Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270110032609/sf3135sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270110032609/sf3135Isup2.hkl |
CCDC reference: 781785
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).
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.
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).
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).
[Ag2(C8H16N2O6S2)(C6H12N4)2(H2O)2]·12H2O | F(000) = 1088 |
Mr = 1048.70 | Dx = 1.663 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 5910 reflections |
a = 6.3902 (3) Å | θ = 2.6–26.1° |
b = 31.1619 (14) Å | µ = 1.12 mm−1 |
c = 10.5428 (5) Å | T = 165 K |
β = 93.770 (1)° | Block, colourless |
V = 2094.85 (17) Å3 | 0.41 × 0.28 × 0.19 mm |
Z = 2 |
Bruker Nonius KappaCCD diffractometer | 4128 independent reflections |
Radiation source: fine-focus sealed tube | 3382 reflections with 2σ(I) |
Graphite monochromator | Rint = 0.030 |
ω scan | θmax = 26.1°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −7→5 |
Tmin = 0.200, Tmax = 0.303 | k = −38→33 |
11631 measured reflections | l = −12→13 |
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)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.094 | H-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 parameters | Δρmax = 0.61 e Å−3 |
0 restraints | Δρmin = −0.60 e Å−3 |
[Ag2(C8H16N2O6S2)(C6H12N4)2(H2O)2]·12H2O | V = 2094.85 (17) Å3 |
Mr = 1048.70 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 6.3902 (3) Å | µ = 1.12 mm−1 |
b = 31.1619 (14) Å | T = 165 K |
c = 10.5428 (5) Å | 0.41 × 0.28 × 0.19 mm |
β = 93.770 (1)° |
Bruker Nonius KappaCCD diffractometer | 4128 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3382 reflections with 2σ(I) |
Tmin = 0.200, Tmax = 0.303 | Rint = 0.030 |
11631 measured reflections |
R[F2 > 2σ(F2)] = 0.030 | 0 restraints |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.14 | Δρmax = 0.61 e Å−3 |
4128 reflections | Δρmin = −0.60 e Å−3 |
244 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Ag1 | 0.13588 (3) | 0.248329 (7) | 0.41464 (2) | 0.01581 (10) | |
S1 | 0.10125 (12) | 0.34865 (2) | 0.58448 (7) | 0.01485 (18) | |
N1 | 0.4592 (4) | 0.22064 (8) | 0.5056 (2) | 0.0134 (5) | |
N2 | 0.6664 (4) | 0.15842 (8) | 0.5784 (2) | 0.0130 (5) | |
