The X-ray crystal structure of Hg(p-MeC6H4)(O2CC6F5) from synchrotron radiation

The X-ray crystal structure of Hg(p-MeC₆H₄)(O₂CC₆F₅) reveals near linear C—Hg—O units stacked into columns with intermolecular Hg–O bonding and overall distorted square-planar stereochemistry for mercury. Hg(p-MeC₆H₄)(O₂CC₆F₅) crystallizes in triclinic space group with a = 6.405(4), b = 7.285(3), c = 14.630(9) Å, = 84.07(3), = 81.21(3), = 86.87(3)° with calculated density 2.490 g cm^–3 for Z = 2.     

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 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.     

Crystal structure of aquo (hydroxo) (ethylenediaminetetraacetato) sodium(I) tin(IV), NaSn(OH)(edta)(H2O)

NaSn(OH)(edta)(H₂O) is monoclinic, space groupP2₁/c, witha=9.747(3)Å,b=9.121(3)Å,c=16.430(6)Å, =98.69(4)°, ų, andZ=4. The coordination environment of Sn(IV) is a capped octahedron. Sn–O distances range from 1.990(6)Å to 2.351(7)Å. Na(I) is five coordinated to three different edta molecules. Na–O distances range from 2.283(9)Å to 2.414(7)Å. The edta ligand presents the E, G/R conformation. The crystal structure is composed of sheets parallel to (001): inside a sheet Sn(OH)(edta) molecules are connected to each other by the Na(I) interactions.     

Polymeric and mixed carboxylate compounds: Crystal structure of [Zn(tiglate)0.54 (benzoate)1.46]x

The crystal structure of [Zn(O₂CC(CH₃)CHCH₃)_0.54(O₂CC₆H₅)_1.46]_x has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic system, space group P2₁/c witha=10.311(1),b=13.170(1),c=19.000(2) Å,=91.895(7)°,V=2578.7 ų,Z=4,D _x=1.525g cm^–3, (Mo K)=0.71073 Å,=1–95 mm^–1, F(000)=1206,T=295K,R=0.046 for 4548 unique reflections. The two different carboxylates are randomly scrambled along a one dimensional polymer, made up of binuclear units connected by a syn-anti carboxylate bridge. Each binuclear unit contains three syn-syn carboxylates which bridge two zinc atoms. Vibrational data indicate that [Zn(O₂CC(CH₃)CHCH₃)₂]_x has the same polymeric structure; orientation of tiglate is the same as for the mixed ligand compound. Recrystallization of mixed carboxylate species produces either an alteration in carboxylate ligand ratio, or a total separation of the two carboxylates, giving two different compounds.     

Structure of (chloranilato)bis(tri-n-butylphosphine)palladium(II)

(Chloranilato)bis(tri-n-butylphosphine)palladium(II), [Pd(C₆Cl₂O₄){P(C₄H₉)₃}₂] (chloranilic acid=2,5-dichloro-3,6-dihydroxy-p-benzoquinone): FW=718.02,P2₁/c,a=21.729(6),b=17.293(5),c=21.010(9) Å,=112.62(3)°,V=7287.42 ų,Z=8,D _c=1.309mg m^–3, Mo, =0.710730 Å,=0.76 mm^–1,F(000)=3008, finalR=0.087, 2594 observed reflections. Palladium is ligated by a distorted square planar P₂O₂ coordination sphere in the title compound. The two molecules per asymmetric unit differ in the arrangement of phosphine n-butyl chains, yielding two unique metal centers.     

Crystal structure of [Co(o-SC6H4NH2){P(OMe)3}3]PF6

A cobalt-thiolato-phosphite complex [Co(o-SC₆H₄NH₂){P(OMe)₃}₃]PF₆ has been prepared and characterized by X-ray crystallography. The complex crystallizes in the triclinic space group with a = 10.590(4), b = 11.122(3), c = 13.577(5) Å, = 101.85(1), = 108.50(1), = 101.75(1)°, V = 1420.6(8) ų, and Z = 2. The structure comprises discrete [Co(o-SC₆H₄NH₂){P(OMe)₃}₃]⁺ cations and PF ₆ ^– anions where the metal atom is coordinated in a highly distorted square-pyramidal environment by one chelate o-SC₆H₄NH ₂ ^– (abt) and two P(OMe)₃ ligands in the basal positions, and a third P(OMe)₃ in the axial site with Co–N,, 1.847(5), Co–S, 2.166(2), Co–P, 2.157(2), 2.147(2), and 2.125(2) Å.     

