Synthesis and Structure of [Fe<Subscript>3</Subscript>O(O<Subscript>2</Subscript>CCH<Subscript>2</Subscript>OMe)<Subscript>6</Subscript>(H<Subscript>2</Subscript>O)<Subscript>3</Subscript>][FeCl<Subscript>4</Subscript>]

Abstract  The structure of [Fe₃O(O₂CCH₂OMe)₆(H₂O)₃][FeCl₄] · 2.5H₂O has been determined. The three iron atoms and the μ₃-oxo are coplanar. Each carboxylic ligand is bidentate and links two iron atoms in the cluster. The clusters are linked by intra-trimer hydrogen bonding to form a zigzag motif that forms sheets via hydrogen bonding involving disordered waters of hydration. The [FeCl₄]⁻ anion is intercalated between the hydrogen-bonded sheets. Crystal data: space group P2₁/n, a = 10.276(2), b = 22.793(5), c = 17.091(3) ?, β = 96.66(3)°, V = 3976(1) ?³, Z = 4, R = 0.0837, wR ₂ = 0.1836. Graphical Abstract  The structure of [Fe₃O(O₂CCH₂OMe)₆(H₂O)₃][FeCl₄] · 2.5H₂O has been determined in which the clusters are linked by intra-trimer hydrogen bonding to form a zigzag motif that forms sheets via hydrogen bonding involving disordered waters of hydration.      

Synthesis,Characterization, and Structure of a Cyano-bridged Two-dimensional Cu<Superscript>II</Superscript>Co<Superscript>III</Superscript> Coordination Polymer Derived from <Emphasis Type="Italic">Trans</Emphasis>-1,2-diaminocyclohexane as Blocking Ligand

Abstract  The synthesis, characterization, and structure of a cyano-bridged two-dimensional supramolecule, [Cu^II(trans-chxn)₂]₃[Co^III(CN)₆]₂·2H₂O (1; chxn = 1,2-diaminocyclohexane), have been described. The title compound crystallizes in the triclinic Pī space group with the unit cell parameters: a = 9.141(5) ?, b = 12.406(5) ?, c = 15.064(5) ?, α = 95.190(5)°, β = 94.460(5)°, γ = 109.510(5)°, V = 1593.0(12) ?³, and Z = 1. The compound contains two crystallographically different copper(II) and cobalt(III) centers. Each of the two copper(II) ions is hexacoordinated by two diamines and two bridging cyanides. Two trans cyanides of one type of hexacyanometalate link one type of copper(II) center to result in one-dimensional chain, while two pairs of trans cyanides of the second type of hexacyanometalate link both the types of copper(II) ions to result in the second dimension. There are extensive hydrogen bonding interactions within the two-dimensional cyano-bridged sheet involving the solvated water molecule, amine groups, and cyanide nitrogens. Index Abstract  Synthesis, characterization, and structure of a cyano-bridged two-dimensional Cu^IICo^III coordination polymer derived from trans-1,2-diaminocyclohexane as blocking ligand Malabika Nayak, Samit Majumder, Pascale Lemoine, and Sasankasekhar Mohanta* The synthesis, characterization, and structure of a cyano-bridged two-dimensional supramolecule, [Cu^II(trans-chxn)₂]₃[Co^III(CN)₆]₂ · 2H₂O (chxn = 1,2-diaminocyclohexane), have been described.      

Crystal Structure of a Rearranged Cage Compound, 3-Hydroxy-4-aza-8-oxoheptacyclo [9.4.1.0<Superscript>2,10</Superscript>.0<Superscript>3,14</Superscript>.0<Superscript>4,9</Superscript>.0<Superscript>9,13</Superscript>.0<Superscript>12,15</Superscript>]tetradecane

