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Acta Crystallogr Sect E Struct Rep Online. 2008 June 1; 64(Pt 6): m810–m811.
Published online 2008 May 14. doi:  10.1107/S1600536808013676
PMCID: PMC2961587

Poly[[diaqua­[μ4-4,4′-carbonyl­bis(benzene-1,2-dicarboxyl­ato)]bis­(dipyrido[3,2-a:2′,3′-c]phenazine)dicadmium(II)] monohydrate]

Abstract

In the title compound, {[Cd2(C17H6O9)(C18H10N4)2(H2O)2]·H2O}n, the CdII atom is seven-coordinated by five O atoms from two different 4,4′-carbonyl­bis(benzene-1,2-dicarboxyl­ate) (BPTC) anions and one water mol­ecule, and by two N atoms from one chelating dipyrido[3,2-a:2′,3′-c]phenazine (L) ligand in a distorted penta­gonal-bipyramidal geometry. The BPTC anions link the CdII atoms, forming a one-dimensional chain structure. The L ligands are attached on both sides of the chain. A twofold rotation axis passes through the complex molecule. The crystal structure involves O—H(...)O hydrogen bonds.

Related literature

For related literature, see: Li et al. (2007 [triangle]); Wu et al. (1997 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-0m810-scheme1.jpg

Experimental

Crystal data

  • [Cd2(C17H6O9)(C18H10N4)2(H2O)2]·H2O
  • M r = 1197.67
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-0m810-efi1.jpg
  • a = 15.698 (3) Å
  • b = 6.7028 (13) Å
  • c = 21.428 (4) Å
  • β = 102.45 (3)°
  • V = 2201.7 (8) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 1.05 mm−1
  • T = 293 (2) K
  • 0.27 × 0.24 × 0.21 mm

Data collection

  • Rigaku R-AXIS RAPID diffractometer
  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995 [triangle]) T min = 0.742, T max = 0.801
  • 20222 measured reflections
  • 5022 independent reflections
  • 3508 reflections with I > 2σ(I)
  • R int = 0.093

Refinement

  • R[F 2 > 2σ(F 2)] = 0.049
  • wR(F 2) = 0.125
  • S = 1.04
  • 5022 reflections
  • 352 parameters
  • 6 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 0.70 e Å−3
  • Δρmin = −0.84 e Å−3

Data collection: PROCESS-AUTO (Rigaku, 1998 [triangle]); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL-Plus (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXL97.

Table 1
Selected geometric parameters (Å, °)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808013676/rz2212sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808013676/rz2212Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by the Program for Young Academic Backbone in Heilongjiang Provincial University (No. 1152 G053) and Mudanjiang Medical University.

supplementary crystallographic information

Comment

Dipyrido[3,2-a:2',3'-c]phenazine (L) has been widely used to recognize the secondary structure of DNA in rutenium(II) complexes (Wu et al., 1997). Recently, the L ligand has received intense interest in the chemistry of coordination polymers (Li et al., 2007). In the present paper, we selected H4BPTC = 3,3',4,4'-benzophenone tetracarboxylic acid as a bridging ligand and L as a chelating ligand, generating a new cadmium(II) coordination polymer, [Cd2(L)2(BPTC)(H2O)2].2H2O.

Selected bond lengths and angles for the title compound are given in Table 1. Each CdII atom is seven-coordinated by five O atoms from two different BPTC anions and one water molecule, and two N atoms from one chelating L ligand in a distorted pentagonal bipyramidal coordination geometry (Fig. 1). The BPTC anions link the CdII atoms to form a one-dimensional chain structure (Fig. 2). The L ligands are attached on both sides of the chain. Intermolecular O—H···O H-bonds (Table 2) and the π–π interactions (between L ligands of neighboring chains, with the shortest atom-to-atom distance of 3.43 (2) Å) stabilize the crystal structure.

Experimental

Dipyrido[3,2 - a:2',3'-c]-phenazine (0.5 mmol) and 3,3',4,4'-benzophenone tetracarboxylic acid (0.25 mmol) were mixed with an aqueous solution (12 ml) of cadmium chloride dihydrate (0.5 mmol) with stirring. The solution was heated in a 25 ml Teflon-lined reaction vessel at 390 K for 120 h and then cooled to room temperature over a period of 16 h. Colourless crystals of the title compound were collected.

Refinement

All H atoms on C atoms were positioned geometrically (C—H = 0.93 Å) and refined as riding, with Uiso(H) = 1.2Ueq(C). The water H atoms were located in a difference Fourier map and refined with a distance restraint of O–H = 0.85 Å, and with Uiso(H) = 1.2Ueq(O).

