C 66 H 97 N 8 O 41.50 Zn 3 ,monoclinic, P12 1 /c1(no. 14), a =12.762(2) Å, b =18.957(2) Å, c =18.057(2) Å, b =90.05°, V =4368.7 Å 3 , Z =2,Rgt(F) =0.064, wR ref (F 2 ) =0.223, T =298 K.
Source of materialAmixture of benzene-1,3,5-tricarboxylic acid (BTC, 0.022 g, 0.1 mmol), Zn(CH 3COO)2 (0.018 g, 0.1 mmol), 2,2'-bipy (0.016 g, 0.1 mmol), NaOH (0.2 M, 1.5 mL) and H 2O( 10 mL) was stirred for about 30 min. The resulting solution was sealed in aTeflonlined stainless autoclave and heated to 393 Kfor 3days. The bottle was cooled to ambient temperature spontaneously. Colourless single crystals (about 71% yield, based on Zn input) were separated by vacuum filtration and drying in air. Elemental analysis -found: C, 42.76 %; H, 5.16 %; N, 6.13 %; calulated for C 66H97N8O41.50Zn3:C ,42.55 %; H, 5.22 %; N, 6.01 %.
Experimental detailsThe C-bound Ha toms were geometrically placed (d(C-H) = 0.93 Å)and refined as riding with U iso(H) =1.2 Ueq(C). The Obound Ha toms were located in difference maps and refined as riding in their as-found relative positions with U iso (H) =1 .2 U eq (O). The high residual-values are caused by the quality of the crystal. The lattice water molecules (O20, O21, O22, O23 and O24) are disordered. The water Hatoms were not located.
DiscussionMetal-containing hydrogen-bonded networks have the advantage of tenability owing to the intrinsic flexibility of hydrogen bonds, and give access to physical properties that are less common in organic solids [1][2][3][4]. Nevertheless, how to control hydrogenbonding interactions toward formation of ordered solid remains to be ac hallenging subject. 1,3,5-Benzenetricarboxylic acid (BTC) is agood ligand for the construction of supramolecular architectures [5][6][7][8][9][10][11][12], because the multicarboxylate groups of the molecule may be completely or partially deprotonated, and these anions may act as bridging ligands in various coordination modes.The title compound has adiscrete crystal structure based on Zn ions, phen ligands and BTC ligands. The asymmetrical unit contains two Zn atoms. The Zn1 center has distorted octahedral coordination with four nitrogen atoms from two cis-positioned phen ligands and two water molecules. The Zn2 is located on acrystallographic inversion center, and coordinates to six terminal coordinated water molecules. The Zn-Od istances range from 2.008(3) to 2.147(3) Å,and the Zn-Ndistances are in the range 2.123(4) -2 .186(4) Å.T he bond angles around the zinc center range from 77.22 (2) 2+ are contained in the 2D hydrogen bonded host framework, and encapsulated in the 1D channels along [100] being hydrogen-bonded to the carboxylate oxygen atoms of BTC and forming a3Dextended framework.