/* hbcbcgcdhd_aro_pfg_500.c This pulse sequence will allow one to perform the following experiment: 2D correlation of cb and hd of aromatic residues. F1 CB F2(acq) HD of aromatic Uses two channels: 1) 1H - carrier (tof) @ 4.7 ppm [H2O] 2) 13C - carrier dof @ 35 ppm shift to dofaro @ 125 ppm (The centre of F1 is 35ppm (dof)) Set dm = 'nnny', dmm = 'cccp' [13C decoupling during acquisition]. Set dm2 = 'nnnc', dmm2 = 'cccc' Must set phase = 1,2 for States-TPPI acquisition in t1 [cb]. Flags fsat 'y' for presaturation of H2O fscuba 'y' to apply scuba pulse after presaturation of H2O mess_flg 'y' for 1H (H2O) purging before relaxtion delay f1180 'y' for 180deg linear phase correction in F1 otherwise 0deg linear phase correction in F1 Standard Settings fsat='n', fscuba='n', mess_flg='y', f1180='n' The flag f1180 should be set to 'y' if t1 is to be started at halfdwell time. This will give -90, 180 phasing in f1. If it is set to 'n' the phasing will be 0,0 and will still give a perfect baseline. Written by T. Yamazaki July 12, 1993 REF: T. Yamazaki, J. D. Forman-Kay and L. E. Kay J. Am. Chem. Soc. 115, 11054, (1993) BMRB Pulse Sequence Accession Number: 63 */ #include #include /* #include "delays.h" */ #define PI 3.1416 static int phi1[1] = {1}, phi2[1] = {0}, phi3[4] = {0,1,2,3}, phi4[8] = {0,0,0,0,2,2,2,2}, phi5[1] = {0}, rec[8] = {0,2,0,2,2,0,2,0}; static double d2_init=0.0; pulsesequence() { /* DECLARE VARIABLES */ char fsat[MAXSTR], fscuba[MAXSTR], f1180[MAXSTR], /* Flag to start t1 @ halfdwell */ mess_flg[MAXSTR], /* water purging */ ar180a[MAXSTR], /* waveform shape for aromatic 180 pulse with C transmitter at dof */ cb180b[MAXSTR], /* waveform shape for aliphatic 180 pulse with C transmitter at dofar */ ar180b[MAXSTR]; /* waveform shape for aromatic 180 pulse with C transmitter at dofar */ int phase, ni, t1_counter; /* used for states tppi in t1 */ double tau1, /* t1 delay */ taua, /* ~ 1/4JCbHb = 1.7 ms */ taub, /* ~ 1/4JCgCd = 2.7 ms */ tauc, /* ~ 1/4JCgCd = 2.1 ms */ taud, /* ~ 1/4JCdHd = 1.5 ms */ taue, /* = 1/4JCbHb = 1.8 ms */ tauf, /* ~ 1/2JCdHd = 3.1 ms */ TCb, /* carbon constant time period for recording the Cb chemical shifts */ dly_pg1, /* delay for water purging */ pwar180a, /* 180 aro pulse at d_ar180a and dof */ pwcb180b, /* 180 cb pulse at d_cb180b and dofar */ pwc, /* 90 c pulse at dhpwr */ pwsel90, /* 90 c pulse at d_sel90 */ pwar180b, /* 180 c pulse at d_ar180b */ d_ar180a, d_cb180b, d_sel90, d_ar180b, dofar, tsatpwr, /* low level 1H trans.power for presat */ tpwrmess, /* power level for water purging */ tpwrml, /* power level for 1H decoupling */ pwmlev, /* 90 pulse at tpwrml */ dhpwr, /* power level for high power 13C pulses on dec1 */ sw1, /* sweep width in f1 */ at, gp11, /* gap between 90-90 for selective 180 of Cb */ fab, /* chemical shift difference of Ca-Cb (Hz) */ gt0, gt1, gt2, gt3, gt4, gt5, gt6, gt7, gzlvl0, gzlvl1, gzlvl2, gzlvl3, gzlvl4, gzlvl5, gzlvl6, gzlvl7; /* variables commented out are already defined by the system */ /* LOAD VARIABLES */ getstr("fsat",fsat); getstr("f1180",f1180); getstr("fscuba",fscuba); getstr("mess_flg",mess_flg); getstr("ar180a",ar180a); getstr("ar180b",ar180b); getstr("cb180b",cb180b); taua = getval("taua"); taub = getval("taub"); tauc = getval("tauc"); taud = getval("taud"); taue = getval("taue"); tauf = getval("tauf"); TCb = getval("TCb"); pwcb180b = getval("pwcb180b"); pwar180a = getval("pwar180a"); pwsel90 = getval("pwsel90"); pwar180b = getval("pwar180b"); pwc = getval("pwc"); d_ar180a = getval("d_ar180a"); d_cb180b = getval("d_cb180b"); d_sel90 = getval("d_sel90"); d_ar180b = getval("d_ar180b"); dofar = getval("dofar"); dly_pg1 = getval("dly_pg1"); tpwr = getval("tpwr"); tsatpwr = getval("tsatpwr"); tpwrmess = getval("tpwrmess"); tpwrml = getval("tpwrml"); pwmlev = getval("pwmlev"); dhpwr = getval("dhpwr"); dpwr = getval("dpwr"); phase = (int) ( getval("phase") + 0.5); sw1 = getval("sw1"); ni = getval("ni"); at = getval("at"); fab = getval("fab"); gt0 = getval("gt0"); gt1 = getval("gt1"); gt2 = getval("gt2"); gt3 = getval("gt3"); gt4 = getval("gt4"); gt5 = getval("gt5"); gt6 = getval("gt6"); gt7 = getval("gt7"); gzlvl0 = getval("gzlvl0"); gzlvl1 = getval("gzlvl1"); gzlvl2 = getval("gzlvl2"); gzlvl3 = getval("gzlvl3"); gzlvl4 = getval("gzlvl4"); gzlvl5 = getval("gzlvl5"); gzlvl6 = getval("gzlvl6"); gzlvl7 = getval("gzlvl7"); /* LOAD PHASE TABLE */ settable(t1,1,phi1); settable(t2,1,phi2); settable(t3,4,phi3); settable(t4,8,phi4); settable(t5,1,phi5); settable(t6,8,rec); /* CHECK VALIDITY OF PARAMETER RANGES */ if( 0.5*ni*1/(sw1) > TCb - 2*POWER_DELAY - WFG_START_DELAY - pwar180a - WFG_STOP_DELAY) { printf(" ni is too big\n"); abort(1); } if((dm[A] == 'y' || dm[B] == 'y' || dm[C] == 'y' )) { printf("incorrect dec1 decoupler flags! "); abort(1); } if(dm2[A] == 'y' || dm2[B] == 'y' || dm2[C] == 'y' || dm2[D] == 'y' ) { printf("incorrect dec2 decoupler flags! "); abort(1); } if( tsatpwr > 6 ) { printf("TSATPWR too large !!! "); abort(1); } if( tpwrml > 53 ) { printf("tpwrml too large !!! "); abort(1); } if( tpwrmess > 56 ) { printf("tpwrmess too large !!! "); abort(1); } if( dpwr > 48 ) { printf("don't fry the probe, DPWR too large! "); abort(1); } if( dpwr2 > 49 ) { printf("don't fry the probe, DPWR2 too large! "); abort(1); } if( dhpwr > 63 ) { printf("don't fry the probe, DHPWR too large! "); abort(1); } if( pw > 20.0e-6 ) { printf("dont fry the probe, pw too high ! "); abort(1); } if( pwcb180b > 500.0e-6 ) { printf("dont fry the probe, pwcb180b too high ! "); abort(1); } if( pwar180a > 500.0e-6 ) { printf("dont fry the probe, pwar180a too high ! "); abort(1); } if (pwar180b > 500.0e-6) { printf("dont fry the probe, pwar180b too long !"); abort(1); } if (pwsel90 > 100.0e-6) { printf("dont fry the probe, pwsel90 too long !"); abort(1); } if(d_ar180a > 58) { printf("dont fry the probe, d_ar180a too high !"); abort(1); } if(d_cb180b > 58) { printf("dont fry the probe, d_cb180b too high !"); abort(1); } if (d_ar180b > 58) { printf("dont fry the probe, d_ar180b too high ! "); abort(1); } if (d_sel90 > 46) { printf("dont