scholarly journals Studies of rhenium–carboxylate complexes. I. Tris(μ-i-butyrato)di(chlororhenium(III)) perrhenate

1969 ◽  
Vol 47 (22) ◽  
pp. 4213-4220 ◽  
Author(s):  
C. Calvo ◽  
N. C. Jayadevan ◽  
C. J. L. Lock
Keyword(s):  
Oxygen Atom ◽  
Single Crystal ◽  
Bond Length ◽  
Three Dimensional ◽  
Isobutyric Acid ◽  
The Other ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Groups ◽  
R Value

One of the compounds obtained by reacting rhenium(III) chloride with isobutyric acid while exposed to oxygen has been shown by single crystal X-ray diffraction to be tris(μ-i-butyrato)di(chlororhenium(III)) perrhenate. The crystals are monoclinic with lattice parameters a = 8.980(5) Å, b = 17.790(8) Å, c = 15.361(8) Å, and β = 114.4(1)°. The space group is P21/c and there are 4 formula units per cell. A total of 1729 independent reflections were examined and the structure was refined by full three dimensional least squares to an R value of 0.114. Two Re environments are found, one consisting of a dimer unit bridged by three carboxylate groups with a chlorine atom per rhenium and the other as a perrhenate group. This latter group, showing a mean Re—O distance of 1.74 Å, shares an oxygen atom with a Re in the dimer unit, and this Re—O bond length is 2.28 Å long. The structure consists of a packing of chains of alternate dimers and perrhenate groups running parallel to the c axis.

Crystal Structure of the Pyridinium Salt of the Polymeric Tris(thiocyanato)dicuprate(I) Anion

1979 ◽  
Vol 32 (12) ◽  
pp. 2757 ◽  
Author(s):  
CL Raston ◽  
B Walter ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Single Crystal ◽  
Title Compound ◽  
Three Dimensional ◽  
Pyridinium Salt ◽  
The Other ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network

The title compound, [C5H6N]+ [Cu2(SCN)3]-, has been prepared and its crystal structure determined by single-crystal X-ray diffraction at 295(1) K. Crystals are monoclinic, Cc, a 11.238(7), b 11.644(4), c 10.020(4)Ǻ, β 102.67(3)°, Z 4, the structure being refined to a residual of 0.037 for the 960 'observed' reflections. The structure comprises a three-dimensional network of copper(I) atoms linked by bridging thiocyanate groups, the pyridinium counterions occupying sites in the network cavities. Both copper atoms are four-coordinate, one having an environment of one nitrogen atom [Cu-N, 1.926(9)Ǻ] and three sulfur atoms [Cu-S, 2.319(3), 2.421(3), 2.448(3)Ǻ], while the other is coordinated by two atoms of each type [Cu-N, 1.935(9), 1.947(10); Cu-S, 2.430(3), 2.493(4) Ǻ].

Studies of rhenium–carboxylate complexes. III. The crystal and molecular structure of tetra-μ-n-butyratodirhenium(III) diperrhenate

1970 ◽  
Vol 48 (2) ◽  
pp. 219-224 ◽  
Author(s):  
C. Calvo ◽  
N. C. Jayadevan ◽  
C. J. L. Lock ◽  
R. Restivo
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
The Other ◽  
Formula Unit ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
X Ray ◽  
3 Dimensional ◽  
Carboxylate Groups ◽  
R Value

One of the compounds obtained by the reaction of rhenium(III) chloride with n-butyric acid while exposed to oxygen has been shown by single crystal X-ray diffraction to be tetra-μ-n-butyratodi-rhenium(III) diperrhenate. The crystals are triclinic with lattice parameters a = 7.836(8) Å, b = 10.746(8) Å, c = 8.773(8) Å, α = 88.9(1)°, β = 106.5(1)°, and γ = 98.0(1)°. The space group is [Formula: see text] and there is one formula unit per cell. A total of 1593 independent reflections were examined and the structure was refined by full 3-dimensional least-squares to an R value of 0.123. Two rhenium environments are found, one consisting of a dimer unit bridged by 4 carboxylate groups and the other a per-rhenate group. This latter group, showing a mean Re—O distance of 1.75 Å, shares an oxygen atom with a rhenium atom in the dimer unit, and this Re—O bond length is 2.18 Å long. The structure results from packing of short chains, consisting of the dimer unit and the 2 perrhenate groups, running roughly parallel to the [111] direction.

