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.

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.

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.

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.

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 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.

Single Crystal X-Ray Structural Characterization of [BiX2(S2CNEt2)]Infinity∞, X=Cl, Br

1994 ◽  
Vol 47 (2) ◽  
pp. 405 ◽  
Author(s):  
PK Bharadwaj ◽  
AM Lee ◽  
BW Skelton ◽  
BR Srinivasan ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Sulfur Atom ◽  
Structural Characterization ◽  
Structure Determination ◽  
Room Temperature ◽  
X Ray ◽  
Structure Determinations

Single-crystal room-temperature X-ray structure determinations of the title compounds have been carried out. The two compounds are isomorphous, and isomorphous with the previously determined iodide analogue, being monoclinic, P 21/c, a ≈ 10.0, b ≈ 14.9, c ≈ 7.8 Ǻ, β ≈ 92°, Z = 4 formula units; residuals were 0.037, 0.036 for 2197, 1654 'observed' reflections for X = Cl , Br respectively. As in the iodide, the complexes are infinite polymers, with successive bismuth atoms bridged by the two halides and one sulfur atom of the ligand , which also chelates each bismuth. The structure determination of C5H5NCONEt2]2 [Cl5Bi(NC5H5)], isostructural with its thiocarbamoyl analogue, is also recorded.

Lewis-Base Adducts of Group 11 Metal-Compounds. XXXIII. Structural Characterization of Two Novel 'Trigonal Planar' Halobis(N-Base)Copper(I) Complexes

1988 ◽  
Vol 41 (3) ◽  
pp. 335 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Lewis Base ◽  
Metal Compounds ◽  
Base Complex ◽  
X Ray ◽  
Structure Determinations

Single-crystal X-ray structure determinations are recorded for two unusual trigonal planar XCuL2 species, X = halogen, L = monodentate N- base. For iodobis (2-methylquinoline)copper(I) (1) crystals are orthorhombic, P212121, a 15.079(7), b 12.592(7), c 9.585(4)Ǻ, Z 4. R was 0.028 for 1285 independent 'observed' reflections; the copper(I) environment is trigonal planar [I-Cu, 2.533(2); Cu-N, 2.034(6), 2.0l5(7)Ǻ; I-Cu-N are 119.1(2), 120.4(2) and N-Cu-N, 120.4(2)°]. For the mixed base complex bromo (3,5-dimethylpyridine)(2,4,6-trimethylpyridine )copper(I) (2), crystals are triclinic, pī , a 13.643(5), b 8.434(5), c 8.163(4)Ǻ, α 59.65(4), β 79.76(4), γ 89.68(4)°, Z 2; R was 0.046 for 1551 'observed' reflections. Br-Cu is 2.418(2); Cu-N, 1.971(5), 1.963(6)Ǻ; Br-Cu-N are 113.5(2), 110.0(2) and N-Cu-N, 136.4(3)°.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXVIII Synthesis and Structural Systematics of Some 1 : 3 Adducts of Silver(I) Compounds with Triphenylstibine, [(Ph3Sb)3AgX], X = Cl, I, SCN, NCS, CN, ONO2

1997 ◽  
Vol 50 (6) ◽  
pp. 587 ◽  
Author(s):  
Effendy ◽  
John D. Kildea ◽  
Allan H. White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Room Temperature ◽  
Lewis Base ◽  
Nitrate Complex ◽  
X Ray ◽  
Ethanol Solvate ◽  
New Form ◽  
Pseudo Halides

