metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 69| Part 1| January 2013| Pages m43-m44

catena-Poly[[tetra­kis­(hexa­methyl­phospho­ramide-κO)bis­­(nitrato-κ2O,O′)erbium(III)] [silver(I)-di-μ-sulfido-tungstate(VI)-di-μ-sulfido]]

aInstitute of Molecular Engineering and Advanced Materials, School of Chemical Engineering, Nanjing University of Science and Technology, 200 Xiaolingwei, Nanjing 210094, Jiangsu, People's Republic of China, and bInstitute of Science and Technology, Jiangsu University, 301 Xuefu Road, Zhenjiang 212013, People's Republic of China
*Correspondence e-mail: chizhang@mail.njust.edu.cn

(Received 29 November 2012; accepted 6 December 2012; online 12 December 2012)

In the title compound, {[Er(NO3)2(C6H18N3OP)4][AgWS4]}n, the polymeric anionic chain {[AgWS4]}n extends along [001]. The ErIII atom in the cation is coordinated by eight O atoms from two bidentate nitrate anions and four hexa­methyl­phospho­ramide ligands in a distorted square-anti­prismatic geometry. Together with the two nitrate ligands, the cation is monovalent, which leads to the anionic chain having a [WS4Ag] repeat unit. The polymeric anionic chain has a distorted linear configuration, with W—Ag—W and Ag—W—Ag angles of 161.37 (2) and 153.548 (12)°, respectively. The title complex is isotypic with the Y, Yb, Eu, Nd, La, Dy, Sm, Lu and Tb analogues.

Related literature

For one-dimensional Mo(W)/S/Ag anionic polymers, see: Niu et al. (2004[Niu, Y. Y., Zheng, H. G., Hou, H. W. & Xin, X. Q. (2004). Coord. Chem. Rev. 248, 169-183.]); Zhang et al. (2010[Zhang, J. F., Meng, S. C., Song, Y. L., Zhao, H. J., Li, J. H., Qu, G. J., Sun, L., Humphrey, M. G. & Zhang, C. (2010). Chem. Eur. J. 16, 13946-13950.]). For their unique properties, see: Zhang, Song et al. (2007[Zhang, C., Song, Y. L. & Wang, X. (2007). Coord. Chem. Rev. 251, 111-141.]). For isotypic compounds, see: Zhang, Cao et al. (2007[Zhang, J.-F., Cao, Y., Qian, J. & Zhang, C. (2007). Acta Cryst. E63, m2248-m2249.]); Cao et al. (2007[Cao, Y., Zhang, J.-F., Qian, J. & Zhang, C. (2007). Acta Cryst. E63, m2076-m2077.]); Zhang, Qian et al. (2007[Zhang, J., Qian, J., Cao, Y. & Zhang, C. (2007). Acta Cryst. E63, m2386-m2387.]); Tang, Zhang & Zhang (2008[Tang, G., Zhang, J. & Zhang, C. (2008). Acta Cryst. E64, m478.]); Tang, Zhang, Zhang & Lu (2008[Tang, G., Zhang, J., Zhang, C. & Lu, L. (2008). Acta Cryst. E64, m399-m400.]); Zhang (2010[Zhang, J. (2010). Acta Cryst. E66, m1479.]); Zhang (2011a[Zhang, J. (2011a). Acta Cryst. E67, m1206-m1207.],b[Zhang, J. (2011b). Acta Cryst. E67, m1365.]); Zhang (2012a[Zhang, J. (2012a). Acta Cryst. E68, m770-m771.],b[Zhang, J. (2012b). Acta Cryst. E68, m843-m844.]).

[Scheme 1]

Experimental

Crystal data
  • [Er(NO3)2(C6H18N3OP)4][AgWS4]

  • Mr = 1428.09

  • Monoclinic, P 21 /c

  • a = 15.763 (3) Å

  • b = 29.579 (6) Å

  • c = 11.368 (2) Å

  • β = 90.83 (3)°

  • V = 5299.8 (17) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 4.43 mm−1

  • T = 150 K

  • 0.2 × 0.17 × 0.15 mm

Data collection
  • Rigaku Saturn724+ diffractometer

  • Absorption correction: multi-scan (CrystalClear; Rigaku, 2008[Rigaku (2008). CrystalClear. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.428, Tmax = 0.514

  • 26753 measured reflections

  • 9597 independent reflections

  • 8722 reflections with I > 2σ(I)

  • Rint = 0.044

  • Standard reflections: 0

Refinement
  • R[F2 > 2σ(F2)] = 0.047

  • wR(F2) = 0.092

  • S = 1.08

  • 9597 reflections

  • 532 parameters

  • H-atom parameters constrained

  • Δρmax = 0.91 e Å−3

  • Δρmin = −1.04 e Å−3

Data collection: CrystalClear (Rigaku, 2008[Rigaku (2008). CrystalClear. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

One-dimensional Mo(W)/S/Ag anionic polymers have attracted much attention for their configurational isomerism (Niu et al., 2004; Zhang, Meng et al., 2010) and unique properties as functional materials, such as third-order nonlinear optical (NLO) materials (Zhang, Song et al., 2007). Different solvent-coordinated rare-earth cations proved effective to obtain various configurations of anionic chains (Niu et al., 2004). The title compound, {[Er(hmp)4(NO3)2][WS4Ag]}n (hmp = hexamethylphosphoramide) with a wave-like anionic chain, was prepared by following such route using Er(III)-hmp complex as counterion.

