Crystal structure and luminescence and thermochromic properties of bis-1,10-phenanthrolinium hexachlorotellurate(IV)

The structure of bisphenanthrolinium hexachlorotellurate(IV) (C₁₂H₉N₂)₂TeCl₆ is determined by X-ray diffraction analysis: a = 7.6619(8), b = 8.0034(8), c = 10.959(1) Å, α = 82.680(2)°, β = 81.379(2)°, γ = 85.569(2)°; space group P \(\bar 1\), Z = 1, and ρ_calcd = 1.774 g/cm³. The crystal structure is built of the [TeCl₆]^2? anions and phenanthrolinium cations. The electronic and geometric aspects determining the spectral luminescence and thermochromic properties are discussed.     

Crystal structure,luminescence, and thermochromic properties of bis(tetraethylammonium) hexabromotellurate(IV)

The atomic structure of ((C₂H₅)₄N)₂TeBr₆ crystals (a = 17.930(8) Å, b = 11.133(5) Å, c = 15.022(7) Å, β = 109.28(9)°, space group C2/c, Z = 4, ρ_calcd = 2.036 g/cm³) has been studied by X-ray diffraction. The ((C₂H₅)₄N)₂TeBr₆ crystal structure consists of isolated [TeBr₆]^2? anions and ((C₂H₅)₄N)⁺ cations. The electronic and geometric aspects that influence the luminescence and thermochromic properties of the complex have been considered.     

Crystallochemical study of ruthenium(III) tris-dipivaloylmethanate

The structure of ruthenium(III) dipivaloylmethanate is determined by single crystal X-ray diffraction at temperature of 150 K. The crystallographic data for C₃₃H₅₇O₆Ru are as follows: a = 9.6119(11) Å, b = 17.4603(19) Å, c = 21.519(2) Å, β = 95.187(2)°, C2/c space group, V = 3596.7(7) ų, Z = 4, d_calc = = 1.202 g/cm³, R = 0.0642. The structure is molecular, the metal atom coordinates six oxygen atoms of three ligands of β-diketone. The Ru–O distances are in the range of 1.99 Å to2.03 Å. The complexes have a distorted single layer hexagonal packing with the Ru…Ru distances being 9.84 Å within the layer, and 10.93 Å between the layers.     

X-ray study of rhodium(III) sulfates

Compounds with compositions [Rh(H₂O)₆]₂(SO₄)₃·4H₂O (I), (H₃O)[Rh(H₂O)₆](SO₄)₂ (II), [Rh(H₂O)₅OH](SO₄)·0.5H₂O (III), and [Rh(H₂O)₆]₂(SO₄)·(H₂SO₄) _x ·5H₂O (IV) have been studied. The crystal structures of II, III, and IV were determined. All compounds crystallized in the monoclinic crystal system. Crystal data for II: a = 7.279(2) Å, b = 10.512(7) Å, c = 15.806(3) Å, β = 96.71(3)°, space group P2₁/n, Z = 2, d _calc = 2.334 g/cm³; III: a = 20.433(4) Å, b = 7.820(2) c = 11.215(2) Å, β = 114.14(1)°, space group C2/c, Z = 8, d _calc = 2.559 g/cm³; IV: a = 6.2250(4 Å), b = 27.0270(12) Å, c = 7.2674(5) Å, β = 97.04(3)°, space group P2₁/c, Z = 4, d _calc = 2.143 g/cm³. The compounds were studied by IR spectroscopy and powder X-ray diffraction. All of the isolated crystalline phases are sparingly soluble in ethanol and well soluble in water.     

