Synthesis and Crystal Structure of Supramolecular Complex of Zn( ) Bridged by Phthalate

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1 , ACTA CHIMICA SINICA Vol 62, 2004 No 14, Zn( ) a, b a Ξ, b c Ξ ( a ) ( b ) ( c ) Zn (NO 3 ) 2, phen ( ) phth ( ) {[ Zn 2 (phen) 2 (phth) 2 ( H 2 O) 2 ] 2H 2 O} n X, P2 (1) / n a = (3) nm, b = (3) nm, c = (7) nm, = (5), Z = 4, V = (10) nm 3, D c = g/ cm 3, = mm - 1, F(000) = 912, R 1 = , wr 2 = ,,, 2,,, Synthesis and Crystal Structure of Supramolecular Complex of Zn( ) Bridged by Phthalate SUN, Ya2Guang a, b WEI, De2Zhou a GAO, En2Jun Ξ, b DING, Fu c ( a School of Resource & Civil Engineering, Northeastern University, Shenyang ) ( b Laboratory of Coordination Chemistry, Shenyang Institute of Chemical Technology, Shenyang ) ( c Institute of Chemical Science and Engineering, Liaoning University, Shenyang ) Abstract Novel supramolecular complex {[ Zn 2 (phen) 2 (phth) 2 ( H 2 O) 2 ] 2H 2 O} n (phen = phenanthroline ; phth = phthalate) has been synthesized by the reaction of phen and phth with zinc( ) salt Elemental analysis, IR spectra and X2ray crystal structure analysis were carried out to determine the composition and crystal structure of title complex The title complex belongs to monoclinic system with space group P2 (1) / n, a = (3) nm, b = (3) nm, c = (7) nm, = (5), Z = 4, V = (10) nm 3, D c = g/ cm 3, = mm - 1, F (000) = 912, R 1 = , wr 2 = , and the zinc atom rendered five2coordinate in a distorted trigonal bipyramidal configuration The complex formed 12D helix chain bridged by phth and 22D network structure by 2 action of neighbouring helix chain Keywords zinc complex, supramolecular, phthalate, crystal structure, [6,7], [1 4],,, {[ Zn 2 ( phen) 2 ( phth) 2 ( H 2 O) 2 ], 2H 2 O} n X [5] :, Ξ E2mail : com cn Received November 5, 2003 ; revised February 2, 2004 ; accepted March 22, 2004 (No ) (No )

2 No 14 : Zn( ) , :, P2 (1) / n Finnigan EA 1112 C, H, a = (3) nm, b = (3) nm, c = (7) nm, = (5), V = (10) nm 3, Z = 4, D c = Mg/ m 3, = mm - 1, F(000) = 912, R 1 = , wr 2 = , e/ nm 3 2 N ; Nicolet470 ( KBr ) 2 1 ; Bruker Smart CCD X, mmol 20 ml 012 mmol phen N C 1503 cm cm - 1, Zn 2 + COO, 20 ml, 011 mmol as (COO - ) 1595 cm - 1 s (COO - ) 1383 cm - 1 as s 20 ml,, ph 012 mol/ L KOH ph 7126, 5 h ph 7108, 200 cm - 1,, 25 ml, 200 cm - 1, 212 cm - 1, ( ),,30 d X IR : 3404 (s), 1612 (s), 1595 (s), 1518 (s), 1493 (m), 1449 (s), 1383 (s), 1224 (m), 1147 (m), 1086 (m), ( s), 759 ( s) cm - 1 Anal calcd for C 20 H 16 N 2 O 6 Zn : C 1, 53189, N 6128, H 3162 ; found C 53180, N 6119, H mm 0116 mm 0114 mm, Bruker 2 1,, Smart CCD X, Mo K,Zn(1A) N(1A) Zn (1A) N (2A) : ( = nm), , nm, Zn (1A) O (1A), Zn (1A) O (5A) / 2, (293 K) Zn(1A) O (4B) : , , 3786, nm, Zn O Zn N,N(2A),O(4B) O (5A) 1 Figure 1 Molecular structure of complex

