• Korean Journal of Crystallography
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• v.9 no.1
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• pp.71-76
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• 1998

Crystal structure of Bis(ethylenediamine)palladium(II)-Bis(oxalato)palladate(II0 has been determined by X-ray crystallography. Crystal data : (Pd(C2H8N2)2.Pd(C2O4)2), Fw=509.04, Monocline, Space Group P21/c (no=14), a=6.959(2), b=13.506(2), c=15.339(2) Å, β=99.94(3), Z=4, V=1420 Å3, Dc=2.380 gcm-3, μ=25.46cm-1, F(000)=992. The intensity data were collected with Mo-Kα radiation (λ=0.7107 Å) on an automatic four-circle diffractometer with a graphite monochromater. The structure was solved by Patterson method and refined by full matrix least-square methods using unit weights. The final R and S values were R=0.021, Rw=0.030, Rall=0.032 abd S=2.1 for 1472 observed reflections. The essentially planar complex anions form diade of interplanar distances of 3.41 Å and their diads are stacked along aaxis with interplanar separation of 3.44 Å.

• Korean Journal of Crystallography
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• v.7 no.1
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• pp.36-43
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• 1996

The crystal structure Tris(ethylenediamine)nickel(II)Dichromate has been determined by X-ray crystallography. Crystal data: a=8.268(2), b=13.865(2), c=14.921(2)Å, γ=102.04(2)°, V=1672.9(5)Å3, Z=4, Monocline, P21/b (space group No.=14), Dcalc=1.806 gcm-3, μ=24.05 cm-0.1. The intensity data were collected with Mo-Kα radiation(λ=0.7107Å) on an automatic four-circle diffractometer with a graphite monochromator. The structure was solved by Patterson method and refined by full matrix least-square methods using unit weights. The final R and S values were R=0.045, Rw=0.051, Rall=0.059 and S=2.171for 2248 observed reflections. The two carbon atoms of a ring of Ni(en)-ion were split into crossed four atoms. In consideration of α- and β-angles of two rings of a disordered ethylenediamine of Nien3-ion and the hydrogen bonds between Ni(en)3-cation and Cr2O7-anion, the configuration of Ni(en)3-ion is assumed to be disordered with Λδδδ and Λδδλ.

• Journal of the Korean Chemical Society
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• v.29 no.2
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• pp.73-79
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• 1985

The crystal and molecular structure of acetone 4-benzylthiosemicarbazone, $C_{11}H_{15}N_3S$, has been determined by the single crystal X-ray diffraction methods. The crystals are monoclinic, space group $P2_1/c$ with unit cell dimensions, a = 10.249(7), b = 11.403(9), c = 10.149(7)TEX>${\AA}$, ${\beta}$ = 90.9$(1)^0$ and z = 4. The intensities were collected on an automatic four-circle diffractometer with graphite-monochromated Mo-$K_{\alpha}$ radiation. The structure was solved by direct methods and refined by full matrix least-squares methods. The final R was 0.045 for 1554 observed reflections. S-C(8)-N(2)-N(3)-C(9)-C(10) atoms make a zigzag planar chain. There are no unusual bond lengths and angles. There are two independent hydrogen bonds in the crystal structure. One is N-H${\cdots}$S intermolecular hydrogen bond with the length of 3.555${\AA}$ and makes dimer-like units. The other is N-H${\cdots}$N intramolecular hydrogen bond with the length of 2.568${\AA}$. The structure was compared with those of other thiosemicarbazone derivatives.

