The structure of [Ir2(CO)2(μ-H)(μ-CO)(Ph2PCH2PPh2)2][BF4] and comparisons with its rhodium analogue and other related doubly bridged A-frames

1986 ◽  
Vol 64 (3) ◽  
pp. 464-469 ◽  
Author(s):  
Bruce R. Sutherland ◽  
Martin Cowie
Keyword(s):  
Solid State ◽  
Iridium Complex ◽  
Monoclinic Space Group ◽  
Diphosphine Ligands ◽  
Space Group ◽  
Coordination Sites ◽  
Metal Metal ◽  
Hydride Ligand

The structure of [Ir2(CO)2(μ-H)(μ-CO)(DPM)2][BF4] (DPM = Ph2PCH2PPh2) has been determined crystallographically. It crystallizes in the monoclinic space group P21/n (a = 13.7740(6) Å, b = 15.277(2) Å, c = 23.581(2) Å, β = 97.015(5)°, V = 4924.9 Å3, Z = 4) and on the basis of 6628 unique observations and variation of 272 parameters, the structure converged to R = 0.031 and Rw = 0.043. This metal–metal bonded complex is similar to its rhodium analogue, having the two essentially identical Ir centres bridged by the carbonyl, hydride, and two diphosphine ligands. The major difference between this compound and the rhodium species (in the solid state) relates to the orientation of the phenyl groups of the diphosphine ligands; in the iridium complex four of these groups block the sites adjacent to the bridging hydride ligand, whereas these sites are relatively unobstructed in the rhodium analogue. This difference may result in different coordination sites for substrate molecules and therefore in different chemistry.

[Fe4S4I2(C6H10(NHCSNHMe)2)]: ein neutraler Eisen-Schwefel-Cluster mit zweizähnigem Liganden / [Fe4S4I2(C6H10(NHCSNHMe)2)]: A Neutral Iron-Sulfur Cluster with a Bidentate Ligand

1992 ◽  
Vol 47 (9) ◽  
pp. 1266-1270 ◽  
Author(s):  
Siegfried Pohl ◽  
Ulrich Bierbach
Keyword(s):  
Solid State ◽  
Bidentate Ligand ◽  
Striking Feature ◽  
Monoclinic Space Group ◽  
Thiourea Derivative ◽  
Iron Sulfur Cluster ◽  
Sulfur Cluster ◽  
Space Group ◽  
Iron Sulfur ◽  
Neutral Ligands

The reaction of [Fe4S4I2(SC(NMe2)2)2] with racemic trans-1,2-bis(3-methylthioureido)-cyclohexane in tetrahydrofuran (thf) yields [Fe4S4I2(C6H10(NHCSNHMe)2)] · 4 thf (2). 2 crystallizes in the monoclinic space group C 2/c with a = 1471.7(2), b = 1329.7(2), c = 2339.3(3) pm, β = 107.70(1), V = 4362.3 × 106 pm3, Z = 4, R = 0.057. The cluster exhibits C2 symmetry in the solid state. The replacement of the monodentate neutral ligands results in a cluster in which the bifunctional thiourea derivative bridges two different iron sites of the slightly compressed [Fe4S4] core. The most striking feature are the differences of the Fe–Fe distances which are 269.8 pm between thiourea coordinated atoms and 280.7 pm between Fe atoms with iodide ligation. The Fe–S thiourea distance was found to be 229.3 pm.

scholarly journals Novel Structures and Magnetic Properties of Two [Mn2] Complexes with 2,4-di-2-pyridyl-2,4-pentanediol as the Ligand

2019 ◽  
Vol 5 (3) ◽  
pp. 43
Author(s):  
En-Che Yang ◽  
Yu-Ying Chang ◽  
Shi-Yi Huang ◽  
Ling-Xuan Hong ◽  
Gene-Hsiang Lee ◽  
...  
Keyword(s):  
Magnetic Properties ◽  
Magnetic Property ◽  
The Other ◽  
Antiferromagnetic Coupling ◽  
Monoclinic Space Group ◽  
Ferromagnetic Coupling ◽  
Manganese Ions ◽  
Space Group ◽  
Metal Metal ◽  
Novel Structures

Two ligands, 2,4-di-2-pyridyl-2,4-pentanediol (rD and mD), were employed to synthesize two Mn2 complexes, [Mn2(rD)2Br2] (1) and [Mn2(mD)2(H2O)2]Br2 (2). Compound 1 crystallized in a tetragonal space group, P41212, with a novel hamburger shaped structure. A detailed study indicated that compound 1 did not contain a metal–metal bond, but antiferromagnetic coupling was observed between the Mn(III) ions. Compound 2 crystallized in a monoclinic space group, C2/c, with one Mn(II) and the other with Mn(IV). The two manganese ions were bridged by two alkoxide ligands, resulting in ferromagnetic coupling. Magnetic property studies confirm the above assignments.

