Acid Co(II) and Ni(II) trifluoroacetate complexes: Synthesis and crystal structure

Anhydrous and partially hydrated acid trinuclear trifluoroacetates of divalent transition metals of the composition [M₃(CF₃COO)₆(CF₃COOH)₆)](CF₃COOH) and [M₃(CF₃COO)₆(CF₃COOH)₂(H₂O)₄)](CF₃COOH)₂, respectively, where M = Co (I, III) Ni (II, IV), were synthesized and studied by X-ray diffraction. Complexes I and II were obtained by crystallization from solutions of M(CF₃COO)₂ · 4H₂O in trifluoroacetic anhydride; complexes III and IV were synthesized under the same conditions with the use of 99% trifluoroacetic acid as a solvent. Crystals I are triclinic: space group $P\bar 1$ , a = 13.199(6) Å, b = 14.649(6) Å, c = 15.818(6) Å, α = 90.04(4)°, β = 114.32(4)°, γ = 108.55(4)°, V = 2611.3(19) ų, Z = 2, R = 0.0480. Crystals II are trigonal: space group $R\bar 3$ , a = 13.307(2) Å, c = 53.13(1) Å, V = 8148(2) ų, Z = 6, R = 0.1112. Crystals III are triclinic: space group $P\bar 1$ , a = 9.001(8) Å, b = 10.379(9) Å, c = 12.119(9) Å, α = 83.67(5)°, β = 72.33(5)°, γ = 83.44(5)°, V = 1068.3(15) ų, Z = 1 Å, R = 0.1031. Crystals IV are triclinic: space group $P\bar 1$ , a = 9.121(18) Å, b = 10.379(2) Å, c = 12.109(2) Å, α = 84.59(3)°, β = 72.20(3)°, γ = 82.80(3)°, V = 1080.94(40) ų, Z = 1, R = 0.0334.     

Crystal and molecular structure of two new Schiff bases: Paeonol-ethylenediamine and paeonol-1,3-propylenediamine

Two new Schiff bases were prepared by the condensation reaction of paeonol with ethylenediamine (for compound 1) and 1,3-propylenediamine (for compound 2). The compounds were studied with single crystal X-ray diffraction method. Compound 1 is monoclinic, space group P2₁/c, a = 10.956(15) Å, b = 6.767(10) Å, c = 12.494(18) Å; β = 104.66(2)°, V = 896(2) ų, Z = 2. Compound 2 is triclinic, space group P-1, a = 6.878(2) Å, b = 12.141(4) Å, c = 12.414(4) Å; α = 101.023(6)°, β = 103.415(6)°, γ = 102.337(6)°, V = 952.8(6) ų, Z = 2. The molecular structures of 1 and 2 are similar; the molecule being centrosymmetric in 1 but asymmetric in 2.     

Copper(I) halide complexes with ethylenediaminium L0(H+)2, N,N,N′,N′-tetraallylethylenediaminium L4(H+)2, and N,N,N,N′,N′-pentaallylethylenediaminium L5(H+). Synthesis and crystal structures of the complexes [L0(H+)2]0.5CuCl2, [L0(H+)2]0.5CuBr1.67Cl0.33, [{L4(H+)2}0.5Cu2Cl3], and [L5(H+)Cu4Br6]

