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′)holmium(III)] [silver(I)-di-μ-sulfido-tungstate(VI)-di-μ-sulfido]]

aHuaiyin Advanced Vocational and Technical School of Health, Huaian 223300, Jiangsu Province, People's Republic of China, bSchool of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, People's Republic of China, and cJiangsu Key Laboratory for Chemistry of Low-Dimensional Materials, School of Chemistry and Chemical Engineering, Huaiyin Normal University, Huaian 223300, Jiangsu Province, People's Republic of China
*Correspondence e-mail: hysytanggd@hotmail.com

(Received 28 October 2011; accepted 3 November 2011; online 9 November 2011)

In the title salt, {[Ho(NO3)2(C6H18N3OP)4][AgWS4]}n, the anion forms a W/S/Ag polymeric chain along the a axis. The holmium atom in the cation is coordinated by eight O atoms from two nitrate and four hexa­methyl­phospho­ramide ligands in a distorted square-anti­prismatic geometry. Together with the two nitrate ligands, the complex cation in the title compound is univalent, which leads the anion to be univalent as well. The polymeric anionic chain with W—Ag—W and Ag—W—Ag angles of 161.429 (17) and 153.608 (10) °, respectively, presents a distorted linear configuration. The title complex is isotypic with the corresponding Y, Yb, Eu, Nd, La and Dy analogues.

Related literature

For one-dimensional Mo(W)/S/Ag anionic polymers, see: Niu et al. (2004[Niu, Y. Y., Zheng, H. G., Hou, H. W. & Xin, X. Q. (2004). Coord. Chem. Rev. 248, 169-183.]). For isotypic compounds, see: Zhang, Cao et al. (2007[Zhang, J.-F., Cao, Y., Qian, J. & Zhang, C. (2007). Acta Cryst. E63, m2248-m2249.]); Cao et al. (2007[Cao, Y., Zhang, J.-F., Qian, J. & Zhang, C. (2007). Acta Cryst. E63, m2076-m2077.]); Zhang, Qian et al. (2007[Zhang, J., Qian, J., Cao, Y. & Zhang, C. (2007). Acta Cryst. E63, m2386-m2387.]); Tang, Zhang & Zhang (2008[Tang, G., Zhang, J. & Zhang, C. (2008). Acta Cryst. E64, m478.]); Tang, Zhang, Zhang & Lu (2008[Tang, G., Zhang, J., Zhang, C. & Lu, L. (2008). Acta Cryst. E64, m399-m400.]); Zhang (2010[Zhang, J. (2010). Acta Cryst. E66, m1479.], 2011[Zhang, J. (2011). Acta Cryst. E67, m1206-m1207.]).

[Scheme 1]

Experimental

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

  • Mr = 1425.76

  • Monoclinic, P 21 /c

  • a = 15.767 (3) Å

  • b = 29.616 (6) Å

  • c = 11.383 (2) Å

  • β = 90.88 (3)°

  • V = 5314.7 (17) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 4.33 mm−1

  • T = 173 K

  • 0.18 × 0.15 × 0.10 mm

Data collection
  • Rigaku Mercury2 diffractometer

  • Absorption correction: multi-scan (CrystalClear; Rigaku, 2008[Rigaku (2008). CrystalClear. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.463, Tmax = 0.648

  • 24559 measured reflections

  • 9655 independent reflections

  • 8942 reflections with I > 2σ(I)

  • Rint = 0.024

Refinement
  • R[F2 > 2σ(F2)] = 0.031

  • wR(F2) = 0.073

  • S = 1.03

  • 9655 reflections

  • 532 parameters

  • H-atom parameters constrained

  • Δρmax = 0.87 e Å−3

  • Δρmin = −0.86 e Å−3

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

Supporting information


Comment top

One-dimensional Mo(W)/S/Ag anionic polymers have attracted much attention for their configurational isomerism (Niu et al., 2004). Different solvent-coordinated rare-earth cations proved effective to obtain various configurations of anionic chains (Niu et al., 2004). The title compound {[Ho(hmp)4(NO3)2][WS4Ag]}n (hmp = hexamethylphosphoramide) with a wave-like anionic chain was prepared by following such route using Ho(III)-hmp complex as counterion.

The title complex is isostructural with Y (Zhang, Cao et al., 2007; Zhang, 2011), 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. The holmium(III) atom in the cation (Fig. 1) 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, which leads to an anionic chain with a univalent repeat unit. As illustrated in Fig. 2, the anionic chain in the title compound has a distorted linear configuration with W—Ag—W and Ag—W—Ag angles of 161.429 (17) and 153.608 (10) °, respectively,

Related literature top

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

Experimental top

AgI (1 mmol) was added to a solution of [NH4]2WS4 (1 mmol) in hexamethylphosphoramide (8 ml) with thorough stirring for 30 minutes. The solution underwent additional stirring for two minute, then Ho(NO3)3.6H2O (0.5 mmol) was added. After filtration the orange filtrate was carefully laid on the surface with 12 ml i-PrOH. Orange block crystals were obtained after about one week.

