Poly[[bis­(nitrato-κO)bis­(μ4-pyridine-4-carboxyl­ato)tetra­kis­(μ3-pyridine-4-carboxyl­ato)octa­silver(I)] hemihydrate]

Meng, Z.-H.

doi:10.1107/S1600536811028261

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 8| August 2011| Page m1112

doi:10.1107/S1600536811028261

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Poly[[bis(nitrato-κO)bis(μ₄-pyridine-4-carboxylato)tetrakis(μ₃-pyridine-4-carboxylato)octasilver(I)] hemihydrate]

Zhao-Hui Meng ^a ^*

^aCollege of Chemistry and Pharmacy Engineering, Nanyang Normal University, Nanyang 473061, People's Republic of China
^*Correspondence e-mail: nysymzh@126.com

(Received 5 July 2011; accepted 14 July 2011; online 23 July 2011)

In the title coordination polymer, {[Ag₈(C₆H₄NO₂)₆(NO₃)₂]·0.5H₂O}_n, two Ag^I ions are two-coordinate within an AgN₂ set and six are three-coordinate within AgN₂O and AgO₃ sets. The Ag—N and Ag—O distances are in the ranges 2.150 (5)–2.198 (5) and 2.142 (4)–2.702 (5) Å, respectively. A two-dimensional coordination network is formed parallel to (100). The O atom of the disordered solvent water molecule is located on an inversion center.

Related literature

For examples of silver(I) coordination compounds containing isonicotinic acid, see: Du & Zhao (2004 ); Jaber et al. (1994 ); Yang et al. (2004 ).

Experimental

Crystal data

[Ag₈(C₆H₄NO₂)₆(NO₃)₂]·0.5H₂O
M_r = 1728.59
Monoclinic, P 2₁ /c
a = 18.006 (4) Å
b = 18.255 (4) Å
c = 13.166 (3) Å
β = 104.017 (4)°
V = 4199.0 (17) Å³
Z = 4
Mo Kα radiation
μ = 3.74 mm⁻¹
T = 296 K
0.23 × 0.17 × 0.15 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2008 ) T_min = 0.480, T_max = 0.604
21106 measured reflections
7391 independent reflections
6057 reflections with I > 2σ(I)
R_int = 0.040

Refinement

R[F² > 2σ(F²)] = 0.041
wR(F²) = 0.106
S = 1.01
7391 reflections
637 parameters
H-atom parameters constrained
Δρ_max = 1.52 e Å⁻³
Δρ_min = −1.68 e Å⁻³

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT; 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: 10.1107/S1600536811028261/gk2394sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811028261/gk2394Isup2.hkl

checkCIF report

Comment top

Herein, using isonicotinic acid as bridging ligand, we report a two-dimensional coordination polymer {[Ag₈(C₆H₄NO₂)₆(NO₃)₂].0.5H₂O}_n. The asymmetric unit of the title compound contains eight crystallographically independent Ag^Iatoms, six C₆H₄NO₂ligands, two nitrate ligands and half water molecule (Fig. 1). In the structure of title compound, two Ag^I atoms are two-coordinate (Ag1, Ag2) and six are three-coordinate. The bond lengths Ag—N and Ag—O range from 2.150 (5) to 2.198 (5) Å and 2.142 (4) to 2.702 (5)) Å, respectively. The two dimensional polymeric structure of the title coordination polymer is parallel to (1 0 0). The disordered water molecule that is located on inversion center connects via hydrogen bonds adjacent coordination polymers (Fig. 2). It is also in a short contact [2.832 (4) Å] to two Ag(2) atoms from the neighbouring polymers.

Related literature top

For examples of silver(I) coordination compounds containing isonicotinic acid, see: Du & Zhao (2004); Jaber et al. (1994); Yang et al. (2004).

Experimental top

All chemicals were of reagent grade quality obtained from commercial sources and used without further purification. The title compound was synthesized from a mixture of AgNO₃ (0.34 g, 2 mmol), C₆H₅NO₂ (0.26 g, 1.2 mmol) and H₂O (12 g, 667 mmol) in a molar ratio of 2: 1.2: 667 by hydrothermal reaction. The mixture was stirred for half an hour, and then transferred into a Teflon-lined stainless steel autoclave (50 ml) and treated at 160 °C for 3 days. After the mixture was slowly cooled to room temperature, colorless rod-shaped crystals were obtained.

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 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. View of the asymmetric unit of the title compound with displacement ellipsoids drawn at the 30% probability level. Hadrogen atoms are omitted for clarity.
	Fig. 2. Crystal packing viewed along the b axis (H atoms are omitted for clarity).

