The coordination of 2-(hydroxymethyl)pyridine to oxorhenium(V). Synthesis and crystal structure of [ReOCl(C<Subscript>5</Subscript>H<Subscript>4</Subscript>N–CH<Subscript>2</Subscript>O)<Subscript>2</Subscript>]

The title compound was prepared from the reaction of (n-Bu₄N)[ReOCl₄] with a twofold molar excess of 2-(hydroxymethyl)pyridine in benzene. It has a distorted octahedral coordination geometry, and it crystallizes in the monoclinic space group P2₁/n, with cell dimensions a = 14.4545(4), b = 7.0168(2), c = 14.5269(4) Å, = 116.995(1), V = 1312.85(7) ų, and Z = 4.     

Synthesis and Structural Characterization of [2-(2-1H-Imidazoly)-1H-imidazolium nitrate] and [2-(2-1H-Imidazoly)-2H-imidazolium phthalyl glycinate] Based on the 2,2′-bi-1H-Imidazole Molecule

Abstract  

Two new compounds (H₃biim)(NO₃)(1) and (H₄biim)(phthgly)₂ (2) (H₂biim=biimidazole; Hphthgly=N-phthaloylglycine) have been synthesized and characterized by luminescence and single crystal X-ray diffraction study. Compound 1 crystallizes in the monoclinic space group C2/c, where a = 14.8078(15), b = 5.9233(6), c = 20.028(2) ?, β = 92.7910(10)°, V = 1754.6(3) ?³ and Z = 8. Compound 2 crystallizes in the monoclinic space group P2(1)/n, where a = 15.3775(14), b = 5.3200(6), c = 6.4689(18)?, β = 115.418(2)° V = 1216.9(2)?³ and Z = 4. In 1, the N–H groups of H₃biim⁺ and the oxygen atoms of NO₃ ⁻ are linked by hydrogen bonds leading to H₃biim⁺(N,N)–R₂²(10) and N–H···O interactions forming infinite 1D helical chains along the b-axis. Compound 2 consists of a planar diprotonated biimidazole moiety and two phthgly anions which connect to the dication by hydrogen bonds phthgly⁻(O,O)–R₂²(9).     

Structures and crystallization behavior of cis-α-[Co(trien)(NO2)2]·ClO4 (I), cis-β-[Co(trien)(NO2)2]Br·2H2O (II), and cis-β-[Co(trien)(NO2)2]·ClO3 (III)

Structures, conformations, and crystallization behavior of compounds cis--[Co(trien)(NO₂)₂]·ClO₄ (I), cis--[Co(trien)(NO₂)₂]Br·2H₂O (II), and cis--[Co(trien)(NO₂)₂]·ClO₃ (III) are reported. Compound (I) crystallized in space group Pbca, with a = 12.3323(9), b = 13.0265(9) and c = 18.1597(13) Å; compound (II) crystallized in space group Pca2₁, with a = 8.1844(7), b = 14.7011(14) and c = 12.4875(12) Å, while compound (III) also crystallized in space group Pca2₁, with a = 12.4897(8), b = 8.8499(6) and c = 12.6500(8) Å. In all three cases, the Co(III) ions were six-coordinated with nitrogens from trien and two nitrates. Inter- and intramolecular hydrogen bonding interactions are discussed to explain the conglomerate versus racemate crystallization behavior adopted by these three compounds, with comparison of their known analogue compounds of cis-/-[Co(trien)(NO₂)₂]X, where X = halide and NO^– ₃. For the cis--[Co(trien)(NO₂)₂]⁺ cation, the conformation of the cation itself determines the intramolecular hydrogen bonding pattern, and the interaction of counteranions can be ignored, while in cis--[Co(trien)(NO₂)₂]·ClO₄, the perchlorate interrupts the intramolecular hydrogen bonding pattern observed in the halide analog.     

