Crystal and Molecular Structure of (S)-N-(2-Hydroxyphenyl)pyrrolidine-2-carboxamide

Abstract  

(S)-N-(2-Hydroxyphenyl)pyrrolidine-2-carboxamide was synthesized from Cbz-l-proline through two steps and characterized by NMR and MS. The crystal structure was determined from single-crystal X-ray diffraction data. It crystallizes in the monoclinic space group, P2₁, with unit cell dimensions a = 7.284(6) ?, b = 10.262(9) ?, and c = 7.975(7) ?, α = 90.00°, β = 114.451(14)°, γ = 90.00° and Z = 2. The absolute configuration of the chiral center is determined as S. In the crystal structure, intermolecular and intramolecular hydrogen bonds are responsible for the formation of a 1-dimensional network.     

Synthesis and Crystal Structure of MnII(OAc)2[15-MC MnIII(N)shi-5](Im)3(EtOH)3 (shi3??=?salicylhydroximate, ?OAc?=?acetate, Im?=?imidazole, and EtOH?=?ethanol)

Abstract  

The metallacrown complex Mn^II(OAc)₂[15-MC_Mn^III _(N)shi-5](Im)₃(EtOH)₃ has been synthesized and characterized by single-crystal X-ray diffraction and infrared spectroscopy. The compound crystallizes in the monoclinic space group P2₁/c with a = 24.3326(15) ?, b = 24.0354(15) ?, c = 27.0531(17) ?, α = 90.00°, β = 100.3883(11)°, γ = 90.00°, V = 15562.5(17) ?³, Z = 4, and Z′ = 2. Four of the five manganese(III) ions of the metallacrown ring adopt a distorted octahedral coordination geometry, and the fifth manganese(III) ion is five coordinate and exhibits a distorted square pyramidal environment. The configuration of the manganese(III) ions about the ring follows a pattern of ΔΛΔPP, with P representing planar. In addition, the imidazole units are bound to three separate ring manganese(III) ions, and the imidazole units are directed to the outside of the molecule. A manganese(II) ion is encapsulated in the central core of the molecule, and the central ion is seven coordinate with a face-capped trigonal prismatic geometry.     

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.      

Synthesis,Crystal Structure and IR Spectra of Complexes of Mn(II) by Indole-2-Carboxylic or Isoquinoline-1-Carboxylic Acids and 1,10-Phenanthroline

Abstract  

Two ternary complexes of manganese(II) indole-2-carboxylate (2-IC⁻) or isoquinolinecarboxylate (IQC⁻) with 1,10-phenanthroline (phen) in methanol or in dimethylacetamide (DMA) were synthesized and studied by X-ray diffraction and IR spectra. [Mn(C₉H₆NO₂)₂(C₁₂H₈N₂)₂]·CH₄O (1) crystallizes in the triclinic space group P-1 with cell parameters of a = 10.548(2) ?, b = 14.168(3) ?, c = 14.580(3) ?, α = 62.35(2)°, β = 69.16(2)°, γ = 78.61(2)°, V = 1802.4(6) ?³ and Z = 2; [Mn(C₁₀H₆NO₂)₂(C₁₂H₈N₂)].C₄H₉NO (2) crystallizes in the monoclinic space group P2₁/a with cell parameters of a = 15.304(5) ?, b = 12.871(5) ?, c = 17.421(5) ?, β = 114.39(1), V = 3125(2) ?³ and Z = 4. In 1, Mn is six-coordinate by two bidentate phen ligands and two 2-IC⁻ ligands and exhibits a very distorted octahedral geometry. This complex is solvated by methanol involved in hydrogen bonding. In 2, Mn atom is surrounded by one bidentate phen ligand and two bidentate IQC⁻ ligands. The complex exhibits a distorted octahedral geometry around the Mn^II atom. The crystal structure is completed by a disordered DMA solvate molecule. The IR spectra of both compounds are slightly different in the range 4000–2400 cm⁻¹ which may be attributed to hydrogen bond lack in 2.     

