Synthesis and Structure of (17-Hydroxy-4,4,9,9,11- pentamethyl-5,8,12,13,15-pentaazaheptadec- 11-en-2-one hydrazone)nickel(II) Perchlorate; a Compound with a Hexadentate gem-Diamine Ligand

1997 ◽  
Vol 50 (1) ◽  
pp. 69 ◽  
Author(s):  
Neil F. Curtis ◽  
Olga P. Gladkikh
Keyword(s):  
Oxygen Atom ◽  
Secondary Amine ◽  
Ground State ◽  
Starting Material ◽  
Octahedral Coordination ◽  
Triplet Ground State ◽  
Triclinic Space Group ◽  
Space Group ◽  
Oxygen Atoms

(4,4,9,9-Tetramethyl-5,8-diazadodecane-2,11-dione dihydrazone)nickel(II) perchlorate reacts with 2- aminoethanol and methanal to form blue-violet (17-hydroxy-4,4,9,9,11-pentamethyl-5,8,12,13,15- pentaazaheptadec-11-en-2-one hydrazone)nickel(II) perchlorate. The structure of a methanol solvate was determined [C18H43Cl2N7NiO10, Mr 647·2, triclinic, space group P -1, a 8·992(7), b 10·86(2), c 15·02(1) Å, α 79·95(2), β 76·85(5), γ 78·83(2)°, Z 2, R 0·0637 for 2992 reflections]. The ligand has one terminal hydrazone function of the starting material linked to the 2-aminoethanol residue by a gem-diamine function derived from methanal. The ligand is hexadentate, with the triplet ground state nickel(II) ion in octahedral coordination by three secondary amine and two hydrazone nitrogen atoms and a hydroxy oxygen atom, with the terminal hydrazone nitrogen and the hydroxy oxygen atoms coordinated trans.

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.

Polysulfonylamine, LXIII [1] / Polysulfonylamines, LXIII [1]

1995 ◽  
Vol 50 (1) ◽  
pp. 128-138 ◽  
Author(s):  
Dagmar Henschel ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Hydrogen Bond ◽  
Phenyl Group ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
Amine Molecule ◽  
Chain Sequence ◽  
O 193 ◽  
Oxygen Atoms

Complexes of Uncharged Molecules, Crystal StructureThe thermally labile ternary complexes 18C6 · 2MeOH · 2 HN(SO2Ph)2 (2a), 18C6 · 2MeOH · 2HN(SO2–C6H4-4-Cl)2 (2b) and 18C6 · 3 MeOH · HN(SO2Me)(SO2Ph) (3) were obtained by co-crystallization of 18-crown-6 (18C6) and the appropriate di(organosulfonyl)amine from methanolic solutions and characterized by low-temperature X-ray diffraction. The crystal structures of 2a (monoclinic, space group P21/n) and 2b (triclinic, space group P1̄) consist of monomeric, centrosymmetric formula units. Each di(arenesulfonyl)-amine molecule is connected to a methanol molecule by an N-Η ··· O hydrogen bond (H ··· O 203 pm in 2a, 190 pm in 2b). The methanol molecules are linked to three alternate crown oxygen atoms via one O-Η ··· O(crown) hydrogen-bond and two weaker C-Η ··· O(crown) interactions (OH ··· O 201 pm in 2a, 186 pm in 2b; CH ··· O 236 and 247 pm in 2a, 240 and 254 pm in 2b); two symmetry-related oxygen atoms of the crown are involved in O-Η ··· O and the other four in C-Η ··· O interactions. The structure of complex 3 (monoclinic, space group P21) is built of infinite chains parallel to [101]. The methyl group of the di(organosulfonyl)amine is bonded by C-Η ··· O(crown) interactions to a set of three alternate oxygen atoms of the cyclic polyether (H ··· O 228, 245 and 247 pm). Starting from the acidic NH function, a sequence of three methanol molecules catenated by hydrogen bonds curves around the bulky phenyl group and links with its terminal MeOH through one O-H ··· O(crown) and two C-Η ··· O(crown) bonds to the second set of alternate oxygen atoms in the adjacent symmetry-equivalent crown (OH ··· O 193 pm, CH ··· O 248 and 250 pm). Within the chain sequence N-H ··· O′(Me)H′ ··· O″(Me)H″ ··· O‴(Me)H, the H ··· O distances are H ··· O′ 184, H′ ··· O″ 189 and H″··· O‴ 183 pm. In the structures of 2a, 2b and 3, the crown rings adopt the frequently observed D3d pseudosymmetry.

