A new hydrated ammonium hydroxy­borate, (NH4)2[B10O14(OH)4]·H2O

The structure of a new synthetic compound, di­ammonium tetra­hydroxy­deca­borate monohydrate, has been determined by single‐crystal X‐ray diffraction. It crystallizes in triclinic space group and all atoms occupy general sites. The title compound is composed of [B₁₀O₁₅(OH)₄]⁴⁻ ions as the fundamental building blocks, and these are linked end‐to‐end by sharing two common O atoms, thus producing infinite chains of composition [B₁₀O₁₄(OH)₄]_n^2n–. These chains are linked by hydrogen bonds, thus forming borate sheets. Water mol­ecules and ammonium ions between these sheets connect adjacent sheets via hydrogen bonds.     

Methyl 4‐amino‐2,3‐dihydro‐6‐methoxy‐1,3‐dioxo‐1H‐pyrrolo[3,4‐c]pyridine‐7‐carboxylate forms hydrogen‐bonded sheets built from R22(8) and R66(42) rings

In the title compound, C₁₀H₉N₃O₅, which was formed by the reaction of 6‐amino‐2‐methoxy‐4(3H)‐pyrimidinone with di­methyl acetyl­enedi­carboxyl­ate, the mol­ecules are linked by N—H?O hydrogen bonds [N?O 2.8974 (15) and 3.0300 (15) Å, and N—H?O 165 and 174°] into planar sheets built from alternating R₂²(8) and R₆⁶(42) rings.     

A `tetrameric' 3,4‐di‐p‐tolyl‐1,2,5‐oxadiborole derivative

In the title compound, 1,1,6a,7,9a,10‐hexa­chloro‐2,3,5,6,8,9,11,12‐octa‐p‐tolyl‐1,6a,9a,12a‐tetraborata‐3a,4a,7,10‐tetrabora‐4a¹,6b,9b,12b‐tetraoxonia‐4‐oxatetra­cyclo­penta­[1,2‐a:2,1,5‐de:1,2‐g:1,2‐i]­naphthalene di­chloro­methane pentasolvate, C₆₄H₅₆B₈Cl₆O₅·5CH₂Cl₂, two condensed oxadiborole rings are attached to two further oxadiborole rings in a type of donor–acceptor bonding, thus forming a ten‐membered alternating (B—O)₅ naphthalene‐like arrangement as the central building block.     

The channel structure of the mercury(II) selenite(IV) oxide hydrate HgSeO3·HgO·H2O

The main building units of the title compound, dimercury(II) selenite(IV) oxide hydrate, are strongly distorted [Hg1O₆] and [Hg2O₇] polyhedra, and a pyramidal Se^IVO₃ group. Slightly corrugated hexagonal rings made up of six [Hg1O₆] octahedra spread parallel to the ab plane and are connected via [Hg2O₇] polyhedra parallel and perpendicular to this direction, which results in a three‐dimensional arrangement with channels propagating parallel to the c axis. The Se^IVO₃ groups are situated below and above the rings and bridge both types of Hg atoms. The non‐bonding orbitals are stereochemically active and protrude into the channels of the three‐dimensional network. Additional water mol­ecules are located at the centres of the channels and show weak interactions with the Se^IV lone pairs and the O atoms of the Se^IVO₃ groups.     

Crystal engineering with heteroboranes. II. 1,2‐Di­carboxy‐1,2‐dicarba‐closo‐dodecaborane(12) ethanol hemisolvate

The title compound, 1,2‐(COOH)₂‐1,2‐closo‐C₂B₁₀H₁₀·0.5C₂H₆O or C₄H₁₂B₁₀O₄·0.5C₂H₆O, forms a tetramer by incorporating ethanol (solvent) mol­ecules through hydrogen bonding. Two eight‐membered rings [graph set R(8)] are formed by hydrogen bonding between two carboxyl­ic acid groups, whereas two ten‐membered rings [R(10)] are formed by hydrogen bonding between two carboxyl­ic acid groups and the OH group of an ethanol mol­ecule (solvent). Two crystallographically independent tetramers are present in the crystal structure.     

8‐Hydroxyquinaldinic acid and its nickel(II) complex

The molecules of 8‐hydroxy­quinolinium‐2‐carboxyl­ate, C₁₀H₇NO₃, have a planar structure, in which the carboxyl group is ionized and the ring N atom is protonated. The derived nickel(II) complex, bis(8‐hydroxy­quinoline‐2‐carboxyl­ato‐κ³O²,N,O⁸)­nickel(II) trihydrate, [Ni(C₁₀H₆NO₃)₂]·3H₂O, contains an octahedral central Ni^II ion coordinated by the hydroxyl O atom, the ring N atom and the carboxyl­ate O atom of each of the two tridentate ligands, with a perpendicular orientation of the quinoline rings.     

