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Acta Crystallogr Sect E Struct Rep Online. 2010 October 1; 66(Pt 10): m1193–m1194.
Published online 2010 September 4. doi:  10.1107/S1600536810029235
PMCID: PMC2983176

catena-Poly[[tetra­kis­(hexa­methyl­phospho­ramide-κO)bis­(nitrato-κ2 O,O′)dysprosium(III)] [silver(I)-di-μ-sulfido-tungstate(VI)-di-μ-sulfido]]

Abstract

Hexa­methyl­phospho­ramide (hmp), tetra­thio­tungstate, silver sulfide and dysprosium nitrate were self-assembled, forming an anionic [AgWS4]nn chain in the title compound, {[Dy(NO3)2(C6H18N3OP)4][AgWS4]}n. The central Dy atom in the cation is coordinated by eight O atoms from two didentate nitrate and four hmp ligands, giving rise to a distorted square anti­prismatic structure. Together with the two nitrate ligands, the cation is univalent, which leads to the anionic chain having a [WS4Ag] repeat unit. The polymeric anionic chain, with W—Ag—W and Ag—W—Ag angles 161.16 (2) and 153.606 (11)°, respectively, presents a distorted linear configuration. The title compound is isotypic with other rare earth complexes.

Related literature

For one-dimensional Mo(W)/S/Ag anionic polymers, see: Niu et al. (2004 [triangle]). For their unique properties, see: Zhang et al. (2007a [triangle]). For the structures of isotypic compounds, see: Cao et al. 2007 [triangle]) for Yb; Zhang et al. (2007b [triangle],c [triangle]) for Y and Eu; Tang et al. (2008a [triangle],b [triangle]) for Nd and La.

An external file that holds a picture, illustration, etc.
Object name is e-66-m1193-scheme1.jpg

Experimental

Crystal data

  • [Dy(NO3)2(C6H18N3OP)4][AgWS4]
  • M r = 1423.33
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-m1193-efi3.jpg
  • a = 15.790 (3) Å
  • b = 29.659 (6) Å
  • c = 11.376 (2) Å
  • β = 90.94 (3)°
  • V = 5326.8 (18) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 4.24 mm−1
  • T = 153 K
  • 0.25 × 0.2 × 0.15 mm

Data collection

  • Rigaku Saturn724+ diffractometer
  • Absorption correction: multi-scan (CrystalClear; Rigaku, 2007 [triangle]) T min = 0.376, T max = 0.529
  • 24513 measured reflections
  • 9675 independent reflections
  • 8851 reflections with I > 2.0σ(I)
  • R int = 0.029

Refinement

  • R[F 2 > 2σ(F 2)] = 0.035
  • wR(F 2) = 0.081
  • S = 1.08
  • 9675 reflections
  • 532 parameters
  • H-atom parameters constrained
  • Δρmax = 1.12 e Å−3
  • Δρmin = −0.87 e Å−3

Data collection: CrystalClear (Rigaku, 2007 [triangle]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810029235/pv2306sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810029235/pv2306Isup2.hkl

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

Acknowledgments

This work was supported by the National Natural Science Foundation of China (No. 50472048) and the Program for New Century Excellent Talents in Universities (NCET-05–0499).

supplementary crystallographic information

Comment

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

The title complex is isostructural with Yb (Cao et al. 2007), Y (Zhang et al. 2007b), Eu (Zhang et al. 2007c), Nd (Tang et al. 2008a), and La (Tang et al. 2008b) isomorphs. Dy3- in the cation of the title complex is coordinated by eight O atoms from two nitrate and four hmp ligands. Parts of dimethylamine groups from hmp ligands have large librations reflecting a small degree of thermal disorder. 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. The anionic chain in the title compound (Fig. 2) has a distorted linear configuration with W—Ag—W and Ag—W—Ag angles of 161.16 (2) and 153.606 (11) °, respectively, as reported in the other isostructural complexes quoted above.

Experimental

Ag2S (1 mmol) was added to a solution of [NH4]2WS4 (2 mmol in 30 mL hmp) with thorough stirring for 6 h. The solution underwent an additional stirring for two minute after Dy(NO3)3.6H2O (1 mmol) was added. After filtration the orange-red filtrate was carefully laid on the surface with 30 ml i-PrOH. Orange-red block crystals were obtained after ten days.

Refinement

H atoms were positioned geometrically and refined with riding model, with C—H = 0.96 Å and Uiso = 1.5Ueq(C). The final difference map had a residual electron density in the close proximity of W1 (1.0 Å).

Figures

Fig. 1.
The molecular structure of the cation in the title compound, with atomic labels and 30% probability displacement ellipsoids; H atoms have been omitted for clarity.
Fig. 2.
The molecular structure of a portion of the anionic chain in the title compound, with atomic labels and 30% probability displacement ellipsoids, Symmetry code: (i) x, 1/2 - y, -1/2 + z.

