Related literature
For a related structure, see: Nie & Qu (2011).
Experimental
Data collection
Bruker APEX CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996) Tmin = 0.622, Tmax = 0.754 7253 measured reflections 3387 independent reflections 2190 reflections with I > 2σ(I) Rint = 0.058
|
Ag1—N1 | 2.180 (3) | Ag1—O3i | 2.621 (3) | Ag1—O6 | 2.153 (3) | Ag2—N2 | 2.245 (3) | Ag2—N3 | 2.262 (3) | Ag2—O1ii | 2.516 (4) | Ag2—OW2 | 2.576 (4) | Symmetry codes: (i) -x, -y, -z-1; (ii) x+1, y, z+1. | |
D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A | OW1—H1A⋯O5 | 0.88 (2) | 1.89 (2) | 2.751 (4) | 168 (6) | OW1—H1B⋯O5iii | 0.89 (2) | 2.00 (2) | 2.883 (5) | 173 (6) | OW2—H2A⋯O2iii | 0.88 (2) | 1.91 (3) | 2.757 (5) | 161 (6) | OW2—H2B⋯OW1iv | 0.89 (2) | 2.03 (3) | 2.794 (6) | 143 (2) | O4—H4A⋯O6 | 0.82 | 1.84 | 2.556 (4) | 146 | Symmetry codes: (iii) -x, -y+1, -z-1; (iv) -x, -y+1, -z. | |
Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.
Supporting information
To a mixture of 5-sulfosalicylic acid (0.109 g, 0.5 mmol) and NaOH (0.040 g, 1.0 mmol) in water (5 ml) was added AgNO3 (0.170 g, 1.0 mmol), giving a clear solution. Then ethanol (15 ml) was added to the solution, and white precipitate appeared. The precipitate was collected and dissolved in water. To the solution was added pyrazine (0.081 g, 1 mmol) in methanol (5 ml) and white precipitate formed. The precipitate was dissolved by dropwise addition of acetonitrile. Colorless crystals were obtained from the filtrate after standing in a dark room for several days (yield: 0.150 g, 51%).
H atoms bound to C atoms and hydroxyl O atom were positioned geometrically and refined using a riding model, with C—H = 0.93 and O—H = 0.82 Å and with Uiso(H) = 1.2(1.5 for hydroxyl)Ueq(C, O). Water H atoms were located from a difference Fourier map and refined with a retraint of O—H = 0.88 Å and with Uiso(H) = 1.5Ueq(O).
Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
Poly[[diaquabis(µ
3-3-carboxylato-4-hydroxybenzenesulfonato)tri-µ
2- pyrazine-tetrasilver(I)] dihydrate]
top Crystal data top [Ag4(C7H4O6S)2(C4H4N2)3(H2O)2]·2H2O | Z = 1 |
Mr = 1176.14 | F(000) = 574 |
Triclinic, P1 | Dx = 2.316 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.646 (5) Å | Cell parameters from 2192 reflections |
b = 10.340 (4) Å | θ = 3.2–27.5° |
c = 11.375 (4) Å | µ = 2.50 mm−1 |
α = 78.751 (3)° | T = 293 K |
β = 73.436 (4)° | Block, colorless |
γ = 82.882 (5)° | 0.21 × 0.15 × 0.12 mm |
V = 843.2 (7) Å3 | |
Data collection top Bruker APEX CCD diffractometer | 3387 independent reflections |
Radiation source: fine-focus sealed tube | 2190 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.058 |
