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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 64| Part 3| March 2008| Page m478
doi:10.1107/S1600536808001256

catena-Poly[[tetra­kis(hexa­methyl­phos­pho­ramide-κO)bis­­(nitrato-κ2O,O′)neodymium(III)] [silver(I)-di-μ2-sulfido-tungsten(VI)-di-μ2-sulfido]]

Guodong Tang,a,b Jinfang Zhanga and Chi Zhanga*

aSchool of Chemical Engineering, Nanjing University of Science and Technology, 200 Xiaolingwei, Nanjing 210094, Jiangsu, People's Republic of China, and bHuaiyin Teachers' College, Huaian 223001, Jiangsu, People's Republic of China
*Correspondence e-mail: chizhang@mail.njust.edu.cn

(Received 20 December 2007; accepted 12 January 2008; online 15 February 2008)

In the title compound, {[Nd(NO3)2(C6H18N3OP)4][AgWS4]}n, the central Nd atom of the monovalent cation is coordinated by eight O atoms from two nitrate and four hexa­methyl­phospho­ramide ligands. The monovalent anion, {[WS4Ag]−}n, forms a polymeric chain in a distorted linear configuration with W—Ag—W and Ag—W—Ag angles of 163.81 (3) and 154.786 (12)°, respectively. Thirteen C and three N atoms are disordered equally over two positions. One C atom is disordered over two positions with site occupancy factors of 0.6 and 0.4.

Related literature

For related structures, see: Lang et al. (1993[Lang, J. P., Li, J. G., Bao, S. A., Xin, X. Q. & Yu, K. B. (1993). Polyhedron, 12, 801-806.]); Huang et al. (1996[Huang, Q., Wu, X. T., Wang, Q. M., Sheng, T. L. & Lu, J. X. (1996). Angew. Chem. Int. Ed. Engl. 35, 868-870.], 1997[Huang, Q., Wu, X. T., Sheng, T. L., Wang, Q. M. & Lu, J. X. (1997). Polyhedron, 16, 217-222.]); Zhang, Qian et al. (2007[Zhang, J., Qian, J., Cao, Y. & Zhang, C. (2007). Acta Cryst. E63, m2386-m2387.]); Zhang, Cao et al. (2007[Zhang, J.-F., Cao, Y., Qian, J. & Zhang, C. (2007). Acta Cryst. E63, m2248-m2249.]). For a review of polymeric Mo(W)/S/Ag(Cu) clusters, 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 references therein). For third-order non-linear optical properties, see: Zhang, Song et al. (2007[Zhang, C., Song, Y. L. & Wang, X. (2007). Coord. Chem. Rev. 251, 111-141.]).

[Scheme 1]

Experimental

Crystal data

  • [Nd(NO3)2(C6H18N3OP)4][AgWS4]

  • Mr = 1405.07

  • Monoclinic, P 21 /c

  • a = 15.8250 (19) Å

  • b = 29.873 (4) Å

  • c = 11.4345 (13) Å

  • β = 90.689 (3)°

  • V = 5405.2 (12) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 3.76 mm−1

  • T = 153 (2) K

  • 0.2 × 0.15 × 0.1 mm
Data collection

  • Rigaku Mercury diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.132, Tmax = 0.329 (expected range = 0.275–0.687)

  • 46733 measured reflections

  • 9877 independent reflections

  • 9086 reflections with I > 2σ(I)

  • Rint = 0.045
Refinement

  • R[F2 > 2σ(F2)] = 0.050

  • wR(F2) = 0.108

  • S = 1.14

  • 9877 reflections

  • 506 parameters

  • 28 restraints

  • H-atom parameters constrained

  • Δρmax = 1.42 e Å−3

  • Δρmin = −1.36 e Å−3

Data collection: CrystalClear (Rigaku Corporation, 2000[Rigaku Corporation (2000). CrystalClear. Version 1.3. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC, 2002[Rigaku/MSC (2002). CrystalStructure. Version 3.00. Rigaku/MSC, The Woodlands, Texas, USA.]); 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: SHELXL97; software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808001256/pv2063sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808001256/pv2063Isup2.hkl

checkCIF report


Comment top

One-dimensional Mo(W)/S/Ag anionic polymers have attracted much attention for their configurational isomerism (Niu et al., 2004, and references therein) and potential applications, especially in 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, and references therein). The title compound, {[Nd(hmp)4(NO3)2][WS4Ag]}n (hmp = hexamethylphosphoramide) with a wave-like anionic chain was prepared by following such route using Nd(III)-hmp complex as counterion.

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, unlike other solvent-coordinated rare-earth cations, in the literature (Niu et al., 2004, and references therein), which are trivalent and induce trivalent repeat units. For example, [Nd(dmf)8]3+ induces an anionic chain with a trivalent repeat unit [W4S16Ag5]3- (Huang et al., 1996).

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 163.81 (3) and 154.786 (12) °, respectively, unlike those in {(γ-MePyH)[WS4Ag]}n (Lang et al. 1993) and {[NH3C(CH2OH)3][WS4Ag](2DMF)}n (Huang et al., 1997), showing an ideal linear chain and a nearly linear chain, respectively. This observation suggests that cations with bigger bulk lead to more distorted anionic chains.

Similar angles for W—Ag—W and Ag—W—Ag are found in two distorted linear chains in {[Eu(hmp)4(NO3)2][WS4Ag]}n (Zhang, Qian et al., 2007) and {[Y(hmp)4(NO3)2][WS4Ag]}n (Zhang, Cao et al., 2007), implying that different rare earth cations with the same coordination environments will result in the same anionic structures.

Related literature top

For related structures, see: Lang et al. (1993); Huang et al. (1996, 1997); Zhang, Qian et al. (2007); Zhang, Cao et al. (2007). For a review of polymeric Mo(W)/S/Ag(Cu) clusters, see: Niu et al. (2004, and references therein). For third-order nonlinear optical properties, see: Zhang, Song et al. (2007).

Experimental top

Ag2S (0.25 g, 1 mmol) was added to a solution of (NH4)2WS4 (0.70 g, 2 mmol in 30 ml h mp) with thorough stirring for 10 h. The solution underwent an additional stir for one minute after Nd(NO3)36H2O (0.44 g, 1 mmol) was added. After filtration the orange-red filtrate was carefully laid on the surface with 30 ml i-PrOH. Orange-red block crystals were obtained after ten days. Yield: 1.129 g in pure form, 40.2% (based on W).

