catena‐Poly­[[bis­(thio­cyanato‐κN)cadmium(II)]‐di‐μ‐thio­urea‐κ4S:S]

The Cd^II ion in the title complex, [Cd(SCN)₂{SC(NH₂)₂}₂]_∞, is situated at a centre of symmetry, and is bound to two N atoms belonging to thio­cyanate groups and to four S atoms of bridging thio­urea ligands. The structure consists of infinite chains of slightly distorted edge‐shared Cd‐centred octahedra. The bridging S atoms of two thio­urea ligands comprise the common edge. Some thermal properties are described.     

Diacetatobis­(tri­methyl­ene­thio­urea)­zinc(II) monohydrate

In the title compound, [Zn(CH₃COO)₂(C₄H₈N₂S)₂]·H₂O, the Zn atom is tetrahedrally coordinated in the ZnO₂S₂ form. N—H?O and O—H?O intramolecular and intermolecular hydrogen bonds are formed by the four N atoms and the water mol­ecule. N—H?O intermolecular hydrogen bonds and C—H?S and C—H?O intermolecular interactions interconnect columns formed by the mol­ecules into layers. Adjacent layers are then linked by other N—H?O and O—H?O intermolecular hydrogen bonds to form a three‐dimensional framework throughout the structure. The orientations of the acetate planes are such that the Zn atom lies within them.     

trans‐Di­chlorotetrakis(4‐methyl­pyridine)­silicon bis­(triiodide) chloro­form solvate

At 173 K, the dication of the title compound, C₂₄H₂₈Cl₂N₄Si²⁺·2I₃^?·CHCl₃, is located on a crystallographic fourfold rotation axis. The chloro ligands occupy axial positions and the four 4‐methyl­pyridine ligands lie in the equatorial plane. The almost linear I₃^? ion is located on a crystallographic mirror plane and displays two significantly different I—I bond lengths. Furthermore, chloro­form mol­ecules, which are disordered about a centre of inversion, fill the remaining gaps in the crystal structure.     

trans‐Di­chloro­bis­(tri­phenyl­phosphine‐P)­platinum(II)

Two different crystals (A and B) were used to structurally characterize trans‐[PtCl₂(PPh₃)₂] and to study random and systematic errors in derived parameters. The compound is isomorphous with trans‐[PdCl₂(PPh₃)₂] and with one of the polymorphs of trans‐[PtMeCl(PPh₃)₂] reported previously. Half‐normal probability plot analyses based on A and B show realistic s.u.'s and negligible systematic errors. R.m.s. calculations give very good agreement between A and B, 0.0088 Å. Important geometrical parameters are Pt—P = 2.3163 (11) Å, Pt—Cl = 2.2997 (11) Å, P—Pt—Cl = 87.88 (4) and 92.12 (4)°. Half‐normal probability plots and r.m.s. calculations were also used to compare the title compound with the palladium analogue, showing small systematic differences between the compounds. The torsion angles around the Pt—P bond were found to be very similar to those reported for isomorphous complexes, as well as to the torsion angles around the Pt—As bond in trans‐[PtCl₂(AsPh₃)₂]. The NMR coupling constants for the title compound are similar to Pt—P coupling constants reported for analogous trans complexes.     

Tetrakis­[1‐(3‐chloro­propyl)‐1,2,4‐tri­azole‐κN4]­bis­(tetrafluoroborato‐κF)copper(II)

In the title complex, [Cu(BF₄)₂(1tpc)₄] [1tpc is 1‐(3‐chloro­propyl)‐1,2,4‐triazole, C₅H₈ClN₃], the copper(II) centres reside in a tetragonally distorted octahedral coordination environment. Four 1tpc ligands are coordinated to the metal atom via the N4 atom of the triazole rings in a square‐planar arrangement, with Cu—N bond lengths in the range 2.002 (2)–2.019 (2) Å. Two tetra­fluoro­borate anions, in the axial positions above and below the square plane, are weakly coordinated to the copper(II) centre, with Cu—F distances of 2.4009 (18) and 2.5096 (18) Å.     

