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

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ISSN: 2056-9890

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

aMolecular Materials Research Center, Scientific Research Academy, School of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang 212013, People's Republic of China
*Correspondence e-mail: zjf260@ujs.edu.cn

(Received 15 October 2010; accepted 21 October 2010; online 30 October 2010)

Hexamethyl­phospho­ramide (hmp), tetra­thio­molybdate, silver sulfide and dysprosium nitrate were self-assembled to form an anionic [AgMoS4]nn chain in the title complex, {[Dy(NO3)2(C6H18N3OP)4][AgMoS4]}n. The central Dy atom in the cation is coordinated by eight O atoms from two nitrate and four hmp ligands, resulting in a distorted square-anti­prismatic environment. Together with the two nitrate ligands, the cation is monovalent, which leads to the anionic chain having an [AgMoS4] repeat unit. The polymeric anionic chain, with Mo—Ag—Mo and Ag—Mo—Ag angles of 161.911 (13) and 154.014 (13)°, respectively, presents a distorted linear configuration. The title complex is isostructural with the W analogue.

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.]). For their unique properties, see: Zhang et al. (2007[Zhang, C., Song, Y. L. & Wang, X. (2007). Coord. Chem. Rev. 251, 111-141.]). For the isotypic W analogue, see: Wei et al. (2010[Wei, H., Zhang, J. & Zhang, C. (2010). Acta Cryst. E66, m1193-m1194.]).

[Scheme 1]

Experimental

Crystal data
  • [Dy(NO3)2(C6H18N3OP)4][AgMoS4]

  • Mr = 1335.43

  • Monoclinic, P 21 /c

  • a = 15.786 (3) Å

  • b = 29.671 (6) Å

  • c = 11.331 (2) Å

  • β = 90.93 (3)°

  • V = 5306.6 (17) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 2.33 mm−1

  • T = 153 K

  • 0.35 × 0.25 × 0.18 mm

Data collection
  • Rigaku Saturn724+ diffractometer

  • Absorption correction: multi-scan (CrystalClear; Rigaku, 2008[Rigaku (2008). CrystalClear. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.503, Tmax = 0.658

  • 25288 measured reflections

  • 10445 independent reflections

  • 9394 reflections with I > 2σ(I)

  • Rint = 0.023

Refinement
  • R[F2 > 2σ(F2)] = 0.032

  • wR(F2) = 0.074

  • S = 1.05

  • 10445 reflections

  • 556 parameters

  • H-atom parameters constrained

  • Δρmax = 1.00 e Å−3

  • Δρmin = −1.00 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: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); 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) and unique properties as functional materials, such as third-order nonlinear optical (NLO) materials (Zhang 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 {[Dy(hmp)4(NO3)2][MoS4Ag]}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 W isomorph (Wei et al., 2010). Dy3- 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. The anionic chain in the title compound has a distorted linear configuration with Mo—Ag—Mo and Ag—Mo—Ag angles of 161.911 (13) and 154.014 (13) °, respectively (Fig. 2).

Related literature top

For one-dimensional Mo(W)/S/Ag anionic polymers, see: Niu et al. (2004). For their unique properties, see: Zhang et al. (2007). For the W isomorph of the title complex, see: Wei et al. (2010).

Experimental top

Ag2S (1 mmol) was added to a solution of [NH4]2MoS4 (2 mmol in 25 mL hmp) with thorough stirring for 5 h. The solution underwent an additional stirring for two minutes after Dy(NO3)3.6H2O (1 mmol) was added. After filtration the black-red filtrate was carefully laid on the surface with 30 ml i-PrOH. Black-red block crystals were obtained after two weeks.

Refinement top

H atoms were positioned geometrically and refined in a riding mode, with Uiso = 1.5Ueq(C) and C—H distance = 0.96 Å.

Structure description top

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., 2007). Different solvent-coordinated rare-earth cations proved effective to obtain various configurations of anionic chains (Niu et al., 2004). The title compound {[Dy(hmp)4(NO3)2][MoS4Ag]}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 W isomorph (Wei et al., 2010). Dy3- 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. The anionic chain in the title compound has a distorted linear configuration with Mo—Ag—Mo and Ag—Mo—Ag angles of 161.911 (13) and 154.014 (13) °, respectively (Fig. 2).

For one-dimensional Mo(W)/S/Ag anionic polymers, see: Niu et al. (2004). For their unique properties, see: Zhang et al. (2007). For the W isomorph of the title complex, see: Wei et al. (2010).

