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NaZn(H2O)2[BP2O8] · H2O: A Novel Open-Framework Borophosphate and its Reversible Dehydration to Microporous Sodium Zincoborophosphate Na[ZnBP2O8] · H2O with CZP-Topology

Crystals of NaZn(H2O)2[BP2O8].H2O were grown under mild hydrothermal conditions at 170 degrees C. The crystal structure (solved by X-ray single-crystal methods: hexagonal, P6(1)22 (no. 178), a = 946.2(2), c= 1583.5(1) pm, V= 1227.8(4).10(6) pm3, Z = 6) exhibits a chiral octahedral-tetrahedral framework related to the CZP topology and contains helical ribbons of corner-linked borate and phosphate tetrahedra. Investigation of the thermal behavior up to 180 degrees C shows a (reversible) dehydration process; this leads to the microporous compound Na[ZnBP2O8].H2O, which has the CZP topology. The crystal structure of Na[ZnBP2O8].H2O was determined by X-ray powder diffraction by using a combination of simulated annealing, lattice-energy minimization, and Rietveld refinement procedures (hexagonal, P6(1)22 (no. 178), a = 954.04(2), c = 1477.80(3) pm, V= 164.88(5).10(6) pm3, Z = 6). The essential structural difference caused by the dehydration concerns the coordination of Zn2- changing from octahedral to tetrahedral arrangement.

RbFe[BP2O8(OH)]: ein neues Borophosphat mit offen-verzweigten Vierer-Einfach-Tetraederketten

RbFe[BP2O8(OH)] bildet sich unter milden hydrothermalen Bedingungen (T = 165–170 °C) aus einer Mischung von RbOH(aq), FeCl2 · 4 H2O, H3BO3 und H3PO4. Die Kristallstruktur der im monoklinen System kristallisierenden Verbindung (Raumgruppe P21/c, Nr. 14) wurde mit Rontgen-Einkristallmethoden bestimmt: a = 935,8(5) pm, b = 833,9(6) pm, c = 965,6(5) pm; β = 101,69(4)°; Z = 4. Der Anionenteilverband besteht aus offen-verzweigten Vierer-Einfach-Ketten [BP2O8(OH)]4–, die durch alternierende Eckenverknupfung von Borat- und Phosphat-Tetraedern gebildet werden. Fe3+ ist oktaedrisch (FeO5(OH)) koordiniert, wahrend Rb+ unregelmasig von zehn Sauerstoff-Funktionen benachbarter Tetraeder umgeben ist. RbFe[BP2O8(OH)]: A New Borophosphate Containing Open-Branched Tetrahedral Vierer-Einfach Chains RbFe[BP2O8(OH)] is formed under mild hydrothermal conditions (T = 165–170 °C) from a mixture of RbOH(aq), FeCl2 · 4 H2O, H3BO3 and H3PO4. The crystal structure of the monoclinic compound was solved by x-ray single crystal methods (space group P21/c, No. 14): a = 935.8(5) pm, b = 833.9(6) pm, c = 965.6(5) pm; β = 101.69(4)°; Z = 4. The anionic partial structure contains open-branched vierer-einfach chains [BP2O8(OH)]4–, which are formed by alternating borate and phosphate tetrahedra sharing common corners. Fe3+ is in an octahedral coordination (FeO5(OH)), while Rb+ is irregularly coordinated by ten oxygen-functions of neighbouring tetrahedra.

(Ni3-xMgx)[B3P3O12(OH)6] · 6 H2O (x ≈ 1.5): A Novel BorophosphateHydrate Containing Isolated Six-Membered Rings of Tetrahedra

A novel borophosphate-hydrate, (Ni3–xMgx)[B3P3O12(OH)6] · 6 H2O (x ≈ 1.5), has been prepared by hydrothermal synthesis (T = 170 °C) from a mixture of NiCl2 · 6 H2O, Mg(OH)2, B2O3 and H3PO4. The crystal structure was determined at 293 K from single-crystal X-ray diffraction data (trigonal, R3c (no. 167), a = 14.957(10) A, c = 13.812(6) A, V = 2676(2) A3, Z = 6, R1 = 0.0276, wR2 = 0.0714 for 779 observed reflections with I > 2σ(I)). The crystal structure contains unbranched six-membered rings [B3P3O12(OH)6]6– of alternating corner linked borate and phosphate tetrahedra, which are stacked along [001] and connected via MIIO2(OH)2(H2O)2 coordination polyhedra. Hydrogen bonding between the tetrahedral six-membered rings and MIIO2(OH)2(H2O)2 octahedra leads to a further cross-linking. With respect to the arrangement of isolated six-membered tetrahedral rings the crystal structure of this borophosphate-hydrate is closely related to the cyclo-hexasilicate dioptase, Cu6[Si6O18] · 6 H2O. (Ni3–xMgx)[B3P3O12(OH)6] · 6 H2O (x ≈ 1.5): Ein neues Borophosphat-Hydrat mit isolierten Tetraeder-Sechserringen Ein neues Borophosphat-Hydrat, (Ni3-xMgx)[B3P3O12(OH)6] · 6 H2O (x ≈ 1.5), wurde unter milden hydrothermalen Bedingungen (T = 170 °C) aus einer Mischung von NiCl2 · 6 H2O, Mg(OH)2, B2O3 und H3PO4 dargestellt. Die Kristallstruktur wurde bei T = 293 K mit Rontgen-Einkristallmethoden bestimmt (trigonal, R3c (Nr. 167), a = 14.957(10) A, c = 13.812(6) A, V = 2676(2) A3, Z = 6, R1 = 0.0276, wR2 = 0.0714 fur 779 beobachtete Reflexe mit I > 2σ(I)). Die Kristallstruktur wird von isolierten sechsgliedrigen [B3P3O12(OH)6]6–-Ringen aus alternierend eckenverknupften Borat- und Phosphat-Tetraedern aufgebaut, die entlang [001] gestapelt sind und uber MIIO2(OH)2(H2O)2-Koordinations-Polyeder verknupft werden. Zusatzliche Verknupfungen ergeben sich durch Wasserstoffbruckenbindungen zwischen den sechsgliedrigen Tetraederringen und den MIIO2(OH)2(H2O)2-Oktaedern. Die Kristallstruktur des Borophosphats ist bezuglich der Anordnung der sechsgliedrigen Ringe aus eckenverknupften Tetraedern eng verwandt mit dem cyclo-Hexasilicat Dioptas, Cu6[Si6O18] · 6 H2O.

