Subhi Al-Jibori

Tikrit University · Department of Chemistry

In the current work, we report the synthesis and characterization of new dithiocarbamate complexes derived from 1,2-benzoisothiazol-3(2H)-one (BitH). The ligand was synthesized by treating the BitH with carbon disulfide in a basic solution. The NMR technique confirmed the preparation of the ligand. The treatment of the Bit-dtcNa with the metal salt...

One pot reaction of K2MCl4 with two equivalents of 2,5-dimercapto-1,3,4-thiadiazole (dmtzsH2) and one equivalent of 1,2-bis(diphenylphosphino)ethane (dppe) in MeOH/CH2Cl2 mixed solvents resulted in the formation of [M(dmtzsH)2(dppe)], M = Pd 1 or Pt 2 in 49 and 77% yield respectively. The same products were obtained in 54 and 80% yield on using two...

Ten mixed‐ligand phenyl mercury(II) complexes containing 1‐methyl‐1H‐tetrazole‐5‐thiol (HmtzS) (1) and phosphine or amine ligands. These complexes fall into two groups: [PhHg(mtzS){Ph2P(CH2)PPh2}]2 (2) and [PhHg(mtzS){Ph2P(CH2)nPPh2}] (3‐6), where n varies, and [PhHg(mtzS)(diamine)] (8‐10), with diamine choices being 2,2′‐bipyridyl (Bipy, 8), 1,10‐...

A silver complex was prepared with benzisothiazolinone ligand, which was used to prepare new phosphorus‐rich complexes with dppe and dppp. All complexes were diagnosed by FTIR, ¹H‐NMR, ³¹P‐NMR, CHN, and molar conductivity. The results proved that phosphines were labile, therefore ³¹P‐NMR was measured by cryoprotection at different temperatures. As...

Preparation of series of new Mercury (II) mixed ligand complexes of benzotriazol dithiocarbamate (DTC) [Hg(DTC)2] and phosphine or amine ligands of the type [Hg(DTC)2(diphosphine)] (2–5), [(Hg(DTC)2(diamine)](6,7), [Hg(DTC)2(SPPh3)2] (8) and [Hg(DTC)2(PPh3)2] (9) has been done. This preparation has yielded good amount of these complexes. These comp...

The reaction between [PtCl 2 (L-L)] (L-L = dppe, dppp, dppb, dppf, Phen and Bipy) or [PtCl 2 (PPh 3) 2 ] with 1-benzyl-3-phenylthiourea (H 2 BPT) in a basic medium (CHCl 3 /EtOH) created new coordinated square planner Pt(II) complexes with [Pt(BPT)(L-L)] (1-4,6,7) and [Pt(BPT)(PPh 3) 2 ] (5) types. These complexes were fully characterized by analyt...

This article reports a cheap and high yield (85%) route for synthesis of 3H-1,2-benzodithiol- 3-thione (btt). Treatment of benzisothiazolinone (Hbit) with P4S10 yielded a mixture of two products which are (btt) and thiobenzisothiazolinone (Htbit). This mixture was charac- terized and confirmed using FT-IR, 1H-,13C- NMR, (COSY, HSQC)-2D-NMR and GC-M...

A series of Pd(II) complexes containing ortho-cyano-aminothiophenolate (ocap) ligands have been prepared and their molecular structures elucidated. Hg(II) ocap complexes, [Hg{SC6H3XN(CN)}]n (X = H, Me) (1), react with Na2S to afford HgS and Na2[ocap] which reacts in situ with K2[PdCl4] to afford palladium ocap complexes [Pd{SC6H3XN(CN)}]n (2). A...

Four palladium (II) and platinum(II) complexes with the formula [MCl2(HPhqS)2] and [M(PhqS)2] (MII = Pd and Pt), were synthesized by treating Na2PdCl4 or K2PtCl4 with 2 mol of 4-Methylene-3-phenyl-3,4-dihydroquinazoline-2(1H)-thione (HPhqS) with or without the present base. The geometry around the Pd(II) and Pt(II) ions was a square planner and the...

Ten newly synthesized ortho-palladated complexes of the type [PdCl(bhq)L] ( 1–10 ) (where bhp = benzo[ H ]quinolate, L = 2-aminobenzothiazole (2-abt), 2-amino-benzimidazole(2-abi), 2-aminothiazole(at), imidazole(im), 2-aminopyridine(2-apy), 2-amino-3-methylpyridine(2-ampy), 2-amino-5-chloropyridine(2-acpy), 3-methyl-pyridine (3-mpy), 2-methylpyridi...