Computing details top

Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear (Rigaku, 2008); data reduction: CrystalClear (Rigaku, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (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 atom labels and 30% probability displacement ellipsoids. All H atoms have been omitted for clarity.
[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, Symmetry code: (i) x, 1/2 - y, -1/2 + z.
catena-Poly[[tetrakis(hexamethylphosphoramide-κO)bis(nitrato- κ2O,O')dysprosium(III)] [molybdenum(VI)-di-µ-sulfido-silver(I)-di-µ-sulfido]] top
Crystal data top
[Dy(NO3)2(C6H18N3OP)4][AgMoS4]F(000) = 2692
Mr = 1335.43Dx = 1.672 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 22208 reflections
a = 15.786 (3) Åθ = 2.7–29.1°
b = 29.671 (6) ŵ = 2.33 mm1
c = 11.331 (2) ÅT = 153 K
β = 90.93 (3)°Block, black-red
V = 5306.6 (17) Å30.35 × 0.25 × 0.18 mm
Z = 4
Data collection top
Rigaku Saturn724+
diffractometer
10445 independent reflections
Radiation source: fine-focus sealed tube9394 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
dtprofit.ref scansθmax = 26.0°, θmin = 2.7°
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2008)
h = 1919
Tmin = 0.503, Tmax = 0.658k = 2936
25288 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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.074H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0305P)2 + 8.9291P]
where P = (Fo2 + 2Fc2)/3
10445 reflections(Δ/σ)max = 0.002
556 parametersΔρmax = 1.00 e Å3
0 restraintsΔρmin = 1.00 e Å3
Crystal data top
[Dy(NO3)2(C6H18N3OP)4][AgMoS4]V = 5306.6 (17) Å3
Mr = 1335.43Z = 4
Monoclinic, P21/cMo Kα radiation
a = 15.786 (3) ŵ = 2.33 mm1
b = 29.671 (6) ÅT = 153 K
c = 11.331 (2) Å0.35 × 0.25 × 0.18 mm
β = 90.93 (3)°
Data collection top
Rigaku Saturn724+
diffractometer
10445 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2008)
9394 reflections with I > 2σ(I)
Tmin = 0.503, Tmax = 0.658Rint = 0.023
25288 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0320 restraints
wR(F2) = 0.074H-atom parameters constrained
S = 1.05Δρmax = 1.00 e Å3
10445 reflectionsΔρmin = 1.00 e Å3
556 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Dy10.737719 (10)0.082623 (5)0.827853 (15)0.01950 (5)
P10.52135 (6)0.13298 (3)0.82207 (9)0.0266 (2)
P20.69790 (7)0.03042 (3)0.69823 (9)0.0289 (2)
P30.95845 (6)0.09627 (3)0.73131 (10)0.0283 (2)
P40.79428 (8)0.14677 (4)1.09803 (10)0.0402 (3)
O10.60267 (15)0.10717 (8)0.8236 (2)0.0274 (6)
O20.70672 (16)0.01805 (8)0.7283 (2)0.0286 (6)
O30.87595 (15)0.08051 (8)0.7800 (2)0.0298 (6)
O40.77256 (16)0.12686 (8)0.9820 (2)0.0300 (6)
O50.80099 (16)0.02668 (9)0.9669 (2)0.0321 (6)
O60.66868 (16)0.04088 (9)0.9901 (2)0.0311 (6)
O70.75133 (17)0.15817 (8)0.7373 (2)0.0331 (6)
O80.72330 (18)0.10333 (9)0.6184 (2)0.0326 (6)
O90.7368 (2)0.00134 (11)1.1224 (3)0.0496 (8)
