Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807026360/bt2378sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807026360/bt2378Isup2.hkl |
CCDC reference: 654697
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.017 Å
- R factor = 0.074
- wR factor = 0.239
- Data-to-parameter ratio = 18.2
checkCIF/PLATON results
No syntax errors found
Alert level A ABSTM02_ALERT_3_A The ratio of expected to reported Tmax/Tmin(RR') is < 0.50 Tmin and Tmax reported: 0.294 0.790 Tmin(prime) and Tmax expected: 0.602 0.790 RR(prime) = 0.488 Please check that your absorption correction is appropriate.
Author Response: The ratio is given by the ABSCOR program. |
PLAT061_ALERT_3_A Tmax/Tmin Range Test RR' too Large ............. 0.48
Author Response: The ratio is given by the ABSCOR program. Although the crystal has a well-defined shape, there appears to be some problem with absorption effects, so that ABSCOR is carry out its proper function of correcting for absorption effects on the full sphere of reflections. |
Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for N13 PLAT413_ALERT_2_B Short Inter XH3 .. XHn H1B .. H1B .. 1.98 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.12 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) 300 Ang. PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 2000 Deg. PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C13 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for S1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C15 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for S2 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C16 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C17 PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 17 PLAT415_ALERT_2_C Short Inter D-H..H-X H1B .. H42 .. 2.12 Ang. PLAT415_ALERT_2_C Short Inter D-H..H-X H5B .. H121 .. 2.10 Ang. PLAT420_ALERT_2_C D-H Without Acceptor N4 - H41 ... ? PLAT420_ALERT_2_C D-H Without Acceptor N4 - H42 ... ? PLAT420_ALERT_2_C D-H Without Acceptor N8 - H81 ... ? PLAT420_ALERT_2_C D-H Without Acceptor N8 - H82 ... ? PLAT420_ALERT_2_C D-H Without Acceptor N12 - H121 ... ? PLAT731_ALERT_1_C Bond Calc 1.300(15), Rep 1.301(7) ...... 2.14 su-Ra F1 -C15 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.299(17), Rep 1.299(8) ...... 2.12 su-Ra F3 -C15 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C F3 O3 S PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 C2 H3 N
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 150
2 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 23 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 6 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 7 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For a study of the complex [µ2-(C4H8N4)6Ag4][µ2-(C4H8N4)6(C2H3N)2Ag4](ClO4)8.2H2O, see Wang et al. (2006).
Silver trifluoromethylsulfonate (0.1 mmol, 26 mg) dissolved in water (2 ml) was mixed with 4-amino-3,5-dimethyl-1,2,4-triazole (0.1 mmol, 12 mg) dissolved in ethanol (2 ml) of ethanol). Ether was then diffused into the solution to yield prisms in about 50% yield.
The two trifluoromethylsulfonate ions are not hydrogen bonded to the tetranuclear cluster. The six sulfur–oxygen bond distances were restrained to within 0.01 Å of each other, as were the six sulfur-oxygen and carbon-fluorine bond distances. The fluroine···fluorine distances were similarly restrained in each ion.
The anisotropic displacement parameters of the solvate acetonitrile molecule were restrained so that the atoms were nearly isotropic.
The carbon-bound H atoms were placed in calculated positions [C—H 0.93 to 0.96 Å; U(H) = 1.2 to 1.5 times Ueq(C)]. The nitrogen- and oxygen-bound H atoms were similarly treated. These were included in the refinement in the riding model approximation. The amino –NH2 groups were assumed to be planar whereas the methyl groups were rotated to fit the electron density. The amino groups are probably not planar as there are short intermolecular H···H interactions; they are probably disordered as there are no strong N···O hydrogen bonds in the crystal structure.
The final difference Fourier map had a large peak at about 1 Å from Ag1 as well as a deep hole at a similar distance from this atom, and is probably a consequence of inadequate absorption. This is supported by the large difference between the expected and calculated transmission factors.
Silver perchlorate reacts with 4-amino-3,5-dimethyl-1,2,4-triazole in acetonitrile to form [µ2-(C4H8N4)6Ag4] [µ2-(C4H8N4)6(C2H3N)2Ag4] 8[ClO4].2H2O, which features two tetranuclear cluster ions. The N-heterocycles in both each bridges two silver atoms. In acetonitrile-coordinated cluster, there are three-coordinate trigonal planar and four-coordinate tetrahedral silver atoms, with the higher coordination arising from coordination by the water molecules. The solvent-free cluster has only trigonal-planar silver atoms (Wang et al., 2006).
The synthesis when with silver trifluoromethylsulfonate in acetonitrile led to the isolation of the acetonitrile-coordinated tetranuclear cluster [µ2-(C4H8N4)6(C2H3N)2Ag4]4+, whose charge is balanced by four trifluoromethylsulfonate ions. The N-heterocycles bridge two silver atoms, and two of the silver atoms are also coordinated by acetonitrile. The salt crystallizes as an acetonitrile disolvate. The N-heterocycle each bridges to two silver atoms, and two of the silver atoms are also coordinated by acetonitrile.
For a study of the complex [µ2-(C4H8N4)6Ag4][µ2-(C4H8N4)6(C2H3N)2Ag4](ClO4)8.2H2O, see Wang et al. (2006).
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: publCIF (Westrip, 2007).
