Bromo­di­methyl(N‐methyl­pyrrolidin‐2‐one‐O)­tin(IV)‐di‐μ‐bromo‐bromo­di­methyl­tin(IV)

The preparation and X‐ray analysis of the title compound, [Sn₂Br₄(CH₃)₄(C₅H₉NO)], are described. The compound contains two Sn atoms in the asymmetric unit, that complexed by N‐methyl­pyrrolidin‐2‐one being hexacoordinated (a), the other exhibiting pentacoordination (b). The most important features are three different Sn—Br bond lengths at both Sn atoms with the following values: (a) 2.5060 (9), 2.7152 (10) and 3.7118 (10) Å; (b) 2.5084 (10), 2.5279 (9) and 3.5841 (10) Å.     

Bis­[N,N′‐diiso­propyl‐N‐(tri­methyl­silyl)­benzamidinium] di‐μ‐chloro‐bis­[tetra­chloro­zirconate(IV)] di­chloro­methane disolvate

The structure of the salt of the di‐μ‐chloro‐bis­[tetra­chloro­zirconate(IV)] anion and the N,N′‐iso­propyl‐N‐(tri­methyl­silyl)benzamidinium cation, (C₁₆H₂₉N₂Si)₂[Zr₂Cl₁₀]·2CH₂Cl₂, is reported. The anion lies about an inversion centre and shows a substantially octahedral coordination around Zr, while the structure of the cation is unequivocally assigned as that of a benzamidinium ion.     

The chloro­(diethyl­amino)­di­methyl­tin dimer

The title compound, di‐μ‐diethyl­amido‐N:N‐bis­[chloro­di­methyl­tin(IV)], consists of discrete [Sn₂Cl₂(CH₃)₄(C₄H₁₀N)₂] dimer mol­ecules, with Sn atoms linked by bridging diethyl­amido groups. The coordination geometry about the metal atom is distorted trigonal bipyramidal, with the two methyl C atoms and one N atom in the equatorial plane, and the Cl and second N atom in axial positions.     

Chloro­(μ‐6‐methyl­pyridine‐2‐carboxyl­ato)bis­(6‐methyl­pyridine‐2‐carboxyl­ato)triphenyl­chromium(III)­tin(IV) chloro­triphenyl­tin(IV)

The title compound, [CrSn(C₆H₅)₃(C₇H₆NO₂)₃Cl][Sn(C₆H₅)₃Cl(CH₄O)], was obtained from the reaction of Ph₃SnCl with the complex [Cr(C₇H₆NO₂)₃] in methanol. The structure contains [Ph₃SnCl(MeOH)] (A) and [Ph₃SnClCr(C₇H₆NO₂)₃] (B) mol­ecules. In mol­ecule A, the Sn atom of Ph₃SnCl is coordinated by one methanol mol­ecule. In mol­ecule B, the Sn atom of Ph₃SnCl is coordinated by one carboxyl­ate O atom of [Cr(C₇H₆NO₂)₃]. Mol­ecules A and B are connected through an O—H⋯O hydrogen bond between a carboxyl­ate O atom and the methanol OH group. Weak C—H⋯Cl inter­actions and O—H⋯O hydrogen bonds extend the components of (I) into a two‐dimensional network.     

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].     

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.     

1‐[(4‐Chloro­benzoyl)­methyl]‐4‐(N,N‐di­methyl­amino)­pyridinium bromide sesquihydrate and 1‐[(4‐bromo­benzoyl)­methyl]‐4‐(N,N‐di­methyl­amino)­pyridinium bromide sesquihydrate

The title compounds, C₁₅H₁₆ClN₂O⁺·Br⁻·1.5H₂O and C₁₅H₁₆BrN₂O⁺·Br⁻·1.5H₂O, are isomorphous. The benzene ring is oriented nearly normal to the pyridine ring in both compounds. The molecular packing is mainly influenced by intermolecular O—H⋯O and O—H⋯Br interactions, as well as weak intramolecular C—H⋯O interactions. The H₂OBr⁻ units form an extended water–bromide chain, with a bridging water mol­ecule on a twofold axis.     