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).     

A reinvestigation of the crystal structure of (4-aminobenzophenone)dichlorocuprate(II) hemiethanolate

The crystal structure of CuCl₂L·1/2 C₂H₅OH has been redetermined, where L=4-aminobenzophenone. C₁₄H₁₄Cl₂CuNO_1.5,M _r=354.5, monoclinic, P2₁/c,a=8.206(1),b=6.196(2),c=29.917 (7) Å, =92.91°,V=1521.8(6) ų,Z=4,D _x=1.55 g cm^–3, (MoK)=0.71069Å, =17.9 cm^–1,F(000)=720,T=295K. The 1984 unique reflections (20<45°), of which 1635 had |F_o|3 (F_o), refined to a finalR of 0.042 andwR=0.049 for the 3 data set. The structure is disordered at room temperature with the ethanol molecules, present at half-occupancy, coordinating to only one half of the Cu(II) ions. The structure is comprised of two types of chains which run parallel tob. One type of chain consists of stacks of CuCl₂L(C₂H₅OH) monomer units, which yield a 4+2 coordination geometry for each Cu atom in the chains. The second type of chains has stacks of binuclear Cu₂Cl₄N₂ species with a 4+1 coordination exhibited by each Cu. The location and orientation of the L ligands appear to be identical in the two stacks. Intermolecular hydrogen bonding between L ligands in adjacent stacks leave space for only one ethanol molecule per two ligands.     

Refinements of the crystal structures of 1,4-diphenylbutadiyne and its complex with two moles of Co2(CO)6

1,4-diphenylbutadiyne, C₁₆H₁₀, crystallizes in monoclinic space group P2₁/n witha=6.6152(6),b=6.0768(7),c=14.634(1) Å, =100.981(8)⁰,V=577.5(2) ų,Z=2. The structure was refined toR=0.077 andR _w=0.069 for 1007 observed reflections with CuK radiation. The molecule lies on an inversion center. Our determination represents and increase in precision of a factor of approximately three over the original determination. The 21 cobalt complex, C₁₆H₁₀[Co₂(CO)₆]₂, also crystallizes in monoclinic space group P2₁/n witha=8.9568(12),b=17.7057(10),c=18.5671(12) Å, =90.606(12)^o,V=2944.3(5) ų,Z=4. The structure was refined toR=0.032 andR _w=0.031 for 4312 observed reflections. The diphenylbutadiyne triple bonds elongate to 1.346(3) Å and the angles at the diyne C atoms decrease to 134.1(3)–144.9(3)^o upon complexation. The Co-Co distance is 2.4580(4)Å. Our data represent an increase in precision by a factor of 2–3 over the original determination.     

Antimony(III) fluoride: inclusion complexes with crown ethers

Four crystalline molecular complexes between antimony(III) fluoride and 18-membered crown ethers have been obtained and their structures investigated by single crystal X-ray diffraction techniques: [18-crown-6·SbF₃], C₁₂H₂₄F₃O₆Sb,P2₁2₁2₁,a=8.328(4),b=11.573(4),c=18.094(4),V=1744(1)³,Z=4; [benzo-18-crown-6·SbF₃], C₁₆H₂₄F₃O₆Sb,P2₁/n,a=10.490(2),b=13.714(1),c=13.442(2), =101.94(1)°,V=1892(1)³,Z=4; [cis-syn-cis-dicyclohexano-18-crown-6·SbF₃·CH₃OH], C₂₁H₄₀F₃O₇Sb,P2₁/n,a=8.270(4),b=23.386(3),c=12.772(1), =96.31(2)°,V=2455(1)³,Z=4; [cis-anti-cis-dicyclohexano-18-crown-6·SbF₃], C₂₀H₃₆F₃O₆Sb,Pna2₁,a=21.091(8),b=12.829(5),c=8.437(3),V=2283(2)³,Z=4. All species are the perching-type complexes with the antimony fluoride above the cavity and the metal lone pair pointed toward the center of the crown ring. The antimony atom interacts with all six crown oxygen atoms with Sb–O distances of 2.837(2)–3.344(2) . The antimony atom is displaced from the least square plane of the crown oxygen atoms at the distances of 1.288–1.383 .     