Two-Dimensional Layers Using Different Combinations of Hydrogen Bonded Rings in Three Ammonium Carboxylate Salts

Abstract  

The crystal structure of the ammonium carboxylate salts (cyclohexylammonium)₂·(terephthalate) (1), (cyclohexylammonium)₂·(trans-1,4-cyclohexanedicarboxylate) (2) and (cyclododecylammonium)₂·(trans-1,4-cyclohexanedicarboxylate) (3) were determined by low temperature single crystal X-ray diffraction. The molecular salts were prepared by solution crystallization of the carboxylic acids with the respective amines in a 1:2 stoichiometric ratio. The crystal structure of 1 belongs to the monoclinic space group Cc with a = 11.5643(7) ?, b = 22.8180(13) ?, c = 8.4163(5) ? and β = 117.020(2)°. The crystal structure of 2 belongs to the monoclinic space group P2₁/n with a = 16.9546(10) ?, b = 6.4352(4) ?, c = 19.3948(12) ? and β = 94.677(4)°. The crystal structure of 3 belongs to the monoclinic space group P2₁/c with a = 8.1714(5) ?, b = 34.3887(17) ?, c = 11.0230(6) ? and β = 95.790(4)°. The changes in cation and anion species produces three distinct types of layers, with corresponding changes in the hydrogen bonded ring patterns linking the ionic species together using charge-assisted N⁺–H···O⁻ hydrogen bonds.     

Synthesis and Crystal Structure of an Iodobismuthate Incorporating Both a Cationic and Anionic Bi (III) Complex Ion

Abstract  

A new iodobismuthate of formula [BiI₂(terpy)₂][BiI₄(terpy)] (terpy = 2,2′:6′,2′′-terpyridine), was prepared solvothermally in an ethanolic mixture composed of bismuth (III) iodide, terpy, and ruthenium (III) iodide. The compound crystallizes in the space group P [`1] \bar{1} , with Z = 2, a = 9.8491(4) ?, b = 15.4181(7) ?, c = 17.5323(8) ?, α = 89.8140(10)°, β = 80.4160(10)°, γ = 77.9020(10)°. Single-crystal X-ray analysis reveals that the compound is composed of a [BiI₂(terpy)₂]⁺ cation and a [BiI₄(terpy)]⁻ anion. It is an uncommon example where an iodobismuthate cation and anion are simultaneously incorporated into the same crystal structure.     

Synthesis and Crystal Structure of Three New Metal-Organic Frameworks in the Ln(III)/2,6-Pyridinedicarboxylate System

Abstract  

In this paper, three new metal-organic frameworks, synthesized by hydrothermal technique, are described. The compounds crystallize in triclinic space group P − 1 with cell parameters, respectively equal to (1) [La(H₂O)₃(dipic)]₂(C₂O₄) · 2H₂O a = 7.9990(1) ?, b = 8.3380(4) ?, c = 9.6180(5) ?, α = 98.194(5)°, β = 100.438(3)°, γ = 102.437(3)°, (2) [Eu(H₂O)₂(C₂O₄)]₂(dipic) · 3H₂O a = 8.2170(6) ?, b = 10.5900(8) ?, c = 13.0670(3) ?, α = 93.951(3)°, β = 103.393(5)°, γ = 107.797(6)°, and (3) [Ce₃(dipic)₃(Hdipic)(SO₄)(H₂O)₃] · 4H₂O a = 11.655(1) ?, b = 12.886(1) ?, c = 16.139(2) ?, α = 106.369(8)°, β = 92.90(1)°, γ = 115.787(7)°. They differ by their dimensionality mono-dimensional for (1), tri-dimensional for (2) and bi-dimensional for (3).     

