metal-organic compounds
catena-Poly[[tetrakis(hexamethylphosphoramide-κO)bis(nitrato-κ2O,O′)erbium(III)] [silver(I)-di-μ-sulfido-tungstate(VI)-di-μ-sulfido]]
aInstitute of Molecular Engineering and Advanced Materials, School of Chemical Engineering, Nanjing University of Science and Technology, 200 Xiaolingwei, Nanjing 210094, Jiangsu, People's Republic of China, and bInstitute of Science and Technology, Jiangsu University, 301 Xuefu Road, Zhenjiang 212013, People's Republic of China
*Correspondence e-mail: chizhang@mail.njust.edu.cn
In the title compound, {[Er(NO3)2(C6H18N3OP)4][AgWS4]}n, the polymeric anionic chain {[AgWS4]−}n extends along [001]. The ErIII atom in the cation is coordinated by eight O atoms from two bidentate nitrate anions and four hexamethylphosphoramide ligands in a distorted square-antiprismatic geometry. Together with the two nitrate ligands, the cation is monovalent, which leads to the anionic chain having a [WS4Ag] repeat unit. The polymeric anionic chain has a distorted linear configuration, with W—Ag—W and Ag—W—Ag angles of 161.37 (2) and 153.548 (12)°, respectively. The title complex is isotypic with the Y, Yb, Eu, Nd, La, Dy, Sm, Lu and Tb analogues.
Related literature
For one-dimensional Mo(W)/S/Ag anionic polymers, see: Niu et al. (2004); Zhang et al. (2010). For their unique properties, see: Zhang, Song et al. (2007). 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); Zhang (2011a,b); Zhang (2012a,b).
Experimental
Crystal data
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Data collection: CrystalClear (Rigaku, 2008); cell CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Supporting information
https://doi.org/10.1107/S1600536812049987/rz5031sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812049987/rz5031Isup2.hkl
1 mmol AgI was added to a solution of [NH4]2WS4 (1 mmol in 10 ml hmp) with thorough stirring for 30 minutes. The solution underwent an additional stir for two minute after 0.5 mmol Er(NO3)3.6H2O was added. After filtration the orange filtrate was carefully laid on the surface with 15 ml i-PrOH. Orange block crystals were obtained after about one week.
H atoms were positioned geometrically and refined with riding model, with Uiso = 1.5Ueq(C) and 0.96 Å for C—H bonds.
One-dimensional Mo(W)/S/Ag anionic polymers have attracted much attention for their configurational
(Niu et al., 2004; Zhang, Meng et al., 2010) 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). The title compound, {[Er(hmp)4(NO3)2][WS4Ag]}n (hmp = hexamethylphosphoramide) with a wave-like anionic chain, was prepared by following such route using Er(III)-hmp complex as counterion.The title complex is isostructural with Y (Zhang, Cao et al., 2007; Zhang, 2011a), Yb (Cao et al., 2007), Eu (Zhang, Qian et al., 2007), Nd (Tang, Zhang & Zhang, 2008), La (Tang, Zhang, Zhang & Lu, 2008), Dy (Zhang, 2010), Sm (Zhang, 2011b), Lu (Zhang, 2012a) and Tb (Zhang, 2012b) isomorphs. ErIII in the cation is coordinated by eight O atoms from two nitrate and four hmp ligands. In possession of two nitrate ligands, the cation in the title compound is univalent (Fig. 1), which leads to an anionic chain with a univalent repeat unit. 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 161.37 (2) and 153.548 (12)°, respectively.
For one-dimensional Mo(W)/S/Ag anionic polymers, see: Niu et al. (2004); Zhang, Meng et al. (2010). For their unique properties, see: Zhang, Song et al. (2007). 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); Zhang (2011a,b); Zhang (2012a,b).
Data collection: CrystalClear (Rigaku, 2008); cell
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).[Er(NO3)2(C6H18N3OP)4][AgWS4] | F(000) = 2828 |