O100.7251 (3)0.17185 (11)0.5514 (3)0.0670 (11)
N10.44407 (19)0.09830 (12)0.8493 (3)0.0319 (7)
N20.5226 (2)0.17305 (12)0.9216 (4)0.0427 (9)
N30.5055 (2)0.15715 (15)0.6955 (3)0.0495 (10)
N40.7203 (2)0.03716 (11)0.5583 (3)0.0367 (8)
N50.6051 (2)0.04792 (13)0.7374 (4)0.0522 (11)
N60.7637 (3)0.06553 (12)0.7669 (3)0.0468 (10)
N71.0342 (2)0.07053 (13)0.8029 (3)0.0414 (9)
N80.9831 (2)0.14915 (12)0.7387 (4)0.0458 (10)
N90.9562 (2)0.08656 (14)0.5884 (3)0.0466 (10)
N100.8965 (3)0.13862 (15)1.1254 (5)0.0758 (16)
N110.7738 (3)0.20013 (12)1.0971 (3)0.0533 (11)
N120.7402 (4)0.12385 (16)1.2004 (4)0.0725 (15)
N130.7356 (2)0.02235 (10)1.0295 (3)0.0310 (7)
N140.7330 (2)0.14538 (11)0.6336 (3)0.0359 (8)
C10.3560 (2)0.10709 (18)0.8134 (4)0.0465 (12)
H1A0.32960.07940.78890.070*
H1B0.35480.12810.74910.070*
H1C0.32590.11950.87890.070*
C20.4534 (3)0.06453 (15)0.9437 (4)0.0402 (10)
H2A0.43170.07661.01590.060*
H2B0.51220.05710.95450.060*
H2C0.42230.03790.92240.060*
C30.4539 (3)0.18330 (17)1.0017 (5)0.0557 (13)
H3A0.47690.18921.07910.084*
H3B0.41590.15811.00500.084*
H3C0.42370.20940.97370.084*
C40.5898 (3)0.20739 (17)0.9192 (6)0.0673 (17)
H4A0.56760.23480.88590.101*
H4B0.63570.19680.87200.101*
H4C0.61010.21300.99820.101*
C50.4640 (4)0.2012 (2)0.6806 (6)0.084 (2)
H5A0.50230.22180.64370.127*
H5B0.44850.21270.75640.127*
H5C0.41410.19780.63190.127*
C60.5176 (4)0.1322 (3)0.5889 (5)0.086 (2)
H6A0.46380.12740.55020.128*
H6B0.54300.10360.60730.128*
H6C0.55390.14890.53760.128*
C70.7262 (3)0.08241 (15)0.5065 (4)0.0511 (13)
H7A0.67220.09080.47320.077*
H7B0.74240.10360.56670.077*
H7C0.76790.08230.44570.077*
C80.6988 (3)0.00220 (17)0.4730 (4)0.0520 (13)
H8A0.73920.00240.41070.078*
H8B0.69960.02660.51140.078*
H8C0.64320.00780.44070.078*
C90.5347 (3)0.01677 (19)0.7464 (6)0.0659 (16)
H9A0.50570.01470.67140.099*
H9B0.55550.01240.76890.099*
H9C0.49610.02750.80470.099*
C100.5811 (4)0.0960 (2)0.7209 (6)0.083 (2)
H10A0.54370.10500.78260.124*
H10B0.63110.11440.72370.124*
H10C0.55290.09970.64580.124*
C110.7531 (5)0.08082 (19)0.8861 (6)0.0775 (19)
H11A0.75700.11310.88850.116*
H11B0.69860.07160.91360.116*
H11C0.79670.06800.93580.116*
C120.8532 (4)0.0681 (2)0.7337 (6)0.084 (2)
H12A0.88730.05220.79090.126*
H12B0.86010.05460.65740.126*
H12C0.87050.09910.73090.126*
C131.1235 (3)0.0808 (2)0.7837 (6)0.077 (2)
H13A1.15320.08170.85830.116*
H13B1.12820.10950.74530.116*
H13C1.14780.05780.73490.116*
C141.0206 (3)0.02790 (17)0.8615 (5)0.0635 (16)
H14A1.03370.00370.80860.095*
H14B0.96240.02570.88430.095*
H14C1.05660.02600.93040.095*
C150.9514 (3)0.18288 (18)0.6533 (7)0.086 (2)
H15A0.90780.20060.68900.129*
H15B0.92860.16780.58490.129*
H15C0.99710.20220.63050.129*
C161.0139 (4)0.1688 (2)0.8498 (6)0.085 (2)
H16A1.05760.19030.83380.127*
H16B1.03650.14540.89970.127*
H16C0.96800.18350.88880.127*
C170.9077 (3)0.04800 (19)0.5440 (4)0.0566 (14)
