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

Zhang, J.

doi:10.1107/S1600536810042728

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 66| Part 11| November 2010| Page m1479

https://doi.org/10.1107/S1600536810042728

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

Jinfang Zhang ^a ^*

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

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

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

Related literature

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

Experimental

Crystal data

[Dy(NO₃)₂(C₆H₁₈N₃OP)₄][AgMoS₄]
M_r = 1335.43
Monoclinic, P 2₁ /c
a = 15.786 (3) Å
b = 29.671 (6) Å
c = 11.331 (2) Å
β = 90.93 (3)°
V = 5306.6 (17) Å³
Z = 4
Mo Kα radiation
μ = 2.33 mm⁻¹
T = 153 K
0.35 × 0.25 × 0.18 mm

Data collection

Rigaku Saturn724+ diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku, 2008 ) T_min = 0.503, T_max = 0.658
25288 measured reflections
10445 independent reflections
9394 reflections with I > 2σ(I)
R_int = 0.023

Refinement

R[F² > 2σ(F²)] = 0.032
wR(F²) = 0.074
S = 1.05
10445 reflections
556 parameters
H-atom parameters constrained
Δρ_max = 1.00 e Å⁻³
Δρ_min = −1.00 e Å⁻³

Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810042728/pv2340sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810042728/pv2340Isup2.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 unique properties as functional materials, such as third-order nonlinear optical (NLO) materials (Zhang et al., 2007). Different solvent-coordinated rare-earth cations proved effective to obtain various configurations of anionic chains (Niu et al., 2004). The title compound {[Dy(hmp)₄(NO₃)₂][MoS₄Ag]}_n (hmp = hexamethylphosphoramide) with a wave-like anionic chain was prepared by following such route using Dy(III)-hmp complex as counterion.

The title complex is isostructural with W isomorph (Wei et al., 2010). Dy^3- in the cation is coordinated by eight O atoms from two nitrate and four hmp ligands. In possession of two nitrate ligands, the cation in the title compound is univalent (Fig. 1), which leads to an anionic chain with a univalent repeat unit. The anionic chain in the title compound has a distorted linear configuration with Mo—Ag—Mo and Ag—Mo—Ag angles of 161.911 (13) and 154.014 (13) °, respectively (Fig. 2).

Related literature top

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

Experimental top

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

Structure description top

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

Computing details top

Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear (Rigaku, 2008); data reduction: CrystalClear (Rigaku, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	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.
	Fig. 2. The molecular structure of a portion of the anionic chain in the title compound, with atom labels and 30% probability displacement ellipsoids, Symmetry code: (i) x, 1/2 - y, -1/2 + z.

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

Crystal data top

[Dy(NO₃)₂(C₆H₁₈N₃OP)₄][AgMoS₄]	F(000) = 2692
M_r = 1335.43	D_x = 1.672 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 22208 reflections
a = 15.786 (3) Å	θ = 2.7–29.1°
b = 29.671 (6) Å	µ = 2.33 mm⁻¹
c = 11.331 (2) Å	T = 153 K
β = 90.93 (3)°	Block, black-red
V = 5306.6 (17) Å³	0.35 × 0.25 × 0.18 mm
Z = 4

Data collection top

Rigaku Saturn724+ diffractometer	10445 independent reflections
Radiation source: fine-focus sealed tube	9394 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.023
dtprofit.ref scans	θ_max = 26.0°, θ_min = 2.7°
Absorption correction: multi-scan (CrystalClear; Rigaku, 2008)	h = −19→19
T_min = 0.503, T_max = 0.658	k = −29→36
25288 measured reflections	l = −13→11

Refinement top

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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.074	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0305P)² + 8.9291P] where P = (F_o² + 2F_c²)/3
10445 reflections	(Δ/σ)_max = 0.002
556 parameters	Δρ_max = 1.00 e Å⁻³
0 restraints	Δρ_min = −1.00 e Å⁻³

Crystal data top

[Dy(NO₃)₂(C₆H₁₈N₃OP)₄][AgMoS₄]	V = 5306.6 (17) Å³
M_r = 1335.43	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 15.786 (3) Å	µ = 2.33 mm⁻¹
b = 29.671 (6) Å	T = 153 K
c = 11.331 (2) Å	0.35 × 0.25 × 0.18 mm
β = 90.93 (3)°

Data collection top

Rigaku Saturn724+ diffractometer	10445 independent reflections
Absorption correction: multi-scan (CrystalClear; Rigaku, 2008)	9394 reflections with I > 2σ(I)
T_min = 0.503, T_max = 0.658	R_int = 0.023
25288 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	0 restraints
wR(F²) = 0.074	H-atom parameters constrained
S = 1.05	Δρ_max = 1.00 e Å⁻³
10445 reflections	Δρ_min = −1.00 e Å⁻³
556 parameters

