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Acta Crystallogr Sect E Struct Rep Online. 2009 February 1; 65(Pt 2): m191.
Published online 2009 January 14. doi:  10.1107/S1600536809000890
PMCID: PMC2968179

(3,5,7-Tribromo­tropolonato-κ2 O,O′)tris­(triphenyl­phosphine-κP)silver(I)

Abstract

The title compound, [Ag(C7H2Br3O2)(C18H15P)3], a silver(I) derivative of 3,5,7-tribromo­tropolone, has three triphenyl­phosphine ligands coordinated to the silver centre, whereas the 3,5,7-tribromo­tropolonate anion coordinates as a bidentate ligand. The compound is an example of a five-coordinate silver complex containing a bidentate ligand.

Related literature

The title compound is structurally related to other silver tropolonato and oxalato derivatives; see: Steyl & Hill (2009 [triangle]); Dean et al. (2001 [triangle]). For diketonato complexes, see: Hill & Steyl (2008 [triangle]); Steyl (2006 [triangle], 2007 [triangle]); Steyl & Hill (2009 [triangle]); Steyl & Roodt (2006 [triangle]). For general background, see: Roodt et al. (2003 [triangle]); Crous et al. (2005 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-0m191-scheme1.jpg

Experimental

Crystal data

  • [Ag(C7H2Br3O2)(C18H15P)3]
  • M r = 1252.50
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-65-0m191-efi1.jpg
  • a = 13.257 (1) Å
  • b = 27.1550 (17) Å
  • c = 14.688 (1) Å
  • β = 93.121 (2)°
  • V = 5279.7 (6) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 2.79 mm−1
  • T = 100 (2) K
  • 0.29 × 0.15 × 0.09 mm

Data collection

  • Bruker APEXII area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 1998 [triangle]) T min = 0.499, T max = 0.788
  • 74600 measured reflections
  • 11519 independent reflections
  • 7888 reflections with I > 2σ(I)
  • R int = 0.107

Refinement

  • R[F 2 > 2σ(F 2)] = 0.046
  • wR(F 2) = 0.165
  • S = 1.07
  • 11519 reflections
  • 631 parameters
  • H-atom parameters constrained
  • Δρmax = 0.72 e Å−3
  • Δρmin = −1.18 e Å−3

Data collection: APEX2 (Bruker, 2005 [triangle]); cell refinement: SAINT-Plus (Bruker, 2004 [triangle]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: DIAMOND (Brandenburg & Putz, 2006 [triangle]); software used to prepare material for publication: SHELXL97.

Table 1
Selected geometric parameters (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809000890/ng2535sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809000890/ng2535Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

Financial assistance from the University of the Free State and Professor A. Roodt is gratefully acknowledged. Mr L. Kirsten is acknowledged for the the data collection. Part of this material is based on work supported by the South African National Research Foundation (NRF) under grant No. GUN 2068915. Opinions, findings, conclusions or recommendations expressed in this material are those of the authors and do not necessarily reflect the views of the NRF.

supplementary crystallographic information

Comment

Recently, solid state studies containing the 3,5,7-tribromotropolone ligand have been reported (Steyl, 2007; Steyl & Roodt, 2006; Roodt et al., 2003; Crous et al., 2005), different metal centers such as Rh(I) and Pd(I) have been investigated. In this regard, we present a silver(I) tris(triphenylphosphine) complex of the 3,5,7-tribromotropolonato moiety.

The Ag—O bond distances are closely related in length while the Ag—P bond distances differ from each other, Table 1. A single phosphorous atom (P1) has a slight increase in bond distance compared to P2 and P3. Comparing the title compound to a similar tropolonato complex (Steyl & Hill, 2009) the Ag—O bond distances increases by ca 0.2 Å, while the Ag—P distances increased by ca 0.1 Å. This trend is indicative of the higher coordination number about the silver metal centre and the weaker coordination properties of the 3,5,7-tribromotropolonato moiety. The bidentate bite angle of the title compound is nearly 10 ° smaller than the related tropolonato or oxolato complex (Steyl & Hill, 2009; Dean et al., 2001).

In previous studies the longest Ag—O bond distance reported for the 3,5,7-tribromotropolonato moiety was ca 2.496 Å (Roodt et al., 2003), while in the title compound this bond length has increased to 2.630 (4) Å. The increase in coordination number of the silver moiety is a direct result of the weaker coordinating ability of the bidentate ligand compared to the related tropolonato complex, which contains only two triphenylphosphine ligands.

Experimental

The title complex was synthesized by the addition of the sodium salt of 3,5,7-tribromotropolone (204 mg, 0.57 mmol) to an dichloromethane solution (10 ml) of the [Cu(PPh3)2NO3] (370 mg, 0.57 mmol). On slow evaporation of the solvent; crystals suitable for X-Ray crystallography was obtained. Yield: 400 mg (58%).