trans‐Di­aqua­bis­(thio­semicarb­azido‐κ2N,S)­nickel(II) dimaleate dihydrate

In the title compound, [Ni(CH₅N₃S)₂(H₂O)₂](C₄H₃O₄)₂·2H₂O, the Ni atom lies on a center of symmetry and is coordinated by N and S atoms from two thio­semicarbazide ligands and the O atoms of two water mol­ecules in a distorted octahedral geometry. In the asymmetric unit, the three components are linked together by one O—H⋯O and two N—H⋯O hydrogen bonds. The packing is built from molecular ribbons parallel to the b direction, stabilized by intramolecular hydrogen bonds, and by one N—H⋯S and two N—H⋯O intermolecular hydrogen bonds. The ribbons are further connected into columns by N—H⋯O interactions and then into a three‐dimensional network by three O—H⋯O hydrogen bonds.     

Chloro­bis­(thio­urea‐κS)copper(I) bis(4,5‐di­aza­fluoren‐9‐one) mono­hydrate

The title compound, [CuCl(CH₄N₂S)₂]·2C₁₁H₆N₂O·H₂O, consists of mol­ecules of a Cu^I–thio­urea complex, free 4,5‐di­aza­fluoren‐9‐one (dafone) and crystalline water. The planar complex mol­ecule has trigonal coordination geometry around the Cu^I atom. The dafone and water mol­ecules, which are hydrogen bonded to the Cu^I complex, are approximately coplanar with this complex. The crystal displays a sheet structure and π–π stacking is observed between neighbouring sheets.     

cis‐Di­chloro­bis­(triphenyphosphite‐P)palladium(II)

In the title compound, [PdCl₂{P(OPh)₃}₂], the Pd^II centre shows slightly distorted square‐planar geometry, with the two chloro ligands in cis positions.     

cis‐Di­chloro­(di­methyl­aminomethyl­ene)­(tri­phenyl­phosphine)palladium(II) acetone solvate

The synthesis and X‐ray structural analysis of the title compound, [PdCl₂(C₃H₇N)(C₁₈H₁₅P)]·C₃H₆O, are described. The crystal structure contains discrete monomeric mol­ecules of the carbene complex and solvent mol­ecules separated by normal van der Waals distances. The Pd atom is four‐coordinate in an essentially square‐planar environment, with the chlorine ligands mutually cis; Pd—P = 2.2495 (7), Pd—Cl = 2.3508 (7) and 2.3600 (7), Pd—C 1.948 (2) and N—C(carbene) 1.274 (3) Å.     

Di­chloro­diethyl­bis­(pyridine‐N)tin(IV)

In the title complex, [Sn(C₂H₅)₂Cl₂(C₅H₅N)₂], the Sn atom lies on an inversion centre and is octahedrally coordinated by two Cl atoms, two ethyl C atoms and two pyridine N atoms in an all‐trans configuration. The dihedral angle between the pyridine ring and the SnNCl plane is 22.4 (2)°.     

Di­chloro­bis­(imidazolidin‐2‐one‐κO)­zinc(II) at 150 K

In the title compound, [ZnCl₂(C₃H₆N₂O)₂], the zinc(II) cation is surrounded by a distorted tetrahedral environment consisting of two Cl anions and two imidazolidin‐2‐one mol­ecules, the latter bound to the metal through their carbonyl O atoms. All atoms that are able to participate in hydrogen bonding are involved in such interactions. A hydrogen‐bonding network mediates the formation of mol­ecular columns parallel to the a axis. Neighboring columns are not bound by significant non‐covalent interactions; the result is an extended pattern of supramolecular aggregation that is intermediate in completeness between the situations observed in two related complexes of cobalt that have been studied previously.     

