trans‐Di­iodo­bis(1,3,5‐tri­aza‐7‐phosphaadamantane)­platinum(II)

The crystal structure of the title compound, trans‐[PtI₂(C₆H₁₂N₃P)₂], describes one of the few platinum(II) complexes containing two of the water‐soluble 1,3,5‐tri­aza‐7‐phosphaadamantane ligands reported to date. The complex crystallizes on an inversion centre with the most important bond lengths and angles being Pt—P 2.3128 (12) Å, Pt—I 2.6022 (6) Å, P—Pt—I 90.94 (3)° and P′—Pt—I 89.06 (3)°.     

Hydro­gen‐bonded adducts of ferrocene‐1,1′‐diyl­bis­(di­phenyl­methanol): a finite cyclic 1:1 adduct with 2,2′‐dipyridyl­amine

In ferrocene‐1,1′‐diyl­bis­(di­phenyl­methanol)–2,2′‐dipyridyl­amine (1/1), [Fe(C₁₈H₁₅O)₂]·C₁₀H₉N₃, (I), there is an intramolecular O—H?O hydrogen bond [H?O 2.03 Å, O?O 2.775 (2) Å and O—H?O 147°] in the ferrocenediol component, and the two neutral molecular components are linked by one O—H?N hydrogen bond [H?N 1.96 Å, O?N 2.755 (2) Å and O—H?N, 157°] and one N—H?O hydrogen bond [H?O 2.26 Å, N?O 3.112 (2) Å and N—H?O 164°] forming a cyclic R(8) motif. One of the pyridyl N atoms plays no part in the intermolecular hydrogen bonding, but participates in a short intramolecular C—H?N contact [H?N 2.31 Å, C?N 2.922 (2) Å and C—H?N 122°].     

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(2‐diphenylphosphinoethyl) sulfide‐κ3P,S,P′](triphenylphosphine‐κP)platinum(II) diperchlorate acetone solvate

In the title compound, [Pt(C₁₈H₁₅P)(C₂₈H₂₈P₂S)]­(ClO₄)₂·­C₃H₆O or [Pt(PPh₃)(PSP)](ClO₄)₂·CH₃COCH₃, where PSP is the potentially tridentate chelate ligand bis(2‐di­phenyl­phosphinoethyl) sulfide, all three donor groups of the PSP ligand are coordinated to the central Pt atom, with Pt—P = 2.310 (1) Å and Pt—S = 2.343 (1) Å. The fourth coordination site is occupied by the P donor of the tri­phenyl­phosphine ligand [Pt—P = 2.289 (1) Å]. The complex cation has exact mirror symmetry, with the S atom, the Pt atom and the P atom of the PPh₃ ligand in the mirror plane. The Pt atom has a distorted square‐planar coordination geometry. A π–π interaction is present between the phenyl rings of the PPh₃ ligand and the terminal –PPh₂ group of the PSP chelate.     

(E)‐2‐[2‐(1‐Naphthyl)­vinyl]‐3‐tosyl‐2,3‐di­hydro‐1,3‐benzo­thia­zole

The title compound, C₂₆H₂₁NO₂S₂, which consists of a benzo­thia­zole skeleton with α‐naphthyl­vinyl and tosyl groups at positions 2 and 3, respectively, was prepared by palladium–copper‐catalyzed heteroannulation. The E configuration of the mol­ecule about the vinyl C=C bond is established by the benzothiazole–naphthyl C—C—C—C torsion angle of 177.5 (4)°. The five‐membered heterocyclic ring adopts an envelope conformation with the Csp³ atom 0.380 (6) Å from the C₂NS plane. The two S—C [1.751 (4) and 1.838 (4) Å] and two N—C [1.426 (5) and 1.482 (5) Å] bond lengths in the thia­zole ring differ significantly.     

