Producing high efficiency solar cells without high‐temperature processing or use of additives still remains a challenge with the two‐step process. Here, the solution processing of MAPbI
3 from PbI
2 films in
N,
N‐dimethylformamide (DMF) is investigated. In‐situ grazing incidence wide‐angle X‐ray scattering (GIWAXS) measurements reveal a sol–gel process involving three PbI
2‐DMF solvate complexes—disordered (P
0) and ordered (P
1, P
2)—prior to PbI
2 formation. When the appropriate solvated state of PbI
2 is exposed to MAI (methylammonium Iodide), it can lead to rapid and complete room temperature conversion into MAPbI
3 with higher quality films and improved solar cell performance. Complementary in‐situ optical reflectance, absorbance, and quartz crystal microbalance with dissipation (QCM‐D) measurements show that dry PbI
2 can take up only one third of the MAI taken up by the solvated‐crystalline P
2 phase of PbI
2, requiring additional annealing and yet still underperforming. The perovskite solar cells fabricated from the ordered P
2 precursor show higher power conversion efficiency (PCE) and reproducibility than devices fabricated from other cases. The average PCE of the solar cells is greatly improved from 13.2(±0.53)% (from annealed PbI
2) to 15.7(±0.35)% (from P
2) reaching up to 16.2%. This work demonstrates the importance of controlling the solvation of PbI
2 as an effective strategy for the growth of high‐quality perovskite films and their application in high efficiency and reproducible solar cells.
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