Refinement top

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

Structure description top

One-dimensional Mo(W)/S/Ag anionic polymers have attracted much attention for their configurational isomerism (Niu et al., 2004). Different solvent-coordinated rare-earth cations proved effective to obtain various configurations of anionic chains (Niu et al., 2004). The title compound {[Ho(hmp)4(NO3)2][WS4Ag]}n (hmp = hexamethylphosphoramide) with a wave-like anionic chain was prepared by following such route using Ho(III)-hmp complex as counterion.

The title complex is isostructural with Y (Zhang, Cao et al., 2007; Zhang, 2011), 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. The holmium(III) atom in the cation (Fig. 1) 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, which leads to an anionic chain with a univalent repeat unit. As illustrated in Fig. 2, the anionic chain in the title compound has a distorted linear configuration with W—Ag—W and Ag—W—Ag angles of 161.429 (17) and 153.608 (10) °, respectively,

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

Computing details top

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

Figures top
[Figure 1] Fig. 1. The molecular structure of the cation in the title compound, with 30% probability displacement ellipsoids. All H atoms have been omitted.
[Figure 2] Fig. 2. The molecular structure of a portion of the anionic chain in the title compound, with30% probability displacement ellipsoids, Symmetry code: (i) x, -y+1/2, z+1/2.
catena-Poly[[tetrakis(hexamethylphosphoramide-κO)bis(nitrato- κ2O,O')holmium(III)] [silver(I)-di-µ-sulfido-tungstate(VI)-di-µ-sulfido]] top
Crystal data top
[Ho(NO3)2(C6H18N3OP)4][AgWS4]F(000) = 2824
Mr = 1425.76Dx = 1.782 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 22657 reflections
a = 15.767 (3) Åθ = 3.7–29.1°
b = 29.616 (6) ŵ = 4.33 mm1
c = 11.383 (2) ÅT = 173 K
β = 90.88 (3)°Block, orange
V = 5314.7 (17) Å30.18 × 0.15 × 0.1 mm
Z = 4
Data collection top
Rigaku Mercury2
diffractometer
9655 independent reflections
Radiation source: fine-focus sealed tube8942 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
dtprofit.ref scansθmax = 25.4°, θmin = 3.7°
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2008)
h = 1718
Tmin = 0.463, Tmax = 0.648k = 3530
24559 measured reflectionsl = 1013
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)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.073H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.030P)2 + 16.6944P]
where P = (Fo2 + 2Fc2)/3
9655 reflections(Δ/σ)max = 0.001
532 parametersΔρmax = 0.87 e Å3
0 restraintsΔρmin = 0.86 e Å3
Crystal data top
[Ho(NO3)2(C6H18N3OP)4][AgWS4]V = 5314.7 (17) Å3
Mr = 1425.76Z = 4
Monoclinic, P21/cMo Kα radiation
a = 15.767 (3) ŵ = 4.33 mm1
b = 29.616 (6) ÅT = 173 K
c = 11.383 (2) Å0.18 × 0.15 × 0.1 mm
β = 90.88 (3)°
Data collection top
Rigaku Mercury2
diffractometer
9655 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2008)
8942 reflections with I > 2σ(I)
Tmin = 0.463, Tmax = 0.648Rint = 0.024
24559 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0310 restraints
wR(F2) = 0.073H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.030P)2 + 16.6944P]
where P = (Fo2 + 2Fc2)/3
9655 reflectionsΔρmax = 0.87 e Å3
532 parametersΔρmin = 0.86 e Å3
Special details top

