metal-organic compounds
Poly[[aquatris(μ3-hexamethylenetetramine-κ3N,N′,N′′)tris(p-toluenesulfonato-κO)trisilver(I)] trihydrate]
aHeilongjiang Agricultural Vocational and Technical College, JiaMuSi, HeiLongJiang 154007, People's Republic of China
*Correspondence e-mail: hljwuhua@yahoo.com.cn
There are three AgI cations, three p-toluenesulfonate (pts) anions, three hexamethylenetetramine (hmt) molecules and four water molecules in the of the title coordination polymer, {[Ag3(C7H7O3S)3(C6H12N4)3(H2O)]·3H2O}n. Two of the pts anions show positional disorder of their O atoms in 0.60:0.40 and 0.50:0.50 ratios. The AgI ion is coordinated by three hmt molecules in an approximate trigonal–planar AgN3 arrangement. In each case, longer Ag—O bonds to a water molecule and a pts anion complete a distorted trigonal–bipyramidal AgN3O2 geometry for the metal ion. In the crystal, the bridging hmt molecules and pts ions generate a wave-like layer parallel to (001) and O—H⋯O hydrogen-bonding interactions consolidate the packing.
Related literature
For background to metal-coordination networks containing both sulfonate anions and N-bonded ligands, see: Côté & Shimizu (2003); Zhang et al. (2001).
Experimental
Crystal data
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Refinement
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Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2006); 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.
Supporting information
https://doi.org/10.1107/S1600536810048567/hb5739sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810048567/hb5739Isup2.hkl
An aqueous solution (10 ml) of p-toluenesulfonic acid (0.038 g, 0.3 mmol) was added to solid Ag2CO3 (0.041 g, 0.15 mmol) and stirred for several stirred for several minutes until no further CO2 was given off; and hexamethylenetetramine (0.028 g, 0.2 mmol) was added in. The white precipitate was dissolved by dropwise addition of an aqueous solution of NH3 (14 M). Colourless blocks were obtained by evaporation of the solution for several days at room temperature.
The disordered O atoms (O1, O2, O3, O7, and O9) of p-toluenesulfonate ligands split over two sites with a total ocuupancy of 1. C–bound H–atoms were geometrically positioned (C—H 0.93 Å) and refined using a riding model, with Uiso = 1.2Ueq (C). The water H atoms were located in a difference Fourier map and refined with Uiso(H)= 1.5Ueq(O).
Metal sulfonate complexes modified by different nitrogen-containing secondary ligands have been of great interest due to their abilities to form various structures, possible extended supramolecular system and good properties (Côté & Shimizu, 2003). Currently, there are some AgI sulfonate coordination polymers building from hexamethylenetetramine ligand because of its multidentate coordination mode (Zhang et al., 2001).
In the
of the title compound, C39H65Ag3N12O13S3, there are three AgI cations, three p-toluenesulfonate anions, three hexamethylenetetramine and four water molecules (Fig. 1). Ag1 cation is four-coordinated by three N atoms from three different hexamethylenetetramine ligands [Ag1—N1 = 2.362 (2), Ag1—N9i = 2.367 (2), and Ag1—N10ii = 2.388 (3)] and one O atom from one p-toluenesulfonate ligand [Ag1—O = 2.644 (6) Å] in a distorted tetrahedral coordination geometry. Ag2 cation is five-coordinated by three N atoms from three different hexamethylenetetramine ligands [Ag2—N5 = 2.347 (2), Ag2—N4 = 2.374 (2) and Ag2—N7ii = 2.365 (2) Å], one O atom from one p-toluenesulfonate ligand and one water molecule [Ag2—O4 = 2.622 (3) and Ag2—O1W = 2.622 (4) Å] in a trigonalbiyramid coordination geometry. Ag3 cation is also four-coordinated by three N atoms from hexamethylenetetramine ligands [Ag3—N3ii = 2.315 (3), Ag3—N8 = 2.358 (3), and Ag3—N11 = 2.394 (2) Å] and one p-toluenesulfonate ligand [Ag3—O9 = 2.438 (5) Å] in a distorted tetrahedral coordination geometry. The AgI cations are bridged by hexamethylenetetramine molecules in tridentate modes to generate a two dimensional wave like layer with the p-toluenesulfonate ligands hanged up and down (Fig. 2). The intermoleclar hydrogen bonding interactions consolidate the layer.For background to metal-coordination networks containing both sulfonate anions and N-bonded ligands, see: Côté & Shimizu (2003); Zhang et al. (2001).
Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell
CrysAlis CCD (Oxford Diffraction, 2006); data reduction: CrysAlis RED (Oxford Diffraction, 2006); 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).Fig. 1. The molecular structure of the title compound with displacement ellipsoids drawn at the 30% probability level. [Symmetry codes: (i) x - 1, y, z; (ii) -x + 3/2, y - 1/2, -z + 3/2]. | |
Fig. 2. The two dimensional wave like layer of the title compound. |
[Ag3(C7H7O3S)3(C6H12N4)3(H2O)]·3H2O | F(000) = 2704 |
Mr = 1329.82 | Dx = 1.779 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 11446 reflections |
a = 17.3181 (5) Å | θ = 3.0–29.3° |
b = 10.7028 (3) Å | µ = 1.37 mm−1 |
c = 26.9110 (11) Å | T = 293 K |
β = 95.657 (3)° | Block, colorless |
V = 4963.7 (3) Å3 | 0.30 × 0.25 × 0.22 mm |
Z = 4 |
Oxford Diffraction Gemini R Ultra diffractometer | 11446 independent reflections |
Radiation source: fine-focus sealed tube | 7890 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
Detector resolution: 10.0 pixels mm-1 | θmax = 29.3°, θmin = 3.0° |
ω scans | h = −23→19 |
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006) | k = −13→8 |
Tmin = 0.672, Tmax = 0.728 | l = −24→36 |
