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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 9| September 2011| Pages m1206-m1207

catena-Poly[[tetra­kis­(hexa­methyl­phospho­ramide-κO)bis­­(nitrato-κ2O,O′)yttrium(III)] [silver(I)-di-μ-sulfido-molybdenum(VI)-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 25 July 2011; accepted 2 August 2011; online 6 August 2011)

In the cation of the title compound, {[Y(NO3)2(C6H18N3OP)4][AgMoS4]}n, the Y atom is coordinated by eight O atoms from two chelating nitrate groups and four hexa­methyl­phospho­ramide (hmp) ligands, which gives rise to a distorted square-anti­prismatic environment. Together with the two nitrate ligands, the overall charge for the complex cation is +1, which leads to the anionic chain having a monovalent repeat unit. The polymeric anionic chain, with Mo—Ag—Mo and Ag—Mo—Ag angles of 161.916 (13) and 153.915 (13)°, respectively, presents a distorted linear configuration. The cations and the anions are linked via weak C—H⋯S hydrogen-bonding inter­actions while the cations exhibit inter­molecular C—H⋯O inter­actions. The structure is isotypic with the corresponding W, Yb, Eu, Nd, La and Dy complexes.

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.]) and for their properties, see: Zhang, Song et al. (2007[Zhang, C., Song, Y. L. & Wang, X. (2007). Coord. Chem. Rev. 251, 111-141.]). For isotypic W, Yb, Eu, Nd, La and Dy complexes, 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.]), respectively.

[Scheme 1]

Experimental

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

  • Mr = 1261.84

  • Monoclinic, P 21 /c

  • a = 15.777 (3) Å

  • b = 29.650 (6) Å

  • c = 11.339 (2) Å

  • β = 90.90 (3)°

  • V = 5303.6 (17) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 2.02 mm−1

  • T = 153 K

  • 0.35 × 0.20 × 0.15 mm

Data collection
  • Rigaku Saturn724+ diffractometer

  • Absorption correction: multi-scan (CrystalClear; Rigaku, 2007[Rigaku (2007). CrystalClear. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.622, Tmax = 0.739

  • 25568 measured reflections

  • 10435 independent reflections

  • 8978 reflections with I > 2σ(I)

  • Rint = 0.033

Refinement
  • R[F2 > 2σ(F2)] = 0.045

  • wR(F2) = 0.091

  • S = 1.02

  • 10435 reflections

  • 556 parameters

  • H-atom parameters constrained

  • Δρmax = 0.86 e Å−3

  • Δρmin = −0.79 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
C5—H5A⋯S2i 0.96 2.79 3.710 (6) 160
C16—H16A⋯O10ii 0.96 2.49 3.292 (6) 141
C18—H18A⋯O10iii 0.96 2.54 3.470 (9) 162
Symmetry codes: (i) -x+1, -y, -z+1; (ii) [x, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]; (iii) x, y, z-1.

Data collection: CrystalClear (Rigaku, 2007[Rigaku (2007). 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, Song et al., 2007). Different solvent-coordinated rare-earth cations proved effective to obtain various configurations of anionic chains (Niu et al., 2004). In hexamethylphosphoramide (hmp), tetrathiomolybdate, silver iodide and dysprosium nitrate were self-assembled to form a one-dimensional anionic [AgMoS4]- chain in the compound, {[bi(nitrato-κ2O,O')tetrakis(hexamethylphosphoramide-κO) yttrium(III)]catena-[tetra-µ2-sulfidosilver(I)molybdenum(VI)]} with a formula of {[Y(hmp)4(NO3)2][MoS4Ag]}n.

In the title complex, Y3- in the cation is coordinated by eight O atoms from two nitrate and four hmp ligands. In the presence of two nitrate ligands, the cation in the title compound is univalent (Fig. 1). The anionic chain in the title compound (Fig. 2) has a distorted linear configuration with Mo—Ag—Mo and Ag—Mo—Ag angles 161.916 (13) and 153.915 (13) °, respectively. The cations and the anions are linked via weak hydrogen bondeing interactions of the type C—H···S while the cations exhibit C—H···O type intermolecular interactions (Table 1). The title complex is isostructural with W (Zhang, Cao et al., 2007), Yb (Cao et al., 2007), Eu (Zhang, Qian et al., 2007), Nd (Tang, Zhang & Zhang, 2008), La (Tang, Zhang, Zhang & Lu, 2008) and Dy (Zhang, 2010) isomorphs.

Related literature top

For one-dimensional Mo(W)/S/Ag anionic polymers, see: Niu et al. (2004) and for their properties, see: Zhang, Song et al. (2007). For isotypic W, Yb, Eu, Nd, La and Dy complexes, 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), respectively.

Experimental top

AgI (2 mmol) was added to a solution of [NH4]2MoS4 (2 mmol, in 28 mL hmp) with thorough stirring for 1.5 h. The solution was stirred for two minute after Y(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 about two weeks.