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

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ho10.738176 (12)0.082625 (6)0.827842 (18)0.01998 (6)
P10.69903 (8)0.03034 (4)0.69978 (12)0.0288 (3)
P20.52206 (7)0.13270 (4)0.82148 (11)0.0276 (3)
P30.79412 (10)0.14676 (5)1.09606 (12)0.0386 (3)
P40.95858 (7)0.09616 (4)0.73141 (12)0.0284 (3)
O10.7068 (2)0.01807 (10)0.7291 (3)0.0276 (7)
O20.60328 (19)0.10691 (11)0.8233 (3)0.0284 (7)
O30.7724 (2)0.12690 (11)0.9803 (3)0.0311 (8)
O40.87641 (19)0.08053 (11)0.7803 (3)0.0314 (8)
O50.8019 (2)0.02693 (11)0.9646 (3)0.0312 (8)
O60.6691 (2)0.04086 (11)0.9882 (3)0.0304 (8)
O70.7370 (3)0.00123 (14)1.1197 (4)0.0522 (11)
O80.7241 (2)0.10309 (11)0.6201 (3)0.0317 (8)
O90.7525 (2)0.15801 (11)0.7384 (3)0.0325 (8)
O100.7262 (3)0.17165 (15)0.5536 (4)0.0666 (14)
N10.7363 (3)0.02232 (14)1.0272 (4)0.0324 (10)
N20.7346 (3)0.14521 (14)0.6350 (4)0.0359 (10)
N30.7204 (3)0.03686 (14)0.5597 (4)0.0368 (10)
N40.6062 (3)0.04810 (17)0.7393 (5)0.0501 (13)
N50.7649 (3)0.06527 (15)0.7670 (4)0.0445 (12)
N60.5229 (3)0.17284 (15)0.9200 (5)0.0438 (12)
N70.4446 (2)0.09754 (15)0.8481 (4)0.0322 (10)
N80.5064 (3)0.15650 (19)0.6950 (4)0.0490 (13)
N90.8961 (4)0.13875 (19)1.1241 (6)0.0706 (19)
N100.7739 (4)0.20017 (15)1.0948 (4)0.0511 (14)
N110.7405 (4)0.12367 (19)1.1984 (5)0.0657 (17)
N121.0341 (3)0.07042 (16)0.8029 (4)0.0413 (12)
N130.9834 (3)0.14887 (15)0.7386 (5)0.0466 (12)
N140.9564 (3)0.08651 (18)0.5892 (4)0.0455 (12)
C10.6968 (4)0.0020 (2)0.4761 (5)0.0538 (16)
H1A0.71370.01090.39880.081*
H1B0.72470.02570.49720.081*
H1C0.63650.00230.47680.081*
C20.7255 (4)0.0825 (2)0.5080 (6)0.0507 (16)
H2A0.73830.08010.42610.076*
H2B0.67220.09770.51680.076*
H2C0.76940.09940.54750.076*
C30.5353 (4)0.0168 (2)0.7485 (7)0.0609 (19)
H3A0.48560.03300.77180.091*
H3B0.52490.00280.67370.091*
H3C0.54870.00590.80600.091*
C40.5810 (5)0.0956 (2)0.7216 (7)0.075 (2)
H4A0.52410.09990.74830.113*
H4B0.61880.11490.76540.113*
H4C0.58360.10300.63960.113*
C50.7544 (6)0.0812 (3)0.8849 (7)0.078 (2)
H5A0.80060.10080.90590.117*
H5B0.70190.09740.89000.117*
H5C0.75360.05590.93780.117*
C60.8534 (5)0.0682 (3)0.7348 (8)0.079 (2)
H6A0.88160.09020.78350.119*
H6B0.88000.03930.74570.119*
H6C0.85720.07700.65390.119*
C70.4540 (4)0.1829 (2)0.9993 (6)0.0592 (18)
H7A0.46980.20801.04860.089*
H7B0.44280.15701.04720.089*
H7C0.40400.19060.95440.089*
C80.5899 (4)0.2076 (2)0.9181 (7)0.065 (2)
H8A0.58150.22860.98110.097*
H8B0.58750.22340.84450.097*
H8C0.64440.19350.92750.097*
C90.3567 (3)0.1067 (2)0.8122 (5)0.0475 (15)
H9A0.32110.08220.83650.071*
H9B0.35320.10970.72830.071*
H9C0.33790.13420.84820.071*
C100.4535 (3)0.0645 (2)0.9432 (5)0.0416 (13)
H10A0.40280.04670.94740.062*
H10B0.46250.08001.01640.062*
H10C0.50100.04520.92830.062*
C110.4636 (5)0.2007 (3)0.6800 (8)0.085 (3)
H11A0.46080.20830.59800.128*
H11B0.49500.22350.72190.128*
H11C0.40720.19890.71020.128*
