Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807043802/sg2189sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807043802/sg2189Isup2.hkl |
CCDC reference: 663594
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.011 Å
- Disorder in solvent or counterion
- R factor = 0.053
- wR factor = 0.167
- Data-to-parameter ratio = 13.5
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT432_ALERT_2_B Short Inter X...Y Contact C14 .. O6' .. 2.83 Ang.
Alert level C 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 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C21 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O7 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O8 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O5' PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O6' PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O7' PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C26 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C26' PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C26" PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C25 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C25' PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl2 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for O5 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for O6 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for O8' PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 29.00 Perc. PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O7' PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 11 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 28.40 Deg. O5' -CL2 -O5 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 39.10 Deg. O8' -CL2 -O7 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 0.710 Tmax scaled 0.710 Tmin scaled 0.592 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 494
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 23 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 17 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For related literature, see: Bu et al. (2003); Li et al. (2005); Xie et al. (2004; 2005); Zheng et al. (2003; 2005).
The ligand 1,4-bis(2-pyrimidinylthio)butane (L) was synthesized by simulating a reported procedures [Bu et al., 2003]. The solution of AgClO4.H2O (23 mg, 0.1 mmol) in MeOH was carefully layered on top of a solution of L (28 mg, 0.1 mmol) in toluene in a test-tube. After ten days at room temperature, colorless block single crystals appeared at the boundary between two solvents with a yield of 40%.
H atoms were included in calculated positions and treated in the subsequent refinement as riding atoms, with C—H = 0.93, 0.97 and 0.98 Å and Uiso(H) = 1.2 Ueq(C). One of perchlorate ions and all of solvent chloroform molecuels are disordered. For the disordered perchlorate ion, each one O atom was refined in two positions with a near 1:1 occupation factors ratio. The Cl—O lengths were restrained to 1.44 (1) Å. Additionally, the displacement parameters were restrained to be nearly isotropic. For chloroform molecuels, C and Cl atoms were refined in three positions with a 1:1:1 occupation factors ratio for one, and in two positions with a 3:1 ratio for half one. All of Cl—O lengths were restrained to 1.72 (1) Å and Cl—O distances to 2.81 (1) Å
