Defending champion, Serena Williams, followed sister Venus out of the French Open on a dramatic fourth day.
Serena lost 6-2 6-2 to Spain's Garbine Muguruza after Venus' poor run of form continued with a 2-6 6-3 6-4 by Slovakian Anna Schmiedlova.
The 17-time grand slam champion never got into her stride against the 20-year-old world No 35.
Top seed Williams had not been knocked out of a grand slam before the fourth round since losing in the first round of the 2012 French Open.
The 32-year-old American made 29 errors and just eight winners in a 64-minute defeat that means she will not add to her Grand Slam titles.
Muguruza had her powerful groundstrokes and pace around the court proving too hot for Williams to handle.
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The 2013 champion’s defeat was her worst in terms of scoreline in her 16-year grand slam career and will send shockwaves through the tournament, which lost Australian Open champions Stan Wawrinka and Li Na in the first round last Monday
It is the first time in her career that Serena has failed to reach the second week of a Grand Slam as the top seed.
Venus, 33, had earlier made a strong start before losing eight of nine games on her way to defeat by 19-year-old Schmiedlova on Court Philippe Chatrier.
It means a projected third-round clash between the Williams sisters will now feature Muguruza and Schmiedlova.