Crystal Structures of Alkali Metal Peroxodiphosphates

Peroxodiphosphates of alkali metals can be prepared from K₄P₂O₈, which is synthesized by electrolysis, in metathesis reactions with the corresponding perchlorates. Single crystals have been obtained by diffusion of methanol into aqueous solutions of the peroxodiphosphates. The crystal structures of Li₄P₂O₈·4H₂O (P2₁/n; a = 8.057(2) Å, b = 5.074(1) Å, c = 12.288(3) Å, β = 100.53(2)°; V = 493.9(2) ų; Z = 2), Na₄P₂O₈·18H₂O (at 130 K: P6₁; a = 9.0984(14) Å, c = 49.926(13) Å; V = 3579.2(12) ų; Z = 6) and K₄P₂O₈ (P2₁/c; a = 5.9041(15) Å, b = 10.254(2) Å, c = 7.356(2) Å, β = 99.05(3)°; V = 439.79(18) ų; Z = 2) have been determined by X‐ray diffraction. In the Li salt the cations are tetrahedrally coordinated by one water molecule and three oxygen atoms of the anions, whereas the Na salt is characterized by binuclear [Na₂(H₂O)₉]²⁺ complexes. At low temperatures, the latter undergoes a phase transition from a structure with disordered anions to a completely ordered phase. K₄P₂O₈ is solvent‐free and exhibits irregular cation coordination. The structure of the peroxodiphosphate anion is very similar in all compounds; the mean O–O distance is 1.49(1) Å. In addition, the structure determination of K₄(HPO₄)₂·3H₂O₂ (P2₁/n; a = 6.076(1) Å, b = 6.579(1) Å, c = 17.215(2) Å, β = 99.73(1)°; V = 678.26(17) ų; Z = 2), which can be mistaken for K₄P₂O₈, is presented.     

[C10N2H10][ZnCl(HPO4)]2: A New Templated Zincophosphate Containing Tetrahedral Nets with 63 Topology

The crystal structure of [C₁₀N₂H₁₀][ZnCl(HPO₄)]₂ contains corrugated tetrahedral layers with 6³ topology. Charge balance is achieved by insertion of diprotonated 4,4′‐bipyridine between the layers. Crystal data: monoclinic, P2₁/n (no. 14), a = 4.8832(2) Å, b = 22.673(2) Å, c = 8.1643(4) Å, β = 104.02(1)°; V = 877.0(1) ų; Z = 4; R1 = 0.041 and wR2 = 0.088 for 1836 reflections [I > 2σ(I)]. Tetrahedral layers are also observed in other organo‐ammonium templated compounds. However, their topologies are characterized by 4.8² nets. With the title compound a layered tetrahedral net with 6³‐topology is reported for the first time.     

Synthese und Charakterisierung von Natriumcyanamid

Synthesis and Characterization of Sodium Cyanamide The synthesis of Na₂CN₂ was carried out by reaction of sodium amide with sodium hydrogen cyanamide at 200 °C, in vacuum. Single crystals were obtained while heating the product (500 °C, 8 days) in silver crucibles. The title compound was characterised by single crystal X‐ray diffraction and IR‐spectroscopy (C2/m; Z = 2, a = 5.0456(3), b = 5.0010(3), c = 5.5359(3) Å; β = 110.078(5)°; R1 = 3.18%, wR2 = 6.35%, GOF = 1.078). The CN₂^2– units are linear exhibiting a C–N bond length of 1.236(1) Å, while sodium is coordinated by five nitrogen atoms forming a square pyramid. The structural relationships to aristotypic Na₂HgO₂ are pointed out.     