H17A0.89560.05200.46140.085*
H17B0.85560.04570.58600.085*
H17C0.94020.02090.55540.085*
C181.0304 (4)0.0961 (2)0.5161 (5)0.0771 (19)
H18A1.07070.07210.52460.116*
H18B1.05590.12390.54160.116*
H18C1.01300.09870.43480.116*
C190.9354 (4)0.0953 (2)1.1108 (7)0.086 (2)
H19A0.99040.09901.07710.129*
H19B0.90070.07701.05930.129*
H19C0.94110.08071.18620.129*
C200.9515 (5)0.1716 (3)1.1851 (7)0.110 (3)
H20A0.94910.16721.26890.166*
H20B0.93280.20151.16570.166*
H20C1.00870.16761.15960.166*
C210.8026 (4)0.22745 (14)0.9966 (4)0.0508 (13)
H21A0.76460.25230.98440.076*
H21B0.80350.20910.92680.076*
H21C0.85860.23871.01330.076*
C220.7481 (6)0.22620 (19)1.2004 (5)0.095 (3)
H22A0.79550.24331.22990.142*
H22B0.72900.20601.26070.142*
H22C0.70290.24631.17820.142*
C230.6502 (5)0.1210 (2)1.1891 (6)0.092 (2)
H23A0.63270.09031.19940.138*
H23B0.63280.13131.11210.138*
H23C0.62460.13951.24810.138*
C240.7796 (7)0.1055 (3)1.3091 (6)0.129 (4)
H24A0.75010.11671.37640.194*
H24B0.83780.11471.31390.194*
H24C0.77640.07321.30760.194*
Mo10.215792 (19)0.271918 (10)0.02476 (3)0.02053 (8)
Ag10.21712 (2)0.234959 (11)0.21455 (3)0.03744 (9)
S10.21612 (7)0.19909 (3)0.01654 (9)0.0339 (2)
S20.21379 (7)0.31529 (3)0.13294 (8)0.0300 (2)
S30.10204 (6)0.28647 (4)0.13144 (9)0.0363 (2)
S40.33020 (6)0.28755 (4)0.12530 (9)0.0346 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Dy10.01679 (9)0.01407 (8)0.02766 (10)0.00034 (6)0.00165 (7)0.00080 (7)
P10.0199 (5)0.0323 (5)0.0277 (5)0.0048 (4)0.0007 (4)0.0059 (4)
P20.0360 (5)0.0195 (5)0.0315 (5)0.0072 (4)0.0106 (4)0.0066 (4)
P30.0175 (4)0.0257 (5)0.0419 (6)0.0010 (4)0.0043 (4)0.0074 (4)
P40.0615 (8)0.0249 (5)0.0336 (6)0.0103 (5)0.0192 (6)0.0016 (5)
O10.0196 (12)0.0274 (13)0.0354 (15)0.0040 (11)0.0013 (11)0.0020 (12)
O20.0334 (14)0.0196 (13)0.0328 (14)0.0018 (11)0.0014 (12)0.0056 (11)
O30.0189 (12)0.0253 (13)0.0452 (17)0.0004 (11)0.0044 (12)0.0057 (12)
O40.0337 (14)0.0222 (13)0.0338 (15)0.0012 (11)0.0065 (12)0.0053 (11)
O50.0253 (14)0.0268 (14)0.0442 (16)0.0009 (11)0.0002 (12)0.0056 (12)
O60.0225 (13)0.0307 (14)0.0402 (16)0.0006 (11)0.0003 (12)0.0064 (12)
O70.0391 (16)0.0206 (13)0.0396 (16)0.0052 (12)0.0016 (13)0.0007 (12)
O80.0412 (16)0.0237 (14)0.0332 (15)0.0043 (12)0.0073 (13)0.0005 (12)
O90.055 (2)0.052 (2)0.0415 (18)0.0042 (16)0.0014 (15)0.0248 (16)
O100.111 (3)0.0411 (19)0.049 (2)0.017 (2)0.014 (2)0.0219 (17)
N10.0194 (15)0.045 (2)0.0317 (18)0.0004 (15)0.0010 (14)0.0059 (16)
N20.0351 (19)0.0321 (19)0.061 (2)0.0031 (16)0.0133 (18)0.0101 (18)
N30.034 (2)0.076 (3)0.038 (2)0.002 (2)0.0073 (17)0.026 (2)
N40.051 (2)0.0295 (18)0.0295 (18)0.0046 (16)0.0091 (16)0.0066 (15)
N50.046 (2)0.047 (2)0.064 (3)0.0217 (19)0.018 (2)0.023 (2)
N60.072 (3)0.0254 (18)0.043 (2)0.0060 (19)0.014 (2)0.0037 (17)
N70.0219 (17)0.051 (2)0.051 (2)0.0029 (16)0.0028 (16)0.0282 (19)
N80.034 (2)0.0281 (19)0.075 (3)0.0016 (16)0.0096 (19)0.0091 (19)