Crystal structure of the ferromagnetic polymer potassium Bis(carbonato)cuprate(II)

1980 ◽  
Vol 33 (2) ◽  
pp. 431 ◽  
Author(s):  
A Farrand ◽  
AK Gregson ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
Three Dimensional ◽  
The Other ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Square Planar

The crystal structure of the title compound, K2Cu(CO3)2, has been determined by single-crystal X-ray diffraction at 295(1) K, and refined by least squares to a residual of 0.027 for 1441 'observed' reflections. Crystals are orthorhombic, space group Fdd2, a 11.425(3), b 17.658(4), c 6.154(2) A, Z 8. The structure comprises potassium cations embedded in an infinite three-dimensional polymeric anionic array of square-planar coordinated copper atoms with bridging carbonate groups [Cu-O 1.934(2), 1.936(2) Ǻ]. Within the latter, the non- coordinating oxygen-carbon bond is shorter [1.259(3) Ǻ] than the other two [1.303(3), 1.307(2) Ǻ] and the O-C-O angle opposite it is correspondingly reduced to 117.1(2)°. The CO3 plane lies at 83.9° to the CuO4 'plane'.

scholarly journals An investigation of polyhedral deformation in two mixed-metal diarsenates: SrZnAs2O7and BaCuAs2O7

2015 ◽  
Vol 71 (4) ◽  
pp. 330-337 ◽  
Author(s):  
Sabina Kovač ◽  
Ljiljana Karanović ◽  
Tamara Đorđević
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
General Formula ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
X Ray ◽  
Open Framework ◽  
Geometrical Characteristics ◽  
Barium Copper

Two isostructural diarsenates, SrZnAs2O7(strontium zinc diarsenate), (I), and BaCuAs2O7[barium copper(II) diarsenate], (II), have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. The three-dimensional open-framework crystal structure consists of corner-sharingM2O5(M2 = Zn or Cu) square pyramids and diarsenate (As2O7) groups. Each As2O7group shares its five corners with five differentM2O5square pyramids. The resulting framework delimits two types of tunnels aligned parallel to the [010] and [100] directions where the large divalent nine-coordinatedM1 (M1 = Sr or Ba) cations are located. The geometrical characteristics of theM1O9,M2O5and As2O7groups of known isostructural diarsenates, adopting the general formulaM1IIM2IIAs2O7(M1II= Sr, Ba, Pb;M2II= Mg, Co, Cu, Zn) and crystallizing in the space groupP21/n, are presented and discussed.

Molecular tapes in the structure of isoguaninium chloride

2017 ◽  
Vol 74 (1) ◽  
pp. 108-112 ◽  
Author(s):  
Urszula Anna Budniak ◽  
Paulina Maria Dominiak
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Charge Density ◽  
Interaction Energy ◽  
Electrostatic Interaction ◽  
Electrostatic Interactions ◽  
The Other ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Structure

Isoguanine, an analogue of guanine, is of intrinsic interest as a noncanonical nucleobase. The crystal structure of isoguaninium chloride (systematic name: 6-amino-2-oxo-1H,7H-purin-3-ium chloride), C5H6N5O+·Cl−, has been determined by single-crystal X-ray diffraction. Structure analysis was supported by electrostatic interaction energy (E es) calculations based on charge density reconstructed with the UBDB databank. In the structure, two kinds of molecular tapes are observed, one parallel to (010) and the other parallel to (50\overline{4}). The tapes are formed by dimers of isoguaninium cations interacting with chloride anions. E es analysis indicates that cations in one kind of tape are oriented so as to minimize repulsive electrostatic interactions.

scholarly journals Intermetallic REPtZn Compounds with TiNiSi-type Structure

2011 ◽  
Vol 66 (7) ◽  
pp. 671-676 ◽  
Author(s):  
Trinath Mishra ◽  
Rainer Pöttgen
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Coordination Number ◽  
High Frequency ◽  
Three Dimensional ◽  
Type Structure ◽  
Rare Earth Compounds ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray

The equiatomic rare earth compounds REPtZn (RE = Y, Pr, Nd, Gd-Tm) were synthesized from the elements in sealed tantalum tubes by high-frequency melting at 1500 K followed by annealing at 1120 K and quenching. The samples were characterized by powder X-ray diffraction. The structures of four crystals were refined from single-crystal diffractometer data: TiNiSi type, Pnma, a = 707.1(1), b = 430.0(1), c = 812.4(1) pm, wR2 = 0.066, 602 F2, 21 variables for PrPt1.056Zn0.944; a = 695.2(1), b = 419.9(1), c = 804.8(1) pm, wR2 = 0.041, 522 F2, 21 variables for GdPt0.941Zn1.059; a = 688.2(1), b = 408.1(1), c = 812.5(1) pm, wR2 = 0.041, 497 F2, 22 variables for HoPt1.055Zn0.945; a = 686.9(1), b = 407.8(1), c = 810.4(1) pm, wR2 = 0.061, 779 F2, 20 variables for ErPtZn. The single-crystal data indicate small homogeneity ranges REPt1±xZn1±x. The platinum and zinc atoms build up three-dimensional [PtZn] networks (265 - 269 pm Pt-Zn in ErPtZn) in which the erbium atoms fill cages with coordination number 16 (6 Pt + 6 Zn + 4 Er). Bonding of the erbium atoms to the [PtZn] network proceeds via shorter RE-Pt distances, i. e. 288 - 293 pm in ErPtZn.

scholarly journals X-Ray Single Crystal Structural Analysis of Magnetically Oriented Microcrystals

2014 ◽  
Vol 70 (a1) ◽  
pp. C1138-C1138
Author(s):  
Chiaki Tsuboi ◽  
Kazuki Aburaya ◽  
Shingo Higuchi ◽  
Fumiko Kimura ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Three Dimensional ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Data Set ◽  
Uv Curable ◽  
X Ray

We have developed magnetically oriented microcrystal array (MOMA) technique that enables single crystal X-ray diffraction analyses from microcrystalline powder. In this method, microcrystals suspended in a UV-curable monomer matrix are there-dimensionally aligned by special rotating magnetic field, followed by consolidation of the matrix by photopolymerization. From thus achieved MOMAs, we have been succeeded in crystal structure analysis for some substances [1, 2]. Though MOMA method is an effective technique, it has some problems as follows: in a MOMA, the alignment is deteriorated during the consolidation process. In addition, the sample microcrystals cannot be recovered from a MOMA. To overcome these problems, we performed an in-situ X-ray diffraction measurement using a three-dimensional magnetically oriented microcrystal suspension (3D MOMS) of L-alanine. An experimental setting of the in-situ X-ray measurement of MOMS is schematically shown in the figure. L-alanine microcrystal suspension was poured into a glass capillary and placed on the rotating unit equipped with a pair of neodymium magnets. Rotating X-ray chopper with 10°-slits was placed between the collimator and the suspension. By using this chopper, it was possible to expose the X-ray only when the rotating MOMS makes a specific direction with respect to the impinging X-ray. This has the same effect as the omega oscillation in conventional single crystal measurement. A total of 22 XRD images of 10° increments from 0° to 220° were obtained. The data set was processed by using conventional software to obtain three-dimensional molecular structure of L-alanine. The structure is in good agreement with that reported for the single crystal. R1 and wR2 were 6.53 and 17.4 %, respectively. RMSD value between the determined molecular structure and the reported one was 0.0045 Å. From this result, we conclude that this method can be effective and practical to be used widely for crystal structure analyses.

Crystal Structure of Calcium Picrate Pentahydrate: A New Eight-Coordinate Stereochemistry for [M(bidentate)2(unidentate)4]

1979 ◽  
Vol 32 (2) ◽  
pp. 301 ◽  
Author(s):  
V Diakiw ◽  
TW Hambley ◽  
DL Kepert ◽  
CL Raston ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Single Crystal ◽  
Title Compound ◽  
Lattice Site ◽  
The Other ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Triangular Face ◽  
X Ray

The crystal structure of the title compound, Ca(C6H2N307)2,5H2O, has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.049 for 1513 'observed' reflections. Crystals are orthorhombic, Pmab, a 24.169(6), b l0.292(7), c 8.554(2) �, Z 4. The stereochemistry about the calcium has not been observed previously for the system [M(bidentate)2- (unidentate)4]; in the present structure, the calcium is coordinated by a pair of bidentate picrate ligands and the four water molecules in an array in which three of the water molecules occupy a triangular face of a square antiprism, the overall array having m symmetry. The remaining water molecule occupies a lattice site with no close interaction with the other species.

