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The self-assembly of tetra­thio­tungstate(VI), silver sulfide and ytterbium(III) nitrate in hexa­methyl­phospho­ramide (hmp) resulted in a one-dimensional anionic W/S/Ag polymer, {[Yb(NO3)2(C6H18N3OP)4][WAgS4]}n. The central Yb coordination polyhedron in the cationic complex [Yb(hmp)4(NO3)2]+ is a distorted square anti­prism. The [YbO8] assembly has an approximate fourfold inversion axis along the bis­ector of one of the chelating nitrate groups. The polymeric anion {[WS4Ag]}n presents a distorted linear configuration, with W—Ag—W and Ag—W—Ag angles of 160.81 (7) and 153.41 (7)°, deviating significantly from the ideal 180°. The anionic chains in the title compound are similar to those in {N(C6H5CH2)(C2H5)3[MoS4Ag]}n: they both have a similar wave-like appearance but have different orientations. The former propagate along the c axis, while the latter have two orientations: one parallel to the a axis and the other parallel to the b axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807031480/br2049sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807031480/br2049Isup2.hkl
Contains datablock I

CCDC reference: 657539

Key indicators

  • Single-crystal X-ray study
  • T = 153 K
  • Mean [sigma](g-S) = 0.001 Å
  • R factor = 0.032
  • wR factor = 0.069
  • Data-to-parameter ratio = 18.1

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? PLAT762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ?
Alert level C PLAT213_ALERT_2_C Atom C13 has ADP max/min Ratio ............. 3.10 prola PLAT213_ALERT_2_C Atom C46 has ADP max/min Ratio ............. 3.40 prola PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.81 Ratio PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.68 Ratio
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for W1 (9) 6.62 PLAT794_ALERT_5_G Check Predicted Bond Valency for Yb1 (3) 3.46 PLAT794_ALERT_5_G Check Predicted Bond Valency for Ag1 (1) 1.18
2 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 3 ALERT type 5 Informative message, check

Comment top

One-dimensional Mo(W)/S/Ag anionic polymers are very impressive in light of configurational isomerism (Niu et al., 2004, 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 {[Yb(hmp)4(NO3)2][WS4Ag]}n (hmp = hexamethylphosphoramide) with a wave-like anionic chain was prepared by following such route using Yb(III)-hmp complex as counterion.

The cationic complex in the title compound is univalent as a result of the inclusion of two nitrate ligands, hence inducing 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(dmso)8]3+ induces a helical chain with a trivalent repeat unit [W3S12Ag3]3- (Huang et al., 1997).

The central Yb in the cationic complex [Yb(hmp)4(NO3)2]+ has distorted square antiprismatic coordination (Fig. 1). The eight O atoms from four hmp and two nitrate ligands may be sorted into two groups (O1, O3, O6, O7 and O2, O4, O8, O9), each group together with the central Yb nearly coplanar. The two planes formed by these two groups are perpendicular to each other. The [YbO8] assembly has an approximate 4-folded inversion axis along the bisector of the O6—Yb1—O7 angle (Fig. 2).

Fig. 3 shows a portion of the polymeric anion in the title compound, which has a distorted linear configuration with W—Ag—W and Ag—W—Ag angles of 160.81 (7) and 153.41 (7) ° heavily deviating 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 156.47 (5) and 157.14 (5) ° for Mo—Ag—Mo and Ag—Mo—Ag are found in another distorted linear chain in {N(C6H5CH2)(C2H5)3[MoS4Ag]}n (Yu et al., 1998). The whole anionic chains in both the title compound and the compound above have similar wave-like appearance but with different orientations. The former propagates along the c axis, while the latter has two orientations: one parallel to a axis and the other parallel to b axis.

Related literature top

An 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 {N(C6H5CH2)(C2H5)3[MoS4Ag]}n (Yu et al., 1998), which has similar wave-like chains but with different chain orientations. For related literature, see: Huang et al. (1997); Niu et al. (2004).

