The new non‐centrosymmetric tin fluoride borate Sn3[B3O7]F was synthesized hydrothermally, and was characterized by single‐crystal and powder X‐ray diffraction, vibrational spectroscopy, DFT calculations, second harmonic generation (SHG) measurements, thermogravimetry, and differential scanning calorimetry. Its SHG response is about 12 times that of quartz. The compound crystallizes in the non‐centrosymmetric orthorhombic space group Pna21 with lattice parameters a=922.4(2), b=769.8(4), and c=1221.9(6) pm (Z=4). Characteristic for the structure are isolated B3O7 moieties, consisting of two corner‐sharing BO3 units and one BO4 tetrahedron. These occupy half of the octahedral voids of a slightly distorted hexagonal closest packing of Sn2+ atoms, with [SnF]+ units in the other half of the octahedral voids. Sn3[B3O7]F is transparent over a wide spectral range with a UV cut‐off edge at about 263 nm.

The first lead(II) borosulfate Pb[B2(SO4)4] was synthesized under harsh conditions via a solvothermal reaction of PbO2 with H3BO3 and oleum (20 % SO3). The compound crystallizes in the orthorhombic space group Pnna (no. 52) with the lattice parameters a = 1251.6(7), b = 1252.1(7), and c = 730.2(4) pm (Z = 4). The structure of Pb[B2(SO4)4] is constructed of one‐dimensional infinite anionic chains according to 1∞[B(SO4)4/2]– and charge compensated by Pb2+ cations, which are coordinated to the chain terminating oxygen atoms of the (SO4) tetrahedra. The lone pair of electrons of the Pb2+ cations is sterically not active. Pb[B2(SO4)4] was characterized by means of single‐crystal and powder X‐ray diffraction, as well as vibrational spectroscopy.

The tin iodide borate Sn3[B3O7]I was synthesized via a hydrothermal synthesis and crystallizes in the centrosymmetric space group Pbca (no. 61) possessing lattice parameters of a = 1071.8(3), b = 852.3(2), and c = 2016.8(5) pm and Z = 8. Characteristic for the structure are infinite chains along the b axis, built up of three membered B3O8 rings consisting of one BO3 unit and two corner-sharing BO4 tetrahedra. The three tin cations are oriented differently: one cation is located layer-like between the infinite chains, and the other two cations show an orientation in a row with the infinite chain. In this structure, only one of the three tin cations exhibits a coordination to the halogen anion. The new centrosymmetric tin iodide borate Sn3[B3O7]I was investigated by single-crystal diffraction, vibrational spectroscopy, powder X-ray diffraction data, thermogravimetry, differential scanning calorimetry, and DFT calculations.

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A new centrosymmetric modification of the lead borate (Pb4O)Pb2B6O14 has been obtained as a side phase through a facile hydrothermal reaction from Pb(BO2)2·H2O, H2O, and KOH as starting materials. The compound (Pb4O)Pb2B6O14-II crystallizes in the space group P1̅ (no. 2) with the lattice parameters a=695.9(3), b=778.0(3), c=1408.3(3) pm, α=97.35(1)°, β=100.39(1)°, and γ=103.02(1)°. The structure consists of anti-parallel arranged B6O14 chains and isolated oxygen-centered OPb4 tetrahedra. The compound Pb6B12O21(OH)6 constitutes the major phase of the synthesis, as verified through a Rietveld analysis. The characterization of (Pb4O)Pb2B6O14-II is based on a Rietveld analysis, single-crystal X-ray diffraction data, and FT-IR spectroscopy.