The structure of the title compound, {[Ag(C
10H
8N
2)]
2(SiF
6)·2H
2O·2C
2H
6O
2}
n, consists of two independent polymeric cationic chains containing Ag
I ions bridged by 4,4′-bipyridine ligands, hexafluorosilicate anions and cocrystallized ethylene glycol and water molecules. The Ag
I ion adopts a linear coordination geometry involving the N-donor ligands. A weak Ag
Ag interaction is observed, resulting in the formation of a double-chain structure. The hexafluorosilicate anions and the solvent molecules are linked by O—H
F, O—H
O and C—H
F hydrogen bonds to form a sheet-like structure parallel to the
bc plane. The double {[Ag(4,4′-bpy)]
+}
n chains are linked to this two-dimensional network by C—H
O and C—H
F hydrogen bonds, forming a three-dimensional network.
Supporting information
CCDC reference: 610817
Key indicators
- Single-crystal X-ray study
- T = 153 K
- Mean (C-C) = 0.016 Å
- R factor = 0.042
- wR factor = 0.093
- Data-to-parameter ratio = 18.1
checkCIF/PLATON results
No syntax errors found
Alert level B
ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
Tmin and Tmax reported: 0.252 0.928
Tmin(prime) and Tmax expected: 0.470 0.928
RR(prime) = 0.536
Please check that your absorption correction is appropriate.
PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.53
PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry ..... 90 PerFit
Alert level C
STRVA01_ALERT_4_C Flack test results are ambiguous.
From the CIF: _refine_ls_abs_structure_Flack 0.360
From the CIF: _refine_ls_abs_structure_Flack_su 0.060
PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.36
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 16
Alert level G
ABSTY01_ALERT_1_G Extra text has been found in the _exptl_absorpt_correction_type
field, which should be only a single keyword. A literature
citation should be included in the _exptl_absorpt_process_details
field.
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 25.86
From the CIF: _reflns_number_total 5161
Count of symmetry unique reflns 2760
Completeness (_total/calc) 186.99%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 2401
Fraction of Friedel pairs measured 0.870
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
3 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
2 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