Isolierte I102−‐Ringe,ein neues Strukturelement in der Polyiodid‐Chemie

The novel compound bis(1,4,7,10‐tetraoxa­cyclo­do­decane)­cadmium(II) decaiodide, [Cd(C₈H₁₆O₄)₂]I₁₀, contains the [Cd(12‐crown‐4)₂]²⁺ complex cation, triiodide ions and iodine mol­ecules. Two triiodide ions and two iodine mol­ecules form isolated twisted I₁₀^2? rings. The geometry of the complex cation is as expected, e.g.d(Cd—O) = 2.366 (4) and 2.394 (4) Å.     

Aqua(benzene‐1,3‐dicarboxylato)zinc(II)

The title compound, poly­[[aqua­zinc(II)]‐μ‐benzene‐1,3‐di­carboxyl­ato‐O¹:O^1′:O²], [Zn(C₈H₄O₄)(H₂O)]_n, forms a metal–organic coordination network that consists of tetrahedral Zn atoms bonded to one water mol­ecule and three carboxyl­ate groups. Isophthalate groups bridge the four‐coordinate Zn centers to generate two‐dimensional architectures in the ac plane. These planar zinc isophthalate motifs are linked by infinite C=O?H—O—H interactions along the a axis to form a chiral framework. The observed polar structural pattern originates due to the distorted tetrahedral Zn centers [O—Zn—O 100.7 (2)–136.0 (1)°] and the alignment of the water mol­ecules. Bridging isophthalate groups align to form approximate centrosymmetric motifs.     

Bis(acesulfamato‐κ2O4,N)bis­(3‐methyl­pyridine)copper(II)

In the crystal structure of the title compound {systematic name: bis­[6‐methyl‐1,2,3‐oxa­thia­zin‐4(3H)‐one 2,2‐dioxide(1−)‐κ²N³,O⁴]bis­(3‐meth­yl­pyridine)copper(II)}, [Cu(C₄H₄NO₄S)₂(C₆H₇N)₂], the Cu^II centre resides on a centre of symmetry and has an octa­hedral geometry that is distorted both by the presence of four‐membered chelate rings and because of the Jahn–Teller effect. The equatorial plane is formed by the N atoms of two methyl­pyridine ligands and by the more basic O atoms of the acesulfamate ligands, while the weakly basic N atoms of these ligands are in elongated axial positions with a misdirected valence. The crystal is stabilized by two inter­molecular C—H⋯O inter­actions involving the methyl and CH groups, and the sulfonyl O atoms of the acesulfamate group.     

Hexalithium hexadecahydrate decavanadate, [Li6(H2O)16V10O28]n

The novel title compound, poly­[octa‐μ‐aqua‐octa­aqua‐μ‐decavanadato‐hexalithium], contains [V₁₀O₂₈]⁶⁻ polyanions with 2/m symmetry linked by centrosymmetric [Li₆(H₂O)₁₆]⁶⁺ cation chains. The [V₁₀O₂₈]⁶⁻ polyanions form a two‐dimensional network with [Li₆(H₂O)₁₆]⁶⁺ chains via O‐polyanion–Li‐chain coordination, with Li—O bond lengths in the range 2.007 (5)–2.016 (5) Å. The hexalithium hexadecahydrate chain is composed of a centrosymmetric pair of LiO₆ octahedra and four distorted LiO₄ tetrahedra. Hydro­gen bonds occur between the polyanion and the Li‐based chains, and within the Li‐based chains.     

Co(en)3[B4O5(OH)4]Cl·3H2O和[Ni(en)3][B5O6(OH)4]2·2H2O的合成、结构以及热力学性质

利用水热法合成了两种过渡金属配合物为模板剂的含水硼酸盐晶体Co(en)3[B4O5(OH)4]Cl·3H2O(1) 和 [Ni(en)3][B5O6(OH)4]2·2H2O (2),并通过元素分析、X射线单晶衍射、红外光谱及热重分析对其进行了表征。化合物1晶体结构的主要特点是在所有组成Co(en)33+, [B4O5(OH)4]2–, Cl– 和 H2O之间通过O–H…O、O–H…Cl、N–H…Cl和N–H…O四种氢键连接形成网状超分子结构。化合物2晶体结构的特点是[B5O6(OH)4]–阴离子通过O–H…O氢键连接形成沿a方向有较大通道的三维超分子骨架,模板剂[Ni(en)3]2+阳离子和结晶水分子填充在通道中。     

