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The title compound, {[Ag2(C8H16N2O6S2)(C6H12N4)2(H2O)2]·12H2O}n, consists of a two-dimensional AgI-hexa­methyl­ene­tetra­mine (6,3) net pillared by the 2,2'-(piperazine-1,4-di­yl)bis­(ethane­sulfonate) ligand, which lies across a centre of inversion. This compound can also be viewed as a (3,4)-connected topology by considering the hexa­methyl­ene­tetra­mine ligand and the AgI ion as the three- and four-connected nodes, respectively. There is a one-dimensional channel along the a axis accommodating a water chain assembled by the (H2O)12 clusters.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270110032609/sf3135sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270110032609/sf3135Isup2.hkl
Contains datablock I

CCDC reference: 781785

Comment top

Increasing attention is being paid to one-dimensional water chains because of their potential application in the biological transport of water, protons and ions (Ludwig, 2001; Konozo et al., 2002; Roux et al., 1999; Sreenivasulu et al., 2004). Recently, metal–organic frameworks (MOFs) (Eddaoudi et al., 2001), in which the isolated metal center or the metal clusters are joined through the organic linkers to form an extended structure, have become a promising research field due to the vital roles of MOFs in gas separation, asymmetric catalysis and enantio-selective separation. Meanwhile, the rational design of MOFs is conducive to the construction of a channel or cavity in the extended structure, providing a unique opportunity to encapsulate the water chains or water clusters. Among the family of MOFs, pillared-layer structures, integrating such merits [characterized by] of well defined pores and structural diversity by modification of the pillar module, have been extensively investigated (Ren et al., 2009). Herein, we report a three-dimensional pillared-layer framework, {[{AgIL1(H2O)}2L2].12H2O}n, (I), where L1 is hexamethylenetetramine and L2 is 2,2'-(piperazine-1,4-diyl)bis(ethanesulfonate), with a (3,4)-connected topology accommodating a water chain which is made up of (H2O)12 clusters in the one-dimensional channel.

The single-crystal X-ray diffraction study reveals that compound (I) is monoclinic and crystallizes in the centrosymmetric space group P21/n. There are one AgI ion, one L1 ligand, half a L2 ligand and seven water molecules in the asymmetric unit. All AgI ions show a distorted five-coordinate trigonal–biyramidal configuration (ζ = 0.6135) (Anthony et al., 1984) with N1, N4B and N3C (symmetry codes: B -1 + x, y, z; C -1/2 + x, 1/2 - y, -1/2 + z) atoms from three L1 ligands in equatorial positions and two O atoms in axial positions (Fig. 1). The coordinated water interacts with the AgI ion very weakly, with a bond length of 3.077 (2) Å. AgI—N bonds ranging from 2.334 (2) to 2.381 (2) Å and AgI—O one [2.514 (2) Å] are identical to the previously reported values (Liu et al., 2009) while the value of N—AgI—N is in the range 113.11 (8)–130.21 (8)°. All the piperazine rings in the L2 ligands adopt the most stable chair configuration, a finding similar to that of previous work (Sun et al., 2004). Since the AgI ion connects three L1 ligands and the L1 ligand coordinates with three AgI ions as well (Fig. 2a), the AgI–hexamethylenetetramine layer can be viewed as a two-dimensional (6, 3) net (Fig. 2b). It is worth noting that the adjacent Ag···Ag distances which are similar (about 5.983, 6.342 and 6.329 Å) show the hexagonal nature of the layer. As shown in Fig. 2(c), pillared by the L2 ligands, compound (I) can further be presented as a (3,4)-connected topology by considering the L1 ligand and AgI ion as a three-connected and four-connected node, respectively. It is of great interest to note that there is a one-dimensional channel along the a axis, providing an available void to investigate the water chain or water cluster.

