Characterization of a Crystalline Residue From a Swimming Pool: Disodium Copper(II) Tetrakis(isocyanurate) Hexahydrate

1992 ◽  
Vol 45 (11) ◽  
pp. 1927 ◽  
Author(s):  
RD Hart ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Chemical Analysis ◽  
Structure Determination ◽  
Title Compound ◽  
Swimming Pool ◽  
Water Molecules ◽  
Formula Unit ◽  
Sodium Ions ◽  
X Ray

Coupled with chemical analysis, a single-crystal X-ray structure determination of lilac deposit from a swimming pool, shows the deposit to be the title compound Na2Cu(C3H2N3O3)4.6H2O. Crystals are triclinic, P1, a 10.459(1), b 10.434(3), c 6.762(4) � , α: 71.73(4), β 83.67(4), γ 62.82(2), Z 1 formula unit; 1265 'observed' diffractometer reflections were refined to R 0.052. The copper atoms are located on crystallographic inversion centres, four-coordinated by a pair of water molecules [Cu-O, 1.937(6) � ] and a pair of ligand nitrogen atoms [Cu-N, 1.941(9) � ]. Interactions from ligand oxygen atoms to sodium ions link the structure into a polymeric array.

Lewis-Base Adducts of Lead(II) Compounds. III. Synthesis and Structural Characterization of Mononuclear (Nitrato-O,O′)bis(1,10-phenanthroline)-(thiocyanato-N)lead(II)

1989 ◽  
Vol 42 (2) ◽  
pp. 335 ◽  
Author(s):  
LM Engelhardt ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Title Compound ◽  
Lone Pair ◽  
Lewis Base ◽  
Lead Atom ◽  
X Ray

The isolation and single-crystal X-ray structure determination of the title compound, [(phen)2Pb(NCS)(O2NO)] is described; crystals are triclinic, P1, a 15.554(7), b 9-670(4), c 8.429(3) α 72.53(3), β 81.90(3), γ 72.88(3)� Z = 2, yielding R 0.052 for 3405 independent 'observed' reflections. The lead atom is seven-coordinate [Pb-N 2.49(1)-2.60(1) (phen), 2.89(1) (NCS); Pb-O 2.75(1), 2.89(1) �] with a large vacancy in the coordination sphere, possibly indicative of a stereochemically active lone pair.

Structural Systematics of Rare Earth Complexes. XII Solvated 1 : 1 Adducts of Some Lanthanoid(III) Carboxylates with 1,10-Phenanthroline and 2,2′:6′,2″-Terpyridine

1999 ◽  
Vol 52 (6) ◽  
pp. 481 ◽  
Author(s):  
Cameron J. Kepert ◽  
Lioubov I. Semenova ◽  
Lu Wei-Min ◽  
Brian W. Skelton ◽  
Allan H. White
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Room Temperature ◽  
Water Molecules ◽  
X Ray ◽  
Structural Characterizations

A room-temperature single-crystal X-ray structure determination of the 1 : 1 adduct of 1,10-phenanthroline (`phen") with lutetium(III) acetate (as its dihydrate) is recorded. Crystals are triclinic, P 1, a 12·430(8), b 10·681(4), c 8·134(8) Å, α 74·76(6), β 84·81(7), γ 74·29(4)°, Z = 2 f.u.; conventional R on |F| was 0·031 for No 3939 independent ‘observed’ (I > 3σ(I)) diffractometer reflections. The complex [(N,N′-phen)(O,O′-ac)Lu(O-ac-O′)4Lu(O,O′-ac)(N,N′-phen)].2H2O is binuclear, the lutetium being eight-coordinated by bidentate phen and ac (acetate) ligands and four oxygen atoms from the bridging acetate ligands. Also recorded is the structural characterization of 1 : 1 Lu(ac)2Cl/tpy (tpy = 2,2′:6′,2″-terpyridine) as its pentahydrate; this complex is triclinic, P 1, a 12·410(3), b 11·559(4), c 9·976(4) Å, α 85·19(3), β 70·30(3), γ 65·70(2)°, Z = 2, R 0·049 for No 4717. The complex is shown to be [(tpy)(H2O)2Lu(O2CCH3)2]Cl.3H2O, with the lutetium nine-coordinated by tridentate tpy, a pair of bidentate acetates and two unidentate water molecules, with the chloride uncoordinated. Structural characterizations of a number of 1 : 1 adducts of variously solvated lanthanoid(III) trichloroacetates, Ln(tca)3, with tpy are also recorded. Yb(tca)3/tpy/MeOH (1 : 1 : 1) is triclinic, P 1, a 14·016(4), b 12·951(5), c 9·604(3) Å, α 73·89(3), β 76·56(3), γ 69·20(3)°, Z = 2 f.u., R 0·057 for No 4465. The complex is mononuclear, the eight-coordinate N3YbO5 array containing tridentate tpy, unidentate methanol, and two unidentate and one bidentate chelating anions. 1 : 1 : 1 Ln(tca)3/tpy/OH2 adducts for Ln = La(-)Nd are triclinic, P 1, a ≈ 13·4, b ≈ 12·47, c ≈ 11·5 Å, α ≈ 114·5, β ≈ 89·9, γ ≈ 115·6°, Z = 1 binuclear array, R 0·061, 0·071 for No 3240, 2394. The two Ln atoms are O,O′-bridged by a pair of anions, the N3LnO6 nine-coordinate lanthanoid environment being completed by a tridentate tpy, one water, one unidentate and one bidentate anion. A 1 : 1 : 1 Lu(tca)3/tpy/OH2 array, by contrast, is triclinic, P 1, a 16·569(8), b 14·815(5), c 14·375(6) Å, α 62·05(3), β 81·35(4), γ 77·97(3)°, Z = 4 ‘mononuclear’ f.u., R 0·067 for No 6710. The array, remarkably, contains species of both of the above types in a 1 : 2 binuclear-to-mononuclear ratio, but with water replacing methanol in the mononuclear array.