Refinement top

H atoms were positioned geometrically and allowed in the refinements in a riding mode, with C—H bonds = 0.98 Å and Uiso = 1.5 times the Ueq of the parent C-atoms. Parts of dimethylamine groups from hmp ligands have large librations, resulting in some disordered C and N atoms. The occupancy factors for C19 and C19' were allowed to be 0.6 and 0.4, respectvely, and for the rest of the disordered atoms 0.5 and 0.5. The disordered non-hydrogen atoms (C1,C3,C5,C9,C10,C11, C12,C17,C19,C20,C21,C22,C23,C24,N10,N11,N12,) were allowed isotropic displacement parameters.

Computing details top

Data collection: CrystalClear (Rigaku Corporation, 2000); cell refinement: CrystalClear (Rigaku Corporation, 2000); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXL97 (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (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. A portion of the anionic chain in the title compound, with atom labels and 30% probability displacement ellipsoids. (symmetry codes: i x, -y + 1/2, z - 1/2; ii x, y, z - 1; iii x, -y + 1/2, z - 1.5)
catena-Poly[[tetrakis(hexamethylphosphoramide-κO)bis(nitrato- κ2O,O')neodymium(III)] [silver(I)-di-µ2-sulfido-tungsten(VI)-di-µ2-sulfido]] top
Crystal data top
[Nd(NO3)2(C6H18N3OP)4][AgWS4]F(000) = 2796.0
Mr = 1405.07Dx = 1.727 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ybcCell parameters from 19261 reflections
a = 15.8250 (19) Åθ = 3.0–25.4°
b = 29.873 (4) ŵ = 3.76 mm−1
c = 11.4345 (13) ÅT = 153 K
β = 90.689 (3)°Block, orange–red
V = 5405.2 (12) Å30.2 × 0.15 × 0.1 mm
Z = 4
Data collection top
Rigaku Mercury
diffractometer		9877 independent reflections
Radiation source: fine-focus sealed tube9086 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.045
Detector resolution: 14.6306 pixels mm-1θmax = 25.4°, θmin = 3.0°
ω scansh = −17→19
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		k = −35→35
Tmin = 0.132, Tmax = 0.329l = −13→13
46733 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.050H-atom parameters constrained
wR(F2) = 0.108 w = 1/[σ2(Fo2) + (0.0328P)2 + 29.5132P]
where P = (Fo2 + 2Fc2)/3
S = 1.14(Δ/σ)max = 0.002
9877 reflectionsΔρmax = 1.42 e Å−3
506 parametersΔρmin = −1.37 e Å−3
28 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00025 (5)
Crystal data top
[Nd(NO3)2(C6H18N3OP)4][AgWS4]V = 5405.2 (12) Å3
Mr = 1405.07Z = 4
Monoclinic, P21/cMo Kα radiation
a = 15.8250 (19) ŵ = 3.76 mm−1
b = 29.873 (4) ÅT = 153 K
c = 11.4345 (13) Å0.2 × 0.15 × 0.1 mm
β = 90.689 (3)°
Data collection top
Rigaku Mercury
diffractometer		9877 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		9086 reflections with I > 2σ(I)
Tmin = 0.132, Tmax = 0.329Rint = 0.045
46733 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.05028 restraints
wR(F2) = 0.108H-atom parameters constrained
S = 1.14 w = 1/[σ2(Fo2) + (0.0328P)2 + 29.5132P]
where P = (Fo2 + 2Fc2)/3
9877 reflectionsΔρmax = 1.42 e Å−3
506 parametersΔρmin = −1.37 e Å−3
Special details top

Experimental. Analysis: calculated for C24H72AgN14NdO10P4S4W: C 20.52, H 5.16, N 13.96%; found: C 20.50, H 5.14, N 14.01%. IR: ν, cm-1, 478.5 m, 446.8 s (W-µ2-S).

