catena‐Poly[[diaquabis(2‐chloronicotinato‐κ2O,O′)cadmium(II)]‐μ‐2‐chloronicotinato‐κ3O,O′:N]

In the title neutral coordination polymer, [Cd(C₆H₃ClNO₂)₂(H₂O)₂]_n, each Cd^II ion is coordinated by one N and four O atoms from three 2‐chloro­nicotinate ligands and by two aqua ligands, defining a distorted monocapped octahedral coordination geometry. Adjacent Cd atoms are linked by the pyridyl N atom and the bidentate carboxyl­ate functional group of a 2‐­chloro­nicotinate ligand, forming a one‐dimensional infinite chain along the b axis. The Cd⋯Cd distance is 8.112 (3) Å. These chains are linked by O—H⋯O and O—H⋯N hydrogen bonds into a three‐dimensional network structure.     

Dibarium zirconium tetraoxalate trihydrate

A new mixed barium zirconium oxalate, tri­aqua­tetra‐μ‐oxalato‐dibarium(II)­zirconium(IV), Ba₂Zr(C₂O₄)₄·3H₂O or [Ba₂Zr(C₂O₄)₄(H₂O)₃]_n, has been synthesized. The complex is built from eightfold‐coordinated Zr atoms and eleven‐ and sixfold‐coordinated Ba atoms, linked by oxalate groups. The Zr atom, the two Ba atoms and one water O atom lie on crystallographic twofold axes, so that each coordination polyhedron has imposed C2 symmetry. Packing in the crystal is also assumed through hydrogen bonds.     

Polymeric (3‐amino‐2‐chloropyridine)nitratosilver(I)

In the title compound {alternative name: poly­[silver(I)‐μ‐(3‐­amino‐2‐chloro­pyridine)‐μ‐nitr­ato]}, [Ag(NO₃)(C₅H₅ClN₂)]_n the Ag^I atom is in an irregular AgN₂O₃ geometry, surrounded by one pyridyl N atom [Ag—N 2.283 (5) Å], one amine N atom [Ag—N 2.364 (6) Å] and three O atoms from different nitrate ions [Ag—O 2.510 (6)–2.707 (6) Å]. The Ag ions are bridged by the 3‐amino‐2‐chloro­pyridine ligands into helical chains. Adjacent uniform chiral chains are further interlinked through the NO₃ bridges into an interesting two‐dimensional coordination network in the solid.     

Chlor­amine‐B sesquihydrate

In the title compound, sodium N‐chloro­benzene­sulfon­amide sesquihydrate, Na⁺·C₆H₅ClNO₂S^?·1.5H₂O, the sodium ion exhibits octahedral coordination by O atoms from three water mol­ecules and by three sulfonyl O atoms of three different N‐­chloro­benzene­sulfon­amide anions. A two‐dimensional polymeric layer consists of units, each comprising two face‐sharing octahedra which share four corners with four other such units, the layer running parallel to the ab plane. The water mol­ecules participate in hydrogen bonds of the types O—H?O, O—H?N and O—H?Cl.     

(12,17‐Diethoxy­carbonyl‐2,3,6,­7,11,­18‐hexa­methyl­corrphy­cenato‐­κ4N)iodoiron(III) chloro­form solvate

The title complex, (diethyl 3,4,8,15,19,20‐hexa­methyl‐21,22,23,24‐tetraazopenta­cyclo­[16.2.1.1^2,5.1^7,11.1^14,17]­tetracosa‐1(20),2(22),3,5,7,9,11,13(24),14,16,18‐undecaene‐9,14‐dicarb­oxyl­ate‐κ⁴N)­iodo­iron(III) chloro­form solvate, [Fe(C₃₂H₃₂­N₄O₄)I]·­CHCl₃, shows an almost planar arrangement of the corrphycene moiety with a slightly distorted trapezoid pyramidal core; the Fe^III atom is 0.416 (1) Å from the plane of the C₂₀N₄ system. The Fe—N distances are 2.049 (3), 2.044 (3), 2.079 (3) and 2.075 (3) Å. The solvated chloro­form forms a C—H?O hydrogen bond [C?O 3.107 (10) Å] to an adjacent carbonyl O atom. This is the first X‐ray structure analysis of a corrphycenatoiron(III) derivative.     

