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

Zeng, J.; Tang, G.; Wei, C.

doi:10.1107/S1600536811046460

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 67| Part 12| December 2011| Pages m1724-m1725

https://doi.org/10.1107/S1600536811046460

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

Juxiang Zeng,^a Guodong Tang ^b,^c ^* and Changmei Wei ^c

^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 ). 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

Crystal data

[Ho(NO₃)₂(C₆H₁₈N₃OP)₄][AgWS₄]
M_r = 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 ) T_min = 0.463, T_max = 0.648
24559 measured reflections
9655 independent reflections
8942 reflections with I > 2σ(I)
R_int = 0.024

Refinement

R[F² > 2σ(F²)] = 0.031
wR(F²) = 0.073
S = 1.03
9655 reflections
532 parameters
H-atom parameters constrained
Δρ_max = 0.87 e Å⁻³
Δρ_min = −0.86 e Å⁻³

Data collection: CrystalClear (Rigaku, 2008); cell refinement: 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

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536811046460/rz2661sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811046460/rz2661Isup2.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). 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.

Structure description 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).

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

	Fig. 1. The molecular structure of the cation in the title compound, with 30% probability displacement ellipsoids. All H atoms have been omitted.
	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
M_r = 1425.76	D_x = 1.782 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 22657 reflections
a = 15.767 (3) Å	θ = 3.7–29.1°
b = 29.616 (6) Å	µ = 4.33 mm⁻¹
c = 11.383 (2) Å	T = 173 K
β = 90.88 (3)°	Block, orange
V = 5314.7 (17) Å³	0.18 × 0.15 × 0.1 mm
Z = 4

Data collection top

Rigaku Mercury2 diffractometer	9655 independent reflections
Radiation source: fine-focus sealed tube	8942 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.024
dtprofit.ref scans	θ_max = 25.4°, θ_min = 3.7°
Absorption correction: multi-scan (CrystalClear; Rigaku, 2008)	h = −17→18
T_min = 0.463, T_max = 0.648	k = −35→30
24559 measured reflections	l = −10→13

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)] = 0.031	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.073	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.030P)² + 16.6944P] where P = (F_o² + 2F_c²)/3
9655 reflections	(Δ/σ)_max = 0.001
532 parameters	Δρ_max = 0.87 e Å⁻³
0 restraints	Δρ_min = −0.86 e Å⁻³

Crystal data top

[Ho(NO₃)₂(C₆H₁₈N₃OP)₄][AgWS₄]	V = 5314.7 (17) Å³
M_r = 1425.76	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 15.767 (3) Å	µ = 4.33 mm⁻¹
b = 29.616 (6) Å	T = 173 K
c = 11.383 (2) Å	0.18 × 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)
T_min = 0.463, T_max = 0.648	R_int = 0.024
24559 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.031	0 restraints
wR(F²) = 0.073	H-atom parameters constrained
S = 1.03	w = 1/[σ²(F_o²) + (0.030P)² + 16.6944P] where P = (F_o² + 2F_c²)/3
9655 reflections	Δρ_max = 0.87 e Å⁻³
532 parameters	Δρ_min = −0.86 e Å⁻³

