Two novel glycine metal halogenides: catena‐poly[[[diaqua­nickel(II)]‐di‐μ‐glycine] dibromide] and catena‐poly[[[tetra­aqua­magnesium(II)]‐μ‐glycine] dichloride]

In catena‐poly[[[diaqua­nickel(II)]‐di‐μ‐glycine] dibromide], {[Ni(C₂H₅NO₂)₂(H₂O)₂]Br₂}_n, (I), the Ni atom is located on an inversion centre. In catena‐poly[[[tetra­aqua­magnesium(II)]‐μ‐glycine] dichloride], {[Mg(C₂H₅NO₂)(H₂O)₄]Cl₂}_n, (II), the Mg atom and the non‐H atoms of the glycine mol­ecule are located on a mirror plane. All other atoms are located on general positions. The atomic arrangements of both compounds are characterized by [MO₆] octa­hedra (M = Ni or Mg) connected by glycine mol­ecules, with the halogenide ions in the inter­stices. In (I), four of the coordinating O atoms are from glycine and two are from water mol­ecules, building layers of octa­hedra and organic mol­ecules. In (II), two of the coordinating O atoms are from glycine and four are from water mol­ecules. The octa­hedra and organic mol­ecules form chains.     

catena‐Poly[[[N,N′‐bis­(salicyl­idene)propane‐1,3‐diaminato]cobalt(III)]‐μ‐azido] and catena‐poly[[[N,N′‐bis(salicyl­idene)propane‐1,3‐diaminato]cobalt(III)]‐μ‐thio­cyanato]

The two title complexes, catena‐poly[[{2,2′‐[1,3‐propane­diylbis(nitrilo­methyl­idyne)]diphenolato}cobalt(III)]‐μ‐azido], [Co(C₁₇H₁₆N₂O₂)(N₃)]_n, (I), and catena‐poly[[{2,2′‐[1,3‐propane­diylbis(nitrilo­methyl­idyne)]diphenolato}cobalt(III)]‐μ‐thio­cyanato], [Co(C₁₇H₁₆N₂O₂)(NCS)]_n, (II), are isomorphous polynuclear cobalt(III) compounds. In both structures, the Co^III atom is six‐coordinated in an octa­hedral configuration by two N atoms and two O atoms of one Schiff base, and two terminal N or S atoms from two bridging ligands. The [N,N′‐bis­(salicyl­idene)propane‐1,3‐diaminato]cobalt(III) moieties are linked by the bridging ligands, viz. azide in (I) and thio­cyanate in (II), giving zigzag polymeric chains with backbones of the type [–Co—N—N—N—Co]_n in (I) or [–Co—N—C—S—Co]_n in (II) running along the c axis.     

One‐dimensional zinc‐based coord­in­ation polymers incorporating cyanate anions

Two one‐dimensional zinc‐based coordination polymers containing cyanate anions are reported. catena‐Poly[sodium [[tricyanato­zinc(II)]‐μ‐1,4‐diaza­bicyclo­[2.2.2]octane‐κ²N:N′]], {Na[Zn(NCO)₃(C₆H₁₂N₂)]}_n, consists of linear [tricyanato­zinc(II)]‐μ‐1,4‐diaza­bicyclo­[2.2.2]octane strands in which the Zn²⁺ cations adopt trigonal–bipyramidal coordination on sites of m2 point symmetry. Na⁺ cations lie between the strands on sites of m point symmetry, coordinated in a distorted octa­hedral geometry by six O atoms of the cyanate anions. catena‐Poly[[dicyanato­zinc(II)]‐μ‐4,4′‐bipyridine‐κ²N:N′], [Zn(NCO)₂(C₁₀H₈N₂)]_n, crystallizes in the space group P2₁/n with Z′ = 5. The structure consists of zigzag strands formed by Zn²⁺ cations linked via 4,4′‐bipyridine. Each Zn²⁺ cation adopts a tetra­hedral coordination, with two sites occupied by 4,4′‐bipyridine and two cyanate anions completing the coordination sphere. The structure is closely comparable with the thio­cyanate and halide analogues [ZnX₂(C₁₀H₈N₂)] (X = NCS, Cl or Br).     