C120.5195 (4)0.1314 (3)0.5891 (6)0.081 (3)
H12A0.50750.15030.52240.121*
H12B0.48230.10570.58730.121*
H12C0.57730.12140.58670.121*
C130.9350 (5)0.0958 (3)1.1115 (8)0.082 (3)
H13A0.99390.09791.13360.123*
H13B0.93010.08611.03120.123*
H13C0.90750.07431.16120.123*
C140.9511 (6)0.1717 (3)1.1833 (9)0.107 (4)
H14A1.00730.15951.19130.161*
H14B0.92930.17821.25960.161*
H14C0.95290.19891.13770.161*
C150.8026 (5)0.22773 (18)0.9958 (5)0.0497 (16)
H15A0.78570.25851.00740.074*
H15B0.77760.21650.92410.074*
H15C0.86330.22610.99120.074*
C160.7480 (7)0.2263 (2)1.1976 (6)0.094 (3)
H16A0.73950.25731.17530.141*
H16B0.79150.22461.25740.141*
H16C0.69610.21421.22740.141*
C170.6491 (5)0.1205 (3)1.1866 (7)0.079 (2)
H17A0.62660.10621.25520.119*
H17B0.63470.10291.11840.119*
H17C0.62550.15021.17860.119*
C180.7782 (8)0.1066 (4)1.3086 (7)0.127 (4)
H18A0.73430.09461.35720.190*
H18B0.80650.13091.34920.190*
H18C0.81840.08331.29150.190*
C191.0209 (4)0.0276 (2)0.8615 (7)0.0601 (19)
H19A1.07310.01800.89820.090*
H19B1.00270.00550.80500.090*
H19C0.97830.03110.92010.090*
C201.1239 (4)0.0796 (3)0.7802 (8)0.084 (3)
H20A1.15870.06110.83080.126*
H20B1.13580.11090.79540.126*
H20C1.13590.07280.69970.126*
C210.9508 (4)0.1826 (2)0.6548 (9)0.086 (3)
H21A0.97310.21180.67510.129*
H21B0.89000.18340.65770.129*
H21C0.96800.17470.57700.129*
C221.0142 (6)0.1686 (3)0.8488 (7)0.089 (3)
H22A1.02560.20010.83730.134*
H22B1.06530.15360.87360.134*
H22C0.97190.16510.90790.134*
C230.9074 (4)0.0485 (2)0.5426 (6)0.0554 (17)
H23A0.91270.04740.45880.083*
H23B0.84880.05220.56220.083*
H23C0.92850.02090.57630.083*
C241.0297 (5)0.0965 (3)0.5170 (7)0.084 (3)
H24A1.01730.08850.43690.126*
H24B1.07760.07930.54490.126*
H24C1.04260.12810.52190.126*
W10.216203 (12)0.227544 (6)0.474103 (16)0.02219 (6)
Ag10.21748 (3)0.234393 (14)0.21359 (3)0.04001 (11)
S10.33062 (8)0.21142 (5)0.37372 (11)0.0363 (3)
S20.10254 (8)0.21235 (5)0.36792 (12)0.0386 (3)
S30.21433 (9)0.18463 (4)0.63272 (11)0.0323 (3)
S40.21647 (9)0.30058 (4)0.51424 (11)0.0357 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ho10.01767 (10)0.01553 (10)0.02679 (12)0.00013 (8)0.00225 (8)0.00061 (8)
P10.0346 (7)0.0203 (6)0.0318 (7)0.0058 (5)0.0097 (6)0.0058 (5)
P20.0199 (6)0.0338 (7)0.0291 (7)0.0049 (5)0.0001 (5)0.0050 (5)
P30.0560 (9)0.0270 (7)0.0322 (8)0.0093 (6)0.0164 (7)0.0007 (6)
P40.0193 (6)0.0272 (6)0.0388 (8)0.0005 (5)0.0046 (5)0.0073 (5)
O10.0327 (18)0.0175 (15)0.0325 (19)0.0031 (14)0.0033 (14)0.0053 (14)
O20.0207 (16)0.0306 (18)0.0339 (19)0.0021 (14)0.0016 (14)0.0015 (15)
O30.0322 (18)0.0273 (17)0.0336 (19)0.0016 (15)0.0049 (15)0.0076 (15)
O40.0188 (16)0.0313 (18)0.044 (2)0.0007 (14)0.0087 (15)0.0043 (15)
O50.0260 (17)0.0270 (18)0.041 (2)0.0001 (14)0.0007 (15)0.0058 (15)
O60.0249 (17)0.0322 (18)0.0342 (19)0.0024 (15)0.0008 (15)0.0030 (15)
O70.059 (3)0.056 (3)0.041 (2)0.003 (2)0.001 (2)0.025 (2)
O80.042 (2)0.0223 (17)0.0312 (19)0.0034 (15)0.0050 (16)0.0008 (14)