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*/UeqOcc. (<1)
W10.713803 (18)0.271347 (9)−0.02311 (2)0.03257 (10)
Ag10.71456 (5)0.23648 (2)0.21805 (5)0.05526 (19)
S10.71465 (15)0.19967 (7)0.02245 (17)0.0526 (5)
S40.59999 (13)0.28497 (8)−0.12827 (18)0.0544 (5)
S30.82772 (13)0.28620 (9)−0.12453 (18)0.0562 (6)
S20.71231 (14)0.31554 (6)0.13071 (16)0.0470 (5)
Nd10.23703 (2)0.083214 (11)0.83521 (3)0.03310 (11)
P10.19278 (16)−0.02955 (7)0.69224 (19)0.0531 (6)
P20.46340 (12)0.09454 (7)0.7383 (2)0.0509 (5)
P30.01781 (11)0.13540 (7)0.82852 (17)0.0392 (4)
P40.29591 (17)0.14957 (8)1.1063 (2)0.0604 (6)
O10.2074 (3)0.01663 (16)0.7322 (5)0.0508 (13)
O40.2729 (3)0.12885 (17)0.9929 (5)0.0504 (13)
O20.3799 (3)0.08064 (17)0.7868 (5)0.0521 (14)
O30.0979 (3)0.10903 (16)0.8307 (5)0.0430 (12)
O50.1659 (3)0.04041 (18)1.0014 (5)0.0517 (14)
O60.2985 (3)0.02619 (19)0.9801 (6)0.0581 (15)
O70.2315 (5)0.0018 (2)1.1332 (7)0.087 (2)
O80.2510 (4)0.15975 (17)0.7396 (5)0.0538 (14)
O90.2232 (4)0.10556 (19)0.6219 (5)0.0566 (14)
O100.2227 (6)0.1734 (3)0.5559 (7)0.108 (3)
N10.2137 (6)−0.0343 (3)0.5527 (6)0.074 (2)
N20.2566 (7)−0.0668 (3)0.7514 (9)0.090 (3)
N30.1001 (6)−0.0461 (3)0.7286 (9)0.101 (4)
N40.5361 (4)0.0702 (3)0.8074 (9)0.102 (4)
N50.4625 (5)0.0856 (4)0.5961 (8)0.090 (3)
N60.4873 (5)0.1474 (3)0.7370 (8)0.083 (3)
N7−0.0604 (4)0.1016 (2)0.8554 (6)0.0487 (16)
N80.0200 (4)0.1751 (2)0.9266 (7)0.0588 (18)
N90.0021 (4)0.1589 (3)0.7038 (6)0.0602 (19)
N130.2327 (5)0.0221 (2)1.0398 (7)0.0567 (19)
N140.2324 (5)0.1468 (3)0.6370 (7)0.0596 (19)
C20.2211 (10)−0.0793 (4)0.4976 (12)0.126 (6)
H2A0.1672−0.08730.46020.189*
H2B0.2355−0.10150.55770.189*
H2C0.2655−0.07860.43870.189*
C40.2563 (13)−0.0823 (6)0.8638 (15)0.160 (7)
H4A0.3027−0.10370.87500.240*
H4B0.2024−0.09720.87900.240*
H4C0.2637−0.05720.91810.240*
C60.0334 (7)−0.0152 (4)0.7584 (12)0.099 (4)
H6A0.05400.01560.75070.149*
H6B0.0161−0.02050.83930.149*
H6C−0.0150−0.01980.70560.149*
C70.5338 (10)0.0962 (7)0.5243 (13)0.171 (9)
H7A0.57300.07080.52380.256*
H7B0.56280.12260.55600.256*
H7C0.51430.10240.44430.256*
C80.4124 (8)0.0485 (5)0.5485 (12)0.114 (5)
H8A0.41860.04740.46340.171*
H8B0.35280.05300.56760.171*
H8C0.43230.02030.58280.171*
C13−0.0526 (6)0.0683 (3)0.9472 (9)0.072 (3)
H13A−0.10480.05070.95080.109*
H13B−0.04260.08321.02240.109*
H13C−0.00500.04840.93030.109*
C14−0.1476 (5)0.1113 (4)0.8189 (9)0.070 (3)
H14A−0.18460.08680.84330.105*
H14B−0.15040.11450.73370.105*
H14C−0.16610.13930.85550.105*
C15−0.0477 (6)0.1853 (4)1.0071 (9)0.077 (3)
H15A−0.02370.19211.08440.116*
H15B−0.08550.15941.01290.116*
H15C−0.07970.21120.97820.116*
C160.0874 (7)0.2085 (3)0.9244 (11)0.084 (3)
H16A0.06490.23680.89410.125*
H16B0.13290.19800.87380.125*
H16C0.10970.21301.00390.125*
C180.0148 (7)0.1332 (5)0.5970 (9)0.097 (4)
H18A0.04290.10490.61630.146*
H18B0.05020.15040.54340.146*
H18C−0.04000.12710.55950.146*
N100.2744 (10)0.2005 (5)1.1022 (12)0.062 (3)*0.50
N10'0.3460 (9)0.1984 (5)1.0899 (12)0.062 (3)*0.50
N110.4021 (11)0.1396 (6)1.1244 (16)0.076 (3)*0.50
N11'0.3634 (11)0.1297 (6)1.1919 (15)0.076 (3)*0.50
N120.2128 (11)0.1727 (6)1.1823 (16)0.083 (4)*0.50
N12'0.2418 (11)0.1248 (6)1.2046 (16)0.083 (4)*0.50
C10.1813 (16)0.0006 (8)0.477 (2)0.085 (5)*0.50
H1A0.1972−0.00570.39620.128*0.50
H1B0.20510.02940.50140.128*0.50
H1C0.11960.00170.48250.128*0.50
C1'0.2149 (16)0.0014 (8)0.471 (2)0.085 (5)*0.50
H1'A0.2288−0.01020.39390.128*0.50
H1'B0.25750.02340.49590.128*0.50
H1'C0.15910.01570.46830.128*0.50
C30.3374 (16)−0.0770 (15)0.692 (3)0.152 (10)*0.50
H3A0.3352−0.06580.61200.227*0.50
H3B0.3463−0.10950.69150.227*0.50
H3C0.3842−0.06260.73500.227*0.50
C3'0.3492 (13)−0.0640 (15)0.743 (4)0.152 (10)*0.50
H3'10.3718−0.04650.80870.227*0.50
H3'20.3641−0.04940.66920.227*0.50
H3'30.3732−0.09420.74490.227*0.50
C50.0938 (15)−0.0971 (6)0.727 (2)0.085 (5)*0.50
H5A0.0536−0.10690.78680.128*0.50
H5B0.1495−0.11010.74460.128*0.50
H5C0.0742−0.10720.65010.128*0.50
C5'0.0559 (14)−0.0855 (7)0.690 (2)0.085 (5)*0.50
H5'A0.0069−0.07670.64200.128*0.50
H5'B0.0369−0.10250.75800.128*0.50
H5'C0.0939−0.10410.64330.128*0.50
C90.6243 (10)0.0721 (8)0.771 (2)0.081 (5)*0.50
H9A0.65480.04590.80090.121*0.50
H9B0.65070.09940.80110.121*0.50
H9C0.62660.07220.68490.121*0.50
C9'0.6235 (11)0.0906 (8)0.819 (2)0.081 (5)*0.50
H9'A0.65170.07860.88950.121*0.50
H9'B0.61850.12320.82640.121*0.50
