Crystal Structure of Two Different Hydrate Phases of Bis[2,4,6-tri(2-pyridyl)-1,3,5-triazine]cobalt(II) Diiodide

1990 ◽  
Vol 43 (7) ◽  
pp. 1269 ◽  
Author(s):  
BN Figgis ◽  
ES Kucharski ◽  
S Mitra ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Ground State ◽  
Room Temperature ◽  
Spin Component ◽  
Asymmetric Unit ◽  
Tridentate Ligands ◽  
X Ray ◽  
Structure Determinations ◽  
Electronic Ground

The title compound crystallizes at room temperature from aqueous solution as two distinct hydrated phases, both monoclinic and characterized by single-crystal X-ray structure determinations. The dihydrate ('blocks') is C2/c, a 42.58(2), b 9.099(8), c 21.14(1)Ǻ, β 112.12(4)°, Z= 8; R was 0.048 for 3784 'observed' reflections. The c. 3.75 hydrate ('Tetrahydrate'?) ('needles') is P21/c, a 9.348(2), b 36.663(8), c 23.071(8)Ǻ, β 93.51(2)°, Z 8; R was 0.050 for 6042 'observed' reflections. There are one and two independent cations in the asymmetric unit of each structure; all cations have the metal atom 'mer' coordinated by a pair of tridentate ligands. In the C2/c phase, Co-N (central) are 2.057(4) and 2.063(4)Ǻ with N-Co-N 175.8(2)°; Co-N (distal) are 2.163(6)-2.187(6)Ǻ. In the P21/c phase, in the first cation, Co-N are 2.045(8) and 2.050(7)Ǻ (central) [with N-Co-N, 167.0(3)°] and 2.193(8)-2.216(8)Ǻ (distal), while, in the second, Co-N (central) are 2.030(8) and 2.042(8)Ǻ with N-Co-N, 168.3(3)°; Co-N (distal) are 2.164(8)-2.227(8)Ǻ. These Co-N distances are longer than those observed in the [Co( tpy )2]2+ cations hitherto studied ( tpy = 2,2′:6′,2′-terpyridine), in which the electronic ground state has an appreciable low-spin component.

A 35-year-old mystery solved: a facile synthetic route and structural confirmation of tetrachlorobis(diethyl ether)tungsten(IV)

2021 ◽  
Vol 77 (4) ◽  
Author(s):  
Thomas E. Shaw ◽  
Alfred P. Sattelberger ◽  
Titel Jurca
Keyword(s):  
Crystal Structure ◽  
Diethyl Ether ◽  
Thermal Instability ◽  
Room Temperature ◽  
Surface Characteristics ◽  
Hirshfeld Surface ◽  
Asymmetric Unit ◽  
Synthetic Route ◽  
X Ray ◽  
Elemental Analyses

The true identity of the diethyl ether adduct of tungsten(IV) chloride, WCl4(Et2O) x , has been in doubt since 1985. Initially postulated as the bis-adduct, WCl4(Et2O)2, questions arose when elemental analyses were more in line with a mono-ether adduct, viz. WCl4(Et2O). It was proposed that this was due to the thermal instability of the bis-adduct. Here, we report the room-temperature X-ray crystal structure and Hirshfeld surface characteristics of trans-tetrachloridobis(diethyl ether)tungsten(IV), trans-WCl4(Et2O)2 or trans-[WCl4(C4H10O)2]. The compound crystallizes, with half of the molecule in the asymmetric unit, in the centrosymmetric space group P21/n. The W—O distance is 2.070 (2) Å, while the W—Cl distances are 2.3586 (10) and 2.3554 (10) Å.