Crystal structure of trans-C2SnO5 pentagonal bipyramidal dibutylbis(phenylacetato)tin(IV) hydrate

The Lewis acidity of tin in a diorganotin dicarboxylate is demonstrated in this first example of a 1/1 adduct of the ester with a neutral ligand. The structure of dibutyltin bisphenylacetate hydrate [(C₄H₉)₂Sn(O₂CCH₂C₆H₅)₂·H₂O] has been determined from 1211 F ₀6F _c MoK reflections and refined to anR _F of 0.061 [space groupP2/a witha=8.416(2),b=10.391(5),c=14.28(1) Å,=98.42(4)° andZ=2]. TheC atoms [Sn-C 2.101(8) Å; C-Sn-C 169.9(5)°] make up the apices and the O_carboxylate [Sn-O 2.234(5), 2.439(7) Å; O-Sn-O 55.7(2)°] and O_water [Sn-O 2.342(8) Å] atoms the equatorial points of thetrans-C₂SnO₅ pentagonal bipyramid around the Sn atom. The molecular symmetry isC ₂, and the Sn and O_water atoms lie along a crystallographic twofold axis. The aqua ligand forms donor H-bonds with neighboring carboxylato groups to link the molecules into a double zigzag chain running parallel toa.     

Crystal and molecular structure of 12(S)-acetoxy-4(S),8(R)-dimethyl-3-oxo-1(R)-5(S)-9(S)-2-oxatricyclo[4.4.7.01,9.3.4.8.01,5]tridecane

The structure of the title compound, a cyclic ether acetate lactone, has been established uniquely by X-ray crystallography. C₁₆H₂₄O₄ is orthorhombic, space groupP2₁2₁2₁, with the cell dimensionsa=7.524(2),b=10.686(2),c=19.472(2) Å,V=1565.6(4) ų,Z=4,M _r=280.4,D _x=1.19 g cm^–3,D _o=1.20 g cm^–3,F(000)=608,T=293 K, finalR=0.050. The two cyclohexane ring junction iscis while the lactone ring junction istrans. Both the cyclohexane rings have the chair conformation and the -lactone ring has an envelope conformation with C(7) being at the tip of the flap. The acetoxy side chain is-equatorial. There is an intramolecular C-H---O interaction C(4)O(4)=2.666(4) Å.N. C. L. Communication No. 5064.     

Crystal structure of dicalcium potassium trihydrogen bis(pyrophosphate) trihydrate

The crystal structure of Ca₂KH₃(P₂O₇)₂·3H₂O has been determined by single crystal X-ray diffraction. Crystals are monoclinic, space groupP2₁/n witha=10.518(3),b=19.253(9),c=7.340(3)Å,=90.07(2)°, andZ=4. The structure was refined toR=0.048 andR _w=0.044 for 1839 reflections withI3(I). The structure consists of a compact assembly of Ca, K, HP₂O₇, and H₂P₂O₇ ions and three water molecules arranged in layers perpendicular to theb-axis. The two independent Ca ions and the HP₂O₇ ion comprise one layer; K and H₂P₂O₇ ions and the three water molecules form an interstitial layer. Coordinations of the two independent Ca ions are quite similar, but the environments of HP₂O₇ and H₂P₂O₇ ions are quite different, probably due to their locations in different layers. The general structural features are quite similar to those of Ca(NH₄)HP₂O₇.Certain commercial materials and equipments are identified in this paper to specify the experimental procedure. In no instance does such identification imply recommendation or endorsement by the National Institute of Standards and Technology or the ADA Health Foundation or that the material or equipment identified is necessarily the best available for the purpose.     

Crystal and molecular structures of tri(o-tolyl)phosphinegold(I) purine-6-thiolate ethanol solvate (1/1) and tri(c-hexyl)phosphinegold(I) 6-methyl-2-thiouracilate

The crystal and molecular structures of the title compounds, [(o-tol)₃PAu(6-MP)]·EtOH and [(c-hexyl)₃PAu(6-Me-2-TU)], have been determined and each show the presence of a linear geometry about the Au atom; both of the thionucleobases function as thiolate ligands. Important interatomic parameters for [(o-tol)₃PAu(6-MP)] are Au–S 2.266(2), Au–P 2.239(2) and S–Au–P 177.03(8)° and for [(c-hexyl)₃PAu(6-Me-2-TU)]: Au–S 2.299(3), Au–P 2.244(3) and S–Au–P 176.1(1)°. Crystals of [(o-tol)₃PAu(6-MP)]·EtOH are monoclinic with space groupP2₁/n, and unit cell dimensionsa=10.067(2),b=10.518(2),c=25.416(4) , =98.42(2)°,Z=4. The structure was refined to finalR=0.040 for 4183 data withI3.0(I). Crystals of [(c-hexyl)₃PAu(6-Me-2-TU)] are monoclinic with space groupP2₁/c, and unit cell dimensionsa=9.692(4),b=15.822(4),c=15.775(3) , =94.00(2)°,Z=4,R=0.033 for 2666 data.     