Refinement

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

Figures

Fig. 1.
: Representation of the title compound (I), showing the numbering scheme and displacement ellipsoids (50% probability). For the carbon rings on the triphenylphosphine ligands, the first digit refers to phosphorous number, second digit to the ring number ...

Crystal data

[Ag(C7H2Br3O2)(C18H15P)3]F(000) = 2504
Mr = 1252.50Dx = 1.576 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5934 reflections
a = 13.257 (1) Åθ = 3.1–22.7°
b = 27.1550 (17) ŵ = 2.79 mm1
c = 14.688 (1) ÅT = 100 K
β = 93.121 (2)°Cuboid, yellow
V = 5279.7 (6) Å30.29 × 0.15 × 0.09 mm
Z = 4

Data collection

Bruker 4K CCD area-detector diffractometer11519 independent reflections
Radiation source: fine-focus sealed tube7888 reflections with I > 2σ(I)
graphiteRint = 0.107
Detector resolution: 512 x 512 pixels mm-1θmax = 27.0°, θmin = 1.6°
[var phi] and ω scansh = −16→16
Absorption correction: multi-scan (SADABS; Bruker,1998)k = −34→34
Tmin = 0.499, Tmax = 0.788l = −18→18
74600 measured reflections

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.046Hydrogen site location: riding model
wR(F2) = 0.165H-atom parameters constrained
S = 1.07w = 1/[σ2(Fo2) + (0.087P)2 + 1.428P] where P = (Fo2 + 2Fc2)/3
11519 reflections(Δ/σ)max = 0.002
631 parametersΔρmax = 0.72 e Å3
0 restraintsΔρmin = −1.18 e Å3

Special details

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)

