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Acta Cryst. (2007). E63, m2528    [ doi:10.1107/S1600536807043802 ]

catena-Poly[bis[[mu]-1,4-bis(2-pyrimidinylthio)butane-[kappa]2N:N']disilver(I) diperchlorate chloroform sesquisolvate]

S.-L. Wang and Y. Zheng

Abstract top

The crystal structure of the title complex, {[Ag2(C12H14N4S2)2](ClO4)2·1.5CHCl3}n, consists of [Ag2(C12H14N4S2)2]n2n+ one-dimensional chain cations, ClO4- anions and solvent chloroform molecules. There are two crystallographically independent AgI centers. The ligand coordinates to the AgI centers in an N,N'-bidentate bridging mode in an anti conformation, resulting in infinite corrugated chains. The one-dimensional chains are linked to form a two-dimensional framework by weak Ag...S interactions [3.052 (4) and 3.348 (5) Å]. One of the perchlorate ions and all of the solvent chloroform molecules are disordered.

Comment top

Some AgI complexes of flexible bis(arylthio)alkyl ligands (aryl = phenyl, benzyl, pyridyl, pyrimidinyl, 4-methyl-2-pyrimidinyl or 5-methyl-1,3,4-thiadiazolyl) have been reported by us and others [Bu et al., 2003; Li et al., 2005; Xie et al., 2004, 2005; Zheng et al., 2003, 2005], which show different structure features. Herein, we report a 1,4-bis(2-pyrimidinylthio)butane(L)—AgI complex, {[Ag2(C12H14N4S2)2]·2ClO4·1.5CHCl3}n (I). The crystal structure of the title complex (I) consists of [AgL]n one-dimensional chain cations, ClO4− anions (as shown in Fig. 1) and solvent chloroform molecules. In the cationic chain, there are two crystallographic independent AgI centers (Ag1 and Ag2), both of which adopt near linear coordination geometry coordinated by two pyrimidine N atoms from two crystallographic independent L ligands. Selected bond distances and angles are listed in Table 1. The ligand coordinates to the AgI centers in a N,N'-bidentate bridging mode with two N donors in an anti-conformation, resulting in an infinite corrugated chain with the intra-molecular Ag—Ag separations of 13.089 (5) and 13.228 (5) Å. It is interesting that by the Ag—S weak coordinations (Ag1—S1B = 3.052 (4) and Ag2—S4C = 3.348 (5) Å) such one-dimensional chains are linked to form a two-dimensional supramolecular framework as shown in Fig. 2.

Related literature top

For related literature, see: Bu et al. (2003); Li et al. (2005); Xie et al. (2004; 2005); Zheng et al. (2003; 2005).

Experimental top

The ligand 1,4-bis(2-pyrimidinylthio)butane (L) was synthesized by simulating a reported procedures [Bu et al., 2003]. The solution of AgClO4·H2O (23 mg, 0.1 mmol) in MeOH was carefully layered on top of a solution of L (28 mg, 0.1 mmol) in toluene in a test-tube. After ten days at room temperature, colorless block single crystals appeared at the boundary between two solvents with a yield of 40%.

Refinement top

H atoms were included in calculated positions and treated in the subsequent refinement as riding atoms, with C—H = 0.93, 0.97 and 0.98 Å and Uiso(H) = 1.2 Ueq(C). One of perchlorate ions and all of solvent chloroform molecuels are disordered. For the disordered perchlorate ion, each one O atom was refined in two positions with a near 1:1 occupation factors ratio. The Cl—O lengths were restrained to 1.44 (1) Å. Additionally, the displacement parameters were restrained to be nearly isotropic. For chloroform molecuels, C and Cl atoms were refined in three positions with a 1:1:1 occupation factors ratio for one, and in two positions with a 3:1 ratio for half one. All of Cl—O lengths were restrained to 1.72 (1) Å and Cl—O distances to 2.81 (1) Å

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART (Bruker, 1998); data reduction: SAINT and SHELXTL (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL (Bruker, 1998).