Structural Systematics of Rare Earth Complexes. XXII. ('Maximally') Hydrated Rare Earth Iodides

2000 ◽  
Vol 53 (10) ◽  
pp. 867 ◽  
Author(s):  
Kevin C. Lim ◽  
Brian W. Skelton ◽  
Allan H. White
Keyword(s):  
Aqueous Solution ◽  
Rare Earth ◽  
Low Temperature ◽  
Single Crystal ◽  
Room Temperature ◽  
Second Phase ◽  
X Ray ◽  
Structure Determinations ◽  
Trivalent Rare Earth ◽  
Trigonal Prismatic

Low-temperature (c. 153 K) single-crystal X-ray structure determinations, carried out on trivalent rare earth iodides crystallized from aqueous solution at room temperature, have defined two series of hydrates, LnI3.nH2O. For Ln = La–Ho, a nonahydrate phase (n = 9) is defined, orthorhombic Pmmn, a ~ 11.5, b ~ 8.0, c ~ 8.8 Å, Z = 2, the second phase (n = 10), monoclinic P21/c, Z = 4 being defined for Ln = Er–Lu, a ~ 8.2, b ~ 12.8, c ~ 17.1 Å, β ~ 103.7˚. Neither of these phases is isomorphous with any of those pertinent to the previously studied chloride or bromide (hydrated) arrays, nor, unlike those, does the halide (iodide) in any case enter the coordination sphere of the lanthanoid. The n = 9 phase takes the form [Ln(OH2)9]I3, the nine-coordinate lanthanoid environment stereochemistry being tricapped trigonal-prismatic, while the n = 10 phase is [Ln(OH2)8]I3.2H2O, the eight-coordinate lanthanoid environment being square-antiprismatic.

scholarly journals Crystal structures of cristobalite-type and coesite-type PON redetermined on the basis of single-crystal X-ray diffraction data

2015 ◽  
Vol 71 (11) ◽  
pp. 1325-1327 ◽  
Author(s):  
Maxim Bykov ◽  
Elena Bykova ◽  
Vadim Dyadkin ◽  
Dominik Baumann ◽  
Wolfgang Schnick ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Crystal Structures ◽  
Rotation Axis ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations ◽  
Anisotropic Displacement Parameters

Hitherto, phosphorus oxonitride (PON) could not be obtained in the form of single crystals and only powder diffraction experiments were feasible for structure studies. In the present work we have synthesized two polymorphs of phosphorus oxonitride, cristobalite-type (cri-PON) and coesite-type (coe-PON), in the form of single crystals and reinvestigated their crystal structures by means of in house and synchrotron single-crystal X-ray diffraction. The crystal structures ofcri-PON andcoe-PON are built from PO2N2tetrahedral units, each with a statistical distribution of oxygen and nitrogen atoms. The crystal structure of thecoe-PON phase has the space groupC2/cwith seven atomic sites in the asymmetric unit [two P and three (N,O) sites on general positions, one (N,O) site on an inversion centre and one (N,O) site on a twofold rotation axis], while thecri-PON phase possesses tetragonalI-42dsymmetry with two independent atoms in the asymmetric unit [the P atom on a fourfold inversion axis and the (N,O) site on a twofold rotation axis]. In comparison with previous structure determinations from powder data, all atoms were refined with anisotropic displacement parameters, leading to higher precision in terms of bond lengths and angles.

Crystal structure of Bis(2,2':6',2''-terpyridyl)cobalt(II) iodide dihydrate at 295 K and at 120 K

1983 ◽  
Vol 36 (8) ◽  
pp. 1527 ◽  
Author(s):  
BN Figgis ◽  
ES Kucharski ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Ground State ◽  
Title Compound ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
A Site ◽  
Tetragonal Cell ◽  
Spin Ground State

The crystal structure of the title compound, [CO(C15H11N3)2] 12.2H2O, has been determined by single crystal X-ray diffraction methods at 295 K and at 120 K, being refined by least squares to residuals of 0.051 and 0.035 respectively for 982 and 1024 'observed' reflections at these temperatures. Both structures are based on a P42/n tetragonal cell, a c. 8.9, c c. 19.4 �, Z 2, in which only a quarter of the cation is independent, being located about a site of 4 symmetry. At room temperature (μoff c. 3.2 BM) Co-N (central, distal) are 1.942(7), 2.104(5) � diminishing to 1.912(5), 2.083(4) � at 120 K, with μoff c. 2.2 BM, corresponding to a fully populated low-spin ground state.

scholarly journals Synthesis and Structure of 2D Cobalt(II)-tartrate Hydrate Coordination Polymers Crystallised from Aqueous Solution