Hexa(isothiocyanato)chromates(III) of Some Yttrium Group Lanthanide(III) and Europium Complexes with Nicotinic Acid: Synthesis and Crystal Structures

Double ionic complexes [M(C₅H₅NCOO)₃(H₂O)₂][Cr(NCS)₆] · nH₂O, where M = Eu (I), n = 1.15; Dy (II), Er (III), n = 1.5; M = Yb (IV), n = 2, have been synthesized by the reaction between M(NO₃)₃, M = Eu, Dy, Er, Yb, K₃[Cr(NCS)₆], and nicotinic acid (C₅H₅NCOO) in an aqueous solution and studied by chemical analysis, IR spectroscopy, and X-ray diffraction. Crystals of complexes I–IV are monoclinic, space group P2₁/n, Z = 4; a = 9.5358(2) Å, b = 25.4871(5) Å, c = 15.4303(4) Å, β = 105.513(1)°, V = 3613.6(1) ų, ρ_calcd = 1.799 g/cm³ for I, a = 9.5901(5) Å, b = 25.8599(15) Å, c = 15.6316(9) Å, β = 106.829(2)°, V = 3710.6(4) ų, ρ_calcd = 1.782 g/cm³ for II, a = 9.5640(3) Å, b = 25.8936(11) Å, c = 15.6498(7) Å, β = 106.895(2)°, V = 3708.3(3) ų, ρ_calcd = 1.791 g/cm³ for III, and a = 9.5049(2) Å, b = 25.6378(4) Å, c = 15.5120(3) Å, β = 106.934(1)°, V = 3616.1(1) ų, ρ_calcd = 1.864 g/cm³ for IV.     

Sc(III), Eu(III), and Gd(III) Complexes with Macrocyclic Cavitand Cucurbit[6]uril: Synthesis and Crystal Structures

Slow evaporation of solutions of Sc and Eu nitrates with macrocyclic cavitand cucurbit[6]uril gives crystals of isostructural complexes [Sc(NO₃)(H₂O)₄(C₃₆H₃₆N₂₄O₁₂)](NO₃)₂ ? 8.5H₂O (space group Pna2₁, a = 32.0065(18) Å, b = 14.7904(8) Å, c = 11.5774(6) Å, V = 5480.6(5) ų, Z = 4) and [Eu(NO₃)(H₂O)₄(C₃₆H₃₆N₂₄O₁₂)](NO₃)₂ ? 6.75H₂O (space group Pna2₁, a = 31.9525(17) Å, b = 14.7203(8) Å, c = 11.8592(6) Å, V = 5578.0(5) ų, Z = 4). The metal to ligand ratio in these complexes is 1 : 1; the complexes are obtained at 0.025–0.1 mol/l concentrations of the metals in solutions. With higher lanthanide concentrations (0.7–1 mol/l), the 2 : 1 complex with cucurbit[6]uril is formed of the composition [{ Gd(NO₃)(H₂O)₅}₂(C₃₆H₃₆N₂₄O₁₂)](NO₃)₄ ? 6.5H₂O (space group \(P\bar 1\), a = 13.3972(6) Å, b = 14.4994(5) Å, c = 18.3290(8) Å, α = 73.5610(10)°, β = 87.2590(10)°, γ = 87.5540(10)°, V = 3409.4(2) ų, Z = 2) and isotypical complex [{Gd(NO₃)(H₂O)₅}₂{(C₅H₅N) ? (C₃₆H₃₆N₂₄O₁₂)}](NO₃)₄ ? 8H₂O with a pyridine molecule inside the cucurbit[6]uril cavity (space group P2₁/n, a = 14.8263(6) Å, b = 13.3688(7) Å, c = 18.5970(9) Å, β = 107.5860(10)°, V = 3513.8(3) ų, Z = 2). According to X-ray diffraction data, the metal atoms of the title complexes coordinate the O atoms in portals of cucurbit[6]uril molecules.     

