Synthesis, Crystal Structures and Polymorphism of New Cadmium and Zinc Thio- and Selenocyanato Coordination Compounds with 4-Acetylpyridine as N-Donor Ligand

2013 ◽  
Vol 68 (5-6) ◽  
pp. 643-652 ◽  
Author(s):  
Julia Werner ◽  
Inke Jess ◽  
Christian Näther
Keyword(s):  
Crystal Structures ◽  
Octahedral Geometry ◽  
Polymorphic Modification ◽  
Distorted Octahedral Geometry ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Donor Ligand ◽  
Space Group ◽  
Molar Ratios ◽  
Distorted Octahedral

Reactions of cadmium(II) thio- and selenocyanate with 4-acetylpyridine in different molar ratios and in different solvents always lead to the formation of compounds of composition Cd(NCS)2(4- acetylpyridine)2 (Cd1-I) and Cd(NCSe)2(4-acetylpyridine)2 (Cd2). Both compounds are isotypic and crystallize in the monoclinic space group C2/c. In their crystal structures the Cd cations are coordinated by two N-bonded 4-acetylpyridine ligands as well as two N- and two S/Se-bonded thio- or selenocyanato anions within a slightly distorted octahedral geometry. The Cd cations are linked into chains by pairwise μ-1,3-coordinating thio- or selenocyanato anions. In one reaction single crystals of a second polymorphic modification of composition Cd(NCS)2(4-acetylpyridine)2 (Cd1-II) were obtained by accident. This modification crystallizes monoclinically in space group P21/c, exhibits the same topology of the coordination network as in Cd1-I and Cd2 but a different arrangement of the chains in the crystal. Similar investigations with Zn(II) have revealed that only one compound of composition Zn(NCS)2(4-acetylpyridine)2 can be prepared that crystallizes in the triclinic space group P1. Its structure consists of discrete complexes in which the Zn(II) cations are tetrahedrally coordinated. A corresponding selenocyanato coordination compound could not be prepared

The Crystal Structures of [N,N’-Bis(3-methoxysalicylidene)-1,3- diaminopropane]nickel(II) and -copper(II)

2004 ◽  
Vol 59 (2) ◽  
pp. 228-232 ◽  
Author(s):  
Ayhan Elmali ◽  
Celal T Zeyrek ◽  
Yalcin Elerman
Keyword(s):  
Crystal Structures ◽  
Mirror Symmetry ◽  
Distorted Octahedral Geometry ◽  
Planar Geometry ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Bond Lengths ◽  
Distorted Octahedral

[N,N′’-Bis(3-methoxysalicylidene)-1,3-diaminopropane]nickel(II) dihydrate [Ni(C19H20N2O4)· 2(H2O)] 1 and [N,N′-bis(3-methoxysalicylidene)-1,4-diaminobutane]copper(II) [Cu(C20H22N2O4)] 2 have been synthesized and their crystal structures determined. Crystals of compound 1 are orthorhombic, space group Pnma, a = 7.509(3), b = 22.070(7), c = 11.532(4) Å, V = 1611.1(12) Å3, Z = 4 and Dc = 1.498 g·cm−3. The molecule 1 has mirror symmetry, but the ligand is not planar. The two parts of the Schiff base moieties are folded so as to form an angle of 21.6(1)°. The Ni atom is in a distorted octahedral geometry and coordinated by the donor atoms of the ligand in the horizontal plane and of two water molecules. Crystals of compound 2 are monoclinic, space group P21/c, a = 9.488(1), b = 21.918(3), c = 8.413(1) Å, β = 91.45(1)°, V = 1749.0(4) Å3, Z = 4 and Dc = 1.587 g·cm−3. The Cu atom is coordinated by an N2O2 donor set from the imine-phenol ligand in a distorted planar geometry, with the two phenolate O atoms deprotonated. The Cu-O bond lengths are 1.854(3) and 1.868(3)Å . The Cu-N bond lengths are 1.931(3) and 1.950(3) Å, the dihedral angle between the two 3-methoxysalicylidene groups is 43.4(1)°.

