Crystal and molecular structure of Bis(4-amino-3,5,6-trichloropicolinato)-manganese(II) dihydrate

1981 ◽  
Vol 34 (4) ◽  
pp. 891 ◽  
Author(s):  
G Smith ◽  
EJ O'Reilly ◽  
CHL Kennard
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Direct Methods ◽  
Polymer Chains ◽  
Monoclinic Space Group ◽  
Carboxylate Oxygen ◽  
Group 12 ◽  
Distorted Octahedral ◽  
A Cell

The manganese(II) complex [Mn(picl)2,2H2O]n of the herbicide picloram has been prepared and the crystal and molecular structure determined from three-dimensional X-ray data collected by counter methods. The crystals of the complex are monoclinic, space group 12/a with two complex units in a cell of dimensions a 23·052(5), b 13·840(2), c 6·441(1) �, β 98·20(1)�. The structure was solved by direct methods and refined by full matrix least squares to unweighted and weighted Rfactors of 0·035 and 0·038 respectively for 887 'observed' reflections. The polymer is best described as having a centrosymmetric two-molecule unit [Mn-O, 2·162(3), 2·246(3) �] with two oxo bridges between manganese centres through two single carboxylate oxygens of the four substituted picolinate ligands. The two molecules are related by a twofold axis. The units form infinite one-dimensional polymer chains in the c direction through oxo bridges involving one oxygen from the other two picolinate ligands [Mn-Mn 3·636(1)�]. The bis(bidentate)picolinate bites are completed by the pyridlne nitrogens [Mn-N, 2·313(4) �] giving a very distorted octahedral MnO4N2 coordination sphere about each manganese [N-Mn-N', 97.0(3)�; O-Mn-O range, 68·9-168.2(3)�; O-Mn-Nrange, 69·9-138·5(3)�]. The lattice waters are involved in hydrogen-bonding interactions which link the polymer in the a crystallographic direction with the uncoordinated carboxylate oxygen ( O···O,2·824, 2·936 �) and the 4-amino groups from the adjacent picolinate ligand (N· ··0, 2·852, 3·030�).

Crystal and Molecular Structure of the Copper(I)-thiolate-selenide Complex [Ph4P][Cu(SeS2CNC4H8)(S2CN2C4H8)] with an Unusual Se-S Bond

1999 ◽  
Vol 54 (10) ◽  
pp. 1313-1317 ◽  
Author(s):  
Qianfeng Zhang ◽  
Jinxi Chen ◽  
Maochun Hong ◽  
Xinquan Xin ◽  
Hoong-Kun Fun
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Space Group ◽  
A Cell

Reaction of a DMF solution of Cu(S2CNC4H8) with [Ph4P]2[WSe4] affords [Ph4P]2[WSe4- (CuS2CNC4H8)3] (1) and [Ph4P][Cu(SeS2CNC4H )(S2CN2C4H8)] (2) in which a Se atom from the decomposition of the WSe42- anion has reacted with the pyrrolidyldithiocarbamate (C4H8dtc) ligand anion to form the new ligand anion SeS2CNC4H8⊖. Complex 2 crystallizes with four formula units in the monoclinic space group P21/c in a cell of dimensions a = 10.5824(2), b = 18.7575(3), c = 18.3268(4) Å and ß = 109.0980(10)°. 6055 independent reflections above background were measured with a diffractometer and the structure was refined anisotropically to R =0.073. The anion contains a three-coordinated copper(I) atom. The C4H8dtc⊖ ligand is bonded to the Cu+ cation in a terminal fashion, while SeS2CNC4H8⊖ chelates the Cu+ cation. The Se-S bond length is 2.231 (4) Å.

The Crystal Structure of KIO3.HIO3

1971 ◽  
Vol 49 (3) ◽  
pp. 468-476 ◽  
Author(s):  
Lilian Y. Y. Chan ◽  
F. W. B. Einstein
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray ◽  
R Factor ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Potassium Hydrogen ◽  
A Cell ◽  
Least Squares Techniques

The crystal structure of potassium hydrogen di-iodate (bi-iodate) KIO3.HIO3 was determined from three dimensional X-ray data collected by counter methods. The structure was refined by full-matrix least-squares techniques to a conventional R factor of 5.0 % for the 1392 observed reflexions. The salt crystallizes in the monoclinic space group P21/c with eight formula units in a cell of dimension a = 7.028(1) Å, b = 8.203(1) Å, c = 21.841(3) Å, β = 98.03(1)°.The iodate units are all basically pyramidal; weak interionic I—O contacts complete a very distorted octahedral environment around three iodine atoms. There is a capped octahedral (7-coordinate) environment around the remaining iodine atom. The I—O bonds are in the range 1.75–1.82 Å and the I—OH bonds are 1.91 and 1.95 Å, variations in length can be correlated with differences in the degree of involvement in (a) hydrogen bonding and (b) interaction with adjacent iodine atoms.