Two bis­(ammonium) 1,5‐naphthalene­disulfonate salts

The title compounds, bis­(ammonium) naphthalene‐1,5‐di­sul­fon­ate, 2NH₄⁺·C₁₀H₆O₆S₂²⁻, and bis­[1‐(hydroxy­methyl)‐3,5,7‐tri­aza‐1‐azoniatri­cyclo­[3.3.1.1^3,7]­decane] 1,5‐naphthalene­di­sul­fon­ate, 2C₇H₁₅N₄O⁺·C₁₀H₆O₆S₂²⁻, were prepared from the acid‐promoted reaction of hexa­methyl­enetetr­amine. In both structures, the di­sulfonate anion is positioned on an inversion center, with each sulfonate group contributing to the supramolecular assemblies via hydrogen bonds. The ammonium cations are linked to sulfonate groups by four distinct N⁺—H⃛⁻O—S contacts [N⃛O = 2.846 (2)–2.898 (2) Å and N—H⃛O = 160 (2)–175 (2)°], whereas the 1‐(hydroxy­methyl)‐3,5,7‐tri­aza‐1‐azoniatri­cyclo­[3.3.1.1^3,7]­decane cations form one O—H⃛⁻O—S [O⃛O = 2.628 (2) Å and O—H⃛O = 176°] and three C—H⃛⁻O—S [C⃛O = 3.359 (2)–3.380 (2) Å and C—H⃛O = 148–155°] interactions to neighboring sulfonate groups.     

Bis­[tetrakis­(tri­phenyl­phosphine‐κP)silver(I)] di‐μ‐tri­fluoro­acetato‐κ4O:O′‐bis[bis­(tri­fluoro­acetato‐κO)stannate(IV)]

The crystal structure of the title compound, [Ag(C₁₈H₁₅P)₄]₂[Sn₂(CH₃)₄(CF₃CO₂)₆], consists of discrete tetrahedral cations and trans‐C₂SnO₄ octahedral dianions [C—Sn—C = 154.6 (2)°]. The dianion lies about a center of inversion and the two Sn atoms are linked unevenly by the carboxyl­ate unit [Sn—O = 2.291 (3) Å and SnO = 2.818 (3) Å].     

Three monoalkoxy‐substituted nido‐platinaboranes: [(PPh3)2PtB10H11‐8‐(OCH3)], [(PPh3)2PtB10H11‐8‐{OCH(CH3)2}] and [(PPh3)2PtB10H10‐9‐{OCH(CH3)2}]

Each of the title compounds, 8‐methoxy‐7,7‐bis­(tri­phenyl­phosphine‐P)‐8,9:10,11‐di‐μH‐7‐platina‐nido‐undecaborane di­chloro­methane hemisolvate, [Pt(CH₁₄B₁₀O)(C₁₈H₁₅P)₂]·0.5CH₂Cl₂, (I), 8‐isopropoxy‐7,7‐bis­(tri­phenyl­phosphine‐P)‐8,9:10,11‐di‐μH‐7‐platina‐nido‐undecaborane di­chloro­methane solvate, [Pt(C₃H₁₈B₁₀O)(C₁₈H₁₅P)₂]·CH₂Cl₂, (II), and 9‐isopropoxy‐7,7‐bis­(tri­phenyl­phosphine‐P)‐8,9:10,11‐di‐μH‐7‐platina‐nido‐undecaborane di­chloro­methane solvate, [Pt(C₃H₁₈B₁₀O)(C₁₈H₁₅P)₂]·CH₂Cl₂, (III), has an 11‐vertex nido polyhedral skeleton, with the 7‐platinum centre ligating to two exo‐polyhedral PPh₃ groups and an alkoxy‐substituted polyhedral borane ligand. Compounds (II) and (III) are isomers. The Pt—B distances are in the range 2.214 (7)–2.303 (7) Å for (I), 2.178 (16)–2.326 (16) Å for (II) and 2.205 (6)–2.327 (6) Å for (III).     