N3 | 0.6578 (4) | 0.22205 (8) | 0.7126 (2) | 0.0119 (5) | |
N4 | 0.8448 (4) | 0.22375 (8) | 0.5163 (2) | 0.0124 (5) | |
N5 | 0.4014 (4) | 0.45794 (8) | 0.4905 (3) | 0.0186 (6) | |
O1 | 0.2183 (4) | 0.32226 (7) | 0.4994 (2) | 0.0228 (5) | |
O2 | 0.1796 (3) | 0.34385 (8) | 0.7168 (2) | 0.0221 (5) | |
O3 | −0.1264 (3) | 0.34186 (8) | 0.5677 (2) | 0.0217 (5) | |
C1 | 0.6677 (5) | 0.17417 (10) | 0.7101 (3) | 0.0135 (6) | |
H1A | 0.7970 | 0.1644 | 0.7583 | 0.016* | |
H1B | 0.5459 | 0.1622 | 0.7515 | 0.016* | |
C2 | 0.8479 (4) | 0.17603 (10) | 0.5185 (3) | 0.0140 (6) | |
H2A | 0.8489 | 0.1651 | 0.4304 | 0.017* | |
H2B | 0.9781 | 0.1661 | 0.5657 | 0.017* | |
C3 | 0.4737 (4) | 0.17325 (10) | 0.5065 (3) | 0.0142 (6) | |
H3A | 0.3497 | 0.1612 | 0.5454 | 0.017* | |
H3B | 0.4730 | 0.1626 | 0.4180 | 0.017* | |
C4 | 0.8426 (5) | 0.23877 (10) | 0.6501 (3) | 0.0133 (6) | |
H4A | 0.9724 | 0.2291 | 0.6982 | 0.016* | |
H4B | 0.8402 | 0.2705 | 0.6516 | 0.016* | |
C5 | 0.6465 (5) | 0.23781 (11) | 0.4468 (3) | 0.0146 (7) | |
H5A | 0.6403 | 0.2696 | 0.4463 | 0.018* | |
H5B | 0.6454 | 0.2279 | 0.3575 | 0.018* | |
C6 | 0.4646 (5) | 0.23582 (10) | 0.6391 (3) | 0.0136 (6) | |
H6A | 0.4560 | 0.2675 | 0.6400 | 0.016* | |
H6B | 0.3411 | 0.2244 | 0.6800 | 0.016* | |
C7 | 0.1393 (5) | 0.40274 (10) | 0.5410 (3) | 0.0195 (7) | |
H7A | 0.0714 | 0.4077 | 0.4551 | 0.023* | |
H7B | 0.0703 | 0.4216 | 0.6011 | 0.023* | |
C8 | 0.3716 (5) | 0.41479 (10) | 0.5409 (3) | 0.0209 (7) | |
H8A | 0.4358 | 0.4132 | 0.6288 | 0.025* | |
H8B | 0.4443 | 0.3938 | 0.4887 | 0.025* | |
C9 | 0.6255 (5) | 0.46459 (11) | 0.4722 (4) | 0.0237 (8) | |
H9A | 0.6734 | 0.4428 | 0.4121 | 0.028* | |
H9B | 0.7076 | 0.4608 | 0.5544 | 0.028* | |
C10 | 0.3351 (5) | 0.49094 (11) | 0.5792 (3) | 0.0226 (8) | |
H10A | 0.4138 | 0.4873 | 0.6626 | 0.027* | |
H10B | 0.1839 | 0.4875 | 0.5919 | 0.027* | |
O1W | 0.4568 (4) | 0.04603 (8) | 0.3106 (3) | 0.0380 (7) | |
H11 | 0.5558 | 0.0495 | 0.3675 | 0.057* | |
H12 | 0.4408 | 0.0191 | 0.3028 | 0.057* | |
O2W | 0.2790 (4) | 0.08554 (9) | 0.6904 (2) | 0.0432 (7) | |
H21 | 0.3915 | 0.0715 | 0.7074 | 0.065* | |
H22 | 0.2502 | 0.0829 | 0.6109 | 0.065* | |
O3W | 0.1161 (3) | 0.16216 (8) | 0.2719 (2) | 0.0248 (5) | |
H31 | −0.0086 | 0.1606 | 0.2389 | 0.037* | |
H32 | 0.1941 | 0.1574 | 0.2112 | 0.037* | |
