The Crystal Structures of Rubidium and 4-Amino-1,2,4-Triazolium Tetrafluoroantimonates(III)

The crystal structures of complex antimony(III) fluorides RbSbF₄ (I) and (C₂N₄H₅)SbF₄ (II) were determined. The crystals of I and II are monoclinic; for I: a = 4.628(1) Å, b = 6.167(1) Å, c = 7.922(1) Å, = 100.582(3)°, V = 222.24(7) ų, Z = 2, (calcd.) = 4.23 g/cm³, (exp.) = 4.25 g/cm³, F(000) = 248, space group P2₁/m, R = 0.0395; for II: a = 4.678(1) Å, b = 7.339(4) Å, c = 10.185(1) Å, = 90.88(2)°, V = 349.6(2) ų, Z = 2, (calcd.) = 2.69 g/cm³, (exp.) = 2.70 g/cm³, F(000) = 264, space group P2₁. The structure of I is formed by Rb⁺ cations and [SbF₄] ^n– _n anionic chains composed of SbF₅E octahedra with two bridging fluorine atoms. The structure of IIis formed by (C₂N₄H₅)⁺ cations and isolated [SbF₄]^– anions in which the antimony polyhedra are SbF₄E trigonal bipyramids. The relationship between the crystal structures and electrophysical and biological properties of single-charged cation tetrafluoroantimonates(III) was studied.     

Copper(I) π-Complexes with Alkyne Ligands: Synthesis and Crystal Structure of M[CuCl2(HOCH2C≡CCH2OH)] (M = K+, NH+ 4)

Crystals of anionic complexes of the composition M[CuCl₂(HOCH₂CCCH₂OH)], where M = NH₄ ⁺ (I), K⁺ (II), were isolated from concentrated aqueous solutions of CuCl and MCl (M = NH₄ ⁺, K⁺) in the presence of 2-butyne-1,4-diol. Their structures were studied by X-ray diffraction analysis. Isostructural crystals I and II are orthorhombic; Z = 8, space group Ibam; a = 6.735(1) and 6.666(2) Å, b = 17.206(3) and 16.874(6) Å, c = 15.172(3) and 15.032(4) Å, V = 1758(1) and 1691(1) ų, respectively. The compounds are built of individual [CuCl₂(HOCH₂CCCH₂OH)] anions; the NH₄ ⁺ (I) or K⁺ (II) cations are arranged in the voids between the anions. The -coordinated Cu(I) atoms have trigonal-planar environment of two chlorine atoms and CC bond of the 2-butyne-1,4-diol molecule. The Cu–(CC) distances in the -core are 1.892(4) and 1.887(6) Å, CC are 1.233(5) and 1.228(5) Å in I and II, respectively. In complex I, additional hydrogen bonds Cl···H–NH₃ (Cl···H 2.43(4) Å) and O···H–NH₃ (O···H 1.97(3) Å) stabilize the structure.     

Nickel(II) Diisobutyldithiophosphinate Complexes with Hexamethylenetetramine and Triethylenediamine: Synthesis and Properties. Crystal and Molecular Structure of [Ni2(C6H12N4){(i-C4H9)2PS2}4]

The paramagnetic compounds [Ni₂(HMTA)(i-Bu₂PS₂)₄] (I) and [Ni₂(TEDA)(i-Bu₂PS₂)₄] (II) (_eff = 3.11 and 3.23 _B, respectively) were synthesized by reacting diamagnetic Ni(i-Bu₂PS₂)₂ with hexamethylenetetramine (HMTA) and triethylenediamine (TEDA) in ethanol. The crystal structure of I was established by single-crystal X-ray diffraction analysis (CAD4 diffractometer, MoK radiation, 1483 F _hkl, R = 0.0648). The crystals are monoclinic: a = 35.212(7) Å, b = 9.313(2) Å, c = 22.622(5) Å; = 129.97(3)°, V = 5685(2) ų, Z = 4, (calcd) = 1.281 g/cm³, space group C2/c. The structure is built of discrete binuclear molecules. The coordination polyhedron of the Ni atom is a distorted tetragonal pyramid with four S atoms of two bidentate cyclic ligands i-Bu₂PS₂ ^– in the base and the N atom of the bidentate bridging ligand HMTA at the axial vertex. Complexes I and II have similar electronic reflection spectra, which agrees with the C _4v symmetry of the ligand field.     

