A composition space diagram is used to establish the stability regions of hybrid fluoroaluminates synthesized by solvothermal reactions in the Al(OH)(3)-HguaCl-HF(aq)-EtOH system. The syntheses are conducted using microwave heating at 190 degrees C for 1 h. The structures of two new guanidinium fluoroaluminates, (H(3)O)(2) x [Hgua](16) x (Al(4)F(18))(3) x H(2)O and [Hgua](2) x (Al(5)F(17)), are reported. (H(3)O)(2) x [Hgua](16) x (Al(4)F(18))(3) x H(2)O, determined from single-crystal X-ray data, consists of discrete (Al(4)F(18))(6-) polyanions, while [Hgua](2) x (Al(5)F(17)), solved from powder X-ray diffraction data in direct space, contains unprecedented Al(5)F(17) layers constructed from the intergrowth of HTB and perovskite columns. A disorder of H(2)O and H(3)O(+) is evidenced in (H(3)O)(2) x [Hgua](16) x (Al(4)F(18))(3) x H(2)O together with a disorder of guanidinium cations in the interlayer space of [Hgua](2) x (Al(5)F(17)).
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