Crystal data

[Dy(NO3)2(C6H18N3OP)4][AgWS4]F(000) = 2820.0
Mr = 1423.33Dx = 1.775 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 22684 reflections
a = 15.790 (3) Åθ = 3.1–29.1°
b = 29.659 (6) ŵ = 4.24 mm1
c = 11.376 (2) ÅT = 153 K
β = 90.94 (3)°Block, orange-red
V = 5326.8 (18) Å30.25 × 0.2 × 0.15 mm
Z = 4

Data collection

Rigaku Saturn724+ diffractometer9675 independent reflections
Radiation source: fine-focus sealed tube8851 reflections with I > 2.0σ(I)
graphiteRint = 0.029
dtprofit.ref scansθmax = 25.4°, θmin = 3.2°
Absorption correction: multi-scan (CrystalClear; Rigaku, 2008)h = −19→13
Tmin = 0.376, Tmax = 0.529k = −35→33
24513 measured reflectionsl = −13→11

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H-atom parameters constrained
S = 1.08w = 1/[σ2(Fo2) + (0.0212P)2 + 31.1497P] where P = (Fo2 + 2Fc2)/3
9675 reflections(Δ/σ)max = 0.002
532 parametersΔρmax = 1.12 e Å3
0 restraintsΔρmin = −0.87 e Å3

