Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807013347/ci2304sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807013347/ci2304Isup2.hkl |
CCDC reference: 642944
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.007 Å
- H-atom completeness 81%
- R factor = 0.036
- wR factor = 0.070
- Data-to-parameter ratio = 16.0
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.80 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.59 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.05
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C8 H10 Ag2 N2 O5 Atom count from _chemical_formula_moiety:C8 H9 Ag2 N2 O4 FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C8 H10 Ag2 N2 O5 Atom count from the _atom_site data: C8 H8 Ag2 N2 O5 ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.593 Tmax scaled 0.406 Tmin scaled 0.229 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C8 H10 Ag2 N2 O5 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 32.00 32.00 0.00 H 40.00 32.00 8.00 Ag 8.00 8.00 0.00 N 8.00 8.00 0.00 O 20.00 20.00 0.00 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 7 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and MaterialsStudio (Accelrys, 2002); software used to prepare material for publication: SHELXTL.
[Ag2(C4H4NO2)2(H2O)] | F(000) = 824 |
Mr = 429.92 | Dx = 2.620 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 5112 reflections |
a = 7.6776 (2) Å | θ = 1.0–27.5° |
b = 8.0431 (2) Å | µ = 3.60 mm−1 |
c = 17.8184 (5) Å | T = 293 K |
β = 97.916 (1)° | Block, white |
V = 1089.83 (5) Å3 | 0.37 × 0.37 × 0.25 mm |
Z = 4 |
Nonius KappaCCD diffractometer | 2481 independent reflections |
Radiation source: fine-focus sealed tube | 1653 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.088 |
Detector resolution: 9 pixels mm-1 | θmax = 27.5°, θmin = 4.5° |
φ scans | h = −9→9 |
Absorption correction: multi-scan (SORTAV; Blessing 1995) | k = −10→10 |
Tmin = 0.386, Tmax = 0.685 | l = −19→23 |
10974 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.036 | H-atom parameters constrained |
wR(F2) = 0.070 | w = 1/[σ2(Fo2) + (0.0262P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.95 | (Δ/σ)max = 0.001 |
2481 reflections | Δρmax = 0.69 e Å−3 |
155 parameters | Δρmin = −0.80 e Å−3 |