H9'C0.65670.08320.75030.121*0.50
C100.5204 (14)0.0235 (5)0.8409 (18)0.067 (4)*0.50
H10D0.57110.00560.82700.101*0.50
H10E0.47320.01160.79410.101*0.50
H10F0.50620.02220.92400.101*0.50
C10'0.5260 (14)0.0337 (6)0.8911 (16)0.067 (4)*0.50
H10G0.58120.02590.92520.101*0.50
H10H0.50210.00750.85100.101*0.50
H10I0.48790.04320.95330.101*0.50
C110.4938 (17)0.1755 (8)0.8378 (19)0.097 (4)*0.50
H11A0.50790.20600.81350.145*0.50
H11B0.53820.16400.89030.145*0.50
H11C0.43970.17560.87870.145*0.50
C11'0.5275 (16)0.1607 (9)0.8511 (18)0.097 (4)*0.50
H11D0.54130.19270.84930.145*0.50
H11E0.57940.14340.86370.145*0.50
H11F0.48820.15490.91490.145*0.50
C120.4574 (17)0.1859 (7)0.677 (2)0.097 (4)*0.50
H12A0.48960.21210.70360.145*0.50
H12B0.39740.19030.69430.145*0.50
H12C0.46450.18190.59300.145*0.50
C12'0.4557 (17)0.1707 (8)0.6275 (18)0.097 (4)*0.50
H12D0.39780.18120.63940.145*0.50
H12E0.45660.14970.56170.145*0.50
H12F0.49240.19630.61050.145*0.50
C17−0.0382 (14)0.2048 (6)0.7073 (19)0.070 (4)*0.50
H17A−0.08090.22360.66840.105*0.50
H17B0.01760.21880.69950.105*0.50
H17C−0.05170.20190.79030.105*0.50
C17'−0.0328 (14)0.2003 (6)0.6628 (19)0.070 (4)*0.50
H17D−0.01370.20600.58290.105*0.50
H17E−0.01380.22470.71400.105*0.50
H17F−0.09460.19860.66340.105*0.50
C190.2618 (17)0.2274 (8)1.207 (2)0.122 (7)*0.60
H19A0.29560.25481.20190.184*0.60
H19B0.27960.21021.27600.184*0.60
H19C0.20190.23521.21320.184*0.60
C19'0.4180 (19)0.2067 (14)1.171 (3)0.122 (7)*0.40
H19D0.44550.23501.15110.184*0.40
H19E0.45880.18221.16540.184*0.40
H19F0.39720.20841.25170.184*0.40
C200.2952 (13)0.2279 (8)1.0033 (18)0.065 (4)*0.50
H20A0.28860.25951.02380.098*0.50
H20B0.25740.22050.93750.098*0.50
H20C0.35380.22220.98100.098*0.50
C20'0.3282 (13)0.2282 (7)0.9940 (18)0.065 (4)*0.50
H20D0.34970.25811.01260.098*0.50
H20E0.26700.22970.98040.098*0.50
H20F0.35570.21700.92340.098*0.50
C210.4426 (17)0.0973 (7)1.097 (2)0.093 (5)*0.50
H21A0.50310.09921.11590.139*0.50
H21B0.43500.09071.01370.139*0.50
H21C0.41700.07331.14340.139*0.50
C21'0.4250 (16)0.0987 (8)1.147 (2)0.093 (5)*0.50
H21D0.48140.11221.15180.139*0.50
H21E0.41130.09181.06500.139*0.50
H21F0.42410.07111.19300.139*0.50
C220.4572 (18)0.1700 (10)1.187 (3)0.129 (7)*0.50
H22A0.51440.15751.19020.193*0.50
H22B0.43630.17451.26600.193*0.50
H22C0.45840.19881.14560.193*0.50
C22'0.330 (2)0.1107 (10)1.303 (2)0.129 (7)*0.50
H22D0.37990.10961.35430.193*0.50
H22E0.27920.11481.34950.193*0.50
H22F0.33560.13581.24790.193*0.50
C24'0.259 (2)0.1105 (12)1.320 (2)0.139 (9)*0.50
H24C0.20540.10371.35900.208*0.50
H24E0.28850.13431.36290.208*0.50
H24F0.29410.08361.31840.208*0.50
C240.214 (2)0.2198 (9)1.222 (3)0.139 (9)*0.50
H24A0.26310.23511.19010.208*0.50
H24B0.21670.22071.30780.208*0.50
H24D0.16210.23491.19510.208*0.50
C23'0.1513 (14)0.1181 (11)1.192 (3)0.111 (6)*0.50
H23A0.12490.12011.26880.167*0.50
H23D0.14040.08851.15800.167*0.50
H23B0.12760.14121.14030.167*0.50
C230.1510 (17)0.1360 (9)1.203 (3)0.111 (6)*0.50
H23C0.16960.10881.16260.167*0.50
H23G0.09530.14491.17260.167*0.50
H23E0.14740.13001.28690.167*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.03803 (17)0.03657 (17)0.02301 (15)0.00284 (12)−0.00287 (11)−0.00256 (11)
Ag10.0819 (5)0.0585 (4)0.0254 (3)0.0011 (3)−0.0014 (3)0.0026 (3)
S10.0818 (15)0.0361 (10)0.0399 (10)0.0074 (10)−0.0006 (10)−0.0064 (8)
S40.0440 (11)0.0787 (15)0.0403 (11)0.0168 (10)−0.0075 (9)−0.0048 (10)
S30.0440 (11)0.0866 (17)0.0382 (11)−0.0086 (11)0.0012 (9)−0.0017 (10)
S20.0686 (13)0.0385 (10)0.0340 (10)−0.0017 (9)−0.0014 (9)−0.0090 (8)
Nd10.02623 (19)0.02392 (19)0.0491 (2)0.00031 (14)−0.00170 (16)0.00114 (16)
P10.0735 (15)0.0375 (11)0.0485 (12)−0.0155 (10)0.0076 (11)−0.0094 (9)
P20.0305 (10)0.0497 (12)0.0726 (15)−0.0009 (9)0.0057 (10)0.0010 (11)
P30.0286 (9)0.0433 (11)0.0455 (11)0.0068 (8)−0.0020 (8)0.0080 (9)
P40.0746 (16)0.0554 (14)0.0508 (13)−0.0077 (12)−0.0208 (12)0.0031 (11)
O10.050 (3)0.030 (3)0.073 (4)−0.002 (2)−0.004 (3)−0.008 (3)
O40.053 (3)0.040 (3)0.058 (3)−0.002 (2)−0.010 (3)−0.007 (3)
O20.028 (3)0.045 (3)0.083 (4)−0.002 (2)0.008 (3)0.010 (3)
O30.029 (2)0.041 (3)0.058 (3)0.007 (2)−0.003 (2)0.000 (2)
O50.039 (3)0.050 (3)0.066 (4)−0.003 (2)−0.008 (3)0.018 (3)
O60.040 (3)0.047 (3)0.087 (4)0.000 (3)−0.011 (3)0.015 (3)
O70.087 (5)0.086 (5)0.089 (5)−0.012 (4)−0.018 (4)0.047 (4)
O80.061 (4)0.035 (3)0.065 (4)−0.009 (3)−0.004 (3)0.006 (3)
