The Preparation, Spectroscopic Characterization and X-Ray Structure of the Salt [Pt(η1 -C6H9)(Cy2PCH2CH2PCy2)(PPh3)]HCO3·3H2O Containing the Discrete, Uncoordinated, Hydrogen-Bonded Dimeric Bicarbonate Dianion [(HCO3)(H2O)3]22-

1999 ◽  
Vol 52 (10) ◽  
pp. 949 ◽  
Author(s):  
Martin A. Bennett ◽  
Glen B. Robertson ◽  
Pramesh N. Kapoor
Keyword(s):  
Low Temperature ◽  
Spectroscopic Characterization ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
R Value ◽  
Unit Cell Dimensions ◽  
Hydrogen Bonded

Reaction of the cyclohexyne–platinum(0) complex [Pt(η2-C6H8)(Cy2PCH2CH2PCy2)]* with water and CO2 in the presence of triphenylphosphine gives the bicarbonate salt of the (η1-cyclohexenyl)platinum(II) cation, [Pt(η1-C6H9)(Cy2PCH2CH2 PCy2)(PPh3)] [HCO3] · 3H2O, which has been characterized by n.m.r. spectroscopy and single-crystal X-ray diffraction at low temperature. Crystals are triclinic, space group P1– with unit cell dimensions a 20.315(2), b 12.782(1), c 10.694(1) Å, α 66.61(1), β 104.73(1), γ 102.11(1)˚, and Z 2. The structure was refined to a final R value of 0.036 with use of 7553 reflections [I > 3σ(I)]. The cation has the expected, somewhat distorted planar coordination geometry; the anion consists of discrete, hydrogen-bonded dimers [(HCO3)(H2O)3]22-.

Cyclopentadienyl-Ruthenium and -Osmium Chemistry. XL. X-Ray Crystal Structures of MBr (PPh3)2(η-C5H5).CH2Cl2 (M = Ru, Os)

1995 ◽  
Vol 48 (11) ◽  
pp. 1887 ◽  
Author(s):  
MI Bruce ◽  
PJ Low ◽  
BW Skelton ◽  
ERT Tiekink ◽  
A Werth ◽  
...  
Keyword(s):  
Structural Parameters ◽  
Molecular Structures ◽  
Coordination Geometry ◽  
Chloro Complexes ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal and molecular structures of MBr (PPh3)2(η-C5H5).CH2Cl2 (M = Ru and Os) have been determined. A revised synthesis of the bromo osmium complex is given. The coordination geometry about the metal atom is based on a distorted octahedron with one face being occupied by the cyclopentadienyl group [average Ru -C(Cp) 2.214(3), Os-C(Cp) 2.177(3)Ǻ] and the other by the bromide [ Ru -Br 2.5683(8), Os-Br 2.5438(9)Ǻ] and the two phosphorus atoms [ Ru -P 2.323(2), 2.329(1); Os-P 2.290(2), 2.297(2)Ǻ]. Structural parameters are compared with those of the corresponding chloro complexes and differ only minimally. Crystals of MBr (PPh3)2(η-C5H5).CH2Cl2 are triclinic, space group Pī , with unit cell dimensions ( Ru [Os]): a 14.374(5) [14.276(4)], b 14.057(4) [13.959(3)], c 10.012(5) [9.903(3)]Ǻ, α 99.43(3) [99.79(2)], β 105.60(3) [105.74(2)], γ 100.42(3) [100.39(2)]°, V 1868(1) [1817.7(9)] Ǻ3, Z 2. The structures were refined by a full-matrix least-squares procedure to R 0.050 [0.036] for 7365 [5108] reflections with I ≥ 3σ(I).