We report reactions of Hg(II) ortho-cyano-aminothiophenolate coordination polymers, [HgfSC 6 H 3 XN(CN)g] n , with donor ligands. Addition of cyclic aromatic amines, such as pyridine (L), leads to breakdown of the polymeric structure to give mononuclear four-coordinate complexes, [Hgfj 2-SC 6 H 3 XN(CN)gL 2 ], while 2,2'-bipy and 1,10-phen (L 2) si...

The reaction of 1-(4-chlorophenyl)-3-phenylthiourea (CPTH²) with [PtCl2(PPh3)2] moiety in a 1:1 molar ratio in a basic solution afforded unexpected Pt(II) thiourea dianion complex. The crystal structure revealed that the second phenyl ring of the parent ligand was substituted with a chlorine atom. Chlorine substitution on the phenyl ring might have...

Addition of 2-aminobenzothiazole (abt) and substituted derivatives to Hg(OAc)2 leads to the high yield formation of ortho-cyano-aminothiophenolate (ocap) complexes [Hg{SC6H3XN(C≡N)}]n (X = H, Me, Cl, Br, NO2) resulting from dehydrogenation...

Two thione and thionate based complexes were synthesized by simply reacting the ligand 2-mercapto-5-methyl-1,3,4-thiadiazole (HmtzS) with palladium(II) salt in a neutral or basic medium in 2:1 molar ratio. Reacting of resulting complex [Pd(mtzS)2] (2) with Ph2P(CH2)nPPh2 (n = 1-4), dppf, Ph3P or Ph3PS yielded mononuclear complexes, [Pd(mtzS)2(Ph2P(...

Four palladium(II) and mercury(II) complexes of the type [MCl 2 (HPAO)] or [M(PAO) 2 ](HPAO = syn-2-pyridine aldoxime) are prepared and characterized using FTIR, 1 H NMR spectra, molar conductivity, and melting point. The results demonstrated that a chelating bidentate behavior of APO through the indo and exocyclic nitrogen atoms. The applicability...

The reaction of [Hg(mbm)2] (mbm = o-SC6H4CONH2) with Na2S releases Na[mbm] which reacts with Pd(II) salts to give [Pd(mbm)2]. While its precise molecular structure is unknown, [Pd(mbm)2] reacts with two equivalents of PPh3 to afford trans-[Pd(κ¹-mbm)2(PPh3)2] in which the mbm ligands bind through a sulfur atom. With dppf, a similar complex, [Pd(κ¹-...

Treatment of one molar equivalent of [PtCl2(diphos)] (diphos = dppe, dppp, dppb or dppf) or [PtCl2(PPh3)2] with one molar equivalent of (H2CPPT) in the presence of Et3N afforded the new heterocyclic thiourea dianion complexes [Pt(κ²⁻CPPT)(diphos)] and [Pt(κ²⁻CPPT)(PPh3)2] (1-5). The synthesized complexes were characterized by FT-IR, ¹H NMR and ³¹P-...

Four Platinum(II) and Palladium(II) heterocyclic thiourea complexes have been prepared; [Pt(CPPT)2](1), [Pd(CPPT)2](2), [Pt(MPPT)2](3), and [Pd(MPPT)2](4) (Where HCPPT=1-(5-chloropyridin-2-yl)-3-phenylthiourea, HMPPT=1-(3-methylpyridin-2-yl)-3-phenylthiourea). Both the ligands and the complexes were characterized by different spectroscopic techniqu...

A series of new platinum(II) mixed ligand complexes of diethyldithiocarbamate (Et2DT) and phosphine or amine ligands of the type [Pt(Et2DT)2(diphosphine)] (3-6), [Pt(Et2DT)2(diamine)](7-8), [Pt(Et2DT)2(PPh3)2] (9) and [Pt(Et2DT)2(SPPh3)2](10) have been prepared in good yield and fully characterized by elemental analysis, conductivity measurements a...

Treatment of one molar equivalent of [M(HCPPT)2] (M=Pd, Pt; H2CPPT = 1-(5-chloropyridin-2-yl)-3-phenylthiourea) with one molar equivalent of κ²-diphos (diphos = dppe, dppp, dppb, and dppf) or two molar equivalent of κ¹-phos afforded eight heterocyclic thiourea dianion complexes (1-8). The spectroscopic data analysis showed clear AX splitting patter...