Alkylation of ethylenediamine with allyl bromide in the presence of NaHCO₃ in benzene-ethanol and acetone-ethanol gave N,N,N′,N′-tetraallylethylenediamine L⁴ and N,N,N,N′,N′-pentaallylethylenediaminium bromide (L₅(H⁺)Br₂), respectively. The ac electrochemical synthesis at copper wire electrodes in solutions of copper(II) halide and an appropriate ligand yielded single crystals of Cu(I) complexes with ethylenediaminium ([L⁰(H⁺)₂]_0.5CuCl₂ (I) and [L⁰(H⁺)₂]_0.5CuBr_1.67Cl_0.33 (II)) and its N-allyl derivatives N,N,N′,N′-tetraallylethylenediaminium ([{L⁴(H⁺)₂}_0.5Cu₂Cl₃] (III)) and N,N,N,N′,N′-pentaallylethylenediaminium ([L⁵(H⁺)Cu₄Br₆] (IV)). The crystal structures of complexes I–IV were determined by X-ray diffraction. The isostructural crystals of complexes I and II are triclinic, space group P $ \bar 1 $ , Z = 2. For I: a = 5.936(3), b = 6.387(3), c = 7.126(4) Å, α = 67.82(4)°, β = 72.98(4)°, γ = 67.55(4)°, V = 227.7(2) ų. For II a = 6.110(3), b = 6.657(3), c = 7.309(3) Å, α = 68.40(3)°, β = 72.38(3)°, γ = 67.23(3)°, V = 250.4(2) ų. In structures I and II, the organic cations are between infinite anionic chains (Cu ₂ ^? ) _n . The crystals of π-complex III are triclinic, space group P $ \bar 1 $ , a = 6.851(4), b = 8.729(4), c = 9.960(4) Å, α = 98.25(3)°, β = 102.29(3)°, γ = 107.30(3)°, V = 541.8(5) ų, Z = 2. In structure III, all the four allyl groups are π-coordinated by the metal atoms of four discrete anions Cu₄Cl ₆ ^2? . The crystals of π-complex IV are monoclinic, space group C2/c, a = 15.228(5), b = 17.095(6), c = 20.182(6) Å, β = 92.43(4)°, V = 5249(3) ų, Z = 8. Only two of five allyl groups at the same N atom are coordinated by copper(I) atoms. Structure IV contains a complex inorganic fragment of the formula (Cu₄Br ₆ ^2? ) _n .     

Structure and characterization of A 2D cobalt(II) complex [Co(L)2] n (L = 3-nitro-5-(pyridine-4-yl)benzoate)

The self-assembly of unsymmetrical tecton 3-nitro-5-(pyridin-4-yl)benzoic acid (HL)with cobalt chloride under hydrothermal conditions affords a new 2D coordination polymer [Co(L)₂] _n (1, L = 3-nitro-5-(pyridin-4-yl)benzoate), which is characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis, powder X-ray diffraction analysis, and single crystal X-ray diffraction. Compound 1 is of the triclinic system, space group P-1 with a = 9.7857(12) Å, b = 10.3417(13) Å, c = 10.8463(13) Å, α = 85.155(2)°, β = 74.785(2)°, γ = 88.962(2)°, V = 1055.4(2) ų. The crystal structural analysis of complex 1 shows that the cobalt center is six-coordinated in an octahedral geometry by four O atoms from four different L ligands and two N atoms from two different L ligands; the Co(II) cations are bridged by μ₃-L into an interesting two-dimensional network structure. It should be pointed out that the thermal analysis results indicate that complex 1 is quite stable up to 420°C.     

Pseudodimorphism of the Trans-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic Acid Clathrates with Acetic and Propionic Acids

The versatile host compound trans-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic acid (1) forms under ambient conditions isostructural complexes with acetic and propionic acids being true clathrates without host-guest type H-bonds. A new modification of the clathrate between 1 and acetic acid (1a) is obtained at sub-room temperature (5 °C) while for preparation of the new crystal form of the clathrate with propionic acid (1b) crystallization temperature should be increased up to 50 °C. Crystal structures of the pseudodimorphs show that homo carboxylic acid dimers existing in the conventional phases are also observed here, demonstrating the new compounds to be of same clathrate type. Crystal data: for 1a: triclinic P-1, a = 8.626(2) Å, b = 9.073(2) Å, c = 12.042(2) Å, α = 76.34(3)°, β = 77.41(3)°, γ = 84.13(3)°, V = 892.5(4) ų, Z = 2, R = 0.0446 for 3171 reflections; for 1b: monoclinic C2/c, a = 13.268(3) Å, b = 12.636(3) Å, c = 21.786(4) Å, β = 90.56(3)°, V = 3652.3(14) ų, Z = 8, R = 0.0618 for 2365 reflections.     