Syntheses and Crystal Structures of the Novel Ternary Thioborates Na3BS3, K3BS3, and Rb3BS3

The orthothioborates Na₃BS₃, K₃BS₃ and Rb₃BS₃ were prepared from the metal sulfides, amorphous boron and sulfur in solid state reactions at temperatures between 923 and 973 K. In a systematic study on the structural cation influence on this type of ternary compounds, the crystal structures were determined by single crystal X‐ray diffraction experiments. Na₃BS₃ crystallizes in the monoclinic space group C2/c (No. 15) with a = 11.853(14) Å, b = 6.664(10) Å, c = 8.406(10) Å, β = 118.18(2)° and Z = 4. K₃BS₃ and Rb₃BS₃ are monoclinic, space group P2₁/c (No. 14) with a = 10.061(3) Å, b = 6.210(2) Å, c = 12.538(3) Å, β = 112.97(2) and a = 10.215(3) Å, b = 6.407(1) Å, c = 13.069(6) Å, β = 103.64(5)°, Z = 4. The potassium and rubidium compounds are not isotypic. All three compounds contain isolated [BS₃]^3– anions with boron in a trigonal‐planar coordination. The sodium cations in Na₃BS₃ are located between layers of orthothioborate anions, in the case of K₃BS₃ and Rb₃BS₃ stacks of [BS₃]^3– entities are connected via the corresponding cations. X‐ray powder patterns were measured and compared to calculated ones obtained from single crystal X‐ray structure determinations.     

Synthesis and Crystal Structure of KSc(HPO4)2

KSc(HPO₄)₂ was obtained by hydrothermal synthesis. The crystal structure was determined from single‐crystal X‐ray data: orthorhombic, space group Pnma (No. 62), a = 14.5095(10), b = 5.4260(4), c = 8.4882(5) Å, V = 668.26(8) ų and Z = 4. The crystal structure of KSc(HPO₄)₂ represents a new structure type containing twelve‐ and four‐membered rings forming channels along [010] built of alternating ScO₆ octahedra and HPO₄^2? groups. Potassium ions reside within the twelve membered ring channels.     

NaSc3[HPO3]2[HPO2(OH)]6: Synthesis,Crystal Structure,and Thermal Decomposition

NaSc₃[HPO₃]₂[HPO₂(OH)]₆ was prepared by use of a phosphorus acid flux route. The crystal structure was determined from single‐crystal X‐ray diffraction data: triclinic, space group P$\bar{1}$ (No. 2), a = 7.4507(11) Å, b = 9.6253(17) Å, c = 9.6141(16) Å, α = 115.798(4)°, β = 101.395(4)°, γ = 101.136(3)°, V = 577.29(16) Å³ and Z = 1. The crystal structure of NaSc₃[HPO₃]₂[HPO₂(OH)]₆ contains two kinds of phosphate(III) groups: HPO₃^2– and HPO₂(OH)^–. Phosphate(III)‐tetrahedra, NaO₆ and ScO₆ octahedra together form a (3,6)‐connected net. During heating hydrogen and water are released and Sc[PO₃]₃ is formed as the main crystalline decomposition product.     

A new 3s–3d heterometallic polymer containing N‐methyliminodiacetic acid: synthesis,structure and characterization

A new complex {[Na₂(H₂O)₃(µ‐L)₂Cu]₄}_∞ (L = N‐methyliminodiacetic acid) has been synthesized and structurally characterized. The complex crystallizes in the monoclinic, space group C2/c, with the unit cell parameters a = 16.556(3) Å, b = 8.0622(13) Å, c = 12.671(2) Å, α = 90°, β = 95.849(2)°, γ = 90°. The central metal Cu (II) ion is coordinated with two nitrogen atoms and four oxygen atoms belonging to two ligands. Simultaneously, the sodium is six‐coordinated with oxygen atoms coming from the ligand and water molecule; the sodium atoms related are bridged by oxygen atoms, forming a sodium chain. The structure consists of CuL₂ moieties linked by sodium chain via the exo oxygen atoms of two ligands, forming a novel three‐dimensional structure. Moreover, elemental analysis, IR, UV‐vis, ESR spectroscopy and thermal stability were determined. Copyright © 2007 John Wiley & Sons, Ltd.     