Refinement top

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

Computing details top

Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear (Rigaku, 2007); data reduction: CrystalClear (Rigaku, 2007); 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.
[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')yttrium(III)] [silver(I)-di-µ-sulfido-molybdenum(VI)-di-µ-sulfido]] yttrium(III)] top
Crystal data top
[Y(NO3)2(C6H18N3OP)4][AgMoS4]F(000) = 2584
Mr = 1261.84Dx = 1.580 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 22373 reflections
a = 15.777 (3) Åθ = 3.0–29.1°
b = 29.650 (6) ŵ = 2.02 mm1
c = 11.339 (2) ÅT = 153 K
β = 90.90 (3)°Block, black-red
V = 5303.6 (17) Å30.35 × 0.20 × 0.15 mm
Z = 4
Data collection top
Rigaku Saturn724+
diffractometer
10435 independent reflections
Radiation source: fine-focus sealed tube8978 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
dtprofit.ref scansθmax = 26.0°, θmin = 3.0°
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2007)
h = 1916
Tmin = 0.622, Tmax = 0.739k = 3136
25568 measured reflectionsl = 1213
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)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.091H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0325P)2 + 8.8309P]
where P = (Fo2 + 2Fc2)/3
10435 reflections(Δ/σ)max = 0.001
556 parametersΔρmax = 0.86 e Å3
0 restraintsΔρmin = 0.79 e Å3
Crystal data top
[Y(NO3)2(C6H18N3OP)4][AgMoS4]V = 5303.6 (17) Å3
Mr = 1261.84Z = 4
Monoclinic, P21/cMo Kα radiation
a = 15.777 (3) ŵ = 2.02 mm1
b = 29.650 (6) ÅT = 153 K
c = 11.339 (2) Å0.35 × 0.20 × 0.15 mm
β = 90.90 (3)°
Data collection top
Rigaku Saturn724+
diffractometer
10435 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2007)
8978 reflections with I > 2σ(I)
Tmin = 0.622, Tmax = 0.739Rint = 0.033
25568 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0450 restraints
wR(F2) = 0.091H-atom parameters constrained
S = 1.02Δρmax = 0.86 e Å3
10435 reflectionsΔρmin = 0.79 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
Y10.76202 (2)0.082657 (11)0.67216 (3)0.02106 (9)
P10.80109 (7)0.03027 (3)0.80037 (9)0.0302 (2)
P20.97799 (6)0.13259 (4)0.67874 (9)0.0279 (2)
P30.70659 (8)0.14681 (4)0.40283 (10)0.0411 (3)
P40.54196 (6)0.09637 (3)0.76889 (10)0.0289 (2)
O10.79306 (16)0.01827 (8)0.7709 (2)0.0286 (6)
O20.89658 (15)0.10701 (9)0.6769 (2)0.0280 (6)
O30.72762 (16)0.12679 (8)0.5191 (2)0.0303 (6)
O40.62457 (16)0.08067 (8)0.7201 (2)0.0311 (6)
O50.69836 (16)0.02710 (9)0.5347 (3)0.0327 (6)
O60.83115 (16)0.04107 (9)0.5110 (2)0.0316 (6)
O70.7627 (2)0.00151 (11)0.3795 (3)0.0509 (8)
O80.77629 (17)0.10293 (8)0.8803 (2)0.0329 (6)
O90.74838 (17)0.15805 (9)0.7615 (2)0.0328 (6)
O100.7740 (3)0.17164 (11)0.9480 (3)0.0663 (11)
N10.7789 (2)0.03678 (11)0.9404 (3)0.0371 (8)
N20.8939 (2)0.04824 (13)0.7609 (4)0.0507 (11)
N30.7348 (3)0.06527 (12)0.7321 (3)0.0458 (10)
N41.05558 (19)0.09750 (12)0.6519 (3)0.0322 (8)
N50.9777 (2)0.17290 (12)0.5800 (4)0.0444 (10)
N60.9940 (2)0.15647 (15)0.8057 (3)0.0511 (11)
N70.6047 (3)0.13896 (15)0.3742 (4)0.0727 (15)
