Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804025139/bt6539sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804025139/bt6539Isup2.hkl |
CCDC reference: 255417
Key indicators
- Single-crystal X-ray study
- T = 170 K
- Mean (C-C) = 0.006 Å
- R factor = 0.032
- wR factor = 0.078
- Data-to-parameter ratio = 21.2
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.94
Alert level C REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 27.98 From the CIF: _diffrn_reflns_theta_full 0.00 From the CIF: _reflns_number_total 3523 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 3737 Completeness (_total/calc) 94.27% PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 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 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS Program Package (Stoe & Cie, 1998); cell refinement: IPDS Program Package; data reduction: IPDS Program Package; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXTL.
[AgBr(C6H7N)] | F(000) = 1056 |
Mr = 280.91 | Dx = 2.400 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 7718 reflections |
a = 8.8523 (6) Å | θ = 2.5–28° |
b = 17.8849 (10) Å | µ = 7.64 mm−1 |
c = 9.9601 (7) Å | T = 170 K |
β = 99.550 (8)° | Block, colourless |
V = 1555.05 (17) Å3 | 0.11 × 0.09 × 0.09 mm |
Z = 8 |
Stoe IPDS diffractometer | 3523 independent reflections |
Radiation source: fine-focus sealed tube | 2208 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
φ scans | θmax = 28.0°, θmin = 2.6° |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998) | h = −11→11 |
Tmin = 0.444, Tmax = 0.502 | k = −23→23 |
13360 measured reflections | l = −13→13 |
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)] = 0.032 | H-atom parameters constrained |
wR(F2) = 0.078 | w = 1/[σ2(Fo2) + (0.0395P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.93 | (Δ/σ)max = 0.001 |
3523 reflections | Δρmax = 0.61 e Å−3 |
166 parameters | Δρmin = −0.69 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: 0.00093 (17) |
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 | 0.85489 (5) | 0.48457 (2) | 0.39523 (4) | 0.03276 (13) | |
Ag2 | 0.64810 (5) | 0.51009 (2) | 0.61457 (4) | 0.03233 (12) | |
Br1 | 0.59663 (6) | 0.40156 (3) | 0.40068 (5) | 0.02656 (13) | |
Br2 | 0.89576 (6) | 0.59790 (3) | 0.59770 (5) | 0.02666 (13) | |
N1 | 0.7784 (5) | 0.5661 (2) | 0.2175 (4) | 0.0238 (8) | |
C1 | 0.6405 (6) | 0.5578 (2) | 0.1390 (5) | 0.0256 (9) | |
H1 | 0.5816 | 0.5147 | 0.1512 | 0.031* | |
C2 | 0.5806 (6) | 0.6099 (2) | 0.0403 (4) | 0.0247 (9) | |
H2 | 0.4836 | 0.6015 | −0.0145 | 0.030* | |
C3 | 0.6626 (6) | 0.6741 (3) | 0.0224 (4) | 0.0247 (10) | |
C4 | 0.8053 (6) | 0.6830 (3) | 0.1042 (5) | 0.0285 (10) | |
H4 | 0.8654 | 0.7261 | 0.0954 | 0.034* | |
C5 | 0.8590 (6) | 0.6273 (3) | 0.1998 (5) | 0.0268 (10) | |
