Synthesis and Crystal Structures of Three Carboxylate- Bridged Tetranuclear Copper(II) - Lanthanide(III) Complexes of Ph3P+CH2CH2CO2−

1999 ◽  
Vol 52 (10) ◽  
pp. 983 ◽  
Author(s):  
Yang-Yi Yang ◽  
Seik Weng Ng ◽  
Xiao-Ming Chen
Keyword(s):  
Oxygen Atom ◽  
Crystal Structures ◽  
Triclinic Space Group ◽  
Coordination Environment ◽  
Space Group ◽  
Bond Angles ◽  
Bond Lengths ◽  
Metal Atoms ◽  
Apical Site

Three tetranuclear copper(II)–lanthanide(III) complexes of triphenylphosphoniopropionate (Ph3P+CH2CH2CO2−,tppp), namely [Cu2Ln2(tppp)8(H2O)8](ClO4)10·2H 2 O [Ln = EuIII, NdIII or CeIII], were synthesized and characterized by crystallography. The EuIII complex crystallizes in the triclinic space group P1 – with a 16.249(7), b 17.185(11), c 17.807(11) Å, α 69.750(10), β 89.230(10), γ 84.070(10)˚, V 4639(5) Å3, Z 1. In the crystal structures, four tppp ligands bridge a pair of CuII and tetraaquo-EuIII atoms (Cu···Eu 3.527(2) Å) through their µ2-carboxylato ends to form a dinuclear subunit; two of these subunits are additionally linked by one of the CuII -bonded carboxylato oxygen ends, across a centre of inversion, to furnish a dimeric tetranuclear [Cu(tppp)4 Eu(H2O)4]2 species (Cu···Cu 3.323(2) Å). This CuII -bonded oxygen atom occupies the apical site of the square-pyramidal coordination environment of the CuII atom. The EuIII atom is eight-coordinated in a square-antiprismatic geometry. The NdIII and CeIII complexes are isomorphous to the EuIII complex, and only minor differences in bond lengths and bond angles involving the metal atoms are noted.

Untersuchungen an Benzamidinyl-2-phosphazen-Liganden / Investigations on Benzamidinyl-2-phosphazen Ligands

1990 ◽  
Vol 45 (10) ◽  
pp. 1383-1387 ◽  
Author(s):  
Herbert W. Roesky ◽  
Reinhard Hasselbring ◽  
Johannes Liebermann ◽  
Mathias Noltemeyer
Keyword(s):  
Triclinic Space Group ◽  
Space Group ◽  
Bond Angles ◽  
Bond Lengths ◽  
Bonding Properties

The new ligands (Me3Si)2NC(4-CF3C6H4)NP(Ph)2N(SiMe3) (2) and (Me3Si)2NC(4-Me2NC6H4)NP(Ph)2N(SiMe3) (3) have been prepared from 4-CF3C6H4CN or 4-Me2NC6H4CN, respectively, with LiN(SiMe3)2, Ph2PCl and Me3SiN3. In solution, 2 as well as 3 form two isomers. Their structures (2a, 2 b and 3a, 3b) were tentatively assigned on the basis of NMR investigations. Crystals of 2 a and 3a are triclinic, space group PĪ. Bond lengths and bond angles of 2a and 3a are very similar. The influence of the para-substituents on the bonding properties are found to be negligible

Isoselenocyanatoborate -Kristallstrukturen von (n-Bu4N)[BH(NCSe)3] und (Ph4P)[B3H7(NCSe)] / Isoselenocyanatoborates -Crystal Structures of (n-Bu4N)[BH(NCSe)3] and (Ph4P)[B3H7(NCSe)]

1998 ◽  
Vol 53 (3) ◽  
pp. 271-274 ◽  
Author(s):  
B. Steuer ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Elemental Selenium ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Structure Determinations ◽  
Average Bond

Abstract The treatment of [B6H6]2- with an excess of (SCN)2 in dichloromethane in the presence of solid KOH gives the hexaisoselenocyanatodiborate anion [B2(NCSe)6]2- as an intermediate (δ(11B) = -10.3 ppm), from which [BH(NCSe)3]- and elemental selenium are formed. The X-ray structure determinations on single crystals of (n-Bu4N)2[BH(NCSe)3] (1) (triclinic, space group Pi with a = 8.512(2), b = 10.885(3), c = 14.895(4) Å, α = 79.52(2), β = 74.86(2), γ = 86.768(2)°, Z = 2) and (Ph4P)[B3H7(NCSe)] (2) (monoclinic, space group C2, a = 7.686(5), b = 10.366(3), c = 17.533(3) A, β = 108.89°, Z = 4) show that the selenocyanate groups are coordinated exclusively via the N atoms with average bond lengths of B-N = 1.52, C-N = 1.15, C-Se = 1.75 A and angles N-C-Se = 179°, B-N-C = 168.7 - 176.8°. The N-B-N angles of 1 range from 107.5 to 109.5°.

