Pulse Program Code for Bruker: ;teo_selhsqmbcto ;2D proton-selective HSQMBC-TOCSY experiment ;for the measurement of the smagnitude and the sign of long-range ;proton-carbon coupling constants #include #include #include "p2=p1*2" "d4=1s/(cnst2*4)" "d11=30m" "d20=p3" "d0=3u" ;"in0=inf1/2" "DELTA1=50u+p16+d16" "DELTA2=d4-larger(p12,p14)/2-50u-p16-d16" "DELTA=p16+d16+50u+p2+d0*2+50u" "FACTOR1=(d9/(p6*115.112))/2+0.5" "l1=FACTOR1*2" 1 ze d11 pl12:f2 2 d1 pl1:f1 3 (p1 ph1) 50u UNBLKGRAD p16:gp6 d16 DELTA2 pl0:f2 pl0:f1 4u (center (p12:sp2 ph1) (p14:sp3 ph6):f2 ) 4u DELTA2 pl2:f2 pl1:f1 50u p16:gp6 d16 p28 ph1 (p1 ph2) (p3 ph3):f2 d0 (p2 ph5) d0 50u p16:gp1*EA d16 pl0:f2 d12 (p24:sp7 ph14):f2 DELTA pl2:f2 (p3 ph4):f2 50u p16:gp4 d16 if "cnst25==0" { (p1 ph2):f1 } else { (p1 ph1):f1 } 50u p16:gp5 d16 DELTA2 pl0:f2 pl0:f1 if "cnst25==0" { (center (p12:sp2 ph1) (p14:sp3 ph1):f2 ) } else { (p12:sp2 ph1) } 4u DELTA2 pl2:f2 pl1:f1 50u p16:gp5 d16 (p1 ph1):f1 ;starts tocsy d12 pl10:f1 4 p6*3.556 ph22 p6*4.556 ph24 p6*3.222 ph22 p6*3.167 ph24 p6*0.333 ph22 p6*2.722 ph24 p6*4.167 ph22 p6*2.944 ph24 p6*4.111 ph22 p6*3.556 ph24 p6*4.556 ph22 p6*3.222 ph24 p6*3.167 ph22 p6*0.333 ph24 p6*2.722 ph22 p6*4.167 ph24 p6*2.944 ph22 p6*4.111 ph24 p6*3.556 ph24 p6*4.556 ph22 p6*3.222 ph24 p6*3.167 ph22 p6*0.333 ph24 p6*2.722 ph22 p6*4.167 ph24 p6*2.944 ph22 p6*4.111 ph24 p6*3.556 ph22 p6*4.556 ph24 p6*3.222 ph22 p6*3.167 ph24 p6*0.333 ph22 p6*2.722 ph24 p6*4.167 ph22 p6*2.944 ph24 p6*4.111 ph22 lo to 4 times l1 5u pl0:f1 300u gron0 p13:sp4:f1 ph7 100u groff d16 ;end tocsy 4u pl1:f1 p1 ph1 DELTA1 (p2 ph1):f1 50u p16:gp2 d16 BLKGRAD if "cnst25==0" { (p3 ph1):f2 } else { d20 } go=2 ph31 d1 mc #0 to 2 F1EA(igrad EA, id0 & ip3*2 & ip6*2 & ip31*2) exit ph1=0 ph2=1 ph3=0 2 ph4=0 0 2 2 ph5=0 ph6=0 ph7=0 ph14=0 0 2 2 ph22=3 ph24=1 ph31=0 2 2 0 ;pl0 : 120dB ;pl1 : f1 channel - power level for pulse (default) ;pl2 : f2 channel - power level for pulse (default) ;pl10: f1 channel - power level for TOCSY-spinlock ;sp2: f1 channel - shaped pulse for selective proton refocussing ;sp3: f2 channel - shaped pulse (180degree inversion) ;spnam3: Crp60,0.5,20.1 ;sp7: f2 channel - shaped pulse (180degree refocussing) ;spnam7: Crp60comp.4 ;sp29: f1 channel - shaped pulse (adiabatic) ;p1 : f1 channel - 90 degree high power pulse ;p2 : f1 channel - 180 degree high power pulse ;p3 : f2 channel - 90 degree high power pulse ;p6 : f1 channel - 90 degree low power pulse ;p12: f1 channel - 180 degree shaped pulse [20-80ms] ;p13: f1 channel - 180 degree shaped pulse (adiabatic) [20 msec] ; smoothed chirp (sweepwidth, 20% smoothing, 10000 points) ;p14: f2 channel - 180 degree shaped pulse for inversion ; = 500usec for Crp60,0.5,20.1 ;p24: f2 channel - 180 degree shaped pulse for refocussing ; = 2msec for Crp60comp.4 ;p16: homospoil/gradient pulse ;p28: f1 channel - trim pulse ;d0 : incremented delay (2D) [3 usec] ;d1 : relaxation delay; 1-5 * T1 ;d4 : 1/(4J)XH ;d9 : TOCSY mixing time ;d11: delay for disk I/O [30 msec] ;d16: delay for homospoil/gradient recovery ;l1: loop for DIPSI cycle: ((p6*115.112) * l1) = mixing time ;cnst2: = J(XH) [6-8 Hz] ;cnst17: = -0.5 for Crp60comp.4 ;cnst25: = 0 (IP) ; = 1 (AP) ;inf1: 1/SW(X) = 2 * DW(X) ;in0: 1/(2 * SW(X)) = DW(X) ;nd0: 2 ;NS: 2 * n ;DS: >= 8 ;td1: number of experiments ;FnMODE: echo-antiecho ;use gradient ratio: ;gpz0: ca. 3% ;gpz1: 80% ;gpz2: 20.1% for C-13 ;gpz4: 50% ;gpz5: 17% ;gpz6: 33% ;use gradient files: ;gpnam1: SINE.100 ;gpnam2: SINE.100 ;gpnam3: SINE.100 ;gpnam4: SINE.100 ;gpnam5: SINE.100 ;gpnam6: SINE.100