Melemium Hydrogensulfate H3C6N7(NH2)3(HSO4)3 – the First Triple Protonation of Melem

We synthesized melemium hydrogensulfate H₃C₆N₇(NH₂)₃(HSO₄)₃ by reaction of melem with 70 % sulfuric acid. The crystal structure was elucidated by single‐crystal XRD (P2₁/n (no. 14), Z = 4, a = 10.277(2), b = 14.921(3), c = 11.771(2) Å, β = 99.24(3)°, V = 1781.5(6) Å³). H₃C₆N₇(NH₂)₃(HSO₄)₃ is the first compound displaying a triple protonation of melem., In this contribution an overview of accessible melemium sulfates depending on the concentration of sulfuric acid is given. Two additional melemium sulfates were identified this way.     

Zur Kenntnis der Kristallstruktur von Melem C6N7(NH2)3

On the Crystal Structure of Melem C₆N₇(NH₂)₃ Single crystals of melem ( 1 ) were grown from both DMSO‐solutions and the gas phase. The structure of melem ( 1 ) was solved by single‐crystal X‐ray diffraction (P2₁/c, Z = 4, a = 741.66(15), b = 862.28(17), c = 1335.9(3) pm, β = 99.91(3)° R1 = 0.037 for 1098 reflections). The structure determination by X‐ray powder diffraction, which has been previously conducted, is in agreement with our data. The increased quality of the structural information allows for a more detailed understanding of the hydrogen bonding network.     

Kristallstruktur von Natrium‐Dihydrogencyamelurat‐Tetrahydrat Na[H2(C6N7)O3] · 4 H2O

Crystal Structure of Sodium Dihydrogencyamelurate Tetrahydrate Na[H₂(C₆N₇)O₃] · 4 H₂O Sodium dihydrogencyamelurate‐tetrahydrate Na[H₂(C₆N₇)O₃]·4 H₂O was obtained by neutralisation of an aqueous solution, previously prepared by hydrolysis of the polymer melon with sodium hydroxide. The crystal structure was solved by single‐crystal X‐ray diffraction ( a = 6.6345(13), b = 8.7107(17), c = 11.632(2) Å, α = 68.96(3), β = 87.57(3), γ = 68.24(3)°, V = 579.5(2) ų, Z = 2, R1 = 0.0535, 2095 observed reflections, 230 parameters). Both hydrogen atoms of the dihydrogencyamelurate anion are directly bound to nitrogen atoms of the cyameluric nucleus, thus proving the preference of the keto‐tautomere in salts of cyameluric acid in the solid‐state. The compound forms a layer‐like structure with an extensive hydrogen bonding network.     

First Characterization of an Extended Ammonium‐Ammonia Complex [{NH4(NH3)4}+(μ‐NH3)2] in the Crystal Structure of [NH4(NH3)4][Co(C2B9H11)2] · 2 NH3

The compound [NH₄(NH₃)₄][Co(C₂B₉H₁₁)₂] · 2 NH₃ ( 1 ) was prepared by the reaction of Na[Co(C₂B₉H₁₁)₂] with a proton‐charged ion‐exchange resin in liquid ammonia. The ammoniate 1 was characterized by low temperature single‐crystal X‐ray structure analysis. The anionic part of the structure consists of [Co(C₂B₉H₁₁)₂]^‐ complexes, which are connected via C‐H···H‐B dihydrogen bonds. Furthermore, 1 contains an infinite equation/tex2gif-stack-2.gif[{NH₄(NH₃)₄}⁺(μ‐NH₃)₂] cationic chain, which is formed by [NH₄(NH₃)₄]⁺ ions linked by two ammonia molecules. The N‐H···N hydrogen bonds range from 1.92 to 2.71Å (DHA = Donor···Acceptor angles: 136‐176°). Additional N‐H···H‐B dihydrogen bonds are observed (H···H: 2.3‐2.4Å).     

