Crystal structures of hexa(N-methylurea)cobalt(II) sulfate and thiosulfate

1980 ◽  
Vol 33 (2) ◽  
pp. 425 ◽  
Author(s):  
BN Figgis ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Complex Cation ◽  
X Ray Diffraction ◽  
Threefold Axis ◽  
X Ray

The crystal structures of the title compounds, [Co(C2H6N2O)6](SO4)(1) and[Co(C2H6N2O)6](S2O3) (2), have been determined at 295 K by X-ray diffraction using diffractometer data and refined by least squares to residuals of 0.042 (1), 0.043 (2) [875 and 926 reflections with I > (3σ(I)]. Crystals are trigonal, R 3c, a 1.4890(1) nm, α 43.34(1)° (1); a 1.4760(3) nm, α 44.53(1)° (2), Z 2. The compounds are isostructural; the complex cation has 3 symmetry, Co-O, 209.6(2) (1), 209.9(2) pm (2); the geometry of the ligand is well defined and precise, but the anions, located at sites of symmetry 32, are disordered. ��� The cobalt environment is distorted from Oh symmetry, being compressed along the threefold axis.

Crystal structures of (RS)-Di-μ-chloro-tetrakis(ethane-1,2-diamine)nickel(II) dichloride and diperchlorate

1978 ◽  
Vol 31 (2) ◽  
pp. 285 ◽  
Author(s):  
GA Bottomley ◽  
LG Glossop ◽  
CL Raston ◽  
AH White ◽  
AC Willis
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Complex Cation ◽  
Dimeric Complex ◽  
X Ray Diffraction ◽  
X Ray ◽  
Coordination Sites

The crystal structures of [(en)2NiCl2Ni(en)2] Cl2 (1) and [(en)2NiCl2Ni(en)2] (ClO4)2 (2) have been redetermined from single- crystal X-ray diffraction data at 295(1) K and refined by least squares to residuals of 0.073 and 0.052 respectively for 1345 and 1605 'observed' reflections respectively. Crystals of (1) are monoclinic, P21/n, a 14.053(4), b 11.309(3), c 6.326(1) Ǻ, β 94.22(2)�, Z 2. Crystals of (2) are monoclinic, P21/n, a 8.885(12), 6 19.707(20), c 7.120(8) Ǻ, β 108.99(4)�, Z 2. In both (1) and (2), a dimeric complex cation is observed, a pair of cis coordination sites about the nickel in each case being occupied by the bridging chlorines; the latter are asymmetric (Ni-Cl, 2.461(3), 2.551(3)(1); 2.461(3), 2.512(3) Ǻ (2)).

Lewis-Base Adducts of Group-11 Metal(I) Compounds. XXIX. Crystal Structures of Bis(Pyridine-4-carbonitrile)silver(I) Nitrate and Bis(4-benzoylpyridine)Silver(I) Nitrate Monohydrate

1987 ◽  
Vol 40 (9) ◽  
pp. 1603 ◽  
Author(s):  
S Gotsis ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Complex Cation ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Silver Atoms ◽  
Close Contacts

The crystal structures of the title compounds, [Ag(C6H4N2),] (NO3), (I), and [Ag(C12H9NO)2] (NO3).H2O, (2), have been determined by single-crystal X-ray diffraction methods at ~295 K, being refined by full-matrix least-squares methods to residuals of 0.042 and 0.044 for 1814 and 3434 independent 'observed' reflections respectively. Crystals of (1) and (2) are triclinic P1; for (1) a, 27.954(7), b 6.354(2), c 3.710(1)�, α 87.55(3), β 86.21(2), γ 89.35(2)�, Z 2; for (2), a 17.036(5), b 8.691(3), c 7.849(3) �, α � 107.74(2), β 97 53(2), γ 91 .11(2)�, Z 2. In both structures the formulation is basically a linearly coordinated complex cation/anion as shown above: in (I), Ag-N are 2.214(4), 2.203(4) � with N-Ag-N, 162.2(2)"; in (2), Ag-N are 2.146(3), 2.147(3) �, N-Ag-N, 175.3(1)�. The shortest Ag-O contact is found in (1) at 2.693(4)�. No close contacts are found between the silver atoms and cyano or ketonic ligand substituents.

