Crystal and molecular structure of (RS,RS)-Tetraammine(4,5-dihydroxy-4,5-dimethyl-1-pyrroline-2-carboxylato)cobalt(III) perchlorate

1975 ◽  
Vol 28 (10) ◽  
pp. 2129 ◽  
Author(s):  
GB Robertson ◽  
PO Whimp
Keyword(s):  
Molecular Structure ◽  
Hydrogen Atom ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Methyl Groups ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Steric Strain ◽  
X Ray ◽  
R Factors

The structure of a cobalt(III) tetraammine complex of 4,5-dihydroxy- 4,5-dimethyl-1-pyrroline-2-carboxylic acid (abbreviated as hmpc), (RS,RS)-[Co(NH3)4(hmpc)] (ClO4)2,H2O, has been determined from three- dimensional X-ray data collected by counter methods. Crystals are monoclinic, space group P21/c, with a 11.984(5), b 8.836(4), c 19.609(7) Ǻ, β 110.58(2)�, Z 4. The structure has been refined to weighted and unweighted R-factors of 0.068 and 0.063, respectively, for the 1616 independent reflections with I/σ(I) ≥ 3.0. Hydrogen atoms could not be located and have not been included in the scattering model. There is considerable steric strain within the substituted pyrroline ligand, and the C=N distance is 1.293(8) Ǻ. Surprisingly, the methyl groups in the 4- and 5-positions are in a cisoid configuration (the torsion angle for the methyl groups about the 4-5 bond is 39.5�), and consequently the hydroxyl oxygen atoms are close [O-O distance, 2.583(8) Ǻ]; this suggests that there may be a bridging hydrogen atom.

Crystal and molecular structure of a cobalt(III) ammine complex of 2-Amino-4-imino-2-methylpentanoic acid

1975 ◽  
Vol 28 (4) ◽  
pp. 729 ◽  
Author(s):  
GB Robertson ◽  
PO Whimp
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Complex Cation ◽  
Three Dimensional ◽  
Cobalt Atom ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Ammine Complex ◽  
Coordination Sites ◽  
Acid Ligand

The crystal and molecular structure of a cobalt(III) ammine complex of 2-amino-4-imino-2-methyl-pentanoic acid, [Co(NH3)3{HN=C(CH3)CH2C(CH3)(NH2)(CO2)}]S2O6, has been determined from three-dimensional X-ray data collected by counter methods. The complex crystallizes in the monoclinic space group P21/c (C52h, No. 14), with a = 7.576(4), b = 18.209(7), c = 14.068(6) Ǻ, β = 125.25(2)�, Z = 4. The structure was solved by conventional Patterson and Fourier methods, and was refined by block-diagonal least-squares methods to weighted and unweighted 12-factors of 0.041 and 0.040 respectively, for the 1479 unique reflections having I/σ(I) ≥ 3.0. All hydrogen atoms have been located and refined. The complex cation is essentially octahedral about the central cobalt atom with three amine groups occupying mutually cis coordination sites; the three remaining sites at the cobalt atom are occupied by the tridentate 2-amino-4-imino-2-methylpentanoic acid ligand. The Co-O distance is 1.914(4) Ǻ, while the Co-N(imine) distance is 1.924(5) Ǻ. The Co-N(NH3) distances range from 1.968(5) to 1.979(5) Ǻ, and are equal within experimental error. Within the tridentate 2- amino-4-imino-2-methylpentanoic acid ligand, the C=N distance is 1.252(7) Ǻ, while at the carboxyl group the ?free? C-O distance [1.233(6) Ǻ] is significantly shorter than the distance from the carbon to the coordinated oxygen atom [1.270(7) Ǻ]. In the S2O6 counter anion, the S-S distance is 2.112(2) Ǻ, and the S-O distances range from 1.434(6) to 1.457(4) Ǻ, averaging 1.439 Ǻ.