0 restraints | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0185 (6) |
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 | 0.87381 (5) | −0.03959 (4) | 0.921975 (19) | 0.03061 (15) | |
Ag2 | 0.84483 (5) | 0.29065 (5) | 0.99945 (2) | 0.04026 (16) | |
O1 | 0.7851 (6) | −0.4117 (4) | 0.9834 (2) | 0.0529 (11) | |
O2 | 0.6696 (5) | 0.1070 (4) | 1.06085 (18) | 0.0415 (9) | |
O3 | 1.0294 (6) | −0.1202 (4) | 0.75477 (18) | 0.0579 (11) | |
O4 | 0.8721 (5) | 0.3471 (4) | 0.87045 (17) | 0.0439 (9) | |
O5 | 0.9515 (6) | 0.3477 (5) | 1.1305 (2) | 0.0623 (12) | |
N1 | 0.7557 (5) | −0.1366 (4) | 1.01049 (18) | 0.0266 (9) | |
N2 | 0.9383 (5) | 0.0905 (4) | 0.8278 (2) | 0.0296 (9) | |
C1 | 0.7264 (7) | −0.3015 (6) | 1.0210 (3) | 0.0318 (11) | |
C2 | 0.6175 (7) | −0.3305 (6) | 1.0832 (3) | 0.0384 (13) | |
H2A | 0.6805 | −0.3977 | 1.1233 | 0.046* | |
H2B | 0.5075 | −0.3850 | 1.0642 | 0.046* | |
C3 | 0.5858 (6) | −0.1564 (6) | 1.1110 (3) | 0.0349 (12) | |
H3A | 0.4610 | −0.1331 | 1.1071 | 0.042* | |
H3B | 0.6386 | −0.1423 | 1.1633 | 0.042* | |
C4 | 0.6724 (6) | −0.0453 (6) | 1.0594 (2) | 0.0295 (11) | |
C5 | 0.9951 (7) | 0.0267 (6) | 0.7630 (3) | 0.0363 (12) | |
C6 | 1.0046 (8) | 0.1605 (6) | 0.7052 (3) | 0.0432 (14) | |
H6A | 0.9190 | 0.1418 | 0.6607 | 0.052* | |
H6B | 1.1210 | 0.1661 | 0.6900 | 0.052* | |
C7 | 0.9632 (8) | 0.3171 (6) | 0.7460 (3) | 0.0440 (14) | |
H7A | 0.8646 | 0.3756 | 0.7178 | 0.053* | |
H7B | 1.0641 | 0.3908 | 0.7533 | 0.053* | |
C8 | 0.9177 (6) | 0.2555 (6) | 0.8211 (3) | 0.0321 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0407 (3) | 0.0267 (2) | 0.0268 (2) | −0.00013 (16) | 0.01290 (16) | 0.00202 (14) |
Ag2 | 0.0531 (3) | 0.0291 (2) | 0.0409 (3) | 0.00130 (18) | 0.01451 (19) | 0.00364 (17) |
O1 | 0.087 (3) | 0.030 (2) | 0.049 (2) | 0.009 (2) | 0.034 (2) | 0.0077 (17) |
O2 | 0.058 (3) | 0.021 (2) | 0.050 (2) | −0.0038 (18) | 0.0245 (19) | −0.0015 (16) |
O3 | 0.107 (4) | 0.030 (2) | 0.044 (2) | 0.013 (2) | 0.035 (2) | 0.0011 (18) |
O4 | 0.075 (3) | 0.0278 (19) | 0.0325 (19) | 0.0019 (18) | 0.0193 (18) | −0.0012 (16) |
O5 | 0.085 (3) | 0.050 (2) | 0.051 (2) | −0.025 (2) | 0.004 (2) | −0.0008 (19) |
N1 | 0.033 (2) | 0.024 (2) | 0.024 (2) | −0.0041 (18) | 0.0112 (17) | 0.0001 (16) |
