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Acta Cryst. (2009). E65, m233    [ doi:10.1107/S1600536809002785 ]

Bis(triphenylphosphine-[kappa]P)(tropolonato-[kappa]2O,O')silver(I) dichloromethane solvate

G. Steyl and T. N. Hill

Abstract top

The title compound, [Ag(C7H5O2)(C18H15P)2]·CH2Cl2, crystallizes with a distorted tetrahedral geometry about the AgI atom, defined by two O atoms from one tropolonate ligand and two P atoms from two triphenylphosphine ligands. It is an example of a new type of tropolone derivative that has not been characterized via solid-state methods.

Comment top

Tropolone type compounds have been of interest since its first discovery in the early 1940's (Dewar, 1945), with applications in pharmacology (Hill & Steyl, 2008) and catalysis (Crous et al., 2005). Although this type of compounds have been extensively studied, to date no structural data exist, which contain both a tropolone moiety and a silver metal centre. In this regard, we present a bis(triphenylphosphine)silver(I) complex of tropolone.

The Ag—O and Ag—P bond distances differ significantly from each other (Table 1). The distortion of these bonds are also reflected in the interplanar angle between the two planes defined by P—Ag—P and O—Ag—O in the order of 84.90 (4)°. A similar oxalate structure with two Ag centres has been reported (Dean et al., 2001). In this complex the P—Ag—P and O—Ag—O bond angles are 126.35 and 71.28 °, respectively. These values compared to the title compound are significantly larger, indicating the structural effect of the tropolonate moiety on the complexes. In previous studies it has been shown that the tropolonate moiety can act as either a bidentate or a monodentate ligand in its coordination behaviour (Steyl, 2006). Effectively, the tropolonate moiety assumes an optimal coordination mode to pack as efficiently as possible. No classical hydrogen bonds are observed in the solid-state structure of the title compound, although weak interactions do exist between the dichloromethane solvate and the silver complex.

Related literature top

For general background, see: Crous et al. (2005); Dewar (1945). For structurally related oxalate derivatives, see: Dean et al. (2001). For related diketonate complexes, see: Hill & Steyl (2008); Steyl (2006).

Experimental top

The title complex was synthesized by the addition of sodium salt of tropolone (0.083 g, 0.57 mmol) to a dichloromethane solution (10 ml) of [Cu(PPh3)2]NO3 (0.374 g, 0.287 mmol). On slow evaporation of the solvent, crystals suitable for X-ray crystallography were obtained (yield 85%).