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
Ho1	0.738176 (12)	0.082625 (6)	0.827842 (18)	0.01998 (6)
P1	0.69903 (8)	−0.03034 (4)	0.69978 (12)	0.0288 (3)
P2	0.52206 (7)	0.13270 (4)	0.82148 (11)	0.0276 (3)
P3	0.79412 (10)	0.14676 (5)	1.09606 (12)	0.0386 (3)
P4	0.95858 (7)	0.09616 (4)	0.73141 (12)	0.0284 (3)
O1	0.7068 (2)	0.01807 (10)	0.7291 (3)	0.0276 (7)
O2	0.60328 (19)	0.10691 (11)	0.8233 (3)	0.0284 (7)
O3	0.7724 (2)	0.12690 (11)	0.9803 (3)	0.0311 (8)
O4	0.87641 (19)	0.08053 (11)	0.7803 (3)	0.0314 (8)
O5	0.8019 (2)	0.02693 (11)	0.9646 (3)	0.0312 (8)
O6	0.6691 (2)	0.04086 (11)	0.9882 (3)	0.0304 (8)
O7	0.7370 (3)	0.00123 (14)	1.1197 (4)	0.0522 (11)
O8	0.7241 (2)	0.10309 (11)	0.6201 (3)	0.0317 (8)
O9	0.7525 (2)	0.15801 (11)	0.7384 (3)	0.0325 (8)
O10	0.7262 (3)	0.17165 (15)	0.5536 (4)	0.0666 (14)
N1	0.7363 (3)	0.02232 (14)	1.0272 (4)	0.0324 (10)
N2	0.7346 (3)	0.14521 (14)	0.6350 (4)	0.0359 (10)
N3	0.7204 (3)	−0.03686 (14)	0.5597 (4)	0.0368 (10)
N4	0.6062 (3)	−0.04810 (17)	0.7393 (5)	0.0501 (13)
N5	0.7649 (3)	−0.06527 (15)	0.7670 (4)	0.0445 (12)
N6	0.5229 (3)	0.17284 (15)	0.9200 (5)	0.0438 (12)
N7	0.4446 (2)	0.09754 (15)	0.8481 (4)	0.0322 (10)
N8	0.5064 (3)	0.15650 (19)	0.6950 (4)	0.0490 (13)
N9	0.8961 (4)	0.13875 (19)	1.1241 (6)	0.0706 (19)
N10	0.7739 (4)	0.20017 (15)	1.0948 (4)	0.0511 (14)
N11	0.7405 (4)	0.12367 (19)	1.1984 (5)	0.0657 (17)
N12	1.0341 (3)	0.07042 (16)	0.8029 (4)	0.0413 (12)
N13	0.9834 (3)	0.14887 (15)	0.7386 (5)	0.0466 (12)
N14	0.9564 (3)	0.08651 (18)	0.5892 (4)	0.0455 (12)
C1	0.6968 (4)	−0.0020 (2)	0.4761 (5)	0.0538 (16)
H1A	0.7137	−0.0109	0.3988	0.081*
H1B	0.7247	0.0257	0.4972	0.081*
H1C	0.6365	0.0023	0.4768	0.081*
C2	0.7255 (4)	−0.0825 (2)	0.5080 (6)	0.0507 (16)
H2A	0.7383	−0.0801	0.4261	0.076*
H2B	0.6722	−0.0977	0.5168	0.076*
H2C	0.7694	−0.0994	0.5475	0.076*
C3	0.5353 (4)	−0.0168 (2)	0.7485 (7)	0.0609 (19)
H3A	0.4856	−0.0330	0.7718	0.091*
H3B	0.5249	−0.0028	0.6737	0.091*
H3C	0.5487	0.0059	0.8060	0.091*
C4	0.5810 (5)	−0.0956 (2)	0.7216 (7)	0.075 (2)
H4A	0.5241	−0.0999	0.7483	0.113*
H4B	0.6188	−0.1149	0.7654	0.113*
H4C	0.5836	−0.1030	0.6396	0.113*
C5	0.7544 (6)	−0.0812 (3)	0.8849 (7)	0.078 (2)
H5A	0.8006	−0.1008	0.9059	0.117*
H5B	0.7019	−0.0974	0.8900	0.117*
H5C	0.7536	−0.0559	0.9378	0.117*
C6	0.8534 (5)	−0.0682 (3)	0.7348 (8)	0.079 (2)
H6A	0.8816	−0.0902	0.7835	0.119*
H6B	0.8800	−0.0393	0.7457	0.119*
H6C	0.8572	−0.0770	0.6539	0.119*
C7	0.4540 (4)	0.1829 (2)	0.9993 (6)	0.0592 (18)
H7A	0.4698	0.2080	1.0486	0.089*
H7B	0.4428	0.1570	1.0472	0.089*
H7C	0.4040	0.1906	0.9544	0.089*
C8	0.5899 (4)	0.2076 (2)	0.9181 (7)	0.065 (2)
H8A	0.5815	0.2286	0.9811	0.097*
H8B	0.5875	0.2234	0.8445	0.097*
H8C	0.6444	0.1935	0.9275	0.097*
C9	0.3567 (3)	0.1067 (2)	0.8122 (5)	0.0475 (15)
H9A	0.3211	0.0822	0.8365	0.071*
H9B	0.3532	0.1097	0.7283	0.071*
H9C	0.3379	0.1342	0.8482	0.071*
C10	0.4535 (3)	0.0645 (2)	0.9432 (5)	0.0416 (13)
H10A	0.4028	0.0467	0.9474	0.062*
H10B	0.4625	0.0800	1.0164	0.062*
H10C	0.5010	0.0452	0.9283	0.062*
C11	0.4636 (5)	0.2007 (3)	0.6800 (8)	0.085 (3)
H11A	0.4608	0.2083	0.5980	0.128*
H11B	0.4950	0.2235	0.7219	0.128*
H11C	0.4072	0.1989	0.7102	0.128*
