3-Methyl-3a,4-Dihydro-3H-Thiochromeno[4,3-c]isoxazol

Abstract  The crystal structure of the title compound, C₁₁H₁₁NOS, was determined by an X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P2₁/c with cell parameters a = 10.533(2) ?, b = 12.7826(19) ?, c = 7.6491(17) ?, β = 107.997(17)^°, V = 979.5(3) ?³ and Z = 4. The S containing heterocycle adopts a sofa conformation, whereas the 5-membered ring adopts an envelope conformation. The crystal packing is characterized by weak C–H···N contacts and π-stacking interactions. Graphical Abstract  The title compound, 3-methyl-3a,4-dihydro-3H-thiochromeno[4,3-c]isoxazol was synthesized by an 1,3 dipolar cycloaddition reaction and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that the aromatic 6-membered ring is planar, whereas the ring containing the S atom adopts a sofa conformation and the 5-membered ring an envelope conformation. The methyl group is in an equatorial position.      

Crystal and Molecular Structure of Diterpenoid Alkaloid 3-Acetylaconitine

Abstract  3-Acetylaconitine (1), C₃₆H₄₉NO₁₂, was isolated from the ammonium hydroxide wetted root of A. szechenyianum Gay. X-ray diffraction analysis demonstrated that it consists of four-six-membered rings A, B, C, D and two-five-membered rings E, F. The fused-ring system A, B, C and D are in chair, chair, chair and boat conformations, respectively; ring E is in a half-chair; and ring F is in an envelope confirmation. The crystal of 3-acetylaconitine is in orthorhombic crystal system with space group P2₁2₁2₁, lattice constants: a = 9.2002(8) ?, b = 11.06454(9) ?, and c = 33.072(3) ?, V = 3543.3(5) ?³, Z = 4. Index Abstract  3-Acetylaconitine, C₃₆H₄₉NO₁₂, was isolated from the ammonium hydroxide wetted root of A. szechenyianum Gay, and its crystal and molecular structure was determined by X-ray diffraction analysis.      

Synthesis and Structural Characterization of Bis(μ2-Iodo)-Bis(Diethyl Ether)-(N-N′-(Bis(2,6-Diisopropylphenyl)Pentane-2,4-Diketiminato)-Lithium-Chromium, a Cr(II) (β-Diketiminato) Complex with a Coordinated LiI Salt

Abstract  Addition of CrI₂ to the lithium salt of N-N′-bis(2,6-diisopropylphenyl)-2,4-diketiminate in diethylether yields a Cr(II) iodide complex with a coordinated, solvated LiI salt. This complex is the intermediate in the synthesis of a bridging iodide complex that is itself a precursor to a side-on bridging dinitrogen complex. This complex crystallizes in the P2₁/n space group with the crystal cell parameters a = 12.3160(19) ?, b = 21.067(3) ?, c = 15.837(3)?, β = 96.767°, V = 4080.6(11) ?³ and Z = 4. Graphical Abstract  Addition CrI2 to the lithium salt of N-N′-bis(2,6- diisopropylphenyl)-2,4-diketiminate in diethylether yields a Cr(II) iodide complex with a coordinated, solvated LiI salt. Herein we report the spectroscopic and structural characterization. An erratum to this article can be found at     

Synthesis and Crystal Structure of a One-Dimensional Chain Cadmium Coordination Polymer Bridged Through 1,2-bis(imidazol-1-yl)ethane