3 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: EXPOSE (Stoe & Cie, 2000); cell refinement: CELL (Stoe & Cie, 2000); data reduction: INTEGRATE (Stoe & Cie, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.
catena-Poly[bis[silver(I)-µ-4,4'-bipyridine-
κ2N:
N']
hexafluorosilicate dihydrate ethylene glycol disolvate]
top
Crystal data top
[Ag(C10H8N2)]2(SiF6)·2H2O·2C2H6O2 | F(000) = 828 |
Mr = 830.37 | Dx = 1.934 Mg m−3 |
Monoclinic, Pc | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P -2yc | Cell parameters from 4500 reflections |
a = 9.8887 (8) Å | θ = 2.3–25.9° |
b = 11.3492 (6) Å | µ = 1.50 mm−1 |
c = 14.6304 (12) Å | T = 153 K |
β = 119.701 (9)° | Needle, colourless |
V = 1426.2 (2) Å3 | 0.50 × 0.10 × 0.05 mm |
Z = 2 | |
Data collection top
Stow IPDS diffractometer | 5161 independent reflections |
Radiation source: fine-focus sealed tube | 3559 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.073 |
Detector resolution: 0.81 pixels mm-1 | θmax = 25.9°, θmin = 2.4° |
ω scans | h = −12→12 |
Absorption correction: empirical (using intensity measurements), refined from ΔF (PLATON; Spek, 2003) | k = −13→13 |
Tmin = 0.252, Tmax = 0.928 | l = −17→17 |
10905 measured reflections | |
Refinement top
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)] = 0.042 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.093 | w = 1/[σ2(Fo2) + (0.0419P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.84 | (Δ/σ)max < 0.001 |
5161 reflections | Δρmax = 1.26 e Å−3 |
285 parameters | Δρmin = −0.96 e Å−3 |
8 restraints | Absolute structure: Flack (1983), with 2401 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.36 (6) |
Special details top
Experimental. Spectroscopic analysis: IR (KBr, cm-1): 3385, 2936, 1599, 1527, 1410, 1220,
1089, 1042, 1002, 883, 807, 738, 621, 564, 511, 482. |
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 | |
C1 | 0.2006 (13) | 0.4271 (8) | 0.0097 (8) | 0.0202 (9) | |
H1 | 0.1089 | 0.4689 | −0.0374 | 0.024* | |
C2 | 0.1980 (14) | 0.3040 (8) | 0.0038 (9) | 0.0202 (9) | |
H2 | 0.1086 | 0.2637 | −0.0481 | 0.024* | |
C3 | 0.3310 (14) | 0.2412 (8) | 0.0767 (9) | 0.0202 (9) | |
C4 | 0.4568 (14) | 0.3069 (8) | 0.1481 (9) | 0.0202 (9) | |
H4 | 0.5488 | 0.2674 | 0.1979 | 0.024* | |
C5 | 0.4522 (12) | 0.4281 (8) | 0.1488 (7) | 0.0202 (9) | |
H5 | 0.5403 | 0.4704 | 0.2000 | 0.024* | |
