New boron-oxygen layer in the structure of barium hydrodecaborate Ba5[B20O33(OH)4] ⋅ H2O

The crystal structure of the new synthetic compound Ba₅[B₂₀O₃₃(OH)₄] ? H₂O was established by the methods of X-ray diffraction (a Stoe IPDS diffractometer, λMoK _α?, 1860 independent reflections, anisotropic refinement, R = 1.95%, localization of hydrogen atoms): a = 9.495(2) Å, b = 6.713(1) Å, c = 11.709(2) Å, β = 95.09(1)°, sp. gr. P2, Z = 1. The structure is based on double pseudohexagonal layers consisting of BO₄-tetrahedra and BO₃ triangles linked into three-membered rings in two mutually perpendicular directions. The double layers adjacent along the [100] direction are linked together through the Ba-polyhedra and hydrogen bonds with the participation of the OH-groups occupying the “end” vertices of two B-triangles. The interlayer space is also filled with a sheet of Ba-polyhedra. The structure of the compound is compared to the structures of topologically similar Ba and Ca borates and hydroborates.     

Crystal and molecular structure of complex compound [Fe3O(CH3COO)6(H2O)3]2[ZnCl4] ⋅ 2H2O

The X-ray crystal structure of trinuclear iron acetate [Fe₃O(CH₃COO)₆(H₂O)₃]₂ [ZnCl₄] ? 2H₂O was determined. The crystal has a ionic structure. It is monoclinic, a = 25.363(7), b = 14.533(4), c = 15.692(4) Å, β = 103.11(2)°, space group _C2/c, and R = 0.0685. The structure of the cationic complex [Fe₃O(CH₃COO)₆(H₂O)₃]⁺ is typical of trinuclear iron(III) compounds containing a μ₃-O bridge: the iron atoms are situated at the vertices of an almost equilateral triangle with the O atom at the center. Each Fe atom is coordinated by four O atoms of bridging carboxy groups, the μ₃-bridging O atom, and the water molecule in the trans position to the latter O atom. Mössbauer spectroscopy evidence indicates the high-spin state (_S = 5/2) of the iron(III) ions.     

Self-assemblies of Ni(II) with phenanthroline and maleate anions: [Ni(H2O)3(phen)L] ⋅ H2O (1) and [Ni(H2O)2(phen)L] ⋅ 2H2O (2) with H2L = maleic acid

The complex [Ni(H₂O)₃(phen)(C₄H₂O₄)] H₂O (1), which was obtained by reaction of phenanthroline, Ni(NO₃)₂ 6H₂O, and maleic acid in CH₃OH/H₂O at pH = 7.05, crystallized in the monoclinic space group P2₁ (no. 4) with cell dimensions: a = 9.350(1) Å, b = 7.631(1) Å, c = 12.821(1) Å, = 106.25(1), and D _calc = 1.607 g/cm³ for Z = 2. The Ni atoms are each octahe drally coordinated by one chelating phen ligand, three H₂O molecules and one monodentate maleato ligand to form [Ni(H₂O)₃(phen)(C₄H₂O₄)] complex molecules with d(Ni–O) = 2.038–2.090 Å, d(Ni–N) = 2.066, 2.089 Å. The formed complex molecules are, via the intermolecular hydrogen bonds, assembled into columnar 1D chains. Interdigitation of the chelating phen ligands of the neighboring chains leads to 2D layers and the crystal H₂O molecules are hydrogen bonded to the oxygen atoms of the maleate not coordinated to the Ni atom. However, reaction of NiCO₃, phen, and maleic acid in CH₃OH/H₂O at pH = 6.33 afforded [Ni(H₂O)₂(phen)(C₄H₂O₄)] 2H₂O (2), which crystallized in the triclinic space group (no. 2) with cell dimensions: a = 7.971(1) Å, b = 8.237(1) Å, c = 13.304(1) Å, = 81.005(6)°, = 87.877(8)°, = 78.322(8)°, and D _calc = 1.671 g/cm³ for Z = 2. The Ni atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of two H₂O molecules and two bis–monodentate maleato ligands with d(Ni–O) = 2.041–2.120 Å and d(Ni–N) = 2.095 Å. The Ni atoms are bridged by the maleato ligands to generate 1D ¹ [Ni(H₂O)₂(phen)(C₄H₂O₄)_2/2] chains along [100]. The supramolecular assemblies of the 1D chains via – stacking inter- actions result in thick 2D layers parallel to (001), between which the noncoordinating H₂O molecules are sandwiched. The paramagnetic [Ni(H₂O)₂(phen)(C₄H₂O₄)_2/2] 2H₂O (2) obeys the Curie–Weiss law _m(T-) = 1.139cm³ mol^–1 K with the Weiss constant = –0.95 K.     

