Ditopic thiacyclophanes containing the S(CH2)2X(CH2)2S (X = O, S) linkage. Synthesis and structures of 2,5,8,17,20,23-hexathia[9](1,2)[9](4,5)cyclophane and 5,20-dioxa-2,8,17,23-tetrathia[9](1,3)[9](4,6)-2,5-bis(ethoxy)cyclophane

1994 ◽  
Vol 72 (7) ◽  
pp. 1728-1734 ◽  
Author(s):  
Stephen J. Loeb ◽  
George K.H. Shimizu
Keyword(s):  
Crystal Structures ◽  
Aromatic Ring ◽  
Ring Closure ◽  
Structural Variations ◽  
Triclinic Space Group ◽  
Space Group ◽  
Target Molecule ◽  
Double Ring ◽  
Linkage Synthesis

The Cs+/DMF mediated reactions of 1,2,4,5-tetra(bromomethyl)benzene and 1,2,4,5-tetra(bromomethyl)3,6-bis(ethoxy)benzene with dithiols HSCH2CH2XCH2CH2SH (X = S,O) were explored in order in order to ascertain the effect of structural variations on the regioselectivity of double ring-closure. Although a structure with bis(ortho) geometry was the target molecule, the major products are those with a bis(meta) structure. Two crystal structures, one with a bis(ortho) structure, 2,5,8,17,20,23-hexathia[9](1,2)[9](4,5)cyclophane, 1, and one with a bis(meta) structure, 5,20-dioxa-2,8,17,23-tetrathia[9](1,3)[9](4,6)−2,5-bis(ethoxy)cyclophane, 7, are reported. 1 crystallized in the triclinic space group [Formula: see text] with a = 8.583(3), b = 11.806(3), c = 5.448(2) Å, α = 97.18(2), β = 107.18(2), γ = 99.40(2)°, V = 511.6(6) Å3, and Z = 1. The structure refined to R = 6.48% and Rw = 7.13% for 1020 reflections with Fo2 > 3σ(Fo2). 7 crystallized in the triclinic space group [Formula: see text] with a = 9.568(2), b = 9.577(2), c = 8.312(2) Å, α = 113.53(2), β = 94.58(2), γ = 114.94(2)°, V = 604.3(7) Å3 and Z = 1. The structure refined to R = 3.86% and Rw = 4.20% for 1129 reflections with Fo2 > 3σ(Fo2). Both compounds sit on a crystallographic centre of symmetry and have the thioether linkages oriented on opposite sides of the central aromatic ring.

Synthesis and Crystal Structures of Three Carboxylate- Bridged Tetranuclear Copper(II) - Lanthanide(III) Complexes of Ph3P+CH2CH2CO2−

1999 ◽  
Vol 52 (10) ◽  
pp. 983 ◽  
Author(s):  
Yang-Yi Yang ◽  
Seik Weng Ng ◽  
Xiao-Ming Chen
Keyword(s):  
Oxygen Atom ◽  
Crystal Structures ◽  
Triclinic Space Group ◽  
Coordination Environment ◽  
Space Group ◽  
Bond Angles ◽  
Bond Lengths ◽  
Metal Atoms ◽  
Apical Site

Three tetranuclear copper(II)–lanthanide(III) complexes of triphenylphosphoniopropionate (Ph3P+CH2CH2CO2−,tppp), namely [Cu2Ln2(tppp)8(H2O)8](ClO4)10·2H 2 O [Ln = EuIII, NdIII or CeIII], were synthesized and characterized by crystallography. The EuIII complex crystallizes in the triclinic space group P1 – with a 16.249(7), b 17.185(11), c 17.807(11) Å, α 69.750(10), β 89.230(10), γ 84.070(10)˚, V 4639(5) Å3, Z 1. In the crystal structures, four tppp ligands bridge a pair of CuII and tetraaquo-EuIII atoms (Cu···Eu 3.527(2) Å) through their µ2-carboxylato ends to form a dinuclear subunit; two of these subunits are additionally linked by one of the CuII -bonded carboxylato oxygen ends, across a centre of inversion, to furnish a dimeric tetranuclear [Cu(tppp)4 Eu(H2O)4]2 species (Cu···Cu 3.323(2) Å). This CuII -bonded oxygen atom occupies the apical site of the square-pyramidal coordination environment of the CuII atom. The EuIII atom is eight-coordinated in a square-antiprismatic geometry. The NdIII and CeIII complexes are isomorphous to the EuIII complex, and only minor differences in bond lengths and bond angles involving the metal atoms are noted.

