Zur Kenntnis ternärer Oxide des Bleis: Über Na2PbO2

On Ternary Oxides of Lead. The Na₆PbO₅ Na₆PbO₅ (pale yellow) crystallizes orthorhombic in Cmcm with a=10.6₈, b=5.70₉, c=10.9₉, å; Z=1. Parameters were refined by least-squares (479 hkO–hk7, MO–K_α) R=0.112₄, R′=0.116, (parameters see text). Isolated PbO₅ groups of pseudotetragonal pyramids lend Pb⁴⁺ Coordination Number (CN) 5. Along [100] and [010] the pyramids are equivalent orientated, but along [001] alternately twisted by 180°. Na+ occupies holes between O^2?, leading to CN 6 (Na″+) and Na″′⁺ and CN 4 (Na′⁺). The MADELUNG part of lattice energy (MAPLE) is calculated and discussed.     

Zur Konstitution von ‚KPbO2’︁

On the Constitution of ‘KPbO₂’ Transparent, orangered single crystals of K₂Pb₂O₄ have been obtained by heating mixtures of K₂O₂ and PbO (K:Pb = 1:1) [Ag-cylinders, 560°C, 40 d, after cooling (15°C/h)]. The space group is P1 , a = 1295.94(9), b = 753.35(7), c = 697.12(8) pm, α = 118.00(1)°, β = 106.15(1)°, γ = 93.44(1)°, Z = 4, d_x = 6.573 und d_pyk = 6.54 g · cm³. The structure is characterized by rutilanalogous chains of edge-connected [PbO₆] octahedra along [001] according to [PbO_4/2O_2/1] = PbO₄. On both sides of such a chain there are respectively three O^2?, which belong to two octahedra, alternating capped with Pb²⁺ or not capped, corresponding to [PbO₄]Pb₂[PbO₄]□₂… = Pb₂O₄. Those capped chains are held together by K(1)…K(4), each of them with C.N. 6. The order of the chains corresponds to the motive of a closest packing. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated and discussed.     

Über ternäre Oxide des Bleis: Zur Kenntnis von Na6PbO4

On Ternary Oxides of Lead. The Na₆PbO₄ New obtained Na₆PbO₄ (colourless to pale yellow), is due to single crystal datas cubic, I43m, with a=11,0₁ Å and Z=8. Parameters were refined by least-squares (705 h01–h51, Mo–K_α) Ra=0.082, R′=0.091 (Parameters see text). In an ordered derivative of Na₂O-structure, there are according to [O′′Na₄Na₄] [O′(PbO₃″′)₄] “isolated” Pb₄O₁₃-groups, which are connected with each other by Na′ and Na″. The MADELUNG part of lattice energy (MAPLE) is calculated and discussed.     

Das erste gemischtvalente Oxoplumbat mit „isolierten”︁ Baugruppen: KNa7[PbIVO4][PbIIO3]

The First Mixed-valent Oxoplumbate with Isolated Anions. On KNa₇[Pb^IVO₄][Pb^IIO₃] For the first time KNa₇Pb₂O₇ has been prepared by reaction of K and Na Oxides with ?PbO₂”? rsp. PbO_red [e. g.: KO_0.48:NaO_0.36:?PbO₂”? = 1:7:2 (Ag-cylinders, reduced Ar-pressure, sealed in supremax-glas ampoules, 600°C, 14 d): redorange single crystals of plated shape]. The structure determination [3269 I_o(hkl), four-circle diffractometer PW 1100 (Fa. Philips), ω-scan, MoKα, R = 9.52%, R_w = 7.67%, absorption not considered] proves the space group P2₁/c with a = 1758.48(10), b = 596.76(3), c = 1066.46(8) pm, β = 90.682(8)°, Z = 4, d_x = 4.311, d_pyk = 4.28 g/cm³. The structure is characterized by isolated [Pb^IVO₄] (symmetry nearly T_d) and [Pb^IIO₃] groups (symmetry nearly C_3v), the latter connected by cations to double-layers. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated and discussed.     