Monomeric [Ni(2,2"-Bipy){(i-C4H9)2PS2}2] and [Ni(Pz)2{(i-C4H9)2PS2}2] and Polymeric [Ni(Pz){(i-C4H9)2PS2}2]nComplexes (Pz = Pyrazine): Synthesis,Structures, and Properties

Diamagnetic [Ni(i-Bu₂PS₂)₂] compound (I) in ethanol reacts with 2,2"-bipyridine or pyrazine to give the paramagnetic complexes [Ni(2,2"-Bipy)(i-Bu₂PS₂)₂] (II), [Ni(Pz)₂(i-Bu₂PS₂)₂] (III), and [Ni(Pz)(i-Bu₂PS₂)₂] _n (IV) (_eff= 2.91–3.12 _B). Single crystals of IIwere grown for X-ray diffraction study. The crystals are monoclinic, a= 14.669(3) Å, b= 19.693(4) Å, c= 12.155(2) Å, = 107.51(3)°, V= 3348(1) ų, Z= 4; _calcd= 1.257 g/cm³, space group P2₁/c. The structure is built from monomeric molecules. The coordination polyhedron of the Ni atom is a distorted octahedron formed by four S atoms of two bidentate chelating i-Bu₂PS^– ₂ligands and by two N atoms of bidentate cyclic 2,2"-Bipy. Preliminary data for complexes IIIand IVindicate that they also contain an octahedral NiN₂S₄fragment. The structures of complexes I(square planar) and ofII–IV(octahedral) were confirmed by data from electron spectroscopy. Electronic absorption spectra were used to determine the rankings of the i-Bu₂PS^– ₂ions and Pz on a spectrochemical scale.     

Palladium Clusters Pd4(SEt)4(OAc)4and Pd6(SEt)12: Structure and Properties

Palladium clusters Pd₄(SEt)₄(OAc)₄(I) and Pd₆(SEt)₁₂(II) were synthesized and studied. Their structure was determined by X-ray diffraction analysis. For I, a= 9.774(2) Å, b= 10.821(2) Å, c= 13.061(3) Å, = 92.88(3)°, V= 1379.6(5) ų, (calcd.) = 2.182 g/cm³, space group P2₁/n, Z= 4, N _ref= 1558, and R= 0.031; for II, a= 10.581(1) Å, b= 10.584(2) Å, c= 11.478(2) Å, = 101.62(1)°, = 104.95(1)°, = 106.74(1)°, V= 1135.2(4) ų, (calcd) = 2.007 g/cm³, space group P1, Z= 1, N _ref= 2828, and R= 0.022. In cluster I, four Pd atoms form a planar cycle. The neighboring palladium atoms are bound by two acetate or by two mercaptide bridges, the Pd···Pd distances being 3.036–3.195 Å. In cluster II, Pd atoms form a planar six-membered cycle with Pd···Pd distances of 3.083–3.127 Å. The neighboring palladium atoms are bound by two mercaptide bridges. The formation of analogous clusters in solution was confirmed by IR spectroscopy.     