Study of Hydrogen Bonding in <Emphasis Type="Italic">N</Emphasis>′-(4,6-disubstituted-pyrimidin-2-yl)-<Emphasis Type="Italic">N</Emphasis>-[2-(2,4-dichlorophenoxypropionyl)]thiourea

Abstract  

Two of N′-N′-(4,6-disubstituted-pyrimidin-2-yl)-N-[2-(2,4-dichlorophenoxypropionyl)]thiourea (4a-4b) had been synthesized and their crystal structures had been determined by X-ray diffraction method. 4a crystallizes in the triclinic space group P-1, with a = 8.053(12) ?, α = 102.84(2)°, b = 10.541(16) ?, β = 106.99(2)°, c = 12.461(19) ?, γ = 94.615(19)°, and D _c  = 1.470 mg/m³ for Z = 2. 4b crystallizes in the triclinic space group P-1, with a = 7.939(5) ?, α = 105.302(10)°, b = 10.183(7) ?, β = 105.729(9)°, c = 12.764(9) ?, γ = 90.698(11)°, and D _c  = 1.517 mg/m³ for Z = 2.     

A Facile Synthesis and Crystallographic Analysis of Seven Trityl Phosphorus Compounds and Two Nickel(II) Phosphine Side-Products

Abstract  The syntheses and X-ray analyses of triphenylmethyl (trityl=Tr) phosphorus compounds are reported and the structural similarities, differences and ³¹P chemical shifts compared. A series of seven trityl-substituted phosphorus-containing compounds have been characterized by single crystal X-ray diffraction. Ph₃CPPh₂, 1, a bulky P(III) compound crystallizes in the triclinic space group , a = 7.5624(6) ?, b = 9.5470(8) ?, c = 16.9722(14) ?, α = 83.4720(10)°, β = 80.541(2)°, γ = 68.1580(10)°, the borane complex of 1, 2, Ph₃CPPh₂(BH₃) crystallizes as monoclinic colorless crystals, P2₁/c, a = 10.0972(12) ?, b = 9.6955(12) ?, c = 25.197(3) ?, β = 90.258(2)°. The analogous methyl substituted, 3, Ph₃CPMe₂(BH₃) is monoclinic, C₂/c, a = 15.628(3) ?, b = 12.770(3) ?, c = 18.406(4) ?, β = 103.968(3)°. Compounds 4–7 are trityl substituted P(V) compounds: Ph₃CP(Ph)(O)(OH), 4, crystallizes in the triclinic space group , a = 8.9847(18) ?, b = 9.7443(19) ?, c = 12.786(3) ?, α = 72.045(3)°, β = 72.031(3)°, γ = 78.769(3)°. Esterification of 4 affords TrCP(O)(Ph)OBn 5, space group, P2₁/c, a = 7.9196(5) ?, b = 31.701(2) ?, c = 19.8062(13) ?, β = 99.7750(10)°. A phosphonate diester was also characterized, Ph₃CP(O)(OEt)₂, 6, triclinic, , a = 7.9521(17) ?, b = 9.2205(19) ?, c = 14.471(3) ?, α = 85.906(4)°, β = 83.031(4)°, γ = 68.283(4)°. Treatment of the trityl H-phosphinic acid, Ph₃CPO₂H_2, with elemental selenium yields yellow crystals of 7, [Ph₃CP(O)(OH)Se]_2, P2₁/c, a = 9.0603(4) ?, b = 22.3652(11) ?, c = 16.9134(7) ?, β = 107.035(2)°. In our efforts to isolate a nickel-phosphine complex, two Ni(II) complexes were crystallographically analyzed, [Ni(OP(H)Ph₂)₆]₂BF₄ ⁻ 8 and 9. Complex 8 with an uncoordinated BF₄ ⁻ ion crystallizes as yellow orthorhombic crystals, Pbca, a = 18.8247(12) ?, b = 18.5518(12) ?, c = 21.0976(14) ?, while crystals of 9 are trigonal, , a = b = 13.1545(12) ?, c = 68.461(9) ?. Graphical Abstract  The syntheses and X-ray analyses of triphenylmethyl (trityl=Tr) phosphorus compounds are reported and the structural similarities, differences and ³¹P chemical shifts compared.      

