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Acta Cryst. (2007). E63, m2248-m2249    [ doi:10.1107/S1600536807036306 ]

catena-Poly[[tetrakis(hexamethylphosphoramide-[kappa]O)bis(nitrato-[kappa]2O,O')yttrium(III)] [silver(I)-di-[mu]-sulfido-tungstate(VI)(Ag-W)-di-[mu]-sulfido]]

J.-F. Zhang, Y. Cao, J. Qian and C. Zhang

Abstract top

The title salt of a one-dimensional anionic W/S/Ag polymer, {[Y(NO3)2(C6H18N3OP)4][WAgS4]}n was produced by the reaction of ammonium tetrathiotungstate(VI), silver(I) sulfide and yttrium(III) nitrate in hexamethylphosphoramide. The cation has the same structure as that in the isostructural Yb compound [Cao et al. (2007). Acta Cryst. E63, m2076-m2077]. Together with the two nitrate ligands, the cation is monovalent, which leads to the anionic chain having a monovalent repeat unit. This contrasts with solvent-coordinated rare-earth cations, which are trivalent and induce trivalent repeat units in the anionic chains. The polymeric {[WS4Ag]n-}n anion, with W-Ag-W and Ag-W-Ag angles of 162.684 (19) and 153.833 (10)°, respectively, presents a distorted linear configuration the same as that of the anionic chain in the isostructural Yb compound, suggesting that different rare-earth cations with the same coordination environments have the same influence on the arrangement of their anionic chains.

Comment top

One-dimensional Mo(W)/S/Ag anionic polymers have attracted much attention for their configurational isomerism (Niu et al., 2004) and potential applications, especially in third-order nonlinear optical (NLO) materials. (Zhang et al., 2007, and references therein). Different solvent-coordinated rare-earth cations proved effective to obtain various configurations of anionic chains (Niu et al., 2004). The title compound {[Y(hmp)4(NO3)2][WS4Ag]}n (hmp = hexamethylphosphoramide) with a wave-like anionic chain was prepared by following such route using Y(III)-hmp complex as counterion.

In possession of two nitrate ligands, the cation in the title compound is univalent (Fig. 1), which leads to an anionic chain with a univalent repeat unit, unlike other solvent-coordinated rare-earth cations, in literature (Niu et al., 2004), which are trivalent and induce trivalent repeat units. For example, [Nd(dmf)8]3+ induces an anionic chain with a trivalent repeat unit [W4S16Ag5]3- (Huang et al., 1997).

As illustrated in Fig. 2, the anionic chain in the title compound has a distorted linear configuration with W—Ag—W and Ag—W—Ag angles of 162.684 (19) and 153.833 (10) °, deviating significantly from the ideal 180 °, which is observed in the reported compound {(γ-MePyH)[MoS4Ag]}n (179.3 (2)–180.0 (1) °)(Lang et al., 1993). Similar angles of 160.81 (7) and 153.41 (7) ° for W—Ag—W and Ag—W—Ag are found in another distorted linear chain in {[Yb(hmp)4(NO3)2][WS4Ag]}n (Cao et al., 2007), which suggests that differernt rare earth cations with the same coordination environments will result in the same anionic structures.

Related literature top

One example of a one-dimensional Mo/S/Ag anionic polymer with an almost ideal linear configuration is {(γ-MePyH)[MoS4Ag]}n (Lang et al., 1993). A more relevant analog of the title compound is {[Yb(hmp)4(NO3)2][WS4Ag]}n (Cao et al., 2007), which has similar wave-like chains. For related literature, see: Huang et al. (1996); Niu et al. (2004); Zhang et al. (2007).