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*/Ueq
Dy10.737898 (16)0.082563 (8)0.82753 (2)0.01918 (7)
P10.69823 (11)−0.03058 (5)0.69847 (15)0.0279 (4)
P20.52175 (10)0.13308 (5)0.82312 (14)0.0264 (3)
P30.95850 (10)0.09625 (5)0.73112 (15)0.0270 (3)
P40.79491 (13)0.14651 (6)1.09706 (16)0.0374 (4)
O10.7239 (3)0.10325 (13)0.6185 (4)0.0314 (10)
O20.7515 (3)0.15839 (13)0.7372 (4)0.0330 (10)
O30.7248 (4)0.17207 (18)0.5529 (5)0.0659 (17)
O40.8012 (3)0.02649 (14)0.9650 (4)0.0296 (10)
O50.6686 (3)0.04061 (14)0.9886 (4)0.0290 (9)
O60.7373 (3)0.00133 (18)1.1211 (5)0.0513 (14)
O70.8757 (3)0.08065 (13)0.7803 (4)0.0299 (10)
O80.7725 (3)0.12697 (14)0.9816 (4)0.0302 (10)
O90.6029 (2)0.10699 (13)0.8235 (4)0.0266 (9)
O100.7065 (3)0.01790 (12)0.7279 (4)0.0265 (9)
N10.7335 (3)0.14548 (17)0.6337 (5)0.0332 (12)
N20.7359 (3)0.02203 (17)1.0282 (5)0.0301 (12)
N30.5230 (4)0.17275 (19)0.9225 (6)0.0427 (15)
N40.4445 (3)0.09787 (18)0.8495 (5)0.0305 (12)
N50.5054 (4)0.1574 (2)0.6976 (5)0.0460 (16)
N61.0341 (3)0.0709 (2)0.8051 (5)0.0404 (15)
N70.9563 (4)0.0862 (2)0.5892 (5)0.0447 (15)
N80.9832 (4)0.14921 (18)0.7390 (6)0.0416 (15)
N90.8966 (5)0.1385 (2)1.1236 (7)0.070 (2)
N100.7754 (5)0.20026 (19)1.0959 (5)0.0480 (17)
N110.7407 (6)0.1235 (2)1.2007 (6)0.067 (2)
N120.7204 (4)−0.03686 (17)0.5586 (5)0.0350 (13)
N130.7634 (4)−0.06550 (18)0.7666 (5)0.0437 (15)
N140.6045 (4)−0.0481 (2)0.7376 (6)0.0475 (16)
C11.0210 (5)0.0280 (3)0.8613 (8)0.060 (2)
H1A1.07240.01860.90030.090*
H1B1.00500.00590.80320.090*
H1C0.97680.03070.91790.090*
C20.7254 (5)−0.0827 (2)0.5060 (7)0.050 (2)
H2A0.7390−0.08020.42430.074*
H2B0.6717−0.09760.51340.074*
H2C0.7685−0.09980.54620.074*
C30.6974 (6)−0.0024 (3)0.4746 (6)0.052 (2)
H3A0.7153−0.01140.39780.078*
H3B0.72450.02540.49620.078*
H3C0.63710.00160.47380.078*
C41.1232 (5)0.0803 (4)0.7827 (9)0.080 (3)
H4A1.15820.06240.83440.120*
H4B1.13450.11170.79630.120*
H4C1.13560.07300.70260.120*
C50.9516 (5)0.1825 (3)0.6534 (11)0.082 (4)
H5A0.97340.21180.67360.124*
H5B0.89080.18320.65450.124*
H5C0.96990.17440.57620.124*
C60.5348 (5)−0.0163 (3)0.7479 (8)0.059 (2)
H6A0.4848−0.03210.77140.089*
H6B0.5245−0.00190.67340.089*
H6C0.54920.00610.80580.089*
C70.9085 (5)0.0481 (3)0.5430 (7)0.057 (2)
H7A0.91400.04690.45910.085*
H7B0.84980.05160.56210.085*
H7C0.92990.02070.57710.085*
C80.8031 (5)0.2273 (2)0.9966 (6)0.0473 (19)
H8A0.78710.25821.00840.071*
H8B0.77680.21620.92560.071*
H8C0.86350.22520.99040.071*
C90.3560 (4)0.1074 (3)0.8127 (7)0.0473 (19)
H9A0.32030.08290.83630.071*
H9B0.35290.11070.72880.071*
H9C0.33740.13470.84920.071*
C100.4541 (5)0.1828 (3)1.0010 (8)0.059 (2)
H10A0.47000.20751.05130.088*
H10B0.44210.15681.04800.088*
H10C0.40450.19090.95570.088*
C110.4536 (4)0.0646 (2)0.9424 (6)0.0401 (17)
H11A0.40290.04680.94620.060*
H11B0.46310.07961.01620.060*
H11C0.50080.04530.92620.060*