O90.040 (2)0.0193 (16)0.038 (2)0.0034 (15)0.0002 (16)0.0032 (15)
O100.105 (4)0.046 (3)0.048 (3)0.017 (3)0.013 (3)0.025 (2)
N10.033 (2)0.025 (2)0.039 (3)0.0024 (18)0.004 (2)0.0028 (19)
N20.042 (3)0.030 (2)0.036 (3)0.002 (2)0.003 (2)0.007 (2)
N30.050 (3)0.031 (2)0.030 (2)0.006 (2)0.009 (2)0.0085 (19)
N40.044 (3)0.044 (3)0.062 (3)0.017 (2)0.021 (2)0.021 (3)
N50.064 (3)0.026 (2)0.044 (3)0.008 (2)0.016 (2)0.003 (2)
N60.035 (2)0.035 (2)0.061 (3)0.007 (2)0.012 (2)0.006 (2)
N70.0196 (19)0.042 (2)0.035 (2)0.0007 (18)0.0021 (17)0.0033 (19)
N80.035 (3)0.073 (4)0.039 (3)0.002 (2)0.007 (2)0.023 (3)
N90.074 (4)0.047 (3)0.089 (5)0.017 (3)0.051 (4)0.002 (3)
N100.094 (4)0.028 (2)0.031 (3)0.009 (3)0.006 (3)0.005 (2)
N110.104 (5)0.051 (3)0.041 (3)0.030 (3)0.004 (3)0.010 (3)
N120.019 (2)0.052 (3)0.053 (3)0.004 (2)0.006 (2)0.026 (2)
N130.039 (3)0.029 (2)0.072 (4)0.004 (2)0.011 (2)0.006 (2)
N140.034 (2)0.064 (3)0.039 (3)0.008 (2)0.009 (2)0.007 (2)
C10.077 (5)0.053 (4)0.031 (3)0.003 (3)0.005 (3)0.001 (3)
C20.065 (4)0.042 (3)0.045 (4)0.007 (3)0.018 (3)0.018 (3)
C30.031 (3)0.065 (4)0.086 (5)0.002 (3)0.002 (3)0.012 (4)
C40.086 (5)0.060 (4)0.080 (5)0.039 (4)0.033 (4)0.026 (4)
C50.101 (6)0.059 (5)0.074 (5)0.029 (4)0.018 (5)0.026 (4)
C60.056 (4)0.093 (6)0.090 (6)0.019 (4)0.006 (4)0.017 (5)
C70.057 (4)0.054 (4)0.067 (5)0.017 (3)0.022 (3)0.008 (3)
C80.059 (4)0.042 (4)0.094 (6)0.007 (3)0.014 (4)0.013 (4)
C90.023 (3)0.069 (4)0.051 (4)0.003 (3)0.004 (2)0.014 (3)
C100.027 (3)0.051 (3)0.047 (3)0.001 (3)0.007 (2)0.014 (3)
C110.059 (4)0.088 (6)0.108 (7)0.015 (4)0.018 (4)0.064 (5)
C120.051 (4)0.153 (8)0.037 (4)0.018 (5)0.008 (3)0.002 (5)
C130.059 (5)0.071 (5)0.114 (7)0.002 (4)0.046 (5)0.009 (5)
C140.111 (7)0.099 (7)0.110 (8)0.049 (6)0.057 (6)0.006 (6)
C150.079 (5)0.028 (3)0.042 (4)0.003 (3)0.006 (3)0.003 (2)
C160.192 (10)0.046 (4)0.045 (4)0.033 (5)0.035 (5)0.023 (3)
C170.100 (6)0.074 (5)0.065 (5)0.029 (5)0.040 (5)0.008 (4)
C180.216 (13)0.112 (8)0.051 (5)0.006 (8)0.001 (7)0.050 (5)
C190.034 (3)0.057 (4)0.089 (5)0.004 (3)0.008 (3)0.038 (4)
C200.027 (3)0.119 (7)0.105 (6)0.000 (4)0.003 (4)0.074 (6)
C210.045 (4)0.045 (4)0.170 (9)0.007 (3)0.019 (5)0.059 (5)
C220.108 (7)0.066 (5)0.095 (6)0.050 (5)0.034 (5)0.037 (5)
C230.047 (3)0.073 (5)0.047 (4)0.003 (3)0.004 (3)0.012 (3)
C240.068 (5)0.135 (8)0.050 (5)0.035 (5)0.021 (4)0.011 (5)
W10.02714 (11)0.02160 (10)0.01777 (10)0.00239 (7)0.00110 (7)0.00105 (7)
Ag10.0619 (3)0.0377 (2)0.0204 (2)0.0004 (2)0.00013 (18)0.00237 (16)
S10.0321 (7)0.0487 (8)0.0280 (7)0.0047 (6)0.0023 (5)0.0021 (6)
S20.0326 (7)0.0531 (8)0.0299 (7)0.0137 (6)0.0052 (5)0.0040 (6)
S30.0469 (7)0.0254 (6)0.0246 (6)0.0010 (6)0.0016 (5)0.0056 (5)
S40.0566 (8)0.0220 (6)0.0285 (7)0.0040 (6)0.0004 (6)0.0015 (5)
Geometric parameters (Å, º) top
Ho1—O32.235 (3)C6—H6A0.9600
Ho1—O22.245 (3)C6—H6B0.9600
Ho1—O42.255 (3)C6—H6C0.9600