Tetraphenylphosphonium-hexachlorodizinkat und -hexachlorodicadmat, (PPh4)2Zn2Cl6 und (PPh4)2Cd2Cl6 / Tetraphenylphosphonium Hexachlorodizincate and Hexachlorodicadmate, (PPh4)2Zn2Cl6 and (PPh4)2Cd2Cl6

1989 ◽  
Vol 44 (9) ◽  
pp. 1037-1040 ◽  
Author(s):  
Jörg Hubertus Wilhelm ◽  
Ulrich Müller
Keyword(s):  
Crystal Structures ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Metal Atoms

The title compounds were obtained by the reactions of PPh4Cl, HCl and ZnS or CdS in CH2Cl2. Their crystal structures were determined by X-ray diffraction. (PPh4)2Zn2Cl6: a = 973.6(1). b = 982.6(2), c = 1296.7(3) pm, α = 107.93(2), β = 94.50(2), γ = 100.91(2)°, R = 0.036 for 2237 unique observed reflexions. (PPh4)2Cd2Cl6: a = 977.1(2), b = 997.5(3). c = 1306.6(3) pm. α = 108.81(2), β = 94.18(2), γ = 100.24(2)°, R = 0.050 for 1921 reflexions. Both compounds are isotypic in the triclinic space group P1̄ and consist of PPh4+ ions and dimeric, centrosymmetric M2Cl6- ions in which the tetrahedrally coordinated metal atoms are linked via chloro bridges.

Die Kristallstrukturen der silylierten Phosphanimine Me3SiNPPh3 und Me3SiNPPh2 - C2H4 - PPh2NSiMe3 / Crystal Structures of the Silylated Phosphanimines Me3SiNPPh3 und Me3SiNPPh2 - C2H4 - PPh2NSiMe3

1995 ◽  
Vol 50 (7) ◽  
pp. 1050-1054 ◽  
Author(s):  
Frank Weller ◽  
Hak-Chul Kang ◽  
Werner Massa ◽  
Thilo Rübenstahl ◽  
Frank Kunkel ◽  
...  
Keyword(s):  
Crystal Structures ◽  
Bond Angle ◽  
Structure Refinement ◽  
Space Group ◽  
Bond Angles ◽  
Bond Lengths ◽  
Single Bonds

The crystal structures of two silylated phosphanimines have been determined. Me3SiNPPh3: Space group P 1̃, Z = 2, structure refinement with 2907 observed unique reflections with Fo > 5 σ(Fo), R = 0.052. Lattice dimensions at 19 °C: a = 876.6(1), b = 1125.8(1), c = 1151.2(1) pm, α = 61.71(1)°, β = 88.08(1)°, γ = 87.18(1)°. The compound forms monomeric molecules with a SiNP bond angle of 140.2° and bond lengths PN of 154.2 pm and SiN of 168.6 pm which correspond with PN double and SiN single bonds. Me3SiNPPh2 - C2H4 -PPh2N SiMe3: Space group P31, Z = 3, structure refinement with 4251 independent reflections, R = 0.061 for 3587 reflections with I > 2σ(I). Lattice dimensions at - 80 °C: a = b = 1591.4(1), c = 1165.8(1) pm. The compound forms monomeric molecules with a c/s-conformation of the PNSiMe3 groups. Bond angles and bond lengths (average) are SiNP = 140.8°, PN = 153.8 pm, SiN = 165.6 pm.

scholarly journals Die Kristallstrukturen von (PPh4)2[TiCl3(NSiMe3)]2 • CH3CN und (PPh4)2[TiCl4(OSPCl2)]2 / The Crystal Structures of (PPh4)2[TiCl3(NSiMe3)]2 · CH3CN and (PPh4)2[TiCl4(OSPCl2)]2

1992 ◽  
Vol 47 (10) ◽  
pp. 1386-1392 ◽  
Author(s):  
René Wollert ◽  
Sigrid Wocadlo ◽  
Kurt Dehnicke ◽  
Helmut Goesmann ◽  
Dieter Fenske
Keyword(s):  
Oxygen Atom ◽  
Crystal Structures ◽  
Titanium Tetrachloride ◽  
Unit Cell ◽  
Acetonitrile Solution ◽  
Formula Unit ◽  
Chlorine Atoms ◽  
Triclinic Space Group ◽  
Space Group

