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The crystal and the molecular structures of the title complex were determined by means of the single-crystal X-ray diffraction method. The crystal of PtC28H23O5N2Cl4, F. W. 804.40, (black-violet in color) is monoclinic, with the space group of P21⁄a, a=18.293(4), b=9.682(2), c=15.797(3) A, β=96.55(2)°, U=2779.6(9) A3, Z=4, Dm=1.90, Dx=1.92 g cm−3, and μ (Mo Kα)=57.37 cm−1. The platinum atom is in a hexa-coordinated octahedral geometry, where one 2-(2-benzoxazolyl)phenolate (bxp−) ion is chelated with its N and phenolato O atoms. The bxp− ligand as well as the free Hbxp molecule are both approximately planar, and their planes are approximately in parallel: They are arranged alternately and are laid roughly along the a-axis. Although the overlappling areas of the neighboring rings are only 23 and 13% respectively of the whole ring area, the interplane distances are 3.42 and 3.49 A.

The titled series of isomorphous complexes, the first octakis(isothiocyanato) complexes of lanthanoids, were obtained. Their crystals are tetragonal, space group P4nc, Z=2. The cell dimensions of the praseodymium complex, for example, are a=15.871(7), c=11.543(6) A, U=2908(3) A3, and Dm=1.29(3), Dx=1.29 g cm−3, μ(MoKα)=11.60 cm−1, with a final R value of 0.069. The metal atom is octa-coordinated by eight isothiocyanate ions in an intermediate geometry between cube and square-antiprism. The benzene included in the praseodymium complex crystals was retained up to 174°C (DTA), and was not removed even after being heated for 12 h at 110°C. In cases of the other isomorphous members, the benzene was removed at lower temperatures, respectively. The isomorphous fluorobenzene adduct was obtained only for the lanthanum complex.

The crystal and molecular structures of the chloroacetato complexes of gadolinium(III), erbium(III), and ytterbium(III) indicated in the title were determined by the single-crystal X-ray diffractio...

The new complexes indicated in the title have been synthesized, and the crystal and molecular structure of the neodymium(III) complex has been determined by the X-ray diffraction method. The crystal is monoclinic, with the space group C2/c, Z=16, a=28.887(4), b=28.913(5), c=24.814(5)A, β=106.72(1)°. The final R value for 7761 reflections is 0.066. The central neodymium(III) atom of the complex is octa-coordinated and is in a dodecahedron geometry; three O,O′-diisopropyl dithiophosphato ligands, chelating by both of the sulfur atoms, span the two m edges of a trapezium as well as one a edge of the other trapezium, and two oxygen atoms of both the benzamide ligate at both tips of the base edge of the latter trapezium. The solid and the acetonitrile solution of the europium(III) complex are orange in color, and they show a charge-transfer band in their near-ultraviolet absorption spectra.

The structure of the title complex was determined by the single-crystal X-ray-diffraction method. It is triclinic, with the space group P\bar1; the cell constants were a=12.529(2), b=15.044(4), c=10.063(1) A, α=104.15(2), β=98.73(1), and γ=87.16(2)°; Z=1, and the final R value was 0.053. The central metal atom is in a tricapped trigonal-prism geometry and is ennea-coordinated with seven oxygen atoms of the carboxylate ligands and with each oxygen atom of one water and one ethanol molecule. The complex is dimeric and the metal atoms are bridged with four carboxylate ions; two of them act as bidentates, and the other two, as tridentates, where one oxygen atom is coordinated to both metal atoms. The other carboxylate ion makes a chelate ring with each metal atom. The dimer is connected through hydrogen bondings to the atoms on both sides along the c-axis.

The crystal and molecular structure of the title complex was determined by a single-crystal X-ray diffraction technique. The crystal is triclinic with a space group P\bar1, a=11.323(4), b=18.383(10), c=9.284(5) A, α=104.62(4), β=114.26(3), γ=77.71(4)°, Z=4; the final R value obtained was 0.034. All cadmium atoms are lined approximately along the [111] axis and each pair of metal atoms are bridged by two thiocyanate ions (SCN), one of which is S-coordinated and the other is N-coordinated to the same side metal atom. Also bonded with two nitrogen atoms of 4-methylpyridine (pic) ligands, the metal atom is 4N2S-hexa-coordinated and is in an octahedral geometry. The cadmium atoms, where the ligated respective pairs of N(SCN), N(pic), and S(SCN) atoms are all in a trans configuration, and the metal atoms where the ligated respective pairs of N(pic) and S(SCN) are in cis, while the pair of the N(SCN) in trans configuration, appear alternatively in the polymer chain.