fry the probe, d_sel90 too high ! "); abort(1); } if( gt0 > 15e-3 || gt1 > 15e-3 || gt2 > 15e-3 || gt3 > 15e-3 || gt4 > 15e-3 || gt5 > 15e-3 || gt6 > 15e-3 || gt7 > 15e-3) { printf("gradients on for too long. Must be < 15e-3 \n"); abort(1); } if( fabs(gzlvl0) > 30000 || fabs(gzlvl1) > 30000 || fabs(gzlvl2) > 30000 ||fabs(gzlvl3) > 30000 || fabs(gzlvl4) > 30000 || fabs(gzlvl5) > 30000 ||fabs(gzlvl6) > 30000 || fabs(gzlvl7) > 30000) { printf("too strong gradient"); abort(1); } if( 2*TCb - taue > 0.1 ) { printf("dont fry the probe, too long TCb"); abort(1); } if( at > 0.1 && (dm[D]=='y' || dm2[D]=='y')) { printf("dont fry the probe, too long at with decoupling"); abort(1); } if( pwc > 20.0e-6) { printf("dont fry the probe, too long pwc"); abort(1); } if( dly_pg1 > 10.0e-3) { printf("dont fry the probe, too long dly_pg1"); abort(1); } /* Phase incrementation for hypercomplex 2D data */ if (phase == 2) tsadd(t2,1,4); /* Calculate modifications to phases for States-TPPI acquisition */ if( ix == 1) d2_init = d2 ; t1_counter = (int) ( (d2-d2_init)*sw1 + 0.5 ); if(t1_counter % 2) { tsadd(t2,2,4); tsadd(t6,2,4); } /* Set up f1180 tau1 = t1 */ tau1 = d2; if(f1180[A] == 'y') { tau1 += ( 1.0 / (2.0*sw1) ); } tau1 = tau1/2.0; /* 90-90 pulse for selective 180 of Cb but not Ca */ gp11 = 1/(2*fab) - 4/PI*pwsel90; if (gp11 < 0.0) { printf("gap of 90-90 negative, check fab and pwsel90"); abort(1); } /* BEGIN ACTUAL PULSE SEQUENCE */ /* Receiver off time */ status(A); rcvroff(); offset(dof,DODEV); rlpower(tsatpwr,TODEV); /* Set transmitter power for 1H presaturation */ rlpower(dhpwr,DODEV); /* Set Dec1 power for hard 13C pulses */ rlpower(dpwr2,DO2DEV); /* Set Dec2 power for 15N decoupling */ /* Presaturation Period */ status(B); if(mess_flg[A] == 'y') { rlpower(tpwrmess,TODEV); rgpulse(dly_pg1,zero,20.0e-6,20.0e-6); rgpulse(dly_pg1/1.62,one,20.0e-6,20.0e-6); rlpower(tsatpwr,TODEV); } if (fsat[0] == 'y') { delay(2.0e-5); rgpulse(d1,zero,20.0e-6,20.0e-6); rlpower(tpwr,TODEV); /* Set transmitter power for hard 1H pulses */ delay(2.0e-5); if(fscuba[0] == 'y') { delay(2.2e-2); rgpulse(pw,zero,2.0e-6,0.0); rgpulse(2*pw,one,2.0e-6,0.0); rgpulse(pw,zero,2.0e-6,0.0); delay(2.2e-2); } } else { delay(d1); } rlpower(tpwr,TODEV); /* Set transmitter power for hard 1H pulses */ txphase(zero); dec2phase(zero); decphase(zero); delay(1.0e-5); /* Begin Pulses */ status(C); /* first ensure that magnetization does infact start on H and not C */ decrgpulse(pwc,zero,2.0e-6,2.0e-6); delay(2.0e-6); rgradient('z',gzlvl0); delay(gt0); rgradient('z',0.0); delay(150.0e-6); /* this is the real start */ rgpulse(pw,zero,0.0,0.0); /* 90 deg 1H pulse */ delay(2.0e-6); rgradient('z',gzlvl1); delay(gt1); rgradient('z',0.0); delay(2.0e-6); delay(taua - gt1 - 4.0e-6); /* taua <= 1/4JCH */ simpulse(2*pw,2*pwc,zero,zero,0.0,0.0); txphase(t1); delay(2.0e-6); rgradient('z',gzlvl1); delay(gt1); rgradient('z',0.0); delay(2.0e-6); delay(taua - gt1 - 