Stabilisierung des reaktiven Methylcarbonat-Ions im Kronenether- Komplex [Cs(18-Krone-6)(CH3CO3)] und dessen Hydrolyseprodukt / Stabilization of the Reactive Methylcarbonate Ion in the Crown Ether Complex [Cs(18-crown-6)(CH3CO3)], and its Hydrolysis Product

2008 ◽  
Vol 63 (9) ◽  
pp. 1101-1106
Author(s):  
Adelė Jonušaite ◽  
Arnold Adam
Keyword(s):  
Crown Ether ◽  
Hydrolysis Product ◽  
Starting Material ◽  
Monoclinic Space Group ◽  
Bidentate Ligands ◽  
Space Group ◽  
Methyl Carbonate ◽  
Hydrolysis Of ◽  
Ether Complex ◽  
Oxygen Atoms

[Cs(18-crown-6)(CH3CO3)] (1) has been obtained by the reaction of CsOCH3 with 18-crown-6 (1,4,7,10,13,16-hexaoxacyclooctadecane) in methanol in a CO2 atmosphere. The compound crystallizes in the monoclinic space group P21/n (no. 14) with a = 12.141(3), b = 8.610(1), c = 17.985(4) Å , β = 91.17(2)° and V = 1879.6(7) Å3. Cs is tenfold coordinated by six oxygen atoms of the crown ether and four oxygen atoms of two methyl carbonate anions which act as bidentate ligands. The slow hydrolysis of the methylcarbonate results in the hydrogencarbonate complex {Cs2(18-crown- 6)2 · [H2(CO3)2] · H2O · CH3OH} (2), the basic structural constitution of the starting material being retained. This new compound crystallizes in the monoclinic space group P21/c with a = 8.657 (7), b = 22.601 (2), c = 19.619 (15) Å, β = 92.09 (6)° and V = 3836.5 (6) Å3.

scholarly journals Crystal structure of β-Zn3(PO4)2

1967 ◽  
Vol 45 (20) ◽  
pp. 2303-2316 ◽  
Author(s):  
J. S. Stephens ◽  
C. Calvo
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Lattice Parameters ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Basic Cation ◽  
Cation Coordination ◽  
Oxygen Atoms

β-Zn3(PO4)2 crystallizes in the monoclinic space group P 21/c with lattice parameters, a = 9.393(3) Å, b = 9.170(6) Å, c = 8.686(3) Å, β = 125.73(10)°, and Z = 4. The three independent cations are strongly ligated to 4, 5, and 5 oxygen atoms, with average Zn—O bond distances of 1.98 ± 0.09 Å, 2.10 ± 0.10 Å, and 2.08 ± 0.13 Å respectively. In addition there are two longer Zn—O distances of 2.51 Å and 2.55 Å in this structure. The PO4 groups exist as independent, nearly regular tetrahedra, with each oxygen atom ligated to two cations. Unlike the structures found for the α and γ phases of Zn3(PO4)2, which contain ribbons and sheets respectively as the basic cation coordination motif, the structure of β-Zn3(PO4)2 contains interconnected sheets.

