Rotational isomers of a 1,2-diphenyl-3,4-diphosphinidenecyclobutene

Chemistry Letters

Volumn , Issue 1, 1997, Pages 87-88

  Yoshifuji, Masaaki ^a   Ichikawa, Yoshito ^a   Toyota, Kozo ^a   Kasashima, Eiji ^b   Okamoto, Yoshio ^b  

^a TOHOKU UNIVERSITY   (Japan)

^b NAGOYA UNIVERSITY   (Japan)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 0031486905     PISSN: 03667022     EISSN: None     Source Type: Journal    
DOI: 10.1246/cl.1997.87     Document Type: Article

References (22)

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19. 13C NMR were diagnostic of the structure of the complexes and the major one was assigned to the anti-type which has two apical CO's and two equatorial CO's, whereas the minor one was assinged to the syn-type, which has two equatorial CO's and two apical non-equivalent CO's.
20. 3, P1 (#2), Z = 2, T = 296 K, R = 0.045, Rw = 0.043; 7430 unique reflections with I > 3σ(I). The structure was solved with SHELXS86; G. M. Sheldrick, SHELX86, Programs for the Automatic Solution of Crystal Structures, University of Göttingen, Germany (1986). Further details of the crystal structure investigation for syn-5C are available on request from the Director of the Cambridge Crystallographic Data Centre, 12 Union Road, GB-Cambridge CB2 1EZ (UK).
21. Some selected bond lengths (Å) and angles (°) of syn-SC: W-P(1), 2.515(2); W-P(2), 2.489(2); W-C(47), 1.955(9); W-C(48), 1.930(9); W-C(49), 1.986(8); W-C(50), 2.014(9); P(1)-C(1), 1.669(6); P(1)-C(5), 1.833(6); P(2)-C(2), 1.662(6); P(2)-C(20), 1.821(7); C(1)-C(2), 1.507(8); C(1)-C(4), 1.483(8); C(2)-C(3), 1.466(8); C(3)-C(4), 1.410(9); P(1)-W-P(2), 77.73(6); P(1)-W-C(47), 90.7(2); P(1)-W-C(48), 91.0(2); P(1)-W-C(49), 169.9(2); P(1)-W-C(50), 99.4(2); P(2)-W-C(47), 90.2(2); P(2)-W-C(48), 94.5(3); P(2)-W-C(49), 92.2(2); P(2)-W-C(50), 173.5(3); C(47)-W-C(48), 175.2(4); C(47)-W-C(49), 89.9(3); C(47)-W-C(50), 83.9(4); C(48)-W-C(49), 89.2(3); C(48)-W-C(50), 91.4(4); C(49)-W-C(50), 90.6(3); W-P(1)-C(1), 111.5(2); W-P(1)-C(5), 137.7(2); C(1)-P(1)-C(5), 110.1(3); W-P(2)-C(2), 112.1(2); W-P(2)-C(20), 135.6(2); C(2)-P(2)-C(20), 111.8(3); P(1)-C(1)-C(2), 118.9(4); P(1)-C(1)-C(4), 153.2(5); C(2)-C(1)-C(4), 87.8(5); P(2)-C(2)-C(1), 119.7(5); P(2)-C(2)-C(3), 151.9(5); C(1)-C(2)-C(3), 88.4(5); C(2)-C(3)-C(4), 92.3(5); C(2)-C(3)-C(35), 130.0(6); C(4)-C(3)-C(35), 137.2(6); C(1)-C(4)-C(3), 91.5(5); C(1)-C(4)-C(41), 132.8(6); C(3)-C(4)-C(41), 135.7(6); P(1)-C(5)-C(6), 113.4(5); P(1)-C(5)-C(10), 126.2(5).
22. Column: Chiralcel OD 25 x 0.46 (i.d.) cm (Daicel); eluent: hexane; flow speed: 0.5 ml/min; tempearture: RT. anti-5C was dissolved in a mixture of hexane-isopropyl alcohol (9:1) in 0.1 mg/mL. First peak appeared at 10.4 min and the second one at 11.6 min.