Polymorphism in bipodal O,O′‐dimeth­yl N,N′‐(m‐phenyl­ene­di­carbonyl)bis(thio­carbamate)

The title compound, C₁₂H₁₂N₂O₄S₂, crystallizes in white and yellow polymeric forms as a result of inter­esting anti–anti and syn–anti conformational isomerism of the thio­carbon­yl and carbon­yl moieties relative to one another. This work is the first reported X‐ray crystallographic structure determination of isomers of this class of bipodal ligand. The white form, anti–anti, (I), crystallizes with the benzene ring lying about a twofold rotation axis, resulting in both of the thio­carbon­yl and carbon­yl moieties being anti relative to each other. The yellow modification crystallizes as syn–anti, (II), with one thio­carbon­yl moiety syn and the other anti relative to the respective carbon­yl groups. The individual mol­ecules of both (I) and (II) are extensively linked through inter­molecular hydrogen bonds. Inter­molecular hydrogen bonding in (II) includes a network of bifurcated N—H⋯O and N—H⋯S hydrogen bonds, while mol­ecules of (I) include bifurcated C—H⋯O hydrogen bonds.     

Bis­(ethyl­enedi­amine)copper(II) bis(O,O′‐diethyl di­thio­phosphate)

In the structure of the title compound, [Cu^II­(en)₂][(EtO)₂P(S)S]₂ (en is ethyl­ene­di­amine) or [Cu(C₂H₈N₂)₂](C₄H₁₀O₂PS₂)₂, the Cu atom lies on a center of inversion and is coordinated in a slightly distorted square coordination geometry by four N atoms from two ethyl­enedi­amine mol­ecules. The diethyl di­thio­phosphate moieties, (EtO)₂P(S)S^?, act as counter‐anions.     

Aqua­(5,6‐di­methyl‐1,10‐phenanthroline‐N,N′)­(glycolato‐O,O′)­copper(II) nitrate

The title compound, [Cu(C₂H₃O₃)(C₁₄H₁₂N₂)(H₂O)]NO₃, is the first example of a mixed copper glycolate compound with a di­imine ligand. The copper(II) compound lies in a slightly distorted square‐pyramidal coordination environment with one water mol­ecule coordinated in the apical position. The glycolate ligand binds to the Cu atom as a chelate through a carboxyl­ate and the α‐OH O atom which, together with the N atoms of the substituted phenanthroline, constitute the base of the pyramid.     

Bis(2,2′‐bipyridyl‐N,N′)­tris­(nitrato‐O,O′)­neodymium

The title compound, [Nd(bipy‐N,N′)₂(NO₃–O,O′)₃], is found to be isomorphous with the La and Lu analogues having three bidentate nitrate and two bipyridyl ligands giving a ten co‐ordinate environment.     

Bis­(acetone‐κO)­bis(N,N′‐di­methyl­ethyl­enedi­amine‐κ2N,N′)copper(II) diperchlorate

The title compound, [Cu(C₄H₁₂N₂)₂(C₃H₆O)₂](ClO₄)₂, is the first structurally characterized Cu^II complex having acetone as axial ligands. The complex adopts an elongated octahedral trans‐[CuN₄O₂] coordination geometry, with the Cu atom having 222 site symmetry. The axial Cu—O(acetone) and in‐plane Cu—N bond lengths are 2.507 (5) and 2.041 (3) Å, respectively.     

Bis(N,N‐di­methyl­thio­carbamoyl­thio)­acetic acid

Bis(N,N‐di­methyl­thio­carbamoyl­thio)­acetic acid, [(CH₃)₂NC(=S)S]₂CHC(=O)OH or C₈H₁₄N₂O₂S₄, exists as a centrosymmetric hydrogen‐bonded dimer [O?O 2.661 (3) Å].     

Salicylaldehyde 4,4′‐(hexane‐1,6‐di­yl)­thio­semicarbazone

The title compound, C₁₄H₁₉N₃OS, is in the thio­keto form, with the thione S and hydrazine N atoms cis with respect to each other so that the S atom is involved in inter‐ and intra­molecular hydrogen bonds simultaneously. Inter­molecular C—H⋯S and C—H⋯O hydrogen bonds result in one‐dimensional polymeric chains of mol­ecules along the a axis. A weak C—H⋯π ring inter­action binds the polymeric chains together.     

