Crystal structures of 2-pyrazinecarboxylato silver(I) and ammine 2,3-pyrazinecarboxylato disilver(I)

X-ray analysis has shown that the complexes of silver(I) with the anionic forms of 2-pyrazinecarboxylic and 2,3-pyrazinedicarboxylic acids are three-dimensional network polymers. Ag(C₅H₃O₂N₂) (1) crystallizes in space groupPna2₁ witha=7.028(2),b=11.510(3),c=6.949(2) Å andZ=4. Silver tetrahedral coordination occurs through three ligands: the first one acts as a bidentate chelator (Ag–O=2.539(4), Ag–N=2.334(4)Å), the second one involves one N pyrazine atom (Ag–N=2.196(4)Å) and the third one bonds through one O-carboxylato atom (Ag–O=2.323(4)Å). The dinuclear complex Ag₂(C₆H₂O₄N₂)(NH₃) (2) crystallizes in space groupP2₁/c witha=7.775(2),b=16.455(2),c=7.174(1) Å, -115.21(1)° andZ =4. Each of the two silver atoms shows a trigonal environment. The first silver atom involves two O carboxylic atoms (Ag–O=2.312(4), 2.374(4)Å) and one N pyrazine atom (Ag–N=2.277(3)Å) belonging to three different ligands. The second one involves one O carboxylic atom (Ag–O=2.364(3)Å) and one N pyrazine atom (Ag–N=2.304(4)Å) from the same chelating ligand and one N ammine atom (Ag–N=2.158(5)Å).     

The crystal structure of hexabenzoylhexaazaisowurtzitane

The crystal and molecular structure of an interesting cage compound is described. Crystal data: C₄₈H₃₆N₆O₆·(CH₃)₂CO; monoclinic; space group: P2 ₁ /n; a = 14.948(3) Å, b = 15.079(3) Å, c = 19.539(4)Å, = 93.93(3)°, V = 4394(2)ų; and Z = 4.     

Synthesis and crystal structures of two copper(I) π-complexes with 1-allyloxybenzotriazole of CuBr?C6H4N3(OC3H5) and 2CuCl?C6H4N3(OC3H5) compositions

Both compounds of CuBr⋅C₆H₄N₃(OC₃H₅) (sp. gr. P1, a = 7.633(1) Å, b = 9.987(1) Å, c = 14.898(2) Å, α = 104.75(1)^∘, β = 94.76(1)^∘, γ = 106.90(1)^∘) (I) and 2CuCl⋅C₆H₄N₃(OC₃H₅) (sp. gr. Cc, a = 11.2483(4) Å, b = 16.7076(6) Å, c = 7.2948(3) Å, β = 118.612(2)^∘) (II) composition were prepared by alternating-current electrochemical synthesis. In I due to a bridging function of organic moieties 16-membered cycles appear which are combined into ribbons {Cu₂Br₂[(C₆H₄N₃(OC₃H₅)]₂}_n. Each of two crystallographically independent copper atom possesses a trigonal-pyramidal arrangement with different degree of tetrahedral distortion. Distinctive numbers of hydrogen bonds around Br1 and Br2 atoms cause rather appreciable distinctions in copper–olefinic bond interaction effectiveness for each metal atom. In II Cu₂Cl₂ rhombs are joined to infinite chains oriented along [010] direction. Each ligand molecule is also coordinated through the C=C—bond of the allylic group to copper atom of one inorganic chain and through the nitrogen atom to a metal atom belonging to another copper-halide chain. Cu1 atoms is tetrahedrally surrounded by three chlorine atoms and nitrogen one, whereas a trigonal-planar arrangement of Cu2 atom is formed by two halogen atoms and slightly disordered olefinic group.     

Influence of the spectator cation on the structure of anionic pyridine-2,6-dicarboxylato complexes of cobalt(II), nickel(II), and copper(II)