Uncommon Behavior of Copper(I) Tetrafluoroborate and Perchlorate in [Cu(DAF)(H2O)]BF4and [Cu(DAF)(ClO4)] π-Complexes (DAF—Diallyl Formamide)

Crystals of [Cu(DAF)(H₂O)]BF₄(I) and [Cu(DAF)(ClO₄)] (II) (DAF is diallyl formamide) were synthesized by an alternate-current electrochemical method, and their structures were determined (MoK radiation, 1247 and 859 independent reflections with I 2(I), R= 0.043 and 0.032 for Iand II, respectively). The complexes crystallize in space group P2₁/n, Z= 4. For I, a= 10.782(3) Å, b= 12.096(5) Å, c= 9.185(3) Å, = 103.62(3)°, and V= 1164.2(7) ų; for II, a= 10.064(3) Å, b= 10.753(6) Å, c= 10.002(3) Å, = 87.52(4)°, and V= 1081.4(8) ų. The copper atom in structures Iand IIcoordinates both C=C bonds in one DAF molecule and oxygen atom of the amide group of another DAF molecule, as well as an oxygen atom of H₂O (in I) or ClO₄(in II) in the axial position. The uncommon behavior of the anions in structures Iand IIis explained by their different values of Pierson hardness.     

Bis[(1,2-bis(2-(o-hydroxyphenoxy)ethyloxy)ethane)-(isothiocyanato)potassium] [K2(NCS)2(C18H22O6)2]: Crystal and Molecular Structure

Complex of podand 1,2-bis(2-(o-hydroxyphenoxy)ethyloxy)ethane (L) with potassium thiocyanate, [K₂(NCS)₂L₂] (I) was synthesized and studied using X-ray diffraction analysis: space group P , a = 7.771 Å, b = 11.711 Å, c = 11.965 Å, = 72.22°, = 79.21°, = 89.07°, Z = 1. Structure I was solved by direct method and anisotropically refined by the full-matrix least-squares method to R = 0.040 for all 4370 independent reflections (CAD4 autodiffractometer, MoK ). Structure I contains [K(NCS)L] monomers of the host–guest type united into centrosymmetrical [K₂(NCS)₂L₂] dimers via two bridging OH groups (one group from two L podands). In the monomer, the L podand appears as though to envelope the octacoordinated K⁺ cation, whose the coordination polyhedron is a strongly distorted hexagonal bipyramid with all six oxygen atoms of the L podand in its base and the N atom of the SCN^– ligand and the O atom of one of OH group of the neighboring (in dimer) L podand at its axial vertices. Molecules of I in crystal are joined through the O–H···N hydrogen bonds to form broad infinite chains along the x-axis.     

Syntheses,crystal structures,and characterizations of two novel cubane-like and double cubane-like molybdenum-copper-sulphur clusters {MoCu3S3(S2COEt)}(O)(Ph3P)3 and {Mo2Cu6S6(SCMe3)2}(O)2(Ph3P)4

Two novel heterometallic cubane-like and double cubane-like clusters, {MoCu₃S₃(S₂COEt)}(O)(Ph₃P)₃ I and {Mo₂Cu₆S₆(SCMe₃)₂}(O)₂(Ph₃P)₄ II, were synthesized by reaction of {MoCu₂S₃}(O)(Ph₃P)₃ with CuS₂COEt and CuSCMe₃, respectively. ClusterI crystallized in the triclinic space group (2) witha=12.766(6) Å,b=22.904(5) Å,c=10.522(3) Å, =99.86(2)°, =109.68(2)°, =86.84(3)°,V=2854(2) ų,Z=2,R=0.049 for 6622 observed reflections (I>5(I)) and 410 variables. ClusterII crystallized in the triclinic space group (2) with dimensionsa=14.212(4) Å,b=14.725(5) Å,c=12.396(8) Å, =110.32(4)°, =90.40(5)°, =62.88(2)°,V=2129(2) ų,Z=1,R=0.039 for 6020 observed reflections (I>3(I)) and 461 variables. ClusterI consists of a neutral cubane-like molecule with the core {MoCu₃S₃(S₂COEt)}²⁺, in which one corner of the cubane-like core is a novel triply bridging bidentate 1,1-dithiolato (xanthate, S₂COEt^–) ligand. ClusterII is a double cubane-like one, in which two cubane-like cores {MoCu₃S₃(SCMe₃)}²⁺ are connected by two Cu-S bonds of the triply bridging monothiolato (SCMe ₃ ^– ) ligand. Two different pathways of unit construction from a small heterometallic cluster {MoCu₂S₃}(O)(Ph₃P)₃ have been outlined. Comparisons of the selected bond lengths and bond angles for the cubane-like core {MoCu₃S₃ X} (X=Cl^–, Br^–, S₂COEt^–, SCMe ₃ ^– ) are given. Spectroscopic properties of the title clusters are also reported.     