Crystal structure of two complexes containing tris-(β-diketonato)magnate anion

Single crystal XRD is used to determine the structures of the complexes (H₂TMEDA)[Mg(ptac)₃]₂ (1, TMEDA = Me₂N(CH₂)₂NMe₂, ptac = ^t BuCOCHCOCF₃) and (H₂TMEDA)[Mg(hfac)₃](hfac) (2, hfac = CF₃COCHCOCF₃) at a temperature of 150 K. The crystallographic data for complex 1: a = 10.2919(3) Å, b = 10.9492(4) Å, c = 15.4159(6) Å, α = 87.117(1)°, β = 89.686(1)°, γ = 79,864(1)°, space group $P\bar 1$ Z = 1, R = 0.0573; for complex 2: a = 12.9446(2) Å, b = 23.0035(4) Å, c = 13.1473(3) Å, β = 98.779(1)°, space group P2₁/n, Z = 4, R = 0.0605. The structures are ionic; the metal atom coordinates six oxygen atoms of three β-diketonate ligands. The distances Mg-O in complex 1 are in the range 2.036(2)–2.0920(19) Å; the same distances in complex 2 are in the range 2.051(2)–2.076(2) Å. The spatial packing is determined by the system of hydrogen bonds between the (H₂TMEDA)²⁺ cations and [Mg(ptac)₃]^? (1) or hfac^? (2) anions. A thermogravimetric study of complex 1 is carried out.     

Structure and properties of tripyridine nitrosocomplexes of ruthenium: mer-[Ru(NO)Py3Cl(OH)]Cl·1.5H2O and mer-[Ru(NO)Py3Cl(H2O)]Cl2·2H2O·0.5HCl

The reaction of K₂[Ru(NO)Cl₅] with pyridine in aqueous ethanol at pH ～ 7–8 affords a nitrosoruthenium hydroxocomplex mer-[Ru(NO)Py₃Cl(OH)]Cl·1.5H₂O (I) (yield ～55%). Treatment of hydroxocomplex I with hydrochloric acid at room temperature gives the aqua complex mer-[Ru(NO)Py₃Cl(H₂O)]Cl₂·2H₂O·0.5HCl (II). The structures of the compounds are determined by X-ray crystallography: I, space group P2₁/n, a = 9.2292(4) Å, b = 11.7781(4) Å, c = 17.4915(7) Å, β = 90.9560(10)°, R = 4.84%; II, space group P-1, a = 7.3528(9) Å, b = 11.5793(11) Å, c = 13.6961(16) Å, α = 84.558(3)°, β = 87.668(4)°, γ = 74.146(4)°, R = 6.22%. Compounds I and II are characterized by powder XRD, ¹H and ¹³C NMR, and IR spectroscopy. The thermal decomposition of compound II in the inert atmosphere is examined by thermal analysis.     

Crystal structures of 3-phenylpropenal thiosemicarbazone and its nickel and zinc chelates

