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Acta Cryst. (2007). E63, m3013-m3014    [ doi:10.1107/S1600536807056371 ]

Poly[[bis[[mu]2-1,3-bis(phenylsulfanyl)propane-[kappa]2S:S']silver(I)] hexafluoridoantimonate diethyl ether hemisolvate\]

M. O. Awaleh, A. Badia and F. Brisse

Abstract top

The title compound, {[Ag(C15H16S2)2]SbF6·0.5C4H10O}n, was obtained from the self-assembly of AgSbF6 and 1,3-bis(phenylsulfanyl)propane. Each AgI ion is coordinated by four S atoms from different ligands, forming a distorted tethrahedral geometry. Each ligand links adjacent AgI ions, forming an extended two-dimensional grid-like framework. SbF6- ions, which are incorporated into the cavities of the network, complete and stabilize the structure. One of the phenyl rings is disordered over two sites, the ratio of occupancies being 0.508 (4):0.492 (4).

Comment top

The self-assembly of metal-organic coordination polymers has attracted a great attention because of their potential as functional materials (Millward & Yaghi, 2005; Wong-Foy et al., 2006). When flexible ligands are involved in supramolecular architectures, the prediction of the topology of the coordination polymer is more difficult because there are several factors affecting the framework formation, such as the type of solvent, the counter-anion, and the metal-to-ligand ratio among others (Withersby et al., 1999, 1997; Noro et al., 2002; Black et al., 1995; Blake et al., 1999; Bu et al., 2002; Carlucci et al., 2002). Neverthless, in order to gain more information about those subtle factors, not yet well understood, we have studied the effect of one parameter at a time on the topology of the networks (Awaleh et al., 2006a,b; 2007). In our continuous effort to study the structure of the metal-organic supramolecular architecture, we report herein a silver(I) coordination polymer forming a lamellar network by using a flexible dithioether, viz. 1,3-bis(phenylsulfanyl)propane (L3-Ph), as building block, namely Poly[Silver(I)-di-µ-1,3-bis(phenylsulfanyl)propane]hexafluoroantimonate acetone solvate (I). In the title complex (I), each AgI center is linked in a tetrahedral manner to a sulfur atom of four different L3-Ph ligands (Fig. 1). The other sulfur atom of each ligand is bound to a neighbouring AgI ion thus forming a two-dimensional cationic coordination polymer where the repeat unit is a rectangular 24-membered macrometallocycle Ag4(L3-Ph)4 (Fig. 2). The phenyl groups of the L3-Ph ligands are located on the same side of the Ag4 plane. The dihedral angle between the phenyl groups is 71.6(20°. The PF6− ions are incorporated in the cavities of the repeating unit to balance the charge of the cationic coordination polymer (Fig. 3). Neighbouring rectangular rings are fused in a parquet-like pattern to form an infinite lamellar (4,4) coordination network (Fig. 3).

Related literature top

For related literature, see: Awaleh et al. (2006a, 2006b, 2007); Black et al. (1995); Blake et al. (1999); Bu et al. (2002); Carlucci et al. (2002); Hartley et al. (1979); Hou et al. (2005); Millward & Yaghi (2005); Noro et al. (2002); Sluis & Spek (1990); Spek (2003); Withersby et al. (1997, 1999); Wong-Foy, Matzger & Yaghi (2006).

Experimental top

The ligand 1,3-bis(phenylsulfanyl)propane, L3-Ph, was synthesized following a publish report (Hartley et al., 1979). For the synthesis of the title compound (I), a solution of AgSbF6 (164 mg, 0.48 mmol) in acetone (5 ml) was added a solution of L3-Ph (0.22 ml, 0.95 mmol) in diethyl ether (5 ml). The mixture was kept under reflux at 323 K for 2 h. The filtrate was recrystallized by diffusion of petroleum ether into the solution at room temperature. A few days later, single crystals suitable for X-ray analysis were deposited. Yield 74% based on AgSbF6. Anal. Found: C, 42.46; H, 3.84. Calculated for C32H37S4O0.5AgSbF6: C, 42.63; H, 4.14. 1H NMR (DMSO-d6, 400 MHz): d 1.84 (qt, 2H, –S-(CH2)-(CH2)-), 3.07 (t, 4H, –S-(CH2)-), 7.28–7.59 (m, 10H, C6H5–). 19F NMR (DMSO-d6, 376.31 MHz): d −137.49 - −102.91 (m, F—Sb).