O90.070 (4)0.047 (3)0.053 (3)−0.006 (3)0.005 (3)0.001 (3)
O100.169 (9)0.073 (5)0.079 (5)−0.023 (5)−0.023 (5)0.039 (4)
N10.108 (7)0.065 (5)0.048 (4)−0.025 (5)0.007 (4)−0.015 (4)
N20.128 (8)0.039 (4)0.102 (7)0.008 (5)0.031 (6)0.007 (5)
N30.099 (7)0.096 (7)0.110 (7)−0.063 (6)0.042 (6)−0.058 (6)
N40.033 (4)0.140 (9)0.133 (8)0.010 (5)0.007 (4)0.089 (7)
N50.062 (5)0.139 (9)0.070 (6)−0.022 (6)0.013 (4)0.007 (6)
N60.062 (5)0.073 (6)0.115 (8)−0.007 (4)0.014 (5)0.022 (5)
N70.027 (3)0.063 (4)0.056 (4)0.001 (3)−0.003 (3)0.011 (3)
N80.048 (4)0.056 (4)0.073 (5)0.007 (3)0.009 (4)−0.010 (4)
N90.052 (4)0.074 (5)0.054 (4)0.004 (4)−0.006 (3)0.020 (4)
N130.060 (5)0.044 (4)0.066 (5)−0.010 (3)−0.021 (4)0.014 (4)
N140.064 (5)0.051 (5)0.064 (5)−0.008 (4)0.003 (4)0.016 (4)
C20.167 (14)0.102 (10)0.112 (11)−0.047 (9)0.064 (10)−0.058 (8)
C40.22 (2)0.128 (14)0.132 (14)0.072 (14)−0.005 (14)0.029 (11)
C60.061 (7)0.112 (10)0.125 (11)−0.011 (7)−0.019 (7)0.019 (8)
C70.127 (13)0.29 (3)0.100 (12)−0.083 (15)0.032 (10)−0.004 (13)
C80.082 (8)0.151 (14)0.109 (10)−0.016 (9)0.004 (7)−0.039 (9)
C130.055 (5)0.077 (7)0.085 (7)−0.001 (5)−0.001 (5)0.031 (6)
C140.032 (4)0.100 (8)0.078 (7)−0.004 (5)−0.002 (4)0.006 (6)
C150.075 (7)0.080 (7)0.077 (7)0.015 (6)0.017 (5)−0.017 (6)
C160.074 (7)0.061 (6)0.116 (9)−0.002 (5)0.007 (6)−0.027 (6)
C180.076 (7)0.149 (12)0.065 (7)−0.005 (8)−0.016 (6)0.002 (7)
Geometric parameters (Å, º) top
W1—S42.192 (2)C16—H16C0.9800
W1—S22.1997 (18)C18—H18A0.9800
W1—S32.200 (2)C18—H18B0.9800
W1—S12.204 (2)C18—H18C0.9800
W1—Ag12.9477 (7)N10—C201.436 (16)
W1—Ag1i2.9690 (7)N10—C191.457 (17)
Ag1—S12.492 (2)N10'—C20'1.437 (16)
Ag1—S22.565 (2)N10'—C19'1.484 (18)
Ag1—S3ii2.613 (2)N11—C221.441 (17)
Ag1—S4ii2.620 (2)N11—C211.453 (17)
Ag1—W1ii2.9690 (7)N11'—C21'1.444 (17)
S4—Ag1i2.620 (2)N12—C241.481 (18)
S3—Ag1i2.613 (2)N12—C231.490 (18)
Nd1—O42.325 (5)N12'—C24'1.410 (18)
Nd1—O32.333 (4)N12'—C23'1.451 (18)
Nd1—O22.335 (5)C1—H1A0.9800
Nd1—O12.356 (5)C1—H1B0.9800
Nd1—O92.535 (6)C1—H1C0.9800
Nd1—O82.545 (5)C1'—H1'A0.9800
Nd1—O62.560 (5)C1'—H1'B0.9800
Nd1—O52.562 (5)C1'—H1'C0.9800
Nd1—N142.957 (7)C3—H3A0.9800
Nd1—N132.968 (7)C3—H3B0.9800
P1—O11.471 (5)C3—H3C0.9800
P1—N31.608 (9)C3'—H3'10.9800
P1—N11.639 (8)C3'—H3'20.9800
P1—N21.642 (10)C3'—H3'30.9800
P2—O21.498 (5)C5—H5A0.9800
P2—N41.568 (8)C5—H5B0.9800
P2—N61.623 (9)C5—H5C0.9800
P2—N51.647 (9)C5'—H5'A0.9800
P3—O31.492 (5)C5'—H5'B0.9800
P3—N91.607 (7)C5'—H5'C0.9800
P3—N71.630 (7)C9—H9A0.9800
P3—N81.632 (7)C9—H9B0.9800
P4—O41.479 (6)C9—H9C0.9800
P4—N11'1.557 (17)C9'—H9'A0.9800
P4—N101.561 (15)C9'—H9'B0.9800
P4—N12'1.602 (18)C9'—H9'C0.9800
P4—N10'1.673 (15)C10—H10D0.9800
P4—N111.716 (17)C10—H10E0.9800
P4—N121.729 (18)C10—H10F0.9800
O5—N131.263 (8)C10'—H10G0.9800
O6—N131.258 (9)C10'—H10H0.9800
O7—N131.230 (9)C10'—H10I0.9800
O8—N141.266 (9)C11—H11A0.9800
O9—N141.252 (9)C11—H11B0.9800
O10—N141.230 (9)C11—H11C0.9800
N1—C1'1.415 (16)C11'—H11D0.9800
N1—C11.444 (16)C11'—H11E0.9800
N1—C21.489 (13)C11'—H11F0.9800
N2—C41.367 (17)C12—H12A0.9800
N2—C3'1.472 (18)C12—H12B0.9800
N2—C31.485 (18)C12—H12C0.9800
N3—C5'1.435 (16)C12'—H12D0.9800
N3—C61.446 (14)C12'—H12E0.9800
N3—C51.528 (16)C12'—H12F0.9800
N4—C10'1.461 (15)C17—H17A0.9800
N4—C91.464 (15)C17—H17B0.9800
N4—C101.468 (15)C17—H17C0.9800
N4—C9'1.515 (15)C17'—H17D0.9800
N5—C71.438 (15)C17'—H17E0.9800
N5—C81.465 (15)C17'—H17F0.9800
N6—C121.416 (16)C19—H19A0.9800
N6—C111.428 (16)C19—H19B0.9800
N6—C11'1.498 (16)C19—H19C0.9800
N6—C12'1.512 (16)C19'—H19D0.9800
N7—C131.450 (11)C19'—H19E0.9800
N7—C141.466 (10)C19'—H19F0.9800
N8—C151.453 (11)C20—H20A0.9800
N8—C161.461 (12)C20—H20B0.9800
N9—C17'1.431 (15)C20—H20C0.9800
N9—C181.459 (13)C20'—H20D0.9800
C2—H2A0.9800C20'—H20E0.9800
C2—H2B0.9800C20'—H20F0.9800
C2—H2C0.9800C21—H21A0.9800
C4—H4A0.9800C21—H21B0.9800
C4—H4B0.9800C21—H21C0.9800
C4—H4C0.9800C21'—H21D0.9800
C6—H6A0.9800C21'—H21E0.9800
C6—H6B0.9800C21'—H21F0.9800
C6—H6C0.9800C22—H22A0.9800
C7—H7A0.9800C22—H22B0.9800
C7—H7B0.9800C22—H22C0.9800
C7—H7C0.9800C22'—H22D0.9800
C8—H8A0.9800C22'—H22E0.9800
C8—H8B0.9800C22'—H22F0.9800
C8—H8C0.9800C24'—H24C0.9800
C13—H13A0.9800C24'—H24E0.9800
C13—H13B0.9800C24'—H24F0.9800
C13—H13C0.9800C24—H24A0.9800
C14—H14A0.9800C24—H24B0.9800
C14—H14B0.9800C24—H24D0.9800
C14—H14C0.9800C23'—H23A0.9800
C15—H15A0.9800C23'—H23D0.9800
C15—H15B0.9800C23'—H23B0.9800
C15—H15C0.9800C23—H23C0.9800