Cluster Chemistry. XLVII. X-Ray Crystal Structure of OsPt2(μ-CO)3(CO)2(PPh3)3

1986 ◽  
Vol 39 (12) ◽  
pp. 2145 ◽  
Author(s):  
MI Bruce ◽  
MR Snow ◽  
ERT Tiekink
Keyword(s):  
Crystal Structure ◽  
X Ray Diffraction ◽  
Cluster Chemistry ◽  
Triclinic Space Group ◽  
X Ray ◽  
Metal Atoms ◽  
Metal Metal ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Triphenylphosphine Ligand

The crystal structure of OsPt2(μ-CO)3(CO)2(PPh3)3 has been determined by single-crystal X-ray diffraction techniques. Crystals are triclinic, space group Pī with unit cell dimensions a 13.593(4), b 15.839(4), c 12.633(8) Ǻ, α 102.97(3), β 108.18(2), γ 84.86(3)° with Z2. The structure was refined by a full-matrix least-squares procedure on 5896 reflections [I ≥ 2.5σ(I)] to final R 0.028 and Rw 0.034. A triphenylphosphine ligand binds each of the metal atoms disposed at the corners of a triangle. Each metal-metal bond is spanned by a bridging carbonyl group. The coordination about the osmium atom is completed by two terminal carbonyl groups.

Phosphinegold(I) Complexes Containing the Purine-6-thiolate Anion, and Their Antiarthritic Activity

1994 ◽  
Vol 47 (4) ◽  
pp. 577 ◽  
Author(s):  
PD Cookson ◽  
ERT Tiekink ◽  
MW Whitehouse
Keyword(s):  
Spectroscopic Data ◽  
Gold Atom ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Thiolate Ligand ◽  
Cell Dimensions ◽  
Ethanol Solvate ◽  
Thiolate Anion ◽  
Unit Cell Dimensions

A series of complexes of the general formulae R3PAu(6-mp), R3P = Et3P, Ph3P, Cy3P, PhMe2P, (o-tol)3P, (m-tol)3P or (p-tol)3P, (AuCl)Ph2P(CH2)nPPh2(Au(6-mp)), n = 2 or 3, and Ph2P(CH2)nPPh2(Au(6-mp))2, n = 1, 2 or 3 and 6-mp is the anion derived from 6-mercaptopurine (purine-6-thiol), have been prepared and characterized by spectroscopic methods (i.r., 1H, 13C, 31P n.m.r. and f.a.b. m.s.) and, in the case of the Ph3PAu(6-mp) complex, by single-crystal X-ray diffraction methods. The spectroscopic data show that the 6-mp ligand coordinates as a thiolate ligand and that the gold atoms exist in linear P-Au-S (or P-Au-Cl) geometries. This has been confirmed by an X-ray study on Ph3PAu(6-mp), isolated as an ethanol solvate; the study shows the gold atom to be linearly coordinated by the phosphorus and sulfur atoms: Au-P(1) 2.237(2), Au-S(6) 2.287(1) Ǻ and P-Au-S 173.71(6)°. Crystals of Ph3PAu(6-mp).EtOH are triclinic, space group Pī, with unit cell dimensions a 11.066(3), b 13.552(3), c 8.705(2) Ǻ, α 91.51(2), β 113.06(2), γ 89.69(2)°, V 1200.8(5) Ǻ3, Z 2. The structure was refined by a full-matrix least-squares procedure to R 0.034 for 3978 reflections with I ≥ 3.0σ(I). Preliminary results of testing for antiarthritic activity among the new complexes in rats are also reported showing that some of them are more potent/less toxic than current gold(I) thiolates used clinically.

Triorganophosphinegold(I) Carbonimidothioates

1993 ◽  
Vol 46 (4) ◽  
pp. 561 ◽  
Author(s):  
VJ Hall ◽  
G Siasios ◽  
ERT Tiekink
Keyword(s):  
Spectroscopic Data ◽  
Gold Atom ◽  
Spectroscopic Methods ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Thiolate Ligand ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The title compounds, R3PAuSC(= NPh )OR′, R = Et, Ph or Cy and R′ = Me, Et, Pr, Pri or Cy, have been prepared and characterized by spectroscopic methods ( i.r., 1H and 13C n.m.r. and f.a.b . m.s .) and, in the case of the R = Ph and R′ = Me compound, by single-crystal X-ray diffraction methods. The spectroscopic data are consistent with the R3PAu moiety being coordinated by the sulfur atom of the thiolate ligand. This has been confirmed by an X-ray study on Ph3PAuSC(= NPh )OMe which shows the gold atom to be linearly coordinated by the phosphorus and sulfur atoms; Au-P(1) 2.258(1), Au-S(1) 2.301(1) Ǻ and P-Au-S 177.7(1)°. Crystals of Ph3PAuSC(= NPh ) OMe are triclinic, space group pī, with unit cell dimensions: a 10.825(1), b 12.553(2), c 8.914(2) Ǻ, α 97.86(2), β 93.79(1), γ 88.60(1)°, V 1197.1 Ǻ3, Z 2. The structure was refined by a full-matrix least-squares procedure to R 0.028 for 4409 reflections with I ≥ 2.5σ(I).