Fig. 1. Thermal ellipsoid plot of the tetranuclear [(C7H8N4)6(C2H3N)2Ag4]4+ cation; ellipsoids are drawn at the 30% probability level. Symmetry code (i): 2 - x, 1 - y, 1 - z. |
[Ag4(C4H8N4)6(C2H3N)2](CF3O3S)4·2C2H3N | Z = 1 |
Mr = 1864.84 | F(000) = 928 |
Triclinic, P1 | Dx = 1.751 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.110 (3) Å | Cell parameters from 12901 reflections |
b = 12.695 (3) Å | θ = 3.2–27.5° |
c = 13.001 (3) Å | µ = 1.31 mm−1 |
α = 108.59 (2)° | T = 295 K |
β = 92.84 (2)° | Prism, colourless |
γ = 108.68 (2)° | 0.38 × 0.24 × 0.18 mm |
V = 1768.9 (7) Å3 |
Rigaku R-AXIS RAPID IP diffractometer | 8026 independent reflections |
Radiation source: fine-focus sealed tube | 5532 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
ω scans | θmax = 27.5°, θmin = 3.2° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −15→15 |
Tmin = 0.294, Tmax = 0.790 | k = −16→16 |
17453 measured reflections | l = −16→16 |
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)] = 0.074 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.239 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.1356P)2 + 1.8203P] where P = (Fo2 + 2Fc2)/3 |
8026 reflections | (Δ/σ)max = 0.001 |
440 parameters | Δρmax = 2.27 e Å−3 |
150 restraints | Δρmin = −1.07 e Å−3 |
[Ag4(C4H8N4)6(C2H3N)2](CF3O3S)4·2C2H3N | γ = 108.68 (2)° |
Mr = 1864.84 | V = 1768.9 (7) Å3 |
Triclinic, P1 | Z = 1 |
a = 12.110 (3) Å | Mo Kα radiation |
b = 12.695 (3) Å | µ = 1.31 mm−1 |
c = 13.001 (3) Å | T = 295 K |
α = 108.59 (2)° | 0.38 × 0.24 × 0.18 mm |
β = 92.84 (2)° |
Rigaku R-AXIS RAPID IP diffractometer | 8026 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 5532 reflections with I > 2σ(I) |
Tmin = 0.294, Tmax = 0.790 | Rint = 0.046 |
17453 measured reflections |
R[F2 > 2σ(F2)] = 0.074 | 150 restraints |
wR(F2) = 0.239 | H-atom parameters constrained |
S = 1.07 | Δρmax = 2.27 e Å−3 |
8026 reflections | Δρmin = −1.07 e Å−3 |
440 parameters |
x | y | z | Uiso*/Ueq | ||
Ag1 | 0.88000 (5) | 0.37448 (5) | 0.53930 (4) | 0.0621 (2) | |
Ag2 | 0.88609 (5) | 0.34115 (5) | 0.27393 (5) | 0.0638 (2) | |
S1 | 0.7324 (2) | −0.2778 (2) | 0.18838 (19) | 0.0805 (6) | |
S2 | 0.35409 (18) | 0.13112 (19) | 0.22789 (16) | 0.0712 (5) | |
F1 | 0.9445 (7) | −0.1622 (9) | 0.2985 (8) | 0.170 (4) | |
F2 | 0.8266 (7) | −0.0761 (8) | 0.3487 (7) | 0.160 (3) | |
F3 | 0.8888 (11) | −0.0812 (11) | 0.2008 (9) | 0.217 (5) | |
F4 | 0.1809 (7) | −0.0452 (7) | 0.2334 (7) | 0.158 (3) | |
F5 | 0.1678 (7) | −0.0141 (7) | 0.0858 (6) | 0.160 (3) | |
F6 | 0.2856 (7) | −0.0934 (6) | 0.1161 (7) | 0.149 (3) | |
O1 | 0.6474 (7) | −0.2360 (8) | 0.1530 (7) | 0.132 (3) | |
O2 | 0.7789 (8) | −0.3403 (8) | 0.0991 (6) | 0.131 (3) | |
O3 | 0.7050 (9) | −0.3320 (9) | 0.2672 (7) | 0.159 (4) | |
O4 | 0.4239 (6) | 0.1125 (7) | 0.3072 (6) | 0.110 (2) | |
O5 | 0.4112 (6) | 0.1538 (7) | 0.1402 (5) | 0.111 (2) | |
O6 | 0.2899 (6) | 0.2062 (6) | 0.2726 (5) | 0.0957 (19) | |
N1 | 0.7678 (5) | 0.1969 (5) | 0.4177 (4) | 0.0578 (13) | |