N2 | 0.040 (3) | 0.024 (2) | 0.027 (2) | 0.0007 (17) | 0.0122 (18) | −0.0012 (16) |
C1 | 0.038 (3) | 0.032 (3) | 0.027 (3) | 0.006 (2) | 0.008 (2) | 0.003 (2) |
C2 | 0.052 (3) | 0.031 (3) | 0.036 (3) | −0.008 (2) | 0.018 (2) | 0.003 (2) |
C3 | 0.038 (3) | 0.034 (3) | 0.035 (3) | 0.001 (2) | 0.014 (2) | 0.000 (2) |
C4 | 0.031 (3) | 0.033 (3) | 0.024 (2) | −0.005 (2) | 0.004 (2) | 0.002 (2) |
C5 | 0.048 (3) | 0.037 (3) | 0.024 (3) | −0.005 (3) | 0.007 (2) | −0.002 (2) |
C6 | 0.065 (4) | 0.038 (3) | 0.030 (3) | 0.005 (3) | 0.019 (3) | 0.007 (2) |
C7 | 0.064 (4) | 0.034 (3) | 0.036 (3) | 0.002 (3) | 0.014 (3) | 0.006 (2) |
C8 | 0.039 (3) | 0.029 (3) | 0.027 (3) | −0.005 (2) | 0.002 (2) | 0.002 (2) |
Ag1—N1 | 2.077 (3) | N2—C8 | 1.340 (5) |
Ag1—N2 | 2.095 (3) | N2—C5 | 1.386 (6) |
Ag1—Ag2i | 3.1418 (5) | C1—C2 | 1.496 (6) |
Ag1—Ag1i | 3.2261 (7) | C2—C3 | 1.516 (6) |
Ag2—O2 | 2.365 (3) | C2—H2A | 0.97 |
Ag2—O4 | 2.380 (3) | C2—H2B | 0.97 |
Ag2—O5 | 2.410 (4) | C3—C4 | 1.501 (6) |
Ag2—O1ii | 2.447 (3) | C3—H3A | 0.97 |
Ag2—Ag1i | 3.1418 (5) | C3—H3B | 0.97 |
O1—C1 | 1.233 (5) | C5—C6 | 1.499 (6) |
O1—Ag2iii | 2.447 (3) | C6—C7 | 1.509 (6) |
O2—C4 | 1.226 (5) | C6—H6A | 0.97 |
O3—C5 | 1.223 (5) | C6—H6B | 0.97 |
O4—C8 | 1.234 (5) | C7—C8 | 1.513 (6) |
N1—C1 | 1.362 (5) | C7—H7A | 0.97 |
N1—C4 | 1.365 (6) | C7—H7B | 0.97 |
N1—Ag1—N2 | 166.55 (15) | C1—C2—H2B | 111.1 |
N1—Ag1—Ag2i | 76.43 (10) | C3—C2—H2B | 111.1 |
N2—Ag1—Ag2i | 117.01 (11) | H2A—C2—H2B | 109.1 |
N1—Ag1—Ag1i | 72.11 (10) | C4—C3—C2 | 104.2 (4) |
N2—Ag1—Ag1i | 114.32 (11) | C4—C3—H3A | 110.9 |
Ag2i—Ag1—Ag1i | 56.517 (13) | C2—C3—H3A | 110.9 |
O2—Ag2—O4 | 134.20 (12) | C4—C3—H3B | 110.9 |
O2—Ag2—O5 | 79.03 (12) | C2—C3—H3B | 110.9 |
O4—Ag2—O5 | 146.73 (13) | H3A—C3—H3B | 108.9 |
O2—Ag2—O1ii | 123.74 (12) | O2—C4—N1 | 124.2 (4) |
O4—Ag2—O1ii | 74.98 (11) | O2—C4—C3 | 124.9 (4) |
O5—Ag2—O1ii | 87.71 (13) | N1—C4—C3 | 110.9 (4) |
O2—Ag2—Ag1i | 78.02 (9) | O3—C5—N2 | 123.7 (4) |
O4—Ag2—Ag1i | 113.98 (9) | O3—C5—C6 | 125.4 (4) |
O5—Ag2—Ag1i | 64.51 (10) | N2—C5—C6 | 110.9 (4) |
O1ii—Ag2—Ag1i | 141.93 (11) | C5—C6—C7 | 103.6 (4) |
C1—O1—Ag2iii | 135.8 (3) | C5—C6—H6A | 111.0 |
C4—O2—Ag2 | 127.0 (3) | C7—C6—H6A | 111.0 |
C8—O4—Ag2 | 130.2 (3) | C5—C6—H6B | 111.0 |