Synthesis and Characterization of a New Organically Templated Aluminophosphite with a Chainlike Structure

A new aluminophosphite (H₄bape)_0.5[Al(OH)(HPO₃)₂] has been synthesized under hydrothermal conditions and its structure was determined by single‐crystal X‐ray diffraction (bape = N,N′‐bis(2‐aminopropyl)ethylenediamine). This compound crystallizes in the triclinic system with the space group (No. 2), a = 6.919(2) Å, b = 8.704(2) Å, c = 9.786(2) Å, α = 77.74(3)°, β = 72.43(3)°, γ = 72.52(3)°, V = 531.08(2) ų, Z = 2. The structure consists of distorted octahedral AlO₆ and pseudo pyramidal HPO₃, which are connected by vertex oxygen atoms to form a chainlike framework with a Al/P ratio of 1/2. The presence of 1D infinite Al‐O‐Al linkage in the framework is noteworthy. The organic templates are fully protonated and interact with the aluminophosphite chains through extensive hydrogen bonds to form a 3D supramolecular network.     

Darstellung und Kristallstruktur von Na2Sn2Se5 Ein neues Chalkogenostannat(IV) mit schichtförmigen Komplexanionen

Preparation and Crystal Structure of Na₂Sn₂Se₅ A Novel Chalcogenostannate(IV) with Layered Complex Anions Na₂Sn₂Se₅ was obtained from a stoichiometric mixture of Na₂Se, Sn, and Se powders through a solid state reaction at 450 °C. It crystallizes orthorhombic, space group Pbca with a = 13.952(6) Å, b = 12.602(2) Å, c = 11.524(2) Å; Z = 8 and undergoes peritectic decomposition at 471(2) °C. The crystal structure was determined at ambient temperature from diffractometer data (MoKα‐radiation) and refined to a conventional R of 0.040 (1490 F_o's, 83 variables). Na₂Sn₂Se₅ is characterized by layered complex anions running parallel to (100) which are built up by SnSe₄ tetrahedra sharing common corners. The mean Sn–Se bond length calculates as 2.252(2) Å. The Na⁺ cations are coordinated to 6 or 7 Se in irregular configurations. The crystal structure can be described as a stacking of distorted c. p. 3⁶ chalcogen layers and mixed square 4⁴ alkali‐chalcogen layers.     

Synthesis and Characterization of an Inorganic‐Organic Hybrid Layered Zinc Phosphite [(C2H3N3)Zn(HPO3)]

A inorganic‐organic hybrid zinc phosphite (C₂H₃N₃)Zn(HPO₃) ( 1 ) has been prepared under solvothermal conditions in the presence of 1,2,4‐triazole (trz) ligand.Its structure was determined by single‐crystal X‐ray diffraction, and further characterized by powder X‐ray diffraction (XRD), FTIR spectroscopy, elemental analysis, ICP analysis, thermogravimetric analysis and fluorescent spectrum. It crystallizes in the monoclinic system, space group P2₁/n, a = 7.5515(6) Å, b = 9.1813(8) Å, c = 10.0125(8) Å, β = 111.267(1)°, V = 646.92(9) ų, Z = 4. The structure consists of left‐handed and right‐handed helical chains that are connected through bridging oxygen atoms to form a two‐dimensional layer structure with 4.8‐net. The compound exhibits intense photoluminescence upon photo‐excitation at 326 nm.     

The Crystal Structure of InGaO3(ZnO)4: A Single Crystal X‐ray and Electron Diffraction Study

The crystal structure of the mixed oxide InGaO₃(ZnO)₄ has been determined from electron diffraction and single‐crystal X‐ray diffraction data. The compound crystallises in a hexagonal space group (P6₃/mmc; No. 194), deduced from convergent beam electron diffraction (CBED). Single crystals of InGaO₃(ZnO)₄ were grown from a K₂MoO₄ flux in sealed platinum tubes. Single crystal structure refinement from XRD data [a = 3.2850(2) Å; c = 32.906(3) Å; Z = 2; 4232 data, R₁ = 0.0685] reveals a compound with oxygen anions forming a closest‐packed arrangement. Within this packing In³⁺ cations occupy octahedral interstices, forming layers of edge sharing octahedra. In between these layers are regions with composition [Zn₄GaO₅]⁺ forming a wurtzite type of structure. Inversions of the ZnO₄ tetrahedra occurs (i) at the InO₆ octahedral layer and (ii) halfway in the wurtzite type region, where the inversion boundary is built by Ga³⁺ in trigonal bipyramidal coordination with a long Ga–O_apical distance of 2.19(1) Å. The site occupation of Zn²⁺ and Ga³⁺, respectively, was confirmed by bond valence sum calculations. The compounds described here have the same structural charactistics as other known members with general formula ARO₃(ZnO)_m with m = integer.     

