Zeitschrift für Kristallographie - New Crystal Structures 213, 299-301
299
© by R. Oldenbourg Verlag, München 1998
Crystal structure of (3aÄ*,6aÄ*,9a/?*,9b/?*)-spiro[(5',5'-dimethyI-l',3'-di·
oxan)-2',6-(decahydro-9a-methoxycarbonyl-9-oxoazuIeno[4,5-c]furan- 1(ЗЯ)-опе)], C19H26O7
к. Peters, Е.-М. Peters
Max-Planck-Institut für Festkörperforschung, Heisenbergsü-aße 1, D-70506 Stuttgart, Germany
T. Panitzsch and W. Tochtermann
Christlan-Albrechts-Universität Kiel, Institut für Organische Chemie, OlshausensCraße 40, D-24098 Kiel, Germany Received April 15, 1997, CSD-No. 409013
C2lO ГЛС22
Fig. 1. Molecule 1.
Source of material: The title compound was prepared as described
Fig. 2. Molecule 2.
Table 2. Final atomic coordinates and displacement parameters (in Â^) in réf. 1.
Atom Site X У ζ £/iso
C19H26O7, t r i c l i n i c , / ' l (No. 2), a =10.224(1) Â, b =11.326(1) Â,
с =16.326(1) Â, α =108.42(1)°, β =92.26(1)°, γ =90.67(1)°, H(3A) H(3B)
2i 2i
0.2997(2) 0.2820(2)
0.3400(2) 0.2316(2)
0.9804(1) 0.8926(1)
0.08 0.08 V = 1 7 9 1 . 7 Â ^ Ζ =4, /i(F) =0.057, Ry^F) =0.059. H(4A) 2i 0.6086(2) 0.1535(2) 0.8798(1) 0.08 H(4B) 2i 0.4798(2) 0.1050(2) 0.9088(1) 0.09 H(5A) 2i 0.5082(2) 0.0152(2) 0.7620(1) 0.08 H(5B) 2i 0.3756(2) 0.0850(2) 0.7801(1) 0.08 Table 1. Parameters used for the X-ray data collection H(7A)
H(7B) 2i 2i
0.6373(2) 0.7763(2)
0.2367(2) 0.2652(2)
0.6135(1) 0.6603(1)
0.08 0.08 H(8A) 2i 0.5730(3) 0.4328(2) 0.6728(1) 0.08 Crystal: colorless prism, 0.5 χ 0.55 χ 0.3 mm H(8B) 2i 0Л22Ю) 0.4599(2) 0.6686(1) 0.08
Wavelength: Mo JCa radiation (0.71073 A) H(IÌA) 2i 0.5774(2) 0.4514(2) 0.9298(1) 0.08
μ: 1.00 cm"' H(12A) 2i 0.5150(2) 0.3007(2) 0.9790(1) 0.08
Diffractometer: Siemens P4 H(13A) 2i 0.6888(2) 0.1707(2) 0.7504(1) 0.08
Scan mode: ω H(15A) 2i 0.2442(2) 0.1671(2) 0.7176(1) 0.08
Tmeasurement- 293 К H(15B) 2i 0.2282(2) 0.2779(2) 0.6800(1) 0.08
29max: 55° H(17A) 2i 0.4018(2) -0.0338(2) 0.5400(1) 0.08
N(AW)„„/,„e: 8095 H(I7B) 2i 0.3544(2) -0.0232(2) 0.6321(1) 0.08
Criterion for Fo: Fo>3a(Fo) H(20A) 2i 1.0648(2) 0.3159(2) 0.8316(2) 0.08
469 H(20B) 2i 0.9951(2) 0.2539(2) 0.8922(2) 0.08
Program; SHF,I XTL-plus H(20C) 2i 1.0140(2) 0.3990(2) 0.9202(2) 0.08
Program; SHF,I XTL-plus
H(21A) 2i 0.2710(3) 0.2462(3) 0.5252(2) 0.08 H(21B) 2i 0.3425(3) 0.1264(3) 0.4720(2) 0.08
300
C19H2607Table 2. (Continued) Table 2. (Continued)