Figures

Fig. 1.
The structure of the title compound , showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. Symmetry codes: (i) x, y - 1, z; (ii) 0.5 - x, y, 0.5 - z.
Fig. 2.
View of the chain structure of the title compound.

Crystal data

[Cd2(C17H6O9)(C18H10N4)2(H2O1)2]·H2OF000 = 1196
Mr = 1197.67Dx = 1.807 Mg m3
Monoclinic, P2/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2yacCell parameters from 13844 reflections
a = 15.698 (3) Åθ = 3.0–27.5º
b = 6.7028 (13) ŵ = 1.05 mm1
c = 21.428 (4) ÅT = 293 (2) K
β = 102.45 (3)ºBlock, colourless
V = 2201.7 (8) Å30.27 × 0.24 × 0.21 mm
Z = 2

Data collection

Rigaku R-AXIS RAPID diffractometer5022 independent reflections
Radiation source: rotating anode3508 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.093
Detector resolution: 10.0 pixels mm-1θmax = 27.5º
T = 293(2) Kθmin = 3.0º
ω scansh = −20→18
Absorption correction: multi-scan(ABSCOR; Higashi, 1995)k = −8→8
Tmin = 0.742, Tmax = 0.801l = −27→27
20222 measured reflections

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.049H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.125  w = 1/[σ2(Fo2) + (0.0614P)2] where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
5022 reflectionsΔρmax = 0.70 e Å3
352 parametersΔρmin = −0.84 e Å3
6 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/UeqOcc. (<1)
C10.7768 (4)0.0149 (8)0.1740 (2)0.0342 (12)
H10.7343−0.06380.18610.041*
C20.8642 (3)−0.0462 (8)0.1917 (3)0.0377 (13)
H20.8794−0.15970.21660.045*
C30.9266 (4)0.0645 (8)0.1717 (3)0.0367 (12)
H30.98480.02550.18190.044*
C40.9015 (3)0.2375 (7)0.1356 (2)0.0286 (11)
C50.8145 (3)0.2937 (7)0.1223 (2)0.0261 (10)
C60.9661 (3)0.3643 (8)0.1135 (2)0.0319 (11)
C70.9401 (4)0.5492 (8)0.0840 (2)0.0339 (12)
C80.8467 (4)0.6054 (7)0.0703 (2)0.0316 (12)
C90.7859 (3)0.4772 (7)0.0878 (2)0.0281 (11)
C100.6728 (4)0.6892 (8)0.0431 (3)0.0423 (14)
H100.61340.71740.03280.051*
C110.8165 (4)0.7825 (8)0.0393 (3)0.0398 (13)
H110.85590.87160.02790.048*
C120.7312 (4)0.8258 (8)0.0259 (3)0.0502 (17)
H120.71120.94460.00550.060*
C131.0803 (4)0.6155 (10)0.0777 (3)0.0455 (15)
C141.1439 (5)0.7468 (10)0.0625 (3)0.0604 (19)
H141.12800.87370.04660.072*
C151.2290 (5)0.6847 (13)0.0715 (3)0.068 (2)
H151.27080.77070.06180.082*
C161.2537 (4)0.4954 (12)0.0950 (3)0.0566 (19)
H161.31160.45620.09980.068*
C171.1943 (4)0.3640 (12)0.1113 (3)0.0550 (17)
H171.21190.23830.12750.066*
C181.1052 (4)0.4256 (9)0.1028 (3)0.0395 (13)
C190.5216 (3)0.5601 (7)0.1603 (3)0.0300 (11)
C200.4599 (3)0.6828 (7)0.1904 (2)0.0250 (10)
C210.4935 (3)1.0024 (7)0.1355 (2)0.0298 (11)
C220.4394 (3)0.8792 (7)0.1726 (2)0.0228 (10)
C230.3716 (3)0.9765 (7)0.1933 (2)0.0264 (10)
H230.35851.10840.18170.032*
C240.3230 (3)0.8755 (7)0.2318 (2)0.0270 (11)
C250.3484 (3)0.6844 (7)0.2525 (2)0.0320 (12)
H250.32010.61920.28050.038*
C260.4164 (3)0.5886 (7)0.2315 (2)0.0311 (11)
H260.43240.45980.24540.037*
C270.25000.9870 (11)0.25000.0338 (17)
N10.7518 (3)0.1804 (6)0.1405 (2)0.0292 (9)
N20.6995 (3)0.5206 (6)0.0737 (2)0.0333 (10)
