Dialkyl- and alkylenedithiophosphates of gallium(III)

Gallium(III) tris-dialkyldithiophosphates, Ga[S₂P(OR)₂]₃ (R = C₂H₅, n-C₃H₇, i-C₃H₇, n-C₄H₉ and i-C₄H₉) and gallium(III) tris-alkylenedithiophosphates, Ga(S₂$\text{POGO}$)₃ [G = -CH₂C(C₂H₅)₂CH₂-, -C(CH₃)₂C(CH₃)₂ and -C(CH₃)₂CH₂CH(CH₃)] have been synthesized for the first time by the reactions of gallium(III) chloride with the alkali metal salt of the corresponding ligand in anhydrous benzene in 1:3 molar ratio respectively.These compounds are crystalline solids or viscous liquids and are soluble in common organic solvents, in which they show monomeric behaviour. Based on elemental analyses, molecular weight determinations, IR and NMR (¹H and ³¹P) spectral data, chelate octahedral structures have been proposed for these derivatives.     

Arsenic-boron derivatives. 5. A 1H and 11B nuclear magnetic resonance study of the methylated arsine adducts of boron trihalides

The ¹H NMR chemical shifts for the adduct series (CH₃)_nAsH_3−nBX₃ and the ¹¹B NMR chemical shifts for the adduct series (CH₃)_nAsH_3−nBX₃, (CH₃)_n- AsH_3−nBX₂Y and (CH₃)_nAsH_3−nBXYZ (where n= 1, 2, 3; X ≠ Y ≠ Z=Cl, Br or I) have been reported. The values of the chemical shifts are examined in view of their use as indicators of acid-base strength. The ¹¹B chemical shifts were found to fit Malinowsky's criteria of pairwise additivity.     

On the possible influence of different pathways of binding of amides with water on “Pyramidalization” of valence bonds of peptide group nitrogen

With the aim to study solvation effects in peptide structure organization, the behavior of the energy of different types of hydration in simple amines and amides has been analyzed. On the example of quantum-chemical DFT and PM3 calculations of amino derivatives of composition CH₃-(CH₂)₃)-NH₂, (CH3)₂-NH, CH₃-NH₂, NH₃, CH₂=CH-NH₂, H-CC-NH₂, O=C(CH)₃-N(CH₃)₂, O=C(CH₃)-NH(CH₃), O=C(CH₃)-NH₂, O=CH-N(CH₃)H, and O=CH-NH₂ it has been shown that: (1) in the given set of molecules, the proton acceptor N…H-O variant of hydrogen bonding of NH₂ group with a water molecule is dominating only for the simplest amines. Being primordially weaker, the proton donor N-H…OH variant of water H-bonding gradually increases in energy in the given set as the basicity of the compound decreases, and for the case of amides of carboxylic acids it becomes already a significant channel of the hydration; (2) the intermolecular N-H…O=C bonding of trans-N-methylacetamides, which models the peptide hydrogen bonds in proteins, induces “planarization” of its initially nonplanar O=C-NH fragments. However, the addition of water molecules to the complex through the proton acceptor N…H-O variant of binding of N atom not only restores but even strengthens the “pyramidalization” of valence bonds of peptide groups.     

The reactivity of bromoform with [Au(CH2)2PPh2]2. The completion of the halomethane series CHyX4−y (y=3,2,1,0; X=Cl,Br, I) and reactivity with [Au(CH2)2PPh2]2

The reaction of [Au(CH₂)₂PPh₂]₂ with excess CHBr₃ in benzene initially gives [Au(CH₂)₂PPh₂]₂₋ (CHBr₂)Br. This observation establishes that halomethanes, CH_yX_4−y (y=3,2,1,0; X=Cl, Br, I), react with [Au(CH₂)₂PPh₂]₂ to initially give Au(II) adducts of the general form [Au(CH₂)₂PPh₂]₂₋(CH_yX_3−y)X (y=3,2,1,0) via oxidative addition across the carbon-halogen bond. The order of reactivity inversely follows the order of carbon-halogen bond dissociation energies of haloalkanes. Methyl chloride is the only halomethane of the series that does not give a Au(II) adduct under similar reaction conditions.     

