The preparation and X-ray crystal structure of Te(N3)3SbF6 containing the triazidotellurium(IV) cation, Te(N3)3+

1989 ◽  
Vol 67 (11) ◽  
pp. 1687-1692 ◽  
Author(s):  
James P. Johnson ◽  
Gregory K. MacLean ◽  
Jack Passmore ◽  
Peter S. White
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Angles ◽  
X Ray Crystallography ◽  
Distorted Octahedral ◽  
Average Bond

The crystal structure of Te(N3)3SbF6 containing the first binary tellurium–nitrogen cation, triazidotellurium(IV) (Te(N3)3+), has been determined by X-ray crystallography. Single crystals of Te(N3)3SbF6 are monoclinic, space group P21/c with a = 9.201(6), b = 8.445(4), c = 13.582(7) Å, β = 100.36(5)°, Z = 4, final R1 = 0.036 for 1286 observed reflections. The structure consists of discrete Te(N3)3+ cations and distorted octahedral SbF6− anions, with some cation–anion interactions. The average Te—Nα—Nβ—Nγ bond distances in Te(N3)3+ are Te—Nα, 1.994(7); Nα—Nβ, 1.237(11); and Nβ—Nγ, 1.116(12) Å. The average bond angles about the Te, Nα, and Nβ atoms are 94.1(3)°, 116.5(6)°, and 173.7(9)°. Structural correlations with other TeX3+ species have yielded an estimate of the electronegativity of the N3− group to be 3.1 ± 0.1. Keywords: tetratellurium (2+) cation, triazidotellurium(IV) cation, electronegativity, azide.

scholarly journals Crystal Structure Investigation of Two Polymeric Chromium(III) Azide Complexes; KCr(pyridine)4(N3)4 and RbCr(pyridine)3(N3)4. A Structure Containing μ(l,3) and μ(1,1,3) Bridging Azido Ligands between Chromium and Rubidium Centered Polyhedra

1992 ◽  
Vol 47 (12) ◽  
pp. 1754-1758 ◽  
Author(s):  
M. A. S. Goher ◽  
M. A. M. Abu-Youssef ◽  
F. A. Mautner ◽  
H. P. Fritzer
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Pyridine Ligands ◽  
Dimensional Network ◽  
Distorted Octahedral

The structures of two polymeric complexes of chromium(III) azide with pyridine, KCr(py)4(N3)4 (1), and RbCr(py)3(N3)4 (2), were determined by X-ray crystallography. Crystal data: 1, C20H20N16CrK, monoclinic, space group C2/c, a = 1611.2(5), b = 1050.6(3), c = 1609.0(5) pm, β = 91.69(3)°, Ζ = 4 and Rw = 0.037 for 923 diffractometer data; 2, C15H15N15CrRb, monoclinic, space group P21/n, a = 1311.9(3), b = 1139.0(4), c = 1523.3(4) pm, β = 109.39(2)°, Ζ = 4 and Rw = 0.046 for 2336 data.The crystal structure of 1 contains six-coordinated chromium and potassium cations with two pyridine ligands and four µ(1,3) bridging azido groups forming a three-dimensional network structure. The chromium atoms are trans-coordinated by the pyridine ligands, whereas the potassium cations are cis-coordinated. The polymeric complex 2 features di-µ(l,1,3) azido bridged CrRbN2 rings, distorted octahedral chromium(III) coordination geometry, sevencoordinated rubidium, and di-μ(1,3) azido bridges which link the binuclear RbCr(pyridine)3(N3)2 moieties into infinite chains parallel to the b axis.

The crystal structure of Bis[2-(pyridin-2-ylamino)-4-(pyridin-2-yl)thiazole]iron(II) Bis(tetrafluoroborate) trihydrate

1984 ◽  
Vol 37 (2) ◽  
pp. 443 ◽  
Author(s):  
AT Baker ◽  
HA Goodwin ◽  
AD Rae
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Complex Cation ◽  
Monoclinic Space Group ◽  
Octahedral Structure ◽  
Space Group ◽  
X Ray ◽  
Disordered Structure ◽  
Distorted Octahedral ◽  
A Cell

The crystal structure of an iron(II) complex of 2-(pyridin-2-ylamino)-4-(pyridin-2-yl)tliazoe (paptH) has been determined by single-crystal X-ray diffractometry. [Fe(paptH)2] [BF4]2.3H2O is monoclinic, space group P21/c, with Z = 4 in a cell of dimensions a 8.968(6), b 9.038(4), c 41.15(2)�, β 94.81(2)�. The disordered structure was refined to a residual R 0.0826 for 2549 observed reflections. The ligands and anions are orientationally disordered, and the waters of crystallization are positionally disordered. Comprehensive constrained refinement, with 220 parameters for 139 atom positions, produced reliable geometry. The complex cation has a distorted octahedral structure of meridional configuration with both paptH ligands functioning as tridentates.