Abstract  Polycyclic hydrocarbon compounds exhibit a wide variety of biological activities, ranging from antiviral to Parkinson’s disease. Several structures such as the adamantanes have reached clinical status and are used therapeutically to treat, amongst others, neurodegenerative disorders such as Alzheimer’s. Polycyclics have also been utilised as carrier molecules to facilitate entry of drugs into the brain. The synthesis, molecular and crystal structure of a new polycyclic compound, 3-hydroxy-4-aza-8-oxoheptacyclo[9.4.1.0^2,10.0^3,14.0^4,9.0^9,13.0^12,15]tetradecane, are reported. NMR spectroscopy was applied for structure elucidation of the novel compound and a rearrangement mechanism is proposed for its formation. This compound crystallises in the orthorhombic system, space group Pbca (no. 61). The unit cell parameters are: a = 12.3763 (7), b = 11.6597 (6), c = 15.0539 (8) ?, V = 2172.3 (2) ?³ , and Z = 8 molecules in the unit cell. The reported structure was confirmed by X-ray analysis, which showed that the title molecules associate into centrosymmetric dimers via N–H···O hydrogen bonding. Index Abstract  The synthesis and structure of a new polycyclic compound, 3-hydroxy-4-aza-8-oxoheptacyclo[9.4.1.0^2,10.0^3,14.0^4,9.0^9,13.0^12,15]tetradecane, are reported in this article.      

[KCl<Subscript>3</Subscript>{H<Subscript>2</Subscript>dabco}]: A Unique 3-D Charge-Assisted Hydrogen-Bonded Hybrid Network of Anionic KCl<Subscript>3</Subscript> Chains and Organic Cations

Abstract  The 3-D hybrid network [KCl₃{H₂dabco}] resulted from the assemblage of KCl and [{H₂dabco}Cl₂] (1,4-diazabicyclo[2.2.2]octane) in H₂O. The compound crystallizes in the trigonal space group R-3c with a = b = 16.0437(2) Å, and c = 22.3094(2) Å. The structure consists in polymeric chains of anionic {KCl₃}²⁻ linked to {H₂dabco}²⁺ units by hydrogen bonds. Each organic cation establishes such charge-assisted H···Cl interactions with two inorganic arrays leading to a 3-D network. Index Abstract  Assemblage of KCl and [{H₂dabco}Cl₂] (1,4-diazabicyclo[2.2.2]octane) in H₂O resulted in a 3-D hybrid network of inorganic {KCl₃}²⁻ chains H-bonded to bridging organic cations.      

Synthesis and Crystal Structure of La(NO<Subscript>2</Subscript>)(SO<Subscript>4</Subscript>)(H<Subscript>2</Subscript>O)

Abstract Single crystals of new open-framework lanthanide sulphate nitrite La(NO₂)(SO₄)(H₂O) has been synthesized, in the presence of 2,6-diformyl-4-chlorophenol. His structure has been determined by X-ray diffraction data: the complex crystallizes in the tetragonal system, space group P4₃, with a = 7.0028(2) (?), b = 7.0028(2) (?), c = 11.8341(4) ?, V = 580.34(3) ?³, Z = 4, D _c = 3.582 Mg m⁻³. The three-dimensional (3D) framework of this compound is built up by the linkages of lanthanide atoms and the oxygen atoms of the sulphate and nitrite groups. The lanthanum atom is 9-fold coordinated. The structure is unfamiliar in lanthanide chemistry and this compound represents the first example of nitrite lanthanide sulphate complex. Graphical Abstract An unfamiliar structure in lanthanide chemistry represented by the first example of nitrite lanthanide sulphate complex is described.      

The Preparation,Characterization and X-ray Structural Analysis of Tetrakis[1,3-dimethyl-2(3H)-imidazoleselone]cadmium(II) Hexafluorophosphate

