;hnca_fb.ref, 8/03/02 #include "Avance.incl" #include "Gradnt_new.incl" ;history ;written on 10/23/91 ;used for sg hncoct/8 10/23/91 ;interchanged C13 and N15 6/12/92 ;used for gv ;put in NH2 purge pulse ph22 7/17/92 ;put additional +/- on last nitrogen 90 pulse 7/17/92 ;used for jacob's calcineurin 7/17/92 ;changed to hnco_fb.sg 9/1/94 included flip-back ;used on NEF hncoct/10 SG 9/1/94 ;changed to hnca_fb.sg 9/2/94 ;changed to hnca_fb.aph 3/1/96 for DMX-500 aph, ik, dif ;copied to hnca_fb.mam and checked 2/10/97 ;copied from hnca_fb.mam ;installed uthscsa drx600 by aph (8/2002) ; ;NOTE1 - Follow the guidelines below for setting up this experiment ;Unless you fully understand what you are doing, do NOT proceed beyond ;the point indicated ;NOTE2 - In the header section that follows, anything between double quotes ;is something you can type at the XWINNMR command line ;NOTE3 - Anything followed by a "s" means a time in seconds, anything followed ;by a "m" means a time in milliseconds, and anything followed by a "u" ;means a time in microseconds ;Set the options below to tailor the pulse program for your needs #define CALPHA ;#define NITROGEN ;The following are for testing, normally: ;"TEST_1D" should be commented OUT ;"ON" should be commented IN ;#define TEST_1D #define ON ;Set the channel assignments to match your hardware settings in "edasp" #define H1 f1 #define C13 f2 #define N15 f3 ;1H pulses, set carrier to H2O ;p1 - square 90 degree 1H @ pl1, typically p1 = 8.5u @ pl1 = -5.2dB ;p2 - square 90 degree 1H @ pl2, typically p2 = 1m @ pl2 = 35.5dB ;p3 - shaped 90 degree 1H @ sp0 , typically p3 = 2m @ sp0 = 35.0dB ; NOTE set "spnam0 seduce1.jc", "spoffs0 0" ;pcpd1 - square 90 at pl30, typically pcpd1 = 50u @ pl30 = 10.0 dB ; NOTE set "cpdprg1 dipsi2" ;13C PULSES - set carrier to 56ppm ;p11 - square 90 @ pl11, for Ca excitation, p11 must equal 53.5u, ; typically pl11 = +8.5dB ;p12 - square 90 @ pl12, for Ca inversion, p12 must equal 23.9u, ; typically pl12 = +1.5dB ;p13 - shaped 180 @ sp1, for CO inversion, typically p13 300u @ sp1 +12.8dB ; NOTE set "spnam1 sinc1.100", "spoffs1 18107" ;p14 - square 90 @ pl14, for CO off-res dante, p14 must equal 84.6u, ; typically pl14 +12.5dB ;15N PULSES, set carrier to 118ppm ;p7 - square 90 degree 15N @ pl7, typically p7 = 45u @ pl7 = -4.5dB ;pcpd3 - square 90 degree 15N @ pl3, typically pcpd3 = 200u @ pl3 = 8.6dB ; NOTE set "cpdprg3 waltz16" ;GRADIENT SETTINGS ;Note1 - grad times are preset, you do not need to adjust these ;Note2 - set grad params according to table below, note integer in first ;column is substituted to yield the parameter that is to be adjusted ;example for grad# 0, set "gpnam0 sine.64", "gpx0 0", "gpy0 0", "gpz0 12" ; ;grad# gpnam# gpx# gpy# gpz# ;0 sine.32 0 0 50 ;N15 evolution ;in21 - incremented delay, set to 1/(4*SW), typically 150u ;in22 - incremented delay, set to 1/(4*SW), typically 150u ;in23 - incremented delay, set to 1/(4*SW), typically 150u ;l4 - number of complex points, maximum is trunc(d23/in23), ;typically l4 = 45 ;N15 Conversion/Processing ;Conversion, Dim=z, yMODE Complex, aq2D States ;Example processing... ;| nmrPipe -fn SP -off 0.45 -end 0.98 -pow 2 -c 0.5 \ ;| nmrPipe -fn ZF -size 128 \ ;| nmrPipe -fn FT \ ;| nmrPipe -fn PS -p0 0.0 -p1 0.0 -di -verb \ ;| nmrPipe -fn POLY -auto -ord 1 \ ;| nmrPipe -fn TP \ ;C13 evolution ;in0 - incremented delay, set to 1/(2*SW), typically 122u ;NOTE, in0 must also fulfill the constraint that the following ;expression for d0 >= 0 ;d0 = in0-p11*0.637-p14-2u ;C13 Conversion/Processing ;Conversion, Dim=y, yMODE Complex, aq2D States ;Example processing... ;| nmrPipe -fn SP -off 0.45 -end 0.98 -pow 2 -c 1.0 \ ;| nmrPipe -fn ZF -size 512 \ ;| nmrPipe -fn FT \ ;| nmrPipe -fn PS -p0 -180.0 -p1 360.0 -di -verb \ ;| nmrPipe -fn POLY -auto -ord 1 \ ;| nmrPipe -fn TP \ ;DO NOT ADJUST ANYTHING BELOW THIS POINT "p20=1m" ;gp0=+50% "p19=1m" ;gp0=+50% "p18=1.5m" ;gp0=+50% "p17=400u" ;gp0=+50% #define CO_180 (p15 ph11 p15 ph12 p15 ph13 p15 ph14 p15 ph15 p15 ph16 p15 ph11 p15 ph12 p15 ph13 p15 ph14 p15 ph15 p15 ph16 p15 ph11 p15 ph12 p15 ph13 p15 ph14 p15 ph15 p15 ph16):C13 "p15=p14/9" "d0=in0 - p11*0.637 - p14 - 2u" ;180/360 phase correction ;d1=1.0s relaxation delay "d4=2.25m" "d7=950u" "d11=50m" "d12=7m" ;universal dd,ip delay "d17=p12*2" "d18=p1" "d22=6.81m" "d21=d22-5.4m" "d23=d22" "d26=p7 - p1" "d28=p14 - p7" ;in0=1/2*SW, typical value: 144u ;in21=in22=in23=1/(4sw) ze 10u 2 d11 do:N15 20u BLKGRAD #ifdef CALPHA d12 3 d12*2 4 d12 #endif #ifdef NITROGEN d12 5 d12*4 6 10u #endif 7 10u d1 pl7:N15 1m UNBLKGRAD (p7 ph10):N15 p20:gp0 ;1m gradient 500u pl12:C13 10u pl1:H1 #ifdef ON ;******* start INEPT from 1H to 15N ******* (p1 ph0):H1 d4 (d26 p1*2 ph1):H1 (p7*2 ph2):N15 d4 (p1 ph2):H1 2u 20u pl2:H1 (p2 ph24:r):H1 2u p19:gp0 ;1m gradient 1m pl1:H1 (p7 ph3):N15 ;******* n15 evolution ******* 5.4m (p1 ph1):H1 4u 4u pl30:H1 d21 cpds1:H1 (p13:sp1 ph10):C13 2u d22 pl12:C13 d17 ;d17=p12*2 2u (p7*2 ph5):N15 2u (p12*2 ph6):C13 2u d23 (p13:sp1 ph10):C13 d23 d18 ;d18=p1 8u pl11:C13 (p7 ph7):N15 (p11 ph4):C13 ;******* calpha evolution ******* 2u d0 pl14:C13 ;t1/2 (d28 p7*2 ph10):N15 CO_180 2u d0 pl11:C13 ;t1/2 ;****** return magnetization to 15N ***** (p11 ph20):C13 (p7 ph10):N15 4u 4u pl12:C13 d18 ;d18=p1 10m d17 ;d17=p12*2 2u (p7*2 ph10):N15 2u (p12*2 ph20):C13 4.6m 4u do:H1 4u pl1:H1 (p1 ph27):H1 5.4m (p7 ph0):N15 5u p18:gp0 ;gradient 1m (p3:sp0 ph25):H1 50u pl1:H1 ;****** INEPT back to 1H with Watergate ****** (p1 ph0):H1 5u p17:gp0 ;400u gradient 950u pl2:H1 (p2 ph24:r):H1 2u 5u pl1:H1 (p1*2 ph0):H1 2u 5u pl2:H1 (p7*2 ph10):N15 (p2 ph24:r):H1 2u p17:gp0 ;400u gradient (2u ph0) d7 pl3:N15 #endif #ifndef TEST_1D go=2 ph31 cpd3:N15 1m BLKGRAD d11 do:N15 wr #0 if #0 zd #ifdef CALPHA d12 ip4 lo to 3 times 2 d12 id0 d12 ip31*2 lo to 4 times l3 d12 rd0 #endif #ifdef NITROGEN d12 ip3 lo to 5 times 2 d12 id21 d12 id22 d12 dd23 d12 ip31*2 lo to 6 times l4 #endif #else ;***** 1D test for sample heating ***** lo to 7 times 1000 500m pl1:H1 p1 ph31 10u go=2 ph31; cpd3:N15 d11 wr #0 #endif 5u do:N15 10u exit ph0=0 ph1=1 ph2=1 ph3=0 ph4=0 0 2 2 ph5=0 0 0 0 1 1 1 1 2 2 2 2 3 3 3 3 ph6=0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 ph7=0 2 ph10=0 ph11=(6)0 ph12=(6)5 ph13=(6)4 ph14=(6)3 ph15=(6)2 ph16=(6)1 ph20=0 ph21=0 ph24=2 ;adjust -x w/ phcor24 for pl2 (rel to pl1) ph25=2 ;adjust -x w/ phcor25 for sp0 (rel to pl1) ph27=3 ;adjust -y w/ phcor27 for pl1 (rel to pl30) ph31=0 2 2 0 2 0 0 2