Refinement top

H atoms were positioned geometrically and refined using a riding model, with C—H = 0.95 (CH) and 0.99 (CH2) Å and with Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT-Plus (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level. H atoms have been omitted for clarity.
Bis(triphenylphosphine-κP)(tropolonato-κ2O,O')silver(I) dichloromethane solvate top
Crystal data top
[Ag(C7H5O2)(C18H15P)2]·CH2Cl2Z = 2
Mr = 838.45F(000) = 856
Triclinic, P1Dx = 1.490 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.0175 (3) ÅCell parameters from 9106 reflections
b = 12.9925 (4) Åθ = 2.3–28.3°
c = 13.8394 (7) ŵ = 0.81 mm−1
α = 100.487 (2)°T = 100 K
β = 93.760 (2)°Cuboid, yellow
γ = 116.809 (1)°0.19 × 0.11 × 0.08 mm
V = 1869.33 (12) Å3
Data collection top
Bruker APEXII CCD
diffractometer		8178 independent reflections
Radiation source: fine-focus sealed tube6931 reflections with I > 2σ(I)
graphiteRint = 0.046
φ and ω scansθmax = 27.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)		h = −13→15
Tmin = 0.862, Tmax = 0.938k = −16→16
33544 measured reflectionsl = −17→17
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.070H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0283P)2 + 0.6452P]
where P = (Fo2 + 2Fc2)/3
8178 reflections(Δ/σ)max = 0.002
460 parametersΔρmax = 0.51 e Å−3
0 restraintsΔρmin = −0.41 e Å−3
Crystal data top
[Ag(C7H5O2)(C18H15P)2]·CH2Cl2γ = 116.809 (1)°
Mr = 838.45V = 1869.33 (12) Å3
Triclinic, P1Z = 2
a = 12.0175 (3) ÅMo Kα radiation
b = 12.9925 (4) ŵ = 0.81 mm−1
c = 13.8394 (7) ÅT = 100 K
α = 100.487 (2)°0.19 × 0.11 × 0.08 mm
β = 93.760 (2)°
Data collection top
Bruker APEXII CCD
diffractometer		8178 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)		6931 reflections with I > 2σ(I)
Tmin = 0.862, Tmax = 0.938Rint = 0.046
33544 measured reflectionsθmax = 27.0°
Refinement top
R[F2 > 2σ(F2)] = 0.030H-atom parameters constrained
wR(F2) = 0.070Δρmax = 0.51 e Å−3
S = 1.05Δρmin = −0.41 e Å−3
8178 reflectionsAbsolute structure: ?
460 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ag0.743570 (16)0.720243 (14)0.744274 (12)0.01303 (5)
P20.86325 (5)0.62927 (5)0.65456 (4)0.01241 (12)
P10.71316 (5)0.87540 (5)0.69503 (4)0.01207 (12)
O10.79674 (15)0.70564 (14)0.90673 (11)0.0184 (4)
C2360.6628 (2)0.49295 (19)0.49875 (17)0.0156 (5)
H2360.61300.47700.55010.019*
O20.57859 (15)0.56103 (15)0.78664 (12)0.0223 (4)
C1151.0246 (2)1.1352 (2)0.61838 (19)0.0231 (6)
H1151.05051.16220.56030.028*
C2110.8758 (2)0.50995 (19)0.69797 (16)0.0132 (5)
C1310.6271 (2)0.93724 (19)0.76747 (16)0.0134 (5)
C1160.9035 (2)1.0442 (2)0.61294 (17)0.0174 (5)
H1160.84651.00990.55140.021*
