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The title compound, trans-[RhCl(C18H12Cl3P)2(CO)]·C3H6O, contains an Rh(I) atom in a distorted square-planar coordination with a P—Rh—P angle of 175.27 (2)° and Rh—P bond lengths of 2.3127 (4) and 2.3219 (4) Å. The rhodium complexes link each other through weak intermolecular contacts between the acetone methyl groups and the carbonyl O atom. Interactions between the acetone solvent molecule and the Cl—Rh unit results in a reduced P—Rh—Cl angle of 86.675 (15)°.
doi:10.1107/S1600536810039814
PMCID: PMC3009219
PMID: 21588819
The title compound, [PtCl2(C21H33P)2]·C3H6O, crystallizes with an accompanying acetone solvent molecule. The metal atom shows a distorted square-planar coordination environment, with a P—Pt—P angle of 172.41 (3)° as the most prominent feature. Both isopropyl fragments were treated as disordered over two conformations with occupancy ratios of 0.55 (2):0.45 (2) and 0.58 (2):0.42 (2). The solvent molecule was also disordered over two orientations in a 1:1 ratio. The crystal studied was a non-merohedral twin with a twin component of 32.4%.
doi:10.1107/S1600536811051841
PMCID: PMC3254293
PMID: 22259321
In the title complex, trans-[PtCl2{P(C6H11)2(4-Me2NC6H4)}2]·2CH2Cl2, the PtII atom is located on an inversion centre, resulting in a trans-square-planar geometry. Important geometric parameters are the Pt—P and Pt—Cl bond lengths of 2.3258 (6) and 2.3106 (6) Å, respectively, and the P—Pt—Cl angles of 89.64 (2) and 90.36 (2)°. The effective cone angle for the dicyclohexyl[4-(dimethylamino)phenyl]phosphane unit was calculated to be 164°. The compound crystallizes with two dichloromethane solvent molecules; one of which is severely disordered and was treated using the SQUEEZE routine in PLATON [Spek (2009 ▶). Acta Cryst. D65, 148–155].
doi:10.1107/S1600536812048465
PMCID: PMC3588798
PMID: 23468763
In the title compound, [PtCl2(C21H21O3P)2]·2C3H6O, the asymmetric unit contains a PtII ion situated on an inversion center, one chloride anion, one tris(4-methoxylphenyl)phosphane (L) ligand and one acetone solvent molecule. The PtII ion is coordinated by two P atoms [Pt—P = 2.3196 (5) Å] from two L ligands and two chloride anions [Pt—Cl = 2.3075 (5) Å] in a distorted square-planar geometry with P—Pt—Cl angles of 88.016 (16) and 91.984 (16)°. The effective cone angle of the phosphane ligand was calculated to be 156°. Weak C—H⋯O and C—H⋯Cl hydrogen bonds hold molecules together.
doi:10.1107/S1600536812045643
PMCID: PMC3588736
PMID: 23468701
The title compound, [Rh(C5H7O2)(C18H12Cl3P)(CO)], contains the bidentate acetylacetonate ligand coordinated to the RhI atom, forming a chelate ring [Rh—O = 2.0327 (15) and 2.0613 (14) Å]. The RhI atom is additionally coordinated by one P [Rh—P = 2.2281 (6) Å] and one carbonyl C [Rh—C = 1.812 (2) Å] atom, resulting in a slightly distorted square-planar geometry. The molecules are packed to minimize steric hindrance with the phosphanes positioned above and below the slightly distorted square geometrical plane.
doi:10.1107/S1600536812012536
PMCID: PMC3343893
PMID: 22589861
The title compound, [PtCl2(C20H20P)2]·C4H8O2, crystallizes with the Pt atom in a distorted cis-square-planar geometry. The Pt—P bond lengths are 2.2490 (19) and 2.253 (2) Å, and the Pt—Cl bond lengths are 2.344 (2) and 2.3475 (18) Å. Some weak C—H⋯Cl and C—H⋯O interactions involving the solvate molecule were observed.