C120.5800 (7)−0.0956 (3)0.7198 (9)0.080 (3)
H12A0.5232−0.10010.74650.120*
H12B0.6180−0.11480.76350.120*
H12C0.5827−0.10290.63770.120*
C130.5903 (5)0.2069 (3)0.9216 (9)0.062 (2)
H13A0.58230.22770.98520.093*
H13B0.58840.22290.84830.093*
H13C0.64440.19240.93090.093*
C140.7521 (6)−0.0815 (3)0.8850 (8)0.068 (3)
H14A0.7979−0.10130.90630.102*
H14B0.6994−0.09740.88960.102*
H14C0.7515−0.05630.93800.102*
C150.6502 (7)0.1205 (3)1.1889 (9)0.082 (3)
H15A0.62760.10631.25740.123*
H15B0.63570.10311.12050.123*
H15C0.62680.15031.18100.123*
C161.0306 (6)0.0958 (4)0.5173 (8)0.076 (3)
H16A1.01860.08770.43710.115*
H16B1.07820.07870.54630.115*
H16C1.04360.12740.52170.115*
C170.5188 (6)0.1331 (4)0.5901 (7)0.074 (3)
H17A0.50590.15230.52430.111*
H17B0.48250.10710.58740.111*
H17C0.57680.12360.58680.111*
C180.7504 (8)0.2257 (3)1.1997 (8)0.091 (4)
H18A0.74220.25681.17880.137*
H18B0.79400.22341.25910.137*
H18C0.69850.21361.22920.137*
C190.8530 (6)−0.0677 (3)0.7356 (9)0.075 (3)
H19A0.8812−0.08970.78420.113*
H19B0.8787−0.03870.74760.113*
H19C0.8577−0.07620.65450.113*
C201.0133 (7)0.1691 (3)0.8496 (9)0.088 (4)
H20A1.02470.20060.83800.133*
H20B1.06420.15410.87520.133*
H20C0.97070.16570.90820.133*
C210.9359 (6)0.0957 (3)1.1106 (10)0.082 (3)
H21A0.99490.09801.13170.123*
H21B0.93020.08601.03040.123*
H21C0.90910.07421.16100.123*
C220.9519 (8)0.1714 (4)1.1835 (11)0.105 (5)
H22A1.00820.15941.19040.158*
H22B0.93050.17761.26040.158*
H22C0.95300.19891.13870.158*
C230.7820 (10)0.1057 (4)1.3109 (9)0.119 (5)
H23A0.73960.09361.36150.179*
H23B0.81150.12981.35070.179*
H23C0.82160.08251.29120.179*
C240.4636 (6)0.2014 (3)0.6817 (9)0.077 (3)
H24A0.46090.20870.59950.116*
H24B0.49540.22410.72310.116*
H24C0.40730.20000.71200.116*
W10.216043 (15)0.227581 (7)0.47517 (2)0.02023 (7)
Ag10.21731 (4)0.234185 (17)0.21464 (4)0.03708 (13)
S10.10252 (11)0.21233 (6)0.36887 (14)0.0353 (4)
S20.21400 (11)0.18483 (5)0.63413 (13)0.0298 (3)
S30.33048 (10)0.21154 (6)0.37526 (14)0.0340 (4)
S40.21630 (11)0.30059 (5)0.51519 (14)0.0326 (4)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Dy10.01654 (13)0.01366 (12)0.02736 (15)−0.00042 (10)0.00137 (10)−0.00093 (11)
P10.0336 (9)0.0183 (7)0.0322 (9)−0.0052 (6)0.0095 (7)−0.0047 (7)
P20.0185 (8)0.0312 (8)0.0296 (8)0.0052 (6)0.0002 (6)0.0048 (7)
P30.0173 (8)0.0245 (8)0.0394 (9)0.0004 (6)0.0043 (7)0.0078 (7)
P40.0558 (12)0.0242 (8)0.0316 (9)−0.0101 (8)−0.0166 (8)0.0004 (7)
O10.041 (3)0.022 (2)0.031 (2)0.0000 (19)0.004 (2)−0.0011 (19)
O20.038 (3)0.020 (2)0.041 (3)−0.0046 (18)−0.002 (2)0.003 (2)
O30.106 (5)0.043 (3)0.049 (3)−0.017 (3)−0.012 (3)0.025 (3)
O40.021 (2)0.026 (2)0.042 (3)0.0001 (17)−0.0023 (19)0.007 (2)
O50.026 (2)0.027 (2)0.034 (2)0.0015 (18)−0.0001 (19)0.0042 (19)
O60.051 (3)0.056 (3)0.047 (3)−0.004 (3)−0.003 (2)0.026 (3)
O70.022 (2)0.025 (2)0.043 (3)−0.0013 (17)0.0023 (19)0.0056 (19)