N-Methyl-2-piperidone adduct and dimethyl sulfoxide adduct of cobalt(II)mercury(II) thiocyanate were synthesized and their crystal and molecular structures were determined by the single-crystal X-ray diffraction technique. The former adduct is triclinic with a space group P\bar1, a=8.488(3), b=17.206(7), c=8.466(3) A, α=103.72(1)°, β=90.00(1)°, γ=100.85(1)°, Z=2, while the latter adduct is orthorhombic with a space group P212121, a=8.418(3), b=27.389(10), c=8.407(3) A, Z=4, and the final R values obtained were 0.059 and 0.066, respectively. In these adducts each mercury atom is in the tetrahedral geometry, coordinated with four sulfur atoms of the thiocyanate (SCN) ions, and each cobalt atom is in the octahedral geometry, coordinated with four nitrogen atoms of SCN ions and two oxygen atoms of the Lewis-base molecules which occupy the trans-positions. Each pair of different kinds of metal atoms are bridged by an SCN ion forming a 16-membered ring of Co2Hg2(SCN)4; these are linked, forming a two-dimensiona...

Five isomorphous lanthanoid(III) complexes were synthesized, and the structure of the terbium (1) and erbium (2) complexes were determined by the use of the single-crystal X-ray diffraction method. Crystals of 1 and 2 are monoclinic, with the space group P21/n, and the cell constants are: (1) a=25.076(8), b=15.446(3), c=14.579(8) A, β=100.77(4)°; (2) a=25.036(20), b=15.228(4), c=14.805(19) A, β=99.50(12)°. The structures were solved by the heavy-atom method and refined by the block-diagonal least-squares method. The final R values of 1 and 2 are 0.061 and 0.055 respectively. They consist of discrete complex cations and dithiophosphate anions. The central metal atom of the cationic complex is hepta-coordinated, and it is in a pentagonal bipyramidal geometry, where four sulfur atoms of two dithiophosphate ions and one oxygen atom of a benzamide ligand take the equatorial positions, while two benzamide oxygen atoms are in the axial positions.

The crystal and molecular structures of the title complexes were determined by the single-crystal X-ray diffraction method. Both of them are triclinic, with the space group P\bar1. The crystallographic data: 2-methylpyridine (α-pic) adduct, a=11.076(3), b=18.478(8), c=9.299(3)A, α=104.60(3), β=114.84(2), γ=81.12(3)°, Z=4, final R value is 0.037; 3-methylpyridine (β-pic) adduct, a=8.7667(16), b=16.655(4), c=5.8447(10)A, α=91.406(18), β=100.571(14), γ=92.525(18)°, Z=2, final R value is 0.041. In both complexes, all cadmium atoms are in 4N2S-hexa-coordination, being in an octahedral geometry; they are oriented as any pair of side-by-side metal atoms being bridged by two thiocyanate ions. In the α-pic adduct, the chain is oriented approximately along the [111] axis. In the chain, the metal atoms in two kinds of orientations appear alternately: Around one kind of the metal atoms three kinds of ligating atoms are all in trans-configurations, and around the other kind of the metal atoms the respective pairs of N...

The title complex was newly synthesized and its crystal and molecular structure was determined by the single-crystal X-ray diffraction technique. The crystal is monoclinic, space group C2⁄c, a=16.005(4), b=10.520(2), c=15.338(4) A, β=114.68(2)°, and Z=4. In the complex, the central metal atom is hexa-coordinated being in a deformed octahedral geometry: Two 2-(2-benzoxazolyl)phenolato ligands form six-membered chelate rings being coordinated with their oxazolyl nitrogen and phenolato oxygen atoms, while the nitrate ion acts as a bidentate with its two oxygen atoms. As the benzoxazolyl ring is parallel and overlapped with that of the neighboring complex along the c-axis, where the interplane distance is 3.557 A, some interaction between the rings is expected. As this complex in solid state is deep violet, almost black, in color, some charge-transfer bands are expected to exist in its electronic spectra. The bis[2-(2-benzothiazolyl)phenolato]nitratoiron(III) was found to be isomorphous to the title complex.

The crystals of the title complex resolve spontaneously. The enantiomeric crystals were separated under a microscope. They are orthorhombic, space group P212121. This is a square planar complex with 2Cl in cis-positions. The ligand acts as a unidentate with its N atom. The absolute configuration was correlated with the CD spectrum in microcrystalline state.

