The crystallochemistry of tetracyanocomplexes. The crystal and molecular structure of Cd(NH3)2Ni(CN)4.0·5 H2O

1987 ◽  
Vol 52 (8) ◽  
pp. 1915-1921 ◽  
Author(s):  
Charles Kappenstein ◽  
Juraj Černák
Keyword(s):  
Molecular Structure ◽  
Water Molecule ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
Water Molecules ◽  
Intermolecular Distances

Cd(NH3)2Ni(CN)4.0·5 H2O is orthorhombic, Imma, with parameters a = 0·7622(4), b = 1·4992(13), c = 0·8961(6) nm, Z = 4, d(exp) = 2·07(4), d(calc.) = 2·066 Mg m-3. The structure, which was refined by the least squares method to R = 0·038 for 1 508 independent reflections, is isostructural with Ni(NH3)2Ni(CN)4.0·5 H2O and consists of infinite layers of the [Cd(NC)4Ni] type. Two water molecules in the unit cell occupy 4 equivalent positions between the layers. The shortest intermolecular distances 0·3023(2) (H2O···Ni) and 0·3371(1) nm (H2O···NH3) indicate zeolitic character of the water molecule.

The crystal structure of nickel(II) dimethyldithiocarbamate

1980 ◽  
Vol 45 (8) ◽  
pp. 2147-2151 ◽  
Author(s):  
Jan Lokaj ◽  
Ján Garaj ◽  
Viktor Kettmann ◽  
Viktor Vrábel
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structural Analysis ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
Special Position ◽  
X Ray ◽  
Triclinic Unit Cell

Crystal and molecular structure of nickel(II) dimethyldithiocarbamate, Ni[S2CN(CH3)2]2 was solved by X-ray structural analysis and refined by the least squares method to R = 0.06 for 1065 reflections. The compound crystallizes in a space group P I and the triclinic unit cell has the dimensions: a = 6.521 (7), b = 6.798 (9), c = 7.633 (4), α = 67.21 (8)°, β = 67.34 (6)° γ =85.59 (9)°. The experimentally observed density is 1.75 g cm-3 and the calculated value for Z = 1 is 1.73 g cm-3. In the structure , the Ni atom occupies a special position in the centre of symmetry and is coordinated by four sulphur atoms in a plane: Ni-S 0.2218 (4) and 0.2198 nm S1-Ni-S2 angle 79.62 (8)°. The ligand S2CNC2 is nearly planar.

The crystal and molecular structure of 1,1-bis(diphenylphosphino)-2,2-dimethylhydrazine

1976 ◽  
Vol 54 (5) ◽  
pp. 738-743 ◽  
Author(s):  
J. Brian Faught
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
Space Group ◽  
Block Diagonal

The structure of 1,1-bis(diphenylphosphino)-2,2-dimethylhydrazine, [(C6H5)2P]2NN(CH3)2 has been determined crystallographically. The compound crystallizes from n-heptane in the space group P21/c with a = 8.910(1), b = 9.686(1), c = 27.489(4) Å, and β = 102.94(2)° with four molecules per unit cell. The structure was solved from 2669 independent reflections with I > 3σ(I) and refined by block diagonal least squares methods to R = 0.032 and Rω = 0.048. Each diphenylphosphino group is bonded to the same hydrazine nitrogen and the geometry about this nitrogen is nearly planar. The average dimensions of the structure are P—C = 1.828 ± 0.005, P—N = 1.715 ± 0.014, N—N = 1.451, and N—C = 1.457 ± 0.003 Å, [Formula: see text], [Formula: see text], [Formula: see text], [Formula: see text], and [Formula: see text].

Crystal and molecular structure of 3-ethyl-4-hydroxy-1,2,3(4H)-benzotriazine and 6-chloro-4-hydroxy-3-methyl-4-phenyl-1,2,3-benzotriazine

1985 ◽  
Vol 63 (3) ◽  
pp. 581-585 ◽  
Author(s):  
Kwong Khee Lai ◽  
Carl H. Schwalbe ◽  
Keith Vaughan ◽  
Ronald J. Lafrance ◽  
Clive D. Whiston
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Tetrahedral Geometry ◽  
Orthorhombic System ◽  
Full Matrix ◽  
X Ray ◽  
R Factor

The crystal structures of the title compounds have been determined from X-ray data collected on a four-circle diffractometer and refined by the full-matrix least-squares method. The former compound crystallizes in the orthorhombic system, space group Pbcn, with a = 14.346(8), b = 7.239(1), c = 17.276(2) Å, and has been refined to a conventional R factor of 0.043 for 890 observed reflections. Corresponding results for the latter compound are monoclinic, P21/n, a = 12.222(4), b = 7.482(2), c = 14.170(8) Å, β = 94.06(4)°, R = 0.060 for 2128 observed data. The triazine rings of both compounds exhibit short N(1)—N(2) bonds and tetrahedral geometry at C(4); however, the ring is puckered in the first compound but flat in the second. Molecules in both crystals are linked by [Formula: see text] hydrogen bonds.