The structures of anionic pyridine-2,6-dicarboxylato (pdc^2–) complexes of cobalt, nickel, and copper have been studied. The stoichiometries and structures are very much dependent on whether KOH, Et₄NOH, or NaOH is used in the synthesis to deprotonate the H₂pdc ligand. Crystallographic results are: (1) K₂[Co(pdc)₂] · 7H₂O, orthorhombic, Pnna, Z = 4, a = 20.637(2)Å, b = 13.480(1)Å, c = 8.200(1)Å (2) K₂[Ni(pdc)₂] · 7H₂O, orthorhombic, Pnna, Z = 4, a = 20.648(1)Å, b = 13.375(1)Å, c = 8.2393(8)Å (3) [Co₂(H₂O)₅(pdc)₂] · 2H₂O, monoclinic, P2₁/c, Z = 4, a = 8.3880(6)Å, b = 27.384(2)Å, c = 9.6110(8)Å, = 98.271(6)° (4) [Ni(Hpdc)₂] · 3H₂O, monoclinic, P2₁/c, Z = 4, a = 13.679(1)Å, b = 10.0450(9)Å, c = 13.767(2)Å, = 115.184(7)° (5) Na₆[Co(H₂O)₆][Co(pdc)₂]₄ · 28H₂O, monoclinic, P2₁/n, Z = 2, a = 13.363(1)Å, b = 8.437(1)Å, c = 40.689(3)Å, = 91.288(5)° (6) Na[Ni(Hpdc)(pdc)] · 11.5H₂O, monoclinic, C2/m, Z = 4, a = 15.200(2)Å, b = 22.299(2)Å, c = 8.3596(7)Å, = 118.894(7)° (7) Na[Cu(Hpdc)(pdc)] · 3H₂O, monoclinic, P2₁/n, Z = 4, a = 9.516(4)Å, b = 14.917(6)Å, c = 12.247(5)Å, = 92.00(5)°. The potassium and sodium complexes have extensive K⁺—H₂O and Na⁺—H₂O networks. The fact the Et₄N⁺ ion does not appear in any of the complexes is likely due to the fact that it is incapable of forming the intricate cation—water and hydrogen-bonding networks observed in all of the other structures.     

Crystal structure of bis(2,3,5-trimethylpyridine N-oxide) 2,4,6-trinitrophenolate: Cation complex tied by the extremely strong OHO hydrogen bonding

The salt of bis(2,3,5-trimethylpyridine N-oxide) 2,4,6-trinitrophenolate, C₂₂H₂₅N₅O₉, crystallizes in monoclinic space group C2/c with a=12.411(2)Å, b=15.326(3)Å, c=13.559(3)Å, =113.13(1)°, V=2371.8(8)ų, Z=4, D _c=1.410 mg/m³, F(000)=1056. The molecule of 2,3,5-trimethylpyridine N-oxide is protonated. Two pyridine N-oxide molecules are linked by extremely strong OHO hydrogen bonding (2.378(4)Å) to form a cation complex. CHO hydrogen bonding and – interactions also play important role in stablizing the structure of the salt.     

Crystal structures of [WI2(CO)3{Ph2P(CH2) n PPh2}] (n = 2 or 3)

[WI₂(CO)₃{Ph₂P(CH₂)₂PPh₂}] (1) crystallizes out in the monoclinic space group P2₁/n, with a = 13.852(7) Å, b = 14.789(19) Å, c = 14.915(19) Å, = 102.86(1)°, Z = 4. [WI₂(CO)₃{Ph₂P(CH₂)₃PPh₂}] (2) crystallizes out in the monoclinic space group P2₁/n, with a = 10.499(15) Å, b = 14.58(2) Å, c = 20.75(3) Å, = 103.59(1)°, Z = 4. Both structures show the metal in a seven-coordinate environment with a carbonyl in the unique capping position, two further carbonyls and a phosphorus in the capped face, and two iodides and the second phosphorus in the uncapped face.     

Characterization of the coordination network formed on self-assembly of 1,2-bis(3′-pyridyl)ethyne with copper(I) iodide

The self-assembly of 1,2-bis(3-pyridyl)ethyne with copper(I) iodide is described. The X-ray crystal structure of the resultant pale yellow crystalline solid reveals that the sheets of the two-dimensional coordination network are stacked such that channels are formed. The structure (C₁₂H₈Cu₂I₂N₂) is monoclinic with a = 9.285(2) Å, b = 4.1502(9) Å, c = 22.096(5) Å, = 97.380(11)°, and space group P2 ₁/c.     

