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Caroline Wozniacki's wait for a first grand slam title goes on after she was beaten 6-1 6-7 6-3 by Kaia Kanepi in the French Open third round.
The Dane has had a poor year, dropping from world number one to number nine, but had looked in decent form in her opening two matches at Roland Garros.
Kanepi, a powerful Estonian seeded 23rd, had far too much for Wozniacki for most of the first two sets, while the 21-year-old also lost her cool, vociferously disputing a line call with both the umpire and then the supervisor.
But from 6-1 5-1 Kanepi began to get tense and Wozniacki let loose, saving two match points in the eighth game of the second set and then fighting back to take it on a tie-break.
She could not carry the momentum into the decider, though, and again found herself trailing 5-1.
Kanepi missed one more match point when she served a double fault, but this time there was no way back for Wozniacki, the Estonian finally getting the job done on her fifth chance after two minutes short of three hours.
Wozniacki, who has recently begun working with former Australian Open champion Thomas Johansson, said: "It's disappointing to lose, especially in a round like this. Of course I'd hoped for more but it wasn't possible this time.
"I definitely fought to the end, I didn't give up and I can be happy with that. But it wasn't enough."
The 21-year-old pulled no punches in her criticism of the officials, saying: "When the ball is clearly out, I don't think there should be anything to argue about.
"If they cannot see, they should have other umpires on the lines or have HawkEye on these courts. It's a disgrace that mistakes like this are made."
There will be no third French Open final in a row for Italy's Francesca Schiavone, who lost to Varvara Lepchenko on Saturday.
The 14th-seeded Italian was beaten in a three-hour epic by Lepchenko.
Lepchenko came from a set down to post a 3-6 6-3 8-6 victory, one which is likely to earn her a place on the US Olympic team.
Schiavone, who beat Sam Stosur in 2010 then lost to Li Na last year, took the first set reasonably comfortably but was pegged back by Lepchenko.
The third set was a topsy-turvy affair, with the American serving for the match at 5-3 only for Schiavone to level, but Lepchenko broke again and then saved four break points on her own serve before finally taking it 3-6 6-3 8-6.
The Ukraine-born player's win leaves Venus Williams' Olympic hopes in doubt. The ranking cut-off point to determined Olympic places comes at the conclusion of the French Open.
Lepchenko will now play Wimbledon champion Petra Kvitova for a place in the quarter-finals.
Kvitova survived a test in the third round, eventually getting past Nina Bratchikova 6-2 4-6 6-1.
The Czech has a tendency to be erratic and, after powering through the first set, she found herself trailing 5-1 in the second to her Russian opponent, who is ranked 109th in the world.
Kvitova always looked to have too much power and quality, though, and, although she could not save the set, she was relatively untroubled in coming through the decider.
The 22-year-old is much more of a force on faster surfaces and will be looking to reach the quarter-finals at Roland Garros for the first time.
Defending champion Li Na, meanwhile, rallied from a set down to defeat American Christina McHale 3-6 6-2 6-1.
The seventh seed from China needed almost two hours on a sunsoaked Court Suzanne Lenglen at Roland Garros to see off the world number 36.
Li struggled with her serve in the early stages and went a break down in sixth game before immediately breaking back.
But McHale was making the most of her superior pace and broke again to take the opening set after 48 minutes.
Li upped her game in the second set, finding better angles to open up a 4-1 lead and a second break enabled her to level the match.
She then reeled off five games in a row in the decider to wrap up the victory and set up a last-16 meeting with Kazakh qualifier Yaroslava Shvedova, a 6-4 7-5 winner over Carla Suarez-Navarro.
Second seed Maria Sharapova was never troubled as she eased past Peng Shuai to reach the last 16.
The Russian won 6-2 6-1 and has dropped only five games in three matches so far, having beaten Alexandra Cadantu 6-0 6-0 and Ayumi Morita 6-1 6-1 in the previous rounds.
She will now take on Czech Klara Zakopalova, the conqueror of another seeded Russian in Anastasia Pavlyuchenkova, for a place in the quarter-finals.
Sharapova made a perfect start on Saturday, converting her second break point in the opening game.
She won again on the Peng serve but the Chinese player immediately clawed back one of the breaks to trail 3-1.
That became 4-2 before an unplayable deep forehand set up the first of two break points for Sharapova as she moved within one game of winning the set at 5-2, then served out for the set.
Even Sharapova's sometimes fragile serve was consistent, with a first-serve percentage of 61% through the match and only one double fault.
And she again broke at the first opportunity in the second set and led 4-0 before the 28th seed got a game on the board.
It was her only one, though, with Sharapova closing out a 66-minute victory with the minimum of fuss.