The fascinating feature of the title compound, (I), is the self-assembly of the (H2O)12 clusters into a water chain within its one-dimensional channel of the (3, 4)-connected topology. As shown in Fig. 3(a), the (H2O)12 clusters are composed of the (H2O)10 clusters and two pendent water (O4Wx and O4Wxi) (Fig. 3b). Five water molecules (O1W, O2W, O5W, O6W and O7W) and their symmetric equivalents form a centrosymmetric decamer, which can also be viewed as two cyclic pentamers (Fig. 3c). The simplified structure of the (H2O)12 clusters is shown in Fig. 3(d). Besides the cyclic hexamers (O1W, O5W, O6W and their symmetric equivalents) with the chair conformation, which are also found in the previous structures concerning the (H2O)12 clusters (Song et al., 2007), the cyclic pentamers and octamers (O1W, O2W, O5W, O7W and their symmetric equivalents) are observed in these clusters. The hydrogen-bonding distances between two oxygen atoms of the water cluster are in the range 2.741–2.866 Å, resulting in an average of 2.805 Å, while the angles of the hydrogen bonds among (H2O)12 clusters span the range 150–178°. The 14 hydrogen bonds are mainly responsible for the stability of the (H2O)12 clusters. The individual (H2O)12 clusters are connected through O6W—H···O7W hydrogen bonds, generating an extended water chain which is further anchored into the one-dimensional channel by the hydrogen-bonding interactions between the guest water chain and host framework (O5W—H···N5, O6W—H···N2, O4W—H···O3 and O5W—H···N5).

Related literature top

For related literature, see: Anthony & Rao (1984); Eddaoudi et al. (2001); Konozo et al. (2002); Liu et al. (2009); Ludwig (2001); Ren et al. (2009); Roux & MacKinnon (1999); Song & Ma (2007); Sreenivasulu & Vittal (2004); Sun et al. (2004).

Experimental top

1, 4-Piperazinediethanesulfonic acid (0.5 mmol, 0.15 g) and hexamine (0.5 mmol, 0.07 g) were added to an aqueous solution (10 ml) of acetic acid silver (0.5 mmol, 0.084 g). After the mixture was stirred for 15 min, the precipitate was dissolved by dropwise addition of aqueous solution of NH3 (14M). Colorless crystals of complex (I) were obtained by evaporation of the solution for 2 d at room temperature.

Refinement top

All H atoms bound to C atoms were refined using a riding model, with a C—H distance of 0.97 Å and Uiso(H) = 1.2Ueq(C) for CH2 atoms. The water H atoms were located in a difference Fourier map and their positions were initially refined under the application of an O—H bond-length restraint of 0.85 (1) Å. In the final refinement, these H atoms were constrained to ride on their parent atom with Uiso(H) values set at 1.5Ueq(O).