The M–O bond lengths and some bond angles of the acetato ligands in the title compounds were compared with each other using their structural data as obtained by the single-crystal X-ray diffraction method. With the increase in the atomic number of the central metal atom, the length of the weakest M–O bond in the bridge increases, even though all the other M–O bonds are shortened. This fact can be explained as follows: as the number of ligating oxygen atoms around the central metal atom is almost at a maximum in these complexes, the sharing space of the tenth coordinating atom on the coordination sphere decreases when the radius of the central metal atom is shortened as a result of the lanthanoid contraction effect.

The title complex was synthesized and its crystal and molecular structure were determined by the single-crystal X-ray diffraction technique. The crystal is orthorhombic with a space group P21nb, a=14.953(4), b=15.955(4), c=7.6838(9) A. The crystal was solvent by means of the heavy-atom method and the final R value was 0.059. The mercury atom is in the tetrahedral geometry, coordinated with four sulfur atoms of the thiocyanate (SCN) ions, and the cobalt atoms is in the octahedral geometry, coordinated with four nitrogen atoms of SCN ion and two oxygen atoms of N-methylformamide which occupy the cis positions. Each pair of different kinds of metal atoms is bridged by an SCN ion and are in a three-dimensional network. Twenty-four membered rings of Co3Hg3(SCN)6, where the metal atoms are arranged hexagonally in a chair-form, are condensed two-dimensionally approximately parallel to the (100) plane. All mercury atoms on one plane are bridged by SCN ions to the cobalt atoms of the polymeric plane next to the [1...

The crystal and molecular structure of tetrakis{(isopropylthio)acetato}bis(quinoline)dicopper(II) (1), bis(dibenzylamine)bis{(ethylthio)acetato}copper(II) (2), and bis{(isopropylthio)acetato}tris(isoquinoline)copper(II) (3) were determined by the X-ray diffraction method. The final R values obtained are 0.041, 0.055, and 0.078 for 1, 2, and 3 respectively. 1 is green in color and is orthorhombic with the space group Pcab. It has a dimer structure similar to that of the copper(II) acetate hydrate, where four (alkylthio)acetate liagnds bridge both copper(II) atoms. 2 is violet in color and is monoclinic with the space group A2/a. It has a square-palnar geometry, and no atoms are coordinated to the copper(II) atom from the axial direction, probably because of the steric effect of the large dibenzylamine molecules. 3 is blue in color and is triclinic with the space group P\bar1. It has potentially a hepta-coordinate geometry, where one nitrogen atom and two oxygen atoms ligate from the axial direction of the ...

Two types of lanthanoid(III) m-hydroxybenzoates, indicated in the title, have been synthesized, and the crystal and molecular structures of four representative complexes, where M=La (1), Nd (2), Sm (3), and Er (4), were determined by the single-crystal X-ray diffraction method. They are all triclinic, space group P\bar1, and the cell constants are as follows: (1) a=12.351(11), b=15.533(10), c=9.250(4) A, α=109.86(4), β=101.40(6), γ=62.95(6)°; (2) a=12.287(4), b=15.542(7), c=9.194(3) A, α=109.64(3), β=101.46(3), γ=62.83(3)°; (3) a=10.580(1), b=12.006(5), c=10.105(2) A, α=111.14(2), β=90.27(1), γ=97.16(2)°; (4) a=10.586(4), b=11.943(6), c=10.027(5) A, α=111.11(3), β=90.53(4), γ=97.26(4)°. The final R values obtained were (1) 0.039, (2) 0.038, (3) 0.030, and (4) 0.039. The central metal atoms of both types of complexes are octa-coordinated, and each is in a square-antiprism geometry. In 1 and 2, one free acid molecule is present, and the molecule is hydrogen-bonded to the oxygen atoms of the coordinated wate...

The crystal and molecular structure of the title complex has been determined by the X-ray diffraction method. The crystal was triclinic, space group P\bar1, a=12.80(1), b=16.65(1), c=8.659(9) A, α=...

The crystal and molecular structure of the two new thiocyanatocadmate(II) complexes indicated in the title were determined by the single-crystal X-ray-diffraction technique. [(CH3)4N]2[Cd(SCN)4] is tri-clinic, with a space group of P\bar1; a=7.300(2), b=13.019(4), c=5.8920(9) A, α=96.32(2), β=93.080(18), γ=104.63(2)°, and Z=1, while [(CH3)4N][Cd(SCN)3] is orthorhombic with a space group of Pna21; a=10.506(3), b=13.797(5), c=9.4506(18) A, Z=4. In both complexes, the cadmium atom is in an octahedral geometry. In 1, the metal atom is at the center of symmetry, and respective pairs of side-by-side metal atoms are bridged by two thiocyanate (SCN) ions, where one SCN ion is S-coordinated and the other is N-coordinated to the same-side metal atom. Also bonded with two nitrogen atoms of unidentate SCN ions, the metal atom is 4N2S-hexa-coordinated, and they line up along the c-axis in a polymeric form. In 2, respective pairs of side-by-side metal atoms are bridged by three SCN ions, two of those SCN ions being S-c...

