Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807054591/lh2537sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807054591/lh2537Isup2.hkl |
CCDC reference: 672595
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.034
- wR factor = 0.107
- Data-to-parameter ratio = 15.9
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.06 PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 4 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O3 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C19 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.10
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Ag1 (9) 0.76 PLAT804_ALERT_5_G ARU-Pack Problem in PLATON Analysis ............ 10 Times PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 3
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 2 ALERT type 5 Informative message, check
A mixture of L (0.30 g, 1 mmol), AgNO3 (0.17 g, 1 mmol), fumaric acid (0.12 g, 1 mmol) and H2O (10 ml) was stirred for 1 h and then sealed in a 25 ml Teflonlined stainless steel container. The container was heated to 423 K and held at that temperature for 72 h, then cooled to room temperature at a rate of 10 K h-1. Colorless crystals of the title compound were collected in 56% yield based on Ag.
All H atoms bonded to C atoms were positioned geometrically and refined as riding atoms with C—H = 0.93 A ° and Uiso(H) = 1.2Ueq(C). The water H-atoms were located in a difference Fourier map, and were refined freely with Uiso(H) = 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, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
[Ag(C18H16N2O2)(C4H2O4)0.5]·H2O | Z = 2 |
Mr = 475.24 | F(000) = 480 |
Triclinic, P1 | Dx = 1.694 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 8.5730 (8) Å | Cell parameters from 4127 reflections |
b = 9.7120 (9) Å | θ = 1.8–28.5° |
c = 12.0990 (11) Å | µ = 1.12 mm−1 |
α = 88.845 (2)° | T = 293 K |
β = 71.867 (1)° | Block, colorless |
γ = 77.047 (2)° | 0.42 × 0.36 × 0.35 mm |
V = 931.65 (15) Å3 |
Bruker APEX CCD area-detector diffractometer | 4127 independent reflections |
Radiation source: fine-focus sealed tube | 3629 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.018 |
ω scans | θmax = 28.5°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.632, Tmax = 0.676 | k = −12→12 |
5611 measured reflections | l = −15→8 |
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)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.107 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0611P)2 + 0.3593P] where P = (Fo2 + 2Fc2)/3 |
4127 reflections | (Δ/σ)max = 0.001 |