Syntheses and Crystal Structures of Two Sodium Ruthenates: Na2RuO4 and Na2RuO3

Na₂RuO₄, prepared from Na₂O₂ and RuO₂ via high oxygen pressure synthesis, crystallises monoclinic in space group P2₁/c (a = 10.721(6), b = 7.033(4), c = 10.871(6) Å, β = 119.10(4)°, Z = 8, 2503 unique reflections, R₁ = 0.049). Structure determination from single crystal data shows that the compound consists of infinite chains of RuO₅ trigonal bipyramids connected through their axial vertices. The Na cations connect the pseudohexagonally packed equation/tex2gif-stack-1.gif[RuO₃O_2/2] chains and are coordinated by six or seven oxygen atoms, respectively. The compound exhibits an one‐dimensional spin system with μ = 2.80 μ_B and Θ = —222 K and a three‐dimensional antiferromagnetic ordering below 50 K. Na₂RuO₃ was obtained from Na₂RuO₄ at 850 °C under a flow of argon. The structure was determined from X‐ray powder diffraction. It is closely related to the α‐NaFeO₂ and the Li₂SnO₃ structure types, layered variants of the NaCl type. In Na₂RuO₃ the Na and Ru atoms are partially disordered. This partially disordered state was approximated by a Rietveld refinement of two superimposed structural models (model I: R 3¯ m, a = 3.12360(5), c = 16.0370(4) Å, Z = 2; model II: C2/c, a = 5.4141(4), b = 9.3663(6), c = 10.8481(4) Å, β = 99.636(9)°, Z = 8).     

Kristallzucht und Strukturverfeinerung von Quecksilber(II)‐amidchlorid – HgClNH2

Crystal Growth and Refinement of the Crystal Structure of Mercury(II) Amide Chloride – HgClNH₂ Single crystals were prepared by recrystallization of HgClNH₂ from aqueous NH₃/NH₄⁺ solution at 160 °C. They were used for a single‐crystal X‐ray structure redetermination. The previously reported [W. N. Lipscomb, Acta. Crystallogr. 1951 , 4, 266.] structural topology determined on basis of X‐ray powder diffraction data is now confirmed. However, a higher symmetry is found: Space group type Pmma (instead of Pmm2), a = 6.709(1) Å, b = 4.351(1) Å, c = 5.154(1) Å, Z = 2. The crystal structure contains zig‐zag‐chains [Hg(NH₂)_2/2]⁺. Four Cl atoms complete the coordination sphere of Hg to a distorted octahedron. These share common faces and edges in layers [HgCl_4/4(NH₂)_2/2]. These layers are connected via hydrogen bonds N–H…Cl.     

Crystal Structure of Tetra- and Pentasodium Salts of Nitrilotris(methylenephosphonic Acid)

Tetra- and pentasodium salts of nitrilotris(methylenephosphonic acid) N(CH₂PO₃)₃H₆ (NTP) have been studied by single-crystal X-ray diffraction and spectroscopy. [Na₈(H₂O)₁₂{NH(CH₂PO₃)₃H}₂] · H₂O crystallizes in triclinic system, space group P1?, Z = 1, a = 7.1515(2) Å, b = 11.1590(3) Å, c = 12.0583(3) Å; α = 92.077(2)°, β = 106.145(2)°, γ = 5.628(2)°, CCDC No. 1432091. The crystal structure comprises two-dimensional layers lying along planes (011?), where dimeric molecules are linked by bridges each comprising four Na hydration octahedra. The [Na₅(H₂O)₁₁{NH(CH₂PO₃)₃}] · 2H₂O crystals are monoclinic, space group P2₁/n, Z = 4, a = 6.3024(2) Å, b = 21.5639(7) Å, c = 18.1608(6) Å; β = 91.261(3)°, CCDC No. 1497161. The crystal packing comprises alternating layers in planes [020] made of two-dimensional nets of Na hydration polyhedra, and columns of Na hydration octahedra lying in planes [040], with acid moieties in between.     