Figures top
[Figure 1] Fig. 1. Displacement ellipsoid plot (30% probability) of a fragment of the one-dimensional structure of (I) with disordered solvent chloroform molecules omitted for clarity. [symmetry codes: (A) x, y, 1 + z]
[Figure 2] Fig. 2. Two-dimensional supramolecular layer of (I) showing Ag—S weak coordinaolyPtion. [symmetry codes: (B) 1 − x, −y, −z; (C) −x, 1 − y, 1 − z]
catena-Poly[bis[µ-1,4-bis(2-pyrimidinylthio)butane-κ2 N:N']disilver(I) diperchlorate chloroform sesquisolvate] top
Crystal data top
[Ag2(C12H14N4S2)2](ClO4)2·1.5CHCl3Z = 1
Mr = 2300.95F000 = 1142
Triclinic, P1Dx = 1.775 Mg m−3
Hall symbol: -P 1Mo Kα radiation
λ = 0.71073 Å
a = 11.197 (4) ÅCell parameters from 883 reflections
b = 12.394 (4) Åθ = 3.3–25.5º
c = 16.897 (6) ŵ = 1.56 mm−1
α = 73.715 (5)ºT = 293 (2) K
β = 73.060 (6)ºBlock, colorless
γ = 86.618 (6)º0.28 × 0.26 × 0.22 mm
V = 2152.5 (13) Å3
Data collection top
Bruker SMART 1000 CCD area-detector
diffractometer		8803 independent reflections
Radiation source: fine-focus sealed tube4653 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.023
T = 293(2) Kθmax = 26.5º
φ and ω scanθmin = 1.3º
Absorption correction: multi-scan
(SADABS; Bruker, 1998)		h = −14→7
Tmin = 0.834, Tmax = 1.000k = −15→14
12535 measured reflectionsl = −20→21
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)] = 0.053H-atom parameters constrained
wR(F2) = 0.167  w = 1/[σ2(Fo2) + (0.0759P)2 + 1.7172P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max < 0.001
8803 reflectionsΔρmax = 0.74 e Å−3
652 parametersΔρmin = −0.44 e Å−3
494 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Crystal data top
[Ag2(C12H14N4S2)2](ClO4)2·1.5CHCl3γ = 86.618 (6)º
Mr = 2300.95V = 2152.5 (13) Å3
Triclinic, P1Z = 1
a = 11.197 (4) ÅMo Kα
b = 12.394 (4) ŵ = 1.56 mm−1
c = 16.897 (6) ÅT = 293 (2) K
α = 73.715 (5)º0.28 × 0.26 × 0.22 mm
β = 73.060 (6)º
Data collection top
Bruker SMART 1000 CCD area-detector
diffractometer		8803 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1998)		4653 reflections with I > 2σ(I)
Tmin = 0.834, Tmax = 1.000Rint = 0.023
12535 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.053494 restraints
wR(F2) = 0.167H-atom parameters constrained
S = 1.02Δρmax = 0.74 e Å−3
8803 reflectionsΔρmin = −0.44 e Å−3
652 parameters
Special details top