Atom Site > τ f i s o Atom Site χ у Ζ Í/.SO
H(21C) 2/ 0.4177(3) 0.2269(3) 0.5487(2) 0.08 H(12B) 2/ -0.0548(2) -0.8111(2) -0.9791(1) 0.08 H(22A) 2i 0.1601(3) -0.0015(3) 0.5026(2) 0.08 H(13B) 2/ 0.1519(2) -0.6721(2) -0.7516(1) 0.08 H(22B) 2i 0.0922(3) 0.1174(3) 0.5605(2) 0.08 H(15C) 2/ -0.2873(2) -0.6699(2) -0.7182(1) 0.08 H(22C) 2/ 0.1310(3) 0.0110(3) 0.5985(2) 0.08 H(15D) 2i -0.3008(2) -0.7780(2) -0.6780(1) 0.08 HOC) 2i -0.2687(2) -0.8553(2) -0.9797(1) 0.08 H(17C) 2/ -0.1023(2) -0.4632(2) -0.5418(1) 0.08 H(3D) 2i -0.2744(2) -0.7420(2) -0.8947(1) 0.08 H(17D) 2/ -0.1620(2) -0.4756(2) -0.6342(1) 0.08 H(4C) 2i 0.0549(2) -0.6615(2) -0.8820(1) 0.08 H(20D) 2/ 0.5134(2) -0.8072(2) -0.8311(2) 0.08 H(4D) 2i -0.0768(2) -0.6152(2) -0.9121(1) 0.08 H(20E) 2i 0.4347(2) -0.7535(2) -0.8952(2) 0.08 H(5C) 2i -0.0278(2) -0.5199(2) -0.7660(1) 0.08 H(20F) 2/ 0.4520(2) -0.8976(2) -0.9182(2) 0.08 H(5D) 2i -0.1637(2) -0.5910(2) -0.7827(1) 0.08 H(21D) 2/ -0.0909(3) -0.7206(3) -0.5463(2) 0.08 H(7C) 2i 0.1175(2) -0.7339(2) -0.6126(1) 0.08 H(21E) 2/ -0.2347(3) -0.7435(3) -0.5238(2) 0.08 H(7D) 2i 0.2505(2) -0.7609(2) -0.6589(1) 0.08 H(21F) 2i -0.1573(3) -0.6213(3) -0.4706(2) 0.08 H(8C) li 0.0454(3) -0.9315(2) -0.6694(1) 0.08 H(22D) li -0.3392(3) -0.4953(3) -0.5031(2) 0.08 H(8D) 2i 0.1959(3) -0.9551(2) -0.6645(1) 0.08 H(22E) li -0.4169(3) -0.6161(3) -0.5587(2) 0.08 H(IIB) 2/ 0.0112(2) -0.9598(2) -0.9262(1) 0.08 H(22F) li -0.3836(3) -0.5116(3) -0.5992(2) 0.08
Table 3. Final atomic coordinates and displacement parameters (in Л^)
Atom Site X г Un U22 t/33 Un Un Uli
0(1) li 0.4068(2) 0.5178(1) 0.8160(1) 0.0386(8) 0.0394(8) 0.063(1) 0.0089(7) 0.0011(7) 0.0233(7) C d ) li 0.4105(2) 0.4413(2) 0.8523(1) 0.0288(9) 0.0320(9) 0.037(1) 0.0043(8) 0.0038(8) 0.0046(8) 0(2) li 0.3008(1) 0.3991(1) 0.8774(1) 0.0265(7) 0.0506(9) 0.0536(9) 0.0027(6) 0.0070(6) 0.0158(7) C(3) li 0.3275(2) 0.3089(2) 0.9221(1) 0.034(1) 0.046(1) 0.049(1) -0.0020(9) 0.0111(9) 0.014(1) C(4) li 0.5147(2) 0.1554(2) 0.8770(1) 0.040(1) 0.034(1) 0.0329(9) -0.0008(8) -0.0001(8) 0.0166(8) C(5) li 0.4692(2) 0.0954(2) 0.7821(1) 0.041(1) 0.0294(9) 0.0340(9) -0.0063(8) -0.0010(8) 0.0120(7) C(6) li 0.5022(2) 0.1658(2) 0.7190(1) 0.0296(9) 0.0286(9) 0.0250(8) -0.0005(7) -0.0007(7) 0.0067(7) C(7) li 0.6845(2) 0.2797(2) 0.6668(1) 0.045(1) 0.050(1) 0.0287(9) -0.012(1) 0.0074(9) 0.0093(9) C(8) li 0.6593(3) 