3 1364 Vol 62, ( 10 4 ) ( 10 5 nm) Table 1 Nonhydrogen fractional atomic coordinates ( 10 4 ) and equivalent isotropic temperature factors ( 10 5 nm) of complex Atom x y z U eq Atom x y z U eq Zn(1) 8059(1) 3913(1) 6617(1) 29 (1) C(13) 4542 (3) 4107 (3) 7658(1) 27 (1) N(1) 8654(3) 5501(3) 5923(3) 29 (1) C(14) 4403 (3) 5113 (3) 8149(1) 26 (1) N(2) 6796(3) 3278(3) 5816(1) 33 (1) C(15) 3171 (3) 5128 (4) 8483(2) 35 (1) C(1) 9589(4) 6574(4) 5978(2) 38 (1) C(16) 2102 (3) 4164 (4) 8328(2) 41 (1) C(2) 9992(4) 7459(4) 5478(2) 46 (1) C(17) 2248 (4) 3164 (4) 7840(2) 46 (1) C(3) 9415(4) 7217(4) 4903(2) 46 (1) C(18) 3467 (4) 3138 (4) 7508(2) 39 (1) C(4) 8400(4) 6112(4) 4825(1) 38 (1) C(19) 5812 (3) 4147 (4) 7261(1) 30 (1) C(5) 7729(4) 5775(4) 4236(2) 48 (1) C(20) 5613 (3) 6086 (4) 8335(1) 28 (1) C(6) 6733(4) 4724(4) 4194(2) 48 (1) O(1) 6582 (2) 2995 (2) 7235(1) 37 (1) C(7) 6357(4) 3857(4) 4724(2) 40 (1) O(2) 6084 (2) 5295 (3) 6961(1) 41 (1) C(8) 5327(4) 2735(4) 4713(2) 50 (1) O(3) 6749 (2) 5493 (3) 8431(1) 48 (1) C(9) 5071(4) 1939(4) 5241(2) 51 (1) O(4) 5360 (2) 7475 (2) 8385(1) 35 (1) C(10) 5839(4) 2219(4) 5786(2) 44 (1) O(5) 9123 (2) 5144 (2) 7313(1) 37 (1) C(11) 7036(3) 4107(4) 5298(1) 32 (1) O(6) 6227 (2) 8348 (3) 6614(1) 45 (1) C(12) 8056(3) 5268(4) 5351(1) 30 (1) 2 (nm) ( ) Table 2 Selected bond distances (nm) and angles ( ) of complex Zn(1) O(4) (2) O(4) # 1 Zn(1) O(5) (9) Zn(1) O(5) (2) O(4) # 1 Zn(1) O(1) (9) Zn(1) O(1) (2) O(5) Zn(1) O(1) (9) Zn(1) N(1) (3) O(4) # 1 Zn(1) N(1) (9) Zn(1) N(2) (3) O(1) Zn(1) N(1) (9) C(19) O(1) (3) O(4) # 1 Zn(1) N(2) (10) C(19) O(2) (3) O(5) Zn(1) N(2) (9) O(1) Zn(1) N(2) (10) N(1) Zn(1) N(2) (10) O(2) C(19) C(13) (3) C(19) O(1) Zn(1) (19) O(2) C(19) O(1) (3) Symmetry code : # 1 - x + 3/ 2, y - 1/ 2, - z + 3/ 2,N(1A) O (1A),,N(1A) Zn (1A) O (1A) (9), 180, N (2A), O (4B) O(5A) [ N ( 2A) Zn ( 1A) O ( 5A) (9), O(4B) Zn(1A) O(5A) (9), N(2A) Zn (1A) O(4B) (10) ] , , N(2A), O(4B) O (5A),,, [9 14] [9] [10] [11],, [ Co (phth) 2 (bipy) ] [11],, 2 Zn, [ 100 ] Figure 2 12D chain structure of complex ( 2)

No 14 : Zn( ) 1365, 0 44 nm 0 61 nm,,,x ac 3 : Zn 2 +, ( 4) phen, phth 5, 013355 nm, [15], 2 3 {[Zn 2 (phen) 2 (phth) 2 (H 2 O) 2 ] 2H 2 O} n 3 ac

Int Ed 2000, 39, 3052 2 Hagrman, P J ; Hagrman, D ; Zubieta, J Angew Chem, Int Ed 1999, 38, 2639 3 Batten, S R ; Robson, R Angew Chem, Int Ed 1998,