Protonated Melonate Ca[HC6N7(NCN)3]·7H2O – Synthesis,Crystal Structure,and Thermal Properties

Calcium hydrogenmelonate heptahydrate Ca[HC₆N₇(NCN)₃] · 7H₂O was obtained by metathesis reaction in aqueous solution. The structure of the molecular salt was elucidated by single‐crystal X‐ray diffraction. The crystal structure consists of alternating layers of planar monopronated melonate ions, Ca²⁺ and crystal water molecules. The anions of adjacent layers are staggered so that no π–π stacking occurs. The melonate entities are interconnected by hydrogen bonds within and between the layers. Ca[HC₆N₇(NCN)₃] · 7H₂O was investigated by solid‐state NMR and FTIR spectroscopy, TG and DTA measurements.     

Hexamincyclotriphosphazenhemiammoniakat,P3N3(NH2)6 · 0,5 NH3, ein Produkt der Hochdruckammonolyse von weißem Phosphor

Hexaminecyclotriphosphazenehemiammoniate, P₃N₃(NH₂)₆ · 0.5 NH₃, a Product of High Pressure Ammonolysis of White Phosphorus White phosphorus gives at NH₃-pressures ≥5 kbar and temperatures above 250°C in a disproportionation reaction P₃N₃(NH₂)₆ · 0.5 NH₃; besides these products red phosphorus is formed. The yield on P₃N₃(NH₂)₆ · 0.5 NH₃ increases with T and is about 70–80% at 400°C as to the disproportionation reaction of the amount of white phosphorus. X-ray structure determination was successful on single crystals of P₃N₃(NH₂)₆ · 0.5 NH₃. Pbca, N = 8 a = 11.395(3) Å, b = 12.935(4) Å, c = 12.834(4) Å R = 0.035, R_w = 0.041 with w = 1, N (F_o²) ≥ 3σ(F_o²) = 1371, N(Var.) = 166. The molecules are connected by N? H? N-bridgebonds with 3.04 Å ≤ d(N …? N) ≤ 3,19 Å and d (N? H) = 0.87 Å. The compound is furthermore characterized by IR-data and its thermical behaviour.     

Tris(1,10‐phenanthroline‐κ2N,N′)cadmium(II) bis(perchlorate) 3.5‐hydrate: a water chain stabilized by perchlorate anions

The title compound, [Cd(C₁₂H₈N₂)₃](ClO₄)₂·3.5H₂O, contains a cross‐shaped one‐dimensional channel along the c axis which encapsulates an ordered water chain. This water chain features a centrosymmetric cyclic water hexamer unit with a chair‐like conformation. Neighbouring hexamers are linked by bridging water molecules. The host perchlorate anions recognize and stabilize the guest water chain via three kinds of hydrogen‐bond patterns, leading to the formation of a complex one‐dimensional {[(H₂O)₇(ClO₄)₄]⁴⁻}_n anionic chain. One perchlorate acts as a single hydrogen‐bond acceptor dangling on the chain, the second perchlorate on the chain serves as a double hydrogen‐bond acceptor for only one water molecule to form an R₂²(6) ring, where both entities lie on a twofold axis, while the third perchlorate, which also lies on a twofold axis, accepts two hydrogen bonds from two equivalent water molecules and is involved in the construction of an R₆⁵(14) ring.     

