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The RuII atom in the title compound, [RuCl2(C31H29N2P)(CO)2]·CH2Cl2, exhibits a distorted octahedral coordination environment. The bond angles of the cis substituents at the RuII atom range from 82.72 (9) to 97.20 (3)°. This molecule is of interest in the field of catalytic transfer hydrogenation.
doi:10.1107/S1600536812032515
PMCID: PMC3414164
PMID: 22904771
The title compound, [FeRu(C5H5)(C2N3)(C17H14P)2], was obtained by reaction of Cp(dppf)RuCl [dppf = 1,1′-bis(diphenylphosphanyl)ferrocene] with sodium dicyanamide in dichloromethane. The RuII atom is capped by an η5-cyclopentadienyl (Cp) ring, a chelating dppf and a terminal C2N3 unit, giving three-legged piano-stool geometry. The C—N—C angle of the N(CN)2 ligand [120.8 (6)°] is significantly smaller than that in the corresponding diruthenium complex [127.2 (9)°; Zhang et al. (2003 ▶). Inorg. Chem.
42, 633–640] due to steric hindrance between the two {Cp(PPh3)2Ru} building blocks. Disorder was found in the dichloromethane solvent molecule, which was refined as disordered over two positions, with a site-occupancy ratio of 0.53:0.47 (2).
doi:10.1107/S1600536812014274
PMCID: PMC3344313
PMID: 22590079
The asymmetric unit of the title triangulo-triruthenium compound, 2[Ru3(C25H22P2)(C19H17PS)(CO)9]·CH2Cl2, contains one triangulo-triruthenium complex molecule and one half-molecule of the dichloromethane solvent. The dichloromethane solvent molecule lies across a crystallographic inversion center leading to the molecule being disordered over two positions of equal occupancy. The bis(diphenylphosphanyl)methane ligand bridges an Ru—Ru bond and the monodentate phosphane ligand bonds to the third Ru atom. All phosphane ligands are equatorial with respect to the Ru3 triangle. In addition, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three phosphane-substituted benzene rings make dihedral angles of 87.18 (11), 59.59 (10) and 89.28 (11)° with each other. The dihedral angles between the two benzene rings are 78.48 (11) and 87.58 (11)° for the two diphenylphosphanyl groups. In the crystal, the molecules are stacked along the a axis. Weak intermolecular C—H⋯π interactions stabilize the crystal structure.
doi:10.1107/S1600536811000778
PMCID: PMC3051800
PMID: 21522879
In the dimeric title compound, [Pd2Cl4{P(C8H9)3}2]·CH2Cl2, the metal complex molecule is situated about an inversion centre and is accompanied by a dichloromethane solvent molecule situated on a twofold rotation axis. The PdII atom has a slightly distorted square-planar coordination sphere. The effective cone angle for the tris(3,5-dimethylphenyl)phosphane ligand was calculated to be 169°. In the crystal, the metal complex and solvent molecules are linked via C—H⋯Cl interactions, generating chains along [10-2]. There are also C—H⋯π and weak π–π interactions present [centroid–centroid distance = 3.990 (2) Å, plane–plane distance = 3.6352 (15) Å and ring slippage = 1.644 Å], forming of a three-dimensional structure.
doi:10.1107/S1600536812048556
PMCID: PMC3588800
PMID: 23468765
In the title compound, [RuCl2(C6H14N2)(C28H28P2)]·CH2Cl2, the RuII ion is coordinated in a slightly distorted octahedral environment, formed by two cis-oriented chloride ligands, two cis P atoms of a 1,4-bis(diphenylphosphanyl)butane ligand and two cis-chelating N atoms of a bidentate cyclohexane-1,2-diamine ligand. In the crystal, pairs of molecules form inversion dimers via N—H⋯Cl hydrogen bonds. In addition, intramolecular N—H⋯Cl and weak C—H⋯Cl, C—H⋯N, N—H⋯π and C—H⋯π hydrogen bonds are observed. One of the Cl atoms of the solvent molecule is disordered over two sites with refined occupancies of 0.62 (1) and 0.38 (1).
doi:10.1107/S1600536812014080
PMCID: PMC3344316
PMID: 22590082
In the title compound, [Ag{P(C6H11)2(C6H5)}2]ClO4·CH2Cl2, the AgI atom in the mononuclear complex cation is coordinated by two P atoms of the phosphane ligands [Ag—P = 2.3993 (4) and 2.4011 (4) Å; P—Ag—P = 177.473 (18)°] and the perchlorate anion acts as the counter-anion. There is an Ag⋯Operchlorate interaction of 2.873 (2) Å, which contributes to the slightly non-linear bond angle about the AgI atom. Weak intermolecular C—H⋯O hydrogen-bonding interactions involving phenyl, cyclohexyl and dichloromethane H-atom donors and perchlorate O-atom acceptors contribute to the stabilization of the crystal structure.