The title complex is isostructural with Y (Zhang, Cao et al., 2007; Zhang, 2011a), Yb (Cao et al., 2007), Eu (Zhang, Qian et al., 2007), Nd (Tang, Zhang & Zhang, 2008), La (Tang, Zhang, Zhang & Lu, 2008), Dy (Zhang, 2010), Sm (Zhang, 2011b), Lu (Zhang, 2012a) and Tb (Zhang, 2012b) isomorphs. ErIII in the cation is coordinated by eight O atoms from two nitrate and four hmp ligands. 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. 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 161.37 (2) and 153.548 (12)°, respectively.

Related literature top

For one-dimensional Mo(W)/S/Ag anionic polymers, see: Niu et al. (2004); Zhang, Meng et al. (2010). For their unique properties, see: Zhang, Song et al. (2007). For isotypic compounds, see: Zhang, Cao et al. (2007); Cao et al. (2007); Zhang, Qian et al. (2007); Tang, Zhang & Zhang (2008); Tang, Zhang, Zhang & Lu (2008); Zhang (2010); Zhang (2011a,b); Zhang (2012a,b).

Experimental top

1 mmol AgI was added to a solution of [NH4]2WS4 (1 mmol in 10 ml hmp) with thorough stirring for 30 minutes. The solution underwent an additional stir for two minute after 0.5 mmol Er(NO3)3.6H2O was added. After filtration the orange filtrate was carefully laid on the surface with 15 ml i-PrOH. Orange block crystals were obtained after about one week.

Refinement top

H atoms were positioned geometrically and refined with riding model, with Uiso = 1.5Ueq(C) and 0.96 Å for C—H bonds.