Syntheses,Structures and Magnetic Properties of Two Mixed‐Valent Disc‐like Hepta‐nuclear Compounds of [FeIIFeIII6(tea)6](ClO4)2 and [MnII3MnIII4(nmdea)6(N3)6]·CH3OH (tea = N(CH2CH2O)33−, nmdea = CH3N(CH2CH2O)22−)

Two mixed‐valent disc‐like hepta‐nuclear compounds of [Fe^IIFe^III₆(tea)₆](ClO₄)₂ ( 1Fe , tea = N(CH₂CH₂O)₃^3?) and [Mn^II₃Mn^III₄(nmdea)₆(N₃)₆]·CH₃OH ( 2Mn , nmdea = CH₃N(CH₂CH₂O)₂^2?) have been synthesized by the reaction of Fe(ClO₄)₂·6H₂O with triethanolamine (H₃tea) for the former and reaction of Mn(ClO₄)₂·6H₂O with diethanolamine (H₂nmdea) and NaN₃ for the later, respectively. 1Fe has the cationic cluster with a planar [Fe^IIFe^III₆] core consisting of one central Fe^II and six rim Fe^III atoms in hexagonal arrangement. The Fe ions are linked by the oxo‐bridges from the alcohol arms in the manner of edge‐sharing of their coordination octahedra. 2Mn is a neutral cluster with a [Mn^II₃Mn^III₄] core possessing one central Mn^II atom surrounded by six rim Mn ions, two Mn^II and four Mn^III. The structure is similar to 1Fe but involves six terminal azido ligands, each coordinate one rim Mn ion. 1Fe showed dominant antiferromagnetic interaction within the cluster and long‐range ordering at 2.7 K. The cluster probably has a ground state of low spin of S = 5/2 or 4/2. The long‐range ordering is weak ferromagnetic, showing small hysteresis with a remnant magnetization of 0.3 Nβ and a coercive field of 40 Oe. Moreover, the isofield of lines 1Fe are far from superposition, indicating the presence of significant zero–field splitting. Ferromagnetic interactions are dominant in 2Mn . An intermediate spin ground state 25/2 is observed at low field. In high field of 50 kOe, the energetically lowest state is given by the m_s = 31/2 component of the S = 31/2 multiplet due to the Zeeman effect. Despite of the large ground state, no single‐molecule magnet behavior was found above 2 K.     

The Crystal Structures of Two No–Metal Tricyanomelaminates: Diammonium Tricyanomelaminate Dihydrate [NH4]2[C6N9H] · 2 H2O and Dimelaminium Tricyanomelaminate Melamine Dihydrate [C3N6H7]2[C6N9H] · C3N6H6 · 2 H2O

Diammonium tricyanomelaminate dihydrate [NH₄]₂[C₆N₉H] · 2 H₂O ( 1 ) and dimelaminium tricyanomelaminate melamine dihydrate [C₃N₆H₇]₂[C₆N₉H] · C₃N₆H₆ · 2 H₂O ( 2 ) were obtained by metathesis reactions from Na₃[C₆N₉] in aqueous solution and characterized by single‐crystal X‐ray diffraction and ¹⁵N solid‐state NMR spectroscopy ( 1 ). Both salts contain mono‐protonated tricyanomelaminate (TCM) anions and crystallize as dihydrates. Considering charge balance requirements, the crystal structure of 1 (C2/c, a = 3181.8(6) pm, b = 360.01(7) pm, c = 2190.4(4) pm, β = 112.39(3)°, V = 2319.9(8) 10⁶ · pm³) can best be described by assuming a random distribution of an ammonium ion – crystal water pair over two energetically similar sites. Apart from two melaminium cations, 2 (P2₁/c, a = 674.7(5) pm, b = 1123.6(5) pm, c = 3400.2(5) pm, β = 95.398(5), V = 2566(2) 10⁶ · pm³) contains one neutral melamine per formula unit acting as an additional “solvent” molecule and yielding a donor‐acceptor type of π–stacking interaction.     