Experimental top

1 mmol A g2S was added to a solution of [NH4]2WS4 (2 mmol in 30 mL h mp) with thorough stir for 12 h. The solution underwent an additional stir for one minute after 1 mmol Y(NO3)36H2O was added. After filtration the orange-red filtrate was carefully laid on the surface with 30 ml i-PrOH. Red block crystals were obtained after ten days. Yield: 1.138 g in pure form, 42.2% (based on W). Analysis calculated for C24H72AgN14O10P4S4WY: C 21.36, H 5.38, N 14.53%; found: C 21.39, H 5.40, N 14.49%. IR: ν, cm-1, 478.9 m, 447.4 s (W-µ2-S).

Refinement top

Some N and P atoms have low Ueq as compared to neighbors and a few C atoms have large ADP max/min ratio. Splitting these atoms to resolve disorder will cause the refinement unstable or ADP non positive definite, so no further treatments were applied to these atoms. H atoms were positioned geometrically and refined with riding model, with Uiso = 1.5Ueq for methyl H atoms and 0.97 Å for C—H bonds.

Computing details top

Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXTL (Sheldrick, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The molecular structure of the cation in the title compound, with atom labels and 30% probability displacement ellipsoids. All H atoms have been omitted.
[Figure 2] Fig. 2. The molecular structure of a portion of the anionic chain in the title compound, with atom labels and 30% probability displacement ellipsoids.
catena-Poly[[tetrakis(hexamethylphosphoramide-κO)bis(nitrato- κ2O,O')yttrium(III)] [silver(I)-di-µ-sulfido-tungstate(VI)(Ag—W)-di-µ-sulfido]] top
Crystal data top
[Y(NO3)2(C6H18N3OP)4][WAgS4]F(000) = 2712.0
Mr = 1349.74Dx = 1.675 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 18559 reflections
a = 15.789 (3) Åθ = 3.0–25.4°
b = 29.661 (6) ŵ = 3.91 mm−1
c = 11.430 (2) ÅT = 223 K
β = 90.83 (3)°Block, red
V = 5352.3 (18) Å30.50 × 0.45 × 0.32 mm
Z = 4
Data collection top
Rigaku Mercury CCD
diffractometer		9804 independent reflections
Radiation source: fine-focus sealed tube9045 reflections with I > 2σ(I)
graphiteRint = 0.049
Detector resolution: 14.6306 pixels mm-1θmax = 25.4°, θmin = 3.0°
ω scansh = −19→18
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		k = −35→34
Tmin = 0.173, Tmax = 0.286l = −13→13
