



Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807063490/bq2042sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536807063490/bq2042Isup2.hkl |
CCDC reference: 677453
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean
(C-C) = 0.006 Å
- R factor = 0.041
- wR factor = 0.066
- Data-to-parameter ratio = 17.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.29 Ratio
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
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 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
AgNO3 (85 mg, 0.5 mmol) and pyrazole (34 mg, 0.5 mmol) were dissolved in ammonium hydroxide (20%, 10 ml). The solution was filtered and filtrate was allowed to stand for 15 days. Colorless crystals of (I) were collected, in about 50% yield.
H atoms were included in calculated positions and treated in the subsequent refinement as riding atoms, with C—H = 0.93 Å and Uiso(H) = 1.2 Ueq(C,N).
Data collection: SMART (Bruker, 1998); cell refinement: SMART (Bruker, 1998); data reduction: SHELXTL (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL (Bruker, 1998).
[Ag(C3H3N2)] | F(000) = 656 |
Mr = 174.94 | Dx = 2.797 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 6390 reflections |
a = 6.4084 (13) Å | θ = 3.1–27.7° |
b = 6.4989 (13) Å | µ = 4.66 mm−1 |
c = 19.948 (4) Å | T = 293 K |
V = 830.8 (3) Å3 | Block, colorless |
Z = 8 | 0.40 × 0.20 × 0.20 mm |
Bruker Smart CCD area-detector diffractometer | 951 independent reflections |
Radiation source: fine-focus sealed tube | 778 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
ϕ and ω scan | θmax = 27.5°, θmin = 3.8° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −8→7 |
Tmin = 0.340, Tmax = 0.400 | k = −8→8 |
7019 measured reflections | l = −25→25 |
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)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.066 | H-atom parameters constrained |
S = 1.26 | w = 1/[σ2(Fo2) + (0.0145P)2 + 0.695P] where P = (Fo2 + 2Fc2)/3 |
951 reflections | (Δ/σ)max = 0.004 |
55 parameters | Δρmax = 0.38 e Å−3 |
0 restraints | Δρmin = −0.55 e Å−3 |
[Ag(C3H3N2)] | V = 830.8 (3) Å3 |
Mr = 174.94 | Z = 8 |
Orthorhombic, Pbca | Mo Kα radiation |
a = 6.4084 (13) Å | µ = 4.66 mm−1 |
b = 6.4989 (13) Å | T = 293 K |
c = 19.948 (4) Å | 0.40 × 0.20 × 0.20 mm |
Bruker Smart CCD area-detector diffractometer | 951 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | 778 reflections with I > 2σ(I) |
Tmin = 0.340, Tmax = 0.400 | Rint = 0.044 |
7019 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 0 restraints |
wR(F2) = 0.066 | H-atom parameters constrained |
S = 1.26 | Δρmax = 0.38 e Å−3 |
951 reflections | Δρmin = −0.55 e Å−3 |
55 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 | 0.23552 (5) | 0.32951 (6) | 1.004623 (15) | 0.04206 (16) | |
N1 | 0.3965 (5) | 0.3598 (6) | 0.91516 (17) | 0.0345 (9) | |
N2 | 0.5800 (5) | 0.2552 (6) | 0.90915 (17) | 0.0364 (9) | |
C1 | 0.3418 (7) | 0.4213 (7) | 0.8548 (2) | 0.0403 (12) | |
H1A | 0.2217 | 0.4958 | 0.8450 | 0.048* | |
C2 | 0.4861 (7) | 0.3606 (7) | 0.8087 (2) | 0.0448 (12) | |
H2A | 0.4851 | 0.3836 | 0.7627 | 0.054* | |