The first salt of an isolated penta­chloro­plumbate(II) trianion

The title compound, tris(cyclo­hexane‐1,2‐diamine‐κ²N,N′)cobalt penta­chloro­plum­bate sesquihydrate, [Co(C₆H₁₄N₂)₃][PbCl₅]·1.5H₂O, crystallizes in the monoclinic space group C2/c, with a tricationic cobalt complex, a penta­chloro­plumbate trianion, one water mol­ecule in a general position and a second water mol­ecule on a crystallographic twofold axis. The compound is the first example of an isolated [PbCl₅]³⁻ moiety; the Pb atom is coordinated in a square‐pyramidal fashion, with four longer bonds to Cl atoms in the basal plane and a shorter distance to the apex. The ionic constituents and the solvent mol­ecules form a three‐dimensional network of hydrogen bonds.     

A fluoro­phenylboron‐functionalized zirconium silsesquioxane complex

Bis(η⁵‐cyclo­penta­dienyl)[rel‐(1R,5S,7R,14S)‐(1,3,5,7,9,11,14‐hepta­cyclo­pentyl‐7,14‐dioxidotri­cyclo­[7.3.3^1,9.1^5,11]­hepta­siloxan‐3‐yloxy)­bis­(penta­fluoro­phenyl)­borane(2−)]­zirconium, [Zr(C₅H₅)₂(C₄₇H₆₃BF₁₀O₁₂Si₇)], consists of [ZrCp₂] (Cp is cyclopentadienyl) and [(C₆F₅)₂B] moieties bound to a silsesquioxane core. The silsesquioxane binds to the Zr atom through two of its O atoms to form a distorted tetrahedron. The [(C₆F₅)₂B] moiety is bound to the silsesquioxane through an O atom, forming an Si—O—B bond angle of 168.4 (4)°. The steric and electronic effects of the Zr atom and the borate moieties force the silsesquioxane core to distort. These distortions can be seen by examination of the Si—O—Si bond angles.     

Three complexes of bis(N‐methyl­benzo­hydro­xamato‐O,O′)copper(II)

The first single‐crystal studies of three bis‐transoid Cu–hydrox­amate salts, bis(3‐methoxy‐4,N‐dimethyl­benzo­hydrox­amato‐O,O′)copper(II), [Cu(C₁₀H₁₂NO₃)₂], bis(4‐chloro‐N‐methyl­benzo­hydro­xamato‐O,O′)copper(II), [Cu­(C₈­H₇­Cl­NO₂)₂], bis(N‐methyl‐3,5‐di­nitro­benzo­hydro­xamato‐O,O′)copper(II)–chloro­form (1/2), [Cu­(C₈­H₆­N₃O₆)₂]·­2CHCl₃, are presented. The Cu atom in each of the title compounds sits at a center of inversion and displays a nearly square‐planar geometry with the hydro­xamate‐O atoms connected to it in a syn configuration. The N atoms are in a transoid configuration. Each five‐membered Cu–hydro­xamate ring is planar, thus providing evidence that a planar N atom is present in each ring. The phenyl groups are twisted with respect to the hydro­xamate group by ～40–54°. The angular strain of the sp² carbonyl oxy­gen is significant (～10° from ideal).     

Di­chloro­bis(3,5‐di­methyl­pyrazole‐N2)methyl­phenyl­tin(IV)

The title compound, [SnCl₂(CH₃)(C₆H₅)(C₅H₈N₂)₂], was obtained by reaction of di­chloro­methyl­phenyl­tin(IV) and 3,5‐di­methyl­pyrazole (dmpz) in chloro­form, and was recrystallized from acetone. The structure consists of octahedral all‐trans [SnMePhCl₂(dmpz)₂] mol­ecules, with the Sn atom coordinated to two C [Sn—C 2.127 (5) and 2.135 (4) Å], two Cl [Sn—Cl 2.5753 (8) Å] and two N atoms [Sn—N 2.357 (3) Å]. The dmpz ligands, bound to the metal through their unprotonated N atoms, form weak intra‐ and intermolecular hydrogen bonds with the Cl ligands via their NH groups, giving rise to a polymeric chain along the c axis.     