Synthesis and structure investigation of Co(III) complex salts with the perrhenate anion

Complex salts of the composition [Co(NH₃)₆](ReO₄)₃·2H₂O (I), [Co(en)₃](ReO₄)₃ (II), [Co(NH₃)₅H₂O](ReO₄)₃·2H₂O (III), and [Co(NH₃)₅Cl](ReO₄)₂·0.5H₂O (IV) are obtained. Their crystal structures are determined by single crystal XRD. Crystallographic characteristics: (I) a = 9.9797(3) Å, b = 12.6994(3) Å, c = 14.7415(4) Å, β = 102.870(1)°, C2/c space group; (II) a = 8.0615(3) Å, b = 8.4483(4) Å c = 8.8267(4) Å, α = 61.923(2)°, β = 89.552(2)°, γ = 72.295(2)°, P1 space group; (III) a = 8.0086(4) Å, b = 12.9839(6) Å, c = 17.5122(7) Å, β=91.858(1)°, P2₁/n space group; (IV) a = 14.9446(3) Å, b = 14.6562(4) Å, c = 12.2434(4) Å, Cmc2₁ space group.     

Crystal structure and fluorescence of a 2D cadmium(II) coordination polymer based on flexible bis(2-methylbenzimidazole) and benzenedicarboxylate co-ligands

A new coordination polymer, {[Cd(bbmb)(bdc)]} _n (bbmb = 1,1′-(1,4-butanediyl)bis-(2-methylbenzimidazole), H₂bdc = 1,3-benzenedicarboxylic acid) was synthesized under hydrothermal conditions. The complex was structurally characterized by single crystal X-ray diffraction analyses, infrared spectroscopy (IR), elemental analyses. The compound crystallizes in the monoclinic system, space group P2₁/c with a = 10.860(6) Å, b = 13.115(7) Å, c = 21.009(9) Å, β = 120.94(2)°, V = 2567(2) ų, Z = 4, C₂₈H₂₆CdN₄O₄, M _r = 594.93, D _c = 1.540 g/cm³, μ = 0.893 mm^–1. Each cadmium center is six coordinated with four O atoms from two bdc^2– anions, and two N atoms of two bbmb ligands. The complex features a 4-connected 2D (4, 4) sheet with a point symbol {4².6^2}. Fluorescence properties of the title complex were investigated.     

Crystal structure of <Emphasis Type="Italic">tris</Emphasis>-(dipivaloylmethanato) (ethylendiamine)yttrium(III)

The structure of a mixed-ligand complex tris-(dipivaloylmethanato)(ethylendiamine)yttrium(III) [Y(en)(dpm)₃] is studied at 150(2) K by single crystal XRD. The crystallographic data for C₃₅H₆₅N₂O₆Y are as follows: space group P2₁/c, a = 10.3771(3) Å, b = 26.3566(8) Å, c = 14.8412(4) Å, β = 100.385(2)°, V = 3992.6(2) ų, Z = 4. The structure is molecular. The coordination environment of yttrium atoms is square antiprismatic; the Y–О distances are 2.2597(13)-2.3760(12) Å and Y–N distances are 2.5381(16) Å and 2.5499(17) Å.     

Crystal structures of copper(II) and zinc(II) complexes derived from 3-(2-pyridyl)pyrazole

Two dinuclear complexes [Zn(μ-L)(NO₃)(H₂O)]₂ (1) and [Cu₂(μ-L)₂(HL)₂](NO₃)₂(C₁₂H₈Br₂)_0.5·H₂O (2), (HL = 3-(2-pyridyl)pyrazole, C₁₂H₈Br₂ = 4,4′-dibromobiphenyl) are synthesized under hydrothermal conditions and characterized by elemental analysis and X-ray single crystal diffraction. Crystal data for 1: triclinic, \(P\bar 1\), a = 8.8478(7) Å, b = 15.0550(11) Å, c = 16.4310(12) Å, α = 107.588(4)°, β = 112.498(3)°, γ = 115.595(3)°, V = 2099.8(9) ų, Z = 2; for 2: triclinic, \(P\bar 1\), a = 7.2870(15) Å, b = 8.6840(17) Å, c = 9.3290(19) Å, α = 107.588(4)°, β = 112.498(3)°, γ = 115.595(3)°, V = 528.77(18) ų, Z = 1. Complex 1 and 2 are both dinuclear structures which are further packed into a 1D supramolecular chain and a 3D supramolecular framework via weak C–H…O hydrogen bond interactions respectively.     