Synthesis and Crystal Structure of Acid Phosphites RbH2PO3, CsH2PO3, and TlH2PO3

The reaction of Rb, Cs, or Tl carbonates with a solution of phosphorous acid gave crystalline acid phosphites RbH₂PO₃(I), CsH₂PO₃(II), and TlH₂PO₃(III). The crystal structures of the compounds were studied by a single-crystal X-ray diffraction analysis at 150 K: I, monoclinic system, a= 7.530(2) Å, b= 8.634(2) Å, c= 12.426(2) Å, = 102.46(3)°, V= 788.8(3) ų, Z= 8, space group P2₁/c, R ₁= 0.0409; II, monoclinic system, a= 7.930(2) Å, b= 8.929(2) Å, c= 13.163(3) Å, = 104.84(3)°, V= 900.9(4) ų, Z= 8, space group P2₁/c, R ₁= 0.0239; III, orthorhombic system, a= 6.603(1) Å, b= 6.785(1) Å, c= 8.836(2) Å, V= 395.9(1) ų, Z= 4, space group Pna2₁, R ₁= 0.0350. The PHO₃tretrahedra in structures I–IIIare joined via hydrogen bonds into infinite zigzag-like chains [HPHO₃] ^n– _n, which form layers alternating with layers of metal cations. The layers of anionic chains are wavelike in Iand IIand planar in III. Apparently, IIIis not isostructural to Ior IIdue to the fact that Tl(I) has a stereochemically active pair of electrons.     

Crystal Structure of Thallium Tridecafluorotetraantimonate(III) TlSb4F13

The crystal structure of thallium fluoroantimonate(III) complex TlSb₄F₁₃ (I), which is isostructural to KSb₄F₁₃ (II), is determined. Crystals I are tetragonal: a = 9.634(2) Å, c = 6.590(2) Å, V = 611.7(2) ų, Z = 2, (calcd) = 5.094 g/cm³, F(000) = 804.0, space group I4¯. The structure consists of tetrameric [Sb₄F₁₃]^– anions formed by SbF₃ groups connected by the fluoride ion and the l⁺ cations.     

Neptunium(V) Carbamide Complexes. The structure of [NpO2(HCOO){OC(NH2)2}3]

A new complex of Np(V) [NpO₂(HCOO){OC(NH₂)₂}₃] (I) was synthesized and its crystal structure was determined: a = 6.674(1) Å, b = 13.164(2) Å, c = 7.020(1) Å, = 101.35(1)°, space group P2₁, Z = 2, V = 604.7(2) ų, R = 0.048, wR(F ²) = 0.128. The structure consists of infinite chains of [NpO₂(HCOO){OC(NH₂)₂}₃]. The coordination polyhedron of the Np atom is a pentagonal bipyramid with the O atoms of three carbamide molecules and two formate ions in the equatorial plane. The absorption spectra were measured in IR and near-IR regions for compound I and for the [NpO₂Cl{OC(NH₂)₂}₄] complex, whose structure was reported in the previous publication.     