Experimental top

0.5 mmol A g2S was added to a solution of [NH4]2WS4 (1 mmol in 20 mL h mp) with thorough stir for 10 h. The solution underwent an additional stir for one minute after 0.5 mmol Yb(NO3)36H2O was added. After filtration the orange-red filtrate was carefully laid on the surface with 20 ml i-PrOH. Red block crystals were obtained after ten days. Yield: 0.836 g in pure form, 58.3% (based on W). Analysis calculated for C24H72AgN14O10P4S4WYb: C 20.08, H 5.42, N 13.67%; found: C 20.44, H 5.57, N 13.38%. IR: ν, cm-1, 480m, 447 s, 436s h (W-µ2-S).

Refinement top

A few C atoms and O5 have notably larger Ueq than others or have large ADP max/min ratio (Alert level C). 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 and C—H bond length 0.98 Å for methyl H atoms.

Structure description top

One-dimensional Mo(W)/S/Ag anionic polymers are very impressive in light of configurational isomerism (Niu et al., 2004, 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 {[Yb(hmp)4(NO3)2][WS4Ag]}n (hmp = hexamethylphosphoramide) with a wave-like anionic chain was prepared by following such route using Yb(III)-hmp complex as counterion.

The cationic complex in the title compound is univalent as a result of the inclusion of two nitrate ligands, hence inducing 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(dmso)8]3+ induces a helical chain with a trivalent repeat unit [W3S12Ag3]3- (Huang et al., 1997).

The central Yb in the cationic complex [Yb(hmp)4(NO3)2]+ has distorted square antiprismatic coordination (Fig. 1). The eight O atoms from four hmp and two nitrate ligands may be sorted into two groups (O1, O3, O6, O7 and O2, O4, O8, O9), each group together with the central Yb nearly coplanar. The two planes formed by these two groups are perpendicular to each other. The [YbO8] assembly has an approximate 4-folded inversion axis along the bisector of the O6—Yb1—O7 angle (Fig. 2).

Fig. 3 shows a portion of the polymeric anion in the title compound, which has a distorted linear configuration with W—Ag—W and Ag—W—Ag angles of 160.81 (7) and 153.41 (7) ° heavily deviating 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 156.47 (5) and 157.14 (5) ° for Mo—Ag—Mo and Ag—Mo—Ag are found in another distorted linear chain in {N(C6H5CH2)(C2H5)3[MoS4Ag]}n (Yu et al., 1998). The whole anionic chains in both the title compound and the compound above have similar wave-like appearance but with different orientations. The former propagates along the c axis, while the latter has two orientations: one parallel to a axis and the other parallel to b axis.

An 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 {N(C6H5CH2)(C2H5)3[MoS4Ag]}n (Yu et al., 1998), which has similar wave-like chains but with different chain orientations. For related literature, see: Huang et al. (1997); Niu et al. (2004).