Mr = 1428.09 | Dx = 1.790 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 16527 reflections |
a = 15.763 (3) Å | θ = 3.2–29.1° |
b = 29.579 (6) Å | µ = 4.43 mm−1 |
c = 11.368 (2) Å | T = 150 K |
β = 90.83 (3)° | Block, orange |
V = 5299.8 (17) Å3 | 0.2 × 0.17 × 0.15 mm |
Z = 4 |
Rigaku Saturn724+ diffractometer | 9597 independent reflections |
Radiation source: fine-focus sealed tube | 8722 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
ω scans | θmax = 25.4°, θmin = 3.2° |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2008) | h = −15→18 |
Tmin = 0.428, Tmax = 0.514 | k = −35→33 |
26753 measured reflections | l = −13→11 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.092 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.024P)2 + 26.5377P] where P = (Fo2 + 2Fc2)/3 |
9597 reflections | (Δ/σ)max = 0.001 |
532 parameters | Δρmax = 0.91 e Å−3 |
0 restraints | Δρmin = −1.04 e Å−3 |
[Er(NO3)2(C6H18N3OP)4][AgWS4] | V = 5299.8 (17) Å3 |
Mr = 1428.09 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 15.763 (3) Å | µ = 4.43 mm−1 |
b = 29.579 (6) Å | T = 150 K |
c = 11.368 (2) Å | 0.2 × 0.17 × 0.15 mm |
β = 90.83 (3)° |
Rigaku Saturn724+ diffractometer | 9597 independent reflections |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2008) | 8722 reflections with I > 2σ(I) |
Tmin = 0.428, Tmax = 0.514 | Rint = 0.044 |
26753 measured reflections |
R[F2 > 2σ(F2)] = 0.047 | 0 restraints |
wR(F2) = 0.092 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.024P)2 + 26.5377P] where P = (Fo2 + 2Fc2)/3 |
9597 reflections | Δρmax = 0.91 e Å−3 |
532 parameters | Δρmin = −1.04 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Er1 | 0.261717 (18) | 0.082599 (10) | 0.17242 (3) | 0.02182 (9) | |
P1 | 0.30083 (12) | −0.03020 (6) | 0.29957 (18) | 0.0304 (4) | |
P2 | 0.47743 (11) | 0.13250 (6) | 0.17898 (17) | 0.0283 (4) | |
P3 | 0.20599 (14) | 0.14671 (7) | −0.09571 (19) | 0.0396 (5) | |
P4 | 0.04219 (11) | 0.09630 (6) | 0.26880 (18) | 0.0301 (4) | |
O1 | 0.2929 (3) | 0.01824 (14) | 0.2704 (4) | 0.0286 (11) | |
O2 | 0.3962 (3) | 0.10679 (15) | 0.1766 (4) | 0.0270 (11) | |
O3 | 0.2272 (3) | 0.12660 (16) | 0.0203 (4) | 0.0332 (12) | |
O4 | 0.1247 (3) | 0.08070 (15) | 0.2201 (5) | 0.0314 (12) | |
O5 | 0.1983 (3) | 0.02697 (16) | 0.0365 (5) | 0.0333 (12) | |
O6 | 0.3308 (3) | 0.04094 (15) | 0.0120 (4) | 0.0309 (11) | |
O7 | 0.2627 (4) | 0.00150 (19) | −0.1184 (5) | 0.0517 (16) | |
O8 | 0.2475 (3) | 0.15793 (16) | 0.2617 (5) | 0.0355 (12) | |
O9 | 0.2759 (3) | 0.10278 (16) | 0.3788 (4) | 0.0326 (12) | |
O10 | 0.2730 (5) | 0.1713 (2) | 0.4458 (6) | 0.0662 (19) | |
N1 | 0.2634 (4) | 0.0222 (2) | −0.0254 (6) | 0.0325 (14) | |
N2 | 0.2654 (4) | 0.1450 (2) | 0.3649 (6) | 0.0387 (16) | |
N3 | 0.2788 (4) | −0.0367 (2) | 0.4396 (5) | 0.0369 (15) | |
N4 | 0.2357 (5) | −0.0654 (2) | 0.2322 (6) | 0.0455 (18) | |
N5 | 0.3945 (4) | −0.0479 (2) | 0.2606 (6) | 0.0471 (18) | |
N6 | 0.4773 (4) | 0.1728 (2) | 0.0807 (7) | 0.0453 (18) | |
N7 | 0.5551 (3) | 0.0976 (2) | 0.1525 (5) | 0.0321 (14) | |
N8 | 0.4928 (4) | 0.1561 (3) | 0.3049 (6) | 0.0478 (18) | |
N9 | 0.1046 (5) | 0.1388 (3) | −0.1233 (8) | 0.072 (3) | |
N10 | 0.2258 (5) | 0.2001 (2) | −0.0937 (6) | 0.051 (2) | |
N11 | 0.2596 (6) | 0.1239 (3) | −0.1975 (7) | 0.063 (2) | |
N12 | −0.0330 (4) | 0.0706 (2) | 0.1969 (6) | 0.0448 (18) | |
N13 | 0.0175 (4) | 0.1493 (2) | 0.2613 (7) | 0.0478 (18) | |
N14 | 0.0442 (4) | 0.0864 (2) | 0.4119 (6) | 0.0444 (17) | |
C1 | 0.2737 (6) | −0.0824 (3) | 0.4912 (8) | 0.055 (2) | |
H1A | 0.2610 | −0.0801 | 0.5733 | 0.082* | |
H1B | 0.3269 | −0.0977 | 0.4821 | 0.082* | |
H1C | 0.2297 | −0.0993 | 0.4518 | 0.082* | |