ϕ and ω scans | θmax = 27.5°, θmin = 3.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.622, Tmax = 0.754 | k = −12→13 |
7253 measured reflections | l = −12→14 |
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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.073 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.88 | w = 1/[σ2(Fo2) + (0.0213P)2] where P = (Fo2 + 2Fc2)/3 |
3387 reflections | (Δ/σ)max < 0.001 |
256 parameters | Δρmax = 0.70 e Å−3 |
5 restraints | Δρmin = −1.09 e Å−3 |
Crystal data top [Ag4(C7H4O6S)2(C4H4N2)3(H2O)2]·2H2O | γ = 82.882 (5)° |
Mr = 1176.14 | V = 843.2 (7) Å3 |
Triclinic, P1 | Z = 1 |
a = 7.646 (5) Å | Mo Kα radiation |
b = 10.340 (4) Å | µ = 2.50 mm−1 |
c = 11.375 (4) Å | T = 293 K |
α = 78.751 (3)° | 0.21 × 0.15 × 0.12 mm |
β = 73.436 (4)° | |
Data collection top Bruker APEX CCD diffractometer | 3387 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2190 reflections with I > 2σ(I) |
Tmin = 0.622, Tmax = 0.754 | Rint = 0.058 |
7253 measured reflections | |
Refinement top R[F2 > 2σ(F2)] = 0.033 | 5 restraints |
wR(F2) = 0.073 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.88 | Δρmax = 0.70 e Å−3 |
3387 reflections | Δρmin = −1.09 e Å−3 |
256 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ag1 | 0.29090 (6) | 0.17665 (4) | −0.29686 (4) | 0.03972 (13) | |
Ag2 | 0.39877 (5) | 0.41619 (4) | 0.22945 (4) | 0.03870 (13) | |
C1 | 0.1323 (5) | 0.1138 (4) | −0.6235 (4) | 0.0216 (9) | |
C2 | 0.2275 (6) | −0.0059 (4) | −0.6494 (4) | 0.0253 (10) | |
C3 | 0.1985 (6) | −0.0669 (4) | −0.7399 (4) | 0.0288 (10) | |
H3 | 0.2663 | −0.1448 | −0.7589 | 0.035* | |
C4 | 0.0686 (6) | −0.0115 (4) | −0.8019 (4) | 0.0263 (10) | |
H4 | 0.0493 | −0.0518 | −0.8630 | 0.032* | |
C5 | −0.0332 (5) | 0.1047 (4) | −0.7726 (4) | 0.0219 (9) | |
C6 | −0.0001 (5) | 0.1680 (4) | −0.6871 (4) | 0.0214 (9) | |
H6 | −0.0656 | 0.2474 | −0.6709 | 0.026* | |
C7 | 0.1616 (6) | 0.1842 (5) | −0.5288 (4) | 0.0266 (10) | |
C8 | 0.3541 (6) | 0.1792 (5) | −0.0457 (4) | 0.0311 (11) | |
H8 | 0.3830 | 0.0903 | −0.0517 | 0.037* | |
C9 | 0.3716 (6) | 0.2241 (4) | 0.0570 (4) | 0.0299 (11) | |
H9 | 0.4142 | 0.1646 | 0.1171 | 0.036* | |
C10 | 0.2678 (6) | 0.4298 (5) | −0.0175 (4) | 0.0317 (11) | |
H10 | 0.2345 | 0.5181 | −0.0100 | 0.038* | |
C11 | 0.2525 (6) | 0.3863 (5) | −0.1201 (5) | 0.0322 (11) | |
H11 | 0.2101 | 0.4459 | −0.1802 | 0.039* | |
C12 | 0.5470 (6) | 0.3813 (5) | 0.4676 (4) | 0.0288 (10) | |
H12 | 0.5817 | 0.2972 | 0.4474 | 0.035* | |
C13 | 0.4107 (6) | 0.5879 (5) | 0.4325 (4) | 0.0294 (11) | |
H13 | 0.3477 | 0.6518 | 0.3871 | 0.035* | |