N80.7272 (3)0.20021 (12)0.4047 (3)0.0525 (11)
N90.7609 (4)0.12405 (15)0.2997 (4)0.0691 (14)
N100.4666 (2)0.07045 (13)0.6975 (3)0.0422 (9)
N110.5444 (2)0.08704 (14)0.9118 (3)0.0465 (10)
N120.5170 (2)0.14923 (12)0.7602 (4)0.0480 (10)
N130.7639 (2)0.02248 (11)0.4719 (3)0.0317 (8)
N140.7659 (2)0.14511 (11)0.8656 (3)0.0358 (8)
C10.8019 (3)0.00241 (16)1.0252 (4)0.0525 (13)
H1A0.76060.00151.08630.079*
H1B0.80400.02640.98660.079*
H1C0.85660.00921.05910.079*
C20.7730 (3)0.08223 (15)0.9925 (4)0.0526 (13)
H2A0.82740.09091.02410.079*
H2B0.75540.10340.93290.079*
H2C0.73230.08201.05460.079*
C30.9646 (3)0.01683 (18)0.7541 (5)0.0639 (16)
H3A0.99340.01540.82920.096*
H3B0.94360.01260.73340.096*
H3C1.00330.02690.69520.096*
C40.9180 (4)0.09588 (19)0.7776 (5)0.0766 (19)
H4A0.95650.10470.71700.115*
H4B0.86820.11440.77330.115*
H4C0.94510.09950.85340.115*
C50.7462 (4)0.08073 (19)0.6131 (5)0.0776 (19)
H5A0.73660.11270.60940.116*
H5B0.80300.07420.58910.116*
H5C0.70670.06560.56150.116*
C60.6461 (4)0.0679 (2)0.7649 (6)0.084 (2)
H6A0.61190.05220.70750.126*
H6B0.63900.05430.84100.126*
H6C0.62890.09890.76780.126*
C71.0464 (3)0.06450 (15)0.5568 (4)0.0413 (11)
H7A1.06760.07710.48510.062*
H7B0.98760.05690.54620.062*
H7C1.07800.03780.57670.062*
C81.1434 (3)0.10681 (18)0.6883 (4)0.0482 (12)
H8A1.16990.07940.71440.072*
H8B1.14390.12830.75160.072*
H8C1.17380.11880.62270.072*
C90.9107 (4)0.20743 (17)0.5839 (6)0.0700 (17)
H9A0.93290.23430.61990.105*
H9B0.86420.19640.62910.105*
H9C0.89140.21410.50510.105*
C101.0469 (3)0.18315 (17)0.5010 (5)0.0571 (14)
H10A1.02450.18930.42350.086*
H10B1.08470.15780.49770.086*
H10C1.07720.20910.52970.086*
C110.9814 (4)0.1307 (3)0.9123 (5)0.086 (2)
H11A1.03490.12630.95220.129*
H11B0.95710.10190.89250.129*
H11C0.94370.14680.96300.129*
C121.0358 (4)0.2006 (2)0.8221 (6)0.086 (2)
H12A0.99810.22080.86170.129*
H12B1.04990.21290.74660.129*
H12C1.08660.19680.86880.129*
C130.5659 (4)0.0960 (2)0.3871 (6)0.086 (2)
H13A0.51160.09960.42320.129*
H13B0.60130.07710.43580.129*
H13C0.55840.08230.31090.129*
C140.5508 (5)0.1719 (2)0.3134 (7)0.118 (3)
H14A0.55230.16670.22990.177*
H14B0.57110.20180.33020.177*
H14C0.49360.16900.34010.177*
C150.7525 (5)0.22617 (18)0.3010 (5)0.091 (2)
H15A0.70480.24290.27100.137*
H15B0.77220.20590.24120.137*
H15C0.79730.24660.32280.137*
C160.6976 (3)0.22754 (14)0.5052 (4)0.0491 (13)
H16A0.73690.25170.52010.074*
H16B0.69400.20880.57400.074*
H16C0.64270.23980.48660.074*
C170.8509 (5)0.1213 (2)0.3117 (6)0.087 (2)
H17A0.86890.09090.29830.131*
H17B0.86780.13050.38980.131*
H17C0.87670.14090.25500.131*
C180.7224 (7)0.1064 (3)0.1906 (6)0.132 (4)
H18A0.74840.12050.12400.197*
H18B0.66280.11290.18940.197*
H18C0.73080.07440.18690.197*
C190.4800 (3)0.02788 (17)0.6395 (5)0.0615 (16)
H19A0.46350.00380.69080.092*
H19B0.53890.02480.62110.092*
H19C0.44660.02670.56810.092*
C200.3765 (3)0.0808 (2)0.7169 (6)0.078 (2)
H20A0.34650.08100.64260.116*
H20B0.37180.10990.75360.116*
H20C0.35260.05830.76720.116*
C210.4702 (4)0.0970 (3)0.9843 (5)0.083 (2)
H21A0.42920.07330.97510.124*
H21B0.44550.12510.95950.124*
H21C0.48760.09911.06570.124*
