Post 2: Cyanopyridine Study part 1

Cyanopyridine Study

(4NCPy)5Cu4I4

Authentic samples of the compound were made using the KI method which involves making a 5mL solution of 5M KI and dissolving 1.5mmol CuI then slowly pipetting 1mL of a 5M KI solution with 2mmol 4NC-Py dissolved. Resulting solid was filtered, washed, and put on vac line.
Crystals of the (4NCPY)5Cu4I4 compound were grown by dissolving CuI and 4NCPy in acetonitrile and layering with ether. When run on the X-ray diffractometer these crystals gave the following structure:

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Comparisons of the powder pattern of the authentic sample to the theoretical powder pattern given by the single crystal solution gave a very convincing match as show above:

 

(3NCPy)4Cu4I4

Authentic samples of the compound were made using the KI method which involves making a 5mL solution of 5M KI and dissolving 1.5mmol CuI then slowly pipetting 1mL of a 5M KI solution with 1.5mmol 3NC-Py dissolved. Resulting solid was filtered, washed, and put on vac line.

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Crystals of the (3NCPY)4Cu4I4 compound were grown by dissolving CuI and 3CNPy in acetonitrile and layering with CH2Cl2. When run on the X-ray diffractometer these crystals gave the following structure

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Comparisons of the powder pattern of the authentic sample to the theoretical powder pattern given by the single crystal solution gave a very convincing match as show bellow:

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(3NCPy)4Cu2I2

Authentic samples of this compound were made by dissolving 5mmol of 3CNPy in 5mL of acetonitrile, and dissolving 1mmol of CuI into 10mL acetonitrile. Then CuI solution added dropwise into the acetonitrile solution. Resulting solid was filtered, washed, and put on vac line. The photos below depict this powder under room light as well as under black light

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Crystals of the (3NCPY)4Cu2I2 compound were grown by dissolving CuI and 3CNPy in acetonitrile and layering with ether. When run on the X-ray diffractometer these crystals gave the following structure

 

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Comparisons of the powder pattern of the authentic sample to the theoretical powder pattern given by the single crystal solution gave a very convincing match as show bellow:

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AA was run on all the bulk samples, the results of which are summarized in this table

Compound Cu mass % Theoretical Cu mass %
(4NCPy)5Cu4I4 20.37 pg22 19.8
(3NCPy)4Cu4I4 21.98 pg29 21.6
(3NCPy)4Cu2I2 18.25 pg22 16.0