doi:10.1107/S1600536811009822
PMCID: PMC3099967
PMID: 21753995
The PtII atom in the title compound, [Pt(C29H31NP2)2](PF6)2·2CH2Cl2, is coordinated by four P atoms from two bis(diphenylphosphanyl)pentylamine ligands with an average Pt—P distance of 2.300 (1) Å. The coordination around the PtII atom shows a highly distorted square-planar geometry, as evidenced by the P—Pt—P bite angles of 70.45 (3) and 70.64 (3)°. The asymmetric unit contains two hexafluoridophosphate ions, the metal complex and two dichloromethane solvent molecules. One of the chloride atoms of one of the dichloromethane molecules is disordered over two sites in a 0.515 (3):0.485 (3) ratio. C—H⋯F hydrogen bonds stabilize the crystal packing.
doi:10.1107/S1600536810025560
PMCID: PMC3007544
PMID: 21588157
The title compound, [Pd2{P(C10H7)2(C10H6)}2Cl2]·2CH2Cl2, shows cyclometalation of one naphthalen-1-yl substituent of each of the phosphane ligands to the Pd dimer in a trans orientation; the complete dimer is generated by a centre of inversion. Two dichloromethane solvent molecules create C—H⋯Cl interactions with the metal complex, generating supermolecular layers in the ab plane. Additional C—H⋯π and π–π [centroid–centroid distances = 3.713 (3), 3.850 (4) and 3.926 (3) Å] interactions join these planes into a three-dimensional supermolecular network.
doi:10.1107/S1600536812048222
PMCID: PMC3588801
PMID: 23468766
In the title compound, [Pd(CH3)Cl(C25H22NPS)]·0.5C2H2Cl2, the PdII atom is coordinated by the N,P-bidentate ligand, a methyl group and a chloride ion, generating a distorted square-planar PdCClNS coordination geometry, with the N and Cl atoms trans. The thiophene ring is equally disordered over two orientations and the dichloromethane solvent molecule is disordered about an inversion centre.
doi:10.1107/S1600536810017824
PMCID: PMC2979533
PMID: 21579327
The title complex, [RuCl2(C25H26N2)]·CH2Cl2, is best thought of as containing an octahedrally coordinated Ru center with the arene occupying three sites. Two Ru—Cl bonds and one Ru–carbene bond complete the distorted octahedron. The carbene portion of the ligand is a benzimidazole ring. This ring is connected to the C6H2(CH3)3 arene group by a CH2 bridge. This leads to a system with very little apparent strain. A dichloromethane solvent molecule completes the crystal structure. Further stabilization is accomplished via C—H⋯N and C—H⋯Cl interactions.
doi:10.1107/S160053680900350X
PMCID: PMC2968587
PMID: 21582038
In the title complex, [RhCl(C44H32OP2)]·CH3OH, the RhI ion is coordinated by a naphthyl group of a partially oxidized 2,2′-bis(diphenylphosphanyl)-1,1′-binaphthyl (BINAP) ligand in a η4 mode, one P atom of the diphenylphosphanyl group and one Cl atom. The P=O group does not interact with the RhI ion but accepts an O—H⋯O hydrogen bond from the methanol solvent molecule.
doi:10.1107/S1600536812003418
PMCID: PMC3297224
PMID: 22412414
The asymmetric unit of the title compound, [FeRuCl(C5H5)(C10H14)(C37H31P2)]PF6, contains two independent, geometrically similar RuII complexes of a chiral ferrocenyldiphosphane with piano-stool coordination through the η6-bound p-cymene ligand, two chelating phosphorus donor atoms, and an exo-oriented chloride ion. The mean bond lengths of the two Ru complexes are Ru—C = 2.276 Å, Ru—P = 2.3816 Å, and Ru—Cl = 2.3924 Å. Both chloride ligands form only intramolecular C—H⋯Cl interactions. Seven weak intermolecular C—H⋯F interactions involving mainly arene H atoms consolidate the crystal packing, which reveals an approximate c/2 pseudo-translation relating the two independent Ru complex molecules.
doi:10.1107/S1600536811036506
PMCID: PMC3201293
PMID: 22058697
In the title solvated complex, [NiCl2(C31H27NP2)]·CH2Cl2, the Ni2+ ion is coordinated by two chloride ions and two P atoms of the chelating N,N-bis(diphenylphosphanyl)benzyl ligand to generate a strongly distorted cis-NiCl2P2 square-planar geometry for the metal ion. In the crystal, the components are linked by C—H⋯Cl interactions.