K[B6PO10(OH)4]: Ein Borophosphat mit gestreckten Bändern aus Tetraeder-Vierer-Ringen und offen-zyklischen Verzweigungen über planare B2O3(OH)2-Gruppen / K[B6PO10(OH)4]: A Borophosphate Containing Rods of Tetrahedral Vierer-Rings with Additional Open-Loop Branchings via Planar B2O3(OH)2 Groups

K[B6PO10(OH)4] was prepared under mild hydrothermal conditions (T = 170 °C) from a concentrated solution of K2B4O 7 ∙ 4H2O , KH2PO4, and HCl (18%). The crystal structure of the tetragonal compound was solved by X-ray single crystal methods (space group P 4/ncc, No 130): a = 1209.66(13), c = 759.05(7) pm; Z = 4. The anionic partial structure consists of infinite rods of ∞1[B6PO10(OH)4]− which are built of vierer-rings of alternating BO4 and PO4 tetrahedra with additional open-loop branchings via planar B2O3(OH )2 groups at the BO4 units by sharing common oxygen functions. Potassium (K+) is located within structural channels running along [001]; the eightfold coordination by oxygen (OH-groups) results in a (slightly) distorted tetragonal antiprism.

Oligomere Tetraeder-Anionen in Borophosphaten: Sechserringe mit offenen und cyclischen Phosphat-Verzweigungen in der Kristallstruktur von K6Cu2[B4P8O28(OH)6] / Oligomeric Tetrahedral Anions in Borophosphates: Six-Membered Rings with Open and Cyclic Phosphate Branchings in the Crystal Structure of K6Cu2[B4P8O28(OH)6]

Abstract Crystals of K6Cu2[B4PhO28(OH)6] were grown under hydrothermal conditions at 160 °C. The crystal structure (monochnic, P21/c (Nr. 14), a = 961.8(1), b = 1755.0(1), c = 942.0(1) pm, β = 112.29(1)°, Z = 2) contains oligomeric tetrahedral anions based on six-membered rings {B4P2O10O8/2} with additional branchings by hydrogenphosphate-groups (open branching: 4 x HPO3O1/2; cyclic branching: 2 x HPO2O2/2). The complex borophosphate anion is represented by the formula [B4P8O28(OH)6]10-. Cu2+ is in a tetragonal pyramidal and K+ in an irregular coordination by eight and nine oxygen ligands, respectively.

Fe[B2P2O7(OH)5]: Ein neues Boro-phosphat mit unverzweigten Vierer-Einfach Tetraederketten / Fe[B2P2O7(OH)5]: A New Borophosphate Containing Non-Branched Tetrahedral Vierer-Einfach Chains

Abstract Single crystals of Fe[B2P2O7(OH)5] were grown under hydrothermal conditions at 170 °C. The crystal structure (monoclinic, C 2/c (Nr. 15), a = 1774.7(5), b = 672.0(2), c = 705.9(2) pm, β = 109.01(2)°, Z = 4, Dx= 2.808 g/cm3) contains vierereinfach tetrahedral chains 1∞[B2P2O7(OH)5]3-, which are formed by alternating borate and phosphate groups connected via common corners: 1∞[BO2/2(OH)(OH0.5)-PO2/2O(OH)-BO2/2(OH)-(OH0.5)-PO2/2O(OH)]. Fe3+ is in an octahedral coordination (Fe(O)2(OH)4).

Oligomere Tetraeder-Anionen in Borophosphaten: Darstellung und Kristall­strukturen von NaFe[BP2O7(OH)3] und K2Fe2[B2P4O16(OH)2 ]/Oligomeric Tetrahedral Anions in Borophosphates: Synthesis and Crystal Structures of NaFe[BP2O7(OH)3] and K2Fe2[B2P4O16(OH)2]

Abstract Crystals of the title compounds were grown under hydrothermal conditions. The crystal structures were determined by single crystal data. NaFe[BP2O7(OH)3] (monoclinic, C 2/c, a = 1042.0(2), b = 821.5(1), c = 921.7(1) pm, β = 116.60(1)°, Z=4): The crystal structure contains isolated anions [BP2O7(OH)3]4-, which correspond to trinuclear units PO1/2O3-BO2/2(OH)2 -PO1/2O2(OH) of corner sharing tetrahedra. Fe3+ is coordinated octahedrally by oxygen, Na+ is 8 -fold coordinated by oxygen forming cubes. K2Fe2[B2P4O16(OH)2] (triclinic, P1̄, a = 516.7(1), b = 808.9(1), c = 834.0(1) pm, α = 87.06(f), β = 80.21(1), γ = 86.59(1)°, Z = 1): The crystal structure contains isolated anions [B2P4O16(OH)2]8-. Four-membered rings of tetrahedra with two additional terminal phosphate groups are formed by condensation of two trinuclear units P O1/2O3 -BO3/2(OH) -PO2/2O2. Fe3+ is in an octahedral and K+ in an irregularly 10-fold coordination by oxygen.