• Journal of the Korean Chemical Society
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• v.38 no.11
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• pp.827-832
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• 1994

The crystal structure of bis(N-methylphenazinium) bis(oxalato)palladate(II) has been determined by X-ray crystallography. Crystal data: ((C_{13}H_{11}N_2)_2[Pd(C_2O_4)_2]) $M_w$ = 672.93, Triclinic, Space Group P1 (No = 2), a = 7.616(8), b = 9.842(3), c = $20.335(7)\AA$, $\alpha$ = 103.53(3), $\beta$ = 90.00(5), $\gamma$ = $112.38(5)^{\circ}$, Z = 2, $V = 1363(2){\AA}^3\;D_c = 1.639\;gcm^{-3},\;{\mu} = 7.3\;cm^{-1},\;F(000) = 680.0$. The intensity data were collected with $Mo-K\alpha$ radiation (${\lambda}$= 0.7107\;\AA)$ on an automatic four-circle diffractometer with a graphite monochromater. The structure was solved by Patterson method and refined by full matrix least-square methods using Killean & Lawrence weights. The final R and S values were $R = 0.069,\;R_w = 0.050,\;R_{all} = 0.069$ and S = 5.45 for 3120 observed reflections. Both cation and anion complexes are essentially planar and have dihedral angles of 6.3(6) and $57.06(6)^{\circ}$ between their planes. The planar complex anions are sandwiched between slightly bent cations. The interplanar separations of two triads are 3.328 and 3.463 $\AA$, respectively. The triads are stacked along b-axis, but their orientations are different based on dihedral angle $59.08(9)^{\circ}$ of two complex anions.

• Journal of the Korean Chemical Society
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• v.37 no.6
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• pp.599-603
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• 1993

Crystal structure of bis(1,2-diaminopropane)palladium(II) bis(oxalato)palladate(II) has been determined by X-ray crystallography. Crystal data: $Pd_2C_{10}H_{10}N_{4}O_{8}$, $M_W$ = 573.09, orthorhombic, space group $P_{ccn}$ (No = 56), a = 16.178(5), b = 16.381(6), c = 6.685(2)$\{AA}$, V = 1771.6 $\{AA}^3$, $M_W$W = 573.09, $D_c$ = 2.014 g${\cdot}c\;m^{-3}$, Z = 4, T = 294K, F(000) = 1056.0 and $\mu$ = 20.466 c$m^{-1}$. The intensity data were collected with $Mo-K\alpha$ radiation (${\lambda}$ = 0.7107 $\AA)$ on an automatic four-circle diffractometer with a graphite monochromater. The structure was solved by Patterson method and refined by full matrix least-squares methods using Pivot weights. The final R and S values were R = 0.065, $R_W = 0.059, R_{all}$ = 0.065 and S = 4.315 for 605 observed reflections. Both cation and anion complexes are essentially planar and have dihedral angle of $18(l)^{\circ}$ between thier planes. In the crystal structure, they do not have the Magnus's salt type mixed stacks; instead, the complex anions form regular stacks along the c-axis with the M-M bond length of $3.343(5)\AA$ and their stacks are surrounded by the complex cations through hydrogen bonds with the nitrogen-oxygen distances of 2.94(3) and $3.31(4)\AA.$

• Journal of the Korean Chemical Society
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• v.36 no.4
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• pp.536-539
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• 1992

Eight-membered ring spiro orthocarbonate (C$_{25}H_{20}O_4$, M$_r$ = 384) is monoclinic, space group C2/c, with a = 15.319(4), b = 9.057(3), c = 13.168(3)${\AA}$, ${\beta}$ = 98.53(3)$^{\circ}$, Z = 4, F(000) = 808, T = 290 K, ${\mu}$(Mo-K${\alpha}$) = 0.55 cm$_1$, D$_c$ = 1.36 g/cm$^3$ and D$_m$ = 1.40 g/cm$^3$. The intensity data were collected with Mo-K${\alpha}$ radiation (${\lambda}$ = 0.7107 ${\AA}$) on an automatic four-circle diffractometer with a graphite monochromater. The structure was solved by direct methods and refined by full matrix least-squares methods. The final R value was 0.052 for 1412 observed reflections. The molecule has C$_2$point symmetry. The eight-membered ring has a chair conformation with pseudo-C$_s$ symmetry. The naphthyl ring is planar with the C-C bond lengths being in the range of 1.352∼1.444${\AA}$ and bond angles of 117.2∼123.5$^{\circ}$. The bond lengths of C(1)-C(9), C(8)-C(9) and C(9)-C(10) are somewhat longer than those of the other C-C bonds.