C2 | 0.3022 (6) | −0.0022 (3) | 0.5231 (8) | 0.054 (2) | |
H2A | 0.2852 | −0.0113 | 0.6003 | 0.081* | |
H2B | 0.2744 | 0.0256 | 0.5022 | 0.081* | |
H2C | 0.3626 | 0.0021 | 0.5224 | 0.081* | |
C3 | 0.2467 (7) | −0.0811 (3) | 0.1146 (10) | 0.076 (3) | |
H3A | 0.2009 | −0.1011 | 0.0934 | 0.114* | |
H3B | 0.2996 | −0.0971 | 0.1096 | 0.114* | |
H3C | 0.2471 | −0.0558 | 0.0618 | 0.114* | |
C4 | 0.1460 (6) | −0.0679 (4) | 0.2662 (11) | 0.084 (4) | |
H4A | 0.1171 | −0.0898 | 0.2179 | 0.126* | |
H4B | 0.1200 | −0.0388 | 0.2554 | 0.126* | |
H4C | 0.1426 | −0.0766 | 0.3473 | 0.126* | |
C5 | 0.4648 (5) | −0.0170 (3) | 0.2516 (9) | 0.060 (3) | |
H5A | 0.5145 | −0.0333 | 0.2284 | 0.089* | |
H5B | 0.4751 | −0.0029 | 0.3265 | 0.089* | |
H5C | 0.4516 | 0.0057 | 0.1939 | 0.089* | |
C6 | 0.4187 (7) | −0.0955 (3) | 0.2793 (10) | 0.077 (3) | |
H6A | 0.4756 | −0.1002 | 0.2528 | 0.115* | |
H6B | 0.3805 | −0.1148 | 0.2358 | 0.115* | |
H6C | 0.4157 | −0.1026 | 0.3615 | 0.115* | |
C7 | 0.5461 (6) | 0.1830 (3) | 0.0021 (9) | 0.060 (3) | |
H7A | 0.5306 | 0.2081 | −0.0470 | 0.090* | |
H7B | 0.5573 | 0.1571 | −0.0462 | 0.090* | |
H7C | 0.5960 | 0.1904 | 0.0474 | 0.090* | |
C8 | 0.4101 (6) | 0.2069 (3) | 0.0814 (10) | 0.069 (3) | |
H8A | 0.4190 | 0.2281 | 0.0189 | 0.103* | |
H8B | 0.4111 | 0.2225 | 0.1555 | 0.103* | |
H8C | 0.3561 | 0.1924 | 0.0703 | 0.103* | |
C9 | 0.6430 (5) | 0.1065 (3) | 0.1885 (8) | 0.052 (2) | |
H9A | 0.6784 | 0.0820 | 0.1639 | 0.078* | |
H9B | 0.6464 | 0.1094 | 0.2726 | 0.078* | |
H9C | 0.6619 | 0.1341 | 0.1528 | 0.078* | |
C10 | 0.5464 (5) | 0.0644 (3) | 0.0569 (7) | 0.0403 (19) | |
H10A | 0.5972 | 0.0466 | 0.0527 | 0.060* | |
H10B | 0.5372 | 0.0799 | −0.0164 | 0.060* | |
H10C | 0.4989 | 0.0450 | 0.0719 | 0.060* | |
C11 | 0.5348 (6) | 0.2001 (4) | 0.3221 (10) | 0.085 (4) | |
H11A | 0.5376 | 0.2070 | 0.4045 | 0.127* | |
H11B | 0.5031 | 0.2231 | 0.2814 | 0.127* | |
H11C | 0.5912 | 0.1987 | 0.2915 | 0.127* | |
C12 | 0.4797 (6) | 0.1309 (5) | 0.4108 (9) | 0.085 (4) | |
H12A | 0.4919 | 0.1498 | 0.4777 | 0.127* | |
H12B | 0.5167 | 0.1051 | 0.4123 | 0.127* | |
H12C | 0.4218 | 0.1210 | 0.4133 | 0.127* | |
C13 | 0.0645 (7) | 0.0960 (4) | −0.1105 (11) | 0.082 (4) | |
H13A | 0.0056 | 0.0985 | −0.1321 | 0.124* | |
H13B | 0.0695 | 0.0862 | −0.0302 | 0.124* | |
H13C | 0.0913 | 0.0743 | −0.1606 | 0.124* | |
C14 | 0.0490 (8) | 0.1713 (4) | −0.1835 (11) | 0.099 (5) | |
H14A | −0.0070 | 0.1587 | −0.1911 | 0.148* | |
H14B | 0.0707 | 0.1777 | −0.2601 | 0.148* | |
H14C | 0.0467 | 0.1987 | −0.1385 | 0.148* | |
C15 | 0.1981 (6) | 0.2275 (3) | 0.0056 (7) | 0.049 (2) | |
H15A | 0.2141 | 0.2584 | −0.0068 | 0.073* | |
H15B | 0.2244 | 0.2166 | 0.0768 | 0.073* | |
H15C | 0.1375 | 0.2255 | 0.0120 | 0.073* | |
C16 | 0.2511 (9) | 0.2258 (4) | −0.1981 (9) | 0.092 (4) | |
H16A | 0.2589 | 0.2570 | −0.1773 | 0.137* | |
H16B | 0.2077 | 0.2234 | −0.2579 | 0.137* | |
H16C | 0.3033 | 0.2138 | −0.2275 | 0.137* | |
C17 | 0.3500 (7) | 0.1209 (4) | −0.1868 (9) | 0.078 (3) | |
H17A | 0.3722 | 0.1064 | −0.2554 | 0.116* | |
H17B | 0.3648 | 0.1035 | −0.1183 | 0.116* | |
H17C | 0.3735 | 0.1507 | −0.1796 | 0.116* | |
C18 | 0.2210 (11) | 0.1070 (5) | −0.3088 (9) | 0.127 (6) | |
H18A | 0.2645 | 0.0948 | −0.3577 | 0.190* | |
H18B | 0.1932 | 0.1315 | −0.3492 | 0.190* | |
H18C | 0.1803 | 0.0839 | −0.2916 | 0.190* | |
C19 | −0.0203 (5) | 0.0279 (3) | 0.1385 (10) | 0.067 (3) | |
H19A | −0.0725 | 0.0184 | 0.1013 | 0.100* | |
H19B | −0.0028 | 0.0056 | 0.1953 | 0.100* | |
H19C | 0.0227 | 0.0311 | 0.0803 | 0.100* | |
C20 | −0.1227 (5) | 0.0803 (4) | 0.2196 (11) | 0.084 (4) | |
H20A | −0.1578 | 0.0618 | 0.1693 | 0.126* | |
H20B | −0.1341 | 0.1116 | 0.2040 | 0.126* | |
