Die Kristallstrukturen von PPh4[WOCl4], (PPh4)2[WOCl5] · 2CH2CI2 und (PPh4)2[ReOCl5] · 2CH2Cl2 / The Crystal Structures of PPh4[WOCl4], (PPh4)2[WOCl5] · 2CH2CI2 and (PPh4)2[ReOCl5] · 2CH2Cl2

1984 ◽  
Vol 39 (7) ◽  
pp. 850-854 ◽  
Author(s):  
Dieter Fenske ◽  
Karlheinz Stahl ◽  
Evamarie Hey ◽  
Kurt Dehnicke
Keyword(s):  
Oxygen Atom ◽  
Chlorine Atom ◽  
Complex Space ◽  
Unit Cell ◽  
Axial Position ◽  
Formula Unit ◽  
Tetragonal Pyramid ◽  
Space Group ◽  
Oxygen Ligand ◽  
Oxygen Distance

Both tungsten compounds are formed by reaction of water and oxygen with the acetylene complex PPh4[WCl5(Ph - C ≡ C - C (Br) = C(Br) -Ph)] in CH2Cl2 solutions, and in the presence of PPh4Cl. PPh4[WOCl4] crystallizes in the tetragonal space group P4/n, with two formula units in the unit cell of dimensions a = b = 1269, c = 760 pm at -110 °C (1416 observed in dependent reflexions, R = 0 .054). The [WOCl4]⊖ ion forms a tetragonal pyramid with the oxygen ligand in axial position and a tungsten -oxygen distance of 168 pm. (PPh4)2 [WOCl5 · 2CH2Cl2 crystallizes in the tricline space group P 1̄, with one formula unit per unit cell with a = 1011, b = 1113, c = 1240 pm, α = 70.3°, β = 79.4°, γ = 80.9° at - 110 °C (3781 observed in dependent reflexions, R = 0 .087). The structure contains [WOCl5]2⊖ an ions where the oxygen atom and the chlorine atom in transposition are disordered. (PPh4)2[ReOCl5] · 2CH2Cl2 is formed by the reaction of ReCl5 with PPh4Cl in the presence of water. The compound is isotypic with the corresponding tungsten complex (space group P 1̄, Z = 1, a = 1006, b = 1109, c = 1239 pm , α = 7 0.5°, β = 79.6°, γ = 80.9° at -110 °C; 5436 observed in dependent reflexions R = 0 .050).

Crystal structure of Cu3(AsO4)2

1968 ◽  
Vol 46 (6) ◽  
pp. 917-927 ◽  
Author(s):  
Sandra J. Poulsen ◽  
C. Calvo
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Bond Distance ◽  
Unit Cell ◽  
Monoclinic Crystal ◽  
Space Group ◽  
Bond Lengths ◽  
Oxygen Distance ◽  
Atom Bond ◽  
Oxygen Atoms

Cu3(AsO4)2 forms a monoclinic crystal with lattice parameters a = 6.327(5) Å, b = 8.642(5) Å, c = 11.313(5) Å, β = 92.04(4)°, and Z = 4. The space group is P21/c. The two orthoarsenate anions in the unit cell have average AsO bond lengths of 1.68 Å and 1.70 Å with mean deviations of 0.02 Å and 0.01 Å respectively. The three cations are fivefold coordinated to oxygen atoms with mean cation oxygen atom bond lengths of 2.005 Å, 2.053 Å, and 2.017 Å for the three independent cations. The range of bond distances extends from 1.892 Å to 2.362 Å. Only one additional cation oxygen distance of less than 3 Å occurs and this lies at 2.76 Å. The cation polyhedra form sheets parallel to the ab plane by corner and edge sharing of common oxygen atoms. Adjacent sheets are bonded through the long Cu—O bond distance cited above and by the AsO43− anions. Each of the arsenic atoms shares three oxygen atoms with one sheet and one with the adjacent one.

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.