Poly[[bis(nitrato-κO)bis(µ₄-pyridine-4-carboxylato)tetrakis(µ₃- pyridine-4-carboxylato)octasilver(I)] hemihydrate] top

Crystal data top

[Ag₈(C₆H₄NO₂)₆(NO₃)₂]·0.5H₂O	F(000) = 3280
M_r = 1728.59	D_x = 2.733 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 7885 reflections
a = 18.006 (4) Å	θ = 2.5–28.3°
b = 18.255 (4) Å	µ = 3.74 mm⁻¹
c = 13.166 (3) Å	T = 296 K
β = 104.017 (4)°	Rod, colorless
V = 4199.0 (17) Å³	0.23 × 0.17 × 0.15 mm
Z = 4

Data collection top

Bruker APEXII CCD diffractometer	7391 independent reflections
Radiation source: fine-focus sealed tube	6057 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.040
ϕ and ω scans	θ_max = 25.0°, θ_min = 1.2°
Absorption correction: multi-scan (SADABS; Bruker, 2008)	h = −21→20
T_min = 0.480, T_max = 0.604	k = −15→21
21106 measured reflections	l = −15→15

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)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.106	H-atom parameters constrained
S = 1.01	w = 1/[σ²(F_o²) + (0.0468P)² + 11.8118P] where P = (F_o² + 2F_c²)/3
7391 reflections	(Δ/σ)_max = 0.001
637 parameters	Δρ_max = 1.52 e Å⁻³
0 restraints	Δρ_min = −1.68 e Å⁻³

Crystal data top

[Ag₈(C₆H₄NO₂)₆(NO₃)₂]·0.5H₂O	V = 4199.0 (17) Å³
M_r = 1728.59	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 18.006 (4) Å	µ = 3.74 mm⁻¹
b = 18.255 (4) Å	T = 296 K
c = 13.166 (3) Å	0.23 × 0.17 × 0.15 mm
β = 104.017 (4)°

Data collection top

Bruker APEXII CCD diffractometer	7391 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2008)	6057 reflections with I > 2σ(I)
T_min = 0.480, T_max = 0.604	R_int = 0.040
21106 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.041	0 restraints
wR(F²) = 0.106	H-atom parameters constrained
S = 1.01	w = 1/[σ²(F_o²) + (0.0468P)² + 11.8118P] where P = (F_o² + 2F_c²)/3
7391 reflections	Δρ_max = 1.52 e Å⁻³
637 parameters	Δρ_min = −1.68 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.