N90.0308 (19)0.068 (3)0.041 (2)0.0083 (18)0.0069 (17)0.0096 (19)
N100.081 (3)0.046 (3)0.098 (4)0.016 (2)0.058 (3)0.004 (3)
N110.104 (4)0.0243 (18)0.031 (2)0.010 (2)0.002 (2)0.0090 (16)
N120.118 (4)0.055 (3)0.044 (3)0.033 (3)0.004 (3)0.013 (2)
N130.0316 (18)0.0231 (16)0.0383 (19)0.0052 (14)0.0022 (15)0.0013 (15)
N140.040 (2)0.0271 (18)0.041 (2)0.0042 (15)0.0057 (17)0.0062 (16)
C10.021 (2)0.071 (3)0.047 (3)0.002 (2)0.0017 (19)0.012 (2)
C20.035 (2)0.044 (2)0.042 (2)0.002 (2)0.0052 (19)0.013 (2)
C30.053 (3)0.048 (3)0.066 (3)0.014 (2)0.021 (3)0.010 (3)
C40.058 (3)0.044 (3)0.100 (5)0.008 (3)0.019 (3)0.023 (3)
C50.060 (4)0.089 (5)0.104 (5)0.014 (3)0.014 (3)0.064 (4)
C60.059 (4)0.166 (7)0.032 (3)0.022 (4)0.008 (3)0.001 (4)
C70.070 (3)0.039 (3)0.045 (3)0.007 (2)0.021 (3)0.019 (2)
C80.069 (3)0.052 (3)0.036 (3)0.003 (3)0.008 (2)0.000 (2)
C90.031 (3)0.068 (4)0.098 (5)0.001 (3)0.007 (3)0.016 (3)
C100.096 (5)0.069 (4)0.086 (4)0.049 (4)0.041 (4)0.034 (3)
C110.106 (5)0.056 (4)0.071 (4)0.025 (3)0.010 (4)0.022 (3)
C120.058 (4)0.090 (5)0.103 (5)0.019 (3)0.005 (4)0.026 (4)
C130.020 (2)0.112 (5)0.098 (5)0.004 (3)0.005 (3)0.066 (4)
C140.036 (3)0.055 (3)0.100 (4)0.007 (2)0.009 (3)0.044 (3)
C150.049 (3)0.046 (3)0.164 (7)0.002 (3)0.011 (4)0.052 (4)
C160.104 (5)0.062 (4)0.089 (5)0.041 (4)0.033 (4)0.020 (3)
C170.044 (3)0.077 (4)0.048 (3)0.004 (3)0.003 (2)0.014 (3)
C180.058 (3)0.125 (6)0.049 (3)0.026 (4)0.018 (3)0.008 (3)
C190.061 (4)0.067 (4)0.128 (6)0.003 (3)0.046 (4)0.014 (4)
C200.114 (6)0.095 (5)0.120 (6)0.044 (5)0.073 (5)0.004 (5)
C210.081 (4)0.027 (2)0.044 (3)0.003 (2)0.002 (3)0.004 (2)
C220.190 (8)0.049 (3)0.046 (3)0.029 (4)0.025 (4)0.022 (3)
C230.118 (6)0.087 (5)0.074 (4)0.041 (4)0.053 (4)0.009 (4)
C240.223 (11)0.113 (7)0.052 (4)0.018 (7)0.011 (5)0.043 (4)
Mo10.02501 (16)0.02009 (15)0.01645 (15)0.00239 (12)0.00122 (12)0.00120 (12)
Ag10.0581 (2)0.03582 (17)0.01837 (15)0.00052 (15)0.00063 (14)0.00160 (12)
S10.0556 (7)0.0198 (4)0.0263 (5)0.0047 (4)0.0004 (5)0.0027 (4)
S20.0447 (6)0.0226 (4)0.0228 (5)0.0001 (4)0.0013 (4)0.0054 (4)
S30.0304 (5)0.0506 (6)0.0278 (5)0.0131 (5)0.0062 (4)0.0032 (5)
S40.0299 (5)0.0467 (6)0.0272 (5)0.0055 (5)0.0024 (4)0.0028 (5)
Geometric parameters (Å, º) top
Dy1—O42.246 (3)C6—H6A0.9600
Dy1—O12.253 (2)C6—H6B0.9600
Dy1—O32.258 (2)C6—H6C0.9600
Dy1—O22.273 (2)C7—H7A0.9600
Dy1—O82.459 (3)C7—H7B0.9600
Dy1—O72.476 (3)C7—H7C0.9600
Dy1—O62.483 (3)C8—H8A0.9600
Dy1—O52.487 (3)C8—H8B0.9600
Dy1—N142.883 (3)C8—H8C0.9600
Dy1—N132.902 (3)C9—H9A0.9600
P1—O11.495 (3)C9—H9B0.9600
P1—N31.619 (4)C9—H9C0.9600
P1—N11.629 (3)C10—H10A0.9600
P1—N21.639 (4)C10—H10B0.9600
P2—O21.484 (3)C10—H10C0.9600
P2—N51.622 (4)C11—H11A0.9600
P2—N41.642 (3)C11—H11B0.9600
P2—N61.657 (4)C11—H11C0.9600
P3—O31.498 (3)C12—H12A0.9600
P3—N81.618 (4)C12—H12B0.9600
P3—N71.625 (3)C12—H12C0.9600