Special details top

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

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Dy1	0.737719 (10)	0.082623 (5)	0.827853 (15)	0.01950 (5)
P1	0.52135 (6)	0.13298 (3)	0.82207 (9)	0.0266 (2)
P2	0.69790 (7)	−0.03042 (3)	0.69823 (9)	0.0289 (2)
P3	0.95845 (6)	0.09627 (3)	0.73131 (10)	0.0283 (2)
P4	0.79428 (8)	0.14677 (4)	1.09803 (10)	0.0402 (3)
O1	0.60267 (15)	0.10717 (8)	0.8236 (2)	0.0274 (6)
O2	0.70672 (16)	0.01805 (8)	0.7283 (2)	0.0286 (6)
O3	0.87595 (15)	0.08051 (8)	0.7800 (2)	0.0298 (6)
O4	0.77256 (16)	0.12686 (8)	0.9820 (2)	0.0300 (6)
O5	0.80099 (16)	0.02668 (9)	0.9669 (2)	0.0321 (6)
O6	0.66868 (16)	0.04088 (9)	0.9901 (2)	0.0311 (6)
O7	0.75133 (17)	0.15817 (8)	0.7373 (2)	0.0331 (6)
O8	0.72330 (18)	0.10333 (9)	0.6184 (2)	0.0326 (6)
O9	0.7368 (2)	0.00134 (11)	1.1224 (3)	0.0496 (8)
O10	0.7251 (3)	0.17185 (11)	0.5514 (3)	0.0670 (11)
N1	0.44407 (19)	0.09830 (12)	0.8493 (3)	0.0319 (7)
N2	0.5226 (2)	0.17305 (12)	0.9216 (4)	0.0427 (9)
N3	0.5055 (2)	0.15715 (15)	0.6955 (3)	0.0495 (10)
N4	0.7203 (2)	−0.03716 (11)	0.5583 (3)	0.0367 (8)
N5	0.6051 (2)	−0.04792 (13)	0.7374 (4)	0.0522 (11)
N6	0.7637 (3)	−0.06553 (12)	0.7669 (3)	0.0468 (10)
N7	1.0342 (2)	0.07053 (13)	0.8029 (3)	0.0414 (9)
N8	0.9831 (2)	0.14915 (12)	0.7387 (4)	0.0458 (10)
N9	0.9562 (2)	0.08656 (14)	0.5884 (3)	0.0466 (10)
N10	0.8965 (3)	0.13862 (15)	1.1254 (5)	0.0758 (16)
N11	0.7738 (3)	0.20013 (12)	1.0971 (3)	0.0533 (11)
N12	0.7402 (4)	0.12385 (16)	1.2004 (4)	0.0725 (15)
N13	0.7356 (2)	0.02235 (10)	1.0295 (3)	0.0310 (7)
N14	0.7330 (2)	0.14538 (11)	0.6336 (3)	0.0359 (8)
C1	0.3560 (2)	0.10709 (18)	0.8134 (4)	0.0465 (12)
H1A	0.3296	0.0794	0.7889	0.070*
H1B	0.3548	0.1281	0.7491	0.070*
H1C	0.3259	0.1195	0.8789	0.070*
C2	0.4534 (3)	0.06453 (15)	0.9437 (4)	0.0402 (10)
H2A	0.4317	0.0766	1.0159	0.060*
H2B	0.5122	0.0571	0.9545	0.060*
H2C	0.4223	0.0379	0.9224	0.060*
C3	0.4539 (3)	0.18330 (17)	1.0017 (5)	0.0557 (13)
H3A	0.4769	0.1892	1.0791	0.084*
H3B	0.4159	0.1581	1.0050	0.084*
H3C	0.4237	0.2094	0.9737	0.084*
C4	0.5898 (3)	0.20739 (17)	0.9192 (6)	0.0673 (17)
H4A	0.5676	0.2348	0.8859	0.101*
H4B	0.6357	0.1968	0.8720	0.101*
H4C	0.6101	0.2130	0.9982	0.101*
C5	0.4640 (4)	0.2012 (2)	0.6806 (6)	0.084 (2)
H5A	0.5023	0.2218	0.6437	0.127*
H5B	0.4485	0.2127	0.7564	0.127*
H5C	0.4141	0.1978	0.6319	0.127*
C6	0.5176 (4)	0.1322 (3)	0.5889 (5)	0.086 (2)
H6A	0.4638	0.1274	0.5502	0.128*
H6B	0.5430	0.1036	0.6073	0.128*
H6C	0.5539	0.1489	0.5376	0.128*
C7	0.7262 (3)	−0.08241 (15)	0.5065 (4)	0.0511 (13)
H7A	0.6722	−0.0908	0.4732	0.077*
H7B	0.7424	−0.1036	0.5667	0.077*
H7C	0.7679	−0.0823	0.4457	0.077*
C8	0.6988 (3)	−0.00220 (17)	0.4730 (4)	0.0520 (13)
H8A	0.7392	−0.0024	0.4107	0.078*
H8B	0.6996	0.0266	0.5114	0.078*
H8C	0.6432	−0.0078	0.4407	0.078*
C9	0.5347 (3)	−0.01677 (19)	0.7464 (6)	0.0659 (16)
H9A	0.5057	−0.0147	0.6714	0.099*
H9B	0.5555	0.0124	0.7689	0.099*
H9C	0.4961	−0.0275	0.8047	0.099*
C10	0.5811 (4)	−0.0960 (2)	0.7209 (6)	0.083 (2)
H10A	0.5437	−0.1050	0.7826	0.124*
H10B	0.6311	−0.1144	0.7237	0.124*
H10C	0.5529	−0.0997	0.6458	0.124*
C11	0.7531 (5)	−0.08082 (19)	0.8861 (6)	0.0775 (19)
H11A	0.7570	−0.1131	0.8885	0.116*
H11B	0.6986	−0.0716	0.9136	0.116*
H11C	0.7967	−0.0680	0.9358	0.116*