Structures and properties of layered barium borates Ba0.975[B6O9(OH)(O0.975Br0.025) · B2O(OH)3], Ba2[B5O8(OH)2](OH), Na2Ba2[B20O34(OH)4], and Ba5[B20O33(OH)4]H2O

A new hexaborate, Ba_0.975[B₆O₉(OH)(O_0.975Br_0.025) · B₂O(OH)₃], was synthesized under hydrothermal conditions. This compound is structurally similar to tunnelite and the synthetic borates Pb[B₆O₁₀(OH) · B₂O(OH)₃], Pr[B₆O₁₀(OH) · B₂O(OH)₄], and Nd[B₆O₁₀ · B₃O₃(OH)₄] · H₂O studied earlier. In the new hexaborate and the refined pentaborate Ba₂[B₅O₈(OH)₂]OH, in which the polyanions adopt an orientation in layers unusual for pentaborates, thermal vibrations of the terminal groups were revealed. This fact reflects the real crystal structure. The nonlinear optical properties of the crystals of the polar pentaborate Na₄Ba₄[B₂₀O₃₄(OH)₄] were determined. The crystal structure of the related pentaborate Ba₅[B₂₀O₃₃(OH)₄]H₂O was considered. The factors most likely responsible for the difference in the second-harmonic generation signal for this pair were revealed.     

Structure of hexakis(imidazole)cadmium(II) carbonate trihydrate: [Cd(Im)6]CO3 ⋅ 3H2O

The crystal and molecular structure of the title compound [Cd(Im)₆]CO₃ 3H₂O, where Im = imidazole, has been determined by X-ray crystallography. The crystal structure consists of discrete Cd(Im)₆ ²⁺ cations, CO₃ ^2– anions and three uncoordinated water molecules. It crystallizes in the hexagonal system, space group P6₃/m, with lattice parameters a = 9.0552(l) Å, c = 21.745(l) Å, and Z = 2; The Cd(II) ion assumes centrosymmetric octahedron geometry. The bond distance of Cd–N is 2.361(l) Å. A three-dimensional intermolecular hydrogen bond network is formed between the free carbonate anions, the imidazole ligands, and the free water molecules.     

Geometrical model of the structure of the heterocomplex compound [Cr(OCN2H4)6]3+[Co(DH)2(NO2)2] 3 − ⋅ 2H2O

The structural organization of the new heterocomplex compound with carbamide has been considered on the basis of division of the crystal space into Dirichlet polyhedra of the system of Delone points (centers of the complex ions). It is demonstrated that the coordination numbers for all domains (Dirichlet domains) of the complex ions in the structure obey the “rule of fourteen,” whereas the polyhedra providing the structural organization of the crystal are distorted Fedorov cuboctahedra.     

Crystal structure of triaquamaleatostrontium(II) monohydrate, [Sr(C4H2O4)(OH2)3]·H2O

[Sr(C₄H₂O₄)(OH₂)₃]·H₂O is monoclinic, P2₁/n, witha=11.476(2),b=7.027(1),c=12.344(2) Å, =115.74(3)°,V=896.67 ų,Z=4. The Sr atom is surrounded by nine oxygen atoms which come from four different maleate anions and three water molecules. The Sr–O distances range from 2.546(2) to 2.808(2) Å. The C–O distances are equal within the standard deviation 1.263(3) to 1.258(3) Å). In the maleate anion, the planes that contain the carboxylate groups form an angle of 74.44(9)°. Both carboxylate groups deviate significantly from planarity. The different coordination modes of the carboxylate group and the extensive hydrogen bonding present are responsible for the polymeric nature of the structure.     