Notizen: Solid State Structure of N,N-Dibenzylhydroxylamine

1995 ◽  
Vol 50 (4) ◽  
pp. 699-701 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Jürgen Riede ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of N,N-dibenzylhydroxylamine (1) has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P 21/n with four formula units in the unit cell. N,N-dibenzylhydroxylamine dimerizes to give N2O2H2 sixmembered rings as a result of the formation of two hydrogen bonds O - H ··· N in the solid state.

Darstellung und Kristallstruktur von [P(C6H5)4]Cl3 / Preparation and Crystal Structure of [P(C6H5)4]Cl3

1995 ◽  
Vol 50 (8) ◽  
pp. 1171-1174 ◽  
Author(s):  
M. Jansen ◽  
S. Strojek
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Monoclinic Space Group ◽  
Space Group

Preparation and crystal structure of [P(C6H5)4]Cl3 are reported. [P(C6H5)4]Cl3 crystallizes in the monoclinic space group P21/c with a = 1093.4(4), b = 789.1(1), c = 2682.7(7) pm, β = 90.39(1)°, V = 2200.27·106 pm3, and Z = 4. The geometry of the trichloride anion in the solid state is almost linear (Cl-Cl-Cl = 178.44(4)°) and unsymmetrical (d(Cl-Cl) = 226.3(1) and 230.7(1) pm).

Mono- and difunctional furan-based 1,2,3,5-dithiadiazolyl radicals; preparation and solid state structures of 2,5-[(S2N2C)OC4H2(CN2S2)] and 2,5-[(S2N2C)OC4H2(CN)]

1992 ◽  
Vol 70 (3) ◽  
pp. 919-925 ◽  
Author(s):  
A. Wallace Cordes ◽  
Charles M. Chamchoumis ◽  
Robin G. Hicks ◽  
Richard T. Oakley ◽  
Kelly M. Young ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
The Mean ◽  
Solid State Structures ◽  
Solid State Characterization

The preparation and solid state characterization of the bifunctional radical furan-2,5-bis(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN2S2)] and the related monofunctional radical 2-cyanofuran-5-(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN)] are described. The crystal structure of 2,5-[(S2N2C)OC4H2(CN2S2)] is orthorhombic, space group Pna21, and consists of interleaved arrays of dimers, for which the mean interannular [Formula: see text] contact is 3.137 Å. The crystal structure of the monofunctional radical 2,5-[(S2N2C)OC4H2(CN)] is monoclinic, space group P21/n, and consists of a ribbon-like network of dimers (mean interannular [Formula: see text] interconnected by close head-to-tail [Formula: see text] contacts. The dimer units form stacks parallel to z, with a mean interdimer [Formula: see text] separation of 3.956 Å. The similarities and differences between these two crystal structures and those of related benzene-substituted systems are discussed. Keywords: dithiadiazolyl radicals, furan-based diradicals, cyanofuran-based radicals, radical dimers, crystal structures.

Solid-state chemistry of polycarboxylate crown ether cation complexes: cooperative binding of water and metal ions by flexible chorands

1993 ◽  
Vol 71 (2) ◽  
pp. 239-253 ◽  
Author(s):  
Philip J. Dutton ◽  
Thomas M. Fyles ◽  
Valia Veettil Suresh ◽  
Frank R. Fronczek ◽  
Richard D. Gandour
Keyword(s):  
Solid State ◽  
Crown Ether ◽  
Sodium Salt ◽  
Metal Salt ◽  
Alkali Metal Salt ◽  
Cation Binding ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cesium Salt

