Structure of the Tris(diallyldithiocarbamate)cobalt(III) Complex

1992 ◽  
Vol 57 (2) ◽  
pp. 332-338 ◽  
Author(s):  
Eleonóra Kellö ◽  
Jan Lokaj ◽  
Viktor Vrábel
Keyword(s):  
Least Squares ◽  
Metal Atom ◽  
Least Squares Method ◽  
Heavy Atom ◽  
Distorted Octahedron ◽  
Monoclinic System ◽  
Space Group ◽  
Twofold Axis ◽  
Diagonal Approximation ◽  
Heavy Atom Method

The structure of [Co{S2CN(CH2-CH=CH2)2}3] was determined by the heavy atom method, all nonhydrogen atoms being refined by anisotropic diagonal approximation using the least squares method to the value of R= 0.067 for 1 024 reflections with I ≥ 1.96σ(I). The substance is isostructural with [Fe{S2CN(CH2-CH=CH2)2}3], crystallizes in the monoclinic system, space group C2/c, lattice parameters a = 1.8763(9), b = 1.0209(5), c = 1.5402(7) nm, β = 106.18(4)°, Z = 4. Cobalt is coordinated by 3 dithiocarbamate ligands in the bidentate way, the average Co-S lenght is 0.2267(2) nm. The metal atom and two ligand atoms are located on the twofold axis. The CoS6 polyhedron is a trigonally distorted octahedron.

Crystal Structure of Adeninium Trichloromercurate(II),

1975 ◽  
Vol 53 (15) ◽  
pp. 2345-2350 ◽  
Author(s):  
Monique Authier-Martin ◽  
André L. Beauchamp
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Title Compound ◽  
Heavy Atom ◽  
Chloride Ions ◽  
Water Molecules ◽  
Hydrogen Atoms ◽  
Space Group ◽  
Heavy Atom Method

The title compound belongs to space group P21/c with a = 23.99(1), b = 4.245(2), c = 25.98(1) Å, β = 117.58(7)°, and Z = 8. The structure was solved by the heavy-atom method and refined by block-diagonal least squares on 2589 independent observed reflections. All non-hydrogen atoms were refined anisotropically and some of the hydrogen atoms were located but their parameters were not refined. The final values of R and Rw were 0.042 and 0.047, respectively.The two nonequivalent mercury atoms have very similar environments. Two short Hg—Cl bonds (2.34–2.38 Å) at ∼ 165° define a quasi-molecular HgCl2 unit. Overall octahedral coordination is completed with two chloride ions at 2.76–2.84 Å and two chlorine atoms at 3.19–3.26 Å on neighboring HgCl2 quasi-molecules. HgCl6 octahedra share edges to form twofold ribbons in the b direction. This pattern of octahedra is identical with the onereported for β-NH4HgCl3. The cations are pairs of N(1)-protonated adenine molecules linked by two N(10)—H(10)… N(7) hydrogen bonds and stacked in the b direction. Water molecules act as acceptors in moderately strong hydrogen bonds with acidic protons H(1) and H(9) of adeninium ions. Other generally weaker hydrogen bonds exist between the various parts of the structure.

Chemistry of proximal π-bond systems. Part IV. The structure of 5,6-dimethylenebicyclo[2,2,1]hept-2-ene molybdenum tricarbonyl

1976 ◽  
Vol 54 (12) ◽  
pp. 1958-1966 ◽  
Author(s):  
Bryan F. Anderson ◽  
Glen B. Robertson ◽  
Douglas N. Butler
Keyword(s):  
Metal Atom ◽  
Heavy Atom ◽  
Least Square ◽  
Molybdenum Atom ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths ◽  
R Factor ◽  
Heavy Atom Method