scholarly journals Formation and structural characterization of a potassium amidinoguanidinate

2018 ◽  
Vol 74 (12) ◽  
pp. 1795-1799
Author(s):  
Volker Lorenz ◽  
Phil Liebing ◽  
Liane Hilfert ◽  
Sabine Busse ◽  
Frank T. Edelmann
Keyword(s):  
Structural Characterization ◽  
Structure Determination ◽  
Title Compound ◽  
Coordination Mode ◽  
Chain Structure ◽  
Polymeric Chain ◽  
X Ray ◽  
Potassium Hydride

The first potassium amidinoguanidinate complex, catena-poly[[bis(μ-1-amidinato-N,N′,N′′,N′′′-tetraisopropylguanidinato-κ5 N 1:N 1,N 2:N 2,N 4)dipotassium]-μ-1,2-dimethoxyethane-κ2 O:O′], [K2(C14H32N4)2(C4H10O2)] n or [{ i PrN= CHN( i Pr)N(N i Pr)2K}2(μ-DME)] n where DME is 1,2-dimethoxyethane, has been synthesized and structurally characterized. The title compound was isolated in 76% yield from a reaction of N,N′-diisopropylcarbodiimide with potassium hydride in DME. The single-crystal X-ray structure determination of the title compound revealed a polymeric chain structure comprising cage-like dimeric units, with the amidinoguanidinate ligand displaying a mixed σ-/π-coordination mode.

Synthesis and X-Ray Structural Characterization of the 1:1 Adduct of Bismuth(III) With the 'saltren' Anion ['saltren' ≡ N(CH2CH2N=CHC6H4OH)3]: A Novel Seven-Coordinate Bismuth(III) Complex

1994 ◽  
Vol 47 (9) ◽  
pp. 1799 ◽  
Author(s):  
PK Bharadwaj ◽  
AM Lee ◽  
S Mandal ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Title Compound ◽  
X Ray

The synthesis and single-crystal X-ray structure determination of the title compound are recorded; crystals are monoclinic, P 21/c, a 10.309(8), b 18.817(7), c 15.542(6) Ǻ, β 121.80(5)°, Z 4; R was 0.038 for 2894 independent, 'observed' [I > 3σ(I)] reflections. The molecule has quasi-3 symmetry, with seven-coordinate bismuth [Bi-N(apical), 2.82(1); Bi-N, 2.512(8)-2.563(9); Bi-O, 2.197(8)-2.300(8)Ǻ].

New Coordination Compounds of Fe(III) with Organic Ligands

2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Mihaela Flondor ◽  
Ioan Rosca ◽  
Doina Sibiescu ◽  
Mihaela-Aurelia Vizitiu ◽  
Daniel-Mircea Sutiman ◽  
...  
Keyword(s):  
Chemical Analysis ◽  
Complex Compounds ◽  
Organic Ligands ◽  
X Ray Diffraction ◽  
X Ray ◽  
Elemental Chemical Analysis ◽  
Structural Formulae ◽  
Paramagnetic Properties