Abstract The cadmium(II) complex [Cd(phba)₂(bim)(H₂O)₂]_n (1) (phba = 4-hydroxybenzoate, bim = 1,2-bis(imidazol-1-yl)ethane) has been synthesized and structurally characterized by X-ray diffraction analysis. It crystallizes in the monoclinic space group C2/c, a = 23.820(4) ?, b = 9.5331(14) ?, c = 11.1086(19) ?, β = 111.519(4)°, V = 2346.7(7) ?³, Z = 4. The coordination geometry of Cd(II) atom is distorted octahedral; it is coordinated by two nitrogen atoms from the imidazole rings of two symmetry-related bim molecules, and four oxygen atoms from two symmetry-related phba anions and two water molecules. The Cd(II) atoms are bridged by bim molecules to form a one-dimensional chain. Graphical abstract Synthesis and crystal structure of a one-dimensional chain cadmium coordination polymer bridged through 1,2-bis(imidazol-1-yl)ethane Yuping Zhang, Liyan Wang, Shouwu Wang, Baolong Li, Yong Zhang The cadmium(II) complex [Cd(phba)2(bim)(H2O)2]n (1) has been synthesized and structurally characterized by X-ray diffraction analysis. The coordination geometry of Cd(II) atom is distorted octahedral; it is coordinated by two nitrogen atoms from the imidazole rings of two symmetry-related bim ligands, and four oxygen atoms from two symmetry-related phba anions and two water molecules. The Cd(II) atoms are bridged by bim ligands to form a one-dimensional chain.     

Synthesis,Characterization and Crystal Structure of Bis(isothiocyanato)-bis(pyridine) Zinc(II) Crystal

Abstract  Bis(isothiocyanato)-bis(pyridine) zinc(II) crystal has been prepared at room temperature and characterized by elemental analysis, IR spectrum and X-ray single crystal determination. The complex crystallizes in monoclinic space group P2₁/m with unit cell parameters: a = 5.5786(3), b = 11.0587(5), c = 12.1616(6) ?, β = 96.776(3)°, V = 745.03(6) ?³, Z = 2, D _x  = 1.514 g cm⁻³. The X-ray structure determination has revealed that the crystal is centered-symmetrical and the crystallographic symmetry face runs the two isothiocyanate ligands and the Zn(II) cation. Index Abstract  The title compound, bis(isothiocyanato)-bis(pyridine) zinc(II), was synthesized by zinc compound, KSCN and C₅H₅N (pyridine) and its crystal structure was determined. Single crystal X-ray structure determination reveals that the crystal is centered-symmetrical, and the crystallographic symmetry face runs the two isothiocyanate ligands and the Zn(II) cation.      

Crystal Structure of the Radical-Cation Salt (<Emphasis Type="Italic">o</Emphasis>-Me<Subscript>2</Subscript>TTF)I<Subscript>3</Subscript> with Close Intermolecular Sulfur Contacts

Abstract  The synthesis and crystal structure of the organic radical-cation salt (o-Me₂TTF)I₃ is described. The salt crystallizes in the monoclinic space group P2 ₁ /n with a = 10.927(2) ?, b = 11.904(2) ?, c = 12.660(2) ?, β = 115.174(5)°. The bond length of the central C=C bond in o-Me₂TTF is 1.401(1) ?, indicating an approximate oxidation state of +1 for the o-Me₂TTF radical cation. Graphical Abstract  The X-ray crystallographic structure of the radical cation salt (o-Me₂TTF)I₃ has been determined and its structural properties and synthetic preparation are discussed.      

Crystal and Molecular Structures of Di-1-Adamantylthiophosphinic Chloride, <Emphasis Type="Italic">P</Emphasis>,<Emphasis Type="Italic">P</Emphasis>-Diphenyl-<Emphasis Type="Italic">N</Emphasis>-Benzyl Phosphinothioic- and Selenoic- Amides

Abstract  Synthesis and X-ray structural determination of three phosphorus compounds are reported. (3b) is monoclinic P2(1)/c with a = 11.852(1), b = 12.825(1), c = 12.445(1) ?, β = 103.693(1)o; (4a) and (4b) are monoclinic P2(1)/n with a = 12.1422(16), b = 9.0860(12), c = 14.845(2) ?, β = 96.498(3)o for (4a), and a = 12.2714(16), b = 9.2812(12), c = 14.800(2) ?, β = 97.176(2)o for (4b). They all exhibit distorted tetrahedral geometry about the P atom. Ph₂P(X)NHC₇H₇ (X=S (4a) and X=Se (4b)) show typical P–S and P–Se double bond distances and P–N single bonds, while P–S bond in 1-Ad₂P(S)Cl (3b) is comparable to P–S single bonded probably due to the largeness of 1-adamantyl groups. Graphical Abstract  Synthesis and X-ray structural determination of 1-Ad₂P(S)Cl (3b), Ph₂P(S)NHC₇H₇ (4a) and Ph₂P(Se)NHC₇H₇ (4b) are reported.      