Crystal structure of aqua[S-prolinato-N-monoacetato)copper(II) dihydrate [Cu(Proma)H2O] ⋅ 2H2O

The crystal structure of [Cu(C₇H₉NO₄)H₂O] ? 2H₂O is determined by X-ray diffraction (λMo, R = 0.0316 for 857 reflections). The crystals are tetragonal, a = 8.219(1) Å, c = 17.449(3) Å, Z = 4, ρ_calcd = 1.627 g cm^?3, and space group P4₃. The coordination polyhedron of the Cu atom is a tetragonal pyramid with the O atom of the acetate arm of the prolinatomonoacetate ion (Proma) in the apical position [Cu-O 2.312(6) Å]. The O atom of the water molecule and the N and O atoms of the prolinate group of the Proma ligand lie in the basal plane. The Cu-N bond length is 2.044(6) Å, and the Cu-O bond lengths are 1.932(7) and 1.927(6) Å. The O atom of the acetate arm of the neighboring Proma ion completes the basal plane [Cu-O 1.951(6) Å], thus linking the copper complexes into infinite chains.     

New rubidium pentaborate Rb[B5O7(OH)2] · 0.5H2O with a 5: [4Δ + 1T] anionic block and its relation to larderellite (NH4)[B5O7(OH)2] · H2O on the basis of the OD theory

A new rubidium pentaborate is synthesized under hydrothermal conditions. Its crystal structure is studied by the heavy-atom method without any a priori knowledge of chemical formula. The chemical formula is Rb[B₅O₆(OH)₄] · 0.5H₂O, sp. gr. $\bar P1$ , lattice parameters a = 7.679(4) Å, b = 9.253(6) Å, c = 12.053(9) Å, α = 98.55(5)°, β = 106.80(5)°, γ = 91.71°, R = 0.0573, R _w = 0.0638, S = 1.07. The anionic part of the structure consists of a chain of fundamental building blocks 5:[4Δ + 1T] built by four B triangles bound to one B tetrahedron, which are common to Na, K, Rb, and Cs pentaborates. This new pentaborate is closely related to the mineral larderellite (NH₄)[B₅O₆(OH)₄] · H₂O but possesses an original structure, which manifests itself in the different morphology of the new pentaborate and the absence of perfect cleavage. The Dornberger-Schiff OD theory allows one to describe in detail the structural relationships, predict possible hypothetical structures, and write the OD groupoid.     

Hydrothermal crystallization and X-ray structure determination of a new decavanadate with mixed cations [Mn(H2O)6]2[N(CH3)4]2[V10O28]·2H2O

A new decavanadate with mixed cations, [Mn(H₂O)₆]₂[N(CH₃)₄]₂[V₁₀O₂₈]·2H₂O (1), was crystallized from a hydrothermal reaction between MnCO₃ and V₂O₅ in the presence of N(CH₃)₄Br at 100°C. The structure of 1, as determined by x-ray single crystal analysis, consists of cations and anions of hexa-aqua manganese [Mn(H₂O)₆]²⁺, tetramethyl ammonium [N(CH₃)₄]⁺ and decavanadate [V₁₀O₂₈]^6–. The extended H-bonding between the [Mn(H₂O)₆]²⁺ and [V₁₀O₂₈]^6– ions gives rise to a pseudo- two-dimensional network in the crystal lattice x-ray crystallographic data for 1: monoclinic P2₁/n, a = 9.1499(5), b = 12.8725(7), c = 18.625(1) Å, = 92.252(1)°, V = 2192.0(2) ų, MZ = 2, and D _calcd = 2.22 g cm^–3.     