259 parameters | Δρmax = 1.17 e Å−3 |
3 restraints | Δρmin = −0.57 e Å−3 |
[Ag(C18H16N2O2)(C4H2O4)0.5]·H2O | γ = 77.047 (2)° |
Mr = 475.24 | V = 931.65 (15) Å3 |
Triclinic, P1 | Z = 2 |
a = 8.5730 (8) Å | Mo Kα radiation |
b = 9.7120 (9) Å | µ = 1.12 mm−1 |
c = 12.0990 (11) Å | T = 293 K |
α = 88.845 (2)° | 0.42 × 0.36 × 0.35 mm |
β = 71.867 (1)° |
Bruker APEX CCD area-detector diffractometer | 4127 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3629 reflections with I > 2σ(I) |
Tmin = 0.632, Tmax = 0.676 | Rint = 0.018 |
5611 measured reflections |
R[F2 > 2σ(F2)] = 0.034 | 3 restraints |
wR(F2) = 0.107 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | Δρmax = 1.17 e Å−3 |
4127 reflections | Δρmin = −0.57 e Å−3 |
259 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 | ||
Ag1 | 0.64106 (3) | 0.45095 (3) | 0.55161 (2) | 0.04642 (11) | |
C1 | 0.4381 (4) | 0.4066 (3) | 0.8046 (3) | 0.0479 (8) | |
H1 | 0.5187 | 0.3215 | 0.7871 | 0.058* | |
C2 | 0.3196 (5) | 0.4286 (4) | 0.9124 (3) | 0.0547 (9) | |
H2 | 0.3224 | 0.3613 | 0.9680 | 0.066* | |
C3 | 0.1954 (4) | 0.5524 (4) | 0.9376 (3) | 0.0476 (7) | |
H3 | 0.1127 | 0.5687 | 1.0101 | 0.057* | |
C4 | 0.1949 (3) | 0.6511 (3) | 0.8549 (3) | 0.0352 (6) | |
C5 | 0.3232 (3) | 0.6225 (3) | 0.7493 (3) | 0.0362 (6) | |
H5 | 0.3262 | 0.6902 | 0.6937 | 0.043* | |
C6 | 0.0622 (4) | 0.7879 (3) | 0.8736 (3) | 0.0391 (6) | |
H6A | 0.1143 | 0.8682 | 0.8640 | 0.047* | |
H6B | 0.0016 | 0.7916 | 0.8175 | 0.047* | |
C7 | −0.1839 (4) | 0.9076 (3) | 1.0236 (3) | 0.0416 (7) | |
C8 | −0.2800 (4) | 0.9094 (3) | 1.1393 (3) | 0.0470 (8) | |
H8 | −0.2509 | 0.8372 | 1.1858 | 0.056* | |
C9 | −0.4204 (4) | 1.0199 (3) | 1.1857 (3) | 0.0448 (7) | |
H9 | −0.4861 | 1.0209 | 1.2631 | 0.054* | |
C10 | −0.4615 (4) | 1.1267 (3) | 1.1173 (3) | 0.0378 (6) | |
C11 | −0.3624 (4) | 1.1257 (3) | 1.0023 (3) | 0.0427 (7) | |
H11 | −0.3894 | 1.1998 | 0.9566 | 0.051* | |
C12 | −0.2235 (4) | 1.0157 (3) | 0.9544 (3) | 0.0418 (7) | |
H12 | −0.1581 | 1.0148 | 0.8769 | 0.050* | |
C13 | −0.7012 (4) | 1.2405 (3) | 1.2734 (3) | 0.0409 (7) | |
H13A | −0.6349 | 1.2422 | 1.3252 | 0.049* | |
H13B | −0.7448 | 1.1556 | 1.2856 | 0.049* | |
C14 | −0.8441 (3) | 1.3692 (3) | 1.2985 (3) | 0.0354 (6) | |
C15 | −0.9936 (3) | 1.3643 (3) | 1.3841 (3) | 0.0356 (6) | |
H15 | −1.0021 | 1.2801 | 1.4208 | 0.043* | |
C16 | −0.8321 (4) | 1.4946 (3) | 1.2444 (3) | 0.0444 (7) | |
H16 | −0.7342 | 1.5014 | 1.1858 | 0.053* | |
C17 | −0.9688 (4) | 1.6107 (4) | 1.2789 (3) | 0.0515 (8) | |
H17 | −0.9628 | 1.6967 | 1.2444 | 0.062* | |
C18 | −1.1126 (4) | 1.5963 (3) | 1.3645 (3) | 0.0457 (7) | |
