Novak Djokovic blamed mental and physical exhaustion after another desperate day for the Serbian at the Olympic Games meant he will leave Tokyo empty-handed.
The world number one lost 6-4 6-7 (6-8) 6-3 to Pablo Carreno Busta in the singles bronze medal match, smashing one racket against a net post and tossing another into the stands in gestures of frustration.
Djokovic then cited a shoulder injury as he pulled out of the mixed doubles third-place match. That decision meant Ash Barty and John Peers of Australia took bronze, with Djokovic and his unfortunate Serbia partner Nina Stojanovic finishing fourth.
"I am dealing with injuries. Not one, more than one," Djokovic said in an interview with Serbian media, according to tennismajors.com. "I hope that it won't stop me from going to the US Open, which is my next big goal.
"I feel bad for Nina because we did not fight for a medal in mixed, but my body said 'enough'. I have played under medications and abnormal pain and exhaustion."
The 34-year-old Djokovic said he had put his "very last source of energy" into the tournament and was satisfied with his effort, with a semi-final defeat to Alexander Zverev on Friday having left him resigned to a battle for what by his standards was perceived as a consolation prize.
But Djokovic added: "I know I've not played well today, and yesterday in the second and third set.
"The exhaustion, both physical and mental, got to me and it's unfortunate that in the most important matches I just didn't deliver, but I gave it all."
Djokovic suggested the Paris Olympics in 2024 were a possible target, although he must be becoming sick of Olympic tennis by now, having only one bronze to show for four attempts to win gold.
He took bronze in 2008 but lost to Argentina's Juan Martin del Potro both in the third-place match at London 2012 and the first round at Rio 2016.
Now there is more Games agony to digest, as well as a need to reboot ahead of the upcoming North American hardcourt swing and that US Open campaign. His hopes of a calendar Golden Slam are over but a sweep of the grand slams remains a possibility, having already landed the Australian Open, French Open and Wimbledon titles.
"I've had some heart-breaking losses at the Olympics Games," Djokovic said. "I know that those losses have usually made me stronger. I know that I will bounce back. I will try to keep going for the Paris Olympic Games. I will fight for my country to win medals."
Carreno Busta's reaction was thoroughly refreshing, with the Spaniard jubilant to secure a medal.
He said: "This week has been a very harsh week mentally for me. When I saw Novak lost, and I had to play him for this medal, I had my doubts.
"But last night I slept like I haven't slept in Tokyo. I slept for nine hours straight, that was an advantage to me. I came on to the court today knowing Spain was behind me.
"This is even more incredible than winning other tournaments. I've won Davis Cup, I've gone far in other tournaments, but winning an Olympic medal is indescribable. Words fail me, I felt Spain rallying behind me. A bronze medal is a dream come true for me."
The knock-on effort of Djokovic's withdrawal from the mixed doubles meant Barty and Peers added to Australia's medals haul without having to step on court for the third-place play-off.
Barty insisted she and Peers were worthy bronze medallists, saying: "It's incredible. It's unique circumstances and heartbreaking for Team Serbia not to get out on court.
"But for Johnny and I this is a dream come true for us. I feel like we've really deserved this one."
Sinner avoids O'Connell upset at US Open
Jannik Sinner beat Australia's Christopher O'Connell in straight sets to reach the fourth round of the US Open on Saturday, avoiding a similar fate to Carlos Alcaraz and Novak Djokovic.
The men's draw at Flushing Meadows has been blown wide open by early exits for Alcaraz and Djokovic, but the top seed remains in the hunt after a composed performance.
He reached the fourth round for a fourth consecutive year with a routine 6-1 6-4 6-2 victory, setting the tone with several huge groundstrokes in the opening set.
O'Connell never looked likely to fight back as Sinner smashed 46 winners in a ruthless performance, wrapping up his win in one hour and 56 minutes.
The Australian Open champion will face either Tommy Paul or Gabriel Diallo for a place in the last eight, and he was relieved to survive an opening week full of surprises.
"Everything can happen in this sport, so I try to stay on my side of the net and I'm trying to take the tournament day by day," Sinner said in his on-court interview after the win.
"Each opponent is a very tough challenge and [I am] also enjoying every moment on the court. There have been already a couple of upsets, so let's see what's coming.
"But I'm very happy to still be here and hopefully I can play as many matches as possible. But as I said, we go day by day and then we'll see how it goes."
Data Debrief: Sinner heating up
Sinner lost his first set of the tournament to Mackenzie McDonald but has been largely untouchable since then.
He has only lost 18 games across his last nine sets of tennis, an average of two per set.
The Italian's winning streak now stands at seven straight matches, meanwhile, following his triumphant Cincinnati Open run.
US Open: Sabalenka overcomes first set scare to progress in late start
Aryna Sabalenka came from a set down to keep her US Open dream alive as she beat Ekaterina Alexandrova in the early hours at Flushing Meadows.
Sabalenka emerged on court at the Arthur Ashe Stadium at seven minutes past midnight following Novak Djokovic's shock exit from the tournament, and consecutive upsets looked to be on the cards.
However, the Belarusian responded from a disappointing opening set as she looks to avenge her defeat in the showpiece match against Coco Gauff a year ago.
The world number two set up a meeting with Belgium's Elise Mertens as she emerged a 2-6 6-1 6-2 victor in one hour and 40 minutes in New York.
"I don't know what I did, I was just trying to stay low, put as many balls as I can back on that side," Sabalenka said.
"She played incredible tennis in the first set. It was really tough to change it."
"I'm really happy I was able to turn around this match and get this really difficult win. Thanks so much for staying that late."
Data Debrief: Sabalenka survives late, late show
Sabalenka's encounter with Alexandrova was the latest starting match at the US Open, beating Gabriela Sabatini and Beverley Bowes' meeting in 1987 that started at midnight.
The Belarusian, however, will be hoping for a much improved performance in the next round, having produced 27 unforced errors throughout the contest and serving four double faults.
US Open: Djokovic played 'worst tennis ever' in Popyrin loss
Defending US Open champion Novak Djokovic suffered a shock exit at Flushing Meadows as he lost in four sets to Alexei Popyrin.
Djokovic arrived at the tournament with confidence following his gold medal triumph at the Paris Olympics, and was tipped to lift a record-extending 25th grand slam title.
However, the Serbian's hopes of a fifth success in New York were dashed as he followed fellow favourite Carlos Alcaraz out of the competition in the third round.
Popyrin emerged victorious in three hours and 18 minutes, prevailing 6-4 6-4 2-6 6-4 to confirm Djokovic's earliest exit from the tournament in 18 years.
"I have played some of the worst tennis I have ever played," Djokovic said.
"Honestly, the way I felt and the way I played from the beginning of this tournament, third round is a success."
"I tried my best, I didn't have any physical issues. I just felt out of gas, and you could see that. From the first match, I just didn't find myself on this court.
"Life moves on. I'll try to recalibrate and look forward to what's next."
Data Debrief: Another one bites the dust
Djokovic was far from his clinical best, serving a career-high 14 double faults in a grand slam match and committing 49 unforced errors.
The Serbian will also end the year without winning a grand slam title, the first time he has done so since 2017.
But the day belonged to Popyrin, saving 12 of the 16 break points he faced against the world number two, finding particular success with his forehand as 31 of his 49 winners came from that shot.
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