Abstract A new compound, [Cd(dmise)₄][PF₆]₂, has been synthesized and characterized via standard solid and solution state methods including single crystal X-ray crystallography (dmise = 1,3-dimethyl-2(3H)-imidazoleselone). The title compounds crystallizes in orthorhombic space group P bcn with a = 12.783(3), b = 22.206(4), c = 13.153(3) ?, V = 3733.8(13) ?³, Z = 4. The complex is a high melting, yellow water soluble 2:1 electrolyte solid that state has a flattened tetrahedral CdSe₄ coordination geometry. To date this is the only structural study reported for a homoleptic selenourea complex of cadmium. Graphical abstract The Preparation, characterization and X-ray structural analysis of Tetrakis[1,3-dimethyl-2(3H)-imidazoleselone]cadmium(II) hexafluorophosphate Daniel J. Williams, Bradley J. McKinney, Ben Baker, Kevin P. Gwaltney and Donald VanDerveer Tetrakis[1,3-dimethyl-2(3H)-imidazoleselone][PF₆]₂ is prepared in 82% yield by direct combination of cadmium acetate dihydrate, ammonium hexafluorophosphate, and the ligand in boiling acetonitrile. X-ray crystallography shows a structure with a distorted tetrahedral coordination sphere around the cadmium. This is the first report of a structural characterization of a homoleptic cadmium selenourea complex. Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users.     

Crystal Structures of Energetic Compounds. I. Safe Small-Scale Preparation and X-Ray Structure Determination of the High-Energy Cobalt(III) Complex [Co(NH<Subscript>3</Subscript>)<Subscript>5</Subscript>N<Subscript>3</Subscript>](N<Subscript>3</Subscript>)<Subscript>2</Subscript>

Abstract  Well-formed dark red single-crystals of the potentially explosive cobalt(III) azido complex [Co(NH₃)₅N₃](N₃)₂ (nitrogen content: 72.59%) have been grown using a safe small-scale preparation from [Co(NH₃)₅N₃]Cl₂ and sodium azide. The complex crystallizes in the orthorhombic system, space group Pnma with unit cell parameters a = 12.921(3) ?, b = 10.346(2) ?, c = 8.0315(16) ?, V = 1,073.7(4) ?³ and Z = 4. Five NH₃ ligands and the azide anion surround the Co³⁺ ion in a nearly perfect octahedral geometry. Two azide anions are non-coordinating, and no water of crystallization is present in the crystal structure. Graphical Abstract  Well-formed dark red single-crystals of the potentially explosive cobalt(III) azido complex [Co(NH₃)₅N₃](N₃)₂ (nitrogen content: 72.59%) have been grown using a safe small-scale preparation from [Co(NH₃)₅N₃]Cl₂ and sodium azide. Five NH₃ ligands and the azide anion surround the Co³⁺ ion in a nearly perfect octahedral geometry. Two azide anions are non-coordinating, and no water of crystallization is present in the crystal structure.      

The Synthesis and Crystal Structure of 5-(4-Bromophenylamino)-2-methylsulfanylmethyl-2<Emphasis Type="Italic">H</Emphasis>-1,2,3-triazol-4-carboxylic Acid Ethyl Ester

Abstract  The 5-(4-bromophenylamino)-2-methylsulfanylmethyl-2H-1,2,3-triazol-4-carboxylic acid ethyl ester 6 was synthesized from p-bromoaniline. The yielded product 6 was investigated with X-ray crystallographic, NMR, MS, and IR techniques. Compound 6, C₁₃H₁₅BrN₄O₂S, Mr = 371.26, crystallizes in the monoclinic space group P2₁/n with unit cell parameters a = 5.5220(1), b = 26.996(5), c = 10.596(2) ?, β = 103.83(3). V = 1533.8(5) ?³, Z = 4, Dx = 1.608 mg m⁻³. The final R ₁ was 0.0844; wR ₂ was 0.1560. H-bond is discussed. Index Abstract  The structure of 5-(4-bromophenylamino)-2-methylsulfanylmethyl-2H-1,2,3-triazol-4-carboxylic acid ethyl ester from 5-amino-1-(4-bromophenyl)-1,2,3-triazol-4-carboxylic acid ethyl ester is studied. H-bond is discussed.      