Some AgI complexes of flexible bis(arylthio)alkyl ligands (aryl = phenyl, benzyl, pyridyl, pyrimidinyl, 4-methyl-2-pyrimidinyl or 5-methyl-1,3,4-thiadiazolyl) have been reported by us and others [Bu et al., 2003; Li et al., 2005; Xie et al., 2004, 2005; Zheng et al., 2003, 2005], which show different structure features. Herein, we report a 1,4-bis(2-pyrimidinylthio)butane(L)—AgI complex, {[Ag2(C12H14N4S2)2].2ClO4.1.5CHCl3}n (I). The crystal structure of the title complex (I) consists of [AgL]n one-dimensional chain cations, ClO4- anions (as shown in Fig. 1) and solvent chloroform molecules. In the cationic chain, there are two crystallographic independent AgI centers (Ag1 and Ag2), both of which adopt near linear coordination geometry coordinated by two pyrimidine N atoms from two crystallographic independent L ligands. Selected bond distances and angles are listed in Table 1. The ligand coordinates to the AgI centers in a N,N'-bidentate bridging mode with two N donors in an anti-conformation, resulting in an infinite corrugated chain with the intra-molecular Ag—Ag separations of 13.089 (5) and 13.228 (5) Å. It is interesting that by the Ag—S weak coordinations (Ag1—S1B = 3.052 (4) and Ag2—S4C = 3.348 (5) Å) such one-dimensional chains are linked to form a two-dimensional supramolecular framework as shown in Fig. 2.
For related literature, see: Bu et al. (2003); Li et al. (2005); Xie et al. (2004; 2005); Zheng et al. (2003; 2005).
Data collection: SMART (Bruker, 1998); cell refinement: SMART (Bruker, 1998); data reduction: SAINT and SHELXTL (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL (Bruker, 1998).
[Ag2(C12H14N4S2)2](ClO4)2·1.5CHCl3 | Z = 1 |
Mr = 2300.95 | F(000) = 1142 |
Triclinic, P1 | Dx = 1.775 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.197 (4) Å | Cell parameters from 883 reflections |
b = 12.394 (4) Å | θ = 3.3–25.5° |
c = 16.897 (6) Å | µ = 1.56 mm−1 |
α = 73.715 (5)° | T = 293 K |
β = 73.060 (6)° | Block, colorless |
γ = 86.618 (6)° | 0.28 × 0.26 × 0.22 mm |
V = 2152.5 (13) Å3 |
Bruker SMART 1000 CCD area-detector diffractometer | 8803 independent reflections |
Radiation source: fine-focus sealed tube | 4653 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
φ and ω scan | θmax = 26.5°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −14→7 |
Tmin = 0.834, Tmax = 1.000 | k = −15→14 |
12535 measured reflections | l = −20→21 |
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)] = 0.053 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.167 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0759P)2 + 1.7172P] where P = (Fo2 + 2Fc2)/3 |
8803 reflections | (Δ/σ)max < 0.001 |
652 parameters | Δρmax = 0.74 e Å−3 |
494 restraints | Δρmin = −0.44 e Å−3 |
[Ag2(C12H14N4S2)2](ClO4)2·1.5CHCl3 | γ = 86.618 (6)° |
Mr = 2300.95 | V = 2152.5 (13) Å3 |
Triclinic, P1 | Z = 1 |
a = 11.197 (4) Å | Mo Kα radiation |
b = 12.394 (4) Å | µ = 1.56 mm−1 |
c = 16.897 (6) Å | T = 293 K |
α = 73.715 (5)° | 0.28 × 0.26 × 0.22 mm |
β = 73.060 (6)° |
Bruker SMART 1000 CCD area-detector diffractometer | 8803 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | 4653 reflections with I > 2σ(I) |
Tmin = 0.834, Tmax = 1.000 | Rint = 0.023 |
12535 measured reflections |
R[F2 > 2σ(F2)] = 0.053 | 494 restraints |
wR(F2) = 0.167 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.74 e Å−3 |
8803 reflections | Δρmin = −0.44 e Å−3 |
652 parameters |
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 | 0.42920 (6) | −0.16870 (5) | 0.08567 (3) | 0.0729 (2) | |
Ag2 | −0.16104 (6) | 0.47906 (5) | 0.57281 (3) | 0.0785 (2) | |
S1 | 0.33368 (16) | 0.03171 (13) | −0.04970 (10) | 0.0557 (4) | |
S2 | −0.06388 (16) | 0.26616 (15) | −0.29450 (11) | 0.0639 (5) | |
S3 | 0.30282 (17) | 0.00309 (15) | 0.19341 (11) | 0.0657 (5) | |
S4 | −0.03039 (19) | 0.30037 (18) | 0.47281 (13) | 0.0812 (6) | |
N1 | 0.4087 (4) | −0.1739 (4) | −0.0381 (3) | 0.0470 (11) | |
N2 | 0.3745 (5) | −0.0766 (5) | −0.1712 (3) | 0.0623 (14) | |
N3 | −0.1815 (5) | 0.4539 (4) | −0.2911 (3) | 0.0578 (13) | |
N4 | −0.1477 (5) | 0.3492 (5) | −0.1600 (3) | 0.0661 (15) | |
N5 | 0.3957 (4) | −0.1960 (4) | 0.2249 (3) | 0.0506 (12) | |
