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Simultaneous measurements of Raman spectroscopy and synchrotron two-dimensional (2D) wide-angle x-ray diffraction (WAXD) have been successfully demonstrated for in situ study of an anisotropic system: isotactic polypropylene (iPP) fiber under tensile deformation. A fiber-optic probe was used to remotely deliver the incident laser beam on the sample as well as to collect the Raman signal based on the confocal arrangement, whereas high resolution 2D WAXD patterns were obtained simultaneously at the same position during deformation of polymers. The combined techniques yielded complementary information on the molecular structural evolution in both crystalline and amorphous phases. 2D WAXD results showed that the α-form iPP crystals were converted into the mesophase upon stretching at room temperature. Corresponding Raman spectra showed that characteristic bands from the crystal phase became weaker or disappeared during the transition from the crystal phase to the mesophase. However, the bands associated with the helical structure were still present, indicating the remainder of the helical conformation in the mesomorphic phase. The persistence of the Raman band at 812 cm[sup -1] in the mesophase implied that the structural difference between the crystal phase and the mesophase in iPP is due to the packing defects, rather than the conformational deviations from the (...TGTG...) sequence in chains. The variations in the Raman intensity ratio (I812/I843) indicated that the overall orientation of the fiber increased during stretching. The demonstrated techniques will be particularly useful for in situ studies of anisotropic polymers, where orientational dependent structural information from both crystalline and amorphous phases needs to be collected simultaneously. © 2003 American Institute of Physics. [ABSTRACT FROM AUTHOR]