Unexpected oxidation of a diphos­phine by bis­(1,3‐diphenylpropane‐1,3‐dionato)­cobalt(II), [Co(dbm)2]

The reaction of bis­(1,3‐diphenylpropane‐1,3‐dionato)cobalt(II), [Co(dbm)₂], with bis­(diphenyl­phosphino)ethane (dppe) affords the coordination polymer catena‐poly[[bis­(1,3‐diphenyl­propane‐1,3‐dionato‐κ²O,O′)cobalt(II)]‐μ‐ethyl­enebis(diphenyl­phosphine oxide)‐κ²O:O′], trans‐[Co(C₁₅H₁₁O₂)₂(C₂₆H₂₄O₂P₂)]_n, as a result of oxidation of the diphos­phine. The Co atom is octa­hedral, with a CoO₆ coordination sphere, and the chelating dbm ligands adopt a trans configuration. The Co atom also lies on a centre of inversion, with a further symmetry centre bis­ecting the bridging ethyl­enebis(diphenyl­phosphine oxide) ligand.     

One‐dimensional polymeric chain structure of bis­(aniline)­di­thio­cyanato­cadmium(II)

In the title compound, catena‐poly­[[bis­(aniline‐N)cadmium(II)]‐di‐μ‐thio­cyanato‐S:N;N:S], [Cd­(SCN)₂­(C₆H₇N)₂], the Cd^II atom lies on an inversion centre and is in a distorted octahedral geometry. The coordination sphere contains two thio­cyanate (SCN) S atoms, two iso­thio­cyanate (NCS) N atoms and two aniline N atoms. The six‐coordinated Cd atoms run parallel to the b axis and are doubly bridged with neighbouring Cd atoms by SCN and NCS ligands. Thus, this complex has a one‐dimensional coordination polymeric chain structure in which the aniline ligand is in the trans conformation.     

A new chain‐like cadmium(II) coordination polymer containing chains of water mol­ecules

The title cadmium(II) polymer, catena‐poly[[[bis­(4‐amino­pyridine‐κN)­aqua­cadmium(II)]‐μ‐1,4‐phenyl­enediacetato‐κ⁴O,O′:O′′,O′′′] dihydrate], {[Cd(C₁₀H₈O₄)(C₅H₆N₂)₂(H₂O)]·2H₂O}_n, comprises one‐dimensional wave‐like chains, in which the Cd atom is coordinated by 1,4‐phenyl­enediacetate and 4‐amino­pyridine molecules. The 1,4‐phenylenediacetate ligands lie about inversion centres. Extensive hydrogen‐bonding inter­actions between the chains lead to a three‐dimensional structure. Free water mol­ecules form chains in the structure.     

catena‐Poly[bis­(tert‐butyl­ammonium) [plumbate(II)‐tri‐μ‐iodo] iodide dihydrate]

The title compound, {(C₄H₁₂N)₂[PbI₃]I·2H₂O}_n, crystallizes as an organic–inorganic hybrid. The six‐coordinate Pb atom lies on a centre of inversion and all the I atoms lie on mirror planes; the two independent cations both lie across mirror planes. The structure contains anionic chains along [100] of fused [PbI₃]⁻ units forming face‐sharing octa­hedra. Four cations enclose channels occupied by isolated iodide ions and water mol­ecules of hydration.     

A novel nickel(II) coordination polymer incorporating 1,4‐phenylene­diacetic acid and 1,10‐phenanthroline

The title nickel(II) coordination polymer, viz. poly[[bis­(1,10‐phenanthroline)tris­(μ₃‐1,4‐phenyl­enediacetato)trinickel(II)] dihydrate], {[Ni₃(C₁₀H₈O₄)₃(C₁₂H₈N₂)₂]·2H₂O}_n, consists of linear trinuclear building blocks with two crystallographically unique Ni atoms. One Ni^II atom and the geometric centre of one 1,4‐phenyl­enediacetate ligand in the trinuclear unit both lie on inversion centres, while the other unique Ni^II atom lies near the inversion centre, together with another 1,4‐phenyl­enediacetate ligand. Each pair of adjacent trinuclear units is bridged by 1,4‐phenyl­enediacetate ligands, forming two kinds of infinite chains along the a and b axes, respectively. These two kinds of chains crosslink to yield a two‐dimensional network in the ab plane. The two‐dimensional sheets further stack along the c axis viaπ–π stacking inter­actions and hydrogen bonds, forming a three‐dimensional supramolecular structure.     