In this paper the synthesis and the study of some complex compounds of Fe(III) with ligands derived from: 2-(4-chloro-phenylsulfanyl)-1-(2-hydroxy-3,5-diiodo-phenyl)-ethanone (HL1), 1-(3,5-dibromo-2-hydroxy-phenyl)-2-phenylsulfanyl-ethanone(HL2), and 2-(4-chloro-phenylsulfanyl)-1-(3,5-dibromo-2-hydroxy-phenyl)-ethanone (HL3) is presented. The characterization of these complexes is based on method as: the elemental chemical analysis, IR and ESR spectroscopy, M�ssbauer, the thermogravimetric analysis and X-ray diffraction. Study of the IR and chemical analysis has evidenced that the precipitates form are a complexes and the combination ratio of M:L is 1:2. The central atoms of Fe(III) presented paramagnetic properties and a octaedric hybridization. Starting from this precipitation reactions, a method for the gravimetric determination of Fe(III) with this organic ligands has been possible. Based on the experimental data on literature indications, the structural formulae of the complex compounds are assigned.

Structure Determination of 3,5-Biscyclohexylidene-1,2,4-trithiolane / Structure Determination of 3,5-Biscyclohexylidene-1,2,4-trithiolane

1980 ◽  
Vol 35 (8) ◽  
pp. 1015-1018 ◽  
Author(s):  
Werner Winter ◽  
Hanspeter Bühl ◽  
Herbert Meier
Keyword(s):  
General Formula ◽  
Structure Determination ◽  
Title Compound ◽  
Direct Methods ◽  
Spectroscopic Techniques ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Final Structure

Abstract Fragmentation of 1,2,3-thiadiazoles (1) leads to the compounds 5 - 8 with an increasing proportion of sulphur. Numerous structural possibilities exist for the products 7 with the general formula (R2C2)2S3. The number of proposals can be reduced by spectroscopic techniques, but the final structure determination is accomplished by an X-ray analysis of the title compound 7a. 7a crystallizes in the space group P21/c (Z = 4) with cell parameters of a = 9.714(1), b = 16.188(8), c = 9.149(2) Å and β = 98.93(1)°. The structure is solved by direct methods and refined to R = 0.053 with 1955 diffractometer data (I ≥ 2σ(I)). The trithiolane ring has a puckered conformation and the whole molecule shows nearly perfect C2-symmetry, which is not required crystallographically.

Structural Characterization of the Reaction Products of Vanadium(II) and Endrin as 2 Isomers of 1,8,exo-9,10,11-Pentachloropentacyclo[6.2.1.13,6.02,7.04,10]dodecan-5-one

1989 ◽  
Vol 42 (6) ◽  
pp. 959
Author(s):  
DE Clegg ◽  
PC Healy ◽  
GJ Patch ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Title Compound ◽  
Reaction Products ◽  
X Ray

Two dechlorinated products (B) and (D), formed in the reaction between endrin (C12H8Cl6O) and vanadium(II) for the purpose of confirmation of identity, are shown by single-crystal X-ray structure determination to be isomers of the title compound, C12H9Cl5O. Crystals of both are monoclinic, P21/c. For isomer (B), a 7.432(8), b 12.76(1), c 14.55(2) � , β 108.32(9)�, Z=4; R was 0.038 for 2594 observed reflections. For isomer (D), a 9.037(4), b 12.004(4), c 14.436(6) � , β 124.91(2)°, Z= 4; R was 0.041 for 1826 reflections. The geometries of the two isomers are compared.

Approaches to the total synthesis of triterpenes. VIII. The ABC + D/E approach. Synthesis and X-ray structure determination of 1β,4a β-dimethyl-7-methoxy-1α- (7′,7′-ethyleneketal-6′,6′-dimethyl-3′-ketooctyl)-3,4,4a,9,10,10aα-hexahydro- 2(l-H)phenanthrone

1982 ◽  
Vol 60 (4) ◽  
pp. 509-513 ◽  
Author(s):  
John W. ApSimon ◽  
Rick P. Sequin ◽  
Carol P. Huber
Keyword(s):  
Total Synthesis ◽  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
Trimethylsilyl Ether ◽  
Synthetic Route ◽  
X Ray ◽  
Pentacyclic Triterpenes ◽  
Ongoing Work

The title compound was made following a projected synthetic route to pentacyclic triterpenes. The key step in the route is the alkylative trapping of the enolate derived from the enol trimethylsilyl ether 8. The stereochemical consequence of this reaction is confirmed by a single crystal X-ray structure determination on 4, which although of no further utility in the projected synthesis, nevertheless served as a useful template for this determination. In this way, ongoing work in a parallel series of compounds rests on a firm stereochemical footing.

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