doi:10.1107/S1600536811035628
PMCID: PMC3201384
PMID: 22058690
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
The reaction of (η3-allyl)[(1,2,5,6-η)-cycloocta-1,5-diene]rhodium(I) with tris(2,4-di-tert-butylphenyl)phosphite in toluene produces the title compound, [Rh(C42H62O3P)(C8H12)]·C7H8, by spontaneous metallation at one of the nonsubstituted phenyl ortho-C atoms of the phosphite molecule. The coordination geometry at the RhI ion is distorted square-planar. The toluene solvent molecule is disordered over two different orientations, with site-occupation factors of 0.810 (2) and 0.190 (2).
doi:10.1107/S1600536812002851
PMCID: PMC3274931
PMID: 22346878
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
The title compound, [PdCl2(C21H33P)2], forms a monomeric complex with a trans-square-planar coordination geometry about the PdII atom which lies on an inversion centre. The Pd—P bond lengths are 2.3760 (13) Å, while the Pd—Cl bond lengths are 2.3172 (14) Å. The observed structure was found to be closely related to that of trans-dichloridobis[dicyclohexyl(phenyl)phosphane-κP]palladium(II), [PdCl2{P(C6H11)2(C6H5)}2] [Burgoyne et al. (2012 ▶). Acta Cryst. E68, m404].
doi:10.1107/S1600536812040810
PMCID: PMC3515096
PMID: 23284323
In the title compound, [PtCl2(C18H15P)2]·CHCl3, each PtII centre adopts a nearly square-planar coordination geometry formed by two P atoms [Pt—P = 2.2481 (17) and 2.2658 (19) Å] and two Cl anions [Pt—Cl = 2.3244 (19) and 2.3548 (17) Å]. The Cl atoms of the chloroform solvent molecule are disordered over two orientations in a 0.778 (11):0.222 (11) ratio. The crystal packing is stabilized by weak intermolecular C—H⋯Cl hydrogen bonds, exhibiting voids with a volume of 215 Å3.
doi:10.1107/S1600536809029961
PMCID: PMC2970157
PMID: 21577392
In the title compound, [PdCl2(C15H11NO3)2]·CHCl3, the PdII atom adopts a slightly distorted square-planar coordination geometry composed of two Cl atoms in cis positions and two C atoms from isocyanophenyl ligands. The molecular conformation is stabilized by π–π stacking interactions [shortest centroid–centroid distance = 3.600 (1) Å] between substituted benzene rings of different ligands. The crystal packing is characterized by C—H⋯O and C—H⋯Cl interactions involving the chloroform solvent molecules.
doi:10.1107/S1600536812045801
PMCID: PMC3588737
PMID: 23468702
The absolute configuration of the title molecule, [Fe(C5H5)(C38H34NP2)]·CHCl3, is R,R
p. The molecular structure is similar to the structure of the solvent-free compound [Fukuzawa, Yamamoto & Kikuchi (2007 ▶). J. Org. Chem. 72, 1514–1517], but some torsion angles about the P—Cphenyl bonds differ by up to 25°. The P atoms and the N atom have a distorted trigonal-pyramidal geometry. The chloroform solvate group donates a C—H⋯π bond to the central benzene ring and is also involved in six intermolecular C—H⋯Cl contacts with H⋯Cl distances between 2.96 and 3.13 Å.
doi:10.1107/S160053680803955X
PMCID: PMC2959829
PMID: 21581228
Both the platininum complex and the solvent molecule of the title compound, [PtBr2(C18H15P)2]·CHCl3, are located on a twofold rotation axis. The CH unit and the Cl atoms of the CHCl3 molecule are disordered over two equally occupied positions. The complex shows a trans square-planar geometry about the Pt atom.