C1—N1—C4 | 109.6 (4) | C7—C6—H6B | 111.0 |
C1—N1—Ag1 | 124.6 (3) | H6A—C6—H6B | 109.0 |
C4—N1—Ag1 | 125.1 (3) | C6—C7—C8 | 104.0 (4) |
C8—N2—C5 | 109.9 (4) | C6—C7—H7A | 111.0 |
C8—N2—Ag1 | 121.8 (3) | C8—C7—H7A | 111.0 |
C5—N2—Ag1 | 128.2 (3) | C6—C7—H7B | 111.0 |
O1—C1—N1 | 123.0 (4) | C8—C7—H7B | 111.0 |
O1—C1—C2 | 125.0 (4) | H7A—C7—H7B | 109.0 |
N1—C1—C2 | 112.0 (4) | O4—C8—N2 | 124.8 (4) |
C1—C2—C3 | 103.2 (4) | O4—C8—C7 | 123.9 (4) |
C1—C2—H2A | 111.1 | N2—C8—C7 | 111.3 (4) |
C3—C2—H2A | 111.1 | ||
O4—Ag2—O2—C4 | 63.8 (4) | O1—C1—C2—C3 | 178.5 (5) |
O5—Ag2—O2—C4 | −114.1 (4) | N1—C1—C2—C3 | −0.9 (6) |
O1ii—Ag2—O2—C4 | 166.1 (4) | C1—C2—C3—C4 | 2.6 (5) |
Ag1i—Ag2—O2—C4 | −48.2 (4) | Ag2—O2—C4—N1 | −12.6 (7) |
O2—Ag2—O4—C8 | −61.9 (5) | Ag2—O2—C4—C3 | 167.2 (3) |
O5—Ag2—O4—C8 | 114.3 (4) | C1—N1—C4—O2 | −177.0 (4) |
O1ii—Ag2—O4—C8 | 175.3 (5) | Ag1—N1—C4—O2 | −6.3 (7) |
Ag1i—Ag2—O4—C8 | 34.7 (4) | C1—N1—C4—C3 | 3.3 (5) |
N2—Ag1—N1—C1 | 123.6 (6) | Ag1—N1—C4—C3 | 173.9 (3) |
Ag2i—Ag1—N1—C1 | −56.9 (3) | C2—C3—C4—O2 | 176.5 (5) |
Ag1i—Ag1—N1—C1 | −115.7 (4) | C2—C3—C4—N1 | −3.7 (5) |
N2—Ag1—N1—C4 | −45.7 (8) | C8—N2—C5—O3 | 177.8 (5) |
Ag2i—Ag1—N1—C4 | 133.8 (4) | Ag1—N2—C5—O3 | −6.1 (8) |
Ag1i—Ag1—N1—C4 | 75.0 (3) | C8—N2—C5—C6 | −3.3 (6) |
N1—Ag1—N2—C8 | 47.9 (8) | Ag1—N2—C5—C6 | 172.7 (3) |
Ag2i—Ag1—N2—C8 | −131.6 (3) | O3—C5—C6—C7 | −175.9 (6) |
Ag1i—Ag1—N2—C8 | −68.2 (4) | N2—C5—C6—C7 | 5.3 (6) |
N1—Ag1—N2—C5 | −127.7 (6) | C5—C6—C7—C8 | −4.9 (5) |
Ag2i—Ag1—N2—C5 | 52.8 (4) | Ag2—O4—C8—N2 | 10.5 (7) |
Ag1i—Ag1—N2—C5 | 116.1 (4) | Ag2—O4—C8—C7 | −167.5 (4) |
Ag2iii—O1—C1—N1 | 159.0 (4) | C5—N2—C8—O4 | −178.3 (5) |
Ag2iii—O1—C1—C2 | −20.4 (9) | Ag1—N2—C8—O4 | 5.3 (7) |
C4—N1—C1—O1 | 179.1 (5) | C5—N2—C8—C7 | −0.1 (6) |
Ag1—N1—C1—O1 | 8.4 (7) | Ag1—N2—C8—C7 | −176.5 (3) |
C4—N1—C1—C2 | −1.4 (6) | C6—C7—C8—O4 | −178.4 (5) |
Ag1—N1—C1—C2 | −172.2 (3) | C6—C7—C8—N2 | 3.4 (6) |
Symmetry codes: (i) −x+2, −y, −z+2; (ii) x, y+1, z; (iii) x, y−1, z. |
Bond/Compound | {[AgSI]2.H2O}n | [AgBOD]2 | [AgBOD.(Ph3P)2] |
Ag—N | 2.077 (3)-2.095 (3) | 2.147 (6) | 2.225 (7) |
Ag—O | 2.365 (3)-2.447 (3) | 2.170 (5) | 2.964 (8) |
Ag—Ag | 3.1418 (5)-3.2261 (7) | 2.8042 (12) | - |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register