3-Phenylpropenal thiosemicarbazone hydrate C₆H₅-HC=CH-CH=N-NH-C(S)-NH₂ · H₂O (HL · H₂O, I) and two chelates [Ni(L)₂] · nCH₃OH (II) and [Zn(L)₂] (III) are studied by X-ray diffraction. The crystals of I are orthorhombic: a = 6.227(1) Å, b = 7.763(2) Å, c = 25.585(5) Å, β = 90°, space group P2₁2₁2₁, Z = 4, R = 0.0426. A nonplanar molecule of I has an E conformation. The crystals of II are triclinic: a = 6.551(2) Å, b = 10.752(3) Å, c = 10.885(3) Å, α = 64.751(5)°, β = 82.753(5)°, γ = 89.857(5)°, space group, Z = 1, R = 0.0661. In a centrosymmetric molecule of II, the central atom coordinates two deprotonated ligands L through the immine nitrogen atom and thioamide sulfur atom at the vertices of a distorted square. The crystals of III are monoclinic: a = 25.342(2) Å, b = 9.150(2) Å, c = 21.340(3) Å, α = 90°, β = 111.84(2)°, γ = 90°, space group C2/c, Z = 8, R = 0.0556. In a molecule of complex III, two deprotonated bidentate ligands L are coordinated by the zinc ion through the immine nitrogen atoms and thioamide sulfur atoms to form a distorted tetrahedron at the central atom. In both II and III, ligand L after coordination by the metal ion changes the E conformation with respect to the N(1)-C(2) bond for the Z conformation. In crystals I-III, molecules are packed to form infinite layers parallel to the planes (001) and (010).     

Mixed-ligand complexes based on asymmetric gadolinium β-diketonates: Synthesis, crystal structure, and theoretical modeling

Mixed-ligand complexes of asymmetric gadolinium β-diketonates with 2,2′-bipyridyl (Bipy)—[Gd(Pa)₃(Bipy)] (HPa is pivaloylacetone) (I) and [Gd(Pta)₃(Bipy)] (HPta is pivaloyltrifluoroacetone) (II)-have been obtained by direct interaction of initial reagents and their structures have been studied by X-ray crystallography. Crystals of I are monoclinic: a = 9.536(1) Å, b = 15.037(1) Å, c = 13.280(1) Å, β = 109.56(1)°, V = 1798.7(3) ų, Z = 2, space group P2₁. Crystals of II are triclinic: a = 9.6696(17) Å, b = 12.1348(9) Å, c = 18.243(3) Å, α = 100.257(12)°, β = 103.997(2)°, γ = 101.438(11)°, V = 1977.4(5), Z = 2, space group P $\bar 1$ . The coordination polyhedron of the central gadolinium atom in I and II is a distorted square antiprism formed by six oxygen atoms of the three β-diketonate ligands (av. Gd-O, 2.35(2) and 2.351(5) Å in I and II, respectively) and two nitrogen atoms of the Bipy ligand (av. Gd-N, 2.47(2) and 2.584(7) Å in I and II, respectively). Although the molecular structures of these complexes are similar, they have different crystal packings. In II, the planes of the Bipy ligands of neighboring molecules related by an inversion center are bound by stacking interaction (the distance between the Bipy planes is 3.45 Å). The structure and properties of these mixed-ligand complexes have been discussed based on the results of quantum-chemical density functional theory calculations (DFT/B3PW91). The nature of the substituents in the β-diketonate ligand has an effect on the structure and properties of the complexes. The correlation between the Gd-Dik and Gd (Dik)₃-Bipy bond energies has been studied.     

Synthesis and crystal structures of dimeric schiff base oxovanadium(V) complexes with antimicrobial activity

Two new dimeric oxovanadium(V) complexes, [VO₂L₁]₂ · 2H₂O (I) and [VO₂L₂]₂ (II), where L¹ and L² are the monoanionic form of 5-methoxy-2-[(2-methylaminoethylimino)methyl]phenol (HL¹) and 5-diethylamino-2-[(2-methylaminoethylimino)methyl]phenol (HL²), respectively, have been synthesized and characterized by elemental analysis, FT-IR spectra, and single crystal X-ray determination. The crystal of I is monoclinic: space group P2₁, a = 6.858(2), b = 16.630(3), c = 12.306(2) Å, β = 103.985(2)°, V = 1361.9(5) ų, Z = 2. The crystal of II is triclinic: space group $P\bar 1$ , a = 7.378(2), b = 8.838(2), c = 13.312(3) Å, α = 102.576(2)°, β = 92.044(2)°, γ = 113.017(2)°, V = 772.7(3) ų, Z = 2. The V...V distances are 3.140(1) Å in I and 3.254(1) Å in II. The V atoms in the complexes are in octahedral coordination. The effect of the complexes on the antimicrobial activity against Staphylococcus aureus, Escherichia coli, and Candida albicans was studied.     