C220.5925 (3)0.04816 (19)0.9571 (5)0.0579 (14)
H22A0.60440.05231.03970.087*
H22B0.64480.04560.91550.087*
H22C0.55980.02120.94580.087*
C230.4854 (4)0.1689 (2)0.6514 (6)0.084 (2)
H23A0.44460.19190.66890.126*
H23B0.45900.14590.60390.126*
H23C0.53160.18200.60930.126*
C240.5484 (3)0.18326 (18)0.8443 (7)0.088 (2)
H24A0.58920.20220.80640.132*
H24B0.57460.16850.91080.132*
H24C0.50190.20140.87050.132*
Ag10.28258 (2)0.234941 (11)0.28632 (3)0.03952 (10)
Mo10.28386 (2)0.272038 (10)0.52560 (3)0.02233 (9)
S10.28577 (7)0.31537 (3)0.36778 (9)0.0317 (2)
S20.28360 (7)0.19915 (3)0.48461 (9)0.0352 (2)
S30.39752 (7)0.21324 (4)0.13208 (9)0.0378 (3)
S40.16939 (7)0.21227 (4)0.12641 (9)0.0364 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Y10.01862 (18)0.01585 (18)0.0287 (2)0.00010 (14)0.00161 (15)0.00090 (14)
P10.0377 (6)0.0205 (5)0.0326 (6)0.0066 (5)0.0093 (5)0.0066 (4)
P20.0209 (5)0.0341 (6)0.0288 (5)0.0052 (4)0.0006 (4)0.0057 (4)
P30.0625 (8)0.0261 (6)0.0340 (6)0.0101 (6)0.0188 (6)0.0007 (5)
P40.0199 (5)0.0265 (5)0.0406 (6)0.0010 (4)0.0037 (4)0.0072 (5)
O10.0334 (15)0.0177 (13)0.0347 (15)0.0030 (11)0.0023 (12)0.0047 (11)
O20.0202 (13)0.0299 (14)0.0341 (15)0.0032 (11)0.0017 (11)0.0005 (12)
O30.0327 (15)0.0236 (14)0.0343 (16)0.0016 (12)0.0055 (12)0.0072 (12)
O40.0202 (13)0.0273 (14)0.0461 (17)0.0004 (11)0.0070 (12)0.0061 (12)
O50.0262 (15)0.0275 (14)0.0442 (17)0.0004 (12)0.0006 (13)0.0062 (13)
O60.0261 (14)0.0297 (15)0.0389 (16)0.0016 (12)0.0001 (12)0.0057 (13)
O70.055 (2)0.057 (2)0.0414 (19)0.0048 (17)0.0023 (16)0.0232 (17)
O80.0421 (17)0.0208 (14)0.0358 (16)0.0028 (12)0.0050 (13)0.0014 (12)
O90.0387 (16)0.0217 (14)0.0379 (17)0.0019 (12)0.0008 (13)0.0035 (12)
O100.108 (3)0.0392 (19)0.051 (2)0.014 (2)0.012 (2)0.0215 (17)
N10.053 (2)0.0271 (18)0.0318 (19)0.0061 (17)0.0107 (17)0.0075 (15)
N20.046 (2)0.042 (2)0.065 (3)0.0185 (19)0.017 (2)0.021 (2)
N30.069 (3)0.0247 (18)0.044 (2)0.0089 (19)0.013 (2)0.0039 (17)
N40.0211 (16)0.042 (2)0.0333 (19)0.0021 (15)0.0008 (14)0.0064 (16)
N50.034 (2)0.035 (2)0.065 (3)0.0059 (17)0.0132 (19)0.0097 (19)
N60.037 (2)0.077 (3)0.039 (2)0.001 (2)0.0042 (18)0.025 (2)
N70.074 (3)0.049 (3)0.093 (4)0.016 (2)0.056 (3)0.001 (2)
N80.100 (3)0.0285 (19)0.029 (2)0.010 (2)0.004 (2)0.0087 (16)
N90.113 (4)0.051 (3)0.043 (3)0.029 (3)0.005 (3)0.010 (2)
N100.0196 (17)0.053 (2)0.054 (2)0.0008 (16)0.0040 (16)0.0263 (19)
N110.036 (2)0.064 (3)0.040 (2)0.0086 (19)0.0055 (17)0.0086 (19)
N120.037 (2)0.031 (2)0.076 (3)0.0032 (17)0.010 (2)0.008 (2)
N130.035 (2)0.0238 (17)0.036 (2)0.0065 (15)0.0016 (16)0.0043 (15)
N140.038 (2)0.030 (2)0.039 (2)0.0040 (16)0.0026 (17)0.0066 (17)
C10.074 (4)0.050 (3)0.034 (3)0.005 (3)0.005 (2)0.001 (2)
C20.068 (3)0.042 (3)0.048 (3)0.010 (2)0.021 (3)0.019 (2)
C30.036 (3)0.066 (4)0.089 (4)0.004 (3)0.011 (3)0.017 (3)
C40.088 (4)0.060 (4)0.082 (4)0.041 (3)0.035 (4)0.029 (3)
C50.105 (5)0.058 (4)0.070 (4)0.026 (3)0.013 (4)0.024 (3)
C60.059 (4)0.091 (5)0.102 (5)0.023 (3)0.008 (4)0.023 (4)
C70.032 (2)0.049 (3)0.044 (3)0.001 (2)0.003 (2)0.012 (2)
C80.024 (2)0.071 (3)0.049 (3)0.002 (2)0.001 (2)0.009 (3)
