;;Dimensionality: 5 ;;Experiment: ZAONH ;;Phaseoverlap: 00000 ;;trosy: 0 ;;DimProjections: 2 ;;Hfreq: BF1 ;;Cfreq: BF2 ;;Nfreq: BF3 ;;Carrier1: CNST 7 ;;Carrier2: CNST 30 ;;Carrier3: CNST 29 ;;Carrier4: O3P ;;Carrier5: O1P ;;----------------end header------------------ ;USERA5: 5D ZAONH st ;Conventional name: 5D-APSY-HACACONH ;Sebastian Hiller, 2004-2007 ;adapted to manageapsy: Fred Damberger ETH ZH 11/2007 ;**************************************************************** ;* * ;* The following one-letter codes for the nuclei are used: * ;* * ;* HA = Z w1 v * ;* CA = A w2 w * ;* CO = O w3 x * ;* N = N w4 y * ;* H = H w5 z * ;* * ;* * ;* The angles are defined as: * ;* * ;* alpha between y and x * ;* beta between xy and w * ;* gamma between wxy and v * ;* * ;* * ;**************************************************************** ;pl1 : power for 1H hard pulse ;pl2 : power for 13C hard pulse ;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 ;p9 : 180 deg [220u@750MHz] iburp1_128 sp9 ;p11 :180 deg [350u@750MHz] reburp_128 sp11 ;p13 : 180 degree 13Cab (null@CO) sp13 ;p14 : 90 degree 13Cab (null@CO) sp14 ;p15 : 180 deg [220u@750MHz] iburp1_128 sp15 ;p19 : 180 deg [350u@750MHz] reburp_128 ;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: angle alpha 90=CO ;cnst2: angle beta 90=CA ;cnst3: angle gamma 90=HA all 0=N ;cnst21: SW1 (HA) [Hz] ;cnst22: SW2 (CA) [Hz] ;cnst23: SW3 (CO) [Hz] ;cnst24: SW4 (N) [Hz] "cnst21=cnst21" "cnst22=cnst22" "cnst23=cnst23" "cnst24=cnst24" ;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) ;sp9 : 180 deg, p9, iburp1_128 ;sp11 : 180 deg, p11, reburp_128 ;sp13 : 180 deg, p13, BLOCK.32 ;sp14 : 90 deg, p14, BLOCK.32 ;sp15 : 180 deg, p15, iburp1_128 ;sp16 : 90 deg, p16, BLOCK.32 ;sp17 : 180 deg, p17, BLOCK.32 ;sp19 : 180 deg, p19, reburp_128 ;spnam9 : iburp1_128 ;spnam11 : reburp_128 ;spnam13 : BLOCK.32 ;spnam14 : BLOCK.32 ;spnam15 : iburp1_128 ;spnam16 : BLOCK.32 ;spnam17 : BLOCK.32 ;spnam19 : reburp_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 "p13=866000/(bf2*(cnst29-cnst30))" "p14=968000/(bf2*(cnst29-cnst30))" "p16=968000/(bf2*(cnst29-cnst30))" "p17=866000/(bf2*(cnst29-cnst30))" "spoff9=bf2*((cnst30-cnst29)/1000000)" "spoff11=0.0" "spoff13=0.0" "spoff14=0.0" "spoff15=bf2*((cnst29-cnst30)/1000000)" "spoff16=0.0" "spoff17=0.0" "spoff19=0.0" "l1=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 = 4.7m-p1-20u" ; delay for 1H in-phase "d8 = 4.7m" ; 1/4J CO-CA "d9 =11.4m" ; 1/4J CO-N "d10=13.5m" ; 1/2J CA-CB "d12=11.0m" ; 1/2J CO-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= abs(in1*sin(0.0174533*cnst3))/2" "in17= (d17-20u)/l1" "in18= 0u" ;----------------------A "d22 = d8-p15" "d21 = d10-d8" "d20 = d10-p15-10u" "in22= abs(in1*sin(0.0174533*cnst2)*cos(0.0174533*cnst3))/2" "in20= (d20-20u)/l1" "in21= 