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If it is a toxic relationship then you really wouldn't want to do them a favor in the first place. Also, no one should get mad because they hear the word "no".
You're right. Anyone should be able to wait for your answer because after all they are the ones asking you for something? They can't assume that you're going to jump up and do them a favor the instant they ask you.
I like being able to leave people with something positive. The "Sandwich Approach" is a good idea. This is the nice way to say "no".
It seems that the important thing here is to take care of yourself. If you want to say "no" and you don't, you're definitely not putting yourself first.