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 coordination geometry of the [YbO8] assembly.
[Figure 3] Fig. 3. 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')ytterbium(III)] [silver(I)-di-µ-sulfido-tungstate(VI)(Ag—W)-di-µ-sulfido]] top
Crystal data top
[Yb(NO3)2(C6H18N3OP)4][WAgS4]F(000) = 2836
Mr = 1433.87Dx = 1.808 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ybcCell parameters from 17963 reflections
a = 15.7241 (9) Åθ = 3.0–25.4°
b = 29.5280 (18) ŵ = 4.64 mm1
c = 11.3464 (7) ÅT = 153 K
β = 90.798 (1)°Block, red
V = 5267.6 (5) Å30.55 × 0.45 × 0.30 mm
Z = 4
Data collection top
Rigaku Mercury CCD (2 x 2 bin mode)
diffractometer
9611 independent reflections
Radiation source: fine-focus sealed tube9126 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
dtprofit.ref scansθmax = 25.4°, θmin = 3.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1718
Tmin = 0.097, Tmax = 0.243k = 3535
47611 measured reflectionsl = 1313
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)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.069H-atom parameters constrained
S = 1.18 w = 1/[σ2(Fo2) + (0.017P)2 + 19.3445P]
where P = (Fo2 + 2Fc2)/3
9611 reflections(Δ/σ)max = 0.002
532 parametersΔρmax = 0.93 e Å3
0 restraintsΔρmin = 1.05 e Å3
Crystal data top
[Yb(NO3)2(C6H18N3OP)4][WAgS4]V = 5267.6 (5) Å3
Mr = 1433.87Z = 4
Monoclinic, P21/cMo Kα radiation
a = 15.7241 (9) ŵ = 4.64 mm1
b = 29.5280 (18) ÅT = 153 K
c = 11.3464 (7) Å0.55 × 0.45 × 0.30 mm
β = 90.798 (1)°
Data collection top
Rigaku Mercury CCD (2 x 2 bin mode)
diffractometer
9611 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
9126 reflections with I > 2σ(I)
Tmin = 0.097, Tmax = 0.243Rint = 0.040
47611 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0330 restraints
wR(F2) = 0.069H-atom parameters constrained
S = 1.18 w = 1/[σ2(Fo2) + (0.017P)2 + 19.3445P]
where P = (Fo2 + 2Fc2)/3
9611 reflectionsΔρmax = 0.93 e Å3
532 parametersΔρmin = 1.05 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
Yb10.238238 (12)0.082437 (7)0.826783 (18)0.01266 (6)
P10.29365 (10)0.14628 (5)1.09340 (12)0.0261 (3)
P20.02328 (8)0.13163 (5)0.82032 (11)0.0188 (3)
P30.20073 (8)0.03022 (4)0.70195 (11)0.0188 (3)
P40.45674 (8)0.09666 (4)0.73072 (12)0.0184 (3)
O20.10510 (19)0.10586 (11)0.8224 (3)0.0185 (7)
O40.3741 (2)0.08048 (11)0.7800 (3)0.0213 (8)
O30.2073 (2)0.01886 (11)0.7298 (3)0.0187 (7)
O10.2719 (2)0.12614 (11)0.9769 (3)0.0205 (8)
O50.2267 (3)0.17135 (14)0.5539 (4)0.0495 (12)
O60.2519 (2)0.15767 (11)0.7393 (3)0.0225 (8)
O70.2241 (2)0.10250 (11)0.6210 (3)0.0225 (8)
O80.3020 (2)0.02711 (12)0.9616 (3)0.0216 (8)
