Abdel-Fattah Shihada

Darstellung und schwingungsspektren von trimethylzinndiorganothiophosphinaten Me3SnOSPR′R″ (R′R″ = Me2, MePh, Ph2). Die kristallstruktur von Me3SnOSPMe2

Abstract A series of trimethyltin diorganothiophosphinates Me 3 SnOSPR′R″ (R′R″ = Me 2 , MePh, Ph 2 ) was prepared from (Me 3 Sn) 2 O and R′R″PSCl in cyclohexane solution. A close study of the vibrational spectra is given; 31 P NMR and mass spectra are also reported. The structural investigation of Me 3 SnOSPMe 2 by means of X-ray diffraction ( R 5.2%, 1697 observed independent reflexions) shows the compound to consists of chains, in which planar SnMe 3 units and tetrahedral OSPMe 2 groups are linked by the O- and S-atoms of the thiophosphinate.

Syntheses, Spectroscopic Studies, and Crystal Structures of Me2Sn(O2PPh2)2, Ph2Pb(O2PMe2)2, and Ph2Pb(O2PPh2)2

Me2Sn(O2PPh2)2 (1), Ph2Pb(O2PMe2)2 (2), and Ph2Pb(O2PPh2)2 (3) have been synthesized by the reactions of Me2SnCl2 or Ph3PbCl with the corresponding diorganophosphinic acid in methanol. X-ray diffraction studies show that the diorganophosphinate groups behave as double bridges between the metal atoms leading to polymeric ring-chain structures with M2O4P2 (M = Pb, Sn) eight-membered rings. The organic groups bonded to the metal atoms are in trans-position in the resulting octahedral arrangement around the metal atoms. The IR and the mass spectra were reported and discussed. Synthesen, spektroskopische Untersuchungen und Kristallstrukturen von Me2Sn(O2PPh2)2, Ph2Pb(O2PMe2)2 und Ph2Pb(O2PPh2)2 Me2Sn(O2PPh2)2 (1), Ph2Pb(O2PMe2)2 (2) und Ph2Pb(O2PPh2)2 (3) wurden durch Reaktion von Me2SnCl2 bzw. Ph3PbCl mit der entsprechenden Diorganophosphinsaure in Methanol dargestellt. Rontgenkristallstrukturuntersuchungen zeigen, das die Diorganophosphinatgruppen als Doppelbrucken zwischen den Metallatomen wirken und so polymere Ringkettenstrukturen mit M2O4P2 (M = Sn, Pb)-Achtringen aufbauen. Die organischen Substituenten an den Metallatomen stehen innerhalb der oktaedrischen Umgebung der Metallatome in trans-Stellung. Die IR-und Massenspektren der Verbindungen werden diskutiert.

Über die kristallstrukturen von Me3SnO2PCl2 und Me3SnO2PMe2 und das Schwingungsspektrum von Me3SnO2PMe2

Abstract Me 3 SnO 2 PMe 2 is prepared by treatment of Me 3 SnNEt 2 with Me 2 PO 2 H in methylene chloride. The vibrational spectrum is discussed. Crystal structure determinations from X-ray diffraction data have been carried out with single crystals of Me 3 SnO 2 PMe 2 ( R 0.076, 819 observe independent reflexions), and Me 3 SnO 2 PCl 2 ( R 0.051, 1127 observed independent reflexions), showing polymer chains of SnMe 3 groups and O 2 PX 2 (X = Cl, Me) units in both cases. The phosphinate chains form vast helices whereas the dichlorophosphate forms almost planar chains.