Crystal and molecular structure of [Cu2(3,5-dihydroxybenzoate)4 (acetonitrile)2] ⋅ 8H2O

The crystal and molecular structure of the title compound, [Cu₂(3,5-dihydroxybenzoate)₄ (acetonitrile)₂] 8H₂O 1, is reported. Crystal data for 1: tetragonal, space group I 4/m, a = 11.720(2) Å, c = 15.304(3) Å, V = 2102.4(6), and D _c = 1.53 g/cm³, for Z = 2. The metal and organic components crystallize to form a Cu paddle-wheel complex, of idealized D_4h symmetry, that assembles in the solid-state, along with eight equivalents of water, to form a 3D hydrogen-bonded network held together by O–H O hydrogens bonds. The metal complexes pack to form a 2D layered structure.     

Tiettaite K4Na12Fe3+Si16O41(OH)4 ⋅ 2H2O: A Mineral with a Novel Type of Microporous Heteropolyhedral Framework

Crystallography Reports - Microporous silicate tiettaite from the Khibiny alkaline massif (Kola Peninsula, Russia) has been studied using X-ray diffraction analysis, electron probe microanalysis,...     

Synthesis, Structure and Properties of (H2NCH2CH2NH3)3 {(VO)6 [B10O16 (OH)6]2} · 11H2O

Abstract A new polyoxovanadoborate cluster (H₂NCH₂CH₂NH₃)₃ {(VO)₆[B₁₀O₁₆(OH)₆]₂} · 11H₂O was prepared by hydrothermal technique and characterized by single crystal X-ray diffraction analysis, IR and TGA. The crystal of the new compound belongs to monoclinic system, space group C2/c with a = 20.198(1) ?, b = 13.4476(8) ?, c = 21.602(1) ?, β = 97.067(1)°, V = 5822.8(5) ?³, Z = 4, D _c = 1.956 g cm⁻³, M = 1714.4, μ = 1.066 mm⁻¹, S = 1.905, R = 0.059, R _w = 0.0966. Index Abstract A new polyoxovanadoborate cluster (H2NCH2CH2NH3)3{(VO)6 [B10O16(OH)6]2} · 11H2O was prepared by hydrothermal technique and characterized by single crystal X-ray diffraction analysis, IR and TGA.      

Refined crystal structure of lovozerite Na2CaZr[Si6O12(OH,O)6] · H2O

The structure of Na,Ca,Zr-silicate lovozerite, Na₂CaZr[Si₆O₁₂(OH,O)₆] · H₂O, from the Khibiny alkaline massif (the Kola Peninsula) was refined by single-crystal X-ray diffraction analysis (Syntex $P\bar 1$ diffractometer, λMoK _α radiation, 2θ/θ scanning technique). The refinement (R _hkl = 0.077, 1531 independent reflections; anisotropic thermal parameters) confirmed the trigonal system proposed for the mineral earlier (sp. gr. R3; a = 10.18(1) Å, c = 13.13(2) Å, Z = 3) and revealed the presence of two additional positions (C and B) statistically occupied by Ca and Na atoms (and partly by Mn) and H₂O molecules, respectively.     

Eightfold-coordinated diethylenetriaminepentaacetates: Crystal structures of K[M(Dtpa)] ⋅3H2O (M = Zr or Hf) and NH4[Sn(Dtpa)] ⋅ H2O

The crystal structures of K[M(Dtpa)] ? 3H₂O (M = Zr or Hf) and NH₄[Sn(Dtpa)] ? H₂O are studied by X-ray diffraction. The coordination number of the metal atom in all the compounds is eight. The NH₄[Sn(Dtpa)] ? H₂O complex is isostructural to the (H₅O₂)[M(Dtpa)] ? H₂O (M = Sn or Hf) compounds studied earlier.     

