Crystal structures of 2-Hydroxyimino-1-phenylethan-1-one and ethyl 3-Oxo-2-sodiooxyiminobutanoate

1978 ◽  
Vol 31 (4) ◽  
pp. 745 ◽  
Author(s):  
CL Raston ◽  
RP Sharma ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Sodium Ion ◽  
Water Molecules ◽  
Sodium Ions ◽  
X Ray Diffraction ◽  
X Ray

The crystal structures of the title compounds, PhCOCH=NOH (5) and Na+[MeCOC(=NO-)CO2Et],-2H2O (10), have been determined by single-crystal X-ray diffraction at 295 K and refined by least squares to R 0.051, 0.062 (815, 1199 'observed' reflections) respectively. Crystals of (5) are monoclinic, P21/n, a 14.177(6), b 5.075(4), c 11.049(6) Ǻ, β 112.89(3)°, Z4. Crystals of (10) are tetragonal, 141/a, a 19.41(1), c 10.643(5)Ǻ Z 16. In (5), within the C=NOH group, C-N is 1.263(4) and N-O is 1.375(4)Ǻ; in (10) C-N is 1.318(6) and N-O is 1.321(5)Ǻ. In (10), the (presumably) negative C=NO- group does not coordinate the sodium ion; the latter is bridged by water molecules, occupying four close coordination positions [2.405(4)-2.552(4)Ǻ] in an interesting bridged polymeric array while the remaining two coordination positions are occupied by two ligand C=O groups [2.363(4), 2.393(4) Ǻ], the ligands also bridging sodium ions.

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 Structure of Disodium(I) cis-Bis(ethane-1,2-diamine)disulfitocobaltate(III) Perchlorate Trihydrate

1979 ◽  
Vol 32 (2) ◽  
pp. 291 ◽  
Author(s):  
CL Raston ◽  
AH White ◽  
JK Yandell
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
Sodium Ions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oxygen Atoms

The crystal structure of the title compound, Na2C104 [CO(C2N2H8)2(SO3)2],3H2O, has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.033 for 2693 'observed' reflections. Crystals are monoclinic, P21/c, a 16.271(3), b 12.298(2), c 9.567(2) �, β 105.85(1)�, Z 4. The Co-S distances differ significantly, probably a consequence of interaction of the sulfite oxygen atoms with adjacent sodium ions [Co-S, 2.206(1), 2.233(1) �]; the Co-N distances trans to the sulfite groups are significantly longer [2.015(3), 2.003(4) �] than those trans to each other [1.964(4), 1.959(3) �].

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)).

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].

Structural studies in the iron(III)/chloride/α,α'-diimine system. II. Ionic derivatives of stoichiometry FeCl3(phen,bpy)1,1.5

1983 ◽  
Vol 36 (10) ◽  
pp. 2043 ◽  
Author(s):  
BN Figgis ◽  
JM Patrick ◽  
PA Reynolds ◽  
BW Skelton ◽  
AH White ◽  
...  
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations ◽  
Derivatives Of

