Crystal and Molecular Structure of tetrakis(4-Methylpyridine)nickel(II)perchlorate, [Ni(II)(C6H7N)4][ClO4]2

1973 ◽  
Vol 51 (12) ◽  
pp. 1952-1958 ◽  
Author(s):  
N. Bose ◽  
H. Lynton
Keyword(s):  
Molecular Structure ◽  
Hydrogen Atom ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Nickel Atom ◽  
Monoclinic Space Group ◽  
Perchlorate Ion ◽  
Square Planar ◽  
Final Agreement ◽  
Atomic Parameters

Crystals of tetrakis(4-methylpyridine)nickel(II)perchlorate, Ni(C6H7N)4(ClO4)2, are monoclinic, space group C2/c, with a = 18.38(1), b = 10.71(1), c = 15.58(1) Ǻ, β = 109.83(5)°, and four molecules in the unit cell. The final atomic parameters were obtained from a block-diagonal least squares refinement using anisotropic thermal parameters. The hydrogen atom positions were established but the parameters were not refined. The final agreement residual for 1199 observed reflections is R = 0.049. The structure consists of discrete Ni(C6H7N)42+ and ClO4− groups. The perchlorate ion is disordered. The 4-methyl-pyridine rings are in a square planar arrangement about the nickel atom.

Crystal and Molecular Structure of Hexaaquocobalt(II)–Hexafluorosilicate(IV), [Co(H2O)6][SiF6]

1973 ◽  
Vol 51 (2) ◽  
pp. 227-229 ◽  
Author(s):  
H. Lynton ◽  
P-Y. Siew
Keyword(s):  
Molecular Structure ◽  
Hydrogen Atom ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Thermal Parameters ◽  
Final Agreement ◽  
Heavy Atom Method ◽  
Atomic Parameters

The structure of hexaaquocobalt(II)-hexafluorosilicate(IV) has been determined by the heavy atom method. The compound crystallizes in the space group [Formula: see text], with three molecules in the hexagonal unit cell of dimensions a = 9.358(16), c = 9.712(14) Å. The atomic parameters were refined by block diagonal least squares using anisotropic thermal parameters. The hydrogen atom positions were established but the parameters were not refined. The final agreement residual for 151 observed reflections is R = 0.043.The structure consists of discrete Co(H2O)62+ and (SiF6)2− octahedra joined systematically by [Formula: see text] hydrogen bonds into chains parallel to the [Formula: see text] axis.

Crystal and Molecular Structure of Dichlorobis(4-methylpyridine)zinc(II), Zn(4-CH3Py)2Cl2

1971 ◽  
Vol 49 (21) ◽  
pp. 3418-3424 ◽  
Author(s):  
H. Lynton ◽  
M. C. Sears
Keyword(s):  
Molecular Structure ◽  
Hydrogen Atom ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
Thermal Parameters ◽  
Zinc Atom ◽  
Final Agreement ◽  
Atomic Parameters ◽  
Block Diagonal

Crystals of dichlorobis(4-methylpyridine)zinc(II), Zn(4-CH3Py)2Cl2, are monoclinic, space groupP21/c, with a = 14.294(13), b = 7.885(8), c = 13.473(11) Å, β = 100.60(5)° and 4 molecules in the unit cell. The final atomic parameters were obtained from a block-diagonal least squares refinement using anisotropic thermal parameters. The hydrogen atom positions were established but the parameters were not refined. The final agreement residual for 1348 observed reflections is R = 0.043. The zinc atom is tetrahedrally coordinated.

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.

scholarly journals The crystal and molecular structure of NaBF3OH

1970 ◽  
Vol 48 (3) ◽  
pp. 405-409 ◽  
Author(s):  
M. J. R. Clark ◽  
H. Lynton
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Hydroxyl Group ◽  
Hexagonal System ◽  
X Ray ◽  
Cell Parameters ◽  
Anisotropic Temperature ◽  
Final Agreement ◽  
Atomic Parameters

The crystal and molecular structure of sodium hydroxytrifluoborate, NaBF3OH, has been established by X-ray analysis. This compound crystallizes in the hexagonal system, space group P63 with cell parameters a = 8.084 Å and c = 7.958 Å. There are 6 molecules in the unit cell. Atomic parameters have been obtained from a block-diagonal least-squares refinement using anisotropic temperature parameters for boron and fluorine, and isotropic temperature parameters for sodium. The final agreement residual for 195 observed reflections is R = 0.090.The [BF3OH]− anions are distorted tetrahedra. It was not possible to distinguish between the positions of the fluorine atoms and the isoelectronic hydroxyl group.

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 and molecular structure of anti-1,2,4,5-tetraphenyl-3,6-dicarbomethoxytricyclo[3.1.0.02,4]hexane

1978 ◽  
Vol 56 (10) ◽  
pp. 1364-1367 ◽  
Author(s):  
M. J. Bennett ◽  
J. T. Purdham
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Experimental Error ◽  
Crystal And Molecular Structure ◽  
Structural Data ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
Bond Lengths ◽  
Highly Strained ◽  
Least Squares Techniques

1,2,4,5-Tetraphenyl-3,6-dicarbornethoxytricyclo[3.1.0.02,4]hexane crystallizes in the monoclinic space group P21/c with a = 10.044(4), b = 9.500(2), c = 14.172(4) Å, β = 104.38(2)°, and Z = 2. Using 1032 unique reflections with I > 3σ(I), the structural data were refined by full matrix least-squares techniques to R = 0.038. The molecule was found to be in the anti-configuration. All bond lengths within the highly strained central tricyclic framework were equal within experimental error and average 1.531 Å.