doi:10.1107/S1600536811042759
PMCID: PMC3246988
PMID: 22219808
In the title compound, [CoRu(C17H14P)2ClH(C18H15P)(CO)]PF6·2CH2Cl2, the RuII atom is coordinated by three P atoms from a chelating 1,1′-bis(diphenylphosphanyl)cobaltocenium ligand and a triphenylphosphine ligand, one CO ligand, one Cl atom and one H atom in a distorted octahedral geometry. In the cobaltocenium unit, the two cyclopentadienyl rings are almost parallel, making a dihedral angle of 1.2 (3)°. The F atoms of the hexafluoridophosphate anion are disordered over two sets of sites, with an occupancy ratio of 0.849 (11):0.151 (11). Intramolecular C—H⋯Cl hydrogen bonds occur in the complex cation. The complex cations, hexafluoridophosphate anions and dichloromethane solvent molecules are linked by intermolecular C—H⋯F hydrogen bonds.
doi:10.1107/S1600536811044035
PMCID: PMC3238603
PMID: 22199494
The title compound, [Pd(C26H45S4)Cl]·CH2Cl2, crystallizes with a disordered dichloromethane solvent molecule [occupancy ratio = 0.67 (4):0.33 (4)]. Two of the tert-butyl groups are also disordered [occupancy ratios = 0.70 (5):0.30 (5) and 0.63 (4):0.37 (4)]. Although the pincer ligand offers the possibility for coordination of two different metal atoms, the present structure shows only the coordination of a single PdII atom in a typical S—C—S tridentate pincer manner. The PdII atom is in a slightly distorted square-planar environment with the two tert-butylsulfanyl groups arranged in a trans conformation and with a chloride ligand trans to the σ-bonded aromatic C atom. The structure exhibits a durene-like ligand frame, forming a dihedral angle of 13.6 (4)° with the metal coordination (Pd/S/S/Cl/C) environment. It is noteworthy that the tert-butyl groups are found in a syn arrangement, this being different to that found previously by Loeb, Shimizu & Wisner [(1998). Organometallics, 17, 2324–2327].
doi:10.1107/S1600536813003036
PMCID: PMC3588519
PMID: 23476488
The crystal structure of the title compound, [PtCl2(C25H22NPS)]·0.5CH2Cl2, was determined to establish the coordination properties of the (phosphanyl)benzylidene–methanamine ligand to platinum. In the unit cell two molecules of cis-[PtCl2(C25H22NPS)] are accompanied by a dichloromethane solvent molecule. The square-planar Pt2+ coordination sphere is slightly distorted with the bidentate ligand coordinated via the P and the amine N atoms, and the Cl atoms located cis at the two remaining coordination sites. Parts of the thiophene ring and the solvate molecule were modeled as disordered with occupancy ratios of 0.55 (2):0.45 (2) and 0.302 (10):0.198 (10), respectively. Weak C—H⋯Cl interactions stabilize the crystal packing.
doi:10.1107/S1600536811056108
PMCID: PMC3274858
PMID: 22346805
The asymmetric unit of the title complex, [Sb(C44H28N4)Cl2][Sb2Cl8]0.5·CH2Cl2, is composed of a SbV complex cation wherein the Sb atom is hexacoordinated by four N atoms of the pyrrole rings of the tetraphenylporphyrinate (TPP) ligands and two chloride ions, a half di-μ-chlorido-bis[trichloridoantimonate(III)] counter-anion and a dichloromethane solvent molecule. In the cation, the average Sb—N distance is 2.066 (2) Å, while the Sb—Cl distances are 2.3410 (11) and 2.3639 (12) Å. The central unit of the cation, SbN4C20, is far from being planar, with deviations of atoms from the least-squares plane ranging from −0.110 (4) to 0.124 (4) Å. The Sb—Cl distances in the anion, which is located about an inversion center, lie in the wide range 2.3715 (13)–2.7489 (13) Å, the longest distances being between the Sb and bridging Cl atoms. The crystal structure is stabilized by intermolecular C—H⋯Cl interactions involving the cations, the anions and the solvent molecules. The solvent molecule is disordered over two orientations in a 0.901 (13):0.099 (13) ratio.
doi:10.1107/S1600536812018351
PMCID: PMC3379064
PMID: 22719285
In the cation of the title compound, [Pd(C26H19NO3P)(C26H24P2)]CF3O3S·CH2Cl2·0.5C6H14, the PdII atom has a slightly tetrahedrally distorted square-planar coordination geometry. The PdC3P and PdC2P2 five-membered metallacycles adopt envelope and twist conformations, respectively. In the crystal, intermolecular C—H⋯O hydrogen bonds link cations and anions into a three-dimensional network. The dichloromethane solvent molecule is disordered over three orientations with a site-occupancy ratio of 0.5/0.3/0.2. The n-hexane solvent molecule has a crystallographically imposed centre of symmetry.