C12	0.8532 (4)	−0.0681 (2)	0.7337 (6)	0.084 (2)
H12A	0.8873	−0.0522	0.7909	0.126*
H12B	0.8601	−0.0546	0.6574	0.126*
H12C	0.8705	−0.0991	0.7309	0.126*
C13	1.1235 (3)	0.0808 (2)	0.7837 (6)	0.077 (2)
H13A	1.1532	0.0817	0.8583	0.116*
H13B	1.1282	0.1095	0.7453	0.116*
H13C	1.1478	0.0578	0.7349	0.116*
C14	1.0206 (3)	0.02790 (17)	0.8615 (5)	0.0635 (16)
H14A	1.0337	0.0037	0.8086	0.095*
H14B	0.9624	0.0257	0.8843	0.095*
H14C	1.0566	0.0260	0.9304	0.095*
C15	0.9514 (3)	0.18288 (18)	0.6533 (7)	0.086 (2)
H15A	0.9078	0.2006	0.6890	0.129*
H15B	0.9286	0.1678	0.5849	0.129*
H15C	0.9971	0.2022	0.6305	0.129*
C16	1.0139 (4)	0.1688 (2)	0.8498 (6)	0.085 (2)
H16A	1.0576	0.1903	0.8338	0.127*
H16B	1.0365	0.1454	0.8997	0.127*
H16C	0.9680	0.1835	0.8888	0.127*
C17	0.9077 (3)	0.04800 (19)	0.5440 (4)	0.0566 (14)
H17A	0.8956	0.0520	0.4614	0.085*
H17B	0.8556	0.0457	0.5860	0.085*
H17C	0.9402	0.0209	0.5554	0.085*
C18	1.0304 (4)	0.0961 (2)	0.5161 (5)	0.0771 (19)
H18A	1.0707	0.0721	0.5246	0.116*
H18B	1.0559	0.1239	0.5416	0.116*
H18C	1.0130	0.0987	0.4348	0.116*
C19	0.9354 (4)	0.0953 (2)	1.1108 (7)	0.086 (2)
H19A	0.9904	0.0990	1.0771	0.129*
H19B	0.9007	0.0770	1.0593	0.129*
H19C	0.9411	0.0807	1.1862	0.129*
C20	0.9515 (5)	0.1716 (3)	1.1851 (7)	0.110 (3)
H20A	0.9491	0.1672	1.2689	0.166*
H20B	0.9328	0.2015	1.1657	0.166*
H20C	1.0087	0.1676	1.1596	0.166*
C21	0.8026 (4)	0.22745 (14)	0.9966 (4)	0.0508 (13)
H21A	0.7646	0.2523	0.9844	0.076*
H21B	0.8035	0.2091	0.9268	0.076*
H21C	0.8586	0.2387	1.0133	0.076*
C22	0.7481 (6)	0.22620 (19)	1.2004 (5)	0.095 (3)
H22A	0.7955	0.2433	1.2299	0.142*
H22B	0.7290	0.2060	1.2607	0.142*
H22C	0.7029	0.2463	1.1782	0.142*
C23	0.6502 (5)	0.1210 (2)	1.1891 (6)	0.092 (2)
H23A	0.6327	0.0903	1.1994	0.138*
H23B	0.6328	0.1313	1.1121	0.138*
H23C	0.6246	0.1395	1.2481	0.138*
C24	0.7796 (7)	0.1055 (3)	1.3091 (6)	0.129 (4)
H24A	0.7501	0.1167	1.3764	0.194*
H24B	0.8378	0.1147	1.3139	0.194*
H24C	0.7764	0.0732	1.3076	0.194*
Mo1	0.215792 (19)	0.271918 (10)	−0.02476 (3)	0.02053 (8)
Ag1	0.21712 (2)	0.234959 (11)	0.21455 (3)	0.03744 (9)
S1	0.21612 (7)	0.19909 (3)	0.01654 (9)	0.0339 (2)
S2	0.21379 (7)	0.31529 (3)	0.13294 (8)	0.0300 (2)
S3	0.10204 (6)	0.28647 (4)	−0.13144 (9)	0.0363 (2)
S4	0.33020 (6)	0.28755 (4)	−0.12530 (9)	0.0346 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Dy1	0.01679 (9)	0.01407 (8)	0.02766 (10)	−0.00034 (6)	0.00165 (7)	−0.00080 (7)
P1	0.0199 (5)	0.0323 (5)	0.0277 (5)	0.0048 (4)	0.0007 (4)	0.0059 (4)
P2	0.0360 (5)	0.0195 (5)	0.0315 (5)	−0.0072 (4)	0.0106 (4)	−0.0066 (4)
P3	0.0175 (4)	0.0257 (5)	0.0419 (6)	−0.0010 (4)	0.0043 (4)	0.0074 (4)
P4	0.0615 (8)	0.0249 (5)	0.0336 (6)	−0.0103 (5)	−0.0192 (6)	0.0016 (5)
O1	0.0196 (12)	0.0274 (13)	0.0354 (15)	0.0040 (11)	0.0013 (11)	−0.0020 (12)
O2	0.0334 (14)	0.0196 (13)	0.0328 (14)	−0.0018 (11)	0.0014 (12)	−0.0056 (11)
O3	0.0189 (12)	0.0253 (13)	0.0452 (17)	−0.0004 (11)	0.0044 (12)	0.0057 (12)
O4	0.0337 (14)	0.0222 (13)	0.0338 (15)	−0.0012 (11)	−0.0065 (12)	−0.0053 (11)
O5	0.0253 (14)	0.0268 (14)	0.0442 (16)	0.0009 (11)	−0.0002 (12)	0.0056 (12)
O6	0.0225 (13)	0.0307 (14)	0.0402 (16)	0.0006 (11)	0.0003 (12)	0.0064 (12)
O7	0.0391 (16)	0.0206 (13)	0.0396 (16)	−0.0052 (12)	−0.0016 (13)	0.0007 (12)