Perchlorato, Nitrato, and Acetylacetonato Complexes of Copper(I). The Crystal and Molecular Structure of Perchloratobis(tricyclohexyiphosphine)Copper(I)

1975 ◽  
Vol 53 (13) ◽  
pp. 1949-1957 ◽  
Author(s):  
Roderic J. Restivo ◽  
Abraham Costin ◽  
George Ferguson ◽  
Arthur J. Carty
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Infrared Spectra ◽  
Copper Atom ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Cell Dimensions

Copper(I) perchlorate, nitrate, and acetylacetonate complexes of the types Cu(triphos)ClO4 (triphos = CH3C(CH2PPh2)3), Cu(Cy3P)2ClO4 (Cy3P = P(C6H11)3), Cu(triphos)NO3, Cu(Cy3P)2(HFac)(HFac = hexafluoroacetylacetonate), and Cu (Cy3P)2(TtFac) (TtFac = thienyltrifluoroacetylacetonate) have been synthesized by reduction of the corresponding perchlorate, nitrate, and acetylacetonates with tertiary phosphines. Infrared spectra indicate the presence of monodentate perchlorate groups in Cu(triphos)ClO4 and in Cu(Cy3P)2ClO4 and the crystal structure of the latter has been determined by a three-dimensional X-ray analysis using diffractometer data. The crystals are monoclinic, space group C2/c, with cell dimensions a = 18.159(6), b = 9.493(2), c = 22.182(3) Å, and β = 95.41(2)° and four molecules per unit cell. The structure was refined by block-diagonal least squares methods to a final R of 0.051 for 2617 reflections using anisotropic thermal parameters for the nonhydrogen atoms. The structure consists of discrete Cu(Cy3P)2ClO4 molecules with symmetry C2 separated by normal van der Waals distances. The copper atom is three-coordinate and the perchlorate anion is monodentate but disordered over two sites. Principal dimensions include: Cu—P 2.262(1) Å, Cu—O 2.220(7) Å, [Formula: see text][Formula: see text] and 99.8(2)°, and [Formula: see text]

An Intermediate in the Conversion of an Acetylene to a Vinyl Derivative: The Crystal and Molecular Structure of trans-Chloromethylbis(trimethylarsine)-platinum(II) Hexafluorobut-2-yne

1972 ◽  
Vol 50 (14) ◽  
pp. 2276-2284 ◽  
Author(s):  
Brian W. Davies ◽  
Richard J. Puddephatt ◽  
Nicholas C. Payne
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Free Ligand ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Monodentate Ligand ◽  
X Ray ◽  
Trigonal Bipyramidal

The crystal and molecular structure of trans-chloromethylbis(trimethylarsine)platinum(II) hexafluorobut-2-yne has been determined from three dimensional X-ray diffraction data recorded by diffractometric methods. The structure has been refined by full-matrix least-squares methods on F using 1156 reflections to an agreement factor R = 0.077. The crystals are monoclinic, space group [Formula: see text] with a = 6.803(8), b = 14.93(2), c = 20.20(2) Å, β = 104.9(1)°, and Z = 4. The coordination of the platinum atom is trigonal bipyramidal, with the acetylene considered a monodentate ligand, and the two trimethylarsine ligands occupying the equatorial plane. The chlorine atom and the methyl ligand occupy the apical positions, with Pt—Cl and Pt—C distances of 2.47(1) Å and 2.10(4) Å, respectively. The long Pt—Cl bond length indicates the strong trans-influence of the methyl ligand. The observed C—C bond length of 1.32(4) Å in the acetylene ligand is lengthened from the value of 1.22(9) Å measured in the free ligand. The geometry of the coordinated ligand is discussed in terms of the bonding scheme proposed by Greaves etal.

