Villarreal was eliminated on penalties by third-division club Unionistas on Monday in a Copa del Rey match which had been hit the day before by a power outage.
The third-round match was suspended before the start of extra time on Sunday. The teams drew 1-1 in regulation and neither side scored again in extra time on Monday. Unionistas won 7-6 in the shootout to reach the round of 16 when it will host Barcelona.
The only other topflight club to lose to a lower-division club in this round was Las Palmas, which lost 2-0 to second-division team Tenerife on Sunday.
Real Betis lost 1-0 to Alaves in a match between first-division clubs on Saturday.
Defending champion Real Madrid advanced past fourth-division team Arandina 3-1 on Saturday, while Atletico Madrid beat third-tier team Lugo 3-1. Barcelona edged fourth-division side Barbastro 3-2 on Sunday.
Madrid, Atletico, Barcelona and Osasuna made their Copa debuts in this round.
Madrid will play at city rival Atletico in a standout fixture of Monday’s round-of-16 draw. Osasuna will host Real Sociedad, Valencia is set to face Celta Vigo and Sevilla will have a trip to Getafe.
Also, it’s Athletic Bilbao vs. Alaves, Girona vs. Rayo Vallecano and Tenerife vs. Mallorca.
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