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1.  10,16-Dichloro-6,20-dioxa-3,23-diaza­tetra­cyclo­[23.3.1.07,12.014,19]nona­cosa-1(29),7,9,11,14(19),15,17,25,27-nona­ene-4,22-dione methanol monosolvate 
In the title compound, C25H22Cl2N2O4·CH3OH, the macrocyclic mol­ecule adopts a slightly distorted C 2-symmetric conformation. The macrocyclic mol­ecules are linked via N—H⋯O hydrogen bonds between the amide groups into chains extending along the [010] direction. The methanol mol­ecules bridge these chains via N—H⋯O and O—H⋯O hydrogen bonds with the formation of a two-dimensional polymeric structure parallel to (001). The methanol mol­ecule is disordered over two positions with the occupancy ratio of 9:1. The disorder of the solvent molecule is caused by weak intermolecular C—H⋯Cl hydrogen bonding.
doi:10.1107/S1600536812007052
PMCID: PMC3297870  PMID: 22412673
2.  Discrete water clusters in tetra-μ-cyanido-tetra­cyanidobis(1,4,7-triisopropyl-1,4,7-triaza­cyclo­nona­ne)dicopper(II)dinickel(II) tetra­hydrate 
The title tetra­cyanido­nickelate–copper complex, [Cu2Ni2(CN)8(C15H33N3)2]·4H2O, was synthesized by self-assembly using potassium tetracyanidonickelate(II) and dichlorido(1,4,7-triisopropyl-1,4,7-triazacyclononane)copper(II). The asymmetric unit contains half of a complex mol­ecule and two water mol­ecules. The entire complex has -1 symmetry and contains Ni(II) in a slightly distorted square-planar and Cu(II) in a square-pyramidal coordination environment. The crystal packing shows a discrete tetra­mer water cluster. Within the cluster, the four water mol­ecules are fully coplanar and each water monomer acts both as single O—H⋯O and O—H⋯N hydrogen-bond donor and acceptor.
doi:10.1107/S1600536812024282
PMCID: PMC3393158  PMID: 22807726
3.  8,15-Dioxa-10,13-di­aza­tetra­cyclo­[14.4.0.02,7.09,14]icosa-1(16),2,4,6,9(14),10,12,17,19-nona­ene 
The asymmetric unit of the title compound, C16H10N2O2, contains one half-mol­ecule, the complete mol­ecule being generated by twofold rotation symmetry. The plane of the pyrazine ring forms a dihedral angle of 64.87 (6)° with that of the benzene ring, and the planes of the two benzene rings are inclined to one another by 54.20 (6)°. The O atom deviates from the plane of the benzene ring by 0.1549 (8) Å. There are no significant inter­molecular inter­actions in the crystal.
doi:10.1107/S1600536813011318
PMCID: PMC3648330  PMID: 23723950
4.  6,10,16,19-Tetra­oxatrispiro­[4.2.2.4.2.2]nona­deca­ne 
The asymmetric unit of the title compound, C15H24O4, contains one half-mol­ecule; a twofold rotation axis passes through the central C atom. The non-planar six- and five-membered rings adopt chair and envelope conformations, respectively. In the crystal structure, inter­molecular C—H⋯O hydrogen bonds link the mol­ecules.
doi:10.1107/S1600536808001785
PMCID: PMC2960158  PMID: 21201519
5.  [μ-N,N,N′,N′-Tetra­kis(2-pyridyl­meth­yl)butane-1,4-diamine]­bis­[diacetato­cadmium(II)] nona­hydrate 
The title dinuclear complex, [Cd2(CH3CO2)4(C28H32N6)]·9H2O, is located on a crystallographic inversion center. The unique CdII ion displays a 5 + 2 coordination. A distorted square-pyramidal geometry is formed by the dipicolyl­amine unit of the ligand via the N atoms in a meridional fashion and two O atoms of the acetate ligands with short Cd—O distances. The coordination is completed by two loosely bound O atoms of the acetate ligands. The Cd—N distances involving the pyridine N atoms differ slightly from each other and the Cd—N distance involving the tertiary N atom is the longest. In the crystal structure, complex mol­ecules and solvent water mol­ecules are connected into a three-dimensional network via inter­molecular O—H⋯O hydrogen bonds. One of the water mol­ecules lies on a twofold rotation axis.