“Fragmentierung” und “Aggregation” bei Bleioxiden Über das Oligooxoplumbat(IV) K2Li6[Pb2O8]

“Fragmentation” and “Aggregation” on Lead Oxides. On the Oligooxoplumbate(IV) K₂Li₆[Pb₂O₈] For the first time, the dinuclear Oxoplumbate(IV) K₂Li₆[Pb₂O₈] has been prepared as transparent colourless single crystals by heating mixtures of K₂PbO₃, Li₂O, and “PbO₂” with K:Li:Pb = 1:3:1 e. g. [Ag-cylinders, sealed under vacuum in Supremax-glass ampoule, 660°C, 120 d]. The structure determination verifies the space group P1 with a = 6.9720(9), b = 5.9252(6), c = 5.9312(7) Å, α = 88.05(1)°, β = 107.94(1)°, γ = 107.30(1)°; d_x = 4.95 g · cm^?3, d_pyk = 4.91 g · cm^?3; Z = 1, [2107 symmetry independent hkl, fourcircle-diffractometer Philips PW 1100, ω—2Θ—scan, MoKα, R = 5.07%, R_w = 4.59%, absorption not considered]. The structure is characterized by the group [Pb₂O₈] — two edge connected (equatorial/apical) trigonal bipyramids — that is observed for the first time. Several ways of synthesis are given. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Effective Ionic Radii, MEFIR, are calculated.     

Neue Oxoplumbate(II) A2PbO2 (A = K,Rb, Cs) mit zweikernigen Gruppen [OPbO2PbO]

New Oxoplumbates(II) A₂PbO₂ (A = K, Rb, Cs), with Binuclear Groups [OPbO₂PbO] Unknown K₂PbO₂, Rb₂PbO₂ and Cs₂PbO₂ (yellowish powder, yellowish transparent single crystals, respectively) have been prepared, The compounds crystallize triclinic with a = 10.90₁ Å, b = 7.60₆ Å, c = 7.32₈ Å, α = 119.3₅°, β = 88.4₂°, γ =117,7₃°, (K₂PbO₂); a = 10.90₇ Å, b = 8.51₀ Å, c = 7.81₅ Å, α = 124.0₀°, β = 84.9₇°, γ = 120.6₈° (Rb₂PbO₂) and a = 11.64₄ Å, b = 8.90₅ Å, c = 8.04₀ Å, α = 123.3₂°, β = 85.7₀°, γ = 120.4₉° Z = 4, space group P1 -C/_i¹. For K₂PbO₂ we find R = 8.6₅% and R_w = 9.3₂% (2283 independent reflections). Parameters see text. There are isolated [Pb₂O₄]groups, which are connected in a complicated way by mutual K⁺ ions forming layers. The Madelung Part of the Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, these by means of mean Fictive Ionic Radii, MEFIR, are calculated and discussed.     

Zur Kristallstruktur von Li8PbO6 [1]

On the Structure of Li₈PbO₆ For the first time single crystals of Li₈PbO₆ have been prepared by heating of mixtures of Na₂PbO₃ and Li₂O [Ag-cylinders, 650°C, 150 d]. The structure [382 I₀(hkl), four circle diffractometer PW 1100, ω/2Θ-scan, MoKα, R = 3.07%, R_w = 3.00%, space group R3 ; a = 555.09(4), c = 1564.13(17) pm, D_x = 4.28 g · cm^?3, D_pyk = 4.24 g · cm^?3, Z = 3] is characterized by the motive of a hexagonal-closed O^2? packing. Half of the octahedral sites are occupied by Pb⁴⁺ and Li⁺ and half of the tetrahedral sites only by Li⁺. The Madelung Part of Lattice Energy, MAPLE, and the Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated.     

New silicate-germanate Cs2Pb2[(Si0.6Ge0.4)2O7] from the series A2Pb2[B2O7], A = K,Cs, B = Si,Ge with the umbrella-like [PbO3]4- group