Refinement top

All non-H atoms were refined by full-matrix least-squares with anisotropic displacement parameters. H atoms were generated geometrically (C—H distances of 0.93 A for aromatic H, 0.97 A for the other) and were included in the refinement in the riding model approximation; their temperature factors were set to 1.2 times those of the equivalent isotropic temperature factors of the parent site. An electron density map showed two regions centered at (1/2, 0, 0) and (1/2, 1/2, 1/2), containing peaks due to severely disordered solvent. No consistent models for diethyl ether molecules, which was the only solvent present, could be assembled from these peaks. This part of the structure was modeled by using the SQUEEZE procedure of PLATON (Spek, 2003), which indicated the presence of two cavities of 205 Å3, each occupied by 40 electrons, which is consistent with the presence of one CH3CH2OCH2CH3 molecule per cavity (half of diethyl ether molecule per asymmetric unit)·The contribution of the disordered solvent was calculated with BYPASS (van der Sluis & Spek, 1990) and a new data set without the solvent contribution was generated. The final model consisting of the ordered part only was refined. One phenyl group of one 1,3-bis(phenylsulfanul)propane ligand was found to be disordered·This group was split over two sites with occupancies of 58 and 42%.

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: UdMX (local program; Maris, 2004).

Figures top
[Figure 1] Fig. 1. The aysmmetric unit of the title compound. Ellipsoid are drawn at the 30% probability level. The disordered components are labeled with suffixes A and B.
[Figure 2] Fig. 2. View of the 24-membered Ag4(L3-Ph)4 macrometallocyclic repeat unit of the title compound.
[Figure 3] Fig. 3. View of the two-dimensional molecular-rectangle network of the title compound.
Poly[[bis[µ2-1,3-bis(phenylsulfanyl)propane-κ2S:S']silver(I)] hexafluoridoantimonate diethyl ether hemisolvate] top
Crystal data top
[Ag(C15H16S2)2]SbF6·0.5C4H10OF000 = 1712
Mr = 901.52Dx = 1.657 Mg m−3
Monoclinic, P21/cCu Kα radiation
λ = 1.54178 Å
Hall symbol: -P 2ybcCell parameters from 7995 reflections
a = 13.5794 (2) Åθ = 3.3–72.8º
b = 13.0497 (2) ŵ = 12.87 mm−1
c = 20.5848 (3) ÅT = 220 (2) K
β = 97.7910 (10)ºBlock, colorless
V = 3614.10 (9) Å30.27 × 0.14 × 0.11 mm
Z = 4
Data collection top
Bruker SMART 2K
diffractometer		7095 independent reflections
Radiation source: X-ray Sealed Tube5413 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.049
Detector resolution: 5.5 pixels mm-1θmax = 72.9º
T = 220(2) Kθmin = 3.3º
ω scansh = −16→16
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		k = −13→15
Tmin = 0.162, Tmax = 0.239l = −25→25
43960 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.044H-atom parameters constrained
wR(F2) = 0.114  w = 1/[σ2(Fo2) + (0.0718P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.95(Δ/σ)max = 0.001
7095 reflectionsΔρmax = 1.07 e Å−3
375 parametersΔρmin = −0.92 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[Ag(C15H16S2)2]SbF6·0.5C4H10OV = 3614.10 (9) Å3
Mr = 901.52Z = 4
Monoclinic, P21/cCu Kα
a = 13.5794 (2) ŵ = 12.87 mm−1
b = 13.0497 (2) ÅT = 220 (2) K
c = 20.5848 (3) Å0.27 × 0.14 × 0.11 mm
β = 97.7910 (10)º
Data collection top
Bruker SMART 2K
diffractometer		7095 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		5413 reflections with I > 2σ(I)
Tmin = 0.162, Tmax = 0.239Rint = 0.049
43960 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.044375 parameters
wR(F2) = 0.114H-atom parameters constrained
S = 0.95Δρmax = 1.07 e Å−3
7095 reflectionsΔρmin = −0.92 e Å−3
Special details top

Experimental. X-ray crystallographic data for I were collected from a single-crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 2 K Charged-Coupled Device (CCD) Area Detector using the program SMART and normal focus sealed tube source graphite monochromated Cu—Kα radiation. The crystal-to-detector distance was 4.908 cm, and the data collection was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning. The initial unit-cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 9.0 degree scan in 30 frames over four different parts of the reciprocal space (120 frames total). One complete sphere of data was collected, to better than 0.8Å resolution. Upon completion of the data collection, the first 101 frames were recollected in order to improve the decay correction analysis.