C1110.8651 (2)1.00316 (19)0.69726 (16)0.0131 (5)
C1320.6443 (2)1.0510 (2)0.77170 (16)0.0160 (5)
H1320.70571.10100.73830.019*
C2310.7939 (2)0.56327 (18)0.52340 (16)0.0119 (4)
C2330.8062 (2)0.5380 (2)0.34768 (17)0.0164 (5)
H2330.85550.55290.29600.020*
C2320.8649 (2)0.58525 (19)0.44675 (16)0.0145 (5)
H2320.95420.63290.46240.017*
C1220.6516 (2)0.7563 (2)0.49517 (16)0.0165 (5)
H1220.71030.72990.51310.020*
C20.6043 (2)0.5279 (2)0.86135 (16)0.0163 (5)
C1210.6314 (2)0.83422 (19)0.56701 (16)0.0130 (4)
C2160.8462 (2)0.40129 (19)0.63496 (17)0.0149 (5)
H2160.81680.38620.56590.018*
C2211.0266 (2)0.73307 (19)0.65092 (15)0.0124 (4)
C1330.5721 (2)1.0925 (2)0.82465 (17)0.0211 (5)
H1330.58481.17080.82800.025*
C2350.6052 (2)0.4466 (2)0.40016 (18)0.0187 (5)
H2350.51600.39850.38420.022*
C1230.5874 (2)0.7175 (2)0.39882 (17)0.0188 (5)
H1230.60260.66520.35070.023*
C2261.0571 (2)0.8503 (2)0.65170 (16)0.0155 (5)
H2260.99390.87490.65650.019*
C1240.5006 (2)0.7547 (2)0.37165 (17)0.0200 (5)
H1240.45550.72700.30540.024*
C1360.5374 (2)0.8647 (2)0.81740 (16)0.0170 (5)
H1360.52620.78730.81640.020*
C2221.1212 (2)0.6993 (2)0.64488 (17)0.0182 (5)
H2221.10190.62000.64520.022*
C2150.8596 (2)0.3150 (2)0.67277 (18)0.0191 (5)
H2150.83930.24100.62940.023*
C1260.5451 (2)0.8718 (2)0.53879 (17)0.0169 (5)
H1260.53050.92500.58640.020*
C1141.1078 (2)1.1868 (2)0.7076 (2)0.0233 (6)
H1141.19021.24990.71110.028*
C2241.2722 (2)0.8965 (2)0.63878 (18)0.0203 (5)
H2241.35570.95220.63440.024*
C1120.9504 (2)1.0542 (2)0.78683 (17)0.0183 (5)
H1120.92581.02580.84460.022*
C1131.0710 (2)1.1464 (2)0.79192 (19)0.0227 (5)
H1131.12821.18180.85330.027*
C2231.2432 (2)0.7803 (2)0.63844 (18)0.0203 (5)
H2231.30680.75610.63380.024*
C10.7289 (2)0.6063 (2)0.92667 (16)0.0152 (5)
C1340.4822 (2)1.0193 (2)0.87219 (17)0.0227 (6)
H1340.43221.04700.90770.027*
C1250.4804 (2)0.8322 (2)0.44196 (18)0.0198 (5)
H1250.42180.85850.42360.024*
C2340.6762 (2)0.4693 (2)0.32393 (17)0.0178 (5)
H2340.63580.43810.25620.021*
C30.5113 (2)0.4195 (2)0.87918 (17)0.0200 (5)
H30.43310.38470.83500.024*
C70.7775 (2)0.5754 (2)1.00616 (17)0.0207 (5)
H70.86070.63341.03790.025*
C2130.9307 (2)0.4435 (2)0.83629 (18)0.0224 (5)
H2130.95960.45790.90540.027*
C2251.1789 (2)0.9311 (2)0.64553 (17)0.0191 (5)
H2251.19871.01070.64590.023*
C1350.4643 (2)0.9060 (2)0.86865 (18)0.0239 (6)
H1350.40180.85600.90140.029*
C2140.9023 (2)0.3358 (2)0.77313 (18)0.0208 (5)
H2140.91220.27670.79870.025*
C2120.9173 (2)0.5296 (2)0.79969 (17)0.0192 (5)
H2120.93630.60280.84370.023*
C60.7276 (3)0.4775 (2)1.04662 (18)0.0258 (6)
H60.78310.47801.09910.031*
C40.5130 (3)0.3559 (2)0.94783 (18)0.0244 (6)
H40.43640.28540.94350.029*