C6 | 0.3282 (15) | 0.1106 (8) | 0.0751 (10) | 0.0168 (9) | |
C7 | 0.1928 (13) | 0.0489 (8) | 0.0539 (8) | 0.0168 (9) | |
H7 | 0.1003 | 0.0906 | 0.0380 | 0.020* | |
C8 | 0.1946 (13) | −0.0722 (8) | 0.0564 (8) | 0.0168 (9) | |
H8 | 0.1021 | −0.1126 | 0.0422 | 0.020* | |
C9 | 0.4527 (13) | −0.0755 (8) | 0.0991 (8) | 0.0168 (9) | |
H9 | 0.5441 | −0.1189 | 0.1152 | 0.020* | |
C10 | 0.4607 (13) | 0.0451 (8) | 0.0987 (7) | 0.0168 (9) | |
H10 | 0.5551 | 0.0834 | 0.1143 | 0.020* | |
C11 | 0.1882 (11) | 0.4463 (8) | 0.2626 (7) | 0.0187 (9) | |
H11 | 0.0958 | 0.4893 | 0.2190 | 0.022* | |
C12 | 0.1808 (14) | 0.3241 (8) | 0.2595 (9) | 0.0187 (9) | |
H12 | 0.0876 | 0.2846 | 0.2117 | 0.022* | |
C13 | 0.3148 (15) | 0.2603 (8) | 0.3290 (9) | 0.0187 (9) | |
C14 | 0.4450 (14) | 0.3241 (7) | 0.4008 (9) | 0.0187 (9) | |
H14 | 0.5355 | 0.2841 | 0.4518 | 0.022* | |
C15 | 0.4418 (12) | 0.4456 (8) | 0.3973 (8) | 0.0187 (9) | |
H15 | 0.5293 | 0.4887 | 0.4481 | 0.022* | |
C16 | 0.3147 (17) | 0.1304 (9) | 0.3282 (10) | 0.0195 (8) | |
C17 | 0.1851 (14) | 0.0643 (8) | 0.3097 (8) | 0.0195 (8) | |
H17 | 0.0932 | 0.1026 | 0.2994 | 0.023* | |
C18 | 0.1906 (14) | −0.0575 (9) | 0.3065 (9) | 0.0195 (8) | |
H18 | 0.1022 | −0.1013 | 0.2961 | 0.023* | |
C19 | 0.4419 (14) | −0.0519 (9) | 0.3347 (8) | 0.0195 (8) | |
H19 | 0.5313 | −0.0915 | 0.3419 | 0.023* | |
C20 | 0.4457 (14) | 0.0699 (9) | 0.3421 (8) | 0.0195 (8) | |
H20 | 0.5374 | 0.1118 | 0.3567 | 0.023* | |
C21 | 0.7604 (12) | 0.7098 (9) | 0.4568 (8) | 0.025 (2) | |
H21A | 0.7909 | 0.7859 | 0.4391 | 0.030* | |
H21B | 0.8496 | 0.6548 | 0.4824 | 0.030* | |
C22 | 0.7126 (11) | 0.7274 (9) | 0.5402 (8) | 0.026 (2) | |
H22A | 0.6100 | 0.7670 | 0.5084 | 0.032* | |
H22B | 0.7029 | 0.6499 | 0.5674 | 0.032* | |
C23 | 0.8862 (12) | 0.3409 (9) | 0.3456 (8) | 0.025 (2) | |
H23A | 0.8087 | 0.3912 | 0.2883 | 0.031* | |
H23B | 0.9911 | 0.3641 | 0.3591 | 0.031* | |
C24 | 0.8755 (12) | 0.3593 (10) | 0.4433 (8) | 0.031 (2) | |
H24A | 0.8691 | 0.4447 | 0.4545 | 0.037* | |
H24B | 0.7797 | 0.3215 | 0.4348 | 0.037* | |
Ag1 | 0.31571 (7) | 0.67717 (6) | 0.08137 (5) | 0.0250 (2) | |
Ag2 | 0.32234 (7) | 0.69514 (6) | 0.31672 (5) | 0.0252 (2) | |
F1 | 0.8630 (9) | 0.1899 (5) | 0.7792 (6) | 0.0310 (18) | |
F2 | 0.6398 (10) | 0.3172 (5) | 0.6862 (7) | 0.0286 (19) | |
F3 | 0.8883 (7) | 0.3948 (6) | 0.8089 (5) | 0.0295 (15) | |
