Crystal structures of 4-(oxiran-2-ylmethoxy) benzoic acid and 4-acetoxybenzoic acid

Compounds 4-(oxiran-2-ylmethoxy)benzoic acid (2) and 4-acetoxybenzoic acid (4) are synthesized by a new synthetic route and studied by X-ray crystallography. Compound 2 crystallizes in the monoclinic system, P2₁/n space group, a = 5.1209(2) ?, b = 30.3429(16) ?, c = 5.9153(3) ?, β = 96.725(3)°, V = 912.81(8) ?³, Z = 4. Compound 4 crystallizes in the triclinic system, P-1 space group, a = 7.3400(4) ?, b = 8.0819(3) ?, c = 15.6548(9) ?, α = 85.754(3)°, β = 84.268(2)°, γ = 70.023(3)°, V = 867.63(8) ?³, Z = 4. The crystal structure of 2 comprises two crystallographically independent molecules of the compound. In the crystal structures of 2 and 4, pairs of molecules form carboxyl dimers.     

Crystal structure of a new mononuclear complex of Mn(II) with a bbbi ligand (bbbi = 1,4-bis(benzimidazol-1-yl)-2-butene)

A new mononuclear complex Mn(bbbi)₂(H₂O)₄(ClO₄)₂·(bbbi)₂·(H₂O)₂ 1 (bbbi = 1,4-bis(benzimidazol-1-yl)-2-butene) is synthesized under hydrothermal conditions and characterized by IR spectroscopy, elemental analysis, and single crystal X-ray structural analysis. Crystal data for 1: triclinic, , a = 8.8478(7) ?, b = 15.0550(11) ?, c = 16.4310(12) ?, α = 108.657(7)°, β = 104.044(7)°, Γ = 99.317(7)°, V = 1942.2(3) ?³, Z = 1, final R = 0.0621. Each manganese atom is octahedrally coordinated by four aqua ligands and two nitrogen atoms of two distinct bbbi ligands. The molecule is stabilized by hydrogen bonding and π…π interactions.     

Crystal structure of [Cu(NH3)4](ReO4)2

At T = 150 K, the crystal structure of [Cu(NH₃)₄](ReO₄)₂ is studied: a = 6.5167(3) ?, b = 6.7790(3) ?, c = 7.4627(3) ?, α = 67.336(1)°, β = 80.004(1)°, γ = 70.687(1)°, V = 286.70(2) ?³, P-1 space group, Z = 1, d _x = 3.661 g/cm³. We analyze the packing of ions using the translation sublattice isolation technique.     

Crystal structure of [Pd(P(i-Pr)3)2(acac)]BF4

A single crystal X-ray diffraction study is carried out for [Pd(P(i-Pr)₃)₂(acac)]BF₄, T = 150(2) K. Crystal data: a = 10.2935(4) ?, b = 11.3591(5) ?, c = 13.8728(6) ?, α = 89.154(2)°, β = 68.448(1)°, γ = 85.032(1)°, P-1 space group, V = 1502.75(11) ?³, Z = 2, d _x = 1.354 g/cm³.     

Crystal structure of 2-(6-chloro-4-P-tolylamino)pyrido[3,2-d]pyrimidin-1-ium-1-yl)acetate oxonium bromide

The crystals of 2-(6-chloro-4-(p-tolylamino)pyrido[3,2-d]pyrimidin-1-ium-1-yl)acetate (zwitterionic form) oxonium bromide, C₁₆H₁₃ClN₄O₂·Br⁻·H₃O⁺ (I) were prepared and studied by single-crystal X-ray diffraction method. The compound crystallizes in the triclinic space group P-1 with a = 8.3121(8) ?, b = 9.3885(8) ?, c = 13.2903(12)?, α = 106.788(2)°, β = 95.204(3)°, γ = 110.871(2)°, V = 905.81(14) ?³, Z = 2; final R = 0.053, wR2 = 0.150. It is interesting that methylene C in the BrCH₂COOH molecule binds to the N1 of the pyrimidine ring. In the crystal studied, two neighboring organic molecules are connected by hydrogen bonds through carboxylate oxygen, oxonium and bromide ions to form a dimer.     