Computing details top

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

Figures top
[Figure 1] Fig. 1. The molecular structure of the cation in the title compound, with 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 30% probability displacement ellipsoids. Symmetry code: (i) x,-y + 1/2,z + 1/2.
catena-Poly[[tetrakis(hexamethylphosphoramide-κO)bis(nitrato- κ2O,O')erbium(III)] [silver(I)-di-µ-sulfido-tungstate(VI)-di-µ-sulfido]] top
Crystal data top
[Er(NO3)2(C6H18N3OP)4][AgWS4]F(000) = 2828
Mr = 1428.09Dx = 1.790 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 16527 reflections
a = 15.763 (3) Åθ = 3.2–29.1°
b = 29.579 (6) ŵ = 4.43 mm1
c = 11.368 (2) ÅT = 150 K
β = 90.83 (3)°Block, orange
V = 5299.8 (17) Å30.2 × 0.17 × 0.15 mm
Z = 4
Data collection top
Rigaku Saturn724+
diffractometer
9597 independent reflections
Radiation source: fine-focus sealed tube8722 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.044
ω scansθmax = 25.4°, θmin = 3.2°
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2008)
h = 1518
Tmin = 0.428, Tmax = 0.514k = 3533
26753 measured reflectionsl = 1311
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)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.092H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.024P)2 + 26.5377P]
where P = (Fo2 + 2Fc2)/3
9597 reflections(Δ/σ)max = 0.001
532 parametersΔρmax = 0.91 e Å3
0 restraintsΔρmin = 1.04 e Å3
Crystal data top
[Er(NO3)2(C6H18N3OP)4][AgWS4]V = 5299.8 (17) Å3
Mr = 1428.09Z = 4
Monoclinic, P21/cMo Kα radiation
a = 15.763 (3) ŵ = 4.43 mm1
b = 29.579 (6) ÅT = 150 K
c = 11.368 (2) Å0.2 × 0.17 × 0.15 mm
β = 90.83 (3)°
Data collection top
Rigaku Saturn724+
diffractometer
9597 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2008)
8722 reflections with I > 2σ(I)
Tmin = 0.428, Tmax = 0.514Rint = 0.044
26753 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0470 restraints
wR(F2) = 0.092H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.024P)2 + 26.5377P]
where P = (Fo2 + 2Fc2)/3
9597 reflectionsΔρmax = 0.91 e Å3
532 parametersΔρmin = 1.04 e Å3
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
Er10.261717 (18)0.082599 (10)0.17242 (3)0.02182 (9)
P10.30083 (12)0.03020 (6)0.29957 (18)0.0304 (4)
P20.47743 (11)0.13250 (6)0.17898 (17)0.0283 (4)
P30.20599 (14)0.14671 (7)0.09571 (19)0.0396 (5)
P40.04219 (11)0.09630 (6)0.26880 (18)0.0301 (4)
O10.2929 (3)0.01824 (14)0.2704 (4)0.0286 (11)
O20.3962 (3)0.10679 (15)0.1766 (4)0.0270 (11)
O30.2272 (3)0.12660 (16)0.0203 (4)0.0332 (12)
O40.1247 (3)0.08070 (15)0.2201 (5)0.0314 (12)
O50.1983 (3)0.02697 (16)0.0365 (5)0.0333 (12)
O60.3308 (3)0.04094 (15)0.0120 (4)0.0309 (11)
O70.2627 (4)0.00150 (19)0.1184 (5)0.0517 (16)
O80.2475 (3)0.15793 (16)0.2617 (5)0.0355 (12)
O90.2759 (3)0.10278 (16)0.3788 (4)0.0326 (12)
O100.2730 (5)0.1713 (2)0.4458 (6)0.0662 (19)
N10.2634 (4)0.0222 (2)0.0254 (6)0.0325 (14)
N20.2654 (4)0.1450 (2)0.3649 (6)0.0387 (16)
N30.2788 (4)0.0367 (2)0.4396 (5)0.0369 (15)
N40.2357 (5)0.0654 (2)0.2322 (6)0.0455 (18)
N50.3945 (4)0.0479 (2)0.2606 (6)0.0471 (18)
N60.4773 (4)0.1728 (2)0.0807 (7)0.0453 (18)
N70.5551 (3)0.0976 (2)0.1525 (5)0.0321 (14)
N80.4928 (4)0.1561 (3)0.3049 (6)0.0478 (18)