C12	0.5195 (4)	0.1314 (3)	0.5891 (6)	0.081 (3)
H12A	0.5075	0.1503	0.5224	0.121*
H12B	0.4823	0.1057	0.5873	0.121*
H12C	0.5773	0.1214	0.5867	0.121*
C13	0.9350 (5)	0.0958 (3)	1.1115 (8)	0.082 (3)
H13A	0.9939	0.0979	1.1336	0.123*
H13B	0.9301	0.0861	1.0312	0.123*
H13C	0.9075	0.0743	1.1612	0.123*
C14	0.9511 (6)	0.1717 (3)	1.1833 (9)	0.107 (4)
H14A	1.0073	0.1595	1.1913	0.161*
H14B	0.9293	0.1782	1.2596	0.161*
H14C	0.9529	0.1989	1.1377	0.161*
C15	0.8026 (5)	0.22773 (18)	0.9958 (5)	0.0497 (16)
H15A	0.7857	0.2585	1.0074	0.074*
H15B	0.7776	0.2165	0.9241	0.074*
H15C	0.8633	0.2261	0.9912	0.074*
C16	0.7480 (7)	0.2263 (2)	1.1976 (6)	0.094 (3)
H16A	0.7395	0.2573	1.1753	0.141*
H16B	0.7915	0.2246	1.2574	0.141*
H16C	0.6961	0.2142	1.2274	0.141*
C17	0.6491 (5)	0.1205 (3)	1.1866 (7)	0.079 (2)
H17A	0.6266	0.1062	1.2552	0.119*
H17B	0.6347	0.1029	1.1184	0.119*
H17C	0.6255	0.1502	1.1786	0.119*
C18	0.7782 (8)	0.1066 (4)	1.3086 (7)	0.127 (4)
H18A	0.7343	0.0946	1.3572	0.190*
H18B	0.8065	0.1309	1.3492	0.190*
H18C	0.8184	0.0833	1.2915	0.190*
C19	1.0209 (4)	0.0276 (2)	0.8615 (7)	0.0601 (19)
H19A	1.0731	0.0180	0.8982	0.090*
H19B	1.0027	0.0055	0.8050	0.090*
H19C	0.9783	0.0311	0.9201	0.090*
C20	1.1239 (4)	0.0796 (3)	0.7802 (8)	0.084 (3)
H20A	1.1587	0.0611	0.8308	0.126*
H20B	1.1358	0.1109	0.7954	0.126*
H20C	1.1359	0.0728	0.6997	0.126*
C21	0.9508 (4)	0.1826 (2)	0.6548 (9)	0.086 (3)
H21A	0.9731	0.2118	0.6751	0.129*
H21B	0.8900	0.1834	0.6577	0.129*
H21C	0.9680	0.1747	0.5770	0.129*
C22	1.0142 (6)	0.1686 (3)	0.8488 (7)	0.089 (3)
H22A	1.0256	0.2001	0.8373	0.134*
H22B	1.0653	0.1536	0.8736	0.134*
H22C	0.9719	0.1651	0.9079	0.134*
C23	0.9074 (4)	0.0485 (2)	0.5426 (6)	0.0554 (17)
H23A	0.9127	0.0474	0.4588	0.083*
H23B	0.8488	0.0522	0.5622	0.083*
H23C	0.9285	0.0209	0.5763	0.083*
C24	1.0297 (5)	0.0965 (3)	0.5170 (7)	0.084 (3)
H24A	1.0173	0.0885	0.4369	0.126*
H24B	1.0776	0.0793	0.5449	0.126*
H24C	1.0426	0.1281	0.5219	0.126*
W1	0.216203 (12)	0.227544 (6)	0.474103 (16)	0.02219 (6)
Ag1	0.21748 (3)	0.234393 (14)	0.21359 (3)	0.04001 (11)
S1	0.33062 (8)	0.21142 (5)	0.37372 (11)	0.0363 (3)
S2	0.10254 (8)	0.21235 (5)	0.36792 (12)	0.0386 (3)
S3	0.21433 (9)	0.18463 (4)	0.63272 (11)	0.0323 (3)
S4	0.21647 (9)	0.30058 (4)	0.51424 (11)	0.0357 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ho1	0.01767 (10)	0.01553 (10)	0.02679 (12)	−0.00013 (8)	0.00225 (8)	−0.00061 (8)
P1	0.0346 (7)	0.0203 (6)	0.0318 (7)	−0.0058 (5)	0.0097 (6)	−0.0058 (5)
P2	0.0199 (6)	0.0338 (7)	0.0291 (7)	0.0049 (5)	0.0001 (5)	0.0050 (5)
P3	0.0560 (9)	0.0270 (7)	0.0322 (8)	−0.0093 (6)	−0.0164 (7)	−0.0007 (6)
P4	0.0193 (6)	0.0272 (6)	0.0388 (8)	−0.0005 (5)	0.0046 (5)	0.0073 (5)
O1	0.0327 (18)	0.0175 (15)	0.0325 (19)	−0.0031 (14)	0.0033 (14)	−0.0053 (14)
O2	0.0207 (16)	0.0306 (18)	0.0339 (19)	0.0021 (14)	0.0016 (14)	−0.0015 (15)
O3	0.0322 (18)	0.0273 (17)	0.0336 (19)	−0.0016 (15)	−0.0049 (15)	−0.0076 (15)
O4	0.0188 (16)	0.0313 (18)	0.044 (2)	−0.0007 (14)	0.0087 (15)	0.0043 (15)
O5	0.0260 (17)	0.0270 (18)	0.041 (2)	−0.0001 (14)	0.0007 (15)	0.0058 (15)
O6	0.0249 (17)	0.0322 (18)	0.0342 (19)	−0.0024 (15)	0.0008 (15)	0.0030 (15)
O7	0.059 (3)	0.056 (3)	0.041 (2)	−0.003 (2)	−0.001 (2)	0.025 (2)