O8	0.0412 (16)	0.0237 (14)	0.0332 (15)	−0.0043 (12)	0.0073 (13)	−0.0005 (12)
O9	0.055 (2)	0.052 (2)	0.0415 (18)	−0.0042 (16)	−0.0014 (15)	0.0248 (16)
O10	0.111 (3)	0.0411 (19)	0.049 (2)	−0.017 (2)	−0.014 (2)	0.0219 (17)
N1	0.0194 (15)	0.045 (2)	0.0317 (18)	0.0004 (15)	0.0010 (14)	0.0059 (16)
N2	0.0351 (19)	0.0321 (19)	0.061 (2)	0.0031 (16)	0.0133 (18)	−0.0101 (18)
N3	0.034 (2)	0.076 (3)	0.038 (2)	−0.002 (2)	−0.0073 (17)	0.026 (2)
N4	0.051 (2)	0.0295 (18)	0.0295 (18)	−0.0046 (16)	0.0091 (16)	−0.0066 (15)
N5	0.046 (2)	0.047 (2)	0.064 (3)	−0.0217 (19)	0.018 (2)	−0.023 (2)
N6	0.072 (3)	0.0254 (18)	0.043 (2)	0.0060 (19)	0.014 (2)	0.0037 (17)
N7	0.0219 (17)	0.051 (2)	0.051 (2)	0.0029 (16)	0.0028 (16)	0.0282 (19)
N8	0.034 (2)	0.0281 (19)	0.075 (3)	−0.0016 (16)	0.0096 (19)	0.0091 (19)
N9	0.0308 (19)	0.068 (3)	0.041 (2)	−0.0083 (18)	0.0069 (17)	0.0096 (19)
N10	0.081 (3)	0.046 (3)	0.098 (4)	−0.016 (2)	−0.058 (3)	−0.004 (3)
N11	0.104 (4)	0.0243 (18)	0.031 (2)	−0.010 (2)	0.002 (2)	−0.0090 (16)
N12	0.118 (4)	0.055 (3)	0.044 (3)	−0.033 (3)	−0.004 (3)	0.013 (2)
N13	0.0316 (18)	0.0231 (16)	0.0383 (19)	−0.0052 (14)	−0.0022 (15)	0.0013 (15)
N14	0.040 (2)	0.0271 (18)	0.041 (2)	−0.0042 (15)	0.0057 (17)	0.0062 (16)
C1	0.021 (2)	0.071 (3)	0.047 (3)	0.002 (2)	−0.0017 (19)	0.012 (2)
C2	0.035 (2)	0.044 (2)	0.042 (2)	−0.002 (2)	0.0052 (19)	0.013 (2)
C3	0.053 (3)	0.048 (3)	0.066 (3)	0.014 (2)	0.021 (3)	−0.010 (3)
C4	0.058 (3)	0.044 (3)	0.100 (5)	−0.008 (3)	0.019 (3)	−0.023 (3)
C5	0.060 (4)	0.089 (5)	0.104 (5)	0.014 (3)	−0.014 (3)	0.064 (4)
C6	0.059 (4)	0.166 (7)	0.032 (3)	−0.022 (4)	−0.008 (3)	0.001 (4)
C7	0.070 (3)	0.039 (3)	0.045 (3)	−0.007 (2)	0.021 (3)	−0.019 (2)
C8	0.069 (3)	0.052 (3)	0.036 (3)	−0.003 (3)	−0.008 (2)	0.000 (2)
C9	0.031 (3)	0.068 (4)	0.098 (5)	−0.001 (3)	−0.007 (3)	0.016 (3)
C10	0.096 (5)	0.069 (4)	0.086 (4)	−0.049 (4)	0.041 (4)	−0.034 (3)
C11	0.106 (5)	0.056 (4)	0.071 (4)	0.025 (3)	0.010 (4)	0.022 (3)
C12	0.058 (4)	0.090 (5)	0.103 (5)	0.019 (3)	0.005 (4)	0.026 (4)
C13	0.020 (2)	0.112 (5)	0.098 (5)	0.004 (3)	0.005 (3)	0.066 (4)
C14	0.036 (3)	0.055 (3)	0.100 (4)	0.007 (2)	0.009 (3)	0.044 (3)
C15	0.049 (3)	0.046 (3)	0.164 (7)	0.002 (3)	0.011 (4)	0.052 (4)
C16	0.104 (5)	0.062 (4)	0.089 (5)	−0.041 (4)	0.033 (4)	−0.020 (3)
C17	0.044 (3)	0.077 (4)	0.048 (3)	−0.004 (3)	0.003 (2)	−0.014 (3)
C18	0.058 (3)	0.125 (6)	0.049 (3)	−0.026 (4)	0.018 (3)	0.008 (3)
C19	0.061 (4)	0.067 (4)	0.128 (6)	−0.003 (3)	−0.046 (4)	0.014 (4)
C20	0.114 (6)	0.095 (5)	0.120 (6)	−0.044 (5)	−0.073 (5)	0.004 (5)
C21	0.081 (4)	0.027 (2)	0.044 (3)	−0.003 (2)	0.002 (3)	−0.004 (2)
C22	0.190 (8)	0.049 (3)	0.046 (3)	−0.029 (4)	0.025 (4)	−0.022 (3)
C23	0.118 (6)	0.087 (5)	0.074 (4)	−0.041 (4)	0.053 (4)	−0.009 (4)
C24	0.223 (11)	0.113 (7)	0.052 (4)	0.018 (7)	0.011 (5)	0.043 (4)
Mo1	0.02501 (16)	0.02009 (15)	0.01645 (15)	0.00239 (12)	−0.00122 (12)	−0.00120 (12)
Ag1	0.0581 (2)	0.03582 (17)	0.01837 (15)	0.00052 (15)	−0.00063 (14)	0.00160 (12)
S1	0.0556 (7)	0.0198 (4)	0.0263 (5)	0.0047 (4)	0.0004 (5)	−0.0027 (4)
S2	0.0447 (6)	0.0226 (4)	0.0228 (5)	−0.0001 (4)	0.0013 (4)	−0.0054 (4)
S3	0.0304 (5)	0.0506 (6)	0.0278 (5)	0.0131 (5)	−0.0062 (4)	−0.0032 (5)
S4	0.0299 (5)	0.0467 (6)	0.0272 (5)	−0.0055 (5)	0.0024 (4)	−0.0028 (5)