Synthesis,Crystal Structure and Bioactivities of <Emphasis Type="Italic">N</Emphasis>-(2,6-Difluorobenzoyl)-<Emphasis Type="Italic">N</Emphasis>′-[5-(Pyrid-4-yl)-1,3,4-Thiadiazol-2-yl]Urea

Abstract N-(2,6-difluorobenzoyl)-N′-[5-(pyrid-4-yl)-1,3,4-thiadiazol-2-yl]urea, 3, has been synthesized by reaction of 2-amino-5-(pyrid-4-yl)-1,3,4-thiadiazole with 2,6-difluorobenzoyl isocyanate, and its structure was characterized with X-ray crystallographic, NMR, MS and IR techniques. It crystallizes in the triclinic space group P − 1, with a = 7.0821(9) ?, b = 9.4896(13) ?, c = 11.6594(15) ?, α = 82.311(2)°, β = 82.328(2)°, and γ = 87.641(2)°. In the title compound, the urea scaffold in each molecule is essentially planar due to the presence of intramolecular N–H···O hydrogen bond. The molecules are linked by intermolecular complementary N–H···O hydrogen bonds into centrosymmetric R ₂²(8) dimers. Intermolecular π–π stacking interactions are also present. The preliminary bioassay shows that the title compound exhibits excellent fungicidal activities against Rhizoctonia solani, Botrytis cinerea and Dothiorella gregaria. Index Abstract N-(2,6-difluorobenzoyl)-N′-[5-(pyrid-4-yl)-1,3,4-thiadiazol-2-yl]urea has been synthesized and characterized with X-ray crystallographic, NMR, MS and IR techniques. The preliminary bioassay shows that the title compound exhibits excellent fungicidal activities.      

Structure of bis[α-(1,2,4-triazole-1-yl)-acetophenone] dichorozinc(II) complex [ZnCl2(C2H2N3CH2COPh)2]

The crystal and molecular structure of [ZnCl₂(N⁴-trzCH₂COPh)₂] (trz = 1,2,4-triazole) has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group C2/c, with lattice parameters a = 26.7892(4) Å, b = 4.9392(2) Å, c = 20.7872(1) Å, = 127.517 (1), and z = 4. The complex has C ₂ symmetry. The coordination geometry of each Zn atom is distorted tetrahedral formed by two Cl atoms and two tertiary N atoms of the -(1,2,4-triazole-1-yl)-acetophenone ligands. The two equivalent Zn–Cl and Zn–N bonds form bond angles around the Zn(II) atom in the range 101.4(1)–120.8(1). C–H O intermolecular interactions link the molecules in infinite chains in the [101] direction.     

Synthesis and Crystal Structure of [Cu(BDBPH)(ClO<Subscript>4</Subscript>)<Subscript>2</Subscript>] (BDBPH = Butane-2,3-dione bis(2′-pyridylhydrazone)

Abstract  

Butane-2,3-dione bis(2′-pyridylhydrazone) (BDBPH), a Schiff-base condensate, was synthesized by 1:2 mol ratio condensation of butane-2,3-dione with 2-hydrazino pyridine in dehydrated methanol. BDBPH has been characterised by C, H and N microanalyses, FT-IR, ¹H NMR and UV–Vis spectra. Reaction of 1:1 stoichiometric proportion of BDBPH with copper(II)perchlorate hexahydrate in methanol affords a mononuclear copper(II) complex, [Cu(BDBPH)(ClO₄)₂] (1). 1 crystallizes in the monoclinic space group P [`1] \overline{1} with a = 8.4230(2), b = 9.7869(3), c = 12.3508(3) ?, α = 103.784(2), β = 90.900(2), γ = 94.906(2)^°, V = 984.51(5) ?³ and Z = 2. The copper(II) compound is octahedral and one-electron paramagnetic. Bond Valence Sum (BVS) model calculation was also performed to assign the oxidation number of the copper center.     

Synthesis and Crystal Structures of <Emphasis Type="Italic">N</Emphasis>′-(5-Bromo-2-hydroxy-3-methoxybenzylidene)-4-methoxybenzohydrazide and 4-{[1-(5-bromo-2-hydroxy3-methoxyphenyl)methylidene]amino}-1-methyl-2-phenyl-1,2-dihydropyrazol-3-one

Abstract  

Two Schiff bases, N′-(5-bromo-2-hydroxy-3-methoxybenzylidene)-4-methoxybenzohydrazide (1) and 4-{[1-(5-bromo-2-hydroxy3-methoxyphenyl)methylidene]amino}-1-methyl-2-phenyl-1,2-dihydropyrazol-3-one (2), have been synthesized by the reaction of 5-bromo-3-methoxysalicylaldehyde with 4-methoxybenzohydrazide and 4-aminoantipyrine, respectively. The compounds were characterized by elemental analysis and X-ray single crystal determination. Compound (1) crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a = 14.919(1), b = 8.249(2), c = 41.515(4) ?, β = 111.054(2)°, V = 4768.1(13) ?³, Z = 12, R ₁ = 0.0765, and wR ₂ = 0.1733. Compound (2) crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a = 7.826(1), b = 13.791(1), c = 17.090(2) ?, β = 100.137(2)°, V = 1815.7(3) ?³, Z = 4, R ₁ = 0.0334, and wR ₂ = 0.0736. Both molecules of the compounds display E configuration with respect to the C=N double bonds. In the crystal structure of (1), molecules are linked via intermolecular N–H···O hydrogen bonds, forming chain structure along the a axis. In the crystal structure of (2), molecules are linked via weak Br···O interactions, forming chain structure along the c axis.     

