Most of the answers so far (lsof, sync, etc. ) seem to have missed the fact that the OP rebooted the box after deletion. Since no process or file handle will survive that, let me ask:

Is there any reason that there could be hard links on this volume?  Some backup systems use those for files that don't change between backup runs. Apple's Time Machine is one example of a system that does such, but there are many others. 

Using find or ls -l paired with egrep, check for hard links. You won't get the disk space back until the last link to a file has been rm'd. 

Let us know what the ultimate solution is, please.

Thanks!
Thomas 

On May 21, 2012, at 4:45 PM, B-o-B De Mars <mr.chew.baka at gmail.com> wrote:

> On 5/21/2012 4:42 PM, Shawn Fertch cried from the depths of the abyss:
>> If you do an lsof against the directory, what processes do you see running?
> 
> If i lsof the dir the contained the dir I deleted it is showing smbd.  I restared it a couple times.  No change.
> 
> I think I'm just going to let it be for now, and check it in the morning.
> 
> Thanks to all who replied!
> 
> Mr. B-o-B
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