Crystal Structure of [Zn(2-Bromobenzoato)<Subscript>2</Subscript>]<Subscript><Emphasis Type="Italic">n</Emphasis></Subscript> and [Zn(2-Bromobenzoato)<Subscript>2</Subscript>(<Emphasis Type="Italic">N</Emphasis>-Methylnicotinamide)]<Subscript>2</Subscript>

Abstract  

The syntheses and structural characterizations of two novel 2-bromobenzoatozinc(II) complexes—[Zn(2-BrC₆H₄COO)₂] _n (I) and [Zn(2-BrC₆H₄COO)₂(mnad)]₂ (II), where mnad is N-methylnicotinamide are reported. Compound (I) crystallized with a monoclinic lattice (space group P2₁/c) and is polymeric in solid state. Its cell parameters are: a = 7.37220(10) Å, b = 19.9639(3) Å, c = 30.2756(5) Å, β = 94.7510(7)°, V = 4440.59(12) ų, Z = 4. The coordination environments of all zinc atoms are distorted tetrahedra built from four carboxylate oxygen atoms coming from four 2-bromobenzoato ligands. Compound (II) crystallized with a monoclinic lattice (space group P2₁/c) with a = 11.7488(2) Å, b = 20.3683(3) Å, c = 9.30130(10) Å, β = 100.3941(11)°, V = 2189.30(5) ų, Z = 2. This dimeric molecule features a paddle-wheel [Zn₂O₈] cage in solid state; the coordination environment of the central atom is square pyramidal consisting of four carboxylate oxygen atoms and the pyridine N atom of the mnad ligand.     

Structures of Three New (Phenylsulfonyl)Indole Derivatives

Abstract  

Three new 1-(phenylsulfonyl)indole derivatives, 3-acetyl-2-ethyl-1-(phenylsulfonyl)indole, (I), 2-benzyl-1-(phenylsulfonyl)indole, (II), and 3-trimethylsilylethynyl-1-(phenylsulfonyl)indole, (III), have been synthesized and their crystal structures determined by single crystal X-ray crystallography. (I), C₁₈H₁₇NO₃S, is triclinic with space group P-1 and cell constants: a = 8.6129(2) Å, b = 8.8366(2) Å, c = 11.0108(2) Å, α = 72.7920(1)°, β = 75.0120(1)°, γ = 77.2550(1)°, V = 763.79(3) ų and Z = 2. (II), C₂₁H₁₇NO₂S, is monoclinic with space group P21/n and cell constants: a = 10.8355(18) Å, b = 10.6987(19) Å, c = 14.472(3) Å, β = 75.0120(1), V = 1675.2(5) ų and Z = 4. (III), C₁₉H₁₉NO₂SSi, is monoclinic with, space group P21/c and cell constants: a = 12.9596(1) Å, b = 10.543(3) Å, c = 13.543(2) Å, β = 93.58°, V = 1846.8(6)ų and Z = 4. All three have the same (phenylsulfonyl)indole skeleton with different ligands attached to the 2- and 3-sites of the indole ring. The angle between the mean planes of the indole and benzyl groups is 76.9(6)° (I), 82.9(3)° (II), 89.6(2)° (III) and between the sulfonyl group with the indole and benzyl rings is 61.2(9)° (I), 59.0((5)° (II), 51.5(6)°, 42.5(8)° (III) and 51.5(6)°(I), 44.3(8)° (II), 47.2(8)° (III), respectively. In addition to the ligand substitutions, weak intermolecular C–H···O hydrogen bond interactions and π stacking interactions between the π orbitals of nearby indole and phenyl rings influence these twist angles. Comparison to a MOPAC AM1 computational calculation supports these observations.     

The Crystal Structures of Some 1-Aryl-5-methyl-1,2,3-triazole Derivatives

Abstract  The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C₉H₈BrN₃, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2) ?, α = 90.00, β = 116.01(3), γ = 90.00o. V = 949.6(3) ?³, Z = 4, Dx = 1.665 Mg m⁻³. The final R was 0.0477. Compound 4b, C₁₃H₁₁N₃, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?³, Z = 8, D _m = 1.304 Mg m⁻³. The final R was 0.0565. Index Abstract  The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C9H8BrN3, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2)  ?, α = 90.00, β = 116.01(3), γ =90.00o. V = 949.6(3) ?³, Z = 4, Dx = 1.665 Mg m⁻³. The final R was 0.0477. Compound 4b, C13H11N3, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?³, Z = 8, D _m = 1.304 Mg m⁻³. The final R was 0.0565.      

