Calcium-bis[N,N'-bis(trimethylsilyl)benzamidinat]-THF (1/2) - Synthese, spektroskopische Charakterisierung und Struktur/Calcium-bis[N,N'-bis(trimethylsilyl)benzamidinate]-THF (1/2) - Syntheses, Spectroscopic Characterization and Structure

1992 ◽  
Vol 47 (4) ◽  
pp. 453-459 ◽  
Author(s):  
Matthias Westerhausen ◽  
Wolfgang Schwarz
Keyword(s):  
Title Compound ◽  
High Field ◽  
Spectroscopic Characterization ◽  
Calcium Atom ◽  
Space Group ◽  
Bond Lengths ◽  
H Nmr ◽  
Distorted Octahedral ◽  
Anionic Charge ◽  
Field Shift

The reaction of calcium-bis[bis(trimethylsilyl)amide]-THF (1/2) with benzonitrile in THF nearly quantitatively yields the title compound calcium-bis[N,N'-bis(trimethylsilyl)- benzamidinate]-THF (1/2). Under similar conditions pivalonitrile substitutes an ether ligand of calcium-bis[bis(trimethylsilyl)amide]-DME (1/2) without the formation of the corresponding amidinate derivative. The calcium-di(benzamidinate) [H5C6-C(NSiMe3)2]2Ca · 2THF crystallizes in the space group Pbcn with {a = 188.8(6); b = 1286.0(3); c = 1802.5(5) pm; Z = 4}. The calcium atom is hexa-coordinate with a distorted octahedral trans-configuration and with Ca - O and Ca - N bond distances of 238 and 243 pm, respectively. The bond lengths within the NCN moiety with values of 132 pm are characteristic of a diazaallylic system. The short N - Si bond lengths of about 170.5 pm as well as the high field shift of the 29Si{1H} NMR signal are evidence for an effective backdonation of the anionic charge from the nitrogen to the silicon atoms.

Calcium-bis { [tris(trimethylsilyl)silyl]tellanid } · 4 THF-Synthese, spektroskopische Charakterisierung und Struktur / Calcium-bis{[tris(trimethylsilyl)silyl]tellanide} · 4THF-Synthesis, Spectroscopic Characterization and Structure

1992 ◽  
Vol 47 (9) ◽  
pp. 1225-1232 ◽  
Author(s):  
Gerd Becker ◽  
Karl Wilhelm Klinkhammer ◽  
Wolfgang Schwarz ◽  
Matthias Westerhausen ◽  
Thomas Hildenbrand
Keyword(s):  
Coordination Sphere ◽  
Structure Determination ◽  
Spectroscopic Characterization ◽  
Octahedral Coordination ◽  
Trans Position ◽  
Calcium Atom ◽  
X Ray ◽  
H Nmr ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral

Calcium bis{[tris(trimethylsilyl)silyl]tellanide} · 4THF is obtained by metallation of [tris(trimethylsilyl)silyl]tellane using dimeric calcium bis[bis(trimethylsilyl)amide] in toluene, followed by recrystallisation from tetrahydrofuran. The compound is characterized by a remarkable highfield shift of the 125Te{1H}-NMR resonance (-2204 ppm vs. Me2Te). The X-ray structure determination (triclinic, P1; Z = 1; a = 1042.6(2), b = 995.7(2), c = 1379.6(3) pm; α = 90.06(2), β = 92.76(2), γ = 94,03(2)° at -100 °C) shows a distorted octahedral coordination sphere of the calcium atom (Ca-Te 319; Ca-O 236 and 241 pm). The two [tris(trimethylsilyl)silyl]-tellanide ligands are in a trans position; the angle Ca-Te-Si is widened to 129°.