Solvothermal Synthesis and Crystal Structure of a 18-Membered Macrocycle Schiff Base Dinuclear Copper(II) Complex: Cu2(NO3)4(APTY)4 (APTY = 1,5-dimethyl-2-phenyl-4-{[(1E)-pyridine-4-ylmethylene]amino}-1,2-dihydro-3H-pyrazol-3-one)

Abstract  A new 18-membered macrocycle Schiff base dinuclear copper(II) complex: Cu₂(NO₃)₄(APTY)₄ (1) (APTY = 1,5-dimethyl-2-phenyl-4-{[(1E)-pyridine-4-ylmethylene]amino}-1,2-dihydro-3H-pyrazol-3-one), has been successfully synthesized by solvothermal treatment of Cu(NO₃)₂ · 6H₂O with APTY. Compound 1 crystallizes in the triclinic space group P-1 with cell parameters: a = 10.556(2) ?, b = 12.075(2) ?, c = 15.230(3) ?, α = 74.75(3), β = 81.50(3), γ = 70.60(3)°, V = 1762.7(6) ?³, R1 = 0.0493, wR2 = 0.1400, Z = 1, D _calc = 1.455 g/cm³, F(000) = 798, S = 1.009. In the compound molecules, each of the six-coordinated Cu^II atoms are bridged by APTY ligands into 18-membered macrocycle, and each the Cu²⁺ atoms exhibits a significantly distorted octahedral geometry. The crystal packing is stabilized by C–H···O hydrogen-bonding interactions into a three-dimensional supramolecular framework. Index Abstract  A new 18-membered macrocycle Schiff base dinuclear copper(II) complex: Cu₂(NO₃)₄(APTY)₄ (1), has been successfully synthesized by solvothermal treatment (APTY = 1,5-dimethyl-2-phenyl-4-{[(1E)-pyridine-4-ylmethylene]amino}-1,2-dihydro-3H-pyrazol-3-one). The six-coordinated Cu²⁺ atom exhibit significantly distorted octahedral geometry. The crystal packing is stabilized by C–H···O hydrogen-bonding interactions into a three-dimensional supramolecular framework.     

Synthesis and Crystal Structure of a Polymorph of the DMF Solvate of the Dicoppertetracarboxylate Paddlewheel Complex Cu<Subscript>2</Subscript>(p-aminobenzoate)<Subscript>4</Subscript>(DMF)<Subscript>2</Subscript>

Abstract  Reaction between p-aminobenzoic acid (HpABA) and Cu(NO₃)₂ · 2.5H₂O in basic MeOH/DMF affords green crystals of the dicopper paddlewheel complex, Cu₂(pABA)₄(DMF)₂ · 2DMF, 1, identified by single crystal X-ray crystallography: triclinic P-1, with a = 10.3728(2) ?, b = 10.617(2) ?, c = 11.128(2) ?, α = 81.705(3)°, β = 79.984(2)°, γ = 65.965(2)° and Z = 2. The crystal structure of 1 reveals that it is the second polymorph of Cu₂(pABA)₄(DMF)₂ · 2DMF and experiments on the stability of 1 indicate that it can be converted to Form I through desolvation followed by exposure to DMF. Graphical Abstract  Crystal structure of a polymorphic discrete dicoppertetracarboxylate is investigated for the conversion between the two forms influenced by hydrogen bonds.      

A Unusual Bridging Mode of Diphenylhydantoin in Pentaaquabis[(5,5-Diphenylhydantoinato)Potassium]

Abstract  A new complex of diphenylhydantoin, pentaaquabis[(5,5-diphenylhydantoinato)potassium], has been synthesized and the structure has been solved by X-ray diffraction. The crystals are monoclinic, space group C2/c, with a = 34.959(5) ?, b = 8.273(4) ?, c = 11.692(2) ?, β = 109.069(13)°, M _r = 670.80, V = 3196.0(17) ?³, Z = 4 and R = 0.050. The potassium cations are assembled in dimers bridged through the carbonyl O atoms of the anions. The metal atom is in a distorted octahedral coordination environment. Index Abstract  In pentaaquabis[(5,5-diphenylhydantoinato)potassium] the potassium cations are coupled in dimers through the carbonyl O atoms of the anions.      