Crystal and Molecular Structure of Dithiocyanato(triphenylarsine)mercury(II)

1975 ◽  
Vol 53 (22) ◽  
pp. 3383-3387 ◽  
Author(s):  
Joseph Hubert ◽  
André L. Beauchamp ◽  
Roland Rivest
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Coordination Number ◽  
Diffraction Data ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Heavy Atom Method

The crystal and molecular structure of dithiocyanato(triphenylarsine)mercury(II) has been determined from X-ray diffraction data. The crystals are monoclinic, space group P21/c, with a = 10.290(7), b = 21.199(23), c = 10.719(7) Å, β = 112.00(2)°, and Z = 4. The structure has been solved by the heavy-atom method and refined by block-diagonal least-squares calculations. The agreement factor R obtained for 2607 'observed' reflections is 0.030. The crystal consists of single molecules. The 'characteristic' coordination number of mercury is three, with two sulfur and one arsenic atoms at the apexes of a triangle. The nitrogen atoms of the thiocyanate groups are at 2.67 and 2.74 Å from the adjoining mercury atoms and therefore link the different molecules together.

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.

Crystal and Molecular Structure of Difluorochlorine(III)-hexafluoroarsenate(V), ClF2AsF6

1971 ◽  
Vol 49 (15) ◽  
pp. 2539-2543 ◽  
Author(s):  
H. Lynton ◽  
J. Passmore
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Chlorine Atom ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Arsenic Atom ◽  
Space Group

Crystals of difluorochlorine(III)hexafluoroarsenate(V), ClF2AsF6, are monoclinic, space group A2/a, a = 10.676(9), b = 7.673(7), c = 8.064(7) Å, β = 113.40(5)°. The structure was refined by three dimensional least squares methods to R = 0.045 for 185 independent observed reflections. The chlorine atom has two nearest fluorine neighbors at 1.541(14) Å, with a F—Cl—F angle of 103.17(0.70)°, and two longer fluorine bonds at 2.339(14) Å. All five atoms lie in a plane. The arsenic atom is octahedrally coordinated to six fluorine atoms and is connected to two ClF2+ groups via trans fluorine bridges.

Studies of Some Tetraazacyclopentadecadiene Complexes of Nickel(II). The Crystal and Molecular-Structure of (1RS,8SR)-(5,7,7,13,15,15-Hexamethyl-1,4,8,12-Tetraazacyclopentadeca-4,1 2-Diene)Nickel(II) Perchlorate Hydrate

1986 ◽  
Vol 39 (10) ◽  
pp. 1509 ◽  
Author(s):  
NF Curtis ◽  
GJ Gainsford
Keyword(s):  
Molecular Structure ◽  
Ground State ◽  
Crystal And Molecular Structure ◽  
Macrocyclic Ligand ◽  
Isomeric Form ◽  
Monoclinic Space Group ◽  
Singlet Ground State ◽  
Triplet Ground State ◽  
Square Planar ◽  
Coordination Plane

The crystal and molecular structure has been determined by X-ray diffractometry for the singlet ground state nickel(II) compound of a fifteen- membered tetraaza macrocyclic ligand , formed by reaction of a mixture of tris ( ethanediamine )nickel(II) and tris (propane-1,3- diamine )nickel(II) perchlorates with acetone. The compound, (1RS,8SR)- 5,7,7,13,15,15-hexamethyl-1,4,8,12-tetraazacyclopentadeca-4,12- diene )nickel(II) perchlorate hydrate, [Ni( hmpd )](ClO4)2.H2O, is monoclinic, space group P21/C, a 1158.76(14), b 1319.53(22), c 1630.35(21) pm, β 96.209(10)°, R 0.046, Rw 0.062 for 2798 reflections. The nickel(II) ion is in tetrahedrally distorted square-planar coordination [mean Ni-N distances 188.9 pm ( imine ), 191.9 pm (amine), displacements of nitrogens c. �20 pm from mean coordination plane]. Triplet ground state compounds [Ni( hmpd )( acac )]ClO4 and [{Ni( hmpd )}2C2O4](ClO4)2, with the macrocycle in folded coordination, were prepared and converted into an isomeric form of [Ni( hmpd )](ClO4)2. The 3,5,7,7,13,15,15-heptamethyl homologue of [Ni( hmpd )]2+ was prepared by reaction of tris (propane-1,2-diamine)- and tris (propane-1,3-diamine)- nickel(II) perchlorates with acetone. The electronic (d-d), 1H N.M.R. and 13C N.M.R . spectra of compounds of these macrocyclic cations, and of (5,5,7,13,15,15-hexamethyl-1,4,8,12-tetraazacyclopentadeca-7,12-diene) nickel(II) are reported.

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