Confacial bioctahedral complexes of tungsten(IV) containing tungsten-to-tungsten bonds: X-ray crystal structures of di-μ-ethanethiolato-μ-sulfidobis[dichloro(dimethyl sulfide)-tungsten(IV) (W—W)] and tetraphenylphosphonium di-μ-ethane thiolato-μ-sulfido- bis[trichlorotungstate(IV) (W—W)]

1982 ◽  
Vol 60 (11) ◽  
pp. 1333-1338 ◽  
Author(s):  
P. Michael Boorman ◽  
Penelope W. Codding ◽  
K. Ann Kerr ◽  
Kelly J. Moynihan ◽  
Vikram D. Patel
Keyword(s):  
Single Crystal ◽  
Bond Length ◽  
Diffraction Study ◽  
Crystal Structures ◽  
Dimethyl Sulfide ◽  
Heavy Atom ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

The complex (Me2S)Cl2W(μ-S)(μ-SEt)2WCl2(Me2S), 1, has been prepared by reaction of [WCl4(Me2S)2] with 1 mol-equiv. of SiMe3(SEt) in CH2Cl2 solution. A single-crystal X-ray diffraction study shows that the molecule has a confacial bioctahedral structure with a W—W bond length of 2.526(2) Å. The structure was solved by heavy atom methods and refined to R = 0.061 and Rw = 0.061 for 2715 reflections with I ≥ 3σ(1). Crystals of 1 are triclinic, space group [Formula: see text], with a = 9.661(1), b = 10.695(1), c = 13.253(4) Å, α = 61.84(2), β = 66.98(2), and γ = 66.44(1)°, Z = 2.Reaction of 1with 2 mol-equiv. of Ph4PCl in CH2Cl2 solution yields (Ph4P)2[Cl3W(μ-S)(μ-SEt)2WCl3], 2. Crystals of 2 are triclinic, space group [Formula: see text], with a = 10.153(1), b = 13.043(1), c = 21.876(3) Å, α = 95.16(1), β = 96.48(2), and γ = 108.90(1)°, Z = 2. The structure was refined to R = 0.041, Rw = 0.048 for 2384 reflections with I ≥ 3σ(1); 2 also has a confacial bioctahedral structure with a W—W bond length of 2.522(1) Å.

scholarly journals Crystal Structures of Two Macrocyclic Bischalcones Possessing 26-Membered Rings

2015 ◽  
Vol 2015 ◽  
pp. 1-5
Author(s):  
Rina Mondal ◽  
Nayim Sepay ◽  
Debajyoti Ghoshal ◽  
Asok K. Mallik
Keyword(s):  
Hydrogen Bonding ◽  
Single Crystal ◽  
Crystal Structures ◽  
Membered Ring ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Hydrogen Bonding Interactions

Single crystal X-ray diffraction of two macrocyclic bischalcones, namely, (2E,25E)-11,17,33,37-tetraoxapentacyclo[36.4.0.05,10.018,23.027,32]dotetraconta-1(42),2,5,7,9,18,20,22,25,27,29,31,38,40-tetradecaene-4,24-dione(1) and (2E,24E)-11,16,32,37-tetraoxapentacyclo[36.4.0.05,10.017,22.026,31]dotetraconta-1(42),2,5,7,9,17,19,21,24,26,28,30,38,40-tetradecaene-4,23-dione(2), each containing a 26-membered ring, has been studied. Compound 1 belongs to the monoclinic system, space group C2/c with a = 34.3615(9) Å, b = 12.7995(3) Å, c = 14.6231(3) Å, β = 96.912(2)°,  V = 6,384.6(3) Å3, and Z = 8. Compound 2 is triclinic, space group P-1 with a = 10.066(2) Å, b = 10.670(3) Å, c = 16.590(3) Å, α = 85.95(2), β = 89.244(14), γ = 62.211(13), V = 1572.0(6) Å3, and Z = 2. Intermolecular C–H⋯O hydrogen bonding interactions are present in both compounds.