21413 measured reflections |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.097 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.99 | w = 1/[σ2(Fo2) + (0.054P)2] where P = (Fo2 + 2Fc2)/3 |
11446 reflections | (Δ/σ)max = 0.002 |
650 parameters | Δρmax = 0.90 e Å−3 |
12 restraints | Δρmin = −1.05 e Å−3 |
[Ag3(C7H7O3S)3(C6H12N4)3(H2O)]·3H2O | V = 4963.7 (3) Å3 |
Mr = 1329.82 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 17.3181 (5) Å | µ = 1.37 mm−1 |
b = 10.7028 (3) Å | T = 293 K |
c = 26.9110 (11) Å | 0.30 × 0.25 × 0.22 mm |
β = 95.657 (3)° |
Oxford Diffraction Gemini R Ultra diffractometer | 11446 independent reflections |
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006) | 7890 reflections with I > 2σ(I) |
Tmin = 0.672, Tmax = 0.728 | Rint = 0.021 |
21413 measured reflections |
R[F2 > 2σ(F2)] = 0.038 | 12 restraints |
wR(F2) = 0.097 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.99 | Δρmax = 0.90 e Å−3 |
11446 reflections | Δρmin = −1.05 e Å−3 |
650 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ag1 | 0.314657 (14) | 0.08332 (2) | 0.713161 (11) | 0.03692 (8) | |
Ag2 | 0.667686 (12) | 0.06405 (2) | 0.717069 (11) | 0.03702 (8) | |
Ag3 | 1.009181 (14) | 0.07397 (3) | 0.816707 (13) | 0.04627 (9) | |
C1 | 0.10904 (18) | 0.1984 (3) | 0.57691 (13) | 0.0351 (8) | |
C2 | 0.1425 (2) | 0.1533 (4) | 0.53604 (14) | 0.0463 (9) | |
H2 | 0.1955 | 0.1370 | 0.5383 | 0.056* | |
C3 | 0.0967 (3) | 0.1325 (4) | 0.49154 (15) | 0.0538 (11) | |
H3 | 0.1199 | 0.1021 | 0.4642 | 0.065* | |
C4 | 0.0182 (3) | 0.1555 (4) | 0.48654 (15) | 0.0530 (11) | |
C5 | −0.0141 (2) | 0.1996 (4) | 0.52791 (17) | 0.0565 (11) | |
H5 | −0.0672 | 0.2149 | 0.5256 | 0.068* | |
C6 | 0.0298 (2) | 0.2218 (4) | 0.57274 (15) | 0.0469 (10) | |
H6 | 0.0064 | 0.2523 | 0.6000 | 0.056* | |
C7 | −0.0295 (3) | 0.1341 (5) | 0.43795 (17) | 0.0801 (16) | |
H7A | −0.0827 | 0.1542 | 0.4414 | 0.120* | |
H7B | −0.0257 | 0.0480 | 0.4285 | 0.120* | |
H7C | −0.0108 | 0.1863 | 0.4127 | 0.120* | |
C8 | 1.03065 (19) | 0.2536 (4) | 0.96495 (12) | 0.0377 (8) | |
C9 | 1.0778 (2) | 0.1596 (4) | 0.98513 (14) | 0.0471 (10) | |
H9 | 1.0612 | 0.0769 | 0.9830 | 0.057* | |
C10 | 1.1501 (2) | 0.1887 (5) | 1.00856 (15) | 0.0591 (12) | |
H10 | 1.1816 | 0.1252 | 1.0227 | 0.071* | |
C11 | 1.1766 (2) | 0.3103 (6) | 1.01136 (16) | 0.0645 (13) | |
C12 | 1.1281 (3) | 0.4044 (5) | 0.99292 (17) | 0.0628 (12) | |
H12 | 1.1443 | 0.4871 | 0.9960 | 0.075* | |
C13 | 1.0550 (2) | 0.3767 (4) | 0.96963 (15) | 0.0506 (10) | |
H13 | 1.0223 | 0.4407 | 0.9572 | 0.061* | |
C14 | 1.2587 (3) | 0.3412 (8) | 1.0342 (2) | 0.105 (2) | |
H14A | 1.2669 | 0.4298 | 1.0328 | 0.157* | |
H14B | 1.2957 | 0.2992 | 1.0157 | 0.157* | |
H14C | 1.2651 | 0.3140 | 1.0683 | 0.157* | |
C15 | 0.6257 (2) | 0.1507 (3) | 0.89555 (14) | 0.0399 (8) | |
C16 | 0.5692 (2) | 0.0757 (4) | 0.91222 (15) | 0.0472 (9) | |
H16 | 0.5222 | 0.0651 | 0.8928 | 0.057* | |
C17 | 0.5822 (3) | 0.0165 (4) | 0.95755 (16) | 0.0578 (11) | |
H17 | 0.5434 | −0.0338 | 0.9685 | 0.069* | |
C18 | 0.6505 (3) | 0.0297 (4) | 0.98689 (17) | 0.0608 (12) | |
C19 | 0.7078 (3) | 0.1047 (5) | 0.96987 (19) | 0.0638 (12) | |
H19 | 0.7547 | 0.1148 | 0.9894 | 0.077* | |
C20 | 0.6959 (2) | 0.1644 (4) | 0.92434 (16) | 0.0514 (10) | |
H20 | 0.7349 | 0.2136 | 0.9131 | 0.062* | |
C21 | 0.6636 (4) | −0.0304 (6) | 1.03776 (19) | 0.0922 (18) | |
H21A | 0.7148 | −0.0104 | 1.0526 | 0.138* | |
H21B | 0.6585 | −0.1194 | 1.0344 | 0.138* | |
H21C | 0.6259 | 0.0003 | 1.0586 | 0.138* | |
C22 | 0.42034 (16) | 0.3050 (3) | 0.68223 (13) | 0.0289 (7) | |
H22A | 0.4236 | 0.3202 | 0.7179 | 0.035* | |
H22B | 0.3727 | 0.3426 | 0.6672 | 0.035* | |
C23 | 0.41350 (18) | 0.1495 (3) | 0.61824 (13) | 0.0340 (8) | |
H23A | 0.4117 | 0.0605 | 0.6113 | 0.041* | |
H23B | 0.3661 | 0.1866 | 0.6026 | 0.041* | |
C24 | 0.55120 (18) | 0.1488 (3) | 0.61999 (13) | 0.0369 (8) | |
H24A | 0.5952 | 0.1855 | 0.6057 | 0.044* | |
H24B | 0.5510 | 0.0598 | 0.6131 | 0.044* | |
C25 | 0.55931 (16) | 0.3047 (3) | 0.68477 (13) | 0.0290 (7) | |
H25A | 0.6039 | 0.3428 | 0.6716 | 0.035* | |
H25B | 0.5637 | 0.3189 | 0.7205 | 0.035* | |
C26 | 0.49138 (16) | 0.1145 (3) | 0.69615 (13) | 0.0302 (7) | |
H26A | 0.4958 | 0.1293 | 0.7319 | 0.036* | |
H26B | 0.4907 | 0.0249 | 0.6908 | 0.036* | |
C27 | 0.48138 (19) | 0.3383 (3) | 0.60693 (13) | 0.0386 (8) | |
H27A | 0.4345 | 0.3764 | 0.5910 | 0.046* | |
H27B | 0.5253 | 0.3755 | 0.5927 | 0.046* | |
C28 | 0.77641 (16) | 0.2991 (3) | 0.73890 (13) | 0.0299 (7) | |
H28A | 0.7571 | 0.2935 | 0.7715 | 0.036* | |
H28B | 0.7382 | 0.3438 | 0.7169 | 0.036* | |
C29 | 0.84460 (16) | 0.1052 (3) | 0.75281 (14) | 0.0316 (7) | |
H29A | 0.8264 | 0.0977 | 0.7856 | 0.038* | |
H29B | 0.8515 | 0.0216 | 0.7400 | 0.038* | |
C30 | 0.81468 (19) | 0.1839 (3) | 0.66969 (14) | 0.0384 (8) | |
H30A | 0.8211 | 0.1012 | 0.6559 | 0.046* | |
H30B | 0.7767 | 0.2283 | 0.6474 | 0.046* | |
C31 | 0.94465 (18) | 0.1821 (3) | 0.70622 (15) | 0.0424 (9) | |
H31A | 0.9943 | 0.2245 | 0.7080 | 0.051* | |
H31B | 0.9515 | 0.0990 | 0.6929 | 0.051* | |
C32 | 0.90727 (17) | 0.2980 (3) | 0.77631 (14) | 0.0347 (8) | |
H32A | 0.9563 | 0.3426 | 0.7797 | 0.042* | |
H32B | 0.8892 | 0.2916 | 0.8092 | 0.042* | |
C33 | 0.87806 (19) | 0.3752 (3) | 0.69322 (14) | 0.0385 (8) | |
H33A | 0.8409 | 0.4213 | 0.6709 | 0.046* | |
H33B | 0.9270 | 0.4199 | 0.6952 | 0.046* | |
C34 | 1.17915 (16) | 0.1141 (3) | 0.78134 (13) | 0.0294 (7) | |
H34A | 1.1504 | 0.1247 | 0.7488 | 0.035* | |
H34B | 1.1854 | 0.0252 | 0.7875 | 0.035* | |
C35 | 1.29800 (17) | 0.1580 (3) | 0.83154 (13) | 0.0333 (8) | |
H35A | 1.3052 | 0.0697 | 0.8388 | 0.040* | |
H35B | 1.3489 | 0.1960 | 0.8322 | 0.040* | |