O80.030 (2)0.026 (2)0.035 (2)−0.0003 (18)−0.0073 (19)−0.0091 (19)
O90.016 (2)0.025 (2)0.039 (2)0.0034 (16)0.0001 (17)0.0007 (19)
O100.032 (2)0.0165 (19)0.031 (2)−0.0024 (17)0.0003 (18)−0.0009 (18)
N10.037 (3)0.025 (3)0.038 (3)−0.003 (2)0.000 (2)0.008 (3)
N20.031 (3)0.024 (3)0.036 (3)−0.004 (2)−0.001 (2)0.002 (2)
N30.032 (3)0.036 (3)0.061 (4)0.007 (3)0.007 (3)−0.006 (3)
N40.017 (3)0.038 (3)0.036 (3)0.000 (2)−0.002 (2)0.008 (3)
N50.035 (3)0.068 (4)0.035 (3)−0.004 (3)−0.007 (3)0.022 (3)
N60.020 (3)0.050 (4)0.051 (4)−0.001 (2)0.002 (3)0.027 (3)
N70.033 (3)0.057 (4)0.044 (4)−0.008 (3)0.006 (3)0.005 (3)
N80.037 (3)0.025 (3)0.063 (4)−0.002 (2)0.010 (3)0.007 (3)
N90.072 (5)0.050 (4)0.087 (6)−0.013 (4)−0.049 (4)0.001 (4)
N100.086 (5)0.025 (3)0.032 (3)−0.008 (3)0.004 (3)−0.006 (3)
N110.110 (7)0.049 (4)0.043 (4)−0.028 (4)−0.005 (4)0.006 (3)
N120.047 (4)0.026 (3)0.032 (3)−0.003 (2)0.007 (3)−0.004 (2)
N130.067 (4)0.020 (3)0.044 (3)0.007 (3)0.018 (3)0.008 (3)
N140.041 (4)0.042 (3)0.060 (4)−0.019 (3)0.018 (3)−0.018 (3)
C10.035 (4)0.060 (5)0.085 (6)0.005 (4)0.002 (4)0.039 (5)
C20.070 (6)0.032 (4)0.047 (4)−0.008 (4)0.019 (4)−0.014 (3)
C30.071 (6)0.048 (5)0.036 (4)−0.005 (4)−0.003 (4)0.001 (4)
C40.021 (4)0.111 (8)0.108 (8)0.004 (4)0.006 (4)0.065 (7)
C50.046 (5)0.040 (5)0.161 (11)0.008 (4)0.016 (6)0.056 (6)
C60.028 (4)0.064 (5)0.086 (7)0.001 (4)−0.003 (4)0.012 (5)
C70.040 (5)0.075 (6)0.054 (5)0.001 (4)0.003 (4)−0.016 (5)
C80.073 (6)0.028 (4)0.041 (4)−0.005 (3)0.004 (4)−0.004 (3)
C90.021 (4)0.066 (5)0.055 (5)−0.003 (3)−0.002 (3)0.010 (4)
C100.056 (5)0.054 (5)0.067 (6)0.020 (4)0.021 (4)−0.006 (4)
C110.026 (4)0.048 (4)0.046 (4)−0.001 (3)0.007 (3)0.008 (4)
C120.090 (7)0.054 (5)0.098 (8)−0.039 (5)0.045 (6)−0.026 (5)
C130.053 (5)0.038 (4)0.096 (7)−0.005 (4)0.016 (5)−0.013 (5)
C140.081 (7)0.054 (5)0.069 (6)0.020 (5)0.013 (5)0.015 (5)
C150.105 (9)0.072 (6)0.071 (7)−0.039 (6)0.044 (6)−0.005 (5)
C160.064 (6)0.113 (8)0.053 (5)−0.020 (6)0.023 (5)0.006 (6)
C170.055 (6)0.131 (9)0.036 (5)−0.007 (6)−0.008 (4)0.007 (5)
C180.177 (12)0.049 (5)0.050 (5)−0.039 (6)0.045 (7)−0.030 (5)
C190.050 (6)0.081 (7)0.095 (8)0.017 (5)0.011 (5)0.022 (6)
C200.104 (9)0.073 (7)0.089 (8)−0.053 (6)0.035 (6)−0.030 (6)
C210.057 (6)0.068 (6)0.119 (9)−0.006 (5)−0.042 (6)0.017 (6)
C220.117 (10)0.085 (8)0.113 (10)−0.040 (7)−0.070 (8)0.008 (7)
C230.206 (16)0.110 (10)0.043 (6)0.025 (10)0.019 (8)0.032 (6)
C240.058 (6)0.074 (6)0.100 (8)0.014 (5)−0.005 (5)0.051 (6)
W10.02434 (13)0.01905 (12)0.01724 (12)−0.00250 (9)−0.00159 (9)0.00094 (9)
Ag10.0573 (3)0.0347 (3)0.0192 (2)0.0006 (2)−0.0009 (2)0.0018 (2)
S10.0298 (9)0.0480 (10)0.0279 (8)−0.0136 (7)−0.0060 (7)0.0045 (8)
S20.0448 (10)0.0215 (7)0.0231 (8)0.0000 (6)0.0021 (7)0.0063 (6)
S30.0306 (9)0.0442 (9)0.0272 (8)0.0058 (7)0.0018 (7)0.0042 (7)
S40.0520 (11)0.0186 (7)0.0271 (8)−0.0041 (7)0.0002 (7)0.0019 (6)