Synthesis and Structural Characterization of Bis[(cyclohexylamino)pent-2-en-4-onato]-Chromium(II)

Abstract  Addition of one equivalent of CrI₂ to two equivalents of lithium cyclohexylamino-pent-2-en-4-onate results in bis[(cyclohexylamino)pent-2-en-4-onato]-chromium(II). Crystallization in diethylether reaction solvent forms the hemi-etherate A with the asymmetric unit showing two target compounds and one molecule of cocrystallized diethylether in the P-1 space group with crystal cell parameters a = 12.931(4) Å, b = 13.207(4) Å, c = 16.104(5) Å, α = 66.559(5)°, β = 77.670(5)°, γ = 81.562(5)°, V = 2,459.1(14) Å³ and Z = 4. Drying A in vacuo and recrystallization in pentane yields a nonsolvated crystalline phase B with an asymmetric unit displaying only one molecule of the target compound in the P2₁/c space group with crystal cell parameters a = 14.290(7) Å, b = 14.082(7) Å, c = 11.246(6) Å, β = 94.807(8)°, V = 2,255.1(19) Å³ and Z = 4. Graphical Abstract  A Cr(II) complex supported by two β-enaminoketiminato ligands, bis[(cyclohexylamino)pent-2-en-4-onato]-chromium(II), has been synthesized and has been structurally characterized in two different crystal phases.      

Synthesis,Crystal Structures and Magnetic Properties of Two Three-Dimensional Cerium(III) and Erbium(III) Coordination Polymers

Abstract  

Two lanthanide(III) coordination polymers, namely [Ce(pzdc)_1.5(H₂O)] _n (1), [Er(pzdc)(μ₂-OH)(H₂O)] _n ·nH₂O (2) (H₂pzdc = pyrazine-2,5-dicarboxylic acid), have been hydrothermally synthesized and characterized by single crystal X-ray diffraction and magnetic measurements. Polymer 1 crystallizes in triclinic space group P-1, with a = 6.2875(6), b = 6.7396(6), c = 13.3858(14) Å, α = 82.858(4), β = 83.118(4), γ = 63.452(4)°, V = 502.16(8) Å³, and Z = 2. Polymer 2 crystallizes in monoclinic space group P2(1)/c, with a = 11.706(4), b = 6.151(2), c = 14.063(5) Å, β = 92.255(3), V = 502.16(8) Å³, and Z = 4. Single-crystal X-ray diffraction studies show that compound 1 possess a 3D framework structure consisted of double chains. Compound 2 features a 3D open framework structure with a dinuclear Er(III) secondary building unit. Magnetic studies for complex 1 show stronger antiferromagnetic coupling between the Ce(III) ions.     

Synthesis and Crystal Structure of a Depside Derivative 2-(2-Methoxy-2-oxoethyl)phenyl 2-(3,4-Dimethoxyphenyl)acetate

Abstract  

A depside derivative, 2-(2-methoxy-2-oxoethyl)phenyl 2-(3,4-dimethoxyphenyl)acetate (3), was synthesized through a facile approach in high yields. Its structure was confirmed by ¹H NMR, ¹³C NMR, ESI mass spectra, elemental analyses and X-ray single crystal diffraction study. Crystal structure analysis revealed that compound 3 crystallized in the monoclinic, space group P2₁/c with the following unit cell parameters: a = 10.173(2) Å, b = 10.459(2) Å, c = 16.516(3) Å, α = 90°, β = 102.30(3)°, γ = 90°, V = 1717.0(6) Å³, Z = 4.     

