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The asymmetric unit of the title compound, [Ag(NH
3)
2][Ag(C
7H
5N
2O
4)
2], comprises half an [Ag(NH
3)
2]
+ cation and half an [Ag(anbz)
2]
- anion (anbz is 2-amino-5-nitrobenzoate). Both Ag
I ions are located on inversion centres. The cation has a linear coordination geometry with two symmetry-related ammine ligands. The Ag
I cation in the anionic part shows a rare four-coordinate planar geometry completed by two chelating symmetry-related anbz ligands. Intra- and intermolecular N-H
O hydrogen bonds create a slightly undulating two-dimensional supramolecular sheet. Adjacent sheets are only
ca 3.3 Å apart. Ag
O, Ag
N and
-
stacking interactions consolidate the packing of the molecules in the solid state.
Supporting information
CCDC reference: 786797
Data collection: CrysAlis CCD (Oxford Diffraction, 2008); cell refinement: CrysAlis RED (Oxford Diffraction, 2008); data reduction: CrysAlis RED (Oxford Diffraction, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010).
Diamminesilver(I)
bis(2-amino-5-nitrobenzoato-
κ2O1,
O1')silver(I)
top
Crystal data top
[Ag(NH3)2][Ag(C7H5N2O4)2] | Z = 1 |
Mr = 612.07 | F(000) = 300 |
Triclinic, P1 | Dx = 2.225 Mg m−3 |
a = 7.1361 (5) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 7.4070 (6) Å | Cell parameters from 3627 reflections |
c = 9.9686 (6) Å | θ = 3.1–30.4° |
α = 87.064 (6)° | µ = 2.20 mm−1 |
β = 79.170 (6)° | T = 173 K |
γ = 62.077 (8)° | Block, colourless |
V = 456.86 (6) Å3 | 0.10 × 0.10 × 0.08 mm |
Data collection top
Oxford Xcalibur diffractometer with Sapphire3 Gemini Ultra detector | 1800 independent reflections |
Radiation source: Oxford Enhance (Mo) X-ray source | 1627 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.014 |
Detector resolution: 16.1903 pixels mm-1 | θmax = 26.0°, θmin = 3.1° |
ω scans | h = −8→8 |
Absorption correction: multi-scan [CrysAlisPro (Oxford Diffraction, 2009); empirical (using intensity measurements) absorption correction
using
spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm] | k = −9→8 |
Tmin = 0.810, Tmax = 0.843 | l = −11→12 |
3721 measured reflections | |
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)] = 0.017 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.048 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0303P)2 + 0.1257P] where P = (Fo2 + 2Fc2)/3 |
1800 reflections | (Δ/σ)max < 0.001 |
140 parameters | Δρmax = 0.47 e Å−3 |
