;;Dimensionality: 5 ;;Experiment: NOBAH ;;Phaseoverlap: 00000 ;;trosy: 0 ;;DimProjections: 2 ;;Hfreq: BF1 ;;Cfreq: BF2 ;;Nfreq: BF3 ;;Carrier1: O3P ;;Carrier2: CNST 29 ;;Carrier3: CNST 31 ;;Carrier4: CNST 31 ;;Carrier5: O1P ;;----------------end header------------------ ;Conventional name: 5D-APSY-HNCOCACB ;Sebastian Hiller, Christian Wasmer, 2006 ;**************************************************************** ;* * ;* The following one-letter codes for the nuclei are used: * ;* * ;* N = N w1 v * ;* CO = O w2 w * ;* CB = B w3 x * ;* CA = A 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 ;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 ;cnst3: gamma ;cnst41: SW1 (N) [Hz] ;cnst42: SW2 (CO) [Hz] ;cnst43: SW3 (CB) [Hz] ;cnst44: SW4 (CA) [Hz] ;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) ;cnst31: Cb+Ca chemical shift (offset) ;sp9 : 180 deg, p9, iburp1_128 ;sp10 : 90 deg, p10, gauss128_5 ;sp11 : 180 deg, p11, GAussCascadeQ3_128 180u @ 600 ;sp12 : 90 deg, p12, eburp1_128 ;sp13 : 180 deg, p13, BLOCK.32 ;sp14 : 90 deg, p14, GaussCascadeQ5_128 350u @ 600 ;sp15 : 180 deg, p15, iburp1_128 ;sp16 : 90 deg, p16, BLOCK.32 ;sp17 : 180 deg, p17, BLOCK.32 ;sp18 : 180 deg, p18, gauss128_5 ;sp19 : 180 deg, p19, GaussCascQ5_TR_128 350u @ 600 ;sp20 : 90 deg, p20, gauss128_5 ;spnam9 : iburp1_128 ;spnam10 : gauss128_5 ;spnam11 : GAussCascadeQ3_128 ;spnam12 : eburp1_128 ;spnam13 : BLOCK.32 ;spnam14 : GaussCascadeQ5_128 ;spnam15 : iburp1_128 ;spnam16 : BLOCK.32 ;spnam17 : BLOCK.32 ;spnam18 : gauss128_5 ;spnam19 : GaussCascQ5_TR_128 ;spnam20 : gauss128_5 #define GRADIENT1 10u p21:gp1 190u #define GRADIENT2 10u p23:gp10 190u #define GRADIENT3 10u p23:gp8 190u #define GRADIENT4 10u p22:gp7 190u #define GRADIENT5 10u p22:gp6 190u #define GRADIENT6 10u p23:gp10 190u #define GRADIENT7 10u p21:gp3 190u #define GRADIENT8 10u p22:gp2 190u #define GRADIENT9 10u p21:gp6 190u ;cnst51 : set to o3p ;cnst52 : set to cnst 29 ;cnst53 : set to cnst 31 ;cnst54 : set to cnst 31 ;cnst55 : set to o1p ;cnst59 : dummy "cnst59=cnst41+cnst42+cnst43+cnst44+cnst51+cnst52+cnst53+cnst54+cnst55" ;----------------------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)" "spoff10=0.0" "spoff11=0.0" "spoff12=0.0" "spoff13=0.0" "spoff14=0.0" "spoff15=bf2*((cnst29-cnst30)/1000000)" "spoff16=0.0" "spoff17=0.0" "spoff18=bf2*((cnst29-cnst31)/1000000)" "spoff19=0.0" "spoff20=0.0" "cnst10=abs(sin(0.017453293*cnst1))" "cnst11=abs(cos(0.017453293*cnst1))" "cnst12=abs(sin(0.017453293*cnst2))" "cnst13=abs(cos(0.017453293*cnst2))" "cnst14=abs(sin(0.017453293*cnst3))" "cnst15=abs(cos(0.017453293*cnst3))" "l1=td1/2" "p2=2*p1" "p6=2*p5" "d0 = 1.0m" ; dummy "in0= in1" ; dummy ;------------------------------basic delays "d2 = 2.7m" ; 1/2 J_NH "d3 = 13.75m" ; 1/2 J "d4 = 4.5m" ; 1/2 J "d6 = 6.8m" ; 1/2 J_AB "d7 = 4.75m" ; 1/2 J_OA ;----------------------fixed delays define delay INEPT_1 "INEPT_1=d2-p21-200u" define delay INEPT_W "INEPT_W=d2-(p22+200u+p1*2.3846+d5*2.5)" define delay WGATE "WGATE=d5/2-p5" "d31=d3-2*d2" ;----------------------------indirect dimensions ;----------------------N "d11=5u" "d12=d3-10u-p9-p17" "d13=5u" "d14=d3" "d30=2*d2" "in11=cnst14*in1/2" "in14=(d14-20u)/l1" "in13=0u" ;----------------------O "d15=5u" "d16=d4-10u-p6" "d17=5u" "d18=d4" "in15=cnst12*cnst15*in1/2" "in18=(d18-20u)/l1" "in17=0u" ;----------------------B "d23=10u" "d24=10u" "in23=2*cnst10*cnst13*cnst15*in1/2" ;----------------------A "d21=d6-d7-p15" "d25=10u" "d20=d6-p15-20u" "d26=d6-p15-10u-p21-200u" "d27=d7-10u-p6-p21-200u" "in25=cnst11*cnst13*cnst15*in1/2" "in26=in25" ;-------------------- #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 