Reaction of mercury(II) acetate [Hg(Ac)2] or mercury(II) chloride [HgCl2] with two moles equivalent of Na[bit] (bit = benzisothiozolinate) afforded [Hg(bit)2] as white solid in 96 and 70% yield respectively. Treatment of [Hg(bit)2] with the bidentate ligands; 2,2-bipyridine (bipy), 1, 10-phenanthroline (phen) or ethylene diamine (en) in absolute et...

Treatment of two molar equivalents of 1,8-diaminonaphthalene-2-thione with one molar equivalent of the metal's(II) salt (Pd, Pt, Hg, Cd, Zn) afforded both neutral thione complexes and thionate derived complexes. The prepared ligand and its complexes (1-8) were characterized via different spectroscopic technics including: FT-IR, ¹H, ¹³C-NMR, and mas...

The addition of sodium hydroxide to a mixture of phenyl mercury acetate and 2-aminobenzothiazole in warm ethanol led to the high yield (84%) formation of [Ph-Hg(LH)]n (1), LH = the 2-cyanoaminothiaphenolate anion (SC6H4NHCN)⁻, resulting from monodeprotonation of 2-aminobenzothiazole and facile carbon–sulfur bond breakage. Reaction of 1 with Ph3P or...

The complex [Pb(tsac)2H2O] has been used as a synthon for the synthesis of a series of lead(II) thiosaccharinate mixed ligand complexes with the tertiary phosphines; PPh3, Ph2P(CH2)nPPh2, n = 1, dppm; n = 2, dppe; n = 3, dppp or the heterocyclic; 2-aminobenzothiophene (abtH), 2-acetamidopyrimidine (aampH) and 2-benzimidazolethiol (bimsH). The prepa...

Eight palladium(II) pyrrolidine dithiocarbamate complexes were prepared and fully characterized. Reactions of the dimeric cyclopalladated complexes, [Pd(ppy)(μ-Cl)]2 (ppyH= phenylpyridine) or [Pd(N-BAZ)(μ-Cl)]2 (N-BAZH = N,N-dimethylbenzylamine) with two moles equivalent of ammonium pyrrolidine dithiocarbamate NH4(PyDT) afford [Pd(PyDT)(ppy)] and [...

New palladium(II) and platinum(II) 1,1'-bis(diphenylphosphino) ferrocene (dppf) complexes with heterocyclic N-acetamide co-ligands [Pt(1-O-amp)(1-N-amp)(2-dppf)], [M(2-dap)(2-dppf)], (M= Pd, Pt , ampH = N-(2-pyridyl-3-methyl)acetamide, dapyH2 = 2,6-diacetamidopyridine) have been prepared and characterized. The salts K2[PtCl2(sac)2] and Na2[PdC...

Treatment of 1,4-benzothiazin-3-one (Hbto) with mercury(II) acetate Hg(OAc)2 in 2:1 mol ratio affords [Hg(bto)2] (1) in 99% yield. The resulted complex was used as a synthon to prepare new mixed-ligand complexes with monophosphines or diphosphines of the types [Hg(bto)2(L)2] or [Hg(bto)2(L-L)]; where L = triphenylphosphine (Ph3P) (2) or triphenylph...

Benzotriazole (Hbta) complexes with Hg(II) and Pd(II) of the types: [Hg(bta)2] (1), [Hg(bta)2(diphos)]; diphos = dppe (2), dppp (3) or dppb (4), [Hg(bta)2(PPh3)2] (5), [Pd(Hbta)2Cl2] (6), [Pd(bta)Cl]2 (7) and [PdCl(bta)(PPh3)]2.DMSO (8) were prepared and characterized by elemental analyses, conductivity measurements, infrared, ¹H- and ³¹P-{¹H} NMR...

Trans-[PdCl2(bzta)2] (bzta = 2-acetylaminobenzothiazole) (1a), trans-[PdCl2(bzmta)2] (bzmtaH = 2-acetylamino-6-methylbenzothiazole) (1b), trans-[PdCl2(bzcta)2] {bzcta = 2-acetylamino(6-chlorobenzothiazole)} (1c), cis-[PtCl2(bzta)2] (2a), cis-[PtCl2(bzmta)2] (2b) and cis-[PtCl2(bzcta)2] (2c) have synthesized and fully characterized; the molecular st...