O90.1695 (2)0.04121 (12)0.9860 (3)0.0207 (8)
O100.2385 (3)0.00200 (14)1.1183 (3)0.0351 (10)
N80.2224 (3)0.03703 (15)0.5613 (4)0.0247 (10)
N70.1072 (3)0.04816 (16)0.7417 (4)0.0324 (12)
N90.2668 (3)0.06466 (15)0.7692 (4)0.0289 (11)
N100.4539 (3)0.08728 (17)0.5880 (4)0.0302 (11)
N110.5331 (3)0.07057 (16)0.8027 (4)0.0296 (11)
N120.4823 (3)0.14966 (15)0.7396 (4)0.0308 (11)
N30.3956 (3)0.13927 (18)1.1205 (5)0.0464 (15)
N10.2403 (4)0.12298 (18)1.1978 (4)0.0438 (14)
N50.0076 (3)0.15537 (19)0.6931 (4)0.0369 (13)
N40.0235 (3)0.17178 (16)0.9188 (4)0.0325 (11)
N60.0541 (3)0.09614 (15)0.8465 (4)0.0226 (10)
N210.2344 (3)0.14476 (15)0.6356 (4)0.0246 (10)
N220.2367 (3)0.02247 (14)1.0250 (4)0.0211 (9)
N20.2722 (3)0.20015 (15)1.0922 (4)0.0328 (12)
C410.5280 (4)0.0972 (3)0.5153 (6)0.053 (2)
H41A0.51500.08950.43290.079*
H41B0.57660.07920.54310.079*
H41C0.54190.12940.52120.079*
C110.2776 (7)0.1064 (3)1.3076 (6)0.084 (3)
H11A0.23280.09381.35700.126*
H11B0.30560.13151.34930.126*
H11C0.31940.08281.29050.126*
C420.4062 (4)0.0479 (2)0.5434 (5)0.0376 (15)
H42A0.35730.04230.59390.056*
H42B0.44330.02120.54380.056*
H42C0.38630.05390.46270.056*
C430.5204 (4)0.0278 (2)0.8610 (6)0.0465 (18)
H43A0.57370.01810.89900.070*
H43B0.50240.00500.80290.070*
H43C0.47640.03110.92070.070*
C450.5143 (5)0.1695 (3)0.8496 (7)0.058 (2)
H45A0.52600.20170.83760.087*
H45B0.56680.15400.87400.087*
H45C0.47150.16600.91100.087*
C460.4502 (4)0.1842 (2)0.6566 (8)0.058 (2)
H46A0.42950.16950.58440.088*
H46B0.49630.20520.63740.088*
H46C0.40360.20100.69290.088*
C230.0359 (5)0.1997 (3)0.6780 (7)0.062 (2)
H23A0.03860.20750.59400.093*
H23B0.00410.22310.72100.093*
H23C0.09370.19770.70880.093*
C240.0203 (4)0.1299 (3)0.5860 (6)0.065 (3)
H24A0.04890.10130.60490.098*
H24B0.05550.14750.53220.098*
H24C0.03490.12360.54830.098*
C250.1423 (3)0.1056 (2)0.8095 (5)0.0366 (15)
H25A0.17900.08050.83350.055*
H25B0.14530.10900.72370.055*
H25C0.16160.13370.84690.055*
C210.0897 (4)0.2067 (2)0.9178 (7)0.0493 (18)
H21A0.08030.22810.98240.074*
H21B0.08740.22290.84250.074*
H21C0.14560.19240.92790.074*
C220.0466 (4)0.1823 (2)0.9967 (6)0.0440 (17)
H22A0.08850.15770.99340.066*
H22B0.07360.21070.97150.066*
H22C0.02490.18551.07760.066*
C330.1965 (4)0.0027 (2)0.4767 (5)0.0369 (14)
H33A0.21410.01180.39770.055*
H33B0.22340.02620.49760.055*
H33C0.13450.00070.47780.055*
C340.2277 (4)0.0827 (2)0.5100 (5)0.0356 (14)
H34A0.24530.10430.57120.053*
H34B0.26940.08280.44660.053*
H34C0.17180.09150.47810.053*
C310.0825 (5)0.0956 (2)0.7234 (6)0.0499 (19)
H31A0.02460.10030.75200.075*
H31B0.12200.11540.76680.075*
H31C0.08440.10280.63920.075*
C320.0357 (4)0.0167 (2)0.7454 (6)0.0444 (17)