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)
Ag10.42920 (6)−0.16870 (5)0.08567 (3)0.0729 (2)
Ag2−0.16104 (6)0.47906 (5)0.57281 (3)0.0785 (2)
S10.33368 (16)0.03171 (13)−0.04970 (10)0.0557 (4)
S2−0.06388 (16)0.26616 (15)−0.29450 (11)0.0639 (5)
S30.30282 (17)0.00309 (15)0.19341 (11)0.0657 (5)
S4−0.03039 (19)0.30037 (18)0.47281 (13)0.0812 (6)
N10.4087 (4)−0.1739 (4)−0.0381 (3)0.0470 (11)
N20.3745 (5)−0.0766 (5)−0.1712 (3)0.0623 (14)
N3−0.1815 (5)0.4539 (4)−0.2911 (3)0.0578 (13)
N4−0.1477 (5)0.3492 (5)−0.1600 (3)0.0661 (15)
N50.3957 (4)−0.1960 (4)0.2249 (3)0.0506 (12)
N60.3364 (5)−0.1174 (5)0.3424 (3)0.0678 (15)
N7−0.1665 (5)0.4764 (4)0.4460 (3)0.0569 (13)
N8−0.1288 (6)0.3764 (6)0.3418 (4)0.092 (2)
C10.4380 (6)−0.2656 (5)−0.0663 (4)0.0578 (16)
H10.4620−0.3295−0.03060.069*
C20.4338 (7)−0.2683 (6)−0.1456 (4)0.0695 (19)
H20.4505−0.3332−0.16400.083*
C30.4035 (7)−0.1699 (6)−0.1966 (4)0.071 (2)
H30.4033−0.1680−0.25200.085*
C40.3755 (5)−0.0837 (5)−0.0925 (4)0.0468 (14)
C50.2764 (6)0.1281 (5)−0.1320 (4)0.0593 (17)
H5A0.27360.2025−0.12340.071*
H5B0.33550.1318−0.18760.071*
C60.1485 (6)0.0977 (5)−0.1340 (4)0.0560 (16)
H6A0.08980.0860−0.07710.067*
H6B0.15240.0285−0.15060.067*
C70.1041 (6)0.1919 (5)−0.1980 (4)0.0579 (16)
H7A0.09250.2588−0.17780.069*
H7B0.16810.2093−0.25300.069*
C8−0.0167 (6)0.1621 (5)−0.2106 (4)0.0626 (17)
H8A−0.08240.1525−0.15680.075*
H8B−0.00760.0907−0.22450.075*
C9−0.1360 (6)0.3644 (5)−0.2418 (4)0.0516 (15)
C10−0.2405 (7)0.5294 (6)−0.2526 (5)0.076 (2)
H10−0.27240.5917−0.28490.091*
C11−0.2563 (8)0.5199 (6)−0.1689 (5)0.084 (2)
H11−0.29900.5733−0.14280.101*
C12−0.2065 (7)0.4279 (7)−0.1241 (5)0.081 (2)
H12−0.21400.4200−0.06650.097*
C130.4284 (6)−0.2900 (6)0.2747 (4)0.0578 (16)
H130.4594−0.34900.25120.069*
C140.4171 (6)−0.3015 (6)0.3597 (4)0.0686 (19)
H140.4403−0.36670.39450.082*
C150.3699 (7)−0.2118 (7)0.3907 (5)0.080 (2)
H150.3610−0.21740.44820.096*
C160.3492 (5)−0.1141 (5)0.2626 (4)0.0523 (15)
C170.2660 (6)0.1047 (6)0.2555 (5)0.0723 (19)
H17A0.32980.10240.28430.087*
H17B0.26970.17920.21610.087*
C180.1413 (6)0.0876 (6)0.3214 (5)0.073 (2)
H18A0.14160.02100.36820.087*
H18B0.07730.07730.29590.087*
C190.1135 (7)0.1928 (7)0.3564 (5)0.079 (2)
H19A0.18160.20500.37790.095*
H19B0.11090.25810.30910.095*
C20−0.0037 (8)0.1840 (7)0.4250 (6)0.094 (3)
H20A−0.00430.11490.46980.113*
H20B−0.07230.17880.40190.113*
C21−0.1173 (6)0.3937 (6)0.4123 (4)0.0617 (17)
C22−0.2316 (7)0.5505 (6)0.4029 (4)0.0705 (19)
H22−0.26520.61110.42360.085*
C23−0.2506 (7)0.5406 (7)0.3290 (5)0.080 (2)
H23−0.29770.59200.29980.096*
C24−0.1982 (8)0.4534 (8)0.3005 (5)0.095 (3)
H24−0.20970.44500.25020.114*
Cl10.6523 (2)0.60581 (16)0.06711 (13)0.0779 (5)
O10.6813 (9)0.7093 (7)0.0011 (6)0.177 (4)
O20.7267 (9)0.5929 (7)0.1195 (6)0.184 (4)