Crystal structures of rhodium(III) aqua ion with tetrahedral anions

The crystal structures of compounds of the composition [Rh(H₂O)₆]₂(SO₄)₃·5H₂O (I) and [Rh(H₂O)₆]PO₄ (II) are determined. Crystallographic data for I: a = 7.272(9) Å, b = 27.047(1) Å, c = 12.464(9) Å, β = 97.038(10)°, P2₁ space group, Z = 4, d _x = 2.184 g/cm³; for II: a = 9.746(6)Å, b = 6.877(7) Å, c = 23.623(6) Å, β = 100.601(10)°, C2/c space group, Z = 8, d _x = 2.611 g/cm³. Compounds are analyzed by IR spectroscopy and powder XRD. Crystalline phase I is well soluble in water, whereas II is almost insoluble.     

Crystal structure of a complex of nickel(II) with 2-amino-4-imino-2-pentene

The structure of a nickel(II) complex with 2-amino-4-iminopentane is determined by X-ray crystallography at 150 K. Crystal data for C₁₀H₁₈N₄Ni are: a = 10.9802(3)Å, b = 13.5780(4)Å, c = 8.0935(2)Å, β = 107.304(1)°, space group P2₁/c, V = 1152.04(5) ų, Z = 4, d _x = 1.459 g/cm³, R = 0.0283. The structure is molecular; the metal atom is coordinated by four nitrogen atoms of two β-diimine ligands. The Ni-N distances in Ni(NacNac)₂ fall within 1.8571–1.8623 Å. The molecules in the crystal are joined by only van der Waals interactions.     

Crystal structures of tetrafluoroantimonates(III) of single and double protonated 3-amino-1,2,4-triazolium cations

Crystal structures are determined by X-ray crystallography for tetrafluoroantimonates(III) of single and double protonated 3-amino-1,2,4-triazolium cations of the composition (C₂H₅N₄)SbF₄ (I) (monoclinic: a = 4.7723(6) Å, b = 19.643(2) Å, c = 7.6974(9) Å, β = 97.239(2)°, Z = 4, Cc space group) and (C₂H₆N₄)(SbF₄)₂ (II) (monoclinic: a = 4.7617(3) Å, b = 15.512(1) Å c = 7.4365(5)Å β = 107.706(1)°, Z = 2, P2₁/n space group). The structure of I is built from complex [SbF₄]^? anions and single charged (C₂H₅N₄)⁺ cations; the structure of II is built from the same anion and double charged 3-amino-1,2,4-triazolium cation: (C₂H₆N₄)²⁺. In the structure, weak interactions Sb…F join the anions in polymeric layers [SbF₄] _n ^n? that are assembled in a 3D framework by N-H…F hydrogen bonds. The formation of the double protonated 3-amino-1,2,4-triazolium cation (C₂H₆N₄)²⁺, found in the crystal structure of II, is observed for the first time.     

Synthesis and structural investigation of hafnium(IV) complexes with acetylacetone and trifluoroacetylacetone

Two volatile hafnium(IV) complexes with acetylacetone and trifluoroacetylacetone (HL) have been prepared and their structures have been studied at ?30°C. Crystal data for C₂₀H₂₈HfO₈: a = 21.5493(4) Å, b = 8.36720(10) Å, c = 13.9905(3) Å; β = 116.5550(10)°, space group C2/c, Z = 4, d _calc = 1.692 g/cm³, R = 0.015. Crystal data for C₂₀H₁₆F₁₂HfO₈: a = 8.1039(12) Å, b = 11.4499(14) Å, c = 15.790(2) Å; α = 99.341(4)°, β = 103.175(4)°, γ = 108.185(4)°, space group P?1, Z = 2, d _calc = 2.003 g/cm³, R = 0.074. Both structures are molecular and comprise isolated complex molecules HfL₄. The hafnium atom is coordinated with eight oxygen atoms of four β-diketonate ligands, Hf-O distances varying from 2.153 Å to 2.191 Å. The molecules make van der Waals contacts in the structures.     