New silicate-germanate Cs₂Pb₂[(Si_0.6Ge_0.4)₂O₇] was synthesized in multi-components hydrothermal solution with 20 w.% concentration of Cs₂CO₃ mineralizer, pH = 10. Novel mixed compound belongs to the structure type A₂Pb₂[B₂O₇] previously indicated for powders with A = K, B=Si or Ge. Singe crystal structure determination of Cs₂Pb₂[(Si_0.6Ge_0.4)₂O₇] revealed the need for the correction of the space group of the earlier suggested structural model from P-3 to P-3m1, as well as for the splitting of the Pb-atom position. Umbrella-like groups [PbO₃]^4- are located between [(Si,Ge)O₄]^4- tetrahedra in mica-like honeycomb layers and play the role of tetrahedra with the Pb-lone-pair as the forth apex. Crystal chemical comparison revealed similarities and differences with the classical structure type of α-celsian Ba[Al₂Si₂O₈] with the tetrahedral double layer. Recently investigated nonlinear optical acentric borates Pb₂(BO₃)(NO₃) and Pb₂(BO₃)Cl are both related to this structural type, possessing umbrella-like groups [PbO₃]^4- and honeycomb layers [Pb₂(BO₃)]⁺ with the BO₃-triangles on the tetrahedral positions.     

Über quaternäre Oxoplumbate(IV). Zur Kenntnis von Rb2Li14[Pb3O14] und Cs2Li14[Pb3O14]

On Quaternary Oxoplumbates(IV). On the Knowledge of Rb₂Li₁₄[Pb₃O₁₄] and Cs₂Li₁₄[Pb₃O₁₄] For the first time, Rb₂Li₁₄[Pb₃O₁₄] and Cs₂Li₁₄[Pb₃O₁₄] have been prepared by heating of mixtures of Li₂O, β-?PbO₂”? and Rb₂PbO₃, Cs₂PbO₃ respectively with Li:Pb:A = 14:3:2, (A = Rb, Cs). [Ag-cylinders, sealed under vacuum in Duran-glass ampoule, 590 and 550°C, 40 d, powder (650°C, 200 d, single crystals of Rb₂Li₁₄[Pb₃O₁₄])]. Rb₂Li₁₄[Pb₃O₁₄] is nearly colourless with ivory nuance, Cs₂Li₁₄[Pb₃O₁₄] is pale yellow. According to powder and single crystal investigations, both are isotypic with K₂Li₁₄[Pb₃O₁₄]. Structure refinement of Rb₂Li₁₄[Pb₃O₁₄]: 1015 symmetry independent reflexions, four-circle-diffraktometer PW 1100 (Fa. Philips), ω-scan, MoKα, R = 5.73%, R_W = 5.33%, absorption not considered, space group Immm with a = 1284.71(9), b = 793.90(4), c = 727,35(5) pm, d_x-ray = 4.99 g · cm^?3, d_pyc = 5.01 g · cm^?3, Z = 2. Cs₂Li₁₄[Pb₃O₁₄]: a = 1295.28(12), b = 796.69(8), c = 732.44(7) pm, d_x-ray = 5.31 g · cm^?3, d_pyc = 5.28 g · cm^?3, Z = 2. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Effective Ionic Radii, MEFIR, are calculated.     

Iodoplumbate mit polymeren Anionen – Synthese und Kristallstrukturen von [Na3(OCMe2)12][Pb4I11(OCMe2)], (Ph4P)2[Pb5I12] und (Ph4P)4[Pb15I34(dmf)6]

Iodoplumbates with Polymeric Anions – Synthesis and Crystal Structures of [Na₃(OCMe₂)₁₂][Pb₄I₁₁(OCMe₂)], (Ph₄P)₂[Pb₅I₁₂], and (Ph₄P)₄[Pb₁₅I₃₄(dmf)₆] Reactions of PbI₂ with NaI in polar organic solvents followed by crystallization with large cations yield iodoplumbate complexes with various compositions and structures. [Na₃(OCMe₂)₁₂][Pb₄I₁₁(OCMe₂)] 3 , (Ph₄P)₂[Pb₅I₁₂] 4 and (Ph₄P)₄[Pb₁₅I₃₄(dmf)₆] 7 contain one-dimensional infinite anionic chains of face- or edge-sharing PbI₆ or PbI₅L (L = acetone, DMF) octahedra. [Na₃(OCMe₂)₁₂][Pb₄I₁₁(OCMe₂)] 3 : Space group P1 (No. 1), a = 1120.3(5), b = 1265.3(6), c = 1608.3(8) pm, α = 74.64(4), β = 70.40(4), γ = 85.24(4)°, V = 2071(2) · 10⁶ pm³; (Ph₄P)₂[Pb₅I₁₂] 4 : Space group C2/c (No. 15), a = 787.00(10), b = 2812.0(5), c = 3115.9(5) pm, β = 96.240(13)°, V = 6885(2) · 10⁶ pm³; (Ph₄P)₄[Pb₁₅I₃₄(dmf)₆] 7 : Space group P2₁/n (No. 14), a = 2278.8(4), b = 1782.6(3), c = 2616.8(4) pm, β = 114.432(13)°, V = 9678(3) · 10⁶ pm³.     

