Ian Thorpe saw his dream of a freestyle treble disappear as Pieter van den Hoogenband took gold in the 100m final.
The Australian superstar, after his gold medals in the 400m and 200m, still claimed a superb bronze from lane eight, his fourth medal of the Games.
South African Roland Mark Schoeman went out hard but had to settle for silver, six hundredths of a second adrift.
Van den Hoogenband, the defending champion, won in 48.17secs, with Schoeman touching in 48.23.
Schoeman had qualified fastest for the final and reached the halfway stage in 22.60, more than half a second under world record pace.
But Van den Hoogenband, who was fifth after the first 50, timed his run to perfection, edging past the South African in the final two strokes.
"I'm not sure when I caught him, I was in a kind of trance, in a flow, doing my job and not thinking," said the Dutchman.
"I'm so happy, really. I was touching the wall and the camera was zooming in and I'd won. It's great."
Thorpe, who scraped into the final as the eighth qualifier, had a slow start and was sixth when he turned for home, but surged through to edge out South African Ryk Neethling for the bronze.
"I guess I have the set (of medals) now," said Thorpe. "I didn't think that
was going to happen, but I'm really happy with my swims here."