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. A view of the local coordination of the AgI atom in (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. All H atoms and isolated water molecules have been omitted for clarity. [Symmetry codes: (i) x-1/2, -y+1/2, z-1/2; (ii) x-1, y, z; (v) -x+1, -y+1, -z+1.]
[Figure 2] Fig. 2. (a) The connective environment of the AgI ion and the L1 ligand; (b) the (6,3) net; (c) a three-dimensional (3,4)-connected topology.
[Figure 3] Fig. 3. (a) A water chain along the c axis; (b) the (H2O)12 clusters; (c) a cyclic pentamer; (d) the simplified structure of the (H2O)12 clusters. [Symmetry codes: (vi) -x+1, -y, -z+1.]
Poly[diaquabis(µ3-hexamethylenetetramine)[µ2-2,2'-(piperazine-1,4- diyl)bis(ethanesulfonato)]disilver(I)] top
Crystal data top
[Ag2(C8H16N2O6S2)(C6H12N4)2(H2O)2]·12H2OF(000) = 1088
Mr = 1048.70Dx = 1.663 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5910 reflections
a = 6.3902 (3) Åθ = 2.6–26.1°
b = 31.1619 (14) ŵ = 1.12 mm1
c = 10.5428 (5) ÅT = 165 K
β = 93.770 (1)°Block, colourless
V = 2094.85 (17) Å30.41 × 0.28 × 0.19 mm
Z = 2
Data collection top
Bruker Nonius KappaCCD
diffractometer
4128 independent reflections
Radiation source: fine-focus sealed tube3382 reflections with 2σ(I)
Graphite monochromatorRint = 0.030
ω scanθmax = 26.1°, θmin = 1.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 75
Tmin = 0.200, Tmax = 0.303k = 3833
11631 measured reflectionsl = 1213
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.094H-atom parameters constrained
S = 1.14 w = 1/[σ2(Fo2) + (0.0487P)2 + 0.091P]
where P = (Fo2 + 2Fc2)/3
4128 reflections(Δ/σ)max = 0.001
244 parametersΔρmax = 0.61 e Å3
0 restraintsΔρmin = 0.60 e Å3
Crystal data top
[Ag2(C8H16N2O6S2)(C6H12N4)2(H2O)2]·12H2OV = 2094.85 (17) Å3
Mr = 1048.70Z = 2
Monoclinic, P21/nMo Kα radiation
a = 6.3902 (3) ŵ = 1.12 mm1
b = 31.1619 (14) ÅT = 165 K
c = 10.5428 (5) Å0.41 × 0.28 × 0.19 mm
β = 93.770 (1)°
Data collection top
Bruker Nonius KappaCCD
diffractometer
4128 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3382 reflections with 2σ(I)
Tmin = 0.200, Tmax = 0.303Rint = 0.030
11631 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.094H-atom parameters constrained
S = 1.14Δρmax = 0.61 e Å3
4128 reflectionsΔρmin = 0.60 e Å3
244 parameters
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ag10.13588 (3)0.248329 (7)0.41464 (2)0.01581 (10)
S10.10125 (12)0.34865 (2)0.58448 (7)0.01485 (18)
N10.4592 (4)0.22064 (8)0.5056 (2)0.0134 (5)
N20.6664 (4)0.15842 (8)0.5784 (2)0.0130 (5)
N30.6578 (4)0.22205 (8)0.7126 (2)0.0119 (5)
N40.8448 (4)0.22375 (8)0.5163 (2)0.0124 (5)
N50.4014 (4)0.45794 (8)0.4905 (3)0.0186 (6)
O10.2183 (4)0.32226 (7)0.4994 (2)0.0228 (5)
O20.1796 (3)0.34385 (8)0.7168 (2)0.0221 (5)
