Coordination of 3,3'-Bipyridazine With Bivalent Copper, Palladium and Platinum

1990 ◽  
Vol 43 (11) ◽  
pp. 1919 ◽  
Author(s):  
HA Goodwin ◽  
D Onggo ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Vibrational Spectra ◽  
Complex Cation ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Planar Conformation ◽  
Bivalent Copper ◽  
Electronic And Vibrational Spectra

Bis ( ligand ) complexes of the diimine 3,3′-bipyridazine (L) with bivalent copper, palladium and platinum are described. Green and violet forms of [CuL2] [BF4]2 were obtained, and the electronic and vibrational spectra suggest coordinated fluoroborate groups in the violet species. In the green complex a tetragonal structure is indicated. Coordination of perchlorate in [PdL2] [ClO4]2 is also indicated but not in [PtL2] [ClO4]2. Structure determination of the latter complex reveals a strictly planar PtN4 moiety, and in fact the whole complex cation is approximately planar. Reduced interligand repulsions, compared to those operative in bis ( ligand ) complexes of 2,2?-bipyridine, are believed to allow the essentially planar conformation. The structure of [PtL2] [ClO4]2 was determined at 295 K by single-crystal X-ray diffraction methods, and was refined to a residual of 0.033 for 1942 'observed' independent reflections. Crystal data: [PtL2][ClO4]2 monoclinic, space group P21/c (C5/2h, No. 14), a 7.919(2), b 13.086(3), c 10.313(3)Ǻ, β 107.16(2)°.

Strukturuntersuchungen an Diaryldichalkogeniden: Die Molekülstrukturen von [2,4,6-(CF3)3C6H2S]2,[2,4,6-Me3C6H2Te]2 und [2-Me2N-4,6-(CF3)2C6H2Te]2 / Structural Investigations of Diaryl Dichalcogenides: The Molecular Structures of [2,4,6-(CF3)3C6H2S]2, [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2

1992 ◽  
Vol 47 (3) ◽  
pp. 305-309 ◽  
Author(s):  
Anja Edelmann ◽  
Sally Brooker ◽  
Norbert Bertel ◽  
Mathias Noltemeyer ◽  
Herbert W. Roesky ◽  
...  
Keyword(s):  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Structural Investigations ◽  
Space Group ◽  
X Ray

Abstract The Molecular Structures of [2,4,6-(CF3)3C6H2S]2 (1) [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2 (3) have been determined by X-ray diffraction. Crystal data: 1: orthorhombic, space group P212121, Z = 4, a = 822.3(2), b = 1029.2(2), c = 2526.6(5) pm (2343 observed independent reflexions, R = 0.042); 2: orthorhombic, space group Iba 2, Z = 8, a = 1546.5(2), b = 1578.4(2), c = 1483.9(1) pm (2051 observed independent reflexions, R = 0.030); 3: monoclinic, space group P 21/c, Z = 4, a = 1118.7(1), b = 1536.5(2), c = 1492.6(2) pm, β = 98.97(1)° (3033 observed independent reflexions, R = 0.025).

scholarly journals The Isomorphous Structures of Ammonium trans-Diiodobis(ethanedial-dioximato-(1–)-N,N′)cobaltate(III) and Ammonium trans-Diiodobis(ethanedial-dioximato-(1–)-N,N′)rhodate(III): Extended Metaloximate Chains with a Novel ···I–M–I···I–M–I··· Zigzagged Structure

1990 ◽  
Vol 45 (11) ◽  
pp. 1508-1512 ◽  
Author(s):  
Michel Mégnamisi-Bélombé ◽  
Bernhard Nuber
Keyword(s):  
Room Temperature ◽  
Ammonium Salts ◽  
Monoclinic Space Group ◽  
Hydroxyl Groups ◽  
Coordination Geometry ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Anionic Complexes ◽  
Complex Anions