O30.6527 (11)0.5225 (6)0.0323 (6)0.200 (5)
O40.5317 (8)0.6208 (9)0.1100 (5)0.192 (4)
Cl20.4539 (2)0.34556 (17)0.39794 (12)0.0774 (5)
O50.3219 (6)0.3444 (10)0.4326 (7)0.094 (4)0.667 (14)
O60.4963 (10)0.4271 (9)0.3167 (5)0.112 (5)0.667 (14)
O70.5051 (12)0.3800 (14)0.4553 (6)0.167 (7)0.667 (14)
O80.4962 (14)0.2406 (7)0.3917 (10)0.215 (9)0.667 (14)
O5'0.3346 (15)0.292 (2)0.4241 (19)0.214 (19)0.333 (14)
O6'0.438 (2)0.4639 (9)0.3833 (18)0.152 (10)0.333 (14)
O7'0.525 (2)0.325 (3)0.3191 (11)0.237 (16)0.333 (14)
O8'0.518 (2)0.3029 (17)0.4592 (13)0.134 (10)0.333 (14)
C250.2886 (11)0.0715 (10)0.5631 (9)0.055 (5)0.422 (11)
H250.31900.12550.50630.066*0.422 (11)
Cl30.1298 (9)0.0784 (11)0.6004 (10)0.153 (5)0.422 (11)
Cl40.3558 (12)0.1004 (13)0.6321 (10)0.169 (5)0.422 (11)
Cl50.3221 (11)−0.0635 (12)0.5547 (14)0.240 (8)0.422 (11)
C25'0.2522 (15)0.0247 (15)0.5881 (9)0.109 (11)0.328 (11)
H25'0.2008−0.04280.62270.131*0.328 (11)
Cl3'0.1541 (12)0.1336 (15)0.5820 (9)0.128 (6)0.328 (11)
Cl4'0.3563 (16)0.0365 (14)0.6398 (10)0.146 (5)0.328 (11)
Cl5'0.3181 (10)0.0060 (9)0.4887 (6)0.116 (4)0.328 (11)
C260.0137 (18)0.7237 (10)0.9183 (10)0.069 (7)0.283 (5)
H26−0.07650.71690.94610.083*0.283 (5)
Cl60.0834 (17)0.7822 (11)0.9757 (8)0.075 (4)0.283 (5)
Cl70.0710 (13)0.5926 (8)0.9178 (7)0.130 (4)0.283 (5)
Cl80.041 (2)0.8061 (12)0.8154 (9)0.166 (8)0.283 (5)
C26'−0.0228 (17)0.7372 (12)0.9237 (9)0.072 (7)0.317 (5)
H26'−0.08950.68160.95940.086*0.317 (5)
Cl6'0.081 (2)0.7375 (16)0.9808 (12)0.120 (6)0.317 (5)
Cl7'0.0455 (14)0.7020 (13)0.8312 (7)0.175 (6)0.317 (5)
Cl8'−0.0879 (7)0.8663 (5)0.9019 (4)0.096 (3)0.317 (5)
Cl6"−0.019 (3)0.616 (2)0.897 (2)0.191 (12)0.15
Cl7"0.108 (2)0.818 (3)0.7986 (16)0.123 (9)0.15
Cl8"0.028 (2)0.770 (3)0.9793 (17)0.103 (9)0.15
C26"0.084 (2)0.715 (2)0.8939 (15)0.106 (12)0.15
H26"0.16390.67900.89680.128*0.15
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.1018 (5)0.0786 (4)0.0495 (3)0.0385 (3)−0.0379 (3)−0.0256 (3)
Ag20.0922 (4)0.0976 (5)0.0553 (3)0.0323 (3)−0.0377 (3)−0.0253 (3)
S10.0675 (11)0.0551 (9)0.0569 (9)0.0170 (8)−0.0354 (8)−0.0198 (8)
S20.0710 (11)0.0731 (11)0.0608 (10)0.0258 (9)−0.0383 (9)−0.0239 (9)
S30.0695 (11)0.0720 (11)0.0593 (10)0.0208 (9)−0.0230 (8)−0.0230 (9)
S40.0862 (14)0.0928 (14)0.0760 (13)0.0394 (11)−0.0336 (10)−0.0379 (11)
N10.059 (3)0.043 (3)0.045 (3)0.009 (2)−0.023 (2)−0.013 (2)
N20.075 (4)0.075 (4)0.049 (3)0.023 (3)−0.033 (3)−0.024 (3)
N30.075 (4)0.053 (3)0.057 (3)0.013 (3)−0.036 (3)−0.016 (3)
N40.079 (4)0.073 (4)0.049 (3)0.021 (3)−0.029 (3)−0.014 (3)
N50.047 (3)0.062 (3)0.045 (3)0.009 (2)−0.018 (2)−0.015 (2)
N60.076 (4)0.086 (4)0.051 (3)0.015 (3)−0.030 (3)−0.024 (3)
N70.058 (3)0.063 (3)0.050 (3)0.012 (3)−0.019 (2)−0.016 (3)
N80.096 (5)0.124 (6)0.087 (5)0.037 (4)−0.048 (4)−0.062 (4)