Di­chloro­bis(2‐chloro‐5‐methyl­pyridine‐κN)copper(II)

In the crystals of the title compound, [CuCl₂(C₆H₆ClN)₂], the Cu atom lies on an inversion centre and is four‐coordinated by two pyridine N atoms and two Cl atoms in trans positions. The coordination geometry is square planar, with Cu—N and Cu—Cl distances of 1.986 (2) and 2.2536 (11) Å, respectively. The two pyridine rings are parallel, but twist from the CuN₂Cl₂ coordination plane by about 95° in the complex mol­ecule. There are three kinds of intermolecular C—H⃛Cl hydrogen bonds in the crystals. Two of these types generate two‐dimensional molecular networks, viewed in the direction of the a axis, and the other connects adjacent molecular networks.     

trans‐Bis(3,5‐di­aza‐1‐azonia‐7‐phosphaadamantane‐κP)­bis­(thiocyanato‐κS)­palladium(II) bis­(thio­cyanate)

The crystal structure of the title compound, trans‐[Pd(NCS)₂(C₆H₁₃N₃P)₂](NCS)₂, is one of the few pal­ladium(II) complexes containing two protonated water‐soluble 1,3,5‐tri­aza‐7‐phos­pha­adamantane (PTA) ligands re­ported to date. The compound displays a distorted square‐planar geometry, with the Pd atom on an inversion centre and with the S atoms of the thio­cyanate counter‐ions occupying the axial positions above and below the equatorial plane described by the phosphine and thio­cyanate ligands. Geometric parameters for the formal coordination polyhedron include a Pd—P distance of 2.2940 (8) Å, a Pd—S distance of 2.3509 (8) Å and a P—Pd—S angle of 89.45 (3)°. The effective cone angle for the PTA ligands was calculated as 114.5°.     

Bis(acesulfamato‐κO4)diaqua­bis­(3‐methyl­pyridine‐κN)nickel(II)

In the crystal structure of the title compound [systematic name: diaqua­bis(6‐methyl‐2,2‐dioxo‐1,2,3‐oxathia­zin‐4‐olato‐κO⁴)bis­(3‐methyl­pyridine‐κN)nickel(II)], [Ni(C₄H₄NO₄S)₂(C₆H₇N)₂(H₂O)₂], the Ni^II centre resides on a centre of symmetry and has a distorted octa­hedral geometry. The basal plane is formed by two carbonyl O atoms of two monodentate trans‐oriented acesulfamate ligands and two trans aqua ligands. The axial positions in the octa­hedron are occupied by two N atoms of two trans pyridine ligands. Mol­ecules are stacked in columns running along the a axis. There are π–π stacking inter­actions between the mol­ecules in each column, with a distance of 3.623 (2) Å between the centroids of the pyridine rings. There are also O—H⋯O inter­actions between the columns.     

Chloro­bis­[N‐ethoxy­carbonyl‐N′‐(p‐methoxy­phenyl)­thio­urea‐κS]copper(I)

The title copper(I) complex, [CuCl(C₁₁H₁₄N₂O₃S)₂], was synthesized by the redox reaction of cupric chloride with the corresponding thio­urea derivative as reducing agent. The Cu^I coordination environment is trigonal planar, involving two S atoms and one Cl atom. The presence of intramolecular hydrogen bonds leads to the formation of a cis conformation and promotes the stability of the complex.     

Bis[bis­(methoxy­carbimido)amine‐κ2N,N′]bis­(perchlorato‐κO)copper(II) bis­[bis­(methoxy­carbimido)amine‐κ2N,N′]bis­(methanol‐κO)copper(II) bis­(perchlorate) methanol disolvate

The title compound, [Cu(ClO₄)₂(C₄H₉N₃O₂)₂][Cu(C₄H₉N₃O₂)₂(CH₄O)₂](ClO₄)₂·2CH₃OH, comprises two independent Cu^II species lying on different inversion sites. In the Cu complexes, a distorted octa­hedral geometry arises (from basic square‐planar N₄ coordination) from the weak coordination of two perchlorate ions (as Cu—O) in one species and two methanol mol­ecules in the other (also as Cu—O). Inter­actions between the O atoms of the perchlorate anions or methanol groups and the imide or amine NH groups afford an extensive inter­molecular hydrogen‐bonding network.     