Organic derivatives of aluminium. Part I. Reactions of alkanolamines with aluminium isopropoxide

Reactions of alkanolamines [R₁R₂NXOH; R₁ = H, CH₃, C₂H₅; R₂ = H, CH₃, C₂H₅ and X = -CH₂CH₂-, -CH₂CH₂CH₂-, -CH₂CHCH₃, -C₆H₄CH₂CH₂-] with aluminium isopropoxide in different molar ratios (1 to 3) yield compounds of the type Al(OPrⁱ)_3?n(OXNR₁R₂)_n, where ‘n’ can be 1, 2 and 3. Most of the derivatives are distillable liquids, soluble in common organic solvents and susceptible to hydrolysis even by atmospheric moisture. The new derivatives are characterized by elemental analysis, IR and ¹H NMR spectra. Molecular weight measurements of Al(OPrⁱ)_3?n(OXNR₁R₂)_n reveal them to be tetrameric in nature.     

Syntheses and crystal structures of di- and trimethyltin (IV) derivatives with phenylphosphonic acid

Three types of methyltin phosphonates, {[(CH₃)₃Sn]₄(O₃PPh)₂}_n (1), {[(CH₃)₃Sn]₂(O₃PPh) · CH₃OH}_n (2) and {[(CH₃)₂SnO₃PPh]₄}_n (3) were synthesized by the reaction of phenylphonic acid with trimethyltin (IV) chloride and dimethyltin (IV) dichloride, respectively. Complexes 1, 2 and 3 were characterized by elemental analysis, IR, NMR (¹H, ¹³C, ³¹P and ¹¹⁹Sn) spectroscopy, TGA and X-ray crystallography diffraction analysis. The X-ray analysis of complex 1 shows that the structure is a polymeric infinite 1D zigzag chain. In complex 2, the oxygen atom of methanol molecule is coordinated to the tin atoms, and a 2D network is generated via O–H?O hydrogen bonds. In complex 3, a novel 2D network containing 12-membered (Sn₃O₆P₃) rings is formed.     

Some metal alloxides

Tetraalloxygermanium(IV), (CH₂·CH·CH₂·O)₄Ge, has been synthesized from germanium tetrachloride, allyl alcohol, and ammonia. The alloxides [(CH₂·CH· CH₂·O)₄Ti]₂and[(CH₂·CH·CH₂O)₅M]₂ (M = Nb and Ta) have been synthesized by reactions of the corresponding metal isopropoxides with allyl alcohol followed by removal of the isopropanol by azeotropic distillation with benzene. These four metal alloxides can be purified by distillation under reduced pressure. The spectroscopic properties of these new compounds are discussed.     

Coordination modes of polydentate ligands. 4. The crystal and molecular structure of an oxo-bridged iron(III) complex containing a pentadentate imino-alkoxy ligand

In the presence of Fe³⁺, template condensation of the fluorinated keto-alcohol CH₃C(O)CH₂C- (CF₃)₂OH with the triamine CH₃C(CH₂NH₂)₃ leads to two products: a fully condensed, imino-alkoxy, iron(III) complex, Fe{CH₃C[CH₂NC(CH₃)CH₂C(CF₃)₂O]₃}, and a partially condensed iron(III) complex, O{FeCH₃C[CH₂NC(CH₃)CH₂C(CF₃)₂O]₂(CH₂NH₂)}₂, in which two six-coordinate iron(III) centers are linked by an oxide ion. A complete crystal and molecular structure determination of the latter has been made.Crystals are monoclinic, space group C2/c, a= 13.886(4); b=23.206(5); c=15.241(4) Å; β= 106.55(2)°; V=4708 ų; Z=4. Least-squares refinement on F of 322 variables using 2627 observations converged at a conventional agreement factor of 3.8%. The Fe to bridging oxide distance is 1.811(1) Å, the FeFe distance 3.468 Å, and the FeOFe angle 146.6(2)°. A comparison is made between this structure and those of natural hemerythrin systems.     

