Lewis-Base Adducts of Group 11 Metal(I) Compounds. LVI. Structural Characterization of μ,μ′-Dibromo-bis[(acetonitrile)(diphenyl-o-tolyl-phosphine)copper( I)] Bis(acetonitrile)

1989 ◽  
Vol 42 (6) ◽  
pp. 945 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Title Compound ◽  
Phosphine Ligand ◽  
Lewis Base ◽  
Stoichiometric Ratio ◽  
X Ray ◽  
Copper Bromide

The title compound, [((2-MeC6H4)Ph2P)( MeCN )CuBr2Cu( MeCN )(PPh2-MeCH)]2MeCN has been isolated in the course of recrystallization of a 1 : 1 stoichiometric ratio of copper(]) bromide and the phosphine ligand from acetonitrile and characterized by a single-crystal X-ray structure determination. Crystals are triclinic, PI, a 13.148(2), b 10.673(2), c 8.101(1) � , α 84.24(4), β 89.42(4), γ 82.02(2)°, Z= 1 dimer ; R was 0.050 for 1772 independent 'observed' reflections. The dimer is centrosymmetric and is the first 1 : 1 : 1 mixed base copper(1) halide : phosphine : nitrile adduct to be so isolated and so characterized.

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 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.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LI. Synthesis and Structural Characterization of Mononuclear Chloro-, Bromo- and Iodo-pyridinebis(triphenylphosphine)copper(I) Complexes

1989 ◽  
Vol 42 (6) ◽  
pp. 895 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Copper Atom ◽  
Lewis Base ◽  
X Ray

Complexes [ XCu ( py )(PPh3)2], X = Cl, Br, I, py = pyridine, have been synthesized and characterized by single-crystal X-ray structure determination. Chloride and iodide derivatives have similar cells [ isomorphous (?) but not isostructural ], triclinic, pi, a = 19.5 A, b = 10.5, c = 9.6 � , α ≈ 66, β ≈ 86, γ ≈ 83�, Z = 2; the bromide is monoclinic, Cc, a 13.568(9), b 15.760(12), c 16.545(8) � , β 95.65(5)�, Z = 4. Cl, Br, I structures were refined to residuals of 0.042, 0.055, 0.039 for 4288, 2241, 4808 'observed' reflections. In all cases, the copper atom is four-coordinate; for such an array, Cu-X lengths are unusually short [2.318(2), 2.459(2), 2.636(1) � (Cl, Br, I) and Cu-N unusually long (2.14(1) � ], while (Cu-P) increase from 2.264 to 2.288 � across the series. The dominant aspect of the complexes is thus that of XCu (PPh3)2 solvated by pyridine.

Structural Characterization of Di-μ-hydroxo-bis[trichloro(tetrahydrofuran)tin(II)] Bis(tetrahydrofuran)

1988 ◽  
Vol 41 (7) ◽  
pp. 1123 ◽  
Author(s):  
SD Chappell ◽  
LM Engelhardt ◽  
CL Raston ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Title Compound ◽  
X Ray

The title compound [( thf )Cl3Sn(OH)2SnCl3( thf )].2thf ( thf = tetrahydrofuran ) has been characterized by single-crystal X-ray structure determination, allowing comparison of its geometry with the recently recorded [( thf )BrCl2Sn(OH)2Cl2Br( thf )].2thf,1 with which it is isomorphous.

Lewis-Base Adducts of Main Group Metal(I) Compounds. XI. Di-μ-iodo-bis(N,N,N′,N″,N″-pentamethyldiethylenetriamine-N,N′,N″-sodium)

1989 ◽  
Vol 42 (8) ◽  
pp. 1393 ◽  
Author(s):  
CL Raston ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Main Group ◽  
Lewis Base ◽  
Coordination Complex ◽  
X Ray ◽  
Group Metal ◽  
Main Group Metal

The synthesis and structural characterization of the 1:1 adduct of sodium(I) iodide and N,N,N′,N″,N″- pentamethyldiethylenetriamine (pmdeta), a novel coordination complex of sodium(I), is recorded. Single-crystal X-ray structure determination shows the compound to be a �,�′- diiodo-bridged dimer, with the tridentate base making up the five-coordinate environment of sodium: [( pmdeta )NaI2Na( pmdeta )]. Crystals are triclinic, P1, a 10.113(2),b 9.470(2), c 8.793(4) � , α 114.48(2), β 92.09(2), γ 96-65(1)°, Z= 1 dimer ; R was 0.037 for 1837 'observed' reflections.

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].