Two types of the mixed complexes indicated in the title have been synthesized, and their crystal and molecular structures of the lanthanum (1) and the europium (2) complexes have been determined by the X-ray diffraction method. Both 1 and 2 are monoclinic, space group P21⁄n, and Z=4. 1, a=17.354(7), b=23.336(4), c=10.955(2) A, β=96.04(2)°, final R value calculated from 4870 reflections is 0.069; 2, a=29.846(7), b=20.070(3), c=14.057(3) A, β=92.13(2)°, final R value calculated from 7811 reflections is 0.077. In 1, the central metal atom is octa-coordinated, and is in a dodecahedral geometry, where all O,O′-diisopropyl dithiophosphato ligands (iPr2dtp) span m-edges of the dodecahedron, chelating through both of the respective sulfur atoms. Dimethyl sulfoxide (dmso) ligands occupy the apexes of the other m-edge. In 2, the europium(III) metal atom of the cationic species is hepta-coordinated and is in a pentagonal-bipyramidal geometry where two oxygen atoms of dmso ligate from respective ends of the axis and ...

The title complex was synthesized, and its crystal and molecular structures were determined by the single-crystal X-ray-diffraction method. It is triclinic, with the space group of P\bar1; the cell constants are a=20.621(4), b=22.288(5), c=7.724(1) A, α=93.30(2), β=96.78(2), γ=107.43(2)°, Z=4, and the final R value is 0.048. Although there are two kinds of crystallographically independent complexes, their structures are almost the same, with only a slight difference in the orientations of the naphthalene rings of the ligands. Both of the central metal atoms are ennea-coordinated and are in the tricapped trigonal-prism geometry: two carboxylato ligands make four-membered chelate rings, and they are also ligated five water oxygen atoms. No carboxylate ions bridge the metal atoms, but the oxygen atoms of the ligands, isolated carboxylate ions, and the crystalline water molecules are linked through hydrogen bondings along the bc-plane. The metal atoms lie on a plane parallel to (100), and the planes are separ...

The title complex was synthesized, and the crystal structure was determined by means of the X-ray diffraction technique. The crystal is monoclinic; space group P21/n, a=16.310(3), b=6.777(1), c=14.576(3) A, β=96.13(1)°, Z=2, Dx=1.58, Dm=1.55(3) g cm−3, μ(Mo Kα)=1.12 mm−1. The molecule has a center of symmetry, and a distorted octahedron is formed around the central cadmium atom; two O,O′-diethyl dithiophosphato ions (dtp) act as bidentate ligands, and each ligand forms a four-membered chelate ring with its two sulfur atoms on the equatorial plane, while two hexamethylenetetramine molecules are coordinated to the metal atom by their nitrogen atoms from the axial direction. Related adducts, Cd(II)(dtp)2·Xn, where X is a donor and n=1 or 2, were also synthesized, and their structures were compared with those of the corresponding Co(II)(dtp)2·Xn−type complexes.

The new complex indicated in the title has been synthesized, and its crystal and molecular structure has been determined by the X-ray diffraction method. The crystal was triclinic; space group P\bar1, Z=2, a=23.071(9), b=11.060(11), c=10.793(13) A, α=120.0(1), β=97.2(2), γ=88.9(2)°. The final R value for 5969 reflections is 0.047. The central lanthanum(III) atom is an octa-coordination and in a dodecahedron geometry, being coordinated with six sulfur atoms of three O,O′-diisopropyl dithiophosphate ligands (iPr2dtp), which span at three m edges, and with two oxygen atoms of both the N,N-dimethylacetamide ligands (dma) at both ends of the remaining m edge. The other [Ln(iPr2dtp)3L2]-type complexes, where Ln=La or Nd; L=dma or N,N-dimethylformamide, have also been obtained. The P=S double bond of the iPr2dtp ligand in the title complex is almost completely delocalized.

Scandium(III) p-toluenesulfonate hexahydrate, as well as the isomorphous yttrium(III) and six lanthanoid(III) (Sm, Gd, Dy, Ho, Er, and Yb) p-toluenesulfonate enneahydrates, were synthesized and the...