C90.063 (4)0.042 (3)0.106 (5)0.007 (3)0.020 (3)0.019 (3)
C100.055 (3)0.050 (3)0.067 (4)0.013 (3)0.019 (3)0.010 (3)
C110.052 (3)0.172 (7)0.032 (3)0.019 (4)0.006 (3)0.003 (4)
C120.060 (4)0.094 (5)0.104 (5)0.014 (3)0.013 (4)0.064 (4)
C130.059 (4)0.073 (4)0.125 (6)0.006 (3)0.046 (4)0.017 (4)
C140.127 (6)0.088 (5)0.136 (7)0.049 (5)0.085 (6)0.008 (5)
C150.181 (8)0.048 (3)0.046 (3)0.030 (4)0.028 (4)0.024 (3)
C160.080 (4)0.028 (2)0.039 (3)0.004 (2)0.005 (3)0.003 (2)
C170.113 (6)0.085 (5)0.065 (4)0.032 (4)0.044 (4)0.006 (4)
C180.233 (11)0.119 (7)0.043 (4)0.021 (7)0.003 (5)0.036 (4)
C190.035 (3)0.054 (3)0.095 (4)0.006 (2)0.006 (3)0.039 (3)
C200.024 (2)0.112 (5)0.097 (5)0.004 (3)0.004 (3)0.063 (4)
C210.058 (4)0.140 (6)0.051 (4)0.030 (4)0.016 (3)0.012 (4)
C220.048 (3)0.077 (4)0.049 (3)0.000 (3)0.004 (2)0.012 (3)
C230.097 (5)0.066 (4)0.089 (5)0.043 (4)0.030 (4)0.025 (4)
C240.049 (3)0.047 (3)0.168 (7)0.006 (3)0.019 (4)0.049 (4)
Ag10.0601 (2)0.03759 (19)0.02085 (17)0.00057 (16)0.00066 (15)0.00184 (13)
Mo10.02685 (18)0.02148 (17)0.01861 (17)0.00241 (13)0.00162 (13)0.00100 (13)
S10.0454 (6)0.0238 (5)0.0258 (5)0.0003 (5)0.0007 (4)0.0051 (4)
S20.0559 (7)0.0213 (5)0.0283 (5)0.0043 (5)0.0002 (5)0.0018 (4)
S30.0325 (6)0.0505 (7)0.0301 (6)0.0137 (5)0.0057 (5)0.0035 (5)
S40.0312 (5)0.0484 (6)0.0297 (6)0.0064 (5)0.0017 (4)0.0029 (5)
Geometric parameters (Å, º) top
Y1—O32.233 (3)C6—H6A0.9600
Y1—O22.242 (2)C6—H6B0.9600
Y1—O42.245 (3)C6—H6C0.9600
Y1—O12.263 (2)C7—H7A0.9600
Y1—O82.442 (3)C7—H7B0.9600
Y1—O92.465 (3)C7—H7C0.9600
Y1—O52.471 (3)C8—H8A0.9600
Y1—O62.472 (3)C8—H8B0.9600
Y1—N142.871 (3)C8—H8C0.9600
Y1—N132.888 (3)C9—H9A0.9600
P1—O11.482 (3)C9—H9B0.9600
P1—N21.628 (4)C9—H9C0.9600
P1—N11.642 (4)C10—H10A0.9600
P1—N31.656 (4)C10—H10B0.9600
P2—O21.492 (3)C10—H10C0.9600
P2—N61.620 (4)C11—H11A0.9600
P2—N51.638 (4)C11—H11B0.9600
P2—N41.639 (3)C11—H11C0.9600
P3—O31.479 (3)C12—H12A0.9600
P3—N91.609 (5)C12—H12B0.9600
P3—N81.616 (4)C12—H12C0.9600
P3—N71.652 (5)C13—H13A0.9600
P4—O41.498 (3)C13—H13B0.9600
P4—N121.619 (4)C13—H13C0.9600
P4—N101.622 (3)C14—H14A0.9600
P4—N111.644 (4)C14—H14B0.9600
O5—N131.271 (4)C14—H14C0.9600
O6—N131.270 (4)C15—H15A0.9600
O7—N131.219 (4)C15—H15B0.9600
O8—N141.272 (4)C15—H15C0.9600
O9—N141.268 (4)C16—H16A0.9600
O10—N141.227 (4)C16—H16B0.9600
N1—C11.444 (6)C16—H16C0.9600
N1—C21.475 (5)C17—H17A0.9600
N2—C31.456 (6)C17—H17B0.9600
N2—C41.475 (6)C17—H17C0.9600
N3—C51.439 (7)C18—H18A0.9600
N3—C61.456 (7)C18—H18B0.9600
N4—C71.461 (5)C18—H18C0.9600
N4—C81.465 (5)C19—H19A0.9600
N5—C101.456 (6)C19—H19B0.9600
N5—C91.472 (6)C19—H19C0.9600
N6—C111.447 (7)C20—H20A0.9600
N6—C121.476 (7)C20—H20B0.9600
N7—C131.422 (7)C20—H20C0.9600
N7—C141.461 (7)C21—H21A0.9600
N8—C151.466 (6)C21—H21B0.9600
N8—C161.480 (6)C21—H21C0.9600
N9—C171.427 (8)C22—H22A0.9600
N9—C181.466 (7)C22—H22B0.9600
N10—C191.440 (5)C22—H22C0.9600
N10—C201.474 (6)C23—H23A0.9600
N11—C221.469 (6)C23—H23B0.9600
N11—C211.470 (6)C23—H23C0.9600
N12—C231.446 (7)C24—H24A0.9600
N12—C241.468 (7)C24—H24B0.9600
C1—H1A0.9600C24—H24C0.9600
C1—H1B0.9600Ag1—S22.4861 (11)