0 restraints | Δρmin = −0.67 e Å−3 |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds 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 > 2sigma(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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ag1 | 1.0000 | 1.0000 | 0.0000 | 0.02992 (8) | |
Ag2 | 1.0000 | 0.5000 | 1.0000 | 0.03407 (8) | |
C1 | 0.4866 (3) | 0.7740 (2) | 0.43000 (19) | 0.0215 (4) | |
H1A | 0.4343 | 0.8069 | 0.3465 | 0.026* | |
C2 | 0.3679 (3) | 0.7409 (3) | 0.5431 (2) | 0.0218 (4) | |
H2A | 0.2307 | 0.7537 | 0.5377 | 0.026* | |
C3 | 0.4429 (3) | 0.6881 (2) | 0.66817 (18) | 0.0171 (3) | |
C4 | 0.6448 (2) | 0.6793 (2) | 0.67621 (17) | 0.0150 (3) | |
C5 | 0.7627 (2) | 0.7147 (2) | 0.56022 (17) | 0.0163 (3) | |
H5A | 0.8975 | 0.7084 | 0.5646 | 0.020* | |
C6 | 0.6876 (3) | 0.7587 (2) | 0.43890 (18) | 0.0193 (4) | |
C7 | 0.7376 (2) | 0.6277 (2) | 0.80357 (17) | 0.0159 (3) | |
N1 | 0.3238 (2) | 0.6480 (2) | 0.77528 (17) | 0.0228 (3) | |
H1B | 0.2000 | 0.6546 | 0.7672 | 0.027* | |
H1C | 0.3698 | 0.6150 | 0.8534 | 0.027* | |
N2 | 0.8142 (2) | 0.7948 (2) | 0.32085 (16) | 0.0239 (3) | |
N3 | 1.2634 (3) | 0.8913 (2) | 0.10419 (17) | 0.0256 (3) | |
H3D | 1.2650 | 0.9990 | 0.1430 | 0.031* | |
H3C | 1.3890 | 0.8211 | 0.0439 | 0.031* | |
H3B | 1.2494 | 0.8070 | 0.1705 | 0.031* | |
O1 | 0.9847 (2) | 0.7918 (2) | 0.33381 (14) | 0.0295 (3) | |
O2 | 0.7486 (2) | 0.8278 (2) | 0.21135 (15) | 0.0348 (3) | |
O3 | 0.90704 (19) | 0.64409 (19) | 0.80411 (13) | 0.0224 (3) | |
O4 | 0.6493 (2) | 0.5696 (2) | 0.90552 (13) | 0.0240 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ag1 | 0.02847 (12) | 0.02926 (12) | 0.02746 (13) | −0.00800 (9) | −0.00981 (9) | 0.00019 (9) |
Ag2 | 0.03202 (13) | 0.05231 (15) | 0.01693 (12) | −0.01760 (11) | −0.01052 (9) | 0.00982 (9) |
C1 | 0.0258 (9) | 0.0168 (8) | 0.0207 (9) | −0.0064 (7) | −0.0112 (7) | −0.0001 (7) |
C2 | 0.0177 (8) | 0.0205 (8) | 0.0296 (10) | −0.0085 (7) | −0.0108 (7) | −0.0009 (7) |
C3 | 0.0149 (7) | 0.0134 (7) | 0.0225 (9) | −0.0064 (6) | −0.0021 (6) | −0.0032 (6) |
C4 | 0.0136 (7) | 0.0132 (7) | 0.0178 (8) | −0.0060 (6) | −0.0023 (6) | −0.0013 (6) |
C5 | 0.0140 (7) | 0.0139 (7) | 0.0191 (8) | −0.0054 (6) | −0.0017 (6) | −0.0017 (6) |
C6 | 0.0215 (8) | 0.0151 (7) | 0.0182 (9) | −0.0069 (7) | −0.0006 (7) | −0.0006 (6) |
C7 | 0.0139 (7) | 0.0156 (7) | 0.0167 (8) | −0.0057 (6) | −0.0021 (6) | −0.0024 (6) |
N1 | 0.0167 (7) | 0.0326 (8) | 0.0243 (8) | −0.0160 (6) | −0.0029 (6) | 0.0002 (7) |
N2 | 0.0289 (8) | 0.0170 (7) | 0.0174 (8) | −0.0057 (6) | 0.0006 (6) | 0.0007 (6) |
N3 | 0.0284 (8) | 0.0288 (8) | 0.0209 (8) | −0.0145 (7) | −0.0047 (6) | 0.0023 (6) |