Synthesis,Properties, and Crystal Structures of Copper(II) Di-(2-picolyl)amine Complexes Containing Inorganic Salts

Abstract These complexes have been characterized by X-ray crystallography, spectroscopic, and cyclic voltammetry. In 1, the copper(II) ion has a distorted square-pyramidal geometry with three nitrogen atoms of the dpa ligand and two oxygen atoms of the nitrate anions. The crystal structure of 2 shows that the copper(II) ions are bridged by tp anion to form a dinuclear complex, in which each copper(II) ion exhibits a distorted square-pyramid with three nitrogen atoms of the dpa ligand, water molecule, and the oxygen atom of the bridging tp ligand. Cyclic voltammetric data indicate that 1 undergoes irreversible one-electron oxidation to the Cu^III and reversible one-electron reduction to the Cu^I, while 2 gives one reversible oxidation and two reversible and irreversible reduced processes. The electronic spectra and redox potentials of the complexes are influenced significantly by the anionic ligands. Graphical Abstract The reaction of [Cu(dpa)Cl₂] with K(NO₃)₂ and Na₂tp yields mononuclear and dinuclear copper(II) complexes [Cu(dpa)(NO₃)₂] (1) and [Cu₂(dpa)₂(H₂O)₂(μ-tp)](tp)·6H₂O (2) (dpa = di-(2-picolyl)amine, tp = terephthalate).      

<Emphasis Type="Italic">Trans-</Emphasis>dichlorodioxobis(triphenylphosphate)molybdenum(VI), MoO<Subscript>2</Subscript>Cl<Subscript>2</Subscript>[OP(OPh)<Subscript>3</Subscript>]<Subscript>2</Subscript>

Abstract  The molecular structure of trans-dichlorodioxobis(triphenylphosphate) molybdenum(VI), MoO₂Cl₂[OP(OPh)₃]₂ has been determined. Crystal data: Monoclinic, Pn, a = 11.767(2), b = 10.341(2), c = 15.682(3) ?, β = 92.27(3)°, V = 1906.8(7) ?⁻³, Z = 2. Trans-dichlorodioxobis(triphenylphosphate)molybdenum(VI) was obtained by the reaction of molybdenum oxide, HCl and triphenylphosphate and was characterized by elemental analysis, IR, and ¹H-NMR spectroscopy. Index Abstract   Trans-dichlorodioxobis(triphenylphosphate)molybdenum(VI), MoO₂Cl₂[OP(OPh)₃]₂ V. Huch¹, R. Kumar², S. Mathur¹, R. Ratnani² The immediate environment around Mo is distorted octahedral with two cis-oxygen atoms and two trans-chlorine atoms along with two triphenylphosphate moieties.      

A Unique Example of a Co-crystal of [Co(AMTTO)2(H2O)2](NO3)2 and [Co(AMTTO)2(CH3CN)2](NO3)2 (AMTTO = 4-amino-5-methyl-1,2,4-triazol-3(2H)-thione)

A co-crystal of cobalt(II) complexes, Co(AMTTO)₂(CH₃CN)₂]²⁺(NO₃)₂. [Co(AMTTO)₂(H₂O)₂]²⁺(NO₃)₂, compound (1) was isolated from the reaction of Co(NO₃)₂?6H₂O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine (AMTTO) in acetonitrile as solvent. Isolated crystals were characterized by elemental analyses, IR spectroscopy as well as X-ray diffraction studies. Crystal data for 1 at 95 K revealed a monoclinic space group P2₁/n, a?=?11.7903(5), b?=?12.1279(5), c?=?14.1443(6) Å, β?=?99.244(4)°, Z?=?2, R₁?=?0.0339. Compound 1 consists of two co-crystallized Co(II) complexes [Co(AMTTO)₂(CH₃CN)₂]²⁺ and [Co(AMTTO)₂(H₂O)₂]²⁺ and four nitrate counter anions In both complexes, cobalt(II) ions are in an octahedral arrangement. Two S, N bidentate AMTTO ligands are coordinated to both Co(II) ions. The coordination sphere of Co1 is completed by two acetonitrile molecules, and these positions are occupied by water molecules for Co2.

Graphic Abstract

A co-crystal of cobalt(II) compound was isolated from the reaction of Co(NO₃)₂?6H₂O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine in acetonitrile as solvent.