H20C | −0.1347 | 0.0737 | 0.3003 | 0.126* | |
C21 | 0.0485 (6) | 0.1832 (3) | 0.3428 (12) | 0.085 (4) | |
H21A | 0.0259 | 0.2122 | 0.3211 | 0.127* | |
H21B | 0.1093 | 0.1842 | 0.3405 | 0.127* | |
H21C | 0.0309 | 0.1757 | 0.4209 | 0.127* | |
C22 | −0.0138 (8) | 0.1691 (4) | 0.1509 (10) | 0.092 (4) | |
H22A | −0.0252 | 0.2007 | 0.1623 | 0.138* | |
H22B | −0.0651 | 0.1540 | 0.1266 | 0.138* | |
H22C | 0.0282 | 0.1655 | 0.0913 | 0.138* | |
C23 | 0.0923 (5) | 0.0480 (3) | 0.4562 (8) | 0.053 (2) | |
H23A | 0.0877 | 0.0466 | 0.5403 | 0.079* | |
H23B | 0.1509 | 0.0514 | 0.4358 | 0.079* | |
H23C | 0.0703 | 0.0207 | 0.4220 | 0.079* | |
C24 | −0.0291 (7) | 0.0965 (4) | 0.4838 (9) | 0.085 (4) | |
H24A | −0.0169 | 0.0887 | 0.5642 | 0.127* | |
H24B | −0.0771 | 0.0794 | 0.4559 | 0.127* | |
H24C | −0.0418 | 0.1282 | 0.4787 | 0.127* | |
W1 | 0.783523 (17) | 0.227488 (9) | 0.52651 (2) | 0.02184 (8) | |
Ag1 | 0.78222 (4) | 0.26566 (2) | 0.28700 (5) | 0.03871 (16) | |
S1 | 0.78533 (12) | 0.18464 (6) | 0.36793 (16) | 0.0312 (4) | |
S2 | 0.78321 (13) | 0.30066 (6) | 0.48679 (17) | 0.0361 (5) | |
S3 | 0.66880 (12) | 0.21148 (7) | 0.62708 (17) | 0.0353 (4) | |
S4 | 0.89701 (12) | 0.21219 (7) | 0.63272 (17) | 0.0382 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Er1 | 0.01984 (16) | 0.01636 (16) | 0.02925 (18) | 0.00031 (11) | 0.00027 (13) | 0.00062 (13) |
P1 | 0.0344 (10) | 0.0222 (10) | 0.0347 (11) | 0.0047 (8) | 0.0069 (9) | 0.0060 (8) |
P2 | 0.0217 (9) | 0.0340 (11) | 0.0293 (10) | −0.0055 (8) | −0.0002 (8) | −0.0064 (8) |
P3 | 0.0588 (14) | 0.0271 (11) | 0.0324 (11) | 0.0096 (9) | −0.0183 (10) | −0.0012 (9) |
P4 | 0.0204 (9) | 0.0275 (10) | 0.0425 (12) | 0.0011 (7) | 0.0024 (8) | −0.0075 (9) |
O1 | 0.037 (3) | 0.016 (2) | 0.033 (3) | 0.003 (2) | 0.001 (2) | 0.002 (2) |
O2 | 0.023 (2) | 0.025 (3) | 0.033 (3) | 0.0008 (19) | 0.001 (2) | 0.001 (2) |
O3 | 0.033 (3) | 0.030 (3) | 0.036 (3) | 0.000 (2) | −0.005 (2) | 0.005 (2) |
O4 | 0.023 (2) | 0.026 (3) | 0.045 (3) | 0.003 (2) | 0.004 (2) | −0.004 (2) |
O5 | 0.026 (3) | 0.026 (3) | 0.048 (3) | 0.002 (2) | −0.004 (2) | −0.007 (2) |
O6 | 0.024 (3) | 0.028 (3) | 0.040 (3) | 0.000 (2) | 0.003 (2) | −0.002 (2) |
O7 | 0.056 (4) | 0.051 (4) | 0.048 (4) | 0.004 (3) | −0.005 (3) | −0.026 (3) |
O8 | 0.038 (3) | 0.025 (3) | 0.043 (3) | 0.004 (2) | −0.001 (3) | 0.000 (2) |
O9 | 0.044 (3) | 0.023 (3) | 0.032 (3) | 0.001 (2) | 0.005 (2) | 0.001 (2) |
O10 | 0.100 (5) | 0.045 (4) | 0.053 (4) | 0.018 (4) | −0.009 (4) | −0.020 (3) |
N1 | 0.027 (3) | 0.031 (3) | 0.039 (4) | 0.003 (3) | −0.005 (3) | −0.007 (3) |
N2 | 0.047 (4) | 0.029 (4) | 0.040 (4) | 0.005 (3) | −0.001 (3) | −0.009 (3) |
N3 | 0.052 (4) | 0.029 (3) | 0.030 (4) | 0.005 (3) | 0.006 (3) | 0.005 (3) |
N4 | 0.059 (5) | 0.025 (3) | 0.054 (5) | −0.009 (3) | 0.024 (4) | −0.007 (3) |
N5 | 0.043 (4) | 0.043 (4) | 0.056 (5) | 0.019 (3) | 0.015 (3) | 0.021 (4) |
N6 | 0.037 (4) | 0.036 (4) | 0.064 (5) | −0.004 (3) | 0.014 (3) | 0.013 (3) |
N7 | 0.020 (3) | 0.045 (4) | 0.031 (3) | 0.001 (3) | 0.001 (3) | −0.003 (3) |
N8 | 0.036 (4) | 0.069 (5) | 0.039 (4) | 0.000 (3) | −0.003 (3) | −0.022 (4) |
N9 | 0.072 (6) | 0.043 (5) | 0.101 (7) | 0.019 (4) | −0.055 (5) | 0.000 (5) |
N10 | 0.092 (6) | 0.030 (4) | 0.033 (4) | 0.012 (4) | 0.002 (4) | 0.011 (3) |
N11 | 0.092 (6) | 0.049 (5) | 0.049 (5) | 0.025 (4) | 0.003 (5) | −0.009 (4) |
N12 | 0.023 (3) | 0.053 (4) | 0.058 (5) | 0.000 (3) | 0.006 (3) | −0.032 (4) |
N13 | 0.039 (4) | 0.034 (4) | 0.070 (5) | 0.003 (3) | 0.009 (4) | −0.010 (4) |
N14 | 0.037 (4) | 0.058 (5) | 0.038 (4) | 0.010 (3) | 0.000 (3) | −0.004 (3) |
C1 | 0.067 (6) | 0.040 (5) | 0.057 (6) | 0.015 (4) | 0.020 (5) | 0.024 (4) |