O8	0.042 (2)	0.0223 (17)	0.0312 (19)	−0.0034 (15)	0.0050 (16)	−0.0008 (14)
O9	0.040 (2)	0.0193 (16)	0.038 (2)	−0.0034 (15)	−0.0002 (16)	0.0032 (15)
O10	0.105 (4)	0.046 (3)	0.048 (3)	−0.017 (3)	−0.013 (3)	0.025 (2)
N1	0.033 (2)	0.025 (2)	0.039 (3)	−0.0024 (18)	−0.004 (2)	0.0028 (19)
N2	0.042 (3)	0.030 (2)	0.036 (3)	−0.002 (2)	0.003 (2)	0.007 (2)
N3	0.050 (3)	0.031 (2)	0.030 (2)	−0.006 (2)	0.009 (2)	−0.0085 (19)
N4	0.044 (3)	0.044 (3)	0.062 (3)	−0.017 (2)	0.021 (2)	−0.021 (3)
N5	0.064 (3)	0.026 (2)	0.044 (3)	0.008 (2)	0.016 (2)	0.003 (2)
N6	0.035 (2)	0.035 (2)	0.061 (3)	0.007 (2)	0.012 (2)	−0.006 (2)
N7	0.0196 (19)	0.042 (2)	0.035 (2)	0.0007 (18)	0.0021 (17)	0.0033 (19)
N8	0.035 (3)	0.073 (4)	0.039 (3)	−0.002 (2)	−0.007 (2)	0.023 (3)
N9	0.074 (4)	0.047 (3)	0.089 (5)	−0.017 (3)	−0.051 (4)	−0.002 (3)
N10	0.094 (4)	0.028 (2)	0.031 (3)	−0.009 (3)	0.006 (3)	−0.005 (2)
N11	0.104 (5)	0.051 (3)	0.041 (3)	−0.030 (3)	−0.004 (3)	0.010 (3)
N12	0.019 (2)	0.052 (3)	0.053 (3)	0.004 (2)	0.006 (2)	0.026 (2)
N13	0.039 (3)	0.029 (2)	0.072 (4)	−0.004 (2)	0.011 (2)	0.006 (2)
N14	0.034 (2)	0.064 (3)	0.039 (3)	−0.008 (2)	0.009 (2)	0.007 (2)
C1	0.077 (5)	0.053 (4)	0.031 (3)	−0.003 (3)	−0.005 (3)	−0.001 (3)
C2	0.065 (4)	0.042 (3)	0.045 (4)	−0.007 (3)	0.018 (3)	−0.018 (3)
C3	0.031 (3)	0.065 (4)	0.086 (5)	−0.002 (3)	−0.002 (3)	0.012 (4)
C4	0.086 (5)	0.060 (4)	0.080 (5)	−0.039 (4)	0.033 (4)	−0.026 (4)
C5	0.101 (6)	0.059 (5)	0.074 (5)	0.029 (4)	0.018 (5)	0.026 (4)
C6	0.056 (4)	0.093 (6)	0.090 (6)	0.019 (4)	0.006 (4)	0.017 (5)
C7	0.057 (4)	0.054 (4)	0.067 (5)	0.017 (3)	0.022 (3)	−0.008 (3)
C8	0.059 (4)	0.042 (4)	0.094 (6)	−0.007 (3)	0.014 (4)	−0.013 (4)
C9	0.023 (3)	0.069 (4)	0.051 (4)	−0.003 (3)	−0.004 (2)	0.014 (3)
C10	0.027 (3)	0.051 (3)	0.047 (3)	0.001 (3)	0.007 (2)	0.014 (3)
C11	0.059 (4)	0.088 (6)	0.108 (7)	0.015 (4)	−0.018 (4)	0.064 (5)
C12	0.051 (4)	0.153 (8)	0.037 (4)	−0.018 (5)	−0.008 (3)	0.002 (5)
C13	0.059 (5)	0.071 (5)	0.114 (7)	−0.002 (4)	−0.046 (5)	0.009 (5)
C14	0.111 (7)	0.099 (7)	0.110 (8)	−0.049 (6)	−0.057 (6)	0.006 (6)
C15	0.079 (5)	0.028 (3)	0.042 (4)	−0.003 (3)	0.006 (3)	−0.003 (2)
C16	0.192 (10)	0.046 (4)	0.045 (4)	−0.033 (5)	0.035 (5)	−0.023 (3)
C17	0.100 (6)	0.074 (5)	0.065 (5)	−0.029 (5)	0.040 (5)	−0.008 (4)
C18	0.216 (13)	0.112 (8)	0.051 (5)	0.006 (8)	−0.001 (7)	0.050 (5)
C19	0.034 (3)	0.057 (4)	0.089 (5)	0.004 (3)	0.008 (3)	0.038 (4)
C20	0.027 (3)	0.119 (7)	0.105 (6)	0.000 (4)	0.003 (4)	0.074 (6)
C21	0.045 (4)	0.045 (4)	0.170 (9)	0.007 (3)	0.019 (5)	0.059 (5)
C22	0.108 (7)	0.066 (5)	0.095 (6)	−0.050 (5)	0.034 (5)	−0.037 (5)
C23	0.047 (3)	0.073 (5)	0.047 (4)	−0.003 (3)	0.004 (3)	−0.012 (3)
C24	0.068 (5)	0.135 (8)	0.050 (5)	−0.035 (5)	0.021 (4)	0.011 (5)
W1	0.02714 (11)	0.02160 (10)	0.01777 (10)	−0.00239 (7)	−0.00110 (7)	0.00105 (7)
Ag1	0.0619 (3)	0.0377 (2)	0.0204 (2)	0.0004 (2)	−0.00013 (18)	0.00237 (16)
S1	0.0321 (7)	0.0487 (8)	0.0280 (7)	0.0047 (6)	0.0023 (5)	0.0021 (6)
S2	0.0326 (7)	0.0531 (8)	0.0299 (7)	−0.0137 (6)	−0.0052 (5)	0.0040 (6)
S3	0.0469 (7)	0.0254 (6)	0.0246 (6)	0.0010 (6)	0.0016 (5)	0.0056 (5)
S4	0.0566 (8)	0.0220 (6)	0.0285 (7)	−0.0040 (6)	0.0004 (6)	0.0015 (5)