O30.1264 (3)0.34186 (8)0.5677 (2)0.0217 (5)
C10.6677 (5)0.17417 (10)0.7101 (3)0.0135 (6)
H1A0.79700.16440.75830.016*
H1B0.54590.16220.75150.016*
C20.8479 (4)0.17603 (10)0.5185 (3)0.0140 (6)
H2A0.84890.16510.43040.017*
H2B0.97810.16610.56570.017*
C30.4737 (4)0.17325 (10)0.5065 (3)0.0142 (6)
H3A0.34970.16120.54540.017*
H3B0.47300.16260.41800.017*
C40.8426 (5)0.23877 (10)0.6501 (3)0.0133 (6)
H4A0.97240.22910.69820.016*
H4B0.84020.27050.65160.016*
C50.6465 (5)0.23781 (11)0.4468 (3)0.0146 (7)
H5A0.64030.26960.44630.018*
H5B0.64540.22790.35750.018*
C60.4646 (5)0.23582 (10)0.6391 (3)0.0136 (6)
H6A0.45600.26750.64000.016*
H6B0.34110.22440.68000.016*
C70.1393 (5)0.40274 (10)0.5410 (3)0.0195 (7)
H7A0.07140.40770.45510.023*
H7B0.07030.42160.60110.023*
C80.3716 (5)0.41479 (10)0.5409 (3)0.0209 (7)
H8A0.43580.41320.62880.025*
H8B0.44430.39380.48870.025*
C90.6255 (5)0.46459 (11)0.4722 (4)0.0237 (8)
H9A0.67340.44280.41210.028*
H9B0.70760.46080.55440.028*
C100.3351 (5)0.49094 (11)0.5792 (3)0.0226 (8)
H10A0.41380.48730.66260.027*
H10B0.18390.48750.59190.027*
O1W0.4568 (4)0.04603 (8)0.3106 (3)0.0380 (7)
H110.55580.04950.36750.057*
H120.44080.01910.30280.057*
O2W0.2790 (4)0.08554 (9)0.6904 (2)0.0432 (7)
H210.39150.07150.70740.065*
H220.25020.08290.61090.065*
O3W0.1161 (3)0.16216 (8)0.2719 (2)0.0248 (5)
H310.00860.16060.23890.037*
H320.19410.15740.21120.037*
O4W0.1721 (4)0.15996 (8)0.8148 (2)0.0278 (6)
H410.20080.13570.78330.042*
H420.21890.15940.89210.042*
O5W0.6491 (4)0.03766 (8)0.7523 (2)0.0368 (6)
H510.72320.04370.69060.055*
H520.73340.03620.81790.055*
O6W0.7489 (4)0.06993 (8)0.5165 (2)0.0333 (6)
H610.73540.09550.54290.050*
H620.87090.06790.48960.050*
O7W0.1417 (4)0.08731 (8)0.4260 (2)0.0327 (6)
H710.11530.10820.37560.049*
H720.24140.07370.39450.049*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.01266 (15)0.02147 (16)0.01334 (15)0.00151 (9)0.00130 (10)0.00385 (9)
S10.0164 (4)0.0137 (4)0.0145 (4)0.0032 (3)0.0017 (3)0.0015 (3)
N10.0111 (13)0.0178 (14)0.0116 (12)0.0012 (10)0.0022 (10)0.0005 (11)
N20.0107 (13)0.0163 (14)0.0120 (13)0.0006 (10)0.0015 (10)0.0010 (11)
N30.0114 (13)0.0142 (14)0.0103 (12)0.0004 (9)0.0026 (10)0.0007 (10)
N40.0108 (13)0.0144 (14)0.0123 (13)0.0006 (10)0.0023 (10)0.0000 (10)
N50.0145 (14)0.0134 (15)0.0286 (16)0.0020 (10)0.0061 (11)0.0004 (12)
O10.0290 (13)0.0165 (13)0.0235 (13)0.0022 (9)0.0067 (10)0.0045 (10)
O20.0229 (12)0.0312 (15)0.0125 (11)0.0038 (10)0.0021 (9)0.0040 (10)
O30.0177 (12)0.0247 (14)0.0224 (12)0.0078 (9)0.0001 (10)0.0041 (10)
C10.0128 (15)0.0168 (17)0.0114 (15)0.0005 (11)0.0032 (12)0.0014 (12)
C20.0110 (15)0.0179 (17)0.0131 (15)0.0015 (12)0.0019 (12)0.0015 (13)
C30.0112 (15)0.0165 (17)0.0149 (15)0.0029 (11)0.0011 (12)0.0019 (13)
C40.0117 (15)0.0137 (16)0.0145 (16)0.0021 (11)0.0017 (12)0.0008 (12)