The crystal structures of the 1 : 1 adducts of FeCl3 with 2,2'-bipyridine (bpy) (1) and 1,10-phenanthroline (phen) (2), as recrystallized from nitromethane, have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by least squares to residuals of 0.038 and 0.032 for 1341 and 3968 'observed' reflections; the result for (2) is a redetermination. Crystals of (1) are orthorhombic, Pbnb, a 15.013(4), b 13.510(5), c 12.471(3) Ǻ, Z 4. Crystals of (2) are triclinic, P1, a 15.823(5), b 11.021(5), c 8.200(3) Ǻ, α 80.27(3), β 76.78(3), γ 89.64(3)°, Z 2. Both complexes haw the stoichiometry (FeCl3)1(bpy,phen)1, but are formulated as cis-[Fe(bpy,phen)2Cl2] [FeCl4]; in both compounds, the Fe-N distance is c. 2.20, (trans to Cl), 2.1, Ǻ(cis to Cl), while Fe-Cl, c. 2.2, Ǻ, is short. The structure determinations of Fe2Cl6(phen,bpy)3 as [Fe(phen)2Cl2]+ [Fe(phen)Cl4]- (3) and [Fe(bpy)2Cl2]+ [Fe(bpy)Cl4]- (4) are also reported. Compound (3) (from acetonitrile solution) is triclinic, P1, a 16.502(5), b 11.857(3), c 10.653(3) Ǻ, α 84.92(2), β 72.66(2), γ 74.80(2)°, Z 2, and was refined to a residual of 0.034 for 5540 'observed' reflections. The cation geometry is similar to that of (2); in the anion, the two Fe-CI bonds trans to each other are long [2.377(1) and 2.365(1) Ǻ] while those trans to the Fe-N bonds are short [2.287(1) and 2.318(1) Ǻ]. Fe-N distances are 2.216(3) and 2.220(3) A. Compound (4) (as its nitromethane solvate) is also triclinic, P1, a 14.480(7), b 12.645(5), c 10.678(4) Ǻ, α 95.68(3), β 109.21(3), γ 9258(3)°, Z 2; a residual of 0.042 was obtained for 4962 'observed' reflections. Cation and anion metal geometries are similar to those of (3).

Structural studies in the iron(III)/chloride/α,α'-diimine system. I. The six-coordinate mononuclear fac-[FeCl3(phen)X] system, X = MeOH, H2O, Cl-

1983 ◽  
Vol 36 (10) ◽  
pp. 2031 ◽  
Author(s):  
PC Healy ◽  
JM Patrick ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Iron Complexes ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Chlorine Atoms ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

The crystal structures of three iron complexes [FeCI3(phen)(MeOH)].MeOH (I), [FeCl3(phen)(H2O)] (2) and [phenH]+ [FeCl4(phen)]- (3) have been determined by single-crystal X-ray diffraction methods at 295(1) K, and refined by least squares to residuals of 0.044 (1600 'observed' reflections), 0.040 (806) and 0.050 (2496), respectively. Crystals of (1) are monoclinic, P21/c, a 8.005(9), b 14.805(11), c 14.830(12) A, P 101.03(7)°, Z 4; for (2), triclinic, space group P1 , a 10.591(8), b 10.227(7), c 6.613(3) Ǻ, α 108.21(5), β 100.69(5), γ 91.98(6)°2, 2 ; for (3), triclinic, P1, a 18.560(8), b 10.302(5), c 6.981(3) Ǻ, α 106.79(4), β 94.50(4), γ 103.15(4)°, Z 2. In all structures, the iron atoms are six-coordinate, with the disposition of the three chlorine atoms being fac in (1) and (2).

Crystal structures of rac- and meso-o-Phenylenebis(iodomethylarsine), the latter as its lattice complex with the methiodide of 1,3-Dimethyl-1,3-dihydro-2,1,3-benzoxadiarsole

1977 ◽  
Vol 30 (11) ◽  
pp. 2417 ◽  
Author(s):  
K Henrick ◽  
CL Raston ◽  
AH White ◽  
SB Wild
Keyword(s):  
Charge Transfer ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Iodine Species ◽  
Iodide Anion ◽  
The Mean