4 No 14 : Zn( ) 1365, 0 44 nm 0 61 nm,,,x ac 3 : Zn 2 +, ( 4) phen, phth 5, nm, [15], 2 3 {[Zn 2 (phen) 2 (phth) 2 (H 2 O) 2 ] 2H 2 O} n 3 ac Figure 3 Projection of tubular channel formed by helical chain in ac plane 4 Figure 4 22D network of complex References 1 Zaworotko, M J Angew Chem, Int Ed 2000, 39, Hagrman, P J ; Hagrman, D ; Zubieta, J Angew Chem, Int Ed 1999, 38, Batten, S R ; Robson, R Angew Chem, Int Ed 1998, 37, Evans, O R ; Lin, W Acc Chem Res 2002, 35, Wang, K Bioinorganic Chemistry, Tsinghua University Press, Beijing, 1988, pp (in Chinese)

5 1366 Vol 62, 2004 (,,,, 1998, pp ) 6 Blondin, G ; Girerd, J J Chem Rev 1990, 90, Tahir, M M ; Karlim, K D J Am Chem Soc 1992, 114, Deacon, G B ; Phillips, R J Coord Chem Rev 1980, 33, Baca, S G ; Simonov, Y A ; Gdaniec, M ; Gerbeleu, N ; Filippova, I G ; Timco, G A Inorg Chem Commun 2003, 6, Brechin, E K ; Graham, A ; Parkin, A ; Parson, S ; Seddon, A M ; Winpenny, R E P J Chem Soc, Dalton Trans 2000, Lightfoot, P ; Snedden, A J Chem Soc, Dalton Trans 1999, Yao, J C ; Huang, W ; Li, B ; Gou, S ; Xu, Y Inorg Chem Commun 2002, 5, Ma, C ; Wang, W ; Zhu, H ; Chen, C ; Liu, Q Inorg Chem Commun 2001, 4, Chen, C ; Zhu, H ; Huang, D ; Wen, T ; Liu, Q ; Liao, D ; Cui, J Inorg Chim Acta 2001, 320, Janiak, C J Chem Soc, Dalton Trans 2000, 3885 (A SONG, J P ; LING, J )

Graphical Abstract Vol 62, 2004 Synthesis of Hydrothermally Stable Mesoporous Aluminosilicates with Tubular Morphology from MFI Zeolitic Precursors and Sodium Silicates ZHENG, Jun2Lin ; ZHANG, Ye ;

co2assembly of sodium silicates, sodium aluminates and MFI aluminosilicate precursors Coassembling with soluble silica species, protozeolitic nanoclusters serving as one part of precursors enhanced

6 Graphical Abstract Vol 62, 2004 Synthesis of Hydrothermally Stable Mesoporous Aluminosilicates with Tubular Morphology from MFI Zeolitic Precursors and Sodium Silicates ZHENG, Jun2Lin ; ZHANG, Ye ; WU, Dong ; SUN, Yu2Han Acta Chimica Sinica 2004, 62 (14), 1357 Hydrothermally stable mesoporous aluminosilicates with hollow tubular morphology and hexagonal nanochannels were prepared through co2assembly of sodium silicates, sodium aluminates and MFI aluminosilicate precursors Coassembling with soluble silica species, protozeolitic nanoclusters serving as one part of precursors enhanced the hydrothermal stability Synthesis and Crystal Structure of Supra2 molecular Complex of Phthalate Zn( ) Bridged by SUN, Ya2Guang ; WEI, De2Zhou ; GAO, En2 Jun ; DING, Fu Acta Chimica Sinica 2004, 62 (14), 1362 Novel supramolecular complex {[Zn 2 (phen) 2 (phth) 2 (H 2 O) 2 ] 2H 2 O} n (phen = phenanthroline ; phth = phthalate) has been synthesized by the reaction of phen and phth with zinc( ) salt The zinc atom rendered five2coordinate in a distorted trigonal bipyramidal configuration The complex formed 12D helix chain bridged by phth and 22D network structure by 2 action of neighbouring helix chain Chemical Modification of Carbon Nanotubes and Tribological Properties as Lubricant Additive CHEN, Chuan2Sheng ; CHEN, Xiao2Hua ; LIU, Tian2Gui ; YANG, Dong ; ZHANG, Gang ; YI, Guo2Jun Acta Chimica Sinica 2004, 62 (14), 1367 After CNTs were modified with stearic acid, the peaks at about 3752, 1723 and 1543 cm - 1 (Fig a) corresponding to carbonyl groups, oxygen2hydrogen bonds and C C bonds, respectively, disappeared, and two new peaks at about 2924 and 2866 cm - 1 were observed, attributed to cymene group ( Fig b) The results showed that the CNTs were coated with stearic acid by chemical reaction Executive editor PAN, Bing2Feng ; computer typesetter DONG, Hua2Zhen

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