4.0e-6); rgpulse(pw,t1,0.0,0.0); txphase(zero); delay(2.0e-6); rgradient('z',gzlvl2); delay(gt2); rgradient('z',0.0); delay(150.0e-6); decphase(t2); rlpower(d_sel90,DODEV); decrgpulse(pwsel90,t2,0.0,0.0); decphase(zero); rlpower(d_ar180a,DODEV); decshaped_pulse(ar180a,pwar180a,zero,0.0,0.0); /* bs effect */ delay(taue - POWER_DELAY - WFG_START_DELAY - pwar180a - WFG_STOP_DELAY - POWER_DELAY - PRG_START_DELAY); /* H decoupling on */ rlpower(tpwrml,TODEV); obsprgon("waltz16",pwmlev,90.0); xmtron(); /* TURN ME OFF DONT FORGET */ /* Hldecoupling on */ delay(TCb + tau1 - taue - POWER_DELAY); decphase(t3); rlpower(d_sel90,DODEV); decrgpulse(pwsel90,t3,0.0,0.0); delay(gp11); decrgpulse(pwsel90,t3,0.0,0.0); decphase(zero); rlpower(d_ar180a,DODEV); decshaped_pulse(ar180a,pwar180a,zero,0.0,0.0); delay(TCb - tau1 - POWER_DELAY - WFG_START_DELAY - pwar180a - WFG_STOP_DELAY - POWER_DELAY); decphase(zero); rlpower(d_sel90,DODEV); decrgpulse(pwsel90,zero,0.0,0.0); /* H decoupling off */ xmtroff(); obsprgoff(); rlpower(tpwr,TODEV); /* H decoupling off */ offset(dofar,DODEV); delay(2.0e-6); rgradient('z',gzlvl3); delay(gt3); rgradient('z',0.0); delay(150.0e-6); decphase(t4); rlpower(d_sel90,DODEV); decrgpulse(pwsel90,t4,0.0,0.0); decphase(zero); rlpower(d_cb180b,DODEV); decshaped_pulse(cb180b,pwcb180b,zero,0.0,0.0); /* B.S. */ delay(2.0e-6); rgradient('z',gzlvl4); delay(gt4); rgradient('z',0.0); delay(2.0e-6); delay(taub - POWER_DELAY - WFG_START_DELAY - pwcb180b - WFG_STOP_DELAY - gt4 - 4.0e-6 - POWER_DELAY - WFG_START_DELAY); decphase(zero); rlpower(d_ar180b,DODEV); decshaped_pulse(ar180b,pwar180b,zero,0.0,0.0); rlpower(d_cb180b,DODEV); decshaped_pulse(cb180b,pwcb180b,zero,0.0,0.0); delay(2.0e-6); rgradient('z',gzlvl4); delay(gt4); rgradient('z',0.0); delay(2.0e-6); delay(taub - WFG_STOP_DELAY - POWER_DELAY - WFG_START_DELAY - pwcb180b - WFG_STOP_DELAY - gt4 - 4.0e-6 - POWER_DELAY); rlpower(d_sel90,DODEV); decrgpulse(pwsel90,zero,0.0,0.0); delay(2.0e-6); rgradient('z',gzlvl5); delay(gt5); rgradient('z',0.0); delay(100.0e-6); delay(tauc - POWER_DELAY - gt5 - 102.0e-6); decphase(t5); rlpower(dhpwr,DODEV); decrgpulse(2*pwc,t5,0.0,0.0); delay(2.0e-6); rgradient('z',gzlvl5); delay(gt5); rgradient('z',0.0); delay(100.0e-6); txphase(zero); delay(tauf - gt5 - 102.0e-6); rgpulse(2*pw,zero,0.0,0.0); delay(tauc - tauf - 2*pw - POWER_DELAY); decphase(zero); rlpower(d_sel90,DODEV); decrgpulse(pwsel90,zero,0.0,0.0); txphase(zero); delay(2.0e-6); rgradient('z',gzlvl6); delay(gt6); rgradient('z',0.0); delay(150.0e-6); rgpulse(pw,zero,0.0,0.0); delay(2.0e-6); rgradient('z',gzlvl7); delay(gt7); rgradient('z',0.0); delay(2.0e-6); delay(taud - gt7 - 4.0e-6 - POWER_DELAY); decphase(zero); rlpower(dhpwr,DODEV); simpulse(2*pw,2*pwc,zero,zero,0.0,0.0); delay(2.0e-6); rgradient('z',gzlvl7); delay(gt7); rgradient('z',0.0); delay(2.0e-6); delay(taud - gt7 - 4.0e-6 - 2*POWER_DELAY); rlpower(dpwr,DODEV); /* Set power for decoupling */ rlpower(dpwr2,DO2DEV); /* Set power for decoupling */ rgpulse(pw,zero,0.0,0.0); /* rcvron(); */ /* Turn on receiver to warm up before acq */ /* BEGIN ACQUISITION */ status(D); setreceiver(t6); }