1m ip4 1m ip5 #endif #ifdef Y 1m ip4 #endif goto 4 d0 10u id0 10u id15 10u id23 4 1m ;------------------------------------Switch constant-time for 15N if "in14 < in11" goto 5 10u "in14=in11" 10u goto 6 5 1m 10u "in13=in11-in14" 10u 6 1m ;------------------------------------Switch constant-time for 13CO if "in18 < in15" goto 7 10u "in18=in15" 10u goto 8 7 1m 10u "in17=in15-in18" 10u 8 1m ;----------------------------------------- 2 5m LBLSTS1, 5m LBLF1, 5m 10u do:f3 10u LOCKH_OFF 10u pl9:f1 d1 cw:f1 10u do:f1 10u 10u fq=cnst29 (bf ppm):f2 10u 20u pl1:f1 20u pl2:f2 20u pl3:f3 20u LOCKH_ON ;-----------------------------------------INEPT HN -> N (p1 ph20):f1 GRADIENT1 INEPT_1 (refalign (p2 ph20):f1 center (p6 ph20):f3) GRADIENT1 INEPT_1 (p1 ph11):f1 ;-----------------------------------------z-Filter GRADIENT2 20u pl11:f1 ;-----------------------------------------N-evolution, INEPT N -> CO (p5 ph1):f3 (refalign (d11 p9:sp9 ph20 d12 p17:sp17 ph20):f2 lalign (d30 5u cpds1):f1) d13 (p6 ph20):f3 d14 (p5 ph20):f3 ;-----------------------------------------z-Filter GRADIENT3 ;-----------------------------------------CO evolution (p16:sp16 ph2):f2 d15 (p6 ph20):f3 d16 (p9:sp9 ph20):f2 d17 (p17:sp17 ph20):f2 d18 (p9:sp9 ph20):f2 5u (p16:sp16 ph21):f2 ;-----------------------------------------z-Filter GRADIENT4 10u 10u fq=cnst31 (bf ppm):f2 10u 10u pl2:f2 10u ;-----------------------------------------INEPT CA -> CB (p14:sp14 ph20):f2 5u do:f1 10u (p15:sp15 ph20):f2 d20 5u cpds1:f1 (p11:sp11 ph20):f2 d21 (p15:sp15 ph20):f2 d7 ;-----------------------------------------CB evolution (p19:sp19 ph6):f2 GRADIENT7 d23 (p4 ph20):f2 GRADIENT7 d24 (p14:sp14 ph5):f2 ;-----------------------------------------CA evolution d25 (p6 ph20):f3 GRADIENT9 d27 (p15:sp15 ph20):f2 d21 (p11:sp11 ph3):f2 GRADIENT9 d26 (p15:sp15 ph20):f2 10u (p19:sp19 ph4):f2 ;-----------------------------------------CA evolution ; (p10:sp10 ph3):f2 ; d19 ; (refalign (p15:sp15 ph20):f2 center (p6 ph20):f3) ; d19 ; (p11:sp11 ph20):f2 ; 10u ; (refalign (p15:sp15 ph20):f2 center (p6 ph20):f3) ; 10u ; (p10:sp10 ph12):f2 ;-----------------------------------------z-Filter GRADIENT5 10u 10u fq=cnst29 (bf ppm):f2 10u 10u pl2:f2 10u ;-----------------------------------------INEPT CA -> CO (p16:sp16 ph20):f2 5u (p9:sp9 ph20):f2 d4 (p17:sp17 ph20):f2 5u (p9:sp9 ph20):f2 d4 (p16:sp16 ph21):f2 ;-----------------------------------------z-Filter GRADIENT6 ;-----------------------------------------INEPT CO -> N (p5 ph20):f3 d3 (refalign (p6 ph20 d3):f3 lalign (p17:sp17 ph20):f2 lalign (d31 5u do):f1) (p5 ph20):f3 ;-----------------------------------------z-Filter GRADIENT3 10u 10u pl1:f1 10u ;-----------------------------------------INEPT N -> HN (p1 ph20):f1 GRADIENT8 INEPT_W (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 GRADIENT8 INEPT_W pl13:f3 ;-----------------------------------------acquisition go=2 ph31 cpd3:f3 #ifdef Pv 1m do:f3 wr #0 if #0 zd 30u ip1 #endif #ifdef Pw 1m do:f3 wr #0 if #0 zd 30u ip2 #endif #ifdef Px 1m do:f3 wr #0 if #0 zd 10u ip3 10u ip4 10u ip5 #endif #ifdef Py 1m do:f3 wr #0 if #0 zd 30u ip4 #endif lo to LBLSTS1 times 2 1m id11 1m id13 1m dd14 1m id15 1m id17 1m dd18 1m id23 1m id25 1m dd26 lo to LBLF1 times ST1CNT 10u do:f1 10u do:f2 10u do:f3 10m LOCKH_OFF exit ;-------------------phases for phasecycle ph6 = 0 2 ph11= 1 1 3 3 3 3 1 1 ph31= 0 2 2 0 2 0 0 2 ;-------------------phases for States-TPPI ph1 = 0 ph2 = 0 ph3 = 0 ph4 = 0 2 ph5 = 0 0 2 2 ;-------------------fixed phases ph20 = 0 ph21 = 1 ph22 = 2 ph23 = 3