0u" ;----------------------O "d27 = d9-d8-p6" "d26 = 10u" "in8 = abs(in1*sin(0.0174533*cnst1)*cos(0.0174533*cnst2)*cos(0.0174533*cnst3))/2" "in9 = (d9-20u)/l1" "in26= 0u" ;----------------------N "d31 = d12" "d28 = 10u" "d16 = d12-p17-10u-d2*2" "d30 = d12-p17-10u" "d29 = d12-p17-p9-20u" "in30=abs(in1*cos(0.0174533*cnst1)*cos(0.0174533*cnst2)*cos(0.0174533*cnst3))/2" "in31=(d31-20u)/l1" "in16=in30" "in28=0u" ;-------------------- #include define loopcounter ST1CNT "ST1CNT = td1 / (2)" 1 10u ze #ifdef A2 1m ip31 1m ip31 #endif #ifdef V 1m ip1 #endif #ifdef W 1m ip2 #endif #ifdef X 1m ip3 #endif #ifdef Y 1m dp4 #endif goto 4 d0 4 1m ;------------------------------------Switch constant-time for CA if "in20 < in22" goto 5 10u "in20=in22" 10u goto 6 5 1m 10u "in21=in22-in20" 10u 6 1m ;------------------------------------Switch constant-time for 13CO if "in9 < in8" goto 7 10u "in9=in8" 10u goto 8 7 1m 10u "in26=in8-in9" 10u 8 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 2 5m LBLSTS1, 5m LBLF1, 5m 10u do:f3 10u LOCKH_OFF d1 50u fq=cnst30 (bf ppm):f2 50u fq=cnst7 (bf ppm):f1 20u pl1:f1 20u pl2:f2 20u pl13:f3 20u LOCKH_ON ;-----------------------------------------INEPT 1H13CA (p1 ph6):f1 GRADIENT1 d19 (p13:sp13 ph23):f2 d18 (p2 ph23):f1 GRADIENT1 d17 (p1 ph1):f1 ;-----------------------------------------z filter GRADIENT2 50u fq=0(sfo hz):f1 10u 10u pl11:f1 10u 10u cpds3:f3 10u ;-----------------------------------------INEPT 13Ca13CO (p14:sp14 ph2):f2 (d6 p1 ph21 5u cpds1):f1 (d22 p15:sp15 ph20):f2 d21 (p11:sp11 ph20):f2 d20 (p15:sp15 ph20):f2 10u (p14:sp14 ph20):f2 ;-----------------------------------------zzz 10u do:f3 GRADIENT5 50u fq=cnst29 (bf ppm):f2 10u 10u pl2:f2 10u 10u pl3:f3 10u ;-----------------------------------------INEPT 13CO15N (p16:sp16 ph5):f2 d8 (p9:sp9 ph20):f2 d27 (p6 ph20):f3 d26 (p19:sp19 ph20):f2 d9 (p9:sp9 ph20):f2 10u (p16:sp16 ph3):f2 ;-----------------------------------------z filter GRADIENT3 ;-----------------------------------------15N evolution (p5 ph4):f3 d31 (p6 ph20):f3 d28 (p17:sp17 ph20):f2 (d16 5u do):f1 (d30):f3 (d29 p9:sp9 ph20):f2 (p5 ph20):f3 ;-----------------------------------------INEPT 15N1H GRADIENT6 10u 10u pl1:f1 10u (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 1m do:f3 wr #0 if #0 zd #ifdef Pv 10u ip1 #endif #ifdef Pw 10u ip2 #endif #ifdef Px 10u ip3 #endif #ifdef Py 10u dp4 #endif lo to LBLSTS1 times 2 1m id19 1m id18 1m dd17 1m id22 1m id21 1m dd20 1m id8 1m id26 1m dd9 1m id16 1m dd31 1m id30 1m id28 lo to LBLF1 times ST1CNT 10u do:f1 10u do:f2 10u do:f3 10u LOCKH_OFF exit ;-------------------phases for phasecycle ph6 = 3 3 1 1 ph5 = 0 2 ph31= 0 2 2 0 ;-------------------fixed phases ph20= 0 ph21= 1 ph22= 2 ph23= 3 ;-------------------phases for States-TPPI ph1= 0 ph2= 0 ph3= 0 ph4= 0