Champions Barcelona suffered a shock defeat at the hands of Real Mallorca as their title celebrations fell a little flat.
Atletico Madrid moved into pole position to secure the final UEFA Champions League berth with a crucial success over top-four hopefuls Valencia.
And it was a big day at the foot of the Primera Liga with crucial home victories for Numancia, Sporting Gijon, Real Betis, Espanyol and Racing Santander.
Barcelona's status as champions had been confirmed before their surprise 2-1 defeat at Real Mallorca .
Pep Guardiola named a much-changed side but saw his charges go in front in the 10th minute courtesy of Samuel Eto'o, before missing a series of opportunities to put the game to bed.
Mallorca made the hosts pay in the second half as Juan Arango fired home a spectacular free-kick before Cleber Santana glanced home a second 12 minutes from time.
Eto'o was awarded a questionable injury-time penalty after tumbling in the box, but drilled his spot-kick against the foot of the post before the final whistle sounded.
Atletico Madrid edged ahead of Valencia in the battle for the fourth and final UEFA Champions League berth with a priceless 1-0 home victory.
Diego Forlan scored the only goal of the game from the penalty spot in the 30th minute after Sergio Aguero tumbled theatrically over goalkeeper Cesar.
Atletico had a host of second-half chances but could not find a way beyond Cesar again, while Aguero was booked for diving, much to the Valencia No.1's satisfaction.
Relegation scrapNumancia jumped off the bottom - dumping Recreativo Huelva at the foot of the table - after a 1-0 victory over their rivals.
The game exploded into life late on when Iago Bouzsn conceded a penalty after fouling Gorka Brit in the area.
Three Recreativo players were then booked, including Andres Lamas, who had to walk after receiving his second yellow card.
When order was restored, substitute Jose Barkero stepped up to net the winner from the spot a minute from time to leave Numancia now just two points from safety.
Sporting Gijon also remain in the drop-zone - but now only on goal difference - after an equally crucial home victory over Malaga.
The hosts took the lead through Autet Gerard in the 24th minute, before Robson Weligton equalised 14 minutes later.
But Miguel Helder Rosario netted into his own goal after 53 minutes to seal the victory for the home side, who are now only behind Osasuna on goal difference.
Marching orders
Real Betis maintained their three-point gap on the drop zone with a 2-0 home victory over Almeria.
Mark Gonzalez put the hosts ahead with a sixth-minute opener before Jose Manuel Chico received his marching orders for the visitors after a professional foul on 20 minutes.
Almeria then held out until the 65th minute before an Arturo Arzu goal put the issue beyond doubt.
Espanyol also eased their relegation fears with a crucial 1-0 home victory over Athletic Bilbao.
Fernandez Luis Garcia netted the all-important winner from the penalty spot in the 70th minute after Carlos Gurpegui had fouled.
Meanwhile, Racing Santander leap-frogged Valladolid in the table after edging a five-goal thriller.
Oscar Serrano put the hosts ahead on five minutes before Manuel Victor (14) and Henok Goitom (22) put Valladolid in front.
But the visitors lost Jauregi Inaki Bea for a second bookable offence early in the second period before goals from Jonathan on 60 minutes and Nikola Zigic with four minutes to go sealed the win for the hosts.
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Primera Liga round-up
Primera Liga round-up
