 368 :1724, 915, 760, cm - 1, :1724, 910, 739, 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, ; LUMO, ; E (L - H) 3, ; Gaussian298w DFT2B3LYP II (a1u ) : HOMO, ;, LANL2DZ LUMO, ; E(L - H) 3, LUMO - HOMO :,, ; II I, 1 % 2 %, II I 3 E(L - H) I : 1731, 916, 754,, EHOMO - ELUMO cm - 1, 1723, 913, 3 ( %) Table 3 Atomic net charge populations ( %) Mulliken layout analysis I Cu O(3) O(4) N(3) N(4) II Zn(1) O(5) O(5A) N(1A) N(2A) Natural population analysis I Cu O(3) O(4) N(3) N(4) II Zn(1) O(5) O(5A) N(1A) N(2A) Ohba, M ; Maruono, N ; Okawa, H ; Enokl, T ; Latour, J Gaussian298w References 1 Sammes, P G ; Yahoglu, G J Chem Soc Rev 1994, Kinosshita, M Jpn J Appl Phys 1994, 33, 5718 M J Am Chem Soc 1994, 116, Ohba, M ; Fukita, N ; Okawa, H J Chem Soc, Dalton Trans 1997, Ohba, M ; Okawa, H ; Ito, T ; Ohto, A J Chem Soc, Chem Commun 1995, Ohba, M ; Okawa, H ; Fukita, N ; Hashimoto, Y J Am Chem Soc 1997, 119, Henderson, L J Jr ; Fronzek, F R ; Cherry, W R J
6 2264 Vol 62, 2004 Am Chem Soc 1984, 106, Pyle, M ; Rahman, R ; Meshoyrer, J P ; Kumar, C V ; Turro, N J ; Barton, J K J Am Chem Soc 1989, 111, Wang, Y X ; Rillema, D P Tetrahedron 1997, 53, 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, 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, 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 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 ) (A ZAO, X J ; DONG, H Z )
[ Co( aipamp apamp) ( amp) Cl] [ ZnCl 4 ]
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