The crystal and molecular structures of the chloroacetato–dimethyl sulfoxide (dmso) mixed complex of neodymium(III) indicated in the title were determined by the single-crystal X-ray diffraction method. The crystal is monoclinic, space group P21⁄n, a=21.106(21), b=15.871(8), c=15.748(7) A, β=93.29(5)°, Z=4 (including 12 metal atoms in a unit cell). There are three kinds of crystallographically independent metal atoms, Nd(1), Nd(2), and Nd(3): Nd(1) and Nd(3) are ennea-coordinated (approximately tricapped trigonalprism geometry), and Nd(2) is deca-coordinated (approximately bicapped square-antiprism geometry) including a slightly long M–O bonding. All dmso molecules are directly coordinated to the metal atoms as unidentate, while all the carboxylate ions bridge metal atoms acting as bidentate or tridentate ligands. The bridging atoms are arranged in a chain which is approximately formed along the [101] axis. Also, the isomorphous lanthanum(III) and praseodymium(III) complexes were obtained and their struct...

Eight isomorphous 2-naphthalenesulfonato complexes of lanthanoids(III) (Pr, Nd, Sm, Eu, Gd, Dy, Er, and Yb) were synthesized, and the structures of five of them were determined by the single-crystal X-ray-diffraction method. They are monoclinic, with the space group of P21; the cell constants of the PrIII complex, for example, were a=18.228(8), b=7.498(4), c=14.177(9) A, β=107.75(4)°, Z=2, and its final R value was 0.043. The unit-cell size of the complex decreases with the increase in the atomic number of the metal atom. The central metal atom is in a square-antiprism geometry and is octa-coordinated with two unidentate 2-naphthalenesulfonato ligands and six water–oxygen atoms. Nonligated oxygen atoms of the sulfonato ions form hydrogen-bonds with the coordinated and lattice water molecules to form a double-layered network along the ab-plane. All the naphthalene rings stand together to form hydrophobic sheets between the hydrogen-bonding networks.

The new complex indicated in the title was synthesized and its crystal and molecular structures were determined by the use of a single-crystal X-ray diffraction method. The crystal is tetragonal, with the space group P\bar4, and the cell constants are a=12.124(5) and c=7.985(2) A. The structure was solved using the heavy-atom method, and the final R value was 0.039. Two kinds of crystallographically independent mercury atoms in the unit cell are tetra-coordinated and they are in the tetrahedral geometry, where four sulfur atoms of the thiocyanate ions are ligated, respectively. The cobalt atom is hexa-coordinated, and is in an octahedral geometry, where four nitrogen atoms of the thiocyanate ions are coordinated equatorially, and two water oxygen atoms axially. Thiocyanate ions span mercury and cobalt atoms to form two-dimensional networks parallel to the (001) plane. The planar polymeric complexes are linked to the c-axis direction, through hydrogen bonds between coordinated water molecules and N,N-dimet...

The crystal and molecular structures of the hydrated lanthanum(III), neodymium(III), and europium(III) chloroacetates indicated in the title were determined by the single-crystal X-ray diffraction method; these three salts as well as the praseodymium(III) salt are apparently isomorphous. By the same synthetic technique, gadolinium(III) or heavier lanthanoid(III) did not give the isomorphous salts. Their crystals are monoclinic with the space group of P21⁄c, and the cell constants of the neodymium(III) salt, for example, are, a=14.805(4), b=18.765(4), c=14.403(5) A, β=95.13(3)°. There are crystallographically independent three kinds of nine-coordinated metal atoms: Nd(1), Nd(2), and Nd(3). Among them, Nd(1) and Nd(2) are best approximated as being in a tricapped trigonal prism geometry. The Nd(3) is best regarded as being in a monocapped square-antiprism geometry, although one more additional oxygen atom, O(35), approaches one side face. In the lanthanum(III) complex, O(35) is thought to be ligated to La(3...

The crystals of the title new lanthanum(III) complex, LaC45H86N11S7, F.W. 1144.59 are orthorhombic space group Bm21b, a=17.438(7), b=21.507(9), c=16.616(6) A, U=6232(4) A3, Dm=1.21(3), Dx=1.22 g cm−3, and μ(Mo Kα)=9.63 cm−1. The central lanthanum(III) atom has a unicapped trigonal-prism 7N-hepta-coordination geometry: seven thiocyanato nitrogen atom are ligated. There are no bridgings between the complexes and/or counter cations. Each benzene molecule is surrounded by the thiocynate ions and ethyl groups of the cations. Although these crystals lose benzene at about 60 °C, they are stable for more than several weeks ambient temperature, and can be regarded as a kind of inclusion compound. The isomorphous praseodymium(III) complex was also obtained.