Geometric parameters (Å, º) top

Dy1—O4	2.246 (3)	C6—H6A	0.9600
Dy1—O1	2.253 (2)	C6—H6B	0.9600
Dy1—O3	2.258 (2)	C6—H6C	0.9600
Dy1—O2	2.273 (2)	C7—H7A	0.9600
Dy1—O8	2.459 (3)	C7—H7B	0.9600
Dy1—O7	2.476 (3)	C7—H7C	0.9600
Dy1—O6	2.483 (3)	C8—H8A	0.9600
Dy1—O5	2.487 (3)	C8—H8B	0.9600
Dy1—N14	2.883 (3)	C8—H8C	0.9600
Dy1—N13	2.902 (3)	C9—H9A	0.9600
P1—O1	1.495 (3)	C9—H9B	0.9600
P1—N3	1.619 (4)	C9—H9C	0.9600
P1—N1	1.629 (3)	C10—H10A	0.9600
P1—N2	1.639 (4)	C10—H10B	0.9600
P2—O2	1.484 (3)	C10—H10C	0.9600
P2—N5	1.622 (4)	C11—H11A	0.9600
P2—N4	1.642 (3)	C11—H11B	0.9600
P2—N6	1.657 (4)	C11—H11C	0.9600
P3—O3	1.498 (3)	C12—H12A	0.9600
P3—N8	1.618 (4)	C12—H12B	0.9600
P3—N7	1.625 (3)	C12—H12C	0.9600
P3—N9	1.644 (4)	C13—H13A	0.9600
P4—O4	1.476 (3)	C13—H13B	0.9600
P4—N12	1.603 (5)	C13—H13C	0.9600
P4—N11	1.616 (4)	C14—H14A	0.9600
P4—N10	1.656 (5)	C14—H14B	0.9600
O5—N13	1.268 (4)	C14—H14C	0.9600
O6—N13	1.266 (4)	C15—H15A	0.9600
O7—N14	1.264 (4)	C15—H15B	0.9600
O8—N14	1.268 (4)	C15—H15C	0.9600
O9—N13	1.223 (4)	C16—H16A	0.9600
O10—N14	1.223 (4)	C16—H16B	0.9600
N1—C1	1.466 (5)	C16—H16C	0.9600
N1—C2	1.472 (5)	C17—H17A	0.9600
N2—C3	1.457 (5)	C17—H17B	0.9600
N2—C4	1.472 (6)	C17—H17C	0.9600
N3—C6	1.433 (7)	C18—H18A	0.9600
N3—C5	1.471 (7)	C18—H18B	0.9600
N4—C8	1.454 (6)	C18—H18C	0.9600
N4—C7	1.469 (5)	C19—H19A	0.9600
N5—C9	1.451 (6)	C19—H19B	0.9600
N5—C10	1.488 (6)	C19—H19C	0.9600
N6—C11	1.437 (7)	C20—H20A	0.9600
N6—C12	1.469 (7)	C20—H20B	0.9600
N7—C14	1.446 (5)	C20—H20C	0.9600
N7—C13	1.463 (5)	C21—H21A	0.9600
N8—C16	1.463 (7)	C21—H21B	0.9600
N8—C15	1.474 (6)	C21—H21C	0.9600
N9—C17	1.461 (6)	C22—H22A	0.9600
N9—C18	1.467 (6)	C22—H22B	0.9600
N10—C19	1.437 (8)	C22—H22C	0.9600
N10—C20	1.465 (7)	C23—H23A	0.9600
N11—C22	1.466 (6)	C23—H23B	0.9600
N11—C21	1.475 (6)	C23—H23C	0.9600
N12—C23	1.427 (8)	C24—H24A	0.9600
N12—C24	1.474 (8)	C24—H24B	0.9600
C1—H1A	0.9600	C24—H24C	0.9600
C1—H1B	0.9600	Mo1—S3	2.1912 (12)
C1—H1C	0.9600	Mo1—S4	2.2003 (12)
C2—H2A	0.9600	Mo1—S2	2.2027 (10)
C2—H2B	0.9600	Mo1—S1	2.2110 (11)
C2—H2C	0.9600	Mo1—Ag1	2.9247 (6)
C3—H3A	0.9600	Mo1—Ag1ⁱ	2.9614 (7)
C3—H3B	0.9600	Ag1—S1	2.4830 (11)
C3—H3C	0.9600	Ag1—S2	2.5569 (11)
C4—H4A	0.9600	Ag1—S4ⁱⁱ	2.6116 (13)
C4—H4B	0.9600	Ag1—S3ⁱⁱ	2.6178 (13)
C4—H4C	0.9600	Ag1—Mo1ⁱⁱ	2.9614 (7)
C5—H5A	0.9600	S3—Ag1ⁱ	2.6178 (13)
C5—H5B	0.9600	S4—Ag1ⁱ	2.6116 (13)
C5—H5C	0.9600