C50.6098 (3)0.3790 (2)1.02256 (19)0.0281 (6)
H50.59330.32151.06080.034*
Cl10.82465 (6)0.96237 (6)0.01672 (5)0.03396 (16)
C010.9005 (3)1.1161 (3)0.0739 (2)0.0347 (7)
H01A0.88771.12760.14420.042*
H01B0.99261.14950.07360.042*
Cl20.84113 (7)1.19298 (7)0.01169 (5)0.03632 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag0.01416 (9)0.01288 (9)0.01448 (9)0.00751 (7)0.00373 (7)0.00533 (6)
P20.0128 (3)0.0121 (3)0.0143 (3)0.0071 (2)0.0035 (2)0.0041 (2)
P10.0126 (3)0.0120 (3)0.0140 (3)0.0069 (2)0.0042 (2)0.0046 (2)
O10.0174 (9)0.0154 (8)0.0183 (8)0.0046 (7)0.0003 (7)0.0043 (7)
C2360.0139 (12)0.0145 (12)0.0195 (12)0.0066 (10)0.0044 (9)0.0067 (9)
O20.0160 (9)0.0265 (10)0.0211 (9)0.0052 (8)0.0008 (7)0.0123 (7)
C1150.0213 (14)0.0205 (13)0.0322 (14)0.0099 (11)0.0124 (11)0.0135 (11)
C2110.0109 (11)0.0157 (12)0.0168 (11)0.0077 (10)0.0054 (9)0.0081 (9)
C1310.0132 (11)0.0142 (11)0.0121 (11)0.0068 (10)0.0015 (9)0.0014 (9)
C1160.0196 (13)0.0154 (12)0.0200 (12)0.0096 (10)0.0049 (10)0.0070 (10)
C1110.0123 (11)0.0113 (11)0.0192 (11)0.0083 (9)0.0043 (9)0.0039 (9)
C1320.0171 (12)0.0176 (12)0.0141 (11)0.0085 (10)0.0021 (9)0.0045 (9)
C2310.0153 (11)0.0078 (10)0.0147 (11)0.0072 (9)0.0017 (9)0.0027 (8)
C2330.0185 (12)0.0166 (12)0.0179 (11)0.0104 (10)0.0049 (9)0.0063 (9)
C2320.0120 (11)0.0120 (11)0.0210 (12)0.0062 (10)0.0030 (9)0.0056 (9)
C1220.0170 (12)0.0182 (12)0.0180 (12)0.0099 (10)0.0054 (9)0.0077 (9)
C20.0186 (12)0.0181 (12)0.0149 (11)0.0102 (10)0.0066 (9)0.0049 (9)
C1210.0111 (11)0.0124 (11)0.0145 (11)0.0038 (9)0.0025 (9)0.0057 (9)
C2160.0141 (12)0.0159 (12)0.0167 (11)0.0073 (10)0.0039 (9)0.0071 (9)
C2210.0128 (11)0.0117 (11)0.0117 (10)0.0056 (9)0.0012 (9)0.0012 (8)
C1330.0264 (14)0.0221 (13)0.0207 (12)0.0179 (12)0.0012 (10)0.0018 (10)
C2350.0118 (12)0.0137 (12)0.0262 (13)0.0028 (10)−0.0008 (10)0.0048 (10)
C1230.0219 (13)0.0179 (12)0.0177 (12)0.0093 (11)0.0072 (10)0.0056 (10)
C2260.0162 (12)0.0159 (12)0.0184 (11)0.0105 (10)0.0041 (9)0.0049 (9)
C1240.0206 (13)0.0200 (13)0.0155 (12)0.0063 (11)−0.0003 (10)0.0054 (10)
C1360.0189 (12)0.0171 (12)0.0175 (11)0.0091 (10)0.0067 (10)0.0068 (9)
C2220.0179 (12)0.0139 (12)0.0236 (12)0.0088 (10)0.0027 (10)0.0034 (10)
C2150.0166 (12)0.0131 (12)0.0274 (13)0.0068 (10)0.0053 (10)0.0042 (10)
C1260.0161 (12)0.0144 (12)0.0211 (12)0.0081 (10)0.0037 (10)0.0036 (9)
C1140.0138 (13)0.0137 (12)0.0420 (16)0.0049 (10)0.0077 (11)0.0092 (11)
C2240.0138 (12)0.0197 (13)0.0233 (13)0.0045 (10)0.0028 (10)0.0051 (10)
C1120.0179 (12)0.0173 (12)0.0216 (12)0.0095 (11)0.0053 (10)0.0050 (10)
C1130.0193 (13)0.0171 (13)0.0306 (14)0.0102 (11)−0.0020 (11)0.0008 (10)