C16—H16A0.9800C23—H23G0.9800
C16—H16B0.9800C23—H23E0.9800
S4—W1—S2108.09 (8)N7—C13—H13A109.5
S4—W1—S3110.27 (8)N7—C13—H13B109.5
S2—W1—S3108.49 (8)H13A—C13—H13B109.5
S4—W1—S1108.23 (9)N7—C13—H13C109.5
S2—W1—S1113.22 (7)H13A—C13—H13C109.5
S3—W1—S1108.53 (9)H13B—C13—H13C109.5
S4—W1—Ag1124.95 (6)N7—C14—H14A109.5
S2—W1—Ag157.59 (5)N7—C14—H14B109.5
S3—W1—Ag1124.76 (6)H14A—C14—H14B109.5
S1—W1—Ag155.63 (5)N7—C14—H14C109.5
S4—W1—Ag1i58.73 (6)H14A—C14—H14C109.5
S2—W1—Ag1i147.62 (6)H14B—C14—H14C109.5
S3—W1—Ag1i58.49 (6)N8—C15—H15A109.5
S1—W1—Ag1i99.16 (5)N8—C15—H15B109.5
Ag1—W1—Ag1i154.786 (12)H15A—C15—H15B109.5
S1—Ag1—S293.26 (7)N8—C15—H15C109.5
S1—Ag1—S3ii119.74 (8)H15A—C15—H15C109.5
S2—Ag1—S3ii120.87 (8)H15B—C15—H15C109.5
S1—Ag1—S4ii120.13 (8)N8—C16—H16A109.5
S2—Ag1—S4ii118.69 (8)N8—C16—H16B109.5
S3ii—Ag1—S4ii87.06 (7)H16A—C16—H16B109.5
S1—Ag1—W146.87 (5)N8—C16—H16C109.5
S2—Ag1—W146.40 (4)H16A—C16—H16C109.5
S3ii—Ag1—W1136.97 (5)H16B—C16—H16C109.5
S4ii—Ag1—W1135.97 (5)N9—C18—H18A109.5
S1—Ag1—W1ii149.31 (5)N9—C18—H18B109.5
S2—Ag1—W1ii117.42 (5)H18A—C18—H18B109.5
S3ii—Ag1—W1ii45.88 (5)N9—C18—H18C109.5
S4ii—Ag1—W1ii45.65 (4)H18A—C18—H18C109.5
W1—Ag1—W1ii163.81 (3)H18B—C18—H18C109.5
W1—S1—Ag177.50 (6)C20—N10—C19111.7 (18)
W1—S4—Ag1i75.63 (6)C20—N10—P4121.7 (14)
W1—S3—Ag1i75.63 (6)C19—N10—P4123.0 (15)
W1—S2—Ag176.02 (6)C20'—N10'—C19'121 (2)
O4—Nd1—O392.58 (18)C20'—N10'—P4122.4 (13)
O4—Nd1—O288.6 (2)C19'—N10'—P4115.9 (18)
O3—Nd1—O2157.18 (18)C22—N11—C21113 (2)
O4—Nd1—O1158.12 (19)C22—N11—P4122.4 (17)
O3—Nd1—O194.92 (18)C21—N11—P4123.9 (16)
O2—Nd1—O192.36 (19)C21'—N11'—P4118.7 (16)
O4—Nd1—O9127.51 (19)C24—N12—C23131 (2)
O3—Nd1—O979.69 (19)C24—N12—P4122.0 (18)
O2—Nd1—O981.6 (2)C23—N12—P4106.9 (17)
O1—Nd1—O974.15 (19)C24'—N12'—C23'103 (2)
O4—Nd1—O877.58 (19)C24'—N12'—P4134.4 (19)
O3—Nd1—O877.30 (18)C23'—N12'—P4121.9 (19)
O2—Nd1—O880.71 (18)N1—C1—H1A109.5
O1—Nd1—O8124.14 (19)N1—C1—H1B109.5
O9—Nd1—O849.99 (18)H1A—C1—H1B109.5
O4—Nd1—O678.53 (19)N1—C1—H1C109.5
O3—Nd1—O6125.83 (19)H1A—C1—H1C109.5
O2—Nd1—O676.72 (19)H1B—C1—H1C109.5
O1—Nd1—O680.42 (19)N1—C1'—H1'A109.5
O9—Nd1—O6145.6 (2)N1—C1'—H1'B109.5
O8—Nd1—O6147.32 (18)H1'A—C1'—H1'B109.5
O4—Nd1—O579.80 (19)N1—C1'—H1'C109.5
O3—Nd1—O576.02 (17)H1'A—C1'—H1'C109.5
O2—Nd1—O5126.49 (18)H1'B—C1'—H1'C109.5
O1—Nd1—O582.12 (19)N2—C3—H3A109.5
O9—Nd1—O5144.21 (18)N2—C3—H3B109.5
O8—Nd1—O5143.91 (19)H3A—C3—H3B109.5
O6—Nd1—O549.82 (17)N2—C3—H3C109.5
O4—Nd1—N14102.8 (2)H3A—C3—H3C109.5
O3—Nd1—N1475.88 (19)H3B—C3—H3C109.5
O2—Nd1—N1481.6 (2)N2—C3'—H3'1109.5
O1—Nd1—N1499.0 (2)N2—C3'—H3'2109.5
O9—Nd1—N1424.87 (19)H3'1—C3'—H3'2109.5
O8—Nd1—N1425.19 (19)N2—C3'—H3'3109.5
O6—Nd1—N14158.3 (2)H3'1—C3'—H3'3109.5
O5—Nd1—N14151.87 (19)H3'2—C3'—H3'3109.5
O4—Nd1—N1375.94 (19)N3—C5—H5A109.5
O3—Nd1—N13100.9 (2)N3—C5—H5B109.5
O2—Nd1—N13101.4 (2)H5A—C5—H5B109.5
O1—Nd1—N1382.5 (2)N3—C5—H5C109.5
O9—Nd1—N13156.55 (19)H5A—C5—H5C109.5
O8—Nd1—N13153.4 (2)H5B—C5—H5C109.5
O6—Nd1—N1324.93 (18)N3—C5'—H5'A109.5
O5—Nd1—N1325.05 (18)N3—C5'—H5'B109.5
N14—Nd1—N13176.6 (2)H5'A—C5'—H5'B109.5
O1—P1—N3110.4 (4)N3—C5'—H5'C109.5
O1—P1—N1110.5 (4)H5'A—C5'—H5'C109.5
N3—P1—N1114.9 (5)H5'B—C5'—H5'C109.5
O1—P1—N2114.4 (4)N4—C9—H9A109.5
N3—P1—N2104.1 (6)N4—C9—H9B109.5
N1—P1—N2102.2 (5)H9A—C9—H9B109.5
O2—P2—N4109.3 (4)N4—C9—H9C109.5
O2—P2—N6118.6 (4)H9A—C9—H9C109.5
N4—P2—N6106.6 (5)H9B—C9—H9C109.5
O2—P2—N5108.9 (4)N4—C9'—H9'A109.5
N4—P2—N5114.8 (6)N4—C9'—H9'B109.5
N6—P2—N598.5 (5)H9'A—C9'—H9'B109.5
O3—P3—N9111.6 (3)N4—C9'—H9'C109.5
O3—P3—N7108.4 (3)H9'A—C9'—H9'C109.5
N9—P3—N7109.2 (4)H9'B—C9'—H9'C109.5
O3—P3—N8111.1 (3)N4—C10—H10D109.5
N9—P3—N8107.1 (4)N4—C10—H10E109.5
N7—P3—N8109.3 (4)H10D—C10—H10E109.5
O4—P4—N11'123.5 (7)N4—C10—H10F109.5
O4—P4—N10109.3 (6)H10D—C10—H10F109.5
N11'—P4—N10122.5 (8)H10E—C10—H10F109.5
O4—P4—N12'107.1 (7)N4—C10'—H10G109.5
N11'—P4—N12'75.6 (9)N4—C10'—H10H109.5
N10—P4—N12'110.7 (9)H10G—C10'—H10H109.5
O4—P4—N10'112.3 (6)N4—C10'—H10I109.5
N11'—P4—N10'94.6 (8)H10G—C10'—H10I109.5
N12'—P4—N10'137.7 (8)H10H—C10'—H10I109.5
O4—P4—N11105.3 (6)N6—C11—H11A109.5
N10—P4—N11112.7 (8)N6—C11—H11B109.5
N12'—P4—N11111.5 (9)H11A—C11—H11B109.5
N10'—P4—N1172.6 (8)N6—C11—H11C109.5
O4—P4—N12115.3 (6)H11A—C11—H11C109.5
N11'—P4—N12110.9 (9)H11B—C11—H11C109.5
N10—P4—N1257.2 (8)N6—C11'—H11D109.5
N12'—P4—N1254.2 (8)N6—C11'—H11E109.5