C2 | 0.067 (6) | 0.053 (6) | 0.042 (5) | 0.009 (5) | −0.001 (5) | 0.013 (5) |
C3 | 0.097 (8) | 0.055 (6) | 0.077 (8) | −0.023 (6) | 0.010 (7) | −0.030 (6) |
C4 | 0.062 (7) | 0.086 (8) | 0.104 (10) | −0.018 (6) | 0.003 (7) | −0.033 (7) |
C5 | 0.034 (5) | 0.059 (6) | 0.086 (8) | 0.003 (4) | −0.010 (5) | −0.008 (6) |
C6 | 0.091 (8) | 0.057 (6) | 0.083 (8) | 0.038 (6) | 0.035 (6) | 0.025 (6) |
C7 | 0.060 (6) | 0.049 (6) | 0.072 (7) | −0.021 (5) | 0.026 (5) | 0.008 (5) |
C8 | 0.069 (7) | 0.035 (5) | 0.103 (9) | −0.004 (5) | 0.018 (6) | 0.022 (5) |
C9 | 0.034 (5) | 0.072 (6) | 0.050 (6) | 0.005 (4) | −0.004 (4) | −0.011 (5) |
C10 | 0.030 (4) | 0.054 (5) | 0.036 (5) | −0.002 (4) | 0.010 (3) | −0.013 (4) |
C11 | 0.061 (7) | 0.091 (8) | 0.102 (9) | −0.002 (6) | −0.024 (6) | −0.070 (8) |
C12 | 0.052 (6) | 0.160 (12) | 0.043 (6) | 0.016 (7) | −0.011 (5) | −0.003 (7) |
C13 | 0.068 (7) | 0.062 (7) | 0.116 (10) | 0.001 (6) | −0.045 (7) | −0.012 (7) |
C14 | 0.111 (10) | 0.074 (8) | 0.108 (10) | 0.036 (7) | −0.065 (8) | −0.002 (7) |
C15 | 0.077 (6) | 0.026 (4) | 0.043 (5) | 0.009 (4) | 0.010 (5) | −0.001 (4) |
C16 | 0.172 (13) | 0.057 (7) | 0.047 (7) | 0.024 (7) | 0.034 (7) | 0.022 (5) |
C17 | 0.100 (9) | 0.075 (7) | 0.059 (7) | 0.034 (7) | 0.035 (6) | 0.008 (6) |
C18 | 0.217 (17) | 0.130 (12) | 0.034 (6) | −0.022 (12) | 0.002 (8) | −0.046 (7) |
C19 | 0.035 (5) | 0.064 (6) | 0.101 (9) | −0.005 (4) | 0.005 (5) | −0.042 (6) |
C20 | 0.029 (5) | 0.110 (9) | 0.114 (10) | 0.001 (5) | 0.003 (5) | −0.076 (8) |
C21 | 0.052 (6) | 0.037 (5) | 0.165 (13) | −0.011 (4) | 0.029 (7) | −0.049 (7) |
C22 | 0.103 (9) | 0.083 (8) | 0.091 (9) | 0.058 (7) | 0.031 (7) | 0.037 (7) |
C23 | 0.040 (5) | 0.078 (7) | 0.040 (5) | −0.002 (5) | 0.002 (4) | 0.005 (5) |
C24 | 0.069 (7) | 0.128 (10) | 0.058 (7) | 0.045 (7) | 0.019 (6) | −0.012 (7) |
W1 | 0.02715 (16) | 0.02019 (15) | 0.01811 (15) | 0.00253 (11) | −0.00214 (11) | −0.00094 (11) |
Ag1 | 0.0607 (4) | 0.0356 (3) | 0.0198 (3) | 0.0003 (3) | −0.0010 (3) | 0.0023 (2) |
S1 | 0.0455 (11) | 0.0234 (9) | 0.0246 (9) | −0.0004 (8) | 0.0008 (8) | −0.0048 (7) |
S2 | 0.0564 (13) | 0.0218 (9) | 0.0301 (10) | 0.0037 (8) | 0.0015 (9) | −0.0032 (8) |
S3 | 0.0301 (10) | 0.0457 (12) | 0.0301 (10) | −0.0059 (8) | 0.0016 (8) | −0.0020 (9) |
S4 | 0.0353 (11) | 0.0491 (12) | 0.0300 (10) | 0.0155 (9) | −0.0064 (9) | −0.0044 (9) |
Er1—O3 | 2.225 (5) | C6—H6A | 0.9600 |
Er1—O4 | 2.235 (5) | C6—H6B | 0.9600 |
Er1—O2 | 2.237 (4) | C6—H6C | 0.9600 |
Er1—O1 | 2.256 (4) | C7—H7A | 0.9600 |
Er1—O9 | 2.428 (5) | C7—H7B | 0.9600 |
Er1—O5 | 2.460 (5) | C7—H7C | 0.9600 |
Er1—O8 | 2.460 (5) | C8—H8A | 0.9600 |
Er1—O6 | 2.468 (5) | C8—H8B | 0.9600 |
Er1—N2 | 2.863 (6) | C8—H8C | 0.9600 |
Er1—N1 | 2.872 (6) | C9—H9A | 0.9600 |
P1—O1 | 1.476 (5) | C9—H9B | 0.9600 |
P1—N5 | 1.634 (7) | C9—H9C | 0.9600 |
P1—N4 | 1.644 (7) | C10—H10A | 0.9600 |
P1—N3 | 1.646 (6) | C10—H10B | 0.9600 |
P2—O2 | 1.489 (5) | C10—H10C | 0.9600 |
P2—N8 | 1.609 (7) | C11—H11A | 0.9600 |
P2—N7 | 1.634 (6) | C11—H11B | 0.9600 |
P2—N6 | 1.633 (7) | C11—H11C | 0.9600 |
P3—O3 | 1.481 (5) | C12—H12A | 0.9600 |
P3—N11 | 1.593 (8) | C12—H12B | 0.9600 |
P3—N10 | 1.610 (7) | C12—H12C | 0.9600 |
P3—N9 | 1.640 (8) | C13—H13A | 0.9600 |
P4—O4 | 1.494 (5) | C13—H13B | 0.9600 |
P4—N13 | 1.619 (7) | C13—H13C | 0.9600 |
P4—N12 | 1.620 (6) | C14—H14A | 0.9600 |
P4—N14 | 1.653 (7) | C14—H14B | 0.9600 |
O5—N1 | 1.260 (8) | C14—H14C | 0.9600 |
O6—N1 | 1.266 (7) | C15—H15A | 0.9600 |
O7—N1 | 1.223 (8) | C15—H15B | 0.9600 |
O8—N2 | 1.262 (8) | C15—H15C | 0.9600 |
O9—N2 | 1.269 (8) | C16—H16A | 0.9600 |
O10—N2 | 1.208 (8) | C16—H16B | 0.9600 |
N3—C2 | 1.438 (10) | C16—H16C | 0.9600 |