H18 | −1.2037 | 1.6740 | 1.3870 | 0.055* | |
C19 | 0.6094 (4) | 0.1537 (3) | 0.5074 (3) | 0.0428 (7) | |
C20 | 0.5740 (4) | 0.0108 (3) | 0.4968 (3) | 0.0416 (7) | |
H20 | 0.6633 | −0.0679 | 0.4847 | 0.050* | |
N1 | 0.4431 (3) | 0.5020 (3) | 0.7234 (2) | 0.0388 (5) | |
N2 | −1.1269 (3) | 1.4750 (3) | 1.4167 (2) | 0.0372 (5) | |
O1 | 0.7521 (4) | 0.1564 (3) | 0.5123 (4) | 0.0778 (10) | |
O2 | 0.4997 (3) | 0.2597 (2) | 0.5080 (3) | 0.0596 (7) | |
O3 | −0.0494 (3) | 0.7919 (2) | 0.9878 (2) | 0.0562 (7) | |
O4 | −0.5989 (3) | 1.2410 (2) | 1.15538 (19) | 0.0470 (5) | |
O1W | 1.0451 (6) | −0.0306 (5) | 0.3447 (3) | 0.0956 (12) | |
H1A | 1.107 (6) | −0.084 (7) | 0.378 (5) | 0.143* | |
H1B | 0.946 (3) | −0.015 (8) | 0.392 (5) | 0.143* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.02882 (14) | 0.05097 (17) | 0.04432 (17) | −0.00020 (10) | 0.00425 (10) | −0.00846 (11) |
C1 | 0.0378 (16) | 0.0375 (15) | 0.0535 (19) | 0.0032 (12) | −0.0014 (14) | −0.0017 (14) |
C2 | 0.0462 (18) | 0.0487 (18) | 0.051 (2) | 0.0015 (15) | 0.0014 (15) | 0.0091 (15) |
C3 | 0.0387 (16) | 0.0505 (18) | 0.0394 (16) | −0.0026 (14) | 0.0027 (13) | −0.0011 (13) |
C4 | 0.0270 (13) | 0.0354 (14) | 0.0377 (15) | −0.0021 (11) | −0.0054 (11) | −0.0094 (11) |
C5 | 0.0308 (13) | 0.0347 (14) | 0.0372 (15) | −0.0031 (11) | −0.0051 (12) | −0.0056 (11) |
C6 | 0.0317 (14) | 0.0396 (14) | 0.0357 (15) | 0.0029 (11) | −0.0032 (12) | −0.0101 (11) |
C7 | 0.0293 (14) | 0.0362 (14) | 0.0451 (17) | 0.0034 (11) | 0.0011 (12) | −0.0083 (12) |
C8 | 0.0381 (16) | 0.0410 (16) | 0.0443 (17) | 0.0069 (13) | 0.0009 (14) | 0.0013 (13) |
C9 | 0.0352 (15) | 0.0450 (16) | 0.0370 (16) | 0.0042 (13) | 0.0036 (13) | −0.0042 (13) |
C10 | 0.0260 (13) | 0.0372 (14) | 0.0393 (15) | 0.0046 (11) | −0.0023 (11) | −0.0095 (11) |
C11 | 0.0346 (15) | 0.0451 (16) | 0.0386 (16) | 0.0049 (12) | −0.0072 (13) | −0.0017 (13) |
C12 | 0.0309 (14) | 0.0505 (17) | 0.0320 (14) | 0.0004 (12) | 0.0010 (12) | −0.0076 (12) |
C13 | 0.0269 (13) | 0.0400 (15) | 0.0434 (16) | 0.0025 (11) | −0.0002 (12) | −0.0058 (12) |
C14 | 0.0253 (12) | 0.0361 (14) | 0.0371 (15) | 0.0008 (10) | −0.0038 (11) | −0.0090 (11) |
C15 | 0.0259 (13) | 0.0349 (13) | 0.0384 (15) | −0.0008 (10) | −0.0031 (11) | −0.0072 (11) |
C16 | 0.0296 (14) | 0.0473 (17) | 0.0466 (17) | −0.0040 (12) | −0.0017 (13) | −0.0006 (13) |
C17 | 0.0450 (18) | 0.0400 (16) | 0.057 (2) | −0.0034 (14) | −0.0036 (16) | 0.0044 (14) |
C18 | 0.0321 (15) | 0.0407 (16) | 0.0528 (19) | 0.0047 (12) | −0.0058 (14) | −0.0073 (13) |
C19 | 0.0439 (17) | 0.0377 (15) | 0.0421 (17) | −0.0125 (13) | −0.0046 (13) | 0.0008 (12) |