Structural Systematics of Metal Acetylide Complexes: X-Ray Studies of Some 'Extended-Chain' Gold σ-Acetylide Complexes

1997 ◽  
Vol 50 (10) ◽  
pp. 991 ◽  
Author(s):  
Ian R. Whittall ◽  
Mark G. Humphrey ◽  
David C. R. Hockless
Keyword(s):  
Ground State ◽  
Structural Data ◽  
Monoclinic Space Group ◽  
Confidence Limits ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Back Bonding ◽  
Ground State Geometry

The structures of Au(4-C≡CC6H4XYC6H4-4′-NO2)(PPh3) (XY = (E )-CH=CH (1), (Z)-CH=CH (2), C≡C (3), N=CH (4)) have been determined by single-crystal X-ray diffraction analyses, refining by full-matrix least-squares analysis. For (1), crystals are triclinic, space group P-1, with a8·847(1), b 17·870(4), c 19·705(3) Å, α116·25(1), β 93·33(1), γ 92·64(2)˚, Z 4, 6747 unique reflections (703 parameters), converging at R 0·025 and Rw 0·029. For (2), crystals are monoclinic, space group P 21/a, with a 10·718(6), b 19·398(5), c14·469(3) Å, β 108·96(2)˚, Z 4, 3295 unique reflections (352 parameters), converging atR 0·040 and Rw 0·034. For (3), crystals are triclinic, space group P-1, with a 10·671(4), b 17·599(7), c 18·220(8) Å, α 116·31(3), β 105·00(4), γ 95·08(4)˚, Z 4, 4828 unique reflections (703 parameters), converging at R 0·043 and Rw 0·030. For (4), crystals are triclinic, space group P-1, with a 8·8314(6), b 17·834(2), c 20·001(2) Å, α 115·249(7), β 90·930(7), γ 94·082(7)˚, Z 4, 4724 unique reflections (703 parameters), converging at R 0·035 and Rw 0·034. Despite the [ligated metal donor]-bridge-[nitro acceptor] composition of these complexes, Au–C and C≡C distances are normal and consistent with minimal allenylidene contribution to the ground-state geometry. Within the 3σ confidence limits, the structural data do not provide evidence for π*-back-bonding in these complexes

Synthese und Kristallstruktur von l,13-Bis(8-chinolyl)- 1,4,7,10,13-pentaoxatridecan-diquecksilber(I)-diperchlorat

1991 ◽  
Vol 46 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Klaus Brodersen ◽  
Jörg Zimmerhackl
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
R Value ◽  
Torsional Angles ◽  
L 13 ◽  
Oxygen Atoms

1,13-Bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane-dimercury(I)-diperchlorate is formed by the reaction of 1,13-bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane in ethanol with an aqueous solution of dimercury(I)-diperchlorate.It crystallizes in the triclinic space group P Ī with a = 1020.6(2), b = 1200.6(8), c = 1441.1(6) pm , α = 69.60(5)°, β = 83.04(13)°, y = 66.53(4)° and Z = 2. The crystal structure was determined by X -ray diffraction and refined to an R-value o f 0.079. The Hg22+ -ion is coordinated to both nitrogen atoms and four oxygen atoms of one molecule of the ligand. By changing four C - O torsional angles from trans to gauche, the ligand adopts a helical, chiral configuration around the Hg22+-ion. The CIO4--ions are not coordinated to the Hg22+-ion.

Oxofluoro-oxalato-vanadate des vierwertigen Vanadins: Schwingungsspektrum und Struktur von Na3[VOF(C2O4)2] • 6 H2O.

1976 ◽  
Vol 31 (5) ◽  
pp. 537-540 ◽  
Author(s):  
Helmut Rieskamp ◽  
Rainer Mattes
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Fluorine Atom ◽  
Direct Methods ◽  
Terminal Oxygen Atom ◽  
Triclinic Space Group ◽  
Trans Effect ◽  
Space Group ◽  
X Ray ◽  
In Cis

The Na and NH4 salts of the [VOF(C2O4)2]3--ion have been prepared. The crystal structure of the former has been determined from X-ray diffractometer data. The crystals are triclinic, space group P with Z = 2. The structure was solved by `direct methods' and refined to R 0.050 for 1749 reflections. In the anion, vanadium(IV) is octahedrally coordinated by a terminal oxygen atom, a fluorine atom in cis-position to the former, and two bidentate oxalate ligands. The terminal V—O-bond exhibits a strong ‘trans’ effect.