A new complex of silver monovalent ions with benzisothiazolinone was reported. This silver coordination polymer was characterized by FTIR, elemental analysis, 1H-NMR and 13C-{1H}-NMR). These measurements show that the bit anion in its silver complex behaves as μ-bridge linking two silver(I) ions as a bidentate ligand through the oxygen and nitrogen...

Six palladium (II) and platinum (II) mixed ligand complexes of metronidazole (mnz) and saccharinate (sac) or benzothiazolinolate (bit) complexes of the type [ML2(mnz)2], M = Pd or Pt, L = sac or bit, have been prepared in moderate to high yield. The newly prepared complexes have been characterized by elemental (C,H,N,S) analysis, conductivity measu...

Six palladium (II) and platinum (II) mixed ligand complexes of metronidazole (mnz) and saccharinate (sac) or benzothiazolinolate (bit) complexes of the type [ML2(mnz)2], M = Pd or Pt, L = sac or bit, have been prepared in moderate to high yield. The newly prepared complexes have been characterized by elemental (C,H,N,S) analysis, conductivity measu...

Mn 2 (bit) 4 (H 2 O) 2 ] complex was used in this study as a novel precursor for the synthesis of MnO 2 nanoflowers. The inorganic precursor was synthesized from the reaction between chloride salt of Mn(II) and benzisothiazolinate. The chemical composition and the nanostructure of the prepared MnO 2 catalyst was characterized using several identifi...

Reaction of Na2[PdCl4] with two equivalents of 4,5-benzo-3H-1,2-dithiole-3-thione (btt) affords cis-[PdCl2(κ¹-btt)2] (1), which provides a convenient entry into mixed-ligand btt complexes. Addition of one equivalent of a range of diamines or diphosphines gives the salts [Pd(κ¹-btt)2(κ²-diamine)]Cl2 (2a–d) (diamine = en, dap, bipy, phen) and [Pd(btt...

Reacti on of two equivalents of sodium benzisothiozolinate (Nabit) with one equivalent of zinc acetate in aqueous solution afford [Zn(bit) 2 (H 2 O)] 2 (1). Treatment of (1) with three equivalents of triphenyl phosphine (PPh 3) gave [Zn(PPh 3) 2 ( 1-2-mbm)( 1-2-mbn)] (2), (2-mbm=2-mecaptobenzamide, 2-mbn=2-mercaptobenzonitrile). Treatment of (1)...

Initially, a novel series of mixed ligand Pd(II) complexes of 2H[1,4]benzothiazin-3(4H)-one (Hbto) and diamine or phosphine ligands were successfully prepared with yields of 61 to 92%. The treatment of Na2PdCl4 with Hbto in acetone with 1:2 Pd to Hbto ratio affords cis-[PdCl2(Hbto)2] (1) that delivers an appropriate entry into mixed-ligand Hbto com...

Fullerene biopolymer-magnetite nano inorganic composite is produced from newly prepared fullerene (C 60 )soluble eggshell membrane protein (SESMP)composite mixed with Fe 3 O 4 NPs. UV–Vis, FTIR, VSM, SEM, EDX and STEM are demonstrated that a stable Fe 3 O 4 can be retained on the surface of C 60 -ESMP bio nanocomposite by a multi-step chemical reac...

Phosphines react with the benzisothiazolinate (bit) paddlewheel dimer, [Ni2(m-bit)4.2H2O], resulting in sulfur-nitrogen bond scission and a series unexpected transformations leading to novel Ni(II) complexes containing 2-cyanophenylthiolate and related thiolate ligands.

Addition of sodium benzisothiazolinate, Na(bit), to metal salts MX⁠2·nH⁠2O (M=Mn, Co, Ni, Cu) affords a simple high yielding route to benzisothiazolinate-bridged paddlewheel dimers [M⁠2(μ-bit)⁠4·2H⁠2O]. Upon reaction with amines these serve as useful synthons to access benzisothiazolinate chemistry. Addition of 4-aminopyridine (4-ampy) in ethanol l...

Reacti on of two equivalents of sodium benzisothiozolinate (Nabit) with one equivalent of zinc acetate in aqueous solution afford [Zn(bit) 2 (H 2 O)] 2 (1). Treatment of (1) with three equivalents of triphenyl phosphine (PPh 3) gave [Zn(PPh 3) 2 ( 1-2-mbm)( 1-2-mbn)] (2), (2-mbm=2-mecaptobenzamide, 2-mbn=2-mercaptobenzonitrile). Treatment of (1)...

