Th. von Haugwitz and W. Tochtermann

Zeitschrift für Kristallographie - New Crystal Structures 213, 99-100 99

© by R. Oldenbourg Verlag, München 1998

Crystal structure of (2/?*,5S*)-2,5-dihydro-5-hydroxy-2-methoxy-3,4- hexamethylene-2,5-(6,13-dioxooctano)-furan, C19H28O5

K. Peters, E.-M. Peters

Max-Planck-lnstitut für Festköφeгforschung, Heisenbergstraße 1, D-70506 Stuttgart, Germany

Th. von Haugwitz and W. Tochtermann

Christian-Albrechts-Universitat Kiel, Institut für Organische Chemie. Olshausenstraße 40, D-24098 Kiel, Germany

Received February 11, 1997, CSD-No. 402840

Source of material: The title compound was prepared as described in ref. 1.

T a b l e 1. Parameters used for the X-ray data collection

Crystal: colorless prism, size 0.6 χ 0.7 χ 0.4 mm Wavelength: M o /Ca radiation (0.71073 Λ)

μ: 0.90 c m " '

Diffractometer: Siemens P4

Scan mode: ω

Tmeasuremenl- 293 К

29тал: 55°

N(A*:/)im<í«·: 4078 Criterion for Fo'· f o > 3 a ( f o )

N(j>aram)refi/¡e>r· 225

Program: SHELXTL-plus

T a b l e 3. Final atomic coordinates and displacement parameters (in Â^)

C19H28O5, monocUnic, РШсХ ( N o . 14), a = 1 4 . 1 4 1 ( 4 ) Â ,

¿»=13.017(4) К с =9.670(3) К β =93.92(2)°, V=1775.8Â^ Ζ=4,

T a b l e 2. Final atomic coordinates and displacement parameters (in Â^)

Atom Site X У ζ t/iso

H(5) 4e 0.101(2) 0.447(2) 0.029(3) 0.08(1) H(7A) 4c 0.4473(2) 0.7246(2) 0.1896(3) 0.08 H(7B) 4e 0.3449(2) 0.7094(2) 0.1197(3) 0.08 H(8A) 4e 0.3514(2) 0.8729(2) 0.2028(3) 0.08 H(8B) 4e 0.3942(2) 0.8358(2) 0.3480(3) 0.08 H(9A) 4e 0.2512(2) 0.7688(2) 0.3992(3) 0.08 H(9B) 4e 0.2381(2) 0.8851(2) 0.3601(3) 0.08 H(IOA) 4e 0.1932(2) 0.7439(2) 0.1523(3) 0.08 H(IOB) 4e 0.1466(2) 0.8515(2) 0.1738(3) 0.08 H ( l l A ) 4e 0.0749(2) 0.7763(2) 0.3671(3) 0.08 H ( l l B ) 4e 0.0341(2) 0.7391(2) 0.2208(3) 0.08 H(12A) 4e 0.0674(2) 0.6077(2) 0.3991(3) 0.08 H(12B) 4e 0.1734(2) 0.6218(2) 0.3646(3) 0.08 H(14A) 4e 0.4438(2) 0.4086(2) 0.3905(3) 0.08 H(14B) 4e 0.3772(2) 0.3122(2) 0.3885(3) 0.08 H(15A) 4e 0.3756(2) 0.4684(3) 0.5826(3) 0.08 H(15B) 4e 0.4251(2) 0.3618(3) 0.6095(3) 0.08 H(16A) 4e 0.2972(2) 0.3594(3) 0.7260(3) 0.08 H(16B) 4e 0.2759(2) 0.2867(3) 0.5984<3) 0.08 H(17A) 4e 0.1630(3) 0.4228(3) 0.6752(3) 0.08 H(17B) 4e 0.2103(3) 0.4792(3) 0.5544(3) 0.08 H(18A) 4e 0.1010(2) 0.3015(2) 0.5287(3) 0.08 H ( I 8 B ) 4e 0.0738(2) 0.4092(2) 0.4651(3) 0.08 H(19A) 4e 0.1156(2) 0.3105(2) 0.2878(3) 0.08 H(19B) 4e 0.2090(2) 0.2752(2) 0.3710(3) 0.08 H(20A) 4e 0.4437(2) 0.4203(2) -0.0216(3) 0.08 H(20B) 4e 0.3344(2) 0.4256(2) -0.0043(3) 0.08 H(20C) 4e 0.3996(2) 0.3577(2) 0.0965(3) 0.08