doi:10.1107/S1600536810034550
PMCID: PMC2983136  PMID: 21587357
6.  Bis{[μ-bis­(diphenyl­phosphan­yl)methane-1:2κ2 P:P′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-[(4-methyl­sulfanylphen­yl)diphenyl­phosphane-3κP]-triangulo-triruthen­ium(0)} dichloro­methane monosolvate 
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
7.  [μ-Bis(diphenyl­arsino)methane-1:2κ2 As:As’]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-(triphenyl phosphite-3κP)-triangulo-triruthenium(0) 
The asymmetric unit of the title triangulo-triruthenium compound, [Ru3(C25H22As2)(C18H15O3P)(CO)9], contains two crystallographically independent but similar mol­ecules. The bis­(diphenyl­arsino)methane ligand bridges an Ru—Ru bond and the monodentate phosphite ligand bonds to the third Ru atom. Both the phosphite 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. One of the triphenyl­phosphite benzene rings in one of the mol­ecules is disordered over two positions with refined site occupancies of 0.60 (3) and 0.40 (3). In the crystal packing, the mol­ecules are stacked along a axis. Intra­molecular C—H⋯O hydrogen bonds stabilize the mol­ecular structure and weak inter­molecular C—H⋯π inter­actions further stabilize the crystal structure. The crystal studied was a non-merohedral twin, the refined ratio of the twin components being 0.618 (1):0.382 (1).
doi:10.1107/S1600536810001200
PMCID: PMC2979706  PMID: 21579683
8.  [μ-Bis(diphenyl­arsino)methane-1:2κ2 As:As′][bis­(4-methoxy­phen­yl)phenyl­phosphine-3κP]-nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-triangulo-tri­ruthenium(0) dichloro­methane 0.15-solvate 
The asymmetric unit of the title triangulo-triruthenium compound, [Ru3(C25H22As2)(C20H19O2P)(CO)9]·0.15CH2Cl2, contains one mol­ecule of the triangulo-triruthenium complex and one partially occupied dichloro­methane solvent mol­ecule. The dichloro­methane solvent lies across a crystallographic inversion center leading to the mol­ecule being disordered over two positions of equal occupancy. The bis­(diphenyl­arsino)methane ligand bridges an Ru—Ru bond and the monodentate arsine ligand bonds to the third Ru atom. Both the 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 phospho­rus-bound benzene rings make dihedral angles of 72.7 (3), 80.9 (3) and 70.8 (2)° with each other. The dihedral angles between the two benzene rings are 79.9 (3) and 81.5 (2)° for the two diphenyl­arsino groups.
doi:10.1107/S1600536810001194
PMCID: PMC2979782  PMID: 21579684
9.  Bis{[μ-bis­(diphenyl­phosphino)methane-1:2κ2 P:P′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-[tris­(4-methoxy­phen­yl)arsine-3κAs]-triangulo-triruthenium(0)} dichloro­methane solvate 
The asymmetric unit of the title triangulo-triruthenium compound, 2[Ru3(C21H21AsO3)(C25H22P2)(CO)9]·CH2Cl2, contains one triangulo-triruthenium complex mol­ecule and one half-mol­ecule of the dichloro­methane solvent. The dichloro­methane solvent lies across a crystallographic inversion center leading to the mol­ecule being disordered over two positions of equal occupancy. The bis­(diphenyl­phosphino)methane ligand bridges an Ru—Ru bond and the monodentate arsine ligand bonds to the third Ru atom. Both the arsine and phosphine 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 arsine-substituted benzene rings make dihedral angles of 82.00 (6), 76.67 (7) and 66.09 (6)° with each other. The dihedral angles between the two benzene rings are 80.12 (8) and 78.34 (7)° for the two diphenyl­phosphino groups. In the crystal packing, the mol­ecules are linked together into chains down the b axis via inter­molecular C—H⋯O hydrogen bonds. An inter­molecular C—H⋯O hydrogen bond and weak inter­molecular C—H⋯π inter­actions further stabilize the crystal structure.