Synthesis and structure of M 0.5Bi3P2O10 (M = Ca, Sr, Ba, Pb) series

2003 ◽  
Vol 59 (5) ◽  
pp. 606-610 ◽  
Author(s):  
Digamber G. Porob ◽  
T. N. Guru Row
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Ternary Systems ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Ceramic Method ◽  
Space Group ◽  
X Ray

A series of M 0.5Bi3P2O10 compounds with M = Ca, Sr, Ba and Pb have been synthesized in MO–Bi2O3–P2O5 ternary systems by the ceramic method and the crystal structures were then solved using single-crystal X-ray diffraction data. These compounds are isostructural with Bi6.67P4O20 (triclinic, space group P\bar 1, Z = 2). The structures consist of infinite chains of Bi2O2 units along the c axis formed by linking BiO8 and BiO6 polyhedra. These chains are interconnected by MO8 polyhedra forming two-dimensional layers in the ac plane. The phosphate tetrahedra are sandwiched between these layers.

Structural studies in the iron(III)/chloride/α,α'-diimine system. I. The six-coordinate mononuclear fac-[FeCl3(phen)X] system, X = MeOH, H2O, Cl-

1983 ◽  
Vol 36 (10) ◽  
pp. 2031 ◽  
Author(s):  
PC Healy ◽  
JM Patrick ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Iron Complexes ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Chlorine Atoms ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

The crystal structures of three iron complexes [FeCI3(phen)(MeOH)].MeOH (I), [FeCl3(phen)(H2O)] (2) and [phenH]+ [FeCl4(phen)]- (3) have been determined by single-crystal X-ray diffraction methods at 295(1) K, and refined by least squares to residuals of 0.044 (1600 'observed' reflections), 0.040 (806) and 0.050 (2496), respectively. Crystals of (1) are monoclinic, P21/c, a 8.005(9), b 14.805(11), c 14.830(12) A, P 101.03(7)°, Z 4; for (2), triclinic, space group P1 , a 10.591(8), b 10.227(7), c 6.613(3) Ǻ, α 108.21(5), β 100.69(5), γ 91.98(6)°2, 2 ; for (3), triclinic, P1, a 18.560(8), b 10.302(5), c 6.981(3) Ǻ, α 106.79(4), β 94.50(4), γ 103.15(4)°, Z 2. In all structures, the iron atoms are six-coordinate, with the disposition of the three chlorine atoms being fac in (1) and (2).

Reactivity of electron-rich binuclear hydrides. Synthesis, structure, and reactions of [{(i-Pr)2PCH2CH2P(i-Pr)2}Rh]2(μ-H)(μ-OC6H5)

1986 ◽  
Vol 64 (1) ◽  
pp. 174-179 ◽  
Author(s):  
Michael D. Fryzuk ◽  
May-Ling Jang ◽  
Terry Jones ◽  
Frederick W. B. Einstein
Keyword(s):  
Single Crystal ◽  
Diffraction Study ◽  
Mononuclear Complex ◽  
Spectroscopic Techniques ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray ◽  
Hydrogen Bonded

The reaction of phenol with the binuclear rhodium hydride [{(i-Pr)2PCH2CH2P(i-Pr)2}Rh]2(μ-H)2 generates [{(i-Pr)2PCH2CH2P(i-Pr)2}Rh]2(μ-H)(μ-OC6H5), 2, which was characterized by both solution spectroscopic techniques and a single crystal X-ray diffraction study. The structure was solved using Patterson and Fourier methods and refined to R = 0.019 (Rw = 0.027) for 6062 reflections; crystals of the compound are triclinic, space group [Formula: see text], with a = 9.018(2), b = 12.988(2), c = 17.558(3) Å, α = 99.42(1), β = 92.62(2), γ = 91.85(2)°, and Z = 2. Further reaction with excess phenol leads to the mononuclear complex (η5-C6H5O)Rh{(i-Pr)2PCH2CH2P(i-Pr)2}•2C6H5OH, which contains two phenol units hydrogen bonded to the oxygen of the η5-cyclohexy]dienylone ligand. The presence of the bridging phenoxide ligand in 2 results in reduced reactivity as compared to the starting binuclear hydride dimer.