Structural comparison of octahedral MoO22+ complexes of bidentate and linear tetradentate N,S-donor ligands

The structures of MoO₂[NH₂C(CH₃)₂CH₂S]₂ and MoO₂[SC(CH₃)₂CH₂NHCH₂CH₂NHCH₂C(CH₃)₂S] have been determined using X-ray diffraction intensity data collected by counter techniques. MoO₂[NH₂C(CH₃)₂CH₂S]₂ crystallizes in space group Pbca with a = 11.234(3), b = 11.822(3) and c = 20.179(5) Å, V = 2680(2) ų and Z = 8. Its structure is derived from octahedral coordination with cis oxo groups [MoO = 1.705(3) and 1.705(3)], trans thiolate donors cis to the oxo groups [MoS = 2.416(1) and 2.402(1) and N donors trans to oxo [MoN = 2.325(3) and 2.385(4) Å]. MoO₂[SC(CH₃)₂CH₂NHCH₂CH₂NHCH₂C(CH₃)₂S] crystallizes in the space group P2₁/c with a = 10.798(5), b = 6.911(2), c = 20.333(9) Å, β = 95.20°, V = 1511(2) Å₃ and Z = 4. Its structure is very similar to that of MoO₂[NH₂C(CH₃)₂CH₂S]₂ with MoO = 1.714(2) and 1.710(2), MoS = 2.415(1) and 2.404(1) and MoN = 2.316(3) and 2.362(3). The small differences in the geometries of the two compounds are attributed to the constraints of the extra chelate ring in the complex with the tetradentate ligand. The structures in this paper stand in contrast to those reported for complexes of similar ligands wherein steric hindrance produces complexes with a skew trapezoidal bipyramidal structure.     

Optically active aromatic amino acids. part V: Some N-t-butyloxycarbonyl-O-methyl-L-tyrosine analogues with ring substitution at position 3

Six new derivatives of Boc-L -Tyr(Me)-OH have been prepared, with the following substituents at ring position 3: −CO₂Me, −CO₂Et, −CHO, −CH₂OH, −CH₂OBzl and −(E)−CH=NOH. © 1997 European Peptide Society and John Wiley & Sons, Ltd. J. Pep. Sci.3: 354–360 No. of Figures: 2. No. of Tables: 1. No. of References: 16     

The structure of U3(O)(OCMe3)10, and unusual trinuclear U(IV) oxo-alkoxide

In an attempt to prepared tetrakis(tert-butoxy)uranium(IV) a trinuclear oxo-alkoxide of uranium(IV) was obtained instead. The compound has the formula U₃O[(CH₃)₃CO]₁₀ and it crystallizes in the hexagonal space group P6₃mc with a = b = 18.256(4) Å, c = 10.013(2) Å, Z = 2. The trinuclear unit is strikingly reminiscent of that in Mo₃O(OCH₂CMe₃)₁₀. In contrast to the molybdenum compound where there is metal-metal bonding, the U?U distance of 3.574(1) Å indicates a non-bonded interaction.     

Design and synthesis of cholecystokinin-4 dipeptide analogues with anxiolytic and anxiogenic activities

A new series of dipeptide analogues of the general formula Ph(CH₂) _n CO-NH(CH₂) _m CO-Trp-NH₂ (n = 1, 3–5; m = 1–3) was designed based on the structure of the endogenous tetrapeptide cholescystokinin-4 (CCK-4) and the topochemical Shemyakin-Ovchinnikov-Ivanov principle. The L-tryptophan derivatives exhibited anxiolytic properties and the D-tryptophan derivatives, anxiogenic properties. The dipeptide Ph(CH₂)₅CO-Gly-L-Trp-NH₂ (GB-115) with the activity in rats of 0.05–0.2 mg/kg after oral and intraperitoneal administration was chosen for further studies as a promising anxiolytic agent.     

Reactions of methylcobalamin with tin and lead compounds

Reactions of CH₃[Co] with (CH₃)_nM^(4?n)+ (n = 2, 3; M = Sn, Pb) at concentrations high enough to detect (CH₃)₄M in the head space (yields 7.08×10^?5?2.06×10^?5%), indicate that dismutation is the major route of production. Similarly, kinetic reactions at lower concentrations show that no demethylation of CH₃[Co] by (CH₃)₃M⁺ (M = Sn, Pb) occurs after 60 days. From the methylation of SnCl₂ by CH₃[Co] at pD 1.0 and under aerobic conditions, the following hydrolysis species were observed in the 400 MHz ¹H NMR spectrum: CH₃- Sn(OH)Cl₂·2H₂O (63.6%), [CH₃Sn(OH)(H₂O)₄]²⁺ (17.6%) and CH₃Sn(OH)₂Cl·nH₂O (18.8%). No methylation products were observed from similar reactions with Pb(II) salts.     

