;;Dimensionality: 4 ;;Experiment: zaNH ;;Phaseoverlap: 0000 ;;trosy: 0 ;;DimProjections: 2 ;;Hfreq: BF1 ;;Cfreq: BF2 ;;Nfreq: BF3 ;;Carrier1: CNST 7 ;;Carrier2: CNST 30 ;;Carrier3: O3P ;;Carrier4: O1P ;;----------------end header------------------ ;set USERA5: 4D zaNH st ;Conventional name: 4D-APSY-HACANH ;shiller, 2004, optimized 5/2005 ;modified for manageapsy: Fred Damberger ETH ZH 11/2007 ;**************************************************************** ;* * ;* The following one-letter codes for the nuclei are used: * ;* * ;* HA = Z w1 w * ;* CA = A w2 x * ;* N = N w3 y * ;* H = H w4 z * ;* * ;* * ;* The angles are defined as: * ;* * ;* alpha between y and x * ;* beta between xy and w * ;* * ;* * ;**************************************************************** ;pl1 : power for 1H hard pulse ;pl2 : power for 13C hard pulse [not used] ;pl3 : power for 15N hard pulse ;pl9 : power for H2O presat ;pl11 : power for 1H DIPSI2 decoupling ;pl13 : power for 15N WALTZ decoupling ;p1 : 90 degree hard pulse 1H ;p2 : 180 degree 1H ;p3 : 90 degree hard pulse 13C ;p4 : 180 degree 13C ;p5 : 90 degree hard pulse 15N ;p6 : 180 degree 15N ;p11 :180 deg, [350u] reburp_128 sp11 ;p15 : 180 deg, [220u] iburp1_128 sp15 ;p25 : purge pulse 1m ;pcpd1 : 90 degree cpd-pulse 1H (DIPSI2, 80us) ;pcpd3 : 90 degree cpd-pulse 15N (WALTZ, 160us) ;cpdprg1 : dipsi2 ;cpdprg3 : waltz16 ;p21 : 600u ;p22 : 800u ;p23 : 1000u ;gpz1 : 25 % ;gpz2 : 30 % ;gpz3 : 35 % ;gpz4 : 40 % ;gpz5 : 45 % ;gpz6 : 50 % ;gpz7 : 55 % ;gpz8 : 60 % ;gpz9 : 65 % ;gpz10 : 70 % ;gpz11 : 75 % ;gpz12 : 80 % ;d1 : relaxation delay ;d5 : 3-9-19-delay. 200/130u at 500/750MHz ;cnst1: alpha ;cnst2: beta ;cnst41: SW1 (HA) [Hz] ;cnst42: SW2 (CA) [Hz] ;cnst43: SW4 (N) [Hz] "cnst41=cnst41" "cnst42=cnst42" "cnst43=cnst43" ;cnst51: set to CNST7 HA [ppm] ;cnst52: set to CNST30 CA [ppm] ;cnst53: set to O3P N [ppm] ;cnst54: set to O1P H [ppm] "cnst51=cnst51" "cnst52=cnst52" "cnst53=cnst53" "cnst54=cnst54" ;cnst7: 1H carrier in HA ;cnst8: 1H carrier in amide region ;cnst29: CO chemical shift (offset, 174 ppm) ;cnst30: Ca chemical shift (offset, 53 ppm) ;sp11 : 180 deg, p11, reburp_128 ;sp13 : 180 deg, p13, BLOCK.32 ;sp14 : 90 deg, p14, BLOCK.32 ;sp15 : 180 deg, p15, iburp1_128 ;spnam11 : reburp_128 ;spnam13 : BLOCK.32 ;spnam14 : BLOCK.32 ;spnam15 : iburp1_128 #define GRADIENT1 10u p22:gp3 190u #define GRADIENT2 10u p22:gp7 190u #define GRADIENT3 10u p22:gp1 190u #define GRADIENT4 10u p22:gp5 190u #define GRADIENT5 10u p22:gp10 190u #define GRADIENT6 10u p22:gp4 190u ;----------------------offsets "p11=350*188.6198/bf2" ;350u @ 750MHz spectrometer "p13=866000/(bf2*(cnst29-cnst30))" "p14=968000/(bf2*(cnst29-cnst30))" "p15=220*188.6198/bf2" ;220u @ 750MHz spectrometer "spoff11=0.0" "spoff13=0.0" "spoff14=0.0" "spoff15=bf2*((cnst29-cnst30)/1000000)" "in11=abs(in1*sin(0.0174533*cnst2))/2" ; HA "in12=abs(in1*sin(0.0174533*cnst1)*cos(0.0174533*cnst2))/2" ;CA "in13=abs(in1*cos(0.0174533*cnst1)*cos(0.0174533*cnst2))/2" ;N "l3=td1/2" "p2=2*p1" "p6=2*p5" "d0 = 1.0m" ; dummy "in0= in1" ; dummy ;------------------------------basic delays "d2 = 2.7m" ; 1/4J H-N "d3 = 1.8m" ; 1HA-13CA inept