0.4184(2) 0.6924(1) 0.067(2) 0.048(1) 0.036(1) -0.007(1) 0.002(1) 0.0237(9) C(9) li 0.6720(2) 0.4632(2) 0.7891(1) 0.0263(9) 0.0317(9) 0.040(1) -0.0002(7) 0.0017(8) 0.0161(8) 0(9) li 0.7055(2) 0.5651(1) 0.8360(1) 0.0440(9) 0.0307(7) 0.0533(9) -0.0034(6) 0.0033(7) 0.0126(6) C(10) li 0.6441(2) 0.3526(2) 0.8236(1) 0.0228(8) 0.0258(8) 0.0234(8) -0.0004(7) -0.0003(6) 0.0081(6) C ( l l ) li 0.5297(2) 0.3880(2) 0.8849(1) 0.0251(9) 0.0281(9) 0.0247(8) -0.0009(7) 0.0020(7) 0.0052(7) C(I2) li 0.4764(2) 0.2894(2) 0.9224(1) 0.032(1) 0.040(1) 0.0259(8) -0.0026(8) 0.0045(8) 0.0105(7) C(13) li 0.6354(2) 0.2345(2) 0.7406(1) 0.0261(9) 0.0285(8) 0.0255(8) -0.0003(7) 0.0023(7) 0.0065(7) 0(14) li 0.4103(1) 0.2571(1) 0.71674(8) 0.0300(7) 0.0313(7) 0.0342(7) 0.0005(6) -0.0062(6) 0.0073(5) C(15) li 0.2822(2) 0.2097(2) 0.6816(1) 0.030(1) 0.052(1) 0.045(1) -0.0009(9) -0.0100(9) 0.014(1) C(16) li 0.2906(2) 0.1192(2) 0.5900(1) 0.043(1) 0.052(1) 0.041(1) -0.010(1) -0.016(1) 0.010(1) C(17) li 0.3888(2) 0.0223(2) 0.5968(1) 0.048(1) 0.039(1) 0.036(1) -0.012(1) -0.0089(9) 0.0040(8) 0(18) li 0.5122(1) 0.0785(1) 0.63431(8) 0.0398(8) 0.0329(7) 0.0271(6) -0.0032(6) -0.0023(6) -0.0001(5) C(19) li 0.7677(2) 0.3468(2) 0.8776(1) 0.0272(9) 0.0284(9) 0.0323(9) -0.0010(7) -0.0025(7) 0.0101(7) 0(19) li 0.7712(2) 0.3566(2) 0.95315(9) 0.0388(8) 0.080(1) 0.0320(7) 0.0019(8) -0.0086(6) 0.0193(7) 0(20) li 0.8720(1) 0.3338(1) 0.83007(9) 0.0222(6) 0.0489(8) 0.0460(8) 0.0018(6) 0.0002(6) 0.0221(7) C(20) li 0.9970(2) 0.3249(2) 0.8720(2) 0.023(1) 0.055(1) 0.072(2) 0.0006(9) -0.007(1) 0.025(1) C(21) li 0.3345(3) 0.1857(3) 0.5283(2) 0.074(2) 0.073(2) 0.045(1) -0.002(1) -0.018(1) 0.026(1) C(22) li 0.1559(3) 0.0556(3) 0.5601(2) 0.053(2) 0.083(2) 0.077(2) -0.019(2) -0.024(1) 0.008(2) 0(1A) li -0.1432(1) -1.0192(1) -0.80831(9) 0.0387(8) 0.0372(7) 0.0517(9) -0.0063(6) 0.0038(7) 0.0205(6) C d ) li -0.1440(2) -0.9450(2) -0.8472(1) 0.0268(9) 0.0293(9) 0.0326(9) -0.0031(7) 0.0001(7) 0.0051(7) 0(2) li -0.2568(1) -0.9050(1) -0.87253(9) 0.0250(7) 0.0477(8) 0.0461(8) -0.0030(6) -0.0031(6) 0.0158(7) C(3) li -0.2334(2) -0.8197(2) -0.9215(1) 0.033(1) 0.046(1) 0.050(1) -0.0012(9) -0.0125(9) 0.019(1) C(4) li -0.0386(2) -0.6637(2) -0.8790(1) 0.039(1) 0.0327(9) 0.0297(9) 0.0010(8) -0.0013(8) 0.0167(7) C(5) li -0.0706(2) -0.6005(2) -0.7846(1) 0.044(1) 0.0306(9) 0.0341(9) 0.0081(9) 