Bicyclo[2.1.1]hex-2-ene
Anthony Linares

Summary
Interested in understanding the chemical and physical properties of the rigid, strained hydrocarbon, Bicyclo[2.1.1]hex-2-ene, Zebelman and Bauer analyzed the structure via electron diffraction1. The theoretical and reduced experimental intensity curves and the final radial distribution curve (RDC) provide information regarding the proposed interatomic distances. The group assumed C2v symmetry to calculate the geometrical parameters, which were refined using a least squares analysis of the reduced intensities. The C-H bond lengths were not varied during the analysis; instead, they were estimated from the final RDC. For the limited data concerning bond angles, there are error limits as large as 3.8°, indicative of the restrictions of the experimental technique.
Concerned that the least-squares analysis of the electron diffraction study of Bicyclo[2.1.1]hex-2-ene converged to a false structure, Wang and Harmony observed four isotopic species of the molecule using microwave spectroscopy2. Implementing Costain and Kraitchman’s equations, an rs structure for the carbon skeleton was obtained. The rotational constants were determined using the rigid rotor approximation, which models rigid polycyclic molecules fairly well (Table 2). Wang and Harmony note the exclusion of vibrational-rotational interactions. These interactions are expected to exceed the pure experimental errors. When comparing the MW structure with the ED structure, Wang and Harmony found that the <C1 C2 C3 angle, the dihedral angle θ, and the nonbonded C5… C6 from the ED study differ significantly from the experimental MW uncertainties (Table 1). They propose that the radial distribution function and ED data are “incapable of an unambiguous resolution of the molecular structure.”
An energy calculation using the Merck Molecular Force Field (MMFF94) was conducted to test the reliability of the MW and ED structures. The MW structure was found to be more energetically stable (62.10110 kcal/mol) when compared with the ED structure (98.01748 kcal/mol).
References
1. D. L. Zebelman and S. H. Bauer, “Structures of Strained Polycyclics: Bond Ditances and Angles in Tricyclo[3.3.0.02,6]Oct-3ene and in Bicyclo[2.1.1]hex-2-ene”, Tetrahedron., 28, 2727-2740 (1972).
2. C.S. Wang and M. D. Harmony, “Microwave Spectrum, Structure, and Dipole Moment of [2.1.1]hex-2-ene”, J. of A.C.S., 98, 1108-1111 (1976).
Comparison of structures generated by various means
- Microwave structure of Wang and Harmony
They derived C2v symmetry from the relative intensities (application of the Pauli Exclusion Principle)and ignored vibrational-rotational interactions. Rs structure only provided for carbon skelton, thus, locations of hydrogens were based on angles determined from ED study and optimal geometry.
- Electron diffraction structure of Zebelman and Bauer
They assumed C2v symmetry and C-H bond lengths. Error limits for bond lengths and bond angles are larger than that of the MW experiment. The bond angles, dihedral angle θ, and the nonbonded C5… C6 from the ED stucture differ significantly from MW study.
- Structure using molecular mechanics with MMFF94 force field
C1-C2 and C1-C5 bond distances differ from the MW and ED structures by ~0.02 -0.03 A each. The bond angles are within reasonable agreement of the MW results. In a striking reversal, the MMFF yields poorer results for the bond angles than the Class I Tripos force field.
- Structure using molecular mechanics with Tripos force field
The calculations underestimate the C1-C2 and C1-C5 bond distances of both the MW and ED structure. Bond angles support MW structure.
- Structure from semi-empirical quantum mechanics and the AM1 Hamiltonian
C-C single and double bonds are over estimated by ~0.01-0.02 A each. The bond angles are in good agreement with the MW values.
- Structure from ab initio quantum mechanics, Hartree-Fock with 3-21G basis set
C-C single bond are over estimated and the C=C double bond is underestimated. Interestingly, this calculation has the best agreement for the bond angles and dihedral angle when compared with the MW study.
Table 1: Tabular Results of Structural Parameters from Various Methods
|
|
MW |
ED |
MMFF94 |
Tripos |
SE-AM1 |
HF 3-21G |
|
Distance(C1,C2) |
1.52782568 |
1.53699369 |
1.49440642 |
1.50534657 |
1.53555031 |
1.54668891 |
|
Distance(C1,C5) |
1.56796073 |
1.56445573 |
1.58864177 |
1.54960672 |
1.58010668 |
1.58005994 |
|
Distance(C2,C3) |
1.3408 |
1.332 |
1.34145985 |
1.33430659 |
1.36158205 |
1.32312253 |
|
Distance(C5...C6) |
2.14885159 |
1.826 |
2.09070449 |
2.15916627 |
2.15279861 |
2.14885159 |
|
Angle(C1,C2,C3) |
103.324052 |
108.401943 |
102.937673 |
102.964144 |
103.522341 |
103.890905 |
|
Angle(C5,C1,C2) |
100.391372 |
95.3700153 |
104.837462 |
98.8301495 |
99.0887022 |
99.5236835 |
|
Angle(C5,C1,C6) |
85.3276533 |
71.4068206 |
82.2975258 |
88.3228097 |
85.8780093 |
85.6858065 |
|
Angle(C1,C5,C4) |
81.4034049 |
94.7576652 |
78.5160143 |
80.851829 |
82.3075671 |
81.6418963 |
|
Dihedral(C6,C1,C4,C5) |
126.740563 |
119.046425 |
116.383388 |
132.464747 |
129.576234 |
127.93877 |
Table 2:
Rotational Constants and Moment of Inertia in MHz (Wang and Harmony)