Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803024966/br6123sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803024966/br6123Isup2.hkl |
CCDC reference: 227743
Key indicators
- Single-crystal X-ray study
- T = 180 K
- Mean (C-C) = 0.009 Å
- R factor = 0.029
- wR factor = 0.070
- Data-to-parameter ratio = 23.7
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.97
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.222 0.453 Tmin and Tmax expected: 0.163 0.453 RR = 1.360 Please check that your absorption correction is appropriate. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.36 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.69 Ratio PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C11 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C21 PLAT331_ALERT_2_C Small Av. Phenyl C-C Dist. C11 - C12_f = 1.36 Ang. PLAT331_ALERT_2_C Small Av. Phenyl C-C Dist. C21 - C26 = 1.36 Ang. PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT420_ALERT_2_C D-H Without Acceptor N1 - *H1A ... ? PLAT420_ALERT_2_C D-H Without Acceptor N1 - *H1B ... ? PLAT420_ALERT_2_C D-H Without Acceptor N1 - *H1C ... ? PLAT420_ALERT_2_C D-H Without Acceptor N2 - *H2A ... ? PLAT420_ALERT_2_C D-H Without Acceptor N2 - *H2B ... ? PLAT420_ALERT_2_C D-H Without Acceptor N2 - *H2C ... ? PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) . 1.21 Ratio
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 28.58 From the CIF: _reflns_number_total 2564 From the CIF: _diffrn_reflns_limit_ max hkl 17. 23. 21. From the CIF: _diffrn_reflns_limit_ min hkl -17. -18. -17. TEST1: Expected hkl limits for theta max Calculated maximum hkl 17. 25. 22. Calculated minimum hkl -17. -25. -22.
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 11 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1994); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1997); software used to prepare material for publication: SHELXTL.
(C6H8N)[AgI2] | F(000) = 3264 |
Mr = 455.80 | Dx = 2.949 Mg m−3 |
Orthorhombic, Cmca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2bc 2 | Cell parameters from 7996 reflections |
a = 13.3019 (10) Å | θ = 3–20° |
b = 18.6809 (15) Å | µ = 7.92 mm−1 |
c = 16.5245 (15) Å | T = 180 K |
V = 4106.2 (6) Å3 | Laths, light yellow |
Z = 16 | 0.54 × 0.20 × 0.10 mm |
Siemens SMART diffractometer | 2564 independent reflections |
Radiation source: fine-focus sealed tube | 2172 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
Detector resolution: 8.192 pixels mm-1 | θmax = 28.6°, θmin = 2.2° |
ω scans | h = −17→17 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −18→23 |
Tmin = 0.222, Tmax = 0.453 | l = −17→21 |
12054 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)] = 0.029 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.070 | w = 1/[σ2(Fo2) + (0.038P)2 + 11.3P] where P = (Fo2 + 2Fc2)/3 |