xyzUiso*/Ueq
Ag0.18844 (3)0.125664 (14)0.68777 (3)0.01393 (12)
Br70.20169 (5)−0.04255 (2)0.89448 (5)0.03177 (18)
Br50.51227 (5)−0.13951 (2)0.75005 (5)0.03368 (18)
Br30.53351 (5)0.04342 (2)0.59589 (5)0.0392 (2)
P20.00007 (10)0.11235 (5)0.67588 (9)0.0134 (3)
P10.27008 (10)0.16932 (5)0.55760 (10)0.0149 (3)
P30.25150 (10)0.15700 (5)0.84172 (10)0.0154 (3)
C10.2851 (4)0.0111 (2)0.7538 (4)0.0188 (12)
O10.2149 (3)0.04018 (13)0.7698 (3)0.0217 (9)
O20.3253 (3)0.06463 (14)0.6370 (3)0.0269 (10)
C3310.1569 (4)0.15493 (19)0.9278 (3)0.0162 (12)
C3350.0551 (4)0.1884 (2)1.0431 (4)0.0257 (14)
H3350.03750.21541.08020.031*
C221−0.0631 (4)0.1724 (2)0.6815 (4)0.0170 (12)
C1210.2327 (4)0.23395 (19)0.5429 (4)0.0151 (11)
C1110.2443 (4)0.1441 (2)0.4426 (4)0.0171 (12)
C211−0.0487 (4)0.08484 (19)0.5679 (4)0.0154 (11)
C1320.4522 (4)0.1880 (2)0.6530 (4)0.0265 (14)
H1320.41030.19700.70070.032*
C234−0.1611 (4)0.0118 (2)0.8766 (4)0.0235 (13)
H234−0.1935−0.01000.91630.028*
C3330.0318 (5)0.1043 (2)0.9974 (4)0.0257 (14)
H333−0.00210.07361.00210.031*
C223−0.1490 (4)0.2413 (2)0.6089 (4)0.0241 (14)
H223−0.17750.25680.55550.029*
C1160.1990 (4)0.1717 (2)0.3717 (4)0.0209 (13)
H1160.18440.20560.38090.025*
C20.3516 (4)0.0270 (2)0.6797 (4)0.0189 (12)
C225−0.1072 (5)0.2430 (2)0.7696 (4)0.0274 (14)
H225−0.10860.25950.82660.033*
C3320.1061 (4)0.1095 (2)0.9360 (4)0.0191 (12)
H3320.12330.08250.89890.023*
C1220.2955 (4)0.2692 (2)0.5055 (4)0.0206 (12)
H1220.36230.26050.49150.025*
C224−0.1507 (4)0.2647 (2)0.6918 (4)0.0258 (14)
H224−0.18210.29610.69570.031*
C3210.2960 (4)0.2205 (2)0.8439 (4)0.0183 (12)
C1130.2411 (5)0.0736 (2)0.3436 (4)0.0275 (15)
H1130.25650.03990.33360.033*
C2120.0186 (4)0.07450 (19)0.5013 (4)0.0200 (12)
H2120.08820.08210.51160.024*
C3110.3563 (4)0.12088 (19)0.8937 (4)0.0199 (12)
C40.4843 (5)−0.0432 (2)0.6857 (4)0.0259 (14)
H40.5454−0.05220.65930.031*
C3220.3932 (4)0.2336 (2)0.8765 (4)0.0229 (13)
H3220.43710.20960.90410.027*
C1310.4080 (4)0.1730 (2)0.5686 (4)0.0201 (13)
C222−0.1059 (4)0.1953 (2)0.6030 (4)0.0190 (12)
H222−0.10510.17910.54570.023*
C3360.1288 (4)0.1942 (2)0.9810 (4)0.0202 (12)
H3360.16040.22530.97470.024*
C50.4426 (4)−0.0778 (2)0.7413 (4)0.0210 (13)
C3340.0063 (4)0.1432 (2)1.0518 (4)0.0256 (14)
H334−0.04400.13931.09480.031*
C1240.1642 (4)0.3295 (2)0.5106 (4)0.0228 (13)
H1240.14040.36210.49900.027*
C236−0.0213 (4)0.0302 (2)0.7841 (4)0.0175 (12)
H2360.04190.02130.76140.021*
C215−0.1836 (5)0.0513 (2)0.4706 (5)0.0342 (16)
H215−0.25290.04330.45930.041*
C3250.2657 (5)0.3049 (2)0.7960 (5)0.0361 (17)
H3250.22210.32920.76910.043*
C60.3602 (4)−0.0740 (2)0.7951 (4)0.0186 (12)
H60.3456−0.10220.83030.022*
C1120.2642 (4)0.0942 (2)0.4274 (4)0.0222 (13)
H1120.29380.07450.47530.027*
C1230.2613 (4)0.3164 (2)0.4890 (4)0.0232 (13)
H1230.30400.34000.46290.028*
C213−0.0155 (5)0.0532 (2)0.4202 (4)0.0266 (14)
H2130.03030.04670.37420.032*
C231−0.0663 (4)0.07515 (19)0.7595 (4)0.0167 (12)
C3130.5055 (5)0.0732 (2)0.8722 (5)0.0304 (15)
H3130.55520.06150.83310.037*