0.0003(9) 0.0119(7) C(6) li -0.0295(2) -0.6678(2) -0.7196(1) 0.0285(9) 0.0265(8) 0.0232(8) 0.0018(7) 0.0009(7) 0.0052(6) C(7) li 0.1577(2) -0.7774(2) -0.6655(1) 0.046(1) 0.050(1) 0.0269(9) 0.012(1) -0.0068(9) 0.0087(8) C(8) li 0.1291(3) -0.9161(2) -0.6892(1) 0.065(2) 0.053(1) 0.037(1) 0.006(1) -0.003(1) 0.027(1) C(9) li 0.1290(2) -0.9637(2) -0.7856(1) 0.0272(9) 0.034(1) 0.039(1) 0.0010(8) -0.0005(8) 0.0177(8) 0(9) li 0.1560(2) -1.0654(1) -0.8311(1) 0.0458(9) 0.0300(7) 0.0559(9) 0.0070(6) 0.0013(7) 0.0143(6) C(10) li 0.0950(2) -0.8556(2) -0.8220(1) 0.0219(8) 0.0265(8) 0.0250(8) 0.0010(7) 0.0013(6) 0.0089(7) C ( l l ) li -0.0285(2) -0.8944(2) -0.8823(1) 0.0255(9) 0.0281(8) 0.0220(8) 0.0004(7) 0.0006(7) 0.0051(6) C(12) li -0.0853(2) -0.7985(2) -0.9222(1) 0.033(1) 0.036(1) 0.0235(8) -0.0001(8) -0.0037(7) 0.0099(7) C(13) li 0.0991(2) -0.7355(2) -0.7405(1) 0.0254(9) 0.0295(9) 0.0252(8) 0.0001(7) -0.0018(7) 0.0065(7) 0(14) li -0.1229(1) -0.7581(1) -0.71513(8) 0.0299(7) 0.0307(6) 0.0324(7) -0.0010(5) 0.0069(5) 0.0062(5) C(15) li -0.2456(2) -0.7103(2) -0.6809(1) 0.033(1) 0.049(1) 0.045(1) 0.0012(9) 0.0131(9) 0.0069(9) C(16) li -0.2240(2) -0.6167(2) -0.5903(1) 0.047(1) 0.050(1) 0.042(1) 0.007(1) 0.018(1) 0.005(1) C(17) li -0.1242(2) -0.5202(2) -0.5983(1) 0.051(1) 0.037(1) 0.039(1) 0.011(1) 0.011(1) 0.0026(9) 0(18) li -0.0072(1) -0.5775(1) -0.63567(8) 0.0392(8) 0.0306(7) 0.0277(6) 0.0018(6) 0.0015(6) -0.0005(5) C(19) li 0.2106(2) -0.8511(2) -0.8779(1) 0.0271(9) 0.0289(9) 0.0330(9) 0.0036(7) 0.0061(7) 0.0100(7)
С | 9 Н 2 б 0 7
301
Table 3. (Continued)
Atom Site X y Ζ и и U22 и,} Un Un U23.
0 ( I 9 ) 2/ 0.2045(2) -0.8681(2) -0.95425(9) 0.0449(9) 0.071(1) 0.0289(7) -0.0018(8) 0.0110(7) 0.0I20<7) 0 ( 2 0 ) 2i 0.3216(1) -0.8311(1) -0.82979(9) 0.0228(7) 0.0512(8) 0.0481(8) 0.0005(6) 0.0049(6) 0.0234(7) C(20) 2i 0.4403(2) -0.8216(2) -0.8721(2) 0.027(1) 0.054( I ) 0.078(2) 0.003( I ) 0.018(1) 0.030(1) C(2I) 2i -0.1718(3) -0.6816(3) -0.5269(2) 0.085(2) 0.069(2) 0.040(1) -0.002(2) 0.020(1) 0.018(1) C(22) Ii -0.3529(3) -0.5541(3) -0.5600(2) 0.062(2) 0.084(2) 0.087(2) 0.020(2) 0.037(2) 0.002(2)
References
Panitzsch. T.: Synthese von Tremulanen und Merulanen. Dissertation.
Universität Kiel. Germany 1997.
Sheldrick. G. M.: Program Package SHELXTL-plus. Release 4.1.
Siemens Analytical X-Ray Instruments Inc.. Madison ( WI53719), USA 1990.