N3—C1 | 1.476 (9) | C17—H17A | 0.9600 |
N4—C3 | 1.429 (12) | C17—H17B | 0.9600 |
N4—C4 | 1.472 (12) | C17—H17C | 0.9600 |
N5—C5 | 1.442 (11) | C18—H18A | 0.9600 |
N5—C6 | 1.473 (11) | C18—H18B | 0.9600 |
N6—C7 | 1.446 (10) | C18—H18C | 0.9600 |
N6—C8 | 1.462 (11) | C19—H19A | 0.9600 |
N7—C9 | 1.463 (9) | C19—H19B | 0.9600 |
N7—C10 | 1.470 (9) | C19—H19C | 0.9600 |
N8—C12 | 1.433 (13) | C20—H20A | 0.9600 |
N8—C11 | 1.470 (12) | C20—H20B | 0.9600 |
N9—C13 | 1.425 (12) | C20—H20C | 0.9600 |
N9—C14 | 1.464 (11) | C21—H21A | 0.9600 |
N10—C15 | 1.461 (10) | C21—H21B | 0.9600 |
N10—C16 | 1.471 (11) | C21—H21C | 0.9600 |
N11—C17 | 1.430 (13) | C22—H22A | 0.9600 |
N11—C18 | 1.482 (12) | C22—H22B | 0.9600 |
N12—C19 | 1.444 (10) | C22—H22C | 0.9600 |
N12—C20 | 1.468 (10) | C23—H23A | 0.9600 |
N13—C21 | 1.445 (11) | C23—H23B | 0.9600 |
N13—C22 | 1.463 (12) | C23—H23C | 0.9600 |
N14—C23 | 1.450 (10) | C24—H24A | 0.9600 |
N14—C24 | 1.457 (11) | C24—H24B | 0.9600 |
C1—H1A | 0.9600 | C24—H24C | 0.9600 |
C1—H1B | 0.9600 | W1—S4 | 2.1909 (19) |
C1—H1C | 0.9600 | W1—S1 | 2.2043 (18) |
C2—H2A | 0.9600 | W1—S3 | 2.205 (2) |
C2—H2B | 0.9600 | W1—S2 | 2.2108 (19) |
C2—H2C | 0.9600 | W1—Ag1 | 2.9474 (8) |
C3—H3A | 0.9600 | W1—Ag1i | 2.9685 (8) |
C3—H3B | 0.9600 | Ag1—S2 | 2.496 (2) |
C3—H3C | 0.9600 | Ag1—S1 | 2.5674 (19) |
C4—H4A | 0.9600 | Ag1—S3ii | 2.620 (2) |
C4—H4B | 0.9600 | Ag1—S4ii | 2.621 (2) |
C4—H4C | 0.9600 | Ag1—W1ii | 2.9685 (8) |
C5—H5A | 0.9600 | S3—Ag1i | 2.620 (2) |
C5—H5B | 0.9600 | S4—Ag1i | 2.621 (2) |
C5—H5C | 0.9600 | ||
O3—Er1—O4 | 88.67 (18) | N5—C5—H5C | 109.5 |
O3—Er1—O2 | 92.88 (17) | H5A—C5—H5C | 109.5 |
O4—Er1—O2 | 157.15 (17) | H5B—C5—H5C | 109.5 |
O3—Er1—O1 | 157.85 (17) | N5—C6—H6A | 109.5 |
O4—Er1—O1 | 93.63 (17) | N5—C6—H6B | 109.5 |
O2—Er1—O1 | 93.44 (16) | H6A—C6—H6B | 109.5 |
O3—Er1—O9 | 128.68 (17) | N5—C6—H6C | 109.5 |
O4—Er1—O9 | 81.22 (17) | H6A—C6—H6C | 109.5 |
O2—Er1—O9 | 80.05 (17) | H6B—C6—H6C | 109.5 |
O1—Er1—O9 | 73.38 (16) | N6—C7—H7A | 109.5 |
O3—Er1—O5 | 79.08 (17) | N6—C7—H7B | 109.5 |
O4—Er1—O5 | 75.53 (17) | H7A—C7—H7B | 109.5 |
O2—Er1—O5 | 127.14 (17) | N6—C7—H7C | 109.5 |
O1—Er1—O5 | 80.18 (16) | H7A—C7—H7C | 109.5 |
O9—Er1—O5 | 143.35 (17) | H7B—C7—H7C | 109.5 |
O3—Er1—O8 | 76.60 (18) | N6—C8—H8A | 109.5 |
O4—Er1—O8 | 80.12 (17) | N6—C8—H8B | 109.5 |
O2—Er1—O8 | 78.09 (16) | H8A—C8—H8B | 109.5 |
O1—Er1—O8 | 125.51 (17) | N6—C8—H8C | 109.5 |
O9—Er1—O8 | 52.13 (16) | H8A—C8—H8C | 109.5 |
O5—Er1—O8 | 145.74 (16) | H8B—C8—H8C | 109.5 |
O3—Er1—O6 | 79.83 (17) | N7—C9—H9A | 109.5 |
O4—Er1—O6 | 127.23 (16) | N7—C9—H9B | 109.5 |
O2—Er1—O6 | 75.36 (16) | H9A—C9—H9B | 109.5 |
O1—Er1—O6 | 81.28 (16) | N7—C9—H9C | 109.5 |
O9—Er1—O6 | 143.29 (16) | H9A—C9—H9C | 109.5 |
O5—Er1—O6 | 51.78 (16) | H9B—C9—H9C | 109.5 |
O8—Er1—O6 | 143.25 (17) | N7—C10—H10A | 109.5 |
O3—Er1—N2 | 102.64 (19) | N7—C10—H10B | 109.5 |
O4—Er1—N2 | 80.79 (18) | H10A—C10—H10B | 109.5 |
O2—Er1—N2 | 76.62 (18) | N7—C10—H10C | 109.5 |
O1—Er1—N2 | 99.48 (18) | H10A—C10—H10C | 109.5 |
O9—Er1—N2 | 26.14 (17) | H10B—C10—H10C | 109.5 |
O5—Er1—N2 | 156.23 (18) | N8—C11—H11A | 109.5 |
O8—Er1—N2 | 26.05 (17) | N8—C11—H11B | 109.5 |
O6—Er1—N2 | 151.96 (17) | H11A—C11—H11B | 109.5 |
O3—Er1—N1 | 76.12 (18) | N8—C11—H11C | 109.5 |
O4—Er1—N1 | 101.18 (17) | H11A—C11—H11C | 109.5 |
O2—Er1—N1 | 101.32 (17) | H11B—C11—H11C | 109.5 |
O1—Er1—N1 | 81.82 (17) | N8—C12—H12A | 109.5 |
O9—Er1—N1 | 155.20 (16) | N8—C12—H12B | 109.5 |
O5—Er1—N1 | 25.89 (16) | H12A—C12—H12B | 109.5 |
O8—Er1—N1 | 152.64 (18) | N8—C12—H12C | 109.5 |
O6—Er1—N1 | 26.06 (15) | H12A—C12—H12C | 109.5 |
N2—Er1—N1 | 177.59 (19) | H12B—C12—H12C | 109.5 |
O1—P1—N5 | 109.0 (3) | N9—C13—H13A | 109.5 |