A polymeric zinc thio­sulfate complex containing anionic and cationic chains based on tetra­hedral and octa­hedral zinc sites

catena‐Poly[[[tetra­aqua­zinc(II)]‐μ‐4,4′‐bipyridine‐κ²N:N′] [[μ‐thio­sulfato‐κ²O:S‐bis­[(thio­sulfato‐κS)zinc(II)]]‐di‐μ‐4,4′‐pyridine‐κ⁴N:N′] dihydrate], {[Zn(C₁₀H₈N₂)(H₂O)₄][Zn₂(S₂O₃)₃(C₁₀H₈N₂)₂]·2H₂O}_n, is a polymeric zinc complex built up from thio­sulfate‐containing anionic chains, where the Zn atom is tetra­hedrally coordinated, and aqua‐containing cationic chains incorporating octa­hedrally coordinated Zn. In each type of chain, the 4,4′‐bipyridine units act as spacers, and the chains run along three non‐inter­secting almost orthogonal directions in space. The profusion of hydrogen‐bond donors (all the H atoms of the water mol­ecules) and acceptors (the thio­sulfate O and S atoms) generates a very complex hydrogen‐bonding scheme.     

Two two‐dimensional MnII and NaI coordination polymers constructed by the flexible benzene‐1,4‐dioxy­acetate ligand

Two new two‐dimensional coordination polymers, poly­[[[aqua(2,2′‐bi­pyridine‐κ²N,N′)manganese(II)]‐μ₃‐p‐phenyl­enebis­(oxy­acet­ato)‐κ³O:O′:O′′] dihydrate], {[Mn(C₁₀H₈O₆)(C₁₀H₈N₂)(H₂O)]·2H₂O}_n, (I), and poly­[[di‐μ‐aqua‐bis­[aqua­sodium(I)]]‐μ₄‐p‐phenyl­enebis­(oxy­acetato)‐κO:O′,O′′:O′′′,O′′′′:O′′′′′], [Na₂(C₁₀H₈O₆)(H₂O)₄]_n, (II), have been synthesized and characterized by X‐ray single‐crystal diffraction. In (I), there are two 1,4‐BDOA²⁻ [p‐phenyl­enebis­(oxy­acetate) or, more commonly, benzene‐1,4‐dioxy­acetate] ligands, each lying about inversion centres, while in (II), there is one such ligand and it also has crystallographically imposed inversion symmetry. In (I), each Mn^II atom displays an octahedral MnN₂O₄ configuration, defined by three carboxyl O atoms of different 1,4‐BDOA²⁻ groups, two N atoms of one 2,2′‐bi­pyridine ligand and one water mol­ecule. In (II), each Na^I atom is octahedrally coordinated by one ether O atom, two carboxyl O atoms of different 1,4‐BDOA²⁻ ligands and three water mol­ecules. The metal ions in complexes (I) and (II) are bridged by 1,4‐BDOA²⁻ groups into two‐dimensional layer structures. Furthermore, three‐dimensional supramolecular networks are constructed via hydrogen bonds in (I) and (II), and by additional π–π stacking interactions in (I).     

N‐Benzyl‐2′‐iodo­cinnamanilide and N‐benzyl‐2′‐iodo‐4′‐methyl‐2‐phenyl­cinnamanilide

The aromatic ring of the cinnamic moiety in N‐benzyl‐2′‐iodo­cinnamanilide, C₂₂H₁₈INO, (I), and N‐benzyl‐2′‐iodo‐4′‐methyl‐2‐phenyl­cinnamanilide, C₂₉H₂₄INO, (II), makes a dihedral angle with the iodo­phenyl ring of 72.1 (2) and 81.0 (2)° in (I) and (II), respectively. In (I), mol­ecules exist as discrete components, while in (II), they form infinite chains along the b axis, through I?O non‐bonded interactions.     