Crystal structure of a nickel(II) complex with the macrocyclic ligand 4-methyl-1,3,5,8,11,14-hexaazatricyclooctadecane

The crystal structure of the macrocyclic complex [Ni(PCHA)](ClO₄)₂ (II) (PCHA = 4-methyl-1,3,5,8,11,14-hexaazatricyclooctadecane) is described. In the presence of succinate acid, [Ni(PCHA)](ClO₄)₂ (II) is obtained by recrystallization of orange crystals of [Ni(PCHA)](ClO₄)₂ (I), whose structure has previously been identified. The [Ni(PCHA)](ClO₄)₂ (II)crystal belongs to the monoclinic P2(1)/c space group with a = 15.8561(3) ?, b = 9.4409(2) ?, c = 13.9297(2) ?, α = 90°, β = 94.8840(10)°, γ = 90°, M _r = 526.02, Z = 4, V = 2077.65(7) ?³. The structure is ionic with [Ni(L)]²⁺ and two perchlorate anions with a supermolecular interaction.     

Crystal and molecular structures of 2-(4-chlorophenyl)-5,7-dimethoxyquinolin-4-yl phenyl bis(2-chloroethyl) phosphoramidate

2-(4-Chlorophenyl)-5,7-dimethoxyquinolin-4-yl phenyl bis(2-chloroethyl)phosphoramidate is synthesized and characterized by NMR, IR and single crystal X-ray crystallography. The crystal is triclinic, P[`1]P\bar 1 space group, with a = 9.5188(19) ?, b = 12.856(3) ?, c = 13.250(3) ?, V = 1412.0(5) ?)³, and Z = 2 (at 291(2) K). The crystal packing arrangement indicates that the molecule is stacked through π...π aromatic stacking interactions.     

Preparation, Structure, and Thermal Decomposition of Co(II) Complexeswith 2,3- and 2,5-Dichlorobenzoic Acid and Imidazole

Summary.  The reaction products of Co(II)-2,3- and -2,5-dichlorobenzoate with imidazole (1, 2; CoL ₂⋯2imdċ2H₂O, L=C₇H₃Cl₂O, imd=imidazole) were characterized by their spectroscopic and thermochemical properties. The compounds crystallize in the monoclonic system with space group = P2₁/c, a=13.848(3), b=12.841(3) ?, c= 7.064(2) ?, β=98.12 °, V=1243.5(4) ?³, Z=2 for 1 and space group =P2₁/n, a=13.293(3), b= 6.964(2), c=13.800(3) ?, β=108.92(3) °, V=1208.6(4) ?³, Z=2 for 2. The complexes lose their crystal water in one step at 333 K and subsequently decompose to CoO with intermediate formation of Co₃O₄. Received August 9, 1999. Accepted (revised) February 11, 2000     

Crystal structure of [Pd(NH3)4][Rh(NH3)(NO2)5]

An XRD analysis is used to study the single crystal of [Pd(NH₃)₄][Rh(NH₃)(NO₂)₅] double complex salt at T = 150(2) K. Crystallographic characteristics are as follows: a = 7.6458(5) ?, b = 9.8813(6) ?, c = 9.5788(7) ?, β = 109.469(2)°, V = 682.30(8) ?³, P2₁/m space group, Z = 2, d _x = 2.553 g/cm³. The geometry of the complex [Rh(NH₃)(NO₂)₅]²⁻ anion is described for the first time: Rh-N(NO₂) distances are 2.020(4)–2.060(3) ?, Rh-N(NH₃) 2.074(4) ?, N(NO₂)-Rh-N(NH₃) trans-angle is 178.8(2)°.     

Preparation, Structure, and Thermal Decomposition of Co(II) Complexeswith 2,3- and 2,5-Dichlorobenzoic Acid and Imidazole

 The reaction products of Co(II)-2,3- and -2,5-dichlorobenzoate with imidazole (1, 2; CoL ₂⋯2imdċ2H₂O, L=C₇H₃Cl₂O, imd=imidazole) were characterized by their spectroscopic and thermochemical properties. The compounds crystallize in the monoclonic system with space group = P2₁/c, a=13.848(3), b=12.841(3) ?, c= 7.064(2) ?, β=98.12 °, V=1243.5(4) ?³, Z=2 for 1 and space group =P2₁/n, a=13.293(3), b= 6.964(2), c=13.800(3) ?, β=108.92(3) °, V=1208.6(4) ?³, Z=2 for 2. The complexes lose their crystal water in one step at 333 K and subsequently decompose to CoO with intermediate formation of Co₃O₄.     