C10.070 (4)0.056 (4)0.054 (4)0.014 (3)−0.026 (3)−0.018 (3)
C20.075 (5)0.073 (5)0.073 (5)0.019 (4)−0.026 (4)−0.040 (4)
C30.084 (5)0.087 (5)0.053 (4)0.021 (4)−0.029 (4)−0.031 (4)
C40.047 (3)0.051 (3)0.047 (3)0.008 (3)−0.021 (3)−0.014 (3)
C50.069 (4)0.048 (4)0.068 (4)0.010 (3)−0.038 (3)−0.009 (3)
C60.058 (4)0.051 (4)0.064 (4)0.008 (3)−0.031 (3)−0.011 (3)
C70.062 (4)0.051 (4)0.067 (4)0.013 (3)−0.033 (3)−0.014 (3)
C80.067 (4)0.058 (4)0.072 (4)0.016 (3)−0.038 (4)−0.016 (3)
C90.051 (4)0.053 (4)0.053 (4)0.003 (3)−0.026 (3)−0.008 (3)
C100.101 (6)0.065 (5)0.079 (5)0.017 (4)−0.055 (5)−0.021 (4)
C110.117 (7)0.078 (5)0.080 (5)0.039 (5)−0.052 (5)−0.039 (4)
C120.100 (6)0.093 (6)0.054 (4)0.020 (5)−0.033 (4)−0.019 (4)
C130.053 (4)0.064 (4)0.054 (4)0.004 (3)−0.015 (3)−0.015 (3)
C140.072 (5)0.078 (5)0.055 (4)0.012 (4)−0.027 (3)−0.010 (4)
C150.088 (6)0.110 (7)0.049 (4)0.011 (5)−0.024 (4)−0.029 (4)
C160.045 (4)0.064 (4)0.051 (4)0.005 (3)−0.015 (3)−0.019 (3)
C170.063 (5)0.077 (5)0.081 (5)0.011 (4)−0.017 (4)−0.033 (4)
C180.063 (5)0.080 (5)0.078 (5)0.010 (4)−0.016 (4)−0.032 (4)
C190.074 (5)0.095 (6)0.070 (5)0.008 (4)−0.018 (4)−0.027 (4)
C200.085 (6)0.082 (6)0.106 (7)0.014 (5)−0.006 (5)−0.035 (5)
C210.049 (4)0.083 (5)0.056 (4)0.010 (3)−0.014 (3)−0.028 (4)
C220.082 (5)0.070 (5)0.064 (4)0.018 (4)−0.033 (4)−0.018 (4)
C230.087 (6)0.087 (6)0.070 (5)0.007 (5)−0.039 (4)−0.011 (4)
C240.104 (7)0.131 (8)0.078 (6)0.027 (6)−0.052 (5)−0.049 (5)
Cl10.1006 (15)0.0713 (12)0.0836 (13)0.0258 (11)−0.0431 (12)−0.0431 (11)
O10.219 (9)0.123 (6)0.202 (9)−0.044 (6)−0.141 (8)0.031 (6)
O20.260 (11)0.137 (6)0.210 (9)0.036 (7)−0.186 (9)−0.015 (6)
O30.373 (14)0.105 (5)0.167 (8)0.045 (7)−0.098 (9)−0.097 (6)
O40.171 (8)0.297 (12)0.091 (5)0.111 (8)−0.031 (5)−0.054 (6)
Cl20.0968 (15)0.0741 (13)0.0672 (12)0.0153 (11)−0.0386 (11)−0.0156 (10)
O50.081 (7)0.116 (10)0.085 (7)0.032 (6)−0.017 (5)−0.039 (6)
O60.143 (9)0.102 (8)0.080 (7)−0.014 (7)−0.054 (6)0.020 (6)
O70.153 (11)0.258 (19)0.084 (8)−0.054 (12)−0.074 (7)0.013 (10)
O80.286 (18)0.105 (9)0.156 (14)0.063 (10)0.059 (12)−0.023 (9)
O5'0.25 (3)0.12 (2)0.30 (4)−0.08 (2)−0.22 (3)0.07 (2)
O6'0.21 (2)0.091 (15)0.18 (2)0.056 (15)−0.074 (19)−0.058 (15)
O7'0.38 (4)0.27 (4)0.10 (2)0.13 (3)−0.10 (2)−0.12 (2)
O8'0.19 (2)0.098 (16)0.146 (19)0.057 (16)−0.128 (17)−0.007 (14)
C250.082 (12)0.038 (9)0.059 (10)0.013 (8)−0.042 (9)−0.017 (7)
Cl30.121 (8)0.157 (10)0.181 (12)−0.005 (6)−0.026 (6)−0.066 (8)
Cl40.147 (8)0.201 (14)0.189 (11)0.049 (9)−0.061 (7)−0.097 (10)
Cl50.188 (10)0.206 (13)0.36 (2)0.014 (9)−0.034 (12)−0.183 (15)
C25'0.090 (18)0.13 (2)0.092 (18)0.015 (17)−0.013 (15)−0.022 (17)
Cl3'0.086 (7)0.208 (15)0.093 (7)0.054 (8)−0.030 (5)−0.053 (9)
Cl4'0.176 (11)0.161 (13)0.137 (8)0.050 (10)−0.102 (8)−0.047 (9)