The crystal and molecular structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, a phosphorus–silicon heterocycle

1979 ◽  
Vol 57 (2) ◽  
pp. 174-179 ◽  
Author(s):  
A. Wallace Cordes ◽  
Paul F. Schubert ◽  
Richard T. Oakley
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Single Bond ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths

The crystal structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, (PhPSi2Me4)2, has been determined by single crystal X-ray diffraction. The crystals are monoclinic, space group P21/c, with a = 9.866(1), b = 11.921(1), and c = 11.324(2) Å, β = 104.31(1)°, Z = 2, and ρcalcd = 1.15 g/cm3. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.060 and Rw of 0.078, for 1173 reflections with intensities greater than 3σ. The (PhPSi2Me4)2 molecule lies on a crystallographic centre of symmetry, and the six-membered P2Si4 ring has a chair conformation with equatorial phenyl groups. The endocyclic angles at P (104.4(1)°) and Si (104.9(2)°) are intermediate between those found in cyclic hexaphosphine and hexasilane molecules, and the Si—Si and P—Si distances of 2.345(3) and 2.252(4) Å, respectively, correspond to single bond lengths, with no appreciable evidence for secondary pπ → dπ bonding between phosphorus and silicon. The Si—C (1.867(8) Å) and P—C (1.828(7) Å) bond lengths are also normal. The variations in the Si—P—C (101.6(2)°, 108.6(2)°), P—Si—C (range 106.2(3)–120.0(3)°), and Si—Si—C (range 105.8(3)–113.7(3)°) angles indicate that the positions of the exocyclic methyl and phenyl groups are influenced by both intra- and intermolecular steric forces.

scholarly journals Synthesis and Molecular Structure of cis-Tetracarbonyl[N-(diphenylphosphino-kP)-naphthalen-1-yl-P,P-diphenylphosphinous amide-kP]chromium(0)

2014 ◽  
Vol 2014 ◽  
pp. 1-4
Author(s):  
Harbi Tomah Al-Masri
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Direct Methods ◽  
Molar Ratio ◽  
Planar Geometry ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
Space Group ◽  
Distorted Octahedral ◽  
Least Squares Techniques

The reaction of N,N-bis(diphenylphosphanyl)naphthylamine C10H7-1-N(PPh2)2 with (C5H10NH)2Cr(CO)4 (1 : 1 molar ratio) in dichloromethane afforded cis-[Cr(CO)4{C10H7-1-N(PPh2)2}] (1). This complex was crystallized in the monoclinic space group P21/n. The structure was solved by direct methods and refined by full-matrix least squares techniques to an R factor of 0.0313 for 6488 observed reflections. The Cr-metal is coordinated by four terminal CO molecules and a P,P′-bidentate N,N-bis(diphenylphosphanyl)naphthylamine ligand in a distorted octahedral array. The N-atom adopts a planar geometry with the two P-atoms and C-atom attached to it. The four-membered metallacycle ring P2CrN is nearly planar.

Crystal and molecular structure of a cobalt(III) ammine complex of 2-Amino-4-imino-2-methylpentanoic acid

1975 ◽  
Vol 28 (4) ◽  
pp. 729 ◽  
Author(s):  
GB Robertson ◽  
PO Whimp
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Complex Cation ◽  
Three Dimensional ◽  
Cobalt Atom ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Ammine Complex ◽  
Coordination Sites ◽  
Acid Ligand