Orthorhombic modification of tri­phenyl­tin 3‐ureidopropionate

The Sn atom in catena‐poly­[tri­phenyl­tin(IV)‐μ‐(3‐ureidopropionato‐O¹:O³)], [Sn(C₆H₅)₃(C₄H₇N₂O₃)]_n, is five‐coordinate and has a trans‐C₃SnO₂ trigonal‐bipyrmidal geometry arising from bridging through the O atom of the ureido fragment of an adjacent carboxyl­ate group. Infinite chains propagate helically along the c axis and adjacent chains are linked by N—H?O [N?O 2.851 (4) Å] hydrogen bonds into layers.     

cis‐[1,4‐Bis(di­phenyl­phosphino)­butane](μ‐tetra­thio­tungstato)­palladium(II) N,N′‐di­methyl­form­amide hemisolvate hemihydrate

In the title compound, [1,4‐bis(di­phenyl­phosphino)­butane‐2κ²P,P′]­di‐μ‐thio‐1:2κ⁴S‐di­thio‐1κ²S‐palladium(II)­tung­sten(VI) N,N′‐di­methyl­form­amide hemisolvate hemihydrate, [PdWS₄­(C₂₈H₂₈P₂)]·0.5C₃H₇NO·0.5H₂O, the Pd atom is coordinated by two S atoms from the distorted‐tetrahedral [WS₄]²⁻ anion and two P atoms from the dppb mol­ecule [dppb is 1,4‐bis(di­phenyl­phos­phino)­butane] in an approximately square‐planar configuration. A puckered seven‐membered ring is formed by the Pd atom and the dppb ligand.     

Octa­kis(3‐propyl­ammonium) octa­deca­iodo­penta­plumbate(II): a new layered stucture based on layered perovskites

The title compound, (C₃H₁₀N)₈[Pb₅I₁₈], crystallizes as an inorganic–organic hybrid. As such, the structure consists of two‐dimensional sheets of corner‐ and face‐sharing [PbI₆]⁴⁻ octa­hedra, separated by layers of 3‐propyl­ammonium cations, which hydrogen bond to the I atoms. The asymmetric unit contains six independent Pb atoms; four are on general positions and the other two are on special positions, viz. a centre of inversion and a twofold axis. The inorganic sheets show a never before seen motif.     

A new optically pure half‐sandwich Cp–Ru diphosphine complex with a chiral metal centre, (S)‐Ru(η5‐C5H5)(EPHOS)Cl {EPHOS is (+)‐(1R,2S)‐2‐[(diphenylphosphino)methylamino]‐1‐phenylpropyl diphenylphosphinite}

The crystal structure of the title compound, chloro(η⁵‐cyclopenta­dienyl){(1R,2S)‐2‐[(di­phenyl­phosphino)­methyl­amino]‐1‐phenyl­propyl di­phenyl­phosphinite‐κ²P,P′}ruthenium(II), [Ru(C₅H₅)Cl(C₃₄H₃₃NOP₂)], is reported. The pseudo‐octa­hedral complex is chiral and the configuration at the Ru atom is S. The seven‐membered metallacycle adopts a boat‐like conformation.     

catena‐Poly[tetra­kis(3‐phenyl­propyl­ammonium) [iodo­plumbate(II)‐tri‐μ‐iodo‐plumbate(II)‐tri‐μ‐iodo‐iodo­plumbate(II)‐di‐μ‐iodo]]

The title compound, {(C₉H₁₄N)₄[Pb₃I₁₀]}_n, crystallizes as an organic–inorganic hybrid. As such, the structure consists of a two‐dimensional inorganic layer of [Pb₃I₁₀]_n⁴ⁿ⁻ ions extending along [100]. The asymmetric unit contains two independent Pb atoms, viz. one in a general position and the other on an inversion centre. Each Pb atom is octa­hedrally coordinated by six iodide ions and exhibits both face‐ and corner‐sharing with adjacent atoms in the inorganic layer. These anionic layers alternate with 3‐phenyl­propyl­ammonium cations, which hydrogen bond to the iodides. Simple face‐to‐edge σ–π stacking inter­actions are observed between the aromatic rings that stabilize the overall three‐dimensional structure. This net structure has only been observed five times previously.     

