Three new compounds of dibutyltin(IV) with N-alkylcyclohexyldithiocarbamate were successfully synthesized using in situ methods. Elemental analysis data of these complexes were in agreement with the general formula of (C4H9)2Sn[S2CNR(C6H11)]2 (R = CH3, C2H5, i-C3H7). Infrared spectra showed that the thioureide bands, ν(C=N) appeared
in the region of 1475 - 1479 cm-1, ν(C=S) bands in the region of 978 - 998 cm-1 and ν(Sn-S) bands in the region of 375 – 389 cm-1. Crystal structure of dibutyltin(IV) ethylcyclohexyldithiocarbamate showed a triclinic system and space group P-1. The crystal structure of the dithiocarbamate ligands were bidentically chelated to the tin atom with Sn-S unsymmetrical: Sn(1)-S(1) = 2.9255(11) and Sn(1)-S(2) = 2.5419(10); Sn(1)-S(3) = 2.8922(9) and Sn(1)-S(4) = 2.5293(10)Å. These compounds were screened for antibacterial activity against four bacteria species using the disc diffusion method. The results showed that (C4H9)
2Sn[S2CN(i-C3H7)(C6H11)]2 was mildly active against those three bacteria. Whereas all of
these compounds exhibited in vitro cytotoxicity activity toward human leukemic promyelocites HL-60 cell line with CD50 values lower than 1.00 µg/mL.
Tujuh kompleks praseodimium (Pr) ditiokarbamat 1,10-fenantrolin baru telah berjaya disintesis menggunakan kaedah in-situ hasil daripada tindak balas lapan jenis amina dengan garam praseodimium(III) bersama dengan karbon disulfida. Kaedah metatesis dan kondensasi merupakan kaedah yang paling berjaya telah menghasilkan praseodimium ditiokarbamat 1,10 fenantrolin dengan formula umum Pr[S2CNR1R2]3phen (R1 = etil dan metil; R2 = butil, heptil, isopropil, isobutil, benzil dan sikloheksil; phen= 1,10-fenantrolin). Kesemua kompleks telah dicirikan menggunakan kaedah analisis unsur, inframerah, termogravimetri dan konduktiviti. Analisis unsur telah menunjukkan kesemua kompleks bersetuju dengan formula umum yang dicadangkan. Spektrum inframerah (FTIR) menunjukkan jalur tioureda v(C-N) terletak dalam kawasan julat 1454 – 1484 cm-1 dan jalur ν(C-H) pula terletak dalam kawasan 2853-2973 cm-1. Jalur v(C-S) yang wujud secara tunggal dalam kawasan 959 – 999 cm-1 mengesahkan ia berikatan secara bidentat. Data spektroskopi NMR 13C moeti NCS2 untuk kesemua kompleks terletak dalam julat 192 – 212 ppm. Struktur hablur tunggal Pr[S2CN(CH3)(C7H7)]3phen mempunyai sistem hablur triklinik (kumpulan ruang Pī) dan geometri dodekahedron dengan a = 10.7165(16) Å , b = 12.2897(19) Å, c = 16.586(2) Å, α = 73.887(2)o; β = 74.879(2)o dan γ = 71.837(2)o and Z = 2. Tiga ditiokarbamat dan satu ligan fenantrolin telah berkoordinat kepada atom Pr di pusat secara bidentat.
Organotin compounds especially the dialkyltin derivatives are reported to possess anti-tumour properties. The diorganotin(IV) complexes of the type Me2SnL1, Me2SnL2, Bu2SnL1, Bu2SnL2 and Ph2SnL1 (L1 and L2 is the anion of the thiosemicarbazone ligand formed by the condensation reaction of 2,3-dihydroxybenzaldehyde with thiosemicarbazide or its N(4)-methyl substituent) were synthesized using 1:1 metal-to-ligand reactant ratios. The newly synthesized complexes were characterized using elemental analysis, infrared and nuclear magnetic resonance (1H, 13C, 119Sn) spectroscopic techniques. Complex formation between the organotin(IV) moiety and the anions of 2,3-dihydroxybenzaldehyde thiosemicarbazone and 2,3-dihydroxybenzaldehyde 4-methylthiosemicarbazone occurred with chelation at the o-dihydroxy positions. The complexes are proposed to have tetrahedral geometry.