Cl5'0.129 (7)0.106 (7)0.130 (8)0.033 (5)−0.045 (6)−0.057 (6)
C260.042 (15)0.093 (15)0.091 (15)0.031 (12)−0.028 (11)−0.049 (13)
Cl60.072 (8)0.092 (8)0.070 (5)0.006 (7)−0.035 (6)−0.022 (5)
Cl70.160 (10)0.104 (7)0.139 (9)0.040 (7)−0.043 (8)−0.060 (6)
Cl80.26 (2)0.143 (12)0.129 (11)−0.003 (13)−0.142 (14)−0.001 (9)
C26'0.048 (13)0.101 (14)0.083 (13)0.050 (11)−0.034 (10)−0.045 (12)
Cl6'0.144 (11)0.127 (12)0.132 (9)0.073 (9)−0.099 (9)−0.055 (8)
Cl7'0.245 (14)0.205 (13)0.111 (8)0.104 (12)−0.071 (8)−0.100 (9)
Cl8'0.114 (6)0.089 (5)0.085 (5)0.028 (4)−0.045 (4)−0.013 (4)
Cl6"0.17 (2)0.22 (2)0.18 (2)−0.085 (19)0.005 (19)−0.08 (2)
Cl7"0.117 (16)0.16 (2)0.106 (14)−0.044 (14)−0.066 (12)−0.018 (13)
Cl8"0.079 (15)0.137 (19)0.131 (16)0.023 (13)−0.047 (13)−0.081 (15)
C26"0.12 (2)0.108 (19)0.105 (19)0.007 (19)−0.038 (18)−0.046 (18)
Geometric parameters (Å, °) top
Ag1—N12.188 (4)C14—C151.373 (10)
Ag1—N52.201 (5)C14—H140.9300
Ag2—N72.171 (5)C15—H150.9300
Ag2—N3i2.177 (5)C17—C181.493 (9)
S1—C41.758 (6)C17—H17A0.9700
S1—C51.808 (6)C17—H17B0.9700
S2—C91.732 (6)C18—C191.556 (10)
S2—C81.812 (6)C18—H18A0.9700
S3—C161.749 (6)C18—H18B0.9700
S3—C171.812 (7)C19—C201.462 (10)
S4—C211.764 (7)C19—H19A0.9700
S4—C201.812 (8)C19—H19B0.9700
N1—C11.339 (7)C20—H20A0.9700
N1—C41.344 (7)C20—H20B0.9700
N2—C41.312 (7)C22—C231.364 (9)
N2—C31.335 (8)C22—H220.9300
N3—C101.324 (9)C23—C241.341 (11)
N3—C91.359 (7)C23—H230.9300
N3—Ag2ii2.177 (5)C24—H240.9300
N4—C91.310 (7)Cl1—O31.323 (6)
N4—C121.333 (9)Cl1—O21.356 (7)
N5—C131.333 (7)Cl1—O41.363 (8)
N5—C161.347 (7)Cl1—O11.424 (7)
N6—C161.303 (7)Cl2—O81.380 (7)
N6—C151.330 (9)Cl2—O8'1.398 (9)
N7—C211.324 (8)Cl2—O5'1.419 (10)
N7—C221.327 (8)Cl2—O51.422 (7)
N8—C211.312 (8)Cl2—O7'1.424 (9)
N8—C241.361 (10)Cl2—O61.425 (6)
C1—C21.366 (8)Cl2—O71.427 (8)
C1—H10.9300Cl2—O6'1.427 (9)
C2—C31.370 (9)C25—Cl41.684 (9)
C2—H20.9300C25—Cl31.710 (9)
C3—H30.9300C25—Cl51.728 (9)
C5—C61.515 (8)C25—H250.9800
C5—H5A0.9700C25'—Cl4'1.682 (10)
C5—H5B0.9700C25'—Cl3'1.688 (10)
C6—C71.522 (8)C25'—Cl5'1.701 (10)
C6—H6A0.9700C25'—H25'0.9800
C6—H6B0.9700C26—Cl81.701 (10)
C7—C81.511 (8)C26—Cl71.713 (10)
C7—H7A0.9700C26—Cl61.724 (10)
C7—H7B0.9700C26—H260.9800
C8—H8A0.9700C26'—Cl7'1.692 (10)
C8—H8B0.9700C26'—Cl8'1.708 (10)
C10—C111.345 (9)C26'—Cl6'1.717 (10)
C10—H100.9300C26'—H26'0.9800
C11—C121.368 (9)Cl6"—C26"1.709 (10)
C11—H110.9300Cl7"—C26"1.714 (10)
C12—H120.9300Cl8"—C26"1.713 (10)
C13—C141.372 (8)C26"—H26"0.9800
C13—H130.9300
N1—Ag1—N5161.96 (18)C17—C18—H18B110.0
N7—Ag2—N3i168.73 (19)C19—C18—H18B110.0
C4—S1—C5101.9 (3)H18A—C18—H18B108.3
C9—S2—C8102.3 (3)C20—C19—C18114.0 (7)
C16—S3—C17103.4 (3)C20—C19—H19A108.7
C21—S4—C20103.4 (4)C18—C19—H19A108.7
C1—N1—C4116.4 (5)C20—C19—H19B108.7
C1—N1—Ag1121.1 (4)C18—C19—H19B108.7