Ethynyl and Propynylpyrene Inhibitors of Cytochrome P450

Abstract  

The single-crystal X-ray structures and in vivo activities of three aryl acetylenic inhibitors of cytochromes P450 1A1, 1A2, 2A6, and 2B1 have been determined and are reported herein. These are 1-ethynylpyrene, 1-propynylpyrene, and 4-propynylpyrene. To investigate electronic influences on the mechanism of enzyme inhibition, the experimental electron density distribution of 1-ethynylpyrene has been determined using low-temperature X-ray diffraction measurements, and the resulting net atomic charges compared with various theoretical calculations. A total of 82,390 reflections were measured with Mo Kα radiation to a (sinθ/λ)_max = 0.985 Å⁻¹. Averaging symmetry equivalent reflections yielded 8,889 unique reflections. A least squares refinement procedure was used in which multipole parameters were added to describe the distortions of the atomic electron distributions from spherical symmetry. A map of the model electron density distribution of 1-ethynylpyrene was obtained. Net atomic charges calculated from refined monopole population parameters yielded charges that showed that the terminal acetylenic carbon atom (C18) is more negative than the internal carbon (C17). Net atomic charges calculated by ab initio, density functional theory, and semi-empirical methods are consistent with this trend suggesting that the terminal acetylenic carbon atom is more likely to be the site of oxidation. This is consistent with the inhibition mechanism pathway that results in the formation of a reactive ketene intermediate. This is also consistent with assay results that determined that 1-ethynylpyrene acts as a mechanism-based inhibitor of P450s 1A1 and 1A2 and as a reversible inhibitor of P450 2B1. Crystallographic data: 1-ethynylpyrene, C₁₈H₁₀, P2₁/c, a = 14.571(2) Å, b = 3.9094(5) Å, c = 20.242(3) Å, β = 105.042(2)°, V = 1,113.5(2) Å³; 1-propynylpyrene, C₁₉H₁₂, P2₁/n, a = 8.970(2) Å, b = 10.136(1) Å, c = 14.080(3) Å, β = 99.77(2)°, V = 1,261.5(4) Å³; 4-propynylpyrene, C₁₉H₁₂, Pbca, a = 9.904(1) Å, b = 13.174(2) Å, c = 19.401(1) Å, V = 2,531.4(5) Å³.     

The molecular structures of three germacrolides related to parthenolide

The germacrolide-class sesquiterpene lactone, 1,10-epoxyparthenolide, C₁₅H₂₀O₄,1, crystallizes with two independent molecules in monoclinic space groupP2₁ witha=10.6845(5),b=9.0763(4),c=15.4326(7) ?, β=105.887(4)°,V=1439.4(3) ?³,Z=4.R=0.037 for 2425 observed data. Its 11βH, 13-dihydro-derivative 1,10-epoxydihydroparthenolide, C₁₅H₂₂O₄,2, crystallizes in orthorhombic space groupP2₁2₁2₁ witha=7.6414(10),b=12.559(2),c=14.6821(14) ?,V=1409.0(3) ?³ Z=4.R=0.031 for 1555 observed data. The corresponding unexposidized compound, 11βH,13-dihydrocostunolide, C₁₅H₂₂O₂,3, crystallizes with three independent molecules in orthorhombic space groupP2₁2₁2₁ witha=7.3576(5),b=23.505(3),c=24.185(2) ?,V=4182(1) ?³,Z=12.R=0.070 for 2767 observed data. In all, the 10-membered rings adopt approximate chair-chair conformations. In all, the double bonds or epoxidized double bonds are E, both methyl groups on the 10-ring are β, and the α-methylene-γ-lactone (or α-methyl-γ-lactone) istrans-fused at C6 and C7 with H6 β and H7 α. In the dihydro compounds, the H at C11 is β.     

Bis[(2,3,4-Trimethoxy-Benzylidenepropylideneamino)Phenyl]Ether: Synthesis,Characterization and Crystal Structure

Abstract  

New Schiff base compound bis[(2,3,4-trimethoxy-benzylidenepropylideneamino)phenyl]-ether (1) was synthesized and characterized by elemental analyses (CHN), FT-IR and ¹H-NMR spectroscopy and single-crystal X-ray diffraction. The title compound 1 crystallizes in triclinic system, space group P-1, with a = 6.8255(4) Å, b = 10.4346(4) Å, c = 19.4166(8) Å, α = 86.588(3)°, β = 85.019(4)°, γ = 89.042(4)°, V = 1375.12(11) Å³ and Z = 2. It displays a trans configuration about the C=N double bonds.     

Crystal Structures of a Series of 1,1-Spiro-bis(1,2,3,4-tetrahydronaphthalene)-Based Derivatives