S = 0.98 | (Δ/σ)max = 0.008 |
2564 reflections | Δρmax = 0.94 e Å−3 |
108 parameters | Δρmin = −0.88 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.000123 (14) |
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 | 0.36172 (4) | 0.0000 | 0.0000 | 0.03405 (14) | |
Ag2 | 0.12269 (4) | 0.0000 | 0.0000 | 0.03398 (14) | |
I1 | 0.5000 | 0.06985 (2) | 0.10824 (3) | 0.02963 (12) | |
I2 | 0.0000 | 0.05097 (2) | 0.12836 (3) | 0.02795 (12) | |
I3 | 0.24213 (2) | 0.116424 (16) | −0.059278 (19) | 0.03059 (10) | |
N1 | 0.7500 | 0.0143 (4) | 0.2500 | 0.0537 (19) | |
H1A | 0.7757 | −0.0020 | 0.2976 | 0.081* | 0.50 |
H1B | 0.7884 | −0.0020 | 0.2083 | 0.081* | 0.50 |
H1C | 0.6859 | −0.0020 | 0.2441 | 0.081* | 0.50 |
C11 | 0.7500 | 0.0934 (3) | 0.2500 | 0.0159 (10) | |
C12 | 0.7512 (3) | 0.1294 (3) | 0.3208 (3) | 0.0304 (10) | |
H12A | 0.7519 | 0.1035 | 0.3703 | 0.037* | |
C13 | 0.7514 (3) | 0.2028 (3) | 0.3223 (4) | 0.0394 (12) | |
H13A | 0.7525 | 0.2278 | 0.3723 | 0.047* | |
C14 | 0.7500 | 0.2397 (3) | 0.2500 | 0.0431 (19) | |
H14A | 0.7500 | 0.2906 | 0.2500 | 0.052* | |
N2 | 0.0000 | 0.2582 (3) | 0.0606 | 0.069 (2) | |
H2A | −0.0645 | 0.2533 | 0.0430 | 0.104* | 0.50 |
H2B | 0.0305 | 0.2146 | 0.0611 | 0.104* | 0.50 |
H2C | 0.0340 | 0.2880 | 0.0267 | 0.104* | 0.50 |
C21 | 0.0000 | 0.2885 (3) | 0.1433 (3) | 0.0199 (11) | |
C22 | 0.0000 | 0.2451 (3) | 0.2075 (5) | 0.0369 (15) | |
H22A | 0.0000 | 0.1947 | 0.1999 | 0.044* | |
C23 | 0.0000 | 0.2730 (4) | 0.2852 (5) | 0.0393 (16) | |
H23A | 0.0000 | 0.2422 | 0.3309 | 0.047* | |
C24 | 0.0000 | 0.3470 (4) | 0.2949 (5) | 0.0388 (16) | |
H24A | 0.0000 | 0.3677 | 0.3475 | 0.047* | |
C25 | 0.0000 | 0.3897 (4) | 0.2272 (5) | 0.0418 (17) | |
H25A | 0.0000 | 0.4403 | 0.2329 | 0.050* | |
C26 | 0.0000 | 0.3599 (4) | 0.1515 (5) | 0.0366 (15) | |
H26A | 0.0000 | 0.3897 | 0.1049 | 0.044* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0403 (3) | 0.0302 (3) | 0.0317 (3) | 0.000 | 0.000 | −0.00030 (18) |
Ag2 | 0.0399 (3) | 0.0339 (3) | 0.0281 (3) | 0.000 | 0.000 | −0.00258 (18) |
I1 | 0.0315 (2) | 0.0296 (2) | 0.0277 (2) | 0.000 | 0.000 | −0.00363 (16) |
I2 | 0.0309 (2) | 0.0269 (2) | 0.0260 (2) | 0.000 | 0.000 | −0.00406 (15) |
I3 | 0.03666 (18) | 0.02651 (17) | 0.02860 (18) | −0.00148 (11) | −0.00169 (11) | 0.00564 (11) |
N1 | 0.067 (5) | 0.045 (4) | 0.049 (5) | 0.000 | 0.006 (3) | 0.000 |
C11 | 0.014 (2) | 0.020 (3) | 0.014 (3) | 0.000 | 0.0018 (18) | 0.000 |
C12 | 0.027 (2) | 0.042 (3) | 0.022 (2) | 0.0009 (18) | −0.0009 (17) | −0.0021 (19) |
C13 | 0.039 (3) | 0.038 (3) | 0.041 (3) | 0.002 (2) | 0.001 (2) | −0.014 (2) |
C14 | 0.037 (4) | 0.025 (4) | 0.067 (6) | 0.000 | 0.002 (3) | 0.000 |