N6 | 0.3364 (5) | −0.1174 (5) | 0.3424 (3) | 0.0678 (15) | |
N7 | −0.1665 (5) | 0.4764 (4) | 0.4460 (3) | 0.0569 (13) | |
N8 | −0.1288 (6) | 0.3764 (6) | 0.3418 (4) | 0.092 (2) | |
C1 | 0.4380 (6) | −0.2656 (5) | −0.0663 (4) | 0.0578 (16) | |
H1 | 0.4620 | −0.3295 | −0.0306 | 0.069* | |
C2 | 0.4338 (7) | −0.2683 (6) | −0.1456 (4) | 0.0695 (19) | |
H2 | 0.4505 | −0.3332 | −0.1640 | 0.083* | |
C3 | 0.4035 (7) | −0.1699 (6) | −0.1966 (4) | 0.071 (2) | |
H3 | 0.4033 | −0.1680 | −0.2520 | 0.085* | |
C4 | 0.3755 (5) | −0.0837 (5) | −0.0925 (4) | 0.0468 (14) | |
C5 | 0.2764 (6) | 0.1281 (5) | −0.1320 (4) | 0.0593 (17) | |
H5A | 0.2736 | 0.2025 | −0.1234 | 0.071* | |
H5B | 0.3355 | 0.1318 | −0.1876 | 0.071* | |
C6 | 0.1485 (6) | 0.0977 (5) | −0.1340 (4) | 0.0560 (16) | |
H6A | 0.0898 | 0.0860 | −0.0771 | 0.067* | |
H6B | 0.1524 | 0.0285 | −0.1506 | 0.067* | |
C7 | 0.1041 (6) | 0.1919 (5) | −0.1980 (4) | 0.0579 (16) | |
H7A | 0.0925 | 0.2588 | −0.1778 | 0.069* | |
H7B | 0.1681 | 0.2093 | −0.2530 | 0.069* | |
C8 | −0.0167 (6) | 0.1621 (5) | −0.2106 (4) | 0.0626 (17) | |
H8A | −0.0824 | 0.1525 | −0.1568 | 0.075* | |
H8B | −0.0076 | 0.0907 | −0.2245 | 0.075* | |
C9 | −0.1360 (6) | 0.3644 (5) | −0.2418 (4) | 0.0516 (15) | |
C10 | −0.2405 (7) | 0.5294 (6) | −0.2526 (5) | 0.076 (2) | |
H10 | −0.2724 | 0.5917 | −0.2849 | 0.091* | |
C11 | −0.2563 (8) | 0.5199 (6) | −0.1689 (5) | 0.084 (2) | |
H11 | −0.2990 | 0.5733 | −0.1428 | 0.101* | |
C12 | −0.2065 (7) | 0.4279 (7) | −0.1241 (5) | 0.081 (2) | |
H12 | −0.2140 | 0.4200 | −0.0665 | 0.097* | |
C13 | 0.4284 (6) | −0.2900 (6) | 0.2747 (4) | 0.0578 (16) | |
H13 | 0.4594 | −0.3490 | 0.2512 | 0.069* | |
C14 | 0.4171 (6) | −0.3015 (6) | 0.3597 (4) | 0.0686 (19) | |
H14 | 0.4403 | −0.3667 | 0.3945 | 0.082* | |
C15 | 0.3699 (7) | −0.2118 (7) | 0.3907 (5) | 0.080 (2) | |
H15 | 0.3610 | −0.2174 | 0.4482 | 0.096* | |
C16 | 0.3492 (5) | −0.1141 (5) | 0.2626 (4) | 0.0523 (15) | |
C17 | 0.2660 (6) | 0.1047 (6) | 0.2555 (5) | 0.0723 (19) | |
H17A | 0.3298 | 0.1024 | 0.2843 | 0.087* | |
H17B | 0.2697 | 0.1792 | 0.2161 | 0.087* | |
C18 | 0.1413 (6) | 0.0876 (6) | 0.3214 (5) | 0.073 (2) | |
H18A | 0.1416 | 0.0210 | 0.3682 | 0.087* | |
H18B | 0.0773 | 0.0773 | 0.2959 | 0.087* | |
C19 | 0.1135 (7) | 0.1928 (7) | 0.3564 (5) | 0.079 (2) | |
H19A | 0.1816 | 0.2050 | 0.3779 | 0.095* | |
H19B | 0.1109 | 0.2581 | 0.3091 | 0.095* | |
C20 | −0.0037 (8) | 0.1840 (7) | 0.4250 (6) | 0.094 (3) | |
H20A | −0.0043 | 0.1149 | 0.4698 | 0.113* | |
H20B | −0.0723 | 0.1788 | 0.4019 | 0.113* | |
C21 | −0.1173 (6) | 0.3937 (6) | 0.4123 (4) | 0.0617 (17) | |
C22 | −0.2316 (7) | 0.5505 (6) | 0.4029 (4) | 0.0705 (19) | |
H22 | −0.2652 | 0.6111 | 0.4236 | 0.085* | |
C23 | −0.2506 (7) | 0.5406 (7) | 0.3290 (5) | 0.080 (2) | |
H23 | −0.2977 | 0.5920 | 0.2998 | 0.096* | |
C24 | −0.1982 (8) | 0.4534 (8) | 0.3005 (5) | 0.095 (3) | |
H24 | −0.2097 | 0.4450 | 0.2502 | 0.114* | |
Cl1 | 0.6523 (2) | 0.60581 (16) | 0.06711 (13) | 0.0779 (5) | |
O1 | 0.6813 (9) | 0.7093 (7) | 0.0011 (6) | 0.177 (4) | |
O2 | 0.7267 (9) | 0.5929 (7) | 0.1195 (6) | 0.184 (4) | |
O3 | 0.6527 (11) | 0.5225 (6) | 0.0323 (6) | 0.200 (5) | |
O4 | 0.5317 (8) | 0.6208 (9) | 0.1100 (5) | 0.192 (4) | |
Cl2 | 0.4539 (2) | 0.34556 (17) | 0.39794 (12) | 0.0774 (5) | |
O5 | 0.3219 (6) | 0.3444 (10) | 0.4326 (7) | 0.094 (4) | 0.667 (14) |
O6 | 0.4963 (10) | 0.4271 (9) | 0.3167 (5) | 0.112 (5) | 0.667 (14) |
O7 | 0.5051 (12) | 0.3800 (14) | 0.4553 (6) | 0.167 (7) | 0.667 (14) |
O8 | 0.4962 (14) | 0.2406 (7) | 0.3917 (10) | 0.215 (9) | 0.667 (14) |
O5' | 0.3346 (15) | 0.292 (2) | 0.4241 (19) | 0.214 (19) | 0.333 (14) |
O6' | 0.438 (2) | 0.4639 (9) | 0.3833 (18) | 0.152 (10) | 0.333 (14) |