Syntheses and crystal structures of two new sodium borates [Na2(H2O)3][B5O8(OH)2] and Na[enH2][B7O10(OH)4]

2016 ◽  
Vol 71 (1) ◽  
pp. 15-21 ◽  
Author(s):  
Yan-Jing Wang ◽  
Ai-Quan Jia ◽  
Xing-Shun Chen ◽  
Hua-Tian Shi ◽  
Qian-Feng Zhang
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Building Blocks ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

AbstractTwo new sodium borates [Na2(H2O)3][B5O8(OH)2] (1) and Na[enH2][B7O10(OH)4] (2) have been synthesized and their structures have been determined by single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic system space group C2/c with a = 11.118(2), b = 16.442(2), c = 13.572(2) Å, β =112.90(1)°, V = 2285.4(5) Å3, and Z = 4. Compound 2 crystallizes in the triclinic space group P1̅, with a = 7.4974(9), b = 8.349(2), c = 11.746(2), α = 93.98(1), β = 97.25(1), γ = 101.18(1)°, V = 712.2(2) Å3, and Z = 2. Compound 1 possesses {Na2B5O8(OH)2·3H2O}n chains which form through the connection of the fundamental building blocks (FBBs) [B5O8(OH)2]2– by sharing Na+ ions, while compound 2 has infinite {Na[B7O10(OH)4]}n sheets which form via the connection of the FBBs [B7O10(OH)4]3– by common Na+ ions.

Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalyse von cis-[ReCl4X2]2-, X = NCS, NCSe / Crystal Structures, Vibrational Spectra and Normal Coordinate Analysis of cis-[ReCl4X2]2-, X = NCS, NCSe

1998 ◽  
Vol 53 (11) ◽  
pp. 1329-1334 ◽  
Author(s):  
L. Homolya ◽  
S. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Normal Coordinate Analysis ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Valence Force ◽  
Space Group ◽  
X Ray ◽  
Valence Force Field ◽  
Ir And Raman

The crystal structures of cis-(n-Bu4N)2[ReCl4(NCS)2] (triclinic, space group P1̅, a = 11,245( 1), b = 20.174(3), c = 21.320(8) Å, a =109.06(2), β = 96.46(2), γ = 98.22(5)°, Z = 4) and cis-(Ph4P)2[ReCl4(NCSe)2]·2CH2Cl2 (triclinic, space group P1̅, a = 10.341(2), b = 13.436(3), c = 19.616(4) Å, α = 92.70(2), β = 92.02(2), γ = 89.99( 1)°, Z= 2) have been determined by single crystal X-ray diffraction analysis. Both ambidentate ligands NCS and NCSe are bonded via the N atom. Using the molecular parameters of the X-ray determinations the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts have been assigned by normal coordinate analysis based on a modified valence force field. The valence force constants fd(ReN) are 1,78(NCS) and 1,79(NCSe) mdyn/ Å.

scholarly journals Darstellung und Kristallstrukturen von (PH4P)4Sb8I28 und (Ph4P)Sb3I10(Ph = C6H5) / Synthesis and Crystal Structures of (PH4P)4Sb8I28 and (Ph4P)Sb3I10(Ph = C6H5)

1987 ◽  
Vol 42 (12) ◽  
pp. 1493-1499 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Detlev Haase
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Lone Pair ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Molar Ratios ◽  
Polymeric Chains ◽  
Bond Strengths