Structure cristalline et moléculaire du cis-dithiocyanatobis(phénanthroline-1,10)mercure(II), Hg(SCN)2(C12H8N2)2

1974 ◽  
Vol 52 (16) ◽  
pp. 2923-2927 ◽  
Author(s):  
André L. Beauchamp ◽  
Bernard Saperas ◽  
Roland Rivest
Keyword(s):  
Heavy Atom ◽  
Octahedral Geometry ◽  
Van Der Waals Interactions ◽  
Distorted Octahedral Geometry ◽  
Triclinic Space Group ◽  
Bond Lengths ◽  
R Factor ◽  
Distorted Octahedral ◽  
Phenanthroline Ligands ◽  
Heavy Atom Method

The compound cis-Hg(SCN)2(Phen)2 belongs to the triclinic space group [Formula: see text] with a = 13.252(5), b = 11.077(4), c = 8.443(3) Å, α = 105.20(3), β = 83.25 (3), γ = 90.92(3)°, and Z = 2. The structure was solved by the heavy atom method and refined on 1718 independent reflections to an R factor of 0.069. The crystal contains discrete molecules, in which mercury is coordinated to four nitrogen atoms from two phenanthroline molecules and to two sulfur atoms from thiocyanate groups. These donor atoms define a distorted octahedral geometry around mercury. The Hg—N bond lengths are in the range 2.42(2)–2.52(2) Å, whereas the Hg—S bonds are equal to 2.622(8) and 2.582(8) Å. The molecules are packed in layers parallel to the (110) planes and the layers are held together by normal van der Waals interactions. Within the layers, the packing of the complex is characterized by parallel stacking of phenanthroline ligands at distances of ∼3.4 Å. The terminal nitrogen atoms of the thiocyanate groups are uncoordinated.

Synthesis and Structure of cis-Dioxobis(pyrimidine-2-thiolato-N,S)molybdenum(VI)

1992 ◽  
Vol 45 (11) ◽  
pp. 1933 ◽  
Author(s):  
PR Traill ◽  
AG Wedd ◽  
ERT Tiekink
Keyword(s):  
Least Squares ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Distorted Octahedral ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The characterization of two MoVI complexes, cis -[MoO2(2-pymS)2] and cis -[MoO2(2-pyS)2] (where 2-pymSH is pyrimidine-2-thiol and 2-pySH is pyridine-2-thiol), and their reaction with Ph3P are reported. The X-ray structure of cis -[MoO2(2-pymS)2] shows the molybdenum atom to exist in a distorted octahedral geometry defined by two mutually cis oxygen atoms and two chelating 2-pymS ligands so that the two sulfur atoms occupy approximate trans positions. Crystals of cis -[MoO2(2-pymS)2] are monoclinic, space group P 21/n, with unit cell dimensions: a 9.301(3), b 12.121(2), c 11.303(3) �, β 112.62(3)�, V 1176.3 �3, Z 4. The structure was refined by a full-matrix least-squares procedure to R 0.067 for 1858 reflections with I ≥ 2.5 (I).

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.

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.

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.

The Preparation of a Mixed-Ligand Cobalt(III) Complex of DPPZ and Ethylenediamine: Crystal Structures of [Co(en)2(DPPZ)] (ClO4)3.0·5H2O, [Co(en)2(bpy)]Br(ClO4)2 and [Co(en)2(phen)] Br3

1999 ◽  
Vol 52 (8) ◽  
pp. 817 ◽  
Author(s):  
Alison M. Funston ◽  
Robert W. Gable ◽  
W. David McFadyen ◽  
Peter A. Tregloan
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Mixed Ligand ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Triclinic Space Group ◽  
Space Group ◽  
Octahedral Environment

The complex [Co(en)2(DPPZ)] (ClO4)3 (3) has been synthesized, and the crystal structures of this complex and those of [Co(en)2(bpy)] Br(ClO4)2 (1) and [Co(en)2(phen)] Br3 (2) have been determined. Crystal data for (1): M 614 . 13, monoclinic, space group C2/c (No. 15), a 16 . 7834(16), b 16 . 308(3), c 8 . 3167(15) Å, β 104 . 932(11)°, V 2199 . 4(6) Å, F(000) 1240, Z 4, Dc 1 . 855 g cm−3, µ 2 . 895 cm−1 , Mo Kα (graphite monochromatized) radiation, γ 0 . 71073 Å, T 293(1) K. Crystal data for (2): M 599 . 07, triclinic, space group P1 (No. 2), a 7 . 7113(11), b 10 . 633(2), c 12 . 9884(18) Å, α 85 . 745(15), b 78 . 258(11), γ 74 . 967(16)°, V 1006 . 7(3) Å, F(000) 588, Z 2, Dc 1 . 976 g cm−3, µ6 . 819 cm−1 , MoKα (graphite monochromatized) radiation, γ 0 . 71073 Å, T 293(1) K. Crystal data for (3): M 773 . 44, monoclinic, space group P 21/c (No. 14), a 20 . 296(2), b 9 . 6197(11), c 15 . 725(2) Å, β 92 . 850(10)°, V 3066 . 4(6) Å, F(000) 1579, Z 4, Dc 1 . 675 g cm−3 , µ 0 . 898 cm−1 , MoKα(graphite monochromatized) radiation, γ 0 . 71073 Å, T 293(1) K. In all three complexes the cobalt is in the usual octahedral environment, with the cations being linked by hydrogen bonds between the amine hydrogens and the anions into extended structures.