F4 | 0.7830 (7) | 0.4288 (5) | 0.6245 (5) | 0.0327 (15) | |
F5 | 1.0031 (9) | 0.3017 (5) | 0.7160 (7) | 0.0264 (18) | |
F6 | 0.7554 (8) | 0.2208 (6) | 0.5960 (5) | 0.0280 (15) | |
N1 | 0.3239 (18) | 0.4888 (7) | 0.0774 (12) | 0.0202 (9) | |
N2 | 0.3228 (15) | −0.1369 (6) | 0.0780 (10) | 0.0168 (9) | |
N3 | 0.3154 (19) | 0.5053 (8) | 0.3223 (12) | 0.0187 (9) | |
N4 | 0.3174 (16) | −0.1168 (7) | 0.3176 (11) | 0.0195 (8) | |
O1 | 0.6288 (12) | 0.6626 (8) | 0.3677 (7) | 0.034 (2) | |
H1A | 0.6368 | 0.6743 | 0.3139 | 0.051* | |
O2 | 0.8268 (8) | 0.7978 (6) | 0.6253 (5) | 0.0332 (18) | |
H2A | 0.8449 | 0.7683 | 0.6830 | 0.050* | |
O3 | 0.8582 (10) | 0.2200 (6) | 0.3141 (6) | 0.037 (2) | |
H3 | 0.8038 | 0.1890 | 0.3371 | 0.055* | |
O4 | 1.0060 (12) | 0.3112 (6) | 0.5313 (8) | 0.035 (2) | |
H4A | 1.0499 | 0.3636 | 0.5772 | 0.052* | |
O5 | 0.7885 (10) | −0.0030 (7) | 0.8606 (7) | 0.035 (2) | |
H1O | 0.804 (13) | 0.054 (8) | 0.831 (8) | 0.052* | |
H2O | 0.873 (7) | −0.006 (9) | 0.917 (5) | 0.052* | |
O6 | 0.8472 (13) | 0.0089 (7) | 0.5633 (8) | 0.042 (3) | |
H3O | 0.817 (14) | 0.062 (7) | 0.590 (9) | 0.064* | |
H4O | 0.810 (15) | −0.054 (6) | 0.575 (11) | 0.064* | |
Si1 | 0.8215 (6) | 0.3115 (2) | 0.7020 (4) | 0.0178 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.017 (2) | 0.0222 (18) | 0.019 (2) | 0.0003 (19) | 0.0071 (17) | 0.0015 (18) |
C2 | 0.017 (2) | 0.0222 (18) | 0.019 (2) | 0.0003 (19) | 0.0071 (17) | 0.0015 (18) |
C3 | 0.017 (2) | 0.0222 (18) | 0.019 (2) | 0.0003 (19) | 0.0071 (17) | 0.0015 (18) |
C4 | 0.017 (2) | 0.0222 (18) | 0.019 (2) | 0.0003 (19) | 0.0071 (17) | 0.0015 (18) |
C5 | 0.017 (2) | 0.0222 (18) | 0.019 (2) | 0.0003 (19) | 0.0071 (17) | 0.0015 (18) |
C6 | 0.012 (2) | 0.0237 (18) | 0.0135 (18) | 0.000 (2) | 0.0050 (16) | −0.0003 (19) |
C7 | 0.012 (2) | 0.0237 (18) | 0.0135 (18) | 0.000 (2) | 0.0050 (16) | −0.0003 (19) |
C8 | 0.012 (2) | 0.0237 (18) | 0.0135 (18) | 0.000 (2) | 0.0050 (16) | −0.0003 (19) |
C9 | 0.012 (2) | 0.0237 (18) | 0.0135 (18) | 0.000 (2) | 0.0050 (16) | −0.0003 (19) |
C10 | 0.012 (2) | 0.0237 (18) | 0.0135 (18) | 0.000 (2) | 0.0050 (16) | −0.0003 (19) |
C11 | 0.014 (2) | 0.0244 (17) | 0.018 (2) | 0.0012 (17) | 0.0071 (17) | −0.0001 (16) |
C12 | 0.014 (2) | 0.0244 (17) | 0.018 (2) | 0.0012 (17) | 0.0071 (17) | −0.0001 (16) |
