Barcelona were made to wait for the Primera Liga title following a 3-3 draw with Villarreal at Camp Nou.
After closest rivals Real Madrid lost to Valencia on Saturday evening, Pep Guardiola's men went into their match well aware that success would secure a 19th league crown.
But the UEFA Champions League and Copa del Rey finalists disappointed their expectant home supporters, who are eager for a memorable treble triumph, as they threw away a 3-1 first-half lead.
Seydou Keita opened the scoring in the 11th minute after firing in with his left foot from the side of the area.
But Joseph Llorente then silenced the Catalan on 22 minutes as he slotted a close range equaliser for Villarreal, who hold Champions League aspirations with three games remaining.
Barca's star striker Samuel Eto'o, however, restored Barca's lead nine minutes before half-time following good work from Andres Iniesta, and Daniel Alves then added a third from a free-kick in first-half injury time.
Guardiola's side's were rocked in the second half as a 78th minute Matias Fernandez penalty - after Eric Abidal, who was dismissed at Chelsea in midweek, was sent off for fouling Nihat - set up a nervy finish.
And then in time added on at the end of the match Llorente latched onto a long ball to net a dramatic, scrappy equaliser to put Barca's celebrations on hold.
Ten-man Atletico Madrid came back from two goals down at half-time to record a dramatic 3-2 win against flailing Espanyol at the Vicente Calderon.
The Champions League hopefuls were facing an uphill challenge after 32 minutes when Luis Perea was sent off, and a Nene penalty (38) and Daniel Jarque (40) goal quickly added to the home side's problems.
But eight minutes after the interval Atletico grabbed a lifeline as Diego Forlan netted an excellent goal before Sergio Aguero scored an equaliser on the hour-mark.
Atletico then bombarded the goal of Espanyol, who are not safe from relegation, and Forlan sparked wild celebrations as he hit the winner in the second minute of injury time.
At the other end of the table, 10-man Getafe boosted their survival hopes with a thumping 3-0 home win over fellow strugglers Osasuna.
Esteban Molina (27 and 50) hit a brace, with the opener from the penalty spot, while Ikechukwu Uche added a third (54) before Gonzalez Adrian was sent off on the hour-mark.
Recreativo Huelva remain in the relegation zone following a 2-1 home defeat to Deportivo La Coruna, who hold a faint chance of qualifying for the European Cup.
Joan Verdu opened the scoring for Deportivo in the 17th minute, but Perez Colunga pulled one back for the home side one minute before half-time.
Deportivo, though, secured the victory four minutes after the interval as Nunez Alvarez netted.
Sporting Gijon also remain in the bottom three after throwing away the lead in a 3-1 defeat at Almeria.
Gonzalez Carmelo put Sporting in front in the 16th minute, but Miguel Nieto (27) Kalu Uche (55) and substitute Pablo Piatti (90) completed the turn around.
Numancia remain rock bottom and four points from safety after a 0-0 draw at Valladolid.
Racing Santander are still not safe from the drop after losing 1-0 at Malaga as Albert Martos struck the only goal of the game from the penalty spot on 88 minutes.
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