The molecular structure of acetato[2-(pyridin-2′-yl)phenyl]mercury(II)

The crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in the monoclinic crystal system witha=8.152(4),b=17.994(7),c=8.634(9) Å, =108.92(5)°, space group P2₁/c (N:14),V=1198.02 ų,Z=4. The mercuryl(II) atom forms two strong, almost colinear bonds (bond angle 176.1(4)°) with a carbon of the phenyl ring (Hg–C=1.99(1) Å) and one of the acetate oxygen atoms (Hg–O(1)=2.005(7) Å). These primary bonds are supplemented by secondary intramolecular interactions with the pyridine nitrogen (Hg...N=2.727(9) Å) and the other acetate oxygen (Hg...O(2)=2.925(8) Å), although the latter is very weak and the acetate anion therefore practically monodentate. Weak additional intermolecular Hg–C and Hg–O(1)interactions contribute to the lattice structure.     

The Crystal Structure of {[Pt(9S3)Cl<Subscript>2</Subscript>]<Subscript>2</Subscript>[Pt(9S3)<Subscript>2</Subscript>]}Cl<Subscript>2</Subscript>·4H<Subscript>2</Subscript>O: An Improved Synthesis of [Pt(9S3)Cl<Subscript>2</Subscript>]

Abstract  

We wish to report the crystal structure for a solid-state solution, {[Pt(9S3)Cl₂]₂[Pt(9S3)₂]}Cl₂·4H₂O (1), which contains two different complexes of Pt(II) with the trithiacrown 9S3 (1,4,7-trithiacyclononane). One complex [Pt(9S3)Cl₂] is neutral and contains a Pt(II) center with a single 9S3 ligand and two coordinated chloro ligands. The second Pt(II) complex is a dication and contains two coordinated 9S3 ligands and two non-coordinating chloride anions. There are two crystallographically equivalent [Pt(9S3)Cl₂] complexes present for every single [Pt(9S3)₂]²⁺ cation. Four water solvent molecules are also present. In the neutral complex ([Pt(9S3)Cl₂], the Pt(II) center is surrounded by a cis-[S₂Cl₂ + S₁] ligand environment formed by the two chloro ligands and two of the three sulfur atoms from the 9S3 ligand. These two sulfurs are positioned 2.225(2) and 2.242(2) ? from the Pt(II), but the third sulfur shows a long distance interaction at 3.311(2) ? to form an elongated square pyramidal structure. This axial Pt–S distance is the longest observed in 57 crystal structures of Pt(II) 9S3 complexes. The cation [Pt(9S3)₂]²⁺ displays two centrosymmetrically coordinated 9S3 ligands forming a [S₄ + S₂] environment with an elongated octahedral shape. In the dication, the two equatorial Pt–S distances are 2.297(2) and 2.306(2) ? with the axial sulfur at 3.065(2) ?. The most interesting intermolecular aspects of the structure are hydrogen bonding interactions between two of the water molecules and two chloride counter-ions, resulting in a nearly square O₂Cl₂ ring. This ring shares an edge with a six-membered ring formed by four waters and two chlorides which are hydrogen bonded. The hydrogen bonding interactions, which result from the presence of water in the crystal, appear to be an important component in stabilizing the lattice for the unusual solid-state solution structure. Crystal Data for (1): P2 ₁ /n, a = 7.8327(10) ?, b = 25.152(4) ?, c = 12.382(2) ?, V = 2314.3(6) ?³, Z = 2. We also report an improved synthetic procedure for the preparation of two thiacrown complexes [Pt(9S3)Cl₂] and [Pt(10S3)Cl₂], which are commonly used as precursors for other heteroleptic thioether complexes. The new syntheses proceed at room temperature without the need for long reflux times and produce large crystals which are easily isolable without filtration. The simplicity of these new preparations results in improved yields over previously employed methods.     