O4W | 0.1721 (4) | 0.15996 (8) | 0.8148 (2) | 0.0278 (6) | |
H41 | 0.2008 | 0.1357 | 0.7833 | 0.042* | |
H42 | 0.2189 | 0.1594 | 0.8921 | 0.042* | |
O5W | 0.6491 (4) | 0.03766 (8) | 0.7523 (2) | 0.0368 (6) | |
H51 | 0.7232 | 0.0437 | 0.6906 | 0.055* | |
H52 | 0.7334 | 0.0362 | 0.8179 | 0.055* | |
O6W | 0.7489 (4) | 0.06993 (8) | 0.5165 (2) | 0.0333 (6) | |
H61 | 0.7354 | 0.0955 | 0.5429 | 0.050* | |
H62 | 0.8709 | 0.0679 | 0.4896 | 0.050* | |
O7W | 0.1417 (4) | 0.08731 (8) | 0.4260 (2) | 0.0327 (6) | |
H71 | 0.1153 | 0.1082 | 0.3756 | 0.049* | |
H72 | 0.2414 | 0.0737 | 0.3945 | 0.049* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.01266 (15) | 0.02147 (16) | 0.01334 (15) | −0.00151 (9) | 0.00130 (10) | 0.00385 (9) |
S1 | 0.0164 (4) | 0.0137 (4) | 0.0145 (4) | −0.0032 (3) | 0.0017 (3) | 0.0015 (3) |
N1 | 0.0111 (13) | 0.0178 (14) | 0.0116 (12) | −0.0012 (10) | 0.0022 (10) | 0.0005 (11) |
N2 | 0.0107 (13) | 0.0163 (14) | 0.0120 (13) | −0.0006 (10) | 0.0015 (10) | −0.0010 (11) |
N3 | 0.0114 (13) | 0.0142 (14) | 0.0103 (12) | 0.0004 (9) | 0.0026 (10) | −0.0007 (10) |
N4 | 0.0108 (13) | 0.0144 (14) | 0.0123 (13) | −0.0006 (10) | 0.0023 (10) | 0.0000 (10) |
N5 | 0.0145 (14) | 0.0134 (15) | 0.0286 (16) | −0.0020 (10) | 0.0061 (11) | 0.0004 (12) |
O1 | 0.0290 (13) | 0.0165 (13) | 0.0235 (13) | −0.0022 (9) | 0.0067 (10) | −0.0045 (10) |
O2 | 0.0229 (12) | 0.0312 (15) | 0.0125 (11) | −0.0038 (10) | 0.0021 (9) | 0.0040 (10) |
O3 | 0.0177 (12) | 0.0247 (14) | 0.0224 (12) | −0.0078 (9) | −0.0001 (10) | 0.0041 (10) |
C1 | 0.0128 (15) | 0.0168 (17) | 0.0114 (15) | −0.0005 (11) | 0.0032 (12) | 0.0014 (12) |
C2 | 0.0110 (15) | 0.0179 (17) | 0.0131 (15) | 0.0015 (12) | 0.0019 (12) | −0.0015 (13) |
C3 | 0.0112 (15) | 0.0165 (17) | 0.0149 (15) | −0.0029 (11) | 0.0011 (12) | −0.0019 (13) |
C4 | 0.0117 (15) | 0.0137 (16) | 0.0145 (16) | −0.0021 (11) | 0.0017 (12) | −0.0008 (12) |
C5 | 0.0120 (16) | 0.0194 (17) | 0.0122 (15) | 0.0005 (12) | −0.0007 (12) | 0.0054 (13) |
C6 | 0.0124 (16) | 0.0161 (16) | 0.0124 (15) | 0.0023 (12) | 0.0026 (12) | −0.0014 (13) |
C7 | 0.0182 (17) | 0.0126 (17) | 0.0277 (18) | −0.0016 (12) | 0.0014 (14) | 0.0042 (14) |
C8 | 0.0181 (17) | 0.0125 (17) | 0.0322 (19) | −0.0017 (12) | 0.0018 (14) | 0.0020 (15) |
C9 | 0.0177 (18) | 0.0165 (18) | 0.038 (2) | −0.0007 (13) | 0.0078 (15) | −0.0031 (15) |
