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Rafael Nadal is out of the US Open after he was beaten by France's Lucas Pouille 6-1 2-6 6-4 3-6 7-6.
The two-time champion looked to be heading into the quarter-finals when he moved a break ahead in the fifth set, but Pouille recovered to take the set into a tie-break, which he won with his fourth match point.
Nadal found himself 4-2 ahead in the deciding set in Arthur Ashe Stadium, but Pouille broke back, winning four of the next six games to set up a tie-break. Sensing an upset Pouille moved 6-3 ahead only for Nadal to save three match points.
However, facing match point for the fourth time, Nadal missed a simple forehand as Pouille booked his place in the quarter-finals.
"It took everything," Pouille said. "It is my first match on the centre court against Rafa. I couldn't dream better than this.
"With three match points I thought, 'you are going to win this one'. At 6-6, I was not the same. Honestly I am the most happy in this tournament.
"It is never over until the last point. I was a break down in the fifth, I came back. It is never finished until the last point is over."
Nadal has struggled with a wrist injury in recent months and the 14-time grand slam winner admits he is missing something from his game.
"I need something else. I need something more that was not there today. I'm going to keep working to try to find," Nadal said.
"But, yes, it was a very, very close match where anything could happen. I just congratulate the opponent that probably he played with better decisions than me the last couple of points.
"Mental or physical doesn't matter. I am out of the tournament. Physical, for sure, no. I fight till the end. Of course it was not a physical thing.
"It was not a mental thing. It was sport and in sport you lose or you win. The opponent wants to win the same, like you."
Pouille will play compatriot Gael Monfils in the next round.
Elsewhere, world number one Novak Djokovic ended Kyle Edmund's run at Flushing Meadows.
Djokovic was never really troubled by his opponent, dropping just seven games, on his way to a 6-2 6-1 6-4 win.
Having come through a tough opening match, Djokovic was given a walkover into the third round before his opponent was forced to retire early but he was pleased to be given a test as he prepares for a quarter-final meeting with Jo-Wilfried Tsonga.
"It feels great to play a match. The first complete match I played was a first-round night session," Djokovic said.
"Now a fourth round, after a weird couple of rounds. I'm really glad to be back. I thought I came out of the blocks and played high intensity.
"I want to wish Kyle the best. He is only 21 and playing his first Arthur Ashe match, so he deserves applauds."
In the women's draw, Angelique Kerber defeated two-time Wimbledon champion Petra Kvitova to book her place in the last eight.
Kerber overcame Kvitova 6-3 7-5 to set up a meeting with last-year's runner-up Roberta Vinci, while Caroline Wozniacki beat eighth seed Madison Keys 6-3 6-4 to progess to the quarter-finals.
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