DUMBOdqR1225sqbsw: 2D big F1 spectral width R12_2^5 2Q/1Q correlation with DUMBO decoupling pulse program (TopSpin2.1)
Since non-phase cycling is applied to the R1225 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 R1225 reconversion pulse for filtering DQ coherences.
;DUMBOdqR1225sqbsw ;2D DQ-SQ proton-proton shift correlation ;with R12_2^5 DQ excitation/reconversion ;with homonuclear DUMBO decoupling DQ evolution without prepulses during t1 ;and windowed DUMBO acquisition ;S. P. Brown, A. Lesage, B. Elena and L. Emsley, J. Am. Chem. Soc. 126, 13230-13231 (2004). ;modified after Leskes, Madhu and Vega, Chem. Phys. Lett. to remove center artefact ;using STATES-TPPI ;This pulse program was written according to the corresponding DUMBO-sequence from ;the ENS-Lyon Pulse Program Library ;p9 2.4-4.5 usec, depending on probe deadtime, usually: ;for 200 and 300 MHz, CRAMPS probe required or use 4.5 usec, ;acqu or p9 must be as short as possible, avoiding dipolar coupling effects between DUMBO sequences, ;l11 or d9 must be as large as possible to improve S/N ratio, but keeping acqu positive and small, ;p1 : 90 degree 1H detection pulse ;p2 : presaturation 90 degree pulse ;p9 : acquisition window, 1.7-4.5 usec, depending on probe deadtime ;p10: dumbo-1 pulse for t2 ;p20: dumber-22 pulse for t1 ;p25: = inf1, for t1 increment ;d1 : recycle delay ;d5 : z filter delay, 0.1 μs or multiple of 1/cnst31, otherwise no signal ;d10: parameter for t1 value ;d20: delay between saturation pulses ;l0 : 0 as initial t1 ;l1 : number R12_2^5 basic cycle elements, for protons 2-4 in real solids ;l3 : t1-increment multiplier, usually 2-4, to reduce required number of rows ;l11: number of oversampled data points to be averaged into one dwell point ;l20: # of pulses in saturation pulse train, 0 if undesired ;pl1 : 1H presaturation power ;pl7 : 1H power for R12_2^5 recoupling sequence, B1=(N/2n)*cnst31=3*cnst31 in Hz ;pl12: 1H power for pulses P1 ;pl13: dumbo power ;sp1 : 1H power for windowed dumbo-1 (t2) ;sp2 : 1H power for dumber-22 (t1) (usually somewhat less power than sp1 since ; there is no window); first set to pl13 as in setup experiments ;cnst1 : phase for R12_2^5 reconversion pulse due to t1 evolution period ;cnst31: spinning frequency ;FnMode: undefined ;MC2 : STATES-TPPI ;NS : 16*n ;WDW : F1 QSINE 3, F2 QSINE 2 or EM ;zgoptns :-Dpresat or blank ;$COMMENT=homonuclear decoupling with w-DUMBO ;$CLASS=Solids ;$DIM=2D ;$TYPE=homonuclear decoupling ;$SUBTYPE=explicit acquisition ;$OWNER=hf ;cnst11 : to adjust t=0 for acquisition, if digmod = baseopt "acqt0=1u*cnst11" dwellmode auto #include <Avancesolids.incl> #include <Delayssolids.incl> "d3=p9" ;p9 sets the window to make sure it is in microseconds "d9=0.1u*(l11)" ;set the sampling window, defined in Avancesolids.incl "blktr2 = 0.6u" ;this opens the transmitter gate 0.6 usec before the ;pulse, so the transmitter noise is not sampled "l0=0" ;reset F1 dwell counter "inf1=(l3*(2*d3+p20))*2" ;t1 increment "sp1=pl13" "sp2=pl13" define delay dead "dead=1.2u" define delay acqu ;small window, defined by d3, 2.5-4.5 usec depending "acqu=2*p9-1.2u-d9-.1u" ;on probe deadtime ;acqu or p9 must be as short as possible, avoiding dipolar coupling effects ;l11 or d9 must be as large as