三维孔道结构钒磷酸盐[H3N(CH2)3NH3]2[H3N(CH2)3NH2][H2N(CH2)3NH2]-[V(H2O)2(VO)8(OH)4(PO4)4(HPO4)4]·4H2O的水热合成和结构表征

以1,3-丙二胺为模板,水热合成了三维孔道结构钒磷酸盐[H3N(CH2)3NH3]2[H3N(CH2)3NH2][H2N(CH2)3NH2][V(H2O)2(VO)8(OH)4(PO4)4(HPO4)4]·4H2O(DAP-V9P8).用单晶X射线衍射、红外光谱和热重法对该化合物的晶体结构进行了表征.DAP-V9P8的无机骨架由[VO5]、[VO6]、[PO4]和[HPO4]通过共顶点连接而成.孔道中充填的丙二胺分子随所处结晶学位置不同,有三种完全不同的分子构象.其中,位于//b轴直径达1.82nm椭圆形孔道中心的丙二胺分子碳链呈独特的直线状分布.晶体学参数:a=1.4820(9)nm,b=1.0255(4)nm,c=1.8181(9)nm,β=90.391(8)°;P21/n(No.14);R1=0.0772,wR2=0.2004(I＞(2σI)).与等结构的其它化合物进行了系统的结构比较.     

New layer megaborate Sm3[B13O22(OH)3](OH) · 3H2O and its place in the structural systematics

Crystals of a new aqueous rare earth borate Sm₃[B₁₃O₂₂(OH)₃](OH) · 3H₂O, space group P2/c, are obtained under hydrothermal conditions. The structure is determined by the heavy-atom method without preliminary knowledge of the chemical formula. The anionic radical is a boron-oxygen sheet in which two corrugated layers are related by centers of inversion. An independent layer is akin to pentaborate layers; it differs from the layer in (Nd_0.925Na_0.075)Nd[B₉O₁₅(OH)₂]Cl_0.85 · 2.65H₂O by an additional branch in the form of a 4: (3[2?? + 1T] + 1??) group. The intersheet space and large holes of the sheet accommodate Sm atoms, (OH) groups, and water molecules. The new Sm-borate and the related Nd-borate are polyborates (megaborates) with complex anionic radicals. In the Sm-borate, the new two-dimensional [B₁₃O₂₂(OH)₃]_??? complex anionic radical of the 13{(4: [2T + 2??])_?? + (5: [3T + 2??] + 4: (3[2?? + 1T] +1??))_??}_??? formula is built of three different blocks, unlike the [B₉O₁₅(OH)₂]_??? radical of the 9{(4: [2T + 2??])_?? + (5: [3T + 2??])_??}_??? formula in the Nd-borate, which consists of two blocks. The rule of the inverse relationship between the polymerization degrees of the boron-oxygen radical and rare earth polyhedra holds for both borates.     

Crystal structure of [Co(Ox)(NH3)4][Bi(Edta)] ⋅ 3H2O

The crystal structure of [Co(Ox)(NH₃)₄][Bi(Edta)] ? 3H₂O is determined. The crystals are monoclinic, a = 9.291 Å, b = 22.275 Å, c = 11.402 Å, β = 105.79°, V = 2270.7 ų, Z = 4, and space group P2₁/c. The [Bi(Edta)]^? anionic complexes are linked into polymeric chains through two Bi-O bonds with the neighboring complexes.     

A dinuclear cyanide-bridged complex, [(DMF)4(H2O)3LuCo(CN)6]·H2O

The crystal structure of the bimetallic cyanide bridged complex [(DMF)₄(H₂O)₃LuCo(CN)₆]·H₂O (1) was obtained by single-crystal X-ray diffraction. The central lutetium(III) ion is eight coordinate arranged in a square antiprism while the cobalt(III) ion is six coordinate, oriented octahedrally. Molecules in the crystal lattice are held together by a network of hydrogen bonding. Crystallization of 1 occurs in the centrosymmetric monoclinic space group P2₁/c (No. 14) with a = 13.875(2), b = 8.8352(9), c = 24.633(2) Å = 96.392(8)° and Z = 4.