Characterization of Molecular Complexes of 1,4-Naphthoquinone Derivatives

Abstract  

The structures of sulphur atom tethered quinone containing flexible carboxylic acid (3-methyl-1,4-dioxo-1,4-dihydronaphthalen-2-ylsulfanyl)acetic acid (1) and its molecular complex with 4,4′-bipyridine (3) are determined. The compound 1 crystallizes in P-1 (triclinic, a = 7.5378(6) ?, b = 7.6413(7) ?, c = 10.3101(9) ?; α = 89.779 (7)°, β = 81.042 (5)°, γ = 89.101(7)°) and the molecular complex 3 crystallises in P2(1)/n (monoclinic, a = 9.3383(7) ?, b = 3.970(3) ?, c = 42.130(3) ?, β = 91.056(5)°) space groups, respectively. The R₂²(8) type hydrogen bonding between dicarboxylic acid groups present in the parent compound 1 is lost on interaction with 4, 4′-bipyridine; in the molecular complex 3 R₂²(7) type of O···H–C and O–H···N interactions are present between the pyridine rings and carboxylic acid groups. The molecular complex (4) derived from 3-carboxymethylsulfanyl-1,4-dihydroxynaphthalen-2-yl-sulfanyl) acetic acid (2) with triphenylphosphine oxide in 1:2 ratio, crystallises in C2/c space group have monoclinic, a = 26.0494(13) ?, b = 10.5402(5) ?, c = 17.1023(8) ?, β = 108.719 (5)°). The triphenylphosphine oxide molecules are preferentially held by O–H···O interactions between carboxylic acid and P=O bond.     

Synthesis and Crystal Structures of Dioxomolybdenum(VI) Complexes with ONS-Donor Ligands

Abstract  

Three dioxomolybdenum complexes namely dioxo(5-chlorosalicylaldehyde thiosemicarbazonato) dimethylsulfoxide molybdenum(VI) (C1), dioxo(5-chlorosalicylaldehyde 2-ethylthiosemicarbazonato) dimethylsulfoxide molybdenum(VI) (C2) and dioxo(5-chlorosalicylaldehyde N-phenylthiosemicarbazonato) dimethylsulfoxide molybdenum(VI) (C3) were prepared. The compounds all crystallize in the triclinic space group P-1 with a = 7.3184(3) ?, b = 7.5035(3) ?, c = 14.9713(6) ?, α = 85.005(2)°, β = 85.616(2)°, γ = 66.987(2)° for C1, a = 8.2339(1) ?, b = 10.1739(1) ?, c = 10.4017(1) ?, α = 78.486(1)°, β = 89.312(1)°, γ = 81.730(1)° for C2, a = 7.0591(1) ?, b = 9.5603(1) ?, c = 14.5762(2) ?, α = 76.280(1)°, β = 81.351(1)°, γ = 81.985(1)° for C3. In general, the overall geometry of these complexes can be regarded as a distorted octahedron with the tridentate thiosemicarbazonato ligands (L²⁻) bonded to the MoO₂ ²⁺ core, with the imine nitrogen, phenoxyl oxygen, sulfur atom and one of the terminal oxygen atoms of the dioxomolybdenum occupying the equatorial position. The sixth coordination site is occupied by the dimethylsulfoxide (DMSO) solvent molecules. The adjacent molecules of C1 are linked by N–H···N intermolecular hydrogen bonding, forming polymeric chains that run parallel to the bc plane. On the other hand, C2 is a discrete molecule while the molecules of C3 associate via weak N–H···O hydrogen bonding interaction to form a polymeric chain that runs along the a-axis.     

