Barcelona's hopes of an unbeaten LaLiga campaign were ended in their penultimate game as they lost 5-4 at Levante.
The champions had gone 36 matches unbeaten but trailed 5-1 after 56 minutes and their dramatic fightback came up short.
Emmanuel Boateng's treble and Enis Bardhi's brace put lowly Levante in charge, and despite Philippe Coutinho completing his hat-trick and Luis Suarez scoring a penalty, Barca's bid for history came up short.
⏰ Full time in the Ciutat de Valencia stadium
Levante UD 5-4 FC Barcelona
⚽ Boateng (3), Bardhi (2) / Coutinho (3) and Suárez
The other team from Barcelona also scored four goals on Sunday, but Espanyol were celebrating a 4-1 victory over relegated Malaga.
The home side took the lead after just eight minutes when Gerard Moreno slotted in from close range and Sergio Garcia doubled the lead from a similar distance on 27 minutes.
Leo Baptistao then swept home on the half-hour mark to finish off an excellent team goal, before Malaga pulled one back from the penalty spot through Adrian Gonzalez after Naldo had been harshly punished for handball.
Espanyol were also awarded a dubious penalty after 79 minutes when Pablo Piatti went down under a challenge from Roberto Rosales, Piatti converting the spot-kick himself.