N2 | 0.073 (5) | 0.058 (5) | 0.076 (6) | 0.000 | 0.000 | 0.001 (4) |
C21 | 0.018 (3) | 0.016 (2) | 0.026 (3) | 0.000 | 0.000 | 0.001 (2) |
C22 | 0.035 (3) | 0.023 (3) | 0.052 (5) | 0.000 | 0.000 | −0.001 (3) |
C23 | 0.044 (4) | 0.035 (4) | 0.039 (4) | 0.000 | 0.000 | 0.001 (3) |
C24 | 0.031 (3) | 0.040 (4) | 0.046 (4) | 0.000 | 0.000 | −0.008 (3) |
C25 | 0.041 (4) | 0.026 (3) | 0.059 (5) | 0.000 | 0.000 | −0.002 (3) |
C26 | 0.034 (3) | 0.029 (3) | 0.047 (4) | 0.000 | 0.000 | 0.007 (3) |
Ag1—I3i | 2.8670 (4) | C13—H13A | 0.9500 |
Ag1—I3 | 2.8670 (4) | C14—C13iv | 1.380 (7) |
Ag1—I1 | 2.8785 (5) | C14—H14A | 0.9500 |
Ag1—I1ii | 2.8785 (5) | N2—C21 | 1.479 (6) |
Ag2—I2iii | 2.8405 (5) | N2—H2A | 0.9100 |
Ag2—I2 | 2.8405 (5) | N2—H2B | 0.9100 |
Ag2—I3 | 2.8661 (4) | N2—H2C | 0.9100 |
Ag2—I3i | 2.8661 (4) | C21—C22 | 1.335 (9) |
I1—Ag1ii | 2.8785 (5) | C21—C26 | 1.341 (8) |
I2—Ag2iii | 2.8405 (5) | C22—C23 | 1.384 (11) |
N1—C11 | 1.479 (9) | C22—H22A | 0.9500 |
N1—H1A | 0.9100 | C23—C24 | 1.392 (10) |
N1—H1B | 0.9100 | C23—H23A | 0.9500 |
N1—H1C | 0.9100 | C24—C25 | 1.374 (11) |
C11—C12 | 1.349 (6) | C24—H24A | 0.9500 |
C11—C12iv | 1.349 (6) | C25—C26 | 1.369 (11) |
C12—C13 | 1.372 (7) | C25—H25A | 0.9500 |
C12—H12A | 0.9500 | C26—H26A | 0.9500 |
C13—C14 | 1.380 (7) | ||
I3i—Ag1—I3 | 112.60 (2) | C14—C13—H13A | 120.5 |
I3i—Ag1—I1 | 119.087 (12) | C13iv—C14—C13 | 120.0 (6) |
I3—Ag1—I1 | 102.882 (11) | C13iv—C14—H14A | 120.0 |
I3i—Ag1—I1ii | 102.882 (11) | C13—C14—H14A | 120.0 |
I3—Ag1—I1ii | 119.087 (12) | C21—N2—H2A | 109.5 |
I1—Ag1—I1ii | 100.56 (2) | C21—N2—H2B | 109.5 |
I2iii—Ag2—I2 | 109.87 (2) | H2A—N2—H2B | 109.5 |
I2iii—Ag2—I3 | 108.523 (11) | C21—N2—H2C | 109.5 |
I2—Ag2—I3 | 108.622 (11) | H2A—N2—H2C | 109.5 |
I2iii—Ag2—I3i | 108.622 (11) | H2B—N2—H2C | 109.5 |
I2—Ag2—I3i | 108.523 (11) | C22—C21—C26 | 121.5 (6) |
I3—Ag2—I3i | 112.66 (2) | C22—C21—N2 | 120.2 (5) |
Ag1—I1—Ag1ii | 79.44 (2) | C26—C21—N2 | 118.3 (5) |
Ag2iii—I2—Ag2 | 70.13 (2) | C21—C22—C23 | 120.6 (6) |
Ag2—I3—Ag1 | 67.366 (15) | C21—C22—H22A | 119.7 |
C11—N1—H1A | 109.5 | C23—C22—H22A | 119.7 |
C11—N1—H1B | 109.5 | C22—C23—C24 | 118.7 (7) |
H1A—N1—H1B | 109.5 | C22—C23—H23A | 120.6 |
C11—N1—H1C | 109.5 | C24—C23—H23A | 120.6 |
H1A—N1—H1C | 109.5 | C25—C24—C23 | 118.8 (7) |
H1B—N1—H1C | 109.5 | C25—C24—H24A | 120.6 |
C12—C11—C12iv | 120.4 (6) | C23—C24—H24A | 120.6 |
C12—C11—N1 | 119.8 (3) | C26—C25—C24 | 120.6 (7) |
C12iv—C11—N1 | 119.8 (3) | C26—C25—H25A | 119.7 |
C11—C12—C13 | 120.8 (5) | C24—C25—H25A | 119.7 |
C11—C12—H12A | 119.6 | C21—C26—C25 | 119.8 (6) |
C13—C12—H12A | 119.6 | C21—C26—H26A | 120.1 |
C12—C13—C14 | 119.0 (5) | C25—C26—H26A | 120.1 |
C12—C13—H13A | 120.5 |
Symmetry codes: (i) x, −y, −z; (ii) −x+1, −y, −z; (iii) −x, −y, −z; (iv) −x+3/2, y, −z+1/2. |