Crystal structure of 1',2',3',4'-tetrahydronaphthaleno[1',2'e]-3,3-dimethyl-1,2,4-trioxine, C₁₃H₁₆O₃

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Reference

Crystal structure of

1',2',3',4'-tetrahydronaphthaleno[1',2'e]-3,3-dimethyl-1,2,4-trioxine, C ₁₃ H ₁₆ O ₃

BERNARDINELLI, Gérald Hugues, et al .

BERNARDINELLI, Gérald Hugues, et al . Crystal structure of

1',2',3',4'-tetrahydronaphthaleno[1',2'e]-3,3-dimethyl-1,2,4-trioxine, C ₁₃ H ₁₆ O ₃ . Zeitschrift für Kristallographie , 1993, vol. 203, no. 1-2, p. 126-128

DOI : 10.1524/zkri.1993.203.12.126

Available at:

http://archive-ouverte.unige.ch/unige:151909

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Zeitschrift für Kristallographie 203, 126-128 (1993)

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

Crystal structure of l'^'^'^'-tetraliyclro- naphthalenoll^2'el03^imethyl-l,2,4-trioxine, C ^{1 3} H | ⁶ 0 ³

G. Bernardinelli

Laboratoire de Cristallographie, 24 quai Ernest-Ansermet, CH-1211 Geneva, Switzerland

and

C. W. JefTord, T. Hatsui and M. F. Deheza

Departement de Chimie Organique, 30 quai Ernest-Ansermet, CH-1211 Geneva 4, Switzerland (Received February 14, 1992)

Source of material : see réf. 1.

Monoclinic, P12,/cl (no 14), a = 8.926(1), b = 10.040(2), c = 13.793(4) Â, β =

106.740(9)°, V = 1183.7 Â

, Ζ = 4, R = 0.075.

1 '2'3'4'tetrahydronaphthaleno[l '2']-3.3-dimethyl-l ,2,4-trioxine

127

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

D i f f r a c t o m e t e r N u m b e r o f unique

type: Philips P W 1 1 0 0 reflections: 1105

W a v e length : M o K , radiation Criterion for u n o b -

( 0 . 7 1 0 7 A ) served reflections: F„ < 4<r(F0) Crystal c o l o u r l e s s prism, size N u m b e r o f refined

characteristics: 0 . 0 8 x 0 . 1 8 x 0 . 1 8 m m parameters: 145

T e m p e r a t u r e o f Scan m o d e : <u-2é?scan

m e a s u r e m e n t : 2 9 3 Κ μ: 0.81 c m1

2 < W 4 0e Structure solution M u l t a n 87

p r o g r a m used : X T A L 3 . 0

Table 2. Final a t o m i c c o o r d i n a t e s a n d displacement parameters (in Â2)

Atom X y ζ υ«Λ>,, ^u22 u „ u1 2 u2 1

O(l) 0.438(1) 0.864(1) 0.0895(7) 0.052(8) 0.054(8) 0.071(8) -0.015(7) 0.007(6) 0.004(7) 0(2) 0.476(1) 0.722(1) 0.0787(9) 0.043(7) 0.08(1) 0.12(1) 0.005(8) 0.034(7) 0.018(9) 0(3) 0.176(1) 0.811(1) 0.0627(7) 0.051(8) 0.045(7) 0.082(8) -0.013(7) 0.015(6) 0.008(7) CO) 0.284(2) 0.886(2) 0.026(1) 0.04(1) 0.04(1) 0.08(1) -0.01(1) 0.01(1) -0.01(1) C(2) 0.379(2) 0.647(2) 0.126(1) 0.04(1) 0.07(1) 0.06(1) -0.01(1) 0.016(9) 0.01(1) CO) 0.208(2) 0.671(2) 0.065(1) 0.06(1) 0.05(1) 0.04(1) -0.01(1) 0.025(9) 0.010(9) C(4) 0.101(2) 0.599(2) 0.113(1) 0.06(1) 0.03(1) 0.028(9) 0.013(9) 0.011(9) -0.002(9) C(5) -0.041(2) 0.652(1) 0.114(1) 0.06(1) 0.04(1) 0.07(1) 0.00(1) 0.03(1) -0.01(1) C(6) -0.136(2) 0.582(2) 0.160(1) 0.05(1) 0.07(1) 0.06(1) -0.01(1) 0.02(1) -0.01(1) C(7) -0.088(2) 0.461(2) 0.208(1) 0.09(2) 0.06(1) 0.06(1) -0.02(1) 0.03(1) 0.02(1) C(8) 0.052(3) 0.406(2) 0.204(1) 0.11(2) 0.06(1) 0.05(1) -0.03(1) 0.01(1) -0.00(1) C(9) 0.149(2) 0.478(2) 0.159(1) 0.06(1) 0.04(1) 0.03(1) -0.01(1) -0.01(1) -0.009(9) C(10) 0.308(2) 0.418(2) 0.164(1) 0.09(2) 0.05(1) 0.07(1) 0.00(1) 0.00(1) 0.00(1) C(ii) 0.412(2) 0.501(2) 0.121(2) 0.08(1) 0.05(1) 0.15(2) 0.03(1) 0.05(1) 0.01(1) C(12) 0.258(2) 1.031(2) 0.049(1) 0.08(1) 0.06(1) 0.12(2) 0.00(1) 0.03(1) 0.03(1) C(13) 0.271(2) 0.860(2) -0.084(1) 0.10(2) 0.11(2) 0.06(1) -0.05(1) 0.03(1) 0.02(1)

fl(2) 0.4005 0.6788 0.205 0.05066

H<3) 0.1889 0.6329 -0.0118 0.05066 H(5) -0.0772 0.7481 0.0796 0.05066

H(6) -0.2501 0.6238 0.159 0.05066

H(7) -0.1611 0.4106 0.248 0.05066

H(8) 0.0875 0.3079 0.2371 0.05066

H(I0I) 0.3692 0.3992 0.2429 0.05066 H(102) 0.2873 0.324 0.1223 0.05066 H(111) 0.5334 0.4823 0.1624 0.05066 H(t 12) 0.393 0.4744 0.0411 0.05066 H( 121 ) 0.3461 1.0909 0.0275 0.05066 H(122) 0.1422 1.0601 0.0031 0.05066 H(123) 0.2683 1.0498 0.1279 0.05066 H(131) 0.1545 0.8895 -0.1288 0.05066 H(132) 0.3584 0.9203 -0.1044 0.05066 H(133) 0.2894 0.7561 -0.0997 0.05066

Further details o f the structure determination (e.g. structure factors) h a v e b e e n deposited within the relevant d a t a b a s e and c a n be accessed as C o l l e c t i o n N o . 3 2 0 4 0 2 or ordered f r o m the F a c h i n f o r m a t i o n s z e n t r u m Karlsruhe, D - 7 5 1 4 E g g e n s t e i n - L e o p o l d s h a f e n .

128 G. Bernardinelli, C. W. Jefford, T. Hatsui and M. F. Deheza

References:

1. JefTord, C.W., Hatsui, T., Ferrufino Deheza, M., Bernardinelli, G.: Photo-oxygenation of Indene and 1,2-Dihydronaphtalene. Formation of 1,2-Dioxetanes and 1,2,4-Trioxanes.

Chimia 46 (1992) 114-118.