Darstellung, Schwingungsspektren und Normalkoordinatenanalyse von bindungsisomeren Halogenoselenocyanatorhenaten(IV) sowie Kristallstrukturen von mer-(Ph4P)2[ReCl3(NCSe)2cis (SeCN)] und mer-(n-Bu4N)2[ReCl3I(NCSe)2cis] / Synthesis, Vibrational Spectra and Normal Coordinate Analysis of Linkage Isomeric Halogenoselenocyanatorhenates(IV) and Crystal Structures of mer-(Ph4P)2[ReCl3(NCSe)2cis (SeCN)] and mer-(n-Bu4N)2[ReCl3I(NCSe)2cis]

1999 ◽  
Vol 54 (10) ◽  
pp. 1222-1228 ◽  
Author(s):  
S. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Exchange Chromatography ◽  
Normal Coordinate Analysis ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose

By treatment of fac-[ReCl3I3]2- with (SeCN)2 indichloromethane fac-[ReCl3(NCSe)3]2- (1), mer-[ReCl3(NCSe)2cis (SeCN)]2- (2) and mer-[ReCl3I(NCSe)2cis]2- (3) are formed which have been separated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of mer-(Ph-P)2[ReCl3(NCSe)2cis(SeCN)] (triclinic, space group Pl̅, a = 16.099(1), b = 16.729(3), c =21.026(2) Å, α = 70.194(10), ß = 73.958(10), γ = 83.929(10)°, Z = 4) and mer-(n-Bu4N)2[ReCl3|(NCSe)2cis] (monoclinic, space group P21/c, a = 11.838(1), b = 12.796(2), c = 30.767(2) Å, ß = 97.419(6)°, Z = 4) have been determined by single crystal X-ray diffraction analysis. Based on 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. The valence force constants are fd(ReN) = 1.79 (1), 1.71 (2), 1.71 (3) and fd(ReSe) = 1.15 (2) mdyn/Å.

scholarly journals Kristallstrukturen der Tetrachloroniccolate (PPh4)2[NiCl4] und [Na-15-Krone-5]2[NiCl4] / Crystal Structures of the Tetrachloroniccolates (PPh4)2[NiCl4] and [Na- 15-Crown-5]2[NiCl4]

1990 ◽  
Vol 45 (7) ◽  
pp. 995-999 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Ulrich Müller
Keyword(s):  
Crown Ether ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Sodium Ions ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Cl Atoms

The title compounds were obtained from NiS + PPh4Cl + HCl in dichloromethane, from NiCl2 and PPh4Cl and from NiCl2 + Na2S + 15-crown-5 in acetonitrile or CH2Cl2, respectively. Their crystal structures were determined by X-ray diffraction. (PPh4)2[NiCl4]: monoclinic, space group C 2/c, Z = 4, a = 1094.9(3), b = 1946.1(4), c = 2033.5(5) pm, β = 91.48(3)°; R = 0.07 for 2895 unique observed reflexions. [Na-15-crown-5]2[NiCl4]: triclinic, space group P1̄, Z = 2, a = 987.6(1), b = 998.0(1), c = 1779.9(2) pm, α = 104.17(1), β = 95.43(1), γ = 109.95(1)°; R = 0.090 for 4155 unique observed reflexions. In both cases, the [NiCl4]2- ions have distorted tetrahedral structures. With PPh4+ as the cation the distortion corresponds to a twisted tetrahedron which fulfils the point symmetry D2, the deviation from a flattened D2d-tetrahedron being small. In (PPh4)2[NiCl4] cations and anions alternate in layers parallel to (001). In [Na-15-crown-5]2[NiCl4] two of the Cl atoms of the anion are coordinated to sodium ions; one of the crown ether molecules shows positional disorder.

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