The crystal and molecular structure of a cobalt(III) ammine complex of 2-amino-4-imino-2-methyl-pentanoic acid, [Co(NH3)3{HN=C(CH3)CH2C(CH3)(NH2)(CO2)}]S2O6, has been determined from three-dimensional X-ray data collected by counter methods. The complex crystallizes in the monoclinic space group P21/c (C52h, No. 14), with a = 7.576(4), b = 18.209(7), c = 14.068(6) Ǻ, β = 125.25(2)�, Z = 4. The structure was solved by conventional Patterson and Fourier methods, and was refined by block-diagonal least-squares methods to weighted and unweighted 12-factors of 0.041 and 0.040 respectively, for the 1479 unique reflections having I/σ(I) ≥ 3.0. All hydrogen atoms have been located and refined. The complex cation is essentially octahedral about the central cobalt atom with three amine groups occupying mutually cis coordination sites; the three remaining sites at the cobalt atom are occupied by the tridentate 2-amino-4-imino-2-methylpentanoic acid ligand. The Co-O distance is 1.914(4) Ǻ, while the Co-N(imine) distance is 1.924(5) Ǻ. The Co-N(NH3) distances range from 1.968(5) to 1.979(5) Ǻ, and are equal within experimental error. Within the tridentate 2- amino-4-imino-2-methylpentanoic acid ligand, the C=N distance is 1.252(7) Ǻ, while at the carboxyl group the ?free? C-O distance [1.233(6) Ǻ] is significantly shorter than the distance from the carbon to the coordinated oxygen atom [1.270(7) Ǻ]. In the S2O6 counter anion, the S-S distance is 2.112(2) Ǻ, and the S-O distances range from 1.434(6) to 1.457(4) Ǻ, averaging 1.439 Ǻ.

Crystal and Molecular Structure of Difluorochlorine(III)-hexafluoroarsenate(V), ClF2AsF6

1971 ◽  
Vol 49 (15) ◽  
pp. 2539-2543 ◽  
Author(s):  
H. Lynton ◽  
J. Passmore
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Chlorine Atom ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
Arsenic Atom ◽  
Space Group

Crystals of difluorochlorine(III)hexafluoroarsenate(V), ClF2AsF6, are monoclinic, space group A2/a, a = 10.676(9), b = 7.673(7), c = 8.064(7) Å, β = 113.40(5)°. The structure was refined by three dimensional least squares methods to R = 0.045 for 185 independent observed reflections. The chlorine atom has two nearest fluorine neighbors at 1.541(14) Å, with a F—Cl—F angle of 103.17(0.70)°, and two longer fluorine bonds at 2.339(14) Å. All five atoms lie in a plane. The arsenic atom is octahedrally coordinated to six fluorine atoms and is connected to two ClF2+ groups via trans fluorine bridges.

Crystal structure of 2-(2,6-Dichlorophenylcarbamoyl)benzoic acid

1982 ◽  
Vol 35 (9) ◽  
pp. 1933 ◽  
Author(s):  
CHL Kennard ◽  
G Smith ◽  
GF Katekar
Keyword(s):  
Crystal Structure ◽  
Benzoic Acid ◽  
Dihedral Angle ◽  
Acid Amide ◽  
Three Dimensional ◽  
Direct Methods ◽  
Acid Group ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
A Cell

The crystal structure of 2-(2,6-dichlorophenylcarbamoyl)benzoic acid has been determined by direct methods from three-dimensional X-ray diffraction data and refined to R 0.076 for 971 'observed' reflections. Crystals are monoclinic, space group P21/c with Z4 in a cell of dimensions a 12.150(6), b l3.629(6), c 8.368(4) �, β lO3.75(4)�. The molecules form centrosymmetric hydrogen-bonded cyclic dimers [O. . .O, 2.64(1) �] with the carboxylic acid group lying in the approximate plane of the attached benzene ring (dihedral angle 7.63�). This is in turn almost parallel to the 2,6-dichlorophenyl substituent group on the acid amide (dihedral angle 4.14�). The amide group is synclinally related to the ring systems in a similar way to that found in other phthalamic acids.