H32A0.05710.01420.75790.067*
H32B0.00180.02500.81010.067*
H32C0.00390.01800.67050.067*
C350.2548 (5)0.0807 (2)0.8884 (6)0.0486 (18)
H35A0.30190.10080.91090.073*
H35B0.20100.09740.89250.073*
H35C0.25330.05490.94240.073*
C120.1489 (5)0.1192 (3)1.1865 (6)0.058 (2)
H12A0.13030.13131.11000.088*
H12B0.12200.13641.24980.088*
H12C0.13230.08731.19220.088*
C150.4495 (5)0.1718 (3)1.1833 (8)0.073 (3)
H15A0.50780.16011.18850.109*
H15B0.42770.17651.26280.109*
H15C0.44930.20071.14070.109*
C160.4355 (5)0.0951 (3)1.1066 (7)0.058 (2)
H16A0.39650.07471.06420.087*
H16B0.44900.08241.18440.087*
H16C0.48800.09841.06180.087*
C440.6223 (4)0.0802 (3)0.7801 (7)0.053 (2)
H44A0.62710.10970.74100.080*
H44B0.64560.05660.72920.080*
H44C0.65420.08080.85490.080*
C360.3559 (4)0.0672 (3)0.7363 (7)0.0518 (19)
H36A0.36230.05620.65550.078*
H36B0.37520.09870.74120.078*
H36C0.39020.04850.79020.078*
C260.0455 (3)0.0637 (2)0.9430 (5)0.0301 (13)
H26A0.01490.05930.96220.045*
H26B0.07070.03470.91920.045*
H26C0.07480.07531.01240.045*
C130.2469 (6)0.2259 (2)1.1959 (6)0.062 (2)
H13A0.23720.25761.17380.094*
H13B0.29210.22431.25610.094*
H13C0.19440.21311.22740.094*
C140.3010 (4)0.22756 (19)0.9925 (5)0.0350 (14)
H14A0.31630.20760.92710.052*
H14B0.35080.24541.01690.052*
H14C0.25520.24800.96690.052*
W10.716929 (12)0.227369 (6)0.473839 (16)0.01396 (6)
Ag10.71835 (3)0.233860 (14)0.21310 (3)0.02776 (10)
S10.60322 (8)0.21167 (5)0.36755 (11)0.0262 (3)
S20.83218 (8)0.21133 (5)0.37351 (11)0.0247 (3)
S30.71644 (9)0.30071 (4)0.51273 (11)0.0235 (3)
S40.71521 (8)0.18478 (4)0.63354 (11)0.0216 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Yb10.01101 (11)0.00816 (10)0.01884 (11)0.00037 (7)0.00089 (8)0.00117 (8)
P10.0399 (9)0.0151 (7)0.0231 (7)0.0076 (6)0.0123 (6)0.0008 (6)
P20.0123 (6)0.0237 (7)0.0206 (7)0.0034 (5)0.0008 (5)0.0049 (5)
P30.0238 (7)0.0115 (7)0.0211 (7)0.0039 (5)0.0058 (5)0.0049 (5)
P40.0122 (6)0.0158 (7)0.0271 (7)0.0001 (5)0.0030 (5)0.0056 (5)
O20.0125 (17)0.0172 (19)0.0258 (19)0.0036 (13)0.0022 (14)0.0010 (14)
O40.0151 (18)0.0153 (18)0.034 (2)0.0028 (14)0.0050 (15)0.0035 (15)
O30.0245 (19)0.0094 (17)0.0223 (18)0.0024 (14)0.0001 (14)0.0050 (14)
O10.0227 (19)0.0143 (18)0.0243 (19)0.0020 (14)0.0056 (14)0.0043 (14)
O50.084 (4)0.026 (2)0.038 (3)0.010 (2)0.012 (2)0.018 (2)
O60.026 (2)0.0129 (19)0.028 (2)0.0024 (14)0.0002 (15)0.0010 (15)
O70.030 (2)0.0136 (19)0.0237 (19)0.0003 (15)0.0021 (15)0.0001 (15)
O80.0158 (18)0.0185 (19)0.030 (2)0.0004 (14)0.0014 (15)0.0017 (15)
O90.0168 (18)0.0175 (19)0.028 (2)0.0015 (14)0.0008 (14)0.0031 (15)
O100.039 (2)0.036 (2)0.030 (2)0.0021 (19)0.0018 (18)0.0169 (19)