Abstract  

The structures of four spirobisnaphthalenes based monomers 1, 2, 3a and 3b are reported. Each compound represents a methoxylated precursor which after deprotection led to the formation of a monomer successfully used for the synthesis of Polymers of intrinsic microporosity. The spiro-centre represents the site of contortion that, since its rigidity, leads to inefficient packing in the solid state inducing microporosity in the final polymer. Compound 1 crystallized in the monoclinic P2/c space group with unit cell parameters a = 8.1659(19) ?, b = 7.5298(18) ?, c = 19.130(5) ?, β = 97.935(4)°, V = 1165.0(5) ?³, Z = 2, D = 1.210 Mg m⁻³. Compound 2 crystallized in the monoclinic P2₁/n space group with unit cell parameters a = 12.6940(9) ?, b = 7.7267(6) ?, c = 19.9754(15) ?, β = 97.220(1)°, V = 1943.7(3) ?³, Z = 4, D = 1.355 Mg m⁻³. Compound 3a crystallized in the monoclinic P2₁/c space group with unit cell parameters a = 16.8137(14) ?, b = 10.5577(9) ?, c = 31.344(3) ?, β = 103.618(1)°, V = 5407.5(8) ?³, Z = 8, D = 1.308 Mg m⁻³. Compound 3b crystallized in the monoclinic Pc space group with unit cell parameters a = 15.594 ?, b = 12.564 ?, c = 18.339 ?, β = 90.224(1)°, V = 3593.0 ?³, Z = 4, D = 1.236 Mg m⁻³.     

Syntheses and Crystal Structures of Two 2-Aminoisoflavones

Abstract  

2-Amino-7,4′-dimethoxyisoflavone (I), C₁₇H₁₅NO₄ and 2-amino-7-methoxy-4′-hydroxyisoflavone (II), C₁₆H₁₃NO₄ were synthesized and their crystal structures were determined by single-crystal X-ray diffraction. They all crystallize in the monoclinic crystal system, space group P21/c. The cell dimensions of I are a = 15.6673(17) ?, b = 7.3998(8) ?, c = 13.2919(14) ?, β = 111.4460(10)°, D _c = 1.377 mg/mm³, V = 1,434.3(3) A³, Z = 4 and those of II are a = 10.990(7) ?, b = 11.879(7) ?, c = 10.422(6) ?, β = 96.904(11)°, D _c = 1.393 mg/mm³, V = 1,350.8(14) A³, Z = 4. A combination of F-type and T-type aromatic–aromatic interaction and hydrogen bonding links the molecules of I into a tri-dimensional framework structure. In the crystal structure of II, paired tri-centered hydrogen bond generates a R₄²(21) ring and the R₄²(21) rings link the molecules into a sheet.     

Cross Coupling of Substituted Anilines with Quinoline: Synthesis and Structural Characterization of HN(py)quin,PhN(py)quin,MesN(py)quin,and [PhN(py)(H-quin)]BF<Subscript>4</Subscript>

Abstract  

The molecular structure of (2,6-ⁱPr₂C₆H₃)N(quin)₂ (1) and both the methanol and toluene solvates of its copper complex [Cu{(2,6-ⁱPr₂C₆H₃)N(quin)₂}₂]BF₄, 2·MeOH and 2.2(C₆H₅Me), respectively, have been determined. The quinolyl rings in 1 adopt anti-syn (C_Ar–N–C–N_quin) conformation as a result of π–π stacking. The cation in 2·MeOH crystallizes on a C₂ axis, while the cation in 2·2(C₆H₅Me) is crystallographically independent. As a result of intramolecular π–π stacking there are significant changes within the coordination geometry about the copper centers between the two solvates, suggesting that the coordination around copper is supple. Crystal data: 1 group P2₁/c, a = 8.614(1), b = 16.137(3), c = 17.601(4) ?, β = 93.32(3)°, V = 2,442.5(9) ?³, Z = 4, R = 0.0544, wR ₂ = 0.1340. 2·MeOH group P3₂21, a = 13.254(1), b = 13.254(1), c = 27.214(5) ?, V = 4,140(1) ?³, Z = 3, R = 0.0392, wR ₂ = 0.0917. 2.2(C₆H₅Me) group P1, a = 11.677(2), b = 16.261(3), c = 17.077(3) ?, α = 93.63(3), β = 97.30(3), γ = 96.26(3)°, V = 3,187(1) ?³, Z = 4, R = 0.0526, wR ₂ = 0.1221.     