Darstellung und Kristallstruktur von Diamminmagnesiumdiazid Mg(NH3)2(N3)2

Preparation and Crystal Structure of Diammin Magnesium Diazide Mg(NH₃)₂(N₃)₂ Diammin magnesium diazide was synthesized from Mg₃N₂ and NH₄N₃ in liquid ammonia and crystallized at 150 °C under autogenous atmosphere of HN₃ and NH₃ using sealed ampoules. Mg(NH₃)₂(N₃)₂ is a colorless, microcrystalline powder which can detonate above 180 °C. Caution, preparation and manipulation of Mg(NH₃)₂(N₃)₂ is very dangerous! The crystal structure was solved from powder data using the Patterson method and a Rietveld refinement was performed (Mg(NH₃)₂(N₃)₂, I 4/m, no. 87; a = 6.3519(1), c = 7.9176(2) Å; Z = 2, R(F²)= 0.1162). The crystal structure of Mg(NH₃)₂(N₃)₂ is related to that of SnF₄. It consists of planes built up from corner sharing Mg(NH₃)₂(N₃)₄ octahedra connected equatorially over their four azide bridges with the ammonia ligands being in trans position. IR data were collected and interpreted in accordance with the structural data.     

Synthesis and Structure of a One‐Dimensional Aluminum Phosphate, [NH3(CH2)2NH2(CH2)3NH3]3+ [Al(PO4)2]3—

A one‐dimensional aluminum phosphate, [NH₃(CH₂)₂NH₂(CH₂)₃NH₃]³⁺ [Al(PO₄)₂]^3—, has been synthesized hydrothermally in the presence of N‐(2‐Aminoethyl‐)1, 3‐diaminopropane (AEDAP) and its structure determined by single crystal X‐ray diffraction. Crystal data: space group = Pbca (no. 61), a = 16.850(2), b = 8.832(1), c = 17.688(4)Å, V = 2632.4(2)ų, Z = 8, R₁ = 0.0389 [5663 observed reflections with I > 2σ(I)]. The structure consists of anionic [Al(PO₄)₂]^3— chains built up from AlO₄ and PO₄ tetrahedra, in which all the AlO₄ vertices are shared and each PO₄ tetrahedron possesses two terminal P=O linkages. The cations, which balances the negative charge of the chains, are located in between the chains and interact with the oxygen atoms through strong N—H···O hydrogen bonds. Additional characterization of the compound by powder XRD and MAS‐NMR has also been performed and described.     

Complexation of the 2, 4, 6‐Triallyloxy‐1, 3, 5‐triazine with Copper(I,II) Chlorides. Syntheses and Crystal Structures of [CuCl2·2C3N3(OC3H5)3], [Cu7Cl8·2C3N3(OC3H5)3], and [Cu8Cl8·2C3N3(OC3H5)3]·2C2H5OH

Interaction of copper(II) chloride with 2, 4, 6‐triallyloxy‐1, 3, 5‐triazine leads to formation of copper(II) complex [CuCl₂·2C₃N₃(OC₃H₅)₃] ( I ). Electrochemical reduction of I produces the mixed‐valence Cu^{I, II} π, σ‐complex of [Cu₇Cl₈·2C₃N₃(OC₃H₅)₃] ( II ). Final reduction produces [Cu₈Cl₈·2C₃N₃(OC₃H₅)₃]·2C₂H₅OH copper(I) π‐complex ( III ). Low‐temperature X‐ray structure investigation of all three compounds has been performed: I : space group P1¯, a = 8.9565(6), b = 9.0114(6), c = 9.7291(7) Å, α = 64.873(7), β = 80.661(6), γ = 89.131(6)°, V = 700.2(2) ų, Z = 1, R = 0.0302 for 2893 reflections. II : space group P1¯, a = 11.698(2), b = 11.162(1), c = 8.106(1) Å, α = 93.635(9), β = 84.24(1), γ = 89.395(8)°, V = 962.0(5) ų, Z = 1, R = 0.0465 for 6111 reflections. III : space group P1¯, a = 8.7853(9), b = 10.3602(9), c = 12.851(1) Å, α = 99.351(8), β = 105.516(9), γ = 89.395(8), V = 1111.4(4) ų, Z = 1, R = 0.0454 for 4470 reflections. Structure of I contains isolated [CuCl₂·2C₃N₃(OC₃H₅)₃] units. The isolated fragment of I fulfils in the structure of II bridging function connecting two hexagonal prismatic‐like cores Cu₆Cl₆, whereas isolated Cu₆Cl₆(CuCl)₂ prismatic derivative appears in III . Coordination behaviour of the 2, 4, 6‐triallyloxy‐1, 3, 5‐triazine moiety is different in all the compounds. In I ligand moiety binds to the only copper(II) atom through the nitrogen atom of the triazine ring. In II ligand is coordinated to the Cu^II‐atom through the N atom and to two Cu^I ones through the two allylic groups. In III all allylic groups and nitrogen atom are coordinated by four metal centers. The presence of three allyl arms promotes an acting in II and III structures the bridging function of the ligand moiety. On the other hand, space separation of allyl groups enables a formation of large complicated inorganic clusters.     

