The reaction of Ag2SO4 and bpp (bpp = 1,3-bis(4-pyridyl)propane) in H 2 O afforded the complex [Ag2(bpp)2(SO4) · 6.5H 2 O · CH 3 OH] n , 1. The IR and TGA have been recorded and the structure has been determined. Crystal data for 1: Space group C 2/c, a = 17.885(4), b = 25.230(6), c = 8.832(2) Å, b = 105.437(4)°. V = 3841(1) Å 3 , Z = 8 with final residuals R1 = 0.0710 and wR2 = 0.1620. The complex shows a three-dimensional supramoleclar structure constructed with two-dimensional infinite [Ag2(bpp)2]n sheetlike layers pillared by Ag-Ag interactions and Ag····O (SO4) interactions in the solid state.
EXPERIMENTAL SECTION
General ProceduresAll chemicals were commercially available and used as received. The IR spectra were recorded on a Jasco FT/IR-460 Plus spectrometer. Elemental analyses were obtained from a PE 2400 series II CHNS/O analyzer. Thermogravimetric analyses (TGA) were conducted on a SDT 2960 using a heating rate of 20°C/min in a nitrogen atmosphere.
Starting MaterialThe reagent Ag 2 SO 4 and bpp (bpp = 1,3-bis(4-pyridyl)propane) were purchased from Aldrich Chemical Co. and used as receivied.
Preparation of [Ag 2 (bpp) 2 (SO 4 ) · 6.5H 2 O · CH 3 OH] nAg 2 SO 4 (0.31 g, 1 mmol) and bpp (0.40 g, 2 mmol) were placed in a flask containing 10 mL H 2O. The mixture was stirred at room temp. for 0.5 hr to yield a white precipitate. The white solid was then filtered off and washed with CH 3OH. Yield for 1: 0.48 g (56%). Anal. Calcd. for C 27H45N4SO11.5Ag2 C, 37.78; H, 5.25; N, 6.53%. Found: C, 37.72; H, 5.13; N, 6.40%. IR (KBr disk): 3052 (br), 2938 (m), 2869 (m), 2503 (m), 1620 (m), 1486 (m), 1432 (m), 1378 (m), 1281 (m), 1227 (m), 1066 (m), 1012 (m), 807 (m), 743 (m), 614 (m), 576 (s), 517 (m). Colorless crystals suitable for X-ray crystallography were obtained by bpp in CH 3OH layered onto a solution of Ag 2SO4 in H2O over 3 days.
X-RAY CRYSTALLOGRAPHYColorless crystals suitable for X-ray crystallography were obtained by bpp in CH 3OH layered onto a solution of Ag2SO4