Hydro­gen‐bonded dimers in N‐(2‐nitro­phenyl­thio)­saccharin

In the title compound, 2‐(2‐nitro­phenyl­thio)‐1,2‐benzo­thia­zol‐3(2H)‐one 1,1‐dioxide, 2‐O₂NC₆H₄S(C₇H₄NO₃S) or C₁₃H₈N₂­O₅S₂, the planes of the saccharin and nitro­phenyl­thiol­ate portions are almost orthogonal. The mol­ecules are linked by C—H?O=S hydrogen bonds [C?O 3.308 (3) Å, H?O 2.44 Å and C—H?O 155°] into cyclic centrosymmetric R²₂(16) dimers, reinforced by aromatic π?π stacking interactions between the nitrated aryl rings.     

Precursor of a β‐lactamase inhibitor: allyl (4S,8S,9R)‐10‐[(E)‐ethyl­idene]‐4‐methoxy‐11‐oxo‐1‐aza­tri­cyclo­[7.2.0.03,8]­undec‐2‐ene‐2‐carboxyl­ate

The molecular structure of the title tricyclic compound, C₁₇H₂₁NO₄, which is the immediate precursor of a potent synthetic inhibitor {Lek157: sodium (8S,9R)‐10‐[(E)‐ethyl­idene]‐4‐methoxy‐11‐oxo‐1‐aza­tri­cyclo­[7.2.0.0^3,8]­undec‐2‐ene‐2‐carboxyl­ate} with remarkable potency, provides experimental evidence for the previously modelled relative position of the fused cyclo­hexyl ring and the carbonyl group of the β‐lactam ring, which takes part in the formation of the initial tetrahedral acyl–enzyme complex. In this hydro­phobic mol­ecule, the overall geometry is influenced by C—H?O intramolecular hydrogen bonds [3.046 (4) and 3.538 (6) Å, with corresponding normalized H?O distances of 2.30 and 2.46 Å], whereas the mol­ecules are interconnected through intermolecular C—H?O hydrogen bonds [3.335 (4)–3.575 (5) Å].     

Hydrothermal Syntheses, Crystal Structure and Thermal Behavior of [(CH_3)_2NH_2]_2[B_5O_6(OH)_4]_2·[HCON(CH_3)_2] and [NH_3CH_2CH_2NH_3]_2·[B_(14)O_(20)(OH)_6]

Two novel organic base templated nonmetal borates [(CH₃)₂NH₂]₂[B₅O₆(OH)₄]₂·[HCON(CH₃)₂] ( ? ) and [NH₃CH₂CH₂NH₃]₂[B₁₄O₂₀(OH)₆] ( II ) have been synthesized under hydrothermal conditions, and characterized by elemental analyses, FT‐IR spectroscopy, X‐ray diffraction, and TG‐DTA. Their crystal structures were determined from single crystal X‐ray diffraction. The crystal structure of compound I is characterized by forming a 3D supramolecular structure with large channels along axes b and c through O? H···O hydrogen‐bonding among the [B₅O₆(OH)₄]^? anions. The crystal structure of compound II is characterized by forming a 3D supramolecular structure with large channels along axis a and direction [111] through O? H···O hydrogen‐bonding among the [B₁₄O₂₀(OH)₆]^4? anions. The templating organic amine cations in I and II are both obtained through in situ hydrothermal reactions, and are both located in the channels of the 3D supramolecular structure, respectively. Their thermal behavior has been also investigated.     

A New Organic‐Inorganic Hybrid Copper Pentaborate with Free Boric Acid Group

The hydrothermal reaction of Cu(CH₃COO)₂·H₂O, H₃BO₃, ethylenediamine and H₂O in a molar ratio of 3:20:9:222 at 140°C for 5 d yields the deep blue crystals of a new copper polyborate [Cu(en)₂B(OH)₃]· [B₅O₅(OH)₇] (en?H₂NCH₂CH₂NH₂) in 70% yield. It crystallizes in monoclinic system, space group P2₁/c, with unit cell dimensions, a=1.2779(2) nm, b=1.0167(15) nm, c=1.5019(2) nm, β=90.30(2)°, Z=4. The crystal structure of this compound consists of [Cu(en)₂B(OH)₃]²⁺ cation and [B₅O₅(OH)₇]^2? anion, which are linked together through hydrogen bonding interactions and electrostatic forces, forming an interesting three‐dimensional framework. The [B₅O₅(OH)₇]^2? anion is constituted of [B₄O₅(OH)₄]^2? anion and discrete B(OH)₃ group which attaches to the side of [B₄O₅(OH)₄]^2? through intramolecular hydrogen bonds. Fundamental vibrational modes of this compound were identified and band assignments were made. The middle bands observed at 882 and 575 cm^?1 in Raman spectrum are the characteristic peak of B(OH)₃ group and [B₄O₅(OH)₄]^2? anion, respectively. Additionally the thermal behavior of title compound was recorded and its decomposition mechanism was discussed.     