N90.1046 (5)0.1388 (3)0.1233 (8)0.072 (3)
N100.2258 (5)0.2001 (2)0.0937 (6)0.051 (2)
N110.2596 (6)0.1239 (3)0.1975 (7)0.063 (2)
N120.0330 (4)0.0706 (2)0.1969 (6)0.0448 (18)
N130.0175 (4)0.1493 (2)0.2613 (7)0.0478 (18)
N140.0442 (4)0.0864 (2)0.4119 (6)0.0444 (17)
C10.2737 (6)0.0824 (3)0.4912 (8)0.055 (2)
H1A0.26100.08010.57330.082*
H1B0.32690.09770.48210.082*
H1C0.22970.09930.45180.082*
C20.3022 (6)0.0022 (3)0.5231 (8)0.054 (2)
H2A0.28520.01130.60030.081*
H2B0.27440.02560.50220.081*
H2C0.36260.00210.52240.081*
C30.2467 (7)0.0811 (3)0.1146 (10)0.076 (3)
H3A0.20090.10110.09340.114*
H3B0.29960.09710.10960.114*
H3C0.24710.05580.06180.114*
C40.1460 (6)0.0679 (4)0.2662 (11)0.084 (4)
H4A0.11710.08980.21790.126*
H4B0.12000.03880.25540.126*
H4C0.14260.07660.34730.126*
C50.4648 (5)0.0170 (3)0.2516 (9)0.060 (3)
H5A0.51450.03330.22840.089*
H5B0.47510.00290.32650.089*
H5C0.45160.00570.19390.089*
C60.4187 (7)0.0955 (3)0.2793 (10)0.077 (3)
H6A0.47560.10020.25280.115*
H6B0.38050.11480.23580.115*
H6C0.41570.10260.36150.115*
C70.5461 (6)0.1830 (3)0.0021 (9)0.060 (3)
H7A0.53060.20810.04700.090*
H7B0.55730.15710.04620.090*
H7C0.59600.19040.04740.090*
C80.4101 (6)0.2069 (3)0.0814 (10)0.069 (3)
H8A0.41900.22810.01890.103*
H8B0.41110.22250.15550.103*
H8C0.35610.19240.07030.103*
C90.6430 (5)0.1065 (3)0.1885 (8)0.052 (2)
H9A0.67840.08200.16390.078*
H9B0.64640.10940.27260.078*
H9C0.66190.13410.15280.078*
C100.5464 (5)0.0644 (3)0.0569 (7)0.0403 (19)
H10A0.59720.04660.05270.060*
H10B0.53720.07990.01640.060*
H10C0.49890.04500.07190.060*
C110.5348 (6)0.2001 (4)0.3221 (10)0.085 (4)
H11A0.53760.20700.40450.127*
H11B0.50310.22310.28140.127*
H11C0.59120.19870.29150.127*
C120.4797 (6)0.1309 (5)0.4108 (9)0.085 (4)
H12A0.49190.14980.47770.127*
H12B0.51670.10510.41230.127*
H12C0.42180.12100.41330.127*
C130.0645 (7)0.0960 (4)0.1105 (11)0.082 (4)
H13A0.00560.09850.13210.124*
H13B0.06950.08620.03020.124*
H13C0.09130.07430.16060.124*
C140.0490 (8)0.1713 (4)0.1835 (11)0.099 (5)
H14A0.00700.15870.19110.148*
H14B0.07070.17770.26010.148*
H14C0.04670.19870.13850.148*
C150.1981 (6)0.2275 (3)0.0056 (7)0.049 (2)
H15A0.21410.25840.00680.073*
H15B0.22440.21660.07680.073*
H15C0.13750.22550.01200.073*
C160.2511 (9)0.2258 (4)0.1981 (9)0.092 (4)
H16A0.25890.25700.17730.137*
H16B0.20770.22340.25790.137*
H16C0.30330.21380.22750.137*
C170.3500 (7)0.1209 (4)0.1868 (9)0.078 (3)
H17A0.37220.10640.25540.116*
H17B0.36480.10350.11830.116*
H17C0.37350.15070.17960.116*
C180.2210 (11)0.1070 (5)0.3088 (9)0.127 (6)
H18A0.26450.09480.35770.190*
H18B0.19320.13150.34920.190*
H18C0.18030.08390.29160.190*
C190.0203 (5)0.0279 (3)0.1385 (10)0.067 (3)
H19A0.07250.01840.10130.100*
H19B0.00280.00560.19530.100*
H19C0.02270.03110.08030.100*
C200.1227 (5)0.0803 (4)0.2196 (11)0.084 (4)
H20A0.15780.06180.16930.126*
H20B0.13410.11160.20400.126*
H20C0.13470.07370.30030.126*
C210.0485 (6)0.1832 (3)0.3428 (12)0.085 (4)
H21A0.02590.21220.32110.127*
H21B0.10930.18420.34050.127*
H21C0.03090.17570.42090.127*
C220.0138 (8)0.1691 (4)0.1509 (10)0.092 (4)
H22A0.02520.20070.16230.138*
H22B0.06510.15400.12660.138*
H22C0.02820.16550.09130.138*
C230.0923 (5)0.0480 (3)0.4562 (8)0.053 (2)
H23A0.08770.04660.54030.079*
H23B0.15090.05140.43580.079*