Geometric parameters (Å, °)

Dy1—O72.250 (4)C6—H6A0.9600
Dy1—O92.252 (4)C6—H6B0.9600
Dy1—O82.253 (4)C6—H6C0.9600
Dy1—O102.278 (4)C7—H7A0.9600
Dy1—O12.463 (4)C7—H7B0.9600
Dy1—O22.483 (4)C7—H7C0.9600
Dy1—O52.484 (4)C8—H8A0.9600
Dy1—O42.482 (4)C8—H8B0.9600
Dy1—N12.888 (5)C8—H8C0.9600
Dy1—N22.905 (5)C9—H9A0.9600
P1—O101.482 (4)C9—H9B0.9600
P1—N141.637 (6)C9—H9C0.9600
P1—N131.644 (6)C10—H10A0.9600
P1—N121.645 (5)C10—H10B0.9600
P2—O91.496 (4)C10—H10C0.9600
P2—N51.617 (6)C11—H11A0.9600
P2—N31.631 (6)C11—H11B0.9600
P2—N41.637 (5)C11—H11C0.9600
P3—O71.504 (4)C12—H12A0.9600
P3—N81.620 (6)C12—H12B0.9600
P3—N61.633 (6)C12—H12C0.9600
P3—N71.642 (6)C13—H13A0.9600
P4—O81.473 (4)C13—H13B0.9600
P4—N111.619 (7)C13—H13C0.9600
P4—N101.623 (6)C14—H14A0.9600
P4—N91.647 (8)C14—H14B0.9600
O1—N11.273 (6)C14—H14C0.9600
O2—N11.265 (7)C15—H15A0.9600
O3—N11.218 (7)C15—H15B0.9600
O4—N21.274 (6)C15—H15C0.9600
O5—N21.272 (6)C16—H16A0.9600
O6—N21.222 (7)C16—H16B0.9600
N3—C101.450 (9)C16—H16C0.9600
N3—C131.469 (9)C17—H17A0.9600
N4—C111.452 (8)C17—H17B0.9600
N4—C91.480 (8)C17—H17C0.9600
N5—C171.438 (11)C18—H18A0.9600
N5—C241.471 (10)C18—H18B0.9600
N6—C11.441 (9)C18—H18C0.9600
N6—C41.462 (9)C19—H19A0.9600
N7—C71.452 (10)C19—H19B0.9600
N7—C161.469 (9)C19—H19C0.9600
N8—C201.462 (11)C20—H20A0.9600
N8—C51.469 (10)C20—H20B0.9600
N9—C211.422 (12)C20—H20C0.9600
N9—C221.469 (11)C21—H21A0.9600
N10—C81.457 (9)C21—H21B0.9600
N10—C181.461 (10)C21—H21C0.9600
N11—C151.436 (13)C22—H22A0.9600
N11—C231.500 (12)C22—H22B0.9600
N12—C31.442 (9)C22—H22C0.9600
N12—C21.487 (8)C23—H23A0.9600
N13—C141.442 (10)C23—H23B0.9600
N13—C191.465 (10)C23—H23C0.9600
N14—C61.455 (10)C24—H24A0.9600
N14—C121.476 (9)C24—H24B0.9600
C1—H1A0.9600C24—H24C0.9600
C1—H1B0.9600W1—S12.1929 (17)
C1—H1C0.9600W1—S32.2025 (17)
C2—H2A0.9600W1—S22.2092 (15)
C2—H2B0.9600W1—S42.2125 (16)
C2—H2C0.9600W1—Ag1i2.9506 (7)
C3—H3A0.9600W1—Ag12.9706 (7)
C3—H3B0.9600Ag1—S4ii2.4922 (17)
C3—H3C0.9600Ag1—S2ii2.5708 (17)
C4—H4A0.9600Ag1—S32.6222 (19)
C4—H4B0.9600Ag1—S12.6244 (19)
C4—H4C0.9600Ag1—W1ii2.9506 (7)
C5—H5A0.9600S2—Ag1i2.5708 (17)
C5—H5B0.9600S4—Ag1i2.4922 (17)
C5—H5C0.9600
O7—Dy1—O9157.26 (15)N8—C5—H5C109.5
O7—Dy1—O888.71 (16)H5A—C5—H5C109.5
O9—Dy1—O892.58 (15)H5B—C5—H5C109.5
O7—Dy1—O1093.63 (15)N14—C6—H6A109.5
O9—Dy1—O1093.58 (15)N14—C6—H6B109.5
O8—Dy1—O10158.03 (15)H6A—C6—H6B109.5
O7—Dy1—O181.23 (15)N14—C6—H6C109.5
O9—Dy1—O180.24 (15)H6A—C6—H6C109.5
O8—Dy1—O1128.50 (15)H6B—C6—H6C109.5
O10—Dy1—O173.38 (14)N7—C7—H7A109.5
O7—Dy1—O280.41 (15)N7—C7—H7B109.5
O9—Dy1—O277.81 (15)H7A—C7—H7B109.5
O8—Dy1—O276.76 (15)N7—C7—H7C109.5
O10—Dy1—O2125.17 (15)H7A—C7—H7C109.5
O1—Dy1—O251.80 (14)H7B—C7—H7C109.5
O7—Dy1—O5127.06 (14)N10—C8—H8A109.5
O9—Dy1—O575.40 (14)N10—C8—H8B109.5
O8—Dy1—O579.80 (15)H8A—C8—H8B109.5
O10—Dy1—O581.40 (14)N10—C8—H8C109.5