The Crystal Structures at 10 K of the Trigonal Salts KMIII(NH3)6(ClO4)2Cl2, MIII = Os and Cr, and the Possibility of Phase Transitions

1999 ◽  
Vol 52 (3) ◽  
pp. 219 ◽  
Author(s):  
Philip A. Reynolds ◽  
Brian N. Figgis ◽  
Alexander N. Sobolev
Keyword(s):  
Differential Scanning Calorimetry ◽  
Transition Temperature ◽  
Crystal Structures ◽  
Low Temperatures ◽  
Simple Structure ◽  
Alkali Metal Cations ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Threefold Axis ◽  
X Ray

The crystal structures of KOs(NH3)3(ClO4)2Cl2 and KCr(NH3)6(ClO4)2Cl2 were determined at 10 K by X-ray diffraction, and for the osmium salt also at 293 K. At 293 K the osmium salt is trigonal, space group R 3m, with the same simple structure as others of this class of double salt. At 10 K, in agreement with previous radius ratio predictions, both crystals are best described as remaining R 3m. All previously studied members, with larger alkali metal cations, are twinned R 3 at low temperatures, with small, symmetry-breaking rotations of the hexaamminemetal(III) and perchlorate ions about the threefold axis. Differential scanning calorimetry on CsRu(NH3)6(ClO4)2Cl2 suggests that the R 3m to R 3 change is very extended in temperature with only a small discontinuity at the transition temperature.

A REFINEMENT OF THE CRYSTAL STRUCTURES OF (NH4)2TeBr6 AND Cs2TeBr6

1966 ◽  
Vol 44 (8) ◽  
pp. 939-943 ◽  
Author(s):  
A. K. Das ◽  
I. D. Brown
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Bromine Atom ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Anisotropic Temperature ◽  
Temperature Factors

(NH4)2TeBr6 and Cs2TeBr6 crystals have the cubic K2PtCl6 structure with space group: [Formula: see text] with a0 = 10.728 ± 0.003 Å and 10.918 ± 0.002 Å respectively. The positional coordinate of the bromine atom, and the anisotropic temperature factors of all atoms in the unit cell, have been refined for both crystals by a full matrix least-squares analysis of the three dimensional X-ray diffraction data (R = 0.08). The Te—Br distance, corrected for probable thermal motions of atoms forming the bond, is 2.70 ± 0.01 Å in both crystals.

The Flavonoids of Combretum quadrangulare: Crystal structures of the Polymorphic Forms of 5-Hydroxy-2-(4'-hydroxy-3',5'-dimethoxyphenyl)-3,7-dimethoxy-4H-1-benzopyran-4-one

1985 ◽  
Vol 38 (8) ◽  
pp. 1177 ◽  
Author(s):  
IR Castleden ◽  
SR Hall ◽  
S Nimgirawath ◽  
S Thadaniti ◽  
AH White
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Β Phase ◽  
Α Phase ◽  
Polymorphic Forms

The following substituted 2-phenyl-4H-1-benzopyran-4-ones have been isolated from the dried flowers of Combretum quadrangulare Kurz ( Combretaceae ): 5-hydroxy-3,3′,4′,5′,7-pentamethoxy ( combretol ) (1), 3′,5-dihydroxy-3,4′,7-trimethoxy ( ayanin ) (2) and 4′,5-dihydroxy- 3,3′,5′,7-tetramethoxy (3). The last substance (3) was obtained as a mixture of two polymorphic forms (α and β) each of which was characterized by X-ray diffraction. Diffractometer data at 295 K were refined by full matrix least squares to residuals of 0.043 (1181 'observed' reflections) for the α-phase and 0.044 (1421) for the β phase of (3). Crystals of the α-phase of (3) are triclinic, Pī, a 12.663(6), b 9.592(4), c 7.444(4) Ǻ, α 102.48(3), β 101.39(4), γ 91.72(4)°,Z 2. Crystals of the β-phase of (3) are monoclinic P21/n, a 17.139(8), b 12.728(6), c 7.845(7) Ǻ, β 95.07(6)°, Z 4. An unambiguous synthesis of (3) was also achieved.

