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

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2004 62 14, 1362 1366 ACTA CHIMICA SINICA Vol 62, 2004 No 14, 1362 1366 Zn( ) a, b a Ξ, b c Ξ ( a 110004) ( b 110142) ( c 110036) 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 = 019643 (3) nm, b = 018976 (3) nm, c = 211410 (7) nm, = 901776 (5), Z = 4, V = 118531 (10) nm 3, D c = 11598 g/ cm 3, = 11367 mm - 1, F(000) = 912, R 1 = 010409, wr 2 = 010818,,, 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 110004) ( b Laboratory of Coordination Chemistry, Shenyang Institute of Chemical Technology, Shenyang 110142) ( c Institute of Chemical Science and Engineering, Liaoning University, Shenyang 110036) 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 = 019643 (3) nm, b = 018976 (3) nm, c = 211410 (7) nm, = 901776 (5), Z = 4, V = 118531 (10) nm 3, D c = 11598 g/ cm 3, = 11367 mm - 1, F (000) = 912, R 1 = 010409, wr 2 = 010818, 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 : ejgao @yahoo com cn Received November 5, 2003 ; revised February 2, 2004 ; accepted March 22, 2004 (No 20022018) (No 200301)

No 14 : Zn( ) 1363 2, :, P2 (1) / n 1 1 1 Finnigan EA 1112 C, H, a = 019643 (3) nm, b = 018976 (3) nm, c = 211410 (7) nm, = 901776 (5), V = 118531 (10) nm 3, Z = 4, D c = 11598 Mg/ m 3, = 11367 mm - 1, F(000) = 912, R 1 = 010409, wr 2 = 010818, 851-320 e/ nm 3 2 N ; Nicolet470 ( KBr ) 2 1 ; Bruker Smart CCD X, 1 2 011 mmol 20 ml 012 mmol phen N C 1503 cm - 1 1422 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), 2 2 851 ( 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 3154 1 3 0120 mm 0116 mm 0114 mm, Bruker 2 1,, Smart CCD X, Mo K,Zn(1A) N(1A) Zn (1A) N (2A) : ( = 01071073 nm), 2130 26138, 012143 012166 nm, Zn (1A) O (1A), Zn (1A) O (5A) / 2, (293 K) 10385 Zn(1A) O (4B) : 012124, 012110 011997, 3786, nm, Zn O Zn N,N(2A),O(4B) O (5A) 1 Figure 1 Molecular structure of complex

1364 Vol 62, 2004 1 ( 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) 0 1997(2) O(4) # 1 Zn(1) O(5) 88 65 (9) Zn(1) O(5) 0 2110(2) O(4) # 1 Zn(1) O(1) 105 61 (9) Zn(1) O(1) 0 2124(2) O(5) Zn(1) O(1) 95 02 (9) Zn(1) N(1) 0 2143(3) O(4) # 1 Zn(1) N(1) 102 51 (9) Zn(1) N(2) 0 2166(3) O(1) Zn(1) N(1) 151 43 (9) C(19) O(1) 0 1275(3) O(4) # 1 Zn(1) N(2) 104 42 (10) C(19) O(2) 0 1244(3) O(5) Zn(1) N(2) 163 66 (9) O(1) Zn(1) N(2) 90 91 (10) N(1) Zn(1) N(2) 77 24 (10) O(2) C(19) C(13) 119 0 (3) C(19) O(1) Zn(1) 96 19 (19) O(2) C(19) O(1) 121 5 (3) Symmetry code : # 1 - x + 3/ 2, y - 1/ 2, - z + 3/ 2,N(1A) O (1A),,N(1A) Zn (1A) O (1A) 151143 (9), 180, N (2A), O (4B) O(5A) [ N ( 2A) Zn ( 1A) O ( 5A) 163166 (9), O(4B) Zn(1A) O(5A) 88165 (9), N(2A) Zn (1A) O(4B) 104142 (10) ] 356173, 360 3127, 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 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, 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, 37, 1461 4 Evans, O R ; Lin, W Acc Chem Res 2002, 35, 511 5 Wang, K Bioinorganic Chemistry, Tsinghua University Press, Beijing, 1988, pp 144 146 (in Chinese)

1366 Vol 62, 2004 (,,,, 1998, pp 144 146 ) 6 Blondin, G ; Girerd, J J Chem Rev 1990, 90, 1359 7 Tahir, M M ; Karlim, K D J Am Chem Soc 1992, 114, 7659 8 Deacon, G B ; Phillips, R J Coord Chem Rev 1980, 33, 227 9 Baca, S G ; Simonov, Y A ; Gdaniec, M ; Gerbeleu, N ; Filippova, I G ; Timco, G A Inorg Chem Commun 2003, 6, 685 10 Brechin, E K ; Graham, A ; Parkin, A ; Parson, S ; Seddon, A M ; Winpenny, R E P J Chem Soc, Dalton Trans 2000, 3242 11 Lightfoot, P ; Snedden, A J Chem Soc, Dalton Trans 1999, 3549 12 Yao, J C ; Huang, W ; Li, B ; Gou, S ; Xu, Y Inorg Chem Commun 2002, 5, 711 13 Ma, C ; Wang, W ; Zhu, H ; Chen, C ; Liu, Q Inorg Chem Commun 2001, 4, 730 14 Chen, C ; Zhu, H ; Huang, D ; Wen, T ; Liu, Q ; Liao, D ; Cui, J Inorg Chim Acta 2001, 320, 159 15 Janiak, C J Chem Soc, Dalton Trans 2000, 3885 (A0311052 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 ; 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