Synthesis and Crystal Structure of a Mixed-Ligand Cobalt(II) Complex with 2-Aminobenzimidazole

Abstract  The cobalt(II) complex, [Co(abz)₂(SCN)₂] 1, has been synthesized by the reaction of cobalt(II) nitrate with ammonium thiocyanate and abz ligands (abz = 2-aminobenzimidazole), and was fully structurally characterized by elemental analysis, IR spectra, X-ray diffraction and thermogravimetric experiments. It crystallizes in the triclinic P-1 space group with a = 8.6316(10), b = 9.3426(10), c = 13.254(2) ?, α = 95.793(2), β = 95.870(2), γ = 115.7380(10), V = 945.1(2) ?³, and Z = 2. The central cobalt(II) atom is four-coordinated to nitrogen donors from two neutral abz ligands and two isothiocyanate anions respectively, adopting a slightly distorted tetrahedral geometry. In addition, the intermolecular N–H···N and N–H···S hydrogen bonds interactions link the discrete mononuclear units into infinite three-dimensional networks. Index Abstract  The essence sentence of the paper: In the mixed-ligand mononuclear complex, [Co(abz)₂(SCN)₂], the four coordinated cobalt(II) atom exhibits a slightly distort tetrahedron, which is further assembled into 3D infinite network by intermolecular hydrogen interactions.      

Crystal Structure of Meso-tetrakis[4-(pentyloxy)phenyl]porphyrin

Abstract  The crystal structure of the title compound, C₆₄H₇₀N₄O₄, has been determined by single crystal X-ray diffraction methods. The title compound crystallizes in the monoclinic space group P2(1)/c with cell dimensions a = 13.8946(3) ?, b = 16.1069(3) ?, c = 12.1974(2) ?, β = 93.4050(10)°, Z = 2. The porphyrin core to be composed of four pyrrole rings linked through methane carbon bridges. Each molecule lies across a crystallographic inversion center. The porphyrin core is planar, which facilitates π-electron delocalization. The inner nitrogen H atoms are found localized on opposite pyrrole rings and these rings differ structurally from the other two pyrrole rings. The imino H atoms form bifurcated intramolecular hydrogen bonds with the adjacent unprotonated N atoms due to the contract porphyrin core. Graphical Abstract  The crystal structure of meso-tetrakis[4-(pentyloxy)phenyl]porphyrin is reported in this paper.      

Synthesis and Structural Studies of [Na(C7H6O4)(H2O)3](C7H5O4)?·?2H2O

Abstract  The mononuclear complex [Na(C₇H₆O₄)(H₂O)₃](C₇H₅O₄) · 2H₂O has been synthesized and characterized by IR, single crystal X-ray and thermal analysis. The compound crystallizes in the monoclinic space group P2₁ with a = 3.623(2) ?, b = 15.872(6) ?, c = 15.650(5) ?, β = 93.13(4)°, V = 896.6(7) ?³ and Z = 2. The central sodium ion is six coordinated with distorted octahedral geometry by two oxygen atoms from two bridging 3,5-dihydroxybenzoate ligands and four ones from different water molecules. The notable feature of the title complex is the formation of a three-dimensional network, through the combination of coordination bonds, hydrogen bonds and π···π interactions. There are one-dimensional channels in the structure, filled in by water molecules. The compound dehydrates in the temperature range of 70–125 °C and then is stable up to 230 °C. Index Abstract  The mononuclear complex [Na(C₇H₆O₄)(H₂O)₃](C₇H₅O₄) · 2H₂O has been synthesized and characterized by IR, single crystal X-ray and thermal analysis.      