C2230.0152 (12)0.0211 (13)0.0278 (13)0.0113 (11)0.0031 (10)0.0056 (10)
C10.0202 (12)0.0164 (12)0.0128 (11)0.0118 (10)0.0055 (9)0.0026 (9)
C1340.0240 (14)0.0336 (15)0.0175 (12)0.0202 (12)0.0061 (10)0.0033 (11)
C1250.0161 (12)0.0200 (13)0.0241 (13)0.0092 (11)−0.0009 (10)0.0065 (10)
C2340.0209 (13)0.0132 (12)0.0178 (12)0.0085 (10)−0.0028 (10)0.0008 (9)
C30.0211 (13)0.0193 (13)0.0161 (12)0.0071 (11)0.0045 (10)0.0025 (10)
C70.0210 (13)0.0271 (14)0.0165 (12)0.0131 (11)0.0029 (10)0.0063 (10)
C2130.0232 (14)0.0280 (14)0.0205 (12)0.0142 (12)0.0031 (10)0.0100 (11)
C2250.0223 (13)0.0136 (12)0.0224 (12)0.0087 (11)0.0055 (10)0.0052 (10)
C1350.0216 (14)0.0314 (15)0.0218 (13)0.0133 (12)0.0095 (11)0.0092 (11)
C2140.0173 (13)0.0207 (13)0.0306 (14)0.0107 (11)0.0069 (11)0.0146 (11)
C2120.0222 (13)0.0202 (13)0.0182 (12)0.0130 (11)0.0039 (10)0.0034 (10)
C60.0353 (16)0.0388 (16)0.0164 (12)0.0257 (14)0.0078 (11)0.0134 (11)
C40.0320 (15)0.0166 (13)0.0232 (13)0.0085 (12)0.0139 (12)0.0065 (10)
C50.0455 (18)0.0265 (15)0.0265 (14)0.0234 (14)0.0185 (13)0.0173 (12)
Cl10.0284 (4)0.0349 (4)0.0261 (3)0.0032 (3)0.0014 (3)0.0117 (3)
C010.0299 (16)0.0410 (17)0.0203 (14)0.0081 (14)−0.0073 (11)0.0050 (12)
Cl20.0302 (4)0.0453 (4)0.0321 (4)0.0184 (3)0.0015 (3)0.0057 (3)
Geometric parameters (Å, °) top
Ag—O12.3612 (16)C123—H1230.9500
Ag—O22.3342 (16)C226—C2251.384 (3)
Ag—P12.4070 (6)C226—H2260.9500
Ag—P22.4981 (5)C124—C1251.384 (3)
P2—C2311.821 (2)C124—H1240.9500
P2—C2211.823 (2)C136—C1351.389 (3)
P2—C2111.824 (2)C136—H1360.9500
P1—C1311.820 (2)C222—C2231.387 (3)
P1—C1111.825 (2)C222—H2220.9500
P1—C1211.829 (2)C215—C2141.382 (3)
O1—C11.271 (3)C215—H2150.9500
C236—C2351.380 (3)C126—C1251.385 (3)
C236—C2311.397 (3)C126—H1260.9500
C236—H2360.9500C114—C1131.383 (3)
O2—C21.261 (3)C114—H1140.9500
C115—C1141.381 (4)C224—C2251.385 (3)
C115—C1161.386 (3)C224—C2231.388 (3)
C115—H1150.9500C224—H2240.9500
C211—C2161.392 (3)C112—C1131.390 (3)
C211—C2121.399 (3)C112—H1120.9500
C131—C1321.386 (3)C113—H1130.9500
C131—C1361.395 (3)C223—H2230.9500
C116—C1111.391 (3)C1—C71.414 (3)
C116—H1160.9500C134—C1351.379 (3)
C111—C1121.395 (3)C134—H1340.9500
C132—C1331.393 (3)C125—H1250.9500
C132—H1320.9500C234—H2340.9500
C231—C2321.395 (3)C3—C41.373 (3)
C233—C2341.383 (3)C3—H30.9500
C233—C2321.390 (3)C7—C61.382 (3)
C233—H2330.9500C7—H70.9500
C232—H2320.9500C213—C2121.376 (3)
C122—C1231.377 (3)C213—C2141.387 (3)
C122—C1211.400 (3)C213—H2130.9500
C122—H1220.9500C225—H2250.9500
C2—C31.427 (3)C135—H1350.9500
C2—C11.486 (3)C214—H2140.9500
C121—C1261.391 (3)C212—H2120.9500
C216—C2151.387 (3)C6—C51.379 (4)
C216—H2160.9500C6—H60.9500
C221—C2221.393 (3)C4—C51.388 (4)
C221—C2261.394 (3)C4—H40.9500