A host–guest complex of di­aqua­bis­[1‐hydroxy‐2(1H)‐pyridine­thionato‐O,S]­magnesium(II) and 2,2′‐di­thio­bis­(pyridine N‐oxide)

The title compound, [Mg(C₅H₄NOS)₂(H₂O)₂]·C₁₀H₈N₂O₂S₂, is a two‐component host–guest material. The 2,2′‐di­thio­bis(pyridine N‐oxide) molecule has crystallographic twofold symmetry. The metal complex lies on an inversion centre and associates via C—H?S interactions into chains which thread the 2,2′‐di­thio­bis­(pyridine N‐oxide) lattice in perpendicular directions. Hydro­gen bonds exist between the water mol­ecules of the di­aqua­magnesium units and the N—O groups of the host lattice.     

Hydrogen bonding in C‐substituted nitroanilines: sheets built from alternating R(12) and R(36) rings in 2‐bromo‐6‐cyano‐4‐nitroaniline

Molecules of the title compound (systematic name: 2‐amino‐3‐bromo‐5‐nitro­benzo­nitrile), C₇H₄BrN₃O₂, are linked by N—H?N and N—H?O hydrogen bonds [H?N 2.19 Å, N?N 3.019 (4) Å and N—H?N 157°, and H?O 2.17 Å, N?O 2.854 (3) Å and N—H?O 134°] to form (10) sheets built from alternating R(12) and R(36) rings, both of which are centrosymmetric.     

Tetrakis(2,2′‐bipyridine‐κ2N,N′)­tetrakis(μ‐salicyl­ato‐κ3O,O′:O′′)‐quadro‐tetrazinc(II) decahydrate

The title compound, [Zn₄(C₇H₄O₃)₄(C₁₀H₈N₂)₄]·10H₂O, crystallizes as a centrosymmetric tetranuclear cyclic complex containing four Zn^II atoms bridged by four carboxyl­ate groups from salicyl­ate ligands, with a syn–anti configuration. Each Zn^II atom has a distorted trigonal–bipyramidal coordination geometry, formed by two N atoms of a 2,2′‐bipyridine ligand and three O atoms from two salicyl­ate ligands. The complex is stabilized by intramolecular π–π interactions between pairs of bi­pyridine rings and a 16‐membered gear‐wheel‐shaped cyclic framework. The hydrogen‐bonding network is formed via the water mol­ecules.     

O‐Benzyl‐N‐tert‐butoxy­carbonyl‐N‐methyl‐l‐tyrosine

The crystal structure of the title compound, alternatively called 3‐[4‐(benzyl­oxy)­phenyl]‐2‐(N‐tert‐butoxy­car­bonyl‐N‐methyl­amino)­propi­onic acid, C₂₂H₂₇NO₅, has been studied in order to ex­amine the role of N‐methyl­ation as a determinant of peptide conformation. The conformation of the tert‐butoxy­carbonyl group is trans–trans. The side chain has a folded conformation and the two phenyl rings are effectively perpendicular to one another. The carboxyl­ate hydroxyl group and the urethane carbonyl group form a strong intermolecular O—H?O hydrogen bond.     

Tris­[(R)‐lact­amide‐κ2O,O′]­zinc(II) tetra­bromo­zincate

The title compound, tris­[(R)‐2‐hydroxy­propan­amide‐κ²O,O′]­zinc(II) tetra­bromo­zincate, [Zn(C₃H₇NO₂)₃][ZnBr₄], contains one monomeric six‐coordinate zinc complex cation and one tetrahedral [ZnBr₄]²⁻ anion. Both Zn^II atoms lie on threefold axes. Coordination in the cation occurs via the amide and hydroxy O atoms [Zn—O = 2.074 (5) and 2.073 (6) Å] and has a distorted octahedral geometry, with cis‐O—Zn—O angles in the range 76.2 (2)–109.2 (2)°. In the crystal structure, the cations and anions are linked by N—H⋯Br and O—H⋯O hydrogen bonds, generating a three‐dimensional network.