N80.036 (3)0.018 (2)0.021 (2)0.0039 (19)0.0079 (19)0.0059 (18)
N70.028 (3)0.026 (3)0.043 (3)0.010 (2)0.012 (2)0.011 (2)
N90.043 (3)0.014 (2)0.029 (3)0.006 (2)0.011 (2)0.0042 (19)
N100.023 (2)0.041 (3)0.027 (3)0.006 (2)0.0049 (19)0.004 (2)
N110.014 (2)0.034 (3)0.041 (3)0.0002 (19)0.0045 (19)0.021 (2)
N120.025 (3)0.017 (2)0.051 (3)0.0044 (19)0.009 (2)0.002 (2)
N30.046 (3)0.031 (3)0.062 (4)0.012 (2)0.034 (3)0.001 (3)
N10.072 (4)0.033 (3)0.027 (3)0.018 (3)0.002 (3)0.007 (2)
N50.022 (3)0.057 (4)0.032 (3)0.000 (2)0.007 (2)0.021 (3)
N40.021 (2)0.029 (3)0.048 (3)0.005 (2)0.009 (2)0.009 (2)
N60.012 (2)0.032 (3)0.024 (2)0.0010 (18)0.0002 (17)0.0026 (19)
N210.029 (3)0.016 (2)0.029 (3)0.0017 (18)0.0002 (19)0.006 (2)
N220.022 (2)0.017 (2)0.024 (2)0.0031 (18)0.0016 (19)0.0028 (18)
N20.066 (4)0.013 (2)0.019 (2)0.005 (2)0.006 (2)0.0069 (19)
C410.043 (4)0.079 (6)0.037 (4)0.016 (4)0.013 (3)0.011 (4)
C110.136 (9)0.088 (7)0.028 (4)0.009 (6)0.004 (5)0.018 (4)
C420.034 (3)0.044 (4)0.035 (3)0.001 (3)0.001 (3)0.005 (3)
C430.025 (3)0.047 (4)0.068 (5)0.006 (3)0.003 (3)0.037 (4)
C450.064 (5)0.044 (4)0.066 (5)0.031 (4)0.021 (4)0.018 (4)
C460.034 (4)0.027 (4)0.114 (7)0.002 (3)0.007 (4)0.040 (4)
C230.045 (4)0.062 (5)0.079 (6)0.013 (4)0.012 (4)0.047 (4)
C240.037 (4)0.134 (8)0.025 (4)0.015 (4)0.007 (3)0.005 (4)
C250.018 (3)0.050 (4)0.042 (4)0.001 (3)0.004 (2)0.011 (3)
C210.041 (4)0.034 (4)0.072 (5)0.002 (3)0.012 (3)0.009 (3)
C220.044 (4)0.036 (4)0.053 (4)0.012 (3)0.020 (3)0.004 (3)
C330.050 (4)0.033 (4)0.027 (3)0.003 (3)0.007 (3)0.000 (3)
C340.049 (4)0.028 (3)0.031 (3)0.006 (3)0.014 (3)0.016 (3)
C310.059 (5)0.037 (4)0.055 (4)0.029 (3)0.022 (3)0.014 (3)
C320.024 (3)0.044 (4)0.065 (5)0.002 (3)0.000 (3)0.007 (3)
C350.065 (5)0.038 (4)0.043 (4)0.019 (3)0.007 (3)0.013 (3)
C120.069 (5)0.056 (5)0.051 (4)0.030 (4)0.026 (4)0.010 (4)
C150.073 (6)0.063 (6)0.081 (6)0.033 (4)0.036 (5)0.004 (5)
C160.042 (4)0.050 (5)0.082 (6)0.002 (3)0.028 (4)0.011 (4)
C440.016 (3)0.074 (5)0.070 (5)0.001 (3)0.002 (3)0.049 (4)
C360.037 (4)0.058 (5)0.061 (5)0.018 (3)0.007 (3)0.012 (4)
C260.019 (3)0.037 (3)0.034 (3)0.003 (2)0.008 (2)0.007 (3)
C130.121 (7)0.031 (4)0.036 (4)0.024 (4)0.025 (4)0.019 (3)
C140.056 (4)0.019 (3)0.030 (3)0.007 (3)0.007 (3)0.002 (2)
W10.01795 (11)0.01220 (10)0.01170 (10)0.00201 (7)0.00149 (7)0.00054 (7)
Ag10.0456 (3)0.0249 (2)0.0128 (2)0.00002 (18)0.00088 (17)0.00176 (16)
S10.0221 (7)0.0358 (8)0.0206 (7)0.0109 (6)0.0054 (5)0.0027 (6)
S20.0228 (7)0.0307 (8)0.0206 (7)0.0043 (5)0.0011 (5)0.0018 (6)
S30.0388 (8)0.0127 (6)0.0190 (6)0.0018 (5)0.0003 (5)0.0006 (5)
S40.0333 (7)0.0148 (6)0.0166 (6)0.0012 (5)0.0001 (5)0.0040 (5)