Preparation,characterisation, and crystal structure analysis of (2<Emphasis Type="Italic">E</Emphasis>,2′<Emphasis Type="Italic">E</Emphasis>)-3,3′-(1,4-phenylene)bis(1-(2-aminophenyl)prop-2-en-1-one

A novel bis-chalcone, (2E,2′E)-3,3′-(1,4-phenylene)bis(1-(2-aminophenyl)prop-2-en-1-one) is synthesized through a base catalyzed Claisen-Schmidt condensation reaction of terephthalaldehyde with 2-aminoacetophenone. Its structure (sp. gr. P\(\bar 1\), Z = 2) is determined from single crystal X-ray diffraction data. There are two independent centrosymmetric molecules with no significant differences in bond lengths and angles between them. The NMR, IR, HRMS, and UV spectral data of the prepared bis-chalcone are presented.     

Synthesis and Characterization of <Emphasis Type="Italic">Cis</Emphasis>-[V<Superscript>IV</Superscript>O(pzc)<Subscript>2</Subscript>(H<Subscript>2</Subscript>O)]·2H<Subscript>2</Subscript>O (pzc: 2-pyrazinecarboxylate)

Abstract  

Hydrothermal synthesis and the structural characterization of V(IV) complex of 2-pyrazinecarboxylate (pzc), is reported. The vanadium is in a distorted octahedral environment. Pairs of pyrazine-2-carboxylate ligands are always cis to each other. The pzc ligands do not link adjacent vanadium atom directly. The remainder of the three-dimensional network is completed by intense hydrogen bonding of uncoordinated water molecules to aqua and pzc ligands. Cis-[V^IVO(pzc)₂(H₂O)]·2H₂O, 1, was characterized by means of elemental analysis (CHNS), TGA, FT-IR, manganometric titration, bond valance sum calculations and single crystal X-ray diffraction methods. Crystal data for 1: monoclinic space group P2 ₁ /c and unit-cell parameters are a = 9.1142(5), b = 16.5822(10), c = 12.8936(7) ?, β = 131.625(3)° and Z = 4. To the best of our knowledge, cis-[V^IVO(pzc)₂(H₂O)] is reported without single crystal structure by Eugenio Garribba and his colleagues in year 2006. Herein we complete full characterization of the title complex with single crystal structure and also 1 will be the first reported example of solid vanadium complex of 2-pyrazinecarboxylates involving intense hydrogen bonding.     

The Synthesis and Crystal Structure of (Hpy)<Subscript>3</Subscript>[PMo<Subscript>12</Subscript>O<Subscript>40</Subscript>]·2(py)

Abstract  

The novel supramolecular networks based on Keggin-type polyoxoanion, formulated (Hpy)₃[PMo₁₂O₄₀]·2(py) has been synthesized hydrothermally and determined by X-ray diffraction. The compound crystallize in Monoclinic, system with space groups and cell parameters, P2 ₁ /n, a = 10.9370(2) ?, b = 19.586(3) ?, c = 12.5500(2) ?, β = 98.618(2)°, V = 2657.8(6) ?³. Organic fragments and Keggin anions are connected via N–H···N, N–H···O contacts to form interesting 1D zigzag chain. The molecule is stabilized in solid state by electrostatic forces and intermolecular hydrogen-bonding interactions to give the confirmation of guest [PMo₁₂O₄₀]³⁻ inserting in organic host.     

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.     

Two Nearly Isoformular Isomeric Dinuclear Platinum(II) Complexes with Planar and Butterfly [Pt<Subscript>2</Subscript>(μ<Subscript>2</Subscript>-S)<Subscript>2</Subscript>] Core Structures

Abstract Two dinuclear Pt^II complexes bearing fluorinated phosphine and thiolate ligands were synthesized from mononuclear starting materials, and characterized. Complex [(PPh₂(C₆F₅))(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh₂(C₆F₅))] has phospine ligands arranged trans and presents a planar [Pt₂(μ₂-S)₂] core structure, imposed by symmetry. In contrast, the almost isoformular complex [(PPh(C₆F₅)₂)(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh(C₆F₅)₂)] revealed to be a butterfly molecule with phosphine ligands in a cis configuration. In both complexes, two pentafluorobenzenethiolate ligands bridge metal centers in an anti conformation. Both compounds have been X-ray characterized. Trans complex: a = 11.8576(13) ?, b = 12.3237(14) ?, c = 13.4644(16) ?, α = 90.528(9)°, β = 113.866(9)°, γ = 107.698(9)°, ; cis complex: a = 24.368(2) ?, b = 15.043(2) ?, c = 37.596(7) ?, β = 93.69(1)°, C2/c. Index Abstract Two Nearly Isoformular Isomeric Dinuclear Platinum(II) Complexes with Planar and Butterfly [Pt ₂ (μ ₂ -S ) ₂ ] Core Structures Sylvain Bernès, Luis Villanueva & Hugo Torrens Two dinuclear Pt^II complexes bearing fluorinated phosphine and thiolate ligands were X-ray characterized, [(PPh₂(C₆F₅))(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh₂(C₆F₅))] and [(PPh(C₆F₅)₂)(SC₆F₅)Pt(μ₂-SC₆F₅)₂Pt(SC₆F₅)(PPh(C₆F₅)₂)]. The [Pt₂(μ₂-S)₂] core is constrained by symmetry to be planar in the former complex, affording a trans arrangement for non-bridging ligands, whereas the latter is a butterfly molecule with a cis configuration. Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users.     

