User:Ellen Petersen/Notebook/MOF/2013/07/05

MOF: Ellen

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PPF-18 & PPF-20 1.) Add solids 5,10,15,20- Tetrakis(4-carboxyl)-21H,23H-porphine (TCPP) (.0079 g, .01 mmol),Zinc nitrate hexahydrate (.0089 g, .03 mmol, N,N’-di-(4-pyridyl)-1,4,5,8-naphthalenetetracarboxydiimide (DPNI) (.0042 g, .01 mmol)to small capped vial 2.) Add 1.0 M nitric acid (50 μL, .05 mmol) in ethanol, N,N-diethyl formamide (DEF)(1.5 mL),Ethanol (0.5 mL) 3.) Sealed and Sonicated to ensure homogeneity 4.) Heated to 80° C in an oven for 24 hours followed by a slow cooling to room temperature for 9 hours (Program 2) 5.) Add solids to a second vial 5,10,15,20- Tetrakis(4-carboxyl)-21H,23H-porphine (TCPP) (.0079 g, .01 mmol),Zinc nitrate hexahydrate (.0089 g, .03 mmol, N,N’-di-(4-pyridyl)-1,4,5,8-naphthalenetetracarboxydiimide (DPNI) (.0168 g, .01 mmol)to small capped vial 6.) Add 1.0 M nitric acid (30 μL, .05 mmol) in ethanol, N,N-dimethyl formamide (DMF)(1.5 mL),Ethanol (0.5 mL) 7.) Sealed and Sonicated to ensure homogeneity 8.) Heated to 80° C in an oven for 24 hours followed by a slow cooling to room temperature for 9 hours (Program 2) _____________________________________________________________________________________________________________________________________________ 07-08-2013 9.) Vacuum Filtration 10.) Very few crystals of PPF-18, not even enough for Powder X-Ray Diffraction sample. 11.) Took Powder X-Ray Diffraction of PPF-20 (See Image Below)