49397 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.085H-atom parameters constrained
S = 1.21 w = 1/[σ2(Fo2) + (0.0187P)2 + 15.0729P]
where P = (Fo2 + 2Fc2)/3
9783 reflections(Δ/σ)max = 0.001
532 parametersΔρmax = 0.64 e Å−3
0 restraintsΔρmin = −0.77 e Å−3
Crystal data top
[Y(NO3)2(C6H18N3OP)4][WAgS4]V = 5352.3 (18) Å3
Mr = 1349.74Z = 4
Monoclinic, P21/cMo Kα radiation
a = 15.789 (3) ŵ = 3.91 mm−1
b = 29.661 (6) ÅT = 223 K
c = 11.430 (2) Å0.50 × 0.45 × 0.32 mm
β = 90.83 (3)°
Data collection top
Rigaku Mercury CCD
diffractometer		9804 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		9045 reflections with I > 2σ(I)
Tmin = 0.173, Tmax = 0.286Rint = 0.049
49397 measured reflectionsθmax = 25.4°
Refinement top
R[F2 > 2σ(F2)] = 0.044 w = 1/[σ2(Fo2) + (0.0187P)2 + 15.0729P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.085Δρmax = 0.64 e Å−3
S = 1.21Δρmin = −0.77 e Å−3
9783 reflectionsAbsolute structure: ?
532 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
H-atom parameters constrained
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*/Ueq
Y10.76115 (3)0.082921 (16)0.17150 (4)0.02278 (12)
P10.70695 (12)0.14734 (5)−0.09585 (14)0.0438 (4)
P20.54106 (9)0.09577 (5)0.26801 (14)0.0342 (3)
P30.97701 (9)0.13288 (5)0.17952 (13)0.0338 (3)
P40.80120 (10)−0.02977 (5)0.30019 (13)0.0353 (4)
O10.7919 (2)0.01860 (11)0.2690 (3)0.0339 (9)
O20.8953 (2)0.10728 (12)0.1756 (3)0.0322 (9)
O30.7269 (2)0.12720 (13)0.0200 (3)0.0371 (9)
O40.7473 (2)0.15830 (12)0.2613 (4)0.0377 (9)
O50.7751 (2)0.10306 (12)0.3780 (3)0.0369 (9)
O60.6976 (2)0.02732 (13)0.0357 (4)0.0381 (9)
O70.8304 (2)0.04127 (13)0.0125 (3)0.0372 (9)
O80.7633 (3)0.00110 (17)−0.1173 (4)0.0650 (14)
O90.7713 (4)0.17139 (17)0.4459 (4)0.0830 (19)
O100.6240 (2)0.08090 (12)0.2196 (3)0.0338 (9)
N10.9766 (3)0.17387 (18)0.0847 (5)0.0561 (15)
N21.0543 (3)0.09826 (18)0.1512 (4)0.0399 (12)
N30.9927 (3)0.1554 (2)0.3074 (5)0.0628 (18)
N40.7792 (3)−0.03569 (17)0.4397 (4)0.0460 (13)
N50.7355 (4)−0.06513 (17)0.2348 (5)0.0560 (15)
N60.8944 (4)−0.0475 (2)0.2622 (5)0.0624 (17)
N70.6078 (5)0.1388 (2)−0.1297 (7)0.091 (3)
N80.7640 (5)0.1249 (2)−0.1959 (5)0.081 (2)
N90.7263 (5)0.20028 (18)−0.0935 (5)0.0643 (18)
N100.4665 (3)0.0697 (2)0.1992 (5)0.0626 (18)
N110.5156 (4)0.14856 (19)0.2598 (6)0.0631 (17)
N120.5426 (4)0.0871 (2)0.4099 (5)0.0603 (16)