O7' | 0.525 (2) | 0.325 (3) | 0.3191 (11) | 0.237 (16) | 0.333 (14) |
O8' | 0.518 (2) | 0.3029 (17) | 0.4592 (13) | 0.134 (10) | 0.333 (14) |
C25 | 0.2886 (11) | 0.0715 (10) | 0.5631 (9) | 0.055 (5) | 0.422 (11) |
H25 | 0.3190 | 0.1255 | 0.5063 | 0.066* | 0.422 (11) |
Cl3 | 0.1298 (9) | 0.0784 (11) | 0.6004 (10) | 0.153 (5) | 0.422 (11) |
Cl4 | 0.3558 (12) | 0.1004 (13) | 0.6321 (10) | 0.169 (5) | 0.422 (11) |
Cl5 | 0.3221 (11) | −0.0635 (12) | 0.5547 (14) | 0.240 (8) | 0.422 (11) |
C25' | 0.2522 (15) | 0.0247 (15) | 0.5881 (9) | 0.109 (11) | 0.328 (11) |
H25' | 0.2008 | −0.0428 | 0.6227 | 0.131* | 0.328 (11) |
Cl3' | 0.1541 (12) | 0.1336 (15) | 0.5820 (9) | 0.128 (6) | 0.328 (11) |
Cl4' | 0.3563 (16) | 0.0365 (14) | 0.6398 (10) | 0.146 (5) | 0.328 (11) |
Cl5' | 0.3181 (10) | 0.0060 (9) | 0.4887 (6) | 0.116 (4) | 0.328 (11) |
C26 | 0.0137 (18) | 0.7237 (10) | 0.9183 (10) | 0.069 (7) | 0.283 (5) |
H26 | −0.0765 | 0.7169 | 0.9461 | 0.083* | 0.283 (5) |
Cl6 | 0.0834 (17) | 0.7822 (11) | 0.9757 (8) | 0.075 (4) | 0.283 (5) |
Cl7 | 0.0710 (13) | 0.5926 (8) | 0.9178 (7) | 0.130 (4) | 0.283 (5) |
Cl8 | 0.041 (2) | 0.8061 (12) | 0.8154 (9) | 0.166 (8) | 0.283 (5) |
C26' | −0.0228 (17) | 0.7372 (12) | 0.9237 (9) | 0.072 (7) | 0.317 (5) |
H26' | −0.0895 | 0.6816 | 0.9594 | 0.086* | 0.317 (5) |
Cl6' | 0.081 (2) | 0.7375 (16) | 0.9808 (12) | 0.120 (6) | 0.317 (5) |
Cl7' | 0.0455 (14) | 0.7020 (13) | 0.8312 (7) | 0.175 (6) | 0.317 (5) |
Cl8' | −0.0879 (7) | 0.8663 (5) | 0.9019 (4) | 0.096 (3) | 0.317 (5) |
Cl6" | −0.019 (3) | 0.616 (2) | 0.897 (2) | 0.191 (12) | 0.15 |
Cl7" | 0.108 (2) | 0.818 (3) | 0.7986 (16) | 0.123 (9) | 0.15 |
Cl8" | 0.028 (2) | 0.770 (3) | 0.9793 (17) | 0.103 (9) | 0.15 |
C26" | 0.084 (2) | 0.715 (2) | 0.8939 (15) | 0.106 (12) | 0.15 |
H26" | 0.1639 | 0.6790 | 0.8968 | 0.128* | 0.15 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ag1 | 0.1018 (5) | 0.0786 (4) | 0.0495 (3) | 0.0385 (3) | −0.0379 (3) | −0.0256 (3) |
Ag2 | 0.0922 (4) | 0.0976 (5) | 0.0553 (3) | 0.0323 (3) | −0.0377 (3) | −0.0253 (3) |
S1 | 0.0675 (11) | 0.0551 (9) | 0.0569 (9) | 0.0170 (8) | −0.0354 (8) | −0.0198 (8) |
S2 | 0.0710 (11) | 0.0731 (11) | 0.0608 (10) | 0.0258 (9) | −0.0383 (9) | −0.0239 (9) |
S3 | 0.0695 (11) | 0.0720 (11) | 0.0593 (10) | 0.0208 (9) | −0.0230 (8) | −0.0230 (9) |
S4 | 0.0862 (14) | 0.0928 (14) | 0.0760 (13) | 0.0394 (11) | −0.0336 (10) | −0.0379 (11) |
N1 | 0.059 (3) | 0.043 (3) | 0.045 (3) | 0.009 (2) | −0.023 (2) | −0.013 (2) |
N2 | 0.075 (4) | 0.075 (4) | 0.049 (3) | 0.023 (3) | −0.033 (3) | −0.024 (3) |
N3 | 0.075 (4) | 0.053 (3) | 0.057 (3) | 0.013 (3) | −0.036 (3) | −0.016 (3) |
N4 | 0.079 (4) | 0.073 (4) | 0.049 (3) | 0.021 (3) | −0.029 (3) | −0.014 (3) |
N5 | 0.047 (3) | 0.062 (3) | 0.045 (3) | 0.009 (2) | −0.018 (2) | −0.015 (2) |
N6 | 0.076 (4) | 0.086 (4) | 0.051 (3) | 0.015 (3) | −0.030 (3) | −0.024 (3) |
N7 | 0.058 (3) | 0.063 (3) | 0.050 (3) | 0.012 (3) | −0.019 (2) | −0.016 (3) |
N8 | 0.096 (5) | 0.124 (6) | 0.087 (5) | 0.037 (4) | −0.048 (4) | −0.062 (4) |
C1 | 0.070 (4) | 0.056 (4) | 0.054 (4) | 0.014 (3) | −0.026 (3) | −0.018 (3) |
C2 | 0.075 (5) | 0.073 (5) | 0.073 (5) | 0.019 (4) | −0.026 (4) | −0.040 (4) |
C3 | 0.084 (5) | 0.087 (5) | 0.053 (4) | 0.021 (4) | −0.029 (4) | −0.031 (4) |
C4 | 0.047 (3) | 0.051 (3) | 0.047 (3) | 0.008 (3) | −0.021 (3) | −0.014 (3) |
C5 | 0.069 (4) | 0.048 (4) | 0.068 (4) | 0.010 (3) | −0.038 (3) | −0.009 (3) |
C6 | 0.058 (4) | 0.051 (4) | 0.064 (4) | 0.008 (3) | −0.031 (3) | −0.011 (3) |
C7 | 0.062 (4) | 0.051 (4) | 0.067 (4) | 0.013 (3) | −0.033 (3) | −0.014 (3) |
C8 | 0.067 (4) | 0.058 (4) | 0.072 (4) | 0.016 (3) | −0.038 (4) | −0.016 (3) |
C9 | 0.051 (4) | 0.053 (4) | 0.053 (4) | 0.003 (3) | −0.026 (3) | −0.008 (3) |