Complexes of the fac-{Re(CO)3} core with tridentate ligands derived from arylpiperazines

Arylpiperazines, XC₆H₄N(CH₂CH₂)₂NH, are readily alkylated to give the N-alkylpiperazines of the type XC₆H₄N(CH₂CH₂)₂N(CH₂)_nNH₂. The amine functions of these derivatives are in turn easily subjected to mono- or dialkylation to provide potentially tridentate ligands of the types XC₆H₄N(CH₂CH₂)₂N(CH₂)_nN(H)(CH₂Y) and XC₆H₄N(CH₂CH₂)₂N(CH₂)_nN(CH₂Y)(CH₂Z), respectively. The latter class of dialkylated derivatives may be symmetrically (Y=Z) or unsymmetrically (Y ≠ Z) substituted. The donor groups Y and Z of this study include pyridine, imidazole, methyl-imidazole, thiazole, carboxylate and thiolate.The reactions of these ligands with [NEt₄]₂[Re(CO)₃Br₃] yield complexes of the type [Re(CO)₃{(YCH₂)N(H)(CH₂)_n(H)_xN(CH₂CH₂)₂N(H)_yC₆H₄X}]ⁿ and [Re(CO)₃{(ZCH₂)(YCH₂)N(CH₂)_n(H)_xN(CH₂CH₂)₂N(H)_yC₆H₄X}]ⁿ where the molecular charge n (0, +1, or +2) depends on the nature of the donor groups Y and Z (whether neutral or anionic or a combination of neutral and anionic) and on the degree of protonation of the piperazine unit (x=0 or 1; y=0 or 1). This variety of tridentate chelators provides complexes with fac-{Re(CO)₃N₃}, {Re(CO)₃N₂O}, {Re(CO)₃NO₂}, {Re(CO)₃N₂S} and {Re(CO)₃NS₂} coordination geometries. The structures of the model compound [Re(CO)₃{(CH₃N₂C₃H₂CH₂)N(H)CH₂CH₂-piperidine}]Br · H₂O, [Re(CO)₃{(CH₃N₂C₃H₂CH₂)N(H)CH₂CH₂-Fphenpip}]Br, [Re(CO)₃{(NC₅H₄CH₂)N(H)CH₂CH₂-Fphenpip}]Br, [Re(CO)₃{(O₂CCH₂)₂NCH₂CH₂CH₂-CH₃OphenpipH}] · xCH₃OH (x≈0.875), [Re(CO)₃{(NC₅H₄CH₂)₂NCH₂CH₂CH₂-CH₃OphenpipH}]Br₂ · 2CH₂Cl₂ · H₂O and [Re(CO)₃{(CH₃N₂C₃H₂CH₂)(O₂CCH₂)NCH₂CH₂CH₂-CH₃OphenpipH₂}]BrCl · 1.5CH₃OH · H₂O are discussed (phenpip: phenylpiperazine, -C₆H₄N(CH₂CH₂)₂N-).     

Synthesis and coordination chemistry of tripodal dialkyl[1,2-bis(diethylcarbamoyl)ethyl]phosphonates with lanthanide nitrates

Trifunctional dialkyl [1,2-bis(diethylcarbamoyl)- ethyl] phosphonates, (RO)₂P(O)CH[C(O)N(C₂H₅)₂]- [CH₂C(O)N(C₂H₅)₂] R  CH₃, C₂H₅, i-C₃H₇, n-C₆H₁₃ were prepared from the respective sodium salts, Na[(RO)₂P(O)CHC(O)N(C₂H₅)₂] and N,N- diethylchloroacetamide, and they were characterized by elemental analysis, mass, infrared and NMR spectroscopy. The molecular structure of (i-C₃H₇O)₂- P(O)CH[C(O)N(C₂H₅)₂][CH₂C(O)N(C₂H₅)₂] was determined by single crystal X-ray diffraction analysis and found to crystallize in the monoclinic space group P2₁/c with a=15.589(6), b=9.783(4), c= 16.283(7) Å, β = 110.90(3)°, Z = 4 and V= 2320(2) ų. The structure was solved by direct methods and blocked least-squares refinement converged with Rf = 5.7% and R_wF= 4.4% on 2266 unique data with F>4σ(F). Important bond distances include PO 1.459(3) Å, CHCO 1.228(3) Å and CHCH₂CO 1.223(3) Å. The coordination chemistry of the ligand with several lanthanides was examined, and the structure of the complex Gd(NO₃)₃{[(i-C₃H₇O)₂P(O)CH[C(O)N(C₂H₅)₂][CH₂C(O)N(C₂H₅)₂]}₂·H₂O was determined. The complex crystallized in the monoclinic space group P2₁/n with a = 13.524(5), b = 22.033(4), c = 19.604(4) Å β = 106.22(2)°, Z = 4 and V= 5609(3) ų. The structure was solved by heavy atom techniques and blocked least-squares refinement converged with R_F = 5.9% and R_wF = 4.1% on 5275 reflections with F > 4σ(F). Both trifunctional ligands were found to bond to Gd(III) through only the phosphoryl oxygen atoms. The remainder of the Gd coordination sphere was composed of three bidentate nitrate oxygen atoms and an oxygen bonded water molecule. Several important bond distances include GdO(phosphoryl)_av = 2.343(5) Å, GdO(nitrate)_av = 2.475(7) Å, GdO(water) = 2.354(5) Å, PO(phosphoryl)_av = 1.467(6) Å, CHCO_av = 1.242(10) Å and CHCH₂CO_av = 1.209(11) Å.     

