;written by beat vogeli 2006 ;3D MQ(1HN,13Ca)+SQ(1HN)-HNCA for measurement of 3J(HN,Ha) ;p1 = 90 deg 1H pulse @pl1 ;p7 = 90 deg 15N pulse @pl7 ;p4 = selective 180 deg (23.7*2us) 13CO and 13CA ;p5 = selective 90 deg (53u) 13CA ;Gradient Pulses ;p20 500u ;gpz0=+30 sine.50 ;p21 250u ;gpz1=-15 sine.50 ;gpz2=-10 sine.50 ;gpz3=+30 sine.50 ;p22 300u ;gpz4=+25 sine.50 ;p23 3400u ;gpz6=+50 rectangular.1 ;gpz7=-50 rectangular.1 ;p24 144.75u ;gpz0=-50 rectangular.1 ;p25 200u ;gpz0=+50 rectangular.1 "d10=in10*0.5" "d11=50m" "d12=2.6m" "d13=13.7m" "d16=13.01m" ; J(CaCb) refocusing "d17=13.5m" "d18=p25-p24" "d19=0.5*p5-0.5*p1" "d20=d17+in10*0.5-20u-200u-p23+2*p4" "d25=p11*0.5-p15*0.5" "d26=p7-p1" "d27=p7-p4" "d28=p4-p1" "d29=p14*0.5-p7" "d30=10u" "d21=d30" "d31=d16-3u" "d24=p1*3.141/2+p7*2+d21*2" "d22=d29+30u" "d23=d29-30u" ; J(HN) evolution correction "l1=1" "l3=32" ; 1/2 of number of points "l4=76" 1 ze 1m setnmr2^0 setnmr8^4 2 d11 1m setnmr2^0 3 3m setnmr8^4 4 3m setnmr2^0 5 3m 6 1m do:f2 do:f4 7 10u pl4:f5 d1 setnmr2^0 1m setnmr2|0 10u pl1:f1 10u pl7:f2 10u pl5:f4 ;------- Clean residual N and Ca ----------------------- (p7 ph20):f2 (p5 ph20):f4 20u p20:gp0 200u ;------- INEPT HN ----------------------- (p1 ph20):f1 d12 (d26 p1*2 ph20 d26):f1 (p7*2 ph20):f2 d12 (p1 ph1):f1 ;------- Z-filter Gradient ----------------------- 20u p22:gp2 200u ;------- INEPT NCa ----------------------- (p7 ph20):f2 3u d13 pl6:f4 pl14:f5 (p7*2 ph20):f2 (d27 p4*2 ph20 d27):f4 3u d13 pl5:f4 (p7 ph21):f2 ;------- Z-filter Gradient ----------------------- 20u p20:gp0 200u (d19 p1 ph2 d19):f1 (p5 ph3):f4 ;------- CT-(Ca,HN)MQ-Evolution ----------------------- 3u 10u (d22 p7*2 ph20 d23):f2 (p14:sp4 ph20):f5 d16 (d25 p15:sp5 ph20 d25):f4 (p11:sp1 ph7):f1 3u d31 pl5:f4 (d22 p7*2 ph20 d23):f2 (p14:sp4 ph20):f5 3u d30 (p5 ph20):f4 (d19 d24 p1*2 ph20):f1 ;------- (HN)SQ-Evolution ----------------------- d21 (p7*2 ph20):f2 d21 (p1 ph20):f1 ;------- Z-filter Gradient ----------------------- 20u p21:gp1 100u (p7 ph21):f2 ;------- CT-(f2)-SQ Evolution ----------------------- d10 (p1*2 ph20 d28 d28):f1 (p4*2 ph20):f5 d17 pl6:f4 (p7*2 ph20):f2 (d27 p4*2 ph20 d27):f4 d20 ;------- Coherence-Encoding Gradient ----------------------- if "l1==1" goto 88 20u p23:gp6 200u goto 89 88 20u p23:gp7 200u ;------- First Backtransfer Element ----------------------- 89 (p1 ph20):f1 (p7 ph20):f2 d12 (d26 p1*2 ph20 d26):f1 (p7*2 ph20):f2 d12 (p1 ph21):f1 if "l1==1" goto 78 (p7 ph4):f2 goto 79 78 (p7 ph5):f2 ;------- Second Backtransfer Element ----------------------- 79 d12 (d26 p1*2 ph20 d26):f1 (p7*2 ph20):f2 d12 (p1 ph20):f1 ;------- Coherence-Encoding Gradient ----------------------- d18 pl17:f2 20u pl18:f4 p24:gp4 100u (p1*2 ph20):f1 20u p25:gp5 100u ;------- Acquisition ----------------------- go=2 ph0 cpds2:f2 cpds3:f4 10u do:f2 do:f4 1m setnmr2^0 d11 wr #0 if #0 zd 10u iu1 lo to 3 times 2 10u ru1 10u id10 10u dd20 lo to 3 times l3 10u ip3 10u rd10 10u rd20 lo to 3 times 2 10u ip0 10u ip0 10u id30 10u dd16 ;------- kappa = 1 ----------------------- 10u id21 ;------- kappa = 2 ----------------------- ; 10u id21 lo to 3 times l4 1m do:f2 1m setnmr2^0 setnmr8^4 1m exit ph20=0 ph21=1 ph22=2 ph23=3 ;------- subspectrum A ----------------------- ph2= 0 0 2 2 ph3= 0 2 ;------- subspectrum B ----------------------- ;ph2= 1 1 3 3 ;ph3= 1 3 ph1= 1 1 ph4= 1 ph5= 3 ph7= 0 2 ph0= 0 2 2 0