Solid State Structure of 6,7-Dihydro-1,4-Di(2′-Pyridyl)-5<Emphasis Type="Italic">H</Emphasis>-Cyclopenta[d]Pyridazine

Abstract  The X-ray structure of 6,7-dihydro-1,4-di(2′-pyridyl)-5H-cyclopenta[d]pyridazine ligand (5-dppn) shows the existence of a trans/trans conformation. The 5-dppn crystallizes in a triclinic space group P-1 with a = 7.1048(15) ?; b = 9.008(2) ?; c = 10.986(3) ?; α = 88.279(16)°; β = 85.454(15)°; γ = 69.104(12)°; V = 654.7(3) ?³ and Z = 2. The analysis of 5-dppn crystal structure demonstrates the presence of edge-edge Ar–H···N and face-face Aliph-H···N centrosymmetric dimer interactions. The unit cell packing arrangement confirmed the presence of two molecules opposite to each other. Index Abstract  The X-ray structure of 6,7-dihydro-1,4-di(2′-pyridyl)-5H-cyclopenta[d]pyridazine ligand (5-dppn) shows the existence of a trans/trans conformation.      

N-[[5-[[(1,4-二氢-2-甲基-4-氧-6-喹唑啉基)甲基]甲氨基]-2-噻吩基]羰基]-L-谷氨酸的一水合甲醇溶剂合物的合成、晶体结构及Hirshfeld表面分析

合成制备了N-[[5-[[(1,4-二氢-2-甲基-4-氧-6-喹唑啉基)甲基]甲氨基]-2-噻吩基]羰基]-L-谷氨酸的一水合甲醇溶剂合物(C21H22N4O6S·CH3OH·H2O(化合物1)的晶体,通过单晶X射线衍射,红外,热重分析表征.分析其含有一个结晶水和一分子甲醇溶剂,晶胞参数为a=7.9730(16)nm,b=13.558(3)nm,c=11.412(2)nm,α=90°,β=91.12(3)°,γ=90°.采用Hirshfeld表面分析方法对分子间作用力分析.Hirshfeld表明作用分析得到的二维指纹图显示,其中O…H,N…H,C…H,S…H的作用力要强与C…O,C…N作用力,其中H…H作用力明显.     

2-pyridylbis(diphenylphosphino)methane chemistry. Synthesis and structures of [Cu(μ−η2:η1(Ph2P)2−CHC5H4N)(THF)]2(BF4)2 and [Ni(Ph2PCH2C5H4N)2]-[NiCl4]·0.85CH2Cl2and [Ni(Ph2PCH2C5H4N)2]-[NiCl4]·0.85CH2Cl2

Reaction of 2-pyridylbis(diphenylphosphino)methane (NPP) with [Cu(NCMe)₄]BF₄ and with [Ni(H₂O)₆]Cl₂ forms [Cu(NPP)(THF)]₂(BF₄)₂ (after recrystallization in the presence of THF) (1) and NiCl₂(NPP) (2) respectively Attempts to recrystallize2 led ultimately to the ligand cleavage product [Ni(Ph₂PCH₂C₅H₄N)₂][NiCl₄]·0.85CH₂Cl₂ (3). Complex1 crystallizes in the monoclinic space groupP2₁/n witha=13.148(2),b=19.221(2),c=13.458(2) ų, β=108.61(1)^o,V=3222.6(8) ÅZ=2. The structure was refined onF ² toR1=0.11,wR2=0.14 (R1=0.044 forI≥2σ(I)) for 5661 observed reflections. Complex3 crystallizes in the triclinic space groupP1 witha=12.795(2),b=17.535(1),c=10.203(1) Å, α=107.564(6), β=114.260(8), γ=78.435(8)^o,V=1982.1(8) ų;Z=2. The structure was refined onF toR1=0.044,R _w=0.059 for 3534 observed reflections. Dinuclear complex1 has crystallographically imposed centrosymmetry with the NPP ligands arranged in a head-to-tail fashion. The Cu...Cu separation of 3.372(1) Å is too long to support significant metal-metal interaction. Complex3 results from the cleavage of a {PPh₂} unit from the NPP ligand and contains an approximately square nickel atom surrounded by two Ph₂PCH₂C₅H₄N ligands coordinated in a head-to-head fashion.     