N130.7646 (3)0.14517 (17)0.3638 (5)0.0454 (13)
N140.7637 (3)0.02239 (16)−0.0259 (4)0.0376 (12)
C10.9801 (5)0.1285 (4)0.4099 (7)0.101 (4)
H1A0.95270.10040.38800.151*
H1B0.94460.14490.46400.151*
H1C1.03440.12220.44700.151*
C21.0456 (4)0.0655 (2)0.0564 (6)0.0548 (18)
H2A0.98610.06140.03700.082*
H2B1.06980.03690.08100.082*
H2C1.07520.0765−0.01180.082*
C31.0453 (5)0.1839 (3)0.0046 (7)0.072 (2)
H3A1.08690.15980.00820.107*
H3B1.07190.21210.02700.107*
H3C1.02270.1863−0.07450.107*
C41.1419 (4)0.1073 (3)0.1885 (7)0.065 (2)
H4A1.14220.12940.25120.098*
H4B1.17340.11900.12290.098*
H4C1.16800.07960.21610.098*
C51.0340 (6)0.1992 (4)0.3275 (10)0.122 (4)
H5A1.04000.21480.25350.183*
H5B1.08950.19450.36290.183*
H5C0.99970.21730.37950.183*
C60.7278 (10)0.1079 (5)−0.3074 (8)0.170 (7)
H6A0.66670.1112−0.30690.255*
H6B0.74220.0763−0.31630.255*
H6C0.75070.1249−0.37200.255*
C70.9100 (5)0.2080 (3)0.0883 (9)0.082 (3)
H7A0.86700.19880.14320.123*
H7B0.88460.21140.01110.123*
H7C0.93420.23660.11320.123*
C80.3773 (5)0.0796 (4)0.2200 (10)0.144 (6)
H8A0.37280.10800.26180.216*
H8B0.35290.05570.26640.216*
H8C0.34710.08180.14570.216*
C90.6478 (6)−0.0669 (4)0.2665 (10)0.104 (3)
H9A0.6414−0.05520.34520.155*
H9B0.6282−0.09790.26360.155*
H9C0.6145−0.04880.21220.155*
C100.7551 (8)0.2262 (3)−0.1959 (8)0.112 (4)
H10A0.77410.2055−0.25580.168*
H10B0.80150.2458−0.17250.168*
H10C0.70860.2442−0.22650.168*
C110.4713 (6)0.0980 (5)0.4814 (8)0.131 (5)
H11A0.43990.12270.44600.196*
H11B0.49120.10680.55870.196*
H11C0.43480.07190.48760.196*
C120.5528 (8)0.1728 (4)−0.1864 (12)0.160 (6)
H12A0.58380.2009−0.19400.239*
H12B0.50320.1778−0.13910.239*
H12C0.53540.1622−0.26340.239*
C130.4851 (8)0.1680 (4)0.1525 (10)0.140 (5)
H13A0.46530.14430.10050.210*
H13B0.53050.18450.11560.210*
H13C0.43870.18850.16880.210*
C140.8032 (5)−0.0008 (3)0.5217 (6)0.068 (2)
H14A0.80550.02790.48140.102*
H14B0.8584−0.00770.55540.102*
H14C0.76170.00080.58330.102*
C150.7738 (5)−0.0808 (2)0.4921 (6)0.066 (2)
H15A0.7577−0.10250.43220.099*
H15B0.7317−0.08070.55300.099*
H15C0.8284−0.08910.52550.099*
C160.6951 (6)0.2277 (2)0.0057 (6)0.069 (2)
H16A0.67760.20790.06840.103*
H16B0.64720.2458−0.02040.103*
H16C0.74000.24740.03390.103*
C170.8541 (7)0.1225 (3)−0.1835 (8)0.100 (3)
H17A0.87120.1346−0.10790.151*
H17B0.88020.1400−0.24500.151*