Treatment of silver(I) nitrate with sodium benzisothiazolinone (Nabit) affords [Ag(bit)] n complex. The produced silver coordination complex was characterized by infrared spectroscopy, elemental analysis, nuclear magnetic resonance (1 H-NMR and 13 C-{ 1 H}-NMR). These measurements showed that the bit anion behaves as a bidentate bridge linking two...

Reactions of [Pd(Me2NCH2C6H4-κ²N,C)(μ-Cl)]2 with two equivalents of sodium saccharinate (Nasac), thiosaccharin (Htsac) or sodium benzisothiozolinate (Nabit) results in the stepwise substitution of the bridging halides to form sequentially [Pd2(Me2NCH2C6H4-κ²N,C)2(μ-Cl)(μ-X)] (X = sac, tsac) and [Pd(Me2NCH2C6H4-κ²N,C)(μ-X)]2 (X = sac, tsac, bit). Th...

Reaction of mercury(II) acetate Hg(Ac)2 with two equivalents of N-hydroxymethylsaccharin (Sac-CH2OH) in the presence of NEt3 afforded the presumably tetrahedral complex [Hg(K2-Sac-CH2O)2] (1). Reaction of (1) with one equivalent of the bidentate ligands (L-L); Ph2P(CH2)nPPh2, (n = 1 dppm; 2 dppe; 3 dppp; 4 dppb), Ph2P(S)(CH2)P(S)Ph2 (dppmS2) Ph2P(O...

The thermal behavior of mixed ligand complexes of platinum (II) and palladium(II) thiosaccharinate (tsac) with diphosphine or bipyridine ligands was studied by thermogravimetry, TG, and differential thermal analysis, DTA. The Platinum complexes showed higher thermal stability than the corresponding palladium complexes. Platinum complexes start deco...

The thermal behavior of mixed ligand complexes of platinum (II) and palladium(II) thiosaccharinate (tsac) with diphosphine or bipyridine ligands was studied by thermogravimetry, TG, and differential thermal analysis, DTA. The Platinum complexes showed higher thermal stability than the corresponding palladium complexes. Platinum complexes start deco...

A comparative study of reactions of saccharinate (sac), thiosaccharinate (tsac) and benzisothiozolinate (bit) with trans-[PdCl2(H2NBz)2] is reported. While in all cases substitution of both chlorides occurs, product types differ for the three closely related ligands. With sodium saccharinate, trans-[Pd(N-sac)2(H2NBz)2] results in which the sac liga...

A range of new cadmium(II) thiosaccharinate (tsac) complexes have been prepared from reactions of the synthon [Cd(tsac)2.H2O] with a variety of two-electron donor ligands including amino- and acetyl-amino heterocycles, 2-mercaptobenzoimidazole, 2-mercaptobenzothiozole and 2-phenylpyridine, as well as the bidentate small bite-angle diphosphane, bis(...

A number of cyclometalated palladium(II) complexes [PdCl(pyC6H4)(L)] containing amino-pyridine or acetylamino-pyridine co-ligands (L) have been prepared from the reaction of [Pd(pyC6H4)(μ-Cl)]2 with two equivalents of these ligands. Crystal structures of four examples have been carried out, each showing a distorted square planer geometry around pal...

Abstract Reaction of Na2PdCl4 with two equivalents of N-hydroxymethylsaccharin (Sac-CH2OH) in the presence of NEt3 afforded trans-[Pd(k2-Sac-CH2O)2]. Further reactionof [Pd(k2-Sac-CH2O)2] with one equivalent of diphosphine (L2), Ph2P(CH2)nPPh2, (n = 1, dppm; 2, dppe and 3, dppp), Ph2P(S)(CH2)P(S)Ph2 (dppmS2) orPh2P(O)(CH2)2P(O)Ph2 (dppeO2) afforded...

A series of square-planar palladium(II) benzisothiazolinate (bit) of the general type [Pd(bit)2L2] have been prepared and characterized by analytical and spectroscopic methods. Two synthetic routes have been employed, namely reactions of [Pd(bit)2]�H2O with two equivalents of ligands (L = amine, amide, phosphine) or nucleophile displacement of chlo...