A new series of lanthanum dialkyldithiocarbamate complexes with 1,10-phenantroline were successfully synthesized using in situ methods. These complexes were characterized using elemental analysis, infrared, thermogravimetric analysis and conductivity. Microelemental analysis data were in agreement with the general formula La(S2CNR’R”)3phen (R’ = ethyl, methyl; R” = butyl, heptyl, isopropyl, isobutyl, benzyl and cyclohexyl; phen = 1,10-phenantroline). Infrared spectra of complexes showed the thioureide n(C-N) bands were in the region of 1450 - 1482 cm-1. The single n(C-S) bands appeared in the region of 959 – 997 cm-1 and n(C-H) bands in the region of 2918-2955 cm-1. The crystal structure of tris(N,N-ethylbenzyldithiocarbamate)(1,10-phenantroline)lantanum(III) adopts an orthorombic system (space group Pccn) with a distorted dodecahedron geometry with a = 19.865(5) Å , b = 42.803(10) Å, c = 10.657(3) Å, a = b = g = 90o and Z = 9. Three dithiocarbamates and one phenanthroline ligands were coordinated to the central La atom in bidentate manner.
Organostannum(IV) complexes derived from dicarboxylic acids have been successfully synthesised from triphenylstannum(IV) hydroxide (Ph3SnOH). The complexes were obtained by refluxing Ph3SnOH and the respective dicarboxylic acids (malonic, succinic, glutaric and adipic acids) using a Dean and Stark apparatus in the appropriate solvent. The free ligands and complexes were characterised by C, Hand Sn elemental analysis and spectroscopic methods such as infrared and nuclear magnetic resonance (1H, 13C NMR). Structure determination of triphenylstannum(IV) succinate, 2, showed that each dicarboxylate anion was bonded monodentatically to two triphenylstannum(IV) moieties. The geometry surrounding each stannum atom is close to a tetrahedron. Spectroscopic data obtained for all complexes were found to be similar and thus it may be concluded that all complexes have the same structure as 2.
New organotin(IV) sec-butylpropyldithiocarbamate complexes have been sucÂcessfully 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( sÂC4H9)(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) Ã…; 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) sekÂbufilpropilditiokarbamat telah berjaya dihablurkan menggunakan pelarut kloroform. Kajian kristalograji sinar-X menunjukkan hablur Me2Sn[s-ÂC4H9)(C5H7)]2 bersistem monoklinik dengan kumpulan ruang P21/n, a = 14.358(2), b = 10.6956(18), c = 17.323(3) Ã…; 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.
A new series of gadolinium complexes with mixed ligands, dialkyl dithiocarbamate and 1,10-Phenantroline were successfully synthesized using “in situ” methods. Microelemental analysis data of complexes are in agreement with the general formula Gd[S2CNR’R”]3Phen (R’ = ethyl, methyl; R” = butyl, heptyl, isopropyl, isobutyl, benzyl and cyclohexyl; Phen = 1,10-phenantroline). These complexes have been characterized using elemental analysis, infrared, thermogravimetric analysis, conductivity and magnetic measurements. Infrared spectra of complexes showed the thioureide n(C-N) bands were in the region of 1450 - 1490 cm-1. The single n(C-S) bands appeared in the region of 959 – 1003 cm-1 and n(C-H) bands in the region of 2853-2931 cm-1. The crystal structure of tris(N,N-methylbenzyldithiocarbamate)(1,10-phenantroline) gadolinium(III) adopts a triclinic system (space group Pī) with a distorted dodecahedron geometry with a = 11.04(6) Å , b = 12.65(7) Å, c = 17.13(10) Å, a =73.86o(8) b =74.54o(8) g = 72.34o(8) and Z = 2. Three dithiocarbamates and one phenanthroline ligands were coordinated to the central Gd atom in bidentate manner.