Co-crystal Structure of 11-Hydroxy-2,3,9-trimethoxy-6<Emphasis Type="Italic">H</Emphasis>-chromeno[3,4-<Emphasis Type="Italic">b</Emphasis>]chromen-12-one and 11-Hydroxy-2,3,9-trimethoxy-chromeno[3,4-<Emphasis Type="Italic">b</Emphasis>]chromene-6,12-dione

Abstract  

A 1:1 co-crystal structure of 11-hydroxy-2,3,9-trimethoxy-6H-chromeno[3,4-b]chromen-12-one and 11-hydroxy-2,3,9-trimethoxy-chromeno[3,4-b]chromene-6,12-dione (stemonone) was crystallized from the reaction mixture of 6-deoxyclitoriacetal and methanesulfonyl chloride, and its structure was characterized by X-ray diffraction. This co-crystal crystallizes in a triclinic crystal system, space group P(−1) with unit cell parameters of a = 8.1317(3) Å, b = 9.8224(4) Å, c = 10.7268(3) Å, α = 78.116(1)°, β = 77.463(1)°, γ = 77.140(1)°, Z = 2 and V = 804.11(3) Å³. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F ² to final values of R ₁ = 0.0501 and wR ₂ = 0.1520.     

Synthesis,Crystal Structures and Fluorescence Properties of Ni (II) and Cu (II) Complexes with 1-(Furan-2-ylmethylene)-4-phenylthiosemicarbazone

Abstract  

Two coordination complexes, NiL ₂ and CuL ₂ {L = bis[1-(furan-2-ylmethylene)-4-phenylthiosemicarbazone]}, were synthesized and determined by X-ray crystallography. Both crystallize in the Orthorhombic system, space group Pbcn, with lattice parameters: a = 11.935 (2) Å, b = 15.314(3) Å, c = 12.952(3) Å and Z = 4 for Ni (II); a = 20.850(4) Å, b = 15.049(3) Å, c = 7.5633(5) Å and Z = 4 for Cu (II). In both complexes, the central metal atom is coordinated in a distorted square-planar with two ligands through two S and N atoms, respectively. The EA, UV, IR and TG-DTG were studied and the possible structures of the complexes were speculated. Moreover, the fluorescence of the complexes were studied. The results reveal that copper complex can emit purple fluorescence in solvents.     

Syntheses,Structural Characterization and Thermoanalysis of Transition-Metal Compounds Derived from 3,5-Dinitropyridone

Abstract  

Nine metal compounds of Mn(II), Zn(II) and Cd(II) derived from dinitropyridone ligands (3,5-dinitropyrid-2-one, 2HDNP; 3,5-dinitropyrid-4-one, 4HDNP and 3,5-dinitropyrid-4-one-N- hydroxide, 4HDNPO) were characterized by elemental analysis, FT-IR and partly by TG-DSC. Three of which were further structurally characterized by X-ray single-crystal diffraction analysis. The structures of the three compounds, Mn(4DNP)₂(H₂O)₄, 4, Zn(4DNPO)₂(H₂O)₄, 8, and Cd(4DNPO)₂(H₂O)₄, 9, crystallize in the monoclinic space group P2(1)/n and Z = 2, with a = 8.9281(9), b = 9.1053(9), c = 10.6881(11) Å, β = 97.9840(10)° for 4; a = 8.4154(7), b = 9.9806(8), c = 10.5695(8) Å, β = 97.3500(10)° for 8; a = 8.5072(7), b = 10.2254(8), c = 10.5075(8) Å, β = 96.6500(10)° for 9. All three complexes are octahedral consisting of four equatorial water molecules, and two nitrogen or oxygen donor ligands (DNP or DNPO). The abundant hydrogen-bonding and π-π stacking interactions seem to contribute to stabilization of the crystal structures of the compounds. The TG-DTG results revealed that the complexes showed a weight loss sequence corresponding to all coordinated water molecules, nitro groups, the breaking of the pyridine rings and finally the formation of metal oxides.     

Pentacarbonyl(trimethylamine)chromium and Pentacarbonyl(trimethylamine)Molybdenum

Abstract  

Pentacarbonyl(trimethylamine)chromium (1) and pentacarbonyl(trimethylamine)molybdenum (2) are isomorphous and crystallize in the space group P2₁/n, a = 6.8267(14) ?, b = 11.269(2) ?, c = 14.692(3) ?, β = 102.89(3)°, V = 1,101.8(4) ?³, Z = 4 for 1 and a = 6.949(5) ?, b = 11.362(5) ?, c = 14.927(5) ?, β = 102.639(5)°, V = 1,150.0(10) ?³, Z = 4 for 2; both compounds possess distorted octahedral molecular geometries that result from the steric influence of the coordinated amine ligand.     