Crystal structures of nickel(II) and copper(Il)-Schiff-bases complexes with tetramic and tetronic acid subunits

1994 ◽  
Vol 209 (12) ◽  
Author(s):  
G. Reck ◽  
B. Schulz ◽  
A. Zschunke ◽  
O. Tietze ◽  
J. Haferkorn
Keyword(s):  
Complex Formation ◽  
Water Molecule ◽  
Crystal Structures ◽  
Schiff Bases ◽  
Water Molecules ◽  
Ligand Molecule ◽  
Tetragonal Pyramid ◽  
Space Group ◽  
Tetronic Acid ◽  
Oxygen Ligand

AbstractN,N′-ethylene-bis-(tetronic-acid-3-formiminato)-copper(II)/K1 crystallizes in space groupN,N′-ethylene-bis-(tetronic-acid-3-formiminato)-nikkel(II)/K2 crystallizes in space groupN,N′-ethylene-bis-(1,5,5-trimethyltetramic-acid-3-formiminato)-copper(II)/K3 crystallizes in space groupIn K1 and K3 copper is coordinated by two nitrogen and two oxygen atoms of the ligand molecule as well as by one water molecule on top of a tetragonal pyramid. In K2 two water molecules are included in the complex formation. These and two nitrogen as well as two oxygen ligand atoms form a nearly regular octahedron.

Refinement of the structure of Mg2As2O7

1970 ◽  
Vol 48 (6) ◽  
pp. 890-894 ◽  
Author(s):  
C. Calvo ◽  
K. Neelakantan
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
Unit Cell ◽  
Full Matrix ◽  
Space Group ◽  
Cell Dimensions ◽  
Central Oxygen ◽  
R Value ◽  
Unit Cell Dimensions

The crystal structure of Mg2As2O7 has been refined by full matrix least squares procedures using 587 observed reflections. The structure of Mg2As2O7 is of the thortveitite type, as reported by Łukaszewicz, with space group C2/m and unit cell dimensions a = 6.567(2) Å, b = 8.524(4) Å, c = 4.739(1) Å, β = 103.8(1)°, and Z = 2. The As—O—As group in the anion appears to be linear but the central oxygen atom undergoes considerable disorder in the plane perpendicular to this group. The AsO bond distances uncorrected for thermal motion are 1.67 Å for the As—O(—As) bond and 1.66 and 1.65 Å for the terminal As—O bonds. The final R value obtained is 0.088.

Crystal structure determination of K2Zn(PO3)4

2009 ◽  
Vol 24 (1) ◽  
pp. 4-7 ◽  
Author(s):  
L. N. Ji ◽  
Y. Q. Chen ◽  
J. B. Li ◽  
J. Luo ◽  
J. K. Liang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Rietveld Method ◽  
Unit Cell ◽  
Formula Unit ◽  
Chemical Formula ◽  
Monoclinic System ◽  
Calculated Density ◽  
Space Group

The crystal structure of K2Zn(PO3)4 was determined and refined using the Rietveld method based on the isostructure model of K2Cu(PO3)4. This compound belongs to the monoclinic system with space group Cc and lattice parameters of a=11.0941(2) Å, b=12.5215(3) Å, c=7.6597(2) Å, and β=102.47(2)°. The chemical formula unit per unit cell is Z=4 and the calculated density is 2.938(3) g∕cm3. Zigzag [PO3]∞ chains formed along the a axis, and their period contains eight PO4 tetrahedrons.

Characterization and X-Ray Structure of the Adduct Formed Between Triphenyltin Chloride and Dicyclohexylphosphinyl-N-methyl(thioformamide): Ph3Sn[Cy2P(O)C(S)N(H)Me]Cl

1995 ◽  
Vol 48 (9) ◽  
pp. 1659 ◽  
Author(s):  
VJ Hall ◽  
ERT Tiekink
Keyword(s):  
Oxygen Atom ◽  
Chlorine Atom ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Stable Adduct ◽  
Cell Dimensions ◽  
Triphenyltin Chloride ◽  
Unit Cell Dimensions

The reaction of Ph3SnCl and Cy2P(O)C(S)N(H)Me yields the air-stable adduct Ph3Sn[Cy2P(O)-C(S)N(H)Me]Cl which features a trigonal bipyramidal tin atom geometry with a chlorine atom [Sn-Cl 2.4236(9)Ǻ] and an oxygen atom [Sn-O 2.523(2)Ǻ], derived from a monodentate phosphinyl(thioformamide) ligand, occupying the axial positions. The pale-yellow crystals are monoclinic, space group P21/c with unit cell dimensions a 10.050(1), b 16.501(1), c 19.273(1) Ǻ, β 102.12(1)°, Z 4; the structure was refined to final R 0.031 by using 5384 reflections.