The ammonium salts of the complex anions trans-diiodobis(ethanedial-dioximato)-cobaltate(III), [Col2(GH)2]-, and trans-diiodobis(ethanedial-dioximato)rhodate(III), [RhI2(GH)2]- (GH- = ethanedial dioximate or glyoximate), have been synthesized and their structures determined from single crystal X-ray diffraction data at room temperature. The crystals of the two salts are monoclinic, space group C2/c. NH4[CoI2(GH)2] (I) crystallizes as dark-brown prisms with a greenish reflectance; its crystal data are: C4H10Col2N5O4, Mr = 504.90; a = 8.910(6), b = 11.700(9), c = 11.691(6) Å; β = 93.55(5)°; V = 1216.4 Å3; Z = 4; Dc = 2.78 Mg m-3. NH4[RhI2(GH)2] (II) crystallizes as yellow-brown blocks with crystal data: C4H10I2N5O4Rh, Mr = 548.88; a = 9.038(4), b = 11.949(5), c = 11.770(3) Å; β = 95.54(3)°; V = 1265.16 A3; Z = 4; Dc = 2.87 Mg m-3. The two structures were refined to a final RW = 0.045 for 1209 observed independent reflections and 95 parameters for I, and to a final RW = 0.040 for 1922 observed independent reflections and 87 parameters for II. The coordination geometry around Co or Rh in the anionic complexes is a distorted (4 + 2) octahedron of four equatorial chelating N atoms and two apical iodides. The H atoms of the hydroxyl groups are involved, as usual, in intramolecular O—H—O bridges with uniform Ο···Ο separations of 2.582 Å for I, and 2.713 Å for II. The rectilinear I—Co—I or I—Rh—I triads form “infinite” zigzag chains extending parallel to the ab plane, with a weak I—I contact of 3.988 Å for I, and 4.010 Å for II.

Synthesis and Crystal Structure Determination of Cyclosporin H

2000 ◽  
Vol 65 (8) ◽  
pp. 1317-1328 ◽  
Author(s):  
Alexandr Jegorov ◽  
Ladislav Cvak ◽  
Aleš Husek ◽  
Petr Šimek ◽  
Anna Heydová ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Amino Acids ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Acid Catalyzed ◽  
Products Of Reaction ◽  
Cyclosporin H

Acid-catalyzed degradation of cyclosporin A was studied in various solvents and products of reaction were monitored by HPLC. Identification of amino acids and their chirality were determined after hydrolysis and derivatization by GC-MS. Cyclosporin H was isolated as the principal product and its structure was determined by X-ray diffraction: Cyclosporin H- diethyl ether-water (1 : 0.5 : 1) crystallizes in the monoclinic space group I2 with a = 12.338(2) Å, b = 18.963(2) Å, c = 34.074(3) Å, β = 96.47(2)°, Z = 4, and V = 7 921.4(17) Å3.

X-Ray Structure, Electrochemical and Electronic Spectroscopic Examination of Cobaloximatic Acid: Hydro-trans-diiodobis(ethanedioximato(1-)-N,N′)cobaltate(III). Extended Intermolecular O-H-O Bridging in the Solid

1993 ◽  
Vol 48 (10) ◽  
pp. 1360-1364
Author(s):  
Michel Mégnamisi-Bélombé ◽  
Irene Jokwi ◽  
Emmanuel Ngameni ◽  
Robert Roux ◽  
Bernhard Nuber
Keyword(s):  
Room Temperature ◽  
Strong Acid ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Acidic Proton ◽  
Spectroscopic Examination