C20 | 0.0426 (16) | 0.0311 (13) | 0.0450 (17) | −0.0042 (12) | −0.0079 (14) | 0.0014 (12) |
N1 | 0.0284 (11) | 0.0365 (12) | 0.0400 (13) | −0.0002 (9) | 0.0010 (10) | −0.0059 (10) |
N2 | 0.0257 (11) | 0.0378 (12) | 0.0397 (13) | 0.0001 (9) | −0.0027 (10) | −0.0107 (10) |
O1 | 0.0632 (18) | 0.0588 (17) | 0.124 (3) | −0.0218 (14) | −0.043 (2) | 0.0142 (18) |
O2 | 0.0475 (14) | 0.0339 (11) | 0.0852 (19) | −0.0040 (10) | −0.0071 (13) | −0.0046 (11) |
O3 | 0.0423 (13) | 0.0443 (12) | 0.0509 (14) | 0.0131 (10) | 0.0132 (11) | 0.0001 (10) |
O4 | 0.0330 (11) | 0.0467 (12) | 0.0403 (12) | 0.0127 (9) | 0.0029 (9) | −0.0047 (9) |
O1W | 0.093 (3) | 0.109 (3) | 0.073 (2) | −0.005 (2) | −0.022 (2) | 0.010 (2) |
Ag1—N2i | 2.202 (2) | C10—O4 | 1.388 (3) |
Ag1—N1 | 2.217 (2) | C11—C12 | 1.386 (4) |
Ag1—O2 | 2.577 (3) | C11—H11 | 0.9300 |
Ag1—Ag1ii | 3.0193 (5) | C12—H12 | 0.9300 |
C1—N1 | 1.335 (4) | C13—O4 | 1.425 (4) |
C1—C2 | 1.367 (5) | C13—C14 | 1.501 (4) |
C1—H1 | 0.9300 | C13—H13A | 0.9700 |
C2—C3 | 1.382 (5) | C13—H13B | 0.9700 |
C2—H2 | 0.9300 | C14—C16 | 1.379 (4) |
C3—C4 | 1.372 (4) | C14—C15 | 1.384 (4) |
C3—H3 | 0.9300 | C15—N2 | 1.343 (3) |
C4—C5 | 1.386 (4) | C15—H15 | 0.9300 |
C4—C6 | 1.512 (4) | C16—C17 | 1.393 (4) |
C5—N1 | 1.341 (4) | C16—H16 | 0.9300 |
C5—H5 | 0.9300 | C17—C18 | 1.375 (5) |
C6—O3 | 1.411 (4) | C17—H17 | 0.9300 |
C6—H6A | 0.9700 | C18—N2 | 1.337 (4) |
C6—H6B | 0.9700 | C18—H18 | 0.9300 |
C7—C12 | 1.377 (5) | C19—O2 | 1.228 (4) |
C7—O3 | 1.382 (3) | C19—O1 | 1.250 (4) |
C7—C8 | 1.384 (4) | C19—C20 | 1.502 (4) |
C8—C9 | 1.393 (4) | C20—C20iii | 1.309 (6) |
C8—H8 | 0.9300 | C20—H20 | 0.9300 |
C9—C10 | 1.366 (4) | N2—Ag1iv | 2.202 (2) |
C9—H9 | 0.9300 | O1W—H1A | 0.85 (6) |
C10—C11 | 1.386 (4) | O1W—H1B | 0.85 (5) |
N2i—Ag1—N1 | 153.76 (10) | C10—C11—H11 | 119.6 |
N2i—Ag1—O2 | 116.46 (9) | C7—C12—C11 | 118.9 (3) |
N1—Ag1—O2 | 89.76 (9) | C7—C12—H12 | 120.5 |
N2i—Ag1—Ag1ii | 106.01 (7) | C11—C12—H12 | 120.5 |
N1—Ag1—Ag1ii | 85.94 (7) | O4—C13—C14 | 108.2 (2) |
O2—Ag1—Ag1ii | 63.49 (6) | O4—C13—H13A | 110.1 |
N1—C1—C2 | 122.8 (3) | C14—C13—H13A | 110.1 |
N1—C1—H1 | 118.6 | O4—C13—H13B | 110.1 |
C2—C1—H1 | 118.6 | C14—C13—H13B | 110.1 |
C1—C2—C3 | 119.0 (3) | H13A—C13—H13B | 108.4 |
C1—C2—H2 | 120.5 | C16—C14—C15 | 118.0 (3) |
C3—C2—H2 | 120.5 | C16—C14—C13 | 123.5 (3) |
C4—C3—C2 | 119.5 (3) | C15—C14—C13 | 118.4 (3) |
C4—C3—H3 | 120.2 | N2—C15—C14 | 123.4 (3) |
C2—C3—H3 | 120.2 | N2—C15—H15 | 118.3 |
C3—C4—C5 | 117.7 (3) | C14—C15—H15 | 118.3 |
C3—C4—C6 | 123.3 (3) | C14—C16—C17 | 119.1 (3) |
C5—C4—C6 | 119.0 (3) | C14—C16—H16 | 120.5 |