The crystal and molecular structures of the title new complexes were determined by means of a single-crystal X-ray diffraction method. The crystals of the neodymium(III) complex, NdC12H28N5O4S4, F. W. 578.87, are triclinic, space group P\bar1, a=14.13(2), b=15.39(1), c=12.92(1) A, α=106.81(8), β=114.70(9), γ=90.09(10)°, U=2418(5) A3, Z=4, Dm=1.57(3), Dx=1.59 g cm−3, μ(MoKα)=25.22 cm−1. The isomorphous europium(III) complex was also obtained: a=14.069(9), b=15.328(9), c=12.865(9) A, α=106.98(5), β=114.57(5), γ=90.07(6)°, U=2390(3) A3, Dm=1.60(3), Dx=1.63 g cm−3, μ(Mo Kα)=30.04 cm−1. Two crystallographically independent neodymium(III) atoms in a unit cell have approximately the same coordination geometry: square antiprism 4O,4N-octa-coodination. A pair of the O atoms as well as N atoms are in cis positions on the top square and in trans positions on the bottom square of each polyhedron, where the lines connecting both pairs of the N atoms on both squares are approximately parallel.

The crystal and molecular structure of the title complex was determined by the single-crystal X-ray diffraction method. The crystallographic data are: monoclinic, space group P21⁄c, a=19.164(6), b=19.020(9), c=18.649(7) A, β=95.06(3)°, and Z=8 (16 metal atoms are in a unit cell). There are two crystallographically independent dimeric [SbBr(C6H5)3]2O molecules, which are almost in the same form. Each antimony atom is bonded with three phenyl carbon atoms equatorially and one bromine as well as one bridging oxygen atoms axially, being in a trigonal-bipyramidal geometry. The Sb–O–Sb′ angles are 170.2(7) and 176.6(8)°, while the Sb–O lengths are in the range of 1.931(13)—1.958(13) A, which are shorter than the sum of their covalent radii of the atoms: 2.15 A.

The structure of the title complex has been determined by the single-crystal X-ray diffraction method. A crystal of Er2C12H8O16Cl18, F. W. 1380.86 is triclinic, with the space group of P\bar1, a=12.787(8), b=15.209(7), c=11.685(7) A, α=102.24(5), β=114.43(5), γ=70.59(4)°, Z=2 (for the dimer formula), Dx=2.36, Dm=2.34(3) Mg m−3, and μ(MoKα)=5.74 mm−1. All the carboxylate ions act as bidentate bridges, and each pair of the side-by-side metal atoms is bridged by four carboxylate ions, or by two carboxylate ions and one water-oxygen atom, alternately, forming a polymeric chain approximately parallel to the [011] axis. The chains are arrayed in layers parallel to the (100) plane, and the respective layers are separated by the trichloromethyl groups.

The crystal and molecular structure of the title complex was determined by means of a single-crystal X-ray diffraction method. A crystal of CdC16H18N4S2, F. W. 442.8, is monoclinic, with the space group of P21⁄n, a=27.390(19), b=5.7709(8), c=5.8733(9) A, β=90.35(3)°, U=928.3(7) A3, Z=2, Dm=1.57(3), Dx=1.58 Mg m−3, and μ(Mo Kα)=1.59 mm−1. The cadmium(II) atom is hexa-coordinated being ligated with two thiocyanato (SCN) sulfur atoms, as well as with two SCN and two benzylamine nitrogen atoms, where the respective pairs of the same kinds of atoms are all in transconfiguration. Each cadmium atom is at the center of symmetry, and the coordination structure around the atom is symmetric. The metal atoms are lined along c-axis, and the pair of the neighboring metal atoms are doubly bridged by SCN ions, although the bridges are a little weaker than the other same type adducts.

The crystal and molecular structure of the mew title complex has been determined by means of a single crystal X-ray diffraction method. It is triclinic with the space group P\bar1, Z=2, a=15.518(5), b=19.827(7), c=7.493(2) A, α=100.90(3), β=103.94(2), γ=82.85(3)°. Both of the metal atoms have almost the same coordination geometry, pentagonal bipyramidal which coordinates the oxygen atoms of five water molecules (2 axial and 3 equatorial ones) and the two hydroxide ions which bridge the both metal atoms. The Sc(1)···Sc(2) distance is 3.403(2) A. The average Sc–O(H2O) bond length is 2.194 A, which is much longer than that of Sc–O(OH), 2.072 A. Benzenesulfonate ions and the other water molecules do not coordinate to the metal atoms, though their oxygen atoms as well as those of the coordinated water are connected with each other by a network involving hydrogen bonding.