Ho1—O12.269 (3)C7—H7A0.9600
Ho1—O82.448 (3)C7—H7B0.9600
Ho1—O92.465 (3)C7—H7C0.9600
Ho1—O52.471 (3)C8—H8A0.9600
Ho1—O62.472 (3)C8—H8B0.9600
Ho1—N22.872 (4)C8—H8C0.9600
Ho1—N12.888 (4)C9—H9A0.9600
P1—O11.477 (3)C9—H9B0.9600
P1—N41.626 (5)C9—H9C0.9600
P1—N51.646 (5)C10—H10A0.9600
P1—N31.646 (4)C10—H10B0.9600
P2—O21.491 (3)C10—H10C0.9600
P2—N81.618 (5)C11—H11A0.9600
P2—N61.634 (5)C11—H11B0.9600
P2—N71.637 (4)C11—H11C0.9600
P3—O31.478 (3)C12—H12A0.9600
P3—N111.603 (6)C12—H12B0.9600
P3—N101.613 (5)C12—H12C0.9600
P3—N91.651 (6)C13—H13A0.9600
P4—O41.492 (3)C13—H13B0.9600
P4—N131.611 (5)C13—H13C0.9600
P4—N121.622 (4)C14—H14A0.9600
P4—N141.644 (5)C14—H14B0.9600
O5—N11.272 (5)C14—H14C0.9600
O6—N11.268 (5)C15—H15A0.9600
O7—N11.224 (5)C15—H15B0.9600
O8—N21.269 (5)C15—H15C0.9600
O9—N21.264 (5)C16—H16A0.9600
O10—N21.219 (6)C16—H16B0.9600
N3—C11.449 (7)C16—H16C0.9600
N3—C21.476 (7)C17—H17A0.9600
N4—C31.456 (8)C17—H17B0.9600
N4—C41.476 (8)C17—H17C0.9600
N5—C51.434 (8)C18—H18A0.9600
N5—C61.451 (8)C18—H18B0.9600
N6—C71.454 (7)C18—H18C0.9600
N6—C81.476 (8)C19—H19A0.9600
N7—C91.464 (6)C19—H19B0.9600
N7—C101.464 (7)C19—H19C0.9600
N8—C121.434 (9)C20—H20A0.9600
N8—C111.482 (9)C20—H20B0.9600
N9—C131.422 (9)C20—H20C0.9600
N9—C141.463 (9)C21—H21A0.9600
N10—C161.466 (8)C21—H21B0.9600
N10—C151.469 (7)C21—H21C0.9600
N11—C171.447 (10)C22—H22A0.9600
N11—C181.470 (9)C22—H22B0.9600
N12—C191.448 (7)C22—H22C0.9600
N12—C201.469 (7)C23—H23A0.9600
N13—C221.460 (9)C23—H23B0.9600
N13—C211.469 (8)C23—H23C0.9600
N14—C241.459 (8)C24—H24A0.9600
N14—C231.461 (8)C24—H24B0.9600
C1—H1A0.9600C24—H24C0.9600
C1—H1B0.9600W1—S22.1929 (14)
C1—H1C0.9600W1—S12.2026 (14)
C2—H2A0.9600W1—S32.2085 (12)
C2—H2B0.9600W1—S42.2106 (13)
C2—H2C0.9600W1—Ag1i2.9498 (6)
C3—H3A0.9600W1—Ag12.9727 (7)
C3—H3B0.9600Ag1—S4ii2.4942 (14)
C3—H3C0.9600Ag1—S3ii2.5689 (14)
C4—H4A0.9600Ag1—S12.6206 (15)
C4—H4B0.9600Ag1—S22.6257 (16)
C4—H4C0.9600Ag1—W1ii2.9498 (6)
C5—H5A0.9600S3—Ag1i2.5689 (14)
C5—H5B0.9600S4—Ag1i2.4942 (14)
C5—H5C0.9600
O3—Ho1—O292.71 (12)N5—C5—H5C109.5
O3—Ho1—O488.84 (13)H5A—C5—H5C109.5
O2—Ho1—O4157.26 (12)H5B—C5—H5C109.5
O3—Ho1—O1158.06 (12)N5—C6—H6A109.5
O2—Ho1—O193.38 (12)N5—C6—H6B109.5
O4—Ho1—O193.58 (12)H6A—C6—H6B109.5
O3—Ho1—O8128.48 (12)N5—C6—H6C109.5
O2—Ho1—O880.02 (12)H6A—C6—H6C109.5
O4—Ho1—O881.28 (12)H6B—C6—H6C109.5
O1—Ho1—O873.39 (11)N6—C7—H7A109.5
O3—Ho1—O976.52 (12)N6—C7—H7B109.5
O2—Ho1—O978.06 (12)H7A—C7—H7B109.5
O4—Ho1—O980.26 (12)N6—C7—H7C109.5
O1—Ho1—O9125.39 (12)H7A—C7—H7C109.5
O8—Ho1—O952.01 (11)H7B—C7—H7C109.5
O3—Ho1—O579.12 (12)N6—C8—H8A109.5
O2—Ho1—O5127.18 (12)N6—C8—H8B109.5
O4—Ho1—O575.38 (12)H8A—C8—H8B109.5
O1—Ho1—O580.41 (12)N6—C8—H8C109.5
O8—Ho1—O5143.50 (11)H8A—C8—H8C109.5
O9—Ho1—O5145.65 (11)H8B—C8—H8C109.5
O3—Ho1—O679.85 (12)N7—C9—H9A109.5
O2—Ho1—O675.47 (11)N7—C9—H9B109.5
O4—Ho1—O6127.03 (12)H9A—C9—H9B109.5
O1—Ho1—O681.32 (11)N7—C9—H9C109.5