O1—Dy1—O5143.50 (14)H8A—C8—H8C109.5
O2—Dy1—O5143.26 (14)H8B—C8—H8C109.5
O7—Dy1—O475.68 (14)N4—C9—H9A109.5
O9—Dy1—O4126.85 (14)N4—C9—H9B109.5
O8—Dy1—O479.13 (15)H9A—C9—H9B109.5
O10—Dy1—O480.31 (14)N4—C9—H9C109.5
O1—Dy1—O4143.56 (14)H9A—C9—H9C109.5
O2—Dy1—O4146.19 (14)H9B—C9—H9C109.5
O5—Dy1—O451.45 (13)N3—C10—H10A109.5
O7—Dy1—N181.10 (15)N3—C10—H10B109.5
O9—Dy1—N176.46 (15)H10A—C10—H10B109.5
O8—Dy1—N1102.63 (16)N3—C10—H10C109.5
O10—Dy1—N199.31 (15)H10A—C10—H10C109.5
O1—Dy1—N126.00 (14)H10B—C10—H10C109.5
O2—Dy1—N125.87 (14)N4—C11—H11A109.5
O5—Dy1—N1151.84 (15)N4—C11—H11B109.5
O4—Dy1—N1156.68 (15)H11A—C11—H11B109.5
O7—Dy1—N2101.25 (15)N4—C11—H11C109.5
O9—Dy1—N2101.07 (15)H11A—C11—H11C109.5
O8—Dy1—N275.85 (15)H11B—C11—H11C109.5
O10—Dy1—N282.28 (14)N14—C12—H12A109.5
O1—Dy1—N2155.65 (14)N14—C12—H12B109.5
O2—Dy1—N2152.51 (15)H12A—C12—H12B109.5
O5—Dy1—N225.82 (13)N14—C12—H12C109.5
O4—Dy1—N225.85 (14)H12A—C12—H12C109.5
N1—Dy1—N2177.11 (15)H12B—C12—H12C109.5
O10—P1—N14108.9 (3)N3—C13—H13A109.5
O10—P1—N13116.9 (3)N3—C13—H13B109.5
N14—P1—N13103.5 (3)H13A—C13—H13B109.5
O10—P1—N12108.0 (3)N3—C13—H13C109.5
N14—P1—N12115.8 (3)H13A—C13—H13C109.5
N13—P1—N12104.0 (3)H13B—C13—H13C109.5
O9—P2—N5110.9 (3)N13—C14—H14A109.5
O9—P2—N3111.8 (3)N13—C14—H14B109.5
N5—P2—N3106.8 (3)H14A—C14—H14B109.5
O9—P2—N4108.0 (3)N13—C14—H14C109.5
N5—P2—N4109.8 (3)H14A—C14—H14C109.5
N3—P2—N4109.5 (3)H14B—C14—H14C109.5
O7—P3—N8119.2 (3)N11—C15—H15A109.5
O7—P3—N6107.4 (3)N11—C15—H15B109.5
N8—P3—N6104.2 (3)H15A—C15—H15B109.5
O7—P3—N7107.8 (3)N11—C15—H15C109.5
N8—P3—N7103.4 (3)H15A—C15—H15C109.5
N6—P3—N7115.2 (3)H15B—C15—H15C109.5
O8—P4—N11111.2 (3)N7—C16—H16A109.5
O8—P4—N10109.6 (3)N7—C16—H16B109.5
N11—P4—N10108.5 (4)H16A—C16—H16B109.5
O8—P4—N9109.1 (4)N7—C16—H16C109.5
N11—P4—N9109.4 (4)H16A—C16—H16C109.5
N10—P4—N9109.1 (4)H16B—C16—H16C109.5
N1—O1—Dy196.0 (3)N5—C17—H17A109.5
N1—O2—Dy195.2 (3)N5—C17—H17B109.5
N2—O4—Dy196.0 (3)H17A—C17—H17B109.5
N2—O5—Dy195.9 (3)N5—C17—H17C109.5
P3—O7—Dy1158.6 (3)H17A—C17—H17C109.5
P4—O8—Dy1167.2 (3)H17B—C17—H17C109.5
P2—O9—Dy1167.6 (3)N10—C18—H18A109.5
P1—O10—Dy1161.3 (3)N10—C18—H18B109.5
O3—N1—O2121.8 (5)H18A—C18—H18B109.5
O3—N1—O1121.5 (6)N10—C18—H18C109.5
O2—N1—O1116.7 (5)H18A—C18—H18C109.5
O3—N1—Dy1174.8 (5)H18B—C18—H18C109.5
O2—N1—Dy158.9 (3)N13—C19—H19A109.5
O1—N1—Dy158.0 (3)N13—C19—H19B109.5
O6—N2—O4122.4 (5)H19A—C19—H19B109.5
O6—N2—O5121.8 (5)N13—C19—H19C109.5
O4—N2—O5115.7 (5)H19A—C19—H19C109.5
O6—N2—Dy1171.8 (4)H19B—C19—H19C109.5
O4—N2—Dy158.2 (3)N8—C20—H20A109.5
O5—N2—Dy158.2 (3)N8—C20—H20B109.5
C10—N3—C13114.4 (6)H20A—C20—H20B109.5
C10—N3—P2125.1 (5)N8—C20—H20C109.5
C13—N3—P2119.5 (5)H20A—C20—H20C109.5
C11—N4—C9114.6 (5)H20B—C20—H20C109.5
C11—N4—P2120.2 (4)N9—C21—H21A109.5
C9—N4—P2122.0 (5)N9—C21—H21B109.5
C17—N5—C24114.3 (7)H21A—C21—H21B109.5