Benzo-18-krone-6 -Acetonitril (1/2): Kristallisation und Tieftemperatur- Röntgenstrukturanalyse / Benzo-18 -crown-6 -Acetonitrile (1/2): Crystallization and Low-Temperature X-Ray Analysis

1998 ◽  
Vol 53 (12) ◽  
pp. 1528-1530 ◽  
Author(s):  
Karna Wijaya ◽  
Oliver Moers ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Data Collection ◽  
Single Crystals ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
Mecn Solution

Abstract Benzo-18 -crown-6 -Acetonitrile (1/2), Crystal Structure Single crystals of the title complex resulted fortuitously during an attempt to co-crystallise MeN(SO2Me)2 with benzo-18-crown-6 from an MeCN solution at -30 °C. The crystal structure has been determined via data collection at -100 °C (monoclinic, space group P21/n, Z = 4). The nitrile molecules are located with their me­ thyl groups above and below the plane of the 18-membered crown ring, the Me hydrogen atoms being rotationally disordered about the MeCN axes; C(methyl)···O(crown) distances range from 309.4(3) to 384.9(3) pm.

The Crystal Structure of (2,2′-Bipyridine)(pyrazine)(2,2′:6′,2″-terpyridine)ruthenium(II) Hexafluorophosphate

1996 ◽  
Vol 49 (4) ◽  
pp. 527 ◽  
Author(s):  
PT Gulyas ◽  
TW Hambley ◽  
PA Lay
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Steric Strain ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Distorted Octahedral ◽  
Back Bonding

The crystal structure of [ Ru ( terpy )( bpy )( pz )] (PF6)2 has been determined by X-ray diffraction methods and refined to a residual of 0.046 for 1855 independent observed reflections. The crystals are monoclinic, space group P 21/a, a 16.836(7), b 10.778(5), c l9.342(5) Ǻ, β 115.11(3)°. The coordination geometry around the ruthenium(II) ion is distorted octahedral, with the various Ru -N bond lengths indicative of considerable interligand steric strain. The Ru -N pyrazine bond is the longest within the structure, consistent with other evidence that n back-bonding to pyrazine is weak in the complex.

Zur Synthese und Kristallstruktur von Zinkboratoxiden mit isolierten, trigonal planaren BO3-Baugruppen: Zn5Mn(BO3)2O4 und ZnFe(BO3)O / Synthesis and Crystal Structure of Zinc Borate Oxides Containing Isolated Trigonal Planar BO3 Units: Zn5Mn(BO3)2O4 and ZnFe(BO3)O

1995 ◽  
Vol 50 (10) ◽  
pp. 1450-1454 ◽  
Author(s):  
Silke Busche ◽  
Karsten Bluhm
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Zinc Borate ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Octahedral Sites ◽  
Distorted Octahedral ◽  
New Compounds ◽  
Group D

Single crystals of the new compounds Zn5Mn(BO3)2O4 (A ) and ZnFe(BO3)O (B) were prepared by using a B2O3 flux technique. Zn5Mn(BO3)2O4 is isostructural with Ni5Ti(BO3)2O4 and ZnFe(BO3)O is isotypic with the mineral warwickite. X-ray investigations on single crystals led to (A ) space group D92h -Pbam, a = 926.41(10), b = 1236.67(8), c = 304.55(3) pm, Z = 2, and (B) space group D162h-Pnma, a = 924.62(4), b = 314.1(10), c = 935.3(2) pm, Z = 4. The structure of Zn5Mn(BO3)2O4 (A ) contains four octahedrally coordinated metal sites, one of these statistically occupied by Zn2+ and Mn4+. In the structure of ZnFe(BO3)O the ions Zn2+ and Fe3+ occupy statistically both distorted octahedral sites. Both structures contain isolated BO3 units and oxygen that is not coordinated to boron.

Preparation and Crystal Structure Determination of [(C2Η5)4N]2Hg3Cl8

1995 ◽  
Vol 50 (1) ◽  
pp. 66-70 ◽  
Author(s):  
Inge Pabst ◽  
Peter Sondergeld ◽  
Mirjam Czjzek ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Analysis ◽  
Structure Determination ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Coordination Type ◽  
X Ray

The title compound has been prepared in two different ways: First, by boiling single crystals of [(C2H5)4N]HgCl3 in a mixture of n-hexane/n-octane [4:1] at T = 350 K, and second, in a synthesis from stoichiometric quantities of the components. X-ray structure analysis gave the stoichiometry [(C2H5)4N]2Hg3Cl8, monoclinic, space group P21, a = 7.538(3), b = 19.909(6), c = 10.274(3) Å, β = 95.13(1)°, V = 1535.7(9) A3, Z = 2. The basic [Hg3Cl8]2--units form broken zig-zag chains along [100]. The Hg–Cl distances within the [Hg3Cl8]2- clusters range from 2.315(3) to 2.755(4) Å. This is a new coordination type for halomercurates.