C50.0120 (16)0.0194 (17)0.0122 (15)0.0005 (12)0.0007 (12)0.0054 (13)
C60.0124 (16)0.0161 (16)0.0124 (15)0.0023 (12)0.0026 (12)0.0014 (13)
C70.0182 (17)0.0126 (17)0.0277 (18)0.0016 (12)0.0014 (14)0.0042 (14)
C80.0181 (17)0.0125 (17)0.0322 (19)0.0017 (12)0.0018 (14)0.0020 (15)
C90.0177 (18)0.0165 (18)0.038 (2)0.0007 (13)0.0078 (15)0.0031 (15)
C100.0204 (18)0.0176 (18)0.031 (2)0.0022 (13)0.0110 (14)0.0022 (14)
O1W0.0381 (16)0.0325 (16)0.0434 (16)0.0002 (12)0.0034 (13)0.0059 (13)
O2W0.0542 (19)0.0450 (19)0.0308 (15)0.0137 (14)0.0050 (13)0.0033 (13)
O3W0.0193 (13)0.0339 (15)0.0216 (12)0.0009 (10)0.0033 (10)0.0018 (11)
O4W0.0242 (13)0.0327 (15)0.0261 (13)0.0052 (10)0.0011 (10)0.0001 (11)
O5W0.0437 (16)0.0348 (17)0.0314 (15)0.0011 (12)0.0015 (12)0.0013 (12)
O6W0.0302 (14)0.0249 (15)0.0455 (16)0.0019 (11)0.0081 (12)0.0033 (12)
O7W0.0330 (15)0.0315 (16)0.0341 (15)0.0079 (11)0.0060 (12)0.0025 (12)
Geometric parameters (Å, º) top
Ag1—N3i2.334 (2)C4—H4A0.9900
Ag1—N4ii2.336 (2)C4—H4B0.9900
Ag1—N12.381 (2)C5—H5A0.9900
Ag1—O12.514 (2)C5—H5B0.9900
S1—O21.458 (2)C6—H6A0.9900
S1—O11.459 (2)C6—H6B0.9900
S1—O31.469 (2)C7—C81.532 (4)
S1—C71.768 (3)C7—H7A0.9900
N1—C31.480 (4)C7—H7B0.9900
N1—C61.483 (4)C8—H8A0.9900
N1—C51.484 (4)C8—H8B0.9900
N2—C21.464 (4)C9—C10v1.515 (5)
N2—C11.472 (4)C9—H9A0.9900
N2—C31.477 (4)C9—H9B0.9900
N3—C61.478 (4)C10—C9v1.515 (5)
N3—C41.484 (4)C10—H10A0.9900
N3—C11.494 (4)C10—H10B0.9900
N3—Ag1iii2.334 (2)O1W—H110.8499
N4—C21.487 (4)O1W—H120.8503
N4—C51.487 (4)O2W—H210.8498
N4—C41.488 (4)O2W—H220.8499
N4—Ag1iv2.336 (2)O3W—H310.8500
N5—C81.463 (4)O3W—H320.8501
N5—C101.471 (4)O4W—H410.8497
N5—C91.472 (4)O4W—H420.8499
C1—H1A0.9900O5W—H510.8503
C1—H1B0.9900O5W—H520.8498
C2—H2A0.9900O6W—H610.8496
C2—H2B0.9900O6W—H620.8496
C3—H3A0.9900O7W—H710.8495
C3—H3B0.9900O7W—H720.8500
N3i—Ag1—N4ii130.21 (8)N2—C3—H3B109.3
N3i—Ag1—N1114.09 (8)N1—C3—H3B109.3
N4ii—Ag1—N1113.10 (8)H3A—C3—H3B108.0
N3i—Ag1—O186.47 (8)N3—C4—N4111.6 (2)
N4ii—Ag1—O1106.97 (8)N3—C4—H4A109.3
N1—Ag1—O191.88 (8)N4—C4—H4A109.3
O2—S1—O1111.86 (14)N3—C4—H4B109.3
O2—S1—O3112.06 (13)N4—C4—H4B109.3
O1—S1—O3112.87 (14)H4A—C4—H4B108.0
O2—S1—C7107.54 (15)N1—C5—N4111.9 (2)
O1—S1—C7107.05 (15)N1—C5—H5A109.2
O3—S1—C7104.95 (14)N4—C5—H5A109.2
C3—N1—C6108.3 (2)N1—C5—H5B109.2
C3—N1—C5108.1 (2)N4—C5—H5B109.2
C6—N1—C5108.2 (2)H5A—C5—H5B107.9
C3—N1—Ag1114.62 (17)N3—C6—N1111.8 (2)
C6—N1—Ag1103.42 (17)N3—C6—H6A109.2
C5—N1—Ag1113.80 (18)N1—C6—H6A109.2
C2—N2—C1109.1 (2)N3—C6—H6B109.2
C2—N2—C3108.6 (2)N1—C6—H6B109.2
C1—N2—C3109.4 (2)H6A—C6—H6B107.9
C6—N3—C4109.1 (2)C8—C7—S1112.6 (2)
C6—N3—C1108.4 (2)C8—C7—H7A109.1
C4—N3—C1107.9 (2)S1—C7—H7A109.1
C6—N3—Ag1iii105.42 (17)C8—C7—H7B109.1
C4—N3—Ag1iii111.32 (17)S1—C7—H7B109.1
C1—N3—Ag1iii114.61 (17)H7A—C7—H7B107.8
C2—N4—C5108.2 (2)N5—C8—C7112.0 (2)
C2—N4—C4107.5 (2)N5—C8—H8A109.2