C133—C1341.378 (3)C5—H50.9500
C133—H1330.9500Cl1—C011.770 (3)
C235—C2341.390 (3)C01—Cl21.768 (3)
C235—H2350.9500C01—H01A0.9900
C123—C1241.390 (3)C01—H01B0.9900
O2—Ag—O168.67 (6)C125—C124—H124120.3
O2—Ag—P1121.43 (4)C123—C124—H124120.3
O1—Ag—P1128.35 (4)C135—C136—C131119.8 (2)
O2—Ag—P2103.97 (4)C135—C136—H136120.1
O1—Ag—P298.81 (4)C131—C136—H136120.1
P1—Ag—P2122.391 (19)C223—C222—C221120.7 (2)
C231—P2—C221103.35 (10)C223—C222—H222119.6
C231—P2—C211103.57 (10)C221—C222—H222119.6
C221—P2—C211103.62 (10)C214—C215—C216120.5 (2)
C231—P2—Ag111.93 (7)C214—C215—H215119.8
C221—P2—Ag114.95 (7)C216—C215—H215119.8
C211—P2—Ag117.80 (7)C125—C126—C121120.6 (2)
C131—P1—C111104.60 (10)C125—C126—H126119.7
C131—P1—C121103.57 (10)C121—C126—H126119.7
C111—P1—C121104.03 (10)C115—C114—C113119.9 (2)
C131—P1—Ag118.60 (7)C115—C114—H114120.1
C111—P1—Ag110.63 (7)C113—C114—H114120.1
C121—P1—Ag114.02 (7)C225—C224—C223119.7 (2)
C1—O1—Ag115.51 (14)C225—C224—H224120.1
C235—C236—C231120.3 (2)C223—C224—H224120.1
C235—C236—H236119.8C113—C112—C111120.3 (2)
C231—C236—H236119.8C113—C112—H112119.8
C2—O2—Ag117.18 (14)C111—C112—H112119.8
C114—C115—C116120.4 (2)C114—C113—C112120.0 (2)
C114—C115—H115119.8C114—C113—H113120.0
C116—C115—H115119.8C112—C113—H113120.0
C216—C211—C212119.0 (2)C222—C223—C224119.9 (2)
C216—C211—P2123.18 (17)C222—C223—H223120.0
C212—C211—P2117.83 (17)C224—C223—H223120.0
C132—C131—C136119.41 (19)O1—C1—C7118.7 (2)
C132—C131—P1122.58 (16)O1—C1—C2117.0 (2)
C136—C131—P1117.97 (16)C7—C1—C2124.2 (2)
C115—C116—C111120.2 (2)C133—C134—C135120.5 (2)
C115—C116—H116119.9C133—C134—H134119.7
C111—C116—H116119.9C135—C134—H134119.7
C116—C111—C112119.1 (2)C124—C125—C126120.4 (2)
C116—C111—P1123.35 (18)C124—C125—H125119.8
C112—C111—P1117.30 (17)C126—C125—H125119.8
C131—C132—C133120.4 (2)C233—C234—C235119.3 (2)
C131—C132—H132119.8C233—C234—H234120.3
C133—C132—H132119.8C235—C234—H234120.3
C232—C231—C236118.8 (2)C4—C3—C2132.4 (2)
C232—C231—P2122.87 (17)C4—C3—H3113.8
C236—C231—P2118.21 (16)C2—C3—H3113.8
C234—C233—C232120.3 (2)C6—C7—C1132.6 (2)
C234—C233—H233119.8C6—C7—H7113.7
C232—C233—H233119.8C1—C7—H7113.7
C233—C232—C231120.5 (2)C212—C213—C214120.5 (2)
C233—C232—H232119.8C212—C213—H213119.7
C231—C232—H232119.8C214—C213—H213119.7
C123—C122—C121120.7 (2)C226—C225—C224120.4 (2)
C123—C122—H122119.6C226—C225—H225119.8
C121—C122—H122119.6C224—C225—H225119.8
O2—C2—C3118.2 (2)C134—C135—C136120.2 (2)
O2—C2—C1117.6 (2)C134—C135—H135119.9
C3—C2—C1124.2 (2)C136—C135—H135119.9
C126—C121—C122118.5 (2)C215—C214—C213119.5 (2)
C126—C121—P1123.10 (16)C215—C214—H214120.2
C122—C121—P1118.31 (17)C213—C214—H214120.2
C215—C216—C211120.2 (2)C213—C212—C211120.3 (2)