C10 | 0.0204 (18) | 0.0176 (18) | 0.031 (2) | −0.0022 (13) | 0.0110 (14) | −0.0022 (14) |
O1W | 0.0381 (16) | 0.0325 (16) | 0.0434 (16) | −0.0002 (12) | 0.0034 (13) | −0.0059 (13) |
O2W | 0.0542 (19) | 0.0450 (19) | 0.0308 (15) | 0.0137 (14) | 0.0050 (13) | −0.0033 (13) |
O3W | 0.0193 (13) | 0.0339 (15) | 0.0216 (12) | −0.0009 (10) | 0.0033 (10) | −0.0018 (11) |
O4W | 0.0242 (13) | 0.0327 (15) | 0.0261 (13) | 0.0052 (10) | −0.0011 (10) | −0.0001 (11) |
O5W | 0.0437 (16) | 0.0348 (17) | 0.0314 (15) | 0.0011 (12) | −0.0015 (12) | 0.0013 (12) |
O6W | 0.0302 (14) | 0.0249 (15) | 0.0455 (16) | −0.0019 (11) | 0.0081 (12) | −0.0033 (12) |
O7W | 0.0330 (15) | 0.0315 (16) | 0.0341 (15) | 0.0079 (11) | 0.0060 (12) | 0.0025 (12) |
Ag1—N3i | 2.334 (2) | C4—H4A | 0.9900 |
Ag1—N4ii | 2.336 (2) | C4—H4B | 0.9900 |
Ag1—N1 | 2.381 (2) | C5—H5A | 0.9900 |
Ag1—O1 | 2.514 (2) | C5—H5B | 0.9900 |
S1—O2 | 1.458 (2) | C6—H6A | 0.9900 |
S1—O1 | 1.459 (2) | C6—H6B | 0.9900 |
S1—O3 | 1.469 (2) | C7—C8 | 1.532 (4) |
S1—C7 | 1.768 (3) | C7—H7A | 0.9900 |
N1—C3 | 1.480 (4) | C7—H7B | 0.9900 |
N1—C6 | 1.483 (4) | C8—H8A | 0.9900 |
N1—C5 | 1.484 (4) | C8—H8B | 0.9900 |
N2—C2 | 1.464 (4) | C9—C10v | 1.515 (5) |
N2—C1 | 1.472 (4) | C9—H9A | 0.9900 |
N2—C3 | 1.477 (4) | C9—H9B | 0.9900 |
N3—C6 | 1.478 (4) | C10—C9v | 1.515 (5) |
N3—C4 | 1.484 (4) | C10—H10A | 0.9900 |
N3—C1 | 1.494 (4) | C10—H10B | 0.9900 |
N3—Ag1iii | 2.334 (2) | O1W—H11 | 0.8499 |
N4—C2 | 1.487 (4) | O1W—H12 | 0.8503 |
N4—C5 | 1.487 (4) | O2W—H21 | 0.8498 |
N4—C4 | 1.488 (4) | O2W—H22 | 0.8499 |
N4—Ag1iv | 2.336 (2) | O3W—H31 | 0.8500 |
N5—C8 | 1.463 (4) | O3W—H32 | 0.8501 |
N5—C10 | 1.471 (4) | O4W—H41 | 0.8497 |
N5—C9 | 1.472 (4) | O4W—H42 | 0.8499 |
C1—H1A | 0.9900 | O5W—H51 | 0.8503 |
C1—H1B | 0.9900 | O5W—H52 | 0.8498 |
C2—H2A | 0.9900 | O6W—H61 | 0.8496 |
C2—H2B | 0.9900 | O6W—H62 | 0.8496 |
C3—H3A | 0.9900 | O7W—H71 | 0.8495 |
C3—H3B | 0.9900 | O7W—H72 | 0.8500 |
N3i—Ag1—N4ii | 130.21 (8) | N2—C3—H3B | 109.3 |
N3i—Ag1—N1 | 114.09 (8) | N1—C3—H3B | 109.3 |
N4ii—Ag1—N1 | 113.10 (8) | H3A—C3—H3B | 108.0 |
N3i—Ag1—O1 | 86.47 (8) | N3—C4—N4 | 111.6 (2) |
N4ii—Ag1—O1 | 106.97 (8) | N3—C4—H4A | 109.3 |
N1—Ag1—O1 | 91.88 (8) | N4—C4—H4A | 109.3 |
O2—S1—O1 | 111.86 (14) | N3—C4—H4B | 109.3 |
O2—S1—O3 | 112.06 (13) | N4—C4—H4B | 109.3 |