(PPh4)2[TiCl3(NSiMe3)]2 · CH3CN has been prepared from [TiCl2NSiMe3)]∞ with PPh4Cl in acetonitrile solution as yellow crystals. The compound crystallizes in the triclinic space group P T with one formula unit per unit cell, 3447 observed unique reflections, R = 0.053. Lattice dimensions at 200 K: a = 1030(1), b = 1253(1), c = 1374(1) pm, α = 77.46(8)°, β = 73.93(8)°, γ = 69.99(9)°. The structure consists of PPh4+ ions and centrosymmetric dimeric anions [TiCl3(NSiMe3)]22-, in which pentacoordinate titanium atoms are associated via the nitrogen atoms of the silylimido groups.(PPh4)2[TiCl4(OSPCl2)]2 has been prepared by the reaction of PPh [OSPCl2] with titanium tetrachloride in CH2C12 solution as orange crystals. (Space group P1̄, Ζ = 1, 3242 observed unique reflections, R = 0.033). Lattice dimensions at 193 K: a = 1114.8(2), b = 1190.6(2), c = 1218.7(2) pm, α = 72.18(1)°, β = 85.45(1)°, γ = 69.19(1)°. The structure consists of PPh4+ ions and centrosymmetric dimeric anions [TiCl4(OSPCl2)]22-, in which hexacoordinate titanium atoms are associated via two chlorine atoms. The OSPCl2- group is coordinated via the oxygen atom.

Die Kristallstrukturen von Ph3PNPh, [Ph3PN(H)Ph][AuI2] und von 2,3-Bis(triphenylphosphoranimino)maleinsäure-N-methylimid / The Crystal Structures of Ph3PNPh, [Ph3PN(H)Ph][AuI2] and of 2,3-Bis(triphenylphosphoranimino)maleic Acid-N-methylimide

1988 ◽  
Vol 43 (2) ◽  
pp. 138-148 ◽  
Author(s):  
Eberhard Böhm ◽  
Kurt Dehnicke ◽  
Johannes Beck ◽  
Wolfgang Hiller ◽  
Joachim Strähle ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Maleic Acid ◽  
Staudinger Reaction ◽  
Space Group ◽  
X Ray ◽  
Bond Angles ◽  
Bond Lengths ◽  
Structure Determinations ◽  
Ray Methods

[Ph3PN(H)Ph][AuI2] (2) is formed by the reaction of AuI with N-Phenyl-iminotriphenylphosphorane, Ph3PNPh in a toluene suspension. 2,3-Bis(triphenylphosphinimino)maleic acid-N-methylimide (3) has been prepared by the Staudinger reaction of 2,3-bis(azido)maleic acid-N-methylimide with PPh3 in THF solution in the form of red crystals. Crystal structure determinations of three iminophosphoranes were carried out by X-ray methods.Ph3PNPh (1): space group P21/c, Z = 4, 2176 independent observed reflexions, R = 0.057. Lattice dimensions (-30 °C): a = 1126.4, b = 1148.6, c = 1476.0 pm; β = 97.21°. The compound forms monomeric molecules with P=N = 160.2 pm and an PNC angle of 130.4°.[Ph3PN(H)Ph][AuI2] (2): space group P1̄, Z = 2, 1780 independent observed reflexions, R = 0.057. Lattice dimensions (18 °C); a = 824.9, b = 1022, c = 1476.2 pm; α = 89.23°, β = 87.41°, γ = 85.65°. The compound consists of ions [Ph3PN(H)Ph]⊕ with P=N = 162.4 pm and PNC = 129.3°, and anions [AuI2]⊖ with Au-I = 261.9 and 259.3 pm, IAuI = 176.8°.(Ph3P)2N2C4O2 (NMe) (3): space group P1̄, Z = 2, 4972 independent observed reflexions, R = 0.050. Lattice dimensions (-90 °C): a = 904.7, b = 993.8, c = 2017.4 pm; α = 101.55°, β = 96.39°, γ = 105.81°. The compound forms monomeric molecules with syn-conformation of the two NPPh3 groups. Bond lengths: P=N = 157.1; 155.3 pm, bond angles: PNC = 133°; 136°

Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalyse von cis-[ReCl4X2]2-, X = NCS, NCSe / Crystal Structures, Vibrational Spectra and Normal Coordinate Analysis of cis-[ReCl4X2]2-, X = NCS, NCSe

1998 ◽  
Vol 53 (11) ◽  
pp. 1329-1334 ◽  
Author(s):  
L. Homolya ◽  
S. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Normal Coordinate Analysis ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Valence Force ◽  
Space Group ◽  
X Ray ◽  
Valence Force Field ◽  
Ir And Raman

