An over-the-air (OTA) experimental evaluation of concurrent 5G New Radio (5G NR) and Wi-Fi transmission using successive interference cancellation (SIC) in a shielded-box environment is presented. A USRP is used as the receiver, which captures the composite waveform containing both air-interface signals and applies sample-domain SIC to suppress the dominant 5G-NR signal and recover Wi-Fi signal from the residual waveform. The framework reports error vector magnitude (EVM), bit error rate (BER), sample-domain cancellation depth, and channel-estimate suppression, and, at the representative \(18\) dB attenuation point, measures \(11.88\) dB cancellation depth and \(26.96\) dB 5G channel suppression. The proposed methodology provides a practical basis for assessing cross-technology coexistence and receiver-side interference suppression under controlled OTA conditions.