Re: COLOC on AC spectrometers

From: Strelenko Yuri A. (strel@cacr.ioc.ac.ru)
Date: Thu Aug 10 2000 - 03:25:49 PDT


Christopher Groombridge wrote:

> Dear Bruker users, Could someone advise on the reality of using COLOC long-range
> carbon-proton correlation on an AC-type Bruker spectrometer? (Unfortunately the
> world of inverse detection and gradients is in a parallel universe). I have the
> COLOC.AU microprogram, and I have tried to follow the parameter choice in "100
> Basic NMR Experiments". The sequence starts to acquire, but appears to hang
> midway through NE=3 (out of 128). I have tried setting the evolution parameter,
> D2=50 ms, which is more than enough for incrementation (IN=200). Am I missing
> something? I would be grateful for experiences. Chris GroombridgeForensic
> Science Service109 Lambeth RoadLondon

Dear Christopher,
    Please, look below variant of COLOC pulse program. We use it many last years.
You are needed to adjust only 45, 90, 180 pulses and decoupler power.

        With best wishes and kind regards, Yuri Strelenko.
================================================
; COLOCS.AU
; X-H SHIFT CORRELATION BY LONG-RANGE COUPLING
; AND WITH H-H DECOUPLING.(SEE ALSO COSYDEC.AU)
; KESSLER ET AL, J.MAGN.RES. 57, 331 (84)
; with TANGO-pulse train before and suppression PT throuh
; one bond coupling using BIRD - pulse train
; (see Magn.Reson.Chem. 1987, v. 25, N10, p.837)
;(c) 1991 by Yu.A.Strelenko (modifications ).

; 1H: D1-45-D4-180-D4-45-D0-180- (D2-D0) -90-D3-90-D4-180-D4-90-D3-BB
; X: -180- -180- -90- -180- -FID
; ------------TANGO-------------COLOC-----------------BIRD-----------
; F2=X-NUCLEUS SHIFTS, F1=1H SHIFTS
; PARTICULARLY GOOD FOR not only QUATERNARY CARBONS

1 ZE
2 D1 S1 DO ;1H RELAXATION, SET DEC. FOR PULSING
3 D4 P5:D PH7 ;
  (P2 PH4 D4):D (P4 PH5) ;TANGO-pulse train
  P5:D PH8 ;
4 (D2) (D0 P2 PH1):D (D0 P4 PH5) ;EVOLUTION OF H SHIFTS
5 (P1 PH2 D3):D (P3 PH3) ;POLARIZATION TRANSFER
  (P1 PH7 D4):D ;
  (P2 PH4 D4):D (P4 PH5) ;BIRD pulse sequence
  P1:D PH7 ;
6 D3 S2 ;second part of REFOCUSSING DELAY
7 GO=2 PH6 BB ;ACQUIRE WITH DEC.
8 D3 DO ;GATE DEC. OFF
9 WR #1 ;STORE FID
10 IF #1 ;INCREMENT FILE NUMBER
11 IN=1 ;LOOP FOR NEXT EXPERIMENT
   EXIT

PH1=B0 B0 B1 B1 B2 B2 B3 B3
PH2=B0 B0 B0 B0 B0 B0 B0 B0
    B1 B1 B1 B1 B1 B1 B1 B1
    B2 B2 B2 B2 B2 B2 B2 B2
    B3 B3 B3 B3 B3 B3 B3 B3
PH3=A0 A0 A0 A0 A0 A0 A0 A0
    A1 A1 A1 A1 A1 A1 A1 A1
    A2 A2 A2 A2 A2 A2 A2 A2
    A3 A3 A3 A3 A3 A3 A3 A3
PH4=B1 B3
PH5=A1 A3
PH6=R0 R0 R2 R2 R0 R0 R2 R2 R2 R2 R0 R0 R2 R2 R0 R0
PH7=B0
PH8=B2

;The optimum D2 = 1/(2J) = 4*D3. { D2=90ms(or 60ms), D3=20ms }
;D4 = 1/(2J), one bond X-H coupling {D4=3.3ms}
;P1,P2=90,180 FOR 1H {7.7 and 15.4 us}
;P3,P4=90,180 FOR X {9.7 and 19.4 us}
;P5 = 45 for H1 {3.6 us}
;S1=1H for pulsing
;S2 = 24H with MOD = 1 (P9 = 110 us).
;ND0=2 BECAUSE OF ECHO TECHNIQUE
;NS=4*N
;PW=0, RD = 3u
;D0=IN/2, SW1=SW(H)/2

--
*********************************************************************
|   Dr. Yuri A. Strelenko        |                                  |
|   N.D.Zelinsky Institute       |    Fax     (7-095) 135 5328      |
|   of Organic Chemistry,        |    Tel     (7-095) 135 9094      |
|   Leninsky prospect 47,        | e-mail    strel@nmr1.ioc.ac.ru   |
|   117913 Moscow B-334,         |                                  |
|          Russia                |                                  |
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