C10 | 0.101 (6) | 0.065 (5) | 0.079 (5) | 0.017 (4) | −0.055 (5) | −0.021 (4) |
C11 | 0.117 (7) | 0.078 (5) | 0.080 (5) | 0.039 (5) | −0.052 (5) | −0.039 (4) |
C12 | 0.100 (6) | 0.093 (6) | 0.054 (4) | 0.020 (5) | −0.033 (4) | −0.019 (4) |
C13 | 0.053 (4) | 0.064 (4) | 0.054 (4) | 0.004 (3) | −0.015 (3) | −0.015 (3) |
C14 | 0.072 (5) | 0.078 (5) | 0.055 (4) | 0.012 (4) | −0.027 (3) | −0.010 (4) |
C15 | 0.088 (6) | 0.110 (7) | 0.049 (4) | 0.011 (5) | −0.024 (4) | −0.029 (4) |
C16 | 0.045 (4) | 0.064 (4) | 0.051 (4) | 0.005 (3) | −0.015 (3) | −0.019 (3) |
C17 | 0.063 (5) | 0.077 (5) | 0.081 (5) | 0.011 (4) | −0.017 (4) | −0.033 (4) |
C18 | 0.063 (5) | 0.080 (5) | 0.078 (5) | 0.010 (4) | −0.016 (4) | −0.032 (4) |
C19 | 0.074 (5) | 0.095 (6) | 0.070 (5) | 0.008 (4) | −0.018 (4) | −0.027 (4) |
C20 | 0.085 (6) | 0.082 (6) | 0.106 (7) | 0.014 (5) | −0.006 (5) | −0.035 (5) |
C21 | 0.049 (4) | 0.083 (5) | 0.056 (4) | 0.010 (3) | −0.014 (3) | −0.028 (4) |
C22 | 0.082 (5) | 0.070 (5) | 0.064 (4) | 0.018 (4) | −0.033 (4) | −0.018 (4) |
C23 | 0.087 (6) | 0.087 (6) | 0.070 (5) | 0.007 (5) | −0.039 (4) | −0.011 (4) |
C24 | 0.104 (7) | 0.131 (8) | 0.078 (6) | 0.027 (6) | −0.052 (5) | −0.049 (5) |
Cl1 | 0.1006 (15) | 0.0713 (12) | 0.0836 (13) | 0.0258 (11) | −0.0431 (12) | −0.0431 (11) |
O1 | 0.219 (9) | 0.123 (6) | 0.202 (9) | −0.044 (6) | −0.141 (8) | 0.031 (6) |
O2 | 0.260 (11) | 0.137 (6) | 0.210 (9) | 0.036 (7) | −0.186 (9) | −0.015 (6) |
O3 | 0.373 (14) | 0.105 (5) | 0.167 (8) | 0.045 (7) | −0.098 (9) | −0.097 (6) |
O4 | 0.171 (8) | 0.297 (12) | 0.091 (5) | 0.111 (8) | −0.031 (5) | −0.054 (6) |
Cl2 | 0.0968 (15) | 0.0741 (13) | 0.0672 (12) | 0.0153 (11) | −0.0386 (11) | −0.0156 (10) |
O5 | 0.081 (7) | 0.116 (10) | 0.085 (7) | 0.032 (6) | −0.017 (5) | −0.039 (6) |
O6 | 0.143 (9) | 0.102 (8) | 0.080 (7) | −0.014 (7) | −0.054 (6) | 0.020 (6) |
O7 | 0.153 (11) | 0.258 (19) | 0.084 (8) | −0.054 (12) | −0.074 (7) | 0.013 (10) |
O8 | 0.286 (18) | 0.105 (9) | 0.156 (14) | 0.063 (10) | 0.059 (12) | −0.023 (9) |
O5' | 0.25 (3) | 0.12 (2) | 0.30 (4) | −0.08 (2) | −0.22 (3) | 0.07 (2) |
O6' | 0.21 (2) | 0.091 (15) | 0.18 (2) | 0.056 (15) | −0.074 (19) | −0.058 (15) |
O7' | 0.38 (4) | 0.27 (4) | 0.10 (2) | 0.13 (3) | −0.10 (2) | −0.12 (2) |
O8' | 0.19 (2) | 0.098 (16) | 0.146 (19) | 0.057 (16) | −0.128 (17) | −0.007 (14) |
C25 | 0.082 (12) | 0.038 (9) | 0.059 (10) | 0.013 (8) | −0.042 (9) | −0.017 (7) |
Cl3 | 0.121 (8) | 0.157 (10) | 0.181 (12) | −0.005 (6) | −0.026 (6) | −0.066 (8) |
Cl4 | 0.147 (8) | 0.201 (14) | 0.189 (11) | 0.049 (9) | −0.061 (7) | −0.097 (10) |
Cl5 | 0.188 (10) | 0.206 (13) | 0.36 (2) | 0.014 (9) | −0.034 (12) | −0.183 (15) |
C25' | 0.090 (18) | 0.13 (2) | 0.092 (18) | 0.015 (17) | −0.013 (15) | −0.022 (17) |
Cl3' | 0.086 (7) | 0.208 (15) | 0.093 (7) | 0.054 (8) | −0.030 (5) | −0.053 (9) |
Cl4' | 0.176 (11) | 0.161 (13) | 0.137 (8) | 0.050 (10) | −0.102 (8) | −0.047 (9) |
Cl5' | 0.129 (7) | 0.106 (7) | 0.130 (8) | 0.033 (5) | −0.045 (6) | −0.057 (6) |
C26 | 0.042 (15) | 0.093 (15) | 0.091 (15) | 0.031 (12) | −0.028 (11) | −0.049 (13) |
Cl6 | 0.072 (8) | 0.092 (8) | 0.070 (5) | 0.006 (7) | −0.035 (6) | −0.022 (5) |
Cl7 | 0.160 (10) | 0.104 (7) | 0.139 (9) | 0.040 (7) | −0.043 (8) | −0.060 (6) |
Cl8 | 0.26 (2) | 0.143 (12) | 0.129 (11) | −0.003 (13) | −0.142 (14) | −0.001 (9) |
C26' | 0.048 (13) | 0.101 (14) | 0.083 (13) | 0.050 (11) | −0.034 (10) | −0.045 (12) |
Cl6' | 0.144 (11) | 0.127 (12) | 0.132 (9) | 0.073 (9) | −0.099 (9) | −0.055 (8) |
Cl7' | 0.245 (14) | 0.205 (13) | 0.111 (8) | 0.104 (12) | −0.071 (8) | −0.100 (9) |
Cl8' | 0.114 (6) | 0.089 (5) | 0.085 (5) | 0.028 (4) | −0.045 (4) | −0.013 (4) |
Cl6" | 0.17 (2) | 0.22 (2) | 0.18 (2) | −0.085 (19) | 0.005 (19) | −0.08 (2) |
