Water, or other inaccessible terrain.
Aquatic/amphibious critters can really mess with a party. Riddle the area with underground tunnels full of water. Don't be afraid to drag/grapple PCs into the water.
Poor-man's version in a dungeon is little tunnels that only small critters can fit through easily. Little Kobold/goblin commandos popping in an out to harass people can really drive them nuts. Tossing out bear traps or caltrops is always fun.
Poorer-man's version is a 3D environment, like a city, + monsters with climb speeds or flying. That can combo pretty well with the small tunnels. Also, that can help to shorten visible ranges for casters and shooters. Long, straight lines are usually better for the PCs than the monsters.
I've had reasonable luck tempting the party into blowing all their abilities with feints. That is, enemies show up, maybe fire an arrow or two. Then, after everybody turns on their rages and the like...they beat feet. You might loose a few, but keep it up and wear them down. Remember to Move-attack-move, the OA is better than taking a full attack.
The biggest thing, IME, is don't fight in open terrain. Monsters really need to use cover, darkness, drowning, cliffs, etc. to make the most of it. Especially don't forget things like grappling, pushing, etc. NEVER have monsters just march up to the PCs, if you can avoid it...that's a recipe for challengeless slaughter. (I suppose if you want a slaughter, go ahead.)
Second biggest thing, but also goes with that. Do anything you can to trickle-out the fight and make it last longer. (Waves are awesome, but terrain can make it work also.) Turn the fight into a chase, if you can. That gives the Players a chance to get frustrated, and burn more slots/abilities on lesser foes.
Also, IMO, the encounter guidelines are pretty useless. I mean, its good for sorta keeping the XP stuff in line with expectations, but not much else as far as difficulty goes. Heck, even CR doesn't seem to mean much.