#include ;hnco-3D to measure Co cross-correlation by doublet intensity ;written by NT 1/17/97 adapted by AB from hncaX-ge by abx ;added cpd decoupling of C' during aq 08/21/99 ; !!! edit /u/exp/stan/nmr/lists/f1/offtemp.gc with O1 val. (water) ;p1 = 90 deg (10us) 1H pulse @pl1 ;p18 = 90 deg (1ms) 1H pulse @pl18 ;p10 = pcpd1 90 H (64us) at pl10 H1 composite decoupling cpdprg1 is waltz16 ;pl11 = pl10-6db (6dB more power for temp. comp.) ;update fq1 with water O1 if you set O1 on water, otherwise leave it @8ppm! ;p2 = 90 deg (50us) 15N pulse @pl2 ;pcpd2 = nitrogen 90 at pl31 for decoupling (cpdprg2 is WALTZ16) ;p4 = selective 180 deg (23.7u*2@600, 19.2u*2@750) CA pulse @pl4 ;pl0= pl8= pl6= 120 dB to preset shape on C ;p6 = 180 deg (191.7us=180deg@600, 150u@750) CO pulse @sp1 using sinc1.0 ;p6 = 90 deg (191.7us=90deg@600, 150u@750)) CO pulse @sp2 using sinc1.0 ;p8 = 180 deg (500us=180deg@600, 400u@750) CA pulse @sp8 using hsec.3 ;pcpd3 low power dec on CO (p90=200u, set to 173.6@750) @pl30 (cpdprg3 is garp) #define NITRO #define C_O ;#define CALIBRATE ; uncomment to calibrate N15 hard 90 #define EXPTCORR ; uncomment if you want "expt" to report ; the correct exp. time (works with XWIN-NMR 2.x) ;Define channel assignments: #define H f1 #define N f2 #define C f3 ; o3p 177p, fq3list: caco.f3 define pulse H1_180 define pulse N15_180 define pulse CA_180 "H1_180=p1*2" "N15_180=p2*2" "CA_180=p4*2" #ifdef CALIBRATE "p12=N15_180" ;should give null signal for p2 exactly 90 degrees #else "p12=p2" #endif "d2=2.65m" "d5=12.5m-5.405m" "d11=50m" "d12=1m" "d26=p2-p1" "d27=l6*0.5*in0+10u" ; in27 = in0/2, use 6dB more power (pl11=pl10-6dB) "d28=p8*0.5-p2" "d29=0.5*p6-p2" "d30=CA_180+10u" ;Gradient pulses (may have to be set manually): "p20=0.4m" "p21=1.1m" "p22=1.0m" "p23=1.0m" "p24=200u" "p25=77us" ;optimize -> max signal with uncommmented 5.4m refocus delay! "p26=2.705m" "p28=0.7m" "p29=1.3m" "d3=d2-p22" "d4=d2-p23" "d6=0.25m-p24-20u" "d7=0.25m-p25" "d8=d1-50u" "d13=5u" ; short delay for EXPTCOR (faexptcorr.incl) ;"d0 = in0 -p6*0.55 -p8*0.5 -2.5u" ;"d0 = in0 -p6*0.55 -p8*0.5 -2.5u -50u" "d0 = in0*1.5 -p6*0.55 -p8*0.5 -2.5u -50u" ; LP 1 pt., phase -90/180 ;"d22=10.5m" ;"d22=16m" ;d22 =16m for in22 = 200u and 64 incs "d22=10.5m" ;d22 =10.5m for in22 = 150u and max. 71 incs "d25=10u" ;in25 = 312u (=in24+in22) "d24=10u" ;in24 = 162u ;"d23=16m-d24-p6-p26-1m-CA_180-d25" "d23=d22-d24-p6-p26-1m-CA_180-d25" #ifdef EXPTCORR "d31=p20+p21+p28+p29+2*(p22+p23)+p24+p25+p26" ; "d31=p20+p21+p28+p29+2*(p22+p23)" #endif 1 ze d12 RESET 10u 99 240u pl18:H (p18 