C36 | 1.24515 (17) | 0.3086 (3) | 0.77130 (12) | 0.0267 (7) | |
H36A | 1.2953 | 0.3488 | 0.7711 | 0.032* | |
H36B | 1.2170 | 0.3202 | 0.7387 | 0.032* | |
C37 | 1.18014 (18) | 0.1554 (3) | 0.86903 (13) | 0.0340 (8) | |
H37A | 1.1516 | 0.1921 | 0.8946 | 0.041* | |
H37B | 1.1871 | 0.0672 | 0.8765 | 0.041* | |
C38 | 1.12622 (16) | 0.3044 (3) | 0.80919 (13) | 0.0297 (7) | |
H38A | 1.0974 | 0.3154 | 0.7767 | 0.036* | |
H38B | 1.0966 | 0.3426 | 0.8339 | 0.036* | |
C39 | 1.24502 (18) | 0.3481 (3) | 0.85897 (13) | 0.0334 (8) | |
H39A | 1.2953 | 0.3883 | 0.8597 | 0.040* | |
H39B | 1.2170 | 0.3865 | 0.8845 | 0.040* | |
O1' | 0.1480 (4) | 0.3411 (7) | 0.6499 (3) | 0.0744 (19)* | 0.50 |
O1 | 0.1172 (3) | 0.2996 (5) | 0.66542 (19) | 0.0419 (12)* | 0.50 |
O2' | 0.1309 (5) | 0.1218 (9) | 0.6678 (3) | 0.108 (3)* | 0.50 |
O2 | 0.1813 (3) | 0.1080 (5) | 0.6571 (2) | 0.0513 (14)* | 0.50 |
O1W | 0.70784 (18) | −0.0600 (3) | 0.63965 (14) | 0.0704 (10) | |
O3' | 0.2382 (4) | 0.1850 (9) | 0.6303 (3) | 0.096 (2)* | 0.50 |
O3 | 0.2377 (3) | 0.2902 (6) | 0.6240 (2) | 0.0566 (14)* | 0.50 |
O2W | 1.06791 (15) | 0.4929 (3) | 0.71250 (11) | 0.0543 (7) | |
O4 | 0.6619 (2) | 0.1634 (3) | 0.80569 (12) | 0.0881 (12) | |
O3W | 0.4316 (2) | 0.4268 (4) | 0.79689 (14) | 0.0760 (10) | |
O5 | 0.53010 (19) | 0.2102 (3) | 0.81959 (11) | 0.0735 (10) | |
O4W | 0.6873 (2) | 0.4746 (4) | 0.62992 (15) | 0.0830 (11) | |
O6 | 0.63193 (17) | 0.3562 (3) | 0.84465 (11) | 0.0600 (8) | |
O7' | 0.8959 (6) | 0.1405 (12) | 0.9688 (4) | 0.109 (3)* | 0.40 |
O7 | 0.9210 (3) | 0.0947 (5) | 0.9404 (2) | 0.0670 (14)* | 0.60 |
O8 | 0.89252 (18) | 0.3193 (4) | 0.93192 (15) | 0.0903 (12) | |
O9 | 0.9709 (3) | 0.2271 (5) | 0.8767 (2) | 0.0475 (13)* | 0.50 |
O9' | 0.9462 (6) | 0.1437 (11) | 0.8920 (4) | 0.124 (3)* | 0.50 |
S1 | 0.16466 (5) | 0.22358 (10) | 0.63466 (4) | 0.0441 (2) | |
S2 | 0.61121 (6) | 0.22628 (9) | 0.83691 (4) | 0.0481 (2) | |
S3 | 0.94276 (6) | 0.21884 (11) | 0.92946 (5) | 0.0599 (3) | |
N1 | 0.41778 (13) | 0.1693 (2) | 0.67309 (10) | 0.0260 (6) | |
N2 | 0.47982 (16) | 0.2043 (3) | 0.59677 (11) | 0.0382 (7) | |
N3 | 0.48729 (13) | 0.3647 (2) | 0.66152 (10) | 0.0280 (6) | |
N4 | 0.55957 (13) | 0.1691 (2) | 0.67493 (10) | 0.0262 (6) | |
N5 | 0.78586 (13) | 0.1722 (2) | 0.71920 (10) | 0.0280 (6) | |
N6 | 0.88871 (15) | 0.2504 (3) | 0.67246 (11) | 0.0395 (7) | |
N7 | 0.85025 (13) | 0.3702 (2) | 0.74346 (11) | 0.0298 (6) | |
N8 | 0.91990 (13) | 0.1713 (2) | 0.75711 (11) | 0.0331 (7) | |
N9 | 1.25674 (13) | 0.1725 (2) | 0.78090 (10) | 0.0258 (6) | |
N10 | 1.20165 (13) | 0.3685 (2) | 0.80957 (10) | 0.0253 (5) | |
N11 | 1.13457 (13) | 0.1694 (2) | 0.81992 (10) | 0.0276 (6) | |
N12 | 1.25592 (14) | 0.2151 (3) | 0.87016 (10) | 0.0328 (6) | |
H1WA | 0.6786 (17) | −0.097 (4) | 0.6160 (12) | 0.049* | |
H1WB | 0.7504 (15) | −0.094 (4) | 0.6411 (14) | 0.049* | |
H2WA | 1.042 (2) | 0.549 (3) | 0.6976 (14) | 0.049* | |
H2WB | 1.088 (2) | 0.448 (3) | 0.6915 (13) | 0.049* | |
H3WA | 0.425 (2) | 0.485 (3) | 0.8145 (14) | 0.049* | |
H3WB | 0.460 (2) | 0.375 (3) | 0.8101 (15) | 0.049* | |
H4WA | 0.7258 (14) | 0.504 (4) | 0.6231 (15) | 0.049* | |
H4WB | 0.6512 (16) | 0.522 (4) | 0.6144 (14) | 0.049* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.03300 (13) | 0.02596 (14) | 0.05419 (18) | −0.00300 (10) | 0.01635 (12) | −0.00403 (12) |
Ag2 | 0.02446 (12) | 0.02352 (13) | 0.06195 (19) | −0.00263 (9) | −0.00151 (11) | 0.00299 (13) |
Ag3 | 0.03051 (13) | 0.02299 (14) | 0.0846 (2) | 0.00125 (10) | 0.00192 (13) | 0.00676 (14) |
C1 | 0.0398 (17) | 0.0307 (19) | 0.034 (2) | 0.0014 (14) | −0.0005 (15) | 0.0044 (16) |
C2 | 0.048 (2) | 0.045 (2) | 0.046 (2) | −0.0009 (18) | 0.0078 (18) | −0.0004 (19) |
C3 | 0.082 (3) | 0.047 (3) | 0.034 (2) | −0.019 (2) | 0.012 (2) | −0.0011 (19) |
C4 | 0.074 (3) | 0.037 (2) | 0.045 (3) | −0.019 (2) | −0.012 (2) | 0.0112 (19) |
C5 | 0.041 (2) | 0.063 (3) | 0.062 (3) | −0.0016 (19) | −0.014 (2) | 0.005 (2) |
C6 | 0.0402 (18) | 0.053 (3) | 0.046 (2) | 0.0076 (17) | −0.0029 (17) | −0.001 (2) |
C7 | 0.113 (4) | 0.068 (4) | 0.052 (3) | −0.034 (3) | −0.027 (3) | 0.017 (3) |
C8 | 0.0446 (18) | 0.041 (2) | 0.0289 (19) | 0.0084 (16) | 0.0097 (15) | 0.0040 (17) |
C9 | 0.050 (2) | 0.051 (3) | 0.041 (2) | 0.0123 (18) | 0.0073 (18) | 0.0049 (19) |
C10 | 0.054 (2) | 0.082 (4) | 0.042 (2) | 0.026 (2) | 0.0055 (19) | 0.010 (2) |
C11 | 0.053 (2) | 0.101 (4) | 0.040 (3) | 0.002 (3) | 0.006 (2) | 0.001 (3) |
C12 | 0.069 (3) | 0.063 (3) | 0.057 (3) | −0.020 (2) | 0.012 (2) | 0.000 (2) |
C13 | 0.057 (2) | 0.045 (2) | 0.050 (2) | 0.0084 (19) | 0.0067 (19) | 0.009 (2) |
C14 | 0.070 (3) | 0.159 (7) | 0.083 (4) | −0.020 (4) | −0.004 (3) | −0.016 (4) |
C15 | 0.052 (2) | 0.0293 (19) | 0.040 (2) | 0.0067 (16) | 0.0141 (17) | −0.0023 (17) |
C16 | 0.060 (2) | 0.041 (2) | 0.041 (2) | −0.0041 (18) | 0.0108 (18) | 0.0017 (19) |
C17 | 0.084 (3) | 0.045 (3) | 0.047 (3) | 0.002 (2) | 0.018 (2) | 0.011 (2) |
C18 | 0.089 (3) | 0.046 (3) | 0.048 (3) | 0.026 (2) | 0.013 (2) | 0.008 (2) |
C19 | 0.068 (3) | 0.055 (3) | 0.066 (3) | 0.022 (2) | −0.008 (2) | 0.000 (2) |
C20 | 0.051 (2) | 0.046 (2) | 0.059 (3) | 0.0081 (18) | 0.013 (2) | 0.002 (2) |
C21 | 0.141 (5) | 0.075 (4) | 0.058 (3) | 0.022 (4) | 0.001 (3) | 0.029 (3) |
C22 | 0.0247 (14) | 0.0204 (16) | 0.043 (2) | 0.0010 (12) | 0.0083 (14) | −0.0054 (14) |
C23 | 0.0317 (16) | 0.0312 (19) | 0.038 (2) | −0.0032 (14) | −0.0018 (15) | −0.0071 (16) |
C24 | 0.0321 (16) | 0.036 (2) | 0.045 (2) | 0.0018 (14) | 0.0124 (15) | −0.0059 (17) |
C25 | 0.0249 (14) | 0.0228 (16) | 0.0388 (19) | −0.0020 (12) | 0.0007 (13) | 0.0013 (15) |