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).     

Crystal structure of (diphenyl)(morpholino)phosphiniminocyclotrithiazene

The title compound (C₆H₅)₂(OC₄H₈N)P=N–S₃N₃ crystallizes in the space group with unit cell parametersa=9.3900(2),b=9.4747(1),c=11.3850(3) Å, =95.73(4), =96.85(6), =104.26(2)^o, and Z=2. The tricoordinated sulfur of the cyclotrithiazene ring deviates from the mean plane of other skeletal atoms by 0.683(4) Å. The angle at this atom is the smallest in the ring and is enclosed by the longest S–N bonds observed in the ring.     

Synthesis and structure of tris(N-methylaminoethanoldithiocarbamato)arsenic(III)

The title compound was synthesized by the interaction of arsenic(III)chloride with freshly prepared N-methylaminoethanoldithiocarbamic acid in methanol. The compound crystallized in the triclinic system, space groupP with two molecules per unit cell, the dimensions area=6.509(10)Å,b=14.077(3)Å,c=14.195(3)Å, =64.16(2)^o, =84.67(2)^o and =84.00(2)^o. The molecule is monomeric with three short (mean 2.320(3)Å) and three long (mean 2.927(2)Å) As-S bonds. Asymmetry in the As-S bonds is due to the presence of stereochemically active lone pair on arsenic and the coordination polyhedron deviates from the usual D₃ symmetry to C₃ symmetry. Disorder exists in one of the dithiocarbamate ligands probably due to the O...O interaction arising from the water molecule. The anisobidenticity of the As-S bond distances is as a consequence of stereochemical requirement of the ligand and the lone pair of electrons on arsenic.     

Synthesis and structural characterization of 2,6-bis-(N-methylenemorpholino)-4-methylphenol (MMP) and 2,6-bis-(N-methylenemorpholino)-4-bromophenol (MBrP)

MMP: C₁₇H₂₆N₂O₃,M _r =306.40, monoclinic, space groupP2₁/c,a=10.927(2),b=10.777(2),c=14.197(2) , =94.04(2)°,V=1667.7(5) ³,D _cal=1.22 Mgm^–3,Z=4,F(000)=664, =5.93 cm^–1,T=293K. FinalR=0.049 andwR=0.063 for 2724 observed reflections. MBrP; C₁₆H₂₃N₂O₃Br,M _r =371.27, monoclinic, space groupP2₁/c,a=10.955(1),b=10.785(1),c=14.213(1) , =94.54(2)°,V=1674.0(4) ³,D _cal=1.48 Mgm^–3,Z=4,F(000)=768, =32.35 cm^–1,T=293K. FinalR=0.055 andwR=0.069 for 2886 observed reflections. MMP and MBrP are isostructural and in both the molecules the morpholino rings assume a chair conformation.DCB Contribution No. 824.     

Anticancer agent development. 4. X-ray crystal structure and intermolecular crystal lattice interactions of methyltrans-4,5-dihydro-4-acetoxymethyl-5-(3,4,5-trimethoxyphenyl)-2-(3,4-methylenedioxyphenyl)-3-furancarboxylate

The title compound, C₂₅H₂₆O₁₀,M ^r=486.48, crystallized from methanol in the acentric space group P2₁,2₁2₁, witha=7.617(3),b, 12.703(3),c=24.408(3) Å,V=2362 ų,D ^calc=1.37 g cm^–3 and=0.66 cm^–1 forZ=4. Least-squares refinement of 1417 observed [F ^o5(F ^o)] reflections led to the final agreement index ofR=0.044. The observed structure reveals atrans relationship for the 4-acetoxymethyl and 5-aryl substituents. The 4,5-dihydrofuran ring system assumes a slight envelope conformation. Several intermolecular van der Waals interactions of note occur in this compound.