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The Greek mathematician Archimedes was the first to approach the subject mathematically. He came to the conclusion that pi (the constant that was at the center of the relationship) had a value somewhere between 223/71 en 22/7. The average was 3,141851. Pretty close. Later a Chinese mathematician called Liu Hui came even closer with a better approximation.

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Q: Who discovered the relationship between the diameter and circumference of a circle?
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