The crystal structures of the title compounds, o-C6H4(AsMeI)2 (1), and o- C6H4(AsMeI)2- [o-C6H4(AsMe)(As+Me2)O] I- (2), have been determined at 295 K by single-crystal X-ray diffraction and refined by least squares to residuals of 0.037 and 0.067 for 2095 and 2913 reflections respectively. Crystals of (1) are triclinic, Pī, a 9.865(5), b 9.837(7), c 7.765(4) Ǻ, α 98.89(5), β 96.71(4), γ 60.72(4)�, Z 2. <As- I> is 2.585 Ǻ and <As-C> 1.97 Ǻ. The angles about the arsenic differ only trivially, the mean being 98.4�. Crystals of (2) are monoclinic, P21/n, a 15.315(4), b 21.511(8), c 7.952(2) Ǻ, β 98.19(2)�, Z 4. In the cation As-O distances are unequal [1.75(1) (quaternary As), 1.86(2) Ǻ]; As-O-As is very small being 115.8(8)�. Charge-transfer interactions between iodine species are present in both derivatives; in (2), there is an interaction between the tertiary arsenics of the meso molecule and the iodide anion, As...I being 3.307(3), 3.551(3) Ǻ, with the geometry of the arsenics approaching that of a tetrahedral disposition. Within the cation, the geometry about the quaternary arsenic is typical of arsenic(v), the bond lengths being shorter than those about the ternary arsenic.

Crystal structure of μ-Oxo-bis-fac-[triaqua-1,10-phenanthrolineiron(III)] Tetrakis(nitrate) monohydrate

1984 ◽  
Vol 37 (7) ◽  
pp. 1405 ◽  
Author(s):  
PC Healy ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
High Spin ◽  
Iron Atom ◽  
Title Compound ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Spin Iron

The crystal structure of the title compound, [(OH2)3(phen)FeOFe(phen)(OH2)3](NO3)4.(H2O)(phen = 1,10-phenanthroline), has been determined by single-crystal X-ray diffraction methods at 295 K, being refined by least-squares methods to a residual of 0.059 for 3467 independent 'observed'reflections. Crystals are monoclinic, P 21/c, a 18.202(6), b 9.771(4), c 19.459(7) �, β 94.46(3)�, Z = 4. Two of the four anions are disordered. Within the cation, the geometry is typical of high-spin iron(III). O(bridge)-Fe are 1.765(4), 1.784(4) �, with Fe-O-Fe 162.0(3)�. The three water molecules in the coordination sphere of each iron atom are fac; those trans to the O-Fe bond have long Fe-(OH2) distances [2.154(5), 2.125(5) �] compared to those trans to the phenanthroline chelates [2.028(5)-2.037(5) �]. Fe-N range from 2.143(6) to 2.166(6) �.

Crystal structures of N,N,N',N'-Tetramethylthiuram monosulphide and Diiodo(N,N,N',N'-tetramethylthiuram monosulphide)mercury(II)

1977 ◽  
Vol 30 (8) ◽  
pp. 1693 ◽  
Author(s):  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Metal Atom ◽  
X Ray Diffraction ◽  
Sulphur Atom ◽  
Full Matrix ◽  
X Ray ◽  
The Common ◽  
Trigonal Prismatic

The crystal structures of the title compounds, Me2NC(S)SC(S)NMe2 (tmtm) and I2Hg(tmtm), have been determined by single-crystal X-ray diffraction at 295 K and refined by full-matrix least squares to residuals of 0.038 and 0.050 respectively for 1080 and 1532 ?observed? reflections. ��� The ligand tmtm is monoclinic, P21/a, a 14.096(4), b 7.457(3), c 10.178(3)Ǻ, β 110.55(3)�, Z4. The complex I2Hg(tmtm) is orthorhombic, P212121, a 12.910(3), b 12.441(3), c 9.863(2) Ǻ, Z4. ��� The structure of the ligand comprises a pair of planar Me2NCS2 fragments linked at the common central sulphur atom with a dihedral of 78.4�. As in the related tetraethylthiuram disulphide, the ?CS2- geometry is very asymmetric: <C=S> 1.657; <C-S> 1.793 Ǻ; <S-C-S> 119.3; <S-C-N> 115.2; <S=C-N> 125.4�; with C-S-C, 103.2(2)�. The metal-atom geometry in I2Hg(tmtm) is pseudo-trigonal prismatic, as in I2Hg(Me2NCS2- S2CNMe2), the prism apex being occupied by a ligand sulphur atom, but considerable changes are observed in the geometry about the metal as a consequence of the change in the ligand ?bite?.

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.

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