N30.9946 (3)0.6766 (7)0.0669 (2)0.0419 (11)
N41.0483 (3)0.2994 (7)0.1226 (2)0.0385 (11)
O10.5763 (2)0.4504 (5)0.19432 (18)0.0386 (9)
O20.5089 (2)0.5605 (5)0.09996 (17)0.0338 (8)
O1W0.5801 (3)0.2021 (6)−0.00419 (19)0.0457 (10)
HW110.563 (4)0.287 (6)−0.033 (2)0.055*
HW120.553 (3)0.096 (5)−0.016 (3)0.055*
O30.5736 (2)0.9818 (6)0.1491 (2)0.0443 (10)
O40.25001.1681 (8)0.25000.0448 (15)
O2W0.7500−0.3982 (12)0.25000.082 (2)
HW220.708 (7)−0.479 (19)0.240 (8)0.099*0.50
HW210.764 (14)−0.40 (2)0.2906 (11)0.099*0.50
O50.4540 (3)1.1233 (6)0.0948 (2)0.0506 (11)
Cd10.60585 (2)0.27952 (5)0.103914 (18)0.02753 (13)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
C10.034 (3)0.038 (3)0.032 (3)−0.002 (2)0.010 (3)0.007 (2)
C20.033 (3)0.039 (3)0.040 (3)0.003 (2)0.006 (3)0.013 (2)
C30.029 (3)0.043 (3)0.035 (3)0.001 (2)0.001 (3)0.005 (2)
C40.028 (3)0.031 (3)0.028 (2)−0.001 (2)0.008 (2)−0.004 (2)
C50.025 (2)0.030 (2)0.026 (2)0.000 (2)0.011 (2)0.002 (2)
C60.024 (3)0.043 (3)0.030 (3)−0.009 (2)0.009 (2)0.000 (2)
C70.035 (3)0.037 (3)0.032 (3)−0.012 (2)0.013 (3)−0.005 (2)
C80.036 (3)0.031 (3)0.031 (3)−0.009 (2)0.014 (3)0.000 (2)
C90.030 (3)0.025 (2)0.031 (3)−0.003 (2)0.010 (2)0.000 (2)
C100.036 (3)0.038 (3)0.058 (4)0.010 (2)0.020 (3)0.011 (3)
C110.046 (3)0.030 (3)0.046 (3)−0.003 (2)0.016 (3)0.005 (2)
C120.063 (4)0.028 (3)0.065 (4)0.008 (3)0.026 (4)0.018 (3)
C130.034 (3)0.066 (4)0.036 (3)−0.023 (3)0.008 (3)−0.008 (3)
C140.051 (4)0.073 (5)0.061 (4)−0.024 (4)0.021 (4)0.009 (3)
C150.041 (4)0.110 (6)0.056 (4)−0.039 (4)0.018 (4)−0.002 (4)
C160.023 (3)0.108 (6)0.042 (4)−0.019 (3)0.013 (3)−0.011 (4)
C170.033 (3)0.095 (5)0.038 (3)−0.007 (3)0.008 (3)−0.001 (3)
C180.024 (3)0.065 (4)0.030 (3)−0.010 (3)0.008 (2)−0.003 (3)
C190.027 (3)0.027 (2)0.040 (3)0.002 (2)0.015 (3)0.002 (2)
C200.015 (2)0.032 (3)0.029 (2)−0.0024 (18)0.005 (2)0.001 (2)
C210.033 (3)0.028 (3)0.031 (3)−0.005 (2)0.013 (2)−0.004 (2)
C220.014 (2)0.029 (2)0.025 (2)−0.0026 (18)0.004 (2)0.0002 (19)
C230.023 (3)0.028 (2)0.030 (3)−0.0025 (19)0.009 (2)0.002 (2)
C240.020 (2)0.033 (3)0.031 (3)−0.004 (2)0.013 (2)−0.002 (2)
C250.032 (3)0.033 (3)0.035 (3)−0.005 (2)0.015 (2)0.004 (2)
C260.027 (3)0.030 (2)0.036 (3)0.002 (2)0.007 (2)0.005 (2)
C270.036 (4)0.038 (4)0.030 (4)0.0000.015 (4)0.000
N10.023 (2)0.031 (2)0.035 (2)−0.0024 (17)0.0090 (19)0.0029 (18)
N20.029 (2)0.032 (2)0.043 (3)0.0060 (18)0.016 (2)0.0032 (19)
N30.034 (3)0.048 (3)0.044 (3)−0.016 (2)0.010 (2)0.000 (2)
N40.029 (2)0.052 (3)0.034 (2)−0.007 (2)0.007 (2)0.000 (2)
O10.029 (2)0.043 (2)0.044 (2)0.0123 (17)0.0088 (19)0.0045 (18)
O20.038 (2)0.0322 (18)0.035 (2)0.0063 (16)0.0155 (18)0.0007 (15)
O1W0.058 (3)0.042 (2)0.033 (2)0.011 (2)0.002 (2)0.0042 (18)
O30.022 (2)0.049 (2)0.066 (3)−0.0033 (17)0.020 (2)0.006 (2)
O40.051 (4)0.032 (3)0.062 (4)0.0000.035 (3)0.000
O2W0.057 (6)0.059 (5)0.119 (7)0.000−0.007 (5)0.000
O50.049 (3)0.048 (2)0.058 (3)−0.003 (2)0.018 (2)0.023 (2)
Cd10.02447 (19)0.02697 (19)0.0338 (2)0.00214 (15)0.01220 (15)0.00352 (16)

