FMP Berlin, NMR facility Spektometerblätter 21.01.2016 www.fmp-berlin.de/schmieder/nmr_stuff.htm
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FMP Berlin, N
MR facility
Spektometerblätter
21.01.2016
www.fmp-berlin.de/schm
ieder/nmr_stuff.htm
spectrum referencing,
SR/SF-values from D
SS
spectrum referencing,
SR/SF-values from D
SS
temperature calibration using methanol
TBVT : 280, 285, 290, 295, 300, 305, 310, 315, 320 [K]
= (OH) - (CH3)
Treal [K] = 403 - 29.53- 23.87 ()2
[ppm] T [K]
1.73 280
1.64 290
1.55 300
1.45 310
1.35 320
temperature calibration using methanol
Linear fitting of T(BVT) vs. T(real) and vice versa
results in two calibration curves
temperature calibrationfmp600 RT-QXI (Z8654/0007), 03.04.2013
Treal = -17.307 + 1.0589 x TBVT
300 K at BVT is 300.36 K
TBVT = 16.344 + 0.9444 x Treal
300 K: set BVT to 299.66 K
Treal = 9.337 + 0.96 x TBVT
300 K at BVT is 297.34 K
TBVT = -9.726 + 1.0417 x Treal
300 K: set BVT to 302.78 K
Treal = 8.6678 + 0.9488 x TBVT
300 K at BVT is 293.31 K
TBVT = -9.136 + 1,0540 x Treal
300 K: set BVT to 307.06 K
psf600 CP-TXI (Z44866/0019), 08.04.2013
sel600 CP-TCI (Z75812/0039), 09.04.2013
Treal = -21.561 + 1.0736 x TBVT
300 K at BVT is 300.52 K
TBVT = 20.083 + 0.9314 x Treal
300 K: set BVT to 299.50 K
RT-BBFO (Z114607/0090), 02.04.2013
temperature calibration
av750 CP-TCI (Z44915/0001), 17.04.2013
Treal = 7,9615 + 0.9505 x TBVT
300 K at BVT is 293.11 K
TBVT = -8.376 + 1.0521 x Treal
300 K: set BVT to 307.25 K
Treal = 5.6765 + 0.9709 x TBVT
300 K at BVT is 296.95 K
TBVT = -5.8466 + 1.03 x Treal
300 K: set BVT to 303.15 K
RT-TXI (Z8344/0003), 23.08.2011Treal = 0.0 + 1.00 x TBVT
300 K at BVT is 300.00 K
TBVT = 0.0 + 1.0 x Treal
300 K: set BVT to 300.00 K
av900 CP-TCI (Z44910/0015), 11.04.2013
carrier-values for protons
o1
400 MHz 1880 Hz
600 MHz 2820 Hz
700 MHz 3280 Hz
750 MHz 3520 Hz
900 MHz 4230 Hz
carrier-values for nitrogens
o3
400 (40) MHz 4850 Hz
600 (60) MHz 7250 Hz
700 (70) MHz 8400 Hz
750 (76) MHz 9000 Hz
900 (91) MHz 11000 Hz
carrier-values for deuterium
o4
400 MHz 210 Hz
600 MHz 320 Hz
700 MHz 370 Hz
750 MHz 400 Hz
900 MHz 480 Hz
carrier-values for carbon
17000 11500 5500 40004500
center of CO region ~175 ppm
7000
center of aliphaticregion ~40 ppm
center of Cregion ~45 ppm
center for decoupling ~70 ppm
400 MHz (100 MHz)
center for HMBC~100 ppm
center of Cregion ~55 ppm
composite pulse CO/C ~115 ppm
10000
carrier-values for carbon
26000 17000 8000 58006500
center of CO region ~175 ppm
10250
center of aliphaticregion ~40 ppm
center of Cregion ~45 ppm
center for decoupling ~70 ppm
600 MHz (150 MHz)
center for HMBC~100 ppm
center of Cregion ~55 ppm
14750
composite pulse CO/C ~115 ppm
carrier-values for carbon
30750 20250 9750 70008000
center of CO region ~175 ppm
12250
center of aliphaticregion ~40 ppm
center of Cregion ~45 ppm
center for decoupling ~70 ppm
700 MHz (175 MHz)
center for HMBC~100 ppm
center of Cregion ~55 ppm
17500
composite pulse CO/C ~115 ppm
carrier-values for carbon
32500 21250 10000 76008125
center of CO region ~175 ppm
12800
center of aliphaticregion ~40 ppm
center of Cregion ~45 ppm
center for decoupling ~70 ppm
750 MHz (188 MHz)
center for HMBC~100 ppm
center of Cregion ~55 ppm
18500
composite pulse CO/C ~115 ppm
carrier-values for carbon
38800 25400 11800 84009600
center of CO region ~175 ppm
15200
center of aliphaticregion ~40 ppm
center of Cregion ~45 ppm
center for decoupling ~70 ppm
900 MHz (225 MHz)
center for HMBC~100 ppm
center of Cregion ~55 ppm
22000
composite pulse CO/C ~115 ppm
400 MHz 600 MHz 700 MHz 750 MHz 900 MHz
(C,CO)120 ppm
12000 Hz 18000 Hz 21000 Hz 22500 Hz 27000 Hz
(C,CO)130 ppm
13000 Hz 19500 Hz 22750 Hz 24375 Hz 29200 Hz
B1 p B1 p B1 p B1 p B1 p
90°, 120 ppm n=1 3.1 81 4.7 54 5.4 46 5.8 43 7.0 36
90°, 130 ppm n=1 3.3 75 5.0 49 5.9 43 6.3 40 7.6 33
180°, 120 ppm n=1 6.9 72 10.4 48 12.1 41 13.0 38 15.6 32
n=2 3.1 162 4.7 108 5.4 92 5.8 86 7.0 72
180°, 130 ppm n=1 7.5 67 11.3 44 13.1 38 14.0 35 16.9 30
n=2 3.3 150 5.0 98 5.9 86 6.3 80 7.6 66
Semi-selective rectangular pulses
Semi-selective rectangular pulses
center CO-region at 175 ppmcenter C-region at 55 ppmcenter C-region at 45 ppm
90° pulses1.null (n=1) at B1 = / 15180° pulses1.null (n=1) at B1 = / 32.null (n=2) at B1 = / 15
eff [°]
/ B1
3 15 = 90° = 180°
J coupling constants in proteins
90 Hz
55 Hz 15 Hz
35 Hz11 Hz
7 Hz
140 HzH
HR
H H
CC
C
O
O
N
HC
R
N
H
CC
phc1 = (t1)0 * sw * (-360°)
phc0 = -0.5 * phc1(t1)0 first value for evolution time (including pulses)
Two scenarios are desirable1. phc1 = 0°, phc0 = 0°, first point multiplied by 0.5
folded peaks have same sign as unfolded 2. phc1 = -180°, phc0 = 90°, first point multiplied by 1
folded peaks have opposite sign as unfolded If that is not possible try to achieve phc1 = n * (-360°) and phc0 = n * 180°and use linear prediction to get back to 1. or 2.