3-Methylpyridine complexes of cobalt(II) and nickel(II) hexafluorophosphate and hexafluoroarsenate. Crystal and molecular structure of Ni(H2O)2(3-CH3C5H4N)6(PF6)2

1983 ◽  
Vol 61 (7) ◽  
pp. 1651-1658 ◽  
Author(s):  
Raymond M. Morrison ◽  
Robert C. Thompson ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Hydrogen Atom ◽  
Water Molecule ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Water Molecules ◽  
Magnetic Studies ◽  
Full Matrix ◽  
Mild Conditions ◽  
Square Planar

Reaction of aqueous solutions containing CO2+ or Ni2+ and PF6−, or AsF6− with excess 3-methylpyridine yields crystals of compounds of composition M(H2O)2(3mpy)6(EF6)2. Blue crystals of diaquohexakis(3-methylpyridine)nickel(II) hexafluorophosphate, C36H46F12NiN6O2P2, are monoclinic, a = 10.497(1), b = 20.074(3), c = 21.836(5) Å, β = 103.93(2)°, Z = 4, space group Cc. The structure was determined with MoKα CAD4 diffractometer data by direct methods, and refined by full-matrix least-squares procedures to R = 0.048 for 2723 reflections with I ≥ 3σ(I). The structure consists of {Ni(3mpy)4[(OH2)(3mpy)]2}2+ cations and PF6− anions. The cation contains a NiN4O2 chromophore with water molecules occupying trans positions of a distorted octahedron about nickel. One additional 3-methylpyridine molecule is H-bonded to each of the water molecules with [Formula: see text] distances of 2.717(11) and 2.719(11) Å. Weak interaction of each water molecule via its second hydrogen atom with a PF6− ion is indicated by the positioning of the anions. The [Formula: see text] distances are 2.958(11) and 2.959(11) Å. Two other complexes of this type, where M is Ni and E is As and where M is Co and E is P, are reported here and on the basis of spectroscopic and magnetic studies are assigned structures similar to the Ni/P complex.Decomposition of the aquo complexes under mild conditions yields compounds of composition M(3mpy)4(EF6)2. Ni(3mpy)4(PF6)2 is assigned a square planar structure with weakly interacting PF6−, anions in axial positions. Both Co(3mpy)4(EF6)2 complexes, where E is P or As, have tetrahedral [Co(3mpy)4]2+ cations and non-coordinated anions.

The crystal and molecular structure of tris-butyl-tin(IV)-(1-pyrrolidinecarbodithioato)-3-propionate

1989 ◽  
Vol 54 (3) ◽  
pp. 684-690 ◽  
Author(s):  
Jan Lokaj ◽  
Viktor Vrábel ◽  
Eleonóra Kellö ◽  
Vladimír Ratay
Keyword(s):  
Molecular Structure ◽  
Structural Analysis ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Analysis Method ◽  
Monoclinic System ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal and molecular structure of Bu3Sn(pyrn-dtc-prop) was solved by the X-ray structural analysis method and refined by the block diagonal least squares method to R = 0.053 for 1 930 observed reflections. The compound crystallizes in the monoclinic system with a space group of P21/c, Z = 4, F(000) = 1 056, with unit cell dimensions of a = 1.4758(5), b = 0.9970(3), c = 1.9166(6) nm; β = 113.90(2)°. The measured and calculated crystal densities were Dm = 1.32 and Dc = 1.31.103 kg m-3. The tin atom is coordinated by three carbon atoms at distances of Sn-C 0.2117(8), 0.2133(8), 0.2158(11) nm and two oxygen atoms O(1) and O(2) at distances of Sn-O 0.2210(5) and 0.2399(5) nm. The coordination polyhedron is a deformed trigonal bipyramid. The S2CN ligand is approximately planar.

Die Kristall- und Molekülstruktur von β -Bromo(2-diäthylaminoäthanolato)kupfer(ll) / The Crystal and Molecular Structure of β-Bromo(2-diethylaminoethanolato)copper(II)

1975 ◽  
Vol 30 (1-2) ◽  
pp. 14-18 ◽  
Author(s):  
R. Mergehenn ◽  
L. Merz ◽  
W. Haase
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Unit Cell ◽  
Triclinic Space Group ◽  
Polymeric Structure ◽  
Space Group ◽  
X Ray

The crystal and molecular structure of β-bromo(diethylaminoethanolato)copper(II) has been determined from three dimensional X-ray diffractometer data. The compound crystallizes in the triclinic space group Pï with one dimer in a unit cell of dimensions α=10.180(II), b=7.999(9), c=6.227(7) Å and a=110.69(4), β=103.12(4), γ=73.82(4)[°]. The structure was refined by least-squares methods using 1944 independent reflexions to give a final R-index of 0,05. The molecule consists of dimeric Cu2O2-units with Cu—O distances of 1.900(4) Å and 1.914(4) A, respectively. The dimers are additional bridged by bromines, so that a “polymeric” structure results; Cu—Br distances are 2.357(2) and 3.660(2) A, respectively. The Cu—Cu distances are 3.003(2) (oxygen bridges) and 4.506(2) Å (bromine bridges).