N1 | 0.2969 (5) | 0.2599 (4) | −0.1363 (3) | 0.0280 (9) | |
N2 | 0.3295 (5) | 0.3496 (4) | 0.0728 (4) | 0.0281 (9) | |
N3 | 0.4568 (5) | 0.4690 (4) | 0.3978 (3) | 0.0288 (9) | |
O1 | −0.3073 (6) | 0.2729 (4) | −0.7854 (4) | 0.0730 (16) | |
O2 | −0.1208 (6) | 0.2172 (5) | −0.9749 (4) | 0.0738 (14) | |
O3 | −0.3110 (6) | 0.0589 (4) | −0.8372 (5) | 0.0805 (17) | |
O4 | 0.3512 (4) | −0.0688 (3) | −0.5882 (3) | 0.0359 (8) | |
H4A | 0.3588 | −0.0253 | −0.5370 | 0.054* | |
O5 | 0.0833 (5) | 0.2950 (3) | −0.5153 (3) | 0.0421 (9) | |
O6 | 0.2710 (4) | 0.1232 (3) | −0.4660 (3) | 0.0353 (8) | |
S1 | −0.20943 (15) | 0.16850 (10) | −0.84628 (11) | 0.0261 (3) | |
OW1 | 0.0538 (5) | 0.4656 (4) | −0.3518 (4) | 0.0460 (10) | |
H1A | 0.072 (8) | 0.403 (5) | −0.397 (5) | 0.069* | |
H1B | 0.021 (8) | 0.542 (3) | −0.393 (5) | 0.069* | |
OW2 | 0.2451 (5) | 0.6472 (4) | 0.1729 (4) | 0.0449 (9) | |
H2A | 0.230 (8) | 0.686 (5) | 0.100 (3) | 0.067* | |
H2B | 0.128 (3) | 0.648 (3) | 0.218 (4) | 0.067* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ag1 | 0.0586 (3) | 0.0419 (3) | 0.0292 (2) | −0.00358 (19) | −0.0243 (2) | −0.01205 (18) |
Ag2 | 0.0527 (2) | 0.0423 (3) | 0.0330 (3) | 0.00471 (18) | −0.0272 (2) | −0.01620 (19) |
C1 | 0.026 (2) | 0.019 (2) | 0.022 (2) | 0.0003 (17) | −0.009 (2) | −0.0059 (18) |
C2 | 0.028 (2) | 0.022 (2) | 0.025 (3) | 0.0019 (18) | −0.011 (2) | 0.0001 (19) |
C3 | 0.034 (2) | 0.023 (2) | 0.030 (3) | 0.0092 (19) | −0.012 (2) | −0.010 (2) |
C4 | 0.033 (2) | 0.025 (3) | 0.026 (3) | −0.0005 (19) | −0.012 (2) | −0.011 (2) |
C5 | 0.026 (2) | 0.022 (2) | 0.020 (2) | 0.0034 (18) | −0.010 (2) | −0.0069 (18) |
C6 | 0.026 (2) | 0.019 (2) | 0.020 (2) | 0.0019 (17) | −0.009 (2) | −0.0044 (18) |
C7 | 0.033 (2) | 0.029 (3) | 0.021 (3) | −0.004 (2) | −0.013 (2) | −0.004 (2) |
C8 | 0.040 (3) | 0.025 (3) | 0.032 (3) | 0.003 (2) | −0.016 (2) | −0.007 (2) |
C9 | 0.035 (2) | 0.029 (3) | 0.030 (3) | 0.001 (2) | −0.017 (2) | −0.004 (2) |
C10 | 0.041 (3) | 0.028 (3) | 0.032 (3) | 0.006 (2) | −0.020 (2) | −0.010 (2) |
C11 | 0.040 (3) | 0.031 (3) | 0.031 (3) | −0.001 (2) | −0.022 (2) | −0.002 (2) |
C12 | 0.039 (3) | 0.022 (3) | 0.026 (3) | 0.003 (2) | −0.011 (2) | −0.006 (2) |
C13 | 0.039 (3) | 0.026 (3) | 0.026 (3) | 0.003 (2) | −0.015 (2) | −0.005 (2) |
N1 | 0.031 (2) | 0.032 (2) | 0.024 (2) | −0.0006 (17) | −0.0104 (18) | −0.0063 (18) |
N2 | 0.030 (2) | 0.033 (2) | 0.026 (2) | −0.0027 (17) | −0.0116 (19) | −0.0080 (18) |
N3 | 0.034 (2) | 0.033 (2) | 0.022 (2) | −0.0005 (17) | −0.0131 (19) | −0.0043 (18) |
O1 | 0.076 (3) | 0.092 (3) | 0.077 (3) | 0.056 (3) | −0.058 (3) | −0.059 (3) |