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 Crystal Structures and Magnetic Properties of Two New Cobalt(II) Complexes with Triazole-Substituted Nitronyl and Imino Nitroxide Radicals

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Jing Chen ◽  
You-Juan Zhang ◽  
Kun-Tao Huang ◽  
Qiang Huang ◽  
Jun-Jie Wang
Keyword(s):  
Magnetic Properties ◽  
Metal Ions ◽  
Crystal Structures ◽  
Magnetic Measurements ◽  
Nitroxide Radicals ◽  
Triclinic Space Group ◽  
Space Group ◽  
Imino Nitroxide

Two new cobalt(II) complexes of formula [Co(hfac)2(NITphtrz) 1 and Co(hfac)2(IMphtrz) 2] have been prepared and characterized structurally [where NITphtrz = 4,4,5,5-tetramethyl-2-(2-phenyl-1,2,3-triazole-4-yl)imidazoline-1-oxyl-3-oxide and IMphtrz = 4,4,5,5-tetramethyl-2-(2-phenyl-1,2,3-triazole-4-yl)imidazoline-1-oxyl]. All of the complexes crystallize in an isomorphous triclinic space group P1- with the Co(II) ion octahedrally coordinated via the bidentate chelating mode. The magnetic measurements show that two complexes exhibit antiferromagnetic interactions between the metal ions and the nitroxide radicals.

The Crystal Structures of 2-(3’-Hydroxypropyl)benzimidazolium Hexa- and Tetrachloroplatinate

2005 ◽  
Vol 60 (2) ◽  
pp. 164-168 ◽  
Author(s):  
A. Elmali ◽  
Y. Elerman ◽  
G. Eren ◽  
F. Gümüş ◽  
I. Svoboda
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Intermolecular Hydrogen Bonds ◽  
Triclinic Space Group ◽  
Space Group

2-(3’-Hydroxypropyl)benzimidazolium (Hhpb) hexa- and tetrachloroplatinate (C10H13N2O)2·[PtCl6] 1 and (C10H13N2O)2·[PtCl4] 2 were synthesized and their crystal structures determined. Compound 1 is monoclinic, space group P21/n, a = 8.800(1), b = 14.389(2), c = 10.264(2) Å, β = 98.540(10)°, V = 1285.3(3) Å3, Z = 2 and Dc = 1.959 g cm−3. Compound 2 is triclinic, space group P1̄, a=7.8480(10), b=9.0460(10), c=9.6980(10) Å ,α =65.420(10), β =68.810(10), γ = 76.770(1)°,V =581.26(4) Å3, Z =1 and Dc =1.969 g cm−3. In both compounds, the Pt atoms reside at a centre of inversion. Compounds 1 and 2 are comprised of 2-(3’-hydroxypropyl)benzimidazolium (Hhpb)+: (C10H12N2O)+ and [PtCl6]2− and [PtCl4]2− ions, respectively, linked by intermolecular hydrogen bonds N...Cl [range from 3.428(3) to 3.584(4) Å ], N···O [2.769(5) Å ] and O···Cl [3.338(4) and 3.321(3) Å ] for 1, and N···Cl [3.162(7) Å ], N···O [2.749(8) Å ] and O···Cl [3.289(6) Å ] for 2.

