SPC5CP2dlsw: 2D large DQ F1 spectral width SPC5 CP pulse program for TopSpin2.1
SPC5CP2dlsw: 2D large DQ F1 spectral width SPC5 CP pulse program for TopSpin2.1
Since non-phase cycling is applied to the SPC5 excitation pulse, four-phase cycling is applied to the detection pulse P1 for selecting the 0Q -> -1Q coherence order jump, and four-phase cycling is applied to the SPC5 reconversion pulse for filtering DQ coherences.
Avoid cross-polarization during SPC5 excitation and reconversion.
2*del360 = pul90 + pul360 + pul270
;spc5cp2dlsw (TopSpin 2.0) ;2D SQ-DQ correlation experiment with SPC5 sequence and cross polarization ;for the original C7 sequence see: Lee et al. Chem Phys Lett 242, 304-309, 1995 ;see Hohwy, Rienstra, Jaroniec and Griffin, JCP 110, 7983, 1999 ;using Mei Hong trick: J. Magn. Reson. 136, 86-91 (1999) ;by JOS 03/03/03, modified by HF 14.5.07 ;Avance III version ;parameters: ;d1 : recycle delay ;d0 : min. delay in t1 evolution ;p1 : excitation pulse f1 at pl1 ;p3 : 1H excitation pulse @ PL12 ;p5 : FSLG 2pi pulse set by lgcalc.incl ;p15 : HH contact pulse ;pcpd2 : decoupling pulse f2 @ PL12, pcpd = 2*P3-0.2us used by TPPM and SPINAL ;pl1 : for X contact pulse ;pl2 : =120dB, not used ;pl11 : for SPC5 recoupling sequence B1=5*cnst31 in Hz ;pl12 : for 1H excitation and decoupling ;pl13 : for LG decoupling cpdprg1 = cwlg or cw13 or tppm13 ;sp0 : proton power level during contact ;spnam0 : for CP on 1H e.g. ramp.64 ;cpdprg1 : decoupling f2 during SPC5, e.g. cw (or cwlg) or tppm ;cpdprg2 : decoupling f2, e.g. tppm15, SPINAL64 ;cnst20 : LG-RF field as adjusted, in Hz used to calculate cnst22 and cnst23 +and - LG frequency ;cnst21 : =0 frequency reset (set by lgclac.incl) ;cnst22 : +LG frequency offset calc. by lgcalc.incl ;cnst23 : -LG frequency offset calc. by lgcalc.incl ;cnst24 : offset for 1H evol. during FSLG: 0 - -2000 ;cnst31 : spinning speed ;l0 : number of composite SPC5 mq excitation and reconversion cycles multiple of 5 ;l3 : number of 2/5 rotor revolution increments for DQ evolution, usually 1 (why else would I use this?) ;in0 :in0=l3*(2s/cnst31)/5 t1 increment, multiples of 2/5th of a rotation period ;ns : 32*n ;FnMode : undefined ;mc2 : STATES-TPPI ;WDW : F1 QSINE 3, F2 QSINE 2 or EM ;$COMMENT=SQ-DQ experiment with SPC5 sequence, optimised for large sweep width, cp for excitation ;$CLASS=Solids ;$DIM=2D ;$TYPE=cross polarisation ;$SUBTYPE=homonuclear correlation ;$OWNER=Bruker define pulse pul360 "pul360=(1s/cnst31)/5" ;360° pulse define pulse pul90 "pul90=(0.25s/cnst31)/5" ; 90° pulse define pulse pul270 "pul270=(0.75s/cnst31)/5" ;270° pulse define loopcounter count ;for STATES-TPPI procedure "count=td1/2" ;and STATES cos/sin procedure define delay del360 "del360=(1s/cnst31)/5" "d31=(1s/cnst31)" "in0=l3*(2s/cnst31)/5" "inf1=l3*(2s/cnst31)/5" "l2=0" define delay dwellf1 "dwellf1=in0" ;cnst11 : to adjust t=0 for acquisition, if digmod = baseopt "acqt0=1u*cnst11" #include <lgcalc.incl> ;calculates cnst22 from cnst20, RF field at pl13 #include <rot_prot.incl> ;protect for too slow rotation ze 1 d31 dwellf1 2 d1 do:f2 ;F2 decoupler off #include <p15_prot.incl> ;make sure p15 does not