The light lanthanoid(III) (La or Nd) 1-hydroxy-2-naphthoate crystals indicated in the title were obtained and their structures were determined by the X-ray diffraction method using their single crystals. They are orthorhombic with the space group P212121, Z=4. The unitcell axis lengths of the lanthanum(III) complex are: a=11.985(4), b=40.21(5), and c=7.017(1) A. The central metal atom is ennea-coordinated and is in a tricapped trigonal-prism geometry, where two carboxylate ions act as the unidentates, and the other coordinating positions are occupied by water oxygen atoms. The non-coordinated carboxylate ion is hydrogen-bonded to two ligated water oxygen atoms with its respective carboxylato oxygen atoms. The complex molecules are not directly bridged by the carboxylate ions, but the complexes are linked by hydrogenbondings in the a- and c-axis directions. Such hydrophilic and the hydrophobic layers of the naphthalene rings, both of them being parallel to the ac-plane, are laid alternately in the crystal.

The title complex (1), which is two-dimensional polymeric and an allotrope of the previously reported linear polymeric complex (2), was obtained and its crystal and molecular structure was determined by means of a single-crystal X-ray diffraction method. Since 1 is more soluble in organic solvents, 1 and 2 could be prepared, separately. The crystal of CdC16H18N4S2, F. W. 442.9, is monoclinic, space group P21⁄c, a=13.958(2), b=5.759(1), c=11.466(2) A, β=99.24(1)°, U=909.8(3) A3, Z=2, Dm=1.61(3), Dx=1.62 g cm−3, μ(Mo Kα)=14.2 cm−1. The cadmium atom is in a trans-2S4N-hexa-coordinated octahedral geometry. Each cadmium atom is at the center of symmetry, and it is bridged to four cadmium atoms by an thiocyanate ion, respectively, and the complex network is extended on the bc-plane.

An X-ray diffraction study of the title complex has been carried out. The crystal is monoclinic, with the space group P21; Z=2; a=8.196(4), b=7.275(3), c=7.740(4) A, β=103.73(4)° Full-matrix least-squares refinements have led to the final R value of 0.030. The structure consists of one-dimensional polymers bridged by chlorine atoms and a carboxyl group. Four chlorine atoms coordinate to a cadmium atom and form a square plane. The planes extend in the direction of the b axis like an infinite folding screen, sharing opposite edges. From the trough positions in the zigzag structure, the carboxyl oxygen atoms of 4-hydroxy-L-proline coordinate forkedly to two cadmium atoms. The ligand is a zwitter ion in the complex.

The title complex, which has a new-type layer structure, has been obtained, and its crystal and molecular structure has been determined by the X-ray diffraction technique. The crystallographic data are: monoclinic, space group P21⁄n, a=18.264(7), b=16.223(7), c=10.623(5) A, β=92.77(5)° and Z=4. The final R value was 0.059. The cobalt atoms are in an octahedral geometry, ligated by three thiocyanato(SCN) nitrogen atoms and three oxygen atoms (N-methyl-2-pyrrolidone) in a meridional configuration; these cobalt atoms are cross-linked to adjacent mercury atoms by SCN ions, forming a characteristic layer structure which consists of twenty-four-membered rings of the [Co3Hg3(SCN)6] unit. The mercury atoms are in the tetrahedral geometry, ligated by four sulfur atoms of SCN ions, three bridging and one unidentate. The complex layers in parallel are piled up in the a-axis direction, and there are no bridgings or hydrogen bondings between them.

The crystal and molecular structure of the title complex was determined by means of the singlecrystal X-ray diffraction method. The crystal of NdC18H22O9F9, F.W. 697.59, is orthorhombic, with a space group Pbna, a=22.068(5), b=22.293(4), c=11.020(2) A, U=5421(2) A3, Z=8, Dm=1.72(3), Dx=1.71 Mg m−3, and μ(Mo Kα)=20.46 cm−1. The central metal atom is octa-coordinated, being ligated with six β-diketonato and two water oxygen atoms, and is in a dodecahedral geometry. Two configurational isomers co-exist in the crystal, with the respective occupancy factors of 74 and 26%. In these isomers, the two chelate rings span in different ways; although the positions of all ligating oxygen atoms are the same, the chelates span two m-edges in one isomer and two g-edges in the other one.

The crystal and molecular structure of the title complex has been determined by the use of the single-crystal X-ray diffraction method. The crystal of CeC21H17O10, F. W. 569.48, was monoclinic; space group P21⁄c, a=13.401(2), b=19.173(5), c=8.079(1) A, β=98.94(1)°, U=2050.6(8) A3, Z=4, Dm=1.84(3), Dx=1.84 Mg m−3, and μ(Mo Kα)=2.31 mm−1. Each cerium(III) atom is ennea-coordinated and is in a tri-capped trigonal-prism geometry. They are in a linear polymer, and each cerium(III) atom is bridged to the next metal atom by three carboxylate ligands.