Präparation und Strukturanalyse der Verbindungen Ba2Pb4F10Br2–xIx (x = 0–2) mit verwandten kristallchemischen Motiven aus der Fluoritund Matlockitstruktur

Preparation and Structure of the Compounds Ba₂Pb₄F₁₀Br_2–xI_x (x = 0–2) with Related Structure Motifs of the Fluorites and Matlockites Colourless single crystals of Ba₂Pb₄F₁₀Br_2–xI_x (x = 0–2) have been obtained under hydrothermal conditions (T = 250 °C, 10 d), starting from stoichiometric amounts of BaF₂, PbF₂, PbBr₂ and PbI₂. The compounds crystallize in the tetragonal space group P4/nmm (No. 129). A complete miscibility in the region x = 0–2 has been observed. The mixed crystals follow Vegard's rule. For the compounds with the composition Ba₂Pb₄F₁₀Br₂ (a = 5.9501(2) Å, c = 9.6768(10) Å, R[F² > 2σ(F²)] = 0.022, wR(F² all reflections) = 0.059), Ba₂Pb₄F₁₀Br_1.1I_0,9 (a = 5.9899(3) Å, c = 9.7848(5) Å, R[F² > 2σ(F²)] = 0.014, wR(F² all reflections) = 0.035) and Ba₂Pb₄F₁₀I₂ (a = 6.6417(3) Å, c = 9.9216(10) Å, R[F² > 2σ(F²)] = 0.023, wR(F² all reflections) = 0.049) complete structure analyses have been performed on the basis of single crystal diffractometer data. Microcrystalline single phase compounds Ba₂Pb₄F₁₀Br_2–xI_x (x = 0–2) have been obtained by coprecipitation from aqueous solutions of KF, KBr (KI) and Ba(CH₃COO)₂, Pb(NO₃)₂ in acetic acid medium. For Ba₂Pb₄F₁₀Br_1.5I_0.5 and Ba₂Pb₄F₁₀Br_0.5I_1.5 powder data of microcrystalline samples were used for the Rietveld analyses (R_Bragg = 0.077 for Ba₂Pb₄F₁₀Br_1,5I_0,5 and R_Bragg = 0.065 for Ba₂Pb₄F₁₀Br_0.5I_1.5). The crystal structure comprises alternating structural features of fluorite related type (CaF₂) around Ba and matlockite related type (PbFCl) around Pb1 and Pb2 along the c axis. Barium shows a {8 + 4} cuboctahedral coordination of fluorine. The coordination polyhedron around the two crystallographically independent lead atoms is a monocapped quadratic antiprism built of {4 + 1} fluorine and {4} bromine or iodine atoms, respectively.     

Über quaternäre Oxoplumbate(IV). Zur Kenntnis von Rb3NaPbO4

On Quaternary Oxoplumbates(IV). On Rb₃NaPbO₄ For the first time, Rb₃NaPbO₄ has been prepared by annealing mixtures of Na₂PbO₃ and RbO_0.84 with Rb:Na:Pb = 4:2:1 [nonhermetic Ag-cylinders, sealed under vacuum in Duran-glass ampoule, 480°C, 180 d (single crystals)]. The colourless crystals are of squatted shape. The structure determination [2943 symmetry independent hkl, four-circle-diffractometer PW 1100 (Fa. Philips), ω-2Θ-scan, AgKα, R = 8.64%, R_W = 6.59%, absorption not considered] confirms the space group P2₁/c with a = 1101.79(26), b = 662.66(11), c = 1115.01(30) pm, β 112.027(21)°. The structure is characterized by isolated [PbO₄]-tetrahedra and [Na₂O₆]-tetrahedra-doubletts, C.N. 5 and 7 for Rb⁺. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Effective Ionic Radii, MEFIR, are calculated.     