O8—Ho1—O6143.41 (11)H9A—C9—H9C109.5
O9—Ho1—O6143.34 (11)H9B—C9—H9C109.5
O5—Ho1—O651.71 (11)N7—C10—H10A109.5
O3—Ho1—N2102.51 (13)N7—C10—H10B109.5
O2—Ho1—N276.59 (12)H10A—C10—H10B109.5
O4—Ho1—N280.92 (13)N7—C10—H10C109.5
O1—Ho1—N299.41 (12)H10A—C10—H10C109.5
O8—Ho1—N226.07 (11)H10B—C10—H10C109.5
O9—Ho1—N225.99 (12)N8—C11—H11A109.5
O5—Ho1—N2156.22 (12)N8—C11—H11B109.5
O6—Ho1—N2152.04 (12)H11A—C11—H11B109.5
O3—Ho1—N175.99 (12)N8—C11—H11C109.5
O2—Ho1—N1101.25 (12)H11A—C11—H11C109.5
O4—Ho1—N1101.13 (12)H11B—C11—H11C109.5
O1—Ho1—N182.16 (12)N8—C12—H12A109.5
O8—Ho1—N1155.54 (11)N8—C12—H12B109.5
O9—Ho1—N1152.43 (12)H12A—C12—H12B109.5
O5—Ho1—N126.00 (11)N8—C12—H12C109.5
O6—Ho1—N125.91 (11)H12A—C12—H12C109.5
N2—Ho1—N1177.37 (13)H12B—C12—H12C109.5
O1—P1—N4108.9 (2)N9—C13—H13A109.5
O1—P1—N5117.1 (2)N9—C13—H13B109.5
N4—P1—N5103.4 (3)H13A—C13—H13B109.5
O1—P1—N3108.4 (2)N9—C13—H13C109.5
N4—P1—N3115.4 (3)H13A—C13—H13C109.5
N5—P1—N3103.9 (2)H13B—C13—H13C109.5
O2—P2—N8110.8 (2)N9—C14—H14A109.5
O2—P2—N6111.4 (2)N9—C14—H14B109.5
N8—P2—N6107.0 (3)H14A—C14—H14B109.5
O2—P2—N7108.4 (2)N9—C14—H14C109.5
N8—P2—N7109.7 (2)H14A—C14—H14C109.5
N6—P2—N7109.5 (2)H14B—C14—H14C109.5
O3—P3—N11111.1 (3)N10—C15—H15A109.5
O3—P3—N10109.8 (2)N10—C15—H15B109.5
N11—P3—N10108.5 (3)H15A—C15—H15B109.5
O3—P3—N9109.1 (3)N10—C15—H15C109.5
N11—P3—N9108.7 (3)H15A—C15—H15C109.5
N10—P3—N9109.5 (3)H15B—C15—H15C109.5
O4—P4—N13119.6 (2)N10—C16—H16A109.5
O4—P4—N12107.6 (2)N10—C16—H16B109.5
N13—P4—N12104.7 (3)H16A—C16—H16B109.5
O4—P4—N14108.0 (2)N10—C16—H16C109.5
N13—P4—N14102.7 (3)H16A—C16—H16C109.5
N12—P4—N14114.6 (3)H16B—C16—H16C109.5
P1—O1—Ho1161.2 (2)N11—C17—H17A109.5
P2—O2—Ho1167.9 (2)N11—C17—H17B109.5
P3—O3—Ho1167.3 (2)H17A—C17—H17B109.5
P4—O4—Ho1158.4 (2)N11—C17—H17C109.5
N1—O5—Ho195.6 (3)H17A—C17—H17C109.5
N1—O6—Ho195.7 (3)H17B—C17—H17C109.5
N2—O8—Ho196.0 (3)N11—C18—H18A109.5
N2—O9—Ho195.3 (3)N11—C18—H18B109.5
O7—N1—O6121.2 (4)H18A—C18—H18B109.5
O7—N1—O5122.6 (4)N11—C18—H18C109.5
O6—N1—O5116.1 (4)H18A—C18—H18C109.5
O7—N1—Ho1172.4 (4)H18B—C18—H18C109.5
O6—N1—Ho158.4 (2)N12—C19—H19A109.5
O5—N1—Ho158.4 (2)N12—C19—H19B109.5
O10—N2—O9122.3 (4)H19A—C19—H19B109.5
O10—N2—O8121.2 (5)N12—C19—H19C109.5
O9—N2—O8116.5 (4)H19A—C19—H19C109.5
O10—N2—Ho1174.9 (4)H19B—C19—H19C109.5
O9—N2—Ho158.7 (2)N12—C20—H20A109.5
O8—N2—Ho157.9 (2)N12—C20—H20B109.5
C1—N3—C2113.9 (5)H20A—C20—H20B109.5
C1—N3—P1119.9 (4)N12—C20—H20C109.5
C2—N3—P1120.5 (4)H20A—C20—H20C109.5
C3—N4—C4114.2 (5)H20B—C20—H20C109.5
C3—N4—P1120.6 (4)N13—C21—H21A109.5
C4—N4—P1120.8 (4)N13—C21—H21B109.5
C5—N5—C6110.0 (6)H21A—C21—H21B109.5
C5—N5—P1124.1 (4)N13—C21—H21C109.5
C6—N5—P1121.5 (4)H21A—C21—H21C109.5
C7—N6—C8114.0 (5)H21B—C21—H21C109.5
C7—N6—P2125.3 (4)N13—C22—H22A109.5
C8—N6—P2119.7 (4)N13—C22—H22B109.5
C9—N7—C10114.2 (4)H22A—C22—H22B109.5
C9—N7—P2122.5 (4)N13—C22—H22C109.5
C10—N7—P2119.9 (3)H22A—C22—H22C109.5
C12—N8—C11115.6 (6)H22B—C22—H22C109.5