ph0):H 240u (p18 ph9):H lo to 99 times 2000 10u 2 10u do:N 10u do:C 10u pl11:H 10u fq1:H d27 cw:H ;dec comp delay 10u do:H 10u fq1:H 3m ;grad. flip delay d11 3 d12*3.0 4 d12*3.0 5 d12*3.0 6 50u do:N 7 5u do:C 50u fq3:C ;switch to CA 10u pl4:C #ifdef EXPTCORR #include #endif d8 LOCK_ON 1m LOCK_OFF 10u pl1:H 10u pl2:N ;------- start 90-degree on N to get rid of boltzmann --------- ;(p2 ph7):N (p4 ph0):C (p2 ph7):N (p4 ph0):C 2u p20:gp1 ;GRAD20(cnst20) ;G1,25,0.4,x/y 950u 50u fq3:C ;switch to CO ;------- start 90-degree on hn ----------------------- (p1 ph0):H d2 (d26 H1_180 ph1):H (N15_180 ph8):N d2 (p1 ph2):H 4u p21:gp2 ;GRAD21(cnst20) ;G2,25,1.1,y 1m (p2 ph7):N ;-------------- end inept to N ---------------------- 5.4m pl10:H 5u cpds1:H d5 pl0:C (p6:sp1 ph0):C (d29 N15_180 ph7):N 12.496m 4u ;do:H (p12 ph7):N 2u p28:gp3 ;GRAD28(cnst20) ;G3,25,0.7,y/z 500u pl0:C ;------------- start evolution on CO --------------------------- (p6:sp2 ph10):C 50u fq3:C ;switch to CA 5u pl0:C d0 (p8:sp8 ph0):C (d28 N15_180 ph7):N 50u fq3:C ;switch to CO d0 (p6:sp2 ph11):C 5u do:H p29:gp4 ;GRAD29(cnst21) ;G4,15,1.3,y 0.5m pl1:H (p1 ph6):H ;purge pulse 5u pl0:C ;--------------- start CT evolution on N ------------------- (p2 ph7):N ; uncomment next 2 lines for S/N test ; 5.4m ; for in-phase, test, comment for spectrum ; 100u do:H d22 pl1:H (N15_180 ph7):N ;set back to ph7!!!!!!!!!!!!! d24 (p6:sp1 ph0):C d23 ;pl4:C p26:gp5*EA ;GRAD26(cnst26) ;G5,+/-25,2.705,z 50u fq3:C ;switch to CA 50u pl4:C 900u (CA_180 ph0):C d25 (p2 ph9):N (d26 p1 ph0):H ;--------- end CT evolution on N -------------------- 2u p22:gp6 ;GRAD22(cnst21) ;G6,15,1.0,x d3 (d26 H1_180 ph0):H (N15_180 ph7):N 2u p22:gp6 ;GRAD22(cnst21) ;G6,15,1.0,x d3 (p1 ph1):H (p2 ph8):N 2u p23:gp6 ;GRAD23(cnst21) ;G6,15,1.0,x d4 (d26 H1_180 ph0):H (N15_180 ph7):N 2u p23:gp6 ;GRAD23(cnst21) ;G6,15,1.0,x d4 (d26 p1 ph0):H 4u p24:gp7 ;GRAD24(cnst24) ;G7,25,0.2,z 20u fq3:C ;switch to CO d6 pl30:C (H1_180 ph0):H 2u p25:gp8 ;GRAD25(cnst25) ;G8,-25,0.0756,z d7 pl31:N 2u cpd3:C (2u ph0) 5u BLKGRAMP go=2 ph31 cpd2:N 10u do:N 10u do:C 10u pl11:H 10u fq1:H d27 cw:H ;dec comp delay 10u do:H 10u fq1:H 1m LOCK_ON d11 wr #0 if #0 zd #ifdef NITRO 3m igrad EA d12*0.5 ip9 d12*0.5 ip9 lo to 3 times 2 d12 dd22 d12 id24 d12 id25 lo to 4 times l4 ;N15 max. l4 is (d22/in22)+1 d12*0.5 rd22 d12*0.5 rd24 d12*0.5 rd25 #endif #ifdef C_O d12 ip10 lo to 5 times 2 d12 id0 d12 dd27 d12 ip31 d12 ip31 lo to 7 times l6 ; #endif d12 d12 do:C d12 do:N exit ph0=0 ph1=1 ph2=1 ;3 ph6= 0 ph7=0 ph8=1 ph9=2 ph10=0 2 ph11=0 ph3=0 ph4=2 ph31=0 2