Crystal Structure of Synthetic Mg-Whitlockite, Ca18Mg2H2(PO4)14

1974 ◽  
Vol 52 (7) ◽  
pp. 1155-1164 ◽  
Author(s):  
Ramanathan Gopal ◽  
Crispin Calvo ◽  
Jun Ito ◽  
W. K. Sabine
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
Formula Unit ◽  
Full Matrix ◽  
Space Group ◽  
R Value ◽  
Unit Density ◽  
A Chain ◽  
Automatic Diffractometer

Crystals of synthetic Mg-whitlockite, Ca18Mg2H2(PO4)14, have been grown by hydrothermal techniques and their structure refined by full-matrix least-squares methods, using 1626 unique reflections measured with a Syntex [Formula: see text] automatic diffractometer, to a final R value of 0.046. The crystals have space group R3c with ZR = 1, a = 13.765(8) Å and α = 44.25(5)° with the equivalent hexagonal parameters a = 10.350(5), c = 37.085(12) Å and ZH = 3. The structure, although similar to that of βCa3(PO4)2, differs significantly. The structure contains interconnected infinite chains of polyhedra paralleling the hexagonal c axis with links in the chains consisting of three CaO8 polyhedra separated by two PO4 tetrahedra. Six of these chains surround a chain of MgO6 octahedra and PO4H groups which lie on the three-fold axes. These chains however contain only half the formula unit density of the calcium containing ones and a proton, presumably disordered, is attached to the oxygen atom on the triad axes.

scholarly journals Lead-antimony sulfosalts from Tuscany (Italy). XIX. Crystal chemistry of chovanite from two new occurrences in the Apuan Alps and its 8 Å crystal structure

2017 ◽  
Vol 81 (4) ◽  
pp. 811-831 ◽  
Author(s):  
Cristian Biagioni ◽  
Yves Moëlo
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Crystal Chemistry ◽  
Electron Microprobe ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Space Group ◽  
Cell Parameters ◽  
New Occurrences ◽  
Apuan Alps

AbstractTwo new occurrences of the lead oxy-sulfosalt chovanite have been identified at the Monte Arsiccio and Pollone mines, Apuan Alps, Tuscany, Italy. Chovanite from Monte Arsiccio occurs as black acicular crystals, up to 5 mm long, associated with rouxelite, robinsonite, sphalerite, valentinite,baryte, dolomite, quartz and Ba-rich K-feldspar ('hyalophane') in metadolostone vugs. Its unit-cell parameters are a = 48.38(5), b = 4.11(4), c = 34.18(4) Å, β = 106.26(2)°, V = 6521(64) Å3, space group C2/m. Very weakreflections indicate the doubling of the b parameter. Electron-microprobe data gave (wt.%): Ag 0.28, Tl 1.51, Pb 45.57, Sb 31.00, As 1.09, S 19.73, Se 0.05, Cl 0.02, sum 99.25. On the basis of ∑Me = 58 apfu, its formula is Ag0.30Tl0.86Pb25.56Sb29.59As1.69S71.52Se0.07Cl0.05.Adding one oxygen atom, it is close to the formula TlPb26(Sb,As)31S72O. Chovanite from Pollone occurs as thick black acicular crystals, up to 1 cm long, associated with baryte and quartz. The high-diffraction quality of the available material allowed the solutionand refinement of the 8 Å crystal structure in the space group P21/c, with unit-cell parameters a = 34.052(3), b = 8.2027(7), c = 48.078(4) Å, β = 106.258(4)°, V = 12891.9(19) Å3. The refinement convergedto R1 = 9.14% on the basis of 19,853 observed reflections with Fo > 4σ(Fo). Electron-microprobe data gave (wt.%): Ag 0.12, Tl 0.54, Pb 48.34, Bi 0.20, Sb 26.71, As 3.37, S 20.23, Cl 0.07, sum 99.57. It corresponds to the formulaAg0.13Tl0.30Pb26.94Bi0.10Sb25.33As5.20S72.85Cl0.20, close to the idealized formula Pb28(Sb,As)30S72O, with a single oxygen atom bound to two (Sb/As) atoms alternating witha vacancy along b as in scainiite and in other Pb oxy-sulfosalts. The crystal chemistry of this 8 Å crystal structure is detailed, taking into account its modular description, the (Sb,As)mSn polymerization, its topological derivation from pellouxite,and the oxygen non-stoichiometry.