Crystal Chemistry of the M11+,2+–M22+,3+–(H)‐Arsenites: the First Cadmium(II) Arsenite,Na4Cd7(AsO3)6

The crystal structures among M1–M2–(H)‐arsenites (M1 = Li⁺, Na⁺, K⁺, Rb⁺, Cs⁺, Ca²⁺, Sr²⁺, Ba²⁺, Cd²⁺, Pb²⁺; M2 = Mg²⁺, Mn^2+,3+, Fe^2+,3+, Co²⁺, Ni²⁺, Cu²⁺, Zn²⁺) are less investigated. Up to now, only the structure of Pb₃Mn(AsO₃)₂(AsO₂OH) was described. The crystal structure of hydrothermally synthesized Na₄Cd₇(AsO₃)₆ was solved from the single‐crystal X‐ray diffraction data. Its trigonal crystal structure [space group R$\bar{3}$ , a = 9.5229(13), c = 19.258(4) Å, γ = 120°, V = 1512.5(5) ų, Z = 3] represents a new structure type. The As atoms are arranged in monomeric (AsO₃)^3– units. The surroundings of the two crystallographically unique sodium atoms show trigonal antiprismatic coordination, and two mixed Cd/Na sites are remarkably unequal showing tetrahedral and octahedral coordinations. Despite the 3D connection of the AsO₃ pyramids, (Cd,Na)O_x polyhedra and NaO₆ antiprisms, a layer‐like arrangement of the Na atoms positioned in the hexagonal channels formed by CdO₄ deformed tetrahedra and AsO₃ pyramids in z = 0, 1/3, 2/3 is to be mentioned. These pseudo layers are interconnected to the 3D network by (Cd,Na)O₆ octahedra. Raman spectra confirmed the presence of isolated AsO₃ pyramids.     

Über quaternäre Oxowolframate (VI) Na6Li2[W2O10] - ein Diwolframat

On Quaternary Oxotungstates (VI). Na₆Li₂[W₂O₁₀] — a Ditungstate For the first time, Na₆Li₂[W₂O₁₀] has been prepared by annealing mixtures of WO₃, Na₂O and Li₂O with W:Na:Li = 1:3:1 [closed Pt-tube in quartz-glass ampoule, 840°C, 60 d (single crystals)]. The colourless crystals are of squatted shape. The structure determination [1813/I₀(h kl), four-cycle diffractometer PW 1100 (Fa. Philips), ω-scan, AgK_α, R = 8.32%, absorption not considered] confirms the space group P1 with a = 784.66(11), b = 602.53(7) c, = 563.81(11) pm α = 106.784(14)°, β = 114.548(14)°, γ = 91.082(13)°, Z = 2, d_x = 4.92 g · cm^?3, d^pyk = 4.85 g · cm^?3. The structure may be described as a distorted derivative of the NaCl-type. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated and discussed.     

Selenostannate aus wäßriger Lösung: Darstellung und Struktur von Na4SnSe4 · 16 H2O

Selenostannates from Aqueous Solutions: Preparation and Structure of Na₄SnSe₄ · 16 H₂0 Pure selenostannates(IV) are prepared from aqueous solutions by reaction of SnSe₂, with alkali selenides, strictly excluding oxygen. Na₄SnSe₄ · 16 H₂O, being obtained from stoicheo-metric 1:2 quantities, is characterized by a complete X-ray structure analysis and by vibrational spectra. The compound is monoclinic (P2₁/m) with a = 8.673(3), b = 16.563(4), c = 8.647(2) Å, β = 92.10(2)°, Z = 2; it contains isolated tetrahedral SnSe₄^4? ions [Sn? Se 2.504(2)?2.527(2) Å, Se? Sn? Se 106.6(1)?111.1(1)°] which are in contact to the hydrated octahedral [Na(OH₂)₆]⁺ ions through Se…?H? O bridges within an extensive hydrogen bridge system. The stretching vibrations of the SnSe₄^4? ion are observed at 195 (n?₁) and 252 cm^?1 (n?₃). The stretching force constant is approximately 1.59 mdyn/Å.     