Perchlorato, Nitrato, and Acetylacetonato Complexes of Copper(I). The Crystal and Molecular Structure of Perchloratobis(tricyclohexyiphosphine)Copper(I)

1975 ◽  
Vol 53 (13) ◽  
pp. 1949-1957 ◽  
Author(s):  
Roderic J. Restivo ◽  
Abraham Costin ◽  
George Ferguson ◽  
Arthur J. Carty
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Infrared Spectra ◽  
Copper Atom ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Cell Dimensions

Copper(I) perchlorate, nitrate, and acetylacetonate complexes of the types Cu(triphos)ClO4 (triphos = CH3C(CH2PPh2)3), Cu(Cy3P)2ClO4 (Cy3P = P(C6H11)3), Cu(triphos)NO3, Cu(Cy3P)2(HFac)(HFac = hexafluoroacetylacetonate), and Cu (Cy3P)2(TtFac) (TtFac = thienyltrifluoroacetylacetonate) have been synthesized by reduction of the corresponding perchlorate, nitrate, and acetylacetonates with tertiary phosphines. Infrared spectra indicate the presence of monodentate perchlorate groups in Cu(triphos)ClO4 and in Cu(Cy3P)2ClO4 and the crystal structure of the latter has been determined by a three-dimensional X-ray analysis using diffractometer data. The crystals are monoclinic, space group C2/c, with cell dimensions a = 18.159(6), b = 9.493(2), c = 22.182(3) Å, and β = 95.41(2)° and four molecules per unit cell. The structure was refined by block-diagonal least squares methods to a final R of 0.051 for 2617 reflections using anisotropic thermal parameters for the nonhydrogen atoms. The structure consists of discrete Cu(Cy3P)2ClO4 molecules with symmetry C2 separated by normal van der Waals distances. The copper atom is three-coordinate and the perchlorate anion is monodentate but disordered over two sites. Principal dimensions include: Cu—P 2.262(1) Å, Cu—O 2.220(7) Å, [Formula: see text][Formula: see text] and 99.8(2)°, and [Formula: see text]

An Intermediate in the Conversion of an Acetylene to a Vinyl Derivative: The Crystal and Molecular Structure of trans-Chloromethylbis(trimethylarsine)-platinum(II) Hexafluorobut-2-yne

1972 ◽  
Vol 50 (14) ◽  
pp. 2276-2284 ◽  
Author(s):  
Brian W. Davies ◽  
Richard J. Puddephatt ◽  
Nicholas C. Payne
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Free Ligand ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Monodentate Ligand ◽  
X Ray ◽  
Trigonal Bipyramidal

The crystal and molecular structure of trans-chloromethylbis(trimethylarsine)platinum(II) hexafluorobut-2-yne has been determined from three dimensional X-ray diffraction data recorded by diffractometric methods. The structure has been refined by full-matrix least-squares methods on F using 1156 reflections to an agreement factor R = 0.077. The crystals are monoclinic, space group [Formula: see text] with a = 6.803(8), b = 14.93(2), c = 20.20(2) Å, β = 104.9(1)°, and Z = 4. The coordination of the platinum atom is trigonal bipyramidal, with the acetylene considered a monodentate ligand, and the two trimethylarsine ligands occupying the equatorial plane. The chlorine atom and the methyl ligand occupy the apical positions, with Pt—Cl and Pt—C distances of 2.47(1) Å and 2.10(4) Å, respectively. The long Pt—Cl bond length indicates the strong trans-influence of the methyl ligand. The observed C—C bond length of 1.32(4) Å in the acetylene ligand is lengthened from the value of 1.22(9) Å measured in the free ligand. The geometry of the coordinated ligand is discussed in terms of the bonding scheme proposed by Greaves etal.

The Crystal and Molecular Structure of 3-Chloro-3-deoxy-1,2;5,6-di-O-isopropylidene-β-D-idose

1972 ◽  
Vol 50 (1) ◽  
pp. 93-98 ◽  
Author(s):  
F. W. B. Einstein ◽  
K. N. Slessor
Keyword(s):  
Molecular Structure ◽  
Furan Ring ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
R Factor ◽  
A Cell ◽  
The Mean ◽  
Least Squares Techniques

The crystal and molecular structure of 3-chloro-3-deoxy-1,2;5,6-di-O-isopropylidene-β-D-idose has been determined from three dimensional X-ray data collected by counter methods. The structure was refined by full-matrix least-squares techniques to a conventional R factor of 5.7% for the 817 observed reflections. The compound crystallizes in the orthorhombic space group P212121 with four molecules in a cell of dimensions a = 9.744(6), b = 26.76(2), c = 5.403(3) Å.The structure analysis has served to confirm the site of halogenation and that it occurs stereospecifically. The conformation of the furan ring is an envelope arrangement with C(4) displaced from the mean plane.

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