scholarly journals Tris(2-acetylcyclopentan-1-onato-κ2 O,O′)aluminium

2012 ◽  
Vol 68 (6) ◽  
pp. m781-m781
Author(s):  
Franc Perdih
Keyword(s):  
Title Compound ◽  
Thermal Motion ◽  
The Other ◽  
Distorted Octahedral Environment ◽  
Bond Lengths ◽  
Octahedral Environment ◽  
Distorted Octahedral

In the title compound, [Al(C7H9O2)3], the AlIII cation is coordinated by six O atoms from three 2-acetylcyclopentanonate ligands in a slightly distorted octahedral environment, with Al—O bond lengths in the range 1.882 (2)–1.896 (2) Å. In the crystal, molecules are linked together via C—H...O interactions. One of the C atoms in one ring has a large thermal motion compared to the other atoms, indicating some possible disorder. However, the treatment of this C atom as disordered over two positions did not give a significant improvement.

Bis(imidazol-2-yl)phosphinic acid hemihydrate, [(C3H3N2)(C3H4N2)PO2].(1/2)H2O

1989 ◽  
Vol 67 (6) ◽  
pp. 1051-1060 ◽  
Author(s):  
Helen E. Howard-Lock ◽  
Colin J.L. Lock ◽  
Sarah Penny ◽  
Mary A. Turner
Keyword(s):  
Single Crystal ◽  
Vibrational Spectroscopy ◽  
Title Compound ◽  
Phosphinic Acid ◽  
Major Product ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
H Nmr ◽  
Zwitterionic Form

The title compound was obtained as the major product of our handling of the literature preparation of tris(imidazol-2-yl)phosphine. The compound was characterized by 1H NMR, mass and vibrational spectroscopy. The structure was determined by single crystal X-ray diffraction. Crystals were triclinic, [Formula: see text], a = 7.677(1), b = 12.658(2), c = 10.072(2) Å, α = 91.18(1),β = 114.44(1),γ = 99.49(1)°, Z = 4. Intensities were measured on a Syntex P21 diffractometer with MoKα radiation and 3088 reflections were used to determine the structure. R = 0.0698, Rw = 0.0534. The phosphinic acid exists in the solid as the zwitterionic form and bond lengths and angles are normal. Keywords: tris(imidazol-2-yl)phosphine, X-ray structure, bis(imidazol-2-yl)phosphinic acid hemihydrate.

scholarly journals Tris(3-chloropentane-2,4-dionato-κ2 O,O′)iron(III)

2012 ◽  
Vol 68 (6) ◽  
pp. m807-m807
Author(s):  
Franc Perdih
Keyword(s):  
Title Compound ◽  
Rotation Axis ◽  
Distorted Octahedral Environment ◽  
Bond Lengths ◽  
Octahedral Environment ◽  
Distorted Octahedral

In the title compound, [Fe(C5H6ClO2)3], the FeIII cation is situated on a twofold rotation axis and is coordinated by six O atoms from three 3-chloropentane-2,4-dionate ligands in a slightly distorted octahedral environment. Fe—O bond lengths are in the range 1.9818 (18)–1.9957 (18) Å. The trans O—Fe—O angles are 169.06 (13) and 171.54 (8)°, whereas the corresponding cis angles are in the range 84.81 (10)–100.68 (12)°. In the crystal, molecules are linked via C—H...Cl interactions.

The crystal and molecular structures of the bispyridine and 1,10-phenanthroline adducts of Bis(ethyl 3-mercaptobut-2-enoato)nickel(II)

1982 ◽  
Vol 35 (2) ◽  
pp. 331 ◽  
Author(s):  
J Sachinidis ◽  
MF Mackay ◽  
MW Grant
Keyword(s):  
Thermodynamic Data ◽  
Molecular Structures ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Crystal And Molecular Structures ◽  
Distorted Octahedral ◽  
In Cis ◽  
Oxygen Atoms

