Villarreal lost their unbeaten Primera Liga record as they crashed to a shock 3-0 defeat at home to Valladolid.
Manuel Pellegrini's side came into this game as the only remaining unbeaten side in the league, but were unable to recover from conceding three first-half goals to an impressive Valladolid outfit.
Jonathan Sesma gave the Valladolid the lead midway through the first half and doubled the visitors' advantage two minutes before the break.
Luis Prieto then added a third in injury time at the end of the first half to give Jose Luis Mendilibar's side an unlikely 3-0 lead at the interval and Villarreal were unable to respond in the second period.
Valladolid were thrashed 6-0 in their last away outing at leaders Barcelona two weeks ago, but restored some pride last weekend with an impressive 1-0 win at home to Real Madrid.
The tough sequence of fixtures continued at El Madrigal, but Valladolid were more than a match for the home side as they produced an impressive first-half display.
Following a tense opening with no real opportunities for either side, Sesma fired the visitors in front after 24 minutes, when he swept home Pedro Leon's pass after Victor Fernandez had seen his shot saved by Diego Lopez.
Villarreal took a while to settle after the goal, but almost equalized in the lead-up to half-time.
Marcos Senna came close with a powerful long-range effort after 37 minutes and Giuseppe Rossi saw his shot saved by Sergio Asenjo shortly afterward.
But Valladolid took advantage of those near misses after 43 minutes, when Sesma pounced on a loose ball following a mix-up in the Villarreal defense and fired his side into a two-goal lead.
Things then went from bad to worse for Villarreal, as Valladolid scored a third in first-half injury time.
Diego Lopez failed to clear Leon's free-kick and Prieto pounced to give Valladolid a barely believable three-goal lead at the break.
Two minutes after the interval, Chile forward Matias Fernandez - who also lost 3-0 at the same ground on Wednesday night as his national team went down in a friendly against Spain - almost made an instant impression after coming on at the break, but saw his effort athletically saved by Asenjo.
And shortly after that, Valladolid almost went four up when Fabian Cannobio found himself one-on-one with Diego Lopez, but Angel Lopez got back to make an important clearance.
Fernandez came close with a free-kick 10 minutes from time, but Villarreal were unable to break down a stubborn Valladolid rearguard and it proved to be a hugely frustrating evening for Pellegrini's side.
Villarreal's first defeat in the league means they will find themselves six points behind leaders Barcelona if the Catalans beat Getafe on Sunday.
Valladolid, meanwhile, climb provisionally to seventh place in the table, their highest position of the season.