H17C0.87200.0913−0.18910.151*
C180.5672 (6)0.0961 (3)−0.1161 (10)0.107 (4)
H18A0.60650.0751−0.07960.160*
H18B0.54970.0847−0.19220.160*
H18C0.51790.0996−0.06720.160*
C190.5932 (5)0.0498 (3)0.4575 (7)0.074 (2)
H19A0.64070.04400.40670.111*
H19B0.55830.02290.46230.111*
H19C0.61410.05770.53500.111*
C200.5465 (6)0.1826 (3)0.3437 (12)0.140 (6)
H20A0.56700.16780.41420.210*
H20B0.50070.20290.36310.210*
H20C0.59230.19960.30910.210*
C210.4794 (5)0.0279 (3)0.1376 (8)0.079 (3)
H21A0.53960.02310.12660.118*
H21B0.45090.02920.06190.118*
H21C0.45640.00320.18270.118*
C220.7468 (7)−0.0825 (3)0.1202 (8)0.105 (4)
H22A0.8064−0.08120.10070.158*
H22B0.7143−0.06460.06450.158*
H22C0.7275−0.11350.11710.158*
C230.9172 (7)−0.0953 (3)0.2798 (9)0.113 (4)
H23A0.8661−0.11300.28900.169*
H23B0.9526−0.09820.34950.169*
H23C0.9480−0.10610.21250.169*
C240.9634 (5)−0.0158 (3)0.2480 (8)0.076 (2)
H24A0.94070.01430.23730.114*
H24B0.9960−0.02410.18000.114*
H24C0.9998−0.01640.31710.114*
W10.283016 (14)0.227680 (7)0.528018 (18)0.02567 (7)
Ag10.28194 (4)0.264566 (17)0.28785 (4)0.04883 (14)
S10.28226 (11)0.30025 (5)0.48562 (13)0.0427 (4)
S20.28502 (11)0.18418 (5)0.37165 (12)0.0391 (4)
S30.16900 (10)0.21196 (6)0.62861 (13)0.0434 (4)
S40.39682 (10)0.21320 (6)0.63391 (13)0.0458 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Y10.0208 (3)0.0182 (2)0.0293 (3)0.0000 (2)0.0008 (2)0.0008 (2)
P10.0625 (11)0.0335 (8)0.0348 (9)0.0083 (8)−0.0171 (8)0.0021 (7)
P20.0214 (7)0.0355 (8)0.0458 (9)0.0016 (6)0.0059 (6)−0.0069 (7)
P30.0229 (7)0.0428 (9)0.0358 (8)−0.0074 (6)−0.0004 (6)−0.0078 (7)
P40.0449 (9)0.0235 (7)0.0378 (8)0.0080 (7)0.0110 (7)0.0088 (6)
O10.040 (2)0.0202 (18)0.042 (2)0.0036 (17)−0.0010 (17)0.0057 (17)
O20.0229 (19)0.035 (2)0.039 (2)−0.0053 (16)−0.0012 (16)−0.0013 (17)
O30.040 (2)0.034 (2)0.036 (2)−0.0008 (18)−0.0110 (18)0.0082 (18)
O40.045 (2)0.026 (2)0.042 (2)0.0064 (18)−0.0023 (19)−0.0024 (18)
O50.048 (2)0.028 (2)0.035 (2)0.0040 (18)0.0047 (18)−0.0005 (17)
O60.031 (2)0.033 (2)0.050 (3)−0.0012 (17)−0.0020 (19)−0.0081 (19)
O70.030 (2)0.037 (2)0.044 (2)−0.0006 (18)0.0008 (18)−0.0082 (19)
O80.067 (3)0.071 (3)0.056 (3)0.005 (3)−0.004 (2)−0.041 (3)
O90.149 (6)0.050 (3)0.049 (3)0.020 (3)−0.019 (3)−0.028 (3)
O100.0194 (19)0.033 (2)0.049 (2)0.0011 (16)0.0035 (16)−0.0067 (18)
