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.

Structure cristalline et moléculaire du cis-dithiocyanatobis(phénanthroline-1,10)mercure(II), Hg(SCN)2(C12H8N2)2

1974 ◽  
Vol 52 (16) ◽  
pp. 2923-2927 ◽  
Author(s):  
André L. Beauchamp ◽  
Bernard Saperas ◽  
Roland Rivest
Keyword(s):  
Heavy Atom ◽  
Octahedral Geometry ◽  
Van Der Waals Interactions ◽  
Distorted Octahedral Geometry ◽  
Triclinic Space Group ◽  
Bond Lengths ◽  
R Factor ◽  
Distorted Octahedral ◽  
Phenanthroline Ligands ◽  
Heavy Atom Method

The compound cis-Hg(SCN)2(Phen)2 belongs to the triclinic space group [Formula: see text] with a = 13.252(5), b = 11.077(4), c = 8.443(3) Å, α = 105.20(3), β = 83.25 (3), γ = 90.92(3)°, and Z = 2. The structure was solved by the heavy atom method and refined on 1718 independent reflections to an R factor of 0.069. The crystal contains discrete molecules, in which mercury is coordinated to four nitrogen atoms from two phenanthroline molecules and to two sulfur atoms from thiocyanate groups. These donor atoms define a distorted octahedral geometry around mercury. The Hg—N bond lengths are in the range 2.42(2)–2.52(2) Å, whereas the Hg—S bonds are equal to 2.622(8) and 2.582(8) Å. The molecules are packed in layers parallel to the (110) planes and the layers are held together by normal van der Waals interactions. Within the layers, the packing of the complex is characterized by parallel stacking of phenanthroline ligands at distances of ∼3.4 Å. The terminal nitrogen atoms of the thiocyanate groups are uncoordinated.

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 and molecular structure of [dimethyl(1-pyrazolyl)(2-pyridyl-methoxy)gallato-N2,O,N3](η3-allyl)dicarbonylinolybdenum(II)

1988 ◽  
Vol 66 (3) ◽  
pp. 355-358 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Nitrogen Atom ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Coordination Geometry ◽  
Pyridyl Nitrogen ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of [dimethyl(1-pyrazolyl)(2-pyridylmethoxy)gallato-N2,O,N3](η3-allyl)dicarbonylmolybdenum(II) are triclinic, a = 9.632(2), b = 9.798(2), c = 10.255(2) Å, α = 80.16(1), β = 87.38(1), γ = 81.75(1)°, Z = 2, space group [Formula: see text]. The structure was solved by conventional heavy-atom methods and was refined by full-matrix least-squares procedures to R = 0.033 and Rw = 0.037 for 3000 reflections with I ≥ 3σ(I). The molecule has pseudo-octahedral coordination geometry with the tridentate [Me2Ga(N2C3H3)(OCH2(C5H4N))]− ligand facially coordinated and the η3-allyl ligand occupying one coordination site trans to the pyridyl nitrogen atom. Important bond lengths are Mo—O = 2.219(2), Mo—N(py) = 2.212(3), Mo—N(pz) = 2.232(2), Mo—C(allyl) = 2.290(4), 2.189(4), 2.341(4), Mo—CO (trans to O) = 1.928(4), and Mo—CO (trans to N) = 1.952(4) Å.

Crystal and molecular structure of fac-[dimethylbis(1-pyrazolyl)gallato-N,N′]-(triphenylphosphine)tricarbonylrhenium(I)

1985 ◽  
Vol 63 (3) ◽  
pp. 703-707 ◽  
Author(s):  
Brenda M. Louie ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths ◽  
Independent Molecules ◽  
Twisted Boat ◽  
Chelate Rings

Crystals of fac-[dimethylbis(1-pyrazolyl)gallato-N,N′](triphenylphosphine)tricarbonylrhenium(I) are triclinic, a = 9.479(2), b = 16.258(4), c = 20.412(6) Å, α = 110.06(1), β = 95.46(1), γ = 92.65(2)°, Z = 4, space group [Formula: see text] The structure was solved by conventional heavy-atom methods and was refined by full-matrix least-squares procedures to R = 0.027 and Rw = 0.031 for 5965 reflections with I ≥ 3σ(I). The two crystallographically independent molecules have nearly identical structures. The coordination about Re is distorted fac-octahedral with mean bond lengths: Re—P = 2.538(4), Re—N = 2.201(5), Re—CO(trans to P) = 1.931(1), and Re—CO(trans to N) = 1.913(9) Å. The ReGaN4 chelate rings have twisted boat conformations with cross-ring [Formula: see text] separations of 3.9396(7) and 3.8981(8) Å.

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 and Molecular Structures of Two Modifications of cis-Dichloro-mer-tris-(dimethylphenylphosphine)hydridoiridium(III)

1988 ◽  
Vol 41 (3) ◽  
pp. 283 ◽  
Author(s):  
GB Robertson ◽  
PA Tucker
Keyword(s):  
Heavy Atom ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Metal Ligand ◽  
Ligand Bond

The structures of two crystalline modifications of mer -(Pme2Ph)3H-cis-Cl2IrIII, (1), have been determined from single-crystal X-ray diffraction data. Modification (A) is monoclinic, space group P21/c with a 12.635(1), b 30.605(3), c 14.992(2)Ǻ, β 110.01(2)° and Z = 8. Modification (B) is orthorhombic, space group Pbca with a 27.646(3), b 11.366(1), c 17.252(2)Ǻ and Z = 8. The structures were solved by conventional heavy atom techniques and refined by full-matrix least- squares analyses to conventional R values of 0.037 [(A), 8845 independent reflections] and 0.028 [(B), 5291 independent reflections]. Important bond lengths [Ǻ] are Ir -P(trans to Cl ) 2.249(1) av. (A) and 2.234(1) (B), Ir -P(trans to PMe2Ph) 2.339(2) av. (A) and 2.344(1), 2.352(1) (B), Ir-Cl (trans to H) 2.492(2), 2.518(2) (A) and 2.503(1) (B) and Ir-Cl (trans to PMe2Ph)2.452(2) av. (A) and 2.449(1)(B). Differences in chemically equivalent metal- ligand bond lengths emphasize the importance of non-bonded contacts in determining those lengths.