C13 | 0.014 (2) | 0.0244 (17) | 0.018 (2) | 0.0012 (17) | 0.0071 (17) | −0.0001 (16) |
C14 | 0.014 (2) | 0.0244 (17) | 0.018 (2) | 0.0012 (17) | 0.0071 (17) | −0.0001 (16) |
C15 | 0.014 (2) | 0.0244 (17) | 0.018 (2) | 0.0012 (17) | 0.0071 (17) | −0.0001 (16) |
C16 | 0.014 (2) | 0.0220 (16) | 0.0193 (19) | −0.0007 (17) | 0.0062 (16) | −0.0009 (17) |
C17 | 0.014 (2) | 0.0220 (16) | 0.0193 (19) | −0.0007 (17) | 0.0062 (16) | −0.0009 (17) |
C18 | 0.014 (2) | 0.0220 (16) | 0.0193 (19) | −0.0007 (17) | 0.0062 (16) | −0.0009 (17) |
C19 | 0.014 (2) | 0.0220 (16) | 0.0193 (19) | −0.0007 (17) | 0.0062 (16) | −0.0009 (17) |
C20 | 0.014 (2) | 0.0220 (16) | 0.0193 (19) | −0.0007 (17) | 0.0062 (16) | −0.0009 (17) |
C21 | 0.018 (5) | 0.031 (6) | 0.023 (5) | −0.008 (4) | 0.008 (4) | −0.009 (4) |
C22 | 0.020 (5) | 0.034 (5) | 0.024 (5) | 0.002 (4) | 0.010 (4) | −0.001 (4) |
C23 | 0.025 (5) | 0.031 (5) | 0.026 (5) | −0.012 (4) | 0.017 (4) | −0.008 (4) |
C24 | 0.028 (6) | 0.030 (5) | 0.045 (7) | −0.002 (5) | 0.026 (5) | −0.002 (5) |
Ag1 | 0.0249 (5) | 0.0195 (4) | 0.0282 (5) | −0.0001 (3) | 0.0114 (4) | 0.0002 (3) |
Ag2 | 0.0233 (5) | 0.0209 (4) | 0.0279 (5) | 0.0002 (4) | 0.0100 (4) | 0.0000 (4) |
F1 | 0.034 (4) | 0.032 (4) | 0.034 (4) | 0.003 (3) | 0.023 (3) | 0.013 (3) |
F2 | 0.015 (4) | 0.043 (4) | 0.028 (4) | 0.002 (2) | 0.011 (3) | −0.005 (3) |
F3 | 0.024 (3) | 0.032 (3) | 0.023 (3) | 0.000 (2) | 0.004 (3) | −0.005 (2) |
F4 | 0.036 (4) | 0.031 (3) | 0.029 (3) | 0.009 (3) | 0.014 (3) | 0.013 (3) |
F5 | 0.017 (4) | 0.035 (4) | 0.026 (4) | 0.000 (2) | 0.010 (3) | 0.003 (2) |
F6 | 0.028 (3) | 0.030 (3) | 0.024 (3) | −0.002 (3) | 0.011 (3) | −0.009 (3) |
N1 | 0.017 (2) | 0.0222 (18) | 0.019 (2) | 0.0003 (19) | 0.0071 (17) | 0.0015 (18) |
N2 | 0.012 (2) | 0.0237 (18) | 0.0135 (18) | 0.000 (2) | 0.0050 (16) | −0.0003 (19) |
N3 | 0.014 (2) | 0.0244 (17) | 0.018 (2) | 0.0012 (17) | 0.0071 (17) | −0.0001 (16) |
N4 | 0.014 (2) | 0.0220 (16) | 0.0193 (19) | −0.0007 (17) | 0.0062 (16) | −0.0009 (17) |
O1 | 0.030 (6) | 0.053 (5) | 0.021 (5) | −0.006 (4) | 0.014 (4) | −0.006 (4) |
O2 | 0.039 (4) | 0.035 (4) | 0.013 (3) | 0.001 (3) | 0.003 (3) | 0.000 (3) |
O3 | 0.068 (6) | 0.024 (3) | 0.027 (4) | −0.010 (3) | 0.029 (4) | −0.001 (3) |
O4 | 0.029 (6) | 0.044 (5) | 0.032 (5) | 0.002 (3) | 0.016 (4) | −0.003 (3) |