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) top
xyzUiso*/UeqOcc. (<1)
Ag10.25367 (2)0.61376 (3)0.245888 (17)0.02260 (10)
Sb10.22596 (3)0.08152 (3)0.166843 (17)0.03613 (11)
S10.21540 (8)0.77327 (9)0.31534 (6)0.0215 (2)
S20.34586 (8)0.48708 (9)0.32496 (6)0.0252 (3)
S30.08207 (8)0.56386 (9)0.18682 (6)0.0227 (2)
S40.35897 (8)0.69189 (9)0.16407 (6)0.0247 (3)
F10.1398 (3)0.1928 (3)0.1844 (2)0.0678 (12)
F20.3345 (3)0.1719 (4)0.1855 (2)0.0820 (15)
F30.3054 (3)−0.0257 (4)0.1523 (2)0.0916 (17)
F40.1130 (3)−0.0011 (3)0.15182 (17)0.0519 (9)
F50.2087 (3)0.1186 (4)0.07860 (18)0.0787 (15)
F60.2400 (3)0.0490 (3)0.25589 (16)0.0488 (9)
C110.1783 (3)0.7220 (4)0.3894 (2)0.0218 (10)
C120.0832 (4)0.6887 (4)0.3940 (2)0.0291 (11)
H120.03430.69270.35780.035*
C130.0607 (4)0.6496 (4)0.4522 (3)0.0368 (13)
H13−0.00390.62850.45550.044*
C140.1326 (5)0.6415 (4)0.5055 (3)0.0444 (15)
H140.11720.61400.54450.053*
C150.2281 (5)0.6742 (4)0.5010 (3)0.0394 (14)
H150.27690.66870.53720.047*
C160.2515 (4)0.7153 (4)0.4431 (3)0.0330 (12)
H160.31570.73820.44020.040*
C170.1015 (4)0.8260 (4)0.2720 (2)0.0251 (10)
H17A0.11350.84920.22900.030*
H17B0.05130.77260.26590.030*
C180.0624 (3)0.9153 (4)0.3087 (2)0.0231 (10)
H18A0.11100.97010.31350.028*
H18B0.05180.89310.35230.028*
C210.2527 (3)0.4021 (4)0.3470 (2)0.0244 (10)
C220.2337 (4)0.3056 (4)0.3204 (3)0.0284 (11)
H220.27140.27990.28960.034*
C230.1570 (4)0.2476 (4)0.3405 (3)0.0317 (12)
H230.14380.18240.32330.038*
C240.1006 (4)0.2860 (4)0.3857 (3)0.0339 (12)
H240.04880.24720.39830.041*
C250.1208 (4)0.3818 (5)0.4123 (3)0.0394 (14)
H250.08290.40730.44310.047*
C260.1969 (4)0.4401 (4)0.3935 (3)0.0318 (12)
H260.21080.50440.41190.038*
C270.4222 (4)0.4080 (4)0.2802 (3)0.0278 (11)
H27A0.37970.36800.24800.033*
H27B0.46320.45170.25670.033*
C280.4891 (4)0.3357 (4)0.3247 (2)0.0270 (11)
H28A0.53090.37520.35750.032*
H28B0.44850.29010.34710.032*
C310.1094 (3)0.5131 (4)0.1110 (2)0.0211 (10)
C320.1117 (4)0.5836 (4)0.0602 (2)0.0277 (11)
H320.09790.65230.06680.033*
C330.1343 (4)0.5510 (4)0.0005 (3)0.0329 (12)
H330.13680.5982−0.03310.040*
C340.1534 (4)0.4484 (4)−0.0101 (3)0.0377 (14)
H340.16810.4267−0.05070.045*
C350.1503 (4)0.3783 (4)0.0401 (3)0.0373 (13)
H350.16290.30940.03300.045*
C360.1286 (4)0.4100 (4)0.1007 (3)0.0290 (11)
H360.12680.36270.13440.035*
C370.0354 (3)0.4546 (4)0.2285 (2)0.0243 (10)
H37A0.08440.40010.23210.029*
H37B0.02510.47460.27240.029*
C41A0.4293 (6)0.5788 (5)0.1447 (4)0.025 (2)0.508 (4)
C42A0.3748 (4)0.4987 (6)0.1131 (4)0.0391 (19)0.508 (4)
H42A0.30680.50570.10070.047*0.508 (4)
C43A0.4222 (5)0.4079 (5)0.1002 (4)0.052 (3)0.508 (4)
H43A0.38570.35430.07910.062*0.508 (4)
C44A0.5239 (5)0.3973 (5)0.1188 (4)0.044 (2)0.508 (4)
H44A0.55560.33660.11020.053*0.508 (4)