Cl7" | 0.117 (16) | 0.16 (2) | 0.106 (14) | −0.044 (14) | −0.066 (12) | −0.018 (13) |
Cl8" | 0.079 (15) | 0.137 (19) | 0.131 (16) | 0.023 (13) | −0.047 (13) | −0.081 (15) |
C26" | 0.12 (2) | 0.108 (19) | 0.105 (19) | 0.007 (19) | −0.038 (18) | −0.046 (18) |
Ag1—N1 | 2.188 (4) | C14—C15 | 1.373 (10) |
Ag1—N5 | 2.201 (5) | C14—H14 | 0.9300 |
Ag2—N7 | 2.171 (5) | C15—H15 | 0.9300 |
Ag2—N3i | 2.177 (5) | C17—C18 | 1.493 (9) |
S1—C4 | 1.758 (6) | C17—H17A | 0.9700 |
S1—C5 | 1.808 (6) | C17—H17B | 0.9700 |
S2—C9 | 1.732 (6) | C18—C19 | 1.556 (10) |
S2—C8 | 1.812 (6) | C18—H18A | 0.9700 |
S3—C16 | 1.749 (6) | C18—H18B | 0.9700 |
S3—C17 | 1.812 (7) | C19—C20 | 1.462 (10) |
S4—C21 | 1.764 (7) | C19—H19A | 0.9700 |
S4—C20 | 1.812 (8) | C19—H19B | 0.9700 |
N1—C1 | 1.339 (7) | C20—H20A | 0.9700 |
N1—C4 | 1.344 (7) | C20—H20B | 0.9700 |
N2—C4 | 1.312 (7) | C22—C23 | 1.364 (9) |
N2—C3 | 1.335 (8) | C22—H22 | 0.9300 |
N3—C10 | 1.324 (9) | C23—C24 | 1.341 (11) |
N3—C9 | 1.359 (7) | C23—H23 | 0.9300 |
N3—Ag2ii | 2.177 (5) | C24—H24 | 0.9300 |
N4—C9 | 1.310 (7) | Cl1—O3 | 1.323 (6) |
N4—C12 | 1.333 (9) | Cl1—O2 | 1.356 (7) |
N5—C13 | 1.333 (7) | Cl1—O4 | 1.363 (8) |
N5—C16 | 1.347 (7) | Cl1—O1 | 1.424 (7) |
N6—C16 | 1.303 (7) | Cl2—O8 | 1.380 (7) |
N6—C15 | 1.330 (9) | Cl2—O8' | 1.398 (9) |
N7—C21 | 1.324 (8) | Cl2—O5' | 1.419 (10) |
N7—C22 | 1.327 (8) | Cl2—O5 | 1.422 (7) |
N8—C21 | 1.312 (8) | Cl2—O7' | 1.424 (9) |
N8—C24 | 1.361 (10) | Cl2—O6 | 1.425 (6) |
C1—C2 | 1.366 (8) | Cl2—O7 | 1.427 (8) |
C1—H1 | 0.9300 | Cl2—O6' | 1.427 (9) |
C2—C3 | 1.370 (9) | C25—Cl4 | 1.684 (9) |
C2—H2 | 0.9300 | C25—Cl3 | 1.710 (9) |
C3—H3 | 0.9300 | C25—Cl5 | 1.728 (9) |
C5—C6 | 1.515 (8) | C25—H25 | 0.9800 |
C5—H5A | 0.9700 | C25'—Cl4' | 1.682 (10) |
C5—H5B | 0.9700 | C25'—Cl3' | 1.688 (10) |
C6—C7 | 1.522 (8) | C25'—Cl5' | 1.701 (10) |
C6—H6A | 0.9700 | C25'—H25' | 0.9800 |
C6—H6B | 0.9700 | C26—Cl8 | 1.701 (10) |
C7—C8 | 1.511 (8) | C26—Cl7 | 1.713 (10) |
C7—H7A | 0.9700 | C26—Cl6 | 1.724 (10) |
C7—H7B | 0.9700 | C26—H26 | 0.9800 |
C8—H8A | 0.9700 | C26'—Cl7' | 1.692 (10) |
C8—H8B | 0.9700 | C26'—Cl8' | 1.708 (10) |
C10—C11 | 1.345 (9) | C26'—Cl6' | 1.717 (10) |
C10—H10 | 0.9300 | C26'—H26' | 0.9800 |
C11—C12 | 1.368 (9) | Cl6"—C26" | 1.709 (10) |
C11—H11 | 0.9300 | Cl7"—C26" | 1.714 (10) |
C12—H12 | 0.9300 | Cl8"—C26" | 1.713 (10) |
C13—C14 | 1.372 (8) | C26"—H26" | 0.9800 |
C13—H13 | 0.9300 | ||
N1—Ag1—N5 | 161.96 (18) | C17—C18—H18B | 110.0 |
N7—Ag2—N3i | 168.73 (19) | C19—C18—H18B | 110.0 |
C4—S1—C5 | 101.9 (3) | H18A—C18—H18B | 108.3 |
C9—S2—C8 | 102.3 (3) | C20—C19—C18 | 114.0 (7) |
C16—S3—C17 | 103.4 (3) | C20—C19—H19A | 108.7 |
C21—S4—C20 | 103.4 (4) | C18—C19—H19A | 108.7 |
C1—N1—C4 | 116.4 (5) | C20—C19—H19B | 108.7 |
C1—N1—Ag1 | 121.1 (4) | C18—C19—H19B | 108.7 |
C4—N1—Ag1 | 122.3 (4) | H19A—C19—H19B | 107.6 |
C4—N2—C3 | 115.9 (5) | C19—C20—S4 | 114.4 (6) |
C10—N3—C9 | 116.8 (5) | C19—C20—H20A | 108.7 |
C10—N3—Ag2ii | 119.4 (4) | S4—C20—H20A | 108.7 |
C9—N3—Ag2ii | 123.8 (4) | C19—C20—H20B | 108.7 |
C9—N4—C12 | 117.2 (6) | S4—C20—H20B | 108.7 |
C13—N5—C16 | 116.8 (5) | H20A—C20—H20B | 107.6 |
C13—N5—Ag1 | 122.2 (4) | N8—C21—N7 | 126.5 (6) |
C16—N5—Ag1 | 120.9 (4) | N8—C21—S4 | 119.8 (5) |
C16—N6—C15 | 116.2 (6) | N7—C21—S4 | 113.7 (5) |
C21—N7—C22 | 116.7 (6) | N7—C22—C23 | 122.0 (7) |
C21—N7—Ag2 | 121.6 (4) | N7—C22—H22 | 119.0 |
C22—N7—Ag2 | 121.3 (4) | C23—C22—H22 | 119.0 |
C21—N8—C24 | 114.8 (7) | C24—C23—C22 | 116.9 (7) |
N1—C1—C2 | 122.2 (6) | C24—C23—H23 | 121.5 |
N1—C1—H1 | 118.9 | C22—C23—H23 | 121.5 |
C2—C1—H1 | 118.9 | C23—C24—N8 | 123.1 (7) |
C1—C2—C3 | 116.0 (6) | C23—C24—H24 | 118.5 |
C1—C2—H2 | 122.0 | N8—C24—H24 | 118.5 |
C3—C2—H2 | 122.0 | O3—Cl1—O2 | 115.5 (6) |