C17—N5—P2120.3 (6)N9—C21—H21C109.5
C24—N5—P2124.7 (6)H21A—C21—H21C109.5
C1—N6—C4113.1 (6)H21B—C21—H21C109.5
C1—N6—P3121.8 (5)N9—C22—H22A109.5
C4—N6—P3121.3 (5)N9—C22—H22B109.5
C7—N7—C16111.5 (7)H22A—C22—H22B109.5
C7—N7—P3120.0 (5)N9—C22—H22C109.5
C16—N7—P3120.5 (6)H22A—C22—H22C109.5
C20—N8—C5113.6 (7)H22B—C22—H22C109.5
C20—N8—P3120.9 (6)N11—C23—H23A109.5
C5—N8—P3122.5 (6)N11—C23—H23B109.5
C21—N9—C22112.7 (8)H23A—C23—H23B109.5
C21—N9—P4122.4 (6)N11—C23—H23C109.5
C22—N9—P4124.0 (8)H23A—C23—H23C109.5
C8—N10—C18115.5 (6)H23B—C23—H23C109.5
C8—N10—P4119.1 (5)N5—C24—H24A109.5
C18—N10—P4123.6 (6)N5—C24—H24B109.5
C15—N11—C23118.4 (9)H24A—C24—H24B109.5
C15—N11—P4119.7 (6)N5—C24—H24C109.5
C23—N11—P4121.9 (8)H24A—C24—H24C109.5
C3—N12—C2113.2 (6)H24B—C24—H24C109.5
C3—N12—P1120.4 (5)S1—W1—S3109.94 (7)
C2—N12—P1120.4 (5)S1—W1—S2108.07 (6)
C14—N13—C19110.2 (7)S3—W1—S2108.76 (6)
C14—N13—P1124.2 (5)S1—W1—S4108.31 (7)
C19—N13—P1120.9 (5)S3—W1—S4108.59 (7)
C6—N14—C12115.7 (7)S2—W1—S4113.16 (6)
C6—N14—P1120.3 (5)S1—W1—Ag1i125.56 (5)
C12—N14—P1120.2 (5)S3—W1—Ag1i124.49 (5)
N6—C1—H1A109.5S2—W1—Ag1i57.64 (4)
N6—C1—H1B109.5S4—W1—Ag1i55.53 (4)
H1A—C1—H1B109.5S1—W1—Ag158.82 (5)
N6—C1—H1C109.5S3—W1—Ag158.69 (5)
H1A—C1—H1C109.5S2—W1—Ag1148.75 (4)
H1B—C1—H1C109.5S4—W1—Ag198.09 (4)
N12—C2—H2A109.5Ag1i—W1—Ag1153.606 (11)
N12—C2—H2B109.5S4ii—Ag1—S2ii93.58 (5)
H2A—C2—H2B109.5S4ii—Ag1—S3121.50 (6)
N12—C2—H2C109.5S2ii—Ag1—S3119.81 (6)
H2A—C2—H2C109.5S4ii—Ag1—S1120.82 (6)
H2B—C2—H2C109.5S2ii—Ag1—S1117.31 (6)
N12—C3—H3A109.5S3—Ag1—S186.63 (5)
N12—C3—H3B109.5S4ii—Ag1—W1ii47.05 (4)
H3A—C3—H3B109.5S2ii—Ag1—W1ii46.54 (3)
N12—C3—H3C109.5S3—Ag1—W1ii137.39 (4)
H3A—C3—H3C109.5S1—Ag1—W1ii135.88 (5)
H3B—C3—H3C109.5S4ii—Ag1—W1151.77 (4)
N6—C4—H4A109.5S2ii—Ag1—W1114.62 (4)
N6—C4—H4B109.5S3—Ag1—W145.86 (4)
H4A—C4—H4B109.5S1—Ag1—W145.63 (4)
N6—C4—H4C109.5W1ii—Ag1—W1161.16 (2)
H4A—C4—H4C109.5W1—S1—Ag175.55 (5)
H4B—C4—H4C109.5W1—S2—Ag1i75.81 (5)
N8—C5—H5A109.5W1—S3—Ag175.45 (5)
N8—C5—H5B109.5W1—S4—Ag1i77.43 (5)
H5A—C5—H5B109.5

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: PV2306).

References

  • Cao, Y., Zhang, J.-F., Qian, J. & Zhang, C. (2007). Acta Cryst. E63, m2076–m2077.
  • Niu, Y. Y., Zheng, H. G., Hou, H. W. & Xin, X. Q. (2004). Coord. Chem. Rev.248, 169–183.
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  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Tang, G., Zhang, J. & Zhang, C. (2008a). Acta Cryst. E64, m478. [PMC free article] [PubMed]
  • Tang, G., Zhang, J., Zhang, C. & Lu, L. (2008b). Acta Cryst. E64, m399–m400. [PMC free article] [PubMed]
  • Zhang, J.-F., Cao, Y., Qian, J. & Zhang, C. (2007b). Acta Cryst. E63, m2248–m2249.
  • Zhang, J., Qian, J., Cao, Y. & Zhang, C. (2007c). Acta Cryst. E63, m2386–m2387.
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