H5 | 0.9570 | 0.6335 | 0.2542 | 0.032* | |
C6 | 0.5975 (7) | 0.7327 (3) | −0.0802 (5) | 0.0391 (14) | |
H6A | 0.4984 | 0.7498 | −0.0602 | 0.059* | |
H6B | 0.5834 | 0.7112 | −0.1719 | 0.059* | |
H6C | 0.6682 | 0.7751 | −0.0751 | 0.059* | |
N11 | 0.7301 (5) | 0.4303 (2) | 0.7932 (4) | 0.0224 (8) | |
C11 | 0.7008 (6) | 0.3573 (2) | 0.7799 (4) | 0.0241 (10) | |
H11 | 0.6448 | 0.3399 | 0.6961 | 0.029* | |
C12 | 0.7476 (6) | 0.3053 (2) | 0.8821 (4) | 0.0250 (10) | |
H12 | 0.7255 | 0.2538 | 0.8662 | 0.030* | |
C13 | 0.8269 (6) | 0.3284 (3) | 1.0075 (5) | 0.0257 (10) | |
C14 | 0.8568 (6) | 0.4045 (2) | 1.0217 (4) | 0.0240 (9) | |
H14 | 0.9107 | 0.4233 | 1.1053 | 0.029* | |
C15 | 0.8087 (5) | 0.4531 (2) | 0.9148 (4) | 0.0215 (9) | |
H15 | 0.8318 | 0.5047 | 0.9273 | 0.026* | |
C16 | 0.8773 (7) | 0.2746 (3) | 1.1210 (5) | 0.0389 (13) | |
H16A | 0.8436 | 0.2241 | 1.0921 | 0.058* | |
H16B | 0.8321 | 0.2890 | 1.2006 | 0.058* | |
H16C | 0.9892 | 0.2756 | 1.1446 | 0.058* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0301 (3) | 0.0326 (2) | 0.0324 (2) | 0.00621 (17) | −0.00425 (17) | 0.00059 (15) |
Ag2 | 0.0326 (3) | 0.0283 (2) | 0.0347 (2) | 0.00393 (17) | 0.00147 (17) | 0.00641 (14) |
Br1 | 0.0248 (3) | 0.0218 (2) | 0.0311 (2) | 0.00221 (17) | −0.0012 (2) | −0.00182 (17) |
Br2 | 0.0222 (3) | 0.0217 (2) | 0.0343 (3) | 0.00100 (17) | −0.0004 (2) | −0.00518 (17) |
N1 | 0.021 (2) | 0.0229 (19) | 0.0256 (19) | 0.0008 (16) | −0.0004 (16) | −0.0018 (14) |
C1 | 0.021 (3) | 0.025 (2) | 0.030 (2) | 0.0006 (18) | 0.0001 (19) | −0.0004 (17) |
C2 | 0.023 (3) | 0.024 (2) | 0.026 (2) | 0.0026 (17) | −0.0005 (18) | −0.0034 (16) |
C3 | 0.025 (3) | 0.027 (2) | 0.023 (2) | 0.0029 (18) | 0.0074 (18) | 0.0019 (16) |
C4 | 0.023 (3) | 0.028 (2) | 0.035 (2) | −0.0063 (19) | 0.006 (2) | −0.0014 (18) |
C5 | 0.018 (3) | 0.032 (2) | 0.028 (2) | −0.0022 (19) | −0.0013 (19) | −0.0048 (18) |
C6 | 0.045 (4) | 0.031 (3) | 0.040 (3) | −0.003 (2) | 0.004 (3) | 0.014 (2) |
N11 | 0.023 (2) | 0.0226 (18) | 0.0218 (17) | 0.0011 (16) | 0.0046 (16) | 0.0029 (14) |
C11 | 0.028 (3) | 0.021 (2) | 0.022 (2) | −0.0027 (18) | 0.0011 (18) | −0.0033 (15) |
C12 | 0.027 (3) | 0.018 (2) | 0.029 (2) | 0.0001 (17) | 0.0030 (19) | 0.0035 (16) |
C13 | 0.020 (3) | 0.029 (2) | 0.028 (2) | 0.0022 (19) | 0.0029 (19) | 0.0042 (17) |
C14 | 0.023 (3) | 0.026 (2) | 0.0221 (19) | −0.0037 (17) | 0.0026 (18) | −0.0019 (16) |
C15 | 0.020 (3) | 0.0203 (19) | 0.0239 (19) | −0.0028 (15) | 0.0012 (17) | −0.0058 (15) |
C16 | 0.043 (4) | 0.037 (3) | 0.032 (3) | 0.000 (2) | −0.008 (2) | 0.011 (2) |
Ag1—N1 | 2.307 (4) | C4—C5 | 1.405 (7) |
Ag1—Br2i | 2.6460 (7) | C4—H4 | 0.9500 |
Ag1—Br1 | 2.7340 (7) | C5—H5 | 0.9500 |
Ag1—Br2 | 2.8397 (6) | C6—H6A | 0.9800 |
Ag1—Ag1i | 3.0792 (8) | C6—H6B | 0.9800 |
Ag1—Ag2 | 3.1078 (6) | C6—H6C | 0.9800 |