C26 | 0.0277 (15) | 0.0214 (16) | 0.042 (2) | −0.0001 (12) | 0.0031 (14) | 0.0052 (15) |
C27 | 0.0376 (17) | 0.036 (2) | 0.041 (2) | −0.0004 (15) | 0.0019 (16) | 0.0133 (17) |
C28 | 0.0247 (14) | 0.0209 (16) | 0.045 (2) | −0.0018 (12) | 0.0051 (14) | −0.0032 (15) |
C29 | 0.0284 (15) | 0.0175 (15) | 0.049 (2) | −0.0039 (12) | 0.0036 (14) | 0.0021 (15) |
C30 | 0.0391 (17) | 0.0300 (19) | 0.047 (2) | −0.0062 (14) | 0.0077 (16) | −0.0074 (17) |
C31 | 0.0277 (16) | 0.0317 (19) | 0.070 (3) | 0.0022 (14) | 0.0169 (17) | −0.0070 (19) |
C32 | 0.0290 (15) | 0.0192 (16) | 0.054 (2) | −0.0006 (12) | −0.0035 (15) | −0.0016 (16) |
C33 | 0.0324 (16) | 0.0243 (17) | 0.060 (2) | −0.0059 (14) | 0.0101 (16) | 0.0052 (17) |
C34 | 0.0310 (15) | 0.0217 (16) | 0.0355 (19) | −0.0044 (12) | 0.0032 (14) | −0.0023 (14) |
C35 | 0.0260 (15) | 0.0293 (18) | 0.044 (2) | 0.0036 (13) | −0.0010 (14) | 0.0061 (16) |
C36 | 0.0279 (14) | 0.0200 (16) | 0.0319 (18) | −0.0024 (12) | 0.0017 (13) | 0.0038 (14) |
C37 | 0.0413 (18) | 0.0284 (18) | 0.0333 (19) | −0.0011 (14) | 0.0083 (15) | 0.0053 (15) |
C38 | 0.0249 (14) | 0.0253 (17) | 0.0388 (19) | 0.0015 (12) | 0.0022 (13) | 0.0016 (15) |
C39 | 0.0340 (16) | 0.0301 (18) | 0.036 (2) | −0.0040 (14) | 0.0019 (14) | −0.0043 (16) |
O1W | 0.0576 (18) | 0.065 (2) | 0.087 (3) | 0.0022 (16) | 0.0022 (17) | −0.0355 (19) |
O2W | 0.0479 (16) | 0.061 (2) | 0.0547 (19) | 0.0042 (14) | 0.0067 (13) | −0.0006 (16) |
O4 | 0.155 (3) | 0.054 (2) | 0.067 (2) | −0.031 (2) | 0.069 (2) | −0.0153 (17) |
O3W | 0.072 (2) | 0.080 (3) | 0.072 (3) | −0.0049 (19) | −0.0161 (19) | −0.003 (2) |
O5 | 0.088 (2) | 0.079 (2) | 0.0488 (18) | −0.0349 (19) | −0.0164 (16) | 0.0206 (17) |
O4W | 0.064 (2) | 0.089 (3) | 0.098 (3) | −0.003 (2) | 0.018 (2) | 0.047 (2) |
O6 | 0.088 (2) | 0.0288 (15) | 0.0622 (19) | −0.0083 (14) | 0.0010 (15) | 0.0022 (14) |
O8 | 0.0663 (19) | 0.076 (3) | 0.123 (3) | 0.0312 (18) | −0.021 (2) | −0.020 (2) |
S1 | 0.0402 (5) | 0.0503 (6) | 0.0398 (5) | 0.0153 (4) | −0.0062 (4) | −0.0039 (5) |
S2 | 0.0757 (6) | 0.0340 (5) | 0.0365 (5) | −0.0147 (5) | 0.0151 (5) | −0.0004 (4) |
S3 | 0.0599 (6) | 0.0515 (7) | 0.0640 (7) | 0.0196 (5) | −0.0161 (5) | −0.0143 (6) |
N1 | 0.0223 (11) | 0.0190 (13) | 0.0370 (16) | −0.0010 (10) | 0.0041 (11) | −0.0018 (12) |
N2 | 0.0402 (15) | 0.0409 (18) | 0.0337 (16) | 0.0007 (13) | 0.0051 (13) | −0.0021 (14) |
N3 | 0.0253 (12) | 0.0176 (13) | 0.0416 (17) | −0.0008 (10) | 0.0059 (11) | 0.0019 (12) |
N4 | 0.0200 (11) | 0.0194 (13) | 0.0393 (16) | −0.0001 (10) | 0.0037 (11) | 0.0003 (12) |
N5 | 0.0218 (11) | 0.0210 (13) | 0.0412 (17) | −0.0042 (10) | 0.0027 (11) | −0.0024 (12) |
N6 | 0.0364 (14) | 0.0339 (17) | 0.0500 (19) | −0.0061 (13) | 0.0140 (13) | −0.0014 (15) |
N7 | 0.0211 (12) | 0.0187 (13) | 0.0487 (18) | −0.0009 (10) | −0.0002 (12) | −0.0014 (13) |
N8 | 0.0220 (12) | 0.0204 (14) | 0.057 (2) | 0.0025 (10) | 0.0030 (12) | −0.0024 (13) |
N9 | 0.0237 (12) | 0.0189 (13) | 0.0351 (16) | 0.0001 (10) | 0.0049 (11) | 0.0012 (12) |
N10 | 0.0238 (11) | 0.0223 (13) | 0.0295 (15) | −0.0006 (10) | 0.0011 (11) | −0.0004 (12) |
N11 | 0.0242 (12) | 0.0230 (14) | 0.0358 (16) | −0.0018 (10) | 0.0036 (11) | 0.0014 (12) |
N12 | 0.0312 (13) | 0.0338 (16) | 0.0325 (16) | 0.0013 (12) | −0.0016 (12) | 0.0067 (13) |
Ag1—N1 | 2.362 (2) | C28—N7 | 1.483 (4) |
Ag1—N9i | 2.367 (3) | C28—H28A | 0.9700 |
Ag1—N10ii | 2.388 (3) | C28—H28B | 0.9700 |
Ag2—N5 | 2.347 (2) | C29—N8 | 1.478 (4) |
Ag2—N7ii | 2.365 (3) | C29—N5 | 1.478 (4) |
Ag2—N4 | 2.374 (2) | C29—H29A | 0.9700 |
Ag3—N3ii | 2.315 (3) | C29—H29B | 0.9700 |
Ag3—N8 | 2.358 (3) | C30—N6 | 1.462 (4) |
Ag3—N11 | 2.394 (2) | C30—N5 | 1.474 (4) |
Ag3—O9 | 2.438 (5) | C30—H30A | 0.9700 |
Ag3—O9' | 2.507 (11) | C30—H30B | 0.9700 |
C1—C2 | 1.380 (5) | C31—N6 | 1.458 (5) |
C1—C6 | 1.389 (5) | C31—N8 | 1.479 (5) |
C1—S1 | 1.767 (3) | C31—H31A | 0.9700 |
C2—C3 | 1.388 (6) | C31—H31B | 0.9700 |
C2—H2 | 0.9300 | C32—N8 | 1.475 (4) |
C3—C4 | 1.375 (6) | C32—N7 | 1.477 (4) |
C3—H3 | 0.9300 | C32—H32A | 0.9700 |
C4—C5 | 1.378 (6) | C32—H32B | 0.9700 |
C4—C7 | 1.494 (6) | C33—N6 | 1.467 (4) |
C5—C6 | 1.381 (6) | C33—N7 | 1.480 (4) |
C5—H5 | 0.9300 | C33—H33A | 0.9700 |
C6—H6 | 0.9300 | C33—H33B | 0.9700 |
C7—H7A | 0.9600 | C34—N11 | 1.477 (4) |
C7—H7B | 0.9600 | C34—N9 | 1.483 (4) |
C7—H7C | 0.9600 | C34—H34A | 0.9700 |
C8—C9 | 1.374 (5) | C34—H34B | 0.9700 |
C8—C13 | 1.385 (5) | C35—N12 | 1.461 (4) |
C8—S3 | 1.755 (4) | C35—N9 | 1.483 (4) |
C9—C10 | 1.381 (6) | C35—H35A | 0.9700 |
C9—H9 | 0.9300 | C35—H35B | 0.9700 |
C10—C11 | 1.379 (7) | C36—N10 | 1.481 (4) |
C10—H10 | 0.9300 | C36—N9 | 1.489 (4) |
C11—C12 | 1.372 (7) | C36—H36A | 0.9700 |
C11—C14 | 1.529 (6) | C36—H36B | 0.9700 |
C12—C13 | 1.388 (6) | C37—N12 | 1.458 (4) |
C12—H12 | 0.9300 | C37—N11 | 1.479 (4) |
C13—H13 | 0.9300 | C37—H37A | 0.9700 |
C14—H14A | 0.9600 | C37—H37B | 0.9700 |
C14—H14B | 0.9600 | C38—N10 | 1.475 (4) |
C14—H14C | 0.9600 | C38—N11 | 1.477 (4) |
C15—C16 | 1.374 (5) | C38—H38A | 0.9700 |
C15—C20 | 1.384 (5) | C38—H38B | 0.9700 |
C15—S2 | 1.769 (4) | C39—N12 | 1.463 (4) |
C16—C17 | 1.373 (6) | C39—N10 | 1.477 (4) |
C16—H16 | 0.9300 | C39—H39A | 0.9700 |
C17—C18 | 1.364 (6) | C39—H39B | 0.9700 |
C17—H17 | 0.9300 | O1'—O1 | 0.837 (7) |
C18—C19 | 1.388 (7) | O1'—S1 | 1.363 (7) |
C18—C21 | 1.509 (6) | O1—S1 | 1.469 (5) |
C19—C20 | 1.379 (6) | O2'—O2 | 0.956 (9) |
C19—H19 | 0.9300 | O2'—S1 | 1.558 (10) |
C20—H20 | 0.9300 | O2—S1 | 1.394 (6) |
C21—H21A | 0.9600 | O2—O3' | 1.520 (10) |
C21—H21B | 0.9600 | O1W—H1WA | 0.87 (2) |
C21—H21C | 0.9600 | O1W—H1WB | 0.82 (2) |