Geometric parameters (Å, °)

C1—N11.333 (6)C17—H170.9300
C1—C21.403 (7)C18—N41.363 (7)
C1—H10.9300C19—O11.240 (6)
C2—C31.370 (7)C19—O21.265 (6)
C2—H20.9300C19—C201.517 (6)
C3—C41.401 (7)C19—Cd12.727 (5)
C3—H30.9300C20—C261.378 (6)
C4—C51.386 (7)C20—C221.389 (6)
C4—C61.478 (6)C21—O31.236 (6)
C5—N11.365 (6)C21—O51.252 (6)
C5—C91.455 (7)C21—C221.526 (6)
C6—N41.335 (7)C21—Cd1i2.744 (5)
C6—C71.411 (7)C22—C231.399 (6)
C7—N31.316 (6)C23—C241.411 (6)
C7—C81.480 (7)C23—H230.9300
C8—C111.392 (7)C24—C251.385 (7)
C8—C91.395 (6)C24—C271.489 (6)
C9—N21.356 (6)C25—C261.400 (6)
C10—N21.328 (6)C25—H250.9300
C10—C121.402 (8)C26—H260.9300
C10—H100.9300C27—O41.214 (9)
C11—C121.339 (9)C27—C24ii1.489 (6)
C11—H110.9300Cd1—N12.352 (4)
C12—H120.9300Cd1—N22.367 (4)
C13—N31.376 (8)Cd1—O12.381 (4)
C13—C181.405 (9)Cd1—O22.411 (3)
C13—C141.420 (8)Cd1—O1W2.323 (4)
C14—C151.374 (10)O1W—HW110.84 (4)
C14—H140.9300O1W—HW120.84 (4)
C15—C161.389 (10)O2W—HW220.85 (2)
C15—H150.9300O2W—HW210.85 (2)
C16—C171.381 (8)Cd1—O3iii2.321 (4)
C16—H160.9300Cd1—O5iii2.572 (4)
C17—C181.432 (8)
N1—C1—C2123.1 (5)C22—C20—C19121.9 (4)
N1—C1—H1118.5O3—C21—O5124.2 (5)
C2—C1—H1118.5O3—C21—C22117.9 (5)
C3—C2—C1118.7 (5)O5—C21—C22117.8 (5)
C3—C2—H2120.6O3—C21—Cd1i57.2 (3)
C1—C2—H2120.6O5—C21—Cd1i68.8 (3)
C2—C3—C4119.0 (5)C22—C21—Cd1i162.6 (3)
C2—C3—H3120.5C20—C22—C23120.1 (4)
C4—C3—H3120.5C20—C22—C21122.3 (4)
C5—C4—C3119.1 (4)C23—C22—C21117.4 (4)
C5—C4—C6119.4 (4)C22—C23—C24120.4 (4)
C3—C4—C6121.5 (5)C22—C23—H23119.8
N1—C5—C4121.9 (4)C24—C23—H23119.8
N1—C5—C9117.0 (4)C25—C24—C23118.4 (4)
C4—C5—C9121.1 (4)C25—C24—C27124.4 (4)
N4—C6—C7122.0 (4)C23—C24—C27117.1 (4)
N4—C6—C4118.2 (5)C24—C25—C26120.5 (4)
C7—C6—C4119.8 (4)C24—C25—H25119.7
N3—C7—C6123.5 (5)C26—C25—H25119.7
N3—C7—C8117.1 (5)C20—C26—C25120.8 (5)
C6—C7—C8119.4 (4)C20—C26—H26119.6
C11—C8—C9118.1 (5)C25—C26—H26119.6
C11—C8—C7122.2 (4)O4—C27—C24ii120.1 (3)
C9—C8—C7119.7 (5)O4—C27—C24120.1 (3)
N2—C9—C8121.2 (5)C24ii—C27—C24119.7 (6)
N2—C9—C5118.5 (4)C1—N1—C5118.1 (4)
C8—C9—C5120.2 (5)C1—N1—Cd1124.5 (3)
N2—C10—C12122.1 (5)C5—N1—Cd1117.2 (3)
N2—C10—H10119.0C10—N2—C9119.1 (4)
C12—C10—H10119.0C10—N2—Cd1124.5 (4)
