Univalent Metal Complexes of (Perfluorophenoxy)acetic Acid. The Crystal Structures of (2,3,4,5,6-Pentafluorophenoxy)acetic Acid, Bis-μ-[(2,3,4,5,6-pentafluorophenoxy)acetato-O,O']-bissilver(I) and catena-Bis-μ-[(2,3,4,5,6-Pentafluorophenoxy)acetato-O]-bismercury(I)

1988 ◽  
Vol 41 (5) ◽  
pp. 683 ◽  
Author(s):  
TCW Mak ◽  
WH Yip ◽  
CHL Kennard ◽  
G Smith ◽  
EJ Oreilly
Keyword(s):  
Acetic Acid ◽  
Metal Complexes ◽  
Crystal Structures ◽  
Side Chain ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
A Cell ◽  
Oxyacetic Acid

The crystal structures of perfluorophenoxyacetic acid [(2,3,4,5,6- pentafluorophenoxy )acetic acid] and its anhydrous complexes with silver(I) and mercury(I) have been determined by X-ray diffraction and refined to residuals R = 0.046, 0.042 and 0.104 for 1235, 1789 and 2750 observed reflections respectively. The acid forms the usual hydrogen- bonded cyclic dimers [O---O, 2.705(3)Ǻ] with the oxyacetic acid side- chain synclinally oriented. Crystals age triclinic, space group Pī with Z 2 in a cell of dimensions a 7.479(1), b 7.592(2), c 8.463(2)Ǻ,α 80.15(2),β 85.34(2),γ 61.31(1)Ǻ. The silver complex, [Ag2L2],(1), has crystals with a 5.992(3), b 30.22(2), c 5.277(2)Ǻ, β 106.42(5)°, space group P21/a and Z 2. The bis-carboxylato (O,O′) dimers have Ag-Ag 2.943(1)Ǻ with Ag-O, 2.203, 2.230(3)Ǻ and O-Ag-O 161.6(2)°. The complex with mercury(I), [Hg2L2]n, (2), is centrosymmetric with the usual linear O-Hg-Hg-O-bonds [Hg-Hg, 2.514(1)Ǻ; Hg-O, 2.13(1)Ǻ; O-Hg-Hg, 173.9(2)°]. Longer peripheral bonds to Hg [Hg-O, 2.63(1)Ǻ] produce a polymeric structure. Crystals of (2) are triclinic, space group Pī with Z 1 in a cell of dimensions a 5.038(1), b 5.970(1), c 15.774(6)Ǻ, α 80.77(2),β 86.42(2),γ 84.38(2)°.

Divalent Metal-Complexes of 2-Fluorophenoxyacetic Acid - the Crystal-Structures of 2-Fluorophenoxyacetic Acid, Tetraaquabis(2-Fluorophenoxyacetato)Zinc(II) Dihydrate and Aquabis(2-Fluorophenoxyacetato)Bis(Pyridine)Copper(II)

1986 ◽  
Vol 39 (11) ◽  
pp. 1823 ◽  
Author(s):  
CHL Kennard ◽  
EJ Oreilly ◽  
S Schiller ◽  
G Smith ◽  
AH White
Keyword(s):  
Metal Complexes ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pyramidal Geometry ◽  
A Cell ◽  
Divalent Metal Complexes

The crystal structures of 2-fluorophenoxyacetic acid ( oflpaH ) and the metal complexes aquabis (2-fluorophenoxyacetato) bis (pyridine)copper(II) (1) and tetraaquabis (2-fluorophenoxyacetato)zinc(II) dihydrate (2) have been determined by X-ray diffraction and refined to residuals R 0.036, 0.041, 0.025 for 641, 863 and 1505 observed reflections respectively. The acid crystallizes in a monoclinic cell, space group P21/c with a 6.207(2), b 19.363(8), c 6.999(2) Ǻ, β 114.81(2)� and Z 4. The molecules form planar, centrosymmetric , hydrogen-bonded cyclic dimers [O...O, 2.618(4)Ǻ]. Complex (1) is orthorhombic, space group P2cb with two molecules in a cell of dimensions a 5.621 (2), b 17.218(7), c 13.288(6)Ǻ while (2) is monoclinic, space group P21/c, a 6.597(2), b 5.279(2), c 30.079(10) Ǻ, β 94.65(3)�; with Z 2. Complex (1) has square-pyramidal geometry with the basal plane containing two trans related carboxyl oxygens [Cu-O, 1.944(4)Ǻ] and two trans related pyridine nitrogens [Cu-N, 2.030(5)Ǻ]. A water molecule occupies the apex of the square pyramid [Cu-OW, 2.199(8)Ǻ]. Complex (2) has octahedral geometry with the MO6 octahedron containing two trans related carboxyl oxygens [Zn-O, 2.122(2)Ǻ] and four water oxygens [Zn-OW, 2.069(2), 2.085(2)Ǻ]. Preliminary X-ray data also confirm that the magnesium(II) and manganese(II) complexes of 2-fluorophenoxyacetic acid are isomorphous with (2) but different from the cobalt(II) derivative.