A theoretical study on the coordination behavior of some phosphoryl,carbonyl and sulfoxide derivatives in lanthanide complexation

The selectivity of phosphoryl P(O)R₃, sulfoxide S(O)R₂, and carbonyl C(O)R₂ (R?=?NH₂, CH₃, OH, and F) derivatives with lanthanide cations (La³⁺, Eu³⁺, Lu³⁺) was studied by density functional theory calculations. Theoretical approaches were also used to investigate energy and the nature of metal–ligand interaction in the model complexes. Atoms in molecules and natural bond orbital (NBO) analyses were accomplished to understand the electronic structure of ligands, L, and the related complexes, L–Ln³⁺. NBO analysis demonstrated that the negative charge on phosphoryl, carbonyl, and sulfoxide oxygen (O_P, O_C, and O_S) has maximum and minimum values when the connected –R groups are –NH₂ and –F. The metal–ligand distance declines as, –F?>?–OH?>?–CH₃?>?–NH₂. Charge density at the bond critical point and on the lanthanide cation in the L–Ln³⁺ complexes varies in the order –F?<?–OH?<?–CH₃?<?–NH₂, due to greater ligand to metal charge transfer, which is well explained by energy decomposition analysis. It was also illustrated that E⁽²⁾ values of Lp(N)?→?σ*(Y–N) vary in the order P=O ? S=O ? C=O and the related values of Lp(N)?→?σ*(Y=O) change as C=O ? S=O ? P=O in (NH₂)_nYO ligands (Y?=?P, C, and S). Trends in the L–Ln³⁺ CP–corrected bond energies are in good accordance with the optimized O_Y?Ln distances. It seems that, comparing the three types of ligands studied, NH₂–substituted are the better coordination ligands.

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Graphical Abstract Density functional theory (B3LYP) calculations were used to compare structural, electronic and energy aspects of lanthanide (La, Eu, Lu) complexes of phosphine derivatives with those of carbonyls and sulfoxides in which the R– groups connected to the P=O, C=O and S=O are –NH₂, –CH₃, –OH and –F.

     

New synthesis of seven-coordinate complexes of molybdenum(II) and tungsten(II) containing bidentate phosphorus ligands, [MI2(CO)3{Ph2P(CH2)nPPh2}] (n = 1–6)

A new high yielding synthesis of the seven-coordinate complexes [MI₂(CO)₃{Ph₂P(CH₂)_nPPh₂}] (M = Mo and W; n = 1–6) is described. The procedure involves reacting the complexes [MI₂(CO)₃(NCMe)₂] in CH₂Cl₂ with an equimolar amount of the bidentate phosphorus ligand. The low temperature (−70 °C) ¹³C NMR spectra of the complexes [Wl₂(CO)₃{Ph₂P(CH₂)_nPPh₂}] (n = 3 and 5) indicates that the geometry is capped octahedral with a carbonyl ligand in the unique capping position.     