N10.045 (3)0.044 (3)0.080 (4)−0.012 (3)0.013 (3)0.011 (3)
N20.025 (3)0.058 (3)0.037 (3)−0.001 (2)−0.001 (2)−0.011 (2)
N30.041 (3)0.097 (5)0.050 (4)0.002 (3)−0.010 (3)−0.034 (3)
N40.062 (4)0.038 (3)0.039 (3)0.007 (3)0.009 (3)0.012 (2)
N50.082 (4)0.030 (3)0.057 (4)−0.011 (3)0.018 (3)−0.005 (3)
N60.058 (4)0.055 (4)0.075 (4)0.026 (3)0.025 (3)0.029 (3)
N70.094 (6)0.061 (4)0.115 (6)0.010 (4)−0.068 (5)0.018 (4)
N80.127 (7)0.068 (4)0.048 (4)0.033 (4)0.000 (4)−0.007 (3)
N90.119 (6)0.037 (3)0.038 (3)0.006 (3)0.002 (3)0.012 (3)
N100.027 (3)0.081 (4)0.080 (4)−0.004 (3)0.006 (3)−0.045 (4)
N110.048 (4)0.041 (3)0.100 (5)0.012 (3)0.013 (3)−0.003 (3)
N120.046 (3)0.087 (5)0.048 (3)0.014 (3)0.011 (3)−0.010 (3)
N130.055 (3)0.038 (3)0.043 (3)0.006 (3)0.001 (3)−0.009 (3)
N140.040 (3)0.031 (3)0.042 (3)0.006 (2)−0.002 (2)−0.006 (2)
C10.066 (6)0.195 (12)0.040 (5)0.022 (6)−0.013 (4)−0.003 (6)
C20.038 (4)0.071 (5)0.056 (4)0.000 (3)0.012 (3)−0.019 (4)
C30.070 (5)0.066 (5)0.080 (6)−0.022 (4)0.020 (4)0.006 (4)
C40.024 (3)0.104 (6)0.067 (5)0.006 (4)−0.007 (3)−0.016 (4)
C50.091 (7)0.118 (9)0.157 (11)−0.026 (6)−0.025 (7)−0.093 (8)
C60.31 (2)0.169 (13)0.037 (5)−0.011 (13)0.000 (8)−0.049 (7)
C70.073 (6)0.051 (5)0.124 (8)0.008 (4)0.019 (5)0.024 (5)
C80.028 (4)0.221 (13)0.183 (11)−0.013 (6)0.015 (5)−0.156 (11)
C90.069 (6)0.115 (8)0.127 (9)−0.025 (6)−0.005 (6)−0.027 (7)
C100.213 (13)0.063 (6)0.060 (6)0.018 (7)0.027 (7)0.033 (5)
C110.095 (8)0.240 (15)0.059 (6)0.075 (9)0.027 (5)−0.009 (7)
C120.164 (12)0.129 (10)0.182 (13)0.066 (9)−0.107 (10)0.007 (9)
C130.195 (13)0.109 (9)0.119 (9)0.094 (9)0.057 (9)0.044 (7)
C140.096 (6)0.068 (5)0.041 (4)0.006 (5)−0.005 (4)0.002 (4)
C150.094 (6)0.051 (4)0.054 (4)0.013 (4)0.027 (4)0.029 (4)
C160.121 (7)0.033 (4)0.053 (5)0.010 (4)0.003 (4)−0.001 (3)
C170.112 (8)0.107 (8)0.085 (7)0.043 (7)0.043 (6)0.011 (6)
C180.082 (7)0.081 (7)0.155 (10)−0.008 (5)−0.074 (7)−0.001 (7)
C190.061 (5)0.097 (7)0.063 (5)0.002 (5)0.000 (4)0.017 (5)
C200.069 (6)0.070 (6)0.281 (17)−0.003 (5)0.012 (8)−0.098 (9)
C210.041 (4)0.069 (5)0.127 (8)−0.010 (4)0.016 (4)−0.053 (5)
C220.135 (9)0.086 (7)0.095 (7)−0.047 (6)0.032 (6)−0.040 (6)
C230.143 (9)0.083 (7)0.115 (8)0.081 (7)0.070 (7)0.049 (6)
C240.039 (4)0.079 (6)0.110 (7)0.004 (4)−0.006 (4)−0.014 (5)
W10.03217 (13)0.02568 (12)0.01909 (11)0.00287 (9)−0.00250 (8)−0.00114 (9)
