Coco Gauff's Olympic singles campaign ended in tears as the teenager lost in straight sets to Donna Vekic.
Gauff, the world number two, was one of the favourites to claim singles gold in Paris, but will instead have to try her luck in the doubles after crashing out in the third round.
The American lost 7-6 (9-7) 6-2 on Tuesday in a contest in which she clashed with chair umpire Jaume Campistol towards the end of the match.
A Vekic return had been called out by a line judge, with Gauff having not kept the ball in play, but Campistol believed the shot had landed in and handed the Croatian the point and a 4-2 lead.
Play was subsequently delayed as an emotional Gauff approached the umpire, saying: "I never argue these calls. But he called it out before I hit the ball.
"It's not even a perception; it's the rules. I always have to advocate for myself.
"It always happens here at [Roland-Garros] to me. Every time. This is like the fourth, fifth time it's happened this year."
Gauff felt she was on the harsh end of a decision in the semi-finals of the French Open earlier this year, in a defeat to Iga Swiatek.
Data Debrief: Vekic a worthy winner
Despite Gauff's complaints, she was not at her best, and Vekic deserved the victory.
Vekic struck 28 winners in total to Gauff's nine, as she claimed the first top-10 scalp of her career on clay.
It is the second time in the space of two Olympic Games that Vekic has ousted a top-three player, having defeated Aryna Sabalenka in Tokyo.
France set up Olympics quarter-final with Argentina following New Zealand win
France set up a quarter-final meeting with Argentina at the Paris Olympics after topping Group A with a comfortable 3-0 win over New Zealand in Marseille.
Thierry Henry's side remain the only side in the tournament to win all of their games so far, and made light work of their opponents on Tuesday.
Jean-Philippe Mateta, who captained the side with Alexandre Lacazette on the bench, started off the scoring after the ball bundled its way into his path before finishing beyond Alex Paulsen in the 19th minute.
In a game that saw Les Bleus accumulate 34 shots at the Orange Velodrome, their dominance was rewarded with two quickfire goals late on.
Desire Doue would double the hosts' advantage from close range, with Arnaud Kalimuendo rounding off the scoring three minutes later to see France remain perfect.
France's triumph saw them win their first three games at the Games for the first time in their history, while also keeping three clean sheets on the spin for the first time at the Olympics.
In the other Group A encounter, the United States qualified for the knockout stages of the tournament for the first time since 2000 as they eased to a 3-0 win over Guinea.
A rampant start to the encounter saw Djordje Mihailovic and Kevin Paredes have Marko Mitrovic's two goals to the good just after the half-hour mark.
Despite finishing the encounter with just 37.8% possession, the United States were clinical in the final third as Paredes put the game beyond doubt in the 75th minute.
They return to action this Friday when they face Group B winners Morocco, who clinched top spot with a 3-0 win over Iraq while also finishing ahead of Argentina.
Swiatek eases to Paris Olympics quarter-finals
Iga Swiatek eased to the quarter-finals of the Paris Olympics as she beat Wang Xiyu in straight sets.
Swiatek, who has claimed four grand slam titles on the clay surface at Roland-Garros, continued her dominance on Tuesday as she emerged a 6-3 6-4 victor.
Wang started the match confidently, moving the world number one around the court early on, but Swiatek found her rhythm, earning a decisive break point in the sixth game before cruising to the first set.
The top seed managed to find a break in the opening game of the second set, but that lead proved difficult to maintain as Wang broke back instantly to take the next two games on the spin.
Swiatek, however, broke for a 3-2 lead and held her serve in the following game, but Wang continued to put on the pressure, winning her next two games to level the game.
The Pole would find yet another break of serve in the ninth game and was able to hold out to secure her passage to the quarter-finals in the French capital.
Swiatek will face Danielle Collins in the next round.
Data Debrief: Swiatek fights off inspired Wang
While the scoreline looked comfortable for Swiatek, it was far from it on Court Philippe-Chatrier.
In the opening set, Swiatek had 11 unforced errors compared to Wang's eight, while also hitting only nine winners.
But in a game filled with break points, Swiatek showcased her ruthless streak, converting four and saving six of the eight she faced.
Alcaraz and Nadal survive scare to reach Olympics doubles quarter-finals
Rafael Nadal and Carlos Alcaraz survived a scare to keep their quest for gold alive as they advanced to the quarter-finals of the Paris Olympics.
The Spanish duo were pushed all the way by Dutch pairing Tallon Griekspoor and Wesley Koolhof, but emerged 6-4 6-6 (2-7) 10-2 victors on Court Suzanne-Lenglen.
Nadal exited the singles following a defeat to long-time rival Novak Djokovic, but started impressively as the pairs exchanged rallies in the opening exchanges.
But a break in the seventh game for the Spaniards saw them assume full control of the first set, with Alcaraz serving out the final game to hold the early advantage.
However, Griekspoor and Koolhof would respond, with the Dutch pair able to dominate a second-set tiebreak, taking the encounter to an exciting conclusion.
But Nadal and Alcaraz would roar to victory, securing their passage to the next stage in the deciding third set after Griekspoor slammed an Alcaraz serve into the net.
Next up for the all-star Spanish duo is a clash with fourth-seeded Americans Rajeev Ram and Austin Krajicek.
Data Debrief: Nadalcaraz continue to shine
The combination of youth and experience worked to its full effect at Roland-Garros, with Nadal and Alcaraz once again showing their gold medal credentials.
Nadal and Alcaraz saved all three of the break points they faced, ending the contest by winning 81% of their first serve points.
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