Villarreal ended Barcelona's unbeaten run in the league this year to book their place in next season's Champions League.
In a fixture in which both teams went for it until the end, Villarreal came out on top, beat Barcelona 3-2 to confirmed their fifth-place finish, and consequently and Champions League slot.
The Yellow Submarines opened the scoring through Ayoze Perez, but Barcelona through Lamine Yamal and Fermin Lopez, respectively, took a 2-1 lead.
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However, Marcelino's side did a comeback of their own, equalising, and then scoring a winner, to open an eight point gap on Real Betis in 5th, with one game left to play.
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Key match details
Villarreal opened the scoring through Ayoze Perez, who scored with a low shot inside the post just three minutes in, capitalising on a swift counterattack. However, this only seemed to energise the hosts. Fermín Lopez had two early chances, including a point-blank save from Luiz Junior, before Barcelona eventually equalised.
Lamine Yamal equalised with his trademark on the 38-minute mark, curling the ball into the far corner. The teenager's skill almost yielded a second goal shortly after, but Fermín sealed the win with a well-taken goal in first-half injury time.
After Santi Comesana's exquisite chip over Marc-Andre ter Stegen early in the second half to restore parity, Villarreal pushed forward, and the game became end-to-end. Despite dominating possession, Barcelona remained vulnerable to long balls. In the end, Tajon Buchanan sealed Villarreal's win with a composed finish in the box, marking Ter Stegen’s return with three goals conceded.