Lewis-Base Adducts of Lead(II) Compounds. XX. Synthesis and Structure of the 1:1 Adduct of Pyridine With Lead(II) Thiocyanate

1996 ◽  
Vol 49 (10) ◽  
pp. 1165 ◽  
Author(s):  
JM Harrowfield ◽  
H Miyamae ◽  
BW Skelton ◽  
AA Soudi ◽  
AH White
Keyword(s):  
Nitrogen Atom ◽  
Single Crystal ◽  
Structure Determination ◽  
Room Temperature ◽  
Lewis Base ◽  
Two Dimensional ◽  
X Ray

The synthesis and room-temperature single-crystal X-ray structure determination are recorded for a 1:1 adduct of lead(II) thiocyanate with pyridine (' py '). [( py ) Pb (SCN)2](∞|∞) is triclinic, Pī , a 10.544(1), b 7.3729(7), c 6.705(2) Ǻ, α 103.91(2), β 95.99(2), γ 100.51(1)°, Z = 2 f.u .; R was 0.041 for 3226 'observed' (I > 3σ(I)) reflections. The structure is a two-dimensional polymer in the be plane with eight-coordinate ( py -N)PbN3S4 linked by the familiar four- membered Pb2S2 and eight-membered Pb2(NCS)2 motifs by way of bridging thiocyanate groups; one of the latter, unusually, has a bifurcating bridging nitrogen atom leading to the introduction of Pb2N2 motifs. The structure of the parent lead(II) thiocyanate is also discussed.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXXIV Synthesis and Structure of the 1 : 1 Adduct of Silver(I) Nitrate with Triphenylstibine

1997 ◽  
Vol 50 (6) ◽  
pp. 671 ◽  
Author(s):  
Effendy ◽  
John D. Kildea ◽  
Allan H. White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Related Species ◽  
Room Temperature ◽  
Structural Data ◽  
Lewis Base ◽  
One Dimensional ◽  
X Ray ◽  
The One

The synthesis and room-temperature single-crystal X-ray structure determination of the 1 : 1 adduct of silver(I) nitrate with triphenylstibine, AgNO3/SbPh3 (1 : 1), is recorded, being monoclinic, Cc,a 12·824(2), b 15·794(4),c 9·796(2) Å, β 117·50(1)°, Z= 4; conventional R on F was 0·030 for 2881 independent ‘observed’ (I > 3σ(I)) reflections. The complex is a one-dimensional polymer with bridging nitrate groups, resembling in this respect its phosphine and arsine analogues. The completion of this study, along with related species recorded in accompanying papers, means that full structural data are now available for the complete array AgNO3/EPh3 (1 : n), E = P, As, Sb, n = 1–4, with the one exception of E = Sb, n = 2.

scholarly journals Synthesis and Single Crystal X-Ray Structure of Bis[4-oxo-3- (2-ethoxycarbonylphenyl)-3,4-dihydroquinazolin-2-yl]disulfide

2009 ◽  
Vol 64 (9) ◽  
pp. 1065-1069 ◽  
Author(s):  
Mehdi Rimaz ◽  
Jabbar Khalafy ◽  
Khadijeh Tavana ◽  
Katarzyna Ślepokura ◽  
Tadeusz Lis ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Structure Determination ◽  
Room Temperature ◽  
Sodium Ethoxide ◽  
Reaction Conditions ◽  
X Ray ◽  
Ethyl Nitroacetate ◽  
C Nmr

Diethyl 2,2´-thiocarbonyl-bis(azanediyl)dibenzoate was synthesized from the reaction of ethyl anthranilate with thiophosgene. Its treatment with sodium ethoxide in ethanol at room temperature gave ethyl 2-(4-oxo-2-thioxo-1,2-dihydroquinazolin-3(4H)-yl) benzoate, whereas in the presence of ethyl nitroacetate and under the same reaction conditions, the corresponding bis(quinazolin)disulfide was formed. Its structure was confirmed by IR, 1H and 13C NMR spectroscopy elemental analysis and single crystal X-ray structure determination.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. XXXVII. A Novel Isomerism in the Heterobimetallic 1:1 Adducts of Copper(I) Halides With Tris(dithiocarbamato)cobalt(III)

1988 ◽  
Vol 41 (6) ◽  
pp. 839 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Lewis Base ◽  
X Ray