Tetrakis(Isothiocyanato)zinc(II) 4,7,13,16,21,24-Hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane: Synthesis and Crystal Structure

The salt tetrakis(isothiocyanato)zinc(II) 4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane, [H₂(Crypt-222)]²⁺ · [Zn(NCS)₄]^2– (I), was synthesized and its structure was determined using X-ray diffraction analysis: space group P2₁/n, a = 13.734 Å, b = 11.627 Å, c = 20.816 Å, = 91.51°, Z = 4. The structure was solved by direct methods and anisotropically refined by the full-matrix least-squares method to R =0.093 for 4920 independent reflections (CAD4 autodiffractometer, CuK radiation). The structural units of crystal I are 2.2.2-cryptand dications (with two protonated nitrogen atoms) and complex anions [Zn(NCS)₄]^2–. The coordination polyhedron of the Zn²⁺ cation is a distorted tetrahedron. The 2.2.2-cryptand dication contains trifurcate N–H(...O)₃ hydrogen bonds.     

Twinned and Disordered Crystal Structure of Solvated Bis[Aqua(2.2.2-Cryptand)Calcium] Hexa(Isothiocyanato)Calcium

Twinned and disordered crystals of solvated bis[aqua(2.2.2-cryptand)calcium] hexa(isothiocyanato)calcium 2[Ca(2.2.2-Crypt)(H₂O)]²⁺ · [Ca(NCS)₆]^4– · Sol (I), where Sol is acetone and/or ethanol and may be water, were synthesized and studied by X-ray diffraction analysis. Structure I (space group P2₁/n, a = 11.841 Å, b = 21.787 Å, c = 12.377 Å, = 90.90°) was solved by the direct method and refined by the full-matrix least squares method in anisotropic approximation to R = 0.079 from 4168 independent reflections (CAD4 automated diffractometer, MoK ). In crystal form, complex I exists as the two aforesaid complex ions [I¹]²⁺ and [I²]^4– in the molar ratio 2 : 1 united through hydrogen bonds. Complex cation I¹ is of the guest–host type. Its Ca²⁺ cation is coordinated by all eight heteroatoms (6O + 2N) of the cryptand ligand and by the O atom of the water molecule; the coordination polyhedron of this Ca²⁺ cation (CN 9) is irregular. The Ca²⁺ cation of complex anion I² (in the crystallographic center of inversion) is coordinated by six N atoms of six neighboring SCN^– anionic ligands; the coordination polyhedron of this Ca²⁺ cation (CN 6) is a slightly distorted octahedron.     

Cu(II) Complexes with Optically Active α-Alkylamino Oximes of Caryophyllene Type: Synthesis,Structure, and Properties

Paramagnetic complexes Cu(HL¹)Cl₂ (I), Cu(HL²)Cl₂ · 2H₂O (II), and Cu(HL¹)Br₂ (III) are synthesized by the reaction of copper(II) halides with the optically active -alkylamino oximes HL¹ and HL² of caryophyllene type. Crystal and molecular structures of complex I are determined. The crystals are orthorhombic: a = 9.038(2) Å, b = 11.990(2) Å, c = 11.990(2) Å, V = 2004.8(7) ų, space group P2₁2₁2₁, Z = 4, (calcd) = 1.812 g/cm³, R ₁ = 0.0632. In a mononuclear complex I, the coordination polyhedron of CuCl₂N₂ is a distorted square. The structures of complexes II and III are suggested on the basis of EPR, IR and Raman spectroscopy data.     

Crystal Structures of Ammonium and Cesium Pentadecafluorotetraantimonates(III)

Antimony(III) fluoride complexes with compositions (NH₄)₃Sb₄F₁₅(I) and Cs₃Sb₄F₁₅(II) are structurally characterized. Crystals Iare triclinic: a= 8.317(3) Å, b= 10.419(6) Å, c= 10.826(3) Å, = 63.71(4)°, = 73.24(3)°, = 77.42(5)°, Z= 2, _calcd= 3.42 g/cm³, _exp= 3.45 g/cm³, space group P , R= 0.051; crystals IIare monoclinic: a= 8.079(2) Å, b= 29.116(8) Å, c= 8.162(2) Å, = 117.08(2)°, Z= 4, _calcd= 4.549 g/cm³, _exp= 4.50 g/cm³, space group P2₁/c, R= 0.036. Structure Iis composed of SbF₄E and SbF₅E polyhedra combined into tetranuclear chains; crystals IIconsist of SbF₄E polyhedra, two of which form a dimer Sb₂F₇E₂, while the other two are isolated (E is the antimony lone electron pair).     