N1—C5—C4 | 123.3 (3) | C17—C16—H16 | 120.5 |
N1—C5—H5 | 118.4 | C18—C17—C16 | 119.0 (3) |
C4—C5—H5 | 118.4 | C18—C17—H17 | 120.5 |
O3—C6—C4 | 107.4 (2) | C16—C17—H17 | 120.5 |
O3—C6—H6A | 110.2 | N2—C18—C17 | 122.6 (3) |
C4—C6—H6A | 110.2 | N2—C18—H18 | 118.7 |
O3—C6—H6B | 110.2 | C17—C18—H18 | 118.7 |
C4—C6—H6B | 110.2 | O2—C19—O1 | 124.1 (3) |
H6A—C6—H6B | 108.5 | O2—C19—C20 | 118.8 (3) |
C12—C7—O3 | 125.2 (3) | O1—C19—C20 | 117.1 (3) |
C12—C7—C8 | 120.7 (3) | C20iii—C20—C19 | 124.6 (4) |
O3—C7—C8 | 114.1 (3) | C20iii—C20—H20 | 117.7 |
C7—C8—C9 | 119.7 (3) | C19—C20—H20 | 117.7 |
C7—C8—H8 | 120.1 | C1—N1—C5 | 117.7 (3) |
C9—C8—H8 | 120.1 | C1—N1—Ag1 | 118.8 (2) |
C10—C9—C8 | 120.0 (3) | C5—N1—Ag1 | 123.5 (2) |
C10—C9—H9 | 120.0 | C18—N2—C15 | 117.9 (3) |
C8—C9—H9 | 120.0 | C18—N2—Ag1iv | 122.60 (19) |
C9—C10—C11 | 119.9 (3) | C15—N2—Ag1iv | 119.5 (2) |
C9—C10—O4 | 124.3 (3) | C19—O2—Ag1 | 99.6 (2) |
C11—C10—O4 | 115.8 (3) | C7—O3—C6 | 117.5 (2) |
C12—C11—C10 | 120.8 (3) | C10—O4—C13 | 115.5 (2) |
C12—C11—H11 | 119.6 | H1A—O1W—H1B | 106 (6) |
N1—C1—C2—C3 | 2.4 (6) | O1—C19—C20—C20iii | 172.3 (4) |
C1—C2—C3—C4 | −0.9 (6) | C2—C1—N1—C5 | −1.6 (5) |
C2—C3—C4—C5 | −1.3 (5) | C2—C1—N1—Ag1 | −179.4 (3) |
C2—C3—C4—C6 | 178.6 (3) | C4—C5—N1—C1 | −0.8 (5) |
C3—C4—C5—N1 | 2.2 (5) | C4—C5—N1—Ag1 | 176.9 (2) |
C6—C4—C5—N1 | −177.7 (3) | N2i—Ag1—N1—C1 | −109.7 (3) |
C3—C4—C6—O3 | 1.5 (4) | O2—Ag1—N1—C1 | 68.1 (3) |
C5—C4—C6—O3 | −178.6 (3) | Ag1ii—Ag1—N1—C1 | 131.5 (3) |
C12—C7—C8—C9 | 1.5 (5) | N2i—Ag1—N1—C5 | 72.7 (3) |
O3—C7—C8—C9 | −179.3 (3) | O2—Ag1—N1—C5 | −109.5 (2) |
C7—C8—C9—C10 | −0.8 (5) | Ag1ii—Ag1—N1—C5 | −46.1 (2) |
C8—C9—C10—C11 | −0.7 (5) | C17—C18—N2—C15 | 0.8 (5) |
C8—C9—C10—O4 | 179.9 (3) | C17—C18—N2—Ag1iv | −178.9 (3) |
C9—C10—C11—C12 | 1.5 (5) | C14—C15—N2—C18 | −0.9 (5) |
O4—C10—C11—C12 | −179.0 (3) | C14—C15—N2—Ag1iv | 178.7 (2) |
O3—C7—C12—C11 | −179.8 (3) | O1—C19—O2—Ag1 | −7.9 (4) |
C8—C7—C12—C11 | −0.7 (5) | C20—C19—O2—Ag1 | 173.8 (2) |
C10—C11—C12—C7 | −0.8 (5) | N2i—Ag1—O2—C19 | 65.7 (2) |
O4—C13—C14—C16 | −30.1 (4) | N1—Ag1—O2—C19 | −113.2 (2) |
O4—C13—C14—C15 | 152.9 (3) | Ag1ii—Ag1—O2—C19 | 161.2 (2) |
C16—C14—C15—N2 | 0.1 (5) | C12—C7—O3—C6 | 4.0 (5) |
C13—C14—C15—N2 | 177.3 (3) | C8—C7—O3—C6 | −175.2 (3) |
C15—C14—C16—C17 | 0.9 (5) | C4—C6—O3—C7 | −178.9 (3) |
C13—C14—C16—C17 | −176.2 (3) | C9—C10—O4—C13 | −1.1 (5) |
C14—C16—C17—C18 | −1.0 (6) | C11—C10—O4—C13 | 179.4 (3) |
C16—C17—C18—N2 | 0.2 (6) | C14—C13—O4—C10 | −179.0 (3) |
O2—C19—C20—C20iii | −9.4 (6) |