AbstractThe compounds (Pn4P)4Sb8I28 (1) and (Ph4P)Sb3I10 (2) were prepared by the reaction of SbI3 and Ph4PI in acetonitrile (molar ratios 2:1 and 3:1 respectively). The structures of 1 and 2 were determined from single crystal X-ray diffraction data.1 crystallizes in the triclinic space group P1̄ with a - 1321.7(5). b = 1346.7(5), c = 2201.8(8) pm, α = 104.18(2). β = 99.92(2), γ = 100.33(2)°; 2: monoclinic, C2/c, a = 2371.1(2), b = 745.0(1), c = 2495.1(2) pm, β = 100.75(1)°.Whereas 1 exhibits isolated Sb8I284- ions, the anions of 2 are built up of polymeric chains [Sb3I10- ]∞. In both compounds the distorted Sbl6 octahedra are linked by common edges. The Sb-I distances are in the range between 277.4 and 354.8 pm (1) and between 277.4 and 342.4 pm (2). The observed structures do not only depend on stoichiometry, the nature of the counter cations, and the possibility of oligomerisation but also on the wide variety of the Sb-I bond strengths and the different bridges formed by iodine.The lone pair of Sb(III) seems to be predominantly 5 s2.

On racemic and L-malates: a comparison of their crystal structures

2004 ◽  
Vol 219 (2) ◽  
Author(s):  
Michel Fleck ◽  
Ekkehart Tillmanns ◽  
Ladislav Bohatý ◽  
Peter Held
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
Powder Diffraction File ◽  
Space Group ◽  
X Ray

AbstractThe crystal structures of eight different L-malates have been determined and refined from single-crystal X-ray diffraction data. The compounds are the monoclinic (space groupIn addition, for all the compounds, powder diffraction data were collected, analysed and submitted to the powder diffraction file (PDF).

scholarly journals High-pressure single crystal X-ray diffraction study of the linear metal chain compound Co3(dpa)4Br2·CH2Cl2

2015 ◽  
Vol 44 (19) ◽  
pp. 9038-9043 ◽  
Author(s):  
S. R. Madsen ◽  
J. Overgaard ◽  
D. Stalke ◽  
B. B. Iversen
Keyword(s):  
High Pressure ◽  
Single Crystal ◽  
Diffraction Study ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Chain ◽  
Chain Compound

The effects of non-hydrostaticity in n-pentane-isopentane were overcome by annealing, and accurate crystal structures of Co3(dpa)4Cl2·CH2Cl2 were determined above 10 GPa.

Orthoborate Halides with the Formula (M+II)5(BO3)3X: Syntheses, Crystal Structures and Raman Spectra of Eu5(BO3)3Cl and Ba5(BO3)3X (X = Cl, Br)

2011 ◽  
Vol 66 (4) ◽  
pp. 359-365 ◽  
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvo
Keyword(s):  
Single Crystal ◽  
Single Crystals ◽  
Crystal Structures ◽  
Raman Spectra ◽  
Direct Synthesis ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Incremental Volume

Single crystals of Eu5(BO3)3Cl were obtained by serendipity by reacting Eu2O3 and Mg with B2O3 at 1300 K in the presence of an NaCl melt for 13 h in silica-jacketed Nb ampoules. Ba5(BO3)3X (X = Cl, Br) crystals were formed by direct synthesis from appropriate amounts of Ba(OH)2, H3BO3 and the respective barium halide (hydrate) in alumina crucibles kept in the open atmosphere at 1300 K for 13 h. The crystal structures of the title compounds were determined with single-crystal X-ray diffraction. All compounds crystallize isotypically to Sr5(BO3)3Cl in the orthorhombic space group C2221 (no. 20, Z = 4) with the lattice parameters a = 1000.34(7), b = 1419.00(9), c = 739.48(5) pm for Eu5(BO3)3Cl, a = 1045.49(5), b = 1487.89(8), c = 787.01(4) pm for Ba5(BO3)3Cl, and a = 1048.76(7), b = 1481.13(9) and c = 801.22(5) pm for Ba5(BO3)3Br. The Raman spectra of all compounds were acquired and are presented and compared to literature data. The incremental volume of the orthoborate (BO3)3− anion has been determined and is compared to the Biltz volume

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