The Crystal and Molecular Structure of trans-Dichloro-mer-trans-bis (triisopropylphosphine)(phosphine)hydridoiridium(III)

1995 ◽  
Vol 48 (7) ◽  
pp. 1277 ◽  
Author(s):  
EJ Ditzel ◽  
GB Robertson
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Crystal And Molecular Structure ◽  
Structure Refinement ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
X Ray ◽  
Molecular Dimensions

The structure of mer-trans-(PPri3)2(PH3)H-trans-Cl2IrIII (1) (Pri = isopropyl), the second third-row transition-metal-PH3 complex to be so characterized, has been determined by single-crystal X-ray diffraction analysis. Crystals are monoclinic, space group C 2/c with a 21.701(2), b 8.735(1), c 15.594(1) Ǻ, β 119.57(1)° and Z 4. Structure refinement by full-matrix least-squares analysis (2811 reflections, 113 parameters) converged with R = 0.016 and Rw = 0.022. Molecules exhibit crystallographically imposed C2 symmetry. The C2 axis passes through the iridium, hydride and PH3 phosphorus atoms, and requires the PH3 hydrogen atoms to be disordered. Important molecular dimensions are Ir-PPri3 2.371(1) Ǻ, Ir-PH3 2.362(1) Ǻ, Ir-Cl 2.374(1) Ǻ and P- Ir -P(trans) 163.21(3)°.

The Crystal and Molecular Structure of Acetamidopentaamminecobalt(III) Perchlorate. A Conjugate Base of Nitrogen Bonded Acetamide

1973 ◽  
Vol 51 (13) ◽  
pp. 2180-2185 ◽  
Author(s):  
Michael Louis Schneider ◽  
George Ferguson ◽  
Robert James Balahura
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Amide Group ◽  
Ground State Structure ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray ◽  
Octahedral Cations ◽  
Conjugate Base

The crystal and molecular structure of acetamidopentaamminecobalt(III) perchlorate, [CH3CONHCo(NH3)5]2+•2ClO4−, has been determined from three-dimensional X-ray data obtained by diffractometer methods. The crystals are monoclinic, space group [Formula: see text] with four formula units in a unit cell of dimensions a = 13.250(6), b = 10.318(6), c = 10.676(5) Å, β = 98.34(3)°. The structure has been refined by block-diagonal least-squares methods with anisotropic thermal parameters to a final residual R of 0.055 for 1340 observed reflexions. The crystal structure consists of discrete octahedral cations and tetrahedral perchlorate anions. The Co—N (amide) distance is short (1.911(8) Å) while the trans Co—N (ammine) bond is long (1.994(8) Å) compared to the equatorial Co—N distances which average 1.963(13) Å. The bond distances in the amide group, C—O 1.267(12) Å and C—N 1.339(12) Å, indicate that a delocalized system plays an important role in the ground state structure of the cation.

Crystal and molecular structure of a platinum(0) complex of cyclooctyne

1980 ◽  
Vol 33 (6) ◽  
pp. 1373 ◽  
Author(s):  
GB Robertson ◽  
PO Whimp
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Space Group ◽  
X Ray ◽  
Coordination Sites ◽  
Square Planar ◽  
R Factors ◽  
Normal Bond ◽  
Least Squares Techniques

The crystal and molecular structure of a platinum(0) complex of cyclooctyne, [(coct)Pt(PPh3)2], has been determined from three- dimensional X-ray data collected by counter methods. The complex crystallizes in the space group P21/n [a non-standard setting of space group P21/c (C2h5, No. 14)], with a 20.660(9), b 12.299(5), c 15.470(7) Ǻ, β 110.26(2)°, Z 4. The structure was solved by conventional Patterson and Fourier methods and was refined by block-diagonal least-squares techniques to weighted and unweighted R-factors of 0.048 and 0.047 respectively, for the 4733 unique reflections with I/σ(I) ≥ 3.0. The molecule is essentially square planar about the 'central' platinum atom, with the triphenylphosphine groups occupying cis coordination sites. The Pt-C distances are equal within experimental error [2.034(9) and 2.037(9) Ǻ] and compare favourably with the corresponding distances in the platinum(0)-cyclohexyne and -cycloheptyne analogues. The acetylenic C=C distance is 1.279(13) Ǻ and shows the normal bond lengthening consequent upon coordination.