Synthesis and Structure of the First Three‐legged Low‐dimensional Iron Phosphate, [H3N(CH2)3NH2(CH2)2NH2(CH2)3NH3][Fe3F6(HPO4)2(PO4)]·3H2O

A hydrothermal reaction of iron acetylacetonate, phosphoric acid, HF, N, N′‐bis(3‐aminopropyl)ethylenediamine and water at 150 °C gave rise to a new iron phosphate, [H₃N(CH₂)₃NH₂(CH₂)₂NH₂(CH₂)₃NH₃][Fe₃F₆(HPO₄)₂(PO₄)] · 3H₂O ( I ). The structure consists of Fe(1)O₄F₂, Fe(2)O₃F₃ octahedral and P(1)O₃(OH) and P(2)O₄ tetrahedral building units connected through their vertices to form fragments of tancoite‐type units. The tancoite‐type units are linked through the phosphate tetrahedra forming an unusual iron phosphate with a hitherto unknown low‐dimensional structure with three‐iron center.Magnetic studies indicate a complex behavior at low temperature and the high‐temperature data (150 — 300 K) has a Curie‐Weiss behavior. The calculated room temperature magnetic moment is 6 μ_B per Fe atom, and the Neel temperature, T_N = 46K. Crystal data: orthorhombic, space group = I2₁2₁2₁ (no. 24), a = 9.9042(11), b = 12.8865(14), c = 19.783(2)Å, U = 2524.9(5), Z = 4.     

Formation of a Hydrogen‐Bonded Heptazine Framework by Self‐Assembly of Melem into a Hexagonal Channel Structure

Self‐assembly of melem C₆N₇(NH₂)₃ in hot aqueous solution leads to the formation of hydrogen‐bonded, hexagonal rosettes of melem units surrounding infinite channels with a diameter of 8.9 Å. The channels are filled with strongly disordered water molecules, which are bound to the melem network through hydrogen bonds. Single‐crystals of melem hydrate C₆N₇(NH₂)₃ ? xH₂O (x≈2.3) were obtained by hydrothermal treatment of melem at 200 °C and the crystal structure (R $\bar 3$ c, a=2879.0(4), c=664.01(13) pm, V=4766.4(13)×10⁶ pm³, Z=18) was elucidated by single‐crystal X‐ray diffraction. With respect to the structural similarity to the well‐known adduct between melamine and cyanuric acid, the composition of the obtained product was further analyzed by solid‐state NMR spectroscopy. Hydrolysis of melem to cyameluric acid during syntheses at elevated temperatures could thus be ruled out. DTA/TG studies revealed that, during heating of melem hydrate, water molecules can be removed from the channels of the structure to a large extent. The solvent‐free framework is stable up to 430 °C without transforming into the denser structure of anhydrous melem. Dehydrated melem hydrate was further characterized by solid‐state NMR spectroscopy, powder X‐ray diffraction, and sorption measurements to investigate structural changes induced by the removal of water from the channels. During dehydration, the hexagonal, layered arrangement of melem units is maintained whereas the formation of additional hydrogen bonds between melem entities requires the stacking mode of hexagonal layers to be altered. It is assumed that layers are shifted perpendicular to the direction of the channels, thereby making them inaccessible for guest molecules.     