H23C0.07030.02070.42200.079*
C240.0291 (7)0.0965 (4)0.4838 (9)0.085 (4)
H24A0.01690.08870.56420.127*
H24B0.07710.07940.45590.127*
H24C0.04180.12820.47870.127*
W10.783523 (17)0.227488 (9)0.52651 (2)0.02184 (8)
Ag10.78222 (4)0.26566 (2)0.28700 (5)0.03871 (16)
S10.78533 (12)0.18464 (6)0.36793 (16)0.0312 (4)
S20.78321 (13)0.30066 (6)0.48679 (17)0.0361 (5)
S30.66880 (12)0.21148 (7)0.62708 (17)0.0353 (4)
S40.89701 (12)0.21219 (7)0.63272 (17)0.0382 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Er10.01984 (16)0.01636 (16)0.02925 (18)0.00031 (11)0.00027 (13)0.00062 (13)
P10.0344 (10)0.0222 (10)0.0347 (11)0.0047 (8)0.0069 (9)0.0060 (8)
P20.0217 (9)0.0340 (11)0.0293 (10)0.0055 (8)0.0002 (8)0.0064 (8)
P30.0588 (14)0.0271 (11)0.0324 (11)0.0096 (9)0.0183 (10)0.0012 (9)
P40.0204 (9)0.0275 (10)0.0425 (12)0.0011 (7)0.0024 (8)0.0075 (9)
O10.037 (3)0.016 (2)0.033 (3)0.003 (2)0.001 (2)0.002 (2)
O20.023 (2)0.025 (3)0.033 (3)0.0008 (19)0.001 (2)0.001 (2)
O30.033 (3)0.030 (3)0.036 (3)0.000 (2)0.005 (2)0.005 (2)
O40.023 (2)0.026 (3)0.045 (3)0.003 (2)0.004 (2)0.004 (2)
O50.026 (3)0.026 (3)0.048 (3)0.002 (2)0.004 (2)0.007 (2)
O60.024 (3)0.028 (3)0.040 (3)0.000 (2)0.003 (2)0.002 (2)
O70.056 (4)0.051 (4)0.048 (4)0.004 (3)0.005 (3)0.026 (3)
O80.038 (3)0.025 (3)0.043 (3)0.004 (2)0.001 (3)0.000 (2)
O90.044 (3)0.023 (3)0.032 (3)0.001 (2)0.005 (2)0.001 (2)
O100.100 (5)0.045 (4)0.053 (4)0.018 (4)0.009 (4)0.020 (3)
N10.027 (3)0.031 (3)0.039 (4)0.003 (3)0.005 (3)0.007 (3)
N20.047 (4)0.029 (4)0.040 (4)0.005 (3)0.001 (3)0.009 (3)
N30.052 (4)0.029 (3)0.030 (4)0.005 (3)0.006 (3)0.005 (3)
N40.059 (5)0.025 (3)0.054 (5)0.009 (3)0.024 (4)0.007 (3)
N50.043 (4)0.043 (4)0.056 (5)0.019 (3)0.015 (3)0.021 (4)
N60.037 (4)0.036 (4)0.064 (5)0.004 (3)0.014 (3)0.013 (3)
N70.020 (3)0.045 (4)0.031 (3)0.001 (3)0.001 (3)0.003 (3)
N80.036 (4)0.069 (5)0.039 (4)0.000 (3)0.003 (3)0.022 (4)
N90.072 (6)0.043 (5)0.101 (7)0.019 (4)0.055 (5)0.000 (5)
N100.092 (6)0.030 (4)0.033 (4)0.012 (4)0.002 (4)0.011 (3)
N110.092 (6)0.049 (5)0.049 (5)0.025 (4)0.003 (5)0.009 (4)
N120.023 (3)0.053 (4)0.058 (5)0.000 (3)0.006 (3)0.032 (4)
N130.039 (4)0.034 (4)0.070 (5)0.003 (3)0.009 (4)0.010 (4)
N140.037 (4)0.058 (5)0.038 (4)0.010 (3)0.000 (3)0.004 (3)
C10.067 (6)0.040 (5)0.057 (6)0.015 (4)0.020 (5)0.024 (4)
C20.067 (6)0.053 (6)0.042 (5)0.009 (5)0.001 (5)0.013 (5)
C30.097 (8)0.055 (6)0.077 (8)0.023 (6)0.010 (7)0.030 (6)
C40.062 (7)0.086 (8)0.104 (10)0.018 (6)0.003 (7)0.033 (7)
C50.034 (5)0.059 (6)0.086 (8)0.003 (4)0.010 (5)0.008 (6)
C60.091 (8)0.057 (6)0.083 (8)0.038 (6)0.035 (6)0.025 (6)
C70.060 (6)0.049 (6)0.072 (7)0.021 (5)0.026 (5)0.008 (5)
C80.069 (7)0.035 (5)0.103 (9)0.004 (5)0.018 (6)0.022 (5)
C90.034 (5)0.072 (6)0.050 (6)0.005 (4)0.004 (4)0.011 (5)
C100.030 (4)0.054 (5)0.036 (5)0.002 (4)0.010 (3)0.013 (4)
C110.061 (7)0.091 (8)0.102 (9)0.002 (6)0.024 (6)0.070 (8)
C120.052 (6)0.160 (12)0.043 (6)0.016 (7)0.011 (5)0.003 (7)
C130.068 (7)0.062 (7)0.116 (10)0.001 (6)0.045 (7)0.012 (7)
C140.111 (10)0.074 (8)0.108 (10)0.036 (7)0.065 (8)0.002 (7)
C150.077 (6)0.026 (4)0.043 (5)0.009 (4)0.010 (5)0.001 (4)
C160.172 (13)0.057 (7)0.047 (7)0.024 (7)0.034 (7)0.022 (5)
C170.100 (9)0.075 (7)0.059 (7)0.034 (7)0.035 (6)0.008 (6)