C4—N1—Ag1122.3 (4)H19A—C19—H19B107.6
C4—N2—C3115.9 (5)C19—C20—S4114.4 (6)
C10—N3—C9116.8 (5)C19—C20—H20A108.7
C10—N3—Ag2ii119.4 (4)S4—C20—H20A108.7
C9—N3—Ag2ii123.8 (4)C19—C20—H20B108.7
C9—N4—C12117.2 (6)S4—C20—H20B108.7
C13—N5—C16116.8 (5)H20A—C20—H20B107.6
C13—N5—Ag1122.2 (4)N8—C21—N7126.5 (6)
C16—N5—Ag1120.9 (4)N8—C21—S4119.8 (5)
C16—N6—C15116.2 (6)N7—C21—S4113.7 (5)
C21—N7—C22116.7 (6)N7—C22—C23122.0 (7)
C21—N7—Ag2121.6 (4)N7—C22—H22119.0
C22—N7—Ag2121.3 (4)C23—C22—H22119.0
C21—N8—C24114.8 (7)C24—C23—C22116.9 (7)
N1—C1—C2122.2 (6)C24—C23—H23121.5
N1—C1—H1118.9C22—C23—H23121.5
C2—C1—H1118.9C23—C24—N8123.1 (7)
C1—C2—C3116.0 (6)C23—C24—H24118.5
C1—C2—H2122.0N8—C24—H24118.5
C3—C2—H2122.0O3—Cl1—O2115.5 (6)
N2—C3—C2123.6 (6)O3—Cl1—O4107.7 (7)
N2—C3—H3118.2O2—Cl1—O4110.6 (6)
C2—C3—H3118.2O3—Cl1—O1109.6 (6)
N2—C4—N1125.8 (5)O2—Cl1—O1110.6 (5)
N2—C4—S1120.5 (4)O4—Cl1—O1101.8 (6)
N1—C4—S1113.7 (4)O8—Cl2—O8'71.6 (10)
C6—C5—S1114.9 (4)O8—Cl2—O5'83.4 (14)
C6—C5—H5A108.5O8'—Cl2—O5'111.0 (9)
S1—C5—H5A108.5O8—Cl2—O5111.4 (7)
C6—C5—H5B108.5O8'—Cl2—O5114.4 (13)
S1—C5—H5B108.5O5'—Cl2—O528.4 (13)
H5A—C5—H5B107.5O8—Cl2—O7'56.9 (12)
C5—C6—C7109.8 (5)O8'—Cl2—O7'108.1 (9)
C5—C6—H6A109.7O5'—Cl2—O7'109.1 (10)
C7—C6—H6A109.7O5—Cl2—O7'128.6 (14)
C5—C6—H6B109.7O8—Cl2—O6110.4 (6)
C7—C6—H6B109.7O8'—Cl2—O6128.3 (11)
H6A—C6—H6B108.2O5'—Cl2—O6120.7 (11)
C8—C7—C6112.7 (5)O5—Cl2—O6112.2 (6)
C8—C7—H7A109.0O7'—Cl2—O653.5 (11)
C6—C7—H7A109.0O8—Cl2—O7109.8 (7)
C8—C7—H7B109.0O8'—Cl2—O739.1 (8)
C6—C7—H7B109.0O5'—Cl2—O7123.1 (15)
H7A—C7—H7B107.8O5—Cl2—O7106.6 (6)
C7—C8—S2113.9 (5)O7'—Cl2—O7124.7 (14)
C7—C8—H8A108.8O6—Cl2—O7106.2 (6)
S2—C8—H8A108.8O8—Cl2—O6'164.1 (12)
C7—C8—H8B108.8O8'—Cl2—O6'111.6 (9)
S2—C8—H8B108.8O5'—Cl2—O6'108.7 (9)
H8A—C8—H8B107.7O5—Cl2—O6'81.9 (11)
N4—C9—N3124.0 (6)O7'—Cl2—O6'108.3 (10)
N4—C9—S2121.1 (5)O6—Cl2—O6'54.8 (10)
N3—C9—S2114.8 (4)O7—Cl2—O6'72.7 (9)
N3—C10—C11122.8 (6)Cl4—C25—Cl3109.9 (7)
N3—C10—H10118.6Cl4—C25—Cl5110.4 (7)
C11—C10—H10118.6Cl3—C25—Cl5107.3 (7)
C10—C11—C12116.8 (7)Cl4—C25—H25109.7
C10—C11—H11121.6Cl3—C25—H25109.7
C12—C11—H11121.6Cl5—C25—H25109.7
N4—C12—C11122.4 (7)Cl4'—C25'—Cl3'112.3 (8)
N4—C12—H12118.8Cl4'—C25'—Cl5'113.8 (9)
C11—C12—H12118.8Cl3'—C25'—Cl5'110.2 (8)
N5—C13—C14121.3 (6)Cl4'—C25'—H25'106.7
N5—C13—H13119.3Cl3'—C25'—H25'106.7
C14—C13—H13119.3Cl5'—C25'—H25'106.7
C13—C14—C15116.7 (6)Cl8—C26—Cl7109.6 (8)
C13—C14—H14121.7Cl8—C26—Cl6110.6 (8)
C15—C14—H14121.7Cl7—C26—Cl6109.8 (8)
N6—C15—C14123.1 (6)Cl8—C26—H26108.9
N6—C15—H15118.5Cl7—C26—H26108.9
C14—C15—H15118.5Cl6—C26—H26108.9
N6—C16—N5126.0 (6)Cl7'—C26'—Cl8'110.1 (8)
N6—C16—S3120.8 (5)Cl7'—C26'—Cl6'111.8 (8)
N5—C16—S3113.3 (4)Cl8'—C26'—Cl6'109.7 (8)
C18—C17—S3115.2 (5)Cl7'—C26'—H26'108.4
C18—C17—H17A108.5Cl8'—C26'—H26'108.4