O1—S1—O3 | 112.87 (14) | H4A—C4—H4B | 108.0 |
O2—S1—C7 | 107.54 (15) | N1—C5—N4 | 111.9 (2) |
O1—S1—C7 | 107.05 (15) | N1—C5—H5A | 109.2 |
O3—S1—C7 | 104.95 (14) | N4—C5—H5A | 109.2 |
C3—N1—C6 | 108.3 (2) | N1—C5—H5B | 109.2 |
C3—N1—C5 | 108.1 (2) | N4—C5—H5B | 109.2 |
C6—N1—C5 | 108.2 (2) | H5A—C5—H5B | 107.9 |
C3—N1—Ag1 | 114.62 (17) | N3—C6—N1 | 111.8 (2) |
C6—N1—Ag1 | 103.42 (17) | N3—C6—H6A | 109.2 |
C5—N1—Ag1 | 113.80 (18) | N1—C6—H6A | 109.2 |
C2—N2—C1 | 109.1 (2) | N3—C6—H6B | 109.2 |
C2—N2—C3 | 108.6 (2) | N1—C6—H6B | 109.2 |
C1—N2—C3 | 109.4 (2) | H6A—C6—H6B | 107.9 |
C6—N3—C4 | 109.1 (2) | C8—C7—S1 | 112.6 (2) |
C6—N3—C1 | 108.4 (2) | C8—C7—H7A | 109.1 |
C4—N3—C1 | 107.9 (2) | S1—C7—H7A | 109.1 |
C6—N3—Ag1iii | 105.42 (17) | C8—C7—H7B | 109.1 |
C4—N3—Ag1iii | 111.32 (17) | S1—C7—H7B | 109.1 |
C1—N3—Ag1iii | 114.61 (17) | H7A—C7—H7B | 107.8 |
C2—N4—C5 | 108.2 (2) | N5—C8—C7 | 112.0 (2) |
C2—N4—C4 | 107.5 (2) | N5—C8—H8A | 109.2 |
C5—N4—C4 | 108.3 (2) | C7—C8—H8A | 109.2 |
C2—N4—Ag1iv | 108.94 (16) | N5—C8—H8B | 109.2 |
C5—N4—Ag1iv | 110.82 (17) | C7—C8—H8B | 109.2 |
C4—N4—Ag1iv | 112.92 (17) | H8A—C8—H8B | 107.9 |
C8—N5—C10 | 111.2 (3) | N5—C9—C10v | 111.2 (3) |
C8—N5—C9 | 109.1 (2) | N5—C9—H9A | 109.4 |
C10—N5—C9 | 108.0 (2) | C10v—C9—H9A | 109.4 |
S1—O1—Ag1 | 129.13 (13) | N5—C9—H9B | 109.4 |
N2—C1—N3 | 110.6 (2) | C10v—C9—H9B | 109.4 |
N2—C1—H1A | 109.5 | H9A—C9—H9B | 108.0 |
N3—C1—H1A | 109.5 | N5—C10—C9v | 110.5 (3) |
N2—C1—H1B | 109.5 | N5—C10—H10A | 109.5 |
N3—C1—H1B | 109.5 | C9v—C10—H10A | 109.5 |
H1A—C1—H1B | 108.1 | N5—C10—H10B | 109.5 |
N2—C2—N4 | 111.8 (2) | C9v—C10—H10B | 109.5 |
N2—C2—H2A | 109.3 | H10A—C10—H10B | 108.1 |
N4—C2—H2A | 109.3 | H11—O1W—H12 | 105.9 |
N2—C2—H2B | 109.3 | H21—O2W—H22 | 106.4 |
N4—C2—H2B | 109.3 | H31—O3W—H32 | 105.2 |
H2A—C2—H2B | 107.9 | H41—O4W—H42 | 106.6 |
N2—C3—N1 | 111.4 (2) | H51—O5W—H52 | 106.2 |
N2—C3—H3A | 109.3 | H61—O6W—H62 | 107.2 |
N1—C3—H3A | 109.3 | H71—O7W—H72 | 105.1 |
N3i—Ag1—N1—C3 | −105.61 (19) | Ag1—N1—C3—N2 | −172.83 (17) |
N4ii—Ag1—N1—C3 | 58.1 (2) | C6—N3—C4—N4 | −57.9 (3) |
O1—Ag1—N1—C3 | 167.42 (19) | C1—N3—C4—N4 | 59.6 (3) |
N3i—Ag1—N1—C6 | 136.70 (17) | Ag1iii—N3—C4—N4 | −173.81 (18) |
N4ii—Ag1—N1—C6 | −59.64 (19) | C2—N4—C4—N3 | −58.9 (3) |