C45A0.5784 (4)0.4775 (7)0.1504 (4)0.035 (3)0.508 (4)
H45A0.64650.47040.16280.042*0.508 (4)
C46A0.5311 (6)0.5682 (6)0.1633 (4)0.0285 (12)0.508 (4)
H46A0.56750.62180.18440.034*0.508 (4)
C41B0.4365 (7)0.6062 (6)0.1305 (4)0.025 (2)0.492 (4)
C42B0.3977 (5)0.5663 (6)0.0698 (4)0.0391 (19)0.492 (4)
H42B0.33470.58590.05020.047*0.492 (4)
C43B0.4529 (6)0.4970 (7)0.0383 (3)0.052 (3)0.492 (4)
H43B0.42700.4703−0.00230.062*0.492 (4)
C44B0.5470 (5)0.4676 (6)0.0676 (4)0.044 (2)0.492 (4)
H44B0.58400.42130.04650.053*0.492 (4)
C45B0.5858 (5)0.5075 (7)0.1283 (4)0.035 (3)0.492 (4)
H45B0.64870.48790.14790.042*0.492 (4)
C46B0.5305 (7)0.5768 (7)0.1598 (3)0.0285 (12)0.492 (4)
H46B0.55650.60360.20040.034*0.492 (4)
C470.4461 (3)0.7731 (4)0.2149 (2)0.0264 (11)
H47A0.40940.81920.23980.032*
H47B0.48820.73070.24580.032*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.01757 (16)0.02028 (19)0.0306 (2)−0.00137 (12)0.00575 (13)−0.00095 (13)
Sb10.0370 (2)0.0407 (2)0.0296 (2)−0.00904 (16)0.00059 (15)0.00587 (15)
S10.0170 (5)0.0194 (6)0.0280 (6)0.0012 (4)0.0021 (4)−0.0011 (4)
S20.0197 (6)0.0202 (6)0.0369 (7)0.0017 (4)0.0081 (5)0.0011 (5)
S30.0186 (5)0.0191 (6)0.0307 (6)−0.0026 (4)0.0046 (5)−0.0005 (4)
S40.0158 (5)0.0276 (7)0.0305 (6)−0.0043 (4)0.0028 (5)0.0039 (5)
F10.079 (3)0.044 (2)0.072 (3)0.024 (2)−0.020 (2)−0.0084 (19)
F20.069 (3)0.106 (4)0.067 (3)−0.053 (3)−0.006 (2)0.015 (3)
F30.081 (3)0.109 (4)0.084 (3)0.059 (3)0.005 (3)−0.019 (3)
F40.044 (2)0.057 (2)0.052 (2)−0.0191 (18)−0.0046 (17)0.0042 (17)
F50.078 (3)0.118 (4)0.037 (2)−0.032 (3)−0.003 (2)0.025 (2)
F60.056 (2)0.050 (2)0.038 (2)−0.0002 (17)−0.0038 (17)0.0128 (15)
C110.024 (2)0.018 (3)0.023 (2)0.0038 (18)0.0019 (19)−0.0032 (18)
C120.032 (3)0.026 (3)0.029 (3)0.003 (2)0.006 (2)0.003 (2)
C130.039 (3)0.038 (3)0.037 (3)0.007 (2)0.017 (3)0.003 (2)
C140.072 (5)0.032 (3)0.032 (3)0.010 (3)0.016 (3)−0.001 (2)
C150.059 (4)0.032 (3)0.023 (3)0.007 (3)−0.009 (3)−0.004 (2)
C160.039 (3)0.024 (3)0.033 (3)0.001 (2)−0.006 (2)−0.004 (2)
C170.026 (3)0.024 (3)0.025 (3)0.0081 (19)0.003 (2)−0.0015 (19)
C180.017 (2)0.022 (3)0.029 (3)0.0027 (18)0.0012 (19)−0.0025 (19)
C210.021 (2)0.021 (3)0.031 (3)0.0000 (18)0.004 (2)0.0051 (19)
C220.023 (2)0.027 (3)0.036 (3)0.003 (2)0.004 (2)−0.001 (2)
C230.029 (3)0.020 (3)0.043 (3)−0.004 (2)−0.003 (2)0.003 (2)
C240.031 (3)0.025 (3)0.046 (3)−0.008 (2)0.006 (2)0.007 (2)
C250.042 (3)0.044 (4)0.036 (3)−0.005 (3)0.019 (3)0.000 (3)
C260.039 (3)0.020 (3)0.039 (3)−0.001 (2)0.013 (2)−0.001 (2)
C270.025 (3)0.028 (3)0.032 (3)0.002 (2)0.012 (2)0.002 (2)
C280.021 (2)0.028 (3)0.032 (3)0.0011 (19)0.006 (2)0.000 (2)
C310.014 (2)0.020 (3)0.028 (3)−0.0007 (17)0.0016 (18)0.0035 (18)
C320.023 (2)0.028 (3)0.031 (3)−0.0026 (19)−0.001 (2)0.008 (2)
C330.034 (3)0.035 (3)0.029 (3)−0.012 (2)0.000 (2)0.009 (2)