N2 | 0.7624 (5) | 0.1844 (5) | 0.3087 (5) | 0.0579 (13) | |
N3 | 0.6319 (5) | 0.0297 (5) | 0.3212 (5) | 0.0582 (13) | |
N4 | 0.5376 (6) | −0.0794 (6) | 0.2984 (6) | 0.0746 (18) | |
H41 | 0.5009 | −0.1217 | 0.2303 | 0.090* | |
H42 | 0.5155 | −0.1049 | 0.3523 | 0.090* | |
N5 | 0.8361 (5) | 0.5079 (5) | 0.6744 (4) | 0.0562 (13) | |
N6 | 0.7571 (5) | 0.5996 (5) | 0.8023 (5) | 0.0561 (13) | |
N7 | 0.9223 (5) | 0.6100 (5) | 0.7420 (5) | 0.0561 (13) | |
N8 | 0.6722 (5) | 0.6246 (6) | 0.8662 (6) | 0.0739 (18) | |
H81 | 0.5984 | 0.5749 | 0.8477 | 0.089* | |
H82 | 0.6928 | 0.6899 | 0.9246 | 0.089* | |
N9 | 0.8379 (5) | 0.4932 (5) | 0.4025 (5) | 0.0561 (13) | |
N10 | 0.9244 (4) | 0.6030 (5) | 0.4585 (5) | 0.0541 (13) | |
N11 | 0.7536 (4) | 0.6201 (5) | 0.4680 (4) | 0.0517 (12) | |
N12 | 0.6623 (5) | 0.6652 (6) | 0.4855 (5) | 0.0665 (16) | |
H121 | 0.5886 | 0.6184 | 0.4565 | 0.080* | |
H112 | 0.6784 | 0.7404 | 0.5254 | 0.080* | |
N13 | 0.7755 (9) | 0.3396 (10) | 0.1152 (8) | 0.114 (3) | |
N14 | 0.250 (3) | −0.308 (3) | 0.189 (2) | 0.264 (11) | |
C1 | 0.6685 (9) | 0.0784 (10) | 0.5277 (8) | 0.097 (3) | |
H1A | 0.7029 | 0.0213 | 0.5322 | 0.145* | |
H1B | 0.5851 | 0.0474 | 0.5278 | 0.145* | |
H1C | 0.7045 | 0.1508 | 0.5897 | 0.145* | |
C2 | 0.6887 (6) | 0.1028 (7) | 0.4236 (6) | 0.0623 (17) | |
C3 | 0.6779 (6) | 0.0828 (6) | 0.2511 (6) | 0.0569 (15) | |
C4 | 0.6397 (8) | 0.0329 (8) | 0.1312 (6) | 0.075 (2) | |
H4A | 0.6872 | 0.0858 | 0.0985 | 0.113* | |
H4B | 0.5582 | 0.0233 | 0.1144 | 0.113* | |
H4C | 0.6487 | −0.0429 | 0.1022 | 0.113* | |
C5 | 0.6178 (7) | 0.4084 (9) | 0.6657 (9) | 0.084 (3) | |
H5A | 0.6170 | 0.3615 | 0.5911 | 0.126* | |
H5B | 0.5589 | 0.4444 | 0.6671 | 0.126* | |
H5C | 0.6010 | 0.3585 | 0.7092 | 0.126* | |
C6 | 0.7363 (6) | 0.5028 (7) | 0.7115 (6) | 0.0579 (16) | |
C7 | 0.8760 (6) | 0.6652 (7) | 0.8194 (6) | 0.0579 (16) | |
C8 | 0.9362 (8) | 0.7778 (9) | 0.9108 (8) | 0.091 (3) | |
H8A | 1.0201 | 0.8008 | 0.9125 | 0.136* | |
H8B | 0.9178 | 0.7680 | 0.9789 | 0.136* | |
H8C | 0.9100 | 0.8382 | 0.9008 | 0.136* | |
C9 | 0.9304 (7) | 0.8075 (7) | 0.5646 (8) | 0.077 (2) | |
H9A | 0.9333 | 0.8188 | 0.6415 | 0.116* | |
H9B | 0.8855 | 0.8506 | 0.5454 | 0.116* | |
H9C | 1.0093 | 0.8363 | 0.5499 | 0.116* | |
C10 | 0.8730 (5) | 0.6783 (6) | 0.4979 (5) | 0.0538 (15) | |
C11 | 0.7364 (6) | 0.5056 (6) | 0.4077 (5) | 0.0559 (15) | |
C12 | 0.6179 (6) | 0.4146 (7) | 0.3571 (7) | 0.069 (2) | |
H12C | 0.6038 | 0.4019 | 0.2800 | 0.104* | |
H12D | 0.5589 | 0.4413 | 0.3922 | 0.104* | |
H12E | 0.6141 | 0.3414 | 0.3662 | 0.104* | |
C13 | 0.6966 (9) | 0.3471 (10) | 0.0752 (8) | 0.089 (3) | |
C14 | 0.5926 (9) | 0.3532 (13) | 0.0198 (10) | 0.115 (4) | |
H14A | 0.5555 | 0.2814 | −0.0426 | 0.172* | |
H14B | 0.6158 | 0.4199 | −0.0045 | 0.172* | |
H14C | 0.5379 | 0.3625 | 0.0699 | 0.172* | |
C15 | 0.8526 (9) | −0.1444 (10) | 0.2621 (8) | 0.116 (4) | |
C16 | 0.2423 (8) | −0.0117 (9) | 0.1627 (7) | 0.104 (3) | |
C17 | 0.148 (2) | −0.3490 (19) | 0.1723 (19) | 0.167 (7) | |