Crystal structure of dimethylgold(III) 8-hydroxyquinolinate and 8-mercaptoquinolinate

A crystal-chemical study of dimethylgold(III) complexes with 8-hydroxyquinoline (CH₃)₂Au(OR) and 8-mercaptoquinoline (CH₃)₂Au(SR) (R = C₉H₆N) was performed. Crystal data for (CH₃)₂Au(OR): a = 8.7133(17) Å, b = 27.875(6) Å, c = 8.6688(17) Å, β = 102.76(3)°, Z = 8, ρ(calc) = 2.401 g/cm³, space group P2₁/c, R = 0.0909; for (CH₃)₂Au(SR): a = 3.5401(7) Å, b = 15.689(3) Å, c = 19.910(4) Å, β = 99.81(3)°, Z = 4, ρ(calc) = 2.361 g/cm³, space group P2₁/c, R = 0.0712. Both structures are molecular and involve neutral (CH₃)₂Au(L) molecules, L = C₉H₆NO or C₉H₆NS. In the structures, the molecules are arranged in stacks joined by van der Waals interactions. The average Au…Au intrastack distances are 3.57 Å and 4.34 Å for (CH₃)₂Au(OR) and 3.5 Å for (CH₃)₂Au(SR).     

Crystal and molecular structure of (hexafluoroacetylacetonato) (pivaloylacetonato)copper(II)

The crystal structure of (hexafluoroacetylacetonato)(pivaloylacetonato)copper(II) has been determined. Crystal data for CuO₄C₁₃H₁₄F₆: a = 8.288(2) Å, b = 8.682(2) Å, c = 12.307(2) Å; α = 90.75(3)°, β = 94.29(3)°, γ = 106.60(3)°; V = 845.7(3) ų, space group \(P\overline 1 \), Z = 2, d_calc = 1.617 g/cm³. The coordination polyhedron of the copper atom is formed by four oxygen atoms of two different β-diketonate ligands with Cu-O distances within 1.874–1.946 Å; the O-Cu-O bond angles are 94.8° and 90.6°. The complexes are united into centrosymmetrical “dimers” with Cu...Cu distances of 4.365 Å.     

Synthesis and crystal structure of a new Schiff base ligand and its cobalt(II) complex

The crystal structures of cobalt(II) Schiff base complex (Co^IIL₂ · H₂O) and Schiff base ligand 3,5-dichlorosalicylidene-2-chlorophenylmethylamine (HL) have been determined by single-crystal X-ray analysis. The geometry around cobalt in Co^IIL₂ · H₂O is distorted tetrahedral. Co^IIL₂ · H₂O crystallizes in the monoclinic system, in space group C2/c, with crystallographic parameters: a = 12.9143(16) Å, b = 8.8326(16) Å, c = 25.115(3) Å, β = 92.791(10)°, V = 2861.4(7) ų, Z = 4, F(000) = 1420, and the final R indices (I > 2σ(I)) are R ₁ = 0.0440, wR ₂ = 0.1272. HL crystallizes in the monoclinic system, in space group P2₁/c, with crystallographic parameters: a = 11.9764(15), b = 8.2331(10), c = 14.2211(17) Å, β = 98.723(6)°, V = 1386.0(3) ų, Z = 4, F(000) = 640, and the final R indices (I > 2σ(I)) are R ₁ = 0.0397, wR ₂ = 0.1018.     