N2—C3—C2 | 123.6 (6) | O3—Cl1—O4 | 107.7 (7) |
N2—C3—H3 | 118.2 | O2—Cl1—O4 | 110.6 (6) |
C2—C3—H3 | 118.2 | O3—Cl1—O1 | 109.6 (6) |
N2—C4—N1 | 125.8 (5) | O2—Cl1—O1 | 110.6 (5) |
N2—C4—S1 | 120.5 (4) | O4—Cl1—O1 | 101.8 (6) |
N1—C4—S1 | 113.7 (4) | O8—Cl2—O8' | 71.6 (10) |
C6—C5—S1 | 114.9 (4) | O8—Cl2—O5' | 83.4 (14) |
C6—C5—H5A | 108.5 | O8'—Cl2—O5' | 111.0 (9) |
S1—C5—H5A | 108.5 | O8—Cl2—O5 | 111.4 (7) |
C6—C5—H5B | 108.5 | O8'—Cl2—O5 | 114.4 (13) |
S1—C5—H5B | 108.5 | O5'—Cl2—O5 | 28.4 (13) |
H5A—C5—H5B | 107.5 | O8—Cl2—O7' | 56.9 (12) |
C5—C6—C7 | 109.8 (5) | O8'—Cl2—O7' | 108.1 (9) |
C5—C6—H6A | 109.7 | O5'—Cl2—O7' | 109.1 (10) |
C7—C6—H6A | 109.7 | O5—Cl2—O7' | 128.6 (14) |
C5—C6—H6B | 109.7 | O8—Cl2—O6 | 110.4 (6) |
C7—C6—H6B | 109.7 | O8'—Cl2—O6 | 128.3 (11) |
H6A—C6—H6B | 108.2 | O5'—Cl2—O6 | 120.7 (11) |
C8—C7—C6 | 112.7 (5) | O5—Cl2—O6 | 112.2 (6) |
C8—C7—H7A | 109.0 | O7'—Cl2—O6 | 53.5 (11) |
C6—C7—H7A | 109.0 | O8—Cl2—O7 | 109.8 (7) |
C8—C7—H7B | 109.0 | O8'—Cl2—O7 | 39.1 (8) |
C6—C7—H7B | 109.0 | O5'—Cl2—O7 | 123.1 (15) |
H7A—C7—H7B | 107.8 | O5—Cl2—O7 | 106.6 (6) |
C7—C8—S2 | 113.9 (5) | O7'—Cl2—O7 | 124.7 (14) |
C7—C8—H8A | 108.8 | O6—Cl2—O7 | 106.2 (6) |
S2—C8—H8A | 108.8 | O8—Cl2—O6' | 164.1 (12) |
C7—C8—H8B | 108.8 | O8'—Cl2—O6' | 111.6 (9) |
S2—C8—H8B | 108.8 | O5'—Cl2—O6' | 108.7 (9) |
H8A—C8—H8B | 107.7 | O5—Cl2—O6' | 81.9 (11) |
N4—C9—N3 | 124.0 (6) | O7'—Cl2—O6' | 108.3 (10) |
N4—C9—S2 | 121.1 (5) | O6—Cl2—O6' | 54.8 (10) |
N3—C9—S2 | 114.8 (4) | O7—Cl2—O6' | 72.7 (9) |
N3—C10—C11 | 122.8 (6) | Cl4—C25—Cl3 | 109.9 (7) |
N3—C10—H10 | 118.6 | Cl4—C25—Cl5 | 110.4 (7) |
C11—C10—H10 | 118.6 | Cl3—C25—Cl5 | 107.3 (7) |
C10—C11—C12 | 116.8 (7) | Cl4—C25—H25 | 109.7 |
C10—C11—H11 | 121.6 | Cl3—C25—H25 | 109.7 |
C12—C11—H11 | 121.6 | Cl5—C25—H25 | 109.7 |
N4—C12—C11 | 122.4 (7) | Cl4'—C25'—Cl3' | 112.3 (8) |
N4—C12—H12 | 118.8 | Cl4'—C25'—Cl5' | 113.8 (9) |
C11—C12—H12 | 118.8 | Cl3'—C25'—Cl5' | 110.2 (8) |
N5—C13—C14 | 121.3 (6) | Cl4'—C25'—H25' | 106.7 |
N5—C13—H13 | 119.3 | Cl3'—C25'—H25' | 106.7 |
C14—C13—H13 | 119.3 | Cl5'—C25'—H25' | 106.7 |
C13—C14—C15 | 116.7 (6) | Cl8—C26—Cl7 | 109.6 (8) |
C13—C14—H14 | 121.7 | Cl8—C26—Cl6 | 110.6 (8) |
C15—C14—H14 | 121.7 | Cl7—C26—Cl6 | 109.8 (8) |
N6—C15—C14 | 123.1 (6) | Cl8—C26—H26 | 108.9 |
N6—C15—H15 | 118.5 | Cl7—C26—H26 | 108.9 |
C14—C15—H15 | 118.5 | Cl6—C26—H26 | 108.9 |
N6—C16—N5 | 126.0 (6) | Cl7'—C26'—Cl8' | 110.1 (8) |
N6—C16—S3 | 120.8 (5) | Cl7'—C26'—Cl6' | 111.8 (8) |
N5—C16—S3 | 113.3 (4) | Cl8'—C26'—Cl6' | 109.7 (8) |
C18—C17—S3 | 115.2 (5) | Cl7'—C26'—H26' | 108.4 |
C18—C17—H17A | 108.5 | Cl8'—C26'—H26' | 108.4 |
S3—C17—H17A | 108.5 | Cl6'—C26'—H26' | 108.4 |
C18—C17—H17B | 108.5 | Cl6"—C26"—Cl8" | 110.6 (9) |
S3—C17—H17B | 108.5 | Cl6"—C26"—Cl7" | 108.9 (9) |
H17A—C17—H17B | 107.5 | Cl8"—C26"—Cl7" | 110.6 (9) |
C17—C18—C19 | 108.7 (6) | Cl6"—C26"—H26" | 108.9 |
C17—C18—H18A | 110.0 | Cl8"—C26"—H26" | 108.9 |
C19—C18—H18A | 110.0 | Cl7"—C26"—H26" | 108.9 |
N5—Ag1—N1—C1 | −76.7 (8) | N3—C10—C11—C12 | 0.8 (12) |
N5—Ag1—N1—C4 | 108.5 (6) | C9—N4—C12—C11 | 1.8 (11) |
N1—Ag1—N5—C13 | 81.4 (7) | C10—C11—C12—N4 | −1.7 (13) |
N1—Ag1—N5—C16 | −103.6 (7) | C16—N5—C13—C14 | −1.2 (9) |
N3i—Ag2—N7—C21 | −69.4 (12) | Ag1—N5—C13—C14 | 174.0 (5) |
N3i—Ag2—N7—C22 | 102.8 (11) | N5—C13—C14—C15 | 0.5 (10) |
C4—N1—C1—C2 | −0.5 (9) | C16—N6—C15—C14 | 0.8 (11) |
Ag1—N1—C1—C2 | −175.6 (5) | C13—C14—C15—N6 | −0.3 (11) |
N1—C1—C2—C3 | 3.0 (10) | C15—N6—C16—N5 | −1.7 (10) |
C4—N2—C3—C2 | −0.3 (10) | C15—N6—C16—S3 | 177.5 (5) |
C1—C2—C3—N2 | −2.6 (11) | C13—N5—C16—N6 | 1.9 (9) |
C3—N2—C4—N1 | 3.3 (9) | Ag1—N5—C16—N6 | −173.4 (5) |
C3—N2—C4—S1 | −177.8 (5) | C13—N5—C16—S3 | −177.3 (4) |