C22—N1 | 1.473 (4) | O3'—O3 | 1.139 (9) |
C22—N3 | 1.480 (4) | O3'—S1 | 1.354 (8) |
C22—H22A | 0.9700 | O3—S1 | 1.504 (6) |
C22—H22B | 0.9700 | O2W—H2WA | 0.83 (2) |
C23—N2 | 1.459 (4) | O2W—H2WB | 0.84 (2) |
C23—N1 | 1.486 (4) | O4—S2 | 1.441 (3) |
C23—H23A | 0.9700 | O3W—H3WA | 0.80 (2) |
C23—H23B | 0.9700 | O3W—H3WB | 0.80 (2) |
C24—N2 | 1.456 (4) | O5—S2 | 1.446 (3) |
C24—N4 | 1.487 (4) | O4W—H4WA | 0.78 (2) |
C24—H24A | 0.9700 | O4W—H4WB | 0.88 (2) |
C24—H24B | 0.9700 | O6—S2 | 1.446 (3) |
C25—N4 | 1.476 (4) | O7'—O7 | 1.036 (11) |
C25—N3 | 1.485 (4) | O7'—S3 | 1.628 (12) |
C25—H25A | 0.9700 | O7—S3 | 1.420 (6) |
C25—H25B | 0.9700 | O7—O9' | 1.509 (12) |
C26—N4 | 1.481 (4) | O8—S3 | 1.389 (3) |
C26—N1 | 1.482 (4) | O9—O9' | 1.089 (11) |
C26—H26A | 0.9700 | O9—S3 | 1.549 (5) |
C26—H26B | 0.9700 | O9'—S3 | 1.296 (11) |
C27—N2 | 1.460 (5) | N3—Ag3iii | 2.315 (3) |
C27—N3 | 1.489 (4) | N7—Ag2iii | 2.365 (3) |
C27—H27A | 0.9700 | N9—Ag1iv | 2.367 (2) |
C27—H27B | 0.9700 | N10—Ag1iii | 2.388 (3) |
C28—N5 | 1.474 (4) | ||
N1—Ag1—N9i | 126.27 (9) | N9—C34—H34B | 109.2 |
N1—Ag1—N10ii | 109.49 (8) | H34A—C34—H34B | 107.9 |
N9i—Ag1—N10ii | 122.48 (8) | N12—C35—N9 | 112.4 (2) |
N5—Ag2—N7ii | 125.05 (9) | N12—C35—H35A | 109.1 |
N5—Ag2—N4 | 115.03 (9) | N9—C35—H35A | 109.1 |
N7ii—Ag2—N4 | 119.83 (8) | N12—C35—H35B | 109.1 |
N3ii—Ag3—N8 | 126.79 (9) | N9—C35—H35B | 109.1 |
N3ii—Ag3—N11 | 113.74 (8) | H35A—C35—H35B | 107.9 |
N8—Ag3—N11 | 111.58 (9) | N10—C36—N9 | 111.9 (2) |
N3ii—Ag3—O9 | 119.04 (15) | N10—C36—H36A | 109.2 |
N8—Ag3—O9 | 87.16 (14) | N9—C36—H36A | 109.2 |
N11—Ag3—O9 | 89.64 (14) | N10—C36—H36B | 109.2 |
N3ii—Ag3—O9' | 94.9 (3) | N9—C36—H36B | 109.2 |
N8—Ag3—O9' | 96.3 (2) | H36A—C36—H36B | 107.9 |
N11—Ag3—O9' | 108.0 (3) | N12—C37—N11 | 112.0 (3) |
O9—Ag3—O9' | 25.4 (3) | N12—C37—H37A | 109.2 |
C2—C1—C6 | 119.2 (3) | N11—C37—H37A | 109.2 |
C2—C1—S1 | 121.3 (3) | N12—C37—H37B | 109.2 |
C6—C1—S1 | 119.5 (3) | N11—C37—H37B | 109.2 |
C1—C2—C3 | 119.6 (4) | H37A—C37—H37B | 107.9 |
C1—C2—H2 | 120.2 | N10—C38—N11 | 112.6 (2) |
C3—C2—H2 | 120.2 | N10—C38—H38A | 109.1 |
C4—C3—C2 | 122.1 (4) | N11—C38—H38A | 109.1 |
C4—C3—H3 | 119.0 | N10—C38—H38B | 109.1 |
C2—C3—H3 | 119.0 | N11—C38—H38B | 109.1 |
C3—C4—C5 | 117.3 (4) | H38A—C38—H38B | 107.8 |
C3—C4—C7 | 121.0 (4) | N12—C39—N10 | 111.9 (3) |
C5—C4—C7 | 121.7 (4) | N12—C39—H39A | 109.2 |
C4—C5—C6 | 122.2 (4) | N10—C39—H39A | 109.2 |
C4—C5—H5 | 118.9 | N12—C39—H39B | 109.2 |
C6—C5—H5 | 118.9 | N10—C39—H39B | 109.2 |
C5—C6—C1 | 119.5 (4) | H39A—C39—H39B | 107.9 |
C5—C6—H6 | 120.2 | O1—O1'—S1 | 79.9 (7) |
C1—C6—H6 | 120.2 | O1'—O1—S1 | 66.0 (6) |
C4—C7—H7A | 109.5 | O2—O2'—S1 | 62.0 (7) |
C4—C7—H7B | 109.5 | O2'—O2—S1 | 80.7 (7) |
H7A—C7—H7B | 109.5 | O2'—O2—O3' | 135.4 (9) |
C4—C7—H7C | 109.5 | S1—O2—O3' | 55.2 (4) |
H7A—C7—H7C | 109.5 | H1WA—O1W—H1WB | 107 (3) |
H7B—C7—H7C | 109.5 | O3—O3'—S1 | 73.6 (6) |
C9—C8—C13 | 119.8 (4) | O3—O3'—O2 | 127.6 (7) |
C9—C8—S3 | 120.6 (3) | S1—O3'—O2 | 57.7 (4) |
C13—C8—S3 | 119.4 (3) | O3'—O3—S1 | 59.8 (5) |
C8—C9—C10 | 119.4 (4) | H2WA—O2W—H2WB | 109 (3) |
C8—C9—H9 | 120.3 | H3WA—O3W—H3WB | 113 (4) |
C10—C9—H9 | 120.3 | H4WA—O4W—H4WB | 104 (3) |
C11—C10—C9 | 121.3 (4) | O7—O7'—S3 | 59.6 (7) |
C11—C10—H10 | 119.4 | O7'—O7—S3 | 81.4 (8) |
C9—C10—H10 | 119.4 | O7'—O7—O9' | 130.5 (10) |
C12—C11—C10 | 119.0 (4) | S3—O7—O9' | 52.4 (5) |
C12—C11—C14 | 119.9 (6) | O9'—O9—S3 | 55.6 (6) |
C10—C11—C14 | 121.1 (5) | O9'—O9—Ag3 | 80.9 (7) |
C11—C12—C13 | 120.3 (5) | S3—O9—Ag3 | 134.4 (3) |
C11—C12—H12 | 119.9 | O9—O9'—S3 | 80.5 (8) |
C13—C12—H12 | 119.9 | O9—O9'—O7 | 140.3 (10) |
C8—C13—C12 | 120.0 (4) | S3—O9'—O7 | 60.2 (5) |
C8—C13—H13 | 120.0 | O9—O9'—Ag3 | 73.7 (6) |
C12—C13—H13 | 120.0 | S3—O9'—Ag3 | 150.6 (7) |
C11—C14—H14A | 109.5 | O7—O9'—Ag3 | 141.3 (7) |
C11—C14—H14B | 109.5 | O3'—S1—O1' | 122.4 (5) |
H14A—C14—H14B | 109.5 | O3'—S1—O2 | 67.1 (4) |
C11—C14—H14C | 109.5 | O1'—S1—O2 | 136.8 (4) |
H14A—C14—H14C | 109.5 | O3'—S1—O1 | 143.2 (4) |
H14B—C14—H14C | 109.5 | O1'—S1—O1 | 34.1 (3) |
C16—C15—C20 | 119.6 (4) | O2—S1—O1 | 110.5 (3) |
C16—C15—S2 | 121.0 (3) | O3'—S1—O3 | 46.6 (4) |
C20—C15—S2 | 119.4 (3) | O1'—S1—O3 | 80.0 (4) |
C17—C16—C15 | 120.0 (4) | O2—S1—O3 | 111.2 (3) |
C17—C16—H16 | 120.0 | O1—S1—O3 | 111.8 (3) |
C15—C16—H16 | 120.0 | O3'—S1—O2' | 104.2 (5) |
C18—C17—C16 | 121.5 (4) | O1'—S1—O2' | 111.7 (5) |
C18—C17—H17 | 119.2 | O2—S1—O2' | 37.3 (3) |
C16—C17—H17 | 119.2 | O1—S1—O2' | 78.6 (4) |
C17—C18—C19 | 118.4 (4) | O3—S1—O2' | 144.1 (4) |
C17—C18—C21 | 121.7 (5) | O3'—S1—C1 | 108.2 (4) |
C19—C18—C21 | 119.8 (5) | O1'—S1—C1 | 107.0 (3) |
C20—C19—C18 | 120.9 (4) | O2—S1—C1 | 108.5 (3) |
C20—C19—H19 | 119.6 | O1—S1—C1 | 107.1 (2) |
C18—C19—H19 | 119.6 | O3—S1—C1 | 107.5 (2) |
C19—C20—C15 | 119.6 (4) | O2'—S1—C1 | 101.2 (4) |
C19—C20—H20 | 120.2 | O4—S2—O5 | 112.7 (2) |
C15—C20—H20 | 120.2 | O4—S2—O6 | 112.10 (18) |
C18—C21—H21A | 109.5 | O5—S2—O6 | 112.3 (2) |
C18—C21—H21B | 109.5 | O4—S2—C15 | 105.4 (2) |
H21A—C21—H21B | 109.5 | O5—S2—C15 | 106.32 (17) |
C18—C21—H21C | 109.5 | O6—S2—C15 | 107.46 (17) |
H21A—C21—H21C | 109.5 | O9'—S3—O8 | 126.5 (5) |
H21B—C21—H21C | 109.5 | O9'—S3—O7 | 67.3 (6) |
N1—C22—N3 | 112.0 (2) | O8—S3—O7 | 122.3 (3) |
N1—C22—H22A | 109.2 | O9'—S3—O9 | 43.9 (5) |
N3—C22—H22A | 109.2 | O8—S3—O9 | 104.8 (3) |
N1—C22—H22B | 109.2 | O7—S3—O9 | 111.0 (3) |
N3—C22—H22B | 109.2 | O9'—S3—O7' | 104.5 (7) |
H22A—C22—H22B | 107.9 | O8—S3—O7' | 90.8 (5) |
N2—C23—N1 | 111.8 (3) | O7—S3—O7' | 39.0 (4) |
N2—C23—H23A | 109.2 | O9—S3—O7' | 147.9 (5) |
N1—C23—H23A | 109.2 | O9'—S3—C8 | 116.8 (4) |