Palladium(II) and platinum(II) complexes containing mixed ligands N-(2-pyridyl)acetamide (AH)

Addition of 2-aminobenzothiazole and substituted derivatives to mercuric acetate in warm ethanol leads to the high yield formation of [Hg{SC6H3XN(C[triple bond, length as m-dash]N)}]n resulting from loss of hydrogen and sulfur-carbon bond cleavage. Addition of phosphines affords a series of complexes in which the new ortho-cyano-aminothiophenolate...

Abstract Reaction of [Hg(sac)2] with two equivalents of substituted pyridines, L, [L = 2-aminopyridine (2-ampy), 2-amino-3-methylpyridine (2-ammpy), 4-vinylpyridine (4-vipy), 4-ethylpyridine (4-etpy), 2-acetylaminothiazole (2-aamtz)] in MeOH affords [Hg(sac)2L2], a crystal structure of [Hg(sac)2(2-ampy)2] revealing a distorted tetrahedral HgN4 coor...

Palladium(II) saccharinate complexes trans-[Pd(sac)2(LH)2] with amino- and acetylamino-pyridine co-ligands: molecular structures of trans-[PdCl2(2-ampyH)2].2dmf (2-ampyH 5 2- amino-3-methylpyridine) and trans-[Pd(j2-2-acmpy)2] (2- acmpyH 5 2-acetylamino-3-methylpyridine)

Reaction of Na-2[PdCl4] with two equivalents of amino- or acetylamino-pyridines (LH) affords trans-[PdCl2-(LH)(2)] {LH = 2-amino-3-methylpyridine (2-ampyH), 3-aminopyridine (3-apyH), 2-acetylamino-3-methylpyridine (2-acmpyH), 3-acetylamino-pyridine (3-acpyH)}. An X-ray crystal structure of trans-[PdCl2(2-ampyH)(2)] shows that the 2-ampy-H ligands a...

The new platinum(II) complexes cis-[Pt(sac)2(NH3)2] (sac = saccharinate) and cis-[Pt(tsac)2(NH3)2] (tsac = thiosaccharinate) have been prepared, the X-ray crystal structure of cis-[Pt(sac)2(NH3)2].H2O reveals that both saccharinate anions are N-bound in a cisarrangement being inequivalent in both the solid-state and in solution at room temperature....

II) saccharinate (sac) and thiosaccharinate (tsac) complexes with supporting amino-and acetylamino-thiazole ligands: Crystal structures of trans-[PdCl 2 (abzt) 2 ]Ádmf (abzt = 2-aminobenzothiazole), trans-[PdCl 2 (bzta) 2 ].dmf (bzta = 2-acetylaminobenzothiazole) and trans-[Pd(sac) 2 (abzt) 2 ]Á2dmf a b s t r a c t Treatment of Na 2 PdCl 4 with two...

Simple palladium(II) and platinum(II) complexes, ML2 (1–2), of N-phenyl-(2-thiazoyl)thiourea have been prepared and fully characterized. The structure of Pd(S2N3C10H8)2 (1) is monoclinic P21/c, a = 12.510(2), b = 5.6963(6), c = 15.322(2) Å, b = 90.07(2)o and Pt(S2N3C10H8)2 (2) is orthorhombic P2 1 2 1 2 1 , a = 7.3021(5), b = 11.8025(9), c = 25.628...

Palladium(II) and platinum(II) thiosaccharinate complexes [M(κ1-tsac)2{κ2-Ph2P(CH2)nPPh2}] (M = Pd, Pt; n = 1–4) have been prepared, palladium complexes from reaction of [Pd(tsac)2]·H2O with diphosphanes and platinum complexes from addition of thiosaccharin to [PtCl2{κ2-Ph2P(CH2)nPPh2}] in the presence of triethylamine. All complexes have been full...

Room temperature addition of sodium saccharinate, Na(sac), to [MCl2(κ2-dppf)] (M = Pd, Pt; dppf = 1,1′-bis(diphenylphosphino)ferrocene) results in the formation of [MCl(sac)(κ2-dppf)] in which the sac ligand is coordinated in a monodentate fashion through nitrogen. All attempts to coordinate a second saccharinate ligand were unsuccessful. In contra...

Treatment of [MCl2(κ2-dppf)] (M = Pd or Pt) with two equivalents of potassium heterocyclic thionate salts (KL) affords mixed ligand complexes [ML2(κ2-dppf)] [L = 5-phenyl-1,3,4-oxadiazole-2-thionate (Phozt), 4,5-diphenyl-1,2,4-triazole-3-thionate (Ph2tzt), benz-1,3-thiazoline-2-thionate (bztzt) and benz-1,3-oxazoline-2-thionate (bzoxt)]. X-ray stru...