C1260.1365 (4)0.2476 (2)0.5652 (4)0.0191 (12)
H1260.09380.22410.59180.023*
C3120.4283 (4)0.1029 (2)0.8365 (4)0.0234 (13)
H3120.42440.11100.77350.028*
C1150.1753 (4)0.1501 (2)0.2878 (4)0.0253 (14)
H1150.14450.16920.23970.030*
C3260.2324 (5)0.2562 (2)0.8032 (4)0.0254 (14)
H3260.16640.24740.78030.031*
C70.2968 (4)−0.0340 (2)0.8035 (4)0.0195 (12)
C3150.4415 (5)0.0779 (2)1.0187 (5)0.0332 (16)
H3150.44630.06921.08140.040*
C235−0.0696 (4)−0.0012 (2)0.8416 (4)0.0222 (13)
H235−0.0398−0.03210.85740.027*
C233−0.2047 (5)0.0565 (2)0.8533 (4)0.0260 (14)
H233−0.26670.06580.87800.031*
C1330.5555 (5)0.1899 (2)0.6675 (5)0.0356 (17)
H1330.58450.19990.72520.043*
C1250.1017 (4)0.2951 (2)0.5492 (4)0.0229 (13)
H1250.03550.30410.56460.027*
C216−0.1505 (4)0.0728 (2)0.5525 (4)0.0291 (15)
H216−0.19700.07940.59790.035*
C226−0.0618 (4)0.19746 (19)0.7645 (4)0.0217 (13)
H226−0.02960.18310.81750.026*
C3240.3626 (5)0.3176 (2)0.8282 (5)0.0355 (16)
H3240.38550.35050.82300.043*
C1140.1960 (5)0.1010 (2)0.2735 (4)0.0302 (15)
H1140.17940.08620.21600.036*
C214−0.1154 (5)0.0415 (2)0.4064 (4)0.0317 (16)
H214−0.13810.02620.35080.038*
C1350.5754 (5)0.1639 (2)0.5133 (6)0.0391 (18)
H1350.61820.15600.46550.047*
C3160.3634 (5)0.1084 (2)0.9857 (4)0.0270 (14)
H3160.31530.12071.02570.032*
C1340.6166 (5)0.1774 (2)0.5989 (6)0.0412 (19)
H1340.68780.17790.60980.049*
C30.4466 (4)0.0034 (2)0.6641 (4)0.0224 (13)
C1360.4705 (5)0.1620 (2)0.4984 (5)0.0286 (15)
H1360.44180.15310.44000.034*
C3140.5119 (5)0.0602 (2)0.9614 (5)0.0360 (17)
H3140.56460.03920.98430.043*
C3230.4253 (5)0.2824 (2)0.8678 (4)0.0298 (15)
H3230.49150.29130.88970.036*
C232−0.1584 (4)0.0880 (2)0.7941 (4)0.0223 (13)
H232−0.18950.11840.77720.027*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ag0.0115 (2)0.0155 (2)0.0148 (2)−0.00044 (15)0.00092 (15)0.00050 (17)
Br70.0295 (4)0.0335 (4)0.0341 (4)0.0099 (3)0.0177 (3)0.0095 (3)
Br50.0424 (4)0.0241 (3)0.0364 (4)0.0178 (3)0.0186 (3)0.0099 (3)
Br30.0361 (4)0.0277 (4)0.0563 (5)0.0034 (3)0.0237 (3)0.0152 (3)
P20.0098 (6)0.0158 (7)0.0146 (7)−0.0010 (5)0.0009 (5)−0.0021 (6)
P10.0127 (7)0.0154 (7)0.0168 (7)−0.0009 (5)0.0032 (6)0.0014 (6)
P30.0143 (7)0.0156 (7)0.0159 (7)−0.0021 (6)−0.0027 (6)0.0009 (6)
C10.013 (3)0.016 (3)0.027 (3)−0.003 (2)−0.004 (2)−0.002 (2)
O10.014 (2)0.017 (2)0.035 (2)0.0029 (16)0.0026 (17)−0.0031 (18)
O20.031 (2)0.019 (2)0.031 (2)0.0087 (18)0.0027 (19)0.0093 (19)
C3310.021 (3)0.017 (3)0.010 (3)0.002 (2)−0.006 (2)0.004 (2)
C3350.022 (3)0.024 (3)0.030 (3)0.004 (3)−0.005 (3)−0.005 (3)
C2210.008 (3)0.019 (3)0.025 (3)−0.006 (2)0.003 (2)0.002 (2)
C1210.014 (3)0.017 (3)0.013 (3)0.000 (2)−0.002 (2)0.008 (2)
C1110.017 (3)0.019 (3)0.016 (3)−0.003 (2)0.006 (2)−0.002 (2)
C2110.013 (3)0.017 (3)0.016 (3)−0.001 (2)0.000 (2)−0.003 (2)
C1320.019 (3)0.026 (3)0.034 (4)−0.002 (3)−0.003 (3)0.008 (3)
C2340.028 (3)0.022 (3)0.021 (3)−0.014 (3)0.007 (3)−0.002 (3)
C3330.030 (3)0.023 (3)0.023 (3)−0.005 (3)−0.005 (3)0.004 (3)
C2230.013 (3)0.020 (3)0.039 (4)0.001 (2)−0.005 (3)0.004 (3)