Geometric parameters (Å, º) top

Ho1—O3	2.235 (3)	C6—H6A	0.9600
Ho1—O2	2.245 (3)	C6—H6B	0.9600
Ho1—O4	2.255 (3)	C6—H6C	0.9600
Ho1—O1	2.269 (3)	C7—H7A	0.9600
Ho1—O8	2.448 (3)	C7—H7B	0.9600
Ho1—O9	2.465 (3)	C7—H7C	0.9600
Ho1—O5	2.471 (3)	C8—H8A	0.9600
Ho1—O6	2.472 (3)	C8—H8B	0.9600
Ho1—N2	2.872 (4)	C8—H8C	0.9600
Ho1—N1	2.888 (4)	C9—H9A	0.9600
P1—O1	1.477 (3)	C9—H9B	0.9600
P1—N4	1.626 (5)	C9—H9C	0.9600
P1—N5	1.646 (5)	C10—H10A	0.9600
P1—N3	1.646 (4)	C10—H10B	0.9600
P2—O2	1.491 (3)	C10—H10C	0.9600
P2—N8	1.618 (5)	C11—H11A	0.9600
P2—N6	1.634 (5)	C11—H11B	0.9600
P2—N7	1.637 (4)	C11—H11C	0.9600
P3—O3	1.478 (3)	C12—H12A	0.9600
P3—N11	1.603 (6)	C12—H12B	0.9600
P3—N10	1.613 (5)	C12—H12C	0.9600
P3—N9	1.651 (6)	C13—H13A	0.9600
P4—O4	1.492 (3)	C13—H13B	0.9600
P4—N13	1.611 (5)	C13—H13C	0.9600
P4—N12	1.622 (4)	C14—H14A	0.9600
P4—N14	1.644 (5)	C14—H14B	0.9600
O5—N1	1.272 (5)	C14—H14C	0.9600
O6—N1	1.268 (5)	C15—H15A	0.9600
O7—N1	1.224 (5)	C15—H15B	0.9600
O8—N2	1.269 (5)	C15—H15C	0.9600
O9—N2	1.264 (5)	C16—H16A	0.9600
O10—N2	1.219 (6)	C16—H16B	0.9600
N3—C1	1.449 (7)	C16—H16C	0.9600
N3—C2	1.476 (7)	C17—H17A	0.9600
N4—C3	1.456 (8)	C17—H17B	0.9600
N4—C4	1.476 (8)	C17—H17C	0.9600
N5—C5	1.434 (8)	C18—H18A	0.9600
N5—C6	1.451 (8)	C18—H18B	0.9600
N6—C7	1.454 (7)	C18—H18C	0.9600
N6—C8	1.476 (8)	C19—H19A	0.9600
N7—C9	1.464 (6)	C19—H19B	0.9600
N7—C10	1.464 (7)	C19—H19C	0.9600
N8—C12	1.434 (9)	C20—H20A	0.9600
N8—C11	1.482 (9)	C20—H20B	0.9600
N9—C13	1.422 (9)	C20—H20C	0.9600
N9—C14	1.463 (9)	C21—H21A	0.9600
N10—C16	1.466 (8)	C21—H21B	0.9600
N10—C15	1.469 (7)	C21—H21C	0.9600
N11—C17	1.447 (10)	C22—H22A	0.9600
N11—C18	1.470 (9)	C22—H22B	0.9600
N12—C19	1.448 (7)	C22—H22C	0.9600
N12—C20	1.469 (7)	C23—H23A	0.9600
N13—C22	1.460 (9)	C23—H23B	0.9600
N13—C21	1.469 (8)	C23—H23C	0.9600
N14—C24	1.459 (8)	C24—H24A	0.9600
N14—C23	1.461 (8)	C24—H24B	0.9600
C1—H1A	0.9600	C24—H24C	0.9600
C1—H1B	0.9600	W1—S2	2.1929 (14)
C1—H1C	0.9600	W1—S1	2.2026 (14)
C2—H2A	0.9600	W1—S3	2.2085 (12)
C2—H2B	0.9600	W1—S4	2.2106 (13)
C2—H2C	0.9600	W1—Ag1ⁱ	2.9498 (6)
C3—H3A	0.9600	W1—Ag1	2.9727 (7)
C3—H3B	0.9600	Ag1—S4ⁱⁱ	2.4942 (14)
C3—H3C	0.9600	Ag1—S3ⁱⁱ	2.5689 (14)
C4—H4A	0.9600	Ag1—S1	2.6206 (15)
C4—H4B	0.9600	Ag1—S2	2.6257 (16)
C4—H4C	0.9600	Ag1—W1ⁱⁱ	2.9498 (6)
C5—H5A	0.9600	S3—Ag1ⁱ	2.5689 (14)
C5—H5B	0.9600	S4—Ag1ⁱ	2.4942 (14)
C5—H5C	0.9600