Bis­(triethanol­amine‐O,O′)­nickel(II) di­acetate

The title compound, [Ni{N(CH₂CH₂OH)₃}₂](CH₃COO)₂, was prepared and the structure determined. It is isostructural with the copper(II) analogue.     

Tris(1,10‐phenanthroline‐N,N′)­iron(II) di­thio­cyanate tri­hydrate

The title mononuclear iron(II) complex, [Fe(C₁₂H₈N₂)₃](NCS)₂·3H₂O, has a slightly distorted octa­hedral coordination. One of the thio­cyanate ions and one of the water mol­ecules of crystallization show positional disorder.     

Bis­(O,O′‐di‐p‐tolyldithiophosphato‐S,S′)(1,10‐phenanthroline‐N,N′)nickel(II)

The title coordination complex, [Ni(C₁₄H₁₄O₂PS₂)₂(C₁₂H₈N₂)] or [Ni(pMePh‐dtp)₂(phen)] (phen is 1,10‐phenanthroline; dtp is di­aryl­di­thio­phosphate), has a non‐crystallographic twofold axis of symmetry through the Ni atom and the phen moiety. Two O,O‐di‐p‐tolyl­di­thio­phosphate (dtp) ions act as bidentate ligands. The central metal atom is coordinated by four S atoms from two dtp groups and two N atoms from the phen ligand. The title compound displays distorted octahedral geometry around the central Ni atom.     

Bis­[N,N‐bis(2‐hydroxy­ethyl)­di­thio­carbamato]­di­methyl­tin(IV)

The title compound, [Sn(CH₃)₂(C₅H₁₀NO₂S₂)₂], has crystallographic mirror symmetry (C—Sn—C on mirror plane) and the coordination polyhedron around the Sn atom is a tetrahedron [C—Sn—C 139.3 (2)° and S—Sn—S 82.3 (1)°] distorted towards a skew‐trapezoidal bipyramid owing to an intramolecular Sn?S contact [3.0427 (6) Å]. The mol­ecules are linked into a linear chain by intermolecular O—H?O hydrogen bonds [O?O 2.646 (3) Å].     

trans‐Bis­[N‐(2‐hydroxy­ethyl)­ethyl­ene­di­amine‐κ2N,N′]­bis­(iso­thio­cyanato‐κN)­nickel(II)

The crystal structure of the title compound, [Ni(NCS)₂(C₄H₁₂N₂O)₂], has two crystallographically independent half‐mol­ecules in the asymmetric unit, with each Ni atom residing on a centre of symmetry. The two mol­ecules exhibit similar coordination geometry but display differences with regard to other structural features. Each Ni^II centre is octahedrally coordinated by two mutually trans chelating hydroxy­ethyl­ethyl­ene­di­amine ligands and two mutually trans iso­thio­cyanate ions. The two independent mol­ecules form chains through different types of non‐covalent interactions. In the case of one of the mol­ecules, only NCS and free OH groups participate in hydrogen bonding, while in the chain based on the second mol­ecule, the NCS, NH, NH₂ and free OH groups are involved in intermolecular hydrogen bonding. The two chains interact with one another through hydrogen bonding, forming planar sheets. The third packing direction is mediated only by van der Waals interactions.     

catena‐Poly­[[[bis(N,N′‐di­phenyl­thio­urea)­cadmium(II)]‐di‐μ‐thio­cyanato] dihydrate]

Bridging by the two thio­cyanato groups in centrosymmetric six‐coordinate bis­(thio­cyanato)­bis­(di­phenyl­thio­urea)­cad­mium(II) dihydrate leads tothe formation of eight‐membered [Cd—SCN→Cd—SCN→] rings that are linked at the metal atom to furnish chains running parallel to the a axis, i.e {[Cd(NCS)₂(C₁₃H₁₂N₂S)₂]·2H₂O}_n.     

[Di‐2‐pyridyl ketone N4,N4‐(butane‐1,4‐di­yl)­thio­semi­carbazonato‐κ3N,N′,S]­di­oxo­vanadium(V)

The V^V atom in the title complex, [V(C₁₆H₁₆N₅S)O₂], is five‐coordinate in a highly distorted square‐pyramidal geometry, with the pyridyl N, the azomethine N and the thiol­ate S atoms of the di‐2‐pyridyl ketone N⁴,N⁴‐(butane‐1,4‐di­yl)­thio­semi­carbazone ligand and one oxo ligand occupying the basal coordination positions, while the second oxo ligand occupies the apical position. The mol­ecules are inter­connected by weak inter­molecular inter­actions, mainly of the C—H⋯O type, involving the oxo atoms.     