P3—N91.644 (4)C13—H13A0.9600
P4—O41.476 (3)C13—H13B0.9600
P4—N121.603 (5)C13—H13C0.9600
P4—N111.616 (4)C14—H14A0.9600
P4—N101.656 (5)C14—H14B0.9600
O5—N131.268 (4)C14—H14C0.9600
O6—N131.266 (4)C15—H15A0.9600
O7—N141.264 (4)C15—H15B0.9600
O8—N141.268 (4)C15—H15C0.9600
O9—N131.223 (4)C16—H16A0.9600
O10—N141.223 (4)C16—H16B0.9600
N1—C11.466 (5)C16—H16C0.9600
N1—C21.472 (5)C17—H17A0.9600
N2—C31.457 (5)C17—H17B0.9600
N2—C41.472 (6)C17—H17C0.9600
N3—C61.433 (7)C18—H18A0.9600
N3—C51.471 (7)C18—H18B0.9600
N4—C81.454 (6)C18—H18C0.9600
N4—C71.469 (5)C19—H19A0.9600
N5—C91.451 (6)C19—H19B0.9600
N5—C101.488 (6)C19—H19C0.9600
N6—C111.437 (7)C20—H20A0.9600
N6—C121.469 (7)C20—H20B0.9600
N7—C141.446 (5)C20—H20C0.9600
N7—C131.463 (5)C21—H21A0.9600
N8—C161.463 (7)C21—H21B0.9600
N8—C151.474 (6)C21—H21C0.9600
N9—C171.461 (6)C22—H22A0.9600
N9—C181.467 (6)C22—H22B0.9600
N10—C191.437 (8)C22—H22C0.9600
N10—C201.465 (7)C23—H23A0.9600
N11—C221.466 (6)C23—H23B0.9600
N11—C211.475 (6)C23—H23C0.9600
N12—C231.427 (8)C24—H24A0.9600
N12—C241.474 (8)C24—H24B0.9600
C1—H1A0.9600C24—H24C0.9600
C1—H1B0.9600Mo1—S32.1912 (12)
C1—H1C0.9600Mo1—S42.2003 (12)
C2—H2A0.9600Mo1—S22.2027 (10)
C2—H2B0.9600Mo1—S12.2110 (11)
C2—H2C0.9600Mo1—Ag12.9247 (6)
C3—H3A0.9600Mo1—Ag1i2.9614 (7)
C3—H3B0.9600Ag1—S12.4830 (11)
C3—H3C0.9600Ag1—S22.5569 (11)
C4—H4A0.9600Ag1—S4ii2.6116 (13)
C4—H4B0.9600Ag1—S3ii2.6178 (13)
C4—H4C0.9600Ag1—Mo1ii2.9614 (7)
C5—H5A0.9600S3—Ag1i2.6178 (13)
C5—H5B0.9600S4—Ag1i2.6116 (13)
C5—H5C0.9600
O4—Dy1—O192.72 (9)N3—C5—H5C109.5
O4—Dy1—O388.71 (10)H5A—C5—H5C109.5
O1—Dy1—O3157.20 (9)H5B—C5—H5C109.5
O4—Dy1—O2157.93 (9)N3—C6—H6A109.5
O1—Dy1—O293.77 (9)N3—C6—H6B109.5
O3—Dy1—O293.36 (9)H6A—C6—H6B109.5
O4—Dy1—O8128.49 (9)N3—C6—H6C109.5
O1—Dy1—O879.97 (10)H6A—C6—H6C109.5
O3—Dy1—O881.37 (10)H6B—C6—H6C109.5
O2—Dy1—O873.47 (9)N4—C7—H7A109.5
O4—Dy1—O776.79 (9)N4—C7—H7B109.5
O1—Dy1—O777.70 (9)H7A—C7—H7B109.5
O3—Dy1—O780.50 (9)N4—C7—H7C109.5
O2—Dy1—O7125.22 (9)H7A—C7—H7C109.5
O8—Dy1—O751.75 (9)H7B—C7—H7C109.5
O4—Dy1—O679.67 (9)N4—C8—H8A109.5
O1—Dy1—O675.55 (9)N4—C8—H8B109.5
O3—Dy1—O6126.97 (9)H8A—C8—H8B109.5
O2—Dy1—O681.58 (9)N4—C8—H8C109.5
O8—Dy1—O6143.55 (9)H8A—C8—H8C109.5
O7—Dy1—O6143.17 (9)H8B—C8—H8C109.5
O4—Dy1—O578.85 (9)N5—C9—H9A109.5
O1—Dy1—O5126.84 (9)N5—C9—H9B109.5
O3—Dy1—O575.75 (9)H9A—C9—H9B109.5
O2—Dy1—O580.39 (9)N5—C9—H9C109.5
O8—Dy1—O5143.94 (9)H9A—C9—H9C109.5
O7—Dy1—O5146.12 (9)H9B—C9—H9C109.5
O6—Dy1—O551.29 (8)N5—C10—H10A109.5
O4—Dy1—N14102.67 (10)N5—C10—H10B109.5
O1—Dy1—N1476.24 (10)H10A—C10—H10B109.5
O3—Dy1—N1481.24 (10)N5—C10—H10C109.5
O2—Dy1—N1499.36 (10)H10A—C10—H10C109.5
O8—Dy1—N1425.94 (9)H10B—C10—H10C109.5
O7—Dy1—N1425.88 (9)N6—C11—H11A109.5
O6—Dy1—N14151.78 (9)N6—C11—H11B109.5
O5—Dy1—N14156.92 (9)H11A—C11—H11B109.5
O4—Dy1—N1375.74 (9)N6—C11—H11C109.5
O1—Dy1—N13101.14 (10)H11A—C11—H11C109.5
O3—Dy1—N13101.26 (10)H11B—C11—H11C109.5