C1160.023 (3)0.016 (3)0.024 (3)−0.007 (2)0.006 (2)−0.002 (2)
C20.022 (3)0.017 (3)0.018 (3)0.002 (2)0.001 (2)−0.008 (2)
C2250.039 (4)0.017 (3)0.028 (4)−0.006 (3)0.009 (3)−0.003 (3)
C3320.026 (3)0.015 (3)0.016 (3)0.000 (2)−0.005 (2)−0.001 (2)
C1220.015 (3)0.023 (3)0.024 (3)0.002 (2)0.000 (2)−0.001 (3)
C2240.019 (3)0.019 (3)0.040 (4)−0.006 (2)0.007 (3)0.000 (3)
C3210.022 (3)0.017 (3)0.016 (3)−0.003 (2)−0.002 (2)0.001 (2)
C1130.026 (3)0.021 (3)0.037 (4)−0.006 (3)0.016 (3)−0.014 (3)
C2120.021 (3)0.016 (3)0.024 (3)−0.003 (2)0.005 (2)−0.002 (2)
C3110.017 (3)0.013 (3)0.029 (3)−0.006 (2)−0.010 (2)0.003 (2)
C40.025 (3)0.021 (3)0.032 (4)0.007 (2)0.009 (3)0.002 (3)
C3220.026 (3)0.019 (3)0.023 (3)−0.005 (2)−0.004 (3)0.002 (3)
C1310.011 (3)0.015 (3)0.034 (3)0.000 (2)0.004 (2)0.009 (3)
C2220.012 (3)0.022 (3)0.023 (3)−0.005 (2)0.000 (2)−0.002 (3)
C3360.020 (3)0.020 (3)0.020 (3)−0.002 (2)−0.001 (2)−0.001 (2)
C50.028 (3)0.016 (3)0.019 (3)0.007 (2)0.002 (2)0.004 (2)
C3340.018 (3)0.040 (4)0.019 (3)0.006 (3)0.002 (2)0.004 (3)
C1240.031 (3)0.015 (3)0.022 (3)0.006 (2)−0.004 (3)−0.001 (2)
C2360.013 (3)0.021 (3)0.018 (3)0.000 (2)−0.002 (2)−0.002 (2)
C2150.016 (3)0.044 (4)0.041 (4)−0.007 (3)−0.009 (3)−0.016 (3)
C3250.040 (4)0.020 (3)0.046 (4)0.002 (3)−0.013 (3)0.007 (3)
C60.020 (3)0.019 (3)0.018 (3)−0.003 (2)0.004 (2)0.002 (2)
C1120.026 (3)0.014 (3)0.027 (3)−0.002 (2)0.012 (3)0.004 (3)
C1230.021 (3)0.020 (3)0.029 (3)−0.002 (2)0.002 (3)0.010 (3)
C2130.025 (3)0.035 (4)0.021 (3)−0.006 (3)0.005 (3)−0.010 (3)
C2310.016 (3)0.019 (3)0.016 (3)−0.002 (2)0.003 (2)0.002 (2)
C3130.021 (3)0.021 (3)0.048 (4)0.000 (3)−0.010 (3)−0.007 (3)
C1260.015 (3)0.020 (3)0.022 (3)−0.004 (2)0.002 (2)0.000 (2)
C3120.018 (3)0.022 (3)0.029 (3)−0.001 (2)−0.008 (3)−0.004 (3)
C1150.027 (3)0.029 (3)0.020 (3)−0.007 (3)0.001 (3)0.001 (3)
C3260.027 (3)0.021 (3)0.027 (3)0.001 (3)−0.008 (3)0.001 (3)
C70.016 (3)0.020 (3)0.022 (3)0.001 (2)0.005 (2)−0.001 (2)
C3150.032 (4)0.032 (4)0.034 (4)−0.010 (3)−0.016 (3)0.020 (3)
C2350.025 (3)0.017 (3)0.024 (3)−0.001 (2)0.000 (3)0.001 (2)
C2330.021 (3)0.024 (3)0.034 (4)−0.006 (3)0.013 (3)−0.001 (3)
C1330.026 (4)0.035 (4)0.045 (4)−0.007 (3)−0.007 (3)0.012 (3)
C1250.018 (3)0.026 (3)0.025 (3)0.001 (2)0.000 (2)−0.004 (3)
C2160.012 (3)0.042 (4)0.034 (4)−0.003 (3)0.004 (3)−0.016 (3)
C2260.031 (3)0.013 (3)0.021 (3)−0.005 (2)0.003 (3)−0.002 (2)
C3240.051 (5)0.017 (3)0.039 (4)−0.005 (3)0.007 (3)0.003 (3)
C1140.032 (4)0.036 (4)0.024 (3)−0.015 (3)0.011 (3)−0.013 (3)
C2140.030 (4)0.044 (4)0.020 (3)0.002 (3)−0.004 (3)−0.020 (3)
C1350.022 (3)0.024 (3)0.074 (6)0.004 (3)0.021 (4)0.014 (4)
C3160.022 (3)0.025 (3)0.034 (4)−0.005 (3)−0.006 (3)0.002 (3)
C1340.016 (3)0.022 (3)0.085 (6)−0.001 (3)−0.003 (4)0.021 (4)
C30.023 (3)0.024 (3)0.021 (3)−0.001 (2)0.008 (3)−0.002 (3)
C1360.022 (3)0.025 (3)0.040 (4)0.003 (3)0.015 (3)0.006 (3)
C3140.029 (4)0.019 (3)0.059 (5)−0.002 (3)−0.014 (3)0.008 (3)
C3230.031 (4)0.030 (3)0.028 (4)−0.017 (3)−0.004 (3)−0.003 (3)
C2320.017 (3)0.022 (3)0.029 (3)0.001 (2)0.006 (2)0.001 (3)