C18 | 0.021 (3) | −0.403 (3) | 0.146 (3) | 0.265 (13) | |
H18A | −0.0037 | −0.4790 | 0.1551 | 0.398* | |
H18B | −0.0053 | −0.4133 | 0.0717 | 0.398* | |
H18C | −0.0137 | −0.3526 | 0.1952 | 0.398* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.0531 (3) | 0.0673 (4) | 0.0490 (3) | 0.0140 (2) | 0.0020 (2) | 0.0068 (2) |
Ag2 | 0.0540 (3) | 0.0680 (4) | 0.0571 (3) | 0.0103 (3) | 0.0154 (2) | 0.0165 (3) |
S1 | 0.0831 (14) | 0.0877 (14) | 0.0694 (13) | 0.0274 (12) | 0.0081 (10) | 0.0298 (11) |
S2 | 0.0701 (11) | 0.0772 (12) | 0.0525 (10) | 0.0166 (9) | 0.0108 (8) | 0.0146 (9) |
F1 | 0.111 (5) | 0.201 (7) | 0.171 (7) | 0.060 (5) | −0.003 (5) | 0.032 (6) |
F2 | 0.139 (5) | 0.150 (6) | 0.147 (6) | 0.057 (5) | 0.001 (5) | −0.007 (5) |
F3 | 0.220 (8) | 0.199 (8) | 0.194 (8) | 0.006 (6) | 0.045 (7) | 0.088 (7) |
F4 | 0.138 (5) | 0.147 (6) | 0.165 (7) | 0.002 (4) | 0.055 (5) | 0.067 (5) |
F5 | 0.136 (5) | 0.156 (6) | 0.127 (6) | 0.009 (5) | −0.038 (5) | 0.023 (5) |
F6 | 0.173 (6) | 0.091 (4) | 0.146 (6) | 0.029 (4) | 0.037 (5) | 0.009 (4) |
O1 | 0.126 (5) | 0.131 (6) | 0.123 (6) | 0.054 (5) | −0.029 (4) | 0.022 (5) |
O2 | 0.137 (6) | 0.129 (6) | 0.112 (6) | 0.050 (5) | 0.019 (5) | 0.022 (5) |
O3 | 0.195 (8) | 0.164 (7) | 0.108 (6) | 0.024 (6) | 0.033 (6) | 0.071 (6) |
O4 | 0.095 (4) | 0.120 (5) | 0.113 (5) | 0.039 (4) | −0.005 (4) | 0.041 (4) |
O5 | 0.113 (5) | 0.122 (5) | 0.089 (5) | 0.023 (4) | 0.036 (4) | 0.039 (4) |
O6 | 0.107 (4) | 0.099 (4) | 0.075 (4) | 0.046 (4) | 0.015 (3) | 0.013 (3) |
N1 | 0.052 (3) | 0.064 (3) | 0.042 (3) | 0.007 (3) | 0.010 (2) | 0.012 (2) |
N2 | 0.060 (3) | 0.060 (3) | 0.042 (3) | 0.011 (3) | 0.015 (2) | 0.012 (2) |
N3 | 0.049 (3) | 0.062 (3) | 0.050 (3) | 0.008 (2) | 0.011 (2) | 0.012 (3) |
N4 | 0.071 (4) | 0.066 (4) | 0.057 (4) | −0.010 (3) | 0.007 (3) | 0.018 (3) |
N5 | 0.050 (3) | 0.067 (3) | 0.041 (3) | 0.016 (3) | 0.009 (2) | 0.010 (2) |
N6 | 0.051 (3) | 0.070 (3) | 0.054 (3) | 0.026 (3) | 0.017 (2) | 0.025 (3) |
N7 | 0.050 (3) | 0.063 (3) | 0.044 (3) | 0.013 (2) | 0.010 (2) | 0.012 (2) |
N8 | 0.058 (3) | 0.086 (4) | 0.073 (4) | 0.023 (3) | 0.028 (3) | 0.023 (4) |
N9 | 0.046 (3) | 0.060 (3) | 0.048 (3) | 0.012 (2) | 0.003 (2) | 0.006 (2) |
N10 | 0.044 (3) | 0.060 (3) | 0.049 (3) | 0.014 (2) | 0.004 (2) | 0.014 (2) |
N11 | 0.049 (3) | 0.061 (3) | 0.042 (3) | 0.020 (2) | 0.008 (2) | 0.013 (2) |
N12 | 0.046 (3) | 0.073 (4) | 0.065 (4) | 0.023 (3) | 0.008 (3) | 0.003 (3) |
N13 | 0.110 (7) | 0.126 (8) | 0.094 (6) | 0.028 (6) | −0.019 (5) | 0.043 (6) |
N14 | 0.259 (14) | 0.272 (14) | 0.261 (15) | 0.092 (10) | 0.042 (10) | 0.099 (10) |
C1 | 0.088 (6) | 0.121 (8) | 0.057 (5) | 0.001 (5) | 0.013 (4) | 0.036 (5) |
C2 | 0.056 (4) | 0.072 (4) | 0.051 (4) | 0.015 (3) | 0.015 (3) | 0.018 (3) |
C3 | 0.056 (4) | 0.050 (3) | 0.048 (3) | 0.008 (3) | 0.004 (3) | 0.006 (3) |
C4 | 0.090 (6) | 0.079 (5) | 0.035 (3) | 0.013 (4) | 0.005 (3) | 0.009 (3) |
C5 | 0.045 (4) | 0.091 (6) | 0.092 (6) | 0.007 (4) | 0.005 (4) | 0.021 (5) |