O2—Dy1—N1382.32 (9)N6—C12—H12A109.5
O8—Dy1—N13155.77 (9)N6—C12—H12B109.5
O7—Dy1—N13152.42 (9)H12A—C12—H12B109.5
O6—Dy1—N1325.72 (8)N6—C12—H12C109.5
O5—Dy1—N1325.76 (9)H12A—C12—H12C109.5
N14—Dy1—N13176.94 (10)H12B—C12—H12C109.5
O1—P1—N3110.93 (19)N7—C13—H13A109.5
O1—P1—N1108.65 (16)N7—C13—H13B109.5
N3—P1—N1110.02 (19)H13A—C13—H13B109.5
O1—P1—N2111.29 (17)N7—C13—H13C109.5
N3—P1—N2106.7 (2)H13A—C13—H13C109.5
N1—P1—N2109.18 (19)H13B—C13—H13C109.5
O2—P2—N5109.23 (18)N7—C14—H14A109.5
O2—P2—N4108.57 (16)N7—C14—H14B109.5
N5—P2—N4115.8 (2)H14A—C14—H14B109.5
O2—P2—N6116.48 (18)N7—C14—H14C109.5
N5—P2—N6103.4 (2)H14A—C14—H14C109.5
N4—P2—N6103.50 (19)H14B—C14—H14C109.5
O3—P3—N8119.56 (17)N8—C15—H15A109.5
O3—P3—N7107.83 (16)N8—C15—H15B109.5
N8—P3—N7104.8 (2)H15A—C15—H15B109.5
O3—P3—N9107.68 (18)N8—C15—H15C109.5
N8—P3—N9102.9 (2)H15A—C15—H15C109.5
N7—P3—N9114.4 (2)H15B—C15—H15C109.5
O4—P4—N12110.9 (2)N8—C16—H16A109.5
O4—P4—N11110.04 (18)N8—C16—H16B109.5
N12—P4—N11108.2 (3)H16A—C16—H16B109.5
O4—P4—N10108.7 (2)N8—C16—H16C109.5
N12—P4—N10109.3 (3)H16A—C16—H16C109.5
N11—P4—N10109.8 (2)H16B—C16—H16C109.5
P1—O1—Dy1168.03 (16)N9—C17—H17A109.5
P2—O2—Dy1161.71 (17)N9—C17—H17B109.5
P3—O3—Dy1158.35 (16)H17A—C17—H17B109.5
P4—O4—Dy1167.58 (17)N9—C17—H17C109.5
N13—O5—Dy195.7 (2)H17A—C17—H17C109.5
N13—O6—Dy195.9 (2)H17B—C17—H17C109.5
N14—O7—Dy195.4 (2)N9—C18—H18A109.5
N14—O8—Dy196.1 (2)N9—C18—H18B109.5
C1—N1—C2114.0 (3)H18A—C18—H18B109.5
C1—N1—P1123.0 (3)N9—C18—H18C109.5
C2—N1—P1120.1 (3)H18A—C18—H18C109.5
C3—N2—C4114.3 (4)H18B—C18—H18C109.5
C3—N2—P1125.4 (3)N10—C19—H19A109.5
C4—N2—P1119.4 (3)N10—C19—H19B109.5
C6—N3—C5115.3 (5)H19A—C19—H19B109.5
C6—N3—P1119.9 (4)N10—C19—H19C109.5
C5—N3—P1123.9 (4)H19A—C19—H19C109.5
C8—N4—C7113.7 (4)H19B—C19—H19C109.5
C8—N4—P2120.2 (3)N10—C20—H20A109.5
C7—N4—P2120.9 (3)N10—C20—H20B109.5
C9—N5—C10115.2 (4)H20A—C20—H20B109.5
C9—N5—P2120.8 (3)N10—C20—H20C109.5
C10—N5—P2120.2 (4)H20A—C20—H20C109.5
C11—N6—C12110.6 (5)H20B—C20—H20C109.5
C11—N6—P2123.9 (4)N11—C21—H21A109.5
C12—N6—P2120.7 (4)N11—C21—H21B109.5
C14—N7—C13113.6 (4)H21A—C21—H21B109.5
C14—N7—P3121.8 (3)N11—C21—H21C109.5
C13—N7—P3122.1 (3)H21A—C21—H21C109.5
C16—N8—C15113.5 (5)H21B—C21—H21C109.5
C16—N8—P3120.5 (4)N11—C22—H22A109.5
C15—N8—P3123.0 (4)N11—C22—H22B109.5
C17—N9—C18112.2 (4)H22A—C22—H22B109.5
C17—N9—P3118.6 (3)N11—C22—H22C109.5
C18—N9—P3120.8 (3)H22A—C22—H22C109.5
C19—N10—C20113.5 (5)H22B—C22—H22C109.5
C19—N10—P4121.8 (4)N12—C23—H23A109.5
C20—N10—P4123.9 (5)N12—C23—H23B109.5
C22—N11—C21114.8 (4)H23A—C23—H23B109.5
C22—N11—P4124.7 (4)N12—C23—H23C109.5
C21—N11—P4118.6 (3)H23A—C23—H23C109.5
C23—N12—C24117.3 (6)H23B—C23—H23C109.5
C23—N12—P4120.1 (4)N12—C24—H24A109.5
C24—N12—P4122.6 (6)N12—C24—H24B109.5
O9—N13—O6121.7 (3)H24A—C24—H24B109.5
O9—N13—O5122.1 (3)N12—C24—H24C109.5
O6—N13—O5116.2 (3)H24A—C24—H24C109.5
