Zeitschrift für Kristallographie - New Crystal Structures 213, П 1 - П % 277
© by R. Oldenbourg Verlag, München 1998
Crystal structure of (2/?*,35*,4/?*,55*)-2,3,4,5-tetrahydroxy-3,4-hexame- thylene-2,5-(6,13-dioxooctano)tetrahydrofuran, CisHisO?
K. Peters, E.-M. Peters
Max-Planck-Institut für Festkörperforschung. Heisenbergstraße 1. D-70506 Stuttgart, Germany
Th. von Haugwitz and W. Tochtermann
Christian-Albrechts-Universität Kiel, Institut für Organische Chemie, OlshausenstraBe 40, D-24098 Kiel, Germany Received April 15, 1997, CSD-No. 409007
Table 2. Final atomic coordinates and displacement parameters (in Â^)
Source of material: The title compound was prepared as described in ref. 1.
C18H28O7, orthorhombic, Pbca (No. 61), a =14.884(5) Â,
¿=11.75(X3) Â, с =20.795(6) Â, V =3636.8 Â ^ Ζ =8, R(F) =0.051,
=0.041.
Table 1. Parameters used for the X-ray data collection
Crystal: colorless prism, size 0.35 χ 0.35 χ 0.55 nun Wavelength: Mo ATaradiaüon (0.71073 Λ)
μ: 1.00 cm"' Diffractometer: Siemens P4 Scan mode: ω Tmeasuremenl- 2 9 3 К
2θα,ακ: 55"
Щ/гкОтщш·: 4173 Criterion f o r Foi Fo>3 a(Fo) N(param)r^nei/: 243
Program: SHELXTL-plus
Atom Site X У ζ Uisc
H(2) 8c 0.108(2) -0.248(2) 0.673(1) 0.057(8) H(3) 8c 0.267(2) 0.055(2) 0.707(1) 0.09(1) H(4) Sc 0.115(2) 0.198(2) 0.695(1) 0.067(9) H(5) 8c -0.097(2) -0.080(2) 0.726(1) 0.08(1) H(7A) 8c 0.1188(2) 0.1109(2) 0.8001(1) 0.08 H(7B) 8c 0.0523(2) 0.2061(2) 0.8231(1) 0.08 H(8A) 8c 0.0018(2) 0.0738(2) 0.9039(1) 0.08 H(8B) 8c 0.0985(2) 0.1231(2) 0.9150(1) 0.08 H(9A) 8c 0.0921(2) -0.0726(2) 0.9356(1) 0.08 H(9B) 8c 0.0666(2) -0.0933(2) 0.8634(1) 0.08 H(IOA) 8c 0.2333(2) -0.0217(2) 0.9102(1) 0.08 H(IOB) 8c 0.2091(2) -0.0077(2) 0.8373(1) 0.08 H ( l l A ) 8c 0.2991(2) -0.1684(2) 0.8581(1) 0.08 H ( l l B ) 8c 0.2191(2) -0.2202(2) 0.8974(1) 0.08 H(12A) 8c 0.1329(2) -0.2314(2) 0.80326(9) 0.08 H(12B) 8c 0.2219(2) -0.3010(2) 0.79478(9) 0.08 H(I4A) 8c 0.1638(1) -0.0425(2) 0.57079(9) 0.08 H(I4B) 8c 0.2527(1) -0.0715(2) 0.60778(9) 0.08 H(15A) 8c 0.2848(2) 0.0608(2) 0.5317(1) 0.08 H(15B) 8c 0.2968(2) 0.1173(2) 0.5995(1) 0.08 H(16A) 8c 0.1747(2) 0.2248(2) 0.5867(1) 0.08 H(16B) 8c 0.2288(2) 0.2358(2) 0.5223(1) 0.08 H(I7A) 8c 0.1025(2) 0.2034(2) 0.4765(1) 0.08 H(17B) 8c 0.1212(2) 0.0756(2) 0.4935(1) 0.08 H(18A) 8c 0.0181(2) 0.2176(2) 0.5714(1) 0.08 H(I8B) 8c -0.0247(2) 0.1378(2) 0.5193(1) 0.08 H(I9A) 8c -0.0528(2) 0.0527(2) 0.6118(1) 0.08 H(I9B) 8c 0.0257(2) -0.0182(2) 0.5815(1) 0.08
Table 3. Final atomic coordinates and displacement parameters (in  ' )
Atom Site X У ζ Un Uli ί/зз Un Un Un