C215—C216—H216119.9C213—C212—H212119.8
C211—C216—H216119.9C211—C212—H212119.8
C222—C221—C226118.8 (2)C5—C6—C7130.0 (3)
C222—C221—P2122.69 (17)C5—C6—H6115.0
C226—C221—P2118.54 (16)C7—C6—H6115.0
C134—C133—C132119.6 (2)C3—C4—C5129.8 (2)
C134—C133—H133120.2C3—C4—H4115.1
C132—C133—H133120.2C5—C4—H4115.1
C236—C235—C234120.8 (2)C6—C5—C4126.3 (2)
C236—C235—H235119.6C6—C5—H5116.9
C234—C235—H235119.6C4—C5—H5116.9
C122—C123—C124120.3 (2)Cl2—C01—Cl1111.60 (15)
C122—C123—H123119.8Cl2—C01—H01A109.3
C124—C123—H123119.8Cl1—C01—H01A109.3
C225—C226—C221120.5 (2)Cl2—C01—H01B109.3
C225—C226—H226119.7Cl1—C01—H01B109.3
C221—C226—H226119.7H01A—C01—H01B108.0
C125—C124—C123119.4 (2)
O2—Ag—P2—C23183.92 (9)C131—P1—C121—C12613.0 (2)
O1—Ag—P2—C231153.99 (8)C111—P1—C121—C126−96.14 (19)
P1—Ag—P2—C231−58.66 (8)Ag—P1—C121—C126143.27 (17)
O2—Ag—P2—C221−158.57 (9)C131—P1—C121—C122−163.60 (17)
O1—Ag—P2—C221−88.49 (9)C111—P1—C121—C12287.28 (18)
P1—Ag—P2—C22158.85 (8)Ag—P1—C121—C122−33.31 (19)
O2—Ag—P2—C211−35.96 (10)C212—C211—C216—C215−0.9 (3)
O1—Ag—P2—C21134.11 (10)P2—C211—C216—C215179.11 (16)
P1—Ag—P2—C211−178.54 (9)C231—P2—C221—C222−86.0 (2)
O2—Ag—P1—C13144.96 (10)C211—P2—C221—C22221.8 (2)
O1—Ag—P1—C131−41.59 (10)Ag—P2—C221—C222151.70 (16)
P2—Ag—P1—C131−178.76 (8)C231—P2—C221—C22692.32 (18)
O2—Ag—P1—C111165.75 (9)C211—P2—C221—C226−159.88 (17)
O1—Ag—P1—C11179.20 (9)Ag—P2—C221—C226−29.94 (19)
P2—Ag—P1—C111−57.97 (8)C131—C132—C133—C134−0.7 (4)
O2—Ag—P1—C121−77.42 (9)C231—C236—C235—C234−0.3 (3)
O1—Ag—P1—C121−163.97 (8)C121—C122—C123—C124−0.5 (3)
P2—Ag—P1—C12158.86 (8)C222—C221—C226—C2250.7 (3)
O2—Ag—O1—C117.65 (14)P2—C221—C226—C225−177.75 (17)
P1—Ag—O1—C1131.53 (13)C122—C123—C124—C1250.9 (3)
P2—Ag—O1—C1−83.99 (14)C132—C131—C136—C1351.5 (3)
O1—Ag—O2—C2−15.03 (15)P1—C131—C136—C135−176.21 (19)
P1—Ag—O2—C2−137.85 (14)C226—C221—C222—C223−0.8 (3)
P2—Ag—O2—C279.12 (15)P2—C221—C222—C223177.51 (18)
C231—P2—C211—C2165.0 (2)C211—C216—C215—C2140.0 (3)
C221—P2—C211—C216−102.68 (19)C122—C121—C126—C1250.4 (3)
Ag—P2—C211—C216129.12 (16)P1—C121—C126—C125−176.20 (18)
C231—P2—C211—C212−175.02 (17)C116—C115—C114—C1131.0 (4)
C221—P2—C211—C21277.34 (18)C116—C111—C112—C1131.3 (3)
Ag—P2—C211—C212−50.86 (19)P1—C111—C112—C113175.55 (17)
C111—P1—C131—C13230.9 (2)C115—C114—C113—C112−0.1 (3)
C121—P1—C131—C132−77.8 (2)C111—C112—C113—C114−1.1 (3)
Ag—P1—C131—C132154.70 (17)C221—C222—C223—C2240.5 (4)
C111—P1—C131—C136−151.45 (18)C225—C224—C223—C2220.0 (4)
C121—P1—C131—C13699.85 (19)Ag—O1—C1—C7158.97 (15)
Ag—P1—C131—C136−27.6 (2)Ag—O1—C1—C2−18.7 (2)
C114—C115—C116—C111−0.7 (3)O2—C2—C1—O15.2 (3)
C115—C116—C111—C112−0.4 (3)C3—C2—C1—O1−173.26 (19)