C12—N8—P2120.0 (5)N14—C23—H23A109.5
C11—N8—P2123.4 (5)N14—C23—H23B109.5
C13—N9—C14112.9 (6)H23A—C23—H23B109.5
C13—N9—P3122.0 (4)N14—C23—H23C109.5
C14—N9—P3124.2 (6)H23A—C23—H23C109.5
C16—N10—C15114.3 (5)H23B—C23—H23C109.5
C16—N10—P3124.7 (4)N14—C24—H24A109.5
C15—N10—P3119.2 (4)N14—C24—H24B109.5
C17—N11—C18116.5 (7)H24A—C24—H24B109.5
C17—N11—P3119.7 (5)N14—C24—H24C109.5
C18—N11—P3123.8 (7)H24A—C24—H24C109.5
C19—N12—C20112.8 (5)H24B—C24—H24C109.5
C19—N12—P4122.2 (4)S2—W1—S1109.79 (5)
C20—N12—P4121.8 (4)S2—W1—S3108.15 (5)
C22—N13—C21113.2 (6)S1—W1—S3108.71 (5)
C22—N13—P4120.6 (5)S2—W1—S4108.28 (6)
C21—N13—P4123.0 (5)S1—W1—S4108.68 (5)
C24—N14—C23111.8 (5)S3—W1—S4113.21 (5)
C24—N14—P4121.0 (5)S2—W1—Ag1i125.57 (4)
C23—N14—P4119.6 (4)S1—W1—Ag1i124.63 (4)
N3—C1—H1A109.5S3—W1—Ag1i57.61 (4)
N3—C1—H1B109.5S4—W1—Ag1i55.61 (3)
H1A—C1—H1B109.5S2—W1—Ag158.81 (4)
N3—C1—H1C109.5S1—W1—Ag158.61 (4)
H1A—C1—H1C109.5S3—W1—Ag1148.78 (4)
H1B—C1—H1C109.5S4—W1—Ag198.01 (4)
N3—C2—H2A109.5Ag1i—W1—Ag1153.608 (10)
N3—C2—H2B109.5S4ii—Ag1—S3ii93.54 (4)
H2A—C2—H2B109.5S4ii—Ag1—S1121.32 (5)
N3—C2—H2C109.5S3ii—Ag1—S1120.05 (5)
H2A—C2—H2C109.5S4ii—Ag1—S2120.71 (5)
H2B—C2—H2C109.5S3ii—Ag1—S2117.52 (5)
N4—C3—H3A109.5S1—Ag1—S286.54 (4)
N4—C3—H3B109.5S4ii—Ag1—W1ii47.00 (3)
H3A—C3—H3B109.5S3ii—Ag1—W1ii46.55 (3)
N4—C3—H3C109.5S1—Ag1—W1ii137.47 (4)
H3A—C3—H3C109.5S2—Ag1—W1ii135.92 (4)
H3B—C3—H3C109.5S4ii—Ag1—W1151.54 (3)
N4—C4—H4A109.5S3ii—Ag1—W1114.88 (3)
N4—C4—H4B109.5S1—Ag1—W145.85 (3)
H4A—C4—H4B109.5S2—Ag1—W145.60 (3)
N4—C4—H4C109.5W1ii—Ag1—W1161.429 (17)
H4A—C4—H4C109.5W1—S1—Ag175.54 (4)
H4B—C4—H4C109.5W1—S2—Ag175.59 (4)
N5—C5—H5A109.5W1—S3—Ag1i75.84 (4)
N5—C5—H5B109.5W1—S4—Ag1i77.39 (4)
H5A—C5—H5B109.5
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2.

Experimental details

Crystal data
Chemical formula[Ho(NO3)2(C6H18N3OP)4][AgWS4]
Mr1425.76
Crystal system, space groupMonoclinic, P21/c
Temperature (K)173
a, b, c (Å)15.767 (3), 29.616 (6), 11.383 (2)
β (°) 90.88 (3)
V3)5314.7 (17)
Z4
Radiation typeMo Kα
µ (mm1)4.33
Crystal size (mm)0.18 × 0.15 × 0.1
Data collection
DiffractometerRigaku Mercury2
Absorption correctionMulti-scan
(CrystalClear; Rigaku, 2008)
Tmin, Tmax0.463, 0.648
No. of measured, independent and
observed [I > 2σ(I)] reflections
24559, 9655, 8942
Rint0.024
(sin θ/λ)max1)0.602
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.031, 0.073, 1.03
No. of reflections9655
No. of parameters532
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.030P)2 + 16.6944P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.87, 0.86

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

 

Acknowledgements

This work was supported by the Jiangsu Postdoctoral Foundation (grant No. 1001010c) and the funds from Jiangsu Province Education Office (serial number JH10–48).

References

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