Tris(dimethylphenylphosphine)ruthenium(0) Complexes of n4-Coordinated Polycyclic Aromatic Hydrocarbons

2000 ◽  
Vol 53 (6) ◽  
pp. 507 ◽  
Author(s):  
Martin A. Bennett ◽  
Mark Bown ◽  
David C. R. Hockless
Keyword(s):  
Coordination Geometry ◽  
Crystal Data ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Tertiary Phosphine ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Polycyclic Aromatic ◽  
R Value ◽  
Axial Site

From the reaction of [Ru2Cl3(PMe2Ph)6] Cl with the appropriate radical anions, yellow complexes of general formula [Ru(PMe2Ph)3(η4-arene)] [arene = naphthalene (C10H8) (1), anthracene (C14H10) (2), and triphenylene (C18H12) (3)] have been isolated in poor yield and characterized by elemental analysis, n.m.r. (1H, 13C, 31P) spectroscopy and single-crystal X-ray diffraction. Crystal data: (1), monoclinic, C2/c, a 31.096(8), b 12.012(4), c 17.078(8) Å, β 104.41(3)˚, V 6178(4) Å3, ? 8, refined to final R value of 0.032 with use of 3641 reflections [I > 3σ(I)]; (2), monoclinic, C2/c, a 55.909(4), b 14.348(5), c 17.573(5) Å, β 105.41(1)˚, V 13590(6) Å3, Z 16 (two molecules per asymmetric unit), refined to final R value of 0.049 with use of 7770 reflections [I > 3σ(I)]; (3), mono-clinic, Pn, a 9.377(3), b 12.229(3), c 15.975(3) Å, β 103.51(2)˚, V 1781.2 (7) Å3, Z 2, refined to final R value of 0.026 with use of 2830 reflections [I > 3σ(I)]. In each case, coordination of the zerovalent metal fragment Ru(PMe2Ph)3 to the diene section of one of the terminal rings causes the aromatic molecule to be folded by c. 40˚ at the outer carbon atoms of the diene. The coordination geometry about ruthenium is approximately square pyramidal, with the diene and two tertiary phosphines in the equatorial plane and the remaining tertiary phosphine in the axial site.

Crystallization and preliminary X-ray diffraction studies of human catalase

1999 ◽  
Vol 55 (9) ◽  
pp. 1614-1615 ◽  
Author(s):  
R. A. P. Nagem ◽  
E. A. L. Martins ◽  
V. M. Gonçalves ◽  
R. Aparício ◽  
I. Polikarpov
Keyword(s):  
Search Model ◽  
Molecular Replacement ◽  
X Ray Diffraction ◽  
Beef Liver ◽  
X Ray ◽  
Diffusion Technique ◽  
Cell Dimensions ◽  
Synchrotron Radiation Diffraction ◽  
Replacement Solution ◽  
Unit Cell Dimensions

The enzyme catalase (H2O2–H2O2 oxidoreductase; E.C. 11.1.6) was purified from haemolysate of human placenta and crystallized using the vapour-diffusion technique. Synchrotron-radiation diffraction data have been collected to 1.76 Å resolution. The enzyme crystallized in the space group P212121, with unit-cell dimensions a = 83.6, b = 139.4, c = 227.5 Å. A molecular-replacement solution of the structure has been obtained using beef liver catalase (PDB code 4blc) as a search model.