Chlorido[N,N′‐dibenzyl‐N′′‐(trichloroacetyl)phosphoramidato‐κ2O,O′](1,10‐phenanthroline‐κ2N,N′)copper(II)

In the title complex, [Cu(C₁₆H₁₆Cl₃N₃O₂P)Cl(C₁₂H₈N₂)], the Cu^II cation presents a square‐pyramidal environment, where the CuO₂N₂ base is formed by two O atoms from carbonyl and phosphoryl groups, and by two N atoms from a 1,10‐phenanthroline molecule. A coordinated Cl atom occupies the apex. N—H...Cl hydrogen bonds link the molecules into one‐dimensional chains. The trichloromethyl group is rotationally disordered over two positions, with occupancies of 0.747 (7) and 0.253 (7).     

Intermolecular contacts in the crystal packing of 2,2′‐(N,N′‐oxalyldiimino)­bis(3‐phenyl­propanamide) di­methyl sulfoxide solvate

In the title compound, C₂₀H₂₂N₄O₄·C₂H₆OS, two distinct hydrogen‐bond systems connect oxal­amide groups in one pattern and primary amide groups in the other to form a two‐dimensional network perpendicular to the c axis. These hydro­philic layers are joined to the three‐dimensional structure through C—H?π interactions. The hydrogen‐bonded waved layers shape holes which are occupied by disordered di­methyl sulfoxide solvent mol­ecules.     

{2‐[(3‐Amino­propyl)­amino­propyl­imino­methyl]­imidazol­ato‐N,N′,N′′,N′′′}­(methanol‐O)­copper(II) per­chlorate

In the title compound, [Cu(C₁₀H₁₈N₅)(CH₄O)]ClO₄, four N atoms from the deprotonated ligand derived from bis(3‐amino­propyl)­amine and 2‐imidazole­carbox­aldehyde are coordinated to the Cu atom. The four N atoms occupy equatorial positions with Cu—N bond distances ranging from 1.998 (2) to 2.046 (3) Å. The methanol O atom occupies one axial position with a Cu—O bond distance of 2.295 (2) Å.     

Tetragonal polymorphic modification of tetrakis­(N,N‐diethyl­di­thio­carbam­ato‐S,S′)­tellurium(IV)

During an investigation of the W/Te/Br₂ system, we prepared crystals of the title compound, C₂₀H₄₀N₄S₈Te, from aceto­nitrile solution by slow addition of diethyl ether. It appeared to be a new tetragonal modification. The calculated density of the tetragonal modification (1.513 Mg m^?3) is slightly greater than found for the known orthorhombic modification (1.46 Mg m^?3). The bond distances and angles are practically the same.     

Ammonium di­chloro­bis­(di­methyl­glyoximato‐N,N′)­iridate(III)

In the title compound, (NH₄)[IrCl₂(C₄H₇N₂O₂)₂], (I), the Ir atom is octahedrally coordinated by two trans Cl^? and two di­methyl­glyoximate chelate ligands in the equatorial plane. A two‐dimensional hydrogen‐bond network between ammonium cations NH₄⁺ and anionic [IrCl₂(C₄H₇N₂O₂)₂]^? complexes is extended along the bc plane.     

N,N′,N′′‐Tris(p‐methoxy­phenyl)­phospho­ric triamide

The title compound, C₂₁H₂₄N₃O₄P, is a self‐complementary hydrogen‐bond (HB) building unit, with (P=)O as the primary HB acceptor and N—H as the HB donor. Each of the four crystallographically distinct and nearly parallel mol­ecules of the unit cell has a net dipole moment along the P=O bond direction and all of the dipoles are directed in the same general crystallographic direction. Head‐to‐tail N—H⋯O=P double‐HB strands stack adjacent mol­ecules into one‐dimensional infinite polar columns. Each polar column is a 2₁ helix and all columns are essentially parallel, resulting in polar order throughout the entire crystal.