In the crystal structure of the title compound, [Ag(C18H36S6O4)]·NO3, the asymmetric unit comprises two structurally independent, but conformationally similar, complexes, both of which have crystallographic 2/m symmetry. The nitrate counterions were modelled as rotationally disordered, with N atoms on 2/m special positions.
Supporting information
CCDC reference: 225663
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.007 Å
- Disorder in solvent or counterion
- R factor = 0.050
- wR factor = 0.123
- Data-to-parameter ratio = 17.6
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor O2 - H2O ... ?
Alert level C
PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . O3
PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... O3
PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... N2
PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... N1
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 30.00 Perc.
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O5
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O6
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O7
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O8
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 27
C1 -S1 -AG1 -S1 -125.90 0.20 1.555 1.555 1.555 5.655
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 28
C1 -S1 -AG1 -S1 125.89 0.17 6.555 1.555 1.555 5.655
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 41
C2 -S2 -AG1 -S2 -174.00100.00 1.555 1.555 1.555 5.655
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 42
C3 -S2 -AG1 -S2 84.00100.00 1.555 1.555 1.555 5.655
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 47
C6 -S3 -AG2 -S3 -54.10 0.20 1.555 1.555 1.555 5.656
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 48
C6 -S3 -AG2 -S3 54.10 0.30 6.555 1.555 1.555 5.656
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 65
C7 -S4 -AG2 -S4 -168.00 8.00 1.555 1.555 1.555 5.656
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 66
C8 -S4 -AG2 -S4 -67.00 8.00 1.555 1.555 1.555 5.656
PLAT731_ALERT_1_C Bond Calc 0.91(5), Rep 0.912(19) ...... 2.63 su-Rat
O1 -H1O 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.89(4), Rep 0.889(19) ...... 2.11 su-Rat
O2 -H2O 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 110(5), Rep 110(2) ...... 2.50 su-Rat
C10 -O2 -H2O 1.555 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.91(5), Rep 0.912(19) ...... 2.63 su-Rat
O1 -H1O 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.91(5), Rep 0.912(19) ...... 2.63 su-Rat
O1 -H1O 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.89(4), Rep 0.889(19) ...... 2.11 su-Rat
O2 -H2O 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.89(4), Rep 0.889(19) ...... 2.11 su-Rat