C340.039 (3)0.042 (4)0.033 (3)−0.019 (3)0.009 (3)−0.006 (2)
C350.045 (3)0.025 (3)0.042 (3)0.002 (2)0.009 (3)−0.003 (2)
C360.031 (3)0.020 (3)0.037 (3)0.0004 (19)0.008 (2)0.004 (2)
C370.022 (2)0.028 (3)0.022 (3)−0.0086 (19)0.0019 (19)0.0016 (19)
C41A0.018 (3)0.031 (6)0.027 (5)−0.007 (3)0.009 (3)0.000 (4)
C42A0.025 (4)0.043 (5)0.048 (5)0.008 (3)−0.003 (4)−0.009 (3)
C43A0.041 (5)0.060 (7)0.051 (6)0.010 (4)−0.010 (4)−0.031 (4)
C44A0.036 (5)0.045 (6)0.053 (6)0.008 (4)0.012 (4)−0.012 (4)
C45A0.023 (3)0.050 (7)0.033 (6)−0.001 (4)0.008 (4)−0.005 (5)
C46A0.022 (3)0.030 (3)0.032 (3)−0.001 (2)0.000 (2)0.002 (2)
C41B0.018 (3)0.031 (6)0.027 (5)−0.007 (3)0.009 (3)0.000 (4)
C42B0.025 (4)0.043 (5)0.048 (5)0.008 (3)−0.003 (4)−0.009 (3)
C43B0.041 (5)0.060 (7)0.051 (6)0.010 (4)−0.010 (4)−0.031 (4)
C44B0.036 (5)0.045 (6)0.053 (6)0.008 (4)0.012 (4)−0.012 (4)
C45B0.023 (3)0.050 (7)0.033 (6)−0.001 (4)0.008 (4)−0.005 (5)
C46B0.022 (3)0.030 (3)0.032 (3)−0.001 (2)0.000 (2)0.002 (2)
C470.019 (2)0.026 (3)0.033 (3)−0.0031 (19)0.002 (2)−0.004 (2)
Geometric parameters (Å, °) top
Ag1—S22.5293 (12)C26—H260.93
Ag1—S32.5621 (12)C27—C281.526 (7)
Ag1—S42.5639 (12)C27—H27a0.97
Ag1—S12.6170 (12)C27—H27b0.97
Sb1—F31.816 (4)C28—C47ii1.517 (6)
Sb1—F51.864 (4)C28—H28a0.97
Sb1—F61.866 (3)C28—H28b0.97
Sb1—F41.866 (3)C31—C361.392 (7)
Sb1—F21.886 (4)C31—C321.395 (6)
Sb1—F11.929 (4)C32—C331.374 (7)
S1—C111.799 (5)C32—H320.93
S1—C171.814 (5)C33—C341.387 (8)
S2—C211.786 (5)C33—H330.93
S2—C271.802 (5)C34—C351.385 (8)
S3—C311.781 (5)C34—H340.93
S3—C371.820 (5)C35—C361.384 (7)
S4—C41b1.741 (6)C35—H350.93
S4—C471.811 (5)C36—H360.93
S4—C41a1.831 (6)C37—C18iii1.530 (6)
C11—C121.378 (7)C37—H37a0.97
C11—C161.385 (7)C37—H37b0.97
C12—C131.374 (7)C41a—C42a1.39
C12—H120.93C41a—C46a1.39
C13—C141.371 (8)C42a—C43a1.39
C13—H130.93C42a—H42a0.93
C14—C151.379 (9)C43a—C44a1.39
C14—H140.93C43a—H43a0.93
C15—C161.384 (7)C44a—C45a1.39
C15—H150.93C44a—H44a0.93
C16—H160.93C45a—C46a1.39
C17—C181.523 (6)C45a—H45a0.93
C17—H17a0.97C46a—H46a0.93
C17—H17b0.97C41b—C42b1.39
C18—C37i1.530 (6)C41b—C46b1.39
C18—H18a0.97C42b—C43b1.39
C18—H18b0.97C42b—H42b0.93
C21—C221.384 (7)C43b—C44b1.39
C21—C261.390 (7)C43b—H43b0.93
C22—C231.396 (7)C44b—C45b1.39
C22—H220.93C44b—H44b0.93
C23—C241.377 (7)C45b—C46b1.39
C23—H230.93C45b—H45b0.93
C24—C251.378 (8)C46b—H46b0.93
C24—H240.93C47—C28iv1.517 (6)
C25—C261.380 (7)C47—H47a0.97
C25—H250.93C47—H47b0.97
S2—Ag1—S3118.58 (4)C25—C26—H26120.2
S2—Ag1—S4114.28 (4)C21—C26—H26120.2
S3—Ag1—S4109.98 (4)C28—C27—S2112.5 (4)
S2—Ag1—S1106.61 (4)C28—C27—H27A109.1
S3—Ag1—S1103.08 (4)S2—C27—H27A109.1
S4—Ag1—S1102.26 (4)C28—C27—H27B109.1
F3—SB1—F592.2 (2)S2—C27—H27B109.1
F3—SB1—F690.18 (19)H27A—C27—H27B107.8