Further studies on the dialkylation chemistry of [Pt2(μ-S)2(PPh3)4] with activated alkyl halides RC(O)CH2X (X = Cl, Br)

Further studies have been carried out into the reactivity of [Pt₂(μ-S)₂(PPh₃)₄] towards a range of activated alkylating agents of the type RC(O)CH₂X (R = organic moiety, e.g. phenyl, pyrenyl; X = Cl, Br). Alkylation of both sulfide centers is observed for PhC(O)CH₂Br, 3-(bromoacetyl)coumarin [CouC(O)CH₂Br], and 1-(bromoacetyl)pyrene [PyrC(O)CH₂Br], giving dications [Pt₂{μ-SCH₂C(O)R}₂(PPh₃)₄]²⁺, isolated as their PF₆⁻ salts. The X-ray structure of [Pt₂{μ-SCH₂C(O)Ph}₂(PPh₃)₄](PF₆)₂ shows the presence of short Pt?O contacts. In contrast, the corresponding chloro compounds [typified by PhC(O)CH₂Cl] and imino analogues [e.g. PhC(NOH)CH₂Br] do not dialkylate [Pt₂(μ-S)₂(PPh₃)₄]. The ability of PhC(O)CH₂Br to dialkylate [Pt₂(μ-S)₂(PPh₃)₄] allows the synthesis of new mixed-alkyl dithiolate derivatives of the type [Pt₂{μ-SCH₂C(O)Ph}(μ-SR)(PPh₃)₄]²⁺ (R = Et or n-Bu), through alkylation of in situ-generated monoalkylated compounds [Pt₂(μ-S)(μ-SR)(PPh₃)₄]⁺ (from [Pt₂(μ-S)₂(PPh₃)₄] and excess RBr). In these heterodialkylated systems ligand replacement of PPh₃ occurs by the bromide ions in the reaction mixture forming monocations [Pt₂{μ-SCH₂C(O)Ph}(μ-SR)(PPh₃)₃Br]⁺. This ligand substitution can be easily suppressed by addition of PPh₃ to the reaction mixture. The complex [Pt₂{μ-SCH₂C(O)Ph}(μ-SBu)(PPh₃)₄]²⁺ was crystallographically characterized. X-ray crystal structures of the bromide-containing complexes [Pt₂{μ-SCH₂C(O)Ph}(μ-SR)(PPh₃)₃Br]⁺ (R = Et, Bu) are also reported. In both structures the coordinated bromide is trans to the SCH₂C(O)Ph ligand, which adopts an axial position, while the ethyl and butyl substituents adopt equatorial positions, in contrast to the structures of the dialkylated complexes [Pt₂{μ-SCH₂C(O)Ph}₂(PPh₃)₄]²⁺ and [Pt₂{μ-SCH₂C(O)Ph}(μ-SBu)(PPh₃)₄]²⁺ (and many other known analogues) where both alkyl groups adopt axial positions.     

Synthesis and crystal and molecular structure of a methyl N,N-diethylcarbamylmethylenephosphonato dysprosium thiocyanate complex

Bis-Methyl N,N-diethylcarbamylmethylenephosphonato dysprosium thiocyanate, Dy[O₂P(OCH₃)CH₂C(O)N(C₂H₅)₂]₂(NCS) was prepared from the combination of ethanolic solutions of Dy(NCS)₃·xH₂O and (CH₃O)₂P(O)CH₂C(O)N(C₂H₅)₂. The complex was characterized by infrared and NMR spectroscopy, and single crystal X-ray diffraction methods. The crystal structure was determined at 25 °C from 3727 independent reflections by using a standard automated diffractometer. The complex was found to crystallize in the monoclinic space group P2₁/c with a = 13.282(4) Å, b = 19.168(5) Å, c = 9.648(2) Å, β = 90.09(2)°, Z = 4, V = 2456.4 ų and ?_cald = 1.72 g cm^?3. The structure was solved by standard heavy atom techniques, and blocked least-squares refinement converged with R_f = 4.7% and R_wF = 4.9%. The Dy atom is seven coordinate and bonded in a bidentate fashion to two anionic phosphonate ligands [O₂P(OCH₃)CH₂C(O)N(C₂H₅)₂^?] through the carbonyl oxygen atoms and one of two phosphonate oxygen atoms. In addition, each Dy atom is coordinated to two phosphonate oxygen atoms from two neighboring complexes and to the nitrogen atom of a thiocyanate ion. This coordination scheme gives rise to a two-dimensional polymeric structure. Some important bond distances include DyNCS 2.433(8) Å, DyO(carbonyl)_avg 2.39(2) Å, DyO(equat. phosphoryl)_avg 2.303(8) Å, DyO(axial phosphoryl)_avg 2.25(2), PO(phosphoryl)_avg 1.493(3) Å and CO(carbonyl)_avg 1.25(1) Å.