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

	x	y	z	U_iso*/U_eq
Ag1	0.76442 (3)	0.09112 (2)	0.37019 (4)	0.04168 (14)
Ag2	0.52204 (4)	0.51064 (3)	0.29474 (6)	0.0731 (2)
Ag3	0.69514 (3)	0.59092 (2)	0.36445 (5)	0.04876 (15)
Ag4	0.85616 (3)	0.58930 (2)	0.43687 (5)	0.05365 (16)
Ag5	0.73415 (3)	0.14657 (2)	0.60134 (4)	0.04101 (13)
Ag6	0.65019 (3)	0.64893 (2)	0.58104 (5)	0.05103 (16)
Ag7	0.81026 (3)	0.64803 (2)	0.65006 (5)	0.05424 (16)
Ag8	0.96867 (3)	0.71827 (3)	0.74350 (4)	0.04974 (16)
C1	0.8346 (3)	0.2460 (3)	0.3692 (4)	0.0321 (12)
H1A	0.8795	0.2193	0.3761	0.039*
C2	0.8397 (3)	0.3210 (3)	0.3714 (4)	0.0346 (13)
H2A	0.8868	0.3442	0.3791	0.042*
C3	0.7728 (3)	0.3617 (3)	0.3619 (4)	0.0308 (12)
C4	0.7046 (3)	0.3241 (3)	0.3456 (4)	0.0333 (12)
H4A	0.6587	0.3497	0.3355	0.040*
C5	0.7040 (3)	0.2483 (3)	0.3441 (4)	0.0351 (13)
H5A	0.6574	0.2239	0.3335	0.042*
C6	0.7750 (3)	0.4435 (3)	0.3741 (4)	0.0321 (12)
C7	0.7793 (3)	0.7381 (3)	0.4018 (4)	0.0325 (12)
C8	0.7765 (3)	0.8202 (3)	0.3910 (4)	0.0290 (12)
C9	0.8430 (3)	0.8631 (3)	0.4116 (5)	0.0364 (13)
H9A	0.8909	0.8410	0.4304	0.044*
C10	0.8370 (3)	0.9371 (3)	0.4040 (5)	0.0378 (14)
H10A	0.8819	0.9645	0.4182	0.045*
C11	0.7065 (3)	0.9316 (3)	0.3558 (5)	0.0386 (14)
H11A	0.6592	0.9549	0.3354	0.046*
C12	0.7076 (3)	0.8572 (3)	0.3625 (5)	0.0376 (14)
H12A	0.6618	0.8312	0.3478	0.045*
C13	0.5378 (3)	0.6716 (3)	0.3558 (5)	0.0345 (13)
C14	0.5225 (3)	0.7494 (3)	0.3154 (4)	0.0314 (12)
C15	0.5159 (3)	0.8054 (3)	0.3857 (5)	0.0378 (13)
H15A	0.5198	0.7948	0.4559	0.045*
C16	0.5038 (3)	0.8759 (3)	0.3499 (5)	0.0396 (14)
H16A	0.5005	0.9126	0.3977	0.047*
C17	0.5029 (3)	0.8405 (3)	0.1828 (5)	0.0385 (13)
H17A	0.4980	0.8519	0.1127	0.046*
C18	0.5172 (3)	0.7664 (3)	0.2162 (4)	0.0322 (12)
H18A	0.5227	0.7303	0.1687	0.039*
C19	0.7952 (3)	0.3043 (3)	0.6191 (4)	0.0312 (12)
H19A	0.8419	0.2802	0.6290	0.037*
C20	0.7946 (3)	0.3794 (3)	0.6228 (4)	0.0329 (12)
H20A	0.8405	0.4051	0.6352	0.039*
C21	0.7261 (3)	0.4178 (3)	0.6082 (4)	0.0304 (12)
C22	0.6593 (3)	0.3759 (3)	0.5905 (5)	0.0374 (13)
H22A	0.6119	0.3986	0.5810	0.045*
C23	0.6643 (3)	0.3014 (3)	0.5873 (5)	0.0372 (13)
H23A	0.6190	0.2746	0.5744	0.045*
C24	0.7258 (3)	0.4997 (3)	0.6084 (4)	0.0321 (12)
C25	0.7286 (3)	0.7952 (3)	0.6344 (4)	0.0314 (12)
C26	0.7287 (3)	0.8778 (3)	0.6362 (4)	0.0272 (11)
C27	0.7969 (3)	0.9165 (3)	0.6531 (5)	0.0336 (13)
H27A	0.8433	0.8916	0.6706	0.040*
C28	0.7958 (3)	0.9911 (3)	0.6442 (5)	0.0368 (13)
H28A	0.8422	1.0159	0.6549	0.044*
C29	0.6649 (3)	0.9926 (3)	0.6096 (4)	0.0350 (13)
H29A	0.6195	1.0190	0.5965	0.042*
C30	0.6611 (3)	0.9183 (3)	0.6164 (4)	0.0325 (12)
H30A	0.6141	0.8950	0.6081	0.039*
C31	0.9641 (3)	0.5647 (3)	0.6772 (5)	0.0326 (12)
C32	0.9812 (3)	0.4839 (3)	0.7003 (4)	0.0303 (12)
C33	0.9862 (3)	0.4364 (3)	0.6201 (4)	0.0334 (12)
H33A	0.9802	0.4538	0.5522	0.040*
C34	1.0004 (3)	0.3628 (3)	0.6419 (5)	0.0371 (13)
H34A	1.0040	0.3314	0.5876	0.045*
C35	1.0030 (3)	0.3805 (3)	0.8162 (5)	0.0388 (14)
H35A	1.0074	0.3617	0.8830	0.047*
C36	0.9906 (3)	0.4552 (3)	0.8002 (5)	0.0366 (13)
H36A	0.9886	0.4858	0.8560	0.044*