Crystal and molecular structure of the tetradecahydrate of cobalt(II) (R,S)-ethylenediamine-N,N'-disuccinato-cobaltate(III)

1980 ◽  
Vol 45 (6) ◽  
pp. 1766-1774 ◽  
Author(s):  
František Pavelčík ◽  
Jiřina Soldánová ◽  
Jaroslav Majer
Keyword(s):  
Molecular Structure ◽  
Oxygen Atom ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Cobalt Atom ◽  
Carboxyl Groups ◽  
Water Molecules ◽  
Crystal Water ◽  
Heavy Atom Method

Crystals of Co3((R,S)-EDDS)2 . 14 H2O are monoclinic with lattice parameters a = 1.1393, b = 1.1856, c = 1.5267 nm, β = 114.6°. The space group is P21/c, Z = 2. The structure was solved by the heavy atom method and refined by the least squares method to R = 0.082. The crystals are composed of binuclear [CO2((R,S-EDDS)2]2- anions, [CO(OH2)6]2+ cations and crystal water molecules. The cobalt atom in [Co2((R,S)-EDDS)2]2- is coordinated octahedrally by two nitrogen atoms and three oxygen atoms from different carboxyl groups in a single [(R,S)-EDDS]4- molecule and one oxygen atom from a neighbouring [(R,S)-EDDS]4- molecule. The [Co(OH2)6]2+ cation is coordinated octahedrally.

Crystal and molecular structure of CuSiF6•4H2O

1969 ◽  
Vol 47 (20) ◽  
pp. 3859-3861 ◽  
Author(s):  
M. J. R. Clark ◽  
J. E. Fleming ◽  
H. Lynton
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Fluorine Atom ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
Space Group ◽  
Anisotropic Temperature ◽  
Cell Dimensions ◽  
Final Agreement ◽  
Atomic Parameters

The structure of CuSiF6•4H2O has been shown to consist of chains of [Cu(H2O)4F2] and [SiF6] octahedra linked through a common fluorine atom. The space group is monoclinic P21/a, with cell dimensions a = 7.22 ± 0.01 Å, b = 9.64 ± 0.01 Å, c = 5.36 ± 0.01 Å and β = 105.2 ± 0.3°. There are 2 molecules in the unit cell and the copper and silicon atoms occupy centers of symmetry. Atomic parameters have been obtained from a block diagonal least squares refinement using anisotropic temperature parameters. The final agreement residual for 574 observed reflections is R = 0.083.

The crystal and molecular structure of fluorene

1955 ◽  
Vol 227 (1169) ◽  
pp. 200-214 ◽  
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Experimental Error ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
Carbon Skeleton ◽  
Two Dimensional ◽  
Trial And Error ◽  
Orthorhombic System ◽  
Space Group

Fluorene, C 13 H 10 , crystallizes in the orthorhombic system, space group Pnam with four molecules per unit cell. The molecule possesses a plane of symmetry which is parallel to the (001) plane of the crystal. The structure has been determined by trial-and-error methods, followed (i) by a least-squares refinement and (ii) by two-dimensional Fourier syntheses. The results from the two methods of refinement are compared and for (ii) a method is given for systematically correcting for overlapping of atoms in projections. The accuracy of the co-ordinates given by these methods is discussed in detail, and it is concluded that the co-ordinates adopted are correct to ±0.017 Å. The carbon skeleton is planar to within the experimental error and the equation of the plane is y = 1.4375 x + 11.0947.

Studies of β-Diketone Complexes of Rhenium. VI. The Crystal and Molecular Structure of cis-Dichloropentane-2,4-dionato-trans-bis(triphenylphosphine)rhenium(III)

1974 ◽  
Vol 52 (9) ◽  
pp. 1704-1708 ◽  
Author(s):  
I. D. Brown ◽  
C. J. L. Lock ◽  
Che'ng Wan
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Full Matrix ◽  
X Ray ◽  
Nearest Neighbours

A compound, obtained in large yields from the reaction of acetylacetone and oxodichloroethoxobis(triphenylphosphine)rhenium(V) in benzene, has been shown by single crystal X-ray diffraction to be cis-dichloropentane-2,4-dionato-trans-bis(triphenylphosphine)rhenium(III). The crystals are monoclinic with a = 13.06(1), b = 18.30(1), c = 16.55(1) Å, and β = 112.7(2)°. The space group is P21/c and there are four molecules per unit cell. A total of 3841 independent reflections, of which 2686 were observed, were examined by film methods, the intensities being measured with a microdensitometer. The structure was refined by full matrix least-squares analysis to an R2 value of 0.068. The ligands are arranged around the rhenium atom in the manner described by the compound name to give a rough octahedron of nearest neighbours and the Re—Cl (2.369 Å av.), Re—O (2.02 Å av.), and Re—P (2.474 Å av.) distances are as expected.

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