The structure of the cobaloximatic acid, hydro-trans-diiodobis(ethanedioximato(1-)-N,N′)cobaltate(III), has been determined by X-ray diffraction. Crystal data: C4H7CoI2N4O4, Mr = 487.87; monoclinic space group P21/a (C2h5 ); a = 10.795(7), b = 9.003(7), c = 11.881(6) Å; β = 97.29(6)°; V = 1145.35 Å3; Z = 4; dc = 2.83 Mg m-3. Rw (R) = 3.6 (3.9)% for 3064 observed independent reflections and 148 parameters. The coordination geometry around CoIII is a distorted (4 + 2) octahedron of four chelating equatorial N atoms and two apical iodides. The compound is most adequately formulated as a monovalent strong acid: H(Co(GH)2I2) (GH- = ethanedioximate or glyoximate). The H atoms of the oxime groups are involved in the usual intramolecular, as well as in much stronger intermolecular O-H-O bridgings (O ••• Ointramol = 2.613-2.631, O ••• Ointramol = 2.454 A). The “acidic” H atom of each molecule participates in the intermolecular bridging which extends throughout the structure, and propagates nearly parallel to the [101] crystallographic direction. The redox properties of the present compound were examined by cyclic voltammetry in acetonitrile solution at room temperature. Redox waves attributed to the reduction of CoIII and to the oxidation of I- were observed, along with a wave which may be linked to the reduction of the “acidic” proton

Die Kristallstruktur von Di-μ-hydroxo-bis[aquotriamminkobalt(III)]-nitrat-2-Hydrat / The Crystal Structure of Di-μ-hydroxo-bis[aquotriamminecobalt (III)] - nitrate-2-hydrate

1971 ◽  
Vol 26 (10) ◽  
pp. 987-989 ◽  
Author(s):  
Karl Wieghardt
Keyword(s):  
Crystal Structure ◽  
Complex Cation ◽  
Monoclinic Space Group ◽  
Spatial Behaviour ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Ray Methods

The crystal structure of Di-µ-hydroxy-bis [aquo-triamminecobalt (III)] nitrate-2-hydrate has been determined by x-ray diffraction using counter techniques. The compound crystallizes in the monoclinic space group C2h5-P21/n with a=9.444 (2), b=9.684 (3), c=10.736 (3) Å, β=90.1 (2)°, Z= 2. A total of 1765 independent reflections was used in solving the structure, which was refined to a conventional R1-factor of 0.047. It was not possible to distinguish by x-ray methods between the oxygen and nitrogen atoms of the NH3- and H2O molecules in the complex cation, because of their similarity in point of electrostatical and spatial behaviour.

scholarly journals Darstellung und Kristallstruktur von [(NH3)5Rh(H7O4)Rh(NH3)5](S2O6)2,5 · H2O (1). Ein gemischtes Aquopentamminrhodium(III)-hydroxopentamminrhodium(III)- dithionat mit einer neuartigen μ-H7O4-Struktureinheit / Preparation and Crystal Structure of [(NH3)5Rh(H7O4)Rh(NH3)5](S2O6)2,5 · H2O (1). A Mixed Aquopentaamminerhodium(III)-hydroxopentaamminerhodium(III) Dithionate with a Novel μ-H7O4 Structural Unit

1988 ◽  
Vol 43 (2) ◽  
pp. 189-195 ◽  
Author(s):  
Walter Frank ◽  
Thomas Stetzer ◽  
Ludwig Heck
Keyword(s):  
Crystal Structure ◽  
Structural Unit ◽  
Small Difference ◽  
Point Group ◽  
Group Symmetry ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
X Ray

The title compound 1 can be obtained from an aqueous solution of aquopentaammine rhodium(III) dithionate and hydroxopentaammine rhodium(III) dithionate. The crystal structure has been determined from single crystal X-ray diffraction data and refined to R = 0.035 for 4390 unique reflections. Crystal data: monoclinic, space group P21/c, a = 1300.9(5) pm. b = 1472.3(6) pm. c = 1478.8(9) pm, β = 106.20(4)°, Z = 4.In the crystal dinuclear rhodium cations with point group symmetry 1 (C1) are found. A central μ-H3O2-bridge is formed by strong hydrogen bonding between aquo and hydroxo ligands; this bridge is additionally coordinated by two molecules of water. The entire bridging system is therefore H7O4-(H3O2- · 2 H2O). O-O distances characterizing the strength of the three hydrogen bonds within this new kind of structural unit are O(H2O-Rh 1)-O(HO-Rh2): 248 pm. O(H2O-Rh 1)-O(H2Oa): 273 pm, O(HO-Rh2)-O(H2Ob): 287 pm. The hydrogen atoms involved in these bridges have been located. The small difference in the Rh 1-O(H2O) - (205.4(3) pm) and Rh2-O(OH)- (204.3(3) pm) distances indicates that the entire H7O4-- moiety serves as a μ-bridging unit between Rh 1 and Rh 2