N1	0.7685 (3)	0.2089 (2)	0.3576 (4)	0.0337 (11)
N2	0.7698 (2)	0.9733 (2)	0.3771 (4)	0.0304 (10)
N3	0.4963 (3)	0.8948 (2)	0.2501 (4)	0.0372 (11)
N4	0.7306 (2)	0.2645 (2)	0.6016 (3)	0.0297 (10)
N5	0.7309 (3)	1.0298 (3)	0.6206 (4)	0.0352 (11)
N6	1.0091 (3)	0.3347 (2)	0.7392 (4)	0.0356 (11)
N7	0.4240 (3)	0.5945 (2)	0.1017 (4)	0.0366 (11)
N8	1.0749 (3)	0.6422 (3)	0.9356 (4)	0.0395 (12)
O1	0.7108 (2)	0.4747 (2)	0.3625 (3)	0.0425 (10)
O2	0.8390 (2)	0.4738 (2)	0.3961 (4)	0.0455 (11)
O3	0.7162 (2)	0.7071 (2)	0.3867 (4)	0.0466 (11)
O4	0.8434 (2)	0.7086 (2)	0.4260 (4)	0.0538 (12)
O5	0.5583 (2)	0.6274 (2)	0.2934 (4)	0.0431 (10)
O6	0.5296 (2)	0.6566 (2)	0.4441 (4)	0.0494 (11)
O7	0.6614 (2)	0.5305 (2)	0.5919 (4)	0.0490 (11)
O8	0.7888 (2)	0.5311 (2)	0.6248 (4)	0.0428 (10)
O9	0.6638 (2)	0.7644 (2)	0.6112 (4)	0.0455 (11)
O10	0.7926 (2)	0.7648 (2)	0.6547 (4)	0.0465 (11)
O11	0.9665 (3)	0.5894 (2)	0.5911 (3)	0.0460 (11)
O12	0.9471 (2)	0.6010 (2)	0.7502 (3)	0.0421 (10)
O13	0.3939 (3)	0.5843 (3)	0.1764 (4)	0.0555 (12)
O14	0.4752 (3)	0.5534 (3)	0.0880 (4)	0.0564 (12)
O15	0.4022 (3)	0.6465 (2)	0.0407 (4)	0.0558 (12)
O16	1.1085 (3)	0.6510 (3)	0.8641 (5)	0.0647 (14)
O17	1.0887 (3)	0.5885 (3)	0.9939 (4)	0.0659 (14)
O18	1.0269 (2)	0.6890 (2)	0.9478 (4)	0.0518 (11)
O1W	0.5000	0.5000	0.5000	0.065 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ag1	0.0553 (3)	0.0149 (2)	0.0555 (3)	−0.00049 (18)	0.0148 (2)	0.00041 (19)
Ag2	0.0813 (4)	0.0253 (3)	0.0924 (5)	−0.0090 (3)	−0.0183 (3)	0.0034 (3)
Ag3	0.0480 (3)	0.0187 (2)	0.0799 (4)	0.00469 (19)	0.0163 (3)	0.0013 (2)
Ag4	0.0476 (3)	0.0209 (2)	0.0847 (4)	0.0022 (2)	0.0010 (3)	−0.0017 (2)
Ag5	0.0528 (3)	0.0155 (2)	0.0547 (3)	−0.00172 (18)	0.0130 (2)	0.00065 (18)
Ag6	0.0421 (3)	0.0197 (2)	0.0842 (4)	0.00300 (19)	0.0015 (3)	−0.0021 (2)
Ag7	0.0426 (3)	0.0182 (2)	0.0974 (4)	0.00448 (19)	0.0082 (3)	−0.0001 (2)
Ag8	0.0529 (3)	0.0203 (2)	0.0690 (3)	−0.00273 (19)	0.0011 (3)	−0.0019 (2)
C1	0.033 (3)	0.026 (3)	0.037 (3)	0.003 (2)	0.009 (2)	0.000 (2)
C2	0.033 (3)	0.030 (3)	0.040 (3)	0.001 (2)	0.008 (2)	−0.002 (3)
C3	0.037 (3)	0.024 (3)	0.030 (3)	0.001 (2)	0.005 (2)	0.004 (2)
C4	0.031 (3)	0.029 (3)	0.041 (3)	0.004 (2)	0.011 (2)	0.000 (2)
C5	0.032 (3)	0.025 (3)	0.046 (3)	−0.001 (2)	0.005 (3)	−0.002 (3)
C6	0.042 (3)	0.022 (3)	0.033 (3)	0.006 (2)	0.011 (2)	0.006 (2)
C7	0.039 (3)	0.017 (3)	0.040 (3)	0.004 (2)	0.007 (3)	0.000 (2)
C8	0.032 (3)	0.023 (3)	0.031 (3)	0.000 (2)	0.007 (2)	0.000 (2)
C9	0.026 (3)	0.026 (3)	0.057 (4)	0.000 (2)	0.010 (3)	−0.008 (3)
C10	0.032 (3)	0.021 (3)	0.064 (4)	−0.007 (2)	0.018 (3)	−0.003 (3)
C11	0.030 (3)	0.025 (3)	0.059 (4)	0.002 (2)	0.007 (3)	0.004 (3)
C12	0.026 (3)	0.025 (3)	0.059 (4)	−0.003 (2)	0.006 (3)	−0.002 (3)
C13	0.020 (3)	0.034 (3)	0.048 (4)	−0.005 (2)	0.004 (2)	0.003 (3)
C14	0.023 (3)	0.022 (3)	0.047 (3)	−0.005 (2)	0.005 (2)	−0.003 (2)
C15	0.038 (3)	0.038 (3)	0.041 (3)	−0.001 (3)	0.016 (3)	−0.003 (3)
C16	0.035 (3)	0.035 (3)	0.049 (4)	−0.002 (3)	0.011 (3)	−0.012 (3)
C17	0.036 (3)	0.038 (3)	0.041 (3)	−0.003 (3)	0.007 (3)	0.006 (3)