     

Diaquabis(phen)Ni(II) Complex with Vitamin B13 Counter-ions

Abstract The synthesis and crystal structure of a new Ni(II) complex of stoichiometry [Ni(phen)₂(H₂O)₂](H₂Or)₂ · 2H₂O, where phen is phenanthroline and H₂Or is oratate monoanion, are reported. The complex [Ni(phen)₂(H₂O)₂](H₂Or)₂ · 2H₂O crystallizes in the monoclinic system with space group C2/c and cell parameters a = 16.1661(8) ?, b = 12.5669(7) ? and c = 16.4752(7) ?. The coordination around Ni(II) is a distorted octahedron with two phen ligands perpendicular to each other and two aqua ligands in cis- position. Orotate ions locate themselves out of the coordination sphere and bridge the [Ni(phen)₂(H₂O)₂]²⁺ moieties through hydogen bonding with aqua ligands. The FT-IR spectrum of the complex and thermal decomposition behaviour are also briefly discussed. Graphical Abstract Diaquabis(phen)Ni(II) Complex with Vitamin B13 Counter-ions Dursun Ali K?se, Birgül Zümreoglu-Karan, Başak Koşar, Orhan Büyükgüng?r A new complex where Vitamin B13 monoanions act as counter ions and bridge the [Ni(phen)₂(H₂O)₂]²⁺ units by hydrogen bonds is described CCDC deposition number is 606339.     

Synthesis and Crystal Structure of the Salt [PPN+]2[Cu2I2Cl2]2−

Abstract The synthesis of the PPN (PPN=Ph₃P=N=PPh₃) salt of di-μ-iodo-dichlorocuprate (I) anion [Cu₂I₂Cl₂]²⁻ is described and the crystal and molecular structures of this compound are reported. It was found that the compound has the formula [PPN]₂[Cu₂I₂Cl₂]_0.7[Cu₂I₄]_0.3 (3). Compound 3 crystallizes in an orthorhombic crystal system, space group Pbca, with a = 19.654(3), b = 16.130(2), c = 20.108(3) ?, V = 6374.3(16) ?³ and Z = 4. The crystal contains 70% [Cu₂I₂Cl₂]²⁻ anions and 30% [Cu₂I₄]²⁻ anions. This was also confirmed by MSES spectroscopy. The anion [Cu₂I₂Cl₂]²⁻ is planar and the Cu atoms have a trigonal planar configuration. Graphical abstract Synthesis and Crystal Structure of the Salt [PPN ⁺ ] ₂ [Cu ₂ I ₂ Cl ₂ ] ²⁻ Andrey A. Yakovenko, Tatiana V. Timofeeva and Mikhail Yu. Antipin The title compound was synthesized and structurally investigated. The crystal contains 70% [Cu₂I₂Cl₂]²⁻ anions and 30% [Cu₂I₄]²⁻ anions. This was confirmed by MS ES spectroscopy.      

Synthesis and Crystal Structure of a New Mo(V) Complex of Cyano Ligands

Abstract  A new complex, [H₃teta][Mo(CN)₈] · H₂O, (teta = 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetra-azacyocloteradeca-4,11-diene), has been synthesized and characterized by IR spectrum, element analysis and single crystal X-ray diffraction: monoclinic, space group P2(1)/c with a = 10.8553(8) ?, b = 12.4854(8) ?, c = 22.6348(15) ?, α = 90.00°, β = 97.3080(10)°, γ = 90.00°, Mr = 609.63, v = 3042.8(4), Z = 4. There are one [H₃teta]³⁺, one [Mo(CN)₈]³⁻ and one water molecule in the asymmetric unit. The complex is interconnected through hydrogen bond and formed into a 3D porous network. Graphical Abstract  A new complex, [H₃teta][Mo(CN)₈] · H₂O, has been synthesized and characterized by IR spectrum, element analysis and single crystal X-ray diffraction. And it shows a 3D porous network through hydrogen bonds.      