0(1) 8c 0.07380(9) -0.0829(1) 0.74576(6) 0.0363(8) 0.0354(7) 0.0419(7) 0.0042(7) 0.0070(6) 0.0010(6) 0(2) 8c 0.1152(1) -0.1880(1) 0.65474(7) 0.0499(9) 0.0318(8) 0.0467(9) -0.0064(7) 0.0004(7) -0.0054(8) C(2) 8c 0.1421(1) -0.1069(2) 0.70047(9) 0.034(1) 0.034(1) 0.038(1) -0.0011(9) 0.0045(9) -0.0056(9) 0(3) 8c 0.2127(1) 0.0770(1) 0.70616(7) 0.0340(8) 0.0375(8) 0.0477(9) -0.0043(7) -0.0031(7) -0.0064(7) C(3) 8c 0.1598(1) 0.0064(2) 0.66479(9) 0.032(1) 0.031(1) 0.039(1) -0.0032(9) -0.0001(9) -0.0043(9) 0(4) 8c 0.0651(1) 0.1810(1) 0.68113(7) 0.045(1) 0.0322(8) 0.0554(9) -0.0007(7) -0.0054<8) -0.0039(7)
278
C18H28O7Table 3. (Continued)
Atom Site X У г ί/м 1/22 Uìì Un ί/|3 t/23
C(4) 8c 0.0634(1) 0.0633(2) 0.66428(9) 0.037(1) 0.030(1) 0.043(1) -0.0026(9) -0.003(1) -0.0038(9) 0(5) 8c -0.0637(1) -0.0564(1) 0.69734(8) 0.0383(9) 0.053(1) 0.056(1) -0.0125(8) 0.0005(8) -0.0072(8) C(5) 8c 0.0126(1) -0.0020(2) 0.7202(1) 0.029(1) 0.036(1) 0.047(1) 0.0002(9) -0.002(1) -0.004(1) 0(6) 8c -0.0897(1) 0.0944(1) 0.78954(7) 0.0360(9) 0.0464(9) 0.066(1) 0.0047(7) 0.0065(8) -0.0078(8) C(6) 8c -0.0108(1) 0.0764(2) 0.7776(1) 0.036(1) 0.031(1) 0.046(1) 0.001(1) 0.003(1) 0.002(1) C(7) 8c 0.0616(2) 0.1254(2) 0.8198(1) 0.042(1) 0.043(1) 0.052(1) 0.002(1) -0.001(1) -0.011(1) C(8) 8c 0.0624(2) 0.0748(2) 0.8882(1) 0.060(2) 0.069(2) 0.049(1) 0.008(1) 0.001(1) -0.015(1) C(9) 8c 0.0998(2) -0.0456(2) 0.8924(1) 0.059(2) 0.062(2) 0.039(1) 0.003(1) 0.004(1) -0.002(1) C(10) 8c 0.1994(2) -0.0529(2) 0.8751(1) 0.055(1) 0.058(2) 0.045(1) 0.003(1) -0.006(1) -0.006(1) C ( l l ) 8c 0.2349(2) -0.1722(2) 0.8618(1) 0.057(2) 0.058(1) 0.047(1) 0.008(1) -0.004(1) 0.004(1) C(12) 8c 0.1970(2) -0.2262(2) 0.79962(9) 0.055(1) 0.040(1) 0.047(1) 0.008(1) -0.002(1) 0.001(1) 0(13) 8c 0.2971(1) -0.1425(1) 0.72302(7) 0.0363(9) 0.0555(9) 0.0582(9) 0.0046(7) 0.0000(8) -0.0013(8) C(13) 8c 0.2199(1) -0.1567(2) 0.74064(9) 0.040(1) 0.032(1) 0.043(1) 0.003(1) 0.000(1) -0.0086(9) C(14) 8c 0.2077(1) -0.0143(2) 0.60064(9) 0.047(1) 0.045(1) 0.043(1) -0.003(1) 0.008(1) -0.002(1) C(15) 8c 0.2540(2) 0.0878(2) 0.5693(1) 0.064(2) 0.065(2) 0.043(1) -0.017(1) 0.007(1) 0.000(1) C(16) 8c 0.1940(2) 0.1853(2) 0.5488(1) 0.088(2) 0.056(2) 0.054(1) -0.023(2) 0.003(1) 0.008(1) C(17) 8c 0.1106(2) 0.1500(2) 0.5110(1) 0.091(2) 0.060(2) 0.051(1) -Ό.008(2) -0.006(1) 0.015(1) C(18) 8c 0.0234(2) 0.1458(2) 0.5498(1) 0.075(2) 0.063(2) 0.050(1) 0.002(1) -0.017(1) 0.007(1) C(19) 8c 0.0099(2) 0.0532(2) 0.6008(1) 0.046(1) 0.049(1) 0.047(1) -0.004(1) -0.009(1) -0.000(1)
References
von Haugwitz, Th.: Synthese neuer makiocyclischer Ketone. Dissertation, Universität Kiel, Germany 1993.
Sheldrick, G. M.: Program Package SHELXTL-plus. Release 4.1.
Siemens Analytical X-Ray Instruments Inc., Madison (W153719), US A 1990.
