Sintesis dan Pencirian Kompleks Organostanum(Iv) sek-Butilpropilditiokarbamat: Struktur Hablur Bis(N, N-­sek –butilpropilditiokarbamato) dimetilstanum(IV)

New organotin(IV) sec-butylpropyldithiocarbamate complexes have been suc­cessfully synthesized by the reaction between N-sec-butyl-N-propylamine, carbon disulfide and organotin(IV) chloride (dimethyltin(IV), dibutyltin(IV) and triphenyltin(lV) chloride) using in-situ method. All the complexes have been characterized using elemental analysis, gravimetric analysis, infrared and NMR (1H and I3C) spectroscopy. Elemental and gravimetric analyses showed that the complexes agree with the suggested formulae, R2Sn[S2CN( s­C4H9)(C3H7)]2 dan R‘3Sn[S2CN(s-C4H9)(C3H7)] (R = CH3 or R = C4H9; R' = C6H5 The presence of the v(C = N) and v(C = S) bands in the infrared spectra confirmed the presence of dithiocarbamate ligand in that complex. The 13C NMR spectra for all the complexes showed a resonance in the region 196.22 - 200.62 ppm, which is attributed to the carbon atom of NCS2 group. The dimethyltin(lV) sec-butylpropyldithiocarbamate, Me2Sn(SBPDtc)2 was recrystallized from CHCl3 and the structure had been determined using X-ray crystallography analysis. The structure of Me2Sn[s-C4H9)(C3H7)]2 is found to be in the monoclinic system with space group P21/n, a = 14.358(2), b = 10.6956(18), c = 17.323(3) Å; α = 90°, β = 99.765(4)°, γ = 90°. The complex is six-coordinated with the tin atom bonded by two dimethyl groups in cis positions and two chelating sec-butylpropyldithiocarbamates in bidentate mode.
Kompleks baru organostanum(IV) sek-butilpropilditiokarbamat telah berjaya disediakan melalui tindak balas di antara N-sek-butil-N-propilamina, karbon disulfida dan sebatian dimetilstanum(lv), dibutilstanum(IV) dan trifenilstanum(IV) klorida menggunakan kaedah in-situ. Kesemua kompleks telah dicirikan menggunakan analisis unsur, analisis gravimetri, spektroskopi inframerah dan spektroskopi resonans magnet nukleus 1H dan 13C. Analisis unsur (CHNS) dan gravimetri menunjukkan sebatian yang disintesis bersetuju dengan formula yang dicadangkan, iaitu R2Sn[S2CN(s-C4H9)(C3H7)]2 dan R'3Sn[S2CN(s-C4H9)(C3H7] (R = CH3 atau C4H9; R' = C6H5). Kehadiran jalur serapan v(C ---- N) dan v(C ---- S) pada spektrum inframerah menunjukkan kehadiran ligan ditiokarbamat dalam sebatian yang disediakan. Spektrum RMN I3C bagi ketiga-tiga kompleks menunjukkan resonan N13CS2 terletak pada julat 196.22- 200.61 ppm. Kompleks dimetilstanum(1V) sek­bufilpropilditiokarbamat telah berjaya dihablurkan menggunakan pelarut kloroform. Kajian kristalograji sinar-X menunjukkan hablur Me2Sn[s-­C4H9)(C5H7)]2 bersistem monoklinik dengan kumpulan ruang P21/n, a = 14.358(2), b = 10.6956(18), c = 17.323(3) Å; α = 90°, β= 99.765(4)°, γ = 90°. Kompleks membentuk geometri enam koordinat dengan atom pusat stanum yang berikat dengan dua kumpulan metil pada kedudukan sis dan mengkelat secara bidentat dengan ligan sek-butil propilditiokarbamat.