Crystal and molecular structures oftrans-dichloro-(ethylene) (4-methylpyridine)platinum(II) andtrans-dichloro(ethylene) (2,4,6-trimethylpyridine)platinum(II)

The crystal and molecular structures oftrans-[PtCl₂(C₂H₄)(4-MeC₅H₄N)] (I) andtrans-[PtCl₂(C₂H₄)(2,4,6-Me₃C₅H₂N)] (II) have been determined by single-crystal x-ray methods.I crystallizes in space groupP2₁/c witha= 4.991(1), b=21.658(3), c=10.675(3) Å, =110.17(2) °,Z=4;II is orthorhombic (Pbca) witha=10.295(6),b=12.393(8),c=20.370(10) Å,Z=8.Full-matrix least-squares refinements have given finalR factors of 0.053 (1520 reflections) forI and 0.042. (1412 reflections) forII. The intensities were recorded by counter methods, and only those reflections havingI>3(I) were used in the analyses.In both complexes, platinum is four-coordinate with the two chlorine atoms, the double bond of the ethylene, and the nitrogen atom of the substituted pyridine. The two structures are discussed in terms of the arrangement of the pyridine ligand with respect to the PtCl₂(C₂H₄) moiety.     

Synthesis and structure of bis(2,6-dimethylpyrazine)(THF)copper(II) nitrate

Attempts to crystallize Cu(2,6-dmpz)(NO₃)₂ (2,6-dmpz = 2,6-dimethylpyrazine) by reaction of 2,6-dmpz with Cu(NO₃)₂·3H₂O in THF resulted in the synthesis of Cu(2,6-dmpz)₂(NO₃)₂·THF. The compound crystallized in the monoclinic space group C2/c and exists as isolated molecules with distorted square pyramidal geometry: a = 11.609(4) Å, b = 10.415(3) Å, c = 18.256(6) Å, = 108.332(4)°. The 2,6-dmpz molecules coordinate to the Cu ions through the distal (remote from the methyl) nitrogens. The molecules are arrayed in stacks parallel to the b-axis.     

Isolation and crystal structures of triethylenediamine-hydroquinone (1/1) and triethylenediamine-phenol (1/2)

Two crystalline adducts of triethylenediamine with hydroquinone [N(CH₂CH₂)₃N·C₆H₄(OH)₂,I] and phenol [N(CH₂CH₂)₃N·2C₆H₅OH,II] have been isolated and characterized by X-ray analysis. ComplexI crystallizes in the monoclinic space groupC2/c, witha=11.944(2),b=9.491(2),c=11.986(2) Å,=121.70(1)°, andZ=4. Both molecular components occupy sites of symmetry 2, and are linked alternately by N H-O hydrogen bonds to form infinite zigzag chains. Crystals ofII are also monoclinic, with space groupP2₁/c,a=12.987(2),b=6.376(1),c=21.350(3) Å,=106.94(1)°, andZ=4. The structure is composed of discrete hydrogen-bonded molecular aggregates corresponding to the stoichiometric formula. The triethylenediamine moieties in both adducts closely approximate to the idealizedD ₃ h conformation. The structures have been refined toR values of 0.097 (I) and 0.092 (II) using, respectively, 479 and 1580 observed MoK data.     

Crystal structures of a series of 3,7-bis-(arylazo)-1,3,5,7-tetraazabicyclo[3.3.1]nonanes

The crystal and molecular structure of a series of 3,7-bis(arylazo)-1,3,5,7-tetraazabicyclo[3.3.1] nonanes (1a–d) have been determined by single crystal X-ray diffraction analysis. All four compounds have the same feature, that the tetraazabicyclononane unit assumes a cage-like structure with the aryltriazene moieties lying parallel to one another so that the aryl rings are held together by – stacking. Crystal data: 1a C₁₇H₁₈N₁₀O₄, triclinic, space group P – 1, a = 9.8899(10), b = 13.0845(13), c = 16.458(2) Å, = 94.095(2)°, = 107.004(2)°, = 111.027(2)°, V = 1863.5(3) ų and Z = 4; 1b, C₁₉H₁₈F₆N₈, orthorhombic, space group Pbca, a = 15.3210(8), b = 10.9512(6), c = 24.5698(13) Å, V = 4122.4(4) ų and Z = 8; 1c C₁₉H₁₈N₁₀, monoclinic, space group P2₁/n a = 6.3742(6), b = 13.7343(13), c = 21.542(2)Å, = 97.738(2)°, V = 1868.8(3) ų, and Z = 4; 1d, C₁₉H₁₈N₁₀, monoclinic, space group P2₁/c, a = 18.205(2), b = 17.398(2), c = 12.784(12) Å, = 109.480(2)°, V = 3818.0(6) ų, and Z = 8.     