N2—C23—H23B | 109.2 | O8—S3—C8 | 108.9 (2) |
N1—C23—H23B | 109.2 | O7—S3—C8 | 108.6 (3) |
H23A—C23—H23B | 107.9 | O9—S3—C8 | 98.7 (2) |
N2—C24—N4 | 111.3 (2) | O7'—S3—C8 | 102.5 (4) |
N2—C24—H24A | 109.4 | C22—N1—C26 | 108.0 (2) |
N4—C24—H24A | 109.4 | C22—N1—C23 | 107.7 (3) |
N2—C24—H24B | 109.4 | C26—N1—C23 | 108.4 (2) |
N4—C24—H24B | 109.4 | C22—N1—Ag1 | 108.63 (17) |
H24A—C24—H24B | 108.0 | C26—N1—Ag1 | 108.22 (18) |
N4—C25—N3 | 111.5 (2) | C23—N1—Ag1 | 115.60 (18) |
N4—C25—H25A | 109.3 | C24—N2—C23 | 109.5 (3) |
N3—C25—H25A | 109.3 | C24—N2—C27 | 108.7 (3) |
N4—C25—H25B | 109.3 | C23—N2—C27 | 108.8 (3) |
N3—C25—H25B | 109.3 | C22—N3—C25 | 108.1 (2) |
H25A—C25—H25B | 108.0 | C22—N3—C27 | 108.0 (2) |
N4—C26—N1 | 111.6 (2) | C25—N3—C27 | 107.9 (2) |
N4—C26—H26A | 109.3 | C22—N3—Ag3iii | 108.95 (17) |
N1—C26—H26A | 109.3 | C25—N3—Ag3iii | 108.15 (18) |
N4—C26—H26B | 109.3 | C27—N3—Ag3iii | 115.50 (19) |
N1—C26—H26B | 109.3 | C25—N4—C26 | 107.6 (2) |
H26A—C26—H26B | 108.0 | C25—N4—C24 | 108.7 (3) |
N2—C27—N3 | 111.7 (3) | C26—N4—C24 | 108.8 (2) |
N2—C27—H27A | 109.3 | C25—N4—Ag2 | 113.34 (17) |
N3—C27—H27A | 109.3 | C26—N4—Ag2 | 104.51 (18) |
N2—C27—H27B | 109.3 | C24—N4—Ag2 | 113.63 (18) |
N3—C27—H27B | 109.3 | C30—N5—C28 | 107.9 (2) |
H27A—C27—H27B | 107.9 | C30—N5—C29 | 108.7 (2) |
N5—C28—N7 | 112.2 (2) | C28—N5—C29 | 108.7 (2) |
N5—C28—H28A | 109.2 | C30—N5—Ag2 | 113.08 (18) |
N7—C28—H28A | 109.2 | C28—N5—Ag2 | 109.63 (16) |
N5—C28—H28B | 109.2 | C29—N5—Ag2 | 108.77 (18) |
N7—C28—H28B | 109.2 | C31—N6—C30 | 108.2 (3) |
H28A—C28—H28B | 107.9 | C31—N6—C33 | 108.7 (3) |
N8—C29—N5 | 111.4 (2) | C30—N6—C33 | 108.7 (2) |
N8—C29—H29A | 109.4 | C32—N7—C33 | 107.9 (2) |
N5—C29—H29A | 109.4 | C32—N7—C28 | 107.5 (2) |
N8—C29—H29B | 109.4 | C33—N7—C28 | 107.4 (3) |
N5—C29—H29B | 109.4 | C32—N7—Ag2iii | 107.44 (19) |
H29A—C29—H29B | 108.0 | C33—N7—Ag2iii | 116.58 (19) |
N6—C30—N5 | 111.6 (3) | C28—N7—Ag2iii | 109.70 (17) |
N6—C30—H30A | 109.3 | C32—N8—C29 | 107.9 (2) |
N5—C30—H30A | 109.3 | C32—N8—C31 | 108.6 (3) |
N6—C30—H30B | 109.3 | C29—N8—C31 | 107.4 (3) |
N5—C30—H30B | 109.3 | C32—N8—Ag3 | 106.1 (2) |
H30A—C30—H30B | 108.0 | C29—N8—Ag3 | 110.9 (2) |
N6—C31—N8 | 112.4 (2) | C31—N8—Ag3 | 115.70 (18) |
N6—C31—H31A | 109.1 | C34—N9—C35 | 107.7 (2) |
N8—C31—H31A | 109.1 | C34—N9—C36 | 107.9 (2) |
N6—C31—H31B | 109.1 | C35—N9—C36 | 107.8 (2) |
N8—C31—H31B | 109.1 | C34—N9—Ag1iv | 106.83 (18) |
H31A—C31—H31B | 107.9 | C35—N9—Ag1iv | 117.58 (17) |
N8—C32—N7 | 112.6 (3) | C36—N9—Ag1iv | 108.72 (18) |
N8—C32—H32A | 109.1 | C38—N10—C39 | 108.0 (2) |
N7—C32—H32A | 109.1 | C38—N10—C36 | 107.7 (2) |
N8—C32—H32B | 109.1 | C39—N10—C36 | 108.3 (2) |
N7—C32—H32B | 109.1 | C38—N10—Ag1iii | 111.35 (17) |
H32A—C32—H32B | 107.8 | C39—N10—Ag1iii | 114.17 (19) |
N6—C33—N7 | 112.3 (3) | C36—N10—Ag1iii | 107.13 (18) |
N6—C33—H33A | 109.1 | C34—N11—C38 | 107.6 (2) |
N7—C33—H33A | 109.1 | C34—N11—C37 | 108.5 (2) |
N6—C33—H33B | 109.1 | C38—N11—C37 | 107.9 (2) |
N7—C33—H33B | 109.1 | C34—N11—Ag3 | 109.81 (18) |
H33A—C33—H33B | 107.9 | C38—N11—Ag3 | 109.83 (16) |
N11—C34—N9 | 111.9 (2) | C37—N11—Ag3 | 113.03 (18) |
N11—C34—H34A | 109.2 | C37—N12—C35 | 108.2 (3) |
N9—C34—H34A | 109.2 | C37—N12—C39 | 109.0 (2) |
N11—C34—H34B | 109.2 | C35—N12—C39 | 108.9 (3) |
C6—C1—C2—C3 | 0.2 (6) | O7—O7'—S3—O9 | 26.1 (12) |
S1—C1—C2—C3 | 178.8 (3) | O7—O7'—S3—C8 | −104.2 (6) |
C1—C2—C3—C4 | 0.0 (6) | C9—C8—S3—O9' | −54.3 (7) |
C2—C3—C4—C5 | −0.5 (6) | C13—C8—S3—O9' | 121.2 (6) |
C2—C3—C4—C7 | 179.1 (4) | C9—C8—S3—O8 | 154.4 (3) |
C3—C4—C5—C6 | 0.8 (7) | C13—C8—S3—O8 | −30.1 (4) |
C7—C4—C5—C6 | −178.8 (4) | C9—C8—S3—O7 | 19.1 (4) |
C4—C5—C6—C1 | −0.5 (7) | C13—C8—S3—O7 | −165.4 (4) |
C2—C1—C6—C5 | 0.0 (6) | C9—C8—S3—O9 | −96.6 (4) |
S1—C1—C6—C5 | −178.6 (3) | C13—C8—S3—O9 | 78.9 (4) |
C13—C8—C9—C10 | −2.0 (5) | C9—C8—S3—O7' | 59.2 (5) |
S3—C8—C9—C10 | 173.5 (3) | C13—C8—S3—O7' | −125.3 (5) |
C8—C9—C10—C11 | −1.2 (6) | N3—C22—N1—C26 | 58.5 (3) |
C9—C10—C11—C12 | 3.7 (6) | N3—C22—N1—C23 | −58.4 (3) |
C9—C10—C11—C14 | −175.8 (4) | N3—C22—N1—Ag1 | 175.7 (2) |
C10—C11—C12—C13 | −3.1 (7) | N4—C26—N1—C22 | −59.4 (3) |
C14—C11—C12—C13 | 176.4 (4) | N4—C26—N1—C23 | 57.0 (3) |
C9—C8—C13—C12 | 2.5 (6) | N4—C26—N1—Ag1 | −176.8 (2) |
S3—C8—C13—C12 | −173.0 (3) | N2—C23—N1—C22 | 59.0 (3) |
C11—C12—C13—C8 | 0.0 (6) | N2—C23—N1—C26 | −57.7 (3) |
C20—C15—C16—C17 | 1.0 (6) | N2—C23—N1—Ag1 | −179.3 (2) |
S2—C15—C16—C17 | 179.0 (3) | N9i—Ag1—N1—C22 | −22.2 (2) |
C15—C16—C17—C18 | −0.2 (6) | N10ii—Ag1—N1—C22 | 172.70 (19) |
C16—C17—C18—C19 | −0.3 (7) | N9i—Ag1—N1—C26 | 94.8 (2) |
C16—C17—C18—C21 | 177.1 (4) | N10ii—Ag1—N1—C26 | −70.3 (2) |
C17—C18—C19—C20 | −0.1 (7) | N9i—Ag1—N1—C23 | −143.4 (2) |
C21—C18—C19—C20 | −177.5 (4) | N10ii—Ag1—N1—C23 | 51.5 (2) |
C18—C19—C20—C15 | 0.8 (6) | N4—C24—N2—C23 | −59.0 (4) |
C16—C15—C20—C19 | −1.3 (6) | N4—C24—N2—C27 | 59.8 (3) |
S2—C15—C20—C19 | −179.4 (3) | N1—C23—N2—C24 | 59.1 (4) |
S1—O2'—O2—O3' | 7.9 (10) | N1—C23—N2—C27 | −59.7 (3) |
O2'—O2—O3'—O3 | 15.1 (17) | N3—C27—N2—C24 | −60.2 (3) |
S1—O2—O3'—O3 | 24.6 (8) | N3—C27—N2—C23 | 59.0 (3) |
O2'—O2—O3'—S1 | −9.5 (12) | N1—C22—N3—C25 | −58.4 (3) |
O2—O3'—O3—S1 | −21.5 (6) | N1—C22—N3—C27 | 58.1 (3) |
S3—O7'—O7—O9' | −19.8 (9) | N1—C22—N3—Ag3iii | −175.7 (2) |
N3ii—Ag3—O9—O9' | −20.0 (6) | N4—C25—N3—C22 | 59.0 (3) |
N8—Ag3—O9—O9' | 111.2 (6) | N4—C25—N3—C27 | −57.6 (3) |
N11—Ag3—O9—O9' | −137.2 (6) | N4—C25—N3—Ag3iii | 176.85 (19) |
N3ii—Ag3—O9—S3 | −3.3 (4) | N2—C27—N3—C22 | −58.0 (3) |
N8—Ag3—O9—S3 | 127.9 (4) | N2—C27—N3—C25 | 58.7 (3) |
