Newly-crowned Wimbledon champion Carlos Alcaraz defeated Croatia's Borna Coric at the Hopman Cup but could not prevent Spain from crashing out of the rebooted team competition on Saturday.
World number one Alcaraz came through against Coric 6-3, 6-7 (6/8), 10-5.
However, Spain were eliminated from contention for the final when Rebeka Masarova was easily defeated by Donna Vekic 6-2, 6-1.
Spain had needed to beat Croatia 3-0 to have any chance of reaching Sunday's final to play Switzerland.
However, they also lost the mixed doubles with Alcaraz and Masarova slipping to a 1-6, 6-4, 14-12 defeat to Coric and Vekic.
Croatia go through to Sunday's final against Switzerland.