Crystals of 5,6-dimethylenebicyclo[2,2,1]hept-2-ene molybdenum tricarbonyl 1 (M = Mo) are monoclinic, a = 7.4451(3) Å, b = 13.5783(7) Å, c = 11.2691(4) Å, β = 92.593(3)°, Z = 4, space group P21/c. The structure was solved by the 'heavy atom' method and was refined by full-matrix least square procedures to a final R = 0.031. The weighted R factor was 0.051. Experimental bond lengths and angles are close to other reported values for bicyclo[2,2,1]hept-2-ene systems except for three major distortions in the triene ligand namely: the closing of the angles C(2)—C(1)—C(6) and C(3)—C(4)—C(5) by about 5.3°, the bending of the butadiene fragment plane C(8)—C(5)—C(6)—C(9) toward the metal atom by about 20° and the twisting of the terminal methylene hydrogens H(8i) and H(9i) out of the butadiene fragment plane (0.44 and 0.53 Å respectively) away from the molybdenum atom.

Crystal structure of N-(2,6-dimethylphenyl)chloromaleinimide

1989 ◽  
Vol 54 (9) ◽  
pp. 2408-2414 ◽  
Author(s):  
Viktor Vrábel ◽  
Eleonóra Kellö ◽  
Jan Lokaj ◽  
Václav Konečný
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Least Squares Method ◽  
Heavy Atom ◽  
Diagonal Matrix ◽  
Lattice Parameters ◽  
Block Diagonal Matrix ◽  
Orthorhombic System ◽  
Heavy Atom Method ◽  
Block Diagonal

The crystal structure of N-(2,6-dimethylphenyl)chloromaleinimide solved by the heavy atom method was refined by the 9 x 9 block-diagonal matrix least-squares method to a final R value 0.08 for 1 147 observed diffractions. The compound crystallizes in the orthorhombic system with Pbca group and lattice parameters a = 13.622(4), b = 13.483(7), c = 12.768(6) Å, Z = 8. Monomeric units, between which interactions of type Cl···H-C and O···H-C occured, formed the crystal structure. Both moieties of the molecule, i.e. the phenyl and the five-membered maleinimide rings were found to be virtually planar and the central planes intersecting these rings form an angle 78.3°.

Structure of Sodium Hydrogen Selenite-Selenious Acid Adduct (1:3), NaHSeO3.3H2SeO3

1992 ◽  
Vol 57 (11) ◽  
pp. 2309-2314 ◽  
Author(s):  
Josef Loub ◽  
Zdeněk Mička ◽  
Jana Podlahová ◽  
Karel Malý ◽  
Jürgen Kopf
Keyword(s):  
Hydrogen Bonds ◽  
Title Compound ◽  
Heavy Atom ◽  
Selenious Acid ◽  
Space Group ◽  
Sodium Hydrogen ◽  
Heavy Atom Method ◽  
Acid Adduct ◽  
Oxygen Atoms

Structure of sodium hydrogen selenite-selenious acid (1:3) was solved by heavy-atom method and refined anisotropically to R = 0.098 for 1223 unique observed reflections. The title compound crystallizes in the Pc space group with a = 5.756(2), b = 4.911(2), c = 20.010(5) Å, β = 100.48(3)°, V = 556(1) Å3, T = 293 K, (a = 5.763(2), b = 4.878(1), c = 20.03(1) Å, β = 100.48(3)°, V = 554(1) Å3, T = 173 K), Z = 2. The structure consist of HSeO3- anions, molecules of selenious acid and Na+ cations which are octahedrally coordinated with oxygen atoms. The structure is stabilized by a system of hydrogen bonds.