The Sodium (Iso)Cyanurates Nax[H3–xC3N3O3]·yH2O (x = 1–3, y = 0, 1): A Key‐Series for Understanding the Crystal Chemistry of Metal (Iso)Cyanurates

The (iso)cyanurates Na[H₂C₃N₃O₃] · H₂O, Na₂[HC₃N₃O₃] · H₂O, Na₂[HC₃N₃O₃], and Na₃[C₃N₃O₃] were synthesized phase pure from Na₂CO₃ · 10H₂O, NaOH, and cyanuric acid, respectively, in aqueous solution by carefully adjusting the crystallization conditions. The crystal structures of all compounds were determined by single‐crystal X‐ray diffraction {Na₂[HC₃N₃O₃] · H₂O: P1 , a = 3.51660(10) Å, b = 7.8300(3) Å, c = 11.3966(4) Å, α = 86.4400(10)°, β = 85.5350(10)°, γ = 85.0720(10)°, Z = 2, R₁ = 0.030, wR₂ = 0.078; Na₂[HC₃N₃O₃]: Pnma, a = 6.3409(6) Å, b = 12.2382(13) Å, c = 6.5919(7) Å, Z = 4, R₁ = 0.045, wR₂ = 0.079; Na₃[C₃N₃O₃]: R3 c, a = 11.7459(3) Å, c = 6.5286(3) Å, Z = 3, R₁ = 0.039, wR₂ = 0.066}. The structures show ribbons (Na[H₂C₃N₃O₃] · H₂O), dimers (Na₂[HC₃N₃O₃] · H₂O), chains (Na₂[HC₃N₃O₃]), or columns (Na₃[C₃N₃O₃]) of hydrogen‐bonded and parallel stacked (iso)cyanurate anions. These motifs are shown to be characteristic for certain degrees of protonation and hydration, and all (iso)cyanurate crystal structures found so far were classified accordingly. X‐ray powder patterns, thermogravimetry curves, IR and UV/Vis spectra were measured for all compounds.     

Structural Investigations and Thermal Behaviour of Mercury(II) Sulfito Complexes

The crystal structures of (NH₄)[HgSO₃Cl] ( 1 ) and of (NH₄)₂[Hg(SO₃)₂] ( 2 ) were determined from single crystal diffractometer data sets. 1 : 22 °C, Pnma, Z = 4, a = 15.430(3), b = 5.525(1), c = 6.679(1) Å, R(F) = 0.0256, R_w(F²) = 0.0642 (all 1056 unique reflections). 2 : ?108 °C, P2₁2₁2₁, Z = 4, a = 6.2240(4), b = 9.3908(6), c = 13.6110(8) Å, R(F) = 0.0179, R_w(F²) = 0.0493 (all 2699 unique reflections). The structure of 1 contains bent Cl‐Hg‐SO₃ entities (site symmetry m; d(Hg‐Cl) = 2.3403(13) Å, d(Hg‐S) = 2.3636(12) Å, ∠(Cl‐Hg‐S) = 164.51(5)°, d(S‐O) 2×1.458(3) Å, 1.468(4) Å, = 1.461Å) linked to undulated ribbons parallel to the b ‐axis by intermolecular secondary bonds SO···Hg (d(O···Hg) = 2×2.595(3) Å). These ribbons in turn aggregate to layers around the bc ‐plane. The layers are stacked along the a ‐axis with interlayer distances of a /2. The structure of 2 is made up of O₃S‐Hg‐SO₃ moieties (d(Hg‐S) = 2.3935(7), 2.3935(8) Å; ∠(Hg‐S‐Hg) = 174.41(3)°; = 1.474Å), that are linked to ribbons parallel to the a axis by coordination of Hg to three remote O atoms (2.801(4) < d(Hg‐O) < 2.844(3) Å). Adjacent ribbons are joined together by an additional Hg‐O contact of 2.733(3) Å, leading to a three‐dimensional anionic framework. Both crystal structures are stabilised by disordered NH₄⁺ cations, placed between the anionic layers or in the vacancies of the framework, via moderate hydrogen bonding interactions N‐H···O with donor‐acceptor distances ranging from 2.8 to 3.2Å. 1 and 2 were further characterised by thermal analysis (TG, DSC). They start to decompose at temperatures above 130 °C.     