The crystal and molecular structure of the title complex was determined by means of a single-crystal X-ray diffraction method. A crystal of Ni2C46H54N10S4, F. W. 992.67, is triclinic with a space group P\bar1, a=13.259(4), b=15.627(5), c=6.5150(16) A, α=90.60(3), β=93.64(2), γ=112.601(19)°, U=1242.9(6) A3, Z=1, Dm=1.32(3), Dx=1.33 Mg m−3, and μ(Mo Kα)=9.60 cm−1. The central metal atom is hexa-coordinated, being ligated with three benzylamine and two thiocyanato (SCN) nitrogen atoms as well as one SCN sulfur atom. Two metal atoms are bridged by two SCN ions; however, the Ni-S bond length is 2.639(3) A, which is a little longer than the sum of the Shannon’s ionic radii. The distance Ni···Ni is 5.717(3) A and the dimeric complexes are discrete in a crystal.

The crystal and molecular structure of the title complex has been determined by the use of the single-crystal X-ray diffraction method. The crystal of LaC40H58O8P3S8, F.W.=1155.20, is triclinic; space group P\bar1, a=13.300(5), b=19.816(8), c=11.257(4) A, α=92.79(4), β=114.92(3), γ=75.40(4)°, U=2598(2) A3, Z=2, Dm=1.48(3), Dx=1.48 g cm−3, and μ(Mo Kα)=1.29mm−1. Each lanthanum(III) atom is octa-coordinated and is in a dodecahedral geometry. The oxygen atoms of dibenzyl sulfoxide molecules are ligated at both ends of the base of a trapezia, and the chelating O,O′-diethyl dithiophosphates span two m edges and one a edge.

The crystal and molecular structure of the title complex was determined using the single-crystal X-ray diffraction method. A crystal of CoHgC14H22N6O4S4, F.W. 726.15, is tetragonal with a space group P\bar4, a=12.082(3), c=8.097(2)A, U=1182.0(5)A3, Z=2, Dx=2.04 Mg m−3, and μ(Mo Kα)=7.72 mm−1. Tetrahedral mercury(II) coordinated with four sulfur atoms and octahedral cobalt(II) coordinated with four nitrogen atoms of SCN− (equatorially) and two oxygen atoms of H2O (axially) are linked by thiocyanate bridges to form planar networks parallel to (001). The planes are connected by N-methyl-2-pyrrolidone (mpd) molecules through the hydrogen bonds with two coordinated water molecules at both side networks. The structure resembles that of the N,N-dimethylacetamide (dma) adduct, CoHg(SCN)4(H2O)2·2dma. These are new types of inclusion compounds.

The crystal and molecular structure of the title complex has been determined by the use of single-crystal X-ray diffraction. The crystal of YbC9H19O8S3, F.W.=524.48, was monoclinic, with a space group of P21/a; a=12.501(6), b=25.096(9), c=10.788(2) A, β=90.25(3)°, U=3384(2) A3, Z=8, Dm=2.07(3), Dx=2.06 Mg m−3, and μ(Mo Kα)=6.20 mm−1. Both Yb(1) and Yb(2) are octa-coordinated and are in a dodecagedral geometry. They are in a linear polymer form, parallel to the c axis; Yb(1) and Yb(2) are arrayed in a line alternatively, bridged by one carboxylate ligand.

The title complex has been synthesized, and its crystals and molecular structure has been determined by the use of the single-crystal X-ray-diffraction method. The crystal of Nd2C60H138O15P6S15, F. W.=2055.03, was monoclinic, with a space group of An; a=23.696(4), b=23.466(4), c=20.208(4) A, β=111.22(2) °, Z=4, V=10475(4) A3, Dm=1.30(3), Dx=1.30 Mg m−3, and μ(Mo Kα)=1.41 mm−1. The complex consists of cationic and anionic species, as is shown in the title. The metal atom of the cationic complex is hepta-coordinated and is in a pentagonal-bipyramidal geometry, while the anionic one is octa-coordinated and is in a dodecahedral geometry.

Bis[(propylthio)acetato]cobalt(II) hexamer has been found, by X-ray crystal structure analysis, to have a structure in which the six cobalt(II) atoms form a ring in a boat configuration which is bridged by the ligands which bond in two different ways; there is no metal–metal interaction.