Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806035008/ac2039sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806035008/ac2039Isup2.hkl |
CCDC reference: 623956
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.031
- wR factor = 0.070
- Data-to-parameter ratio = 15.3
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Ag1 - S1_a .. 11.09 su
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.71 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for Ag1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N3 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 19 N2 -AG1 -N1 -C5 -86.50 0.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 21 N2 -AG1 -N1 -C1 89.40 0.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 29 N1 -AG1 -N2 -C7 177.50 0.50 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 31 N1 -AG1 -N2 -C11 -4.10 0.70 1.555 1.555 1.555 1.555
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.706 Tmax scaled 0.706 Tmin scaled 0.595 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 1 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 3 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 1 ALERT type 3 Indicator that the structure quality may be low 6 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97; molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.
[Ag2(C11H10N2S)2](NO3)2 | F(000) = 736 |
Mr = 744.32 | Dx = 1.931 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 642 reflections |
a = 8.568 (3) Å | θ = 3.2–21.1° |
b = 14.919 (5) Å | µ = 1.74 mm−1 |
c = 10.510 (4) Å | T = 293 K |
β = 107.688 (5)° | Block, colorless |
V = 1280.0 (8) Å3 | 0.30 × 0.25 × 0.20 mm |
Z = 2 |
Bruker SMART 1000 CCD area-detector diffractometer | 2631 independent reflections |
Radiation source: fine-focus sealed tube | 1947 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
φ and ω scans | θmax = 26.5°, θmin = 2.5° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −9→10 |
Tmin = 0.843, Tmax = 1.000 | k = −15→18 |
7289 measured reflections | l = −13→13 |
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)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.070 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0309P)2 + 0.2899P] where P = (Fo2 + 2Fc2)/3 |
2631 reflections | (Δ/σ)max = 0.001 |
172 parameters | Δρmax = 0.44 e Å−3 |
0 restraints | Δρmin = −0.38 e Å−3 |
Experimental. IR (KBr, cm-1): 1580 (s), 1556 (w), 1457 (m), 1385 (s), 1357 (s), 1289 (s), 1124 (m), 1008 (m), 758 (m). |
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 | 0.36147 (4) | 0.114158 (18) | 0.55936 (3) | 0.05665 (12) | |
C1 | 0.0336 (4) | 0.0910 (2) | 0.6187 (4) | 0.0541 (9) | |
H1A | 0.0029 | 0.1312 | 0.5479 | 0.065* | |
C2 | −0.0806 (4) | 0.0658 (3) | 0.6781 (4) | 0.0651 (11) | |
H2A | −0.1865 | 0.0886 | 0.6483 | 0.078* | |
C3 | −0.0372 (5) | 0.0066 (3) | 0.7818 (4) | 0.0671 (11) | |