Darstellung und Strukturaufklärung von Ammonium‐tetraamminlithium‐amidotrithiophosphat‐Ammoniak(1/1) (NH4) [Li(NH3)4] [P(NH2)S3] · NH3

Synthesis and Crystal Structure of Ammonium Tetraamminelithium Amidotrithiophosphate‐Ammonia(1/1)(NH₄)[Li(NH₃)₄][P(NH₂)S₃]·NH₃ Colourless crystals of (NH₄)[Li(NH₃)₄][P(NH₂)S₃]·NH₃ were prepared by the reduction of P₄S₁₀ with a solution of lithium in liquid ammonia. The X‐ray structure determination shows them to contain the pseudo‐tetrahedral amidotrithiophosphate anion [P(NH₂)S₃]²⁻ (point group C_S), which is the hitherto unknown final member of a series of previously characterized amidothiophosphates. The ammonium ion and the ammonia molecule of solvation form an diamminehydrogen(1+)‐ion N₂H₇⁺ with a short, nearly linear hydrogen bond of 2.864(3) Å.     

Kristallstruktur von Hexamincyclotriphosphazen,P3N3(NH2)6

Crystal Structure of Hexamine Cyclotriphosphazene, P₃N₃(NH₂)₆ In the presence of KNH₂ hexamine cyclotriphosphazene semi ammoniate (molar ratio 12:1) in NH₃ gives crystals of solvent free P₃N₃(NH₂)₆ within 5 d at 130°C and p(NH₃) = 110 bar. The structure was solved by X-rax methods: P₃N₃(NH₂)₆: P2₁/c, Z = 4, a = 10.889(6) Å, b = 5.9531(6) Å, c = 13.744(8) Å, β = 97.83(3)°, Z(F_o) = 1 721 with (F_o)² ≥ 3σ(F_o)², Z(var.) = 157, R/R_w = 0,036/0,041 The structure contains columns of molecules P₃N₃(NH₂)₆ all in the same orientation. The six-membered rings within one molecule have boat conformation. The columns are stacked together in a way that one is surrounded by four others shifted by half a lattice constant in direction [010]. Strong hydrogen bridge-bonds N? H…?N connect molecules within the columns and between them.     

Synthese und Einkristallstrukturanalyse von [M(NH3)6]C60 · 6 NH3 (M = Co2+, Zn2+)

Synthesis and Single Crystal Structure Analysis of [M(NH₃)₆]C₆₀ · 6 NH₃ (M = Co²⁺, Zn²⁺) [M(NH₃)₆]C₆₀ · 6 NH₃ (M = Co²⁺, Zn²⁺) was synthesized from K₂C₆₀ by ion exchange in liquid ammonia. According to single crystal structure analyses the new fullerides are isostructural to the respective Mn, Ni and Cd compounds. The deformation patterns of the C₆₀^2– anions are similar within this group of compounds. However, there are no indications for significant deformations of the cages as a whole, which could be attributed to a Jahn‐Teller distortion.     

Supramolecular hydrogen‐bonding patterns in two cocrystals of the N(7)–H tautomeric form of N6‐benzoyladenine: N6‐benzoyladenine–3‐hydroxypyridinium‐2‐carboxylate (1/1) and N6‐benzoyladenine–DL‐tartaric acid (1/1)