Tetrahedral mercury(II) complexes of the types [HgCl(sac)(PPh 3) 2], [HgCl(sac)(diphos)], [Hg(sac) 2(PPh 3) 2] or [Hg(sac) 2(diphos)] and octahedral complexes of the type [Hg(sac) 2(dppe) 2] or [Hg(sac) 2(dppp) 2] {diphos = Ph 2P(CH 2) nPPh 2; n=1, dppm; n=2, dppe; n=3, dppp; n=4,dppb} were prepared and characterized by molar conductance, elemental...

Na 2PdCl 4 reacts with 2-(2'-hydroxylphenyl)benzoxazole (Hpbo), 2-(2'-hydroxyl phenyl)benzothiazole (Hpbt) or the mixed ligands (Hpbo) and (Hpbt) in methanol to give trans- [PdCl 2(Hpbo) 2], trans-[PdCl 2(Hpbt) 2] or trans-[PdCl 2(Hpbo) (Hpbt)], respectively the benzoxazole or benzothiazole ligands behave as monodentate ligands coordinated to palla...

Reaction of [Hg(OAc)2] with two mole proportion of LH(LH= benz-1,3-imidazoline-2-thione, benz-1,3-oxazoline-2-thlone or benz-1,3-thiazoline-2-thlone) in the presence Et3N gave linear complexes of the type [HgL2. Treatment of [HgL2] with two mole proportion of PPh3or one mole proportion of the diphosphine Ph2P(CH3)nPPh2 gave tetrahedral complexes of...

Palladium(II) and platinum(II) complexes containing mixed ligands N-phenyl-N-(2-pyridyl) thiourea (AH) or N-phenyl-N-(2-methylpyridyl) thiourea (BH) and the diphosphine Ph2P(H2)n PPh2 (n = 1-4) have been prepared and characterized by elemental analysis, magnetic susceptibility, molar conductance and i.r. spectral data. 1H n.m.r. data have been used...

The reaction of Na2PdCl4 with 4,5-diphenyl-1,2,4- triazole-3-thione (LH) in acetone gave cis-[PdCl2(LH)2]. Stirring cis[PdCl2(LH)2] in methanol gave a diamagnetic cis-[PdL2]. Reaction of cis[PdL2] with diphosphines gave diamagnetic complexes of the type [PdL2(diphos)] where diphos = 1,2-bis(diphenylphosphino)methane (dppm), 1,2-6(diphenyl-phosphino...

Palladium(II) and platinum(II) complexes containing mixed ligands N-(2-pyridyl)acetamide (AH) or N-(2-pyrimidyl)acetamide (BH) and the diphosphines Ph2P(CH2) n PPh2, (n = 1, 2 or 3) have been prepared. The prepared complexes [Pd(A)2(diphos)] or [Pd(B)2(diphos)] have been used effectively to prepare bimetallic complexes of the type [(diphos)Pd(μ-L)2...

Palladium(II) and platinum(II) complexes containing the mixed ligands tertiary diphosphines Ph2P(CH2) n PPh2, (n = 1–4) and benz-1,3-imidazoline-2-thione, benz-1,3-oxazoline-2-thione or benz-1,3-thiazoline-2-thione have been prepared and characterized by elemental analysis, magnetic susceptibility, molar conductance and i.r. spectral data. 31P–{1H}...

Potassium salt of the ligand 4,5-diphenyl-1,2,4-triazole-3-thione (LK) reacts with K2PtCl4 to give trans-[PtL2], in which (L) behaves as a bidentate chelating ligand coordinated to platinum through the nitrogen atom no.2 of the triazole ring and the sulphur of the thiolate group. Reaction of trans-[PtL2] with the diphosphine Ph 2P(CH2)n PPh2 (n = 1...

The complexes [ML(2)A(2)] or [ML2B] where M = Pd or Pt, L = 5-phenyl-1,3,4-oxadiazole-2-thione ion, A = tertiary monophosphines and B = tertiary diphosphines have been used effectively to prepare bimetallic complexes of the type [A(2)M(mu-L)(2)M'Cl-2] or [BM(mu-L)(2)M'Cl-2], where M' = Co, Pd or SnCl2. The prepared complexes were characterized by e...