Crystal structure of 2-butylamino-3-(4-fluorophenyl) benzofuro[3,2-d]pyrimidin-4(3H)-one

The title compound (C₂₀H₁₈FN₃O₂, Mr = 351.37) is prepared and its crystal structure is determined by single crystal X-ray diffraction. The crystal is tetragonal, the P-42(1)c space group with a = 11.0922(6) ?, b = 11.0922(6) ?, c = 28.6271(15) ?, V = 3522.2(3) ?³, Z = 8, d _x = 1.325 g/cm³, F(000) = 1472, μ = 0.095 mm⁻¹, MoK _α radiation (λ = 0.71073), R = 0.0505, wR = 0.1090 for 2433 observed reflections with I > 2σ(I). The X-ray diffraction analysis reveals that all ring atoms in the benzo[4,5]furo[3,2-d]pyrimidinone moieties are almost coplanar.     

Structure and DFT calculations of 2-{[3-methyl-3-phenyl-cyclobutyl)-thiazol-2-yl]-hydrazonomethyl}-phenol

The title compound 2-{[3-Methyl-3-phenyl-cyclobutyl)-thiazol-2-yl]-hydrazonomethyl}-phenol (C₂₁H₂₁N₃S₁O₁) crystallizes in the P-1 triclinic space group with a = 5.8880(4) ?, b = 9.5618(5) ?, c = 17.0484(10) ?, α = 80.214(5)°, β = 80.532(5)°, γ = 80.116(5)°. In addition to molecular geometry and packing from X-ray experiment, we have also calculated the molecular geometry and vibrational frequencies of the title compound in the ground state using density functional theory DFT (B3LYP) with the 6–31G(d,p) basis set. Apart from this, the structure of the title compound is characterized by ¹H NMR, ¹³C NMR, IR and UV-vis. Spectra, and the experimental emission energies are compared with the HOMO-LUMO energy gaps calculated by the DFT method.     

Crystal structures of new double complex salts [M(NH3)5Br][AuBr4]2·H2O, where M = Ir, Rh and complex salt [Ir(NH3)5Br]Br2

The crystal structures of double complex salts [M(NH₃)₅Br][AuBr₄]₂·H₂O (M = Ir, Rh) are determined by single crystal XRD. The compounds crystallize in the triclinic system, P-1 space group, Z = 4. Crystallographic characteristics: [Ir(NH₃)₅Br][AuBr₄]₂·H₂O: a = 8.2982(3) ?, b = 15.3045(4) ?, c = 17.4378(6) ?, α = 73.064(1)°, β = 88.938(1)°, γ = 86.221(1)°, V = 2113.95(12) ?³, d _x = 4.419 g/cm³, R = 0.0469; [Rh(NH₃)₅Br][AuBr₄]₂·H₂O: a = 8.2855(2) ?, b = 15.2881(3) ?, c = 17.4053(4) ?, α = 73.015(1)°, β = 88.913(1)°, γ = 86.267(1)°, V = 2104.08(8) ?³, d _x = 4.165 g/sm³, R = 0.0480. The crystal structure of [Ir(NH₃)₅Br]Br₂ is determined. The compound crystallizes in the orthorhombic system, Pnma space group, Z = 4. Crystallographic characteristics: a = 13.8521(3) ?, b = 10.8570(2) ?, c = 6.9908(1) ?, V = 1049.31(3) ?³, d _x = 3.273 g/cm³, R = 0.0127.     