N10'—P4—N1294.1 (8)H11D—C11'—H11E109.5
N11—P4—N12139.3 (8)N6—C11'—H11F109.5
P1—O1—Nd1167.7 (4)H11D—C11'—H11F109.5
P4—O4—Nd1168.7 (4)H11E—C11'—H11F109.5
P2—O2—Nd1160.0 (3)N6—C12—H12A109.5
P3—O3—Nd1167.4 (3)N6—C12—H12B109.5
N13—O5—Nd195.8 (4)H12A—C12—H12B109.5
N13—O6—Nd196.0 (4)N6—C12—H12C109.5
N14—O8—Nd195.9 (4)H12A—C12—H12C109.5
N14—O9—Nd196.8 (5)H12B—C12—H12C109.5
C1'—N1—C2113.6 (14)N6—C12'—H12D109.5
C1—N1—C2115.3 (14)N6—C12'—H12E109.5
C1'—N1—P1125.3 (13)H12D—C12'—H12E109.5
C1—N1—P1116.5 (13)N6—C12'—H12F109.5
C2—N1—P1120.5 (8)H12D—C12'—H12F109.5
C4—N2—C3'96 (2)H12E—C12'—H12F109.5
C4—N2—C3112 (2)H17A—C17—H17B109.5
C4—N2—P1127.5 (10)H17A—C17—H17C109.5
C3'—N2—P1122.8 (19)H17B—C17—H17C109.5
C3—N2—P1118.8 (19)N9—C17'—H17D109.5
C5'—N3—C6104.0 (13)N9—C17'—H17E109.5
C6—N3—C5126.3 (12)H17D—C17'—H17E109.5
C5'—N3—P1127.9 (12)N9—C17'—H17F109.5
C6—N3—P1122.3 (8)H17D—C17'—H17F109.5
C5—N3—P1111.4 (11)H17E—C17'—H17F109.5
C10'—N4—C9109.3 (14)N10—C19—H19A109.5
C9—N4—C10106.1 (14)N10—C19—H19B109.5
C10'—N4—C9'110.4 (14)H19A—C19—H19B109.5
C10—N4—C9'121.1 (14)N10—C19—H19C109.5
C10'—N4—P2126.2 (10)H19A—C19—H19C109.5
C9—N4—P2122.3 (11)H19B—C19—H19C109.5
C10—N4—P2116.5 (10)N10'—C19'—H19D109.5
C9'—N4—P2121.5 (11)N10'—C19'—H19E109.5
C7—N5—C8112.3 (11)H19D—C19'—H19E109.5
C7—N5—P2122.0 (9)N10'—C19'—H19F109.5
C8—N5—P2119.1 (8)H19D—C19'—H19F109.5
C12—N6—C1186.0 (16)H19E—C19'—H19F109.5
C12—N6—C11'109.8 (16)N10—C20—H20A109.5
C11—N6—C12'114.6 (16)N10—C20—H20B109.5
C11'—N6—C12'136.9 (17)H20A—C20—H20B109.5
C12—N6—P2135.9 (13)N10—C20—H20C109.5
C11—N6—P2125.4 (13)H20A—C20—H20C109.5
C11'—N6—P2110.4 (12)H20B—C20—H20C109.5
C12'—N6—P2112.4 (12)N10'—C20'—H20D109.5
C13—N7—C14114.5 (7)N10'—C20'—H20E109.5
C13—N7—P3120.2 (5)H20D—C20'—H20E109.5
C14—N7—P3122.5 (6)N10'—C20'—H20F109.5
C15—N8—C16114.3 (8)H20D—C20'—H20F109.5
C15—N8—P3125.3 (7)H20E—C20'—H20F109.5
C16—N8—P3119.6 (6)N11—C21—H21A109.5
C17'—N9—C18103.7 (11)N11—C21—H21B109.5
C17'—N9—P3136.4 (11)H21A—C21—H21B109.5
C18—N9—P3119.4 (7)N11—C21—H21C109.5
O7—N13—O6122.7 (7)H21A—C21—H21C109.5
O7—N13—O5119.6 (8)H21B—C21—H21C109.5
O6—N13—O5117.6 (7)N11'—C21'—H21D109.5
O7—N13—Nd1171.7 (6)N11'—C21'—H21E109.5
O6—N13—Nd159.0 (4)H21D—C21'—H21E109.5
O5—N13—Nd159.2 (4)N11'—C21'—H21F109.5
O10—N14—O9121.2 (8)H21D—C21'—H21F109.5
O10—N14—O8121.8 (8)H21E—C21'—H21F109.5
O9—N14—O8117.0 (7)N11—C22—H22A109.5
O10—N14—Nd1174.2 (7)N11—C22—H22B109.5
O9—N14—Nd158.4 (4)H22A—C22—H22B109.5
O8—N14—Nd158.9 (4)N11—C22—H22C109.5
N1—C2—H2A109.5H22A—C22—H22C109.5
N1—C2—H2B109.5H22B—C22—H22C109.5
H2A—C2—H2B109.5H22D—C22'—H22E109.5
N1—C2—H2C109.5H22D—C22'—H22F109.5
H2A—C2—H2C109.5H22E—C22'—H22F109.5
H2B—C2—H2C109.5N12'—C24'—H24C109.5
N2—C4—H4A109.5N12'—C24'—H24E109.5
N2—C4—H4B109.5H24C—C24'—H24E109.5
H4A—C4—H4B109.5N12'—C24'—H24F109.5
N2—C4—H4C109.5H24C—C24'—H24F109.5
H4A—C4—H4C109.5H24E—C24'—H24F109.5
H4B—C4—H4C109.5N12—C24—H24A109.5
N3—C6—H6A109.5N12—C24—H24B109.5
N3—C6—H6B109.5H24A—C24—H24B109.5
H6A—C6—H6B109.5N12—C24—H24D109.5
N3—C6—H6C109.5H24A—C24—H24D109.5
H6A—C6—H6C109.5H24B—C24—H24D109.5
H6B—C6—H6C109.5N12'—C23'—H23A109.5
N5—C7—H7A109.5N12'—C23'—H23D109.5
N5—C7—H7B109.5H23A—C23'—H23D109.5
H7A—C7—H7B109.5N12'—C23'—H23B109.5
N5—C7—H7C109.5H23A—C23'—H23B109.5
H7A—C7—H7C109.5H23D—C23'—H23B109.5
H7B—C7—H7C109.5N12—C23—H23C109.5
N5—C8—H8A109.5N12—C23—H23G109.5
N5—C8—H8B109.5H23C—C23—H23G109.5
H8A—C8—H8B109.5N12—C23—H23E109.5
N5—C8—H8C109.5H23C—C23—H23E109.5
H8A—C8—H8C109.5H23G—C23—H23E109.5
H8B—C8—H8C109.5
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) x, −y+1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[Nd(NO3)2(C6H18N3OP)4][AgWS4]
Mr1405.07
Crystal system, space groupMonoclinic, P21/c
Temperature (K)153
a, b, c (Å)15.8250 (19), 29.873 (4), 11.4345 (13)
β (°) 90.689 (3)
V (Å3)5405.2 (12)
Z4
Radiation typeMo Kα
µ (mm−1)3.76
Crystal size (mm)0.2 × 0.15 × 0.1
Data collection
DiffractometerRigaku Mercury
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.132, 0.329
No. of measured, independent and
observed [I > 2σ(I)] reflections		46733, 9877, 9086
Rint0.045
(sin θ/λ)max (Å−1)0.602
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.050, 0.108, 1.14
No. of reflections9877
No. of parameters506
No. of restraints28
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0328P)2 + 29.5132P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å−3)1.42, −1.37