O2 | 0.066 (3) | 0.111 (4) | 0.036 (3) | 0.010 (3) | −0.025 (2) | 0.012 (2) |
O3 | 0.082 (3) | 0.041 (3) | 0.143 (5) | −0.019 (2) | −0.087 (4) | 0.020 (3) |
O4 | 0.0398 (18) | 0.035 (2) | 0.041 (2) | 0.0159 (15) | −0.0263 (18) | −0.0129 (16) |
O5 | 0.066 (2) | 0.029 (2) | 0.047 (2) | 0.0100 (17) | −0.037 (2) | −0.0191 (17) |
O6 | 0.0442 (19) | 0.039 (2) | 0.033 (2) | 0.0043 (16) | −0.0252 (18) | −0.0135 (16) |
S1 | 0.0345 (6) | 0.0234 (6) | 0.0274 (7) | 0.0032 (5) | −0.0195 (5) | −0.0074 (5) |
OW1 | 0.068 (3) | 0.041 (2) | 0.036 (2) | 0.001 (2) | −0.026 (2) | −0.0095 (18) |
OW2 | 0.059 (2) | 0.039 (2) | 0.039 (2) | 0.0057 (18) | −0.020 (2) | −0.0083 (18) |
Geometric parameters (Å, º) top Ag1—N1 | 2.180 (3) | C8—H8 | 0.9300 |
Ag1—O3i | 2.621 (3) | C9—N2 | 1.332 (5) |
Ag1—O6 | 2.153 (3) | C9—H9 | 0.9300 |
Ag2—N2 | 2.245 (3) | C10—N2 | 1.346 (6) |
Ag2—N3 | 2.262 (3) | C10—C11 | 1.368 (6) |
Ag2—O1ii | 2.516 (4) | C10—H10 | 0.9300 |
Ag2—OW2 | 2.576 (4) | C11—N1 | 1.343 (6) |
C1—C2 | 1.395 (6) | C11—H11 | 0.9300 |
C1—C6 | 1.408 (5) | C12—N3 | 1.343 (5) |
C1—C7 | 1.491 (6) | C12—C13iii | 1.369 (6) |
C2—O4 | 1.360 (5) | C12—H12 | 0.9300 |
C2—C3 | 1.388 (6) | C13—N3 | 1.340 (5) |
C3—C4 | 1.382 (6) | C13—C12iii | 1.369 (6) |
C3—H3 | 0.9300 | C13—H13 | 0.9300 |
C4—C5 | 1.392 (6) | O1—S1 | 1.415 (3) |
C4—H4 | 0.9300 | O2—S1 | 1.444 (5) |
C5—C6 | 1.366 (5) | O3—S1 | 1.423 (4) |
C5—S1 | 1.778 (4) | O4—H4A | 0.8200 |
C6—H6 | 0.9300 | OW1—H1A | 0.88 (2) |
C7—O5 | 1.241 (5) | OW1—H1B | 0.89 (2) |
C7—O6 | 1.281 (5) | OW2—H2A | 0.88 (2) |
C8—N1 | 1.335 (6) | OW2—H2B | 0.89 (2) |
C8—C9 | 1.383 (6) | | |
| | | |
O6—Ag1—N1 | 171.57 (13) | N2—C10—C11 | 122.4 (4) |
N2—Ag2—N3 | 175.29 (14) | N2—C10—H10 | 118.8 |
N2—Ag2—O1ii | 95.52 (12) | C11—C10—H10 | 118.8 |
N3—Ag2—O1ii | 84.24 (12) | N1—C11—C10 | 121.9 (4) |
N2—Ag2—OW2 | 89.83 (12) | N1—C11—H11 | 119.1 |
N3—Ag2—OW2 | 92.92 (12) | C10—C11—H11 | 119.1 |
O1ii—Ag2—OW2 | 147.05 (16) | N3—C12—C13iii | 121.9 (4) |
C2—C1—C6 | 118.4 (3) | N3—C12—H12 | 119.0 |
C2—C1—C7 | 122.6 (4) | C13iii—C12—H12 | 119.0 |
C6—C1—C7 | 119.0 (4) | N3—C13—C12iii | 122.3 (4) |
O4—C2—C1 | 122.5 (3) | N3—C13—H13 | 118.8 |
O4—C2—C3 | 116.8 (4) | C12iii—C13—H13 | 118.8 |
C1—C2—C3 | 120.8 (4) | C8—N1—C11 | 116.0 (4) |
C4—C3—C2 | 119.8 (4) | C8—N1—Ag1 | 117.5 (3) |
C4—C3—H3 | 120.1 | C11—N1—Ag1 | 126.5 (3) |
C2—C3—H3 | 120.1 | C9—N2—C10 | 115.6 (4) |
C3—C4—C5 | 119.8 (3) | C9—N2—Ag2 | 118.8 (3) |
C3—C4—H4 | 120.1 | C10—N2—Ag2 | 125.1 (3) |
C5—C4—H4 | 120.1 | C13—N3—C12 | 115.8 (4) |
C6—C5—C4 | 120.6 (3) | C13—N3—Ag2 | 123.5 (3) |
C6—C5—S1 | 120.4 (3) | C12—N3—Ag2 | 120.7 (3) |
C4—C5—S1 | 119.1 (3) | S1—O1—Ag2iv | 139.7 (2) |