O3—Ho1—O2	92.71 (12)	N5—C5—H5C	109.5
O3—Ho1—O4	88.84 (13)	H5A—C5—H5C	109.5
O2—Ho1—O4	157.26 (12)	H5B—C5—H5C	109.5
O3—Ho1—O1	158.06 (12)	N5—C6—H6A	109.5
O2—Ho1—O1	93.38 (12)	N5—C6—H6B	109.5
O4—Ho1—O1	93.58 (12)	H6A—C6—H6B	109.5
O3—Ho1—O8	128.48 (12)	N5—C6—H6C	109.5
O2—Ho1—O8	80.02 (12)	H6A—C6—H6C	109.5
O4—Ho1—O8	81.28 (12)	H6B—C6—H6C	109.5
O1—Ho1—O8	73.39 (11)	N6—C7—H7A	109.5
O3—Ho1—O9	76.52 (12)	N6—C7—H7B	109.5
O2—Ho1—O9	78.06 (12)	H7A—C7—H7B	109.5
O4—Ho1—O9	80.26 (12)	N6—C7—H7C	109.5
O1—Ho1—O9	125.39 (12)	H7A—C7—H7C	109.5
O8—Ho1—O9	52.01 (11)	H7B—C7—H7C	109.5
O3—Ho1—O5	79.12 (12)	N6—C8—H8A	109.5
O2—Ho1—O5	127.18 (12)	N6—C8—H8B	109.5
O4—Ho1—O5	75.38 (12)	H8A—C8—H8B	109.5
O1—Ho1—O5	80.41 (12)	N6—C8—H8C	109.5
O8—Ho1—O5	143.50 (11)	H8A—C8—H8C	109.5
O9—Ho1—O5	145.65 (11)	H8B—C8—H8C	109.5
O3—Ho1—O6	79.85 (12)	N7—C9—H9A	109.5
O2—Ho1—O6	75.47 (11)	N7—C9—H9B	109.5
O4—Ho1—O6	127.03 (12)	H9A—C9—H9B	109.5
O1—Ho1—O6	81.32 (11)	N7—C9—H9C	109.5
O8—Ho1—O6	143.41 (11)	H9A—C9—H9C	109.5
O9—Ho1—O6	143.34 (11)	H9B—C9—H9C	109.5
O5—Ho1—O6	51.71 (11)	N7—C10—H10A	109.5
O3—Ho1—N2	102.51 (13)	N7—C10—H10B	109.5
O2—Ho1—N2	76.59 (12)	H10A—C10—H10B	109.5
O4—Ho1—N2	80.92 (13)	N7—C10—H10C	109.5
O1—Ho1—N2	99.41 (12)	H10A—C10—H10C	109.5
O8—Ho1—N2	26.07 (11)	H10B—C10—H10C	109.5
O9—Ho1—N2	25.99 (12)	N8—C11—H11A	109.5
O5—Ho1—N2	156.22 (12)	N8—C11—H11B	109.5
O6—Ho1—N2	152.04 (12)	H11A—C11—H11B	109.5
O3—Ho1—N1	75.99 (12)	N8—C11—H11C	109.5
O2—Ho1—N1	101.25 (12)	H11A—C11—H11C	109.5
O4—Ho1—N1	101.13 (12)	H11B—C11—H11C	109.5
O1—Ho1—N1	82.16 (12)	N8—C12—H12A	109.5
O8—Ho1—N1	155.54 (11)	N8—C12—H12B	109.5
O9—Ho1—N1	152.43 (12)	H12A—C12—H12B	109.5
O5—Ho1—N1	26.00 (11)	N8—C12—H12C	109.5
O6—Ho1—N1	25.91 (11)	H12A—C12—H12C	109.5
N2—Ho1—N1	177.37 (13)	H12B—C12—H12C	109.5
O1—P1—N4	108.9 (2)	N9—C13—H13A	109.5
O1—P1—N5	117.1 (2)	N9—C13—H13B	109.5
N4—P1—N5	103.4 (3)	H13A—C13—H13B	109.5
O1—P1—N3	108.4 (2)	N9—C13—H13C	109.5
N4—P1—N3	115.4 (3)	H13A—C13—H13C	109.5
N5—P1—N3	103.9 (2)	H13B—C13—H13C	109.5
O2—P2—N8	110.8 (2)	N9—C14—H14A	109.5
O2—P2—N6	111.4 (2)	N9—C14—H14B	109.5
N8—P2—N6	107.0 (3)	H14A—C14—H14B	109.5
O2—P2—N7	108.4 (2)	N9—C14—H14C	109.5
N8—P2—N7	109.7 (2)	H14A—C14—H14C	109.5
N6—P2—N7	109.5 (2)	H14B—C14—H14C	109.5
O3—P3—N11	111.1 (3)	N10—C15—H15A	109.5
O3—P3—N10	109.8 (2)	N10—C15—H15B	109.5
