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).

Structural Systematics of Metal Acetylide Complexes. II. X-Ray Studies of Some Nickel σ-Acetylide Complexes

1998 ◽  
Vol 51 (3) ◽  
pp. 219 ◽  
Author(s):  
Ian R. Whittall ◽  
Mark G. Humphrey ◽  
David C. R. Hockless
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Trans Influence

The structures of Ni(C≡CR)(PPh3)(η-C5H5) (R = Ph (1), C6H4-4-NO2 (2), 4-C6H4C6H4-4′-NO2 (3), (E)-4-C6H4CH=CHC6H4-4′-NO2 (4), 4-C6H4C≡CC6H4-4′-NO2 (5), 4-C6H4N=CHC6H4-4′-NO2 (6)) have been determined by single-crystal X-ray diffraction studies, refining by full-matrix least-squares analysis. For (1), crystals are triclinic, space group P-1, with a 10·094(2), b13·429(3), c 18·835(5) Å,α 103·24(2), β 91·50(2), γ 90·10(2)°, Z 4, 5844 unique reflections (595 parameters), converging at R 0·033 and Rw 0·024. For (2), crystals are orthorhombic, space group Pna21, with a 16·799(2), b 8·681(2), c 17·485(2) Å, Z 4, 1774 unique reflections (325 parameters), converging at R 0·031 and Rw 0·029. For (3), crystals are monoclinic, space group P 21/c, with a 11·140(3), b 18·282(4), c 15·296(2) Å, β 105·18(2)°, Z 4, 3132 unique reflections (397 parameters), converging at R 0·039 and Rw 0·024. For (4), crystals are monoclinic, space group P 21/n, with a 12·929(7), b 16·953(8), c 15·601(7) Å, β 112·55(3), Z 4, 3023 unique reflections (397 parameters), converging at R 0·039 and Rw 0·025. For (5), crystals are monoclinic, space group P 21/n, with a 12·710(5), b 16·882(3), c 15·693(4) Å, β 111·37(3)°, Z 4, 3216 unique reflections (397 parameters), converging at R 0·035 and Rw 0·030. For (6), crystals are monoclinic, space group P 21/n, with a 12·594(1), b 16·936(2), c 15·611(1) Å, β 112·476(5)°, Z 4, 3564 unique reflections (397 parameters), converging at R 0·038 and Rw 0·041. For structurally characterized 18-electron (cyclopentadienyl)nickel(II) acetylide complexes, statistically insignificant decreases in the average Ni-C(1) distance and trans influence and an increase in the average C(1)-C(2) parameter are observed on introduction of an acceptor substituent at the alkynyl ligand.

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. II. Ionic derivatives of stoichiometry FeCl3(phen,bpy)1,1.5

1983 ◽  
Vol 36 (10) ◽  
pp. 2043 ◽  
Author(s):  
BN Figgis ◽  
JM Patrick ◽  
PA Reynolds ◽  
BW Skelton ◽  
AH White ◽  
...  
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations ◽  
Derivatives Of

The crystal structures of the 1 : 1 adducts of FeCl3 with 2,2'-bipyridine (bpy) (1) and 1,10-phenanthroline (phen) (2), as recrystallized from nitromethane, have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by least squares to residuals of 0.038 and 0.032 for 1341 and 3968 'observed' reflections; the result for (2) is a redetermination. Crystals of (1) are orthorhombic, Pbnb, a 15.013(4), b 13.510(5), c 12.471(3) Ǻ, Z 4. Crystals of (2) are triclinic, P1, a 15.823(5), b 11.021(5), c 8.200(3) Ǻ, α 80.27(3), β 76.78(3), γ 89.64(3)°, Z 2. Both complexes haw the stoichiometry (FeCl3)1(bpy,phen)1, but are formulated as cis-[Fe(bpy,phen)2Cl2] [FeCl4]; in both compounds, the Fe-N distance is c. 2.20, (trans to Cl), 2.1, Ǻ(cis to Cl), while Fe-Cl, c. 2.2, Ǻ, is short. The structure determinations of Fe2Cl6(phen,bpy)3 as [Fe(phen)2Cl2]+ [Fe(phen)Cl4]- (3) and [Fe(bpy)2Cl2]+ [Fe(bpy)Cl4]- (4) are also reported. Compound (3) (from acetonitrile solution) is triclinic, P1, a 16.502(5), b 11.857(3), c 10.653(3) Ǻ, α 84.92(2), β 72.66(2), γ 74.80(2)°, Z 2, and was refined to a residual of 0.034 for 5540 'observed' reflections. The cation geometry is similar to that of (2); in the anion, the two Fe-CI bonds trans to each other are long [2.377(1) and 2.365(1) Ǻ] while those trans to the Fe-N bonds are short [2.287(1) and 2.318(1) Ǻ]. Fe-N distances are 2.216(3) and 2.220(3) A. Compound (4) (as its nitromethane solvate) is also triclinic, P1, a 14.480(7), b 12.645(5), c 10.678(4) Ǻ, α 95.68(3), β 109.21(3), γ 9258(3)°, Z 2; a residual of 0.042 was obtained for 4962 'observed' reflections. Cation and anion metal geometries are similar to those of (3).

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.

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.

Synthesis and Structures of μ3-Oxo-centered Mixed-valent Trinuclear Iron Complexes with 1-Methyl-imidazole Ligands

2007 ◽  
Vol 62 (9) ◽  
pp. 1117-1122 ◽  
Author(s):  
Ji-Xiang Dai ◽  
Fang-Hui Wu ◽  
Alexander Rothenberger ◽  
Qian-Feng Zhang
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Iron Complexes ◽  
Iron Complex ◽  
Methanol Solution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Elemental Analyses ◽  
Methyl Imidazole ◽  
Imidazole Ligands

Treatment of the μ3-oxo-centered mixed-valent trinuclear iron complex [Fe3(μ3-O)(μ-OAc)6- (H2O)3] (1) in methanol solution with one, two, or three equivalents of 1-methyl-imidazole (C4H6N2) afforded the substitution products [Fe3(μ3-O)(μ-OAc)6(H2O)2(C4H6N2)] (2), [Fe3(μ3-O)(μ-OAc)6- (H2O)(C4H6N2)2] (3), and [Fe3(μ3-O)(μ-OAc)6(C4H6N2)3] (4), respectively. Complexes 2 - 4 were characterized by spectroscopic and elemental analyses, and the crystal structures of complexes 3 · 1.5MeOH· 2H2O and 4 have been determined by single-crystal X-ray diffraction. The results indicate that in 2 - 4 the trinuclear core unit [Fe3(μ3-O)(μ-OAc)6] of 1 is preserved.

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).

Sign in / Sign up

Export Citation Format

Share Document