C5—C6—C1 | 120.5 (4) | C2—O4—H4A | 109.5 |
C5—C6—H6 | 119.7 | C7—O6—Ag1 | 123.7 (3) |
C1—C6—H6 | 119.7 | O1—S1—O3 | 115.8 (3) |
O5—C7—O6 | 124.1 (3) | O1—S1—O2 | 110.9 (3) |
O5—C7—C1 | 120.2 (4) | O3—S1—O2 | 110.4 (3) |
O6—C7—C1 | 115.6 (4) | O1—S1—C5 | 106.73 (19) |
N1—C8—C9 | 121.9 (4) | O3—S1—C5 | 105.6 (2) |
N1—C8—H8 | 119.1 | O2—S1—C5 | 106.9 (2) |
C9—C8—H8 | 119.1 | H1A—OW1—H1B | 110 (6) |
N2—C9—C8 | 122.2 (4) | Ag2—OW2—H2A | 128 (4) |
N2—C9—H9 | 118.9 | Ag2—OW2—H2B | 107.5 (17) |
C8—C9—H9 | 118.9 | H2A—OW2—H2B | 100 (5) |
| | | |
C6—C1—C2—O4 | −176.7 (4) | C11—C10—N2—C9 | −1.2 (7) |
C7—C1—C2—O4 | 1.4 (7) | C11—C10—N2—Ag2 | 170.5 (4) |
C6—C1—C2—C3 | 3.1 (7) | O1ii—Ag2—N2—C9 | 35.7 (4) |
C7—C1—C2—C3 | −178.8 (4) | OW2—Ag2—N2—C9 | −176.9 (4) |
O4—C2—C3—C4 | 177.1 (4) | O1ii—Ag2—N2—C10 | −135.8 (4) |
C1—C2—C3—C4 | −2.7 (7) | OW2—Ag2—N2—C10 | 11.6 (4) |
C2—C3—C4—C5 | −0.4 (7) | C12iii—C13—N3—C12 | 0.2 (8) |
C3—C4—C5—C6 | 3.1 (7) | C12iii—C13—N3—Ag2 | −177.7 (3) |
C3—C4—C5—S1 | −176.0 (4) | C13iii—C12—N3—C13 | −0.2 (8) |
C4—C5—C6—C1 | −2.6 (7) | C13iii—C12—N3—Ag2 | 177.8 (3) |
S1—C5—C6—C1 | 176.4 (3) | O1ii—Ag2—N3—C13 | 147.0 (4) |
C2—C1—C6—C5 | −0.4 (7) | OW2—Ag2—N3—C13 | −0.1 (4) |
C7—C1—C6—C5 | −178.6 (4) | O1ii—Ag2—N3—C12 | −30.8 (4) |
C2—C1—C7—O5 | 174.9 (5) | OW2—Ag2—N3—C12 | −177.9 (4) |
C6—C1—C7—O5 | −7.0 (7) | O5—C7—O6—Ag1 | 15.5 (7) |
C2—C1—C7—O6 | −4.6 (7) | C1—C7—O6—Ag1 | −165.0 (3) |
C6—C1—C7—O6 | 173.5 (4) | Ag2iv—O1—S1—O3 | −50.2 (6) |
N1—C8—C9—N2 | 1.2 (7) | Ag2iv—O1—S1—O2 | 76.5 (5) |
N2—C10—C11—N1 | 0.5 (7) | Ag2iv—O1—S1—C5 | −167.4 (4) |
C9—C8—N1—C11 | −1.8 (7) | C6—C5—S1—O1 | −8.2 (5) |
C9—C8—N1—Ag1 | 176.7 (3) | C4—C5—S1—O1 | 170.9 (4) |
C10—C11—N1—C8 | 1.0 (7) | C6—C5—S1—O3 | −132.0 (4) |
C10—C11—N1—Ag1 | −177.4 (4) | C4—C5—S1—O3 | 47.1 (5) |
C8—C9—N2—C10 | 0.3 (7) | C6—C5—S1—O2 | 110.5 (4) |
C8—C9—N2—Ag2 | −171.9 (3) | C4—C5—S1—O2 | −70.4 (4) |
Symmetry codes: (i) −x, −y, −z−1; (ii) x+1, y, z+1; (iii) −x+1, −y+1, −z+1; (iv) x−1, y, z−1. |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
OW1—H1A···O5 | 0.88 (2) | 1.89 (2) | 2.751 (4) | 168 (6) |
OW1—H1B···O5v | 0.89 (2) | 2.00 (2) | 2.883 (5) | 173 (6) |
OW2—H2A···O2v | 0.88 (2) | 1.91 (3) | 2.757 (5) | 161 (6) |
OW2—H2B···OW1vi | 0.89 (2) | 2.03 (3) | 2.794 (6) | 143 (2) |
O4—H4A···O6 | 0.82 | 1.84 | 2.556 (4) | 146 |
Symmetry codes: (v) −x, −y+1, −z−1; (vi) −x, −y+1, −z. |
Experimental details
Crystal data |
Chemical formula | [Ag4(C7H4O6S)2(C4H4N2)3(H2O)2]·2H2O |
Mr | 1176.14 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 7.646 (5), 10.340 (4), 11.375 (4) |
α, β, γ (°) | 78.751 (3), 73.436 (4), 82.882 (5) |