Atom Site X У ζ ί / ι ι ί/22 ί/зз Un Un {/23

0 ( l ) 4e 0.2504(1) 0.5507(1) 0.1397(2) 0.0429(8) 0.062(1) 0.0376(8) -0.0010(7) -0.0002(6) 0.0053(8) C(2) 4e 0.3366(1) 0.5268(2) 0.2206(2) 0.033(1) 0.059(1) 0.038(1) -0.001(1) 0.0052(9) -0.002(1) 0 ( 2 ) 4e 0.4102(1) 0.5066(1) 0.1342(2) 0.0448(9) 0.073(1) 0.057(1) -0.0088(8) 0.0207(8) -0.0076(9) C(3) 4e 0.3107(1) 0.4390(2) 0.3124(2) 0.035(1) 0.052(1) 0.040(1) 0.0024(9) 0.0070(9) 0.000(1) C(4) 4e 0.2204(1) 0.4156(2) 0.2867(2) 0.038(1) 0.054(1) 0.042(1) -0.000(1) 0.0063(9) -0.000(1) C(5) 4e 0.1762(1) 0.4812(2) 0.1720(2) 0.036(1) 0.064(2) 0.042(1) -0.003(1) -0.0003(9) -0.005(1) 0 ( 5 ) 4e 0.1483(1) 0.4207(2) 0.0584(2) 0.052(1) 0.085(1) 0.054(1) 0.001(1) -0.0117(9) -0.015(1) C(6) 4e 0.3680(2) 0.6265(2) 0.2961(2) 0.040(1) 0.064(2) 0.045(1) -0.005(1) 0.004(1) 0.002(1)

100 CI9H2805

Table 3. (Continued)

Atom Site

У ζ

U^2

Uli

0(6) 4e 0.3792(1) 0.6284<1) 0.4205(2) 0.086(1) 0.071(1) 0.042(1) -0.010(1) -0.0059(9) -0.000(1) C(7) 4e 0.3813(2) 0.7191(2) 0.2062(3) 0.070(2) 0.062(2) 0.050(1) -0.016(1) 0.008(1) 0.003(1) C(8) 4e 0.3499(2) 0.8198(2) 0.2715(3) 0.101(2) 0.063(2) 0.058(2) -0.020(2) 0.005(2) 0.004(1) C(9) 4e 0.2508(2) 0.8179(2) 0.3250(3) 0.105(2) 0.059(2) 0.050(2) 0.005(2) -0.002(2) -0.005(1) C(10) 4e 0.1695(2) 0.7899(2) 0.2194(3) 0.102(2) 0.073(2) 0.058(2) 0.023(2) -0.006(2) 0.012(2) C ( l l ) 4e 0.0885(2) 0.7381(2) 0.2859(3) 0.071(2) 0.092(2) 0.078(2) 0.033(2) -0.004(2) -0.006(2) C(12) 4e 0.1086(2) 0.6265(2) 0.3283(3) 0.043(1) 0.080(2) 0.055(1) 0.012(1) 0.007(1) -0.003(1) C(13) 4e 0.0941(2) 0.5519(2) 0.2105(3) 0.038(1) 0.085(2) 0.053(1) 0.007(1) -0.005(1) -0.002(1) 0(13) 4e 0.0202(1) 0.5469(2) 0.1429(2) 0.051(1) 0.165(2) 0.102(2) 0.030(1) -0.031(1) -0.049(2) C(14) 4e 0.3819(2) 0.3842(2) 0.4095(3) 0.042(1) 0.079(2) 0.061(2) 0.014(1) -0.001(1) 0.004(2) C(15) 4e 0.3719(2) 0.3961(3) 0.5631(3) 0.071(2) 0.093(2) 0.075(2) 0.004(2) -0.016(2) 0.023(2) C(16) 4e 0.2852(2) 0.3568(3) 0.6271(3) 0.120(3) 0.088(2) 0.048(2) -0.015(2) 0.003(2) 0.011(2) C(17) 4e 0.1943(3) 0.4134(3) 0.5911(3) 0.128(3) 0.080(2) 0.061(2) 0.020(2) 0.042(2) 0.008(2) C(18) 4e 0.1250(2) 0.3622(2) 0.4868(3) 0.070(2) 0.077(2) 0.086(2) 0.002(2) 0.036(2) 0.018(2) C(19) 4e 0.1666(2) 0.3318(2) 0.3522(3) 0.047(1) 0.074(2) 0.066(2) -0.016(1) 0.009(1) 0.005(1) C(20) 4e 0.3958(2) 0.4203(2) 0.0441(3) 0.065(2) 0.089(2) 0.078(2) -0.010(2) 0.034(2) -0.022(2)

References

1. von Haugwitz, Th.: Synthese neuermakrocyclìscherKetone. Dissertation, University of Kiel, Germany 1993.

2. Sheldrick, G. M.: Program Package SHELXTL-plus. Release 4.1.

Siemens Analytical X-Ray Instniments Inc., Madison (WI 53719), USA

1990.