doi:10.1107/S1600536809052088
PMCID: PMC2980253  PMID: 21579930
10.  Bis([μ-bis­(diphenyl­arsino)methane-1:2κ2 As:As’]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-{tris­[4-(methyl­sulfan­yl)phen­yl]arsine-3κAs}-triangulo-triruthenium(0)) dichloro­methane monosolvate 
The asymmetric unit of the title triangulo-triruthenium compound, 2[Ru3(C25H22As2)(C21H21AsS3)(CO)9]·CH2Cl2, consists of one triangulo-triruthenium complex mol­ecule and one half of a dichloro­methane mol­ecule which lies across a crystallographic inversion center, leading to the disorder of this mol­ecule over two positions of equal occupancy. The bis­(diphenyl­arsino)methane ligand bridges an Ru—Ru bond and the monodentate arsine ligand bonds to the third Ru atom. All arsine ligands are equatorial with respect to the Ru3 triangle. Each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three methyl­sulfanyl-substituted benzene rings make dihedral angles of 70.02 (8), 82.85 (9) and 89.49 (8)° with each other. The dihedral angles between the two phenyl rings are 78.25 (9) and 86.59 (9)° for the two diphenyl­arsino groups. In the crystal, weak inter­molecular C—H⋯π inter­actions are observed.
doi:10.1107/S1600536810032812
PMCID: PMC3007838  PMID: 21588547
11.  Bis([μ-bis­(diphenyl­phosphino)methane-1:2κ2 P:P′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-{tris­[4-(methyl­sulfan­yl)phen­yl]arsine-3κAs}-triangulo-triruthenium(0)) dichloro­methane monosolvate 
The asymmetric unit of the title triangulo-triruthenium compound, 2[Ru3(C21H21AsS3)(C25H22P2)(CO)9]·CH2Cl2, consists of one triangulo-triruthenium complex mol­ecule and one half of a dichloro­methane mol­ecule which lies across a crystallographic inversion center, leading to the disorder of this mol­ecule over two positions of equal occupancy. The bis­(diphenyl­phosphino)methane ligand bridges an Ru—Ru bond and the monodentate arsine ligand bonds to the third Ru atom. Both the arsine and phosphine ligands are equatorial with respect to the Ru3 triangle. Each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three arsine-substituted benzene rings make dihedral angles of 82.69 (9), 70.43 (9) and 89.45 (9)° with each other. The dihedral angles between the two benzene rings are 85.14 (11) and 77.61 (10)° for the two diphenyl­phosphino groups. In the crystal packing, mol­ecules are linked together into dimers via inter­molecular C—H⋯O hydrogen bonds and these dimers are stacked along the a axis. Weak inter­molecular C—H⋯π inter­actions are also present.
doi:10.1107/S160053681003093X
PMCID: PMC3008007  PMID: 21588546
12.  2-[(1-{[3-(dimethylazaniumyl)propyl]methylamino}ethylidene)azaniumyl]­nona­hydro-closo-deca­borate dimethyl sulfoxide disolvate 
The title compound, 2-B10H9NH=C(CH3)N(CH3)CH2CH2CH2N(CH3)2H·2C2H6OS or C8H29B10N3·2C2H6OS, is zwitterionic with the negative charge localized on the deca­borate cage and the positive charge on the terminal ammonium group. Two mol­ecules of dimethyl sulfoxide (DMSO) and one mol­ecule of the title compound constitute the asymmetric unit. One DMSO mol­ecule is disordered [ratio 0.739 (3):0.261 (3)]. The bonds and angles within the deca­borate cage are within the normal ranges. The amidine fragment of the ligand, which is expected to be planar, is significantly distorted from planarity as exemplified by four torsion angles [B—N—C—C = 8.4 (3), H—N—C—N = 5(2), N—C—N—C = 7.3 (3) and C—C—N—C = 14.8 (3)°] found within this portion of the mol­ecule. The crystal packing consists of head-to-tail-arranged dimers of the title mol­ecule held together by four mol­ecules of DMSO which are attached via strong N—H⋯O and weak C—H⋯O hydrogen bonds.