O1—Ag1—N1—C6 | 49.73 (18) | C5—N4—C4—N3 | 57.8 (3) |
N3i—Ag1—N1—C5 | 19.5 (2) | Ag1iv—N4—C4—N3 | −179.07 (18) |
N4ii—Ag1—N1—C5 | −176.79 (19) | C3—N1—C5—N4 | −58.3 (3) |
O1—Ag1—N1—C5 | −67.4 (2) | C6—N1—C5—N4 | 58.9 (3) |
O2—S1—O1—Ag1 | 94.93 (18) | Ag1—N1—C5—N4 | 173.19 (18) |
O3—S1—O1—Ag1 | −32.5 (2) | C2—N4—C5—N1 | 57.6 (3) |
C7—S1—O1—Ag1 | −147.51 (16) | C4—N4—C5—N1 | −58.7 (3) |
N3i—Ag1—O1—S1 | 124.72 (17) | Ag1iv—N4—C5—N1 | 176.95 (19) |
N4ii—Ag1—O1—S1 | −6.39 (19) | C4—N3—C6—N1 | 58.3 (3) |
N1—Ag1—O1—S1 | −121.26 (17) | C1—N3—C6—N1 | −58.9 (3) |
C2—N2—C1—N3 | 59.7 (3) | Ag1iii—N3—C6—N1 | 177.90 (19) |
C3—N2—C1—N3 | −59.0 (3) | C3—N1—C6—N3 | 58.5 (3) |
C6—N3—C1—N2 | 58.7 (3) | C5—N1—C6—N3 | −58.4 (3) |
C4—N3—C1—N2 | −59.3 (3) | Ag1—N1—C6—N3 | −179.45 (19) |
Ag1iii—N3—C1—N2 | 176.08 (17) | O2—S1—C7—C8 | 65.7 (3) |
C1—N2—C2—N4 | −59.9 (3) | O1—S1—C7—C8 | −54.6 (3) |
C3—N2—C2—N4 | 59.3 (3) | O3—S1—C7—C8 | −174.8 (2) |
C5—N4—C2—N2 | −58.1 (3) | C10—N5—C8—C7 | 70.7 (3) |
C4—N4—C2—N2 | 58.7 (3) | C9—N5—C8—C7 | −170.2 (3) |
Ag1iv—N4—C2—N2 | −178.63 (18) | S1—C7—C8—N5 | 173.3 (2) |
C2—N2—C3—N1 | −59.9 (3) | C8—N5—C9—C10v | −179.6 (3) |
C1—N2—C3—N1 | 59.1 (3) | C10—N5—C9—C10v | −58.6 (4) |
C6—N1—C3—N2 | −58.0 (3) | C8—N5—C10—C9v | 177.9 (3) |
C5—N1—C3—N2 | 59.1 (3) | C9—N5—C10—C9v | 58.2 (4) |
Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) x−1, y, z; (iii) x+1/2, −y+1/2, z+1/2; (iv) x+1, y, z; (v) −x+1, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H11···O6W | 0.85 | 2.03 | 2.866 (4) | 166 |
O1W—H12···O5Wvi | 0.85 | 1.94 | 2.764 (4) | 164 |
O2W—H21···O5W | 0.85 | 1.99 | 2.836 (4) | 178 |
O2W—H22···O7W | 0.85 | 2.03 | 2.867 (3) | 168 |
O3W—H31···O2i | 0.85 | 2.00 | 2.818 (3) | 163 |
O3W—H32···O3vii | 0.85 | 1.96 | 2.797 (3) | 169 |
O4W—H41···O2W | 0.85 | 1.93 | 2.772 (4) | 171 |
O4W—H42···O3iii | 0.85 | 2.04 | 2.885 (3) | 172 |
O5W—H51···O6W | 0.85 | 2.03 | 2.794 (4) | 150 |
O5W—H52···N5iii | 0.85 | 2.06 | 2.897 (4) | 169 |
O6W—H61···N2 | 0.85 | 2.05 | 2.890 (4) | 170 |
O6W—H62···O7Wiv | 0.85 | 1.99 | 2.797 (3) | 158 |
O7W—H71···O3W | 0.85 | 2.01 | 2.841 (3) | 167 |
O7W—H72···O1W | 0.85 | 1.89 | 2.740 (3) | 175 |
Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (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, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Ag2(C8H16N2O6S2)(C6H12N4)2(H2O)2]·12H2O |