Ni(II) Complexes with Diisobutyldithiophosphinate Ions and o-Phenanthroline Molecules. Structure of [Ni(Phen)2(i-Bu2PS2)](i-Bu2PS2)

Paramagnetic compounds [Ni(Phen)(i-Bu₂PS₂)₂] (I), [Ni(Phen)₂(i-Bu₂PS₂)](i-Bu₂PS₂) (II), and [Ni(Phen)₃](i-Bu₂PS₂)₂ (III) (_eff = 3.03–3.14 _B) were synthesized by reacting Ni(i-Bu₂PS₂)₂ chelate with Phen. Their single crystals were grown. X-ray diffraction analysis of II was performed (CAD4 diffractometer, K radiation, 1181 F _hkl, R = 0.0378). The crystals are monoclinic: a = 14.039(2) Å, b = 18.030(2) Å, c = 18.118(2) Å = 105.52(1)°, V = 4418.9(9) ų, Z = 4, (calcd) = 1.259 g/cm³, space group P2₁/c. The structure is built of individual [Ni(Phen)₂(i-Bu₂PS₂)]⁺ cations and i-Bu₂PS₂ ^- anions. The coordination polyhedron of NiN₄S₂ is a distorted octahedron with four N atoms of two bidentate chelate ligands (Phen molecules) and with two S atoms of a bidentate cyclic ligand i-Bu₂PS₂ ^-. The electronic spectroscopy data for molecular complex I and ionic complex III suggest the octahedral structure of the NiN₂S₄ and NiN₆ chromophores, respectively.     

Hydrothermal Syntheses and Structural Characterization of One-Dimensional [Cu4Br2I3(C12H8N2)2] n and Molecular Cu3Br3(C12H8N2)2

The hydrothermal reactions of CuBr₂, CuX (X=Br, I), and phen (phen=1,10-phenanthroline, C₁₂H₈N₂) have lead to the syntheses of two novel complexes of one-dimensional [Cu₄Br₂I₃(phen)₂] _n 1 and trinuclear discrete cluster Cu₃Br₃(phen)₂ 2. Both compounds were characterized by singe-crystal X-ray diffraction. Crystal data for 1. Monoclinic, space group P2 ₁/c with a=14.054(3) Å, b=13.700(3) Å, c=15.920(3) Å, =114.16(3)°, Z=2; 2. Monoclinic, space group C2/c with a=10.040(2) Å, b=14.516(3) Å, c=16.319(3) Å, =94.29(3)°, Z=6.     

The crystal structures ofbis-{(2-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)-methyl]-aminato} Copper(II) andbis-{(3-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)-methyl]-aminato} Copper(II)

Summary TheSchiff base ligands 3-[(2-benzotrifluoride)-2-hydroxy-3H-naphth-3-ylidene)-methyl] aldamine (1) and 3-[(3-benzotrifluoride)-2-hydroxy-3H-naphth-3-ylidene)-methyl] aldamine (2) and their corresponding Cu(II) complexes (I, II) were synthesized. The crystal structures ofbis-{(2-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)]-methyl]-aminato} Copper(II) (I) andbis-{(3-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)-methyl]-aminato} Copper(II) (II) were determined. CompoundI crystallizes in the triclinic crystal system (a=12.561(3),b=16.211(4),c=8.007(2) Å, =96.29(2), =101.42(2), =97.10(2)°, space group ,Z=2); compoundII crystallizes in the monoclinic crystal system (a=5.064(2),b=19.172(4),c=15.111(3) Å, =95.05(2)°, space group P2₁/c,Z=2). The X-ray diffraction study shows that the geometry around the metal atom is square planar for both copper complexes.