C3 | 0.6325 (7) | 0.2581 (7) | 0.8457 (2) | 0.0425 (12) | |
H3A | 0.7528 | 0.1986 | 0.8282 | 0.051* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0444 (3) | 0.0411 (3) | 0.0407 (2) | −0.00048 (16) | 0.00707 (18) | −0.00123 (16) |
N1 | 0.038 (2) | 0.032 (2) | 0.033 (2) | 0.0036 (18) | 0.0039 (16) | −0.0005 (17) |
N2 | 0.037 (2) | 0.037 (2) | 0.036 (2) | 0.0002 (17) | 0.0017 (17) | −0.0002 (18) |
C1 | 0.048 (3) | 0.026 (3) | 0.047 (3) | 0.006 (2) | −0.009 (2) | 0.002 (2) |
C2 | 0.062 (3) | 0.040 (3) | 0.033 (3) | −0.010 (3) | 0.002 (2) | 0.003 (2) |
C3 | 0.044 (3) | 0.036 (3) | 0.048 (3) | −0.001 (2) | 0.011 (2) | −0.006 (2) |
Ag1—N1 | 2.070 (3) | N2—C3 | 1.310 (5) |
Ag1—N2i | 2.063 (4) | C1—C2 | 1.362 (6) |
Ag1—Ag1ii | 3.2547 (6) | C1—H1A | 0.9300 |
Ag1—Ag1i | 3.3718 (7) | C2—C3 | 1.367 (6) |
N1—C1 | 1.316 (5) | C2—H2A | 0.9300 |
N1—N2 | 1.364 (5) | C3—H3A | 0.9300 |
N2i—Ag1—N1 | 169.98 (14) | C1—N1—N2 | 107.5 (3) |
N2i—Ag1—Ag1ii | 76.18 (10) | C1—N1—Ag1 | 133.2 (3) |
N1—Ag1—Ag1ii | 93.82 (10) | N2—N1—Ag1 | 117.3 (3) |
N2i—Ag1—Ag1iii | 107.09 (10) | C3—N2—N1 | 107.4 (3) |
N1—Ag1—Ag1iii | 82.91 (10) | C3—N2—Ag1iv | 133.3 (3) |
Ag1ii—Ag1—Ag1iii | 173.46 (2) | N1—N2—Ag1iv | 118.5 (2) |
N2i—Ag1—Ag1i | 60.31 (10) | N1—C1—C2 | 110.4 (4) |
N1—Ag1—Ag1i | 117.09 (10) | N1—C1—H1A | 124.8 |
Ag1ii—Ag1—Ag1i | 75.415 (18) | C2—C1—H1A | 124.8 |
Ag1iii—Ag1—Ag1i | 111.111 (17) | C1—C2—C3 | 104.1 (4) |
N2i—Ag1—Ag1iv | 115.02 (10) | C1—C2—H2A | 128.0 |
N1—Ag1—Ag1iv | 60.57 (10) | C3—C2—H2A | 128.0 |
Ag1ii—Ag1—Ag1iv | 68.889 (17) | N2—C3—C2 | 110.6 (4) |
Ag1iii—Ag1—Ag1iv | 104.585 (18) | N2—C3—H3A | 124.7 |
Ag1i—Ag1—Ag1iv | 143.72 (3) | C2—C3—H3A | 124.7 |
N2i—Ag1—N1—C1 | 108.9 (8) | C1—N1—N2—C3 | 0.7 (5) |
Ag1ii—Ag1—N1—C1 | 112.0 (4) | Ag1—N1—N2—C3 | 166.6 (3) |
Ag1iii—Ag1—N1—C1 | −73.6 (4) | C1—N1—N2—Ag1iv | 171.5 (3) |
Ag1i—Ag1—N1—C1 | 36.5 (5) | Ag1—N1—N2—Ag1iv | −22.6 (4) |
Ag1iv—Ag1—N1—C1 | 175.2 (5) | N2—N1—C1—C2 | −0.3 (5) |
N2i—Ag1—N1—N2 | −52.6 (9) | Ag1—N1—C1—C2 | −163.1 (3) |
Ag1ii—Ag1—N1—N2 | −49.4 (3) | N1—C1—C2—C3 | −0.1 (6) |
Ag1iii—Ag1—N1—N2 | 124.9 (3) | N1—N2—C3—C2 | −0.8 (5) |
Ag1i—Ag1—N1—N2 | −124.9 (3) | Ag1iv—N2—C3—C2 | −169.6 (3) |
Ag1iv—Ag1—N1—N2 | 13.7 (2) | C1—C2—C3—N2 | 0.6 (6) |
Symmetry codes: (i) x−1/2, −y+1/2, −z+2; (ii) −x+1/2, y−1/2, z; (iii) −x+1/2, y+1/2, z; (iv) x+1/2, −y+1/2, −z+2. |
Experimental details
Crystal data | |
Chemical formula | [Ag(C3H3N2)] |
Mr | 174.94 |
Crystal system, space group | Orthorhombic, Pbca |
Temperature (K) | 293 |
a, b, c (Å) | 6.4084 (13), 6.4989 (13), 19.948 (4) |
V (Å3) | 830.8 (3) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 4.66 |
Crystal size (mm) | 0.40 × 0.20 × 0.20 |
Data collection | |
Diffractometer | Bruker Smart CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 1998) |
Tmin, Tmax | 0.340, 0.400 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7019, 951, 778 |
Rint | 0.044 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.066, 1.26 |
No. of reflections | 951 |
No. of parameters | 55 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.38, −0.55 |
Computer programs: SMART (Bruker, 1998), SHELXTL (Bruker, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997).