A study of the structure and properties of mixed-ligand Cu(II) complexes with hexafluoroacetylacetone and methyl-, phenyl-ketoimines

The synthesis and X-ray single crystal study of two mixed-ligand Cu(II) complexes are performed: (CH₃C(NCH₃)CHC(O)CH₃)(CF₃C(O)CHC(O)CF₃)Cu (1) (space group P2₁/c, a = 7.0848(12) Å, b = 17.854(3) Å, c = 11.837(2) Å, β = 100.495(6)°, V = 1472.4(4) ų, Z = 4), (CH₃C(NC₆H₅)CHC(O)CH₃)· (CF₃C(O)CHC(O)CF₃)Cu (2) (space group P-1, a = 9.1119(4) Å, b = 9.6954(4) Å, c = 11.1447(6) Å, α = 113.784(2)°, β = 92.383(2)°, γ = 95.402(2)°, V = 893.52(7) ų, Z = 2). The structures are molecular, formed from neutral mixed-ligand copper complexes. The central copper atom has the (3O+N) coordination environment with average Cu-O distances of 1.948 Å and Cu-N of 1.932 Å; the chelate O-Cu-N angle (average) is 94.0°. In the structures, the complexes are linked into dimeric associates with Cu…Cu distances of 3.197 Å (for 1) and 3.246 Å (for 2). The volatility of mixed-ligand complexes 1 and 2 is in between of that of the starting homo-ligand complexes.     

Synthesis and crystal structure of lanthanum(III) Iodomercurate(II) complexes with ɛ-Caprolactam

The X-ray diffraction study of the crystalline products of the reaction between potassium tetraiodomercurate(II), ?-caprolactam, and lanthanum(III) nitrate at a ratio of 3: 16: 2 in an aqueous solution has shown the presence of the following three new crystalline compounds: [LaCpl₈]₂[HgI₄]₃ (I), [LaCpl₈][HgI₄]I₃ (II), and [LaCpl₇(H₂O)]₂[HgI₄]₂[Hg₂I₆] (III), where Cpl is ?-caprolactam ?-C₆H₁₁NO. Compounds I and II crystallize in tetragonal crystal system, space groups P4₂/n and $I\bar 4$ , respectively. For compound I, a = 18.59320(10) Å, c = 19.5782(3) Å, V = 6738.32(12) ų, Z = 2, and ρ_calc = 2.067 g/cm³. For compound II, a = 13.2245(10) Å, c = 20.0310(3) Å, V = 3503.17(6) ų, Z = 2, ρ_calc = 2.022 g/cm³. The crystals of compound III are monoclinic (space group P _{2 1}/n, a = 20.1202(6) Å, b = 14.0569(4) Å, c = 46.3228(12) Å, β = 93.4770(10)°, V = 13077.3(6) ų, Z = 4, ρ_calc = 2.274 g/cm³). [La(Cpl)₈]₂[Hg₂I₆]₃ (IV), a new double ionic complex salt, has also been synthesized and studied by X-ray diffraction. The crystals of compound IV are triclinic (space group $P\bar 1$ , a = 12.5021(3) Å, b = 14.6436(3) Å, c = 21.4695(4) Å, α = 84.2300(10)°, β = 87.2230(10)°, γ = 74.9970(10)°, V = 3776.30(14) ų, Z = 1, ρ_calc = 2.452 g/cm³). All complexes have a dicrete ionic structure, and the nearest surrounding of a La atom is distorted square-prismatic or trigonal-dodecahedral. The crystal packing of cations is distorted face-centered cubic (I and II) or body-centered cubic (III and IV) with anions located in its cavities.     