O1—P1—N4 | 117.4 (3) | N9—C13—H13B | 109.5 |
N5—P1—N4 | 103.4 (4) | H13A—C13—H13B | 109.5 |
O1—P1—N3 | 108.2 (3) | N9—C13—H13C | 109.5 |
N5—P1—N3 | 115.4 (3) | H13A—C13—H13C | 109.5 |
N4—P1—N3 | 103.7 (3) | H13B—C13—H13C | 109.5 |
O2—P2—N8 | 110.9 (3) | N9—C14—H14A | 109.5 |
O2—P2—N7 | 108.7 (3) | N9—C14—H14B | 109.5 |
N8—P2—N7 | 109.6 (3) | H14A—C14—H14B | 109.5 |
O2—P2—N6 | 111.6 (3) | N9—C14—H14C | 109.5 |
N8—P2—N6 | 106.9 (4) | H14A—C14—H14C | 109.5 |
N7—P2—N6 | 109.2 (3) | H14B—C14—H14C | 109.5 |
O3—P3—N11 | 111.2 (4) | N10—C15—H15A | 109.5 |
O3—P3—N10 | 109.9 (3) | N10—C15—H15B | 109.5 |
N11—P3—N10 | 108.8 (4) | H15A—C15—H15B | 109.5 |
O3—P3—N9 | 108.7 (4) | N10—C15—H15C | 109.5 |
N11—P3—N9 | 109.0 (5) | H15A—C15—H15C | 109.5 |
N10—P3—N9 | 109.3 (4) | H15B—C15—H15C | 109.5 |
O4—P4—N13 | 119.4 (3) | N10—C16—H16A | 109.5 |
O4—P4—N12 | 107.6 (3) | N10—C16—H16B | 109.5 |
N13—P4—N12 | 104.7 (4) | H16A—C16—H16B | 109.5 |
O4—P4—N14 | 107.8 (3) | N10—C16—H16C | 109.5 |
N13—P4—N14 | 103.0 (4) | H16A—C16—H16C | 109.5 |
N12—P4—N14 | 114.7 (4) | H16B—C16—H16C | 109.5 |
P1—O1—Er1 | 161.3 (3) | N11—C17—H17A | 109.5 |
P2—O2—Er1 | 168.0 (3) | N11—C17—H17B | 109.5 |
P3—O3—Er1 | 167.6 (3) | H17A—C17—H17B | 109.5 |
P4—O4—Er1 | 158.7 (3) | N11—C17—H17C | 109.5 |
N1—O5—Er1 | 95.6 (4) | H17A—C17—H17C | 109.5 |
N1—O6—Er1 | 95.1 (4) | H17B—C17—H17C | 109.5 |
N2—O8—Er1 | 95.1 (4) | N11—C18—H18A | 109.5 |
N2—O9—Er1 | 96.4 (4) | N11—C18—H18B | 109.5 |
O7—N1—O5 | 122.8 (6) | H18A—C18—H18B | 109.5 |
O7—N1—O6 | 120.4 (6) | N11—C18—H18C | 109.5 |
O5—N1—O6 | 116.8 (6) | H18A—C18—H18C | 109.5 |
O7—N1—Er1 | 171.6 (5) | H18B—C18—H18C | 109.5 |
O5—N1—Er1 | 58.5 (3) | N12—C19—H19A | 109.5 |
O6—N1—Er1 | 58.9 (3) | N12—C19—H19B | 109.5 |
O10—N2—O8 | 122.1 (7) | H19A—C19—H19B | 109.5 |
O10—N2—O9 | 121.8 (7) | N12—C19—H19C | 109.5 |
O8—N2—O9 | 116.1 (6) | H19A—C19—H19C | 109.5 |
O10—N2—Er1 | 175.5 (6) | H19B—C19—H19C | 109.5 |
O8—N2—Er1 | 58.9 (3) | N12—C20—H20A | 109.5 |
O9—N2—Er1 | 57.4 (3) | N12—C20—H20B | 109.5 |
C2—N3—C1 | 113.8 (7) | H20A—C20—H20B | 109.5 |
C2—N3—P1 | 120.0 (5) | N12—C20—H20C | 109.5 |
C1—N3—P1 | 120.3 (5) | H20A—C20—H20C | 109.5 |
C3—N4—C4 | 111.1 (8) | H20B—C20—H20C | 109.5 |
C3—N4—P1 | 123.9 (6) | N13—C21—H21A | 109.5 |
C4—N4—P1 | 120.3 (6) | N13—C21—H21B | 109.5 |
C5—N5—C6 | 114.7 (7) | H21A—C21—H21B | 109.5 |
C5—N5—P1 | 120.9 (6) | N13—C21—H21C | 109.5 |
C6—N5—P1 | 120.1 (6) | H21A—C21—H21C | 109.5 |
C7—N6—C8 | 114.2 (7) | H21B—C21—H21C | 109.5 |
C7—N6—P2 | 125.5 (6) | N13—C22—H22A | 109.5 |
C8—N6—P2 | 119.5 (6) | N13—C22—H22B | 109.5 |
C9—N7—C10 | 114.0 (6) | H22A—C22—H22B | 109.5 |
C9—N7—P2 | 122.9 (5) | N13—C22—H22C | 109.5 |
C10—N7—P2 | 119.7 (5) | H22A—C22—H22C | 109.5 |
C12—N8—C11 | 114.8 (8) | H22B—C22—H22C | 109.5 |
C12—N8—P2 | 120.0 (7) | N14—C23—H23A | 109.5 |
C11—N8—P2 | 124.3 (7) | N14—C23—H23B | 109.5 |
C13—N9—C14 | 111.5 (8) | H23A—C23—H23B | 109.5 |
C13—N9—P3 | 122.7 (6) | N14—C23—H23C | 109.5 |
C14—N9—P3 | 124.9 (8) | H23A—C23—H23C | 109.5 |
C15—N10—C16 | 115.1 (7) | H23B—C23—H23C | 109.5 |
C15—N10—P3 | 119.7 (6) | N14—C24—H24A | 109.5 |
C16—N10—P3 | 123.4 (7) | N14—C24—H24B | 109.5 |
C17—N11—C18 | 116.6 (9) | H24A—C24—H24B | 109.5 |
C17—N11—P3 | 120.2 (7) | N14—C24—H24C | 109.5 |
C18—N11—P3 | 123.2 (9) | H24A—C24—H24C | 109.5 |
C19—N12—C20 | 113.0 (6) | H24B—C24—H24C | 109.5 |
C19—N12—P4 | 122.5 (5) | S4—W1—S1 | 108.17 (7) |
C20—N12—P4 | 121.3 (5) | S4—W1—S3 | 109.83 (8) |
C21—N13—C22 | 112.4 (8) | S1—W1—S3 | 108.72 (7) |
C21—N13—P4 | 124.0 (7) | S4—W1—S2 | 108.30 (8) |
C22—N13—P4 | 120.7 (7) | S1—W1—S2 | 113.32 (7) |
C23—N14—C24 | 112.4 (8) | S3—W1—S2 | 108.46 (8) |