Ag1—N1 | 2.070 (3) | Ag1—Ag1ii | 3.2547 (6) |
Ag1—N2i | 2.063 (4) | Ag1—Ag1i | 3.3718 (7) |
N2i—Ag1—N1 | 169.98 (14) | Ag1ii—Ag1—Ag1i | 75.415 (18) |
N2i—Ag1—Ag1ii | 76.18 (10) | Ag1iii—Ag1—Ag1i | 111.111 (17) |
N1—Ag1—Ag1ii | 93.82 (10) | N2i—Ag1—Ag1iv | 115.02 (10) |
N2i—Ag1—Ag1iii | 107.09 (10) | N1—Ag1—Ag1iv | 60.57 (10) |
N1—Ag1—Ag1iii | 82.91 (10) | Ag1ii—Ag1—Ag1iv | 68.889 (17) |
Ag1ii—Ag1—Ag1iii | 173.46 (2) | Ag1iii—Ag1—Ag1iv | 104.585 (18) |
N2i—Ag1—Ag1i | 60.31 (10) | Ag1i—Ag1—Ag1iv | 143.72 (3) |
N1—Ag1—Ag1i | 117.09 (10) |
Symmetry codes: (i) x−1/2, −y+1/2, −z+2; (ii) −x+1/2, y−1/2, z; (iii) −x+1/2, y+1/2, z; (iv) x+1/2, −y+1/2, −z+2. |
The synthesis and structure of silver(I)-pyrazolate, i.e. the title compound, [Ag(C3H3N2)]n (I) has been reported by Masciocchi et al. (1994). In this work, the crystal structure was determined by the Ab-initio X-ray powder diffraction method and refined with the Rietveld technique in the space group of Pbca with a = 6.5295 (4), b = 20.059 (2) and c = 6.4675 (4) %A. The result is almost consistent with the structural determination by the single-crystal diffraction reported herein, with only minor structure parameter deviations.
Compound (I) has an infinite helical chain structure, in which each pyrazolate group bridges two Ag(I) atoms related by a 21 axis and each Ag(I) is linearly coordinated by two N atoms from distinct pyrazolate moieties with the N-Ag-N angle of 169.98 (14) °, being larger than reported 165.5 (1) °, (Figure 1). The bond distances and angles are listed in Table 1. The torsion angle of Ag(1)-N(1)-N(2)-Ag(1B) is 22.6 (4) ° and the dihedral angle between two pyrazoly rings around one Ag(I) center is 60.3 (2) °. Furthermore, such chains are linked by interchain Ag—Ag interactions to form a 2D layer (Figure 2). The intrachain and interaction Ag—Ag separations are 3.3718 (7) [Ag(1)-Ag(1A)] and 3.2547 (6) Å [Ag(1)-Ag(1B)], respectively, which are comparable well with those reported [3.40 (1) and 3.273 (1) Å, respectively].