O4—Dy1—O1	92.72 (9)	N3—C5—H5C	109.5
O4—Dy1—O3	88.71 (10)	H5A—C5—H5C	109.5
O1—Dy1—O3	157.20 (9)	H5B—C5—H5C	109.5
O4—Dy1—O2	157.93 (9)	N3—C6—H6A	109.5
O1—Dy1—O2	93.77 (9)	N3—C6—H6B	109.5
O3—Dy1—O2	93.36 (9)	H6A—C6—H6B	109.5
O4—Dy1—O8	128.49 (9)	N3—C6—H6C	109.5
O1—Dy1—O8	79.97 (10)	H6A—C6—H6C	109.5
O3—Dy1—O8	81.37 (10)	H6B—C6—H6C	109.5
O2—Dy1—O8	73.47 (9)	N4—C7—H7A	109.5
O4—Dy1—O7	76.79 (9)	N4—C7—H7B	109.5
O1—Dy1—O7	77.70 (9)	H7A—C7—H7B	109.5
O3—Dy1—O7	80.50 (9)	N4—C7—H7C	109.5
O2—Dy1—O7	125.22 (9)	H7A—C7—H7C	109.5
O8—Dy1—O7	51.75 (9)	H7B—C7—H7C	109.5
O4—Dy1—O6	79.67 (9)	N4—C8—H8A	109.5
O1—Dy1—O6	75.55 (9)	N4—C8—H8B	109.5
O3—Dy1—O6	126.97 (9)	H8A—C8—H8B	109.5
O2—Dy1—O6	81.58 (9)	N4—C8—H8C	109.5
O8—Dy1—O6	143.55 (9)	H8A—C8—H8C	109.5
O7—Dy1—O6	143.17 (9)	H8B—C8—H8C	109.5
O4—Dy1—O5	78.85 (9)	N5—C9—H9A	109.5
O1—Dy1—O5	126.84 (9)	N5—C9—H9B	109.5
O3—Dy1—O5	75.75 (9)	H9A—C9—H9B	109.5
O2—Dy1—O5	80.39 (9)	N5—C9—H9C	109.5
O8—Dy1—O5	143.94 (9)	H9A—C9—H9C	109.5
O7—Dy1—O5	146.12 (9)	H9B—C9—H9C	109.5
O6—Dy1—O5	51.29 (8)	N5—C10—H10A	109.5
O4—Dy1—N14	102.67 (10)	N5—C10—H10B	109.5
O1—Dy1—N14	76.24 (10)	H10A—C10—H10B	109.5
O3—Dy1—N14	81.24 (10)	N5—C10—H10C	109.5
O2—Dy1—N14	99.36 (10)	H10A—C10—H10C	109.5
O8—Dy1—N14	25.94 (9)	H10B—C10—H10C	109.5
O7—Dy1—N14	25.88 (9)	N6—C11—H11A	109.5
O6—Dy1—N14	151.78 (9)	N6—C11—H11B	109.5
O5—Dy1—N14	156.92 (9)	H11A—C11—H11B	109.5
O4—Dy1—N13	75.74 (9)	N6—C11—H11C	109.5
O1—Dy1—N13	101.14 (10)	H11A—C11—H11C	109.5
O3—Dy1—N13	101.26 (10)	H11B—C11—H11C	109.5
O2—Dy1—N13	82.32 (9)	N6—C12—H12A	109.5
O8—Dy1—N13	155.77 (9)	N6—C12—H12B	109.5
O7—Dy1—N13	152.42 (9)	H12A—C12—H12B	109.5
O6—Dy1—N13	25.72 (8)	N6—C12—H12C	109.5
O5—Dy1—N13	25.76 (9)	H12A—C12—H12C	109.5
N14—Dy1—N13	176.94 (10)	H12B—C12—H12C	109.5
O1—P1—N3	110.93 (19)	N7—C13—H13A	109.5
O1—P1—N1	108.65 (16)	N7—C13—H13B	109.5
N3—P1—N1	110.02 (19)	H13A—C13—H13B	109.5
O1—P1—N2	111.29 (17)	N7—C13—H13C	109.5
N3—P1—N2	106.7 (2)	H13A—C13—H13C	109.5
N1—P1—N2	109.18 (19)	H13B—C13—H13C	109.5
O2—P2—N5	109.23 (18)	N7—C14—H14A	109.5
O2—P2—N4	108.57 (16)	N7—C14—H14B	109.5
N5—P2—N4	115.8 (2)	H14A—C14—H14B	109.5
O2—P2—N6	116.48 (18)	N7—C14—H14C	109.5
N5—P2—N6	103.4 (2)	H14A—C14—H14C	109.5
N4—P2—N6	103.50 (19)	H14B—C14—H14C	109.5
O3—P3—N8	119.56 (17)	N8—C15—H15A	109.5
O3—P3—N7	107.83 (16)	N8—C15—H15B	109.5
N8—P3—N7	104.8 (2)	H15A—C15—H15B	109.5
O3—P3—N9	107.68 (18)	N8—C15—H15C	109.5
N8—P3—N9	102.9 (2)	H15A—C15—H15C	109.5