Several triphenylphosphinosilver (I) complexes, viz. bis [acetatotriphenylphosphineargentum (I)], I, lactatotris (triphenylphosphine) argentum (I), II, N, N-diethanoldithiocarbamatobis (triphenylphosphine) silver (I), III, and NÂethanol, N-methyldithiocarbamatobis (triphenylphosphine) silver (I), IV, have been prepared. Apart from characterization by spectroscopic methods, the structures of I-III, have been characterised by single-crystal x-ray diffraction methods. I crystallized as a dimer with a 4-coordinate geometry around the silver atom, while the lactate complex is a monomer with a five-coordinate silver atom. In the four-coordinate complex III, the Ag - S bond distances are 2.6822 (13) and 2.5991 (12) Ã… indicating different modes of bonding to the dithiocarbamate ligands.
Beberapa kompleks trifenilfosfinoargentum telah disintesis, iaitu bis [asetatotrifenilfosfinargentum (I)], I, laktatotris (trifenilfosfin) argentum (I), II dietanolditiokarbamatobis (trifenilfosfin) argentum (I), III dan metiletanolditiokarbamatobis (trifenilfosfin) argentum (I), IV. Selain daripada pencirian dengan kaedqh spektroskopi, struktur kompleks I-III telah ditentukan dengan kaedah pembelauan sinar-X hablur tunggal. Kompleks asetat terhablur sebagai dimer dengan argentum menunjukkan geomertri 4-koordinat, sementara kompleks laktat adalah monomer dengan argentum berkoordinatan lima. Dalam kompleks dietanolditiokarbamat argentum berkoordinatan empat dengan panjang ikatan Ag - S, 2.6822 (13) dan 2.5991 (12) Ã… menunjukkan dua mod pengikatan yang berbeza dengan ditiokarbamat.
Two adducts of bis(N-benzyl-N-isopropyldithiocarbamato) zinc(II) with 2,2'Â-bipyridine and 1,10-phenanthroline have been successfully synthesized and characterized by elemental analysis and spectroscopic studies. The IR specÂtra of these adducts showed the thioureide band, v(C---- N) which occurred at 1440 and 1438 cm-1 respectively, lower than the parent compound at 1471 cm-1. The 13C NMR spectroscopic data for these compounds showed that the carbon signal from CS2 moiety shifted slightly downfield to 206.6 and 208.5 ppm compared to the parent compound at 205.1 ppm. The single crystal structure of bis (N-benzyl-N-isopropyldithiocarbamato )zinc(II)(bipy) has been determined. The structure of this compound showed monomeric nature with hexacoordination of the metal in a highly distorted octahedral geometry.
Dua sebatian aduk zink(II) benzilisopropilditiokarbamat dengan ligan 2,2-bipiridil dan 1,10-fenantrolin telah berjaya disediakan dan dianalisis menggunakan analisis unsur dan kaedah spektroskopi. Spektrum IR untuk kedua-dua sebatian aduk ini telah menunjukkan kehadiran jalur tioureida, V(C----- N) pada 1440 dan 1438 cm-1 masing-masing yang mana jalur serapan ini didapati teranjak pada nilai yang lebih rendah berbanding sebatian asalnya iaitu pada 1471 cm-1. Data RMN 13C pula menunjukkan kehadiran signal karbon CS2 yang teranjak sedikit ke medan yang lebih rendah iaitu pada 206.6 dan 208.5 ppm masing-masing jika dibandingkan dengan sebatian asalnya pada 205.1 ppm. Struktur hablur tunggal bagi sebatian bis( N-benzilÂ-N-isopropilditiokarbamat)zink(11)(bipy) telah ditentukan. Struktur sebatian ini didapati bersifat monomerik dan berkoordinat enam dengan atom logam pusatnya mempunyai geometri oktahedron yang sangat terherot.