scholarly journals Notizen: PPh3Me[O8(NO)Cl4]; ein fünffach koordinierter Osmiumnitrosylkomplex / PPh3Me[Os(NO)Cl4]; a Pcnta Coordinate Osmium Nitrosyl Complex

1983 ◽  
Vol 38 (8) ◽  
pp. 1031-1033 ◽  
Author(s):  
Bernhard Czeska ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Structure Determination ◽  
Ir Spectrum ◽  
Unit Cell ◽  
Axial Position ◽  
Nitrosyl Complex ◽  
Space Group ◽  
X Ray ◽  
Complex Forms

PPh3Me[Os(NO)Cl4] is prepared by the reac­tion of (NO)2[Os(NO)Cl5] with methyltriphenylphosphonium chloride in CH2Cl2 solution. The complex forms brown, air stable crystals, which are characterized by the IR spectrum as well as by an X-ray structure determination (space group P1̄, two formula units per unit cell, a = 906, b = 1172, c = 1198 pm, α = 76.4, β = 84.8, γ = 82.4°, 3254 independent reflexi­ons, Rw = 8.6%). The structure consists of [P(C6H5)3CH3]⊕ cations and disordered [Os-(NO)Cl4]⊖ anions; the latter have approximate C4V symmetry with a linearly coordinated nitrosyl ligand in the axial position.

The Phenomenon of Intramolecular Attractive S---O Interactions: Synthesis and Structure of (1,10-Phenanthroline)copper(II) Complexes with Isonitroso-(4-methylthiazol-2-yl)acetamide and Isonitroso-(4-methylthiazol-2-yl)-(benzothiazol-2-yl)methanide

1997 ◽  
Vol 52 (3) ◽  
pp. 323-330 ◽  
Author(s):  
Konstantin V. Domasevitch ◽  
Vera V. Ponomareva ◽  
Andrey A. Mokhir ◽  
Eduard B. Rusanov ◽  
Joachim Sieler ◽  
...  
Keyword(s):  
Nitrogen Atom ◽  
Oxygen Atom ◽  
Chlorine Atom ◽  
Carbonyl Oxygen ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
Trigonal Bipyramidal ◽  
Bidentate Chelate

Abstract Isonitroso-(4-methylthiazol-2-yl)acetamide H (L1), isonitroso-(4-methylthiazol-2-yl)(benzo-thiazol-2-yl)methanide H(L2) and their copper(II) complexes of composition [Cu(Phen){L1}(ClO4)] (1) and [Cu(Phen){L2}Cl]*C2H5OH (2) have been prepared. Crystal and molecular structures of the complexes have been determined from X-ray diffractioon data (1: monoclinic, space group P21/c, with a = 11.611(2), b = 10.259(2), c = 17.869(4) Å, β = 104.67(3)°, V = 2059.1(7) Å3, Z = 4; R1 = 0.046 for the 2522 unique reflections with I > 2σ(I). 2: triclinic, space group P1̄, with a = 8.351(1), b = 10.876(1), c = 14.891(2) Å, a = 96.170(8)°, β = 94.201(9)°, γ = 106.721(9)°, V = 1280.1(2) Å3, Z = 2; R1 = 0.034 for the 4038 unique reflections with I > 2σ(I)). In the structure of 1 the coordination polyhedron of Cu2+ is a distorted square pyramid with an oxygen atom of the CIO4 counter anion in the apex (C u -O 2.505(3) Å); in complex 2 the copper atom adopts fivefold coordination of a slightly distorted trigonal-bipyramidal geometry with a chlorine atom in the equatorial plane (Cu-Cl 2.3504(9) A). Ethanol of crystallization gives rise to a hydrogen bond at the chlorine atom. In both structures the oximic anions are coordinated to the metal center in a bidentate chelate manner via the nitrogen atom of the nitroso group and the carbonyl oxygen atom (1) or via the benzothiazole nitrogen atom (2) (Cu-O, Cu-N in the range 1.963(2) -2.031 (2) Å). The thiazole group of the ligands takes no part in the coordination. The nitroso oxygen atoms possess short intramolecular contacts with thiazole sulphur atoms, with d(S--- O) at 2.605(3) (1) and 2.676(3) A (2), which may be attributed to a strong intraligand interaction.

Sign in / Sign up

Export Citation Format

Share Document