New Thiostannates Synthesized Under Solvothermal Conditions: Crystal Structures of (trenH)2Sn3S7 and {[Mn(tren)]2Sn2S6}

2012 ◽  
Vol 67 (10) ◽  
pp. 1098-1106 ◽  
Author(s):  
Nicole Pienack ◽  
Diana Schinkel ◽  
Angela Puls ◽  
Marie-Eve Ordolff ◽  
Henning Lühmann ◽  
...  
Keyword(s):  
Band Gap ◽  
Crystal Structures ◽  
Bond Formation ◽  
Lattice Parameters ◽  
Triclinic Space Group ◽  
Space Group ◽  
Trigonal Bipyramidal ◽  
Solvothermal Conditions

The two new thiostannate compounds (trenH)2Sn3S7 (1) and {[Mn(tren)]2Sn2S6} (2) (tren=tris-2-aminoethylamine) were obtained under solvothermal conditions. Compound 1 crystallizes in the hexagonal space group P63/mmc with a=13.2642(19), c=19.078(3) Å, V =2906.9(7) Å3. The layered [Sn3S7]2- anion is constructed by Sn3S4 semi-cubes sharing common edges. The layers are characterized by large hexagonal pores with dimensions of about 11×11 Å2. Compound 2 crystallizes in the triclinic space group P1̄ with lattice parameters a=7.6485(7), b=8.1062(7), c=12.1805(11) Å, α =97.367(11), β =103.995(11), γ = 108:762(10)°, V =676.17(10) Å3. The [Sn2S6]4- anion is composed of two edge-sharing SnS4 tetrahedra and joins two Mn2+-centered complexes by Mn-S bond formation. The Mn2+ cation is in a trigonal-bipyramidal environment of four N atoms of the tren ligand and one S atom of the thiostannate anion. Both compounds are semiconductors with a band gap of 2:96 eV for 1 and of 2:75 eV for 2.

Kristallstrukturen der iodierten closo-Hexaborate trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P)2[B6H2I4] · 2 CH3CN und (CH2Py2)[B6HI5]/Crystal Structures of the Iodized closo-Hexaborates trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P )2[B6H2I4] · 2 CH3CN and (CH2Py2)[B6HI5]

1998 ◽  
Vol 53 (2) ◽  
pp. 206-210 ◽  
Author(s):  
D. Sonnak ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

Abstract X-ray structure determinations have been performed on single crystals of trans-(Ph4P)2-[B6H4I2] (1) (triclinic, space group P1̄, a = 9.9680(12), b = 10.9690(11), c = 11.0470(14) Å,α = 88.167(9), β = 80.466(12), γ = 68.839(11)°, Z = 1), mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2 (2)(triclinic, space group P1̄, a = 11.8694(11), b = 15.1699(13), c = 17.051(2) Å, α = 75.118(9), β = 71.953(10), γ = 69.331(8)°, Z = 2), trans-(Ph4P )2[B6H2I4] · 2 CH3CN (3) (monoclinic, space group P21/n, a = 14.9665(10), b = 7.6783(10), c = 23.385(3) Å, β = 95.78(9)°, Z = 2), and (CH2Py2)[B6HI5] (4) (orthorhombic, space group Pnma, a = 13.660(2), b = 11.8711(13), c = 13.839(2) Å, Z = 4). The B6 octahedra are compressed in the direction of the B-I bonds, resulting in shortened diagonal B ··· B distances with average values of the groups I-B ··· B-I = 2.37 and I-B ··· B-H = 2.43 Å as compared with H-B ··· B-H = 2.49 Å.

Syntheses, Crystal Structures and an Overview of Alkali Metal Maleates

2009 ◽  
Vol 64 (5) ◽  
pp. 517-524 ◽  
Author(s):  
Michel Fleck ◽  
Ladislav Bohatý
Keyword(s):  
Hydrogen Bond ◽  
Crystal Structures ◽  
Maleic Acid ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
Hydrogen Atom Position ◽  
Potassium Hydrogen ◽  
Intramolecular Hydrogen ◽  
Atom Position