2018 ◽  
Vol 13 (2) ◽  
pp. 213 ◽  
Author(s):  
Mohammad Misbah Khunur ◽  
Yuniar Ponco Prananto
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Chemical Reaction ◽  
Coordination Polymers ◽  
Room Temperature ◽  
Reaction Engineering ◽  
X Ray ◽  
Hexadentate Ligand

Cobalt(II)-tartrate hydrate coordination polymer is successfully crystallisedfrom aqueous solution at room temperature. Unlike previous methods, diammonium tartrate was used and reacted directly with an aqueous solution of cobalt(II). Single crystal X-ray and ATR-IR analyses were performed toward the synthesized crystal. The crystal structure displaysa (6,3) 2D sheet which then grow into a 3D hydrogen-bonded network. Tetra- and hexa-dentate dianionic tartaric ligands are observed in the crystal structure, in which the hexadentate ligand connects four different cobalt centres. This method is considered feasible, affordable, and simple for the production of functional polymeric cobalt(II)-tartrate hydrate. Copyright © 2018 BCREC Group. All rights reservedReceived: 17th July 2017; Revised: 30th October 2017; Accepted: 30th October 2017; Available online:   11st June 2018; Published regularly: 1st August 2018How to Cite: Khunur, M.M., Prananto, Y.P. (2018). Synthesis and Structure of 2D Cobalt(II)-tartrate Hydrate Coordination Polymers Crystallised from Aqueous Solution. Bulletin of Chemical Reaction Engineering & Catalysis, 13 (2): 213-219 (doi:10.9767/bcrec.13.2.1342.213-219)

'Soft' Calixarenes–Structural Aspects of Calixarene Allyl Ethers and of Thiacalixarene Synthesis

1998 ◽  
Vol 51 (2) ◽  
pp. 111 ◽  
Author(s):  
Xavier Delaigue ◽  
Jack M. Harrowfield ◽  
M. Wais Hosseini ◽  
Mauro Mocerino ◽  
Brian W. Skelton ◽  
...  
Keyword(s):  
Room Temperature ◽  
Asymmetric Unit ◽  
X Ray ◽  
Allyl Ethers ◽  
Alternate Form ◽  
Phenolic Oxygen ◽  
Complexation Studies ◽  
Structure Determinations ◽  
Centrosymmetric Dimers ◽  
Structural Aspects

Syntheses and room-temperature single-crystal X-ray structure determinations are recorded for an array of p-t-butylcalix[n]arenes, n = 4 or 6, diversely functionalized at the phenolic oxygen atoms: the 1,3-diallyl 2,4-dimethyl ether for n = 4 (1), the hexaallyl ether for n = 6 (2), and the 1,3-dibenzyl 2,4-bis(dimethylthiocarbamoyl) derivative for n = 4 (3), with a view to establishing ligand baseline conformations for subsequent metal complexation studies, and for exploring any inclusion properties. Compound (1) is monoclinic, P21/c, a 16·751(9), b 20·772(7), c 27·91(1) Å, β 99·39(4)°, Z = 8, conventional R on |F| being 0·060 for No 4396 'observed' (I > 3σ(I )) reflections. Compound (2) is triclinic, P-1, a 19·63(2), b 14·57(2), c 14·188(9) Å, α 107·84(8), β 93·26(7), γ 99·48(10)°, Z = 2, R 0·067 for No 7315. Compound (3), as its methanol monosolvate, is triclinic, P-1, a 15·592(4), b 15·17(3), c 14·31(2) Å, α 88·8(1), β 64·3(1), γ 75·7(1)°, Z = 2, R 0·076 for No 3802. The conformation of (1) is similar to that previously established for an analogue in which two of the t-butyl groups were absent; the conformation of (2) is that of a flattened 1,2,3-alternate form, the asymmetric unit being a pair of half (centrosymmetric) dimers; the conformation of (3) is 1,3-alternate.

scholarly journals Crystal structure of bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II)

2015 ◽  
Vol 71 (5) ◽  
pp. 555-557 ◽  
Author(s):  
Marwa Mghandef ◽  
Habib Boughzala
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Hydrogen Bonds ◽  
Dihedral Angle ◽  
Room Temperature ◽  
Asymmetric Unit ◽  
Slow Evaporation ◽  
Acta Cryst