doi:10.1107/S1600536811016849
PMCID: PMC3120480
PMID: 21754620
The asymmetric unit of the title triangulo-triruthenium compound, [Ru3(C21H21AsO3)(C26H24P2)(CO)9]·CHCl3, consists of one molecule of the triangulo-triruthenium complex and one chloroform solvent molecule. The bis(diphenylphosphanyl)ethane ligand bridges an Ru—Ru bond and the monodentate arsane ligand bonds to the third Ru atom. Both the arsane and phosphine ligands are equatorial with respect to the Ru3 triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three arsane-substituted benzene rings make dihedral angles of 52.72 (19), 63.03 (19) and 88.19 (19)° with each other. The dihedral angles between the two benzene rings are 85.8 (2) and 89.2 (2)° for the two diphenylphosphanyl groups. In the crystal, molecules are linked together into a three-dimensional network via intermolecular C—H⋯O hydrogen bonds. Weak intermolecular C—H⋯π interactions further stabilize the crystal structure.
doi:10.1107/S160053681100047X
PMCID: PMC3051462
PMID: 21522851
The title compound, [Fe(NO)2(C18H12F3P)2]·CHCl3, belongs to the family of metal dinitrosyl compounds with the general formula Fe(NO)2(L)x, referred to collectively as ‘dinitrosyl iron compounds’ (DNICs). Herein we report the structure of a dinitrosyl iron diphosphane complex, (Fe(NO)2
L
2, with L = P(C6H4-p-F)3. The structure includes one metal complex molecule and one chloroform solvent molecule. The iron atom is tetrahedrally coordinated with two phosphane ligands and with two NO groups with Fe—N—O angles of 178.1 (2) and 177.0 (2)°.
doi:10.1107/S1600536811004673
PMCID: PMC3051982
PMID: 21522263
In the title compound, [Pd(CH3)(C26H14F18NOP)(C2H3N)][SbF6]·0.5CH2Cl2, the Pd2+ cation has a distorted square-planar environment, being coordinated by the acetonitrile [Pd—N = 2.078 (8) Å] and methyl [Pd—C = 2.052 (9) Å] groups and the bidentate ligand 2-(1-{bis[2,4,6-tris(trifluoromethyl)phenyl]phosphanyloxy}-1-methylethyl)pyridine (L). In L, one –CF3 group is rotationally disordered between two orientations in a 1:1 ratio. The solvent molecule was treated as disordered between two positions related by an inversion center with occupancies fixed at 0.5. The crystal packing exhibits weak intermolecular C—H⋯F contacts.
doi:10.1107/S1600536811005277
PMCID: PMC3051981
PMID: 21522289
The asymmetric unit of the title triangulo-triruthenium compound, 2[Ru3(C25H22As2)(C18H12Cl3P)(CO)9]·CHCl3, consists of two molecules (A and B) of the triangulo-triruthenium complex and one molecule of chloroform solvent. The bis(diphenylarsino)methane ligand bridges an Ru—Ru bond and the monodentate phosphine ligand bonds to the third Ru atom. Both the phosphine and arsine 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 phosphine-substituted benzene rings make dihedral angles of 73.5 (3), 57.2 (3) and 75.7 (3)° with each other in molecule A, while these angles are 60.7 (3), 86.8 (3) and 54.9 (3)° in molecule B. The dihedral angles between the two benzene rings are 87.3 (3) and 89.6 (3)° for the two diphenylarsino groups in molecule A and 85.6 (3) and 87.7 (3)° in molecule B. In the crystal packing, the molecules are linked into a three-dimensional framework via intermolecular C—H⋯O and C—H⋯Cl hydrogen bonds. Weak intermolecular C—H⋯π interactions furture stabilize the crystal structure. The crystal studied was an inversion twin, the refined ratio of twin components being 0.480 (7):0.520 (7).
doi:10.1107/S1600536809053884
PMCID: PMC2980153
PMID: 21579981
The title rhodium Vaska-type complex, trans-[RhCl{P(C6H11)2(C6H4-4-C3H7)2}2(CO)], crystallizes with an accompanying acetone solvent molecule. The metal atom shows a distorted square-planar coordination environment with selected important geometrical parameters of Rh—P = 2.3237 (6) and 2.3253 (6) Å, Rh—Cl = 2.3724 (6) Å, Rh—C = 1.802 (2) Å, P—Rh—P = 173.42 (2)° and Cl—Rh—C = 179.13 (7)°. Effective cone angles for the two P atoms are 165 and 161°, respectively. Both isopropyl groups and the acetone molecule are disordered with occupancy values of 0.523 (5):0.477 (5), 0.554 (8):0.446 (8) and 0.735 (4):0.265 (4), respectively. The crystal packing is stabilized by weak C—H⋯O and C—H⋯Cl contacts.