The solid-state structures of alkali-metal salt complexes of crown ether tetra- and hexa-carboxylic acids (18C6A4 and 18C6A6) have been determined. The sodium salt of 18C6A6 crystallizes as the trihydrate in orthorhombic space group P212121 (a = 7.6868(12), b = 15.429(3), c = 21.975(2) Å, R = 0.031 for 5192 observed data); the potassium salt of 18C6A6 crystallizes as the the trihydrate in orthorhombic space group P212121 (a = 7.6711(8), b = 15.709(2), c = 21.966(5) Å, R = 0.035 for 2521 observed data); the thallium(I) salt of 18C6A6 crystallizes as the dihydrate in orthorhombic space group P212121 (a = 12.0331(10), b = 12.4333(12), c = 17.366(2) Å, R = 0.035 for 4952 observed data); and the cesium salt of 18C6A6 crystallizes as the dihydrate in monoclinic space group P21 (a = 7.708(3), b = 13.492(2), c = 11.9501(9) Å, β = 94.49(2)°, R = 0.029 for 4480 observed data). The sodium salt of 18C6A4 crystallizes as the dihydrate in monoclinic space group P21 (a = 11.4368(11), b = 7.7068(11), c = 12.6579(12) Å, β = 98.515(8)°, R = 0.035 for 3000 observed data); the thallium(I) salt of 18C6A4 crystallizes as the dihydrate in monoclinic space group P21(a = 11.719(2), b = 7.668(2), c = 12.8403(13) Å, β = 99.052(9)°, R = 0.040 for 3981 observed data); and the cesium salt of 18C6A4 crystallizes as the dihydrate in monoclinic space group P21 (a = 11.787(2), b = 7.637(2), c = 13.001(2) Å, β = 98.705(12)°, R = 0.038 for 3428 observed data). Both chorands exhibit a cooperative relationship of mean cavity radius and guest-ion radius, which closely follows the effective ionic radii of the guests. The hexaacid is a preorganized host for monohydrated cations. It provides a trigonal hydrogen bonding receptor site for the water molecule, and up to nine oxygen donors for cation binding. Guests ranging in size from Na+ to Cs+ are accommodated without distortion of the macrocyclic framework. The tetraacid is similarly tolerant of a range of guests, but greater structural reorganization of the ligand is required to optimize contacts with fully dehydrated cations. Skeletal drawings of donor atoms, in conjunction with polar coordinate maps of torsion angles, reveal how the demands of the guest are accommodated by the host.

Preparation and crystal structure of SbV1.50InIII0.50(PO4)3 and (SbV0.50InIII0.50)P2O7

2008 ◽  
Vol 23 (3) ◽  
pp. 232-240
Author(s):  
Abderrahim Aatiq ◽  
Rachid Bakri ◽  
Aaron Richard Sakulich
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Room Temperature ◽  
Rietveld Method ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Orthorhombic System ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Synthesis and structure of two phosphates belonging to the ternary Sb2O5–In2O3–P2O5 system are realized. Structures of SbV1.50InIII0.50(PO4)3 and (SbV0.50InIII0.50)P2O7 phases, obtained by solid state reaction in air at 950 °C, were determined at room temperature from X-ray powder diffraction using the Rietveld method. SbV1.50InIII0.50(PO4)3 have a monoclinic (space group P21/n) distortion of the Sc2(W O4)3-type framework. Its structure is constituted by corner-shared SbO6 or InO6 octahedra and PO4 tetrahedra. Monoclinic unit cell parameters are a=11.801(2) Å, b=8.623(1) Å, c=8.372(1) Å, and β=90.93(1)°. (Sb0.50In0.50)P2O7 is isotypic with (Sb0.50Fe0.50)P2O7 and crystallizes in orthorhombic system (space group Pna21) with a=7.9389(1) Å, b=16.0664(2) Å, and c=7.9777(1) Å. Its structure is built up from corner-shared SbO6 or InO6 octahedra and P2O7 groups (two group-types). Each P2O7 group shares its six vertices with three SbO6 and three InO6 octahedra, and each octahedron is connected to six P2O7 groups.

Bis(trifluormethyl)disulfan und -trisulfan: Molekülgeometrie im festen Zustand [1] / Bis(trifluoromethyl)disulfane and Trisulfane: Molecular Geometry in the Solid State [1]

1997 ◽  
Vol 52 (1) ◽  
pp. 69-71 ◽  
Author(s):  
Christian Meyer ◽  
Dietrich Mootz ◽  
Birgit Bäck ◽  
Rolf Minkwitz
Keyword(s):  
Solid State ◽  
Electron Diffraction ◽  
Molecular Geometry ◽  
Monoclinic Space Group ◽  
Trans Conformation ◽  
Gaseous State ◽  
Triclinic Space Group ◽  
Space Group ◽  
Solid State Structures ◽  
State 1

