Synthesis of nickel complexes

Synthesis of nickel complexesAbstractThe purpose of this experiment was to investigate the Ligand exchange that occurs when different Nickel complexes and reacted with Triphenylphosphine.IntroductionTriphenylphosphine was firstborn fain by Pfeiffer and Sauvage in 1904ExperimentalTriphenylphosphine (1.408g) was dissolved beneath reflux with Propan-2-ol (15cm3) forming a colourless resultant to which 5 simmering chips were added. Nickel chloride hexahydrate (0.603g) was dissolved in autocratic Ethanol (10cm3) and heated until a green/yellow solution formed. This solution was poured into the reaction mixture through the condenser. Immediately the solution turned dark green, the solution was refluxed for a further 6mins. The reaction was removed from the heat and allow to cool for 4mins, a dark precipitate was visible in the flask. The warm solution was filtered under suction to collect the dark blue/green crystals which were washed with ice cooled absolute ethanol (1x10cm3 + 1x3cm3 ). at once dry the boiling chips were removed with a spatula and the crystals were transferred to a n open sample vial and dried in the desiccator for a week.A further solution of Triphenylphosphine (1.410g) and Propan-2-ol (15cm3) was made and set to reflux as before. 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 condenser. Immediately the solution turned blood red/brown. The solution was refluxed for a further 7mins and then cooled for 5 mins. The warm solution was filtered under suction and the orange/ red crystals washed with ice cooled Ethanol ( 1x10cm3 + 1x8cm3). Once dry the boiling chips were removed as before and the crystals were transferred to the desi ccator for a week.Results and discussionTriphenylphosphine + Propan-2-ol+ Nickle Chloride hexahydrate + Ethanol Bis(triphenylphosphine)nickel(II)chlorideP(C6H5)3 + C3H7OH + NICl2.6H2O + C2H5OH C36H30Cl2NiP2Triphenylphosphine + Propan-2-ol+ Nickle Chloride hexahydrate + Ethanol Bis(triphenylphosphine)nickel(II)chlorideP(C6H5)3 + C3H7OH + NaSCN + C2H5OH + Ni(H2O)6(NO3)2 Ni(PPh3)2(NCS)2EquationsXM = Molar magnetic susceptibility (cgs units)C= Calibration constant = 1.044L= aloofness of sample (cm units)R= Balance reading with FULL samples tubeRo= Balance reading with EMPTY sample tubeM= Relative molecular cant over of samplem= Mass of samples (units grams)XM = XM- (diamagnetic correction)XM = Corrected Molar susceptibilityXM = Molar magnetic susceptibility (cgs units)Diamagnetic correction = Calculated from literature table of diamagnetic corrections (Xd)eff= Magnetic moment (units Bohr Magneton (BM))XM = Corrected Molar susceptibilityT= Temperature (units Kelvin (K))Calculations XM = 294.0798111 x10-6Diamagnetic correction (data obtained from Inorganic Chemistry CMB004 d-block Chemistry laboratory course 2009-10 page 14)Compound Ni(PPh3)2Cl2Diamagnetic correction = (-13 x10-6) + (-46 x10-6) + (-400 x10-6) = -459 x10-6XM = XM- (diamagnetic correction)XM = 294.07981110-6 -(- 459) x10-6 = 753.07981110-6eff =1.33 BMComplex B showed a magnetic moment decrease of -055 to -073 on the first measurement so I re ran the measurement.