Geometric parameters (Å, º) top
W1—S12.1923 (13)P4—O41.500 (3)
W1—S22.2050 (13)P4—N121.618 (5)
W1—S42.2061 (12)P4—N111.636 (4)
W1—S32.2102 (13)P4—N101.643 (5)
W1—Ag1i2.9461 (5)O5—N211.219 (6)
W1—Ag12.9650 (5)O6—N211.263 (5)
Ag1—S3ii2.4920 (13)O7—N211.269 (5)
Ag1—S4ii2.5667 (13)O8—N221.270 (5)
Ag1—S12.6203 (14)O9—N221.267 (5)
Ag1—S22.6207 (14)O10—N221.220 (5)
Ag1—W1ii2.9461 (5)N1—C121.445 (9)
S3—Ag1i2.4920 (13)N1—C111.455 (9)
S4—Ag1i2.5667 (13)N2—C131.461 (8)
Yb1—O12.196 (3)N2—C141.468 (7)
Yb1—O22.205 (3)N3—C161.458 (9)
Yb1—O42.210 (3)N3—C151.461 (8)
Yb1—O32.227 (3)N4—C221.455 (7)
Yb1—O72.416 (3)N4—C211.464 (8)
Yb1—O92.443 (3)N5—C241.446 (9)
Yb1—O82.444 (3)N5—C231.486 (8)
Yb1—O62.444 (3)N6—C261.461 (7)
Yb1—N212.845 (4)N6—C251.471 (6)
Yb1—N222.862 (4)N7—C321.459 (8)
P1—O11.485 (4)N7—C311.468 (7)
P1—N11.615 (5)N8—C331.451 (7)
P1—N21.626 (5)N8—C341.472 (7)
P1—N31.640 (5)N9—C351.448 (8)
P2—O21.495 (3)N9—C361.457 (8)
P2—N51.620 (5)N10—C411.466 (7)
P2—N41.629 (5)N10—C421.470 (8)
P2—N61.636 (4)N11—C431.441 (7)
P3—O31.487 (3)N11—C441.457 (7)
P3—N71.633 (5)N12—C451.461 (8)
P3—N91.635 (5)N12—C461.473 (8)
P3—N81.649 (4)
S1—W1—S2109.91 (5)O1—P1—N2109.8 (2)
S1—W1—S4108.19 (5)N1—P1—N2108.2 (3)
S2—W1—S4108.73 (5)O1—P1—N3109.1 (3)
S1—W1—S3108.18 (5)N1—P1—N3109.0 (3)
S2—W1—S3108.58 (5)N2—P1—N3109.1 (3)
S4—W1—S3113.23 (5)O2—P2—N5110.8 (2)
S1—W1—Ag1i125.79 (4)O2—P2—N4111.5 (2)
S2—W1—Ag1i124.29 (4)N5—P2—N4107.1 (3)
S4—W1—Ag1i57.63 (3)O2—P2—N6108.3 (2)
S3—W1—Ag1i55.62 (3)N5—P2—N6109.5 (2)
S1—W1—Ag158.82 (4)N4—P2—N6109.6 (2)
S2—W1—Ag158.74 (3)O3—P3—N7108.5 (2)
S4—W1—Ag1148.95 (4)O3—P3—N9117.7 (2)
S3—W1—Ag197.81 (3)N7—P3—N9103.8 (3)
Ag1i—W1—Ag1153.412 (8)O3—P3—N8108.1 (2)
S3ii—Ag1—S4ii93.59 (4)N7—P3—N8115.3 (2)
S3ii—Ag1—S1120.54 (5)N9—P3—N8103.7 (2)
S4ii—Ag1—S1117.33 (5)O4—P4—N12120.0 (2)
S3ii—Ag1—S2121.94 (5)O4—P4—N11107.3 (2)
S4ii—Ag1—S2119.44 (5)N12—P4—N11104.1 (3)
S1—Ag1—S286.77 (4)O4—P4—N10107.6 (2)
S3ii—Ag1—W1ii47.05 (3)N12—P4—N10103.2 (3)
S4ii—Ag1—W1ii46.55 (3)N11—P4—N10115.0 (3)
S1—Ag1—W1ii135.81 (3)P1—O1—Yb1167.4 (2)
S2—Ag1—W1ii137.30 (3)P2—O2—Yb1167.7 (2)
S3ii—Ag1—W1152.09 (3)P3—O3—Yb1160.2 (2)
S4ii—Ag1—W1114.27 (3)P4—O4—Yb1157.9 (2)
S1—Ag1—W145.71 (3)N21—O6—Yb194.9 (3)
S2—Ag1—W145.99 (3)N21—O7—Yb196.0 (3)
W1ii—Ag1—W1160.819 (16)N22—O8—Yb195.6 (3)
W1—S1—Ag175.48 (4)N22—O9—Yb195.7 (3)
W1—S2—Ag175.27 (4)C12—N1—C11116.0 (6)
W1—S3—Ag1i77.33 (4)C12—N1—P1119.6 (5)
W1—S4—Ag1i75.81 (4)C11—N1—P1124.3 (6)
O1—Yb1—O292.97 (12)C13—N2—C14115.1 (5)
O1—Yb1—O488.73 (13)C13—N2—P1124.2 (4)
O2—Yb1—O4157.51 (13)C14—N2—P1118.6 (4)
O1—Yb1—O3158.07 (13)C16—N3—C15113.1 (6)
O2—Yb1—O393.00 (12)C16—N3—P1120.9 (4)
