Crystal structure of methyl 2-O-acetyl-3,5-O-isopropylidene-2-p-nitrophenylazo-β-D-xylofuranoside, C17H21N3O8

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Crystal structure of methyl 2- O -acetyl-3,5- O -isopropylidene-2- p -nitrophenylazo- β -D-xylofuranoside, C ₁₇ H ₂₁ N ₃ O ₈

BERNARDINELLI, Gérald Hugues, TRONCHET, Jean Marcel Julien, TRONCHET, Jeannine

BERNARDINELLI, Gérald Hugues, TRONCHET, Jean Marcel Julien, TRONCHET, Jeannine.

Crystal structure of methyl 2- O -acetyl-3,5- O -isopropylidene-2- p -nitrophenylazo- β

-D-xylofuranoside, C ₁₇ H ₂₁ N ₃ O ₈ . Zeitschrift für Kristallographie , 1993, vol. 203, no. 1-2, p.

129-131

Available at:

http://archive-ouverte.unige.ch/unige:151908

Disclaimer: layout of this document may differ from the published version.

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Zeitschrift für Kristallographie 203, 129-131 (1993)

© by R. Oldenbourg Verlag, München 1993 - 0044-2968/93 $3.00+0.00

Crystal structure of methyl 2-0-acetyl-3,5-0-isopro- pylidene-2-/?-nitrophenylazo-/f-D-xylofuranoside, C ¹⁷ H ²¹ N ³ O ⁸

G. Bernardinelli

Laboratoire de Cristallographie, 24 quai Ernest-Ansermet, CH-1211 Geneva, Switzerland and J. M. J. Tronchet and J. F. Tronchet

Institut de Chimie Pharmaceutique, Université de Genève, 30 quai Ernest-Ansermet, CH-1211 Geneva, Switzerland

(Received February 14,1992)

Source of material : see réf. 1.

Monoclinic, P2! (no 4), α = 10.080(3), ¿ = 8.184(1), c = 12.476(3) Α, β =

108.59(2)°, V = 975.6 A

³

, Ζ = 2, R = 0.053.

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130 G. Bernardinelli. J. M. J. Tronche! and J. F. Tronche!

Table 1. Parameters used for the X-ray data collection

DifTractometer Number of unique

type: Philips PW1100 reflections: 1451

Wave length : Mo K., radiation Criterion for unob-

(0.7107 A) served reflections: F,, < 4<t(F

0

) Crystal yellow prism, size Number of refined

characteristics: 0 . 1 6 x 0 . 2 4 x 0.25 mm parameters : 253

Temperature of Scan mode: co-28scan

measurement: 293 Κ μ· 0.96 c m "

1

2 ö

^{m a}

, : 46 Structure solution Multan 87

program used : XTAL3.0

Table 2. Final atomic coordinates and displacement parameters (in Â²)