Mr | 1048.70 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 165 |
a, b, c (Å) | 6.3902 (3), 31.1619 (14), 10.5428 (5) |
β (°) | 93.770 (1) |
V (Å3) | 2094.85 (17) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.12 |
Crystal size (mm) | 0.41 × 0.28 × 0.19 |
Data collection | |
Diffractometer | Bruker Nonius KappaCCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.200, 0.303 |
No. of measured, independent and observed [2σ(I)] reflections | 11631, 4128, 3382 |
Rint | 0.030 |
(sin θ/λ)max (Å−1) | 0.619 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.030, 0.094, 1.14 |
No. of reflections | 4128 |
No. of parameters | 244 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.61, −0.60 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008).
Ag1—N3i | 2.334 (2) | Ag1—N1 | 2.381 (2) |
Ag1—N4ii | 2.336 (2) | Ag1—O1 | 2.514 (2) |
N3i—Ag1—N4ii | 130.21 (8) | N3i—Ag1—O1 | 86.47 (8) |
N3i—Ag1—N1 | 114.09 (8) | N4ii—Ag1—O1 | 106.97 (8) |
N4ii—Ag1—N1 | 113.10 (8) | N1—Ag1—O1 | 91.88 (8) |
Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) x−1, y, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H11···O6W | 0.85 | 2.03 | 2.866 (4) | 166.1 |
O1W—H12···O5Wiii | 0.85 | 1.94 | 2.764 (4) | 164.4 |
O2W—H21···O5W | 0.85 | 1.99 | 2.836 (4) | 177.8 |
O2W—H22···O7W | 0.85 | 2.03 | 2.867 (3) | 167.9 |
O3W—H31···O2i | 0.85 | 2.00 | 2.818 (3) | 162.5 |
O3W—H32···O3iv | 0.85 | 1.96 | 2.797 (3) | 169.3 |
O4W—H41···O2W | 0.85 | 1.93 | 2.772 (4) | 171.4 |
O4W—H42···O3v | 0.85 | 2.04 | 2.885 (3) | 171.6 |
O5W—H51···O6W | 0.85 | 2.03 | 2.794 (4) | 149.8 |
O5W—H52···N5v | 0.85 | 2.06 | 2.897 (4) | 168.6 |
O6W—H61···N2 | 0.85 | 2.05 | 2.890 (4) | 169.7 |
O6W—H62···O7Wvi | 0.85 | 1.99 | 2.797 (3) | 157.9 |
O7W—H71···O3W | 0.85 | 2.01 | 2.841 (3) | 167.1 |
O7W—H72···O1W | 0.85 | 1.89 | 2.740 (3) | 174.9 |
Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (iii) −x+1, −y, −z+1; (iv) x+1/2, −y+1/2, z−1/2; (v) x+1/2, −y+1/2, z+1/2; (vi) x+1, y, z. |
Subscribe to Acta Crystallographica Section C: Structural Chemistry
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- Purchase subscription
- Reduced-price subscriptions
- If you have already subscribed, you may need to register
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).