O4—Yb1—O393.72 (12)C15—N3—P1124.6 (6)
O1—Yb1—O7128.57 (12)C22—N4—C21113.5 (5)
O2—Yb1—O780.04 (12)C22—N4—P2125.3 (4)
O4—Yb1—O781.39 (12)C21—N4—P2120.1 (4)
O3—Yb1—O773.29 (12)C24—N5—C23115.5 (6)
O1—Yb1—O979.85 (12)C24—N5—P2120.2 (5)
O2—Yb1—O975.11 (12)C23—N5—P2123.3 (5)
O4—Yb1—O9127.15 (12)C26—N6—C25114.6 (4)
O3—Yb1—O981.33 (12)C26—N6—P2119.7 (3)
O7—Yb1—O9143.24 (11)C25—N6—P2121.8 (4)
O1—Yb1—O879.33 (12)C32—N7—C31114.2 (5)
O2—Yb1—O8127.23 (12)C32—N7—P3119.8 (4)
O4—Yb1—O875.11 (12)C31—N7—P3120.5 (4)
O3—Yb1—O880.26 (12)C33—N8—C34113.3 (4)
O7—Yb1—O8143.14 (12)C33—N8—P3119.7 (4)
O9—Yb1—O852.13 (11)C34—N8—P3120.5 (4)
O1—Yb1—O676.08 (12)C35—N9—C36111.1 (5)
O2—Yb1—O678.13 (12)C35—N9—P3123.3 (4)
O4—Yb1—O680.54 (12)C36—N9—P3121.3 (4)
O3—Yb1—O6125.83 (12)C41—N10—C42111.7 (5)
O7—Yb1—O652.54 (12)C41—N10—P4120.7 (4)
O9—Yb1—O6142.71 (12)C42—N10—P4118.7 (4)
O8—Yb1—O6145.54 (11)C43—N11—C44113.1 (5)
O1—Yb1—N21102.33 (13)C43—N11—P4122.4 (4)
O2—Yb1—N2176.69 (12)C44—N11—P4121.5 (4)
O4—Yb1—N2181.04 (13)C45—N12—C46112.3 (6)
O3—Yb1—N2199.58 (12)C45—N12—P4121.5 (4)
O7—Yb1—N2126.34 (12)C46—N12—P4123.2 (5)
O9—Yb1—N21151.79 (12)O5—N21—O6122.1 (5)
O8—Yb1—N21156.07 (12)O5—N21—O7121.5 (5)
O6—Yb1—N2126.25 (12)O6—N21—O7116.4 (4)
O1—Yb1—N2276.05 (12)O5—N21—Yb1175.6 (4)
O2—Yb1—N22101.13 (12)O6—N21—Yb158.9 (2)
O4—Yb1—N22101.04 (12)O7—N21—Yb157.7 (2)
O3—Yb1—N2282.10 (12)O10—N22—O9121.9 (4)
O7—Yb1—N22155.38 (12)O10—N22—O8122.4 (4)
O9—Yb1—N2226.12 (11)O9—N22—O8115.7 (4)
O8—Yb1—N2226.20 (11)O10—N22—Yb1171.3 (4)
O6—Yb1—N22152.04 (12)O9—N22—Yb158.1 (2)
N21—Yb1—N22177.28 (13)O8—N22—Yb158.2 (2)
O1—P1—N1111.5 (2)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2.

Experimental details

Crystal data
Chemical formula[Yb(NO3)2(C6H18N3OP)4][WAgS4]
Mr1433.87
Crystal system, space groupMonoclinic, P21/c
Temperature (K)153
a, b, c (Å)15.7241 (9), 29.5280 (18), 11.3464 (7)
β (°) 90.798 (1)
V3)5267.6 (5)
Z4
Radiation typeMo Kα
µ (mm1)4.64
Crystal size (mm)0.55 × 0.45 × 0.30
Data collection
DiffractometerRigaku Mercury CCD (2 x 2 bin mode)
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.097, 0.243
No. of measured, independent and
observed [I > 2σ(I)] reflections
47611, 9611, 9126
Rint0.040
(sin θ/λ)max1)0.602
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.033, 0.069, 1.18
No. of reflections9611
No. of parameters532
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.017P)2 + 19.3445P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.93, 1.05

Computer programs: CrystalClear (Rigaku, 2000), CrystalClear, SHELXTL (Sheldrick, 2000), SHELXTL.

 

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