H3A | −0.1131 | −0.0113 | 0.8239 | 0.081* | |
C4 | 0.1206 (4) | −0.0262 (2) | 0.8236 (4) | 0.0507 (9) | |
H4A | 0.1522 | −0.0671 | 0.8935 | 0.061* | |
C5 | 0.2310 (4) | 0.00243 (19) | 0.7603 (3) | 0.0350 (7) | |
C6 | 0.4076 (4) | −0.02764 (19) | 0.8113 (3) | 0.0371 (7) | |
H6A | 0.4128 | −0.0797 | 0.8677 | 0.045* | |
H6B | 0.4703 | 0.0196 | 0.8674 | 0.045* | |
C7 | 0.5887 (3) | 0.15689 (19) | 0.3806 (3) | 0.0328 (6) | |
C8 | 0.6998 (4) | 0.2042 (2) | 0.3352 (3) | 0.0438 (8) | |
H8A | 0.7300 | 0.1840 | 0.2623 | 0.053* | |
C9 | 0.7646 (4) | 0.2818 (2) | 0.4006 (4) | 0.0496 (8) | |
H9A | 0.8398 | 0.3150 | 0.3723 | 0.060* | |
C10 | 0.7180 (4) | 0.3101 (2) | 0.5071 (4) | 0.0563 (9) | |
H10A | 0.7609 | 0.3625 | 0.5520 | 0.068* | |
C11 | 0.6077 (4) | 0.2604 (2) | 0.5468 (3) | 0.0537 (9) | |
H11A | 0.5764 | 0.2800 | 0.6194 | 0.064* | |
N1 | 0.1888 (3) | 0.06017 (16) | 0.6580 (2) | 0.0404 (6) | |
N2 | 0.5422 (3) | 0.18415 (16) | 0.4852 (2) | 0.0406 (6) | |
N3 | 0.6552 (3) | 0.2208 (2) | 0.9058 (3) | 0.0477 (7) | |
O1 | 0.7117 (4) | 0.21500 (19) | 1.0277 (3) | 0.0740 (8) | |
O2 | 0.6207 (4) | 0.15316 (19) | 0.8354 (3) | 0.0818 (9) | |
O3 | 0.6290 (4) | 0.29634 (17) | 0.8556 (2) | 0.0705 (8) | |
S1 | 0.49373 (10) | 0.05541 (5) | 0.31169 (8) | 0.0417 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0661 (2) | 0.05585 (18) | 0.06118 (19) | 0.00627 (14) | 0.03900 (15) | 0.01714 (14) |
C1 | 0.044 (2) | 0.055 (2) | 0.059 (2) | 0.0089 (16) | 0.0081 (17) | 0.0179 (18) |
C2 | 0.039 (2) | 0.065 (2) | 0.088 (3) | 0.0063 (18) | 0.015 (2) | 0.018 (2) |
C3 | 0.052 (2) | 0.070 (3) | 0.089 (3) | −0.0009 (19) | 0.035 (2) | 0.018 (2) |
C4 | 0.052 (2) | 0.0436 (19) | 0.061 (2) | 0.0024 (16) | 0.0241 (18) | 0.0156 (17) |
C5 | 0.0385 (17) | 0.0306 (15) | 0.0354 (15) | −0.0028 (12) | 0.0102 (13) | −0.0035 (13) |
C6 | 0.0449 (18) | 0.0340 (16) | 0.0305 (15) | −0.0006 (13) | 0.0084 (14) | −0.0017 (13) |
C7 | 0.0343 (16) | 0.0329 (15) | 0.0306 (15) | 0.0058 (13) | 0.0090 (13) | 0.0053 (13) |
C8 | 0.0482 (19) | 0.0412 (18) | 0.0467 (18) | −0.0002 (15) | 0.0212 (16) | 0.0043 (15) |
C9 | 0.0434 (19) | 0.0397 (18) | 0.067 (2) | −0.0030 (15) | 0.0192 (18) | 0.0064 (17) |
C10 | 0.060 (2) | 0.044 (2) | 0.061 (2) | −0.0124 (17) | 0.012 (2) | −0.0110 (18) |
C11 | 0.072 (2) | 0.049 (2) | 0.0416 (19) | 0.0042 (18) | 0.0195 (18) | −0.0050 (17) |
N1 | 0.0408 (15) | 0.0399 (14) | 0.0400 (14) | 0.0024 (12) | 0.0114 (12) | 0.0074 (12) |
N2 | 0.0474 (16) | 0.0397 (15) | 0.0374 (14) | 0.0036 (12) | 0.0170 (12) | 0.0047 (12) |
N3 | 0.0497 (17) | 0.0453 (17) | 0.0519 (18) | −0.0054 (13) | 0.0209 (14) | −0.0027 (15) |
O1 | 0.102 (2) | 0.0681 (17) | 0.0508 (16) | 0.0011 (15) | 0.0211 (15) | 0.0141 (14) |
O2 | 0.093 (2) | 0.0589 (17) | 0.098 (2) | −0.0230 (15) | 0.0365 (18) | −0.0345 (17) |
O3 | 0.103 (2) | 0.0529 (16) | 0.0505 (15) | 0.0034 (14) | 0.0153 (15) | 0.0054 (13) |