The crystal structures of cis-(n-Bu4N)2[ReCl4(NCS)2] (triclinic, space group P1̅, a = 11,245( 1), b = 20.174(3), c = 21.320(8) Å, a =109.06(2), β = 96.46(2), γ = 98.22(5)°, Z = 4) and cis-(Ph4P)2[ReCl4(NCSe)2]·2CH2Cl2 (triclinic, space group P1̅, a = 10.341(2), b = 13.436(3), c = 19.616(4) Å, α = 92.70(2), β = 92.02(2), γ = 89.99( 1)°, Z= 2) have been determined by single crystal X-ray diffraction analysis. Both ambidentate ligands NCS and NCSe are bonded via the N atom. Using the molecular parameters of the X-ray determinations the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts have been assigned by normal coordinate analysis based on a modified valence force field. The valence force constants fd(ReN) are 1,78(NCS) and 1,79(NCSe) mdyn/ Å.

scholarly journals Crystal Structures and Magnetic Properties of Two New Cobalt(II) Complexes with Triazole-Substituted Nitronyl and Imino Nitroxide Radicals

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Jing Chen ◽  
You-Juan Zhang ◽  
Kun-Tao Huang ◽  
Qiang Huang ◽  
Jun-Jie Wang
Keyword(s):  
Magnetic Properties ◽  
Metal Ions ◽  
Crystal Structures ◽  
Magnetic Measurements ◽  
Nitroxide Radicals ◽  
Triclinic Space Group ◽  
Space Group ◽  
Imino Nitroxide

Two new cobalt(II) complexes of formula [Co(hfac)2(NITphtrz) 1 and Co(hfac)2(IMphtrz) 2] have been prepared and characterized structurally [where NITphtrz = 4,4,5,5-tetramethyl-2-(2-phenyl-1,2,3-triazole-4-yl)imidazoline-1-oxyl-3-oxide and IMphtrz = 4,4,5,5-tetramethyl-2-(2-phenyl-1,2,3-triazole-4-yl)imidazoline-1-oxyl]. All of the complexes crystallize in an isomorphous triclinic space group P1- with the Co(II) ion octahedrally coordinated via the bidentate chelating mode. The magnetic measurements show that two complexes exhibit antiferromagnetic interactions between the metal ions and the nitroxide radicals.

Distortion isomers of PtM, Pt2M, PtM2 and PtMM′ (M = non-transition metals) derivatives-structural aspects

2018 ◽  
Vol 0 (0) ◽  
Author(s):  
Milan Melník ◽  
Peter Mikuš
Keyword(s):  
Transition Metals ◽  
Structural Parameters ◽  
Bond Angles ◽  
Bond Lengths ◽  
Metal Atoms ◽  
Independent Molecules ◽  
Structural Aspects

Abstract An analysis of the structural parameters of PtM, Pt2M, PtM2 and PtMM′ (M = non-transition metals) derivatives shows that each complex contains two crystallographically independent molecules within the same crystal. The respective molecules differ by the degrees of distortion and exemplify the distortion isomerism. These are discussed in terms of the coordination with the platinum and the M atoms and the correlations are drawn among the metal atoms, donor atoms, bond lengths and bond angles. A wide variety of non-transition metals (Sn, Ga, In, Tl, Zn, Cd, Hg, Sb) exist, among which the most prevalent is Sn.

Tetrahalogenotellurate(II): Synthese und Kristallstrukturen von Verbindungen mit den Ionen TeX42- (X = Cl, Br, I)/Tetrahalotellurates(II): Syntheses and Crystal Structures of Compounds with TeX42- Ions (X = Cl, Br, I)

1985 ◽  
Vol 40 (2) ◽  
pp. 251-257 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Bernt Krebs
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Square Planar

Abstract The compounds [(C6H5)4As]2 TeCl4 (1), [(C2H5)4 N]2 TeBr4 · CH3CN (2), and [(C2H5)4N]2TeI4 (3) were prepared by the reaction of Te, X2 , and excess (C2H5)4NX (X = Br, I) in acetonitrile solution or by heating of [(C6H5)4 As]2TeCl6 , Te, and (C6H5)4 ASCl for several hours in the same solvent.The structures of 1-3 were determined from single crystal X-ray data.1 crystallizes in the monoclinic space group P21/n with a = 1061.8(2), b = 1614.2(3), c = 1341.7(3) pm, β = 94.21° and Z = 2; 2: tetragonal, P4/mmm, a = 1039.7(2), c = 690.5(1), Z = 1; 3: tetragonal, I4/mmm, a = 1061.7(2), c = 1342.8(4), Z = 2. In 1-3 Te(II) exhibits a square planar coordination. The Te -CI, Te -Br, and Te-I bond lengths were found to be 260.7 (mean), 275.3, and 298.5 pm, respectively.

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