Bis­[1‐(p‐chloro­phenyl)‐5‐iso­propyl­biguanide‐κ2N2,N4]­nickel(II) dichloride di­methyl­form­amide solvate

The asymmetric unit of the title compound, [Ni(C₁₁H₁₆ClN₅)₂]Cl₂·C₃H₇NO, contains one monomeric nickel(II) com­plex cation, two Cl⁻ anions and one di­methyl­form­amide sol­vent mol­ecule. The Ni atom is coordinated to each of two 1‐­(p‐chloro­phenyl)‐5‐iso­propyl­biguanide (proguanil) ligands via two N atoms. The complex exhibits a square‐planar coordination, with the Ni atom lying 0.021 (2) Å out of the basal plane. The crystal packing is characterized by several hydrogen bonds.     

A 1:2 complex of mercury(II) chloride with 1,3‐imidazole‐2‐thione

The Hg atom in the title monomeric complex, di­chloro­bis(3‐imidazolium‐2‐thiol­ato‐S)­mercury(II), [HgCl₂(C₃H₄N₂S)₂], is four‐coordinate having an irregular tetrahedral geometry composed of two Cl atoms [Hg—Cl 2.622 (2) and 2.663 (2) Å] and two thione S atoms [Hg—S 2.445 (2) and 2.462 (2) Å]. The monodentate thione ligand adopts a zwitterionic form and exists as the 3‐imidazolium‐2‐thiol­ate ion. The bond angle S1—Hg—S2 of 130.87 (8)° has the greatest deviation from ideal tetrahedral geometry. Intermolecular hydrogen bonds between two of the four N—H groups and one of the Cl atoms [3.232 (8) and 3.238 (7) Å] stabilize the crystal structure, while the other two N—H groups contribute through the formation of N—H?Cl intramolecular hydrogen bonds with the other Cl atom [3.121 (7) and 3.188 (7) Å].     

A chloro(2‐pyridinecarboxaldehyde)(2,2′:6′,2′′‐ter­pyridine)­ruthenium(II) complex

The aldehyde moiety in the title complex, chloro(2‐pyridinecarboxaldehyde‐N,O)(2,2′:6′,2′′‐terpyridine‐κ³N)ruthenium(II)–chloro­(2‐pyridine­carboxyl­ic acid‐N,O)(2,2′:6′,2′′‐ter­pyridine‐κ³N)­ruthenium(II)–perchlorate–chloro­form–water (1.8/0.2/2/1/1), [RuCl­(C₆H₅NO)­(C₁₅H₁₁N₃)]_1.8[RuCl­(C₆H₅­NO₂)(C₁₅H₁₁N₃)]_0.2­(ClO₄)₂·­CHCl₃·­H₂O, is a structural model of substrate coordination to a transfer hydrogenation catalyst. The title complex features two independent Ru^II complex cations that display very similar distorted octahedral coordination provided by the three N atoms of the 2,2′:6′,2′′‐ter­pyridine ligand, the N and O atoms of the 2‐pyridine­carbox­aldehyde (pyCHO) ligand and a chloride ligand. One of the cation sites is disordered such that the aldehyde group is replaced by a 20 (1)% contribution from a carboxyl­ic acid group (aldehyde H replaced by carboxyl O—H). Notable dimensions in the non‐disordered complex cation are Ru—N 2.034 (2) Å and Ru—O 2.079 (2) Å to the pyCHO ligand and O—C 1.239 (4) Å for the pyCHO carbonyl group.     