V (Å3) | 843.2 (7) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 2.50 |
Crystal size (mm) | 0.21 × 0.15 × 0.12 |
|
Data collection |
Diffractometer | Bruker APEX CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.622, 0.754 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7253, 3387, 2190 |
Rint | 0.058 |
(sin θ/λ)max (Å−1) | 0.650 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.073, 0.88 |
No. of reflections | 3387 |
No. of parameters | 256 |
No. of restraints | 5 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.70, −1.09 |
Selected bond lengths (Å) topAg1—N1 | 2.180 (3) | Ag2—N3 | 2.262 (3) |
Ag1—O3i | 2.621 (3) | Ag2—O1ii | 2.516 (4) |
Ag1—O6 | 2.153 (3) | Ag2—OW2 | 2.576 (4) |
Ag2—N2 | 2.245 (3) | | |
Symmetry codes: (i) −x, −y, −z−1; (ii) x+1, y, z+1. |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
OW1—H1A···O5 | 0.88 (2) | 1.89 (2) | 2.751 (4) | 168 (6) |
OW1—H1B···O5iii | 0.89 (2) | 2.00 (2) | 2.883 (5) | 173 (6) |
OW2—H2A···O2iii | 0.88 (2) | 1.91 (3) | 2.757 (5) | 161 (6) |
OW2—H2B···OW1iv | 0.89 (2) | 2.03 (3) | 2.794 (6) | 143 (2) |
O4—H4A···O6 | 0.82 | 1.84 | 2.556 (4) | 146 |
Symmetry codes: (iii) −x, −y+1, −z−1; (iv) −x, −y+1, −z. |
Acknowledgements
We thank the China Postdoctoral Science Foundation (20100471379) for support.
References
Brandenburg, K. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Bruker (2007). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Nie, X. & Qu, J.-N. (2011). Acta Cryst. E67, m1107–m1108. Web of Science CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
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| CRYSTALLOGRAPHIC COMMUNICATIONS |
ISSN: 2056-9890
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As part of an investigation of the applications of transition metal complexes, there is a need to prepare further examples of these compounds. In this paper, the structure of the title compound is described.
As shown in Fig. 1, there exist two crystallographically independent AgI ions. Ag1 atom is three-coordinated (Table 1), having an approximate T-shaped geometry composed of one sulfonate O atom, one carboxylate O atom from two 3-carboxylate-4-hydroxybenzenesulfonate (L) ligands and one N atom from a pyrazine ligand. Ag2 atom is coordinated by one sulfonate O atom of an L ligand, two N atoms from two pyrazine ligands and one water molecule (Nie & Qu, 2011). The AgI ions are bridged by the L and pyrazine ligands, forming a two-dimensional polymeric layer (Fig. 2). The layers are connected by intermolecular O—H···O hydrogen bonds (Table 2). An intramolecular O—H···O hydrogen bond is present in the L ligand.