N7—P3—N9	114.4 (2)	H15B—C15—H15C	109.5
O4—P4—N12	110.9 (2)	N8—C16—H16A	109.5
O4—P4—N11	110.04 (18)	N8—C16—H16B	109.5
N12—P4—N11	108.2 (3)	H16A—C16—H16B	109.5
O4—P4—N10	108.7 (2)	N8—C16—H16C	109.5
N12—P4—N10	109.3 (3)	H16A—C16—H16C	109.5
N11—P4—N10	109.8 (2)	H16B—C16—H16C	109.5
P1—O1—Dy1	168.03 (16)	N9—C17—H17A	109.5
P2—O2—Dy1	161.71 (17)	N9—C17—H17B	109.5
P3—O3—Dy1	158.35 (16)	H17A—C17—H17B	109.5
P4—O4—Dy1	167.58 (17)	N9—C17—H17C	109.5
N13—O5—Dy1	95.7 (2)	H17A—C17—H17C	109.5
N13—O6—Dy1	95.9 (2)	H17B—C17—H17C	109.5
N14—O7—Dy1	95.4 (2)	N9—C18—H18A	109.5
N14—O8—Dy1	96.1 (2)	N9—C18—H18B	109.5
C1—N1—C2	114.0 (3)	H18A—C18—H18B	109.5
C1—N1—P1	123.0 (3)	N9—C18—H18C	109.5
C2—N1—P1	120.1 (3)	H18A—C18—H18C	109.5
C3—N2—C4	114.3 (4)	H18B—C18—H18C	109.5
C3—N2—P1	125.4 (3)	N10—C19—H19A	109.5
C4—N2—P1	119.4 (3)	N10—C19—H19B	109.5
C6—N3—C5	115.3 (5)	H19A—C19—H19B	109.5
C6—N3—P1	119.9 (4)	N10—C19—H19C	109.5
C5—N3—P1	123.9 (4)	H19A—C19—H19C	109.5
C8—N4—C7	113.7 (4)	H19B—C19—H19C	109.5
C8—N4—P2	120.2 (3)	N10—C20—H20A	109.5
C7—N4—P2	120.9 (3)	N10—C20—H20B	109.5
C9—N5—C10	115.2 (4)	H20A—C20—H20B	109.5
C9—N5—P2	120.8 (3)	N10—C20—H20C	109.5
C10—N5—P2	120.2 (4)	H20A—C20—H20C	109.5
C11—N6—C12	110.6 (5)	H20B—C20—H20C	109.5
C11—N6—P2	123.9 (4)	N11—C21—H21A	109.5
C12—N6—P2	120.7 (4)	N11—C21—H21B	109.5
C14—N7—C13	113.6 (4)	H21A—C21—H21B	109.5
C14—N7—P3	121.8 (3)	N11—C21—H21C	109.5
C13—N7—P3	122.1 (3)	H21A—C21—H21C	109.5
C16—N8—C15	113.5 (5)	H21B—C21—H21C	109.5
C16—N8—P3	120.5 (4)	N11—C22—H22A	109.5
C15—N8—P3	123.0 (4)	N11—C22—H22B	109.5
C17—N9—C18	112.2 (4)	H22A—C22—H22B	109.5
C17—N9—P3	118.6 (3)	N11—C22—H22C	109.5
C18—N9—P3	120.8 (3)	H22A—C22—H22C	109.5
C19—N10—C20	113.5 (5)	H22B—C22—H22C	109.5
C19—N10—P4	121.8 (4)	N12—C23—H23A	109.5
C20—N10—P4	123.9 (5)	N12—C23—H23B	109.5
C22—N11—C21	114.8 (4)	H23A—C23—H23B	109.5
C22—N11—P4	124.7 (4)	N12—C23—H23C	109.5
C21—N11—P4	118.6 (3)	H23A—C23—H23C	109.5
C23—N12—C24	117.3 (6)	H23B—C23—H23C	109.5
C23—N12—P4	120.1 (4)	N12—C24—H24A	109.5
C24—N12—P4	122.6 (6)	N12—C24—H24B	109.5
O9—N13—O6	121.7 (3)	H24A—C24—H24B	109.5
O9—N13—O5	122.1 (3)	N12—C24—H24C	109.5
O6—N13—O5	116.2 (3)	H24A—C24—H24C	109.5
O9—N13—Dy1	172.4 (3)	H24B—C24—H24C	109.5
O6—N13—Dy1	58.33 (17)	S3—Mo1—S4	110.18 (4)
O5—N13—Dy1	58.51 (17)	S3—Mo1—S2	108.06 (4)
O10—N14—O7	122.3 (3)	S4—Mo1—S2	108.64 (4)
O10—N14—O8	121.2 (4)	S3—Mo1—S1	107.96 (4)
O7—N14—O8	116.5 (3)	S4—Mo1—S1	108.45 (4)
O10—N14—Dy1	175.6 (3)	S2—Mo1—S1	113.54 (4)