Polymorphs and pseudo‐polymorphs of μ‐oxo‐bis{[N,N′‐bis(salicylidene)­propane‐1,3‐diamine]oxorhenium(V)}

Two new polymorphs of the title compound, μ‐oxo‐bis{oxo{2,2′‐[propane‐1,3‐diyl­bis­(nitrilo­methyl­idyne)]­diphen­olato}rhenium(V)}, [Re₂O(C₁₇H₁₆N₂O₃)₂], are reported, containing either a conformation other than the one already known in the literature or a disorder involving both the new and the previously reported conformations. Four pseudo‐polymorphs of the title compound are also reported, containing four chloro­form, two chloro­form, two disordered di­chloro­methane or two water solvate mol­ecules accompany­ing each Re complex molecule. Only in the hydrate does the Re complex adopt the old conformation. In all six structures, the complex molecule is located on a crystallographic inversion centre. Independent of the conformation, all ReV ions display the same, somewhat distorted, octahedral coordination. In all the solvates, hydrogen bonds are donated from the solvent to the O atoms bonded to Re, either of the C—H?O or O—H?O type, although the actual position of the solvent mol­ecule can vary. Only in the hydrate is a two‐dimensional hydrogen‐bonded network found; isolated clusters are formed in all the other solvates.     

Chloro­(hist­amine)(1,10‐phenanthro­line)copper(II) chloride monohydrate

In the cationic complex present in the title compound, chloro­[2‐(4‐imidazolyl‐κN¹)­ethyl­amine‐κN](1,10‐phenanthroline‐κ²N,N′)copper(II) chloride monohydrate, [CuCl(C₅H₉­N₃)­(C₁₂H₈N₂)]Cl·H₂O, the metal centre adopts a five‐coordinate geometry, ligated by the two phenanthroline N atoms, two amine N atoms of the hist­amine ligand (one aliphatic and one from the imidazole ring) and a chloro ligand. The geometry around the Cu atom is a distorted compressed trigonal bipyramid, with one phenanthroline N and one imidazole N atom in the axial positions, and the other phenanthroline N atom, the histamine amine N atom and the chloro ligand in the equatorial positions. The structure includes an uncoordinated water mol­ecule, and a Cl⁻ ion to complete the charge. The water mol­ecule is hydrogen bonded to both Cl⁻ ions (coordinated and uncoordinated), and exhibits a close Cu⋯H contact in the equatorial plane of the bipyramid.     

(2‐Methyl­quinolin‐8‐olato)­iron(III) and ‐copper(II) complexes

The crystal structures of tris(2‐methyl­quinolin‐8‐olato‐N,O)­iron(III), [Fe­(C₁₀­H₈­NO)₃], (I), and aqua­bis(2‐methyl­quinolin‐8‐olato‐N,O)­copper(II), [Cu­(C₁₀­H₈NO)₂­(H₂O)], (II), have been determined. Compound (I) has a distorted octahedral configuration, in which the central Fe atom is coordinated by three N atoms and three O atoms from three 2‐methylquinolin‐8‐olate ligands. The three Fe—O bond distances are in the range 1.934 (2)–1.947 (2) Å, while the three Fe—N bond distances range from 2.204 (2) to 2.405 (2) Å. In compound (II), the central Cu^II atom and H₂O group lie on the crystallographic twofold axis and the coordination geometry of the Cu^II atom is close to trigonal bipyramidal, with the three O atoms in the basal plane and the two N atoms in apical positions. The Cu—N bond length is 2.018 (5) Å. The Cu—O bond length in the basal positions is 1.991 (4) Å, while the Cu—O bond length in the apical position is 2.273 (6) Å. There is an intermolecular OW—H?O hydrogen bond which links the mol­ecules into a linear chain along the b axis.     

cis‐Di­chloro­[tris­(di­phenyl­phosphino­ethyl)­amine]­ruthenium(II)–chloro­form–water (1/2.5/1)

In the title compound, [RuCl₂(C₄₂H₄₂NP₃)]·2.5CHCl₃·H₂O, the Ru atom is six‐coordinated, to one tetradentate tris­(di­phenyl­phosphinoethyl)­amine ligand and two Cl atoms, in a distorted octahedral arrangement. Molecules of chloro­form and water stabilize the framework through intermolecular hydrogen bonds.     