C6 | 0.050 (3) | 0.069 (4) | 0.051 (4) | 0.017 (3) | 0.005 (3) | 0.021 (3) |
C7 | 0.054 (4) | 0.068 (4) | 0.048 (3) | 0.019 (3) | 0.013 (3) | 0.018 (3) |
C8 | 0.081 (6) | 0.089 (6) | 0.071 (5) | 0.023 (5) | 0.019 (4) | −0.006 (5) |
C9 | 0.055 (4) | 0.066 (4) | 0.083 (6) | 0.012 (3) | −0.003 (4) | 0.002 (4) |
C10 | 0.048 (3) | 0.065 (4) | 0.042 (3) | 0.017 (3) | 0.006 (2) | 0.013 (3) |
C11 | 0.053 (4) | 0.065 (4) | 0.041 (3) | 0.013 (3) | 0.005 (3) | 0.017 (3) |
C12 | 0.051 (4) | 0.064 (4) | 0.069 (5) | 0.010 (3) | 0.000 (3) | 0.004 (4) |
C13 | 0.088 (6) | 0.103 (7) | 0.060 (5) | 0.019 (5) | −0.003 (4) | 0.025 (5) |
C14 | 0.081 (6) | 0.158 (11) | 0.099 (8) | 0.037 (7) | −0.001 (6) | 0.044 (8) |
C15 | 0.095 (8) | 0.135 (10) | 0.098 (9) | 0.035 (7) | −0.001 (6) | 0.025 (8) |
C16 | 0.110 (8) | 0.090 (7) | 0.095 (8) | 0.017 (6) | 0.024 (7) | 0.030 (6) |
C17 | 0.171 (10) | 0.171 (10) | 0.182 (11) | 0.066 (8) | 0.025 (8) | 0.088 (8) |
C18 | 0.256 (16) | 0.269 (16) | 0.278 (16) | 0.092 (10) | 0.023 (10) | 0.109 (10) |
Ag1—N1 | 2.232 (5) | N10—C10 | 1.291 (9) |
Ag1—N5 | 2.238 (5) | N10—Ag1i | 2.290 (5) |
Ag1—N10i | 2.290 (5) | N11—C11 | 1.354 (9) |
Ag1—Ag2 | 3.3469 (11) | N11—C10 | 1.366 (8) |
Ag2—N2 | 2.267 (6) | N11—N12 | 1.396 (7) |
Ag2—N7i | 2.241 (5) | N12—H121 | 0.8800 |
Ag2—N9 | 2.371 (6) | N12—H112 | 0.8800 |
Ag2—N13 | 2.395 (9) | N13—C13 | 1.110 (13) |
S1—O3 | 1.404 (6) | N14—C17 | 1.15 (3) |
S1—O1 | 1.419 (6) | C1—C2 | 1.496 (11) |
S1—O2 | 1.434 (6) | C1—H1A | 0.9600 |
S1—C15 | 1.776 (12) | C1—H1B | 0.9600 |
S2—O6 | 1.420 (5) | C1—H1C | 0.9600 |
S2—O4 | 1.425 (5) | C3—C4 | 1.469 (9) |
S2—O5 | 1.422 (5) | C4—H4A | 0.9600 |
S2—C16 | 1.781 (11) | C4—H4B | 0.9600 |
F1—C15 | 1.301 (7) | C4—H4C | 0.9600 |
F2—C15 | 1.306 (8) | C5—C6 | 1.486 (10) |
F3—C15 | 1.299 (8) | C5—H5A | 0.9600 |
F4—C16 | 1.301 (7) | C5—H5B | 0.9600 |
F5—C16 | 1.298 (7) | C5—H5C | 0.9600 |
F6—C16 | 1.302 (7) | C7—C8 | 1.466 (11) |
N1—C2 | 1.298 (9) | C8—H8A | 0.9600 |
N1—N2 | 1.370 (8) | C8—H8B | 0.9600 |
N2—C3 | 1.318 (8) | C8—H8C | 0.9600 |
N3—C3 | 1.341 (9) | C9—C10 | 1.493 (10) |
N3—C2 | 1.349 (9) | C9—H9A | 0.9600 |
N3—N4 | 1.415 (8) | C9—H9B | 0.9600 |
N4—H41 | 0.8800 | C9—H9C | 0.9600 |
N4—H42 | 0.8800 | C11—C12 | 1.479 (9) |
N5—C6 | 1.313 (9) | C12—H12C | 0.9600 |
N5—N7 | 1.363 (8) | C12—H12D | 0.9600 |
N6—C6 | 1.347 (9) | C12—H12E | 0.9600 |
N6—C7 | 1.379 (9) | C13—C14 | 1.456 (14) |
N6—N8 | 1.404 (8) | C14—H14A | 0.9600 |
N7—C7 | 1.294 (9) | C14—H14B | 0.9600 |
N7—Ag2i | 2.241 (5) | C14—H14C | 0.9600 |
N8—H81 | 0.8800 | C17—C18 | 1.44 (3) |
N8—H82 | 0.8800 | C18—H18A | 0.9600 |
N9—C11 | 1.291 (9) | C18—H18B | 0.9600 |
N9—N10 | 1.383 (7) | C18—H18C | 0.9600 |
N1—Ag1—N5 | 131.8 (2) | N3—C2—C1 | 126.1 (7) |
N1—Ag1—N10i | 109.7 (2) | N2—C3—N3 | 108.0 (6) |
N5—Ag1—N10i | 117.2 (2) | N2—C3—C4 | 127.2 (7) |
N1—Ag1—Ag2 | 64.14 (15) | N3—C3—C4 | 124.8 (6) |
N5—Ag1—Ag2 | 131.10 (16) | C3—C4—H4A | 109.5 |
N10i—Ag1—Ag2 | 82.56 (14) | C3—C4—H4B | 109.5 |