O2 -H2O 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.89(4), Rep 0.889(19) ...... 2.11 su-Rat
O2 -H2O 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.89(4), Rep 0.889(19) ...... 2.11 su-Rat
O2 -H2O 1.555 1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) . 1.16 Ratio
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3
N O3
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
28 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
10 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
5 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
14 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT and XPREP (Siemens, 1995); program(s) used to solve structure: SIR97 (Altomare, et al. 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Farrugia, 1997)
WinGX32 (Farrugia, 1999); software used to prepare material for publication: enCIFer (CCDC, 2003).
(1,4,7,11,14,17-hexathia-9,9,19,19-tetrahydroxymethylcycloicosane)silver(I)
nitrate
top
Crystal data top
[Ag(C18H36O4S6)]NO3 | F(000) = 1400 |
Mr = 678.71 | Dx = 1.737 Mg m−3 |
Monoclinic, C2/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2y | Cell parameters from 943 reflections |
a = 13.933 (7) Å | θ = 3.0–28.1° |
b = 19.401 (10) Å | µ = 1.30 mm−1 |
c = 11.851 (6) Å | T = 150 K |
β = 125.907 (7)° | Irregular, colourless |
V = 2595 (2) Å3 | 0.43 × 0.34 × 0.25 mm |
Z = 4 | |
Data collection top
Bruker SMART 1000 CCD diffractometer | 3180 independent reflections |
Radiation source: sealed tube | 3036 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.018 |
ω scans | θmax = 28.3°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1999) | h = −18→17 |
Tmin = 0.585, Tmax = 0.723 | k = −25→25 |
12618 measured reflections | l = −15→15 |
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)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.123 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.24 | w = 1/[σ2(Fo2) + (0.0022P)2 + 34.9089P] where P = (Fo2 + 2Fc2)/3 |
3180 reflections | (Δ/σ)max < 0.001 |
181 parameters | Δρmax = 0.85 e Å−3 |
10 restraints | Δρmin = −0.95 e Å−3 |
Special details top
Experimental. The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin
mohair fibre attached to a copper pin. Upon mounting on the diffractometer,
the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied
by an Oxford Cryosystems Crystream and data were collected at this
temperature. 209 standard reflections were obtained by recollecting the first
50 CCD frames at the end of data collection. They were then used for a decay
correction, giving an overall decay of 0.28%. |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
C1 | 0.2937 (4) | −0.0714 (2) | 0.0671 (5) | 0.0265 (9) | |
H1A | 0.3355 | −0.1112 | 0.1299 | 0.032* | |
H1B | 0.2290 | −0.0583 | 0.0746 | 0.032* | |