C5—N4—C4108.3 (2)C7—C8—H8A109.2
C2—N4—Ag1iv108.94 (16)N5—C8—H8B109.2
C5—N4—Ag1iv110.82 (17)C7—C8—H8B109.2
C4—N4—Ag1iv112.92 (17)H8A—C8—H8B107.9
C8—N5—C10111.2 (3)N5—C9—C10v111.2 (3)
C8—N5—C9109.1 (2)N5—C9—H9A109.4
C10—N5—C9108.0 (2)C10v—C9—H9A109.4
S1—O1—Ag1129.13 (13)N5—C9—H9B109.4
N2—C1—N3110.6 (2)C10v—C9—H9B109.4
N2—C1—H1A109.5H9A—C9—H9B108.0
N3—C1—H1A109.5N5—C10—C9v110.5 (3)
N2—C1—H1B109.5N5—C10—H10A109.5
N3—C1—H1B109.5C9v—C10—H10A109.5
H1A—C1—H1B108.1N5—C10—H10B109.5
N2—C2—N4111.8 (2)C9v—C10—H10B109.5
N2—C2—H2A109.3H10A—C10—H10B108.1
N4—C2—H2A109.3H11—O1W—H12105.9
N2—C2—H2B109.3H21—O2W—H22106.4
N4—C2—H2B109.3H31—O3W—H32105.2
H2A—C2—H2B107.9H41—O4W—H42106.6
N2—C3—N1111.4 (2)H51—O5W—H52106.2
N2—C3—H3A109.3H61—O6W—H62107.2
N1—C3—H3A109.3H71—O7W—H72105.1
N3i—Ag1—N1—C3105.61 (19)Ag1—N1—C3—N2172.83 (17)
N4ii—Ag1—N1—C358.1 (2)C6—N3—C4—N457.9 (3)
O1—Ag1—N1—C3167.42 (19)C1—N3—C4—N459.6 (3)
N3i—Ag1—N1—C6136.70 (17)Ag1iii—N3—C4—N4173.81 (18)
N4ii—Ag1—N1—C659.64 (19)C2—N4—C4—N358.9 (3)
O1—Ag1—N1—C649.73 (18)C5—N4—C4—N357.8 (3)
N3i—Ag1—N1—C519.5 (2)Ag1iv—N4—C4—N3179.07 (18)
N4ii—Ag1—N1—C5176.79 (19)C3—N1—C5—N458.3 (3)
O1—Ag1—N1—C567.4 (2)C6—N1—C5—N458.9 (3)
O2—S1—O1—Ag194.93 (18)Ag1—N1—C5—N4173.19 (18)
O3—S1—O1—Ag132.5 (2)C2—N4—C5—N157.6 (3)
C7—S1—O1—Ag1147.51 (16)C4—N4—C5—N158.7 (3)
N3i—Ag1—O1—S1124.72 (17)Ag1iv—N4—C5—N1176.95 (19)
N4ii—Ag1—O1—S16.39 (19)C4—N3—C6—N158.3 (3)
N1—Ag1—O1—S1121.26 (17)C1—N3—C6—N158.9 (3)
C2—N2—C1—N359.7 (3)Ag1iii—N3—C6—N1177.90 (19)
C3—N2—C1—N359.0 (3)C3—N1—C6—N358.5 (3)
C6—N3—C1—N258.7 (3)C5—N1—C6—N358.4 (3)
C4—N3—C1—N259.3 (3)Ag1—N1—C6—N3179.45 (19)
Ag1iii—N3—C1—N2176.08 (17)O2—S1—C7—C865.7 (3)
C1—N2—C2—N459.9 (3)O1—S1—C7—C854.6 (3)
C3—N2—C2—N459.3 (3)O3—S1—C7—C8174.8 (2)
C5—N4—C2—N258.1 (3)C10—N5—C8—C770.7 (3)
C4—N4—C2—N258.7 (3)C9—N5—C8—C7170.2 (3)
Ag1iv—N4—C2—N2178.63 (18)S1—C7—C8—N5173.3 (2)
C2—N2—C3—N159.9 (3)C8—N5—C9—C10v179.6 (3)
C1—N2—C3—N159.1 (3)C10—N5—C9—C10v58.6 (4)
C6—N1—C3—N258.0 (3)C8—N5—C10—C9v177.9 (3)
C5—N1—C3—N259.1 (3)C9—N5—C10—C9v58.2 (4)
Symmetry codes: (i) x1/2, y+1/2, z1/2; (ii) x1, y, z; (iii) x+1/2, y+1/2, z+1/2; (iv) x+1, y, z; (v) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H11···O6W0.852.032.866 (4)166
O1W—H12···O5Wvi0.851.942.764 (4)164
O2W—H21···O5W0.851.992.836 (4)178
O2W—H22···O7W0.852.032.867 (3)168
O3W—H31···O2i0.852.002.818 (3)163
O3W—H32···O3vii0.851.962.797 (3)169
O4W—H41···O2W0.851.932.772 (4)171
O4W—H42···O3iii0.852.042.885 (3)172
O5W—H51···O6W0.852.032.794 (4)150
O5W—H52···N5iii0.852.062.897 (4)169
O6W—H61···N20.852.052.890 (4)170
O6W—H62···O7Wiv0.851.992.797 (3)158
O7W—H71···O3W0.852.012.841 (3)167
O7W—H72···O1W0.851.892.740 (3)175
Symmetry codes: (i) x1/2, y+1/2, z1/2; (iii) x+1/2, y+1/2, z+1/2; (iv) x+1, y, z; (vi) x+1, y, z+1; (vii) x+1/2, y+1/2, z1/2.