S1 | 0.0415 (4) | 0.0368 (4) | 0.0507 (5) | −0.0045 (3) | 0.0200 (4) | −0.0001 (4) |
Ag1—N1 | 2.201 (3) | C7—N2 | 1.342 (4) |
Ag1—S1i | 2.9588 (12) | C7—C8 | 1.381 (4) |
Ag1—N2 | 2.197 (3) | C7—S1 | 1.767 (3) |
C1—N1 | 1.348 (4) | C8—C9 | 1.375 (4) |
C1—C2 | 1.363 (5) | C8—H8A | 0.9300 |
C1—H1A | 0.9300 | C9—C10 | 1.365 (5) |
C2—C3 | 1.363 (5) | C9—H9A | 0.9300 |
C2—H2A | 0.9300 | C10—C11 | 1.363 (5) |
C3—C4 | 1.379 (5) | C10—H10A | 0.9300 |
C3—H3A | 0.9300 | C11—N2 | 1.344 (4) |
C4—C5 | 1.379 (4) | C11—H11A | 0.9300 |
C4—H4A | 0.9300 | N3—O1 | 1.227 (4) |
C5—N1 | 1.339 (4) | N3—O2 | 1.232 (3) |
C5—C6 | 1.512 (4) | N3—O3 | 1.236 (3) |
C6—S1i | 1.795 (3) | S1—C6i | 1.795 (3) |
C6—H6A | 0.9700 | S1—Ag1i | 2.9588 (12) |
C6—H6B | 0.9700 | ||
N1—Ag1—S1i | 73.71 (7) | C8—C7—S1 | 125.2 (2) |
N2—Ag1—N1 | 171.06 (9) | C9—C8—C7 | 118.3 (3) |
N2—Ag1—S1i | 109.04 (7) | C9—C8—H8A | 120.9 |
N1—C1—C2 | 123.0 (3) | C7—C8—H8A | 120.9 |
N1—C1—H1A | 118.5 | C10—C9—C8 | 119.8 (3) |
C2—C1—H1A | 118.5 | C10—C9—H9A | 120.1 |
C1—C2—C3 | 119.1 (3) | C8—C9—H9A | 120.1 |
C1—C2—H2A | 120.5 | C11—C10—C9 | 119.1 (3) |
C3—C2—H2A | 120.5 | C11—C10—H10A | 120.5 |
C2—C3—C4 | 119.2 (3) | C9—C10—H10A | 120.5 |
C2—C3—H3A | 120.4 | N2—C11—C10 | 122.7 (3) |
C4—C3—H3A | 120.4 | N2—C11—H11A | 118.6 |
C5—C4—C3 | 119.1 (3) | C10—C11—H11A | 118.6 |
C5—C4—H4A | 120.5 | C5—N1—C1 | 117.8 (3) |
C3—C4—H4A | 120.5 | C5—N1—Ag1 | 123.9 (2) |
N1—C5—C4 | 122.0 (3) | C1—N1—Ag1 | 118.2 (2) |
N1—C5—C6 | 118.2 (3) | C7—N2—C11 | 117.8 (3) |
C4—C5—C6 | 119.7 (3) | C7—N2—Ag1 | 124.3 (2) |
C5—C6—S1i | 116.9 (2) | C11—N2—Ag1 | 117.9 (2) |
C5—C6—H6A | 108.1 | O1—N3—O2 | 121.1 (3) |
S1i—C6—H6A | 108.1 | O1—N3—O3 | 118.2 (3) |
C5—C6—H6B | 108.1 | O2—N3—O3 | 120.7 (3) |
S1i—C6—H6B | 108.1 | C7—S1—C6i | 103.51 (14) |
H6A—C6—H6B | 107.3 | C7—S1—Ag1i | 117.92 (10) |
N2—C7—C8 | 122.4 (3) | C6i—S1—Ag1i | 84.77 (10) |
N2—C7—S1 | 112.4 (2) | ||
N1—C1—C2—C3 | −0.2 (6) | N2—Ag1—N1—C5 | −86.5 (6) |
C1—C2—C3—C4 | −0.1 (6) | S1i—Ag1—N1—C5 | 22.7 (2) |
C2—C3—C4—C5 | 0.7 (6) | N2—Ag1—N1—C1 | 89.4 (6) |
C3—C4—C5—N1 | −1.1 (5) | S1i—Ag1—N1—C1 | −161.4 (3) |
C3—C4—C5—C6 | 175.6 (3) | C8—C7—N2—C11 | −0.1 (4) |
N1—C5—C6—S1i | −43.2 (3) | S1—C7—N2—C11 | 179.4 (2) |
C4—C5—C6—S1i | 140.0 (3) | C8—C7—N2—Ag1 | 178.3 (2) |
N2—C7—C8—C9 | 0.2 (5) | S1—C7—N2—Ag1 | −2.2 (3) |
S1—C7—C8—C9 | −179.3 (2) | C10—C11—N2—C7 | 0.0 (5) |
C7—C8—C9—C10 | −0.2 (5) | C10—C11—N2—Ag1 | −178.5 (3) |
C8—C9—C10—C11 | 0.1 (5) | N1—Ag1—N2—C7 | 177.5 (5) |
C9—C10—C11—N2 | 0.0 (5) | S1i—Ag1—N2—C7 | 70.9 (2) |
C4—C5—N1—C1 | 0.8 (4) | N1—Ag1—N2—C11 | −4.1 (7) |
C6—C5—N1—C1 | −175.9 (3) | S1i—Ag1—N2—C11 | −110.7 (2) |
C4—C5—N1—Ag1 | 176.7 (2) | N2—C7—S1—C6i | −173.7 (2) |
C6—C5—N1—Ag1 | 0.0 (4) | C8—C7—S1—C6i | 5.8 (3) |
C2—C1—N1—C5 | −0.1 (5) | N2—C7—S1—Ag1i | −82.5 (2) |
C2—C1—N1—Ag1 | −176.3 (3) | C8—C7—S1—Ag1i | 97.0 (3) |
Symmetry code: (i) −x+1, −y, −z+1. |