Structural studies of organoboron compounds. XX.(Salicylaldoximato-O,N)diphenylboron

1984 ◽  
Vol 62 (7) ◽  
pp. 1363-1368 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Hydrogen Bonds ◽  
Least Squares ◽  
Chelate Ring ◽  
Direct Methods ◽  
Structural Studies ◽  
Organoboron Compounds ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths ◽  
Phenolic Oxygen

Crystals of (salicylaldoximato-O,N)diphenylboron are triclinic, a = 10.125(2), b = 10.797(1), c = 14.760(2) Å, α = 89.05(1), β = 86.98(1), γ = 83.18(1)°, Z = 4, space group [Formula: see text]. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.040 and Rw = 0.048 for4145 reflections with I ≥ 3σ(I). The structure consists of two crystallographically independent, but essentially identical, molecules linked by strong [Formula: see text] hydrogen bonds to form continuous spirals along the a axis. The Ph2B moiety is chelated by the phenolic oxygen and oxime nitrogen atoms of the ligand resulting in the formation of a non-planar six-membered chelate ring. Important libration-corrected mean bond lengths are O—B = 1.516(1), N—B = 1.609(2), and C—B = 1.613(2) Å.

The crystal structure and vibrational spectra of cis-dichlorobis(cyclopropylamine)-platinum(II), PtCl2(C3H5NH2)2

1981 ◽  
Vol 59 (18) ◽  
pp. 2737-2745 ◽  
Author(s):  
Helen Elaine Howard-Lock ◽  
Colin James Lyne Lock ◽  
Graham Turner ◽  
Maruta Zvagulis
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Vibrational Spectra ◽  
Vibrational Analysis ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths ◽  
Deuterated Analogue

Crystals of cis-dichlorobis(cyclopropylamine)platinum(II), PtCl2(C3H5NH2)2, are monoclinic, a = 12.770(5), b = 5.838(2), c = 15.113(6) Å, β = 104.46(3)°, Z = 4, space group P21/c. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares to R = 0.057, Rw = 0.055 for 1577 reflections with I > 3σ(I). Bond lengths and angles are normal. A vibrational analysis of the compound and its d2-deuterated analogue was performed.

The Structure of (NO)2[Ho(NO3)5], A 10-Coordinate Species

1975 ◽  
Vol 53 (6) ◽  
pp. 831-835 ◽  
Author(s):  
Gerald E. Toogood ◽  
Chung Chieh
Keyword(s):  
Ethyl Acetate ◽  
Heavy Atom ◽  
Full Matrix ◽  
Trigonal Bipyramidal ◽  
Anhydrous Ethyl Acetate ◽  
Dinitrogen Tetroxide ◽  
Stretching Vibration ◽  
The Mean ◽  
R Value ◽  
Heavy Atom Method

Nitrosonium pentanitratoholmate(III), (NO)2Ho(NO3)5, was prepared from holmium metal and dinitrogen tetroxide in anhydrous ethyl acetate. Its crystals are monoclinic with a = 8.094, b = 11.979, c = 14.170 Å and β = 104.7°,Z = 4, space group P21/c. The structure was solved by the heavy-atom method and refined by full matrix least-squares methods to an R value of 0.085 for 1514 observed reflections measured on the G.E. XRD-6 diffractometer. The structure consists of one Ho(NO3)52− and two NO+ ions. The holmium is 10-coordinated by five essentially symmetric bidentate nitrate groups which arrange themselves in a trigonal bipyramidal fashion around the metal with a mean Ho—O distance of 2.45 Å. The two NO+ ions per metal occupy slightly different environments and give rise to two i.r. bands at 2250 and 2285 cm−1, attributable to the (N, O+) stretching vibration. The mean N—O distance within these ions is 1.00 Å.

Crystal and molecular structure of difluoroboron N-methylacethydroxamate (2,2-difluoro-4,5-dimethyl-1,3-dioxa-4-azonia-2-boranatacyclopent-4-ene)

1977 ◽  
Vol 55 (1) ◽  
pp. 1-7 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter ◽  
W. Kliegel ◽  
D. Nanninga
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of difluoroboron N-methylacethydroxamate are monoclinic, a = 5.097(1), b = 10.653(2), c = 11.520(2) Å, β = 103.57(2)°, Z = 4, space group P21/c. The structure was solved by direct methods and was refined by full-matrix least squares procedures to a final R of 0.056 and Rw of 0.077 for 988 reflections with I ≥ 3σ(I). The structure features a planar five-membered BO2CN ring. Bond lengths (corrected for libration) are: B—F, 1.374(3) and 1.381(3), O—B, 1.496(3) and 1.497(3), O—N, 1.349(2), O—C, 1.346(2), C—N, 1.298(3) and 1.458(3), and C—C, 1.468(3) Å.

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