Crystal and Molecular Structures of Tris(1-Methylimidazol-2-yl)Phosphine,Tris(4-Methylthiazol-2-yl)Phosphine and its Sulfide

Abstract  Two crystal structures of tris(azolyl)phosphines, PR₃ [R′ = 1-methylimidazol-2-yl (1) or R′′ = 4-methylthiazol-2-yl (2)], and the crystal structure of the sulfurisation product of 2, R′′₃PS (3), were determined. All compounds crystallise in polar space groups, 1 in the orthorhombic space group Pna2₁ with cell parameters a = 13.9779(15) ?, b = 9.2492(10) ? and c = 10.2439(11) ?; 2 in the trigonal space group, R3c, with a = 15.2383(10) ? and c = 10.5882(13) ? and 3 in the orthorhombic space group, Cmc2₁, with a = 13.466(3) ?, b = 9.308(2) ? and c = 12.207(3) ?. Graphical Abstract  This article presents two crystal structures of tris(azolyl)phosphines and one of a tris(thiazolyl)phosphine sulfide, a compound which show potential for wide application in coordination chemistry due to their multidentate nature.      

Structures of Bis(1-ethylbenzimidazol-2-yl)alkyl Copper(II) Dichlorides: An Unusual Cocrystallization

Abstract  Two structures containing pseudo-tetrahedral Cu(II)N₂Cl₂ coordination complexes are reported. The first molecular structure (A) of the compound, 1,1′bis(1-ethylbenzimidazol-2-yl)propane copper(II) dichloride (triEtBBIM)Cu(II)Cl₂, 1, is reported. The complex crystallized in the triclinic space group P-1 with a = 8.616(3) ?, b = 9.302(3) ?, c = 14.314(4) ?, α = 85.613(6)°, β = 85.170(6)°, γ = 66.117(6)° and V = 1044.1(5) ?³ with Z = 2. The second structure (B) contains 1 and (3,3′bis(1-ethylbenzimidazol-2-yl)pentane) copper(II) dichloride (tetEtBBIM)Cu(II)Cl₂, 2, both of which, cocrystallize in an equal molar ratio with a nitromethane solvate molecule. The complex crystallized in the monoclinic space group P2₁/c with a = 18.876(4) ?, b = 14.975(3) ?, c = 18.344(4) ?, β = 116.75(3)°, and V = 4630.3(16) ?³ with Z = 4. The cocrystallization of such discrete complexes has been coined a chemical Janus. Graphical Abstract  The title complexes contain pseudo-tetrahedral Cu(II)N₂Cl₂ coordination. One of the structures is the result of an unusual cocrystallization, in which two different discrete Cu(II) molecules cocrystallize in an equimolar ratio with a nitromethane solvate molecule.      

Molecular Structure of Quinolin-1-(2-quinolyl)-2-one mesitylimine: An Unusual Amination Product of 2,4,6-Trimethylaniline and 2-Chloroquinoline

Abstract  The molecular structure of quinolin-1-(2-quinolyl)-2-one mesitylimine has been determined. The Buchwald-Hartwig amination of mesitylaniline with two equivalents of 2-chloroquinoline results in dearomatization of one quinoline heterocycle, forming an imine with the mesitylaniline nitrogen and aminating the second 2-chloroquinoline via the cyclic nitrogen. The mesityl and quinoline moieties are nearly perpendicular to the plane of the central quinolyl structure. Rationalization of the imine formation is found by a consideration of the relative stability of the syn and anti conformations of the reaction intermediate. Crystal data: space group P2₁/c, a = 12.609(3), b = 15.010(3), c = 12.456(3) ?, β = 112.68(3)°; V = 2,175.3(8) ?³, Z = 4, R = 0.0649, wR₂ = 0.1498. Graphical Abstract  The amination of mesitylaniline with two equivalents of 2-chloroquinoline results in dearomatization of one quinoline heterocycle, forming an imine with the mesitylaniline nitrogen and aminating the second 2-chloroquinoline via the cyclic nitrogen.      