Structural Systematics of Rare Earth Complexes. VII. Crystal Structure of Bis(2,2'/6',2␛-Terpyridinium) Octaaquaterbium(III) Heptachloride Hydrate

1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Rare Earth ◽  
Single Crystal ◽  
Structural Characterization ◽  
Title Compound ◽  
Room Temperature ◽  
Chloride Ions ◽  
Full Matrix ◽  
X Ray

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.

Lewis-Base Adducts of Main Group 1 Metal Compounds. V. Diaquabis(quinoline)lithium(I) Bromide Bis(quinoline)

1988 ◽  
Vol 41 (3) ◽  
pp. 409 ◽  
Author(s):  
CL Raston ◽  
BW Skelton ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
Lithium Bromide ◽  
Main Group ◽  
Lewis Base ◽  
Metal Compounds ◽  
X Ray ◽  
Group 1

The title compound, an artefact of recrystallization of lithium bromide from improperly dried quinoline, has been characterized by a single- crystal X-ray structure determination. Crystals are triclinic, Pī , a 16.608(9), b 12.27(1), c 7.962(8)Ǻ, α 101.98(8),β 91.79(7),γ 92.27(6), Z 2; R was 0.058 for 2404 'observed' reflections. The cation is the first to be structurally defined for a [Li(OH2)2 (N-base)2]+ system; Li-O are 1.92(2), 1.93(2)Ǻ and Li-N 2.12(2), 2.14(2)Ǻ.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LIII. Synthesis and Structural Characterization of Binuclear μ,μ'-Dichloro-, Dibromo and Diiodo-bis[(pyridine)(triphenylphosphine)copper(I)] Complexes, and Their Pyridine-4-carbonitrile Analogues

1989 ◽  
Vol 42 (6) ◽  
pp. 913 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Lewis Base ◽  
The Other ◽  
X Ray ◽  
Structure Determinations ◽  
M Phase ◽  
And Inversion ◽  
Iodide Single Crystal

Mixed base pyridine (py)/triphenylphosphine adducts of the copper(1) halides, CuX, have been synthesized for 1 : 1 : 1 stoichiometry for X = chloride and iodide; single-crystal X-ray structure determinations of these show them to be isomorphous and isostructural with that of the bromide recorded elsewhere, being �,�′- dihalo-bridged dimers , [(PPh3)( py )CuX2Cu( py )(PPh3)], monoclinic, C2/c, a ≈ 26.2, b ≈ 14.3, c ≈ 11 .2 � , β ≈ 95, Z = 4 dimers. The bromide has been isolated as a new monoclinic C 2/m polymorph, a 11 .279(8), b 14.268(6), c 13.858(4) �, β 109.33(6)�, Z=4 dimers, and details of its structure are also recorded. The structures of their pyridine-4-carbonitrile (pycn) analogues have also been determined and found to be also binuclear, with no cyano-copper interactions; these also are an isomorphous, isostructural series, monoclinic P21/n, a ≈ 15.4, b ≈ 8.1, c ≈ 17.9 � , β ≈ 101 �, Z = 2 dimers. In each series of dimers, one half of the dimer is crystallographically independent, the generators of the other half being twofold rotor (C2/c phase), mirror (C2/m phase) and inversion centre (P21/n phase) respectively.

The Last Missing Member of the AE2[BN2]Cl Series – Synthesis, Structural and Spectroscopic Characterization of Ba2[BN2]Cl

2008 ◽  
Vol 63 (5) ◽  
pp. 525-529 ◽  
Author(s):  
Olaf Reckeweg ◽  
Jesse Reiherzer ◽  
Armin Schulz ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Title Compound ◽  
Spectroscopic Characterization ◽  
X Ray ◽  
Fundamental Frequencies ◽  
Raman And Ir Spectra

Pale grey-blue, transparent single crystals of Ba2[BN2]Cl (I4132 (no. 214), a = 1462.88(1) pm, Z = 24) are obtained by the reaction of Ba, BaCl2, BN and NaN3 in arc-welded Ta ampoules at 1200 K. The crystal structure was determined by single crystal X-ray structure analysis. The Raman and IR spectra of the title compound show the expected fundamental frequencies (νs = 1038; νas = 1969 and 2087; δ = 616 / 636 cm−1) for a nitridoborate unit with D∞h symmetry. The [N-B-N] structure obtained by X-ray single crystal structure determination corroborates this finding within the standard deviations of the measurement with d(B-N) = 132.3(8) pm and ∡ (N-B-N) = 178.5(13)°. Our results compare well to the data reported for cubic and orthorhombic Ba3[BN2]2 as well as to the isotypic compound Ba2[BN2]Br.

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