C1—H1C0.9600Ag1—S12.5576 (11)
C2—H2A0.9600Ag1—S42.6129 (13)
C2—H2B0.9600Ag1—S32.6193 (13)
C2—H2C0.9600Ag1—Mo12.9274 (6)
C3—H3A0.9600Ag1—Mo1i2.9640 (7)
C3—H3B0.9600Mo1—S3ii2.1899 (12)
C3—H3C0.9600Mo1—S4ii2.2023 (13)
C4—H4A0.9600Mo1—S12.2036 (10)
C4—H4B0.9600Mo1—S22.2106 (11)
C4—H4C0.9600Mo1—Ag1ii2.9640 (7)
C5—H5A0.9600S3—Mo1i2.1899 (12)
C5—H5B0.9600S4—Mo1i2.2023 (12)
C5—H5C0.9600
O3—Y1—O292.78 (10)N3—C5—H5C109.5
O3—Y1—O488.84 (10)H5A—C5—H5C109.5
O2—Y1—O4157.00 (10)H5B—C5—H5C109.5
O3—Y1—O1157.93 (10)N3—C6—H6A109.5
O2—Y1—O193.57 (9)N3—C6—H6B109.5
O4—Y1—O193.46 (10)H6A—C6—H6B109.5
O3—Y1—O8128.62 (9)N3—C6—H6C109.5
O2—Y1—O879.89 (10)H6A—C6—H6C109.5
O4—Y1—O881.21 (10)H6B—C6—H6C109.5
O1—Y1—O873.36 (9)N4—C7—H7A109.5
O3—Y1—O976.50 (9)N4—C7—H7B109.5
O2—Y1—O977.69 (9)H7A—C7—H7B109.5
O4—Y1—O980.40 (9)N4—C7—H7C109.5
O1—Y1—O9125.54 (9)H7A—C7—H7C109.5
O8—Y1—O952.18 (9)H7B—C7—H7C109.5
O3—Y1—O578.98 (9)N4—C8—H8A109.5
O2—Y1—O5127.25 (9)N4—C8—H8B109.5
O4—Y1—O575.56 (9)H8A—C8—H8B109.5
O1—Y1—O580.35 (9)N4—C8—H8C109.5
O8—Y1—O5143.55 (9)H8A—C8—H8C109.5
O9—Y1—O5145.77 (9)H8B—C8—H8C109.5
O3—Y1—O679.78 (10)N5—C9—H9A109.5
O2—Y1—O675.51 (9)N5—C9—H9B109.5
O4—Y1—O6127.24 (9)H9A—C9—H9B109.5
O1—Y1—O681.39 (9)N5—C9—H9C109.5
O8—Y1—O6143.31 (9)H9A—C9—H9C109.5
O9—Y1—O6142.99 (9)H9B—C9—H9C109.5
O5—Y1—O651.74 (9)N5—C10—H10A109.5
O3—Y1—N14102.59 (10)N5—C10—H10B109.5
O2—Y1—N1476.41 (10)H10A—C10—H10B109.5
O4—Y1—N1480.85 (10)N5—C10—H10C109.5
O1—Y1—N1499.45 (10)H10A—C10—H10C109.5
O8—Y1—N1426.13 (9)H10B—C10—H10C109.5
O9—Y1—N1426.09 (9)N6—C11—H11A109.5
O5—Y1—N14156.34 (10)N6—C11—H11B109.5
O6—Y1—N14151.90 (9)H11A—C11—H11B109.5
O3—Y1—N1375.90 (10)N6—C11—H11C109.5
O2—Y1—N13101.34 (10)H11A—C11—H11C109.5
O4—Y1—N13101.30 (10)H11B—C11—H11C109.5
O1—Y1—N1382.13 (9)N6—C12—H12A109.5
O8—Y1—N13155.48 (9)N6—C12—H12B109.5
O9—Y1—N13152.30 (9)H12A—C12—H12B109.5
O5—Y1—N1325.97 (9)N6—C12—H12C109.5
O6—Y1—N1325.95 (9)H12A—C12—H12C109.5
N14—Y1—N13177.29 (10)H12B—C12—H12C109.5
O1—P1—N2109.25 (18)N7—C13—H13A109.5
O1—P1—N1108.25 (16)N7—C13—H13B109.5
N2—P1—N1115.7 (2)H13A—C13—H13B109.5
O1—P1—N3116.87 (18)N7—C13—H13C109.5
N2—P1—N3103.3 (2)H13A—C13—H13C109.5
N1—P1—N3103.61 (19)H13B—C13—H13C109.5
O2—P2—N6110.91 (19)N7—C14—H14A109.5
O2—P2—N5111.61 (17)N7—C14—H14B109.5
N6—P2—N5106.7 (2)H14A—C14—H14B109.5
O2—P2—N4108.68 (16)N7—C14—H14C109.5
N6—P2—N4109.63 (19)H14A—C14—H14C109.5
N5—P2—N4109.31 (19)H14B—C14—H14C109.5
O3—P3—N9111.4 (2)N8—C15—H15A109.5
O3—P3—N8109.84 (18)N8—C15—H15B109.5
N9—P3—N8108.1 (2)H15A—C15—H15B109.5
O3—P3—N7108.8 (2)N8—C15—H15C109.5
N9—P3—N7109.0 (3)H15A—C15—H15C109.5
N8—P3—N7109.6 (2)H15B—C15—H15C109.5
O4—P4—N12119.37 (18)N8—C16—H16A109.5
O4—P4—N10107.70 (16)N8—C16—H16B109.5
N12—P4—N10104.7 (2)H16A—C16—H16B109.5
O4—P4—N11107.76 (18)N8—C16—H16C109.5
N12—P4—N11103.0 (2)H16A—C16—H16C109.5
N10—P4—N11114.7 (2)H16B—C16—H16C109.5
P1—O1—Y1161.37 (17)N9—C17—H17A109.5
P2—O2—Y1168.21 (17)N9—C17—H17B109.5
P3—O3—Y1167.49 (17)H17A—C17—H17B109.5
P4—O4—Y1158.56 (16)N9—C17—H17C109.5
N13—O5—Y195.7 (2)H17A—C17—H17C109.5
N13—O6—Y195.6 (2)H17B—C17—H17C109.5
N14—O8—Y196.1 (2)N9—C18—H18A109.5