Aquadifluoro(1,10-phenanthroline)copper(II) dihydrate: X-ray crystal structure reveals strong hydrogen bonds between ligand fluoride and lattice water molecules

C₁₂H₁₄CuF₂N₂O₃,M=335.797, monoclinic, space groupP2₁/n,a=6.985(2),b=17.406(2),c=10.581(2) Å,=92.41(2)°,V=1285(1) ų,D _c =1.736 g cm^–3,Z=4,F(000)=684,(CuK)=27.0 cm^–1, =1.5418 Å,T=20°C, crystal dimensions=0.75×0.45×0.30 mm. The structure of the title compound shows it to be [Cu(phen)F₂(H₂O)]·2H₂O with pentacoordinate-square pyramidal Cu(II), short Cu-F bonds [1.890(4) and 1.891(4) Å], and short FH-O hydrogen bonds (ca. 2.68 Å) between the complex and lattice water molecule.     

Study on the crystal and molecular structure of triphenyl tin methacrylate: (C6H5)3SnOCOCCH2CH3

The crystal and molecular structure of (C₆H₅)₃SnOCOCCH₂CH₃ has been determined by a single crystal X-ray diffraction study. The crystal is monoclinic with space group P2₁/c,a=11.902(3),b=10.104(4),c=16.721(2) Å,=97.56(1)°,V=1930.4 ų,Z=4 andD _c =1.495 g/ cm³,F(0,0,0)=872,(CuK)=1.5418 Å. The structure was solved by the heavy-atom method and refined by full-matrix least-squares procedures to anR factor of 0.060 based on 2157 independent reflections. The results showed that the Sn-O bond distance is 2.064(4) Å. The average Sn-C bond distance is 2.126 Å. There is a weak coordination through the O of the CO group of the methacrylate residue (Sn-O(2) 2.774(5) Å) except for four normal coordinations. The coordination number at the Sn⁴⁺ is 5.     

Structural characterization of 2,6-bis(N-methylenepiperidino)-4-nitrophenol (MPN) and 2,6-bis-(N-methylenemorpholino)-4-nitrophenol (MMN)3

MPN: C₁₈H₂₇N₃O₃,M _r=333.43, monoclinic,P2₁/n. a=6.207(2),b=21.893(6),c=13.693(3) Å; =96.12(2)^o,V=1850.1(8) ų.,Z=4,D _cal=1.20 mg/m³,F(000)=720, (CuK)=1.5418 Å, andT=298K.R=0.042 andwR=0.049 for 1675 observed reflections. MMN: C₁₆H₂₃N₃O₅,M _r=337.38, triclinic,P,a=9.642(1) Å,b=10.123(5) Å,c=9.341(2) Å, =93.00(3)^o, =90.96(1)^o, =110.46(1)^o, V=852.5(5) ų,D _cal=1.31 mg m^–3.F(000)=360,Z=2, (CuK)=1.5418 Å,R=0.054 andwR=0.074 for 2804 observed reflections. The piperidine and morpholino rings assumechair conformation and orient each other at an angle of 44.8(1)^o (MPN) and 47.1(1)^o (MMN), respectively.Contribution No. 827 from DCB.     

Crystal structure of tetrakis (μ-betaine-O,O′) dichloro-dicopper(II) dichloride tetrahydrated

[Cu₂(bet)₄Cl₂]Cl₂·4H₂O (bet = betaine: IUPAC name: trimethylammonioacetate) is monoclinic, space group P2₁/c, a = 11.0510(10) Å, b = 14.7140(4) Å, c = 11.1620(15) Å, = 107.40(2)°. The dinuclear copper(II) cation [Cu₂(bet)₄Cl₂]²⁺ is counterbalanced by two naked Cl^– ions. The copper(II) ions have a square bipyramidal environment with oxygen atoms from the acetato groups in the basal planes and a chlorine and a copper atom occupying the apical positions. The metal atoms are ₂-bridged by four acetato groups and the molecular symmetry is close to C _2h. The two symmetry-independent chelating betaine molecules are present in their zwitterionic, neutral form.     

Structure, thermal behavior, and IR investigation of bis(3-amino-1,2,4-triazolium)monohydrogen monophosphate

Chemical preparation, calorimetric studies, crystal structure, and IR spectrometric investigation of (C₂H₅N₄)₂HPO₄, denoted ATZP, are described. The compound crystallizes in the monoclinic system with C2/c space group. Its unit cell dimensions are a = 13.589(2) Å b = 11.105(2) Å c = 15.734(3) Å = 104.68(2)°, V = 2296.8(7) ų, and Z = 8. The structure of the title compound consists of a three dimensional network of H-bonds connecting all its components. The IR spectrum of ATZP is reported and discussed on the basis of group theoretical analysis.     