Zinc citrate with alkali metal and ammonium cations: Crystal structure of K4[Zn(Citrate)2]

In the crystal of K₄[Zn(Citrate)₂], two citrate anions coordinate Zn(II) cation with octahedral geometry in the [Zn(Citrate)₂]⁴⁻ complex anion, and the charge is balanced by four potassium ions. Crystal data: monoclinic, P2₁/c, a = 8.502(2) ?, b = 13.210(3) ?, c = 8.942(2) ?, β = 113.132(4)°, V = 923.5(4) ?³, Z = 2, R = 0.0229.     

Crystal structure of the reaction product of copper(II) nitrate with α-(3,3-Dimethyl-3,4-dihydro-1-isoquinolyl)hydroxy-iminoacetonitrile [Cu3(μ3-OH)(μ-L)3(NO3)2(H2O)] · 2H2O

The coordination compound [Cu₃(μ₃-OH)(μ-L)₃(NO₃)₂(H₂O)] · 2H₂O (I), where L is the α-(3,3-dimethyl-3,4-dihydro-1-isoquinolyl)hydroxyiminoacetonitrile anion, has been synthesized. The crystal and molecular structure of I was determined by X-ray diffraction (Enraf-Nonius CAD4, MoK _α radiation, graphite monochromator, ω-scan mode, 2θ_max = 49.96°, 7673 unique reflections, a = 12.745(3) ?, b = 13.726(3) ?, c = 28.835(6) ?, β = 93.44(3)°, V = 5035.2(17) ?³, Z = 4, space group P2₁/c). In the trimer complex I, the copper atoms are combined by a bridging hydroxy group. The copper atoms are additionally linked pairswise by three tridentate chelating bridging organic anions coordinated to the Cu(II) atoms by the N and O atoms of the deprotonated oxime group and by the N atom of the dihydroisoquinoline moiety. Original Russian Text ? V.I. Sokol, V.V. Davydov, N. Yu. Merkur’eva, E.I. Polyakova, Yu.V. Shklyaev, V.S. Sergienko, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 10, pp. 1643–1652.     

Crystal structure of [Cu(en)2](ReO4)2

At T = 150 K the crystal structure of [Cu(en)₂] (ReO₄)₂ (en is ethylenediamine) is studied: a = 6.6229(1) ?, b = 14.2968(3) ?, c = 7.4859(2) ?, β = 102.415(1)°, V = 692.24(3) ?,³, P2₁/c space group, Z = 2, d _x = 3.282 g/cm³. Packing of complex cations is shown to be single layered and pseudohexagonal. Perrhenate anions are located between these layers and additionally coordinate copper atoms with Cu...O distances being 2.504(3) ?.     

Tetrahedral complexes of zinc(II) chloride with N- and O-containing organic ligands: Synthesis and crystal structures of [ZnCl2(C12H12N2O)] and [ZnCl2(H2O)2](Me4Pyz)2

New complex chlorides [ZnCl₂(ODA)] (I) (ODA=oxydianiline, C₁₂H₁₂N₂O) and [ZnCl₂(H₂O)₂](Me₄Pyz)₂ (II) (Me₄Pyz = 2,3,5,6-tetramethylpyrazine) were synthesized and crystallographically characterized. Crystals of I are monoclinic, space group C2/c, a = 22.682(2) ?, b = 12.646(1) ?, c = 9.951(1) ?, β = 93.23(2)°, V = 2849.7(5) ?³, ρ_calc = 1.569 g/cm³, Z = 8. Structure I contains cyclic fragments consisting of two tetrahedral complexes (ZnCl₂N₂) and two coordinated bridging oxydianiline ligands. Crystals of II are monoclinic, space group P2(1)/c, a = 8.972(2) ?, b = 13.862(3) ?, c = 17.528(4) ?, β = 101.72(3)°, V = 2134.5(7) ?³, ρ_calc = 1.384 g/cm³, Z = 4. In structure II, supramolecular pseudo-metallocycles are formed due to formation of hydrogen bonds O(w)-H…N between coordinated water molecules and noncoordinated nitrogen atoms of tetramethylpyrazine molecules.     