N11—Ag3—O9—S3 | −120.5 (4) | N2—C27—N3—Ag3iii | 179.78 (19) |
O9'—Ag3—O9—S3 | 16.7 (5) | N3—C25—N4—C26 | −59.8 (3) |
Ag3—O9—O9'—S3 | 165.5 (4) | N3—C25—N4—C24 | 57.9 (3) |
S3—O9—O9'—O7 | −8.3 (10) | N3—C25—N4—Ag2 | −174.78 (18) |
Ag3—O9—O9'—O7 | 157.3 (14) | N1—C26—N4—C25 | 60.1 (3) |
S3—O9—O9'—Ag3 | −165.5 (4) | N1—C26—N4—C24 | −57.5 (3) |
O7'—O7—O9'—O9 | 34 (2) | N1—C26—N4—Ag2 | −179.2 (2) |
S3—O7—O9'—O9 | 9.4 (12) | N2—C24—N4—C25 | −58.8 (3) |
O7'—O7—O9'—S3 | 25.1 (11) | N2—C24—N4—C26 | 58.1 (3) |
O7'—O7—O9'—Ag3 | 178.1 (10) | N2—C24—N4—Ag2 | 174.1 (2) |
S3—O7—O9'—Ag3 | 153.0 (11) | N5—Ag2—N4—C25 | −39.8 (2) |
N3ii—Ag3—O9'—O9 | 162.5 (6) | N7ii—Ag2—N4—C25 | 136.98 (19) |
N8—Ag3—O9'—O9 | −69.6 (6) | N5—Ag2—N4—C26 | −156.63 (18) |
N11—Ag3—O9'—O9 | 45.6 (6) | N7ii—Ag2—N4—C26 | 20.2 (2) |
N3ii—Ag3—O9'—S3 | 132.5 (14) | N5—Ag2—N4—C24 | 84.9 (2) |
N8—Ag3—O9'—S3 | −99.6 (14) | N7ii—Ag2—N4—C24 | −98.3 (2) |
N11—Ag3—O9'—S3 | 15.5 (15) | N6—C30—N5—C28 | 59.2 (3) |
O9—Ag3—O9'—S3 | −30.1 (10) | N6—C30—N5—C29 | −58.5 (3) |
N3ii—Ag3—O9'—O7 | 5.8 (10) | N6—C30—N5—Ag2 | −179.4 (2) |
N8—Ag3—O9'—O7 | 133.7 (9) | N7—C28—N5—C30 | −59.2 (3) |
N11—Ag3—O9'—O7 | −111.2 (9) | N7—C28—N5—C29 | 58.5 (3) |
O9—Ag3—O9'—O7 | −156.8 (14) | N7—C28—N5—Ag2 | 177.2 (2) |
O3—O3'—S1—O1' | −27.9 (7) | N8—C29—N5—C30 | 58.5 (3) |
O2—O3'—S1—O1' | 132.0 (5) | N8—C29—N5—C28 | −58.7 (3) |
O3—O3'—S1—O2 | −159.9 (6) | N8—C29—N5—Ag2 | −178.0 (2) |
O3—O3'—S1—O1 | −65.9 (9) | N7ii—Ag2—N5—C30 | 115.7 (2) |
O2—O3'—S1—O1 | 94.1 (7) | N4—Ag2—N5—C30 | −67.7 (2) |
O2—O3'—S1—O3 | 159.9 (6) | N7ii—Ag2—N5—C28 | −123.9 (2) |
O3—O3'—S1—O2' | −155.7 (5) | N4—Ag2—N5—C28 | 52.7 (2) |
O2—O3'—S1—O2' | 4.2 (5) | N7ii—Ag2—N5—C29 | −5.1 (2) |
O3—O3'—S1—C1 | 97.2 (5) | N4—Ag2—N5—C29 | 171.48 (19) |
O2—O3'—S1—C1 | −102.9 (3) | N8—C31—N6—C30 | −59.7 (4) |
O1—O1'—S1—O3' | −138.9 (7) | N8—C31—N6—C33 | 58.1 (3) |
O1—O1'—S1—O2 | −48.7 (9) | N5—C30—N6—C31 | 58.7 (4) |
O1—O1'—S1—O3 | −159.1 (7) | N5—C30—N6—C33 | −59.1 (4) |
O1—O1'—S1—O2' | −14.5 (8) | N7—C33—N6—C31 | −58.9 (3) |
O1—O1'—S1—C1 | 95.5 (6) | N7—C33—N6—C30 | 58.7 (4) |
O2'—O2—S1—O3' | 173.3 (8) | N8—C32—N7—C33 | −57.1 (3) |
O2'—O2—S1—O1' | 59.7 (9) | N8—C32—N7—C28 | 58.5 (3) |
O3'—O2—S1—O1' | −113.6 (6) | N8—C32—N7—Ag2iii | 176.5 (2) |
O2'—O2—S1—O1 | 32.9 (7) | N6—C33—N7—C32 | 58.0 (3) |
O3'—O2—S1—O1 | −140.3 (4) | N6—C33—N7—C28 | −57.6 (3) |
O2'—O2—S1—O3 | 157.7 (7) | N6—C33—N7—Ag2iii | 178.89 (19) |
O3'—O2—S1—O3 | −15.5 (5) | N5—C28—N7—C32 | −57.7 (4) |
O3'—O2—S1—O2' | −173.3 (8) | N5—C28—N7—C33 | 58.2 (3) |
O2'—O2—S1—C1 | −84.2 (7) | N5—C28—N7—Ag2iii | −174.2 (2) |
O3'—O2—S1—C1 | 102.5 (4) | N7—C32—N8—C29 | −59.4 (4) |
O1'—O1—S1—O3' | 67.8 (10) | N7—C32—N8—C31 | 56.7 (3) |
O1'—O1—S1—O2 | 146.7 (6) | N7—C32—N8—Ag3 | −178.3 (2) |
O1'—O1—S1—O3 | 22.2 (7) | N5—C29—N8—C32 | 58.7 (4) |
O1'—O1—S1—O2' | 166.3 (7) | N5—C29—N8—C31 | −58.2 (3) |
O1'—O1—S1—C1 | −95.3 (6) | N5—C29—N8—Ag3 | 174.5 (2) |
O3'—O3—S1—O1' | 156.3 (6) | N6—C31—N8—C32 | −57.1 (3) |
O3'—O3—S1—O2 | 19.8 (6) | N6—C31—N8—C29 | 59.4 (3) |
O3'—O3—S1—O1 | 143.9 (5) | N6—C31—N8—Ag3 | −176.2 (2) |
O3'—O3—S1—O2' | 42.9 (9) | N3ii—Ag3—N8—C32 | 145.73 (18) |
O3'—O3—S1—C1 | −98.8 (5) | N11—Ag3—N8—C32 | −67.5 (2) |
O2—O2'—S1—O3' | −6.4 (8) | O9—Ag3—N8—C32 | 21.0 (2) |
O2—O2'—S1—O1' | −140.5 (6) | O9'—Ag3—N8—C32 | 44.7 (3) |
O2—O2'—S1—O1 | −148.7 (7) | N3ii—Ag3—N8—C29 | 28.8 (2) |
O2—O2'—S1—O3 | −37.1 (11) | N11—Ag3—N8—C29 | 175.6 (2) |
O2—O2'—S1—C1 | 105.9 (6) | O9—Ag3—N8—C29 | −95.9 (2) |
C2—C1—S1—O3' | −3.4 (5) | O9'—Ag3—N8—C29 | −72.2 (3) |
C6—C1—S1—O3' | 175.2 (5) | N3ii—Ag3—N8—C31 | −93.7 (2) |
C2—C1—S1—O1' | 130.3 (4) | N11—Ag3—N8—C31 | 53.0 (2) |
C6—C1—S1—O1' | −51.1 (5) | O9—Ag3—N8—C31 | 141.5 (2) |
C2—C1—S1—O2 | −74.7 (4) | O9'—Ag3—N8—C31 | 165.2 (3) |
C6—C1—S1—O2 | 103.9 (4) | N11—C34—N9—C35 | 57.2 (3) |
C2—C1—S1—O1 | 166.0 (4) | N11—C34—N9—C36 | −59.0 (3) |
C6—C1—S1—O1 | −15.4 (4) | N11—C34—N9—Ag1iv | −175.7 (2) |
C2—C1—S1—O3 | 45.7 (4) | N12—C35—N9—C34 | −58.5 (3) |
C6—C1—S1—O3 | −135.7 (4) | N12—C35—N9—C36 | 57.6 (3) |
C2—C1—S1—O2' | −112.6 (5) | N12—C35—N9—Ag1iv | −179.08 (19) |
C6—C1—S1—O2' | 66.0 (5) | N10—C36—N9—C34 | 58.6 (3) |
C16—C15—S2—O4 | −109.5 (3) | N10—C36—N9—C35 | −57.4 (3) |
C20—C15—S2—O4 | 68.6 (3) | N10—C36—N9—Ag1iv | 174.05 (17) |
C16—C15—S2—O5 | 10.3 (4) | N11—C38—N10—C39 | −57.6 (3) |
C20—C15—S2—O5 | −171.6 (3) | N11—C38—N10—C36 | 59.1 (3) |
C16—C15—S2—O6 | 130.8 (3) | N11—C38—N10—Ag1iii | 176.3 (2) |
C20—C15—S2—O6 | −51.1 (3) | N12—C39—N10—C38 | 57.8 (3) |
O9—O9'—S3—O8 | 71.8 (8) | N12—C39—N10—C36 | −58.6 (3) |
O7—O9'—S3—O8 | −114.3 (5) | N12—C39—N10—Ag1iii | −177.78 (18) |
Ag3—O9'—S3—O8 | 101.0 (13) | N9—C36—N10—C38 | −58.4 (3) |
O9—O9'—S3—O7 | −173.9 (8) | N9—C36—N10—C39 | 58.1 (3) |
Ag3—O9'—S3—O7 | −144.8 (15) | N9—C36—N10—Ag1iii | −178.29 (18) |
O7—O9'—S3—O9 | 173.9 (8) | N9—C34—N11—C38 | 59.0 (3) |
Ag3—O9'—S3—O9 | 29.2 (10) | N9—C34—N11—C37 | −57.5 (3) |
O9—O9'—S3—O7' | 173.8 (6) | N9—C34—N11—Ag3 | 178.53 (19) |
O7—O9'—S3—O7' | −12.2 (6) | N10—C38—N11—C34 | −59.3 (3) |
Ag3—O9'—S3—O7' | −157.0 (13) | N10—C38—N11—C37 | 57.6 (3) |
O9—O9'—S3—C8 | −73.8 (7) | N10—C38—N11—Ag3 | −178.8 (2) |
O7—O9'—S3—C8 | 100.2 (4) | N12—C37—N11—C34 | 58.4 (3) |
Ag3—O9'—S3—C8 | −44.6 (15) | N12—C37—N11—C38 | −57.9 (3) |
O7'—O7—S3—O9' | −161.0 (9) | N12—C37—N11—Ag3 | −179.5 (2) |
O7'—O7—S3—O8 | −41.1 (8) | N3ii—Ag3—N11—C34 | 66.1 (2) |
O9'—O7—S3—O8 | 119.9 (5) | N8—Ag3—N11—C34 | −85.2 (2) |
O7'—O7—S3—O9 | −165.5 (7) | O9—Ag3—N11—C34 | −172.0 (2) |
O9'—O7—S3—O9 | −4.5 (6) | O9'—Ag3—N11—C34 | 170.1 (3) |
O9'—O7—S3—O7' | 161.0 (9) | N3ii—Ag3—N11—C38 | −175.77 (19) |