C115—C116—C111—P1−174.29 (17)O2—C2—C1—C7−172.4 (2)
C131—P1—C111—C116−113.66 (19)C3—C2—C1—C79.2 (3)
C121—P1—C111—C116−5.3 (2)C132—C133—C134—C1350.8 (4)
Ag—P1—C111—C116117.54 (17)C123—C124—C125—C126−0.6 (4)
C131—P1—C111—C11272.36 (18)C121—C126—C125—C1240.0 (4)
C121—P1—C111—C112−179.28 (16)C232—C233—C234—C235−1.0 (3)
Ag—P1—C111—C112−56.44 (17)C236—C235—C234—C2330.9 (3)
C136—C131—C132—C133−0.5 (3)O2—C2—C3—C4174.6 (2)
P1—C131—C132—C133177.16 (18)C1—C2—C3—C4−7.0 (4)
C235—C236—C231—C232−0.2 (3)O1—C1—C7—C6178.7 (2)
C235—C236—C231—P2176.33 (17)C2—C1—C7—C6−3.8 (4)
C221—P2—C231—C2326.6 (2)C221—C226—C225—C224−0.2 (3)
C211—P2—C231—C232−101.18 (19)C223—C224—C225—C226−0.1 (4)
Ag—P2—C231—C232130.91 (16)C133—C134—C135—C1360.3 (4)
C221—P2—C231—C236−169.69 (17)C131—C136—C135—C134−1.5 (4)
C211—P2—C231—C23682.48 (18)C216—C215—C214—C2130.6 (3)
Ag—P2—C231—C236−45.43 (19)C212—C213—C214—C215−0.4 (3)
C234—C233—C232—C2310.6 (3)C214—C213—C212—C211−0.5 (3)
C236—C231—C232—C2330.0 (3)C216—C211—C212—C2131.2 (3)
P2—C231—C232—C233−176.29 (17)P2—C211—C212—C213−178.86 (17)
Ag—O2—C2—C3−169.93 (14)C1—C7—C6—C5−2.5 (4)
Ag—O2—C2—C111.5 (2)C2—C3—C4—C5−0.4 (4)
C123—C122—C121—C126−0.1 (3)C7—C6—C5—C41.3 (4)
C123—C122—C121—P1176.62 (17)C3—C4—C5—C62.8 (4)
Table 1
Selected geometric parameters (Å, °) top
Ag—O12.3612 (16)Ag—P12.4070 (6)
Ag—O22.3342 (16)Ag—P22.4981 (5)
O2—Ag—O168.67 (6)O2—Ag—P2103.97 (4)
O2—Ag—P1121.43 (4)O1—Ag—P298.81 (4)
O1—Ag—P1128.35 (4)P1—Ag—P2122.391 (19)
Acknowledgements top

Financial assistance from the University of the Free State and Professor A. Roodt is gratefully acknowledged. Mr L. Kirsten is acknowledged for the data collection. Part of this research is based on work supported by the South African National Research Foundation (NRF) (grant No. GUN2068915). Opinions, findings, conclusions or recommendations expressed in this material are those of the authors and do not necessarily reflect the views of the NRF.

references
References top

Brandenburg, K. & Putz, H. (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany.

Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.

Bruker (2007). APEX2 and SAINT-Plus. Bruker AXS Inc., Madison, Wisconsin, USA.

Crous, R., Datt, M., Foster, D., Bennie, L., Steenkamp, C., Huyser, J., Kirsten, L., Steyl, G. & Roodt, A. (2005). Dalton Trans. pp. 1108–1115.

Dean, P. A. W., Scudder, M., Craig, D. & Dance, I. (2001). CrystEngComm, 3, 84–90.

Dewar, M. J. S. (1945). Nature, 155, 141–145.

Hill, T. N. & Steyl, G. (2008). Acta Cryst. E64, m1580–m1581.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.

Steyl, G. (2006). Acta Cryst. E62, m650–m652.