N2—Ag2—N9 | 97.9 (2) | H4A—C4—H4B | 109.5 |
N2—Ag2—N7i | 130.8 (2) | C3—C4—H4C | 109.5 |
N2—Ag2—N13 | 102.6 (3) | H4A—C4—H4C | 109.5 |
N7i—Ag2—N9 | 114.7 (2) | H4B—C4—H4C | 109.5 |
N7i—Ag2—N13 | 109.4 (3) | C6—C5—H5A | 109.5 |
N9—Ag2—N13 | 95.6 (3) | C6—C5—H5B | 109.5 |
N7i—Ag2—Ag1 | 105.28 (15) | H5A—C5—H5B | 109.5 |
N2—Ag2—Ag1 | 63.63 (14) | C6—C5—H5C | 109.5 |
N9—Ag2—Ag1 | 55.38 (15) | H5A—C5—H5C | 109.5 |
N13—Ag2—Ag1 | 142.1 (3) | H5B—C5—H5C | 109.5 |
O3—S1—O1 | 116.7 (5) | N5—C6—N6 | 108.7 (6) |
O3—S1—O2 | 114.5 (5) | N5—C6—C5 | 128.0 (7) |
O1—S1—O2 | 112.9 (4) | N6—C6—C5 | 123.3 (7) |
O3—S1—C15 | 103.2 (6) | N7—C7—N6 | 108.2 (6) |
O1—S1—C15 | 102.8 (5) | N7—C7—C8 | 127.5 (7) |
O2—S1—C15 | 104.7 (5) | N6—C7—C8 | 124.3 (6) |
O6—S2—O4 | 115.0 (4) | C7—C8—H8A | 109.5 |
O6—S2—O5 | 114.5 (4) | C7—C8—H8B | 109.5 |
O4—S2—O5 | 114.9 (4) | H8A—C8—H8B | 109.5 |
O6—S2—C16 | 103.9 (4) | C7—C8—H8C | 109.5 |
O4—S2—C16 | 102.9 (4) | H8A—C8—H8C | 109.5 |
O5—S2—C16 | 103.6 (4) | H8B—C8—H8C | 109.5 |
C2—N1—N2 | 107.5 (5) | C10—C9—H9A | 109.5 |
C2—N1—Ag1 | 134.9 (5) | C10—C9—H9B | 109.5 |
N2—N1—Ag1 | 116.6 (4) | H9A—C9—H9B | 109.5 |
C3—N2—N1 | 108.0 (6) | C10—C9—H9C | 109.5 |
C3—N2—Ag2 | 136.6 (5) | H9A—C9—H9C | 109.5 |
N1—N2—Ag2 | 115.2 (4) | H9B—C9—H9C | 109.5 |
C3—N3—C2 | 107.4 (6) | N10—C10—N11 | 108.3 (6) |
C3—N3—N4 | 128.8 (6) | N10—C10—C9 | 127.4 (6) |
C2—N3—N4 | 123.8 (6) | N11—C10—C9 | 124.2 (6) |
N3—N4—H41 | 120.0 | N9—C11—N11 | 108.8 (6) |
N3—N4—H42 | 120.0 | N9—C11—C12 | 128.1 (7) |
H41—N4—H42 | 120.0 | N11—C11—C12 | 123.0 (6) |
C6—N5—N7 | 107.9 (5) | C11—C12—H12C | 109.5 |
C6—N5—Ag1 | 130.7 (5) | C11—C12—H12D | 109.5 |
N7—N5—Ag1 | 121.0 (4) | H12C—C12—H12D | 109.5 |
C6—N6—C7 | 106.5 (5) | C11—C12—H12E | 109.5 |
C6—N6—N8 | 125.4 (6) | H12C—C12—H12E | 109.5 |
C7—N6—N8 | 128.1 (6) | H12D—C12—H12E | 109.5 |
C7—N7—N5 | 108.8 (5) | N13—C13—C14 | 178.1 (13) |
C7—N7—Ag2i | 127.3 (5) | C13—C14—H14A | 109.5 |
N5—N7—Ag2i | 123.7 (4) | C13—C14—H14B | 109.5 |
N6—N8—H81 | 120.0 | H14A—C14—H14B | 109.5 |
N6—N8—H82 | 120.0 | C13—C14—H14C | 109.5 |
H81—N8—H82 | 120.0 | H14A—C14—H14C | 109.5 |
C11—N9—N10 | 107.9 (6) | H14B—C14—H14C | 109.5 |
C11—N9—Ag2 | 128.4 (4) | F3—C15—F1 | 106.1 (8) |
N10—N9—Ag2 | 120.3 (4) | F3—C15—F2 | 106.6 (8) |
C10—N10—N9 | 108.2 (5) | F1—C15—F2 | 105.3 (7) |
C10—N10—Ag1i | 131.8 (4) | F3—C15—S1 | 111.5 (8) |
N9—N10—Ag1i | 119.9 (4) | F1—C15—S1 | 113.4 (8) |
C11—N11—C10 | 106.7 (5) | F2—C15—S1 | 113.3 (8) |
C11—N11—N12 | 123.7 (5) | F5—C16—F4 | 106.8 (7) |
C10—N11—N12 | 129.4 (6) | F5—C16—F6 | 106.1 (7) |
N11—N12—H121 | 120.0 | F4—C16—F6 | 107.4 (7) |
N11—N12—H112 | 120.0 | F5—C16—S2 | 112.8 (7) |
H121—N12—H112 | 120.0 | F4—C16—S2 | 111.0 (7) |
C13—N13—Ag2 | 150.4 (10) | F6—C16—S2 | 112.5 (7) |
C2—C1—H1A | 109.5 | N14—C17—C18 | 178 (3) |
C2—C1—H1B | 109.5 | C17—C18—H18A | 109.5 |
H1A—C1—H1B | 109.5 | C17—C18—H18B | 109.5 |
C2—C1—H1C | 109.5 | H18A—C18—H18B | 109.5 |
H1A—C1—H1C | 109.5 | C17—C18—H18C | 109.5 |
