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BCoH09P2Pb, triclinic, PI (no. 2), a = 5.2208(2) A, b = 7.8467(7) A, c = 8.3422(3) A, a = 89.473(8)°, β = 79.219(4)°, γ = 87.521(7)°, V = 335.4 A, Ζ = 2, R&(F) = 0.034, wR^F) = 0.083, Τ = 293 Κ. BH09P2PbZn, triclinic, P\ (no. 2), a = 5.2172(2) A, b = 7.8432(7) A, c = 8.3205(4) A, a = 89.429(8)°, β = 79.239(5)°, γ = 87.536(8)°, V = 334.2 A, Ζ = 2, Rgt(F) = 0.046, wRreffF) = 0.120, Τ = 293 Κ. Source of material PbCo[BP20e(OH)] and PbZn[BP20s(0H)] were synthesized under mild hydrothermal conditions. PbCo[BP20g(OH)] was prepared from the mixtures of0.4007 g Co(OOCCH3)2 · 4H2O (Alfa Aesar), 0.5 g PbB204 · H20 (Alfa Aesar), 0.1987 g H3BO3 (Alfa Aesar) and 0.7880 g H3PO4 (Merck) in the molar ratio 1:1:2:5. 1 ml of HCl (37 %) was added to adjust the pH value to 1. The mixture was filled into a 10 ml autoclave (filling degree 30 %) and heated at 443 Κ for three weeks under autogenous pressure. PbZn[BP2Og(OH)] was prepared from mixtures of 0.2618 g ZnO (Merck), 0.5 g PbB204 · H20 (Alfa Aesar), 0.1987 g H3BO3 (Alfa Aesar) and 0.6304 g H3PO4 (Merck) in the molar ratio 2:1:2:4. The pH of the solution was adjusted to 1.5. The mixture was filled into a 10 ml autoclave (filling degree 30 %) and heated at 443 Κ for three weeks. The chemical composition of the title compounds were confirmed by chemical analyses. Experimental details The hydrogen atom for PbCo[BP20g(OH)] was located in a Fourier difference map and the Ο—Η distance was fixed to 0.80 A during the final refinement. In the case of PbZn[BP2Og(OH)] the Η atom could not be determined from the Fourier difference map. Discussion During past few years compounds with open framework structures like borophosphates have drawn much attention [1]. Our systematic studies on the systems 3/0-Pb02-B203-P20s-H20 (M = Co, Zn) led to two novel borophosphates: PbCo[BP20e(OH)] and PbZn[BP20e(0H)]. The charge of the borophosphate anion ([ΒΡ20β(0Η)]~) is compensated by two different divalent cations. The crystal structures of the title compounds are isotypic to the K-Sc [2], Rb-Sc [3], NILt-In [4], K-In [5], K-Fe [6] and Rb-In [7] analogues. The anionic partial structure contains open branched fourmembered rings [ΒιΡ^ιβίΟΗ^], which are formed by alternating borate and phosphate tetrahedra sharing common corners with two phosphate branches. The condensation of the borophosphate anions with A/Os(OH) (M = Co; Zn) octahedra via common corners results in an overall three-dimensional framework which contains elliptical channels running along [100]. The cross section of the channels is defined by eight-membered rings consisting of two AZ-coordination octahedra, four phosphate tetrahedra and two borate groups. Lead ions reside within the open channels. In the case of PbCo[BP208(OH)], the Co—Ο bond distances range from 2.04 A to 2.18 A. The bond distances for Zn—Ο in PbZn[BP2Os(OH)] range from 2.03 A to 2.21 A. Bond lengths and angles of the borophosphate anions in both compounds are similar to their K-Sc, Rb-Sc, NHt-In, K-In, K-Fe and Rb-In analogues by considering bond lengths d(P—O) and d(Β—Ο) as well as bond angles [2-7]. 1. Lead (II) cobalt(II) (monophosphate-hydrogenmonoboratemonophosphate), PbCo[BP20g(OH)] Table 1. Data collection and handling. Crystal: Wavelength: MDiffractometer, scan mode: 2$max! WA*0measiired, N(hkl)maqM· Criterion for lobs, N(hkl)gc. N(param)K6im)'· Programs: red platelet, size 0.090 χ 0.080 χ 0.025 mm Mo Ka radiation (0.71073 Ä) 280.44 cm" Rigaku AFC-7 & Mercury CCD, φ/ω 67.16° 6406,2233 /obs >2ff(Z

zeitschrift für kristallographie. new crystal structures/zeitschrift für kristallographie. new crystal structures

Crystal structures of lead(II) cobalt(II) (monophosphate-hydrogenmonoborate- monophosphate), PbCo[BP208(OH)], and lead(II) zinc(II) (monophosphate- hydrogenmonoborate-monophosphate), PbZn[BP 2 O 8 (0H)]