Geometric parameters (Å, °)

Ag—O12.630 (4)C311—C3121.393 (8)
Ag—O22.597 (4)C4—C51.380 (8)
Ag—P12.5412 (14)C4—C31.391 (8)
Ag—P22.5198 (14)C4—H40.9500
Ag—P32.5160 (14)C322—C3231.400 (8)
Br7—C71.901 (6)C322—H3220.9500
Br5—C51.915 (5)C131—C1361.391 (8)
Br3—C31.906 (6)C222—H2220.9500
P2—C2211.838 (6)C336—H3360.9500
P2—C2111.838 (5)C5—C61.386 (8)
P2—C2311.849 (5)C334—H3340.9500
P1—C1311.830 (5)C124—C1231.389 (8)
P1—C1211.833 (5)C124—C1251.390 (8)
P1—C1111.837 (6)C124—H1240.9500
P3—C3211.823 (6)C236—C2351.382 (8)
P3—C3311.829 (6)C236—C2311.398 (7)
P3—C3111.833 (6)C236—H2360.9500
C1—O11.252 (6)C215—C2141.368 (9)
C1—C71.429 (8)C215—C2161.387 (8)
C1—C21.502 (8)C215—H2150.9500
O2—C21.238 (7)C325—C3241.387 (9)
C331—C3361.385 (8)C325—C3261.399 (8)
C331—C3321.413 (7)C325—H3250.9500
C335—C3361.380 (8)C6—C71.382 (8)
C335—C3341.398 (8)C6—H60.9500
C335—H3350.9500C112—H1120.9500
C221—C2261.396 (8)C123—H1230.9500
C221—C2221.402 (8)C213—C2141.367 (8)
C121—C1261.385 (7)C213—H2130.9500
C121—C1221.400 (7)C231—C2321.393 (7)
C111—C1161.394 (8)C313—C3141.356 (9)
C111—C1121.401 (8)C313—C3121.385 (8)
C211—C2121.388 (8)C313—H3130.9500
C211—C2161.395 (7)C126—C1251.385 (8)
C132—C1331.375 (8)C126—H1260.9500
C132—C1311.402 (8)C312—H3120.9500
C132—H1320.9500C115—C1141.379 (8)
C234—C2331.382 (8)C115—H1150.9500
C234—C2351.388 (8)C326—H3260.9500
C234—H2340.9500C315—C3141.376 (9)
C333—C3341.377 (8)C315—C3161.393 (8)
C333—C3321.379 (8)C315—H3150.9500
C333—H3330.9500C235—H2350.9500
C223—C2241.376 (8)C233—C2321.386 (8)
C223—C2221.378 (8)C233—H2330.9500
C223—H2230.9500C133—C1341.370 (10)
C116—C1151.387 (8)C133—H1330.9500
C116—H1160.9500C125—H1250.9500
C2—C31.443 (8)C216—H2160.9500
C225—C2261.379 (8)C226—H2260.9500
C225—C2241.384 (9)C324—C3231.375 (9)
C225—H2250.9500C324—H3240.9500
C332—H3320.9500C114—H1140.9500
C122—C1231.377 (8)C214—H2140.9500
C122—H1220.9500C135—C1341.392 (11)
C224—H2240.9500C135—C1361.396 (8)
C321—C3221.395 (8)C135—H1350.9500
C321—C3261.398 (8)C316—H3160.9500
C113—C1121.372 (8)C134—H1340.9500
C113—C1141.380 (9)C136—H1360.9500
C113—H1130.9500C314—H3140.9500
C212—C2131.377 (8)C323—H3230.9500
C212—H2120.9500C232—H2320.9500
C311—C3161.392 (8)
O2—Ag—O159.36 (12)C331—C336—H336119.7
P3—Ag—P2112.98 (5)C4—C5—C6129.8 (5)
P3—Ag—P1112.59 (5)C4—C5—Br5115.4 (4)
P2—Ag—P1118.42 (5)C6—C5—Br5114.7 (4)
P3—Ag—O2105.72 (10)C333—C334—C335119.5 (6)
P2—Ag—O2126.43 (10)C333—C334—H334120.3
P1—Ag—O275.45 (9)C335—C334—H334120.3
P3—Ag—O181.79 (9)C123—C124—C125120.0 (5)
P2—Ag—O190.69 (9)C123—C124—H124120.0
P1—Ag—O1134.81 (9)C125—C124—H124120.0
C221—P2—C211105.1 (2)C235—C236—C231119.5 (5)
C221—P2—C231102.8 (2)C235—C236—H236120.3
C211—P2—C231101.1 (2)C231—C236—H236120.3
C221—P2—Ag108.77 (17)C214—C215—C216119.4 (6)
C211—P2—Ag114.75 (18)C214—C215—H215120.3
C231—P2—Ag122.54 (18)C216—C215—H215120.3