Two isomorphous complexes: di­chloro­[phthalocyaninato(2–)]­tin(IV) and di­chloro­[phthalocyaninato(2–)]­germanium(IV)

Isomorphous triclinic forms of di­chloro­[phthalocyaninato(2−)]­tin(IV), [Sn(C₃₂H₁₆N₈)Cl₂], and di­chloro­[phthalocyaninato(2−)]­ger­manium(IV), [Sn(C₃₂H₁₆N₈)Cl₂], and a monoclinic form of the latter have been obtained from the reaction of pure tin and germanium powder, respectively, with phthalo­nitrile under a stream of ICl vapour. All three crystal structures consist of centrosymmetric [SnPcCl₂] and [GePcCl₂] [Pc is phthalocyaninate(2−)] mol­ecules, which are separated but interacting. In the triclinic forms (Sn and Ge), the Pc macrocycles are not staggered but slipped, and in the monoclinic form (Ge), the mol­ecules are additionally inclined. In both cases, the central Sn or Ge atom is six‐coordinated by the four iso­indole N atoms of the Pc macrocyclic ligand and by two Cl atoms (located trans) into a tetragonal–bipyramidal structure. The arrangement of [SnPcCl₂] and [GePcCl₂] mol­ecules in the crystal structure is determined mainly by intermolecular C—H⃛Cl, π–π and van der Waals interactions.     

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.     

Bis­[4‐(di­methyl­amino)­pyridinium] hexa­chloro­stannate(IV)

In the title compound, 4‐(di­methyl­amino)­pyridine is proton­ated on the pyridine N atom. The N(CH₃)₂ moiety is twisted 4.4 (2)° from the pyridine‐ring plane. The octahedral [SnCl₆]^2? anion is hydrogen bonded via trans‐Cl atoms to pyridinium N atoms from two cations forming (C₇H₁₁N₂)₂[SnCl₆] structural units.     

Poly­[[tetra­aqua(μ7‐hydrogen di­chloro­methyl­enebis­phospho­nato)(μ5‐hydro­gen di­chloro­methyl­enebis­phosphon­ato)­tribarium(II)] monohydrate]

The title compound, {[Ba₃(CHCl₂O₆P₂)₂(H₂O)₄]·H₂O}_n or {[Ba₃(Cl₂CP₂O₆H)(H₂O)₄]·H₂O}_n, is two‐dimensional. The asymmetric unit contains three independent Ba²⁺ atoms, two chelating and bridging Cl₂CP₂O₆H³⁻ ligands and four aqua ligands, connected in layers parallel to the (100) plane. There are pores between the layers in the direction of the b axis filled with lattice water mol­ecules.     

Chloro­bis­(di­methyl­amido)(η5‐2,5‐di­methyl­pyrrolyl)­titanium(IV), [Ti(NMe2)2(DMP)Cl]

The structure of the title compound, [Ti(C₂H₆N)₂(C₆H₈N)Cl], displays a η⁵‐coordination mode for the pyrrolyl ring, confirmed by the values of the slip parameter [0.073 (9) Å] and the fold angle [4.6 (6)°]. This coordination is confirmed by NMR data, which point to the involvement of the complex in a fluxional process in solution above 285 K, passing through an intermediate involving simultaneously a metal–aza­allyl and a metal–olefin bond.     

4,4′‐(Azino­di­methyl­ene)­dipyridinium chloranilate di­chloro­methane disolvate

The di­chloro­methane disolvate of 4,4′‐(azino­di­methyl­ene)­dipyridinium chloranilate, C₁₂H₁₂N₄²⁺·C₆Cl₂O₄²⁻·2CH₂Cl₂, con­sists of one‐dimensional hydrogen‐bonded molecular tapes that propagate along the [10] direction. Both cations and anions lie across centres of inversion. The molecular tapes are planar but do not stack in the expected segregated manner, instead having chloranilate anions sandwiched between azine groups.     

[2‐(Anilino­methyl)­phenyl]­di­phenyl­phosphine and {2‐[(N‐methyl­anilino)­methyl]­phenyl}di­phenyl­phosphine

The title compounds, Ph₂PCH₂N(H)Ph or C₂₅H₂₂NP and Ph₂PCH₂N(CH₃)Ph or C₂₆H₂₄NP, respectively, are isomorphous, with calculated theoretical Tolman angles of 174 and 182°.     

3‐(4‐Chloro­benzoyl)‐7‐(N,N‐di­methyl­amino)‐1‐phenyl­indolizine and 3‐(2,4‐di­chloro­benzoyl)‐7‐(N,N‐di­methyl­amino)‐1‐phenyl­indolizine

In both of the title compounds, C₂₃H₁₉ClN₂O, (I), and C₂₃H₁₈Cl₂N₂O, (II), the molecular packing is influenced by weak intermolecular C—H⋯O and C—H⋯π interactions, but despite the chemical similarity of the compounds, the packing in (II) is entirely different from that observed in (I).     

trans‐Tetra­chloro­bis(4‐methyl­pyridine)­germanium(IV)

The structure of the title compound, [GeCl₄(C₆H₇N)₂], (I), is the first example of an addition compound of GeCl₄ with two aromatic nitro­gen bases. The mol­ecule, with essential D_2h symmetry, has crystallographic C_2h symmetry. The environment around the Ge atom can be described as a slightly distorted octahedron with the 4‐methyl­pyridine ligands occupying axial positions and the four chloro ligands in the equatorial plane. The structure of (I) is isomorphous with the corresponding silicon halides.     