Reaction of copper(I) iodide with tris (N,N- dipropyl -and N, N- diisopropyl-dithiocarbamato )cobalt(III), [Co(S2CNR2)3 ≡ Co( dtc )3](R = Pr or Pri ), yields 1:1 adducts which have been characterized by single-crystal X-ray structure determination. Crystals of the propyl species are monoclinic, P21/c, a 13.722(7), b 16.854(7), c 16.787(8)Ǻ, β 121.66(3)°, R was 0.056 for No 2834 'observed' reflections. The isopropyl derivative is orthorhombic, Ccca , a 33.93 (1), b 13.616(8), c 14.574(5)Ǻ; R was 0.075 for No 726. Each adduct is dimeric [Co( dtc )3](CuI2Cu)[Co( dtc )3]; the propyl derivative has crystallographically imposed i symmetry, whereas the isopropyl adduct has quasi-222 symmetry. Thus, the chiralities of the pair of Co( dtc )3 moieties in the dipropyl adduct are opposite, whereas in the isopropyl adduct they are the same.

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. 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. XVII. Synthetic and Structural Studies of Some 1:1 Adducts of 2,2':6,2'-Terpyridine With Lead(II) Salts

1996 ◽  
Vol 49 (10) ◽  
pp. 1135 ◽  
Author(s):  
LM Engelhardt ◽  
JM Harrowfield ◽  
H Miyamae ◽  
JM Patrick ◽  
BW Skelton ◽  
...  
Keyword(s):  
Water Molecule ◽  
Single Crystal ◽  
Room Temperature ◽  
Lewis Base ◽  
Polymeric Chain ◽  
Lead Atom ◽  
X Ray ◽  
Structure Determinations ◽  
Pass Through ◽  
Nitrate And Nitrite

Syntheses and room-temperature single-crystal X-ray structure determinations are recorded for 1:1 adducts of 2,2':6',2"-terpyridine (' tpy ') with the lead(II) oxoanion salts perchlorate, nitrate and nitrite, ( tpy ) Pb ( oxoanion )2. All structures are monoclinic, C2/c, Z = 4, with approximate ranges a from 9 to 11 Ǻ, b from 16 to 20 Ǻ, c from 9.8 to 13.8 Ǻ, β from 113 to 130° and V from 1650 to 1850 Ǻ3. In all cases the lead(II) atoms are disposed on crystallographic 2 axes which also pass through the axis of the central tpy ring; a pair of symmetry related oxoanions link successive lead atoms in a one-dimensional polymeric chain parallel to the ac cell diagonal, one pair of oxygen atoms functioning as an O,O'-bidentate with another oxygen (replaced by the nitrogen in the nitrite) bridging to the adjacent lead atom; the third anionic oxygen atom in the nitrate is replaced by a water molecule in the nitrite, which thus becomes a monohydrate. Residuals were 0.030, 0.034 and 0.040 for 2122, 1564 and 2059 independent 'observed' (I > 3σ(I)) reflections respectively. Also recorded are the syntheses and room-temperature single-crystal X-ray structure determinations for 1:1 aducts of 2,2':6',2"-terpyridine with lead(II) chloride, bromide and iodide, the chloride and bromide being hydrated. ( tpy )PbCl2.H2O is monoclinic, P 21/c, a 8.938(1), b 15,210(7), c 13.414(3) Ǻ, β 115.17(1)°, Z = 4 f.u .; R was 0.036 for No = 3346 independent, 'observed' reflections. The complex is centrosymmetric, binuclear [( tpy ) (H2O)( Cl ) Pb (μ- Cl )2Pb( Cl )(OH2)( tpy )], with the two lead atoms linked by bridging chlorine atoms; the lead atoms are seven-coordinate N3,O,ClPb(μ- Cl )2. The bromide ( tpy )PbBr2.2/3H2O, triclinic, Pī, a 12.360(6), b 12.452(4), c 18.372(6) Ǻ, α 108.31(3), β 109.44(3), γ 90.56(3)°, Z = 6 f.u ., R being 0.046 for No 7282, is in fact trinuclear [Pb3Br6( tpy )6].2H2O, a novel and elegant oligomer with quasi-2 symmetry in which a central lead atom (on the quasi-2 axis) is seven-coordinated [( tpy ) Pb (μ-Br)4] with the associated bromides bridging to a pair of peripheral lead atoms, also seven coordinated, [( tpy )(Br) Pb (μ-Br)3]. Unsolvated ( tpy )PbI2, triclinic, Pī , a 10.834(3), b 9.023(3), c 8.906(2) Ǻ, α 80.34(2), β 89.40(2), γ 79.78(2)°, Z = 2 f.u ., R 0.031 for No 2347 is, like the chloride, centrosymmetric binuclear, [( tpy )(I) Pb (μ-I)2Pb(I)( tpy )], but with the lead(II) now six-coordinate N3(I) Pb (μ-I)2. In both chloride and iodide, the tpy plane is approximately normal to the Pb ... Pb line with the water molecule of the chloride approximately trans to the central tpy nitrogen; in the iodide that site is occupied by the terminal halide.