Synthesis,Characterization and Crystal Structure of <Emphasis Type="Italic">N,N</Emphasis>′-di[(<Emphasis Type="Italic">E</Emphasis>)-1-(2-hydoxyphenyl)methylidene]-2,6-naphthalenedicarbohydrazide

Abstract  

A new bishydrazone compound, N,N′-di[(E)-1-(2-hydoxyphenyl)methylidene]-2,6-naphthalenedicarbohydrazide (1), has been prepared by condensation reaction of 2,6-naphthalenedicarbohydrazide with salicylaldehyde in ethanol, and characterized by elemental analysis, FT-IR, ¹H- and ¹³C-NMR, ESI–MS and single-crystal X-ray diffraction analysis. The crystal of 1·2DMF belongs to monoclinic, space group P2(1)/n with a = 10.454(1), b = 7.711(1), c = 18.801(2) ?, β = 93.364(1)°, V = 1512.9(3) ?³, Z = 2, D _c  = 1.314 g cm⁻³, μ = 0.093 mm⁻¹, F(000) = 632, Mr = 598.65, the final R ₁ = 0.0861 and wR ₂ = 0.2279 for 7243 observed reflections with I > 2σ(I). The structural analysis reveals that compound 1·2DMF contains one N,N′-di[(E)-1-(2-hydoxyphenyl)methylidene]-2,6-naphthalenedicarbohydrazide molecule and two N,N-dimethylformamide solvent molecules. A 2D supramolecular structure of 1·2DMF was constructed by multiple intermolecular N–H···O and C–H···O hydrogen bonds.     

Molecular structure of [(<Superscript>t</Superscript>Bu)<Subscript>2</Subscript>Al(μ-OC<Subscript>6</Subscript>H<Subscript>4</Subscript>-2-Me)]<Subscript>2</Subscript>

The molecular structure of [(^tBu)₂Al(-OC₆H₅-2-Me)]₂ has been determined. Both the ortho-tolyl methyl groups are oriented towards Al(2). The intramolecular steric interaction between the ortho-methyl groups and the tert-butyl ligands results in the geometry about the bridging oxygen being significantly distorted while the geometries about the aluminum centers show a distortion from tetrahedral that is less than the sterically less hindered [(^tBu)₂Al(-OPh)]₂. Crystal data: group C2/c, a = 13.733(3) Å, b = 15.135(3) Å, c = 15.420(3) Å, = 104.24(3), V = 3106(1) ų, Z = 4, R = 0. 0612, wR₂ = 0.1787.     

Synthesis and Crystal Structure of (PzCH<Subscript>2</Subscript>CHOHCH<Subscript>2</Subscript>PzH)·(Ph<Subscript>2</Subscript>SnCl<Subscript>3</Subscript>) (Pz = 3,5-dimethylpyrazol-1-yl)

Abstract  

Reaction of Ph₂SnCl₂ with 1,3-bis(3,5-dimethylpyrazol-1-yl)-2-propanol (L) in a 1:1 ratio yields L(SnPh₂Cl₂)₂ adduct, which partly hydrolyzes to the title complex (C₂₅H₃₁Cl₃N₄OSn, Mr = 628.58) during crystal growing in the air. The title complex is of monoclinic, space group P2₁/n with a = 9.0338(9), b = 17.890(1), c = 17.340(1) ?, β = 95.533(1)^o, V = 2798.9(5) ?³, Z = 4, Dc = 1.492 Mg/m³, λ(MoKα) = 0.71073 ?, μ = 1.224 mm⁻¹, F(000) = 1272, R = 0.023, wR = 0.054 for 4212 observed reflections with I ≥ 2σ(I). The crystal structure indicates that there is no direct interaction between the pyrazolyl ligand and the tin atom, but this complex forms a supramolecular structure through weak intermolecular C–H⋯Cl and O–H⋯Cl hydrogen bonds.