Ag10.0780 (4)0.0470 (3)0.0214 (2)0.0006 (3)−0.0012 (2)0.0028 (2)
S10.0713 (11)0.0254 (7)0.0312 (8)0.0047 (7)0.0005 (7)−0.0022 (6)
S20.0597 (10)0.0293 (7)0.0283 (7)−0.0007 (7)−0.0002 (7)−0.0057 (6)
S30.0385 (9)0.0605 (10)0.0314 (8)−0.0081 (8)0.0016 (6)−0.0014 (7)
S40.0395 (9)0.0649 (11)0.0328 (8)0.0174 (8)−0.0084 (7)−0.0053 (8)
Geometric parameters (Å, °) top
Y1—O32.233 (4)N2—C21.460 (8)
Y1—O22.238 (3)N2—C41.466 (7)
Y1—O102.243 (3)N3—C11.432 (11)
Y1—O12.259 (3)N3—C51.472 (10)
Y1—O52.441 (4)N4—C141.443 (9)
Y1—O72.466 (4)N4—C151.470 (8)
Y1—O62.468 (4)N5—C221.421 (10)
Y1—O42.471 (4)N5—C91.438 (10)
P1—O31.483 (4)N6—C241.449 (9)
P1—N91.600 (6)N6—C231.477 (9)
P1—N81.610 (7)N7—C181.428 (11)
P1—N71.627 (7)N7—C121.476 (10)
P2—O101.495 (4)N8—C171.429 (11)
P2—N101.605 (5)N8—C61.479 (11)
P2—N111.619 (6)N9—C101.477 (9)
P2—N121.642 (6)N9—C161.486 (9)
P3—O21.497 (4)N10—C211.442 (8)
P3—N31.622 (5)N10—C81.462 (9)
P3—N11.628 (6)N11—C131.432 (12)
P3—N21.631 (5)N11—C201.472 (11)
P4—O11.485 (4)N12—C111.436 (9)
P4—N61.628 (6)N12—C191.466 (9)
P4—N41.646 (5)W1—S42.1943 (16)
P4—N51.647 (6)W1—S32.2000 (16)
O4—N131.260 (6)W1—S22.2050 (14)
O5—N131.270 (6)W1—S12.2063 (15)
O6—N141.275 (6)W1—Ag12.9549 (7)
O7—N141.266 (6)W1—Ag1i2.9791 (7)
O8—N141.221 (6)Ag1—S12.4960 (16)
O9—N131.222 (6)Ag1—S22.5698 (16)
N1—C31.460 (8)Ag1—S3ii2.6236 (17)
N1—C71.462 (9)Ag1—S4ii2.6293 (18)
O3—Y1—O292.57 (14)N13—O5—Y196.2 (3)
O3—Y1—O1088.97 (14)N14—O6—Y195.5 (3)
O2—Y1—O10157.01 (13)N14—O7—Y195.8 (3)
O3—Y1—O1157.99 (14)P2—O10—Y1159.5 (2)
O2—Y1—O193.76 (14)C3—N1—C7114.7 (6)
O10—Y1—O193.32 (14)C3—N1—P3125.0 (5)
O3—Y1—O5128.53 (13)C7—N1—P3119.7 (5)
O2—Y1—O580.13 (14)C2—N2—C4114.6 (5)
O10—Y1—O581.00 (14)C2—N2—P3120.2 (4)
O1—Y1—O573.37 (13)C4—N2—P3122.1 (5)
O3—Y1—O780.11 (14)C1—N3—C5115.4 (7)
O2—Y1—O775.36 (13)C1—N3—P3119.2 (6)
O10—Y1—O7127.40 (13)C5—N3—P3124.5 (7)
O1—Y1—O781.14 (13)C14—N4—C15113.9 (6)
O5—Y1—O7143.13 (13)C14—N4—P4119.7 (5)
O3—Y1—O679.26 (14)C15—N4—P4120.4 (4)
O2—Y1—O6127.21 (13)C22—N5—C9110.7 (7)
O10—Y1—O675.60 (13)C22—N5—P4124.2 (5)
O1—Y1—O680.13 (13)C9—N5—P4120.8 (5)
O5—Y1—O6143.31 (13)C24—N6—C23117.1 (7)
O7—Y1—O651.85 (13)C24—N6—P4120.3 (5)
O3—Y1—O476.59 (14)C23—N6—P4119.5 (5)
O2—Y1—O477.82 (13)C18—N7—C12113.1 (8)
O10—Y1—O480.25 (13)C18—N7—P1123.0 (5)
O1—Y1—O4125.37 (13)C12—N7—P1123.7 (7)