N11—P3—N10	108.5 (3)	H15A—C15—H15B	109.5
O3—P3—N9	109.1 (3)	N10—C15—H15C	109.5
N11—P3—N9	108.7 (3)	H15A—C15—H15C	109.5
N10—P3—N9	109.5 (3)	H15B—C15—H15C	109.5
O4—P4—N13	119.6 (2)	N10—C16—H16A	109.5
O4—P4—N12	107.6 (2)	N10—C16—H16B	109.5
N13—P4—N12	104.7 (3)	H16A—C16—H16B	109.5
O4—P4—N14	108.0 (2)	N10—C16—H16C	109.5
N13—P4—N14	102.7 (3)	H16A—C16—H16C	109.5
N12—P4—N14	114.6 (3)	H16B—C16—H16C	109.5
P1—O1—Ho1	161.2 (2)	N11—C17—H17A	109.5
P2—O2—Ho1	167.9 (2)	N11—C17—H17B	109.5
P3—O3—Ho1	167.3 (2)	H17A—C17—H17B	109.5
P4—O4—Ho1	158.4 (2)	N11—C17—H17C	109.5
N1—O5—Ho1	95.6 (3)	H17A—C17—H17C	109.5
N1—O6—Ho1	95.7 (3)	H17B—C17—H17C	109.5
N2—O8—Ho1	96.0 (3)	N11—C18—H18A	109.5
N2—O9—Ho1	95.3 (3)	N11—C18—H18B	109.5
O7—N1—O6	121.2 (4)	H18A—C18—H18B	109.5
O7—N1—O5	122.6 (4)	N11—C18—H18C	109.5
O6—N1—O5	116.1 (4)	H18A—C18—H18C	109.5
O7—N1—Ho1	172.4 (4)	H18B—C18—H18C	109.5
O6—N1—Ho1	58.4 (2)	N12—C19—H19A	109.5
O5—N1—Ho1	58.4 (2)	N12—C19—H19B	109.5
O10—N2—O9	122.3 (4)	H19A—C19—H19B	109.5
O10—N2—O8	121.2 (5)	N12—C19—H19C	109.5
O9—N2—O8	116.5 (4)	H19A—C19—H19C	109.5
O10—N2—Ho1	174.9 (4)	H19B—C19—H19C	109.5
O9—N2—Ho1	58.7 (2)	N12—C20—H20A	109.5
O8—N2—Ho1	57.9 (2)	N12—C20—H20B	109.5
C1—N3—C2	113.9 (5)	H20A—C20—H20B	109.5
C1—N3—P1	119.9 (4)	N12—C20—H20C	109.5
C2—N3—P1	120.5 (4)	H20A—C20—H20C	109.5
C3—N4—C4	114.2 (5)	H20B—C20—H20C	109.5
C3—N4—P1	120.6 (4)	N13—C21—H21A	109.5
C4—N4—P1	120.8 (4)	N13—C21—H21B	109.5
C5—N5—C6	110.0 (6)	H21A—C21—H21B	109.5
C5—N5—P1	124.1 (4)	N13—C21—H21C	109.5
C6—N5—P1	121.5 (4)	H21A—C21—H21C	109.5
C7—N6—C8	114.0 (5)	H21B—C21—H21C	109.5
C7—N6—P2	125.3 (4)	N13—C22—H22A	109.5
C8—N6—P2	119.7 (4)	N13—C22—H22B	109.5
C9—N7—C10	114.2 (4)	H22A—C22—H22B	109.5
C9—N7—P2	122.5 (4)	N13—C22—H22C	109.5
C10—N7—P2	119.9 (3)	H22A—C22—H22C	109.5
C12—N8—C11	115.6 (6)	H22B—C22—H22C	109.5
C12—N8—P2	120.0 (5)	N14—C23—H23A	109.5
C11—N8—P2	123.4 (5)	N14—C23—H23B	109.5
C13—N9—C14	112.9 (6)	H23A—C23—H23B	109.5
C13—N9—P3	122.0 (4)	N14—C23—H23C	109.5
C14—N9—P3	124.2 (6)	H23A—C23—H23C	109.5
C16—N10—C15	114.3 (5)	H23B—C23—H23C	109.5
C16—N10—P3	124.7 (4)	N14—C24—H24A	109.5
C15—N10—P3	119.2 (4)	N14—C24—H24B	109.5
C17—N11—C18	116.5 (7)	H24A—C24—H24B	109.5
C17—N11—P3	119.7 (5)	N14—C24—H24C	109.5
C18—N11—P3	123.8 (7)	H24A—C24—H24C	109.5
C19—N12—C20	112.8 (5)	H24B—C24—H24C	109.5