Synthesis, Spectral Studies, and Crystal Structure of [Me2ClSnO2AsMe2] and [Et2ClSnO2AsMe2]†

The treatment of Me2SnCl2 and Et2SnCl2 with HO2AsMe2 in methanol leads to [Me2ClSnO2AsMe2] (1) and [Et2ClSnO2AsMe2] (2), respectively. X-ray diffraction studies show that the O2AsMe2 groups function as bidentate bridge ligands between R2ClSn units forming polymeric chain structures. 1 consists of double chains, in which the oxygen atoms of each O2AsMe2 group of one chain interact in a chelate mode with the tin atom of the other affording seven-coordinated tin atoms, whereas the structure of 2 is built of single chains in which the tin atoms exhibt a distorted trigonal-bipyramidal geometry with an axial O-Sn-Cl angle of 160°. The vibrational and mass spectra are given and discussed. Synthesen, spektroskopische Untersuchungen und Kristallstrukturen von [Me2ClSnO2AsMe2] und [Et2ClSnO2AsMe2] Die Umsetzung von Me2SnCl2 und Et2SnCl2 mit HO2AsMe2 in Methanol fuhrt zu [Me2ClSnO2AsMe2] (1) bzw. [Et2ClSnO2AsMe2] (2). Rontgenkristallstrukturuntersuchungen zeigen, das die O2AsMe2-Gruppen als Bruckenliganden zwischen den R2ClSn-Einheiten fungieren, und so polymere Kettenstrukturen bilden. 1 besteht aus Doppelketten, in denen die Sauerstoffatome der O2AsMe2-Gruppen jeder Kette als Chelatliganden mit dem Zinnatom der anderen Kette wechselwirken, wodurch dieses siebenfach koordiniert wird. Die Struktur von 2 besteht aus einfachen Ketten, in denen die Zinnatome eine verzerrt trigonal - bipyramidale Koordination mit einem axialen O-Sn-Cl - Winkel von 160° aufweisen. Die Schwingungs- und Massenspektren werden beschrieben und diskutiert.

Preparation, vibrational spectra and crystal structure of tris(trimethyltin) tetrathiophosphate (Me3SnS)3PS

Abstract Tris(trimethyltin) tetrathiophosphate (Me3SnS)3PS has been prepared by the reaction of (Me3Sn)2S with PSCl3. Its IR and Raman spectra are reported and discussed, and 31P NMR spectral data presented. A X-ray diffraction study shows that crystals of (Me3SnS)3PS consist of discrete monomeric molecules in which both the tin and phosphorus atoms are four-coordinate and the Me3Sn groups are covalently bonded to the sulphur.

Synthesis, spectroscopic studies, and crystal structure of 3-(1-hydroxyiminoethyl)-1-phenyl-4-hydro-1,2,4-triazine-5,6-dione methanol solvate

3-(1-Hydroxyiminoethyl)-1-phenyl-4-hydro-1,2,4-triazin-5,6-dione, has been prepared from the chiral 1-phenyl-3-acetyloxime-5-benzyl-4,5-dihydro-1,2,4-triazin-6-one in the presence of organotin(IV) compounds in methanol solution. It crystallizes as a 1:1 methanol solvate in the monoclinic space group P 2 1 /c with the lattice parameters: a = 1517.6(1), b = 563.64(3), c=1500.34(13) pm and β = 90.35(1)°. The molecules, in which the heterocyclic ring is planar, are dimer via strong oxime-methanol and methanol-dione hydrogen bonds and by additional N-H---O bridges linking the heterocyclic rings.

Synthese, Schwingungs- und Massenspektren von Et2Sn(O2PR2)2 (R = Me, Ph); Kristallstruktur von Et2Sn(O2PPh2)2 / Synthesis, Vibrational Spectra and Mass Spectra of Et2Sn(O2PR2)2 (R = Me, Ph); Crystal Structure of Et2Sn(O2PPh2)2

Et2Sn(O2PPh2)2 has been synthesized by the reaction of (Et2ClSn)2O with Ph2POCl in toluene and by the treatment of (Et2ClSn)2O or Et2SnCl2 with HO2PPh2 in methanol. The reaction of Et2SnO with HO2PMe2 in toluene was used to prepare Et2Sn(O2PMe2)2. An X-ray diffraction study of Et2Sn(O2PPh2)2 (space group P1̅, Z = 1, a = 559,9( 1), b = 983,7(1), c = 1262,4(l)pm, α = 81,85( 1 )°, β = 79,79( 1)°, γ = 75,00(1)°; structure refinement with 2662 independent reflections, R = 0.055) shows that the structure is polymeric and the O2PPh2 ligands function as double bridges between the tin atoms leading to the formation of centrosymmetric Sn2O4P2 eight-membered rings. The ethyl groups are in trans-position in the resulting octahedral environment around tin. The I. R. and Raman spectra of Et2Sn(O2PR2)2 (R = Ph, Me) have been discussed and assigned. The mass spectra of Et2Sn(O2PR2)2 show Sn(O2PR2)+ as the base peak.