Synthesis and crystal structure of platinum(II) acetamidates [Pt(2,2′-bipy)(NHCOCH3)2] and [enPt(μ-NHCOCH3)(μ-OH)Pten](NO3)2

The diamines PtbipyCl₂, and PtenCl₂ and their aqua and hydroxy derivatives react with acetonitrile to give the Pt(II) acetamidates [Pt(2,2′-bipy)(NHCOCH₃)₂] · 4.125 H₂O (I) and [enPt(μ-NHCOCH₃(μ-OH)Pten](NO₃)₂ · H₂O (II), which are characterized by X-ray diffraction. The crystals of I are triclinic, a = 7.137(10) Å, b = 12.655(3) Å, c = 21.914(6) Å, α = 81.82(2)°, β = 82.12(2)°, γ = 77.72(2)°, V = 1908.6(7) ų, space group P $\overline 1 $ , Z = 4, R = 0.033 for 3700 reflections. Complex I is a mononuclear acetamidate with terminal (NHCOCH₃)^? ligands. The crystals of II are monoclinic, a = 11.413(2) Å, b = 10.981(2) Å, c = 14.385(3) Å, β = 105.90(3)°, V = 1733.8(6) ų, space group P2₁/n, R = 0.028 for 2797 reflections. Complex II is a dimer with bridging (NHCOCH₃)^? and (OH)^? groups. The Pt-Pt distance is 3.1667(7) Å.     

Syntheses, crystal structure, and fluorescent properties of a lanthanide complex

A new complex [Dy₂(Pht)₂(HPht)₂(Phen)₂(H₂O)₄] (I), where Pht^2? = dianion of o-phthalic acid; HPht^? = mono-anion of o-phthalic acid; Phen = 1,10-phenanthroline, has been synthesized and the crystal structure was determined by X-ray crystallography. The I crystallizes in the triclinic system, space group $P\bar 1$ with lattice parameters a =10.1126(3) Å, b =10.7029(3) Å, c = 11.9360(3) Å, α = 90.2260(10)°, β = 99.5340(10)°, γ = 100.9810(10)°, V = 1249.87(6) ų, Z = 2, ρ_calcd = 1.881 mg m^?3. The photophysical property of I has been studied with excitation and emission spectra.     

Crystal and molecular structures of ZnPhen(C2H5OCS2)2 and Zn(2,2′-Bipy)(n-C4H9OCS2)2 mixed-ligand coordination compounds

ZnPhen(EtOCS₂)₂ (I) and Zn(2,2′-Bipy)(n-BuOCS₂)₂ (II) mixed-ligand complexes have been synthesized. The structures were solved from X-ray diffraction data (CAD-4 and X8-APEX diffractometers, MoK _α radiation, 1879 and 3637 F _hkl , R = 0.0374 and 0.0315). Crystals I are monoclinic with parameters a = 11.678(3) Å, b = 19.215(3) Å, c = 9.655(1) Å; β = 101.23(1)°; V = 2125.0(7) ų; Z = 4, space group P2₁/c; crystals II are triclinic with parameters a = 8.7875(3) Å, b = 11.833(1) Å, c = 13.3454(6) Å; α = 112.154(2)°, β = 108.503(1)°, γ = 92.787(2)°; V = 1196.2(1) ų; Z = 2, space group 1 $P\bar 1$ . The structures are composed of discrete mononuclear molecules. The polyhedra of the Zn atoms are distorted trigonal bipyramids N₂S₃ formed by coordination of the N atoms of Phen or 2,2′-Bipy molecules and sulfur atoms of the monodentate and cyclic bidentate xanthogenate ligand. In structures I and II, dimer assemblies are formed by π-π interactions of Phen or 2,2′-Bipy molecules.     