The crystal structures of four alkali salts of maleic acid have been determined by single crystal X-ray diffraction: crystals of rubidium hydrogen maleate, RbH(C4H2O4), are very nearly centrosymmetrical, i. e., only one hydrogen atom position in the crystal structure violates the centrosymmetry. Thus, the space group is Pbc21 rather than Pbcm. The compound is isotypic with potassium hydrogen maleate, KH(C4H2O4), which has previously been described in space group Pbcm. It has been reinvestigated to prove that the correct space group is also Pbc21. The isotypic pair of rubidium hydrogen maleate maleic acid, RbH(C4H2O4) H2(C4H2O4), and caesium hydrogen maleate maleic acid, CsH(C4H2O4)H2(C4H2O4), crystallise in the triclinic space group P1̄. The geometry of the maleate units in these compounds corresponds well to data of other metal maleates. The only significant variation, concerning the intra-anionic hydrogen bond, is discussed. Furthermore, an overview of previously reported metal maleate structures is given, with special regard to the symmetry of the intramolecular hydrogen bond.

Synthese und Kristallstruktur der (p-Brombenzyl)triphenylphosphonium-bromide: [(p-Br-C6H4-CH2)P(C6H5)3]+B-;[(p-Br-C6H4-CH2)P(C6H5)3]+Br2- und [(p-Br-C6H4-CH2)P(C6H5)3]+Br3-/ Synthesis and Crystal Structures of (p-Bromobenzyl)triphenylphosphonium Bromides, [(p-Br-C6H4-CH2)P(C6H5)3]+Br-;[(p-Br-C6H4-CH2)P(C6H5)3]+Br- and [(p-Br-C6H4-CH2)P(C6H5)3]+Br3-

1996 ◽  
Vol 51 (10) ◽  
pp. 1443-1448 ◽  
Author(s):  
H. Vogt ◽  
D. Wulff-Molder ◽  
M. Meisel
Keyword(s):  
Crystal Structures ◽  
Weak Interactions ◽  
Orthorhombic Space Group ◽  
Tetrahedral Geometry ◽  
Chlorine Atoms ◽  
Triclinic Space Group ◽  
Space Group ◽  
Triphenylphosphonium Bromide

(p-Bromobenzyl)triphenylphosphonium Bromide, [(p-Br-C6H4-CH2)P(C6H5)3]+Br- · (CH2Cl2)2.5 (1) has been prepared by the reaction of triphenylphosphine with p-bromobenzylbromide and its structure determined (triclinic, space group P1̅, Z = 2, a = 1198.03(12), b = 1245.80(11), c = 1258.42(12)pm, a = 100.170(8), β = 103.543(9), γ = 1 18.158(7)°. The compound exists as Br- anions and [(p-Br-C6H4- CH2)P(C2H5)3]+ cations, with weak interactions between the chlorine atoms of the CH2Cl2 molecules and the bromine bonded in the cation. [p-Br-C6H4-CH2)P(C6H5)3]Br2 (2) and [(p-Br-C6H4-CH2)P(C6H5)3]Br3·(CH2Cl2)1.5 (3) have been obtained by reactions of the corresponding amounts of bromine with 1 in methylenechloride solution. The yellow-red crystals of 2 are orthorhombic, space group Pccn, Z = 8, a = 2060.8(3), b = 1223.6(4), c = 1860.8(3) pm. Compound 2 exists as [p-Br-C6H4-CH2)P(C6HO5)3]+ cations and linear Br2-4 units with a bromide-bromine distance of 297.3(4) pm. The red crystals of (3) are triclinic, space group P1̅, Z = 2, a = 1 171.16(7), b = 1260.97(8), c = 1270.35(7)pm, α = 65.510(5), β = 75.811(5), γ = 62.320(5)°, and contain [(p-Br-C6H4-CH2)P(C6H5)3]+ cations and linear, slightly asymmetrical Br-3 anions. In all cases the cation has a slightly irregular tetrahedral geometry around the P atom.

Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalysen von trans-[PtX2(acac)2], X = CI, Br, I, SCN / Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of trans-[PtX2(acac)2], X = Cl, Br, I, SCN

1996 ◽  
Vol 51 (10) ◽  
pp. 1400-1406 ◽  
Author(s):  
D. Rickert ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Normal Modes ◽  
Force Constants ◽  
Monoclinic Space Group ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Valence Force ◽  
Space Group ◽  
X Ray ◽  
Modes Of Vibration

The crystal structures of trans-[PtCl2(acac)2](monoclinic, space group P21/c, a - 7.616(5), b = 12.759(5), c = 7.892(5) Å, β = 118.459(5)°, Z = 2), trans-[PtBr2(acac)2] (triclinic, space group P1̅, a = 7.502(5), b = 7.665(5), c = 8.155(5) Å, α = 114~508(5), β = 94.537(5), γ = 117.669(5)°. Z = 1) and trans-[Pt(SCN)2(acac)2] (triclinic, space group P1̅ , a = 7.9095(10), b = 7.9393( 10), c = 7.9631 Å, a = 114.051 (10), β = 100.955(10), γ = 100.573(10)°, Z = 1) have been determined by single crystal X-ray diffraction analysis. The crystal structure of trans- [Ptl2(acac)2] is known from the literature. To enhance the spectroscopic resolution, the IR and Raman spectra of the four complexes have been measured at low temperature (10 K). Using the X-ray data, normal coordinate analyses based on a modified valence force field have been performed and the normal modes of vibration for the octahedral skeleton [PtX2O4] have been assigned. With a set of 19 or 23 force constants taking into account the inner-ligand vibrations a good agreement between observed and calculated frequencies has been achieved. The valence force constants are e.g.fd (PtCl) = 2.16, fd (PtBr) = 1.45, fd (PtI) = 1.01, fd (PtS) = 1.80 mdyn/Å, and fd (PtO) ranges from 1.89 to 1.91 mdyn/Å.

Structural Studies of Complexes of Tridentate Terimine Systems. Crystal Structure of Bis(2,2′:6′,2′′-terpyridine)ruthenium(II) Perchlorate Hydrate, Bis(2,2′:6′,2′′-terpyridine)- osmium(II) Perchlorate Hemihydrate and Bis((1,10-phenanthrolin-2-yl)(pyridin-2-yl)amine)iron(II) Tetrafluoroborate Dihydrate

1998 ◽  
Vol 51 (12) ◽  
pp. 1131 ◽  
Author(s):  
Donald C. Craig ◽  
Marcia L. Scudder ◽  
Wendy-Anne McHale ◽  
Harold A. Goodwin
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Metal Ion ◽  
Chelate Ring ◽  
Monoclinic Space Group ◽  
Structural Studies ◽  
Triclinic Space Group ◽  
Space Group ◽  
Membered Chelate Ring ◽  
Group I

The crystal structures of bis(2,2′:6′,2″-terpyridine)ruthenium(II) perchlorate hydrate, bis(2,2′:6′,2″- terpyridine)osmium(II) perchlorate hemihydrate and bis((1,10-phenanthrolin-2-yl)(pyridin-2-yl)- amine)iron(II) tetrafluoroborate dihydrate are described. In the terpyridine complexes the ruthenium-nitrogen distances and the corresponding osmium-nitrogen distances are not significantly different. In both complexes the ligand geometry and the metal ion environment show the distortions usual for bis(terpyridine) systems. Distortions are less marked in the bis((1,10-phenanthrolin-2-yl)(pyridin-2-yl)amine)iron(II) cation in which each tridentate unit forms one five-membered and one six-membered chelate ring. [Ru(trpy)2] [ClO4]2.(H2O)1.1: tetragonal, space group I 41/a, a, b 12·527(2), c 40·202(11) Å, Z 8. [Os(trpy)2] [ClO4]2.(H2O)0·5: monoclinic, space group P 21/n, a 8·842(3), b 8·861(1), c 39·22(2) Å, β93·89(2)°, Z 4. [Fe(phpyam)2] [BF4]2.(H2O)2: triclinic, space group P -1, a 12·43(1), b 12·45(1), c 13·35(1) Å, α 62·70(10), β 78·55(8), γ 72·46(9)°, Z 2.

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