Die Kristallstruktur von Gadolinium (III)-sulfit Trihydrat Gd2(S03)3∙ 3H2O / Crystal Structure of Gadolinium(III)-sulfite Trihydrate Gd2(SO3)3 ∙3H2O

1994 ◽  
Vol 49 (1) ◽  
pp. 60-62 ◽  
Author(s):  
Hans-Ulrich Hummel ◽  
Petra Joerg ◽  
Gerhard Pezzei ◽  
Alexander Wolski
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Room Temperature ◽  
Triclinic Space Group ◽  
Space Group ◽  
Bond Lengths ◽  
Clear Solution ◽  
Oxygen Atoms

Abstract Gd2(SO3)3 • 3 H20 is obtained by passing gaseous SO2 through a suspension of Gd2O3 in H2O at room temperature until a clear solution is formed. Single crystals are obtained by heating to 70(2) °C for 6 days. The compound crystallizes in the triclinic space group P 1 with a = 6.499(6), b = 6.621(3), c = 6.954(3) Å, α = 110.71(5), β = 90.54(3), γ = 106.05(1)° and Z = 1. The two crystallographically different gadolinium atoms are both coordinated by eight oxygen atoms forming distorted square antiprisms. Gd(l) is coordinated by six O atoms of sulfite ligands and two O atoms of water, while Gd(2) is surrounded by seven O atoms of SO3 and one of H2O. Gd-O-bond lengths vary between 2.31(3) and 2.50(3) Å.

scholarly journals Crystal structure of bis{μ-(E)-2-[(2-oxidophenylimino)methyl]quinolin-8-olato-κ4O,N,N′,O′}bis[dibutyltin(IV)]

2017 ◽  
Vol 73 (1) ◽  
pp. 4-7
Author(s):  
Camacho-Camacho Carlos ◽  
Ortiz-Pastrana Naytzé ◽  
Garza-Ortiz Ariadna ◽  
Rojas-Oviedo Irma
Keyword(s):  
Crystal Structure ◽  
Schiff Base ◽  
Metal Atom ◽  
Title Complex ◽  
Unit Cell ◽  
Type Structure ◽  
Triclinic Space Group ◽  
Space Group ◽  
Centrosymmetric Dimers ◽  
Oxygen Atoms

Condensation of 8-hydroxyquinoline-2-carbaldehyde with 2-aminophenol gave the (E)-2-[(2-hydroxyphenylimino)methyl]quinolin-8-ol derivative that reacted with di-n-butyltin oxide with release of H2O to yield the chelate title complex, [Sn2(C4H9)4(C16H10N2O2)2]. The compound crystallizes in the triclinic space groupP-1, with two independent centrosymmetric dimers in the unit cell. Each features a typical pincer-type structure where the dianionic ligand is tetradentate, coordinating to the central tin atom through both phenolate oxygen atoms, as well as through the quinoline and imine N atoms. Each metal atom adopts a distorted pentagonal–bipyramidal SnC2N2O3coordination arising from theN,N′,O,O′-tetradentate deprotonated Schiff base, one bridging phenolate O atom of the neighbouring ligand and two butyl groups in the axial sites.

Crystal structure of Cd2V2O7

1967 ◽  
Vol 45 (20) ◽  
pp. 2297-2302 ◽  
Author(s):  
P. K. L. Au ◽  
C. Calvo
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Lattice Parameters ◽  
The Other ◽  
Distorted Octahedron ◽  
Thermal Activity ◽  
Space Group ◽  
Bond Angles ◽  
Central Oxygen ◽  
Oxygen Atoms

Cadmium pyrovanadate crystallizes in the C2/m space group with lattice parameters a = 7.088(5) Å, b = 9.091(5) Å, c = 4.963(5) Å, β = 103°21(5)′, and z = 2. This crystal is an isostructure of the mineral thortveitite and thus the anion consists of a pair of centrosymmetrically related corner-sharing VO4 tetrahedra while the cation resides within a distorted octahedron of oxygen atoms. The anion has a linear V—O—V group, but, as with the isostructural pyrophosphates, the central oxygen atom shows an anomalously high thermal activity. The V—O bond distances are 1.76 Å for the inner bond and 1.70 Å for the terminal bond. The bond angles about the anion and cation are similar to those found for the other analogues of thortveitite.

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