doi:10.1107/S1600536811020186
PMCID: PMC3151893  PMID: 21837080
13.  Redetermination of hepta­potassium nona­hydrogen bis­[α-hexa­molybdoplatinate(IV)] undeca­hydrate 
Previously reported at a temperature of 298 (2) K [Lee & Joo (2007 ▶). Acta Cryst. E63, i11–i13], the title compound, K7[H9α-Pt2Mo12O48]·11H2O or K7[H4.5α-PtMo6O24]2·11H2O, was redetermined at 146 (2) K in order to determine whether the H atom in the hydrogen bond that crosses the center of symmetry was located at the center of symmetry or disordered around it as assumed in the previous study. During the present low-temperature study it was found on the center of symmetry. One water molecule shows half-occupancy.
doi:10.1107/S1600536810008639
PMCID: PMC2984051  PMID: 21580460
14.  Methyl 9-(4-meth­oxy­phen­yl)-19-methyl-3,12-di­aza­penta­cyclo­[10.7.0.02,10.03,8.013,18]nona­deca-1(19),13(18),14,16-tetra­ene-10-carboxyl­ate 
The title ester, C27H30N2O3, crystallizes with two independent mol­ecules in the asymmetric unit whose geometrical features are similar. In each mol­ecule, the pyrrolidine ring adopts an envelope conformation, with the fused C atom shared with the piperidine ring as the flap, and the piperidine ring adopts a chair conformation. In the crystal, C—H⋯π inter­actions link the inversion-related molecules and form a dimeric arrangement in the unit cell.
doi:10.1107/S1600536813010489
PMCID: PMC3648300  PMID: 23723920
15.  Bis(1-ammonio­ethane-1,1-diyl­diphos­phonato-κ2 O,O′)diaqua­cobalt(II) nona­hydrate 
In the title compound, [Co(C2H8NO6P2)2(H2O)2]·9H2O, the CoII atom has a slightly distorted octa­hedral coordination environment consisting of four deprotonated phospho­nate O atoms of two independent 1-amino­ethyl­idendiphospho­nate anions and complemented by the O atoms of two water mol­ecules in cis positions. The anions exists in the zwitterionic form (protonated amino group and two deprotonated phospho­nate O atoms) and constitute two six-membered chelate rings. The crystal structure also contains nine partly disordered uncoordinated water mol­ecules, which create an extensive three-dimensional network of strong O—H⋯O and N—H⋯O hydrogen bonds.
doi:10.1107/S1600536810013681
PMCID: PMC2979193  PMID: 21579029
16.  [13,27-Dichloro-3,6,9,17,20,23-hexa­azatetracyclo­[23.3.1.111,15.02,6]triaconta-1(29),9,11,13,15(30),16,23,25,27-nona­ene-29,30-diol-κ5 N 17,N 20,N 23,O 29,O 30]bis­(nitrato-κ2 O,O′)europium(III) nitrate methanol hemisolvate 
The title compound, [EuIII(NO3)2(C24H28Cl2N6O2)]NO3·0.5CH3OH, is isostructural with the GdIII and HoIII complexes of the analogous macrocyclic ligand, with both Cl atoms replaced by methyl groups. The Eu atom exhibits a nine-coordinate distorted tricapped trigonal-prismatic coordination geometry. The methanol solvent mol­ecule is disordered about a twofold rotation axis with occupancies of 0.543 (12):0.457 (12).
doi:10.1107/S1600536809013440
PMCID: PMC2969572  PMID: 21582985
17.  Ethyl 23-benzyl-8,11,14-trioxa-23,28,29-triaza­penta­cyclo­[19.7.1.02,7.015,20.022,27]nona­cosa-2,4,6,15(20),16,18,21,26-octa­ene-26-carboxyl­ate 
The title compound, C33H35N3O5, is the product of the multicomponent condensation of 1-benzyl-4-eth­oxy­carbonyl­piperidin-3-one with 1,5-bis­(2-formyl­phen­oxy)-3-oxapentane and ammonium acetate. The mol­ecule comprises a penta­cyclic system containing the aza-14-crown-4-ether macrocycle, tetra­hydro­pyrimidine, tetra­hydro­pyridine and two benzene rings. The aza-14-crown-4-ether ring adopts a bowl conformation with a dihedral angle of 62.37 (5)° between the benzene rings. The tetra­hydro­pyrimidine ring has an envelope conformation with the chiral C atom as the flap, whereas the tetra­hydro­pyridine ring adopts a distorted chair conformation. Two amino groups are involved in intra­molecular N—H⋯O hydrogen bonds. In the crystal, weak C—H⋯O hydrogen bonds link the mol­ecules into layers parallel to the ab plane.