C180.217 (17)0.130 (12)0.034 (6)0.022 (12)0.002 (8)0.046 (7)
C190.035 (5)0.064 (6)0.101 (9)0.005 (4)0.005 (5)0.042 (6)
C200.029 (5)0.110 (9)0.114 (10)0.001 (5)0.003 (5)0.076 (8)
C210.052 (6)0.037 (5)0.165 (13)0.011 (4)0.029 (7)0.049 (7)
C220.103 (9)0.083 (8)0.091 (9)0.058 (7)0.031 (7)0.037 (7)
C230.040 (5)0.078 (7)0.040 (5)0.002 (5)0.002 (4)0.005 (5)
C240.069 (7)0.128 (10)0.058 (7)0.045 (7)0.019 (6)0.012 (7)
W10.02715 (16)0.02019 (15)0.01811 (15)0.00253 (11)0.00214 (11)0.00094 (11)
Ag10.0607 (4)0.0356 (3)0.0198 (3)0.0003 (3)0.0010 (3)0.0023 (2)
S10.0455 (11)0.0234 (9)0.0246 (9)0.0004 (8)0.0008 (8)0.0048 (7)
S20.0564 (13)0.0218 (9)0.0301 (10)0.0037 (8)0.0015 (9)0.0032 (8)
S30.0301 (10)0.0457 (12)0.0301 (10)0.0059 (8)0.0016 (8)0.0020 (9)
S40.0353 (11)0.0491 (12)0.0300 (10)0.0155 (9)0.0064 (9)0.0044 (9)
Geometric parameters (Å, º) top
Er1—O32.225 (5)C6—H6A0.9600
Er1—O42.235 (5)C6—H6B0.9600
Er1—O22.237 (4)C6—H6C0.9600
Er1—O12.256 (4)C7—H7A0.9600
Er1—O92.428 (5)C7—H7B0.9600
Er1—O52.460 (5)C7—H7C0.9600
Er1—O82.460 (5)C8—H8A0.9600
Er1—O62.468 (5)C8—H8B0.9600
Er1—N22.863 (6)C8—H8C0.9600
Er1—N12.872 (6)C9—H9A0.9600
P1—O11.476 (5)C9—H9B0.9600
P1—N51.634 (7)C9—H9C0.9600
P1—N41.644 (7)C10—H10A0.9600
P1—N31.646 (6)C10—H10B0.9600
P2—O21.489 (5)C10—H10C0.9600
P2—N81.609 (7)C11—H11A0.9600
P2—N71.634 (6)C11—H11B0.9600
P2—N61.633 (7)C11—H11C0.9600
P3—O31.481 (5)C12—H12A0.9600
P3—N111.593 (8)C12—H12B0.9600
P3—N101.610 (7)C12—H12C0.9600
P3—N91.640 (8)C13—H13A0.9600
P4—O41.494 (5)C13—H13B0.9600
P4—N131.619 (7)C13—H13C0.9600
P4—N121.620 (6)C14—H14A0.9600
P4—N141.653 (7)C14—H14B0.9600
O5—N11.260 (8)C14—H14C0.9600
O6—N11.266 (7)C15—H15A0.9600
O7—N11.223 (8)C15—H15B0.9600
O8—N21.262 (8)C15—H15C0.9600
O9—N21.269 (8)C16—H16A0.9600
O10—N21.208 (8)C16—H16B0.9600
N3—C21.438 (10)C16—H16C0.9600
N3—C11.476 (9)C17—H17A0.9600
N4—C31.429 (12)C17—H17B0.9600
N4—C41.472 (12)C17—H17C0.9600
N5—C51.442 (11)C18—H18A0.9600
N5—C61.473 (11)C18—H18B0.9600
N6—C71.446 (10)C18—H18C0.9600
N6—C81.462 (11)C19—H19A0.9600
N7—C91.463 (9)C19—H19B0.9600
N7—C101.470 (9)C19—H19C0.9600
N8—C121.433 (13)C20—H20A0.9600
N8—C111.470 (12)C20—H20B0.9600
N9—C131.425 (12)C20—H20C0.9600
N9—C141.464 (11)C21—H21A0.9600
N10—C151.461 (10)C21—H21B0.9600
N10—C161.471 (11)C21—H21C0.9600
N11—C171.430 (13)C22—H22A0.9600
N11—C181.482 (12)C22—H22B0.9600
N12—C191.444 (10)C22—H22C0.9600
N12—C201.468 (10)C23—H23A0.9600
N13—C211.445 (11)C23—H23B0.9600
N13—C221.463 (12)C23—H23C0.9600
N14—C231.450 (10)C24—H24A0.9600
N14—C241.457 (11)C24—H24B0.9600
C1—H1A0.9600C24—H24C0.9600
C1—H1B0.9600W1—S42.1909 (19)
C1—H1C0.9600W1—S12.2043 (18)
C2—H2A0.9600W1—S32.205 (2)
C2—H2B0.9600W1—S22.2108 (19)
C2—H2C0.9600W1—Ag12.9474 (8)
C3—H3A0.9600W1—Ag1i2.9685 (8)
C3—H3B0.9600Ag1—S22.496 (2)
C3—H3C0.9600Ag1—S12.5674 (19)
C4—H4A0.9600Ag1—S3ii2.620 (2)
C4—H4B0.9600Ag1—S4ii2.621 (2)
C4—H4C0.9600Ag1—W1ii2.9685 (8)
C5—H5A0.9600S3—Ag1i2.620 (2)
C5—H5B0.9600S4—Ag1i2.621 (2)
C5—H5C0.9600
O3—Er1—O488.67 (18)N5—C5—H5C109.5
O3—Er1—O292.88 (17)H5A—C5—H5C109.5
O4—Er1—O2157.15 (17)H5B—C5—H5C109.5
O3—Er1—O1157.85 (17)N5—C6—H6A109.5
O4—Er1—O193.63 (17)N5—C6—H6B109.5
O2—Er1—O193.44 (16)H6A—C6—H6B109.5
O3—Er1—O9128.68 (17)N5—C6—H6C109.5
O4—Er1—O981.22 (17)H6A—C6—H6C109.5