The crystal structure of diamminesilver dinitroargentate, [Ag(NH3)2]Ag(NO2)2*

1977 ◽  
Vol 146 (4-6) ◽  
Author(s):  
H. M. Maurer ◽  
Alarich Weiss
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Heavy Atom ◽  
Anisotropic Temperature ◽  
Light Atoms ◽  
Difference Fourier ◽  
Temperature Factors ◽  
Heavy Atom Method ◽  
Silver Atoms ◽  
Block Diagonal

AbstractThe crystal structure of diamminesilver dinitroargentate, [Ag(NHThe point positions of the silver atoms were obtained by the heavy-atom method whereas those of the light atoms were found by difference Fourier syntheses. Coordinates and anisotropic temperature factors were refined by block-diagonal least-squares methods with the result

The crystal structure of dibutyl-bis(pentamethylenedithiocarbamato)tin(IV)

1986 ◽  
Vol 51 (11) ◽  
pp. 2521-2527 ◽  
Author(s):  
Jan Lokaj ◽  
Eleonóra Kellö ◽  
Viktor Kettmann ◽  
Viktor Vrábel ◽  
Vladimír Rattay
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Coordination Polyhedron ◽  
Crystal And Molecular Structure ◽  
Distorted Octahedron ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal and molecular structure of SnBu2(pmdtc)2 has been solved by X-ray diffraction methods and refined by a block-diagonal least-squares procedure to R = 0.083 for 895 observed reflections. Monoclinic, space group C2, a = 19.893(6), b = 7.773(8), c = 12.947(8) . 10-10 m, β = 129.07(5)°, Z = 2, C20H38N2S4Sn. Measured and calculated densities are Dm = 1.38(2), Dc = 1.36 Mg m-3. Sn atom, placed on the twofold axes, is coordinated with four S atoms in the distances Sn-S 2.966(6) and 2.476(3) . 10-10 m. Coordination polyhedron is a strongly distorted octahedron. Ligand S2CN is planar.

The crystal structure of kogarkoite, Na3SO4F

1980 ◽  
Vol 43 (330) ◽  
pp. 753-759 ◽  
Author(s):  
L. Fanfani ◽  
G. Giuseppetti ◽  
C. Tadini ◽  
P. F. Zanazzi
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Least Squares Method ◽  
Thermal Parameters ◽  
Cell Content ◽  
Space Group ◽  
X Ray ◽  
Structural Relationships ◽  
Automatic Diffractometer ◽  
Monoclinic Cell

SummaryThe crystal structure of synthetic kogarkoite has been determined from X-ray data collected on an automatic diffractometer. The refinement was performed by a least-squares method employing anisotropic thermal parameters. The 3157 reflections with I > 3σ(I) converged to a conventional R value of 0.033. The cell content is 12 Na3SO4F, the space-group P21/m, a = 18.074, b = 6.958, c = 11.443 Å, β = 107.71°.Kogarkoite presents a marked trigonal subcell with c′ corresponding to [102] of the monoclinic cell. The tridimensional framework can be considered built up by nine differently stacked layers of Na atoms approximately perpendicular to the c′ axis (five sheets are present in galeite, six in sulphohalite, and seven in schairerite). The very close structural relationships between these minerals are discussed.

Structure cristalline et moléculaire du cyclopentadiényle dicarbonyle triphénylphosphine manganèse, MnC5H5(CO)2P(C6H5)3

1973 ◽  
Vol 51 (18) ◽  
pp. 3027-3031 ◽  
Author(s):  
Claude Barbeau ◽  
Klaus Sorrento Dichmann ◽  
Louis Ricard
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Least Squares Method ◽  
Three Dimensional ◽  
Triphenyl Phosphine ◽  
Triclinic Space Group ◽  
Space Group ◽  
Bond Lengths ◽  
Atomic Parameter

The crystalano molecular structure of cyclopentadienyl manganese dicarbonyl-triphenyl phosphine has been determined by means of three dimensional data obtained by a Buerger precession camera. 2931 independent intensities were utilized in the refinement of the structure using the least-squares method. The final disagreement factor is 0.11. MnC5H5(CO)2P(C6H5)3 crystallizes in the triclinic space group.[Formula: see text]The molecule shows atomic parameter almost identical to those of MnC5H5(CO)3 except for the Mn—C bond lengths which change from 1.80 to 1.73 Å. The Mn—P distance (2.236 Å) and the unchanged parameters for the Mn—C5H5 group confirm the strong donating power of the cyclopentadienyl group. [Journal translation]