C18	0.024 (3)	0.033 (3)	0.042 (3)	−0.010 (2)	0.011 (2)	−0.016 (3)
C19	0.029 (3)	0.020 (3)	0.044 (3)	0.003 (2)	0.007 (2)	0.004 (2)
C20	0.026 (3)	0.027 (3)	0.044 (3)	−0.003 (2)	0.004 (2)	0.002 (2)
C21	0.030 (3)	0.026 (3)	0.035 (3)	−0.002 (2)	0.007 (2)	−0.005 (2)
C22	0.024 (3)	0.031 (3)	0.056 (4)	0.000 (2)	0.008 (3)	−0.004 (3)
C23	0.036 (3)	0.024 (3)	0.053 (4)	−0.010 (2)	0.014 (3)	−0.007 (3)
C24	0.031 (3)	0.025 (3)	0.039 (3)	0.001 (2)	0.007 (2)	−0.001 (2)
C25	0.041 (3)	0.021 (3)	0.033 (3)	0.002 (2)	0.010 (2)	0.000 (2)
C26	0.031 (3)	0.019 (3)	0.031 (3)	0.003 (2)	0.009 (2)	0.002 (2)
C27	0.028 (3)	0.025 (3)	0.048 (3)	0.005 (2)	0.009 (3)	0.000 (2)
C28	0.031 (3)	0.026 (3)	0.056 (4)	−0.001 (2)	0.014 (3)	0.002 (3)
C29	0.030 (3)	0.028 (3)	0.045 (3)	0.003 (2)	0.005 (3)	−0.002 (3)
C30	0.029 (3)	0.026 (3)	0.043 (3)	−0.001 (2)	0.009 (2)	−0.003 (2)
C31	0.021 (3)	0.031 (3)	0.043 (3)	−0.002 (2)	0.003 (2)	−0.005 (3)
C32	0.024 (3)	0.023 (3)	0.044 (3)	−0.003 (2)	0.006 (2)	−0.001 (2)
C33	0.034 (3)	0.030 (3)	0.038 (3)	−0.003 (2)	0.014 (2)	−0.002 (2)
C34	0.040 (3)	0.022 (3)	0.052 (4)	−0.004 (2)	0.015 (3)	−0.006 (3)
C35	0.039 (3)	0.033 (3)	0.041 (3)	0.000 (3)	0.006 (3)	0.008 (3)
C36	0.034 (3)	0.032 (3)	0.042 (3)	−0.001 (2)	0.007 (3)	−0.006 (3)
N1	0.045 (3)	0.021 (2)	0.037 (3)	0.004 (2)	0.014 (2)	0.003 (2)
N2	0.031 (2)	0.016 (2)	0.044 (3)	0.0005 (18)	0.011 (2)	0.0007 (19)
N3	0.034 (3)	0.024 (2)	0.051 (3)	−0.002 (2)	0.007 (2)	−0.002 (2)
N4	0.033 (2)	0.020 (2)	0.037 (2)	−0.0043 (19)	0.011 (2)	−0.0021 (19)
N5	0.040 (3)	0.022 (2)	0.044 (3)	0.001 (2)	0.013 (2)	0.000 (2)
N6	0.038 (3)	0.017 (2)	0.053 (3)	0.002 (2)	0.014 (2)	−0.002 (2)
N7	0.029 (2)	0.026 (3)	0.050 (3)	−0.001 (2)	0.000 (2)	−0.007 (2)
N8	0.031 (3)	0.033 (3)	0.051 (3)	−0.002 (2)	0.003 (2)	0.000 (2)
O1	0.041 (2)	0.0182 (19)	0.067 (3)	0.0049 (17)	0.011 (2)	−0.0009 (19)
O2	0.042 (2)	0.019 (2)	0.073 (3)	−0.0013 (18)	0.008 (2)	−0.002 (2)
O3	0.037 (2)	0.021 (2)	0.082 (3)	−0.0027 (18)	0.016 (2)	−0.001 (2)
O4	0.041 (2)	0.023 (2)	0.094 (4)	0.0031 (19)	0.010 (2)	−0.001 (2)
O5	0.041 (2)	0.020 (2)	0.065 (3)	−0.0001 (17)	0.008 (2)	−0.003 (2)
O6	0.042 (2)	0.053 (3)	0.053 (3)	0.003 (2)	0.011 (2)	0.018 (2)
O7	0.032 (2)	0.022 (2)	0.089 (3)	0.0034 (17)	0.009 (2)	−0.002 (2)
O8	0.033 (2)	0.020 (2)	0.073 (3)	−0.0020 (17)	0.008 (2)	−0.0052 (19)
O9	0.039 (2)	0.020 (2)	0.078 (3)	−0.0022 (17)	0.014 (2)	−0.004 (2)
O10	0.036 (2)	0.019 (2)	0.083 (3)	0.0057 (17)	0.012 (2)	0.002 (2)
O11	0.061 (3)	0.032 (2)	0.042 (2)	0.004 (2)	0.007 (2)	0.0069 (19)
O12	0.056 (3)	0.018 (2)	0.054 (3)	0.0039 (18)	0.015 (2)	−0.0057 (18)
O13	0.042 (3)	0.063 (3)	0.068 (3)	−0.002 (2)	0.025 (2)	0.007 (3)
O14	0.048 (3)	0.050 (3)	0.070 (3)	0.016 (2)	0.012 (2)	−0.006 (2)
O15	0.063 (3)	0.041 (3)	0.059 (3)	0.009 (2)	0.007 (2)	0.010 (2)
O16	0.045 (3)	0.063 (3)	0.092 (4)	−0.002 (2)	0.028 (3)	0.007 (3)
O17	0.085 (4)	0.041 (3)	0.067 (3)	0.013 (3)	0.010 (3)	0.018 (3)
O18	0.043 (2)	0.045 (3)	0.063 (3)	0.013 (2)	0.003 (2)	−0.007 (2)
O1W	0.044 (4)	0.044 (4)	0.101 (6)	−0.004 (3)	0.004 (4)	0.013 (4)