O2—Er1—O980.05 (17)H6B—C6—H6C109.5
O1—Er1—O973.38 (16)N6—C7—H7A109.5
O3—Er1—O579.08 (17)N6—C7—H7B109.5
O4—Er1—O575.53 (17)H7A—C7—H7B109.5
O2—Er1—O5127.14 (17)N6—C7—H7C109.5
O1—Er1—O580.18 (16)H7A—C7—H7C109.5
O9—Er1—O5143.35 (17)H7B—C7—H7C109.5
O3—Er1—O876.60 (18)N6—C8—H8A109.5
O4—Er1—O880.12 (17)N6—C8—H8B109.5
O2—Er1—O878.09 (16)H8A—C8—H8B109.5
O1—Er1—O8125.51 (17)N6—C8—H8C109.5
O9—Er1—O852.13 (16)H8A—C8—H8C109.5
O5—Er1—O8145.74 (16)H8B—C8—H8C109.5
O3—Er1—O679.83 (17)N7—C9—H9A109.5
O4—Er1—O6127.23 (16)N7—C9—H9B109.5
O2—Er1—O675.36 (16)H9A—C9—H9B109.5
O1—Er1—O681.28 (16)N7—C9—H9C109.5
O9—Er1—O6143.29 (16)H9A—C9—H9C109.5
O5—Er1—O651.78 (16)H9B—C9—H9C109.5
O8—Er1—O6143.25 (17)N7—C10—H10A109.5
O3—Er1—N2102.64 (19)N7—C10—H10B109.5
O4—Er1—N280.79 (18)H10A—C10—H10B109.5
O2—Er1—N276.62 (18)N7—C10—H10C109.5
O1—Er1—N299.48 (18)H10A—C10—H10C109.5
O9—Er1—N226.14 (17)H10B—C10—H10C109.5
O5—Er1—N2156.23 (18)N8—C11—H11A109.5
O8—Er1—N226.05 (17)N8—C11—H11B109.5
O6—Er1—N2151.96 (17)H11A—C11—H11B109.5
O3—Er1—N176.12 (18)N8—C11—H11C109.5
O4—Er1—N1101.18 (17)H11A—C11—H11C109.5
O2—Er1—N1101.32 (17)H11B—C11—H11C109.5
O1—Er1—N181.82 (17)N8—C12—H12A109.5
O9—Er1—N1155.20 (16)N8—C12—H12B109.5
O5—Er1—N125.89 (16)H12A—C12—H12B109.5
O8—Er1—N1152.64 (18)N8—C12—H12C109.5
O6—Er1—N126.06 (15)H12A—C12—H12C109.5
N2—Er1—N1177.59 (19)H12B—C12—H12C109.5
O1—P1—N5109.0 (3)N9—C13—H13A109.5
O1—P1—N4117.4 (3)N9—C13—H13B109.5
N5—P1—N4103.4 (4)H13A—C13—H13B109.5
O1—P1—N3108.2 (3)N9—C13—H13C109.5
N5—P1—N3115.4 (3)H13A—C13—H13C109.5
N4—P1—N3103.7 (3)H13B—C13—H13C109.5
O2—P2—N8110.9 (3)N9—C14—H14A109.5
O2—P2—N7108.7 (3)N9—C14—H14B109.5
N8—P2—N7109.6 (3)H14A—C14—H14B109.5
O2—P2—N6111.6 (3)N9—C14—H14C109.5
N8—P2—N6106.9 (4)H14A—C14—H14C109.5
N7—P2—N6109.2 (3)H14B—C14—H14C109.5
O3—P3—N11111.2 (4)N10—C15—H15A109.5
O3—P3—N10109.9 (3)N10—C15—H15B109.5
N11—P3—N10108.8 (4)H15A—C15—H15B109.5
O3—P3—N9108.7 (4)N10—C15—H15C109.5
N11—P3—N9109.0 (5)H15A—C15—H15C109.5
N10—P3—N9109.3 (4)H15B—C15—H15C109.5
O4—P4—N13119.4 (3)N10—C16—H16A109.5
O4—P4—N12107.6 (3)N10—C16—H16B109.5
N13—P4—N12104.7 (4)H16A—C16—H16B109.5
O4—P4—N14107.8 (3)N10—C16—H16C109.5
N13—P4—N14103.0 (4)H16A—C16—H16C109.5
N12—P4—N14114.7 (4)H16B—C16—H16C109.5
P1—O1—Er1161.3 (3)N11—C17—H17A109.5
P2—O2—Er1168.0 (3)N11—C17—H17B109.5
P3—O3—Er1167.6 (3)H17A—C17—H17B109.5
P4—O4—Er1158.7 (3)N11—C17—H17C109.5
N1—O5—Er195.6 (4)H17A—C17—H17C109.5
N1—O6—Er195.1 (4)H17B—C17—H17C109.5
N2—O8—Er195.1 (4)N11—C18—H18A109.5
N2—O9—Er196.4 (4)N11—C18—H18B109.5
O7—N1—O5122.8 (6)H18A—C18—H18B109.5
O7—N1—O6120.4 (6)N11—C18—H18C109.5
O5—N1—O6116.8 (6)H18A—C18—H18C109.5
O7—N1—Er1171.6 (5)H18B—C18—H18C109.5
O5—N1—Er158.5 (3)N12—C19—H19A109.5
O6—N1—Er158.9 (3)N12—C19—H19B109.5
O10—N2—O8122.1 (7)H19A—C19—H19B109.5
O10—N2—O9121.8 (7)N12—C19—H19C109.5
O8—N2—O9116.1 (6)H19A—C19—H19C109.5
O10—N2—Er1175.5 (6)H19B—C19—H19C109.5
O8—N2—Er158.9 (3)N12—C20—H20A109.5
O9—N2—Er157.4 (3)N12—C20—H20B109.5
C2—N3—C1113.8 (7)H20A—C20—H20B109.5
C2—N3—P1120.0 (5)N12—C20—H20C109.5
C1—N3—P1120.3 (5)H20A—C20—H20C109.5
C3—N4—C4111.1 (8)H20B—C20—H20C109.5
C3—N4—P1123.9 (6)N13—C21—H21A109.5
C4—N4—P1120.3 (6)N13—C21—H21B109.5
C5—N5—C6114.7 (7)H21A—C21—H21B109.5
C5—N5—P1120.9 (6)N13—C21—H21C109.5