Crystal structure of nickel(II) bis-(1,1,1,-trifluoro-5,5-dimethyl-2,4-hexanedionate)-1,3-diaminopropane

The structure of the complex of nickel(II) bis-(1,1,1-trifluoro-5,5-dimethyl-2,4-hexanedionate) with 1,3-diaminopropane is determined by single crystal X-ray diffraction at a temperature of 150 K. Crystallographic data for C₂₀H₃₄F₆N₂NiO₅: a = 17.5446(8) ?, b = 18.1171(10) ?, c = 18.6654(7) ?, β = 115.4150(10)°, space group C2/c, V = 5358.8(4) ?³, Z = 8, d _calc = 1.376 g/cm³, R = 0.0435. The structure is molecular; the metal atom coordinates four oxygen atoms of two β-diketonate ligands and two nitrogen atoms of propylenediamine. In the crystal, the molecules are bonded only by van der Vaals interactions.     

Supramolecular pseudometallacycles in a nickel compound with 4,4-diaminodiphenylmethane: Synthesis and structure of {Ni[(CH2(C6H4NH2)2]2(NO3)2(H2O)2}

The [Ni(DDM)₂(NO₃)₂(H₂O)₂] complex (DDM is 4,4-diaminodiphenylmethane [CH₂(C₆H₄NH₂)₂]) is synthesized, and its structure is determined. The crystals are triclinic, space group P , a = 5.846(1) ?, b = 9.450(2) ?, c = 13.390(3) ?, α = 105.63(3)°, β = 98.13(3)°, γ = 105.84(3)°, V = 666.6(2) ?³, ρ_calcd = 1.553 g/cm³, Z = 2. The Ni(II) ion (in the inversion center) is bound to a distorted octahedral array formed by the nitrogen atoms of the primary amino groups of the DDM molecules and the oxygen atoms of the monodentate nitrato groups and water molecules (Ni(1)-N(3) 2.119(2) ?, Ni(1)-O(1) 2.122(2) ?, Ni(1)-O(w) 2.047(2) ?, angles at the Ni atoms vary in the 85.08(9)°–94.92(9)° interval). The structure contains supramolecular metallacycles formed by the O(w)-H…N(2) hydrogen bonds between the coordinated H₂O molecules and the terminal amino groups of DDM. The metallacycles are joined by the Ni²⁺ ions into infinite chains running in the [111] direction. Original Russian Text ? Yu.V. Kokunov, V.V. Kovalev, Yu.E. Gorbunova, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 11, pp. 1838–1843.     

Gossypol clathrates: Structure and thermal behavior of gossypol solvates with two picoline isomers

Gossypol forms stable solvates with 4- and 2-picolines at room temperature. The solvates are investigated by single crystal X-ray diffraction and thermal analysis. Solvate crystals of gossypol with 4-picoline (1) have the 1:3 composition (gossypol:4-picoline) and crystallize in the P2₁/c space group. This substance is isostructural to a trisolvate of gossypol with pyridine. Solvate crystals of gossypol with 2-picoline (2) have the 1:4 composition (gossypol:2-picoline) and crystallize in the P-1 space group. The unit cell parameters for the investigated structures are as follows: 1 monoclinic crystals, C₃₀H₃₀O₈·3C₆H₇N, a = 10.7530(1) ?, b = 20.7834(3) ?, c = 19.1166(2) ?, β = 95.537(1)°, V = 4252.32(9) ?³, M = 797.92, Z = 4, d _x = 1.246 g/cm³, and R = 0.0489 for 4102 reflections; 2 triclinic crystals, C₃₀H₃₀O₈·4C₆H₇N, a = 11.467(1) ? b = 14.962(2) ?, c = 15.570(3) ?, α = 75.62(1)°, β = 69.83(1)°, γ = 79.58(1)°, V = 2414.6(7) ?³, M = 891.04, Z = 2, d _x = 1.226 g/cm³, and R = 0.0528 for 3779 reflections. The results of the single crystal XRD and thermal analysis confirm that gossypol with 4-picoline forms a trisolvat, and a tetrasolvate with 2-picoline. The transition from 4-picoline to 2-picoline proves to change the type of the host-guest association from one-dimensional to zero-dimensional, i.e., to lead to a new crystal structure. Desolvation of compound 2 begins at a lower temperature than that for compound 1, which is explained by their different crystal structures. Keywords: gossypol, 4-picoline, 2-picoline, clathrate formation, crystal structure.