C1—N1—C4—N2 | −2.9 (9) | Ag1—N5—C16—S3 | 7.4 (6) |
Ag1—N1—C4—N2 | 172.1 (5) | C17—S3—C16—N6 | 8.4 (6) |
C1—N1—C4—S1 | 178.1 (4) | C17—S3—C16—N5 | −172.4 (4) |
Ag1—N1—C4—S1 | −6.8 (6) | C16—S3—C17—C18 | −79.3 (6) |
C5—S1—C4—N2 | 8.1 (6) | S3—C17—C18—C19 | −169.3 (5) |
C5—S1—C4—N1 | −172.9 (4) | C17—C18—C19—C20 | −177.0 (7) |
C4—S1—C5—C6 | 74.8 (5) | C18—C19—C20—S4 | 174.7 (6) |
S1—C5—C6—C7 | 173.0 (5) | C21—S4—C20—C19 | 92.6 (7) |
C5—C6—C7—C8 | 173.7 (5) | C24—N8—C21—N7 | 0.5 (12) |
C6—C7—C8—S2 | −173.9 (5) | C24—N8—C21—S4 | 179.8 (6) |
C9—S2—C8—C7 | −82.1 (5) | C22—N7—C21—N8 | −1.7 (11) |
C12—N4—C9—N3 | −1.1 (10) | Ag2—N7—C21—N8 | 170.9 (6) |
C12—N4—C9—S2 | −178.8 (5) | C22—N7—C21—S4 | 179.1 (5) |
C10—N3—C9—N4 | 0.3 (9) | Ag2—N7—C21—S4 | −8.4 (7) |
Ag2ii—N3—C9—N4 | 179.8 (5) | C20—S4—C21—N8 | −10.7 (7) |
C10—N3—C9—S2 | 178.1 (5) | C20—S4—C21—N7 | 168.6 (5) |
Ag2ii—N3—C9—S2 | −2.4 (7) | C21—N7—C22—C23 | 2.0 (11) |
C8—S2—C9—N4 | −2.0 (6) | Ag2—N7—C22—C23 | −170.5 (6) |
C8—S2—C9—N3 | −180.0 (5) | N7—C22—C23—C24 | −1.3 (12) |
C9—N3—C10—C11 | −0.2 (11) | C22—C23—C24—N8 | 0.1 (14) |
Ag2ii—N3—C10—C11 | −179.7 (6) | C21—N8—C24—C23 | 0.3 (13) |
Symmetry codes: (i) x, y, z+1; (ii) x, y, z−1. |
Experimental details
Crystal data | |
Chemical formula | [Ag2(C12H14N4S2)2](ClO4)2·1.5CHCl3 |
Mr | 2300.95 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 11.197 (4), 12.394 (4), 16.897 (6) |
α, β, γ (°) | 73.715 (5), 73.060 (6), 86.618 (6) |
V (Å3) | 2152.5 (13) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.56 |
Crystal size (mm) | 0.28 × 0.26 × 0.22 |
Data collection | |
Diffractometer | Bruker SMART 1000 CCD area-detector |
Absorption correction | Multi-scan (SADABS; Bruker, 1998) |
Tmin, Tmax | 0.834, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12535, 8803, 4653 |
Rint | 0.023 |
(sin θ/λ)max (Å−1) | 0.628 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.053, 0.167, 1.02 |
No. of reflections | 8803 |
No. of parameters | 652 |
No. of restraints | 494 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.74, −0.44 |
Computer programs: SMART (Bruker, 1998), SAINT and SHELXTL (Bruker, 1998), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998).
Ag1—N1 | 2.188 (4) | Ag2—N7 | 2.171 (5) |
Ag1—N5 | 2.201 (5) | Ag2—N3i | 2.177 (5) |
N1—Ag1—N5 | 161.96 (18) | N7—Ag2—N3i | 168.73 (19) |
Symmetry code: (i) x, y, z+1. |
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Some AgI complexes of flexible bis(arylthio)alkyl ligands (aryl = phenyl, benzyl, pyridyl, pyrimidinyl, 4-methyl-2-pyrimidinyl or 5-methyl-1,3,4-thiadiazolyl) have been reported by us and others [Bu et al., 2003; Li et al., 2005; Xie et al., 2004, 2005; Zheng et al., 2003, 2005], which show different structure features. Herein, we report a 1,4-bis(2-pyrimidinylthio)butane(L)—AgI complex, {[Ag2(C12H14N4S2)2].2ClO4.1.5CHCl3}n (I). The crystal structure of the title complex (I) consists of [AgL]n one-dimensional chain cations, ClO4- anions (as shown in Fig. 1) and solvent chloroform molecules. In the cationic chain, there are two crystallographic independent AgI centers (Ag1 and Ag2), both of which adopt near linear coordination geometry coordinated by two pyrimidine N atoms from two crystallographic independent L ligands. Selected bond distances and angles are listed in Table 1. The ligand coordinates to the AgI centers in a N,N'-bidentate bridging mode with two N donors in an anti-conformation, resulting in an infinite corrugated chain with the intra-molecular Ag—Ag separations of 13.089 (5) and 13.228 (5) Å. It is interesting that by the Ag—S weak coordinations (Ag1—S1B = 3.052 (4) and Ag2—S4C = 3.348 (5) Å) such one-dimensional chains are linked to form a two-dimensional supramolecular framework as shown in Fig. 2.