Experimental details

Crystal data
Chemical formula[Ag2(C8H16N2O6S2)(C6H12N4)2(H2O)2]·12H2O
Mr1048.70
Crystal system, space groupMonoclinic, P21/n
Temperature (K)165
a, b, c (Å)6.3902 (3), 31.1619 (14), 10.5428 (5)
β (°) 93.770 (1)
V3)2094.85 (17)
Z2
Radiation typeMo Kα
µ (mm1)1.12
Crystal size (mm)0.41 × 0.28 × 0.19
Data collection
DiffractometerBruker Nonius KappaCCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.200, 0.303
No. of measured, independent and
observed [2σ(I)] reflections
11631, 4128, 3382
Rint0.030
(sin θ/λ)max1)0.619
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.094, 1.14
No. of reflections4128
No. of parameters244
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.61, 0.60

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008).

Selected geometric parameters (Å, º) top
Ag1—N3i2.334 (2)Ag1—N12.381 (2)
Ag1—N4ii2.336 (2)Ag1—O12.514 (2)
N3i—Ag1—N4ii130.21 (8)N3i—Ag1—O186.47 (8)
N3i—Ag1—N1114.09 (8)N4ii—Ag1—O1106.97 (8)
N4ii—Ag1—N1113.10 (8)N1—Ag1—O191.88 (8)
Symmetry codes: (i) x1/2, y+1/2, z1/2; (ii) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H11···O6W0.852.032.866 (4)166.1
O1W—H12···O5Wiii0.851.942.764 (4)164.4
O2W—H21···O5W0.851.992.836 (4)177.8
O2W—H22···O7W0.852.032.867 (3)167.9
O3W—H31···O2i0.852.002.818 (3)162.5
O3W—H32···O3iv0.851.962.797 (3)169.3
O4W—H41···O2W0.851.932.772 (4)171.4
O4W—H42···O3v0.852.042.885 (3)171.6
O5W—H51···O6W0.852.032.794 (4)149.8
O5W—H52···N5v0.852.062.897 (4)168.6
O6W—H61···N20.852.052.890 (4)169.7
O6W—H62···O7Wvi0.851.992.797 (3)157.9
O7W—H71···O3W0.852.012.841 (3)167.1
O7W—H72···O1W0.851.892.740 (3)174.9
Symmetry codes: (i) x1/2, y+1/2, z1/2; (iii) x+1, y, z+1; (iv) x+1/2, y+1/2, z1/2; (v) x+1/2, y+1/2, z+1/2; (vi) x+1, y, z.
 

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