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The structure of zeolite ZSM-23 (structure-type code MTT) loaded with NH4F [ao = 11.129 (1), bo = 5.025 (1) and Co = 21.519 (1) Å and β = 89.85 (4)°] was refined from high-resolution synchrotron X-ray powder data. The Rietveld refinement converged in space group P1211 (No. 4) to RF = 0.090 and Rwp = 0.085, confirming the proposed model of the silicate framework. The use of complementary methods (synchrotron X-ray powder diffraction, 29Si magic angle-spinning nuclear-magnetic-resonance spectroscopy, and distance and angle least-squares refinements) was essential for the determination of the true space-group symmetry, a prerequisite for the successful Rietveld structure refinement.