O5 | 0.034 (4) | 0.035 (4) | 0.043 (5) | 0.001 (3) | 0.025 (4) | 0.005 (4) |
O6 | 0.067 (7) | 0.022 (4) | 0.044 (5) | 0.004 (4) | 0.032 (4) | 0.003 (3) |
Si1 | 0.0139 (8) | 0.0211 (9) | 0.0161 (8) | −0.0006 (11) | 0.0058 (7) | 0.0018 (11) |
Geometric parameters (Å, º) top
C1—N1 | 1.327 (17) | C18—H18 | 0.9500 |
C1—C2 | 1.400 (13) | C19—N4 | 1.347 (15) |
C1—H1 | 0.9500 | C19—C20 | 1.385 (14) |
C2—C3 | 1.408 (15) | C19—H19 | 0.9500 |
C2—H2 | 0.9500 | C20—H20 | 0.9500 |
C3—C4 | 1.381 (16) | C21—O1 | 1.414 (13) |
C3—C6 | 1.482 (13) | C21—C22 | 1.525 (14) |
C4—C5 | 1.377 (13) | C21—H21A | 0.9900 |
C4—H4 | 0.9500 | C21—H21B | 0.9900 |
C5—N1 | 1.365 (16) | C22—O2 | 1.439 (11) |
C5—H5 | 0.9500 | C22—H22A | 0.9900 |
C6—C10 | 1.393 (15) | C22—H22B | 0.9900 |
C6—C7 | 1.403 (16) | C23—O3 | 1.430 (11) |
C7—C8 | 1.375 (13) | C23—C24 | 1.500 (14) |
C7—H7 | 0.9500 | C23—H23A | 0.9900 |
C8—N2 | 1.359 (15) | C23—H23B | 0.9900 |
C8—H8 | 0.9500 | C24—O4 | 1.406 (14) |
C9—N2 | 1.356 (15) | C24—H24A | 0.9900 |
C9—C10 | 1.371 (13) | C24—H24B | 0.9900 |
C9—H9 | 0.9500 | Ag1—N1 | 2.141 (9) |
C10—H10 | 0.9500 | Ag1—N2i | 2.113 (7) |
C11—N3 | 1.306 (17) | Ag2—N3 | 2.159 (9) |
C11—C12 | 1.388 (12) | Ag2—N4i | 2.135 (8) |
C11—H11 | 0.9500 | F1—Si1 | 1.699 (7) |
C12—C13 | 1.407 (16) | F2—Si1 | 1.697 (10) |
C12—H12 | 0.9500 | F3—Si1 | 1.659 (8) |
C13—C14 | 1.395 (15) | F4—Si1 | 1.666 (7) |
C13—C16 | 1.474 (13) | F5—Si1 | 1.707 (10) |
C14—C15 | 1.380 (12) | F6—Si1 | 1.698 (8) |
C14—H14 | 0.9500 | O1—H1A | 0.8400 |
C15—N3 | 1.366 (17) | O2—H2A | 0.8400 |
C15—H15 | 0.9500 | O3—H3 | 0.8400 |
C16—C20 | 1.389 (17) | O4—H4A | 0.8400 |
C16—C17 | 1.391 (16) | O5—H1O | 0.83 (11) |
C17—C18 | 1.385 (14) | O5—H2O | 0.84 (7) |
C17—H17 | 0.9500 | O6—H3O | 0.85 (11) |
C18—N4 | 1.360 (16) | O6—H4O | 0.86 (10) |
| | | |
N1—C1—C2 | 123.7 (10) | O1—C21—C22 | 106.2 (9) |
N1—C1—H1 | 118.1 | O1—C21—H21A | 110.5 |
C2—C1—H1 | 118.1 | C22—C21—H21A | 110.5 |
C1—C2—C3 | 118.5 (10) | O1—C21—H21B | 110.5 |
C1—C2—H2 | 120.8 | C22—C21—H21B | 110.5 |
C3—C2—H2 | 120.8 | H21A—C21—H21B | 108.7 |
C4—C3—C2 | 116.9 (8) | O2—C22—C21 | 110.1 (8) |
C4—C3—C6 | 123.7 (9) | O2—C22—H22A | 109.6 |
C2—C3—C6 | 119.4 (9) | C21—C22—H22A | 109.6 |
C5—C4—C3 | 121.6 (10) | O2—C22—H22B | 109.6 |
C5—C4—H4 | 119.2 | C21—C22—H22B | 109.6 |
C3—C4—H4 | 119.2 | H22A—C22—H22B | 108.2 |
N1—C5—C4 | 121.4 (10) | O3—C23—C24 | 110.3 (8) |