N14—O9—Y195.1 (2)N9—C18—H18B109.5
C1—N1—C2113.2 (4)H18A—C18—H18B109.5
C1—N1—P1120.4 (3)N9—C18—H18C109.5
C2—N1—P1120.7 (3)H18A—C18—H18C109.5
C3—N2—C4115.1 (4)H18B—C18—H18C109.5
C3—N2—P1119.9 (3)N10—C19—H19A109.5
C4—N2—P1120.6 (3)N10—C19—H19B109.5
C5—N3—C6110.9 (5)H19A—C19—H19B109.5
C5—N3—P1123.4 (4)N10—C19—H19C109.5
C6—N3—P1121.1 (4)H19A—C19—H19C109.5
C7—N4—C8114.6 (3)H19B—C19—H19C109.5
C7—N4—P2119.8 (3)N10—C20—H20A109.5
C8—N4—P2122.3 (3)N10—C20—H20B109.5
C10—N5—C9114.8 (4)H20A—C20—H20B109.5
C10—N5—P2125.4 (3)N10—C20—H20C109.5
C9—N5—P2118.8 (3)H20A—C20—H20C109.5
C11—N6—C12115.4 (5)H20B—C20—H20C109.5
C11—N6—P2119.3 (4)N11—C21—H21A109.5
C12—N6—P2124.3 (4)N11—C21—H21B109.5
C13—N7—C14113.5 (5)H21A—C21—H21B109.5
C13—N7—P3121.7 (4)N11—C21—H21C109.5
C14—N7—P3123.7 (5)H21A—C21—H21C109.5
C15—N8—C16115.1 (4)H21B—C21—H21C109.5
C15—N8—P3124.1 (4)N11—C22—H22A109.5
C16—N8—P3118.7 (3)N11—C22—H22B109.5
C17—N9—C18117.3 (6)H22A—C22—H22B109.5
C17—N9—P3119.7 (4)N11—C22—H22C109.5
C18—N9—P3123.0 (6)H22A—C22—H22C109.5
C19—N10—C20113.6 (4)H22B—C22—H22C109.5
C19—N10—P4122.1 (3)N12—C23—H23A109.5
C20—N10—P4121.9 (3)N12—C23—H23B109.5
C22—N11—C21111.9 (4)H23A—C23—H23B109.5
C22—N11—P4118.7 (3)N12—C23—H23C109.5
C21—N11—P4120.8 (3)H23A—C23—H23C109.5
C23—N12—C24112.6 (5)H23B—C23—H23C109.5
C23—N12—P4121.5 (4)N12—C24—H24A109.5
C24—N12—P4123.2 (4)N12—C24—H24B109.5
O7—N13—O6121.5 (3)H24A—C24—H24B109.5
O7—N13—O5122.3 (3)N12—C24—H24C109.5
O6—N13—O5116.1 (3)H24A—C24—H24C109.5
O7—N13—Y1172.4 (3)H24B—C24—H24C109.5
O6—N13—Y158.41 (18)S2—Ag1—S194.11 (3)
O5—N13—Y158.34 (17)S2—Ag1—S4120.83 (4)
O10—N14—O9122.2 (3)S1—Ag1—S4119.99 (4)
O10—N14—O8121.3 (4)S2—Ag1—S3120.28 (4)
O9—N14—O8116.4 (3)S1—Ag1—S3117.40 (4)
O10—N14—Y1175.3 (3)S4—Ag1—S386.92 (4)
O9—N14—Y158.80 (18)S2—Ag1—Mo147.34 (3)
O8—N14—Y157.76 (18)S1—Ag1—Mo146.78 (2)
N1—C1—H1A109.5S4—Ag1—Mo1137.27 (3)
N1—C1—H1B109.5S3—Ag1—Mo1135.75 (3)
H1A—C1—H1B109.5S2—Ag1—Mo1i150.72 (3)
N1—C1—H1C109.5S1—Ag1—Mo1i115.14 (3)
H1A—C1—H1C109.5S4—Ag1—Mo1i45.99 (3)
H1B—C1—H1C109.5S3—Ag1—Mo1i45.67 (3)
N1—C2—H2A109.5Mo1—Ag1—Mo1i161.916 (13)
N1—C2—H2B109.5S3ii—Mo1—S4ii110.05 (5)
H2A—C2—H2B109.5S3ii—Mo1—S1108.06 (5)
N1—C2—H2C109.5S4ii—Mo1—S1108.67 (5)
H2A—C2—H2C109.5S3ii—Mo1—S2108.03 (5)
H2B—C2—H2C109.5S4ii—Mo1—S2108.48 (4)
N2—C3—H3A109.5S1—Mo1—S2113.54 (4)
N2—C3—H3B109.5S3ii—Mo1—Ag1125.42 (4)
H3A—C3—H3B109.5S4ii—Mo1—Ag1124.52 (4)
N2—C3—H3C109.5S1—Mo1—Ag157.75 (3)
H3A—C3—H3C109.5S2—Mo1—Ag155.79 (3)
H3B—C3—H3C109.5S3ii—Mo1—Ag1ii58.82 (4)
N2—C4—H4A109.5S4ii—Mo1—Ag1ii58.57 (4)
N2—C4—H4B109.5S1—Mo1—Ag1ii148.33 (3)
H4A—C4—H4B109.5S2—Mo1—Ag1ii98.13 (3)
N2—C4—H4C109.5Ag1—Mo1—Ag1ii153.915 (13)
H4A—C4—H4C109.5Mo1—S1—Ag175.47 (3)
H4B—C4—H4C109.5Mo1—S2—Ag176.87 (3)
N3—C5—H5A109.5Mo1i—S3—Ag175.50 (4)
N3—C5—H5B109.5Mo1i—S4—Ag175.45 (4)
H5A—C5—H5B109.5
Symmetry codes: (i) x, y+1/2, z1/2; (ii) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C5—H5A···S2iii0.962.793.710 (6)160
C16—H16A···O10i0.962.493.292 (6)141
C18—H18A···O10iv0.962.543.470 (9)162
Symmetry codes: (i) x, y+1/2, z1/2; (iii) x+1, y, z+1; (iv) x, y, z1.

