Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807010835/bq2001sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807010835/bq2001Isup2.hkl |
CCDC reference: 642917
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- H-atom completeness 81%
- Disorder in main residue
- R factor = 0.032
- wR factor = 0.087
- Data-to-parameter ratio = 8.2
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 .... ? PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.23 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N1 PLAT301_ALERT_3_C Main Residue Disorder ......................... 18.00 Perc.
Alert level G 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:C13 H15 Ag1 N4 O7 Atom count from the _atom_site data: C13.02 H12 Ag1 N3.983 O7.08 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 2 From the CIF: _chemical_formula_sum C13 H15 Ag N4 O7 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 26.00 26.04 -0.04 H 30.00 24.00 6.00 Ag 2.00 2.00 0.00 N 8.00 7.97 0.03 O 14.00 14.16 -0.16 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 7 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 6 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 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.
[Ag(C6H12N2)](C7H3N2O7) | Dx = 1.96 Mg m−3 |
Mr = 447 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63/mmc | Cell parameters from 1000 reflections |
Hall symbol: -P 6c 2c | θ = 2.5–24.4° |
a = 11.1991 (16) Å | µ = 1.38 mm−1 |
c = 6.9696 (14) Å | T = 293 K |
V = 757.0 (2) Å3 | Block, yellow |
Z = 2 | 0.51 × 0.30 × 0.26 mm |
F(000) = 443.3 |
Siemens SMART CCD area-detector diffractometer | 288 independent reflections |
Radiation source: fine-focus sealed tube | 279 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
Detector resolution: 0 pixels mm-1 | θmax = 25.0°, θmin = 2.1° |
φ and ω scans | h = −13→8 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −12→13 |
Tmin = 0.600, Tmax = 0.700 | l = −8→8 |
3755 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)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.087 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0786P)2 + 0.2855P] where P = (Fo2 + 2Fc2)/3 |
288 reflections | (Δ/σ)max = 0.001 |
35 parameters | Δρmax = 0.54 e Å−3 |
0 restraints | Δρmin = −0.38 e Å−3 |
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 | 0.3333 | 0.6667 | 1.2500 | 0.0451 (4) | |
N1 | 0.3333 | 0.6667 | 0.9357 (8) | 0.0309 (11) | |
N2 | 0.1471 (3) | 0.8529 (3) | 0.2500 | 0.0575 (18) | 0.661 (16) |
C4 | 0.1471 (3) | 0.8529 (3) | 0.2500 | 0.0575 (18) | 0.34 |
O1 | 0.2658 (10) | 1.1329 (5) | 0.2500 | 0.062 (3) | 0.36 |
O2 | 0.0840 (5) | 0.7256 (4) | 0.2500 | 0.0818 (12) | |
C1 | 0.40496 (17) | 0.59504 (17) | 0.8606 (6) | 0.0490 (9) | |
H1A | 0.3590 | 0.5008 | 0.9070 | 0.059* | 0.50 |
H1B | 0.4992 | 0.6410 | 0.9070 | 0.059* | 0.50 |
C2 | 0.1461 (5) | 1.0731 (2) | 0.2500 | 0.0418 (11) | |
C3 | 0.0712 (3) | 0.9288 (3) | 0.2500 | 0.0463 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0580 (4) | 0.0580 (4) | 0.0192 (5) | 0.0290 (2) | 0.000 | 0.000 |
N1 | 0.0349 (15) | 0.0349 (15) | 0.023 (3) | 0.0174 (7) | 0.000 | 0.000 |
N2 | 0.073 (3) | 0.073 (3) | 0.042 (3) | 0.049 (3) | 0.000 | 0.000 |
C4 | 0.073 (3) | 0.073 (3) | 0.042 (3) | 0.049 (3) | 0.000 | 0.000 |
O1 | 0.035 (6) | 0.059 (5) | 0.083 (9) | 0.018 (3) | 0.000 | 0.000 |
O2 | 0.088 (3) | 0.069 (2) | 0.105 (4) | 0.051 (2) | 0.000 | 0.000 |
C1 | 0.0693 (19) | 0.0693 (19) | 0.031 (2) | 0.052 (2) | −0.0011 (7) | 0.0011 (7) |
C2 | 0.042 (3) | 0.053 (2) | 0.027 (2) | 0.0211 (13) | 0.000 | 0.000 |
C3 | 0.061 (2) | 0.061 (2) | 0.023 (2) | 0.035 (3) | 0.000 | 0.000 |
Ag1—N1i | 2.190 (6) | O1—C2 | 1.160 (11) |
Ag1—N1 | 2.190 (6) | C1—C1v | 1.541 (8) |
N1—C1ii | 1.485 (4) | C1—H1A | 0.9700 |
N1—C1iii | 1.485 (4) | C1—H1B | 0.9700 |
N1—C1 | 1.485 (4) | C2—C3vi | 1.400 (4) |
N2—O2iv | 1.235 (5) | C2—C3 | 1.400 (4) |
N2—O2 | 1.235 (5) | C3—C2vii | 1.400 (4) |
N2—C3 | 1.473 (7) | ||
N1i—Ag1—N1 | 180.000 (2) | N1—C1—H1A | 109.5 |
C1ii—N1—C1iii | 108.3 (3) | C1v—C1—H1A | 109.5 |
C1ii—N1—C1 | 108.3 (3) | N1—C1—H1B | 109.5 |
C1iii—N1—C1 | 108.3 (3) | C1v—C1—H1B | 109.5 |
C1ii—N1—Ag1 | 110.7 (2) | H1A—C1—H1B | 108.1 |
C1iii—N1—Ag1 | 110.7 (2) | O1—C2—C3vi | 121.3 (3) |
C1—N1—Ag1 | 110.7 (2) | O1—C2—C3 | 121.3 (3) |
O2iv—N2—O2 | 119.5 (6) | C3vi—C2—C3 | 117.5 (5) |
O2iv—N2—C3 | 120.3 (3) | C2vii—C3—C2 | 122.5 (5) |
O2—N2—C3 | 120.3 (3) | C2vii—C3—N2 | 118.7 (3) |
N1—C1—C1v | 110.7 (2) | C2—C3—N2 | 118.7 (3) |
Symmetry codes: (i) x, y, −z+5/2; (ii) −x+y, −x+1, z; (iii) −y+1, x−y+1, z; (iv) −y+1, −x+1, z; (v) x, y, −z+3/2; (vi) −y+1, x−y+2, z; (vii) −x+y−1, −x+1, z. |