C12—C11—C8120.6 (5)C9—N2—Cd1116.3 (3)
C12—C11—H11119.7C7—N3—C13115.5 (5)
C8—C11—H11119.7C6—N4—C18115.4 (5)
C11—C12—C10118.9 (5)C19—O1—Cd192.2 (3)
C11—C12—H12120.6C19—O2—Cd190.2 (3)
C10—C12—H12120.6Cd1—O1W—HW11123 (4)
N3—C13—C18121.0 (5)Cd1—O1W—HW12117 (4)
N3—C13—C14119.1 (6)HW11—O1W—HW12107 (3)
C18—C13—C14119.9 (6)C21—O3—Cd1i96.2 (3)
C15—C14—C13119.4 (7)HW22—O2W—HW21105 (3)
C15—C14—H14120.3C21—O5—Cd1i84.2 (3)
C13—C14—H14120.3O3iii—Cd1—O1W102.56 (15)
C14—C15—C16121.0 (6)O3iii—Cd1—N184.39 (13)
C14—C15—H15119.5O1W—Cd1—N1102.54 (15)
C16—C15—H15119.5O3iii—Cd1—N2154.84 (14)
C17—C16—C15121.6 (6)O1W—Cd1—N282.23 (16)
C17—C16—H16119.2N1—Cd1—N270.49 (14)
C15—C16—H16119.2O3iii—Cd1—O188.62 (13)
C16—C17—C18118.6 (7)O1W—Cd1—O1153.69 (14)
C16—C17—H17120.7N1—Cd1—O1102.20 (14)
C18—C17—H17120.7N2—Cd1—O197.78 (14)
N4—C18—C13122.3 (5)O3iii—Cd1—O2119.58 (12)
N4—C18—C17118.0 (6)O1W—Cd1—O299.59 (13)
C13—C18—C17119.6 (5)N1—Cd1—O2142.59 (13)
O1—C19—O2122.6 (4)N2—Cd1—O283.19 (13)
O1—C19—C20119.8 (5)O1—Cd1—O254.58 (12)
O2—C19—C20117.3 (4)O3iii—Cd1—O5iii53.13 (13)
O1—C19—Cd160.7 (3)O1W—Cd1—O5iii82.76 (15)
O2—C19—Cd162.2 (2)N1—Cd1—O5iii136.94 (13)
C20—C19—Cd1167.9 (3)N2—Cd1—O5iii151.32 (14)
C26—C20—C22119.5 (4)O1—Cd1—O5iii85.29 (13)
C26—C20—C19118.2 (4)O2—Cd1—O5iii75.40 (12)

Symmetry codes: (i) x, y+1, z; (ii) −x+1/2, y, −z+1/2; (iii) x, y−1, z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O1W—HW11···O2iv0.84 (4)1.92 (3)2.731 (5)163 (6)
O1W—HW12···O5iv0.84 (4)2.23 (4)2.892 (6)136 (5)
O2W—HW22···O1iii0.85 (2)2.14 (8)2.913 (5)152 (15)

Symmetry codes: (iv) −x+1, −y+1, −z; (iii) x, y−1, z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: RZ2212).

References

  • Higashi, T. (1995). ABSCOR Rigaku Corporation, Tokyo, Japan.
  • Li, C.-B., Fang, W., Dong, E.-J., Liu, B. & Li, Y.-W. (2007). Acta Cryst. E63, m150–m152.
  • Rigaku (1998). PROCESS-AUTO Rigaku Corporation, Tokyo, Japan.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Wu, J.-Z., Li, L., Zeng, T.-X., Ji, L.-N., Zhou, J.-Y., Luo, T. & Li, R.-H. (1997). Polyhedron, 16, 103–107.

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