Geometric parameters (Å, º) top

Ag1—N2ⁱ	2.154 (4)	C14—C15	1.404 (8)
Ag1—N1	2.159 (4)	C15—C16	1.371 (8)
Ag1—Ag5	3.3746 (10)	C15—H15A	0.9300
Ag2—N3ⁱⁱ	2.198 (5)	C16—N3	1.333 (8)
Ag2—O5	2.230 (4)	C16—H16A	0.9300
Ag2—Ag3	3.3643 (10)	C17—N3	1.354 (8)
Ag3—O1	2.142 (4)	C17—C18	1.427 (8)
Ag3—O3	2.161 (4)	C17—H17A	0.9300
Ag3—O5	2.504 (4)	C18—H18A	0.9300
Ag3—Ag4	2.8244 (9)	C19—N4	1.345 (7)
Ag3—Ag6	3.3207 (10)	C19—C20	1.373 (7)
Ag4—O2	2.179 (4)	C19—H19A	0.9300
Ag4—O4	2.191 (4)	C20—C21	1.390 (7)
Ag4—O11	2.472 (4)	C20—H20A	0.9300
Ag4—Ag7	3.2916 (11)	C21—C22	1.396 (8)
Ag5—N5ⁱ	2.150 (5)	C21—C24	1.496 (8)
Ag5—N4	2.154 (4)	C22—C23	1.364 (8)
Ag5—O15ⁱⁱ	2.702 (5)	C22—H22A	0.9300
Ag6—O9	2.149 (4)	C23—N4	1.344 (7)
Ag6—O7	2.173 (4)	C23—H23A	0.9300
Ag6—O6	2.468 (4)	C24—O8	1.242 (6)
Ag6—Ag7	2.8043 (9)	C24—O7	1.260 (6)
Ag7—O10	2.158 (4)	C25—O10	1.248 (7)
Ag7—O8	2.180 (4)	C25—O9	1.265 (7)
Ag7—O12	2.641 (4)	C25—C26	1.508 (7)
Ag7—Ag8	3.0973 (9)	C26—C27	1.386 (7)
Ag8—N6ⁱⁱⁱ	2.164 (4)	C26—C30	1.395 (7)
Ag8—O12	2.182 (4)	C27—C28	1.367 (8)
C1—N1	1.347 (7)	C27—H27A	0.9300
C1—C2	1.371 (8)	C28—N5	1.337 (7)
C1—H1A	0.9300	C28—H28A	0.9300
C2—C3	1.395 (8)	C29—N5	1.345 (7)
C2—H2A	0.9300	C29—C30	1.361 (8)
C3—C4	1.379 (8)	C29—H29A	0.9300
C3—C6	1.500 (8)	C30—H30A	0.9300
C4—C5	1.384 (8)	C31—O11	1.231 (7)
C4—H4A	0.9300	C31—O12	1.265 (7)
C5—N1	1.339 (7)	C31—C32	1.522 (7)
C5—H5A	0.9300	C32—C36	1.387 (8)
C6—O2	1.248 (7)	C32—C33	1.387 (8)
C6—O1	1.265 (7)	C33—C34	1.385 (8)
C7—O3	1.242 (7)	C33—H33A	0.9300
C7—O4	1.244 (7)	C34—N6	1.354 (8)
C7—C8	1.505 (7)	C34—H34A	0.9300
C8—C12	1.383 (7)	C35—N6	1.339 (7)
C8—C9	1.400 (7)	C35—C36	1.390 (8)
C9—C10	1.359 (8)	C35—H35A	0.9300
C9—H9A	0.9300	C36—H36A	0.9300
C10—N2	1.348 (7)	N2—Ag1^iv	2.154 (4)
C10—H10A	0.9300	N3—Ag2^v	2.198 (5)
C11—N2	1.342 (7)	N5—Ag5^iv	2.150 (5)
C11—C12	1.361 (8)	N6—Ag8^vi	2.164 (4)
C11—H11A	0.9300	N7—O14	1.237 (6)
C12—H12A	0.9300	N7—O15	1.244 (6)
C13—O6	1.238 (7)	N7—O13	1.246 (6)
C13—O5	1.269 (7)	N8—O17	1.233 (6)
C13—C14	1.517 (8)	N8—O16	1.246 (7)
C14—C18	1.323 (8)	N8—O18	1.253 (6)