Symmetry codes: (i) x+2, y−1, z−1; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y, −z+1; (iv) x−2, y+1, z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1B···O1 | 0.85 (5) | 2.23 (5) | 2.941 (6) | 141 (7) |
O1W—H1A···O1v | 0.85 (6) | 2.07 (3) | 2.888 (5) | 162 (8) |
Symmetry code: (v) −x+2, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Ag(C18H16N2O2)(C4H2O4)0.5]·H2O |
Mr | 475.24 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 8.5730 (8), 9.7120 (9), 12.0990 (11) |
α, β, γ (°) | 88.845 (2), 71.867 (1), 77.047 (2) |
V (Å3) | 931.65 (15) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.12 |
Crystal size (mm) | 0.42 × 0.36 × 0.35 |
Data collection | |
Diffractometer | Bruker APEX CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.632, 0.676 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5611, 4127, 3629 |
Rint | 0.018 |
(sin θ/λ)max (Å−1) | 0.672 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.107, 1.09 |
No. of reflections | 4127 |
No. of parameters | 259 |
No. of restraints | 3 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.17, −0.57 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1990).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1B···O1 | 0.85 (5) | 2.23 (5) | 2.941 (6) | 141 (7) |
O1W—H1A···O1i | 0.85 (6) | 2.07 (3) | 2.888 (5) | 162 (8) |
Symmetry code: (i) −x+2, −y, −z+1. |
The design and synthesis of supramolecular complexes exhibiting novel structures and properties has provided exciting new prospects for chemists (Fujita et al., 1995; Yaghi et al., 1995; Zaworotko & Moulton, 2001). Among various supramolecular compounds, Ag(I) compounds are attractive because of their diverse structural types (Corespo et al., 1998). In this paper, we isolated a new Ag supramolecular compound, {[Ag(L)(fum)0.5].H2O}n, constructed using 1,4-bis(pyridin-3-ylmethoxy)benzene (L) and fumarate (fum) ligands.
In the title structure, each AgI cation is four-coordinated and shows a tetrahedral geometry, surrounded by two N atoms from different L ligands and two carboxylate oxygen atoms from different fum anions (Fig. 1). The dihedral angle between two pyridine rings in the same L ligand is 23.6 (5)°. All bond distances and angles are normal (Allen et al., 1987). The L ligands exhibit bis-monodentate coordination modes and links AgI cations to generate an extended chain, which is further linked by fumarate anions to generate a double chainlike structure (Fig. 2). The lattice water molecules donate hydrogen bonds to carboxylate oxygen atoms of fumarate anions from adjacent double-chains, thus forming an intereting two-dimensional supramolecular structure (Fig. 3).