Phase correction in the indirect dimension
Phase correction in the indirect dimension“homonuclear spectra”
H90x 90x
t1
p1 p1d0
px
= (2/px
“d0 = n*(in0/2) – 1.28*p1”
phc1 = -360°*[(d0 + 1.28*p1)/in0]
phc0 = -½*phc1
px
Phase correction in the indirect dimension“heteronuclear spectra”
px
= (2/px
“d0 = (n*in0 – 1.28*p1 – p4) /2” phc1 = -180°*[(2*d0 + 1.28*p1 + p4)/in0]
phc0 = -½*phc1
px
H
X
90x 90x
180x
t1/2 t1/2
p1 p1d0 d0
p4
SHared Incrementation Times (SHIT)
H
X
90x 90x
180x
t1a
180x
t1b t1
c
(t1a)0 = /2, t1
a = 1/(2*sw)(t1
b)0 = 0, t1b = t1
a + t1c
(t1c)0 = /2, t1
c = -/2(n-1)
= 1/2J, t1x = increment
(t1x)0 = first value
n number of complex datapoints
sw t1a t1
b(32) t1c(32) t1
b(48) t1c(48) t1
b(64) t1c(64)
3012 166 110 -56 129 -37 139 -27
4000 125 69 -56 88 -37 98 -27
5000 100 44 -56 63 -37 73 -27
6250 80 24 -56 43 -37 53 -27
8333 60 4 -56 23 -37 33 -27
10000 50 0 -50 13 -37 23 -27
sw t1a t1
b(32) t1c(32) t1
b(48) t1c(48) t1
b(64) t1c(64)
3012 166 78 -88 108 -58 123 -43
4000 125 37 -88 67 -58 82 -43
5000 100 12 -88 42 -58 57 -43
6250 80 0 -80 22 -58 37 -43
8333 60 0 -80 2 -58 17 -43
10000 50 0 -80 0 -50 7 -43
= 3.5 msec = 5.5 msec
dB-calculations, pulses correspond to voltage
voltage to power
P(W) =[U(VP-P)]2
400
NMR solvents
Productoperators: calculation
rules(1)
Productoperators: calculation
rules(2)
Product operators: trigonometry
NMR-Facility ( Räume NMR-I)
D1.01D1.04
D1.03
D1.02
D1.05/6
D1.07
NMR-Facility ( Räume NMR-II)
E 1.09
E 1.06
E 1.05
E 1.02
E 1.03
E 1.10
E 1.01
E 1.08
E 1.07
E 1.12
E 1.11
NMR-Facility (Spektrometer)
Spektrometer Raum Tel Netzwerk HH-Nummer Datendisk
AV 300 TRH 3.34 (70)2916 av300.mdc-berlin.de(141.80.190.56) HH007604 /r
AV 400 WB (MRI) B 0.03/04 529 (528) (mri-)av400.fmp-berlin.de (194.95.129.217/(236)) HH005102 /z
AV 400 WB (DNP) E 1.12 546 (549) av400dnp.fmp-berlin.de(194.95.129.228) HH004106 /q
AV 600 (FMP) D 1.04 533 fmp600.fmp-berlin.de(194.95.129.211) 10063006 /x
AV 600 (PSF) D 1.05/06 534 psf600.fmp-berlin.de(194.95.129.235) 10012991 /v
AV 600 (SEL) D 1.02 531 sel600.fmp-berlin.de(194.95.129.234) HH002008 /p
AV 600 WB E 1.06 541 (542) av600.fmp-berlin.de(194.95.129.230) HH001802 /y
AV 700 WB E 1.06 540 (545) av700.fmp-berlin.de(194.95.129.233) HH005904 /s
AV750 D 1.07 532 fmp750.fmp-berlin.de(194.95.129.215) HH009806 /w
AV800 E 1.11 547 (548) av800.fmp-berlin.de(194.95.129.212) 10062996 /m
AV 900 E 1.07-09 540 (543,544) av900.fmp-berlin.de(194.95.129.231) HH005701 /t
NMR-Spektrometer
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