Several new palladium(II) and platinum(II) complexes containing two types of ligands: tertiary monophosphines (L) and 5-phenyl-1,3,4-oxadiazole-2-thione ion (A) or 4,5-diphenyl-1,2,4-triazole-3-thione ion (B) have been prepared. The so obtained complexes trans-[PdA2L2], trans-[PdB 2L2] and cis-[PtA2L2] were characterized by elemental analysis, IR,...

Reaction of potassium salt of the ligand 5-phenyl-1,3,4-oxadiazole-2-thione (LH) with NiCl2.6H2O gave the chelate complex [NiL2]. Recrystalization of [NiL2] from CH2Cl2 or reaction of the ligand (LH) with NiCl2.6H2O gave the tetrahedral hydroxy nickel(II) complex [Ni(OH)(L)(LH)]. Reaction of either [NiL2] or [Ni(OH (L)(LH)] with tertiary monophosph...

Transition metal complexes containing two types of ligands: 5-phenyl-1,3,4-oxadiazole-2-thione ion (L) and tertiary phosphines, have been prepared. The complexes, [ML2A2] [M = Pd or Pt; A = PPh3 or Ph2PCH2CH2P(O)Ph2] and [ML2B] (M = Co, Ni, Pd or Pt; B = Ph2PCH2PPh2 or Ph2PCH2CH2PPh2), were characterized by elemental analysis, molar conductance, i....

The mixed phosphine–phosphine oxide Ph2PCH2CH2P(O)Ph2 (dppeO) reacts with either trans-[PdCl2(PhCN)2], Na2[PdCl4] or trans-[PdCl2(DMSO)2] to give trans-[PdCl2{1-Ph2PCH2CH2P(O)Ph2}2]. Treatment of the latter with the metal chlorides, MCl2 nH2O (M = Mn, Cu, Co, Zn, Hg; n = 4, 2, 6, 1, 0, respectively) or with Me2SnCl2 or SnCl4 5H2O, or with UO2(NO3)2...

Treatment of Vaska's compound with 50% aqueous sodium hydroxide using benzyl(triethyl)ammonium chloride as phase-transfer catalyst gave [Ir(OH)(CO)(PPh3)2] in high yield.

The complex [Pd(dpmMe)2]Cl2 [dpmMe = 1,1-bis-(diphenylphosphino) ethane] was prepared from [PdCl2-(PhCN)2], whilst [Pd2X2(μ-dpmMe)2] complexes were prepared from [PdCl2PhCN2] and [Pd(PPh3)4] (X = Cl), [PdBr(η 3-C3H5)]2 (X = Br), or [Pd2Cl2(μ-dpmMe)2] (X = I). Reaction of [Pd2Cl2(μ-dpmMe)2] with MeO2C-C523-01CCO2Me(L) gave the A-frame complex [PdCl2...

Ph2PCH(Ph)PPh2, prepared by treating Ph2PCH2Ph successively with n-BuLi and Ph2PCl, reacts with group VI metal hexacarbonyls to give [M(CO)4{Ph2PCH(Ph)-PPh2}], where M = Cr, Mo or W. The Cr complex [Cr(CO)4{Ph2PCH(Ph)PPh2}] was deprotonated with MeLi and the resulting carbanion [Cr(CO)4(Ph2-PCPhPPh2)]− acylated with RCOCl (R = Ph or p-tolyl) to giv...

The mixed phosphine-phosphine oxides Ph2P(CH2)n-P(O)Ph2 (n = 1 or 2) react with K2PtCl4 to give cis-{PtCl2- 1-Ph2P(CH2) n P(O)Ph2]2}. Treatment of the latter (n = 2) with transition metal chlorides MCl2nH2O, or with Me2SnCl2, SnCl45H2O, Th(NO3)4xH2O or UO2(NO3)2 6H2O, gives novel heterobimetallic complexes identified as cis-{PtCl2[-Ph2P(CH2)2P(O)Ph...

Complexes of type [M(CO)4PPh2CH2PPh2)], when treated succesively with LiBun and Ph2PCl give complexes of type [M(CO)4{(Ph2P)3CH}] i.e. [M(CO)4(tripod)], in which the triphosphine is bidentate. These may be oxidized (H2O2) to the corresponding phosphine oxide [M(CO)4{(Ph2P)2CHP(O)Ph2}] or converted with sulphur to the corresponding phosphine sulphid...