S3—C17—H17A108.5Cl6'—C26'—H26'108.4
C18—C17—H17B108.5Cl6"—C26"—Cl8"110.6 (9)
S3—C17—H17B108.5Cl6"—C26"—Cl7"108.9 (9)
H17A—C17—H17B107.5Cl8"—C26"—Cl7"110.6 (9)
C17—C18—C19108.7 (6)Cl6"—C26"—H26"108.9
C17—C18—H18A110.0Cl8"—C26"—H26"108.9
C19—C18—H18A110.0Cl7"—C26"—H26"108.9
N5—Ag1—N1—C1−76.7 (8)N3—C10—C11—C120.8 (12)
N5—Ag1—N1—C4108.5 (6)C9—N4—C12—C111.8 (11)
N1—Ag1—N5—C1381.4 (7)C10—C11—C12—N4−1.7 (13)
N1—Ag1—N5—C16−103.6 (7)C16—N5—C13—C14−1.2 (9)
N3i—Ag2—N7—C21−69.4 (12)Ag1—N5—C13—C14174.0 (5)
N3i—Ag2—N7—C22102.8 (11)N5—C13—C14—C150.5 (10)
C4—N1—C1—C2−0.5 (9)C16—N6—C15—C140.8 (11)
Ag1—N1—C1—C2−175.6 (5)C13—C14—C15—N6−0.3 (11)
N1—C1—C2—C33.0 (10)C15—N6—C16—N5−1.7 (10)
C4—N2—C3—C2−0.3 (10)C15—N6—C16—S3177.5 (5)
C1—C2—C3—N2−2.6 (11)C13—N5—C16—N61.9 (9)
C3—N2—C4—N13.3 (9)Ag1—N5—C16—N6−173.4 (5)
C3—N2—C4—S1−177.8 (5)C13—N5—C16—S3−177.3 (4)
C1—N1—C4—N2−2.9 (9)Ag1—N5—C16—S37.4 (6)
Ag1—N1—C4—N2172.1 (5)C17—S3—C16—N68.4 (6)
C1—N1—C4—S1178.1 (4)C17—S3—C16—N5−172.4 (4)
Ag1—N1—C4—S1−6.8 (6)C16—S3—C17—C18−79.3 (6)
C5—S1—C4—N28.1 (6)S3—C17—C18—C19−169.3 (5)
C5—S1—C4—N1−172.9 (4)C17—C18—C19—C20−177.0 (7)
C4—S1—C5—C674.8 (5)C18—C19—C20—S4174.7 (6)
S1—C5—C6—C7173.0 (5)C21—S4—C20—C1992.6 (7)
C5—C6—C7—C8173.7 (5)C24—N8—C21—N70.5 (12)
C6—C7—C8—S2−173.9 (5)C24—N8—C21—S4179.8 (6)
C9—S2—C8—C7−82.1 (5)C22—N7—C21—N8−1.7 (11)
C12—N4—C9—N3−1.1 (10)Ag2—N7—C21—N8170.9 (6)
C12—N4—C9—S2−178.8 (5)C22—N7—C21—S4179.1 (5)
C10—N3—C9—N40.3 (9)Ag2—N7—C21—S4−8.4 (7)
Ag2ii—N3—C9—N4179.8 (5)C20—S4—C21—N8−10.7 (7)
C10—N3—C9—S2178.1 (5)C20—S4—C21—N7168.6 (5)
Ag2ii—N3—C9—S2−2.4 (7)C21—N7—C22—C232.0 (11)
C8—S2—C9—N4−2.0 (6)Ag2—N7—C22—C23−170.5 (6)
C8—S2—C9—N3−180.0 (5)N7—C22—C23—C24−1.3 (12)
C9—N3—C10—C11−0.2 (11)C22—C23—C24—N80.1 (14)
Ag2ii—N3—C10—C11−179.7 (6)C21—N8—C24—C230.3 (13)
Symmetry codes: (i) x, y, z+1; (ii) x, y, z−1.
Table 1
Selected geometric parameters (Å, °) top
Ag1—N12.188 (4)Ag2—N72.171 (5)
Ag1—N52.201 (5)Ag2—N3i2.177 (5)
N1—Ag1—N5161.96 (18)N7—Ag2—N3i168.73 (19)
Symmetry codes: (i) x, y, z+1.
references
References top

Bruker (1998). SMART (Version 5.051), SAINT (Version 5.01), SADABS (Version 2.03) and SHELXTL (Version 6.1). Bruker AXS Inc., Madison, Wisconsin, USA.

Bu, X.-H., Xie, Y.-B., Li, J.-R. & Zhang, R.-H. (2003). Inorg. Chem. 42, 7422–7430.

Li, J.-R., Bu, X.-H., Jiao, J., Du, W.-P., Xu, X.-H. & Zhang, R.-H. (2005). Dalton Trans. pp. 464–474.

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

Xie, Y.-B., Li, J.-R. & Bu, X.-H. (2005). Polyhedron, 24, 413–418.

Xie, Y.-B., Zhang, C., Li, J.-R. & Bu, X.-H. (2004). Dalton Trans. pp. 562–569.

Zheng, Y., Du, M., Li, J.-R., Zhang, R.-H. & Bu, X.-H. (2003). Dalton Trans. pp. 1509–1514.

Zheng, Y., Li, J.-R., Du, M., Zou, R.-Q. & Bu, X.-H. (2005). Cryst. Growth Des. 5, 215–222.