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Kristallstruktur vonbis-{(2-Benzotrifluorid)-[(2-oxo-3H-naphth-3-yliden)-methyl]-aminato}-Kupfer(II) undbis-{(3-Benzotrifluorid)-[(2-oxo-3H-naphth-3-yliden)-methyl]-aminato}-Kupfer(II)

Zusammenfassung DieSchiffschen Basen 3-[(2-Benzotrifluorid)-2-hydroxy-3H-naphth-3-yliden)-methyl]-aldamin (1) und 3-[(3-Benzotrifluorid)-2-hydroxy-3H-naphth-3-yliden)-methyl]-aldamin (2) sowie ihre entsprechenden Cu(II)-Komplexe (I,II) wurden synthetisiert und ihre Struktur im Kristall bestimmt. VerbindungI kristallisiert triklin (a=15.561(3),b=16.211(4),c=8.007(2) Å, =96.29(2), =101.42(2), =97.10(2)°, Raumgruppe ,Z=2); VerbindungII kristallisiert monoklin (a=5.064(2),b=19.172(4),c=15.111(3) Å, =95.05(2)°, Raumgruppe P2₁/c,Z=2). Aus der Röntgenstrukturanalyse ergibt sich eine quadratisch planare Geometrie der Komplexe.

     

Copper(I) Complexes with N-Allylquinolinium Bromide [C9H7N(C3H5)]CuBr2 and [C9H7N(C3H5)]Cu2Br3: Synthesis and Crystal Structure

Crystals of [₉₇N(₃₅)]uBr₂ (IV) and [₉₇N(₃₅)][u₂Br₃] (V) were prepared by ac electrochemical synthesis from uBr₂, N-allylquinolinium bromide, on copper electrodes in the ethanol–benzene medium. X-ray diffraction study has shown that crystals IV and V are monoclinic: space group A2₁/a, a = 13.776(3) Å, b = 14.304(3) Å, c = 13.147(2) Å, = 107.90(1) Å, V = 2465(2) ų, Z = 8 for IV and space group P2₁/n, a = 13.881(2) Å, b = 15.446(2) Å, c = 7.111(1) Å, = 104.64(1)°, V = 1475.0(8) ų, Z = 4 for V. Structures IV and V are built of the N-allylquinolinium cations and different anions i.e., (CuBr₂) ^n- _n forming infinite chains in IV and peculiar {[Cu^I ₄Br₆]^2–} _n arranged in polymeric chains in V. In the latter case, two independent metal atoms have trigonal–pyramidal and trigonal–planar environments. In the structures of both compounds, the C=C bond of the allyl group is not involved in coordination with the Cu(I) atom.     

Dimethyl- and Diethyltin(IV) Compounds with Perfluorobiphenyl-4-Thiolate and Perfluoronaphthalene-2-Thiolate Anions: The Crystal Structure of (CH3)2Sn(C12F9S)2

Compounds (CH₃)₂Sn(C₁₂F₉S)₂ (I), (CH₃)₂Sn(C₁₀F₇S)₂ (II), and (C₂H₅)₂Sn(C₁₀F₇S)₂ (III) were synthesized. Single crystals of Iwere grown and structurally characterized using X-ray diffraction analysis (1590 reflections, R = 0.0209). The crystals are orthorhombic, a = 40.848(8) Å, b = 6.058(1) Å, c = 11.183(2) Å, V = 2767(1) ų, (calcd.) = 2.024 g/cm³, space group Pbcn, Z = 4. The structure is built from monomeric molecules. The coordination polyhedron of the Sn atom (the SnC₂S₂ core) is a distorted tetrahedron. Compounds I–III are volatile when heated in vacuo. Thermolysis of these compounds results in SnO₂ (in air) or SnS₂ (in argon).