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  • Author: Bernhard Neumüller x
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The title compound 1 has been prepared by the reaction of i-PrInCl2 with LiCH(SiMe3)2 in diethylether at -30 °C. The colorless substance 1 was characterized by NMR, IR, and RE spectroscopy, as well as by mass spectrometry. 1 is dimer in solution and the solid state and crystallizes in the space group P21/c with the cell parameters a = 1206.4(3) pm, b = 905.7(2) pm, c = 1591.2(5) pm, and β = 101.18(2)°. The unit cell contains two centrosymmetrical dimeric molecules.

The reactions of isopropyl indium dichloride (1) with LiN(H)t-Bu and of mesityl indium chloride (2) with NaN(SiMe3)2 lead to compounds [i-Pr(Cl)InN(H)t-Bu]2 (3) and [Mes(Cl)InN(SiMe3)2]2 (4), respectively. 3 forms dimers in solution and in the solid state, while the monomer is the predominate species of 4 in solution. 3 crystallizes in 2 isomers. The X-ray analysis of one isomer of 3 is reported.

[(PhCH2)2InN(H)t-Bu]2 (3) and [PhCH2(Cl)InN(SiMe3)2]2 (4) have been prepared by the reaction of (PhCH2)2InCl with LiN(H)t-Bu and of PhCH2InCl2 with NaN(SiMe3)2, respectively. 3 could be isolated in two isomers, while 4 forms only one chloro-bridged isomer in solution and in the solid state. The possibility of a chloro-bridged alkyl(aryl)chloroindium amide is also realized in [Mes(Cl)InN(SiMe3)2]2 (2), as shown by X-ray analysis. The reaction of a 1:1-mixture of i-Pr2InCl/i-PrInCl2 with LiN(H)t-Bu leads to all three possible compounds: [i-Pr(Cl)InN(H)t-Bu]2 (1), {i-Pr2In[N(H)t-Bu]2In(Cl)i-Pr} (5), and [i-Pr2InN(H)t-Bu]2 (6). Two isomers of the new compound 5 are detectable in solution. The crystal structure has been determined for the less sterically hindered isomer 5a, which forms hydrogen-bridged (Cl-H-N-bridge) infinite chains along the c-axis.

Single crystals of MesSn(Cl)Me2 (1) and Mes2SnCl2 (2) were obtained by the reactions of MesGaCl2 with Me3SnF and Mes3SnF, respectively. 1 and 2 are monomeric molecules in the solid state. 1: space group P21/n, Z = 4. lattice dimensions at -70°C: a = 1202,3(1), b = 739,1(1), c = 1441,3(1) pm , β = 102,71(1)°, R1 = 0,0469; 2: space group Pbcn, Z = 4, lattice dimensions at -50°C: a = 1107,0(2), b = 949,9(1), c = 1729,8(2) pm, R1= 0,049.


The title compound 1 was synthesized by the reaction of LiCl with TM EDA (N,N,N′,N′- tetramethylethylendiamine) and water at 120 °C in boiling TM EDA. 1 was crystallized at - 30 °C as colorless crystals and characterized by NMR and IR spectroscopy as well as by an X-ray structure determination. 1 is a polymer in the solid state, built up by an alternating arrangement of stick-like tetranuclear Li complexes and two TMEDA molecules. The complexes and the TMEDA molecules are connected by hydrogen bridges in infinite chains.

Single crystals of [(THF)LiCl]n (1) were obtained by the reaction of (PhCH2)2GaCl with LiSe'Bu in THF/toluene. 1 is polymeric in the solid state and crystallizes in the space group Pbcn, Z = 8, lattice dimensions at -83 °C; a = 1438.6(2), b = 1140.9(2), c = 746.2(1) pm, R1 = 0.0395


[Mg3Br2.4Cl1.6(OEt2)6][Ga(CH2Ph)4]2 · 0.5 toluene (1) can be obtained by the reaction of one equivalent of GaCl3 with four equivalents of PhCH2MgBr in Et2O. Recrystallization of the crude product from toluene at 60°C gives colorless crystals of 1. Treatment of GaCl3 with two equivalents 3,5-Me2C6H3CH2MgBr in Et2O gives after recrystallization from toluene the diorganogallium bromide [(3,5-Me2C6H3CH2)2GaBr]2 (2). 1 and 2 were characterized by NMR, IR and MS techniques as well as by X-ray structure analyses. 1 consists in the dication [Mg3Br2.4C1.6(OEt2)6]2+, two gallate units [Ga(CH2Ph)4]- and a toluene molecule, disordered around a center of inversion. 2 forms centrosymmetric dimers [(3,5-Me2C6H3CH2)2GaBr]2.


Single crystals of [Mo(CO)3(NCMe)(S′Bu)]2 (1) and [{Mo(CO)3}2{Mo(CO)2}{S′Bu}4] (2) were obtained by the reaction of [Mo(CO)3(NCMe)3] with [(PhCH2)2GaS′Bu]2 in 1,4-dio-xane. The X-ray structure determination of 1 showed the presence of a Mo2S2 four-membe-red ring with a Mo-Mo bond length of 296,7(1) pm. Space group Pbca, Z = 4, lattice dimen­sions at -80°C: a = 1588,2(3), b = 905,8(1), c = 1676,0(1) pm, R1 = 0,0555.


Pale brown single crystals of the title compound have been obtained by the reaction of Pb[N(SiMe3)2]2 with molybdenum pentachloride in ether solution as a result of a redox reaction. ClPb[N(SiMe3)2]3 crystallizes in the trigonal space group R3 with three formula units per unit cell. Lattice dimensions at -50 °C: a = b -1828.7(2), c = 854.5(1) pm. The compound forms monomeric molecules with bond lengths Pb-Cl = 247.9(4) pm and Pb - N = 213(2) pm.

Yellow-orange single crystals of [Ph3AsBr]2[TeBr6] have been prepared from saturated solutions of Ph3AsBr2 and TeBr4 in acetonitrile and characterized by a crystal structure determination. Space group R3̄c, Z = 12, lattice dimensions at -70 °C: a = b = 1337.9(2), c = 7953.8(4) pm, R = 0.0691. The structure consists of discrete ions [Ph3AsBr]+ and nearly perfectly octahedral [TeBr6]2-.