Sania and Raina were down 1-8 in the Super Tie break but reeled off seven straight points to make it 8-8 but lost the next two points to make an exit from the Games.
Sania Mirza, who is making a record fourth Olympic appearance, and debutant Ankita Raina are going into the Tokyo Olympics without playing a single competitive match together this year
In women's doubles, the Indian pair of Sania Mirza and Ankita Raina will face the Kichenok twins -- Nadiia and Lyudmyla -- of Ukraine in the opening round.
Sania is set to become the only female athlete to have represented India at four Olympics when she takes to the court along with talented youngster Ankita Raina
Mirza, who has returned to grass court Grand Slam after three years, and Mattek-Sands lost 4-6 3-6 to the Russian pair of Elena Vesnina and Veronika Kudermetova in one hour and 28 minutes.
Sania will now become the first female athlete to represent India at four Olympics when she features at the Tokyo 2020, slated to get underway from July 23 while Ankita Raina will be making her debut at the showpiece event.