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The soundtrack. Specifically, the legendary Firefly intro.
The unbelievably beautiful and sad music during the funeral at the end of "The Message". Even more so when you know that the composer was afraid it was too sad, because he wrote it to mourn the death of the series.
Music in "Safe", where Simon is prepared to die with his sister.
The Hero of Canton, the man they call Jaaaaaayne!
The theme for Jubal Early, aka the Evil Oboe of Evilness from "Objects In Space".
The wonderfully upbeat village dance music during River's dance scene both highlighted one of River's first true moments of lucidity and happiness as well as providing great background for the simultaneous gunbattle. Its one of the best parts of the show and gives the viewer the feeling of the universe in one minute-long scene. Oh, and it gives us an awesome pun: Riverdance. And Simon's proud look.
Firefly Inara's theme is peaceful, elegant, and incredibly gorgeous.
In "The Train Job" when Mal, Zoe and Jayne are in a bar fight and they pull out a gun on the crew and then Wash comes and saves them with Serenity. Greatest entrance ever.
"River's Perception / Saffron", the first part of which is a perfect representation of the show's resident Ophelia and the second part is a spot-on character theme for the titular Manipulative Bitch.
"Captain & Ship" from "Out Of Gas"; a gorgeous, sweeping love theme for Mal and Serenity, highlighting that the ship really is the tenth character in the series and Mal refuses to leave her.
The introductory scene of the Reavers gives us this. And it is awesomely menacing as you see that first Reaver ship in the series loom up out of nowhere.
and Firefly both have decidedly awesome soundtracks composed by Greg Edmonson and David Newman, respectively.
Serenity "Mal Fights Niska / Back Home" from "War Stories".
"Reavers Chase Serenity" from the pilot.
The end credits for Serenity, the tail end of which features an instrumental Theme Tune Cameo for Firefly.