Carbon-bearing boron hydrides, also known as carboranes, are polyhedral clusters composed of hydrogen, boron, and carbon and are closely related to boranes. Because of their esthetically pleasing symmetry as well as unusual chemical properties, carboranes have attracted immense interest. Studies over the past 40 years have revealed them to have chemical features that make them useful in a number of specialized applications such as conducting organic polymers, nuclear waste remediation, and as liquid crystalline materials. It has also been shown that carboranes can be used as boron delivery agents for boron neutron capture therapy against cancer. While a number of strides have been made in synthesizing these molecules, their characterization by NMR spectroscopy is challenging due to boron–boron and boron–hydrogen coupling. This gives rise to broad and unresolved peaks and makes peak assignment difficult and often based on best guesses. NMR structural characterization studies of carborane compounds are sparse, dated, and often performed at low resolution. This report provides a detailed structural characterization of an m-carborane derivative, featuring high-resolution multi-dimensional NMR spectroscopy (2-D 1H–1H, 2-D 11B–11B, 2-D 11B–1H, and 2-D 13C–1H). The asymmetry of the carborane cluster (a consequence of substitution at one of the two cluster carbons) adds a dimension of complexity to the spectra, whose peaks could be assigned nevertheless due to their high resolution.