The solid-state structures of the low-melting compounds bis(trifluoromethyl)disulfane (CF3SSCF3, triclinic, space group P 1̄, Z = 2) and bis(trifluoromethyl)trisulfane (CF3SSSCF3, monoclinic, space group C2/c, Z = 4) have been determined on single crystals with MoK α radiation at -160°C. The trisulfane has trans conformation. The geometry of both molecules agrees well with results of electron diffraction on the gaseous state. A comparison is made also with the crystal structures of the related molecules CF3TeTeCF3 and CF3OOOCF3

scholarly journals The Synthesis and Crystal Structure of N-tert-Butyl-3-(tert-butylimino)-2-nitropropen-1 -amine

1993 ◽  
Vol 48 (8) ◽  
pp. 1138-1142 ◽  
Author(s):  
Daryl L. Ostercamp ◽  
Lisa M. Preston ◽  
Kay D. Onan
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Solid State ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Tert Butyl ◽  
Intramolecular Hydrogen ◽  
Hydrolysis Of

The unit cell of N-tert-butyl-3-(tert-butylimino)-2-nitropropen-1-amine (4) is monoclinic, space group P21/C, with a = 9.669(4), b = 16.415(6), c = 17.341 (7) Å, and Z = 4. Hydrolysis of 4 leads to (E)-3-(N-tert-butylamino)-2-nitro-2-propenal (5), whose unit cell is monoclinic, space group P21/n, with a = 6.821(1), b = 20.707(6), c = 6.303(1)Å, and Z = 4. Compounds 4 and 5 both possess C2 symmetry in the solid state, their “U-shaped” conjugated cores being essentially planar. In each case this planarity is enforced by an intramolecular hydrogen bond.

Ruthenium(II) complexes of the thiacyclophane ligands 2,5,8-trithia[9]-o-cyclophane (TT[9]OC) and 5-oxa-2,8-dithia[9]-o-cyclophane (ODT[9]OC). Structures of RuCl2(DMSO)(TT[9]OC) and RuCl2(PPh3)(ODT[9]OC)

1995 ◽  
Vol 73 (7) ◽  
pp. 1102-1110 ◽  
Author(s):  
Broer de Groot ◽  
Hilary A. Jenkins ◽  
Stephen J. Loeb ◽  
Shannon L. Murphy
Keyword(s):  
Coordination Mode ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Ruthenium Hydride ◽  
H Nmr ◽  
Coordination Sites ◽  
Ligand Displacement ◽  
Displacement Reactions

Ruthenium(II) complexes of the thiacyclophane ligands 2,5,8-trithia[9]-o-cyclophane (TT[9]OC) and 5-oxa-2,8-dithia[9]-o-cyclophane (ODT[9]OC) were synthesized by ligand displacement reactions employing RuCl2(DMSO)4, RuCl2(PPh3)3, and RuHCl(PPh3)3 as starting materials. X-ray crystal structures of two of these complexes, RuCl2(DMSO)(TT[9]OC) and RuCl2(PPh3)(ODT[9]OC), demonstrate how TT[9]OC and ODT[9]OC bind to Ru(II). RuCl2(DMSO)(TT[9]OC) crystallized as the DMSO solvate in the orthorhombic space group Pbca with a = 19.590(5), b = 16.849(4), c = 13.149(4) Å, V = 4340(3) Å3, and Z = 8. The structure refined to R = 5.27% and Rw = 6.27% for 2472 reflections with Fo2 > 3σ(Fo2). RuCl2(PPh3)(ODT[9]OC) crystallized as a ClCH2CH2Cl solvate in the monoclinic space group P21/c with a = 7.912(1), b = 22.419(5), c = 18.794(3) Å, β = 101.12(1),° V = 3271.2(9) Å3, and Z = 4. The structure refined to R = 4.96% and Rw = 5.14% for 1800 reflections with Fo2 > 3σ(Fo2). Both compounds are octahedral with the thiacyclophane ligand bound through three donor atoms in a facial coordination mode, cis chlorine atoms, and the unique ancillary ligand, DMSO or PPh3, bound trans to the central S or O donor of the macrocycle. The X-ray structures support 1H NMR spectral evidence which shows that the ligands are bound in an "endo" mode for L = DMSO and in an "exo" mode when L = PPh3. The reaction of RuHCl(PPh3)3 with TT[9]OC yields the ruthenium hydride complex RuHCl(PPh3)2(TT[9]OC). 1H and 31P NMR spectroscopy are consistent with an octahedral species for which the macrocycle occupies only two coordination sites acting as a bidentate η2-chelating ligand. Keywords: thioether, macrocycle, hydride, crystal structure.

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