doi:10.1107/S1600536811008075
PMCID: PMC3099852
PMID: 21753947
In the title compound, [Pt(C30H31NP2)2](PF6)2·2CH2Cl2, the four-coordinated PtII atom, situated on an inversion centre, exhibits a highly distorted square-planar geometry illustrated by the P—Pt—P bite angle of 70.76 (3)°. The cyclohexyl ring and one of the phenyl rings display 0.630 (7):0.37 (7) and 0.60 (2):0.40 (2) positional disorder, respectively. The dichloromethane solvent molecule displays 0.526 (4):0.474 (4) positional disorder. C—H⋯F hydrogen bonds stabilize the crystal packing.
doi:10.1107/S1600536810028795
PMCID: PMC3007244
PMID: 21588214
In the title complex, [CdFe(C17H14P)2Cl2]·2CH2Cl2, the CdII atom has a distorted tetrahedral coordination geometry by two chloride anions and two P atoms of 1,1′-bis(diphenylphosphanyl)ferrocene. In the crystal, complex molecules are linked into a three-dimensional network by C—H⋯Cl hydrogen bonds involving the dichloromethane solvent molecules.
doi:10.1107/S1600536810046635
PMCID: PMC3011616
PMID: 21589270
Facile ligand substitution is observed when the ruthenium chloride complex [Ru(η5-C9H7)Cl(PPh3)2] is treated with 1,4-bis(diphenylphosphanyl)butane in refluxing toluene yielding the title compound, [Ru(C9H7)Cl(C28H28P2)]. The RuII atom has a typical piano-stool coordination, defined by the indenyl ligand, one Cl atom and two phosphanyl P atoms. The Ru—P bond lengths are 2.2502 (9) and 2.2968 (8) Å.
doi:10.1107/S1600536811015121
PMCID: PMC3089106
PMID: 21754349
In the title compound, [Pd(C7H7O2S)Cl(C44H32P2)]·3CH2Cl2·H2O, the geometry around the metal atom is distorted square planar, with a twist angle between the P—Pd—P and S—Pd—Cl planes of 28.11 (2)°. The two Pd—P bond lengths differ by about 0.04 Å and the biphosphane bite angle is slightly obtuse [92.92 (2)°]. There are three dichloromethane and one water molecule co-crystallized with the palladium molecule, all with atoms in general positions. Alternating water and palladium molecules form four-membered cyclic units through O—H⋯Cl and O—H⋯O hydrogen bonding. One of the dichloromethane solvent molecules is disordered over two positions in a 0.55:0.45 ratio.
doi:10.1107/S1600536811049889
PMCID: PMC3238729
PMID: 22199606
The title compound, [PdCl2(C21H12F9P)2]·CH2Cl2, crystallizes with two independent complex molecules (each having the PdII atom situated on an inversion centre) and a dichloromethane molecule in the asymmetric unit. The independent PdII atoms are in perfectly linear orientations of the ligands in mutually trans positions, but distortions of the Cl—Pd—P angles ranging from 86.151 (19) to 93.849 (19)° are evident. The effective cone angles for the tris[4-(trifluoromethyl)phenyl]phosphane ligand were calculated to be 159 and 161°. In the crystal, weak C—H⋯Cl/F interactions create a three-dimensional supramolecular network. Loose packing at two of the –CF3 groups resulted in large thermal vibrations which were treated as two-component disorders [occupancy ratios 0.50:0.50 and 0.628 (15):0.372 (15)].
doi:10.1107/S1600536812046971
PMCID: PMC3588757
PMID: 23468722
In the title compound, [Pt(NO3)2(C42H42O2P4)2]·4CH3OH, the Pt atom positioned on a crystallographic centre of inversion. The two symmetry-equivalent nitrate anions are weakly coordinated to the PtII ion, creating, together with four P ligand atoms, a distorted octahedral coordination environment. In addition, several close C—H⋯O contacts between the nitrate O atoms and phenyl H atoms are found. Hydrogen bonds from two methanol solvent molecules to one of the O—P groups complete the crystal structure.
doi:10.1107/S160053680801533X
PMCID: PMC2961811
PMID: 21202764
In the crystal structure of the title compound, [Cu(C18H16N6)(C36H28OP2)]PF6·0.5CH2Cl2 or [Cu(DPEPhos)(Bn-bta)]PF6·0.5CH2Cl2 {DPEPhos = bis[(diphenylphosphanyl)phenyl] ether and Bn-bta = 1,1′-dibenzyl-1H,1′H-4,4′-bi-1,2,3triazole}, the Cu atom is coordinated by two N and two P atoms of the ligands in a strongly distorted tetrahedral environment. There are two crystallographically independent complex cations present, which differ significantly in their geometrical parameters. The solvent molecule is disordered but satisfactory atomic positions could not be determined.
doi:10.1107/S1600536807066342
PMCID: PMC2915126
PMID: 21200542