Structural Analysis of the Phase Transitions of (NH<Subscript>4</Subscript>)<Subscript>4</Subscript>HgBr<Subscript>6</Subscript>

Abstract Single crystal diffraction and differential scanning calorimetry DSC techniques have been used to investigate the different phases of (NH₄)₄HgBr₆, tetrammonium mercury hexabromide, from room temperature to 120 K. Two anomalies in thermal behaviour were detected for this compound at 190 and 268 K, by DSC experiment. X-ray diffraction measurements confirm these anomalies. At room temperature the structure is tetragonal P4/mnc (No. 128) with lattice parameters a = b = 9.25560(8) ?; c = 8.8657(11) ?; V = 759.49(9) ?³ and Z = 2. At T = 250 K the structure is orthorhombic Pnnm with lattice parameters a = 8.8436(8) ?; b = 9.2191(8) ?; c = 9.2232(7) ?; V = 751.97(11) ?³ and Z = 2. Below approximately 200 K the structure is monoclinic P2₁/n (No. 14) with: a = 8.8080(9) ?; b = 9.1608(8) ?; c = 9.1498(8) ?; β = 90.230(7)°; V = 738.28(12) ?³ and Z = 2 (T = 120 K). The structure of (NH₄)₄HgBr₆ consists of isolated HgBr₆-octahedra in the whole temperature range which are slightly compressed in c-direction. The ammonium groups are located between the octahedra ensuring the stability of the structure by hydrogen bonding contacts: N–H···Br. The structural phase transformations are described by a rotation of the [HgBr₆]²⁻ octahedra around the c-axis, and this behaviour is attributed to an orientational disorder of ammonium groups. Index abstract Structural analysis of the phase transitions of (NH₄)₄HgBr₆; M. Loukil, A. Kabadou, I. Svoboda, A. Ben Salah and H. Fuess; The phase transformations in (NH₄)₄HgBr₆ are explained by large rotation of [HgBr₆]²⁻ octahedra around the c-axis.      

Crystal and Molecular Structure of <Emphasis Type="Italic">trans</Emphasis>-1,2-bis(2-benzothiazolyl)ethene

Abstract The crystal and molecular structure of trans-1,2-bis(2-benzothiazolyl)ethene is reported. Crystal data for 1: monoclinic, space group C 2/c, a = 24.926(3) ?, b = 4.843(1) ?, c = 11.164(1) ?, β = 105.274(5) °, V = 1300.0(3) ?³, and D _c = 1.50 g/cm³ for Z = 4 and R = 0.028. The molecule crystallizes in the form of a colorless plate and forms one-dimensional slipped π-stacks. Graphical Abstract The title compound crystallizes to form 1D slipped π-stacks in the solid state. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Synthesis and Crystal Structure of a Polymeric Cobalt(II) Complex with 1,2-bis(1,2,4-triazol-1-yl)ethane

Abstract The title complex [Co₂(bte)₃(NCS)₄(H₂O)₂] _n (bte = 1,2-bis(triazol-1-yl)ethane) has been prepared. Single-crystal X-ray analysis reveals that the complex crystallizes in space group P ī with a = 7.7962(2), b = 8.3407(4), c = 14.7735(5) ?, α = 86.835(2), β = 76.2031(9), γ = 80.583(3)°. The crystal consists of two discrete complexes, [Co(bte)(NCS)₂(H₂O)₂] and [Co(bte)₂(NCS)₂]. The structure of [Co(bte)(NCS)₂(H₂O)₂] consists of neutral chain containing Co(II) bridged by bte molecules. The six-co-ordination of Co²⁺ is achieved by means of two trans NCS⁻ ions and water molecules. The structure of [Co(bte)₂(NCS)₂] demonstrates a one-dimensional neutral chain through bte-bridge, in which the Co(II) atom is in a distorted octahedral environment formed by four nitrogen atoms of the triazoles and two nitrogen atoms from two trans thiocyanato liagnds. Index abstract Synthesis and Crystal Structure of a Polymeric Cobalt(II) Complex with 1,2-bis(1,2,4-triazol-1-yl)ethane This paper reports the synthesis and crystal structure of complex [Co₂(bte)₃(NCS)₄(H₂O)₂]_n (bte = 1,2-bis(triazol-1-yl)ethane), which consists two different neutral chains containing Co(II) bridged by bte molecules.      