O9—N13—Dy1172.4 (3)H24B—C24—H24C109.5
O6—N13—Dy158.33 (17)S3—Mo1—S4110.18 (4)
O5—N13—Dy158.51 (17)S3—Mo1—S2108.06 (4)
O10—N14—O7122.3 (3)S4—Mo1—S2108.64 (4)
O10—N14—O8121.2 (4)S3—Mo1—S1107.96 (4)
O7—N14—O8116.5 (3)S4—Mo1—S1108.45 (4)
O10—N14—Dy1175.6 (3)S2—Mo1—S1113.54 (4)
O7—N14—Dy158.76 (18)S3—Mo1—Ag1125.37 (4)
O8—N14—Dy157.99 (18)S4—Mo1—Ag1124.43 (4)
N1—C1—H1A109.5S2—Mo1—Ag157.79 (3)
N1—C1—H1B109.5S1—Mo1—Ag155.76 (3)
H1A—C1—H1B109.5S3—Mo1—Ag1i58.82 (4)
N1—C1—H1C109.5S4—Mo1—Ag1i58.59 (4)
H1A—C1—H1C109.5S2—Mo1—Ag1i148.20 (3)
H1B—C1—H1C109.5S1—Mo1—Ag1i98.27 (3)
N1—C2—H2A109.5Ag1—Mo1—Ag1i154.014 (13)
N1—C2—H2B109.5S1—Ag1—S294.19 (3)
H2A—C2—H2B109.5S1—Ag1—S4ii120.83 (4)
N1—C2—H2C109.5S2—Ag1—S4ii119.97 (4)
H2A—C2—H2C109.5S1—Ag1—S3ii120.26 (4)
H2B—C2—H2C109.5S2—Ag1—S3ii117.20 (4)
N2—C3—H3A109.5S4ii—Ag1—S3ii87.05 (4)
N2—C3—H3B109.5S1—Ag1—Mo147.40 (3)
H3A—C3—H3B109.5S2—Ag1—Mo146.79 (2)
N2—C3—H3C109.5S4ii—Ag1—Mo1137.28 (3)
H3A—C3—H3C109.5S3ii—Ag1—Mo1135.60 (3)
H3B—C3—H3C109.5S1—Ag1—Mo1ii150.66 (3)
N2—C4—H4A109.5S2—Ag1—Mo1ii115.12 (2)
N2—C4—H4B109.5S4ii—Ag1—Mo1ii45.98 (3)
H4A—C4—H4B109.5S3ii—Ag1—Mo1ii45.74 (3)
N2—C4—H4C109.5Mo1—Ag1—Mo1ii161.911 (13)
H4A—C4—H4C109.5Mo1—S1—Ag176.84 (3)
H4B—C4—H4C109.5Mo1—S2—Ag175.42 (3)
N3—C5—H5A109.5Mo1—S3—Ag1i75.44 (3)
N3—C5—H5B109.5Mo1—S4—Ag1i75.43 (3)
H5A—C5—H5B109.5
Symmetry codes: (i) x, y+1/2, z1/2; (ii) x, y+1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[Dy(NO3)2(C6H18N3OP)4][AgMoS4]
Mr1335.43
Crystal system, space groupMonoclinic, P21/c
Temperature (K)153
a, b, c (Å)15.786 (3), 29.671 (6), 11.331 (2)
β (°) 90.93 (3)
V3)5306.6 (17)
Z4
Radiation typeMo Kα
µ (mm1)2.33
Crystal size (mm)0.35 × 0.25 × 0.18
Data collection
DiffractometerRigaku Saturn724+
Absorption correctionMulti-scan
(CrystalClear; Rigaku, 2008)
Tmin, Tmax0.503, 0.658
No. of measured, independent and
observed [I > 2σ(I)] reflections
25288, 10445, 9394
Rint0.023
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.074, 1.05
No. of reflections10445
No. of parameters556
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.00, 1.00

Computer programs: CrystalClear (Rigaku, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

This work was supported by the Foundation of Jiangsu University (08JDG036).

References

First citationNiu, Y. Y., Zheng, H. G., Hou, H. W. & Xin, X. Q. (2004). Coord. Chem. Rev. 248, 169–183.  Web of Science CrossRef CAS Google Scholar
First citationRigaku (2008). CrystalClear. Rigaku Corporation, Tokyo, Japan.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWei, H., Zhang, J. & Zhang, C. (2010). Acta Cryst. E66, m1193–m1194.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationZhang, C., Song, Y. L. & Wang, X. (2007). Coord. Chem. Rev. 251, 111–141.  Web of Science CrossRef CAS Google Scholar

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