scholarly journals Crystal structure of Tetraaqua(ethylenediamine)nickel(II) sulfate dihydrate and of Tetraaqua(2,2'-bipyridyl)nickel(II) sulfate dihydrate

1984 ◽  
Vol 37 (5) ◽  
pp. 921 ◽  
Author(s):  
PC Healy ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Oxygen Atoms

The crystal structures of the title compounds, [Ni(OH2)4(en)] [SO4].2H2O, (1), and [Ni(OH2)4(bpy)]- [SO4].2H2O, (2), have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by full matrix least-squares methods to residuals of 0.028,0.031 for 1852, 4323 independent 'observed' reflections respectively. Crystals of (1) are monoclinic, C2/c, a 9.459(4), b 12.192(7), c 12.294(3) �, β 119.84(4)�, Z 4. In the cation, Ni-N is 2.061(2) �; Ni-O (trans to O, N respectively) are 2.106(2), 2.063(2) �. Instead of being enlarged above 90� as predicted from repulsion theory, the angle between the pair of oxygen atoms trans to nitrogen is diminished, being 87 14(7)�. Crystals of (2) are triclinic, P1, a 11.476(5), b 9.351(5), c 7.793(4) �, α 77.63(4), β 83.52(3), γ87.40(4)�, Z 2. In the cation, Ni-N are both 2.063(2) �. Ni-O (trans to N, O respectively) are 2.060(2), 2.O42(2); 2.O80(2), 2�. The short Ni-O distance [2.042(2)�] is associated with the coordination of a trigonal water molecule.

Crystal structures of Bis[(ethane-1,2-diyl)bis(diphenylphosphine)]-palladium(II) and -platinum(II) dichloride dichloromethane and Dichloro[(ethane-1,2-diyl)bis(diphenylphosphine)]platinum(II) dichloromethane

1984 ◽  
Vol 37 (11) ◽  
pp. 2193 ◽  
Author(s):  
LM Engelhardt ◽  
JM Patrick ◽  
CL Raston ◽  
P Twiss ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Centrosymmetric Molecule ◽  
Platinum Analogue

The crystal structures of the title compounds have been established by single-crystal X-ray diffraction techniques at 295 K, being refined by least squares to residuals of 0.043, 0.036, 0.036 for 2057, 3176 and 3468 independent 'observed' reflections respectively. Crystals of [Pd(diphos)2] C12 (1) (diphos = Ph2P(CH2)2PPh2) are monoclinic, P21/c, with a 12.779(9), b 18.084(10), c 12.942(6) �, β 119.29(5)�, 22; for the isostructural platinum analogue (2), a 12.789(4), b 18.099(7), c 12.965(4) �, β 1l9.39(2)�. Crystals of [PtCl2(diphos)].CH2Cl2, (3), are orthorhombic, P212121, with a 21.360(6), b 13.499(4), c 9.551(5)� Z 4. Complexes (1) and (2) are also solvated but the nature of the solvation is complicated by disorder and less clearcut than in (3). In (1), Pd-P distances are 2.342(2), 2.347(2) � in a centrosymmetric molecule; in (2), Pt-P distances are 2.332(2), 2.335(2) �, while in (3), Pt-P distances are 2.230(2), 2.224(3) � and Pt-Cl are both 2.355(2) � [cf. 2.233(2), 2.226(2), (2.361(2), 2.357(2))� respectively for the previously studied palladium analogue].

