ζ. Kristallogr. NCS 213 (1998) 495-Φ96 495
© by R. Oldenbourg Verlag, München
Crystal structure of (l/?*,8/?*)-8-hydroxy-19-oxa-tricyclo[8.8.1.0^'^]nona- dec-10-Z-ene-9,17,18-trione, (С8ЩЧ2)(С1бН240з)
к . Peters, E.-M. Peters
Max-Planck-Institut für Festkörperforschung. Heisenbergstraße 1. D-70506 Stuttgart, Germany Th. von Haugwitz and W. Tochtermann
Christian-Albrechts-Universität, Institut für Organische Chemie, Olshausenstraße 40, D-24098 Kiel, Germany Received September 26, 1997, CSD-No. 409099
C12
Table 1. Parameters used for the X-ray data collection
Crystal: colorless plate, size 0.35 χ 0.75 χ 0.15 mm Wavelength: Mo Ka radiation (0.71073 Â)
μ: 0.80 cm"'
Diffiractometer: Siemens P4
Scan mode: Wyckoff
'^measurement' 293 К
20max: 55°
4689 Criterion for Fo: Fo>3a(Fc.)
N(param)reßned: 267
Program: SHELXTL-plus
Source of material: The title compound was prepared as described in ref. 1.
C24H28N2O3, triclinic, PI (No. 2), a =9.845(3) Â, b =12.955(5) Â, с =8.937(3) À. α =99.35(3)°, β =110.79(2)°, γ =98.87(3)°, V=1023.4 Â^ Ζ =2, R(F) =0.054, =0.051.
Table 2. Final atomic coordinates and displacement parameters (in A^)
Atom Site X У ζ t/i»
H(4) 2/ 1.011(4) 0.121(2) -0.026(4) 0.10(1) H(8A) 2/ 1.1696(3) 0.4970(2) 0.6754(3) 0.08 H(8B) 2i 1.0479(3) 0.4054(2) 0.5324(3) 0.08 H(9A) 2/ 0.9851(3) 0.4413(2) 0.7660(3) 0.08 H(9B) 2/ 1.1262(3) 0.4031(2) 0.8671(3) 0.08 H(IOA) 2/ 1.0141(3) 0.2318(2) 0.6766(3) 0.08 H(IOB) 2/ 0.9376(3) 0.2612(2) 0.7995(3) 0.08 H(llA) 2) 0.7382(3) 0.2863(2) 0.6034(3) 0.08 H(llB) 2/ 0.8221(3) 0.2984(2) 0.4851(3) 0.08 H(12A) 2) 0.6446(3) 0.1345(2) 0.3951(4) 0.08 H(12B) 2» 0.7347(3) 0.1025(2) 0.5574(4) 0.08 H(13A) 2/ 0.8078(3) 0.0100(2) 0.3748(3) 0.08 H(14A) 2Í 1.3048(3) 0.1102(2) 0.2953(3) 0.08 H(14B) 2/ 1.2031(3) 0.0474(2) 0.1140(3) 0.08 H(15A) 2Í 1.3921(3) 0.1477(2) 0.0870(3) 0.08 H(15B) 2i 1.2654(3) 0.2103(2) 0.0345(3) 0.08 H(16A) 2i 1.5331(3) 0.2995(2) 0.2409(3) 0.08 H(16B) 2i 1.4510(3) 0.2827(2) 0.3597(3) 0.08 H(17A) 2i 1.3294(3) 0.3880(2) 0.1171(3) 0.08 H(17B) 2i 1.4743(3) 0.4526(2) 0.2683(3) 0.08 H(18A) 2i 1.3460(3) 0.4317(2) 0.4391(3) 0.08 H(18B) 2i 1.2817(3) 0.5008(2) 0.3136(3) 0.08 H(19A) 2i 1.0781(3) 0.4040(2) 0.3107(3) 0.08 H(19B) 2i 1.0924(3) 0.3391(2) 0.1550(3) 0.08 H(22A) 2i 1.4971(3) 0.0808(2) 0.6547(3) 0.08 H(23A) 2i 1.7073(3) 0.1268(2) 0.8990(3) 0.08 H(24A) 2i 1.7668(3) 0.2939(2) 1.0859(3) 0.08 H(25A) 2i 1.6113(3) 0.4131(2) 1.0336(3) 0.08
Table 3. Final atomic coordinates and displacement parameters (in Â^)
Atom Site X У ζ l/ii U n U n U12 U l i U l i
