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Nitrosyl Complexes: Preparation of [NiBr(NO)(PPh3)2 ]

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Introduction

Nitrosyl Complexes: Preparation of [NiBr(NO)(PPh3)2 ] Monday 12th January 2009 Introduction and Aims The aims of this experiment are as followed: 1) To distinguish between the linear and bent coordination and draw possible metal to NO coordination modes. 2) To form the product [NiBr (NO) (PPh3)2] and provide a balanced equation for the product. 3) To record the melting point, weight and infra-red spectrum of the product. Assign the band in the infra-red that is due to NO group. Calculate the percentage yield 4) To assign the oxidation state to the metal in the nitroxide complex [NiBr(NO)(PPh3)2] 5) To suggest a method for distinguish between possible square planar and tetrahedral coordination of [NiBr2(PPh3)2] This experiment provides a method for the generation of nitrosyl complexes without the use of free nitric oxide. ...read more.

Middle

Discussion The reaction condition required for the experiment was reflex for 35mintues and use of solvents tetrahydrofuran and petroleum sprit. In this experiment the roles of the reagent are as followed: Sodium nitrite Used to generate NO the ligand [NiBr2(PPh3)2] The ligand complex , were the NO group will displace one of the Br. triphenylphosphine Used to form OPPh3 and used in oxidation . tetrahydrofuran an aprotic solvent and is used to dissolve compounds Petroleum sprit A solvent, used in the formation of the purple solid. Balanced equation [NiBr2(PPh3)2] +NaNO2 +PPh3 � [NiBr (NO) (PPh3)2] +OPPh3 +NaBr Percentage yield calculation. RMM of [NiBr2(PPh3)2] 58.69+79.91+(12.00 x32) +(1.008 x30) +(30.97 x2)=694.69 g mol-1 Moles=g/RMM = 2.5/694.69=0.004moles RMM of [NiBr (NO) (PPh3)2] 16.00+58.69+79.91+14.01+(12.00 x32) ...read more.

Conclusion

Measure the magnetic moment of [NiBr2(PPh3)2] at room temperature. The number that is nearest to the measured magnetic moment at room temperature gives the coordination of [NiBr2(PPh3)2] . e.g. say the magnetic moment at room temperature is 3.15�B for [NiBr2(PPh3)2] then the coordination is tetrahedral. The oxidation state of Ni metal is 2+. Where Br is -1,NO is -1 and PPh3 is 0. Additional learning Conclusion The experiment was a good method to determine the coordination of NO. The method allowed the aims of the experiment to be achieved. The only negative critic would be that the infra-red spectrum was that good. The peaks were not broad enough this could be due to the sample used for the infra-red not being prepared properly. A improvement would be to prepare a good sample for the infra-red. ?? ?? ?? ?? ...read more.

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