SYNTHESIS, SPECTROSCOPIC STUDIES, AND CRYSTAL STRUCTURE OF DIETHYLCHLOROTIN DIMETHYLPHOSPHINATE ET2CLSNO2PME2

Abstract Diethylchlorotin dimethylphosphinate has been synthesized by treating (Et2ClSn)2O with HO2PMe2 in toluene. Single crystal X-ray analysis shows that O2PMe2 groups behave as bidentate bridge ligands between Et2ClSn units leading to a polymeric chain structure in which the tin atoms exhibit a distorted trigonal bipyramidal geometry with the oxygen atoms in the axial positions. The Sn-Cl bond lies on a C2 axis of symmetry in the (C2v) OCClSnCO unit. Et2ClSnO2PMe2 crystallizes in the monoclinic space group C2/c (a = 877.9 (2), b = 1907.8 (4), c = 695.5 (1) pm, β= 106.72 (2)°, Z = 4 and R = 0.043). The characteristic IR bands of Et2ClSnO2PMe2 are assigned and the mass spectrum is reported and discussed.

The Crystal Structures of Et2Sn(O2PMe2)2 and Ph2Sn(O2PMe2)2; Synthesis and Spectral Studies of Ph2Sn(O2PMe2)2

Abstract Ph2Sn(O2PMe2)2 has been synthesized by the reaction of HO2PMe2 with Ph2SnO in toluene or by treating HO2PMe2 with Ph2SnCl2 in methanol. X-ray diffraction studies of Et2Sn(O2PMe2)2 and Ph2Sn(O2PMe2)2 show that the O2PMe2 ligands function as bidentate bridges between the tin atoms. The ethyl and the phenyl groups are in trans-position in the resulting octahedral environment around tin. Et2Sn(O2PMe2)2 crystallizes in the monoclinic space group P21/n (a = 817.11(9), b = 974.1(1), c = 970.1(1) pm, β = 113.749(6)°, Z = 2 and R = 0.032) and consists of a polymeric layer structure with centrosymmetric (SnOPO)4 sixteen-membered rings. Ph2Sn(O2PMe2)2 also crystallizes monoclinically in the space group P21/n (a= 1060.9(1), b = 999.4 (1), c = 1768.9(2) pm, β = 90.93(1)°, Z = 4 and R = 0.057) and has a polymeric ring-chain structure with centrosymmetric (SnOPO)2 eight-membered rings. The IR and Raman spectra of Ph2Sn(O2PMe2)2 have been assigned and discussed in the light of structural information. The Sn(O2PMe2)+ ion represents the base peak in the mass spectrum of Ph2Sn(O2Me2)2.

Synthesis, Vibrational Spectra, Mass Spectrum and Crystal Structure of Tri-n-butyltin Diphenylphosphinate (n-Bu)3SnO2PPh2

Abstract Tri-n-butyltin diphenylphosphinate (n-Bu)3SnO2PPh2 has been synthesized by the reaction of (n-Bu3Sn)2O with Ph2POCl in toluene. An X-ray diffraction study of (n-Bu3)SnO2PPh2 shows that the structure is polymeric and consists of helical chains in which (n-Bu)3Sn groups are linked by O-P-O bridges. The geometry about tin is trigonal bipyramidal, with n-butyl groups in equatorial positions and an axial O-Sn-O angle of 176.2 (2)°. IR and Raman spectra of (n-Bu)3SnO2PPh2 are given and assigned. The mass spectrum is reported and discussed.