O d ) 2i 0.9697(2) 0.2368(1) 0.3415(2) 0.0327(8) 0.0382(8) 0.0435(8) 0.0062(6) 0.0074(7) 0.0091(6) C(2) 2/ 0.9268(2) 0.1287(2) 0.3350(3) 0.039(1) 0.038(1) 0.041(1) 0.0019(9) 0.008(1) 0.0064(9) C(3) 2/ 1.0104(3) 0.06%(2) 0.2586(3) 0.044(1) 0.038(1) 0.033(1) 0.0037(9) 0.003(1) 0.0046(9) 0(3) 2i 0.9978(2) -0.0277(1) 0.2274(2) 0.075(1) 0.0353(8) 0.052(1) 0.0061(8) 0.0218(9) 0.0038(7) C(4) 2i 1.1065(2) 0.1520(2) 0.2101(2) 0.036(1) 0.040(1) 0.031(1) 0.0058(9) 0.0041(9) 0.0061(8) 0(4) 2i 1.0011(2) 0.1615(1) 0.0561(2) 0.0469(9) 0.0532(9) 0.0305(8) 0.0134(7) 0.0040(7) 0.0062(7)
496
(C8H4N2)(Ci6H2403)Table 3. (Continued)
Atom Site X >· 'Ίι U22 f/33 Un f/l3 t/23
C(5) 2i 1.1193(2) 0.2566(2) ojs.-iöc:) 0.030(1) 0.037(1) 0.035(1) 0.0048(8) 0.0068(9) 0.0072(8) C(6) 2i 1.2285(2) 0.2703(2) 0.5131(2) 0.031(1) 0.032(1) 0.037(1) 0.0024(8) 0.0067(9) 0.0080(8) C(7) 2i 1.2397(2) 0.3572(2) 0.6454(2) 0.03.5( 1 ) 0.0.34(1) 0.037(1) 0.0043(8) 0.0060(9) 0.0062(8) C(8) 2i 1.1228(3) 0.4218(2) 0.6422(3) 0.045(1) 0.037(1) 0.047(1) 0.011(1) 0.004(1) 0.0052(9) C(9) 2i 1.0492(3) 0.3933(2) 0.7601(3) 0.054( 1 ) 0.055(1) 0.048( 1 ) 0.025(1) 0.013(1) 0.008(1) C(10) 2i 0.9569(3) 0.2786(2) 0.7075(3) 0.058(2) 0.059( 1 ) 0.057(2) 0.022(1) 0.027(1) 0.018(1) C ( l l ) 2i 0.8077(3) 0.2597(2) 0.5633(3) 0.048( 1 ) 0.057( 1) 0.065(2) 0.015(1) 0.026(1) 0.014(1) C(12) 2i 0.7425(3) 0.1406(2) 0.4761(4) 0.05.4(2) 0.061(2) 0.082(2) 0.006(1) 0.031(1) 0.015(1) C(13) 2i 0.8276(3) 0.0868(2) 0.3918(3) 0.051(1) 0.045(1) 0.061(2) 0.003(1) 0.020(1) 0.009(1) C(14) 2i 1.2396(3) 0.1166(2) 0.1897(3) 0.044(1) 0.052(1) 0.040(1) 0.012(1) 0.008(1) 0.002(1) C(15) 2i 1.3328(3) 0.1890(2) 0.1251(3) 0.054(2) 0.087(2) 0.055(2) 0.010(1) 0.024(1) 0.007(1) C(16) 2i 1.4386(3) 0.2919(2) 0.2515(3) 0.042(1) 0.088(2) 0.064(2) 0.001(1) 0.018(1) 0.022(1) C(17) 2i 1.3867(3) 0.3957(2) 0.2321(3) 0.057(2) 0.079(2) 0.063(2) -0.006(1) 0.021(1) 0.024(1) C(18) 2i 1.2922(3) 0.4298(2) 0.3252(3) 0.063(2) 0.051(1) 0.058(2) -0.006(1) 0.017(1) 0.015(1) C(19) 2i 1.1349(3) 0.3599(2) 0.2731(3) 0.047(1) 0.039(1) 0.045(1) 0.005(1) 0.012(1) 0.0127(9) N(20) 2i 1.3133(2) 0.2007(1) 0.5426(2) 0.0350(9) 0.0393(9) 0.0366(9) 0.0090(8) 0.0089(8) 0.0082(7) C(21) 2i 1.4263(2) 0.2209(2) 0.6946(2) 0.032(1) 0.043(1) 0.036(1) 0.0056(9) 0.0085(9) 0.0112(9) C(22) 2i 1.5199(3) 0.1487(2) 0.7305(3) 0.044(1) 0.054(1) 0.051(1) 0.019(1) 0.015(1) 0.012(1) C(23) 2/ 1.6433(3) 0.1759(2) 0.8742(3) 0.047(1) 0.076(2) 0.062(2) 0.028(1) 0.013(1) 0.025(1) C(24) 2i 1.6779(3) 0.2753(2) 0.9870(3) 0.036(1) 0.087(2) 0.045(1) 0.014(1) 0.001(1) 0.012(1) C(25) 2i 1.5866(3) 0.3453(2) 0.9566(3) 0.037(1) 0.067(2) 0.042(1) 0.005(1) 0.003(1) 0.004(1) C(26) 2i 1.4553(2) 0.3172(2) 0.8113(3) 0.033(1) 0.047(1) 0.036(1) 0.0050(9) 0.0090(9) 0.0092(9) N(27) 2i 1.3550(2) 0.3811(1) 0.7866(2) 0.037(1) 0.0407(9) 0.038(1) 0.0034(8) 0.0048(8) 0.0033(7)
References
1. von Haugwitz, T. : Synthese neuer makrocyclischer Ketone. Dissertation.
Universität Kiel, Germany 1993.
2. Sheldrick, G. M.. Program Package SHELXTL-plus. Release 4.1.
Siemens Analytical X-Ray Instruments Inc., Madison (W153719), US A 1990.