X-ray analyses of monoclinic crystals of the bispyridine and 1,10-phenanthroline adducts of the monothioacetylacetonate complex bis(ethyl 3-mercaptobut-2-enoato)nickel(n), Ni(eosm)2,* have defined their structures. Crystals of the bispyridine adduct Ni(eosm)2,py2, C22H28N2NiO4S2, belong to the space group P21/c with a 8.865(6), b 15.758(4), c 9.136(3)Ǻ, β 109.18(4)°, Z 2. Crystals of the 1,10-phenanthroline adduct Ni(eosm)2,phen, C24H26N2NiO4S2, belong to the space group P21c with a 12.451(2), b 16.949(1), c 15 5921(2) Ǻ, β 130.97(1)°, Z 4. The structures were refined with diffractometer data measured with Cu Ka radiation to R 0.047 (1962 terms) for the bispyridine adduct and R 0.061 (3115 terms) for the phenanthroline adduct. The geometry about the nickel in each complex is distorted octahedral. The molecule of the bispyridine adduct has exact rn symmetry with the two sulfur atoms cis-equatorial and the nitrogen atoms axial. In the phenan- throline adduct, pairs of sulfur, nitrogen and oxygen atoms are in cis configurations. In the bis-pyridine adduct, the Ni-N bond lengths, 2.153(3) and 2.182(4) Ǻ, are significantly longer than those in other bispyridine adducts of nickel(II) species. It is suggested that the long Ni-N distances reflect the relative instability of the bispyridine adduct, and thermodynamic data are presented to support this.

N-TrimethylsilyMminotriphenylphosphoran-Kupfer(II)-chlorid, [Me3 SiNPPh3 · CuCl 2 ]2 Synthese und Kristallstruktur / N-Trimethylsilyl-iminotriphenylphosphorane Copper(II) Chloride, [Me3 SiNPPh3 · CuCl 2] 2 Synthesis and Crystal Structure

1988 ◽  
Vol 43 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Dieter Fenske ◽  
Eberhard Böhm ◽  
Kurt Dehnicke ◽  
Joachim Strähle
Keyword(s):  
Crystal Structure ◽  
Coordination Number ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Title Compound ◽  
Unit Cell ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Bond Lengths ◽  
Moisture Sensitive

Abstract The title compound has been prepared by the reaction of N-trimethylsilyl-iminotriphenylphos-phorane with copper(II) chloride in boiling CCl4 /C2H5OH, and forms moisture sensitive crystals, which are green in transmittance and black in reflexion. [Me3SiNPPh3 · CuCl2 ] 2 was characterized by its IR spectrum as well as by a crystal structure determination (4197 observed, independent reflexions, R = 0.049). The lattice dimensions are at 20 °C: a = 1102.7. b = 1407.3. c = 1560.2 pm; β = 94.27°; space group P21/n with two formula units in the unit cell. The complex consists of centrosymmetric, dimeric molecules with a planar Cu2 Cl2 ring (Cu-CI bond lengths 229 and 231 pm). A terminally bonded CI atom (Cu-CI = 221 pm) and the N atom of the Me3SiNPPh3 ligand (Cu-N = 198.5 pm) complete the coordination number four of the nearly planar surroundings of the Cu atoms.

scholarly journals Synthesis and Single Crystal X-Ray Structure of New (2E)-2-[3-(1H-Imidazol-1-yl)-1-phenylpropylidene]-N-phenylhydrazinecarboxamide

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Mohamed I. Attia ◽  
Hazem A. Ghabbour ◽  
Aida A. El-Azzouny ◽  
Omar A. Al-Deeb ◽  
Maha S. Almutairi ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Single Crystal ◽  
Title Compound ◽  
Spectroscopic Characterization ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Imine Bond

