Multidimensional solid-state nuclear magnetic resonance (NMR) under magic-angle spinning (MAS) conditions has been developed to determine the dihedral angle for a H-1(alpha)-C-13(alpha)-C-13(beta)-H-1(beta) moiety in powdered states. The pulse sequence for this experiment includes (CH)-C-13-H-1 dipolar evolution periods for C-alpha and C-beta, which are correlated through a coherent (CCbeta)-C-13-C-alpha 13 dipolar mixing period. Theoretical analysis based on the symmetry of the spin system indicates that the dipolar correlation spectrum only due to the (CHalpha)-H-alpha and (CHbeta)-H-beta dipolar couplings is strongly dependent on the dihedral angle chi about the (CCbeta)-C-alpha bond axis, but two chi angles give the same spectrum in the chi range from 0 degrees to about 140 degrees, where chi=0 degrees corresponds to the cis conformation. Inclusion of the (CCbeta)-C-alpha dipolar coupling together with the weak (CHbeta)-H-alpha and (CHalpha)-H-beta dipolar couplings, however, breaks the symmetry of the system with respect to chi in the range from 0 degrees to 180 degrees. These properties are confirmed by the spectra calculated for the pulse sequence as a function of chi and the root-mean-square deviation between them. The bond lengths, bond angles, and dihedral angle also alter the dipolar correlation spectrum differently. This enables us the experimental determination of all the structural parameters, which improves the accuracy of the dihedral angle determination. The high resolution due to C-13 isotropic chemical shifts under MAS conditions in this multidimensional NMR permits its application to molecules having a number of C-13-labeled sites. Experimental results are presented for powdered L-valine uniformly labeled with C-13 and N-15 nuclei. Effects of the structural parameters and noise on the dihedral angle determination are evaluated numerically. The accuracies of the determined structural parameters are discussed,