Cyclische Diazastannylene, III1 Die Kristall-und Molekülstruktur der monoklinen Phase von 1.3-Di-tert-butyl-2.2-dimethyl-1.3.2.4λ2 -diazasilastannetidin / The Crystal and Molecular Structure of the Monoclinic Phase of 1,3-Di-feri-butyl-2,2-dimethyl-1,3,2,4λ2 -diazasilastannetidine

1978 ◽  
Vol 33 (1) ◽  
pp. 7-13 ◽  
Author(s):  
M. Veith
Keyword(s):  
Molecular Structure ◽  
Monoclinic Phase ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Site Symmetry ◽  
Space Group ◽  
X Ray ◽  
Tert Butyl ◽  
Cell Dimensions

Abstract The crystal and molecular structure of the monoclinic phase of 1,3-di-tert-butyl-2,2-dimethyl-1,3,2,4λ2 -diazasilastannetidine has been determined from three-dimensional X-ray data collected on a two-circle diffractometer at -120 °C (MoKa radiation, 2623 reflexions, R - 0,050). The crystals are monoclinic, space group C2/c, with cell dimensions a = 10.655(5), b = 25.75(1), c = 17.33(1) Å, β = 106.8(1)° and Z = 12. Four monomeric (crystal site symmetry 2 (C2)) and four dimeric units (crystal site symmetry 1̄ (Ci)) are present in the structure interacting over tin-tin (3.68 Å). Remarkable are the very short Sn-N bond (2.09 Å) in the monomer and the donation bond Sn-N (2.39 Å) in the dimer. The coordination of the tin atoms in the different units is discussed in detail.

Crystal Structure of (NH4)2[Mo3S(S2)6] Containing the Novel Isolated Cluster [MO3S13]2-

1979 ◽  
Vol 34 (3) ◽  
pp. 434-436 ◽  
Author(s):  
A. Müller ◽  
S. Pohl ◽  
M. Dartmann ◽  
J. P. Cohen ◽  
J. M. Bennett ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Ammonium Salt ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
The Novel ◽  
Mean Values ◽  
X Ray

Abstract The novel tri-nuclear metal-sulfur cluster [Mo3S(S2)6]2- can be obtained as its ammonium salt by the reaction of a Moiv containing aqueous solutions with polysulfide. Its crystal and molecular structure has been determined by a single crystal X-ray study. The crystals are monoclinic (space group Cm, with a = 11.577(6) Å, b = 16.448(7) Å, c = 5.716(2) Å, β = 117.30(3)°, V = 967.2 Å3 , Z = 2, dexptl. = 2.54(2) g/cm3 , dcal = 2.54 g/cm3). The structure consists of isolated [Mo3S(S2)6]2- units, with three Mo atoms at the vertices of a triangle. There are bridging as well as terminal S22--ligands lying above and below the Mo3-plane (bond distances: Mo-Mo = 2.722 Å, Mo-S(terminal) = 2.435, Mo-S(bridging) = 2.452, Mo3-S = 2.353(4) Å and S-S = 2.04 Å (mean values)).

Kristall- und Molekülstruktur von 2-[3-(N,N-Diethylammonium)propylimino]-2-phenyl-dithioacetat / Crystal and Molecular Structure of 2-[3-(N,N-Diethylammonium)propylimino]-2-phenyl-dithioacetate

1995 ◽  
Vol 50 (1) ◽  
pp. 81-85 ◽  
Author(s):  
Frank W. Heinemann ◽  
Helmut Hartung ◽  
Nadja Maier
Keyword(s):  
Molecular Structure ◽  
Hydrogen Atom ◽  
Structure Determination ◽  
Crystal And Molecular Structure ◽  
Amino Nitrogen ◽  
Orthorhombic Space Group ◽  
Imino Nitrogen ◽  
X Ray ◽  
Lattice Constants

The title compound, formed by the reaction of acetophenone with 3-diethylamino-1-propylamine and sulfur, crystallizes in the orthorhombic space group P212121 (Z = 4) with lattice constants a = 818.1(2) pm, b = 1225.1(2) pm and c = 1622.4(4) pm. The characterization of the molecule as a zwitterion is established by the observed bond parameters. Both spectroscopic investigations and the results of the X-ray structure determination show that a hydrogen atom is bonded to the amino nitrogen rather than to the imino nitrogen.

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.

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