Platinum complexes of oxopurines: cis‐bis(theophyllinato‐N7)bis(triphenylphosphine)platinum(II) and cis‐chloro(theobrominato‐N1)bis(triphenylphosphine)platinum(II) ethanol hemisolvate

The syntheses and structures of two mixed‐ligand complexes of platinum(II) with deprotonated oxopurine bases and tri­phenyl­phosphine are reported, namely the theophyllinate complex cis‐bis(1,2,3,6‐tetra­hydro‐1,3‐di­methyl­purine‐2,6‐dionato‐κN⁷)­bis(tri­phenyl­phosphine‐κP)­platinum(II), [Pt(C₇H₇N₄O₂)₂(C₁₈H₁₅P)₂], (I), and the theobrominate complex cis‐chloro(1,2,3,6‐tetrahydro‐3,7‐dimethylpurine‐2,6‐dionato‐κN¹)­bis(tri­phenyl­phosphine‐κP)­platinum(II) ethanol hemisolvate, [PtCl(C₇H₇N₄O₂)(C₁₈H₁₅P)₂]·0.5C₂H₅OH, (II). In (I), the coordination geometry of Pt is square planar, formed by the two coordinating N atoms of the theophyl­linate anions in a cis arrangement and two P atoms from the tri­phenyl­phosphine groups. In (II), there are two crystallographically independent mol­ecules. They both exhibit a square‐planar coordination geometry around Pt involving one Cl atom, the coordinating N atom of the theobrominate anion and two P atoms from the tri­phenyl­phosphine groups. The two tri­phenyl­phosphine groups are arranged in a cis configuration in both structures. The heterocyclic rings are rotated with respect to the coordination plane of the metal by 82.99 (8) and 88.09 (8)° in complex (I), and by 85.91 (16) and 88.14 (18)° in complex (II). Both structures are stabilized by intramolecular stacking interactions involving the purine rings and the phenyl rings of adjacent tri­phenyl­phosphine moieties.     

Dicarbonyldi‐μ‐chloro‐cis,cis‐η4‐1,5‐cyclo­octa­dienedirhodium(I)

The title compound, dicarbonyl‐1κ²C‐di‐μ‐chloro‐1:2κ⁴Cl‐[cis,cis‐2(η⁴)‐1,5‐cyclo­octa­diene]­di­rhodium(I), [Rh₂Cl₂(C₈H₁₂)(CO)₂], consists of a di­chloro‐bridged dimer of rhodium, with a non‐bonded Rh?Rh distance of 3.284 (2) Å. One Rh atom is coordinated to two carbonyl ligands, while the other Rh atom is coordinated to the cyclo­octa­diene moiety.     

A lithium complex of pyridine‐2,6‐dicarboxylic acid

The crystal structure of catena‐poly­[[(6‐carboxy­pyridine‐2‐carb­oxyl­ato‐κ³O,N,O′)­lithium(I)]‐μ‐aqua‐κ²O:O], [Li(C₇H₄NO₄)­(H₂O)]_n, contains the Li⁺ ion coordinated to two O atoms and the N atom of the 6‐carboxy­pyridine‐2‐carboxyl­ate ligand, and to two water O atoms, forming a pentavalent coordination geometry. The molecule resides on a mirror plane which contains the Li and N atoms, the para‐CH unit, and the O atom of the coordinated water mol­ecule. The O atom of the water mol­ecule is coordinated to two Li atoms, forming an infinite polymeric chain.     

Barium bis­[6‐amino‐3‐methyl‐5‐nitro­so­pyrimidine‐2,4(1H,3H)‐dionate] trihydrate: coordination polymer chains linked by hydrogen bonds

The title complex, catena‐poly[[triaquabarium(II)]‐di‐μ‐6‐amino‐3‐methyl‐5‐nitro­so­pyrimidine‐2,4(1H,3H)‐dionato], [Ba(C₅H₅N₄O₃)₂(H₂O)₃]_n, forms a coordination polymer chain in which the two distinct anions use different ligating atoms to bridge pairs of cations. Adjacent pairs of cations are also linked by pairs of bridging water mol­ecules. The chains are linked into a single three‐dimensional framework by an extensive series of hydrogen bonds.