doi:10.1107/S1600536813007241
PMCID: PMC3629615  PMID: 23634102
18.  [μ-Bis(diphenyl­arsino)methane-1:2κ2 As:As′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-[diphen­yl(phenyl­sulfanylmeth­yl)phosphine-3κP]-triangulo-triruthenium(0) chloro­form hemisolvate 
The asymmetric unit of the title triangulo-triruthenium cluster, [Ru3(C25H22As2)(C19H17PS)(CO)9]·0.5CHCl3, contains of one mol­ecule of the triangulo-triruthenium complex and half a mol­ecule of the disordered (two positions of equal weight) 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 arsine and phosphine ligands are equatorial with respect to the Ru3 triangle. In addition, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The benzene ring of phenyl­thio­methyl is disordered over two positions with refined site occupancies of 0.788 (11) and 0.212 (11). In the crystal packing, mol­ecules are linked into chains along b axis by inter­molecular C—H⋯O hydrogen bonds. Weak inter­molecular C—H⋯π inter­actions further stabilize the crystal structure.
doi:10.1107/S1600536810001212
PMCID: PMC2979739  PMID: 21579685
19.  Bis{[μ-bis­(diphenyl­arsino)methane-1:2κ2 As:As′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-[tris­(4-methoxy­phen­yl)arsine-3κAs]-triangulo-triruthenium(0)} dichloro­methane solvate 
The asymmetric unit of the title triangulo-triruthenium compound, 2[Ru3(C25H22As2)(C21H21AsO3)(CO)9]·CH2Cl2, contains one triangulo-triruthenium complex mol­ecule and one half of the dichloro­methane solvent. The dichloro­methane solvent lies across a crystallographic inversion center leading to the mol­ecule being disordered over two positions of equal occupancy. The bis­(diphenyl­arsino)methane ligand bridges an Ru—Ru bond and the monodentate arsine ligand bonds to the third Ru atom. Both the 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 trimethoxy­phenyl­arsino benzene rings make dihedral angles of 83.01 (8), 65.81 (8) and 76.20 (8)° with each other. The dihedral angles between the two benzene rings are 82.69 (9) and 78.83 (9)° for the two diphenyl­arsino groups. In the crystal packing, the mol­ecules are stacked along the a axis and weak inter­molecular C—H⋯π inter­actions stabilize the crystal structure.
doi:10.1107/S160053680905315X
PMCID: PMC2979775  PMID: 21579650
20.  [μ-Bis(diphenyl­arsino)methane-1:2κ2 As:As′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-[(penta­fluoro­phen­yl)diphenyl­phosphine-3κP]-triangulo-triruthenium(0) chloro­form monosolvate 
The asymmetric unit of the title triangulo-triruthenium compound, [Ru3(C25H22As2)(C18H10F5P)(CO)9]·CHCl3, contains one mol­ecule of the triangulo-triruthenium complex and one mol­ecule of the disordered 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 arsine and phosphine ligands are equatorial with respect to the Ru3 triangle. In addition, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The phosphine-substituted benzene rings make dihedral angles of 68.43 (15), 65.14 (14) and 89.75 (14)° with each other. The dihedral angles between the two benzene rings are 80.70 (15) and 84.53 (16)° for the two diphenyl­arsino groups. In the crystal packing, the mol­ecules are linked into a plane parallel to bc by inter­molecular C—H⋯O and C—H⋯F hydrogen bonds. Weak inter­molecular C—H⋯π inter­actions further stabilize the crystal structure.