2‐Amino‐5‐nitro­thia­zole monoethanol solvate: triply‐interwoven hydrogen‐bonded sheets containing centrosymmetric R(8) and R(38) rings

2‐Amino‐5‐nitro­thia­zole crystallizes from solution in ethanol as a monosolvate, C₃H₃N₃O₂S·C₂H₆O, in which the thia­zole component has a strongly polarized molecular–electronic structure. The thia­zole mol­ecules are linked into centrosymmetric dimers by paired N—H⋯N hydrogen bonds [H⋯N = 2.09 Å, N⋯N = 2.960 (6) Å and N—H⋯N = 169°], and these dimers are linked by the ethanol mol­ecules, via a two‐centred N—H⋯O hydrogen bond [H⋯O = 1.98 Å, N⋯O = 2.838 (5) Å and N—H⋯O = 164°] and a planar asymmetric three‐centred O—H⋯(O)₂ hydrogen bond [H⋯O = 2.07 and 2.53 Å, O⋯O = 2.900 (5) and 3.188 (5) Å, O—H⋯O = 169 and 136°, and O⋯H⋯O = 55°], into sheets built from alternating (8) and (38) rings. These sheets are triply interwoven.     

[1,3‐Bis(4‐nitrophenyl)triazenido](triphenylphosphine)gold(I)

In the title complex, [Au(C₁₂H₈N₅O₄)(C₁₈H₁₅P)], the coordination geometry about the Au^I ion is linear, with one deprotonated 1,3‐bis(4‐nitro­phenyl)­triazenide ion, [O₂NC₆H₄N=N–NC₆H₄NO₂]⁻, acting as a monodentate ligand (two‐electron donor), and one neutral tri­phenyl­phosphine mol­ecule completing the metal coordination. The triazenide ligand is almost planar (r.m.s. deviation = 0.0767 Å), with the largest interplanar angle being 11.6 (7)° between the phenyl ring of one of the terminal 4‐nitro­phenyl substituents and the plane defined by the N=N—N triad. The Au—N and Au—P distances are 2.108 (5) and 2.2524 (13) Å, respectively. Pairs of mol­ecules generated by centrosymmetry are associated into a supramolecular array via intermolecular C—H⋯O inter­actions, and N⋯C and N⋯O π–π interactions.     

The seven‐membered nickelacycle [NiBr{o‐CH=C(CF3)C6H4CH2PPh2‐κ2C,P}{PPh(CH2Ph)2}]

The crystal and molecular structures of the title compound, 3‐bromo‐3‐(di­benzyl­phenyl­phospho­nio)‐2,2‐di­phenyl‐5‐trifluoromethyl‐1H‐benzo­[e][1,2]­phosphanickelepine, [NiBr(C₂₂H₁₇F₃P)(C₂₀H₁₉P)], which was obtained as the major regioisomer from insertion of HCCCF₃ into the Ni—C bond of the five‐membered phosphanickelacycle [NiBr(o‐C₆H₄CH₂PPh₂‐κ²C,P){PPh(CH₂Ph)₂}], have been determined. Principal geometric data include the Ni—X bond lengths Ni—Br 2.3343 (4) Å, Ni—P 2.1867 (7) and 2.2094 (7) Å, and Ni—C 1.882 (3) Å, and the two trans angles P—Ni—P 171.55 (3)° and Br—Ni—C 176.88 (9)°.     

4‐Iodo­anilinium 3‐nitro­phthalate(1–): tripartite sheets built from O—H...O and N—H...O hydrogen bonds

In the title compound, 4‐iodoanilinium 2‐carboxy‐6‐nitrobenzoate, C₆H₇IN⁺·C₈H₄NO₆⁻, the anions are linked by an O—H...O hydrogen bond [H...O = 1.78 Å, O...O = 2.614 (3) Å and O—H...O = 171°] into C(7) chains, and these chains are linked by two two‐centre N—H...O hydrogen bonds [H...O = 1.86 and 1.92 Å, N...O = 2.700 (3) and 2.786 (3) Å, and N—H...O = 153 and 158°] and one three‐centre N—H...(O)₂ hydrogen bond [H...O = 2.02 and 2.41 Å, N...O = 2.896 (3) and 2.789 (3) Å, N—H...O = 162 and 105°, and O...H...O = 92°], thus forming sheets con­taining R(6), R(8), R(13) and R(18) rings.     