H1B—C1—H1C | 109.5 | H18A—C18—H18C | 109.5 |
N1—C2—N3 | 109.1 (6) | H18B—C18—H18C | 109.5 |
N1—C2—C1 | 124.8 (7) | ||
N1—Ag1—Ag2—N7i | −125.5 (2) | N4—N3—C2—N1 | −177.8 (7) |
N5—Ag1—Ag2—N7i | 110.5 (2) | C3—N3—C2—C1 | −178.3 (9) |
N10i—Ag1—Ag2—N7i | −9.4 (2) | N4—N3—C2—C1 | 4.5 (13) |
N1—Ag1—Ag2—N2 | 2.8 (2) | N1—N2—C3—N3 | −1.5 (8) |
N5—Ag1—Ag2—N2 | −121.2 (3) | Ag2—N2—C3—N3 | −176.5 (5) |
N10i—Ag1—Ag2—N2 | 119.0 (2) | N1—N2—C3—C4 | 179.3 (8) |
N1—Ag1—Ag2—N9 | 124.7 (2) | Ag2—N2—C3—C4 | 4.3 (13) |
N5—Ag1—Ag2—N9 | 0.7 (2) | C2—N3—C3—N2 | 1.4 (8) |
N10i—Ag1—Ag2—N9 | −119.1 (2) | N4—N3—C3—N2 | 178.3 (7) |
N1—Ag1—Ag2—N13 | 78.8 (5) | C2—N3—C3—C4 | −179.4 (8) |
N5—Ag1—Ag2—N13 | −45.2 (5) | N4—N3—C3—C4 | −2.5 (13) |
N10i—Ag1—Ag2—N13 | −165.0 (4) | N7—N5—C6—N6 | −0.4 (8) |
N5—Ag1—N1—C2 | −48.6 (8) | Ag1—N5—C6—N6 | 172.8 (5) |
N10i—Ag1—N1—C2 | 117.3 (7) | N7—N5—C6—C5 | −179.8 (8) |
Ag2—Ag1—N1—C2 | −171.7 (8) | Ag1—N5—C6—C5 | −6.6 (12) |
N5—Ag1—N1—N2 | 118.5 (5) | C7—N6—C6—N5 | 0.1 (8) |
N10i—Ag1—N1—N2 | −75.6 (5) | N8—N6—C6—N5 | −179.0 (6) |
Ag2—Ag1—N1—N2 | −4.6 (4) | C7—N6—C6—C5 | 179.5 (8) |
C2—N1—N2—C3 | 1.0 (8) | N8—N6—C6—C5 | 0.5 (12) |
Ag1—N1—N2—C3 | −169.4 (5) | N5—N7—C7—N6 | −0.6 (8) |
C2—N1—N2—Ag2 | 177.3 (5) | Ag2i—N7—C7—N6 | −174.9 (4) |
Ag1—N1—N2—Ag2 | 6.8 (6) | N5—N7—C7—C8 | 179.2 (9) |
N7i—Ag2—N2—C3 | −101.9 (7) | Ag2i—N7—C7—C8 | 4.9 (12) |
N9—Ag2—N2—C3 | 125.4 (7) | C6—N6—C7—N7 | 0.3 (8) |
N13—Ag2—N2—C3 | 27.9 (8) | N8—N6—C7—N7 | 179.3 (7) |
Ag1—Ag2—N2—C3 | 170.3 (8) | C6—N6—C7—C8 | −179.5 (9) |
N7i—Ag2—N2—N1 | 83.2 (5) | N8—N6—C7—C8 | −0.5 (12) |
N9—Ag2—N2—N1 | −49.4 (5) | N9—N10—C10—N11 | −0.5 (7) |
N13—Ag2—N2—N1 | −146.9 (5) | Ag1i—N10—C10—N11 | 176.2 (4) |
Ag1—Ag2—N2—N1 | −4.5 (4) | N9—N10—C10—C9 | 179.7 (8) |
N1—Ag1—N5—C6 | 4.8 (8) | Ag1i—N10—C10—C9 | −3.5 (12) |
N10i—Ag1—N5—C6 | −160.3 (6) | C11—N11—C10—N10 | −0.4 (7) |
Ag2—Ag1—N5—C6 | 94.9 (6) | N12—N11—C10—N10 | −175.7 (6) |
N1—Ag1—N5—N7 | 177.3 (4) | C11—N11—C10—C9 | 179.4 (8) |
N10i—Ag1—N5—N7 | 12.2 (6) | N12—N11—C10—C9 | 4.1 (11) |
Ag2—Ag1—N5—N7 | −92.6 (5) | N10—N9—C11—N11 | −1.5 (8) |
C6—N5—N7—C7 | 0.6 (8) | Ag2—N9—C11—N11 | −160.3 (5) |
Ag1—N5—N7—C7 | −173.4 (5) | N10—N9—C11—C12 | 177.7 (7) |
C6—N5—N7—Ag2i | 175.2 (5) | Ag2—N9—C11—C12 | 18.8 (11) |
Ag1—N5—N7—Ag2i | 1.2 (7) | C10—N11—C11—N9 | 1.2 (7) |
N7i—Ag2—N9—C11 | 158.4 (6) | N12—N11—C11—N9 | 176.9 (6) |
N2—Ag2—N9—C11 | −59.5 (6) | C10—N11—C11—C12 | −178.0 (7) |
N13—Ag2—N9—C11 | 44.1 (7) | N12—N11—C11—C12 | −2.4 (11) |
Ag1—Ag2—N9—C11 | −109.6 (6) | O3—S1—C15—F3 | −179.1 (8) |
N7i—Ag2—N9—N10 | 1.8 (6) | O1—S1—C15—F3 | −57.3 (8) |
N2—Ag2—N9—N10 | 144.0 (5) | O2—S1—C15—F3 | 60.8 (8) |
N13—Ag2—N9—N10 | −112.5 (5) | O3—S1—C15—F1 | 61.2 (8) |
Ag1—Ag2—N9—N10 | 93.8 (5) | O1—S1—C15—F1 | −177.0 (7) |
C11—N9—N10—C10 | 1.2 (8) | O2—S1—C15—F1 | −58.9 (8) |
Ag2—N9—N10—C10 | 162.1 (5) | O3—S1—C15—F2 | −58.8 (8) |
C11—N9—N10—Ag1i | −175.9 (4) | O1—S1—C15—F2 | 63.0 (8) |
Ag2—N9—N10—Ag1i | −15.0 (6) | O2—S1—C15—F2 | −178.9 (7) |