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.

First crystal-structure determination of natural lansfordite, MgCO3·5H2O

2017 ◽  
Vol 81 (5) ◽  
pp. 1063-1071 ◽  
Author(s):  
Fabrizio Nestola ◽  
Anatoly V. Kasatkin ◽  
Sergey S. Potapov ◽  
Olga YA. Chervyatsova ◽  
Arianna Lanza
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Single Crystal ◽  
Structure Determination ◽  
Room Temperature ◽  
Crystal Structure Determination ◽  
Hydrogen Atoms ◽  
Synthetic Analogues ◽  
X Ray

AbstractThis study presents the first crystal-structure determination of natural MgCO3·5H2O, mineral lansfordite, in comparison with previous structural works performed on synthetic analogues. A new prototype single-crystal X-ray diffractometer allowed us to measure an extremely small crystal (i.e. 0.020 mm × 0.010 mm × 0.005 mm) and refine anisotropically all non-hydrogen atoms in the structure and provide a robust hydrogen-bond arrangement. Our new data confirm that natural lansfordite can be stable for several months at room temperature, in contrast with previous works, which reported that such a mineral could be stable only below 10°C.

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 Lead(II) Compounds. XVI. Synthetic and Structural Studies of Some Adducts of 2-Aminomethylpyridine With Lead(II) Compounds

1996 ◽  
Vol 49 (10) ◽  
pp. 1127 ◽  
Author(s):  
JM Harrowfield ◽  
H Miyamae ◽  
BW Skelton ◽  
AA Soudi ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Room Temperature ◽  
Lewis Base ◽  
Structural Studies ◽  
Problem Structure ◽  
Coordination Environment ◽  
X Ray ◽  
The Third ◽  
Structure Determinations ◽  
Centrosymmetric Dimers

Syntheses and room-temperature single-crystal X-ray structure determinations are recorded for 2:1 adducts of 2-aminomethylpyridine ('amp') with lead(II) nitrate and thiocyanate . [(amp)2Pb(NO3)2]2 is triclinic, Pī, a 11.616(4), b 11.145(6), c 7.341(3) Ǻ, α 83.87(4), β 89.17(3), γ 64.12(3)°, Z = 1 dimer ; R was 0.043 for No 3529 independent 'observed' (I > 3σ(I)) reflections. [(amp)2Pb(SCN)2]2 is also triclinic, Pī , a 12.121(9), b 9.301(14), c 8.615(8) Ǻ, α 70.11(10), β 84.00(7), γ 79.38(10)°, Z = 1 dimer (R 0.033 for No 3467). Both complexes are centrosymmetric dimers ; the coordination environment is made up in each case of a pair of N,N°-bidentate bases, one terminally bound anion (O,O°-chelating nitrate or S-bonded thiocyanate ) and bridging anions. In the case of the thiocyanates, these bridge end-on, so that the lead(II) environment is seven-coordinate PbN5S2; in the nitrate, the anion chelates through two of its oxygen atoms, bridging via the third, so that the lead(II) environment is nine-coordinate PbN4O5. A 'problem structure', [(amp)2Pb(ClO4)2], monoclinic, C2/c (?), a 14.528(3), b 8.203(3), c 15.495(6) Ǻ, β 91.14(3)°, Z = 4 f.u ., R 0.044 for No 1775, is also recorded, the crystal seemingly a disordered aggregate of [(N, N′-amp)2Pb(OClO3)2] moieties.

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