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.

Divalent Metal Complexes of 2-Formylphenoxyacetic Acid: The Crystal Structures of 2-Formylphenoxyacetic Acid, and the Isomorphous Cobalt(II) and Zinc(II) 2-Formylphenoxyacetates

1985 ◽  
Vol 38 (9) ◽  
pp. 1381 ◽  
Author(s):  
CHL Kennard ◽  
EJ O'Reilly ◽  
G Smith ◽  
TCW Mak
Keyword(s):  
Metal Complexes ◽  
Crystal Structures ◽  
Divalent Metal ◽  
Carboxyl Groups ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Planar Molecules ◽  
Divalent Metal Complexes ◽  
Monoclinic Cell

The crystal structures of 2-formylphenoxyacetic acid ( ofpaH ), tetraaquabis (2-formylphenoxyacetato)-cobalt(II) (1) and tetraaquabis (2- formylphenoxyacetato )zinc(II) (2) have been determined by X-ray diffraction and refined to residuals R 0.039, 0.058 and 0.045 for 1197, 1178 and 1230 observed reflections respectively. 2-Formylphenoxyacetic acid crystallizes in a monoclinic cell, space group P21/n with a 8.066(2), b 7.375(1), c 14.206(2) Ǻ, β 98.12(1)° and Z 4. The planar molecules form unusual hydrogen-bonded chain polymers (O…O 2.694(3)Ǻ] linked through the carboxyl groups. The complexes (1) and (2) are isomorphous, the comparative cells being a 5.036(1), b 13.463(3), c 15.083(4) Ǻ, β 96.88(2)° for (1), and a 5.044(1), b 13.481(3), c 15.055(4) Ǻ, β 96.95(2)° for (2), with Z 2 and space group P21. The complexes have four waters and two trans-related carboxyl oxygens [mean M-O distances 2.129(5) and 2.117(3) Ǻ respectively] completing almost regular octahedral stereochemistries . The nickel(II) complex [Ni( ofpa )(H2O)4] is probably not isostructural with (1) and (2), and the copper(II) complex is also different, with formula [Cu( ofpa )2(H2O)2].

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.

Kristallstrukturen, Schwingungsspektren und Normalkoordinaten- analysen von trans-[OsO2(ox)2]2– und trans-[OsO2(mal)2]2–/ Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of trans-[OsO2(ox)2]2– and trans -[OsO2(mal)2]2–

1998 ◽  
Vol 53 (8) ◽  
pp. 823-828 ◽  
Author(s):  
A. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Vibrational Spectra ◽  
Room Temperature ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Ir And Raman

Abstract The crystal structures of trans-(Ph4P)2[OsO2(ox)2] (monoclinic, space group P21/n, a = 12.281(2), b = 14.5440(13), c = 13.9810(12) Å, β = 100.000(8)°, Z = 2) and trans- (n-Bu4N)2[OsO2(mal)2] (triclinic, space group P1̄, a = 10.365(4),b = 10.707(3), c - 11.473(5) A, a = 73.00(2), β = 64.44(3), 7 = 82.55(3)°, Z = 1) have been determined by single crystal X-ray diffraction analysis. The IR and Raman spectra of these complexes were measured at room temperature. Based on the molecular parameters of the X-ray determinations normal coordinate analyses have been performed and the vibrations assigned. The valence force constants of [OsO2(ox)2]2- are fd(Os=O) = 6.7, fd(Os-O) = 2.9, fd(C-O) = 5.05, fd(C=O) = 11.2 and fd(C-C) = 4.7 mdyn/Å and of [OsO2(mal)2]2- fd(Os=O) = 6.7, fd(Os-O) = 2.9, fd(C-O) = 4.86, fd(C=O) =11.1 and fd(C-C) = 4.07 mdyn/Å.

Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalyse von cis-(n-Bu4N)2[ReBr4(NCS)2 ], cis-(n-Bu4N)2[ReBr4(NCSe)2] und cis-(n-Bu4N)2[ReBr4(NCS)(NCSe)] / Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of cis-(n-Bu4N)2[ReBr4(NCS)2], cis-(n-Bu4N)2[ReBr4(NCSe)2,] and cis -(n -Bu4N)2[ReBr4(NCS)(NCSe)]

2000 ◽  
Vol 55 (2) ◽  
pp. 178-184 ◽  
Author(s):  
L. Homolya ◽  
W. Preetz
Keyword(s):  
Low Temperature ◽  
Diffraction Analysis ◽  
Crystal Structures ◽  
Vibrational Spectra ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Ir And Raman

The crystal structures of cis-(n-Bu4N)2[ReBr4(NCS)2] (1) (triclinic, space group P1̄, a = 11.475(6), b = 20.096(16), c = 22.144(11) Å, α = 110.56(6), β = 92.97(5), γ = 99.77(7)°, Z = 4), cis-(n-Bu4N)2[ReBr4(NCS)2] (2) (triclinic, space group P1̄, a = 11.527(3), b = 20.237(7), c = 22.07(2) Å, α = 110.05(4), β = 93.86(6), γ = 99.49(4)°, Z = 4) and cis-{n- Bu4N)2[ReBr4(NCS)(NCSe)] (3) (triclinic, space group P1̄, a = 11.488(2), b = 20.164(6), c = 22.158(5) Å, α = 110.44(2), β = 93.34(2), γ = 99.626(18)°. Z = 4) have been determined by single crystal X-ray diffraction analysis. Based on these molecular parameters 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) = 1.70 (1), 1.70 (2) and 1.72 (3), fd(ReBr) = 1.36 (1), 1.30 (2) and 1.36 mdyn/Å (3).

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.

Metallkomplexe mit biologisch wichtigen Liganden, CIV [1]. ortho-Palladierte Komplexe von N,N-Dimethyl-C-phenyl-glycinmethylester. Synthese von α-Aminosäure-Derivaten durch Insertion von Isocyaniden, CO, Alkenen und Alkinen in die Pd-C-Bindung / Metal Complexes of Biologically Important Ligands, CIV [ 1]. ortho-Palladated Complexes of N,N-Dimethyl-C-phenylglycine-methylester. Synthesis of α-Amino Acid Derivatives by Insertion of Isocyanides, CO, Alkenes, and Alkynes into the Pd-C Bond

1998 ◽  
Vol 53 (4) ◽  
pp. 448-458 ◽  
Author(s):  
Andreas Böhm ◽  
Kurt Polborn ◽  
Karlheinz Sünkel ◽  
Wolfgang Beck
Keyword(s):  
Acetic Acid ◽  
Amino Acid ◽  
Metal Complexes ◽  
Crystal Structures ◽  
Trinuclear Complex ◽  
Amino Acid Derivatives ◽  
X Ray Diffraction ◽  
X Ray ◽  
Derivatives Of ◽  
Amine Ligand

Abstract N,N-Dimethyl-C-phenylglycinemethylester reacts with Pd(OAc)2 in acetic acid to give the orthopalladated, acetato bridged complex 1. Treatment of 1 with sodium halide affords the chloro, bromo, and iodo bridged compounds [Me2NC(H)(CO2Me)C6H4PdX]2 (2a -c) (X = halide). From 2a and 1,1′-bis(diphenylphosphino)ferrocene the phosphine bridged trinuclear complex 3 is obtained. Substitution of the amine ligand of 2a by the phosphino group is observed for the reaction of 2a with Ph2PC(Me)C(Me)PPh2. Insertion of 2,6-dimethyl-phenylisocyanide, CO, alkyl-vinyl-ketones, and diphenylacetylene into the Pd-C bond o f 2a -c provides the orthosubstituted organic and organometallic derivatives of phenylglycine 6a -c, 7, 8a -b and 9a -c. The crystal structures of 1, 4a, 6a, 7 and 9a were determined by X-ray diffraction.

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.

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