N7i—Ag2—N13—C13 | −156 (2) | O6—S2—C16—F5 | 60.0 (7) |
N2—Ag2—N13—C13 | 62 (2) | O4—S2—C16—F5 | −179.9 (6) |
N9—Ag2—N13—C13 | −37 (2) | O5—S2—C16—F5 | −59.9 (7) |
Ag1—Ag2—N13—C13 | 0 (2) | O6—S2—C16—F4 | −59.8 (7) |
N2—N1—C2—N3 | −0.2 (8) | O4—S2—C16—F4 | 60.4 (7) |
Ag1—N1—C2—N3 | 167.7 (5) | O5—S2—C16—F4 | −179.7 (6) |
N2—N1—C2—C1 | 177.5 (8) | O6—S2—C16—F6 | 179.9 (6) |
Ag1—N1—C2—C1 | −14.6 (13) | O4—S2—C16—F6 | −60.0 (7) |
C3—N3—C2—N1 | −0.7 (8) | O5—S2—C16—F6 | 60.0 (7) |
Symmetry code: (i) −x+2, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Ag4(C4H8N4)6(C2H3N)2](CF3O3S)4·2C2H3N |
Mr | 1864.84 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 295 |
a, b, c (Å) | 12.110 (3), 12.695 (3), 13.001 (3) |
α, β, γ (°) | 108.59 (2), 92.84 (2), 108.68 (2) |
V (Å3) | 1768.9 (7) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.31 |
Crystal size (mm) | 0.38 × 0.24 × 0.18 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID IP |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.294, 0.790 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 17453, 8026, 5532 |
Rint | 0.046 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.074, 0.239, 1.07 |
No. of reflections | 8026 |
No. of parameters | 440 |
No. of restraints | 150 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 2.27, −1.07 |
Computer programs: RAPID-AUTO (Rigaku, 1998), RAPID-AUTO, CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), publCIF (Westrip, 2007).
Ag1—N1 | 2.232 (5) | Ag2—N7i | 2.241 (5) |
Ag1—N5 | 2.238 (5) | Ag2—N9 | 2.371 (6) |
Ag1—N10i | 2.290 (5) | Ag2—N13 | 2.395 (9) |
Ag2—N2 | 2.267 (6) | ||
N1—Ag1—N5 | 131.8 (2) | N2—Ag2—N13 | 102.6 (3) |
N1—Ag1—N10i | 109.7 (2) | N7i—Ag2—N9 | 114.7 (2) |
N5—Ag1—N10i | 117.2 (2) | N7i—Ag2—N13 | 109.4 (3) |
N2—Ag2—N9 | 97.9 (2) | N9—Ag2—N13 | 95.6 (3) |
N2—Ag2—N7i | 130.8 (2) |
Symmetry code: (i) −x+2, −y+1, −z+1. |
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Silver perchlorate reacts with 4-amino-3,5-dimethyl-1,2,4-triazole in acetonitrile to form [µ2-(C4H8N4)6Ag4] [µ2-(C4H8N4)6(C2H3N)2Ag4] 8[ClO4].2H2O, which features two tetranuclear cluster ions. The N-heterocycles in both each bridges two silver atoms. In acetonitrile-coordinated cluster, there are three-coordinate trigonal planar and four-coordinate tetrahedral silver atoms, with the higher coordination arising from coordination by the water molecules. The solvent-free cluster has only trigonal-planar silver atoms (Wang et al., 2006).
The synthesis when with silver trifluoromethylsulfonate in acetonitrile led to the isolation of the acetonitrile-coordinated tetranuclear cluster [µ2-(C4H8N4)6(C2H3N)2Ag4]4+, whose charge is balanced by four trifluoromethylsulfonate ions. The N-heterocycles bridge two silver atoms, and two of the silver atoms are also coordinated by acetonitrile. The salt crystallizes as an acetonitrile disolvate. The N-heterocycle each bridges to two silver atoms, and two of the silver atoms are also coordinated by acetonitrile.