O1 | 0.0273 (7) | 0.0316 (7) | 0.0251 (7) | −0.0136 (6) | 0.0045 (5) | 0.0015 (6) |
O2 | 0.0441 (8) | 0.0330 (7) | 0.0177 (7) | −0.0112 (6) | −0.0041 (6) | 0.0046 (6) |
O3 | 0.0203 (6) | 0.0344 (7) | 0.0199 (6) | −0.0179 (5) | −0.0072 (5) | 0.0033 (5) |
O4 | 0.0221 (6) | 0.0355 (7) | 0.0166 (6) | −0.0159 (6) | −0.0027 (5) | 0.0059 (5) |
Geometric parameters (Å, º) top
Ag1—N3i | 2.1193 (16) | C4—C5 | 1.387 (2) |
Ag1—N3 | 2.1193 (16) | C4—C7 | 1.492 (2) |
Ag1—O2 | 3.1195 (15) | C5—C6 | 1.377 (3) |
Ag1—N1ii | 3.1885 (16) | C5—H5A | 0.9500 |
Ag2—O3 | 2.2367 (12) | C6—N2 | 1.437 (2) |
Ag2—O3iii | 2.2367 (12) | C7—O4 | 1.259 (2) |
Ag2—O4 | 2.6541 (13) | C7—O3 | 1.2716 (19) |
Ag2—O2iv | 2.9287 (15) | N1—H1B | 0.8800 |
C1—C2 | 1.362 (3) | N1—H1C | 0.8800 |
C1—C6 | 1.405 (3) | N2—O2 | 1.236 (2) |
C1—H1A | 0.9500 | N2—O1 | 1.237 (2) |
C2—C3 | 1.414 (3) | N3—H3D | 0.9100 |
C2—H2A | 0.9500 | N3—H3C | 0.9100 |
C3—N1 | 1.347 (2) | N3—H3B | 0.9100 |
C3—C4 | 1.429 (2) | | |
| | | |
N3i—Ag1—N3 | 180.0 | C6—C5—C4 | 121.08 (15) |
N3i—Ag1—O2 | 86.84 (5) | C6—C5—H5A | 119.5 |
N3—Ag1—O2 | 93.16 (5) | C4—C5—H5A | 119.5 |
N3i—Ag1—N1ii | 94.79 (5) | C5—C6—C1 | 120.84 (16) |
N3—Ag1—N1ii | 85.21 (5) | C5—C6—N2 | 119.51 (16) |
O2—Ag1—N1ii | 108.73 (4) | C1—C6—N2 | 119.63 (16) |
O3—Ag2—O3iii | 180.000 (1) | O4—C7—O3 | 122.16 (16) |
O3—Ag2—O4 | 53.02 (4) | O4—C7—C4 | 120.22 (14) |
O3iii—Ag2—O4 | 126.98 (4) | O3—C7—C4 | 117.62 (14) |
O3—Ag2—O2iv | 74.82 (4) | C3—N1—H1B | 120.0 |
O3iii—Ag2—O2iv | 105.18 (4) | C3—N1—H1C | 120.0 |
O4—Ag2—O2iv | 88.11 (4) | H1B—N1—H1C | 120.0 |
C2—C1—C6 | 118.92 (16) | O2—N2—O1 | 122.86 (16) |
C2—C1—H1A | 120.5 | O2—N2—C6 | 118.97 (16) |
C6—C1—H1A | 120.5 | O1—N2—C6 | 118.17 (16) |
C1—C2—C3 | 121.91 (16) | Ag1—N3—H3D | 109.5 |
C1—C2—H2A | 119.0 | Ag1—N3—H3C | 109.5 |
C3—C2—H2A | 119.0 | H3D—N3—H3C | 109.5 |
N1—C3—C2 | 119.65 (16) | Ag1—N3—H3B | 109.5 |
N1—C3—C4 | 122.09 (16) | H3D—N3—H3B | 109.5 |
C2—C3—C4 | 118.26 (15) | H3C—N3—H3B | 109.5 |
C5—C4—C3 | 118.92 (15) | C7—O3—Ag2 | 101.61 (10) |
C5—C4—C7 | 118.39 (14) | C7—O4—Ag2 | 82.57 (10) |
C3—C4—C7 | 122.67 (14) | | |
Symmetry codes: (i) −x+2, −y+2, −z; (ii) x+1, y, z−1; (iii) −x+2, −y+1, −z+2; (iv) −x+2, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1B···O3v | 0.88 | 2.09 | 2.9473 (18) | 164 |
N1—H1C···O4 | 0.88 | 2.03 | 2.685 (2) | 131 |
N3—H3D···O3vi | 0.91 | 2.37 | 3.185 (2) | 149 |
N3—H3C···O4ii | 0.91 | 2.21 | 3.077 (2) | 159 |
N3—H3B···O1 | 0.91 | 2.29 | 3.038 (2) | 139 |
Symmetry codes: (ii) x+1, y, z−1; (v) x−1, y, z; (vi) −x+2, −y+2, −z+1. |
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