scholarly journals Redetermination of K2Mg3(OH)2(SO4)3(H2O)2 from single-crystal X-ray data revealing the correct hydrogen-atom positions

2021 ◽  
Vol 77 (1) ◽  
pp. 62-65
Author(s):  
Matthias Weil
Keyword(s):  
Hydrogen Bond ◽  
Single Crystal ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Accuracy And Precision ◽  
Medium Strength ◽  
Anisotropic Displacement Parameters ◽  
Bonding Scheme

In comparison with the previous structure determination of K2Mg3(OH)2(SO4)3(H2O)2, dipotassium trimagnesium dihydroxide tris(sulfate) dihydrate, from laboratory powder X-ray diffraction data [Kubel & Cabaret-Lampin (2013). Z. Anorg. Allg. Chem. 639, 1782–1786], the present redetermination against CCD single-crystal data has allowed for the modelling of all non-H atoms with anisotropic displacement parameters. As well as higher accuracy and precision in terms of bond lengths and angles, the clear localization of the H-atom positions leads also to a reasonable hydrogen-bonding scheme for this hydroxy hydrate. The structure consists of (100) sheets composed of corner- and edge-sharing [MgO6] octahedra and sulfate tetrahedra. Adjacent sheets are linked by the potassium cations and a hydrogen bond of medium strength involving the water molecule. The title compound is isotypic with its CoII and MnII analogues: the three K2 M 3(OH)2(SO4)3(H2O)2 (M = Mg, Co, Mn) structures are quantitatively compared.

Schwermetall-π-Komplexe II [1] Arenkomplexe des Quecksilbers(I)

1987 ◽  
Vol 42 (7) ◽  
pp. 828-834 ◽  
Author(s):  
W. Frank ◽  
B. Dincher
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Aluminium Trichloride

Abstract The crystalline compounds [(CH3C6H5)2Hg,][AlCl4]2 (1), [(1,2-(CH3)2C6H4)2Hg2][AlCl4]2(2), [(1,3,5-(CH3)3C6H3)2Hg2][AlCl4]2 (3), [1,2,4,5-(CH3)4C6H2Hg2][AlCl4]2 (4) and [((CH3)6C6)2Hg2][AlCl4]2-CH3C6H5 (5) have been prepared from mercury(I)chloride, aluminium trichloride and the corresponding arenes and characterized by elem ental analysis. The crystal structure of 5 has been determ ined from single crystal X-ray diffraction data and refined to R - 0.093 for 3269 unique reflections. Crystal data: monoclinic, space group P21/c, a = 2116(1), b = 1095.1(7), c = 1880(1) pm, β - 104,9(1)°, Z = 4. Each atom of a central Hg2 unit (Hg -Hg distance 251.5 pm) is asymmetrically complexed by hexamethylbenzene, the Hg - Carene distances being in the range from 241 to 340 pm. Two distorted AlCl4 tetrahedra complete a “molecular” [arene2Hg2][AlCl4]2 unit. The shortest Hg-Cl distances are 310 and 312 pm, respectively.