The title salt, (C5H6ClN2)2[CoCl4], was synthesized by slow evaporation of an aqueous solution at room temperature. The asymmetric unit consists of two essentially planar (C5H6ClN2)+cations [maximum deviations = 0.010 (3) and 0.014 (3) Å] that are nearly perpendicular to each other [dihedral angle = 84.12 (7)°]. They are bonded through N—H...Cl hydrogen bonds to distorted [CoCl4]2−tetrahedra, leading to the formation of undulating layers parallel to (100). The structure is isotypic with the Zn analogue [Kefiet. al(2011).Acta Cryst.E67, m355–m356.]

Synthese und Kristallstruktur neuer 1,1,1,3,3,3-Hexaamino-1λ5,3λ5- diphosphazenium-Salze/ Synthesis and Crystal Structure of Novel 1,1,1,3,3,3-Hexaamino-1λ5,3λ5- diphosphazenium Salts

1999 ◽  
Vol 54 (11) ◽  
pp. 1363-1370 ◽  
Author(s):  
Kai Landskron ◽  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Temperature Gradient ◽  
Single Crystals ◽  
Room Temperature ◽  
Gauche Conformation ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Acetonitrile Solutions ◽  
Ray Methods

1,1,1,3,3,3-Hexaamino-1λ5,3λ5-diphosphazenium bromide [(NH2)3PNP(NH2)3]Br, nitrate [(NH2)3PNP(NH2)3][NO3], and toluene-4-sulfonate [(NH2)3PNP(NH2)3][CH3C6H4SO3] have been prepared by anion exchange in aqueous solution. Single crystals were obtained from acetonitrile solutions in a temperature gradient between 60 °C and room temperature. The crystal structures were determined by single crystal X-ray methods at room temperature. ([(NH2)3PNP(NH2)3]Br: P1̄̄ , Z = 2, a = 596.2( 1 ),b = 744.5( 1), c = 1114.4( 1) pm, α = 108.78( 1), β = 104.18(1), γ = 90.64(1)°, R 1 = 0.048, wR2 = 0.104; [(NH2)3PNP(NH2)3][NO3]: P1̄̄, Z = 2, a = 550.9( 1), b = 796.3( 1), c = 1115.7( 1) pm, α = 94.45( 1), β= 99.55( 1), γ = 101,53( 1)°, R1 = 0.033, wR2 = 0.095; [(NH2)3PNP(NH2)3][CH3C6H4SO3]: P21/c, Z = 4, a = 804.1(1), b = 596.1(1), c = 3218.7(3) pm, β = 94.59(1)°, R1 = 0.052, wR2 = 0.136). In the solid the three salts consist of discrete [(NH2)3PNP(NH2)3]+ cations and their corresponding anions. The PN4 tetrahedra in [(NH2)3PNP(NH2)3]Br are staggered, while in [(NH2)3PNP(NH2)3][NO3] the eclipsed conformation is preferred. The PN4 tetrahedra of [(NH2)3PNP(NH2)3][CH3C6H4SO3] show gauche conformation.

scholarly journals A new hydrate of magnesium carbonate, MgCO3·6H2O

2020 ◽  
Vol 76 (3) ◽  
pp. 244-249
Author(s):  
Christine Rincke ◽  
Horst Schmidt ◽  
Wolfgang Voigt
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Diffraction Pattern ◽  
Raman Spectra ◽  
Room Temperature ◽  
Magnesium Carbonate ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Phase

During investigations of the formation of hydrated magnesium carbonates, a sample of the previously unknown magnesium carbonate hexahydrate (MgCO3·6H2O) was synthesized in an aqueous solution at 273.15 K. The crystal structure consists of edge-linked isolated pairs of Mg(CO3)(H2O)4 octahedra and noncoordinating water molecules, and exhibits similarities to NiCO3·5.5H2O (hellyerite). The recorded X-ray diffraction pattern and the Raman spectra confirmed the formation of a new phase and its transformation to magnesium carbonate trihydrate (MgCO3·3H2O) at room temperature.

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