Are you using the Res Fix mod to run the game at a different resolution?
If so, it disables the game's default screenshot key(s), you have to use the PrintScreen key instead.
Be aware though that some users have had issues with the game crashing when using the PrintScreen key, even if the rest of the Res Fix is working perfectly. I don't know if anyone has ever figured out why. If you are using Res Fix I would recommend loading a single mission or one of the tutorials and trying out the PrintScreen key to make sure you don't have any problems using it, just in case. That way if there is a problem you won't have crashed in the middle of a career patrol.
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