Two novel cocrystals of the N(7)—H tautomeric form of N⁶‐benzoyladenine (BA), namely N⁶‐benzoyladenine–3‐hydroxypyridinium‐2‐carboxylate (3HPA) (1/1), C₁₂H₉N₅O·C₆H₅NO₃, (I), and N⁶‐benzoyladenine–DL‐tartaric acid (TA) (1/1), C₁₂H₉N₅O·C₄H₆O₆, (II), are reported. In both cocrystals, the N⁶‐benzoyladenine molecule exists as the N(7)—H tautomer, and this tautomeric form is stabilized by intramolecular N—H...O hydrogen bonding between the benzoyl C=O group and the N(7)—H hydrogen on the Hoogsteen site of the purine ring, forming an S(7) motif. The dihedral angle between the adenine and phenyl planes is 0.94 (8)° in (I) and 9.77 (8)° in (II). In (I), the Watson–Crick face of BA (N6—H and N1; purine numbering) interacts with the carboxylate and phenol groups of 3HPA through N—H...O and O—H...N hydrogen bonds, generating a ring‐motif heterosynthon [graph set R₂²(6)]. However, in (II), the Hoogsteen face of BA (benzoyl O atom and N7; purine numbering) interacts with TA (hydroxy and carbonyl O atoms) through N—H...O and O—H...O hydrogen bonds, generating a different heterosynthon [graph set R₂²(4)]. Both crystal structures are further stabilized by π–π stacking interactions.     

Melamine–Melem Adduct Phases: Investigating the Thermal Condensation of Melamine

By studying the thermal condensation of melamine, we have identified three solid molecular adducts consisting of melamine C₃N₃(NH₂)₃ and melem C₆N₇(NH₂)₃ in differing molar ratios. We solved the crystal structure of 2 C₃N₃(NH₂)₃?C₆N₇(NH₂)₃ ( 1 ; C2/c; a=21.526(4), b=12.595(3), c=6.8483(14) Å; β=94.80(3)°; Z=4; V=1850.2(7) ų), C₃N₃(NH₂)₃?C₆N₇(NH₂)₃ ( 2 ; Pcca; a=7.3280(2), b=7.4842(2), c=24.9167(8) Å; Z=4; V=1366.54(7) ų), and C₃N₃(NH₂)₃?3 C₆N₇(NH₂)₃ ( 3 ; C2/c; a=14.370(3), b=25.809(5), c=8.1560(16) Å; β=94.62(3)°; Z=4; V=3015.0(10) ų) by using single‐crystal XRD. All syntheses were carried out in sealed glass ampoules starting from melamine. By variation of the reaction conditions in terms of temperature, pressure, and the presence of ammonia‐binding metals (europium) we gained a detailed insight into the occurrence of the three adduct phases during the thermal condensation process of melamine leading to melem. A rational bulk synthesis allowed us to realize adduct phases as well as phase separation into melamine and melem under equilibrium conditions. A solid‐state NMR spectroscopic investigation of adduct 1 was conducted.     

Competitive Coordination of the Uranyl ion by Perchlorate and Water – The Crystal Structures of UO2(ClO4)2·3H2O and UO2(ClO4)2·5H2O and a Redetermination of UO2(ClO4)2·7H2O (Z. Anorg. Allg. Chem. 2003, 629, 1012–1016)

In the article “Competitive Coordination of the Uranyl ion by Perchlorate and Water – The Crystal Structures of UO₂(ClO₄)₂·3H₂O and UO₂(ClO₄)₂·5H₂O and a Redetermination of UO₂(ClO₄)₂·7H₂O” (Z. Anorg. Allg. Chem. 2003 , 629, 1012–1016), some wrong parameters and bond lengths for UO₂(ClO₄)₂·7H₂O were given in table 1 and table 3 The correct parameters are: a = 1449.5(2) pm, b = 921.6(1) pm, c = 1067.5(2) pm, V = 1422.5(4)·10⁶ pm³, ρ = 2.712 g·cm^?3, μ = 119 cm^?1. The corrected bond lengths for this structure are U–O(1) 175.8(5) pm, U–O(2) 239.1(5) pm, U–O(3) 240.8(5), U–O(4) 242.0(7). A cif file with the correct data has been deposited with the ICSD.