Oxidation of coordinated ethylenediamine in platinum(IV) complexes with bromine. Crystal structures of [Pt(en)Py2Br2]Br2 · H2O, [Pt(HN-C(O)-C(O)-NH)Py2Br2] · H2O, and [Pt(en)PyBr3]NO3

Heating of an aqueous solution of [Pt(en)Py₂Cl₂]Cl₂ · 2H₂O (I) with KBr excess leads to the formation of [Pt(en)Py₂Br₂]Br₂ · H₂O (II). The interaction of a solution of II with bromine water results in the precipitation of polybromide ([Pt(en)Py₂Br₂]Br₂ · Br₂), which within a few days in the reaction solution partly transforms into oximide platinum(IV) complex, [Pt(HN-C(O)-C(O)-NH)Py₂Br₂] · H₂O (III). Complex [Pt(en)PyBr₃]Br · H₂O (IV) with an impurity of II was prepared by reacting KBr excess and the product of [Pt(en)Py₂]Cl₂ oxidation with chlorine in 0.05 N HCl. The action of HNO₃ on the solution of IV produced a nitrate derivative ([Pt(en)PyBr₃]NO₃, V). Complex IV, unlike II, does not react with bromine. The IR spectra of all the obtained compounds were recorded. Complexes II, III, and V were studied by X-ray crystallography. The crystals of II are monoclinic, space group P2₁/c, a = 15.640(2) Å, b = 9.345(1) Å, c = 14.167(2) Å, β = 102.63(1)°, V = 2020.5(5) ų, Z = 4, R _hkl = 0.033. The crystals of III are triclinic, space group P $\bar 1$ , a = 7.108(1) Å, b = 10.946(1) Å, c = 11.020(2) Å, α = 83.63(1)°, β = 80.31(1)°, γ = 75.02(1)°, V = 814.4(2) ų, Z = 2, R _hkl = 0.033. In the near-planar five-membered chelate ring (torsion angle NCCN is 7°), the C-O distances (1.23(1) Å) correspond to double bonds; the C-C (1.53(1) Å) and C-N (1.31(1) Å), distances correspond to ordinary bonds. The crystals of V are monoclinic, space group P2₁/c, a = 8.306(2) Å, b = 8.995(2) Å, c = 20.231(4) Å, β = 97.48(2)°, V = 1498.6(6) ų, Z = 4, R _hkl = 0.037.     

Mononuclear zinc(II) complex with 2,3,5,6-tetra(2-pyridyl)pyrazine

Complex [Zn(Tppz)Cl₂] (I), where Tppz = 2,3,5,6-tetrakis(2-pyridyl)pyrazine, has been synthesized and characterized by elemental analyses, IR, ¹H NMR, cyclic voltammetry, and electronic spectral studies. Solid state structures of the complex have been determined by single-crystal X-ray crystallography. The structural determination shows that the mononuclear complex I is a 1D coordination polymer. Also an ORTEP drawing of complex I shows that the coordination geometry around the Zn(II) center is slightly distorted from regular square-based pyramidal. Crystal data for I: triclinic, spase group P $ \bar 1 $ , a = 10.171(2), b = 10.3550(13), c = 12.239 (2) Å, α = 64.839(9)°, β = 85.736(8)°, γ = 77.842(10)°, V = 1140.3(4) ų, Z = 2.     

Study of new molecular and crystal structures of 4,4,10,10-tetramethyl-1,3,7,9-tetraazospiro[5.5]undecane-2,8-dione and its salts: Monochloride,mononitrate, and tetraiodotellurate