The syntheses and room-temperature single-crystal X-ray structural characterization of 1 : 3 adducts formed between silver(I) (pseudo-) halides, AgX, and triphenylstibine, SbPh3, are described for X = Cl, I, SCN, NCS, CN, NO3 (1)-(6). The chloride, as its methanol solvate (1a), is isomorphous with the arsine analogue: triclinic, P-1, a 13·373(4), b 14·48(6), c 14·702(3) Å, α 83·49(3), β 87·76(2), γ 76·45(3)°; Z = 2, conventional R on F being 0·046 for No 5514 independent ‘observed’ reflections (I > 3σ(I )). A new form (1b) of the chloride has also been authenticated: monoclinic, P 21/c, a 12·832(2), b 54·24(1), c 18·519(8) Å, β 129·68(3)°; Z = 8 (R 0·065 for No 5672). No bromide has been obtained; the iodide (2) is described as monoclinic, P 21/n, a 19·611(4), b 14·473(6), c 17·74(1) Å, β 98·28(3)°; Z = 4 (R 0·036 for No 6769). The thiocyanate crystallizes from acetonitrile or pyridine as an S-bonded form (3) isomorphous with the arsine analogue: monoclinic, P 21/n, a 19·143(7), b 14·288(5), c 18·694(6) Å, β 98·81(2)°; Z = 4 (R 0·037 for No 4482). From 2-methylpyridine, remarkably, a solvate is obtained in which the thiocyanate is N-bonded (4): triclinic, P-1, a 27·261(5), b 14·767(3), c 13·319(1) Å, α 91·53(1), β 101·58(1), γ 92·29(2)°; Z = 4 (R 0·045 for No 6900). The cyanide is also monoclinic, P 21/n, a 19·442(7), b 14·267(3), c 17·741(6) Å, β 97·63(3)°, z = 4; R 0·057 for No 2487. The unsolvated 1 : 3 nitrate complex (6a) is monoclinic, P 21/n, a 19·602(5), b 14·455(1), c 17·727(2) Å, β 97·19(2)°, Z = 4; R was 0·034 for No 6522. The complex is isomorphous with the arsenic and phosphorus analogues, being mononuclear [(Ph3Sb)3Ag(O2NO)]. The ethanol solvate (6b) is triclinic, P-1, a 13·352(5), b 14·548(9), c 14·701(4) Å, α 81·64(4), β 84·45(3), γ 75·32(4)°, Z = 2; R was 0·058 for No 4702. Ag-Sb range between 2·6980(8) and 2·843(3) Å in the precise determinations; Ag-X are 2·481(4) and 2·52(1) Å (the two chlorides), 2·757(1) (I), 2·533(3) (SCN), 2·21(1) (NCS), 2· 09(3) (CN), 2·377(7) Å (unidentate ONO2)

Lewis-Base Adducts of Main Group 1 Metal Compounds. IV. Synthesis and Structure of the XLiL3 System (X = Cl, Br, I, L = 4-t-Butylpyridine, and X = I, L = Quinoline)

1988 ◽  
Vol 41 (3) ◽  
pp. 341 ◽  
Author(s):  
CL Raston ◽  
BW Skelton ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Main Group ◽  
Lewis Base ◽  
Similar Data ◽  
Metal Compounds ◽  
X Ray ◽  
Close Parallel ◽  
Group 1

Complexes [XLiL3], X = Cl , Br, I; L = 4-t-butylpyridine, (1)-(3) have been synthesized by recrystallization of the anhydrous lithium halide from the parent base, and characterized structurally by single-crystal X-ray structure determination. (1) and (2) are isomorphous (monoclinic, P21), a ≈ 11.8, b ≈ 12.1, c ≈ 11.8 Ǻ, β 120°, Z 2 (R 0.051, 0.040 for No 1491, 1499 'observed' reflections); (3) is orthorhombic, Pbca, a 22.119(10), b 21.108(10), c 12.845(10) Ǻ, Z 8, R 0.067 for No 967. (1)- (3) are all pseudo- trigonal and contain four-coordinate XLiN3 arrays [Li-X, 2.33(1); 2.53(1); 2.76(4) Ǻ; Li-N, 2.03(1)-2.11(1); 2.04(1)-2.09(2); 2.03(4)-2.07(4)Ǻ]. Similar data are also recorded for X = I, L = quinoline (4)[monoclinic, P21/c, a 15.684(6), b 7.693(4), c 26.758(12) Ǻ,β 107.71(3)°, Z 4; R 0.072, No 3096; Li-I, 2.78(2); Li-N, 2.08(2)- 2.13(2)Ǻ]. While a close parallel may be drawn between the similarity of the chemistry of lithium(I) and copper(I) in respect of (1)-(3), (4) is unusual being the first XML3 derivative for a quinoline -type ligand; it is a monoquinoline solvate.

Sign in / Sign up

Export Citation Format

Share Document