C6—N5—P1120.1 (6)H21A—C21—H21C109.5
C7—N6—C8114.2 (7)H21B—C21—H21C109.5
C7—N6—P2125.5 (6)N13—C22—H22A109.5
C8—N6—P2119.5 (6)N13—C22—H22B109.5
C9—N7—C10114.0 (6)H22A—C22—H22B109.5
C9—N7—P2122.9 (5)N13—C22—H22C109.5
C10—N7—P2119.7 (5)H22A—C22—H22C109.5
C12—N8—C11114.8 (8)H22B—C22—H22C109.5
C12—N8—P2120.0 (7)N14—C23—H23A109.5
C11—N8—P2124.3 (7)N14—C23—H23B109.5
C13—N9—C14111.5 (8)H23A—C23—H23B109.5
C13—N9—P3122.7 (6)N14—C23—H23C109.5
C14—N9—P3124.9 (8)H23A—C23—H23C109.5
C15—N10—C16115.1 (7)H23B—C23—H23C109.5
C15—N10—P3119.7 (6)N14—C24—H24A109.5
C16—N10—P3123.4 (7)N14—C24—H24B109.5
C17—N11—C18116.6 (9)H24A—C24—H24B109.5
C17—N11—P3120.2 (7)N14—C24—H24C109.5
C18—N11—P3123.2 (9)H24A—C24—H24C109.5
C19—N12—C20113.0 (6)H24B—C24—H24C109.5
C19—N12—P4122.5 (5)S4—W1—S1108.17 (7)
C20—N12—P4121.3 (5)S4—W1—S3109.83 (8)
C21—N13—C22112.4 (8)S1—W1—S3108.72 (7)
C21—N13—P4124.0 (7)S4—W1—S2108.30 (8)
C22—N13—P4120.7 (7)S1—W1—S2113.32 (7)
C23—N14—C24112.4 (8)S3—W1—S2108.46 (8)
C23—N14—P4118.9 (6)S4—W1—Ag1125.65 (6)
C24—N14—P4120.7 (6)S1—W1—Ag157.64 (5)
N3—C1—H1A109.5S3—W1—Ag1124.50 (6)
N3—C1—H1B109.5S2—W1—Ag155.69 (5)
H1A—C1—H1B109.5S4—W1—Ag1i58.79 (6)
N3—C1—H1C109.5S1—W1—Ag1i148.81 (5)
H1A—C1—H1C109.5S3—W1—Ag1i58.66 (5)
H1B—C1—H1C109.5S2—W1—Ag1i97.87 (5)
N3—C2—H2A109.5Ag1—W1—Ag1i153.548 (12)
N3—C2—H2B109.5S2—Ag1—S193.51 (6)
H2A—C2—H2B109.5S2—Ag1—S3ii121.31 (7)
N3—C2—H2C109.5S1—Ag1—S3ii119.92 (6)
H2A—C2—H2C109.5S2—Ag1—S4ii120.66 (7)
H2B—C2—H2C109.5S1—Ag1—S4ii117.59 (7)
N4—C3—H3A109.5S3ii—Ag1—S4ii86.67 (6)
N4—C3—H3B109.5S2—Ag1—W147.03 (5)
H3A—C3—H3B109.5S1—Ag1—W146.49 (4)
N4—C3—H3C109.5S3ii—Ag1—W1137.34 (5)
H3A—C3—H3C109.5S4ii—Ag1—W1135.90 (5)
H3B—C3—H3C109.5S2—Ag1—W1ii151.57 (5)
N4—C4—H4A109.5S1—Ag1—W1ii114.89 (5)
N4—C4—H4B109.5S3ii—Ag1—W1ii45.95 (5)
H4A—C4—H4B109.5S4ii—Ag1—W1ii45.63 (4)
N4—C4—H4C109.5W1—Ag1—W1ii161.37 (2)
H4A—C4—H4C109.5W1—S1—Ag175.87 (6)
H4B—C4—H4C109.5W1—S2—Ag177.28 (6)
N5—C5—H5A109.5W1—S3—Ag1i75.39 (6)
N5—C5—H5B109.5W1—S4—Ag1i75.59 (6)
H5A—C5—H5B109.5
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2.

Experimental details

Crystal data
Chemical formula[Er(NO3)2(C6H18N3OP)4][AgWS4]
Mr1428.09
Crystal system, space groupMonoclinic, P21/c
Temperature (K)150
a, b, c (Å)15.763 (3), 29.579 (6), 11.368 (2)
β (°) 90.83 (3)
V3)5299.8 (17)
Z4
Radiation typeMo Kα
µ (mm1)4.43
Crystal size (mm)0.2 × 0.17 × 0.15
Data collection
DiffractometerRigaku Saturn724+
diffractometer
Absorption correctionMulti-scan
(CrystalClear; Rigaku, 2008)
Tmin, Tmax0.428, 0.514
No. of measured, independent and
observed [I > 2σ(I)] reflections
26753, 9597, 8722
Rint0.044
(sin θ/λ)max1)0.603
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.092, 1.08
No. of reflections9597
No. of parameters532
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.024P)2 + 26.5377P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.91, 1.04

Computer programs: CrystalClear (Rigaku, 2008), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

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).

References

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ISSN: 2056-9890
Volume 69| Part 1| January 2013| Pages m43-m44
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