Experimental details

Crystal data
Chemical formula[Y(NO3)2(C6H18N3OP)4][AgMoS4]
Mr1261.84
Crystal system, space groupMonoclinic, P21/c
Temperature (K)153
a, b, c (Å)15.777 (3), 29.650 (6), 11.339 (2)
β (°) 90.90 (3)
V3)5303.6 (17)
Z4
Radiation typeMo Kα
µ (mm1)2.02
Crystal size (mm)0.35 × 0.20 × 0.15
Data collection
DiffractometerRigaku Saturn724+
diffractometer
Absorption correctionMulti-scan
(CrystalClear; Rigaku, 2007)
Tmin, Tmax0.622, 0.739
No. of measured, independent and
observed [I > 2σ(I)] reflections
25568, 10435, 8978
Rint0.033
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.045, 0.091, 1.02
No. of reflections10435
No. of parameters556
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.86, 0.79

Computer programs: CrystalClear (Rigaku, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C5—H5A···S2i0.962.793.710 (6)160
C16—H16A···O10ii0.962.493.292 (6)141
C18—H18A···O10iii0.962.543.470 (9)162
Symmetry codes: (i) x+1, y, z+1; (ii) x, y+1/2, z1/2; (iii) x, y, z1.
 

Acknowledgements

This work was supported by the Natural Science Foundation of Jiangsu High School (10KJB430005) and the Foundation of Jiangsu University (08JDG036).

References

First citationCao, Y., Zhang, J.-F., Qian, J. & Zhang, C. (2007). Acta Cryst. E63, m2076–m2077.  Web of Science CSD CrossRef IUCr Journals Google Scholar
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 (2007). 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 citationTang, G., Zhang, J. & Zhang, C. (2008). Acta Cryst. E64, m478.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationTang, G., Zhang, J., Zhang, C. & Lu, L. (2008). Acta Cryst. E64, m399–m400.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationZhang, J. (2010). Acta Cryst. E66, m1479.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationZhang, J.-F., Cao, Y., Qian, J. & Zhang, C. (2007). Acta Cryst. E63, m2248–m2249.  Web of Science CSD CrossRef IUCr Journals Google Scholar
First citationZhang, J., Qian, J., Cao, Y. & Zhang, C. (2007). Acta Cryst. E63, m2386–m2387.  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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Volume 67| Part 9| September 2011| Pages m1206-m1207
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