F5—SB1—F6177.6 (2)C47ii—C28—C27110.6 (4)
F3—SB1—F491.2 (2)C47ii—C28—H28A109.5
F5—SB1—F489.82 (17)C27—C28—H28A109.5
F6—SB1—F490.21 (15)C47ii—C28—H28B109.5
F3—SB1—F292.9 (2)C27—C28—H28B109.5
F5—SB1—F291.56 (18)H28A—C28—H28B108.1
F6—SB1—F288.24 (17)C36—C31—C32120.0 (5)
F4—SB1—F2175.6 (2)C36—C31—S3123.9 (4)
F3—SB1—F1178.1 (2)C32—C31—S3116.1 (4)
F5—SB1—F189.3 (2)C33—C32—C31119.8 (5)
F6—SB1—F188.32 (16)C33—C32—H32120.1
F4—SB1—F187.73 (18)C31—C32—H32120.1
F2—SB1—F188.2 (2)C32—C33—C34120.6 (5)
C11—S1—C17103.9 (2)C32—C33—H33119.7
C11—S1—AG1105.44 (15)C34—C33—H33119.7
C17—S1—AG1104.63 (16)C35—C34—C33119.7 (5)
C21—S2—C27104.6 (2)C35—C34—H34120.2
C21—S2—AG1105.26 (16)C33—C34—H34120.2
C27—S2—AG1108.28 (17)C34—C35—C36120.5 (5)
C31—S3—C37104.4 (2)C34—C35—H35119.7
C31—S3—AG1103.08 (15)C36—C35—H35119.7
C37—S3—AG1109.11 (16)C35—C36—C31119.5 (5)
C41B—S4—C47102.9 (3)C35—C36—H36120.3
C47—S4—C41A106.2 (3)C31—C36—H36120.3
C41B—S4—AG1115.2 (3)C18iii—C37—S3111.2 (3)
C47—S4—AG1103.42 (16)C18iii—C37—H37A109.4
C41A—S4—AG1100.2 (3)S3—C37—H37A109.4
C12—C11—C16120.3 (5)C18iii—C37—H37B109.4
C12—C11—S1123.2 (4)S3—C37—H37B109.4
C16—C11—S1116.5 (4)H37A—C37—H37B108
C13—C12—C11119.9 (5)C42A—C41A—C46A120
C13—C12—H12120.1C42A—C41A—S4116.6 (5)
C11—C12—H12120.1C46A—C41A—S4123.3 (5)
C14—C13—C12120.5 (6)C41A—C42A—C43A120
C14—C13—H13119.8C41A—C42A—H42A120
C12—C13—H13119.8C43A—C42A—H42A120
C13—C14—C15119.8 (6)C42A—C43A—C44A120
C13—C14—H14120.1C42A—C43A—H43A120
C15—C14—H14120.1C44A—C43A—H43A120
C14—C15—C16120.3 (5)C45A—C44A—C43A120
C14—C15—H15119.8C45A—C44A—H44A120
C16—C15—H15119.8C43A—C44A—H44A120
C15—C16—C11119.2 (5)C46A—C45A—C44A120
C15—C16—H16120.4C46A—C45A—H45A120
C11—C16—H16120.4C44A—C45A—H45A120
C18—C17—S1112.2 (3)C45A—C46A—C41A120
C18—C17—H17A109.2C45A—C46A—H46A120
S1—C17—H17A109.2C41A—C46A—H46A120
C18—C17—H17B109.2C42B—C41B—C46B120
S1—C17—H17B109.2C42B—C41B—S4114.9 (5)
H17A—C17—H17B107.9C46B—C41B—S4125.1 (5)
C17—C18—C37i110.2 (4)C43B—C42B—C41B120
C17—C18—H18A109.6C43B—C42B—H42B120
C37i—C18—H18A109.6C41B—C42B—H42B120
C17—C18—H18B109.6C42B—C43B—C44B120
C37i—C18—H18B109.6C42B—C43B—H43B120
H18A—C18—H18B108.1C44B—C43B—H43B120
C22—C21—C26120.5 (5)C43B—C44B—C45B120
C22—C21—S2124.4 (4)C43B—C44B—H44B120
C26—C21—S2115.1 (4)C45B—C44B—H44B120
C21—C22—C23118.9 (5)C46B—C45B—C44B120
C21—C22—H22120.6C46B—C45B—H45B120
C23—C22—H22120.6C44B—C45B—H45B120
C24—C23—C22120.6 (5)C45B—C46B—C41B120
C24—C23—H23119.7C45B—C46B—H46B120
C22—C23—H23119.7C41B—C46B—H46B120
C25—C24—C23120.0 (5)C28iv—C47—S4112.7 (3)
C25—C24—H24120C28iv—C47—H47A109
C23—C24—H24120S4—C47—H47A109
C24—C25—C26120.4 (5)C28iv—C47—H47B109
C24—C25—H25119.8S4—C47—H47B109
C26—C25—H25119.8H47A—C47—H47B107.8
C25—C26—C21119.7 (5)
S2—AG1—S1—C11−41.29 (16)C24—C25—C26—C210.7 (9)