Poly[[cobalt(II)‐di‐μ3‐3,5‐diamino­benzoato‐κ3N:N′:O] monohydrate]

In the title compound, {[Co(C₇H₇N₂O₂)₂]·H₂O}_n, the Co^II atom lies on an inversion centre and has octahedral geometry, defined by two O atoms in axial positions and four N atoms in equatorial sites from six different 3,5‐diamino­benzoate ligands. Each 3,5‐diamino­benzoate anion acts as a μ₃‐bridging ligand, linking three adjacent Co^II ions through one O atom and two N atoms to form a three‐dimensional coordination polymer.     

trans‐[N,N′‐Bis­(salicyl­idene)­cyclo­hexane‐1,2‐diaminato]­nickel(II)–chloro­form (1/1)

In the title complex, trans‐{2,2′‐[cyclo­hexane‐1,2‐diyl­bis­(ni­t­rilo­methyl­idyne)]­di­phenol­ato‐κ⁴O,N,N′,O′}­nickel(II)–chloro­form (1/1), [Ni(C₂₀H₂₀N₂O₂)]·CHCl₃, the Ni atom has a square‐planar geometry, slightly tetrahedrally distorted. The Ni—N and Ni—O bonding distances are within the expected ranges for Ni–Schiff base derivatives. The di­imine bridge has a gauche conformation with the cyclo­hexyl ring almost coplanar with the NiN₂O₂ plane. The complex mol­ecules pack in dimers with an Ni?Ni distance of 3.59 (1) Å and form a three‐dimensional structure displaying a herring‐bone configuration. Channels are occupied by solvent mol­ecules, which are involved in C—H?O hydrogen bonds with the ligand O atoms.     

Facial π⋯Cl⋯π inter­actions as the directing motif of the supra­molecular structures of Mg2+ and Ca2+ bis[hydro­tris(pyrazol­yl)­borate] chloro­form disolvates

The isomorphous complexes bis­[hydro­tris(pyrazol­yl)­borato]­mag­nesium(II) chloro­form disolvate, [Mg(C₉H₁₀BN₆)₂]·2CHCl₃, and bis­[hydro­tris(pyrazol­yl)borato]calcium(II) chloro­form disolvate, [Ca(C₉H₁₀BN₆)₂]·2CHCl₃, crystallize in the cubic space group Pa with Z = 4. The metal atoms occupy sites of symmetry, and their coordination is very similar to that found for the unsolvated Mg[HB(Pz)₃]₂ and Ca[HB(Pz)₃]₂ complexes (Pz is pyrazole). The inclusion of chloro­form mol­ecules on threefold rotation axes not only leads to high‐symmetry crystal structures but also plays an important role in stabilizing the three‐dimensional supramolecular architecture through facial Pz⋯Cl⋯Pz inter­actions.     

A ternary complex of aqua(18‐crown‐6)bis(o‐nitrophenolato)barium(II), the triaqua(18‐crown‐6)(o‐nitrophenolato)barium(II) cation and the o‐nitrophenolate anion

In the title compound [systematic name: tri­aqua(1,4,7,10,13,16‐hexaoxa­cyclo­octa­decane‐κ⁶O)(2‐nitro­phenolato‐κO)­barium(II)–aqua(1,4,7,10,13,16‐hexaoxa­cyclo­octa­decane‐κ⁶O)‐ bis(2‐nitro­phenolato‐κ²O,O′)­barium(II)–2‐nitro­phenolate (1/1/1)], [Ba(C₁₂H₂₄O₆)(C₆H₄NO₃)(H₂O)₃][Ba(C₁₂H₂₄O₆)(C₆H₄NO₃)₂(H₂O)](C₆H₄NO₃), the two Ba^II atoms encapsulated by the 18‐crown‐6 rings have different coordinations. Although both Ba^II atoms are coordinated to the six O atoms of the crowns, in the neutral moiety, the Ba^II atom is coordinated to one terminal O atom from a water mol­ecule, two phenolate O atoms and two nitro‐group O atoms, while in the cationic moiety, the Ba^II atom is coordinated to three terminal O atoms from water mol­ecules and one phenolate O atom. Both the crowns are eclipsed and translated along the b direction. In the asymmetric unit, the three components are interconnected by four O—H?O interactions. The packing is stabilized by two intermolecular C—H?O interactions and by one O—H?O interaction.