doi:10.1107/S1600536811033447
PMCID: PMC3200912
PMID: 22058880
The thiopyran unit of the title molecule, C17H15ClO2S, is in chair form. A crystallographic mirror plane bisects the molecule, passing through the O=S and the opposite C=O atoms of the central ring, with statistical disorder of the Cl atom. The geometry around the S atom is tetrahedral and the carbonyl C is planar. The 4-chlorophenyl group at the 2 position and the phenyl ring at the 6 position have equatorial orientations. Intermolecular C—H⋯O and C—H⋯Cl hydrogen bonds are found in the crystal structure. In addition, there is a short O⋯C intermolecular contact [2.970 (5) Å].
doi:10.1107/S1600536808037355
PMCID: PMC2959857
PMID: 21581339
The title compound, [PtCl(C42H78OP4)]Cl·0.5CH2Cl2·4H2O, crystallizes as a contact ion-pair with two close intermolecular C—H⋯Cl− contacts between CH acidic αH atoms of the phosphane ligand and the chloride anion. A chloride ligand together with three coordinating P ligand atoms create a slightly distorted square-planar coordination environment around the PtII center. An intermolecular water O—H⋯Cl− and water O—H⋯OP hydrogen-bond network completes the coordination around the anion. In addition, a disordered CH2Cl2 solvent molecule cocrystallized within a hydrophobic cavity spanned by the dicyclohexylphosphane ligands.
doi:10.1107/S1600536808041615
PMCID: PMC2967900
PMID: 21581527
The title compound, [PdCl2{P(C6H11)2(C6H5)}2], forms a monomeric complex with a trans-square-planar geometry. The Pd—P bond lengths are 2.3343 (5) Å, as the Pd atom lies on an inversion centre, while the Pd—Cl bond lengths are 2.3017 (4) Å. The observed structure was found to be closely related to [PdCl2{P(C6H11)3}2] [Grushin et al. (1994 ▶). Inorg. Chem.
33, 4804–4806], [PdBr2{P(C6H11)3}2] [Clarke et al. (2003 ▶). Dalton Trans. pp. 4393–4394] and [PdCl2P(C6H11)2(C7H7)}2] [Vuoti et al. (2008 ▶). Eur. J. Inorg. Chem. pp. 397–407] (C6H11 is cyclohexyl and C7H7 is o-tolyl). One of the cyclohexyl rings is disordered with the phenyl ring in a 0.587 (9):413 (9) ratio. Five long-range C—H⋯Cl interactions were observed within the structure.
doi:10.1107/S1600536812010100
PMCID: PMC3343813
PMID: 22589787
The title compound, trans-[PdCl2(C16H13PS)2], forms a monomeric complex with a trans-square-planar geometry. The Pd—P bond lengths are 2.3387 (11) Å, as the Pd atom lies on an inversion point, while the Pd—Cl bond lengths are 2.2950 (12) Å.
doi:10.1107/S160053681201478X
PMCID: PMC3344332
PMID: 22590098
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 CuII atom of the title complex, [Cu(C16H12ClNO3)(C3H4N2)]·H2O, has a distorted square-planar coordination geometry formed by a tridentate Schiff base dianion and an imidazole ligand. The imidazole is nearly coplanar with the coordination plane, the dihedral angle between the planes being 3.73 (12)°. In the Schiff base ligand, the two benzene rings are oriented at a dihedral angle of 75.87 (12)°. O—H⋯O and N—H⋯O hydrogen bonding is present in the crystal structure. One H atom of the uncoordinated water molecule is disordered equally over two sites.
doi:10.1107/S1600536810014765
PMCID: PMC2979152
PMID: 21579059