S3—AG1—S1—C1184.28 (16)C22—C21—C26—C25−1.3 (8)
S4—AG1—S1—C11−161.55 (16)S2—C21—C26—C25177.8 (4)
S2—AG1—S1—C17−150.52 (17)C21—S2—C27—C28−73.9 (4)
S3—AG1—S1—C17−24.95 (18)AG1—S2—C27—C28174.3 (3)
S4—AG1—S1—C1789.22 (17)S2—C27—C28—C47ii−178.4 (3)
S3—AG1—S2—C21−20.62 (18)C37—S3—C31—C36−22.9 (5)
S4—AG1—S2—C21−152.88 (17)AG1—S3—C31—C3691.1 (4)
S1—AG1—S2—C2194.94 (18)C37—S3—C31—C32157.5 (4)
S3—AG1—S2—C2790.76 (18)AG1—S3—C31—C32−88.5 (4)
S4—AG1—S2—C27−41.50 (19)C36—C31—C32—C33−1.0 (7)
S1—AG1—S2—C27−153.68 (18)S3—C31—C32—C33178.6 (4)
S2—AG1—S3—C31−94.61 (16)C31—C32—C33—C341.0 (8)
S4—AG1—S3—C3139.51 (16)C32—C33—C34—C35−0.5 (8)
S1—AG1—S3—C31147.95 (16)C33—C34—C35—C36−0.2 (9)
S2—AG1—S3—C3715.91 (18)C34—C35—C36—C310.2 (8)
S4—AG1—S3—C37150.04 (18)C32—C31—C36—C350.4 (7)
S1—AG1—S3—C37−101.52 (18)S3—C31—C36—C35−179.2 (4)
S2—AG1—S4—C41B42.0 (3)C31—S3—C37—C18iii−64.9 (4)
S3—AG1—S4—C41B−94.2 (3)AG1—S3—C37—C18iii−174.5 (3)
S1—AG1—S4—C41B156.8 (3)C41B—S4—C41A—C42A−109 (2)
S2—AG1—S4—C47−69.39 (17)C47—S4—C41A—C42A171.7 (4)
S3—AG1—S4—C47154.36 (17)AG1—S4—C41A—C42A64.4 (4)
S1—AG1—S4—C4745.38 (17)C41B—S4—C41A—C46A75 (2)
S2—AG1—S4—C41A40.1 (3)C47—S4—C41A—C46A−4.4 (5)
S3—AG1—S4—C41A−96.2 (3)AG1—S4—C41A—C46A−111.7 (4)
S1—AG1—S4—C41A154.9 (3)C46A—C41A—C42A—C43A0
C17—S1—C11—C1227.0 (5)S4—C41A—C42A—C43A−176.3 (6)
AG1—S1—C11—C12−82.7 (4)C41A—C42A—C43A—C44A0
C17—S1—C11—C16−154.1 (4)C42A—C43A—C44A—C45A0
AG1—S1—C11—C1696.2 (4)C43A—C44A—C45A—C46A0
C16—C11—C12—C130.6 (8)C44A—C45A—C46A—C41A0
S1—C11—C12—C13179.5 (4)C42A—C41A—C46A—C45A0
C11—C12—C13—C14−1.3 (8)S4—C41A—C46A—C45A176.0 (6)
C12—C13—C14—C151.0 (9)C47—S4—C41B—C42B−152.3 (4)
C13—C14—C15—C160.0 (9)C41A—S4—C41B—C42B103 (2)
C14—C15—C16—C11−0.8 (8)AG1—S4—C41B—C42B95.9 (5)
C12—C11—C16—C150.4 (7)C47—S4—C41B—C46B27.7 (6)
S1—C11—C16—C15−178.5 (4)C41A—S4—C41B—C46B−77 (2)
C11—S1—C17—C1864.8 (4)AG1—S4—C41B—C46B−84.0 (5)
AG1—S1—C17—C18175.1 (3)C46B—C41B—C42B—C43B0
S1—C17—C18—C37i−178.1 (3)S4—C41B—C42B—C43B−179.9 (6)
C27—S2—C21—C22−13.7 (5)C41B—C42B—C43B—C44B0
AG1—S2—C21—C22100.3 (4)C42B—C43B—C44B—C45B0
C27—S2—C21—C26167.2 (4)C43B—C44B—C45B—C46B0
AG1—S2—C21—C26−78.8 (4)C44B—C45B—C46B—C41B0
C26—C21—C22—C230.7 (7)C42B—C41B—C46B—C45B0
S2—C21—C22—C23−178.4 (4)S4—C41B—C46B—C45B179.9 (7)
C21—C22—C23—C240.5 (8)C41B—S4—C47—C28iv65.1 (5)
C22—C23—C24—C25−1.1 (8)C41A—S4—C47—C28iv80.4 (5)
C23—C24—C25—C260.5 (9)AG1—S4—C47—C28iv−174.7 (3)
Symmetry codes: (i) −x, y+1/2, −z+1/2; (ii) −x+1, y−1/2, −z+1/2; (iii) −x, y−1/2, −z+1/2; (iv) −x+1, y+1/2, −z+1/2.
Table 1
Selected geometric parameters (Å, °) top
Ag1—S22.5293 (12)Ag1—S42.5639 (12)
Ag1—S32.5621 (12)Ag1—S12.6170 (12)
S2—Ag1—S3118.58 (4)S2—Ag1—S1106.61 (4)
S2—Ag1—S4114.28 (4)S3—Ag1—S1103.08 (4)
S3—Ag1—S4109.98 (4)S4—Ag1—S1102.26 (4)
Acknowledgements top