Ag2—N11 | 2.302 (4) | N11—C11 | 1.332 (6) |
Ag2—Br1ii | 2.6654 (7) | N11—C15 | 1.356 (6) |
Ag2—Br2 | 2.7245 (7) | C11—C12 | 1.391 (6) |
Ag2—Br1 | 2.8620 (6) | C11—H11 | 0.9500 |
Ag2—Ag2ii | 3.1982 (9) | C12—C13 | 1.390 (6) |
Br1—Ag2ii | 2.6654 (7) | C12—H12 | 0.9500 |
Br2—Ag1i | 2.6460 (7) | C13—C14 | 1.389 (6) |
N1—C5 | 1.334 (6) | C13—C16 | 1.495 (7) |
N1—C1 | 1.344 (6) | C14—C15 | 1.385 (6) |
C1—C2 | 1.395 (6) | C14—H14 | 0.9500 |
C1—H1 | 0.9500 | C15—H15 | 0.9500 |
C2—C3 | 1.386 (7) | C16—H16A | 0.9800 |
C2—H2 | 0.9500 | C16—H16B | 0.9800 |
C3—C4 | 1.394 (7) | C16—H16C | 0.9800 |
C3—C6 | 1.509 (7) | ||
N1—Ag1—Br2i | 120.68 (10) | C3—C2—C1 | 119.9 (5) |
N1—Ag1—Br1 | 102.63 (11) | C3—C2—H2 | 120.0 |
Br2i—Ag1—Br1 | 113.166 (18) | C1—C2—H2 | 120.0 |
N1—Ag1—Br2 | 94.61 (9) | C2—C3—C4 | 117.5 (4) |
Br2i—Ag1—Br2 | 111.811 (19) | C2—C3—C6 | 120.9 (5) |
Br1—Ag1—Br2 | 112.45 (2) | C4—C3—C6 | 121.6 (5) |
N1—Ag1—Ag1i | 120.83 (10) | C3—C4—C5 | 119.2 (4) |
Br2i—Ag1—Ag1i | 58.891 (18) | C3—C4—H4 | 120.4 |
Br1—Ag1—Ag1i | 133.65 (2) | C5—C4—H4 | 120.4 |
Br2—Ag1—Ag1i | 52.920 (16) | N1—C5—C4 | 122.8 (5) |
N1—Ag1—Ag2 | 108.33 (10) | N1—C5—H5 | 118.6 |
Br2i—Ag1—Ag2 | 130.481 (17) | C4—C5—H5 | 118.6 |
Br1—Ag1—Ag2 | 58.250 (15) | C3—C6—H6A | 109.5 |
Br2—Ag1—Ag2 | 54.302 (15) | C3—C6—H6B | 109.5 |
Ag1i—Ag1—Ag2 | 91.131 (18) | H6A—C6—H6B | 109.5 |
N11—Ag2—Br1ii | 124.10 (10) | C3—C6—H6C | 109.5 |
N11—Ag2—Br2 | 104.56 (10) | H6A—C6—H6C | 109.5 |
Br1ii—Ag2—Br2 | 108.030 (18) | H6B—C6—H6C | 109.5 |
N11—Ag2—Br1 | 98.36 (9) | C11—N11—C15 | 116.5 (4) |
Br1ii—Ag2—Br1 | 109.397 (19) | C11—N11—Ag2 | 120.0 (3) |
Br2—Ag2—Br1 | 112.05 (2) | C15—N11—Ag2 | 123.6 (3) |
N11—Ag2—Ag1 | 107.76 (10) | N11—C11—C12 | 123.6 (4) |
Br1ii—Ag2—Ag1 | 127.949 (17) | N11—C11—H11 | 118.2 |
Br2—Ag2—Ag1 | 57.825 (14) | C12—C11—H11 | 118.2 |
Br1—Ag2—Ag1 | 54.323 (15) | C13—C12—C11 | 120.2 (4) |
N11—Ag2—Ag2ii | 126.68 (10) | C13—C12—H12 | 119.9 |
Br1ii—Ag2—Ag2ii | 57.575 (17) | C11—C12—H12 | 119.9 |
Br2—Ag2—Ag2ii | 126.43 (2) | C14—C13—C12 | 116.3 (4) |
Br1—Ag2—Ag2ii | 51.822 (16) | C14—C13—C16 | 121.7 (5) |
Ag1—Ag2—Ag2ii | 89.461 (18) | C12—C13—C16 | 122.0 (4) |
Ag2ii—Br1—Ag1 | 110.57 (2) | C15—C14—C13 | 120.4 (4) |
Ag2ii—Br1—Ag2 | 70.603 (19) | C15—C14—H14 | 119.8 |
Ag1—Br1—Ag2 | 67.427 (16) | C13—C14—H14 | 119.8 |
Ag1i—Br2—Ag2 | 110.69 (2) | N11—C15—C14 | 123.0 (4) |
Ag1i—Br2—Ag1 | 68.189 (19) | N11—C15—H15 | 118.5 |
Ag2—Br2—Ag1 | 67.873 (17) | C14—C15—H15 | 118.5 |
C5—N1—C1 | 118.0 (4) | C13—C16—H16A | 109.5 |
C5—N1—Ag1 | 121.6 (3) | C13—C16—H16B | 109.5 |
C1—N1—Ag1 | 119.9 (3) | H16A—C16—H16B | 109.5 |
N1—C1—C2 | 122.5 (4) | C13—C16—H16C | 109.5 |
N1—C1—H1 | 118.7 | H16A—C16—H16C | 109.5 |
C2—C1—H1 | 118.7 | H16B—C16—H16C | 109.5 |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, −y+1, −z+1. |