N1—C5—H5 | 119.3 | O3—C23—H23A | 109.6 |
C4—C5—H5 | 119.3 | C24—C23—H23A | 109.6 |
C10—C6—C7 | 117.8 (8) | O3—C23—H23B | 109.6 |
C10—C6—C3 | 121.5 (9) | C24—C23—H23B | 109.6 |
C7—C6—C3 | 120.7 (9) | H23A—C23—H23B | 108.1 |
C8—C7—C6 | 119.6 (9) | O4—C24—C23 | 110.6 (9) |
C8—C7—H7 | 120.2 | O4—C24—H24A | 109.5 |
C6—C7—H7 | 120.2 | C23—C24—H24A | 109.5 |
N2—C8—C7 | 123.0 (9) | O4—C24—H24B | 109.5 |
N2—C8—H8 | 118.5 | C23—C24—H24B | 109.5 |
C7—C8—H8 | 118.5 | H24A—C24—H24B | 108.1 |
N2—C9—C10 | 124.1 (9) | N2i—Ag1—N1 | 174.0 (7) |
N2—C9—H9 | 117.9 | N4i—Ag2—N3 | 175.1 (7) |
C10—C9—H9 | 117.9 | C1—N1—C5 | 117.8 (7) |
C9—C10—C6 | 119.0 (9) | C1—N1—Ag1 | 120.9 (9) |
C9—C10—H10 | 120.5 | C5—N1—Ag1 | 121.1 (9) |
C6—C10—H10 | 120.5 | C9—N2—C8 | 116.4 (7) |
N3—C11—C12 | 123.5 (10) | C9—N2—Ag1ii | 123.1 (8) |
N3—C11—H11 | 118.3 | C8—N2—Ag1ii | 120.5 (8) |
C12—C11—H11 | 118.3 | C11—N3—C15 | 118.6 (8) |
C11—C12—C13 | 118.4 (9) | C11—N3—Ag2 | 121.6 (10) |
C11—C12—H12 | 120.8 | C15—N3—Ag2 | 119.4 (9) |
C13—C12—H12 | 120.8 | C19—N4—C18 | 117.1 (8) |
C14—C13—C12 | 117.7 (8) | C19—N4—Ag2ii | 121.7 (9) |
C14—C13—C16 | 121.5 (9) | C18—N4—Ag2ii | 121.1 (8) |
C12—C13—C16 | 120.8 (9) | C21—O1—H1A | 109.5 |
C15—C14—C13 | 119.7 (9) | C22—O2—H2A | 109.5 |
C15—C14—H14 | 120.1 | C23—O3—H3 | 109.5 |
C13—C14—H14 | 120.1 | C24—O4—H4A | 109.5 |
N3—C15—C14 | 121.3 (9) | H1O—O5—H2O | 101 (6) |
N3—C15—H15 | 119.3 | H3O—O6—H4O | 102 (13) |
C14—C15—H15 | 119.3 | F3—Si1—F4 | 92.1 (3) |
C20—C16—C17 | 117.7 (9) | F3—Si1—F2 | 90.3 (4) |
C20—C16—C13 | 119.8 (10) | F4—Si1—F2 | 90.4 (4) |
C17—C16—C13 | 122.5 (10) | F3—Si1—F6 | 177.4 (4) |
C18—C17—C16 | 119.8 (10) | F4—Si1—F6 | 90.5 (4) |
C18—C17—H17 | 120.1 | F2—Si1—F6 | 89.8 (4) |
C16—C17—H17 | 120.1 | F3—Si1—F1 | 89.1 (4) |
N4—C18—C17 | 122.6 (9) | F4—Si1—F1 | 178.4 (6) |
N4—C18—H18 | 118.7 | F2—Si1—F1 | 90.7 (4) |
C17—C18—H18 | 118.7 | F6—Si1—F1 | 88.4 (3) |
N4—C19—C20 | 123.1 (10) | F3—Si1—F5 | 91.2 (4) |
N4—C19—H19 | 118.4 | F4—Si1—F5 | 90.3 (4) |
C20—C19—H19 | 118.4 | F2—Si1—F5 | 178.3 (4) |
C19—C20—C16 | 119.7 (10) | F6—Si1—F5 | 88.7 (4) |
C19—C20—H20 | 120.2 | F1—Si1—F5 | 88.5 (4) |
C16—C20—H20 | 120.2 | | |
| | | |
N1—C1—C2—C3 | 3.0 (19) | C12—C13—C16—C17 | −36.1 (17) |
C1—C2—C3—C4 | −1.3 (18) | C20—C16—C17—C18 | 0.4 (16) |
C1—C2—C3—C6 | 177.2 (10) | C13—C16—C17—C18 | 177.9 (10) |