We gratefully acknowledge Son Excellence Monsieur Ismael Omar Guelleh, Président de la République de Djibouti, for his wonderful support to all kind of research in the Republic of Djibouti, which is one of an abiding feature of this policies as well as the Natural Sciences and Engineering Research Council of Canada. We are deeply thankful to Mohamed Hassan Abdillahi, Secrétaire Général de la Présidence and Président of the Conseil National Scientifique du CERD (Centre d'Étude et de Recherche de Djibouti) for his steady support and his encouragement to the collaboration between the CERD and the Department of Chemistry of the Université de Montréal, and to Dr Jalludin Mohamed, General Director of CERD, for his encouragement in this work.

references
References top

Awaleh, M. O., Badia, A. & Brisse, F. (2006a). Inorg. Chem. 45, 1560–1574.

Awaleh, M. O., Badia, A. & Brisse, F. (2006b). Cryst. Growth Des. 6, 2674–2685.

Awaleh, M. O., Badia, A. & Brisse, F. (2007). Inorg. Chem. 46, 3185–3191.

Black, J. R., Champness, N. R., Levason, W. & Reid, G. (1995). J. Chem. Soc. Dalton Trans. pp. 3439–3445.

Blake, A. J., Champness, N. R., Hubberstey, P., Li, W. S., Withersby, M. A. & Schroder, M. (1999). Coord. Chem. Rev. 183, 117–138.

Bruker (1997). SHELXTL. Release 5.10. Bruker AXS Inc., Madison, USA.

Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, USA.

Bu, X. H., Chen, W., Hou, W. F., Du, M., Zhang, R. H. & Brisse, F. (2002). Inorg. Chem. 41, 3477–3482.

Carlucci, L., Ciani, G., Proserpio, D. M. & Rizzato, S. (2002). CrystEngComm, 4, 413–425.

Hartley, F. R., Murray, S. G., Levason, W., Soutter, H. E. & McAuliffe, C. A. (1979). Inorg. Chim. Acta, 35, 265–277.

Hou, B.-H., Zhou, L.-N., Yin, Q.-X., Wang, J.-K. & Chen, W. (2005). Acta Cryst. E61, o2482–o2483.

Maris, T. (2004). UdMX. Universite de Montreal, Canada.

Millward, A. R. & Yaghi, O. M. (2005). J. Am. Chem. Soc. 127, 17998–17999.

Noro, S. I., Kitaura, R., Kondo, M., Kitagawa, S., Ishii, T., Matsuzaka, H. & Yamashita, M. (2002). J. Am. Chem. Soc. 124, 2568–2583.

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Sluis, P. van der & Spek, A. L. (1990). Acta Cryst. A46, 194–201.

Spek, A. L. (2003). J. Appl. Cryst. 36, 7–13.

Withersby, M. A., Blake, A. J., Champness, N. R., Cooke, P. A., Hubberstey, P., Li, W. S. & Schroder, M. (1999). Inorg. Chem. 38, 2259–2266.

Withersby, M. A., Blake, A. J., Champness, N. R., Hubberstey, P., Li, W. S. & Schroder, M. (1997). Angew. Chem. Int. Ed. Engl. 36, 2327–2329.

Wong-Foy, A. G., Matzger, A. J. & Yaghi, O. M. (2006). J. Am. Chem. Soc. 128, 3494–3495.