C2 | 0.2378 (4) | −0.0952 (3) | −0.0826 (5) | 0.0274 (10) | |
H2A | 0.1899 | −0.0569 | −0.1467 | 0.033* | |
H2B | 0.1832 | −0.1339 | −0.1041 | 0.033* | |
C3 | 0.4178 (4) | −0.1894 (2) | 0.0161 (4) | 0.0228 (9) | |
H3A | 0.4648 | −0.1674 | 0.1092 | 0.027* | |
H3B | 0.3580 | −0.2195 | 0.0109 | 0.027* | |
C4 | 0.5000 | −0.2335 (3) | 0.0000 | 0.0200 (11) | |
C5 | 0.4269 (4) | −0.2791 (2) | −0.1312 (5) | 0.0251 (9) | |
H5A | 0.3782 | −0.2493 | −0.2142 | 0.030* | |
H5B | 0.4815 | −0.3058 | −0.1422 | 0.030* | |
C6 | 0.2151 (4) | −0.0710 (2) | 0.3944 (5) | 0.0298 (10) | |
H6A | 0.1383 | −0.0577 | 0.3755 | 0.036* | |
H6B | 0.2000 | −0.1107 | 0.3336 | 0.036* | |
C7 | 0.2971 (5) | −0.0946 (3) | 0.5451 (6) | 0.0329 (11) | |
H7A | 0.2581 | −0.1328 | 0.5593 | 0.039* | |
H7B | 0.3075 | −0.0561 | 0.6061 | 0.039* | |
C8 | 0.3959 (4) | −0.1920 (2) | 0.4718 (5) | 0.0265 (9) | |
H8A | 0.3392 | −0.2225 | 0.4722 | 0.032* | |
H8B | 0.3542 | −0.1712 | 0.3779 | 0.032* | |
C9 | 0.5000 | −0.2354 (3) | 0.5000 | 0.0234 (12) | |
C10 | 0.4478 (4) | −0.2802 (2) | 0.3694 (5) | 0.0276 (10) | |
H10A | 0.3795 | −0.3065 | 0.3524 | 0.033* | |
H10B | 0.4183 | −0.2499 | 0.2879 | 0.033* | |
O1 | 0.3518 (3) | −0.32523 (19) | −0.1239 (4) | 0.0355 (8) | |
H1O | 0.392 (4) | −0.3655 (14) | −0.087 (7) | 0.053* | |
O2 | 0.5318 (3) | −0.32682 (19) | 0.3822 (4) | 0.0359 (8) | |
H2O | 0.525 (5) | −0.3675 (13) | 0.411 (7) | 0.054* | |
S1 | 0.39684 (14) | 0.0000 | 0.12978 (16) | 0.0224 (3) | |
S2 | 0.34177 (10) | −0.12242 (6) | −0.11692 (12) | 0.0246 (2) | |
S3 | 0.26683 (14) | 0.0000 | 0.34483 (17) | 0.0253 (3) | |
S4 | 0.44196 (11) | −0.12345 (6) | 0.59966 (12) | 0.0288 (3) | |
Ag1 | 0.5000 | 0.0000 | 0.0000 | 0.0376 (2) | |
Ag2 | 0.5000 | 0.0000 | 0.5000 | 0.0392 (2) | |
N1 | 0.0000 | 0.0000 | 0.0000 | 0.036 (2) | |
O3 | 0.0299 (11) | 0.0000 | −0.0881 (14) | 0.063 (4) | 0.50 |
O4 | 0.0148 (9) | −0.0556 (4) | −0.0310 (10) | 0.053 (3) | 0.50 |
N2 | 0.0000 | 0.0000 | −0.5000 | 0.0283 (17) | |
O5 | 0.0000 | 0.0630 (8) | −0.5000 | 0.059 (6)* | 0.30 |
O6 | −0.0304 (12) | −0.0340 (7) | −0.6063 (13) | 0.043 (3)* | 0.30 |
O7 | −0.1072 (18) | 0.0000 | −0.592 (4) | 0.078 (12)* | 0.20 |
O8 | 0.0567 (18) | 0.0552 (9) | −0.452 (2) | 0.040 (4)* | 0.20 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.027 (2) | 0.020 (2) | 0.038 (3) | −0.0016 (18) | 0.023 (2) | −0.0001 (19) |
C2 | 0.019 (2) | 0.024 (2) | 0.034 (2) | 0.0015 (17) | 0.0129 (19) | 0.0004 (19) |
C3 | 0.026 (2) | 0.024 (2) | 0.021 (2) | 0.0026 (17) | 0.0158 (18) | 0.0022 (17) |
C4 | 0.021 (3) | 0.021 (3) | 0.020 (3) | 0.000 | 0.013 (2) | 0.000 |
C5 | 0.029 (2) | 0.022 (2) | 0.024 (2) | −0.0023 (18) | 0.0158 (19) | −0.0033 (17) |
C6 | 0.025 (2) | 0.021 (2) | 0.042 (3) | −0.0008 (18) | 0.019 (2) | −0.002 (2) |