possible but keeping acqu positive define delay cycle "cycle=4*p9+2*p10+.2u" define loopcounter count "count=aq/cycle" ;make sure td datapoints are sampled define delay rest ;make sure sampling proceeds throughout the sequence "rest=aq-(count*cycle)" define loopcounter count1 ;for STATES-TPPI procedure "count1=td1/2" ;and STATES cos/sin procedure define pulse pul180 "pul180=(1.0s/cnst31)/6" ;180° pulse "d31=1.0s/cnst31" "p25=inf1" 1 ze ;acquire into a cleared memory "d10=0.1u" ;make sure a short d10 is used initially 2 d31 #ifdef presat ;set with -Dpresat pres, d20 ;delay between saturation pulses (p2 pl1 ph4):f1 ;saturation loop if required lo to pres times l20 #endif /* presat */ d1 ;recycle delay "cnst1=-180*cnst31*d10" ;phase correction for R12_2^5 reconversion pulse, ;due to t1 DQ evolution period, ;defined by the phase-time relationships 10u reset1:f1 ;synchronise pulse and detection RF 1m rpp10 ;reset phase list pointer 1m rpp20 ;reset phase list pointer 1m rpp11 ;reset the phase ph11 pointer to the first element 1m rpp13 ;reset the phase ph13 pointer to the first element 10u pl7:f1 ;R12_2^5 DQ excitation: 3 (pul180 ph11 ipp11):f1 ;increment phase ph11 pointer (pul180 ph11 ipp11):f1 ;increment phase ph11 pointer lo to 3 times l1 5 d3 ;DQ evolution: d3 (p20:sp2 ph20^):f1 ;dumber22 d3 d3 (p20:sp2 ph20^):f1 ;dumber22 lo to 5 times l0 ;R12_2^5 DQ reconversion: 6 (pul180 ph13+cnst1 ipp13 pl7):f1 ;increase ph13 by cnst1 due to evolution period ;increment phase ph13 pointer (pul180 ph13+cnst1 ipp13):f1 ;increase ph13 by cnst1 due to evolution period ;increment phase ph13 pointer lo to 6 times l1 d5 pl12:f1 ;z filter delay STARTADC ;prepare adc for sampling, set reference frequency, ;defined in Avancesolids.incl RESETPHASE ;reset reference phase (p1 ph1):f1 ;90° detection pulse at pl12 .1u DWL_CLK_ON 7 dead acqu d9 RG_ON .1u RG_OFF ;take l11 complex data points (p10:sp1 ph10^):f1 ;w-dumbo, use 24 usec at 600 MHz or higher dead acqu d9 RG_ON .1u RG_OFF (p10:sp1 ph10^):f1 lo to 7 times count ;make sure td points are sampled rest 1u DWL_CLK_OFF 1m ;DQ filtering (four phase cycling): 1m ip13*16384 ;increments all phases of ph13 by 90° rcyc=2 ;next scan 100m wr #0 if #0 zd ;save data 1m ip11*8192 ;increments all phases of ph11 by 45°, ;90° phase for DQ coherence lo to 2 times 2 ;t1 quadrature detection 8 1m iu0 ;increment counter l0 by 1 lo to 8 times l3 ;for multiple t1 increment "d10=d10+p25" ;p25=inf1=increment for F1 (to make it usec!) ;d10 is the t1 evolution period ;1m rp11 ;reset all phases of ph11 and ph13 ;1m rp13 ;had before the first ip11 and ip13 lo to 2 times count1 ;count1 = td1/2 exit ;finished ph1= 1 1 1 1 2 2 2 2 3 3 3 3 0 0 0 0 ph10= 0 2 ;windowed dumbo phase during t2 ph11=(65536) 13653 51883 ; 75° 285° or 75° -75° ph13=(65536) 30037 2731 ;165° 15° or ph11 + 90° ;an overall constant phase shift of π/2 is applied ;to the reconversion pulse phases ph13 and ph14 for time reversal ph4= 0 ;for presaturation pulse ph20=0 2 ;dumber22 phase during t1 ph30=0 ;needed for acquisition, involved in RESETPHASE ph31=0 2 0 2 1 3 1 3 2 0 2 0 3 1 3 1 ;involved in STARTADC ;ph31 = ph1 + 2*ph13 + 1
RN-DQ/SQ-DUMBO excitation pulse sequence.
BABA-DQ/SQ-SAM excitation pulse sequence.
DQ-DUMBO excitation pulse sequence.