Bis(μ‐hexa­methyl­enetetr­amine)­bis(aqua­di­bromo­cadmium)­di­aqua­di­bromo­cadmium dihydrate

The title compound, poly­[[di­aqua­di­bromo­cadmium‐μ‐(1,3,5,7‐tetra­aza­tri­cyclo[3.3.1.1^3,7]decane‐N¹:N⁵)‐aqua­cad­mium‐di‐μ‐bromo‐aqua­cadmium‐μ‐(1,3,5,7‐tetra­aza­tri­cyclo[3.3.1.1^3,7]decane‐N¹:N⁵)‐di‐μ‐bromo] dihydrate], [Cd₃­Br₆­(C₆­H₁₂­N₄)₂­(H₂O)₄]·­2H₂O, is made up of two‐dimensional neutral rectangular coordination layers. Each rectangular subunit is enclosed by a pair of Cd₃(μ₂‐Br)₆(H₂O)₃ fragments and a pair of (μ₂‐hmt)Cd(H₂O)₂Br₂(μ₂‐hmt) fragments as sides (hmt is hexa­methyl­enetetr­amine). The unique Cd^II atom in the Cd₂Br₂ ring in the Cd₃(μ₂‐Br)₆(H₂O)₃ fragment is in a slightly distorted octahedral CdNOBr₄ geometry, surrounded by one hmt ligand [2.433 (5) Å], one aqua ligand [2.273 (4) Å] and four Br atoms [2.6409 (11)–3.0270 (14) Å]. The Cd^II atom in the (μ₂‐hmt)Cd(H₂O)₂Br₂(μ₂‐hmt) fragment lies on an inversion center and is in a highly distorted octahedral CdN₂O₂Br₂ geometry, surrounded by two trans‐related N atoms of two hmt ligands [2.479 (5) Å], two trans‐related aqua ligands [2.294 (4) Å] and two trans‐related Br atoms [2.6755 (12) Å]. Adjacent two‐dimensional coordination sheets are connected into a three‐dimensional network by hydrogen bonds involving lattice water mol­ecules, and the aqua, bromo and hmt ligands belonging to different layers.     

cis‐Di­bromo‐trans‐di­methyl‐cis‐bis(N,N‐di­methyl­acet­amide)­tin(IV)

The synthesis and X‐ray structure analysis of the title compound, [SnBr₂(CH₃)₂(C₄H₉NO)₂], are described. The crystal contains mol­ecules which are separated by normal van der Waals distances. Organotin(IV) compounds are found in a variety of structural types, in which the Sn atom can, for example, be hexacoordinated. In this case, the preferred solid‐state molecular structure of the central atom is octahedral. The degree of distortion and the configuration depend on the ligands.     

Tetrakis­(di­methyl­amido)­vanadium(IV)

The title compound, [V(C₂H₆N)₄], (I), has non‐crystallographic D_2d molecular symmetry and contains an approximately tetrahedrally coordinated V atom with di­methyl­amido ligands. Each N atom features a nearly trigonal planar geometry. There are two independent mol­ecules of (I) in the asymmetric unit. The results are compared with those previously reported for gas‐phase electron‐diffraction studies [Haaland, Rypdal, Volden & Andersen (1992). J. Chem. Soc. DaltonTrans. pp. 891–895].     

Tris­[di­phenyl(2‐pyridyl)­phosphine]‐μ3‐iodo‐tri‐μ3‐sulfido‐sulfidotrisilvertungsten di­chloro­methane hemisolvate

The title compound, [Ag₃WIS₄(C₁₇H₁₄NP)₃]·0.5CH₂Cl₂, is a cubane‐type heterometallic cluster containing di­phenyl(2‐pyridyl)­phosphine (Ph₂PPy). The pyridyl group of Ph₂PPy remains uncoordinated, so the Ph₂PPy ligand is monodentate and coordinates to one Ag atom. The W atom and three Ag atoms form a distorted tetrahedral geometry, capped by one I atom and three S atoms.