C7 | 0.048 (3) | 0.021 (2) | 0.044 (3) | 0.001 (2) | 0.035 (3) | 0.002 (2) |
C8 | 0.024 (2) | 0.024 (2) | 0.023 (2) | 0.0006 (18) | 0.0090 (18) | −0.0058 (18) |
C9 | 0.023 (3) | 0.020 (3) | 0.021 (3) | 0.000 | 0.010 (2) | 0.000 |
C10 | 0.027 (2) | 0.024 (2) | 0.028 (2) | −0.0007 (18) | 0.0146 (19) | −0.0059 (18) |
O1 | 0.0344 (19) | 0.0292 (19) | 0.040 (2) | −0.0062 (15) | 0.0205 (17) | −0.0030 (16) |
O2 | 0.042 (2) | 0.0271 (18) | 0.047 (2) | 0.0048 (16) | 0.0315 (19) | −0.0007 (16) |
S1 | 0.0218 (7) | 0.0208 (7) | 0.0228 (7) | 0.000 | 0.0121 (6) | 0.000 |
S2 | 0.0256 (5) | 0.0240 (5) | 0.0220 (5) | 0.0025 (4) | 0.0127 (4) | 0.0009 (4) |
S3 | 0.0237 (7) | 0.0297 (8) | 0.0239 (7) | 0.000 | 0.0148 (6) | 0.000 |
S4 | 0.0342 (6) | 0.0239 (6) | 0.0222 (5) | 0.0016 (5) | 0.0132 (5) | −0.0024 (4) |
Ag1 | 0.0300 (4) | 0.0558 (5) | 0.0356 (4) | 0.000 | 0.0241 (4) | 0.000 |
Ag2 | 0.0229 (4) | 0.0498 (5) | 0.0432 (5) | 0.000 | 0.0184 (4) | 0.000 |
N1 | 0.015 (4) | 0.031 (5) | 0.039 (5) | 0.000 | 0.004 (4) | 0.000 |
O3 | 0.035 (7) | 0.100 (13) | 0.063 (9) | 0.000 | 0.033 (7) | 0.000 |
O4 | 0.037 (5) | 0.031 (4) | 0.058 (7) | 0.012 (4) | 0.009 (4) | −0.002 (4) |
N2 | 0.037 (5) | 0.024 (4) | 0.039 (5) | 0.000 | 0.031 (4) | 0.000 |
Geometric parameters (Å, º) top
C1—C2 | 1.532 (7) | O1—H1O | 0.912 (19) |
C1—S1 | 1.812 (5) | O2—H2O | 0.889 (19) |
C1—H1A | 0.9900 | S1—C1iii | 1.812 (5) |
C1—H1B | 0.9900 | S1—Ag1 | 2.6504 (18) |
C2—S2 | 1.798 (5) | S2—Ag1 | 2.9730 (16) |
C2—H2A | 0.9900 | S3—C6iii | 1.805 (5) |
C2—H2B | 0.9900 | S3—Ag2 | 2.632 (2) |
C3—C4 | 1.529 (5) | S4—Ag2 | 2.9842 (16) |
C3—S2 | 1.826 (5) | Ag1—S1iv | 2.6504 (19) |
C3—H3A | 0.9900 | Ag1—S2iv | 2.9730 (16) |
C3—H3B | 0.9900 | Ag1—S2i | 2.9730 (16) |
C4—C3i | 1.529 (5) | Ag1—S2iii | 2.9730 (16) |
C4—C5 | 1.542 (5) | Ag2—S3v | 2.632 (2) |
C4—C5i | 1.542 (5) | Ag2—S4iii | 2.9842 (16) |
C5—O1 | 1.418 (6) | Ag2—S4ii | 2.9842 (16) |
C5—H5A | 0.9900 | Ag2—S4v | 2.9842 (16) |
C5—H5B | 0.9900 | N1—O4 | 1.197 (7) |
C6—C7 | 1.520 (7) | N1—O4iii | 1.197 (7) |
C6—S3 | 1.805 (5) | N1—O4vi | 1.197 (7) |
C6—H6A | 0.9900 | N1—O4vii | 1.197 (7) |
C6—H6B | 0.9900 | N1—O3vi | 1.332 (11) |
C7—S4 | 1.809 (5) | N1—O3 | 1.332 (11) |
C7—H7A | 0.9900 | N2—O5 | 1.222 (16) |
C7—H7B | 0.9900 | N2—O5viii | 1.222 (16) |
C8—C9 | 1.535 (6) | N2—O7 | 1.229 (19) |
C8—S4 | 1.826 (5) | N2—O7viii | 1.229 (19) |
C8—H8A | 0.9900 | N2—O8 | 1.252 (15) |
C8—H8B | 0.9900 | N2—O8ix | 1.252 (15) |
C9—C8ii | 1.535 (6) | N2—O8viii | 1.252 (15) |
C9—C10 | 1.536 (6) | N2—O8iii | 1.252 (15) |
C9—C10ii | 1.536 (6) | N2—O6 | 1.256 (12) |
C10—O2 | 1.415 (6) | N2—O6iii | 1.256 (11) |
C10—H10A | 0.9900 | N2—O6viii | 1.256 (11) |
C10—H10B | 0.9900 | N2—O6ix | 1.256 (11) |
| | | |
C2—C1—S1 | 116.6 (3) | C10—O2—H2O | 110 (2) |
C2—C1—H1A | 108.2 | C1—S1—C1iii | 99.7 (3) |