Die neuen Oxobismutate(III) Cs6Bi4O9, K9Bi5O13 und A2Bi4O7 (A = Rb, Cs) / The New Oxobismutates(III) Cs6Bi4O9, K9Bi5O13 and A2Bi4O7 (A = Rb, Cs)

2002 ◽  
Vol 57 (10) ◽  
pp. 1090-1100
Author(s):  
Franziska Emmerling ◽  
Caroline Röhr
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Alkali Metals ◽  
Mixed Valence ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Mixed Valence Compound

AbstractThe title compounds were synthesized at a temperature of 700 °C via oxidation of elemental Bi with the hyperoxides AO2 or via reaction of the elemental alkali metals A with Bi2O3. Their crystal structures have been determined by single crystal x-ray diffraction. They are dominated by two possible surroundings of Bi by O, the ψ-trigonal-bipyramidal three (B) and the ψ-tetrahedral four (T) coordination. Cs6Bi4O9 (triclinic, spacegroup P1̄, a = 813.82(12), b = 991.60(14), c = 1213.83(18) pm, α = 103.658(2), β = 93.694(3), γ = 91.662(3)°, Z = 2) contains centrosymmetric chain segmentes [Bi8O18]12- with six three- (T) and two four-coordinated (B) Bi(III) centers. K9Bi5O13 (monoclinic, spacegroup P21/c, a = 1510.98(14), b = 567.59(5), c = 2685.6(2) pm, β = 111.190(2)°, Z = 4) is a mixed valence compound with isolated [BivO4]3- tetrahedra and chains [BiIII4O9]6- of two T and two B coordinated Bi. In the compounds A2Bi4O7 (A = Rb/Cs: monoclinic, C2/c, a = 2037.0(3) / 2130.6(12), b = 1285.5(2) / 1301.9(7), c = 1566.6(2) / 1605.6(9) pm, β = 94.783(3) / 95.725(9)°, Z = 8) ribbons [Bi4O6O2/2]2- are formed, which are condensed to form a three-dimensional framework.

Synthesis, structure and selective luminescence sensing for iron(III) ions of a three-dimensional zinc(II) (4,6)-connected coordination network

2019 ◽  
Vol 75 (2) ◽  
pp. 141-149 ◽  
Author(s):  
Feng Su ◽  
Cheng-Yong Zhou ◽  
Lin-Tao Wu ◽  
Xi Wu ◽  
Chun Han ◽  
...  
Keyword(s):  
Three Dimensional ◽  
Electronic Configuration ◽  
Organic Ligands ◽  
Tetracarboxylic Acid ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Groups ◽  
Dimensional Network ◽  
Solvent Stability ◽  
Solvothermal Conditions

Coordination polymers constructed from conjugated organic ligands and metal ions with a d 10 electronic configuration exhibit intriguing properties for chemical sensing and photochemistry. A ZnII-based coordination polymer, namely poly[aqua(μ6-biphenyl-3,3′,5,5′-tetracarboxylato)(μ2-4,4′-bipyridine)dizinc(II)], [Zn2(C16H6O8)(C10H8N2)(H2O)2] n or [Zn2(m,m-bpta)(4,4′-bipy)(H2O)2] n , was synthesized from a mixture of biphenyl-3,3′,5,5′-tetracarboxylic acid [H4(m,m-bpta)], 4,4′-bipyridine (4,4′-bipy) and Zn(NO3)2·6H2O under solvothermal conditions. The title complex has been structurally characterized by IR spectroscopy, elemental analysis, single-crystal X-ray diffraction and powder X-ray diffraction analysis, and features a μ6-coordination mode. The ZnII ions adopt square-pyramidal geometries and are bridged by two syn–syn carboxylate groups to form [Zn2(COO)2] secondary buildding units (SBUs). The SBUs are crosslinked by (m,m-bpta)4− ligands to produce a two-dimensional grid-like layer that exhibits a stair-like structure along the a axis. Adjacent layers are linked by 4,4′-bipy ligands to form a three-dimensional network with a {44.610.8}{44.62} topology. In the solid state, the complex displays a strong photoluminescence and an excellent solvent stability. In addition, the luminescence sensing results indicate a highly selective and sensitive sensing for Fe3+ ions.

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