O5—Y1—O452.00 (12)C17—N8—C6116.1 (9)
O7—Y1—O4143.34 (13)C17—N8—P1121.1 (6)
O6—Y1—O4145.91 (13)C6—N8—P1122.7 (8)
O3—Y1—N13102.53 (15)C10—N9—C16115.4 (6)
O2—Y1—N1376.64 (15)C10—N9—P1123.9 (5)
O10—Y1—N1380.63 (15)C16—N9—P1119.0 (5)
O1—Y1—N1399.44 (15)C21—N10—C8113.3 (6)
O5—Y1—N1326.10 (13)C21—N10—P2123.1 (5)
O7—Y1—N13151.97 (14)C8—N10—P2121.6 (5)
O6—Y1—N13156.14 (14)C13—N11—C20112.7 (8)
O4—Y1—N1325.94 (13)C13—N11—P2121.3 (6)
O3—Y1—N1476.44 (14)C20—N11—P2123.1 (7)
O2—Y1—N14101.15 (14)C11—N12—C19112.7 (7)
O10—Y1—N14101.51 (14)C11—N12—P2121.7 (6)
O1—Y1—N1481.66 (14)C19—N12—P2119.0 (5)
O5—Y1—N14155.02 (13)O9—N13—O4122.1 (5)
O7—Y1—N1425.90 (12)O9—N13—O5121.2 (5)
O6—Y1—N1426.11 (13)O4—N13—O5116.7 (5)
O4—Y1—N14152.93 (13)O8—N14—O7121.3 (5)
N13—Y1—N14177.56 (15)O8—N14—O6122.5 (5)
O3—P1—N9110.0 (3)O7—N14—O6116.2 (4)
O3—P1—N8110.8 (3)S4—W1—S3109.87 (6)
N9—P1—N8108.0 (4)S4—W1—S2108.14 (6)
O3—P1—N7109.9 (3)S3—W1—S2108.73 (6)
N9—P1—N7109.9 (4)S4—W1—S1108.29 (7)
N8—P1—N7108.3 (4)S3—W1—S1108.65 (7)
O10—P2—N10108.4 (2)S2—W1—S1113.14 (6)
O10—P2—N11118.8 (3)Ag1—W1—Ag1i153.833 (10)
N10—P2—N11105.0 (3)S1—Ag1—S293.22 (5)
O10—P2—N12108.6 (3)S1—Ag1—S3ii120.54 (6)
N10—P2—N12114.1 (3)S2—Ag1—S3ii120.92 (6)
N11—P2—N12102.1 (3)S1—Ag1—S4ii120.49 (6)
O2—P3—N3110.9 (3)S2—Ag1—S4ii118.21 (6)
O2—P3—N1111.3 (3)S3ii—Ag1—S4ii86.43 (5)
N3—P3—N1107.0 (3)S1—Ag1—W146.82 (4)
O2—P3—N2108.7 (2)S2—Ag1—W146.40 (3)
N3—P3—N2109.4 (3)S3ii—Ag1—W1137.51 (4)
N1—P3—N2109.5 (3)S4ii—Ag1—W1136.04 (4)
O1—P4—N6109.5 (3)S1—Ag1—W1ii150.48 (4)
O1—P4—N4108.3 (2)S2—Ag1—W1ii116.29 (4)
N6—P4—N4115.4 (3)S3ii—Ag1—W1ii45.70 (4)
O1—P4—N5116.6 (3)S4ii—Ag1—W1ii45.54 (4)
N6—P4—N5103.8 (3)W1—Ag1—W1ii162.684 (19)
N4—P4—N5103.4 (3)W1—S1—Ag177.59 (5)
P4—O1—Y1162.6 (2)W1—S2—Ag176.04 (5)
P3—O2—Y1168.3 (2)W1—S3—Ag1i75.71 (5)
P1—O3—Y1167.3 (3)W1—S4—Ag1i75.68 (5)
N13—O4—Y195.0 (3)
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, −y+1/2, z−1/2.
Acknowledgements top

This work was supported by the National Natural Science Foundation of China (No. 50472048), the Program for New Century Excellent Talents in Universities (NCET-05–0499) and the Graduate Innovation Laboratory Center of Nanjing University of Science and Technology.

references
References top

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