Computer programs: CrystalClear (Rigaku Corporation, 2000), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008).

 

Acknowledgements

This work is supported by the National Natural Science Foundation of China (No. 50472048), the Program for New Century Excellent Talents in Universities (NCET-05-0499), and the Graduate Innovation Laboratory Center of Nanjing University of Science and Tecnology

References

First citationHuang, Q., Wu, X. T., Sheng, T. L., Wang, Q. M. & Lu, J. X. (1997). Polyhedron, 16, 217–222.  CSD CrossRef CAS Web of Science Google Scholar
 First citationHuang, Q., Wu, X. T., Wang, Q. M., Sheng, T. L. & Lu, J. X. (1996). Angew. Chem. Int. Ed. Engl. 35, 868–870.  CSD CrossRef CAS Web of Science Google Scholar
 First citationLang, J. P., Li, J. G., Bao, S. A., Xin, X. Q. & Yu, K. B. (1993). Polyhedron, 12, 801–806.  CAS 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 Corporation (2000). CrystalClear. Version 1.3. Rigaku Corporation, Tokyo, Japan.  Google Scholar
 First citationRigaku/MSC (2002). CrystalStructure. Version 3.00. Rigaku/MSC, The Woodlands, Texas, USA.  Google Scholar
 First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS 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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ISSN: 2056-9890
Volume 64| Part 3| March 2008| Page m478
doi:10.1107/S1600536808001256
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