O7'—O7—S3—C8 | 87.0 (7) | N8—Ag3—N11—C38 | 32.9 (2) |
O9'—O7—S3—C8 | −112.0 (5) | O9—Ag3—N11—C38 | −53.9 (2) |
Ag3—O9—S3—O9' | −20.2 (6) | O9'—Ag3—N11—C38 | −71.8 (3) |
O9'—O9—S3—O8 | −127.9 (7) | N3ii—Ag3—N11—C37 | −55.2 (2) |
Ag3—O9—S3—O8 | −148.0 (3) | N8—Ag3—N11—C37 | 153.4 (2) |
O9'—O9—S3—O7 | 6.0 (7) | O9—Ag3—N11—C37 | 66.6 (2) |
Ag3—O9—S3—O7 | −14.2 (5) | O9'—Ag3—N11—C37 | 48.8 (3) |
O9'—O9—S3—O7' | −11.3 (11) | N11—C37—N12—C35 | −59.2 (3) |
Ag3—O9—S3—O7' | −31.5 (10) | N11—C37—N12—C39 | 59.1 (3) |
O9'—O9—S3—C8 | 119.9 (7) | N9—C35—N12—C37 | 59.7 (3) |
Ag3—O9—S3—C8 | 99.7 (4) | N9—C35—N12—C39 | −58.6 (3) |
O7—O7'—S3—O9' | 18.1 (8) | N10—C39—N12—C37 | −59.0 (3) |
O7—O7'—S3—O8 | 146.3 (6) | N10—C39—N12—C35 | 58.8 (3) |
Symmetry codes: (i) x−1, y, z; (ii) −x+3/2, y−1/2, −z+3/2; (iii) −x+3/2, y+1/2, −z+3/2; (iv) x+1, y, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O8ii | 0.87 (2) | 1.92 (2) | 2.782 (5) | 175 (4) |
O1W—H1WB···O6ii | 0.82 (2) | 2.10 (2) | 2.907 (4) | 166 (4) |
O2W—H2WA···O5iii | 0.83 (2) | 2.16 (2) | 2.958 (4) | 163 (4) |
O2W—H2WB···O1iv | 0.84 (2) | 1.83 (3) | 2.612 (6) | 155 (4) |
O3W—H3WA···O2v | 0.80 (2) | 2.45 (3) | 3.096 (7) | 139 (4) |
O3W—H3WB···O5 | 0.80 (2) | 2.15 (2) | 2.908 (5) | 160 (4) |
O4W—H4WB···O7iii | 0.88 (2) | 1.99 (3) | 2.838 (7) | 160 (4) |
Symmetry codes: (ii) −x+3/2, y−1/2, −z+3/2; (iii) −x+3/2, y+1/2, −z+3/2; (iv) x+1, y, z; (v) −x+1/2, y+1/2, −z+3/2. |
Experimental details
Crystal data | |
Chemical formula | [Ag3(C7H7O3S)3(C6H12N4)3(H2O)]·3H2O |
Mr | 1329.82 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 17.3181 (5), 10.7028 (3), 26.9110 (11) |
β (°) | 95.657 (3) |
V (Å3) | 4963.7 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.37 |
Crystal size (mm) | 0.30 × 0.25 × 0.22 |
Data collection | |
Diffractometer | Oxford Diffraction Gemini R Ultra |
Absorption correction | Multi-scan (CrysAlis RED; Oxford Diffraction, 2006) |
Tmin, Tmax | 0.672, 0.728 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 21413, 11446, 7890 |
Rint | 0.021 |
(sin θ/λ)max (Å−1) | 0.688 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.097, 0.99 |
No. of reflections | 11446 |
No. of parameters | 650 |
No. of restraints | 12 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.90, −1.05 |
Computer programs: CrysAlis CCD (Oxford Diffraction, 2006), CrysAlis RED (Oxford Diffraction, 2006), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008).
Ag1—N1 | 2.362 (2) | Ag2—N4 | 2.374 (2) |
Ag1—N9i | 2.367 (3) | Ag3—N3ii | 2.315 (3) |
Ag1—N10ii | 2.388 (3) | Ag3—N8 | 2.358 (3) |
Ag2—N5 | 2.347 (2) | Ag3—N11 | 2.394 (2) |
Ag2—N7ii | 2.365 (3) |
Symmetry codes: (i) x−1, y, z; (ii) −x+3/2, y−1/2, −z+3/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O8ii | 0.87 (2) | 1.92 (2) | 2.782 (5) | 175 (4) |
O1W—H1WB···O6ii | 0.82 (2) | 2.10 (2) | 2.907 (4) | 166 (4) |
O2W—H2WA···O5iii | 0.83 (2) | 2.16 (2) | 2.958 (4) | 163 (4) |
O2W—H2WB···O1iv | 0.84 (2) | 1.83 (3) | 2.612 (6) | 155 (4) |
O3W—H3WA···O2v | 0.80 (2) | 2.45 (3) | 3.096 (7) | 139 (4) |
O3W—H3WB···O5 | 0.80 (2) | 2.15 (2) | 2.908 (5) | 160 (4) |
O4W—H4WB···O7iii | 0.88 (2) | 1.99 (3) | 2.838 (7) | 160 (4) |
Symmetry codes: (ii) −x+3/2, y−1/2, −z+3/2; (iii) −x+3/2, y+1/2, −z+3/2; (iv) x+1, y, z; (v) −x+1/2, y+1/2, −z+3/2. |
Acknowledgements
We thank the Heilongjiang Province Education Department for support (project `The Study of Silver Sulfonates containing Neutral Ligands', serial No. 11535035).
References
Côté, A. P. & Shimizu, G. K. H. (2003). Coord. Chem. Rev., 245, 49-64. Google Scholar
Oxford Diffraction (2006). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zhang, S.-L., Tong, M.-L., Fu, R.-W., Cheng, X.-M. & Ng, S.-W. (2001). Inorg. Chem. 40, 3562–3569. Web of Science PubMed Google Scholar
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Metal sulfonate complexes modified by different nitrogen-containing secondary ligands have been of great interest due to their abilities to form various structures, possible extended supramolecular system and good properties (Côté & Shimizu, 2003). Currently, there are some AgI sulfonate coordination polymers building from hexamethylenetetramine ligand because of its multidentate coordination mode (Zhang et al., 2001).
In the crystal structure of the title compound, C39H65Ag3N12O13S3, there are three AgI cations, three p-toluenesulfonate anions, three hexamethylenetetramine and four water molecules (Fig. 1). Ag1 cation is four-coordinated by three N atoms from three different hexamethylenetetramine ligands [Ag1—N1 = 2.362 (2), Ag1—N9i = 2.367 (2), and Ag1—N10ii = 2.388 (3)] and one O atom from one p-toluenesulfonate ligand [Ag1—O = 2.644 (6) Å] in a distorted tetrahedral coordination geometry. Ag2 cation is five-coordinated by three N atoms from three different hexamethylenetetramine ligands [Ag2—N5 = 2.347 (2), Ag2—N4 = 2.374 (2) and Ag2—N7ii = 2.365 (2) Å], one O atom from one p-toluenesulfonate ligand and one water molecule [Ag2—O4 = 2.622 (3) and Ag2—O1W = 2.622 (4) Å] in a trigonalbiyramid coordination geometry. Ag3 cation is also four-coordinated by three N atoms from hexamethylenetetramine ligands [Ag3—N3ii = 2.315 (3), Ag3—N8 = 2.358 (3), and Ag3—N11 = 2.394 (2) Å] and one p-toluenesulfonate ligand [Ag3—O9 = 2.438 (5) Å] in a distorted tetrahedral coordination geometry. The AgI cations are bridged by hexamethylenetetramine molecules in tridentate modes to generate a two dimensional wave like layer with the p-toluenesulfonate ligands hanged up and down (Fig. 2). The intermoleclar hydrogen bonding interactions consolidate the layer.