delay "d6 = 4.75m" ; delay for 1H in-phase "d10=13.5m" ; 1/2J CA-CB "d12=11.0m" ; 1/2J CA-N ;----------------------fixed delays define delay IN_HN "IN_HN=d2-(p22+200u+p1*2.3846+d5*2.5)" define delay WGATE "WGATE=d5/2-p5" ;----------------------------indirect dimensions ;----------------------Z "d19 = d3-p22-210u-p13" "d18 = 10u" "d17 = d3-p22-200u" "in19= in11" "in17= (d17-20u)/l3" "in18= 0u" ;----------------------A "d23 = 10u" "d22 = d10-p15-p6-10u" "d21 = 10u" "d20 = d10-p15" "in23= in12" "in20= (d20-20u)/l3" "in21= 0u" ;----------------------N "d31 = d12" "d28 = 10u" "d16 = d12-p13-10u-d2*2" "d30 = d12-p13-10u" "d29 = d12-p13-10u-p15-10u" "in30=in13" "in31=(d31-20u)/l3" "in16=in30" "in28=0u" ;-------------------- #include 1 10u ze #ifdef A2 1m ip31 2m ip31 #endif #ifdef W 3m ip11 #endif #ifdef X 3m ip12 #endif #ifdef Y 3m dp13 #endif goto 20 10u d0 20 1m ;------------------------------------Switch constant-time for CA if "in20 < in23" goto 5 10u "in20=in23" 10u goto 6 5 1m 10u "in21=in23-in20" 10u 6 1m ;------------------------------------Switch constant-time for N if "in31 < in30" goto 9 10u "in31=in30" 10u goto 10 9 1m 10u "in28=in30-in31" 10u 10 1m ;------------------------------------Switch constant-time for HA if "in17 < in19" goto 11 10u "in17=in19" 10u goto 12 11 1m 10u "in18=in19-in17" 10u 12 1m ;-----------------------------------Start 2 5m LBLSTS1, 5m LBLF1, 5m 10u do:f3 10u LOCKH_OFF d1 50u fq=cnst7 (bf ppm):f1 50u fq=cnst30 (bf ppm):f2 20u pl1:f1 20u pl2:f2 20u pl3:f3 20u LOCKH_ON ;-----------------------------------------INEPT 1H13CA (p1 ph6):f1 GRADIENT1 d19 (p13:sp13 ph23):f2 d18 (p2 ph23):f1 GRADIENT1 d17 (p1 ph11):f1 ;-----------------------------------------z filter GRADIENT2 50u fq=0:f1 10u 10u pl11:f1 10u ;-----------------------------------------INEPT 13Ca15N (p14:sp14 ph12):f2 (d6 5u cpds1):f1 (d23 p15:sp15 ph20 d22):f2 (p6 ph20):f3 d21 (p11:sp11 ph8):f2 d20 (p15:sp15 ph20):f2 10u (p14:sp14 ph5):f2 ;-----------------------------------------zzz GRADIENT5 10u ;-----------------------------------------15N evolution (p5 ph13):f3 d31 (p6 ph20):f3 d28 (p13:sp13 ph20):f2 (d16 5u do 10u 10u pl1):f1 (d30):f3 (d29 p15:sp15 ph20):f2 (p5 ph7):f3 ;-----------------------------------------INEPT 15N1H 10u GRADIENT6 (p1 ph20):f1 GRADIENT4 10u IN_HN (p1*0.2308 ph21 d5 p1*0.6923 ph21 d5 p1*1.4615 ph21):f1 WGATE (p6 ph20):f3 WGATE (p1*1.4615 ph23 d5 p1*0.6923 ph23 d5 p1*0.2308 ph23):f1 GRADIENT4 IN_HN pl13:f3 10u LOCKH_OFF (p25 ph20):f1 ;-----------------------------------------acquisition go=2 ph31 cpd3:f3 30m do:f3 wr #0 if #0 zd #ifdef Pw 30u ip11 #endif #ifdef Px 30u ip12 #endif #ifdef Py 30u dp13 #endif lo to LBLSTS1 times 2 1m id19 1m id18 1m dd17 1m id21 1m id23 1m dd20 1m id16 1m dd31 1m id30 1m id28 lo to LBLF1 times l3 10u do:f1 10u do:f2 10u do:f3 10u LOCKH_OFF exit ;-------------------phases for phasecycle ph5 = 0 2 ph6 = 3 3 1 1 ph7 = 0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 ph8 = 0 0 0 0 1 1 1 1 ph31= 2 0 0 2 0 2 2 0 0 2 2 0 2 0 0 2 ;-------------------fixed phases ph20= 0 ph21= 1 ph22= 2 ph23= 3 ;-------------------phases for States-TPPI ph11= 0 ph12= 0 ph13= 0