(2S,RS)‐6‐Phenyl‐1‐(p‐tolyl­sulfinyl)­hexa‐3(E),5(E)‐dien‐2‐ol

The mol­ecule of the title compound, C₁₉H₂₀O₂S, corresponds to a chiral sulfinyldienol with two stereogenic centres, viz. the C atom susbtituted by the hydr­oxy group and the sulfinyl S atom. The mol­ecule displays a V‐shape in the solid state. The dihedral angle defined by the least‐squares planes of the aromatic rings is 72.9 (1)°. The packing pattern exhibits the following inter­molecular hydrogen bonds: one O—H⋯O [H⋯O = 1.98 Å, O⋯O = 2.785 (4) Å and O—H⋯O = 166°] and two C—H⋯O [H⋯O = 2.58 and 2.60 Å, C⋯O = 3.527 (5) and 3.347 (5) Å, and C—H⋯O = 164 and 134°]. These define a chain along b.     

Pt2II and Pt2III dimers containing a Pt2(2,2′‐bipyridine)2(μ‐N,N‐dimethyl­guanidinato)2 unit

The syntheses and crystal structures of the title Pt₂^II and Pt₂^III dimers doubly bridged with N,N‐dimethyl­guanidinate ligands, namely bis­(μ‐N,N‐dimethyl­guanidinato)bis­[(2,2′‐bipyridine)platinum(II)](Pt—Pt) bis­(hexa­fluoro­phosphate) acetonitrile disolvate, [Pt₂^II(C₃H₈N₃)₂(C₁₀H₈N₂)₂](PF₆)₂·2CH₃CN, (I), and guanidinium bis­(μ‐N,N‐dimethyl­guanidinato)bis­[(2,2′‐bipyridine)sulfatoplatinum(III)](Pt—Pt) bis­(hexa­fluoro­phosphate) nitrate hexa­hydrate, (C₃H₁₀N₃)[Pt^III₂(C₃H₈N₃)₂(SO₄)₂(C₁₀H₈N₂)₂]NO₃·6H₂O, (II), are reported. The oxidation of the Pt₂^II dimer into the Pt₂^III dimer results in a marked shortening of the Pt—Pt distance from 2.8512 (6) to 2.5656 (4) Å. The change is mainly compensated for by the change in the dihedral angle between the two Pt coordination planes upon oxidation, from 21.9 (2) to 16.9 (3)°. We attribute the relatively strong one‐dimensional stack of dimers achieved in the Pt₂^II compound in part to the strong Pt^II⋯C(bpy) associations (bpy is 2,2′‐bipyridine) in the crystal structure [Pt⋯C = 3.416 (10) and 3.361 (12) Å].     

An organopalladium(II) compound including enolate oxy­gen‐ and sp3‐carbon‐bound 1,3‐di­methyl­barbiturate ligands: (1,2‐di­amino­ethane)­bis(1,3‐di­methyl­barbiturato)­palladium(II) 5.5‐hydrate

In the title compound, [Pd(C₆H₇N₂O₃)₂(C₂H₈N₂)]·5.5H₂O, the Pd atom is coordinated by two 1,3‐di­methyl­barbiturate anions through a deprotonated tetrahedral carbon and the enolate oxy­gen. The Pd—N bond length of 2.078 (2) Åtrans to the C atom is shorter than the Pt—N distance of 2.098 (3) Å in the Pt analog.     

N‐[Bis(2,4,6‐tri­methyl­phenoxy)­phos­phinoyl]‐P,P,P‐tris(2,4,6‐tri­methyl­phenoxy)phosphazene

The title compound, C₄₅H₅₅NO₆P₂, consists of an acyclic P=N—P(O) monophosphazene chain and five bulky 2,4,6‐tri­methyl­phenoxy side groups which predominantly determine the molecular shape. Although the P—N single [1.586 (3) Å] and P=N double [1.517 (3) Å] bonds are significantly different from each other, both are substantially shorter than the ideal P—N single bond. The P—N—P angle [146.0 (2)°] corresponds to the upper limit reported for acyclic phosphazene derivatives in the literature.     