The high-pressure cadmium borate Cd6B22O39·H2O

2015 ◽  
Vol 70 (3) ◽  
pp. 183-190 ◽  
Author(s):  
Gerhard Sohr ◽  
Nina Ciaghi ◽  
Klaus Wurst ◽  
Hubert Huppertz
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Structural Characteristics ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Pressure High Temperature ◽  
Cell Dimensions ◽  
Temperature Experiment ◽  
Unit Cell Dimensions ◽  
Ir And Raman

AbstractSingle crystals of the hydrous cadmium borate Cd6B22O39·H2O were obtained through a high-pressure/high-temperature experiment at 4.7 GPa and 1000 °C using a Walker-type multianvil apparatus. CdO and partially hydrolyzed B2O3 were used as starting materials. A single crystal X-ray diffraction study has revealed that the structure of Cd6B22O39·H2O is similar to that of the type M6B22O39·H2O (M=Fe, Co). Layers of corner-sharing BO4 groups are interconnected by BO3 groups to form channels containing the metal cations, which are six- and eight-fold coordinated by oxygen atoms. The compound crystallizes in the space group Pnma (no. 62) [R1=0.0379, wR2=0.0552 (all data)] with the unit cell dimensions a=1837.79(5), b=777.92(2), c=819.08(3) pm, and V=1171.00(6) Å3. The IR and Raman spectra reflect the structural characteristics of Cd6B22O39·H2O.

X–Ray Powder Diffraction Data for Synthetic Varieties of Tetrahedrite

1991 ◽  
Vol 6 (1) ◽  
pp. 43-47 ◽  
Author(s):  
Neil E. Johnson
Keyword(s):  
Powder Diffraction ◽  
Experimental Unit ◽  
Regression Equations ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Validation Test ◽  
Cell Dimensions ◽  
Synthetic Varieties ◽  
Unit Cell Dimensions

AbstractA series of five synthetic tetrahedrite-group minerals has been prepared and examined using powder X-ray diffraction in order to update current powder data and provide a validation test of cell dimension prediction equations. The tetrahedrites (nominally (Cu10X2)Sb4S13 with X = Zn, Cd, Mn, Hg and Fe) have the following properties: zincian tetrahedrite, a = 10.3833 (1) Å, Dx = 4.974 (1) g/cm3, F30 = 264 (0.004, 31), M20 = 279; cadmian tetrahedrite, a = 10.5066 (1) Å, Dx = 5.073 (1) g/cm3, F30 = 208 (0.004, 37), M20 = 249; manganoan tetrahedrite, a = 10.4384 (1) Å, Dx = 4.822 (1) g/cm3, F30 = 274 (0.003, 33), M20 = 302; mercurian tetrahedrite, a = 10.5071 (1) Å, Dx = 5.570 (1) g/cm3, F30 = 150 (0.006, 35), M20 = 156; ferroan tetrahedrite, a = 10.3630 (1) Å, Dx = 5.002 (1) g/cm3, F30 = 253 (0.004, 33), M20 = 281. The experimental unit cell dimensions obtained in this study are in excellent agreement with calculated values produced using regression equations developed previously.

Silver(I)-Saccharinato Complexes with 2-(Aminomethyl)pyridine and 2-(2-Aminoethyl)pyridine Ligands: [Ag(sac)(ampy)] and [Ag2(sac)2(μ-aepy)2]

2005 ◽  
Vol 60 (9) ◽  
pp. 978-983 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
William T. A. Harrison
Keyword(s):  
Thermal Analysis ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pyridine Ligands

Two new saccharinato-silver(I) (sac) complexes, [Ag(sac)(ampy)] (1), and [Ag2(sac)2(μ-aepy)2] (2), [ampy = 2-(aminomethyl)pyridine, aepy = 2-(2-aminoethyl)pyridine], have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group P21/c and triclinic space group P1̄, respectively. The silver(I) ions in both complexes 1 and 2 exhibit a distorted T-shaped AgN3 coordination geometry. 1 consists of individual molecules connected into chains by N-H···O hydrogen bonds. There are two crystallographically distinct dimers in the unit cell of 2 and in each dimer, the aepy ligands act as a bridge between two silver(I) centers, resulting in short argentophilic contacts [Ag1···Ag1 = 3.0199(4) Å and Ag2···Ag2 = 2.9894(4) Å ]. Symmetry equivalent dimers of 2 are connected by N-H···O hydrogen bonds into chains, which are further linked by aromatic π(py)···π(py) stacking interactions into sheets.

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