S1—C1—H1A | 108.2 | C1—S1—Ag1 | 109.37 (16) |
C2—C1—H1B | 108.2 | C1iii—S1—Ag1 | 109.37 (16) |
S1—C1—H1B | 108.2 | C2—S2—C3 | 98.7 (2) |
H1A—C1—H1B | 107.3 | C2—S2—Ag1 | 97.77 (16) |
C1—C2—S2 | 114.9 (3) | C3—S2—Ag1 | 105.64 (16) |
C1—C2—H2A | 108.5 | C6—S3—C6iii | 99.5 (3) |
S2—C2—H2A | 108.5 | C6—S3—Ag2 | 109.72 (17) |
C1—C2—H2B | 108.5 | C6iii—S3—Ag2 | 109.72 (17) |
S2—C2—H2B | 108.5 | C7—S4—C8 | 98.8 (2) |
H2A—C2—H2B | 107.5 | C7—S4—Ag2 | 96.61 (16) |
C4—C3—S2 | 112.9 (3) | C8—S4—Ag2 | 107.51 (17) |
C4—C3—H3A | 109.0 | S1—Ag1—S1iv | 180.00 (4) |
S2—C3—H3A | 109.0 | S1—Ag1—S2 | 76.36 (4) |
C4—C3—H3B | 109.0 | S1iv—Ag1—S2 | 103.64 (4) |
S2—C3—H3B | 109.0 | S1—Ag1—S2iv | 103.64 (4) |
H3A—C3—H3B | 107.8 | S1iv—Ag1—S2iv | 76.36 (4) |
C3—C4—C3i | 111.8 (5) | S2—Ag1—S2iv | 180.00 (9) |
C3—C4—C5 | 110.3 (2) | S1—Ag1—S2i | 103.64 (4) |
C3i—C4—C5 | 107.2 (2) | S1iv—Ag1—S2i | 76.36 (4) |
C3—C4—C5i | 107.2 (2) | S2—Ag1—S2i | 73.95 (6) |
C3i—C4—C5i | 110.3 (2) | S2iv—Ag1—S2i | 106.05 (6) |
C5—C4—C5i | 110.0 (5) | S1—Ag1—S2iii | 76.36 (4) |
O1—C5—C4 | 112.0 (4) | S1iv—Ag1—S2iii | 103.64 (4) |
O1—C5—H5A | 109.2 | S2—Ag1—S2iii | 106.05 (6) |
C4—C5—H5A | 109.2 | S2iv—Ag1—S2iii | 73.95 (6) |
O1—C5—H5B | 109.2 | S2i—Ag1—S2iii | 180.00 (6) |
C4—C5—H5B | 109.2 | S3—Ag2—S3v | 180.00 (5) |
H5A—C5—H5B | 107.9 | S3—Ag2—S4iii | 76.50 (4) |
C7—C6—S3 | 116.4 (3) | S3v—Ag2—S4iii | 103.50 (4) |
C7—C6—H6A | 108.2 | S3—Ag2—S4 | 76.50 (4) |
S3—C6—H6A | 108.2 | S3v—Ag2—S4 | 103.50 (4) |
C7—C6—H6B | 108.2 | S4iii—Ag2—S4 | 106.75 (6) |
S3—C6—H6B | 108.2 | S3—Ag2—S4ii | 103.50 (4) |
H6A—C6—H6B | 107.3 | S3v—Ag2—S4ii | 76.50 (4) |
C6—C7—S4 | 115.2 (3) | S4iii—Ag2—S4ii | 180.0 |
C6—C7—H7A | 108.5 | S4—Ag2—S4ii | 73.25 (6) |
S4—C7—H7A | 108.5 | S3—Ag2—S4v | 103.50 (4) |
C6—C7—H7B | 108.5 | S3v—Ag2—S4v | 76.50 (4) |
S4—C7—H7B | 108.5 | S4iii—Ag2—S4v | 73.25 (6) |
H7A—C7—H7B | 107.5 | S4—Ag2—S4v | 180.0 |
C9—C8—S4 | 113.0 (3) | S4ii—Ag2—S4v | 106.75 (6) |
C9—C8—H8A | 109.0 | O4—N1—O4iii | 128.9 (9) |
S4—C8—H8A | 109.0 | O4vi—N1—O4vii | 128.9 (9) |
C9—C8—H8B | 109.0 | O4—N1—O3vi | 115.5 (5) |
S4—C8—H8B | 109.0 | O4iii—N1—O3vi | 115.5 (5) |
H8A—C8—H8B | 107.8 | O4vi—N1—O3 | 115.5 (5) |
C8ii—C9—C8 | 113.4 (5) | O4vii—N1—O3 | 115.5 (5) |
C8ii—C9—C10 | 111.0 (3) | O7—N2—O8 | 121.3 (10) |
C8—C9—C10 | 105.2 (2) | O7viii—N2—O8ix | 121.3 (10) |
C8ii—C9—C10ii | 105.2 (2) | O7viii—N2—O8viii | 121.3 (10) |
C8—C9—C10ii | 111.0 (3) | O8ix—N2—O8viii | 117 (2) |
C10—C9—C10ii | 111.1 (5) | O7—N2—O8iii | 121.3 (10) |
O2—C10—C9 | 112.4 (4) | O8—N2—O8iii | 117 (2) |
O2—C10—H10A | 109.1 | O5—N2—O6 | 121.7 (6) |
C9—C10—H10A | 109.1 | O5viii—N2—O6iii | 121.7 (6) |
O2—C10—H10B | 109.1 | O5viii—N2—O6viii | 121.7 (6) |
C9—C10—H10B | 109.1 | O6iii—N2—O6viii | 116.5 (13) |