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°.

Die Synthese und Kristallstruktur des Borat-Phosphats: α -Zn3(BO3)(PO4) / Synthesis and Crystal Structure of the Borate-Phosphate: α-Zn3(BO3)( PO4)

1997 ◽  
Vol 52 (1) ◽  
pp. 102-106 ◽  
Author(s):  
K. Bluhm ◽  
C. H. Park
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Monoclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

Single crystals of the compound α -Zn3(BO3)(PO4) were obtained at 1050 °C by using B2O3, P2O5 and ZnCO3 as starting materials and subsequent cooling to 600°C with 20°C/h. X-ray investigations on single crystals yield a new crystal structure in the monoclinic space group Cm - (Nr. 8) with a = 972.5(2); b = 1272.0(3); c = 487.4(3) pm; β = 119.80 (4)°; Z = 4. The structure contains isolated trigonally planar BO3 and tetrahedral PO4 units which are not joined together. Zinc occupies three crystallographically different point positions and is trigonal-bipyramidally, tetragonal-pyramidally or distorted tetrahedrally coordinated by oxygen

Darstellung und Kristallstruktur von Na4Ga2S5. Ein Thiogallat mit -Zweier-Doppelketten / Preparation and Crystal Structure of Na4Ga2S5. A Thiogallate with --zweier-Double Chains

1992 ◽  
Vol 47 (7) ◽  
pp. 937-941 ◽  
Author(s):  
Kurt O. Klepp
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Single Crystals ◽  
Monoclinic Space Group ◽  
Alkali Cations ◽  
Space Group ◽  
Distorted Octahedral ◽  
New Type

Transparent single crystals of Na4Ga2S5 were obtained from a melt of Na2S, Ga and S. Na4Ga2S5 is monoclinic, space group P21/c with a = 7.967(1), b = 6.133(2), c = 19.852(9) Å, β = 91.61(2)°, Ζ = 4. Its crystal structure was refined to a conventional R of 0.033 for 1150 observed reflections.The structure of Na4Ga2S5 is of a new type. It is characterized by infinite ribbon like thiogallate anions, -, which are built up by GaS4-tetrahedra (mean Ga-S bond length 2.28 A) sharing apices and edges. The four crystallographically independent alkali cations are coordinated to six sulphur atoms in distorted octahedral configurations.

Synthesis and characterization of [MII(bqb)] (M = Co, Ni, Cu), [N(n-Bu)4][CoIII(bqb)(CN)2], and [N(n-Bu)4][CoIII(bqb)(N3)2] containing deprotonated N,N'-bis(2-quinolinecarboxamide)-1,2-benzene (bqb) – X-ray crystal structures of [NiII(bqb)] and [N(n-Bu)4][CoIII(bqb)(N3)2]

2006 ◽  
Vol 84 (7) ◽  
pp. 971-978 ◽  
Author(s):  
Soria Meghdadi ◽  
Mehdi Amirnasr ◽  
Vratislav Langer ◽  
Alison Zamanpoor
Keyword(s):  
Crystal Structures ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Square Planar ◽  
Distorted Octahedral ◽  
Elemental Analyses

Cobalt(II), nickel(II), copper(II), and two cobalt(III) complexes of a new dianionic ligand, bqb, [H2bqb = N,N'-bis(2-quinolinecarboxamide)-1,2-benzene] have been synthesized and characterized by elemental analyses, IR, and 1H NMR spectroscopy. The crystal and molecular structures of the [Ni(bqb)] (2) and [N(n-Bu)4][CoIII(bqb)(N3)2] (5) complexes were determined by X-ray crystallography. Complex 2 crystallizes in the monoclinic space group C2/c with a distorted square-planar structure including two short Ni–N (1.848 Å) and two long Ni–N (1.958 Å) bonds. The structure consists of sheets formed in the plane parallel to the b axis and diagonal to vectors a and c by intermolecular hydrogen bonds. Complex 5 crystallizes in the monoclinic space group C2 with a distorted octahedral structure. The [N(n-Bu)4]+ ion is disordered at the C3A and C4A atoms of one Bu. The IR and 1H NMR spectra of the complexes are also discussed.Key words: N4-dianionic amido ligand (bqb), (bqb) complexes of Co(II), Ni(II), Cu(II), and Co(III), azide, cyanide, X-ray crystal structures.

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