A new material platform for boron nitride (BN) as a heterogeneous photocatalyst for solar fuels synthesis has recently emerged. One of the bottlenecks of this material is the lack of photoactivity under visible light, which hinders its rate performance. Theoretical studies have predicted that tuning the oxygen content in oxygen-doped BN (BNO) might be used to lower and vary the band gap. However, this is yet to be verified experimentally. We present herein a systematic experimental route facilitating simultaneous tuning of the chemical, magnetic and optoelectronic properties of BNO using a multivariate synthesis parameter space. Deep visible range band gaps (1.50 – 2.90 eV) were experimentally achieved and tuned over an oxygen composition of 2 – 14 at. %, and specific paramagnetic OB3 content of 7 – 294 a.u. g-1, thus supporting theoretical predictions. Through designing a response surface via a design of experiments (DOE) process, the key synthesis parameters influencing the chemical, magnetic and optoelectronic properties of BNO were identified. In addition, model prediction equations relating the aforementioned properties to the synthesis parameter space are presented. Accurate model predictions for the oxygen content and band gap were conducted and validated experimentally. Such a methodology is valuable for further advances in tailoring and optimising BN materials for heterogeneous photocatalytic reactions.