C2—C3—C4—C5 | 0.6 (18) | C16—C17—C18—N4 | −2.0 (15) |
C6—C3—C4—C5 | −177.8 (10) | N4—C19—C20—C16 | −2.2 (15) |
C3—C4—C5—N1 | −1.3 (18) | C17—C16—C20—C19 | 1.6 (17) |
C4—C3—C6—C10 | −36.2 (17) | C13—C16—C20—C19 | −175.9 (9) |
C2—C3—C6—C10 | 145.5 (12) | O1—C21—C22—O2 | −167.9 (8) |
C4—C3—C6—C7 | 141.1 (13) | O3—C23—C24—O4 | 73.0 (11) |
C2—C3—C6—C7 | −37.3 (17) | C2—C1—N1—C5 | −4 (2) |
C10—C6—C7—C8 | −0.5 (17) | C2—C1—N1—Ag1 | −179.4 (9) |
C3—C6—C7—C8 | −177.8 (9) | C4—C5—N1—C1 | 3 (2) |
C6—C7—C8—N2 | −0.4 (15) | C4—C5—N1—Ag1 | 178.5 (9) |
N2—C9—C10—C6 | −0.2 (15) | C10—C9—N2—C8 | −0.6 (18) |
C7—C6—C10—C9 | 0.7 (16) | C10—C9—N2—Ag1ii | −179.2 (8) |
C3—C6—C10—C9 | 178.1 (9) | C7—C8—N2—C9 | 0.9 (17) |
N3—C11—C12—C13 | 4.1 (17) | C7—C8—N2—Ag1ii | 179.5 (8) |
C11—C12—C13—C14 | 3.2 (16) | C12—C11—N3—C15 | −10.5 (19) |
C11—C12—C13—C16 | −179.0 (10) | C12—C11—N3—Ag2 | 176.3 (9) |
C12—C13—C14—C15 | −3.9 (17) | C14—C15—N3—C11 | 10 (2) |
C16—C13—C14—C15 | 178.4 (11) | C14—C15—N3—Ag2 | −177.1 (9) |
C13—C14—C15—N3 | −2.4 (18) | C20—C19—N4—C18 | 0.6 (18) |
C14—C13—C16—C20 | −41.0 (17) | C20—C19—N4—Ag2ii | −175.9 (8) |
C12—C13—C16—C20 | 141.4 (12) | C17—C18—N4—C19 | 1.5 (18) |
C14—C13—C16—C17 | 141.6 (13) | C17—C18—N4—Ag2ii | 178.1 (8) |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···F2iii | 0.84 | 1.89 | 2.721 (14) | 173 |
O2—H2A···O3iv | 0.84 | 1.86 | 2.630 (11) | 151 |
O3—H3···O5v | 0.84 | 2.16 | 2.733 (11) | 126 |
O4—H4A···F5 | 0.84 | 2.40 | 2.719 (14) | 103 |
O5—H1O···F1 | 0.83 (11) | 1.93 (10) | 2.761 (11) | 173 (11) |
O6—H3O···F6 | 0.85 (11) | 1.92 (9) | 2.696 (12) | 152 (10) |
O6—H4O···O2ii | 0.86 (10) | 1.81 (8) | 2.605 (11) | 153 (14) |
C23—H23A···F3iii | 0.99 | 2.52 | 3.049 (12) | 113 |
C1—H1···F3vi | 0.95 | 2.38 | 3.052 (13) | 127 |
C8—H8···O4vii | 0.95 | 2.42 | 3.208 (14) | 140 |
C9—H9···F2v | 0.95 | 2.46 | 3.199 (12) | 134 |
C9—H9···F6v | 0.95 | 2.52 | 3.437 (16) | 161 |
C11—H11···F5viii | 0.95 | 2.54 | 3.280 (12) | 135 |
C12—H12···O2viii | 0.95 | 2.43 | 3.349 (16) | 164 |
C14—H14···F6 | 0.95 | 2.27 | 3.204 (14) | 168 |
C18—H18···F1vii | 0.95 | 2.47 | 3.410 (17) | 172 |
C18—H18···F5vii | 0.95 | 2.52 | 3.231 (13) | 131 |
Symmetry codes: (ii) x, y−1, z; (iii) x, −y+1, z−1/2; (iv) x, −y+1, z+1/2; (v) x, −y, z−1/2; (vi) x−1, y, z−1; (vii) x−1, −y, z−1/2; (viii) x−1, −y+1, z−1/2. |