Darstellung, 11B-NMR- und Schwingungsspektren von Aminohexahydro-closo-hexaborat(1–), [B6H6(NH2)]- sowie Kristallstruktur von Cs[B6H6(NH2)] · H2O / Preparation, 11B NMR and Vibrational Spectra of Aminohexahydro-closo-hexaborate(1–), [B6H6(NH2)]-, and the Crystal Structure of Cs[B6H6(NH2)] · H2O

1995 ◽  
Vol 50 (1) ◽  
pp. 11-14 ◽  
Author(s):  
A. Franken ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Vibrational Spectra ◽  
Nmr Spectra ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Aqueous Alkaline Solution ◽  
Nmr Spectrum ◽  
X Ray ◽  
11B Nmr ◽  
Ir And Raman

Aminohexahydro-closo-hexaborate(1–), Crystal Structure, 11B NMR Spectra, Vibrational SpectraBy reduction of [B6H5(NO2)]2- with Fe2+ in aqueous alkaline solution [B6H6(NH2)]- is formed. The compound has been separated by extraction with dichloromethane in the presence of tetrabutylammoniumbromid and precipitated from the organic phase by adding CsCH3COO/C2H5OH. The Crystal structure of Cs[B6H6(NH2)] · H2O has been determined by single crystal X-ray diffraction analysis; monoclinic space group C2 with a = 22.1075(14), b = 6.491(2), c = 5.9570(4) A, β = 100.168(6)°. The 11B NMR spectrum is consistent with a mono-hetero-substituted octahedral B6 cage with local C4v symmetry. The IR and Raman spectra exhibit characteristic N–H, B–H and B6 vibrations.

Low-temperature crystallization and structure determination of N-(trifluoromethyl)formamide, N-(2,2,2-trifluoroethyl)formamide and 2,2,2-trifluoroethyl isocyanide

1999 ◽  
Vol 55 (1) ◽  
pp. 70-77 ◽  
Author(s):  
G. J. Perpétuo ◽  
J. Buschmann ◽  
P. Luger ◽  
D. Lentz ◽  
D. Dreissig
Keyword(s):  
Crystal Structure ◽  
Low Temperatures ◽  
Crystal Packing ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Low Temperature Crystallization ◽  
Temperature Crystallization

Crystals of N-(trifluoromethyl)formamide, C2H2F3NO, (I), N-(2,2,2-trifluoroethyl)formamide, C3H4F3NO, (II), and 2,2,2-trifluoroethyl isocyanide, C3H2F3N, (III), were grown in situ on an X-ray diffractometer and analysed by single-crystal X-ray diffraction methods at low temperatures. Crystal data: (I) orthorhombic, P212121, a = 4.547 (2) Å, b = 5.947 (3) Å, c = 14.731 (9) Å, V = 398.3 (4) Å3, Z = 4, M r = 113.05, T = 143 K, D x = 1.885 Mg m−3; (II) monoclinic, P21/n, a = 4.807 (1) Å, b = 16.707 (3) Å, c = 6.708 (1) Å, β = 109.90 (1)°, V = 506.6 (2) Å3, Z = 4, M r = 127.07, T = 141 K, D x = 1.666 Mg m−3; (III) orthorhombic, P212121, a = 5.668 (2) Å, b = 9.266 (3) Å, c = 8.626 (2) Å, V = 453.0 (2) Å3, Z = 4, M r = 109.06, T = 163 K, D x = 1.599 Mg m−3. The results showed that in the crystal both formamides (I) and (II) are exclusively present in the form of the Z isomer, although measurements of solutions of (I) have shown that the E isomer prevails [Lentz et al. (1987). Angew. Chem. 99, 951–953]. In addition ab initio calculations for (I) predicted the E isomer to be the more stable one. In compound (III) the isocyanide group is staggered with respect to the trifluoroethyl group. In the crystal packing of (I) and (II) intermolecular N—H\cdotsO hydrogen bonds generate infinite chains. In (I), these chains are linked to form sheets by C—H\cdotsO contacts. In the crystal structure of (III) each isocyanide dipole is surrounded by four electronegative F atoms with intermolecular C\cdotsF contacts between 3.4 and 3.5 Å.

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