doi:10.1107/S1600536809055275
PMCID: PMC2979800  PMID: 21579648
21.  [μ-Bis(diphenyl­arsino)methane-1:2κ2 As:As′][(4-bromo­phen­yl)diphenyl­phosphine-3κP]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-triangulo-tri­ruthenium(0) chloro­form 0.3-solvate 
The asymmetric unit of the title triangulo-triruthenium compound, [Ru3(C25H22As2)(C18H14BrP)(CO)9]·0.3CHCl3, contains one mol­ecule of the triangulo-triruthenium complex and one partially occupied disordered chloro­form solvent mol­ecule. The bis­(diphenyl­arsino)methane ligand bridges an Ru—Ru bond and the monodentate phosphine ligand bonds to the third Ru atom. Both the arsine and phosphine ligands are equatorial with respect to the Ru3 triangle. In addition, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The phosphine-substituted benzene rings make dihedral angles of 67.5 (3), 76.1 (3) and 78.1 (3)° with each other. The dihedral angles between the two benzene rings are 79.0 (4) and 81.4 (3)° for the two diphenyl­arsino groups. In the crystal packing, the mol­ecules are linked into chains along the a axis by inter­molecular C—H⋯O hydrogen bonds.
doi:10.1107/S1600536809055287
PMCID: PMC2979922  PMID: 21579649
22.  Bis{[μ-bis­(diphenyl­arsino)methane-1:2κ2 As:As′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-[tris­(4-chloro­phen­yl)phosphine-3κP]-triangulo-triruthenium(0)} chloro­form monosolvate 
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
23.  (Benzyl­diphenyl­phosphine-3κP)[μ-bis(diphenyl­arsino)methane-1:2κ2 As:As′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-triangulo-triruthenium(0) 
The asymmetric unit of the title triangulo-triruthenium compound, [Ru3(C25H22As2)(C19H17P)(CO)9], consists of two crystallographically independent mol­ecules of the triangulo-triruthenium complex, A and B. 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. With regard to the three phosphine-substituted rings, the benzyl ring makes dihedral angles of 41.0 (3) and 43.9 (3)° with the other two benzene rings in mol­ecule A; these angles are 49.8 (3) and 56.8 (3)° in mol­ecule B. The dihedral angles between the two benzene rings are 76.1 (3) and 88.2 (3)° for the two diphenyl­arsino groups in mol­ecule A and 71.3 (3) and 78.1 (3)° in mol­ecule B. In the crystal packing, mol­ecules are linked into chains via inter­molecular C—H⋯O hydrogen bonds. Weak inter­molecular C—H⋯π inter­actions further stabilize the crystal structure.
doi:10.1107/S1600536809053045
PMCID: PMC2980180  PMID: 21579968
24.  [μ-Bis(diphenyl­phosphan­yl)ethane-1:2κ2 P:P′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-[tris­(4-(meth­oxy­phen­yl)arsane-3κAs]-triangulo-triruthenium(0) chloro­form monosolvate 
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
25.  [μ-Bis(diphenyl­phosphan­yl)ethane-1:2κ2 P:P′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-(triphenyl­stibine-3κSb)-triangulo-triruthenium(0) 
The asymmetric unit of the title triangulo-triruthenium compound, [Ru3(C26H24P2)(C18H15Sb)(CO)9], consists of two crystallographically independent mol­ecules, A and B. The bis­(diphenyl­phosphan­yl)ethane ligand bridges an Ru—Ru bond and the monodentate stibine ligand bonds to the third Ru atom. Both the stibine 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 stibine-substituted benzene rings make dihedral angles of 38.7 (3), 71.5 (3) and 70.0 (3)° with each other in mol­ecule A whereas these angles are 83.9 (3), 88.2 (3) and 56.8 (3)° in mol­ecule B. Similarly, the dihedral angles between the two benzene rings are 80.7 (3) and 87.6 (3)° for the two diphenyl­phosphanyl groups in mol­ecule A and 84.0 (3) and 72.6 (4)° in mol­ecule B. In the crystal, mol­ecules are linked into tetra­mers via inter­molecular C—H⋯O hydrogen bonds. Weak inter­molecular C—H⋯π inter­actions further stabilize the crystal structure.
doi:10.1107/S1600536810054218
PMCID: PMC3051588  PMID: 21522852

Results 1-25 (363425)