Synthesis and Structure of bis(β-Diketiminate) Chromium(II) Complexes

Abstract  

The new ligand 2,4-N,N′-bis(napthylamino)-pent-2-ene (L^napth) (1) has been synthesized and crystallizes in space group P2₁2₁2₁ with crystal cell parameters a = 8.196(3) ?, b = 9.119(3) ?, c = 25.746(10) ?, V = 1924.3(12) ?³ and Z = 4. The complexes bis[2,4-pentane-N,N′-bis(napthyl)ketiminato] chromium(II) (2), bis[2,4-pentane-N,N′-bis(isopropylphenyl)ketiminato] chromium(II) (3), and bis[2,4-pentane-N,N′-bis(tertbutylphenyl)ketiminato] chromium(II) (4) were synthesized and structurally characterized. Complex 2, the first complex reported with a bis(napthyl) β-diketiminate ligand, crystallizes in space group P − 1 with crystal cell parameters a = 12.0824(15) ?, b = 12.2462(16) ?, c = 14.8975(19) ?, α = 87.035(2)°, β = 80.615(2)°, γ = 62.756(2)°, V = 1932.9(4) ?³ and Z = 2. Complex 3 crystallizes in space group P2₁/n with crystal cell parameters a = 13.088(3) ?, b = 22.222(5) ?, c = 14.206(3) ?, β = 102.310(4)°, V = 4036.6(17) ?³ and Z = 4. Complex 4 crystallizes in space group P2₁/n with crystal cell parameters a = 20.831(6) ?, b = 11.575(4) ?, c = 21.373(7) ?, β = 107.241(5)°, V = 4922(3) ?³ and Z = 4. The degree of twist between the ligand planes is dependent on the steric bulk of the ligand.     

Crystal Structures of Two Palladacycles from the C–H Activation of 2-(Thiophen-2-yl)pyridine

Abstract  

A C,N-bound palladacycle dimer has been synthesised by reaction of 2-(thiophen-2-yl)pyridine, LH, with palladium acetate in acetic acid. Characterisation by single crystal X-ray diffraction showed the palladacycle dimer, [(L)Pd(OAc)]₂, to crystallise in the monoclinic space group P2₁/n with cell parameters a = 9.5853(1) ?, b = 19.1332(3) ?, c = 12.3889(2) ?, β = 103.732(1)°. Reaction of [(L)Pd(OAc)]₂ with triphenylphosphine afforded a trans-substituted monomeric complex, [(L)PdPPh₃(OAc)] which was also analysed using single crystal X-ray diffraction. [(L)PdPPh₃(OAc)] crystallises in the monoclinic space group P2₁/c with cell parameters a = 9.4839(1) ?, b = 11.0427(2) ?, c = 26.0770(4) ?, β = 95.022(1)°.     

Crystal Structure and Conformational Analysis of 4-[(<Emphasis Type="Italic">p</Emphasis>-<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>-Dimethylamino)Benzylidene]-2-Phenyloxazole-5-One

Abstract  

Molecular and crystal structure of 4-[(p-N,N-dimethylamino)benzylidene]-2-phenyloxazol-5-one, C₁₈H₁₆N₂O₂, have been determined by single crystal X-ray diffraction study. The title compound is monoclinic, with a = 12.1704(23) ?, b = 3.9810(5) ?, c = 30.9603(56) ?, β = 101.176(15)°, Z = 4, D _x = 1.32 g/cm³, μ(Mo Kα) = 0.087 mm⁻¹, and space group is P12₁/c1. The structure was solved by direct methods and refined to a final R = 0.047 for 3166 reflections with I > 2σ(I). The crystal structure is stabilized by C–H⋯O and C–H⋯N type intra-molecular, C–H⋯O type inter-molecular interactions. To enlighten the flexibility and the geometric isomerism (E or Z) of the title compound, the selected torsion angle is varied from −180 to 180° in every 10° separately and molecular energy profile is calculated and analyzed.     