Ein neuer Strukturtyp zur Formel A2MO4: Pb2MnO4, eine Tunnelstruktur mit einseitig koordinierten Pb2+-Ionen

A New Structure Type of the Formula A₂MO₄: Pb₂Mn₄, a Tunnel Structure with one-sided Coordination of Pb²⁺ Ions Pb₂MnO₄ was prepared and investigated by single crystal X-ray technique (space group D–P4 2₁c; a = 12.773; c = 5.142 Å; Z = 8). Pb₂MnO₄ crystallizes with a new structure type, it is not isotypic to Pb₂PbO₄ or Pb₂PtO₄. The main difference of the new structure type concerns zig-zag-chains of edge connected MnO₆?octahedra. The polyhedra network and the tunnel frame of Pb²⁺ are nevertheless very similar to the Pb₃O₄ structure.     

Natriumkomplexe mit Salicylideniminen: Synthesen,Strukturen, CO2‐Aufnahme und Carboxylierung von 2‐Fluorpropiophenon bzw. Estronmethylether

Chiral salicylidenphenethylamines (R)‐HA or (S)‐HA , 2‐salicylidenfurfuryl‐imines HB , and 2‐salicylidenaminoethanol HC react with sodium hydride or sodium hexamethyldisilylamide to form the sodium complexes [Na(R)‐A] ₄ · 0,5 Et ₂ , [Na(S)‐A] ₄ · 0,5 Et ₂ O (1) , [NaB] ₄ · 0,5 Ph‐Me (2) and [(dme)NaC] ₄ (3) . In the presence of 18‐crown‐6 the complex [Na(18‐crown‐6)(thf) ₂ ] ₂ [Na ₂ (C)] ₄ · THF (4) can also be isolated. The crystal structure analyses of both 1 and 2 show that heterocubane structures with a Na₄O₄ frame work are formed. Additionally, the imine nitrogen atom is bonded at the Na atom which has the coordination number 4 in 1 . Additional coordination of the furfuryl oxygen atom results in the coordination number five for the sodium atom in 2 . In 3 which is also a tetramer, two Na₂O₂ units are connected via two imino‐ethanol bridges Na(1)‐N(=CH‐phenolat)‐CH₂CH₂‐OH‐Na(2A). The crystal structure analysis displays that 4 is an ionic compound consisting of two [(thf)₂Na(18‐crown‐6)]⁺ cations and the dinuclear dianion [Na ₂ (C) ₄ ] ^2? . Both 1 and 2 are carboxylation reagents which transfer CO₂ to 2‐fluoropropiophenone. 1 is more active than 2 , but 3 and 4 are inactive.     

Iodoplumbate mit vier‐ und fünffach koordinierten Pb2+‐Ionen

Iodoplumbates with Tetra‐ and Penta‐coordinated Pb²⁺ Ions In contrast to all known iodoplumbates with octahedrally coordinated Pb²⁺ ions, square pyramidal geometry is observed in the iodoplumbate chains of (Pr₄N)[PbI₃] ( 1 ) and [Mg(dmf)₆][PbI₃]₂ ( 2 ), whereas the isolated anions in (Ph₄P)₂[Pb₂I₆] ( 3 ) and [Bu₃N–(CH₂)₃–NBu₃][PbI₄] ( 4 ) contain tetra‐coordinated lead atoms. (Pr₄N)[PbI₃] ( 1 ): a = 910.86(6), b = 1221.46(7), c = 1907.7(1) pm, V = 2122.5(2) · 10⁶ pm³, space group P2₁2₁2₁; [Mg(dmf)₆][PbI₃]₂ ( 2 ): a = 891.24(9), b = 1025.34(7), c = 1234.82(9) pm, α = 92.938(8), β = 106.457(8), γ = 98.100(7)°, V = 1066.4(2) · 10⁶ pm³, space group P1; (Ph₄P)₂[Pb₂I₆] ( 3 ): a = 1174.5(1), b = 722.29(7), c = 3104.8(4) pm, β = 100.50(1)°, V = 2589.8(5) · 10⁶ pm³, space group P2₁/n; [Bu₃N–(CH₂)₃–NBu₃][PbI₄] ( 4 ): a = 2178.3(1), b = 1008.63(5), c = 1888.3(1) pm, β = 110.003(5)°, V = 3898.6(4) · 10⁶ pm³, space group P2/c.     

Notizüber Li2PbO3 und Na2PbO3

The compounds Li₂PbO₃ (α-and β-modification) and Na₂PbO₃ are prepared by heating mixtures of Li₂O₂/PbO₂ resp. Na₂O₂/PbO₂ in a dry oxygen atmosphere. The monoclinic lattice constants are reported.