C19—N12—P4	122.2 (4)	S2—W1—S1	109.79 (5)
C20—N12—P4	121.8 (4)	S2—W1—S3	108.15 (5)
C22—N13—C21	113.2 (6)	S1—W1—S3	108.71 (5)
C22—N13—P4	120.6 (5)	S2—W1—S4	108.28 (6)
C21—N13—P4	123.0 (5)	S1—W1—S4	108.68 (5)
C24—N14—C23	111.8 (5)	S3—W1—S4	113.21 (5)
C24—N14—P4	121.0 (5)	S2—W1—Ag1ⁱ	125.57 (4)
C23—N14—P4	119.6 (4)	S1—W1—Ag1ⁱ	124.63 (4)
N3—C1—H1A	109.5	S3—W1—Ag1ⁱ	57.61 (4)
N3—C1—H1B	109.5	S4—W1—Ag1ⁱ	55.61 (3)
H1A—C1—H1B	109.5	S2—W1—Ag1	58.81 (4)
N3—C1—H1C	109.5	S1—W1—Ag1	58.61 (4)
H1A—C1—H1C	109.5	S3—W1—Ag1	148.78 (4)
H1B—C1—H1C	109.5	S4—W1—Ag1	98.01 (4)
N3—C2—H2A	109.5	Ag1ⁱ—W1—Ag1	153.608 (10)
N3—C2—H2B	109.5	S4ⁱⁱ—Ag1—S3ⁱⁱ	93.54 (4)
H2A—C2—H2B	109.5	S4ⁱⁱ—Ag1—S1	121.32 (5)
N3—C2—H2C	109.5	S3ⁱⁱ—Ag1—S1	120.05 (5)
H2A—C2—H2C	109.5	S4ⁱⁱ—Ag1—S2	120.71 (5)
H2B—C2—H2C	109.5	S3ⁱⁱ—Ag1—S2	117.52 (5)
N4—C3—H3A	109.5	S1—Ag1—S2	86.54 (4)
N4—C3—H3B	109.5	S4ⁱⁱ—Ag1—W1ⁱⁱ	47.00 (3)
H3A—C3—H3B	109.5	S3ⁱⁱ—Ag1—W1ⁱⁱ	46.55 (3)
N4—C3—H3C	109.5	S1—Ag1—W1ⁱⁱ	137.47 (4)
H3A—C3—H3C	109.5	S2—Ag1—W1ⁱⁱ	135.92 (4)
H3B—C3—H3C	109.5	S4ⁱⁱ—Ag1—W1	151.54 (3)
N4—C4—H4A	109.5	S3ⁱⁱ—Ag1—W1	114.88 (3)
N4—C4—H4B	109.5	S1—Ag1—W1	45.85 (3)
H4A—C4—H4B	109.5	S2—Ag1—W1	45.60 (3)
N4—C4—H4C	109.5	W1ⁱⁱ—Ag1—W1	161.429 (17)
H4A—C4—H4C	109.5	W1—S1—Ag1	75.54 (4)
H4B—C4—H4C	109.5	W1—S2—Ag1	75.59 (4)
N5—C5—H5A	109.5	W1—S3—Ag1ⁱ	75.84 (4)
N5—C5—H5B	109.5	W1—S4—Ag1ⁱ	77.39 (4)
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	[Ho(NO₃)₂(C₆H₁₈N₃OP)₄][AgWS₄]
M_r	1425.76
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	173
a, b, c (Å)	15.767 (3), 29.616 (6), 11.383 (2)
β (°)	90.88 (3)
V (Å³)	5314.7 (17)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	4.33
Crystal size (mm)	0.18 × 0.15 × 0.1

Data collection
Diffractometer	Rigaku Mercury2
Absorption correction	Multi-scan (CrystalClear; Rigaku, 2008)
T_min, T_max	0.463, 0.648
No. of measured, independent and observed [I > 2σ(I)] reflections	24559, 9655, 8942
R_int	0.024
(sin θ/λ)_max (Å⁻¹)	0.602

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.031, 0.073, 1.03
No. of reflections	9655
No. of parameters	532
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.030P)² + 16.6944P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	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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