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    Synthesis of nickel complexes

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    Abstraction

    The intent of this experiment was to look into the Ligand exchange that occurs when different Nickel composites and reacted with Triphenylphosphine.

    Introduction

    Triphenylphosphine was foremost prepared by Pfeiffer and Sauvage in 1904

    Experimental

    Triphenylphosphine ( 1.408g ) was dissolved under reflux with Propan-2-ol ( 15cm3 ) organizing a colorless solution to which 5 boiling french friess were added. Nickel chloride hexahydrate ( 0.603g ) was dissolved in absolute Ethanol ( 10cm3 ) and heated until a green/yellow solution formed. This solution was poured into the reaction mixture through the capacitor. Immediately the solution turned dark green, the solution was refluxed for a farther 6mins. The reaction was removed from the heat and let to chill for 4mins, a dark precipitate was seeable in the flask. The warm solution was filtered under suction to roll up the dark blue/green crystals which were washed with ice cooled absolute ethyl alcohol ( 1x10cm3 + 1x3cm3 ) . Once dry the boiling french friess were removed with a spatula and the crystals were transferred to a n unfastened sample phial and dried in the desiccator for a hebdomad.

    A farther solution of Triphenylphosphine ( 1.410g ) and Propan-2-ol ( 15cm3 ) was made and set to reflux as earlier. Sodium thiocyanate ( 0.601g ) was dissolved in Ethanol ( 11cm3 ) , to this nickel nitrate hexahydrate ( 0.773g ) was added. The flask was warmed until all the green solid has dissolved and a white solid has formed. Once cooled the solution was filtered under suction and the Filtrate ( aqua blue liquid in Buchner flask ) was added to the refluxing Triphenylphosphine through the capacitor. Immediately the solution turned blood red/brown. The solution was refluxed for a farther 7mins and so cooled for 5 mins. The warm solution was filtered under suction and the orange/ ruddy crystals washed with ice cooled Ethanol ( 1x10cm3 + 1x8cm3 ) . Once dry the boiling french friess were removed as earlier and the crystals were transferred to the desiccator for a hebdomad.

    Consequences and treatment

    Triphenylphosphine + Propan-2-ol+ Nickle Chloride hexahydrate + Ethanol & A ; agrave ; Bis ( triphenylphosphine ) Ni ( II ) chloride

    P ( C6H5 ) 3 + C3H7OH + NICl2.6H2O + C2H5OH & A ; agrave ; C36H30Cl2NiP2

    Triphenylphosphine + Propan-2-ol+ Nickle Chloride hexahydrate + Ethanol & A ; agrave ; Bis ( triphenylphosphine ) Ni ( II ) chloride

    P ( C6H5 ) 3 + C3H7OH + NaSCN + C2H5OH + Ni ( H2O ) 6 ] ( NO3 ) 2 & A ; agrave ; [ Ni ( PPh3 ) 2 ] ( NCS ) 2

    Equations

    XM = Molar magnetic susceptibleness ( cgs units )

    C= Calibration changeless = 1.044

    L= Length of sample ( cm units )

    R= Balance reading with FULL samples tube

    Ro= Balance reading with EMPTY sample tubing

    M= Relative molecular weight of sample

    m= Mass of samples ( units gms )

    Ten ‘M = XM- ( diamagnetic rectification )

    Ten ‘M = Corrected Molar susceptibleness

    XM = Molar magnetic susceptibleness ( cgs units )

    Diamagnetic rectification = Calculated from literature tabular array of diamagnetic corrections ( Xd )

    µeff= Magnetic minute ( units Bohr Magneton ( BM ) )

    Ten ‘M = Corrected Molar susceptibleness

    T= Temperature ( units Kelvin ( K ) )

    Calculations

    XM = 294.0798111 x10-6

    Diamagnetic rectification ( informations obtained from Inorganic Chemistry CMB004 d-block Chemistry Laboratory class 2009-10 page 14 )

    Compound: [ Ni ( PPh3 ) 2Cl2 ]

    Diamagnetic rectification = ( -13 x10-6 ) + ( -46 x10-6 ) + ( -400 x10-6 ) = -459 x10-6

    Ten ‘M = XM- ( diamagnetic rectification )

    Ten ‘M = 294.079811×10-6 – ( – 459 ) x10-6 = 753.079811×10-6

    µeff =1.33 BM

    Complex B showed a magnetic minute lessening of -055 to -073 on the first measuring so I re ran the measuring.

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