Amido­bis­[η5‐1,3‐bis­(tri­methyl­silyl)­cyclo­penta­dienyl]­titanium(III)

The title compound, [Ti(C₁₁H₂₁Si₂)₂(NH₂)], crystallizes as a bent metallocene, with the NH₂ group oriented to maximize the π interaction between the N atom and the Ti^III center. The increased π bonding is reflected in a short Ti—N bond length of 1.933 (3) Å.     

Chloro­(3,6,13,16‐tetraethyl‐2,7,12,17‐tetra­methyl­porphycenato‐κ4N)iron(III) chloro­form solvate

The X‐ray crystallographic analysis of the title complex, chloro­[3,10,13,20‐tetraethyl‐4,9,14,19‐tetra­methyl­penta­cyclo[16.2.1.1^2,5.1^8,11.1^12,15]­tetracosa‐2,4,6,8(23),9,12,14,16,18(21),19‐decaene]­iron(III) chloro­form solvate, [Fe(C₃₃H₃₇N₄)Cl]·CHCl₃, reveals a twisted macrocyclic framework with a slightly distorted rectangular pyramidal core, where the deviation of the central Fe^III atom from the least‐squares plane of the C₂₀N₄ core is 0.594 (1) Å. Some important bond distances are as follows: Fe—N 2.019 (3), 2.026 (3), 2.028 (3) and 2.034 (3) Å; Fe—Cl 2.232 (1) Å.     

Bis(acesulfamato‐κ2O4,N)bis­(3‐methyl­pyridine)copper(II)

In the crystal structure of the title compound {systematic name: bis­[6‐methyl‐1,2,3‐oxa­thia­zin‐4(3H)‐one 2,2‐dioxide(1−)‐κ²N³,O⁴]bis­(3‐meth­yl­pyridine)copper(II)}, [Cu(C₄H₄NO₄S)₂(C₆H₇N)₂], the Cu^II centre resides on a centre of symmetry and has an octa­hedral geometry that is distorted both by the presence of four‐membered chelate rings and because of the Jahn–Teller effect. The equatorial plane is formed by the N atoms of two methyl­pyridine ligands and by the more basic O atoms of the acesulfamate ligands, while the weakly basic N atoms of these ligands are in elongated axial positions with a misdirected valence. The crystal is stabilized by two inter­molecular C—H⋯O inter­actions involving the methyl and CH groups, and the sulfonyl O atoms of the acesulfamate group.     

1,2‐Di­cyano‐1,2‐bis­(imidazolidine‐2‐thione)­digold(I) and 2,2‐di­cyano‐1,1‐bis­(di­methyl­thio­urea)­digold(I)

Gold(I) cyanide forms complexes with imidazolidine‐2‐thione (etu) and di­methyl­thio­urea (dmtu) with the formula [Au₂(CN)₂L₂], i.e. the title complexes di­cyano‐1κC,2κC‐bis(imidazolidine‐2‐thione)‐1κS,2κS‐digold(I)(Au—Au), [Au₂(CN)₂(C₃H₆N₂S)₂], and di­cyano‐1κ²C‐bis(N,N′‐di­methyl­thio­urea)‐2κ²S‐digold(I)(Au—Au), [Au₂(CN)₂(C₃H₈N₂S)₂]. In the etu complex, two approximately linear (etu)AuCN groups are held together by a weak homopolar Au—Au bond [3.117 (1) Å], with a torsion angle of 61 (3)° between the two groups. In the dmtu complex, an approximately linear Au(dmtu)₂ group is bound to an approximately linear Au(CN)₂ group by a weak heteropolar Au—Au bond [3.091 (1) Å], with a torsion angle of 83 (5)° between the two groups.