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.     

Synthesis,Structure, and Properties of Nonlinear Optical Crystal Na2SiF6

Nonlinear optical crystals of fluosilicate Na₂SiF₆ are synthesized via hydrothermal method and its structure is determined by single‐crystal X‐ray diffraction (XRD). The space group of Na₂SiF₆ is P321 with cell parameters a = 8.8715(3) Å, c = 5.0484(5) Å, Z = 3, V = 344.09(4) ų. The properties of the crystal are measured by powder XRD, infrared (IR) spectroscopy, ultraviolet/visible (UV/Vis) near‐infrared (NIR) diffuse reflectance spectroscopy, thermogravimetric (TG), and differential scanning calorimetry (DSC) analysis. The bandgap calculated using CASTEP is 7.41 eV, indicating that the cut‐off edge of the Na₂SiF₆ crystal can be down to deep‐UV energy region. The first‐principles studies were performed to elucidate the structure/property relationship of Na₂SiF₆.     

A Novel Dinuclear Copper(II) Complex Molecule: Synthesis and Crystal Structure of Cu2(phen)2(H2O)2(C5H6O4)2 with phen = 1,10‐phenanthroline

Blue crystals of Cu₂(phen)₂(H₂O)₂(C₅H₆O₄)₂ were obtained from a CH₃OH–H₂O solution containing CuCl₂, 1,10‐phenanthroline (phen), glutaric acid and Na₂CO₃. The crystal structure (monoclinic, P2₁/c (no. 14), a = 10.271(1), b = 10.595(1), c = 15.585(1) Å, β = 107.105(3)°, Z = 2, R = 0.0328, wR² = 0.1027 for 3376 observed reflections (F ≥ 2σ(F ) out of 3728 unique reflections) is built up of dinuclear Cu₂(phen)₂(H₂O)₂(C₅H₆O₄)₂ complex molecules centered at inversion centers. The Cu atoms are square‐pyramidally coordinated by two nitrogen atoms of one bidentate chelating phen ligand and three oxygen atoms from two bridging glutarate anions and one axial water molecule (d(Cu–N) = 2.018(2), 2.024(2) Å; basal d(Cu–O) = 1.949(2), 1.956(2) Å; axial d(Cu–O) = 2.382(2) Å). Through the π‐π stacking interactions extending in a direction, the complex molecules are interlinked into 2 D layers parallel to the ac plane. The resultant 2 D layers are held together by hydrogen bonds between water molecules and uncoordinated carboxyl oxygen atoms.     

Synthesis and Characterization of a New Layered Zinc Phosphite (NH4)[{Zn(H2O)4}0.5Zn2(HPO3)3]

A new layered zinc phosphite with the formula (NH₄)[{Zn(H₂O)₄}_0.5Zn₂(HPO₃)₃] has been synthesized under hydrothermal conditions. Its structure was determined by single‐crystal X‐ray diffraction. The compound crystallizes in the triclinic system, space group (No. 2), a = 7.2507(4), b = 9.7982(6), c = 10.2642(6) Å, α = 63.425(2), β = 87.165(2), γ = 72.999(3)°, V = 620.84(6) ų, Z = 2. The connectivity of ZnO₄ tetrahedra, HPO₃ pseudo pyramids and ZnO₂(H₂O)₄ octahedra results in macroanionic layers with 4.8 net.