Crystal structures of a family of layered coordination polymers containing divalent metal ions (Mn<Superscript>2+</Superscript>, Co<Superscript>2+</Superscript>, Ni<Superscript>2+</Superscript> and Zn<Superscript>2+</Superscript>) and the 3-amino 4-methyl benzoate ion

The syntheses and crystal structures of the layered coordination polymers M(C₈H₈NO₂)₂ [M = Mn (1), Co (2), Ni (3) and Zn (4)] are described. These isostructural compounds contain centrosymmetric trans-MN₂O₄ octahedra as parts of infinite sheets; the ligand bonds to three adjacent metal ions in μ³-N,O,O′ mode from both its carboxylate O atoms and its amine N atom. In each case, weak intra-sheet N–H?O and C–H?O hydrogen bonds may help to consolidate the structure. Crystal data: 1, C₁₆H₁₆MnN₂O₄, M _r = 355.25, monoclinic, P2₁/c (No. 14), a = 10.6534(2) Å, b = 4.3990(1) Å, c = 15.5733(5) Å, β = 95.1827(10)°, V = 726.85(3) ų, Z = 2, R(F) = 0.026, wR(F ²) = 0.067. 2, C₁₆H₁₆CoN₂O₄, M _r = 359.24, monoclinic, P2₁/c (No. 14), a = 10.6131(10) Å, b = 4.3374(4) Å, c = 15.3556(17) Å, β = 95.473(4)°, V = 703.65(12) ų, Z = 2, R(F) = 0.041, wR(F ²) = 0.091. 3, C₁₆H₁₆N₂NiO₄, M _r = 359.02, monoclinic, P2₁/c (No. 14), a = 10.6374(4) Å, b = 4.2964(2) Å, c = 15.2827(8) Å, β = 95.9744(14)°, V = 694.66(6) ų, Z = 2, R(F) = 0.028, wR(F ²) = 0.070. 4, C₁₆H₁₆N₂O₄Zn, M _r = 365.68, monoclinic, P2₁/c (No. 14), a = 10.6385(5) Å, b = 4.2967(3) Å, c = 15.2844(8) Å, β = 95.941(3)°, V = 694.89(7) ų, Z = 2, R(F) = 0.038, wR(F ²) = 0.107.     

Synthesis and crystal structures of cobalt(III) and zinc(II) complexes with Schiff bases

Two new cobalt(III) and zinc(II) complexes, [Co(L¹)₂ (H₂O)] · ClO₄ (I) and [Ni(L²)₂ (H₂O)₂] · 2ClO₄ (II), where L¹ is the deprotonated form of 5-methoxy-2-[(2-morpholin-4-ylethylimino)methyl]phenol, and L² is the zwitterionic form of 2-[(2-isopropylaminoethylimino)methyl]-5-methoxyphenol, were synthesized and structurally characterized by elemental analyses, IR spectra, and single-crystal X-ray diffraction. The crystal of I is monoclinic: space group P2₁/c, a = 11.1512(4), b = 28.2424(11), c = 10.9655(4) Å, β = 95.746(2)°, V = 3436.1(2) ų, Z = 4. The crystal of II is triclinic: space group P2₁/c, a = 8.1441(2), b = 10.4531(3), c = 10.8849(3) Å, α = 84.0240(10)°, β = 76.9800(10)°, γ = 74.2280(10)°, V = 867.92(4) ų, Z = 1. Complex I consists of a mononuclear cobalt(III) complex cation and a perchlorate anion. Complex II consists of a crystallographic centrosymmetric mononuclear nickel(II) complex cation and two perchlorate anions. Each metal atom in the complexes is in an octahedral coordination.     

Crystal structure and luminescence of europium(III) acrylate

The atomic structure of europium acrylate crystals [Eu₂(Acr)₅OH·3H₂O]·2(0.5H₂O) was studied by X-ray analysis (a = 24.360(3) Å, b = 18.466(2) Å, c = 8.5818(9) Å, β = 96.087(2)°, space group C2/c, Z = 6, ρ_calc = 2.036 g/cm³). The crystal structure involves chains of binuclear [Eu₂(C₃H₃O₂)₅OH·3H₂O] molecules, running infinitely in the [101] direction and having pairs of C₉H₉EuO₇H₂O molecules alternating with C₆H₆EuO₄OH·2H₂O molecules that link the pairs. The infinite chains are linked by hydrogen bonds and van der Waals interactions. The thermal behavior of luminescence of the europium(III) complex is discussed.