O7—N14—Dy1	58.76 (18)	S3—Mo1—Ag1	125.37 (4)
O8—N14—Dy1	57.99 (18)	S4—Mo1—Ag1	124.43 (4)
N1—C1—H1A	109.5	S2—Mo1—Ag1	57.79 (3)
N1—C1—H1B	109.5	S1—Mo1—Ag1	55.76 (3)
H1A—C1—H1B	109.5	S3—Mo1—Ag1ⁱ	58.82 (4)
N1—C1—H1C	109.5	S4—Mo1—Ag1ⁱ	58.59 (4)
H1A—C1—H1C	109.5	S2—Mo1—Ag1ⁱ	148.20 (3)
H1B—C1—H1C	109.5	S1—Mo1—Ag1ⁱ	98.27 (3)
N1—C2—H2A	109.5	Ag1—Mo1—Ag1ⁱ	154.014 (13)
N1—C2—H2B	109.5	S1—Ag1—S2	94.19 (3)
H2A—C2—H2B	109.5	S1—Ag1—S4ⁱⁱ	120.83 (4)
N1—C2—H2C	109.5	S2—Ag1—S4ⁱⁱ	119.97 (4)
H2A—C2—H2C	109.5	S1—Ag1—S3ⁱⁱ	120.26 (4)
H2B—C2—H2C	109.5	S2—Ag1—S3ⁱⁱ	117.20 (4)
N2—C3—H3A	109.5	S4ⁱⁱ—Ag1—S3ⁱⁱ	87.05 (4)
N2—C3—H3B	109.5	S1—Ag1—Mo1	47.40 (3)
H3A—C3—H3B	109.5	S2—Ag1—Mo1	46.79 (2)
N2—C3—H3C	109.5	S4ⁱⁱ—Ag1—Mo1	137.28 (3)
H3A—C3—H3C	109.5	S3ⁱⁱ—Ag1—Mo1	135.60 (3)
H3B—C3—H3C	109.5	S1—Ag1—Mo1ⁱⁱ	150.66 (3)
N2—C4—H4A	109.5	S2—Ag1—Mo1ⁱⁱ	115.12 (2)
N2—C4—H4B	109.5	S4ⁱⁱ—Ag1—Mo1ⁱⁱ	45.98 (3)
H4A—C4—H4B	109.5	S3ⁱⁱ—Ag1—Mo1ⁱⁱ	45.74 (3)
N2—C4—H4C	109.5	Mo1—Ag1—Mo1ⁱⁱ	161.911 (13)
H4A—C4—H4C	109.5	Mo1—S1—Ag1	76.84 (3)
H4B—C4—H4C	109.5	Mo1—S2—Ag1	75.42 (3)
N3—C5—H5A	109.5	Mo1—S3—Ag1ⁱ	75.44 (3)
N3—C5—H5B	109.5	Mo1—S4—Ag1ⁱ	75.43 (3)
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	[Dy(NO₃)₂(C₆H₁₈N₃OP)₄][AgMoS₄]
M_r	1335.43
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	153
a, b, c (Å)	15.786 (3), 29.671 (6), 11.331 (2)
β (°)	90.93 (3)
V (Å³)	5306.6 (17)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.33
Crystal size (mm)	0.35 × 0.25 × 0.18

Data collection
Diffractometer	Rigaku Saturn724+
Absorption correction	Multi-scan (CrystalClear; Rigaku, 2008)
T_min, T_max	0.503, 0.658
No. of measured, independent and observed [I > 2σ(I)] reflections	25288, 10445, 9394
R_int	0.023
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.032, 0.074, 1.05
No. of reflections	10445
No. of parameters	556
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.00, −1.00

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

Acknowledgements

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

References

Niu, 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
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Wei, H., Zhang, J. & Zhang, C. (2010). Acta Cryst. E66, m1193–m1194. Web of Science CSD CrossRef IUCr Journals Google Scholar
Zhang, C., Song, Y. L. & Wang, X. (2007). Coord. Chem. Rev. 251, 111–141. Web of Science CrossRef CAS Google Scholar

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