exceed 10 msec ;let supervisor change this pulseprogram if ;more is needed #include <aq_prot.incl> ;allows max. 50 msec acquisition time, supervisor ;may change to max. 1s at less than 5 % duty cycle ;and reduced decoupling field 1m rpp11 ;reset the phase program ph11 pointer to the first element 1m rpp12 ;reset the phase program ph12 pointer to the first element 1m rpp13 ;reset the phase program ph13 pointer to the first element 1m rpp14 ;reset the phase program ph14 pointer to the first element 1u fq=cnst21:f2 (p3 pl12 ph1):f2 ;proton 90° pulse (p15 pl1 ph2):f1 (p15:sp0 ph10):f2 ;contact pulse with square or ;ramp shape ramp.100 on F2 (p1 ph4):f1 ;90° pulse putting magnetization back to z-axis ;for SPC5 double-quantum excitation 3 (pul90 pl11 ph11 ipp13 ipp14):f1 (1u cpds1):f2 ;SPC5 DQ excitation ;switch to SPC5 RF condition ;increment reconversion pulse phase ph13 and ph14 pointers ;F2 decoupling during SPC5: cw (or cwlg) or tppm (pul360 ph12 ipp12):f1 ;increment phase ph12 pointer (pul270 ph11 ipp11):f1 ;increment phase ph11 pointer lo to 3 times l0 ;l0 = multiple of 5 ;double-quantum evolution period 4 del360 ipp13 ipp14 cpds2:f2 ;increment reconversion pulse phase ph13 and ph14 pointers del360 ;to the next phase in the lists ;F2 decoupling during DQ evolution: spinal or tppm lo to 4 times l2 ;del360 = (1s/cnst31)/5 5 (pul90 ph13):f1 (1u cpds1):f2 ;SPC5 DQ reconversion ;F2 decoupling during SPC5: cw (or cwlg) or tppm (pul360 ph14 ipp14):f1 ;increment phase ph14 pointer (pul270 ph13 ipp13):f1 ;increment phase ph13 pointer lo to 5 times l0 ;l0 = multiple of 5 (p1 pl1 ph5):f1 (1u cpds2):f2 ;flip into the xy plane ;F2 decoupling with TPPM or SPINAL during acquisition gosc ph31 ;gosc does not loop to 1 ;start ADC with ph31 signal routing 1m do:f2 ;F2 decoupler off ;DQ filtering (four phase cycling): 40u ip13*16384 ;increments all phases of ph13 by 90° 40u ip14*16384 ;increments all phases of ph14 by 90° lo to 1 times ns ;next scan 1m do:f2 ;F2 decoupler off 100m wr #0 if #0 zd ;save data on disk 1m ip11*8192 ;increments all phases of ph11 by 45°, ;90° phase for DQ coherence 1m ip12*8192 ;increments all phases of ph12 by 45°, ;90° phase for DQ coherence lo to 1 times 2 ;t1 quadrature detection 6 1m iu2 ;increment loop counter l2 in 2*Tr/5 lo to 6 times l3 ;1m rp11 ;reset all phases of ph11, ph12, ph13, and ph14 ;1m rp12 ;to their original values, i.e. to the values they ;1m rp13 ;had before the first ip11, ip12, ip13, and ip14 ;1m rp14 ;in case of STATES remove semicolon at beginning of the 4 lines lo to 1 times count ;count = td1/2 1m do:f2 ;F2 decoupler off HaltAcqu, 1m exit ph1= 1 1 1 1 3 3 3 3 ph2= 0 ph4= 3 3 3 3 1 1 1 1 ph5= 0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 1 1 1 1 1 1 1 1 3 3 3 3 3 3 3 3 ph10=0 ph11= (65536) 0 13107 26214 39322 52429 32768 45875 58982 6554 19661 ph12= (65536) 32768 45875 58982 6554 19661 0 13107 26214 39322 52429 ph13= (65536) 16384 29491 42598 55706 3277 49152 62259 9830 22937 36044 ph14= (65536) 49152 62259 9830 22937 36044 16384 29491 42598 55706 3277 ph31= 0 2 0 2 0 2 0 2 2 0 2 0 2 0 2 0 1 3 1 3 1 3 1 3 3 1 3 1 3 1 3 1
Definition of SPC5 excitation pulse.