Synthesis and Structure of Ba<Subscript>5</Subscript>(V<Subscript>2</Subscript>O<Subscript>7</Subscript>)<Subscript>2</Subscript>Cl<Subscript>2</Subscript>

Abstract  A new barium chlorovanadate, Ba₅(V₂O₇)₂Cl₂, was isolated by a high-temperature (850 °C) reaction employing a CsCl/RbCl flux. The structure was determined by single crystal X-ray diffraction methods. This compound crystallizes in an orthorhombic crystal system, Pmmn (No. 59), with a = 11.558(2) ?, b = 15.164(3) ?, c = 10.023(2) ?, Z = 4 and V = 1756.7(6) ?³. The structure of Ba₅(V₂O₇)₂Cl₂ was determined by full-matrix, least-squares methods with R ₁ = 0.0398, wR ₂ = 0.1069 and GOF = 1.048 for all data. This new structure can be described as a composite lattice made up of mixed covalent and ionic moities. The extended framework is orchestrated by stacked [Ba(V₂O₇)Cl]³⁻ slabs that are interconnected by Ba²⁺ cations through Ba–O bonds to the [V₂O₇] units. The Ba²⁺ and Cl^- ions form BN-type “[BaCl]” sheets with pseudo-hexagonal windows that are centered by [V₂O₇]⁴⁻ pyrovanadate units. Graphical Abstract  The structure of a new chlorovanadate, Ba₅(V₂O₇)₂Cl₂, exhibits an interesting BN-type salt lattice that consists of an extended [BaCl] sheet containing pseudo-hexagonal windows that are centered by [V₂O₇] pyrovanadate units.      

Synthesis of <Emphasis Type="Italic">E</Emphasis> Isomer and Crystal Structures of <Emphasis Type="Italic">E</Emphasis> and <Emphasis Type="Italic">Z</Emphasis> Isomers of 3-(2,5-Dimethoxyphenyl)-2-(4-methoxyphenyl)acrylonitrile

Abstract Details of the synthesis of the E isomer of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylonitrile, and the X-ray crystal structures of both the E and Z isomers of this compound are presented. The E isomer crystallizes in the P2₁/c space group with cell parameters, a = 8.5659(17) ?, b = 16.399(3) ?, c = 11.224(2) ?, α = 90°, β = 95.27(3)°, γ = 90°and Z = 4. The Z isomer crystallizes in the Pca2₁ space group with cell parameters, a = 4.1223(8) ?, b = 19.113(4) ?, c = 19.453(4) ?, α = 90°, β = 90°, γ = 90° and Z = 4. Index Abstract Synthesis of E isomer and X-ray crystal structure determination of both E and Z isomers of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylonitrile are presented.      

An X-Ray Crystallographic Study of the Novel Aminal bis-(<Emphasis Type="Italic">p</Emphasis>-Ethoxycarbonylphenylamino-)methane

Abstract  The crystal structure of bis-(p-Ethoxycarbonylphenylamino-)methane (1) has been determined by single crystal X-ray diffraction analysis. The bis-aminal (1) molecule is V-shaped and situated on a twofold axis passing through C1 with the phenyl rings forming a dihedral angle of 70.2(1)°. The carboxylate and phenyl groups are coplanar. The crystal structure of 1 is compared with the structure of the closely related aminals, 2–5. Crystal data: 1 C₁₉H₂₂N₂O₄, tetragonal, space group I4 ₁ cd (N.110), a = 20.4760(7) Ǻ, b = 20.4760(7) Ǻ, c = 8.2984(3) ?, and V = 3477.7(2) ?³, for Ζ = 8. Index Abstract  The crystal structure of bis-(p-ethoxycarbonylphenylamino-)methane (1) has been determined by single crystal X-ray diffraction analysis.