Crystal Structure of N-(tert-Butyl)-1-(3,5-dioxo-2-phenyltetrahydro-4-isoxazolyl)cyclohexane Carboxamide

Abstract  The crystal structure of N-(tert-butyl)-1-(3,5-dioxo-2-phenyltetrahydro-4-isoxazolyl)-cyclohexane-carboxamide 1 has been determined. The title compound crystallized in the orthorhombic space group pbca with cell parameters, a = 10.6556(6) ?, b = 18.0132(11) ?, c = 19.5513(12) ?, v = 3752.7(4) ?³, Z = 8, D _cal = 1.269 Mg/m³ at T = 120 K. The structure refined by full-matrix least-squares procedures to find R ₁ = 0.0463 and wR ₂ = 0.0937 for 3059 reflections. The soxazole ring isn’t coplanar with the phenyl ring. Index Abstract  The crystal structure of N-(tert-butyl)-1-(3,5-dioxo-2-phenyltetrahydro-4-isoxazolyl)-cyclohexane-carboxamide 1 has been studied.      

Crystal Structure and Magnetic Properties of a Novel Octa-coordinated Manganese(II) Complex

Abstract  The self-assembly and structural characterization of the new manganese(II) [MnL ₂](ClO₄)₂(CH₃OH)_0.5 (1) complex has been achieved. The crystallographic data for the complex 1: Orthorhombic Pbca , a = 16.287(2) ?, b = 21.293(2)?, c = 32.718(3) ?, V = 11,347(2) ?³, Z = 8. The two polydentate ligands strand intertwined each other and around the manganese(II) ions forming a mononuclear complex. The Mn(II) ion is eight-coordinated with the eight donor nitrogen atoms of two ligands to form a distorted square antiprismatic coordination geometry. The magnetic properties investigation indicates that there is a weak antiferromagnetic exchange coupling between the Mn(II) ions of the complex. Index Abstract  An octa-coordinated Mn(II) complex which exhibits a distorted square antiprismatic coordination geometry has been achieved by using a bisbidentate Schiff-base ligand.      

Hydrogen Bonding and Sulfur–Sulfur Interactions in the Crystal Structure of the Radical-Cation Salt (BPDT-TTF)2[W6O19]

Abstract  The synthesis and crystal structure of the salt (BPDT-TTF)₂[W₆O₁₉] is described. The compound crystallizes in the triclinic space group P − 1 with a = 10.927(2) ?, b = 11.904(2) ?, c = 12.660(2) ?, α = 101.261(5)°, β = 115.174(5)°, and γ = 114.434(5)°. The bond length of the central C=C bond in BPDT-TTF is 1.384(17) ?, in accord with an oxidation state of +1 for the BPDT-TTF radical-cations and the observed stoichiometry between BPDT-TTF and [W₆O₁₉]²⁻ which is 2:1. Index Abstract  The X-ray crystallographic structure of the radical cation salt (BPDT-TTF)₂[W₆O₁₉] has been determined and its structural features, including examples of interatomic interactions, as well as its synthetic preparation are discussed.      

Structural, Spectroscopic and Thermal Characterisation of bis (dibenzoylmethanato)Cd(II) Adducts with Dimethylsulfoxide and Water

Abstract  Adducts of cadmium(II) dibenzoylmethate, Cd(dbm)₂X₂ (X = DMSO, H₂O) were synthesized and analyzed by thermogravimetric analysis (TGA), differential-scanning calorimetry (DSC), hot-stage microscopy (HSM), single crystal X-ray diffraction, FTIR and Raman spectroscopy, and elemental analysis. Products obtained by thermal decomposition of the two Cd(II) complexes in oxygen, were used for quantitative analysis of cadmium in the adduct molecules. Single-crystal X-ray diffraction analysis of the DMSO adduct revealed that it has cis configuration. The DMSO adduct crystallizes in P2₁/a space group, a = 17.2494(6) ?, b = 8.3251(4) ?, c = 22.2746(9) ?, β = 93.836(3)°, V = 3191.53(7) ?³, Z = 4. Graphical abstract   Structural, Spectroscopic and Thermal Characterisation of bis (dibenzoylmethanato)Cd(II) Adducts With Dimethylsulfoxide and Water Ivan Halasz, Michaela Horvat, Tomislav Biljan, Ernest Meštrović Two adducts of bis(dibenzoylmethanato)Cd(II), Cd(dbm)₂X₂ (X = DMSO, H2O) have been synthesized and characterized.