;hCaNCOCX3D.tcp ; ;version: 1.0/ TS3.2 /2013/06/17 ;version: 1.1/ TS3.2 /2014/02/05 ; ;written for BioToolkit: JOS WTF 10.5.2013 ;double-checked: VEDA SEWE July 2013 ;Flag "-DnoMix" to eliminate COCx mixing introduced by VEDA 2014/02/05 ; ;3D triple cp CNC correlation experiment ;HCa-CP, CaN-CP, NCO-CP, and finally Spin-Diffusion ; ;$CLASS=BioSolids ;$DIM=3D ;$TYPE=Heteronuclear ;$SUBTYPE=hCNCC and TCP ;$COMMENT=hCaNCOCX Triple CP ;Avance II / AVIII version ;Parameters: ;p1 : C 90 at pl1 ;p2 : C 180 at pl1 ;p3 : H 90 at pl2 ;p15 : HC CP at sp41 (f1,C) and sp40 (f2,H) ;p16 : NCa CP at pl5 (f3,N), sp50 (f1,C), pl33 (f2,H) ;p17 : NCO CP at pl6 (f3,N), sp51 (f1,C), pl34 (f2,H) ;p21 : N 90 at pl21 ;p22 : N 180 at pl21 ;pl1 : C pulse power ;pl2 : H pulse power ;pl5 : N NCa CP power ;pl6 : N NCO CP power ;pl12 : H dec power ;pl14 : H DARR power (= 1*cnst31 (MAS freq); for PDSD = 0 W) ;pl21 : N pulse power ;pl33 : H dec power during NCa CP ;pl34 : H dec power during NCO CP ;sp40 : H CP power ;sp41 : C CP power ;sp50 : C NCa CP power ;sp51 : C NCO CP power ;d0 : incremented delay (t1) ;d1 : recycle delay; 1 to 5 times T1 ;d8 : PDSD/DARR mixing time ;d10 : incremented delay (t2) ;d29 : extra time for constant duty cycle (t2) ;d30 : extra time for constant duty cycle (t1) ;pcpd2 : H dec pulse cpdprg2 ;cpdprg2 : Decoupling file cw, tppm (at pl12) ;spnam40 : H ramp use e.g. ramp.10070 for variable amplitude CP ;spnam41 : C ramp use e.g. square.100 for square pulse CP ;spnam50 : CA ramp use e.g. tcn for amplitude modulated tangential pulse CP ;spnam51 : CO ramp use e.g. tcn for amplitude modulated tangential pulse CP ;cnst10 : Frequency reset to Carrier (o1, usually ~100 ppm) ;cnst21 : Frequency offset for CO (~175 ppm) ;cnst22 : Frequency offset for CA (~55 ppm) ;cnst29 : expected td2 for use in constant duty cycle (-DCDC) ;cnst30 : expected td1 for use in constant duty cycle (-DCDC) ;cnst31 : MAS rotation rate in Hz ;inf1: 1/SW(Ca) = 2 * DW(Ca) ;inf2: 1/SW(N) = 2 * DW(N) ;in0 : = inf1 ;in10: = inf2 ;in29: = inf2 ;in30: = inf1 ;l0 : loopcounter for F1 ;l1 : loopcounter for mixing time ;l10: loopcounter for F2 ;ZGOPTNS : -DCDC : for constant duty cycle (parmode must equal DIM) ; -DnoMix : to eliminate COCx mixing ; or blank ;FnMODE : TPPI, States or States-TPPI ;ns: MIN. 4 (full:16) ; ;###################################################### ;# # ;# N-C SPECIFIC CP # ;# Baldus, M.; Petkova, A. T.; Herzfeld, J. H.; # ;# Griffin, R. G. Mol. Phys. 1998,95, 1197-1207. # ;# M. Hong and R.G. Griffin; # ;# J. Am. Chem. Soc. 120, 7113-7114 # ;# # ;# pl5 (15N) = 5*wr/2 pl6 (15N) = 5*wr/2 # ;# sp50(13Ca) = 3*wr/2 sp51(13CO) = 3*wr/2 # ;# # ;###################################################### prosol relations= #include ; defines which channel corresponds to which nucleus #include ; definition of external trigger output #include ; definition of rotor period dependent delays "l1=d8/TauR" ; TauR = time of one rotor period define pulse mixing "mixing=(l1*TauR)" ; mixing = d8 "cnst10=o1" "acqt0=-(p1*2/3.1416)-0.5u" "in0=inf1" ;########################## "d0=1u" ;# t1_init => 0, 0 # "in30=inf1" ;########################## "l0=0" "in10=inf2" ;########################## "d10=1u" ;# t2_init => 0, 0 # "in29=inf2" ;########################## "l10=0" define delay ONTIME ;########################## define loopcounter T1evo ;# Constant Duty Cycle # define loopcounter T2evo ;########################## #ifdef CDC "T1evo=larger(td1,cnst30)" "d30=T1evo*(in30+2u)" "T2evo=larger(td2,cnst29)" "d29=T2evo*(in29+2u)" #endif /* CDC */ aqseq 321 ;########################## ;$EXTERN ;# python insertion point # ;########################## Prepare, ze "d30=d30/2" "d29=d29/2" "ONTIME=aq+d0+d30+d29+p15+p16+p17" ;###################################################### ;# Protections: Pre-Check # ;###################################################### #include ;min. spinning 2.5 kHz #include ;Max. 50 ms acquisition time #include ;p15 max. 10 ms #include ;p16 max. 10 ms #include ;p17 max. 10 ms #include ;PDSD/DARR mixing max. 1 sec #include ;check t1 evolution time #include ;check t2 evolution time #include ;total RF deposition restriction ;###################################################### ;# Start of Active Pulse Program # ;###################################################### Start, 30m do:H d1 trigg 1u fq=cnst22(bf ppm):C ; switch to CO frequency if "l0>0" { "d51=d0-2u" } if "l10>0" { "d52=d10-2u" } ;###################################################### ;# Initial excitation # ;###################################################### (p3 pl2 ph1):H (p15:sp41 ph2):C (p15:sp40 ph0):H ;###################################################### ;# t1 evolution # ;# Polarization is on 13CO # ;###################################################### 0.5u pl12:H if "l0>0" { 0.5u cpds2:H (center (d51) (p21 pl21 ph20 p22 ph21 p21 ph20):N ) 0.5u do:H } ;###################################################### ;# CO-N CP Period (SPECIFIC) # ;# Polarization is on 15N # ;###################################################### (p16:sp50 ph4):C (p16 pl33 ph0):H (p16:sp5 ph3):N (0.5u pl12):H (0.5u fq=cnst10(bf hz)):C ; switch to carrier frequency o1 if "l10>0" { 0.5u cpds2:H (center (d52) (p1 pl1 ph20 p2 ph21 p1 ph20):C ) 0.5u do:H } ;###################################################### ;# N-CA CP Period (SPECIFIC) # ;# Polarization moved to 13CA # ;###################################################### 0.5u fq=cnst21(bf ppm):C ; switch to CA frequency (p17:sp51 ph5):C (p17 pl34 ph0):H (p17:sp6 ph6):N ;###################################################### ;# SPIN DIFFUSION (PDSD, DARR) # ;###################################################### #ifdef noMix #else (p1 pl1 ph8 fq=cnst10(bf hz)):C ;store magn. along Z (mixing ph20 pl14):H (p1 pl1 ph16 ):C (1u pl12):H ;read out #endif /*end of noMix*/ ;####################################################### ;# Acquisition # ;####################################################### (0.5u cpds2):H gosc ph31 ;start ADC with ph31 signal routing #ifdef CDC d30 d29 #endif /*end of CDC*/ 1m do:H lo to Start times ns 30m mc #0 to Start F1PH(calph(ph2, +90), caldel(d0, +in0) & caldel(d30, -in30) & calclc(l0, 1)) F2PH(calph(ph3, +90), caldel(d10, +in10) & caldel(d29, -in29) & calclc(l10,1)) HaltAcqu, 1m exit ;##################################### ;# Phase Cycle # ;##################################### ph0= 0 ; H HCa CP Spin lock and hard pulse during NC CPs ph1= {1}*8 {3}*8 ; H hard pulse ph2= 0 2 ; C HCa CP Spin lock ph3= 0 0 2 2 ; N CaN CP Spin lock ph4= 0 ; C CaN CP Spin lock ph5= 0 ; C NCO CP Spin lock ph6= {0}*4 {2}*4 ; N NCO CP Spin lock ph8= 1 ; C 90 to store magn. along Z ph16=3 ; C 90 read out ph31= 1 3 3 1 3 1 1 3 ; receiver 3 1 1 3 1 3 3 1 ph20= 0 ; C 90/ N 90 hard pulse and H DARR mixing ph21= 1 ; C 180/ N 180 pulse ;####################################################### ;$Id: hCaNCOCX3D.tcp,v 1.1.2.6 2017/02/23 17:10:58 ber Exp $