cis‐[1,2‐Bis(diisopropylphosphino‐κP)‐1,2‐dicarba‐closo‐dodecaborane]dichloroplatinum(II) dichloromethane hemisolvate

The asymmetric unit of the title complex, [PtCl₂(C₁₄H₃₈B₁₀P₂)]·0.5CH₂Cl₂ or cis‐[PtCl₂{1,2‐(PⁱPr₂)₂‐1,2‐C₂B₁₀H₁₀}]·0.5CH₂Cl₂, contains one disordered solvent mol­ecule and two mol­ecules of the complex, in which each Pt^II atom displays slightly distorted square‐planar coordination geometry. The P atoms connected to the cage C atoms are coordinated to the Pt^II atom. The Pt—P distances vary slightly [2.215 (3) and 2.235 (4) Å] and the Pt—Cl distances are equal [2.348 (3) and 2.353 (5) Å].     

7‐{Di­phenyl­[(tri­phenyl­phos­phine)­aurio]­phos­phine(1+)‐P}‐8‐methyl‐7,8‐dicarba‐nido‐undecaborate(1–) dichloro­methane hemi­solvate

The title compound, 7‐[(Ph₂P)Au(PPh₃)]‐8‐(CH₃)‐7,8‐nido‐C₂B₉H₁₀]·­0.5CH₂Cl₂ or [Au(C₁₅H₂₃B₉P)­(C₁₈H₁₅P)]·­0.5CH₂Cl₂, is the first reported gold derivative of the ligand [7‐­(Ph₂P)‐8‐(CH₃)‐7,8‐nido‐C₂B₉H₁₀]^?. It has a mono­nuclear structure with the gold centre in an essentially linear coordination [P—Au—P 174.041 (15)°]. The open C₂B₃ face contains one H atom that is strongly bonded to the central B atom and semi‐bridging to a neighbouring B atom [B—H distances 1.070 (16) and 1.45 (3) Å].     

cis,cis,cis‐(Acetato‐O,O′)­bis­[1,2‐bis­(di­phenyl­phosphino)­ethane‐P,P′]­ruthenium(II) hexa­fluoro­phosphate di­methanol solvate

In the cation of the title complex, cis,cis,cis‐[Ru(η²‐O₂CMe)(dppe)₂]PF₆·2MeOH [dppe is 1,2‐bis­(di­phenyl­phosphino)­ethane, C₂₆H₂₄P₂], the Ru atom is in a pseudo‐octahedral coordination environment with two chelating dppe ligands and one chelating acetate ligand. Intra‐phosphine and intra‐acetate bond lengths and angles are unexceptional. Deviations from idealized octahedral coordination angles at ruthenium [O—Ru—O 59.43 (8)° and P—Ru—P 103.19 (2)°] presumably derive from constraints imposed by the chelate rings. The Ru—P distances for the mutually trans P‐donor atoms [2.3785 (6) Å] are significantly longer than those for the Ru—P linkages trans to the acetate ligand [2.3074 (6) Å]. The Ru1, C1 and C2 atoms lie on a twofold axis, and atom P3 of the anion lies on an inversion centre.     

Hydro­gen‐bond networks in tris(4‐hydroxy­phenyl)­methane and its 1:1 molecular complex with 4,4′‐bi­pyridine

In tris(4‐hydroxy­phenyl)­methane (or 4,4′,4′′‐methane­triyl­tri­phenol), C₁₉H₁₆O₃, mol­ecules are connected by O—H⃛O hydrogen bonds [O⃛O = 2.662 (2) and 2.648 (2) Å] into two‐dimensional square networks that are twofold interpenetrated. In tris(4‐hydroxy­phenyl)­methane–4,4′‐bi­pyridine (1/1), C₁₉H₁₆O₃·C₁₀H₈N₂, trisphenol mol­ecules form rectangular networks via O—H⃛O [O⃛O = 2.694 (3) Å] and C—H⃛O [C⃛O = 3.384 (3) Å] hydrogen bonds. Bi­pyridine mol­ecules hydrogen bonded to phenol moieties [O⃛N = 2.622 (3) and 2.764 (3) Å] fill the voids to complete the structure.