Synthesis and Crystal Structures of Two Novel Complexes with <Emphasis Type="Italic">N</Emphasis>-[2-(5-Bromo-2-Hydroxybenzylideneamino)Ethyl]-4-Methylbenzenesulfonamide as Ligand

Abstract  

Two novel complexes constructed from the sulfonamide Schiff base ligand H ₂ L, N-[2-(5-bromo-2-hydroxybenzylideneamino)ethyl]-4-methylbenzene-sulfonamide, [Cu(HL)₂] (1) and [CuL(H₂O)] (2) are synthesized and characterized via X-ray single-crystal diffraction, elemental analysis, FT-IR and UV–Vis. 1 and 2 both form 1-D supramolecular architectures by π–π stacking interactions. 1 and 2 both crystallize in monoclinic, with space group C2/c and P2/c for 1 and 2, with unit cell parameters a = 27.640(18) ?, b = 7.907(5) ?, c = 17.945(14) ?, β = 118.27(2)°, V = 3454(4) ?³, Z = 4 for 1, and a = 16.758(5) ?, b = 7.272(2) ?, c = 15.080(4) ?, β = 106.334(5)°, V = 1763.6(9) ?³, Z = 4 for 2.     

Molecular Structures of RN(H)Py (R?=?2,4,6-Me3C6H2, 2,6-Et2C6H3, Ph3C), and the Copper Complex [Cu{(2,4,6-Me3C6H2)N(H)Py}2]BF4

Abstract  The molecular structures of RN(H)Py [R = 2,4,6-Me₃C₆H₂ (1), 2,6-Et₂C₆H₃ (2), -CPh₃ (3)] have been determined along with the copper(I) complex [Cu{(2,4,6-Me₃C₆H₂)N(H)Py}₂]BF₄ (4). Each of the amines exists as a hydrogen-bonded head-to-tail dimer. Compound 3 has four independent molecules in the asymmetric unit as a consequence of changes in the relative orientation of the pyridyl and phenyl rings. The copper in 4 is two-coordinate with the conformation of the aryl rings being dominated by inter-cation packing. Crystal data: 1 space group P2₁/c, a = 14.047(3), b = 7.154(1), c = 13.890(3) ?, β = 116.45(3)°; V = 1,249.7(4) ?³, Z = 4, R = 0.0547, wR ₂ = 0.1397; 2 space group P2₁/n, a = 13.035(3), b = 8.120(1), c = 13.562(3) ?, β = 111.87(3)°; V = 1,345.2(5) ?³, Z = 4, R = 0.0669, wR ₂ = 0.1512; 3 space group P2₁/c, a = 26.729(5), b = 17.008(3), c = 18.903(4) ?, β = 92.42(3)°; V = 8,586(3) ?³, Z = 8, R = 0.0911, wR ₂ = 0.163; 4 space group P2₁/c, a = 9.149(1), b = 15.901(3), c = 19.703(4) ?, β = 102.89(3)°; V = 2,794(1) ?³, Z = 4, R = 0.0504, wR ₂ = 0.1291. Graphical Abstract  The hydrogen-bonded head-to-tail dimer structures of RN(H)Py [R = 2,4,6-Me₃C₆H₂, 2,6-Et₂C₆H₃, -CPh₃] have been determined along with the two-coordinate copper complex [Cu{(2,4,6-Me₃C₆H₂)N(H)Py}₂]BF₄      

The preparation and crystal structures of [Ru(bpy) (η2-tpy)(CO)CH2OAc]PF6 and [Ru(η3-tpy)(CO)CH2OAc] PF6 (bpy = 2,2′-bipyridine; tpy = 2,2′:6′,2″ terpyridine)

The first titled compound, 1, was obtained by treating [Ru(bpy)(η²-tpy)(CO)CH₂OH]PF₆ with acetic anhydride. Heating 1 in acetonitrile afforded 2, [Ru((η³-tpy)(MeCN)(CO) CH₂OAc]PF₆. Allowing 2 to stand in CH₂Cl₂ followed by concentration and precipitation afforded the second titled compound, 3 ([Ru((η³-tpy)(CO)–CH₂OAc]PF₆), in which the acetoxymethyl group had become bidentate. Crystal data for 1, monoclinic crystal system, space group C2/c, a=26.001(4) ?, b=13.0395(18) ?, c=20.718(3) ?, β=107.700(2)°, V=6691.7(16) ?³, Z=8; for 3, monoclinic crystal system, space group P2₁/n, a=10.864(2) ?, b=16.922(4) ?, c=11.127(2) ?, β=90.907(3)°, V=2045.4(8) ?³, Z=4.