Synthesis, Crystal Structure and Density Functional Theory Study of (2-(2-Hydroxyphenyl)benzimidazolate-based Al(III) Complex Cocrystallized by DMF Solvate and Neutral (2-(2-Hydroxyphenyl)benzimidazole

Abstract  

The aluminium(III) complex with 2-(2-hydroxyphenyl)benzimidazole, namely [Al₂(μ-OH)₂L₄)]·6DMF·2HL (1·6DMF·2HL) (HL = 2-(2-hydroxyphenyl)benzimidazole), has been synthesized and characterized by X-ray crystallography. It crystallizes in monoclinic space group C2/c with cell parameters a = 23.6752(13) ?, b = 20.8253(12) ?, c = 18.1645(10) ?, α = 90°, β = 91.929(1)°, γ = 90°, Z = 4, V = 8950.8(9) ?³. The dimeric structure of 1, featuring [Al₂(μ-OH)₂] core has been studied with the density functional theory level (DFT) calculation and molecular orbital analyses.     

Synthesis and Crystal Structure of a Fe(III) Complex with an Isonicotinyl Hydrazone Ligand, [Fe(N-Isonicotinamidosalicylaldimine)Cl<Subscript>2</Subscript>]

Abstract  

A new complex [Fe(N-isonicotinamidosalicylaldimine)Cl₂] has been synthesized by template reaction at room temperature and structurally characterized by X-ray single-crystal analysis. The complex crystallizes in triclinic crystal system, Pī space group, a = 7.273(6) ?, b = 10.015(8) ?, c = 10.479(8) ?, α = 71.067(10)°, β = 89.964(11)°, γ = 75.528(10)°, V = 696.4(9) ?³ and Z = 2. The coordination geometry around the Fe(III) ion is a distorted trigonal bipyramid with a O₂N₁Cl₂ donor set. In the crystal structure, N–H···Cl, C–H···O and C–H···Cl hydrogen bonds and π···π stacking interactions involving aromatic and unclosed π-systems link the molecules to form supramolecular double layers.     

Synthesis and Crystal Structure of a Compound with Two Conformational Isomers: 2-(2,6-Difluorobenzamido)-4-methyl-<Emphasis Type="Italic">N–o</Emphasis>-tolylthiazole-5-carboxamide

Abstract  

The single crystal of the title compound (C₁₉H₁₅F₂N₃O₄S) with two conformational isomers was obtained from the solution of the title compound dissolved in the ethyl acetate by slow evaporation at room temperature. The crystal is Orthorhombic, space group Pca2(1) with a = 21.840(2) ?, b = 7.5321(8) ?, c = 22.365(2) ?, α = 90.00°, β = 90.00°, γ = 90.00°, empirical formula is C₃₈H₃₀F₄N₆O₄S₂, Mr = 774.80, V = 3,679.2(6) ?³, Z = 4, D _c = 1.399 g/cm³, μ(MoKα) = 0.215 mm⁻¹, F(000) = 1,600, S = 1.032, the final R = 0.0328, wR ₂ = 0.0811 for 4,708 observed reflections with I > 2σ(I). In the unit cell, there are two independent molecules having only slightly different bond lengths, torsion angles and the corresponding dihedral angles of the two molecules are also different. In the crystal structure, molecules are linked through aromatic π–π stacking and intermolecular N–H···N hydrogen bonds interactions, forming 1D chain structure.     

Crystal Structure and Photoluminescent Properties of Two Cadmium(II) Complexes with Orotic Acid

Abstract  

Assembly of orotic acid (2,6-dioxo-1,2,3,6-tetrahydropyrimidine-4-carboxylic acid, H₃dtpc) and Cd(OAc)₂·2H₂O gave rise to two complexes [Cd₂(H₂dtpc)₂(H₂O)₆] (I) and [Cd(H₂dtpc)(bpy)(H₂O)]_n (II) (bpy = 2,2′-bipyridine). Complex (I) and (II) have been characterized by X-ray single crystal diffraction, IR, PXRD, TGA and fluorescence spectra. Structural analyses reveal that (I) is a binuclear structure, and complex (II) possesses a one-dimensional infinite zig-zag chain architecture and the chains are further assembled into 2D supramolecular network by strong hydrogen bonding interactions. Crystal data for (I): Monoclinic, space group P2(1)/n, a = 9.3221(19) ?, b = 6.6315(13) ?, c = 15.322(3) ?, β = 102.31(3)°, V = 925.4(3) ?³, Z = 4, R1 = 0.0269, and wR2 = 0.0604; for (II): Monoclinic, space group P2(1)/c, a = 9.9880(2) ?, b = 14.5085(2) ?, c = 11.6957(2) ?, β = 107.976(2)°, V = 1612.10(5) ?³, Z = 4, R1 = 0.0234 and wR2 = 0.0554.     