Atom X y I W U , , u „ u „ U n U2 J

O(l) 0.6350(7) -0.1044(8) 0.3204(5) 0.095(5) 0.055(4) 0.053(3) -0.001(4) 0.025(4) 0.002(3) CH 2) 0.3946(6) 0.1182(9) 0.3059(5) 0.063(4) 0.079(5) 0.061(4) -0.006(4) 0.020(3) 0.013(4) 0(3) 0.5424(6) 0.2139(8) 0.2089(4) 0.062(4) 0.076(5) 0.052(3) 0.013(4) 0.025(3) 0.007(4) 0<4) 0.6238(6) -0.1367(9) 0.1336(5) 0.077(4) 0.082(5) 0.054(4) -0.015(4) 0.005(3) -0.009(4) 0<5) 0.9018(6) 0.0715(8) 0.3303(5) 0.051(3) 0.071(5) 0.054(4) - 0.007(4) 0.007(3) -0.001(4) 0(6) 0.9401(8) 0.3415(9) 0.3119(6) 0.115(6) 0.075(6) 0.095(5) -0.028(5) 0.033(5) -0.009(5) 0(7) 0.7459(8) 0.304(1) - 0 3988(5) 0.101(6) 0.157(9) 0.040(4) 0.017(6) 0.016(4) -0.007(5) 0(8) 0.9546(8) 0.210(1) -0.3612(6) 0.108(6) 0.120(7) 0.093(5) -0.001(6) 0.068(5) 0002(5) NO) 0.7602(8) 0.136(1) 0.1344(6) 0.066(5) 0.070(6) 0.054(5) -0.006(5) 0.022(4) - 0 004(4) N(2) 0.8692(7) 0.109(1) 0.1127(6) 0.053(4) 0.065(6) 0.067(5) 0.003(5) 0.022(4) 0.009(4) N<3) 0.853(1) 0.247(1) -0.3344(6) 0.088(6) 0.066(6) 0.054(5) -0.022(6) 0.032(5) -0.013(5) C(1) 0.7113(9) -0.097(1) 0.2411(8) 0.054(5) 0.071(7) 0.062(6) 0.003(6) 0.018(5) 0.003(6) C(2) 0.7633(9) 0.083(1) 0.2479(7) 0.050(5) 0.058(6) 0.052(5) -0.002(5) 0.011(4) 0.006(5) C(3) 0.6688(9) 0.179(1) 0.2996(7) 0.049(5) 0.063(7) 0.045(5) 0.002(5) 0.011(4) -0.009(5) C(4) 0.6414(9) 0.047(1) 0.3784(7) 0.065(6) 0.067(7) 0.040(5) -0.003(6) 0.007(4) 0.010(5) C(5) 0.506(1) 0.076(1) 0.4047(8) 0.078(6) 0.072(7) 0 060(6) -0.013(7) 0.027(5) 0.006(6) C(6) 0.427(1) 0.253(1) 0.2461(7) 0.071(6) 0 090(9) 0.055(6) 0.016(7) 0.019(5) -0.003(6) C(7) 0.302(1) 0.267(1) 0.1389(8) 0.089(7) 0.10(1) 0.069(6) 0.047(7) 0.030(6) 0.016(7) C(8) 0.450(1) 0.411(1) 0.3159(9) 0.098(8) 0.081(8) 0.096(7) 0.003(7) 0.062(7) -0.002(7) C(9) 0.607(1) -0.306(2) 0.1172(9) 0.084(7) 0.12(1) 0.083(7) -0.035(8) 0.029(6) -0.023(8) C(10) 0.9795(9) 0.211(2) 0.3545(7) 0.071(6) 0.100(9) 0.064(6) -0.019(7) 0.034(5) -0.012(7) C(ll) 1.1178(9) 0.179(2) 0.4420(8) 0.048(6) 0.17(1) 0.081(7) -0.022(8) 0.019(5) -0.040(9) Q12) 0.8629(9) 0.157(1) 0.0005(7) 0.053(5) 0.052(6) 0.048(5) - 0.002(5) 0.014(4) -0.007(5) C(13) 0.7619(9) 0.261(1) -0.0680(8) 0.062(6) 0.061(7) 0.059(6) 0.009(6) 0.022(5) -0.008(5) CO 4) 0.7568(9) 0.290(1) -0.1780(7) 0.050(5) 0.071(7) 0.053(6) -0.001(6) 0.006(5) 0.001(5) CO 5) 0.8597(9) 0.219(1) -0.2145(7) 0.057(5) 0.070(7) 0.049(5) -0.018(6) 0.021(5) -0.018(5) CO 6) 0.9633(9) 0.121(1) -0.1472(8) 0.049(5) 0.073(7) 0.074(7) -0.003(6) 0.027(5) -0.003(6) C(17) 0.9651(9) 0.087(1) -0.0380(7) 0.055(6) 0.082(8) 0.060(6) -0.003(6) 0.019(5) 0.007(6) HO) 0.7989 -0.1813 0.2592 0.05066

H(3) 0.7097 0.2934 0.3415 0.05066 H(4) 0.7236 0.0502 0.4604 0.05066 H(51) 0.4794 -0.0354 0.4419 0.05066 H(52) 0.5226 0.1751 0.4667 0.05066 H(71) 0.2088 0.2932 0.1619 0.05066 H(72) 0.3214 0.3679 0.0884 0.05066 H(73) 0.2857 0.1557 0.089 0.05066 H(81) 0.4688 0.5105 0.2659 0.05066 H(82) 0.3562 0.4358 0.3395 0.05066

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Methyl 2-0-acetyl-3,5-0-isopropylidene-2-p-nitrophenylazo-/?-D-xylofuranoside 131

Table 2. (Continued)

Alom ΛΓ > ζ U i ^ U , , U2 2 U3 J U1 2 U , j U2 J

H(83) 0.539 0.3992 0.3935 0.05066 H(91) 0.7077 -0.3616 0.1306 0.05066 H(92) 0.5604 -0.3531 0.1799 0.05066 H(93) 0.5371 -0.3378 0.0335 0.05066 H(11l) 1.092 0.1234 0.5115 0.05066 H(112) 1.1655 0.0833 0.402 0.05066 H(113) 1.1998 0.2648 0.4771 0.05066 H(I3) 0.6856 0.3174 -0.0351 0.05066 H(14) 0.6764 0.3695 -0.2347 0.05066 H(16) 1.0423 0.0702 -0.1805 0.05066 H(17) 1.0445 0.0064 0.0159 0.05066

Further details οΓ the structure determination (e.g. structure factors) have been deposited within the relevant database and can be accessed as Collection No. 320403 or ordered from the Fachinformationszentrum Karlsruhe, D-7514 Eggenstein-Leopoldshafen.

Crystal structure of methyl 2-<i>O</i>-acetyl-3,5-<i>O</i>-isopropylidene-2-<i>p</i>-nitrophenylazo-<i>β</i>-D-xylofuranoside, C<sub>17</sub>H<sub>21</sub>N<sub>3</sub>O<sub>8</sub>