Trifluoromethyl Complexes of Osmium(II) by Halogen Oxidation of an Osmium(0) Difluorocarbene Compound and the Structures of Os(CF3)Cl2(NO)(PPh3)2 and Os(CF3)Cl0.666I1.333(NO)(PPh3)2

1986 ◽  
Vol 39 (9) ◽  
pp. 1315 ◽  
Author(s):  
GR Clark ◽  
TR Greene ◽  
WR Roper
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Crystal Structures ◽  
Octahedral Coordination ◽  
Space Group ◽  
Twofold Axis

Oxidation of Os(=CF2) Cl (NO)(PPh3)2 by the halogens X2(X = Cl , I), unexpectedly yields the trifluoromethyl complexes Os(CF3)CIX(NO)(PPh3)2 in a low yield which is improved by the addition of LiF to the reaction mixture. The crystal structures of both Os(CF3)Cl2(NO)(PPh3)2 and Os(CF3)Cl0.666I1.333(NO)(PPh3)2 have been determined. Crystals of Os(CF3)Cl2(NO)(PPh3)2 are monoclinic, a 24.543(5), b 9.685(1), c 15.951(1) Ǻ, β 115.81(1)°, Z 4, space group C2/c. Least-squares refinement has returned a residual, R, of 0.048 for 3371 observed reflections. The molecule lies on a twofold axis, with the CF3-group and one Cl-ligand statistically interchanged. Crystals of Os(CF3)Cl0.666 I1.333(NO)(PPh3)2 are monoclinic, a 24.562(4), b 9.690(1), c 16.385(2) Ǻ, β 115.51(1)°, Z 4, space group C2/c. Least-squares refinement has returned a residual of 0.058 for 4087 observed reflections. This crystal structure is best described as a 2 : 1 mixture of Os(CF3) ClI (NO)(PPh3)2 and s(CF3)I2(NO)(PPh3)2, (both with CF3 and I statistically disordered about the diad axis, as above). Both complexes exhibit octahedral coordination geometries.

A crystallographic and spectroscopic study of mercury(II) dithiocarbamate

1981 ◽  
Vol 59 (18) ◽  
pp. 2746-2749 ◽  
Author(s):  
Chung Chieh ◽  
Sing Kwen Cheung
Keyword(s):  
Mass Spectrum ◽  
Spectroscopic Study ◽  
Least Squares ◽  
Least Squares Method ◽  
Two Dimensional ◽  
Polymeric Compound ◽  
Full Matrix ◽  
Space Group ◽  
Polymeric Networks ◽  
Ir Bands

Ammonium dithiocarbamate, H2NCS2NH4, decomposes easily but the anion forms a stable mercury(II) complex, the crystals of which are orthorhombic with a = 7.851(3), b = 17.565(7), c = 12.051(3) Å, and space group Pbca. The structure was solved by the Patterson method and refined by the full-matrix least-squares method to an R of 0.038 for 781 reflections. The structure consists of layers of two-dimensional polymeric networks. The dimeric subunits in the layer containing two each of mutually connected Hg atoms and dithiocarbamates are further linked by other bridging dithiocarbamates forming a sheet-like structure. Each Hg atom bonds to four S atoms from four separate dithiocarbamates with Hg—S distances of 2.499(4), 2.508(4), 2.533(4), and 2.629(4) Å. The ir bands observed were: ν(NH2), 3320, 3220, 3125; δ(NH2), 1600; ν(C—N), 1395; ρr(NH2), 1172; and v(C—S), 840 cm−1. The mass spectrum of this polymeric compound gave peaks corresponding to Hg, S2, CNH2, HNCS, S, CS2, S5, S4, S3, and S8 in the order of their intensities.

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