Preparation, Crystal Structure and Spectroscopic Properties of Dimeric [Zn(2-bromobenzoato)2(phenazone)]2 and Monomeric [Zn(2-bromobenzoato)2(thiourea)2]·2H2O

Abstract  

The binuclear zinc complex bis(2-bromobenzoato-O)-bis(μ ₂ -2-bromobenzoato-O,O′)-bis(phenazone-O)-dizinc(II) (I) and the mononuclear dihydrate bis(2-bromobenzoato-O)-bis(thiourea-S)-zinc(II) (II) have been synthesized and characterized by means of elemental analysis and spectroscopic methods (IR, ¹H and ¹³C NMR, EDS). The solid state structures of both compounds were determined by single-crystal X-ray diffractometry. Compound [Zn(2-BrC₆H₄COO)₂(phen)]₂ (phen—phenazone) (I) crystallized as a dimeric compound with a triclinic lattice (space group P − 1), where both zinc atoms, interconnected by two carboxylate groups, possess a distorted tetrahedral coordination environment. The crystallographic data of complex I: a = 9.9410(3) ?, b = 10.7309(3) ?, c = 12.9237(4) ?, α = 93.6004(17)°, β = 92.5898(11)°, γ = 116.2192(16)°, V = 1230.26(6) ?³, Z = 1. Complex [Zn(2-BrC₆H₄COO)₂(tu)₂]·2H₂O (tu—thiourea) (II) crystallized with an orthorhombic lattice (space group Aba2) as a monomeric compound, where the coordination environment of the central zinc atom is a distorted tetrahedron. The crystallographic data of complex II are: a = 9.8595(3) ?, b = 19.7052(5) ?, c = 12.5908(3) ?, V = 2446.18(11) ?³, Z = 4. The modes of the carboxylate binding were assigned from the IR spectra using the magnitude of the separation between the carboxylate stretches (Δ), which correlated well with the crystal structures. The computed theoretical IR spectrum agreed well with the experimental data.     

Synthesis and Structural Comparison for a Series of Cr(II) (iodo) NacNac Complexes

Abstract  A series of complexes of the form [bis(2,6-diisopropylphenyl)pentane-2,4-ketiminato](iodo)(solvent) chromium were synthesized and structurally characterized (solvent = tetrahydrofuran, acetonitrile, α-picoline). The tetrahydrofuran adduct crystallized in the P2₁/n space group with the crystal cell parameters a = 17.628(6) ?, b = 10.218(3) ?, c = 20.646(7) ?, β = 109.209(4)°, V = 3512(2) ?³ and Z = 4. The acetonitrile adduct crystallized in the P2₁/c space group with the crystal cell parameters a = 16.104(7) ?, b = 11.965(5) ?, c = 18.201(8) ?, β = 116.091(6)°, V = 3150(2) ?³ and Z = 4. The α-picoline adduct crystallized in the C2/c space group with the crystal cell parameters a = 39.982(9) ?, b = 11.637(2) ?, c = 16.560(4) ?, β = 108.085(4)°, V = 7325(3) ?³ and Z = 8. For each compound, the coordination around each chromium center is square planar with varying degrees of distortion. Graphical Abstract  A series of Cr(II) complexes of the form LCrI(S) (where L = nacnac = β-diketiminate; S = solvent) were synthesized and structurally characterized.