Structure of 6,13-bis(<Emphasis Type="Italic">N</Emphasis>, <Emphasis Type="Italic">N</Emphasis>-dimethylcarbamoyl) thioquinanthrene

The crystal structure of 6,13-bis-(N,N-dimethylcarbamoyl)thioquinanthrene 3 has been determined as monoclinic, with space group P2(1)/c with lattice parameters a = 10.044(2) Å, b = 21.385(4) Å, c = 10.889(3) Å, = 102.92(3)°, Z = 4 and D_calc = 1.342 Mg/m³. The middle 1,4-dithiin ring in the title compound 3, C₂₄H₂₀N₄O₂S₂ is in a boat conformation with the dihedral angle between the planes of the aromatic rings 132.45(8)°.     

Crystal and molecular structure of diaquabis(thiocyanato-N)bis(5-methyl-[1,2,4]triazolo[1,5-a]pyridine-N3)cobalt(II), [Co(NCS)2(C6H6N4)2(H2O)2]

The X-ray crystal structure of the title compound, [Co(NCS)₂(C₆H₆N₄)₂(H₂O)₂], has been determined. The crystals are monoclinic, space groupC2/c, with cell dimensionsa=15.6901(5),b=7.9248(10),c=16.1278(12) Å,=94.4(8)°V _c=1999.44 ų,M _r=479.18,Z=4,D _x=1.5918 Mg m³,Cu K radiation (graphite crystal monochromator, =1.54051 Å), (CuK)=39.08 cm^–1,F(000)=980.00 andT=290 K. Final conventionalR-factor=0.051, andR _w=0.053 for 1430 observed reflections and 141 variables. The structure was solved using the programsPatsys andDirdif. The Co atom is octahedrally coordinated (CoN₂O₂N₂ chromophore), with only the 5-methyl-[1,2,4]-triazolo[1,5-a]pyrimidine (5mtp) ligands in thetrans positions. The triazolo pyrimidine rings are planar and coordinated through their N(3) atoms. The H₂O ligands are also H-bond donors to N(4) (intramolecularly) and to the S atoms of the NSC anions (intermolecularly).     

Synthesis and X-ray crystallographic characterization of [Cd(NO3)2(15-Crown-5)] and [Cd(NO3)2(18-Crown-6)]

Reaction of 15-crown-5 or 18-crown-6 in 3:1 (v/v) CH₃CN:CH₃OH with Cd(NO₃)₂·4H₂O followed by slow evaporation produces [Cd(NO₃)₂(15-crown-5)] or [Cd(NO₃)₂(18-crown-6)]. Crystals of [Cd(NO₃)₂(15-crown-5)] are orthorhombic with space group Pbca and cell parameters a = 13.562(5), b = 15.941(9), and c = 15.011(7) Å at 295 K. [Cd(NO₃)₂(18-crown-6)] crystallizes in the monoclinic space group C2/c with a = 11.235(2), b = 11.196(5), c = 15.385(3) Å, and = 99.89(2)° at 295 K. The metal center in [Cd(NO₃)₂(15-crown-5)] rests atop the macrocyclic donor array with two cis-bound nitrate anions and adopts a distorted tricapped trigonal prismatic geometry. [Cd(NO₃)₂(18-crown-6)] resides on an equatorial two-fold rotation axis with Cd²⁺ coordinated in the 18-crown-6 cavity and the nitrate anions oriented in twisted trans positions.     

Synthesis and crystal structure of a terephthalato-bridged copper(II) complex [Cu2(tpt)(bpy)2(H2O)4] [Cu2(tpt)3 (bpy)2(H2O)2]

A terephthalato-bridged copper(II) complex [Cu₂(tpt)(bpy)₂(H₂O)₄][Cu₂(tpt)₃(bpy)₂ (H₂O)₂] (1) (tpt = terephthalate, bpy =; 2,2'-bipyridine) was synthesized by the reaction of Cu(ClO₄)₂ 6H₂O and terephthalic acid in the presence of 2,2'-bipyridine in H₂O solution. Crystal structure of 1 was determined by X-ray diffraction analysis in the triclinic space group P , with a = 10.7327(10) Å, b = 11.1658(11) Å, c = 17.3768(16) Å, = 108.063(2), = 91.064(2), = 116.721(2), V = 1737.5(3) ų, and Z = 2. Both the anion and the countercation in 1 are copper(II) complexes linked by terephthalate bridges in the bis(monodentate) (syn–anti) mode. The anion and the countercation are also linked by two hydrogen bonds between coordinating water molecules and terephthalate ligand.