N2ⁱ—Ag1—N1	174.66 (17)	N3—C16—C15	123.5 (5)
N2ⁱ—Ag1—Ag5	106.07 (12)	N3—C16—H16A	118.3
N1—Ag1—Ag5	77.67 (12)	C15—C16—H16A	118.3
N3ⁱⁱ—Ag2—O5	160.41 (18)	N3—C17—C18	122.1 (5)
N3ⁱⁱ—Ag2—Ag3	124.16 (13)	N3—C17—H17A	119.0
O5—Ag2—Ag3	48.09 (10)	C18—C17—H17A	119.0
O1—Ag3—O3	162.63 (16)	C14—C18—C17	119.4 (5)
O1—Ag3—O5	112.27 (14)	C14—C18—H18A	120.3
O3—Ag3—O5	85.10 (14)	C17—C18—H18A	120.3
O1—Ag3—Ag4	82.33 (11)	N4—C19—C20	122.1 (5)
O3—Ag3—Ag4	80.35 (11)	N4—C19—H19A	119.0
O5—Ag3—Ag4	164.91 (9)	C20—C19—H19A	119.0
O1—Ag3—Ag6	112.72 (12)	C19—C20—C21	120.9 (5)
O3—Ag3—Ag6	69.02 (12)	C19—C20—H20A	119.6
O5—Ag3—Ag6	79.26 (10)	C21—C20—H20A	119.6
Ag4—Ag3—Ag6	99.04 (2)	C20—C21—C22	116.6 (5)
O1—Ag3—Ag2	71.38 (11)	C20—C21—C24	120.4 (5)
O3—Ag3—Ag2	125.80 (11)	C22—C21—C24	123.0 (5)
O5—Ag3—Ag2	41.52 (9)	C23—C22—C21	119.4 (5)
Ag4—Ag3—Ag2	153.50 (2)	C23—C22—H22A	120.3
Ag6—Ag3—Ag2	88.33 (2)	C21—C22—H22A	120.3
O2—Ag4—O4	159.94 (18)	N4—C23—C22	124.0 (5)
O2—Ag4—O11	103.94 (15)	N4—C23—H23A	118.0
O4—Ag4—O11	95.94 (15)	C22—C23—H23A	118.0
O2—Ag4—Ag3	81.62 (11)	O8—C24—O7	126.0 (5)
O4—Ag4—Ag3	83.38 (11)	O8—C24—C21	117.3 (5)
O11—Ag4—Ag3	146.30 (11)	O7—C24—C21	116.7 (5)
O2—Ag4—Ag7	118.37 (13)	O10—C25—O9	127.1 (5)
O4—Ag4—Ag7	71.82 (14)	O10—C25—C26	116.4 (5)
O11—Ag4—Ag7	67.49 (11)	O9—C25—C26	116.5 (5)
Ag3—Ag4—Ag7	80.52 (2)	C27—C26—C30	117.3 (5)
N5ⁱ—Ag5—N4	171.68 (17)	C27—C26—C25	120.6 (5)
N5ⁱ—Ag5—Ag1	79.87 (13)	C30—C26—C25	122.0 (5)
N4—Ag5—Ag1	108.24 (12)	C28—C27—C26	120.0 (5)
O9—Ag6—O7	163.67 (17)	C28—C27—H27A	120.0
O9—Ag6—O6	96.89 (16)	C26—C27—H27A	120.0
O7—Ag6—O6	98.96 (16)	N5—C28—C27	122.6 (5)
O9—Ag6—Ag7	83.33 (11)	N5—C28—H28A	118.7
O7—Ag6—Ag7	84.33 (11)	C27—C28—H28A	118.7
O6—Ag6—Ag7	152.96 (11)	N5—C29—C30	123.6 (5)
O9—Ag6—Ag3	115.54 (12)	N5—C29—H29A	118.2
O7—Ag6—Ag3	72.63 (13)	C30—C29—H29A	118.2
O6—Ag6—Ag3	75.24 (11)	C29—C30—C26	119.0 (5)
Ag7—Ag6—Ag3	80.29 (2)	C29—C30—H30A	120.5
O10—Ag7—O8	161.65 (15)	C26—C30—H30A	120.5
O10—Ag7—Ag6	81.73 (11)	O11—C31—O12	125.2 (5)
O8—Ag7—Ag6	79.97 (11)	O11—C31—C32	119.3 (5)
O10—Ag7—Ag8	73.02 (11)	O12—C31—C32	115.5 (5)
O8—Ag7—Ag8	125.32 (11)	C36—C32—C33	118.1 (5)
Ag6—Ag7—Ag8	154.36 (2)	C36—C32—C31	121.8 (5)
O10—Ag7—Ag4	114.52 (13)	C33—C32—C31	120.1 (5)
O8—Ag7—Ag4	67.86 (12)	C34—C33—C32	119.4 (5)
Ag6—Ag7—Ag4	100.15 (3)	C34—C33—H33A	120.3
Ag8—Ag7—Ag4	94.38 (2)	C32—C33—H33A	120.3
N6ⁱⁱⁱ—Ag8—O12	171.76 (17)	N6—C34—C33	122.5 (5)
N6ⁱⁱⁱ—Ag8—Ag7	125.28 (13)	N6—C34—H34A	118.7
O12—Ag8—Ag7	56.90 (11)	C33—C34—H34A	118.7
N1—C1—C2	123.9 (5)	N6—C35—C36	122.6 (5)
N1—C1—H1A	118.0	N6—C35—H35A	118.7
C2—C1—H1A	118.0	C36—C35—H35A	118.7
C1—C2—C3	118.6 (5)	C32—C36—C35	119.5 (5)
C1—C2—H2A	120.7	C32—C36—H36A	120.3
C3—C2—H2A	120.7	C35—C36—H36A	120.3
C4—C3—C2	117.7 (5)	C5—N1—C1	117.3 (5)
C4—C3—C6	120.8 (5)	C5—N1—Ag1	120.0 (4)
C2—C3—C6	121.4 (5)	C1—N1—Ag1	122.6 (4)
C3—C4—C5	120.3 (5)	C11—N2—C10	116.1 (5)
C3—C4—H4A	119.9	C11—N2—Ag1^iv	122.0 (4)
C5—C4—H4A	119.9	C10—N2—Ag1^iv	121.9 (3)
N1—C5—C4	122.1 (5)	C16—N3—C17	116.8 (5)
N1—C5—H5A	118.9	C16—N3—Ag2^v	119.1 (4)
C4—C5—H5A	118.9	C17—N3—Ag2^v	124.0 (4)
O2—C6—O1	126.4 (5)	C23—N4—C19	117.1 (5)
O2—C6—C3	117.7 (5)	C23—N4—Ag5	121.8 (3)
O1—C6—C3	115.9 (5)	C19—N4—Ag5	121.0 (4)
O3—C7—O4	126.8 (5)	C28—N5—C29	117.3 (5)
O3—C7—C8	115.6 (5)	C28—N5—Ag5^iv	120.3 (4)
O4—C7—C8	117.6 (5)	C29—N5—Ag5^iv	122.4 (4)
C12—C8—C9	116.7 (5)	C35—N6—C34	117.9 (5)
C12—C8—C7	121.2 (5)	C35—N6—Ag8^vi	125.5 (4)
C9—C8—C7	122.1 (5)	C34—N6—Ag8^vi	116.6 (4)
C10—C9—C8	119.5 (5)	O14—N7—O15	119.9 (5)
C10—C9—H9A	120.2	O14—N7—O13	120.4 (5)
C8—C9—H9A	120.2	O15—N7—O13	119.6 (5)
N2—C10—C9	123.9 (5)	O17—N8—O16	120.7 (5)
N2—C10—H10A	118.1	O17—N8—O18	120.2 (6)
C9—C10—H10A	118.1	O16—N8—O18	119.0 (5)
N2—C11—C12	123.6 (5)	C6—O1—Ag3	124.3 (4)
N2—C11—H11A	118.2	C6—O2—Ag4	123.7 (4)
C12—C11—H11A	118.2	C7—O3—Ag3	126.4 (4)
C11—C12—C8	120.2 (5)	C7—O4—Ag4	121.6 (4)
C11—C12—H12A	119.9	C13—O5—Ag2	118.1 (4)
C8—C12—H12A	119.9	C13—O5—Ag3	110.0 (3)
O6—C13—O5	125.9 (6)	Ag2—O5—Ag3	90.39 (14)
O6—C13—C14	118.9 (5)	C13—O6—Ag6	114.5 (3)
O5—C13—C14	115.1 (5)	C24—O7—Ag6	121.5 (4)
C18—C14—C15	118.8 (5)	C24—O8—Ag7	126.8 (4)
C18—C14—C13	122.0 (5)	C25—O9—Ag6	122.5 (4)
C15—C14—C13	119.2 (5)	C25—O10—Ag7	124.7 (4)
C16—C15—C14	119.3 (5)	C31—O11—Ag4	123.8 (4)
C16—C15—H15A	120.3	C31—O12—Ag8	113.9 (4)
C14—C15—H15A	120.3