Synthesis, spectroscopic characterization and X-ray crystal structure of a new (2E)-2-[3-(1H-imidazol-1-yl)-1-phenylpropylidene]-N-phenylhydrazinecarboxamide (4) are reported. The stereochemistry of the title compound4, C19H19N5O, about the imine bond [1.296 (4) Å] was assigned to have (E)-configuration. In the urea moiety, the N–H entities aretransto each other, and one of these forms is an intramolecular N–H⋯H hydrogen bond. The compound crystallizes in the monoclinic space groupP21/cwitha= 5.8093 (2) Å,b= 20.5575 (6) Å,c= 14.0355 (5) Å,α= 90.00°,β= 97.365° (2),γ= 90.00°,V= 1662.36 (10) Å3, andZ= 4. The molecules are packed in crystal structure by weak intermolecular hydrogen interactions.

scholarly journals Tris(pyrrolidin-1-yl)carbenium tri-μ-iodido-bis[triiodidobismuthate(III)]

IUCrData ◽  
2016 ◽  
Vol 1 (3) ◽  
Author(s):  
Ioannis Tiritiris ◽  
Georg Knobloch ◽  
Stefan Saur ◽  
Willi Kantlehner
Keyword(s):  
Double Bond ◽  
Title Compound ◽  
Rotation Axis ◽  
Asymmetric Unit ◽  
Charge Delocalization ◽  
Iodide Ions ◽  
Bond Lengths ◽  
Distorted Octahedral ◽  
Methylene Groups ◽  
Bond Character

The asymmetric unit of the title compound, 3(C13H24N3)+[Bi2I9]3−, comprises two cations and one half of a [Bi2I9]3−ion. The C—N bond lengths of the CN3units in both cations range from 1.336 (3) to 1.364 (5) Å, indicating partial double-bond character pointing towards charge delocalization within the NCN planes. All five-membered rings adopt an envelope conformation with the C atoms as the flap. One of the pyrrolidine rings (cation I) is disordered over two alternative envelope conformations. Two sets of positions were found for two of the methylene groups with an occupancy ratio of 0.757 (10):0.243 (10). The second disordered pyrrolidine moiety (cation II) is disordered around a twofold rotation axis and exhibits two half-occupied symmetry equivalent counterparts. The two BiIIIions are coordinated by six iodide ions in a distorted octahedral manner, with the Bi–I bond lengths ranging from 2.9544 (2) to 3.2414 (2) Å. Two [BiI6]3−octahedra are fused together through face-sharing, forming a dinuclear [Bi2I9]3−unit. The bond lengths of bismuth to the terminal iodides [2.9544 (2)–2.9889 (2) Å] are shorter than the bridging ones [3.1450 (2)–3.2414 (2) Å].

Filling up another Gap: Synthesis and Crystal Structure of Ba2H3I

2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Title Compound ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

Colorless and transparent single crystals of Ba2H3I were obtained by reacting Ba with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules at 1100 K for 13 h. The crystal structure of the title compound was determined and refined by means of single-crystal X-ray diffraction. Ba2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Sr2H3I in the space group P3̄m1 (no. 164) with the lattice parameters a = 451.86(12) and c = 811.84(23) pm. The structural results for Ba2H3I are consistent with bond lengths and coordination geometries of related binary and ternary hydrides

Beiträge zur Chemie des Bors, 133 [1] Molekül-und Kristallstruktur von Tris(methylanilido)boran / Contributions to the Chemistry of Boron, 133 [1] Molecular and Crystal Structure of Tris(methylanilido) Borane

1983 ◽  
Vol 38 (6) ◽  
pp. 692-695 ◽  
Author(s):  
Heinrich Nöth
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Boron Atom ◽  
Title Compound ◽  
Molecular And Crystal Structure ◽  
Threefold Axis ◽  
Special Position ◽  
Space Group ◽  
Bond Lengths ◽  
Upper Limit

Abstract The title compound crystallizes in the rhombohedral space group R3, Z = 1. The boron atom occupies a special position on the threefold axis therefore imposing C3 symmetry to the molecule. The C2BN plane is twisted relative to the BN3 plane by 37.1°, and the BN bond length of 144.8(3) pm is on the upper limit of BN bond lengths found for other triaminoborane systems.

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