C131—P1—C121102.7 (2)C324—C325—C326120.0 (6)
C131—P1—C111103.7 (3)C324—C325—H325120.0
C121—P1—C111102.3 (2)C326—C325—H325120.0
C131—P1—Ag115.06 (19)C7—C6—C5127.6 (5)
C121—P1—Ag114.32 (18)C7—C6—H6116.2
C111—P1—Ag116.87 (18)C5—C6—H6116.2
C321—P3—C331104.5 (3)C113—C112—C111120.1 (6)
C321—P3—C311105.2 (2)C113—C112—H112119.9
C331—P3—C311103.2 (3)C111—C112—H112119.9
C321—P3—Ag115.31 (18)C122—C123—C124119.9 (5)
C331—P3—Ag113.83 (17)C122—C123—H123120.0
C311—P3—Ag113.60 (19)C124—C123—H123120.0
O1—C1—C7120.4 (5)C214—C213—C212119.7 (6)
O1—C1—C2115.2 (5)C214—C213—H213120.1
C7—C1—C2124.4 (5)C212—C213—H213120.1
C1—O1—Ag123.6 (4)C232—C231—C236119.6 (5)
C2—O2—Ag124.2 (4)C232—C231—P2124.4 (4)
C336—C331—C332118.6 (5)C236—C231—P2115.9 (4)
C336—C331—P3125.6 (4)C314—C313—C312121.5 (7)
C332—C331—P3115.7 (4)C314—C313—H313119.2
C336—C335—C334120.5 (6)C312—C313—H313119.2
C336—C335—H335119.8C125—C126—C121120.8 (5)
C334—C335—H335119.8C125—C126—H126119.6
C226—C221—C222119.2 (5)C121—C126—H126119.6
C226—C221—P2119.2 (4)C313—C312—C311119.5 (6)
C222—C221—P2121.4 (4)C313—C312—H312120.2
C126—C121—C122119.0 (5)C311—C312—H312120.2
C126—C121—P1118.3 (4)C114—C115—C116120.5 (6)
C122—C121—P1122.6 (4)C114—C115—H115119.7
C116—C111—C112118.7 (5)C116—C115—H115119.7
C116—C111—P1122.5 (4)C321—C326—C325120.1 (6)
C112—C111—P1118.7 (4)C321—C326—H326120.0
C212—C211—C216119.4 (5)C325—C326—H326120.0
C212—C211—P2118.8 (4)C6—C7—C1132.6 (5)
C216—C211—P2121.8 (4)C6—C7—Br7113.4 (4)
C133—C132—C131120.9 (6)C1—C7—Br7113.9 (4)
C133—C132—H132119.6C314—C315—C316120.7 (6)
C131—C132—H132119.6C314—C315—H315119.6
C233—C234—C235119.7 (5)C316—C315—H315119.6
C233—C234—H234120.2C236—C235—C234120.8 (5)
C235—C234—H234120.2C236—C235—H235119.6
C334—C333—C332120.4 (6)C234—C235—H235119.6
C334—C333—H333119.8C234—C233—C232120.2 (6)
C332—C333—H333119.8C234—C233—H233119.9
C224—C223—C222120.1 (6)C232—C233—H233119.9
C224—C223—H223120.0C134—C133—C132120.0 (7)
C222—C223—H223120.0C134—C133—H133120.0
C115—C116—C111120.2 (5)C132—C133—H133120.0
C115—C116—H116119.9C126—C125—C124119.7 (5)
C111—C116—H116119.9C126—C125—H125120.1
O2—C2—C3120.6 (5)C124—C125—H125120.1
O2—C2—C1116.4 (5)C215—C216—C211119.8 (6)
C3—C2—C1122.7 (5)C215—C216—H216120.1
C226—C225—C224120.1 (6)C211—C216—H216120.1
C226—C225—H225120.0C225—C226—C221120.0 (6)
C224—C225—H225120.0C225—C226—H226120.0
C333—C332—C331120.5 (5)C221—C226—H226120.0
C333—C332—H332119.8C323—C324—C325119.9 (6)
C331—C332—H332119.8C323—C324—H324120.0
C123—C122—C121120.6 (5)C325—C324—H324120.0
C123—C122—H122119.7C115—C114—C113119.3 (6)
C121—C122—H122119.7C115—C114—H114120.4
C223—C224—C225120.5 (6)C113—C114—H114120.4
C223—C224—H224119.8C213—C214—C215121.5 (6)
C225—C224—H224119.8C213—C214—H214119.2
C322—C321—C326119.7 (5)C215—C214—H214119.2
C322—C321—P3122.6 (4)C134—C135—C136119.3 (7)