Symmetry codes: (i) x, y−1, z; (ii) −x+1, y−1/2, −z+1/2; (iii) −x+2, y+1/2, −z+3/2; (iv) x, y+1, z; (v) −x+1, y+1/2, −z+1/2; (vi) −x+2, y−1/2, −z+3/2.

Experimental details

Crystal data
Chemical formula	[Ag₈(C₆H₄NO₂)₆(NO₃)₂]·0.5H₂O
M_r	1728.59
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	296
a, b, c (Å)	18.006 (4), 18.255 (4), 13.166 (3)
β (°)	104.017 (4)
V (Å³)	4199.0 (17)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	3.74
Crystal size (mm)	0.23 × 0.17 × 0.15

Data collection
Diffractometer	Bruker APEXII CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2008)
T_min, T_max	0.480, 0.604
No. of measured, independent and observed [I > 2σ(I)] reflections	21106, 7391, 6057
R_int	0.040
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.041, 0.106, 1.01
No. of reflections	7391
No. of parameters	637
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0468P)² + 11.8118P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	1.52, −1.68

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

References

Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Du, M. & Zhao, X. J. (2004). J. Mol. Struct. 694, 235–240. Web of Science CSD CrossRef CAS Google Scholar
Jaber, F., Charbonnier, F., Faure, R. & Petit-Ramel, M. Z. (1994). Z. Kristallogr. 209, 536–538. CrossRef CAS Web of Science Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Yang, Y.-Y., Huang, Z.-Q., Ouyang, G.-F. & Ng, S. W. (2004). Acta Cryst. E60, m1158–m1159. Web of Science CSD CrossRef IUCr Journals Google Scholar

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