This is the first work to synthesize 4,4,10,10-tetramethyl-1,3,7,9-tetraazospiro[5.5]undecane-2,8-dione monohydrate, monochloride, mononitrate, and teteraiodotellurate: C₁₁H₂₀N₄O₂·H₂O (I), C₁₁H₂₁N₄O ₂ ⁺ ·Cl^? (II), C₁₁H₂₁N₄O ₂ ⁺ ·NO ₃ ^? (III), and 2(C₁₁H₂₁N₄O ₂ ⁺ )·TeI ₄ ^2? ·C₃H₆O (IV) and determine their structures. Crystals of I are monoclinic: space group P2₁/c, at 298 K a = 5.7118(7) Å, b = 17.842(2) Å, and c = 13.5905(16) Å; β = 91.621(11)°; V = 1384.5(3) ų; d _x = 1.239 g/cm³, Z = 4. Crystals of II are tetragonal: space group P4₃, at 298 K a = 6.4134(3) Å and c = 34.292(2) Å; V = 1410.47(14) ų; d _x = 1.303 g/cm³; Z = 4. Crystals of III are triclinic: space group \(P\bar 1\) , at 298 K a = 8.7614(14) Å, b = 9.3904(18) Å, and c = 10.028(2) Å; α = 63.27(2)°, β = 78.591(16)°, and γ = 84.308(15)°; V = 722.3(2) ų; d _x = 1.40 g/cm³; Z = 2. Crystals of IV are triclinic: space group \(P\bar 1\) , at 100 K a = 10.4630(4) Å, b = 11.9372(6) Å, and c = 16.4118(5) Å; α = 72.058(3)°, β = 76.406(3)°, and γ = 87.029(3)°; V = 1895.04(12) ų; d _x = 2.06 g/cm³; Z = 2. The synthesis of s and p metals with spirocarbone in acetone medium is found to be impossible due to the protonation by the oxygen atom of the carbonyl group. The main crystalline product of the complexation reaction is a monosalt. Evidence is provided that the recrystallization and drying of the synthesized spirocarbone preparation yields monohydrate (I); its purity and monophasity is confirmed by a Rietveld refinement of the powder X-ray pattern. The lattice parameters at room temperature are: a = 5.6885(12) Å, b = 17.8496(12) Å, and c = 13.518(3) Å; β = 91.449(15)°; V = 1372.1(4) ų. The sample is monophasic.     

Novel crystal structures of potassium salts of chalcohydroxo cluster complexes [Re6Q8(OH)6]4− (Q = S or Se)

Potassium salts of chalcohydroxo rhenium cluster complexes [Re₆Q₈(OH)₆]^4? (Q = S or Se) with the composition K₄[Re₆S₈(OH)₆]·4H₂O (1) and K₄[Re₆Se₈(OH)₆]·5H₂O (2) are produced by evaporation of the corresponding strongly alkaline aqueous solutions. The composition of the compounds is determined by the single crystal X-ray diffraction study. The compounds crystallize in the triclinic space group P $\bar 1$ with the following unit cell parameters: a = 8.408(2) Å, b = 9.096(2) Å, c = 9.222(2) Å, α = 95.110(4)°, β = 107.085(4)°, γ = 113.026(4)°, V = 603.5(3) ų, Z = 1, d _x = 4.689 g/cm³ (for 1) and a = 8.782(3) Å, b = 9.155(4) Å, c = 9.325(4) Å, α = 105.481(7)°, β = 109.266(6)°, γ = 99.104(6)°, V = 656.6(4) ų, Z = 1, d _x = 5.305 g/cm³ (for 2).     

Ionic mobility and <Superscript>19</Superscript>F MAS NMR spectra of lithium octafluorozirconate Li<Subscript>4</Subscript>ZrF<Subscript>8</Subscript>

A new 1D cadmium coordination polymer [Cd(PhCOO)₂(bbbm)] _n (1) (bbbm = 1,1′-(1,4-butanediyl)bis-1H-benzimidazole ) is synthesized under hydrothermal conditions and characterized by elemental analysis, IR, TG, and X-ray single-crystal diffraction. Compound 1 crystallizes in the triclinic system, space group P-1 with a = 10.4289(17) Å, b = 12.5198(9) Å, c = 12.6130(9) Å, α = 118.4260(10)°, β = 95.1990(10)°, γ = 94.3820(10)°, V = 1428.8(3) ų, Z = 2. In the structure of 1, each cadmium center is six-coordinated in a strongly distorted octahedron by two N and four O atoms; an infinite one-dimensional linear chain was built by the flexible bbbm ligand that adopts a bis-monodentate bridging mode linking Cd^II atoms.