C23—N14—P4 | 118.9 (6) | S4—W1—Ag1 | 125.65 (6) |
C24—N14—P4 | 120.7 (6) | S1—W1—Ag1 | 57.64 (5) |
N3—C1—H1A | 109.5 | S3—W1—Ag1 | 124.50 (6) |
N3—C1—H1B | 109.5 | S2—W1—Ag1 | 55.69 (5) |
H1A—C1—H1B | 109.5 | S4—W1—Ag1i | 58.79 (6) |
N3—C1—H1C | 109.5 | S1—W1—Ag1i | 148.81 (5) |
H1A—C1—H1C | 109.5 | S3—W1—Ag1i | 58.66 (5) |
H1B—C1—H1C | 109.5 | S2—W1—Ag1i | 97.87 (5) |
N3—C2—H2A | 109.5 | Ag1—W1—Ag1i | 153.548 (12) |
N3—C2—H2B | 109.5 | S2—Ag1—S1 | 93.51 (6) |
H2A—C2—H2B | 109.5 | S2—Ag1—S3ii | 121.31 (7) |
N3—C2—H2C | 109.5 | S1—Ag1—S3ii | 119.92 (6) |
H2A—C2—H2C | 109.5 | S2—Ag1—S4ii | 120.66 (7) |
H2B—C2—H2C | 109.5 | S1—Ag1—S4ii | 117.59 (7) |
N4—C3—H3A | 109.5 | S3ii—Ag1—S4ii | 86.67 (6) |
N4—C3—H3B | 109.5 | S2—Ag1—W1 | 47.03 (5) |
H3A—C3—H3B | 109.5 | S1—Ag1—W1 | 46.49 (4) |
N4—C3—H3C | 109.5 | S3ii—Ag1—W1 | 137.34 (5) |
H3A—C3—H3C | 109.5 | S4ii—Ag1—W1 | 135.90 (5) |
H3B—C3—H3C | 109.5 | S2—Ag1—W1ii | 151.57 (5) |
N4—C4—H4A | 109.5 | S1—Ag1—W1ii | 114.89 (5) |
N4—C4—H4B | 109.5 | S3ii—Ag1—W1ii | 45.95 (5) |
H4A—C4—H4B | 109.5 | S4ii—Ag1—W1ii | 45.63 (4) |
N4—C4—H4C | 109.5 | W1—Ag1—W1ii | 161.37 (2) |
H4A—C4—H4C | 109.5 | W1—S1—Ag1 | 75.87 (6) |
H4B—C4—H4C | 109.5 | W1—S2—Ag1 | 77.28 (6) |
N5—C5—H5A | 109.5 | W1—S3—Ag1i | 75.39 (6) |
N5—C5—H5B | 109.5 | W1—S4—Ag1i | 75.59 (6) |
H5A—C5—H5B | 109.5 |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, −y+1/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Er(NO3)2(C6H18N3OP)4][AgWS4] |
Mr | 1428.09 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 150 |
a, b, c (Å) | 15.763 (3), 29.579 (6), 11.368 (2) |
β (°) | 90.83 (3) |
V (Å3) | 5299.8 (17) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 4.43 |
Crystal size (mm) | 0.2 × 0.17 × 0.15 |
Data collection | |
Diffractometer | Rigaku Saturn724+ |
Absorption correction | Multi-scan (CrystalClear; Rigaku, 2008) |
Tmin, Tmax | 0.428, 0.514 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 26753, 9597, 8722 |
Rint | 0.044 |
(sin θ/λ)max (Å−1) | 0.603 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.047, 0.092, 1.08 |
No. of reflections | 9597 |
No. of parameters | 532 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.024P)2 + 26.5377P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.91, −1.04 |
Computer programs: CrystalClear (Rigaku, 2008), SHELXTL (Sheldrick, 2008).
Acknowledgements
This work was supported by the National Natural Science Foundation of China (No. 50472048) and the Program for New Century Excellent Talents in Universities (NCET-05–0499).
References
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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
One-dimensional Mo(W)/S/Ag anionic polymers have attracted much attention for their configurational isomerism (Niu et al., 2004; Zhang, Meng et al., 2010) 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). The title compound, {[Er(hmp)4(NO3)2][WS4Ag]}n (hmp = hexamethylphosphoramide) with a wave-like anionic chain, was prepared by following such route using Er(III)-hmp complex as counterion.
The title complex is isostructural with Y (Zhang, Cao et al., 2007; Zhang, 2011a), Yb (Cao et al., 2007), Eu (Zhang, Qian et al., 2007), Nd (Tang, Zhang & Zhang, 2008), La (Tang, Zhang, Zhang & Lu, 2008), Dy (Zhang, 2010), Sm (Zhang, 2011b), Lu (Zhang, 2012a) and Tb (Zhang, 2012b) isomorphs. ErIII in the cation is coordinated by eight O atoms from two nitrate and four hmp ligands. In possession of two nitrate ligands, the cation in the title compound is univalent (Fig. 1), which leads to an anionic chain with a univalent repeat unit. 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 161.37 (2) and 153.548 (12)°, respectively.