A win in the 4x200m freestyle race ahead of the USA and Australia and a new Games record in the men's trap shooting final from Nathan Hales, 28, took Team GB's gold medal tally to four.
It was a dazzling floor routine, including a double straight somersault by Biles, the most decorated gymnast in history, that sealed a gold medal for the US, three years after she had pulled out of events at the Tokyo Games following a mental health crisis.
The US team coach had spoken of this being a 'redemption tour' following a silver in Tokyo and the crowd in the Bercy arena roared its approval of Biles' final dangerously difficult routine set to music by Taylor Swift and Beyonce even before she landed alast aerial assault that pushed Italy into silver, Brazil into bronze and Great Britain heartbreakingly into fourth.
Biles had suffered from "the twisties", a traumatic mental block that caused the American to lose herself in the air whenever she attempted to twist, but she was laughing along with her teammates Jade Carey, Jordan Chiles, Sunisa Lee and Hezly Rivera last night, and soaked up the adoration from a raucous crowd.
The British gymnast Becky Downie, 32, said: "We did everything we possibly could. We went for broke.
To be that close in such a big comp is really hard but hopefully these guys will be back and have more finals." There had been much better news earlier in Paris for Team GB with Nathan Hales, 28, setting an Olympic record in the men's trap competition to win a third gold medal of the Games for Britain, beating the silver medallist, Qi Ying of China.
"I just try and keep everything as we always do and treat it exactly the same way I treat finals in training", the 28 year old from Chatham said.
Team GB's swimmers - James Guy, Tom Dean, Matt Richards and Duncan Scott, also retained their gold medal in the 4x 200m freestyle race ahead of the USA and Australia.
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