H10A—C10—H10B | 107.9 | O5—N2—O6ix | 121.7 (6) |
C5—O1—H1O | 108 (2) | O6—N2—O6ix | 116.5 (13) |
| | | |
S1—C1—C2—S2 | 58.7 (4) | C1iii—S1—Ag1—S2i | −178.82 (17) |
S2—C3—C4—C3i | 49.74 (19) | C1—S1—Ag1—S2iii | 109.41 (18) |
S2—C3—C4—C5 | −69.4 (4) | C1iii—S1—Ag1—S2iii | 1.18 (17) |
S2—C3—C4—C5i | 170.7 (3) | C2—S2—Ag1—S1 | 23.63 (16) |
C3—C4—C5—O1 | −61.3 (5) | C3—S2—Ag1—S1 | −77.68 (15) |
C3i—C4—C5—O1 | 176.8 (4) | C2—S2—Ag1—S1iv | −156.37 (16) |
C5i—C4—C5—O1 | 56.8 (3) | C3—S2—Ag1—S1iv | 102.32 (15) |
S3—C6—C7—S4 | −59.5 (5) | C2—S2—Ag1—S2iv | −174 (100) |
S4—C8—C9—C8ii | −48.2 (2) | C3—S2—Ag1—S2iv | 84 (100) |
S4—C8—C9—C10 | −169.7 (3) | C2—S2—Ag1—S2i | 132.43 (17) |
S4—C8—C9—C10ii | 70.1 (5) | C3—S2—Ag1—S2i | 31.12 (14) |
C8ii—C9—C10—O2 | 60.5 (5) | C2—S2—Ag1—S2iii | −47.57 (17) |
C8—C9—C10—O2 | −176.4 (4) | C3—S2—Ag1—S2iii | −148.88 (14) |
C10ii—C9—C10—O2 | −56.2 (3) | C6—S3—Ag2—S3v | −54.1 (2) |
C2—C1—S1—C1iii | 86.0 (4) | C6iii—S3—Ag2—S3v | 54.1 (3) |
C2—C1—S1—Ag1 | −28.7 (4) | C6—S3—Ag2—S4iii | −109.77 (19) |
C1—C2—S2—C3 | 56.7 (4) | C6iii—S3—Ag2—S4iii | −1.48 (18) |
C1—C2—S2—Ag1 | −50.5 (3) | C6—S3—Ag2—S4 | 1.48 (18) |
C4—C3—S2—C2 | 169.6 (3) | C6iii—S3—Ag2—S4 | 109.77 (19) |
C4—C3—S2—Ag1 | −89.8 (3) | C6—S3—Ag2—S4ii | 70.23 (19) |
C7—C6—S3—C6iii | −86.3 (4) | C6iii—S3—Ag2—S4ii | 178.52 (18) |
C7—C6—S3—Ag2 | 28.7 (4) | C6—S3—Ag2—S4v | −178.52 (18) |
C6—C7—S4—C8 | −57.8 (4) | C6iii—S3—Ag2—S4v | −70.23 (19) |
C6—C7—S4—Ag2 | 51.1 (4) | C7—S4—Ag2—S3 | −23.77 (18) |
C9—C8—S4—C7 | −172.3 (3) | C8—S4—Ag2—S3 | 77.62 (16) |
C9—C8—S4—Ag2 | 87.9 (3) | C7—S4—Ag2—S3v | 156.23 (18) |
C1—S1—Ag1—S1iv | −125.9 (2) | C8—S4—Ag2—S3v | −102.38 (16) |
C1iii—S1—Ag1—S1iv | 125.89 (17) | C7—S4—Ag2—S4iii | 47.39 (18) |
C1—S1—Ag1—S2 | −1.18 (17) | C8—S4—Ag2—S4iii | 148.78 (15) |
C1iii—S1—Ag1—S2 | −109.41 (18) | C7—S4—Ag2—S4ii | −132.61 (18) |
C1—S1—Ag1—S2iv | 178.82 (17) | C8—S4—Ag2—S4ii | −31.22 (15) |
C1iii—S1—Ag1—S2iv | 70.59 (18) | C7—S4—Ag2—S4v | −168 (8) |
C1—S1—Ag1—S2i | −70.59 (18) | C8—S4—Ag2—S4v | −67 (8) |
Symmetry codes: (i) −x+1, y, −z; (ii) −x+1, y, −z+1; (iii) x, −y, z; (iv) −x+1, −y, −z; (v) −x+1, −y, −z+1; (vi) −x, −y, −z; (vii) −x, y, −z; (viii) −x, −y, −z−1; (ix) −x, y, −z−1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1O···O4x | 0.91 (2) | 1.96 (3) | 2.857 (9) | 167 (6) |
O1—H1O···O4xi | 0.91 (2) | 2.09 (3) | 2.963 (10) | 160 (4) |
O2—H2O···O5xii | 0.89 (2) | 1.86 (3) | 2.728 (13) | 164 (4) |
O2—H2O···O6xiii | 0.89 (2) | 2.02 (4) | 2.862 (14) | 157 (6) |
O2—H2O···O8xii | 0.89 (2) | 2.06 (4) | 2.905 (19) | 159 (6) |
O2—H2O···O8xiv | 0.89 (2) | 2.10 (3) | 2.94 (2) | 157 (3) |
Symmetry codes: (x) −x+1/2, −y−1/2, −z; (xi) x+1/2, −y−1/2, z; (xii) x+1/2, y−1/2, z+1; (xiii) x+1/2, −y−1/2, z+1; (xiv) −x+1/2, y−1/2, −z. |