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Have removed cooler etc. Used Kryonaut paste.
Now running a few degrees cooler than before.
It's stable at 4.1, haven't had time to take it further. When I do, I'll try sneaking it up to 4.5 and only then will I try again with that offset stuff.
Thanks for the help so far guys
Iain
The Kryonaut paste (which is fantastic) is not your problem, your problem is your Freezer 7, which you should not be overclocking with. It really is awful. I have one. Not on my main machine though. Get a Hyper 212 or one of the new competing Cryorig coolers if you want proper cooling performance.
With the Kryonaut paste you should be fine for 4.5ish on your current setup with that Freezer 7 but don't carry it over to your next build or anything.
I wouldn't bother with offset voltage. With most 2500K's I just set vcore to 1.35 and use whatever level of LLC I need to actually get 1.35 in Windows, multiplier to 45, BCLK 100, and stress test. If it passes with flying colours gradually decrease vcore by .005 (1.35, 1.345, 1.34, etc), again applying the LLC required to get what you put into the bios to read true in windows, and keep going down until you find the vcore where you crash or bluescreen, then go back to the last "fully stable" vcore and you'll have a properly tweaked OC. On the other hand if your machine fails @1.35/4.5Ghz, gradually increase vcore by .005 until stable.
BTW if this isn't a 2500K you've had for 7 years and just never OC'd, and is, rather, a previously enjoyed 2500K you bought on the cheap, remember that it has likely been abused the crud out of and has likely degraded. They're tough, but they do degrade.