The Crystal-Structures of (±)-(E)-2-(1-Amino-Ethylidene)-4,4,6-Trimethylcyclohexane-1,3-Dione [(±)-Aminoangustione] and (E)-2-(1-Aminoethylidene)-4,6,6-Trimethylcyclohex-4-Ene-1,3-Dione (Aminodehydroangustione)

1986 ◽  
Vol 39 (6) ◽  
pp. 923 ◽  
Author(s):  
JR Cannon ◽  
VA Patrick ◽  
AH White
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray

The crystal structures of (�)-(E)-2-(1-aminoethylidene)-4,4,6- trimethylcyclohexane-1,3-dione [(�)- aminoangustione ] (8) and (E)-2-(1- aminoethylidene )-4,6,6-trimethylcyclohex-4-ene-1,3-dione ( aminodehydroangustione ) (9) have been determined by X-ray diffraction. Diffractometer data at 295 K were refined by full-matrix least-squares to residuals of 0.057 (712 'observed' reflections) for (8) and 0.061 (571) for (9). Crystals of (8) are tetragonal I 41/a, a 21.68(1), c 9.426(6)Ǻ, Z 16; crystals of (9) are orthorhombic Pmab , a 7.077(2), b 11.421(6), c 13.283(4)Ǻ, Z 4.

Crystal structures of nitron and its non-stoichiometric hydrochloride

1980 ◽  
Vol 33 (10) ◽  
pp. 2237 ◽  
Author(s):  
JR Cannon ◽  
CL Raston ◽  
AH White
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Molecular Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Block Diagonal

The crystal structures of the hemi-ethanolate of nitron, C20H16N4(C2H6O)0.5, and of a non-stoichiometric hydrochloride of nitron, C20H16N4(HCl)1.7(H2O)3.3, have been determined by X-ray diffraction from diffractometer data at 295 K and refined by block diagonal least squares to residuals of 0.069 (2049 'observed' reflections) and 0.055 (1915), respectively. Crystals of the hemi-ethanolate of nitron are monoclinic P21/n, a 12.697(6), b 15.821(5), c 19.064(6) Ǻ, β 108.79(3)°, Z 8. Crystals of the non-stoichiometric hydrochloride of nitron are also monoclinic C2/c, a 25.41(1), b 5.968(6), c 29.40(2) Ǻ, β 103.53(5)°, Z 8. Despite some unusual features in their molecular geometry, these structures are consistent with the mesoionic character of nitron.

Crystal structures of trans-Dichloro- and Dibromo-bis(2,6-dimethylpyridine)copper(II)

1977 ◽  
Vol 30 (9) ◽  
pp. 1947 ◽  
Author(s):  
JA Campbell ◽  
CL Raston ◽  
JN Varghese ◽  
AH White
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Compound A ◽  
Full Matrix ◽  
X Ray ◽  
Square Planar

The crystal structures of the title compounds have been determined at 295(1) K by X-ray diffraction and refined by full-matrix least squares to residuals of 0.045 and 0.067 for 1224 and 1955 ?observed? reflections respectively. The compounds are isomorphous (triclinic, Pī, Z 1). Dichloro compound: a 8.068(2), b 8.024(2), c 7.646(2) Ǻ, α 93.84(2), β 113.44(2), γ 117.11(2)�. Dibromo compound: a 7.999(2), b 7.921(2), c 7.849(2) Ǻ, α 94.37(2), β 112.85(2), γ 115.99(2)�. The copper atoms are square-planar coordinated with two halide and two base ligands coordinated necessarily trans by virtue of the siting of the molecule on a centre of symmetry. Cu-X, Cu-N are 2.264(2), 2.011(3) (dichloro); 2.425(1), 1.997(4) Ǻ (dibromo). The plane of the lutidine is almost normal to the CuN2X2 plane.

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