C326—C321—P3117.5 (4)C134—C135—H135120.4
C112—C113—C114121.1 (6)C136—C135—H135120.4
C112—C113—H113119.4C311—C316—C315119.5 (6)
C114—C113—H113119.4C311—C316—H316120.3
C213—C212—C211120.1 (5)C315—C316—H316120.3
C213—C212—H212119.9C133—C134—C135120.8 (6)
C211—C212—H212119.9C133—C134—H134119.6
C316—C311—C312119.2 (5)C135—C134—H134119.6
C316—C311—P3123.0 (5)C4—C3—C2132.3 (6)
C312—C311—P3117.7 (4)C4—C3—Br3114.8 (4)
C5—C4—C3127.2 (6)C2—C3—Br3112.9 (4)
C5—C4—H4116.4C131—C136—C135120.3 (7)
C3—C4—H4116.4C131—C136—H136119.8
C321—C322—C323119.3 (5)C135—C136—H136119.8
C321—C322—H322120.4C313—C314—C315119.5 (6)
C323—C322—H322120.4C313—C314—H314120.3
C136—C131—C132118.7 (5)C315—C314—H314120.3
C136—C131—P1123.8 (5)C324—C323—C322121.1 (6)
C132—C131—P1117.5 (4)C324—C323—H323119.4
C223—C222—C221120.1 (6)C322—C323—H323119.4
C223—C222—H222120.0C233—C232—C231120.2 (5)
C221—C222—H222120.0C233—C232—H232119.9
C335—C336—C331120.5 (5)C231—C232—H232119.9
C335—C336—H336119.7
P3—Ag—P2—C22167.3 (2)C216—C211—C212—C2130.9 (9)
P1—Ag—P2—C221−67.4 (2)P2—C211—C212—C213179.0 (5)
O2—Ag—P2—C221−159.9 (2)C321—P3—C311—C31694.6 (5)
O1—Ag—P2—C221148.7 (2)C331—P3—C311—C316−14.6 (5)
P3—Ag—P2—C211−175.37 (19)Ag—P3—C311—C316−138.4 (4)
P1—Ag—P2—C21149.9 (2)C321—P3—C311—C312−89.3 (5)
O2—Ag—P2—C211−42.6 (2)C331—P3—C311—C312161.5 (4)
O1—Ag—P2—C211−94.0 (2)Ag—P3—C311—C31237.7 (5)
P3—Ag—P2—C231−52.3 (2)C326—C321—C322—C3230.2 (9)
P1—Ag—P2—C231173.0 (2)P3—C321—C322—C323173.8 (5)
O2—Ag—P2—C23180.5 (2)C133—C132—C131—C136−2.7 (9)
O1—Ag—P2—C23129.1 (2)C133—C132—C131—P1177.6 (5)
P3—Ag—P1—C13149.6 (2)C121—P1—C131—C136−101.7 (5)
P2—Ag—P1—C131−175.5 (2)C111—P1—C131—C1364.6 (5)
O2—Ag—P1—C131−51.7 (2)Ag—P1—C131—C136133.4 (4)
O1—Ag—P1—C131−51.7 (2)C121—P1—C131—C13278.0 (5)
P3—Ag—P1—C121−68.98 (19)C111—P1—C131—C132−175.7 (4)
P2—Ag—P1—C12165.92 (19)Ag—P1—C131—C132−46.8 (5)
O2—Ag—P1—C121−170.2 (2)C224—C223—C222—C221−0.4 (8)
O1—Ag—P1—C121−170.2 (2)C226—C221—C222—C223−2.1 (8)
P3—Ag—P1—C111171.6 (2)P2—C221—C222—C223−177.3 (4)
P2—Ag—P1—C111−53.5 (2)C334—C335—C336—C331−1.4 (8)
O2—Ag—P1—C11170.3 (2)C332—C331—C336—C3352.4 (8)
O1—Ag—P1—C11170.3 (2)P3—C331—C336—C335179.1 (4)
P2—Ag—P3—C321−110.3 (2)C3—C4—C5—C6−6.4 (11)
P1—Ag—P3—C32127.1 (2)C3—C4—C5—Br5176.8 (5)
O2—Ag—P3—C321107.6 (2)C332—C333—C334—C3351.3 (9)
O1—Ag—P3—C321162.4 (2)C336—C335—C334—C333−0.4 (9)
P2—Ag—P3—C33110.4 (2)C4—C5—C6—C72.4 (11)
P1—Ag—P3—C331147.86 (19)Br5—C5—C6—C7179.3 (5)
O2—Ag—P3—C331−131.7 (2)C114—C113—C112—C111−1.5 (9)
O1—Ag—P3—C331−76.8 (2)C116—C111—C112—C1131.3 (8)
P2—Ag—P3—C311128.2 (2)P1—C111—C112—C113176.8 (4)
P1—Ag—P3—C311−94.4 (2)C121—C122—C123—C1240.9 (9)
O2—Ag—P3—C311−13.9 (2)C125—C124—C123—C1220.3 (9)
O1—Ag—P3—C31141.0 (2)C211—C212—C213—C214−1.2 (9)
C7—C1—O1—Ag177.8 (4)C235—C236—C231—C2320.8 (8)
C2—C1—O1—Ag−3.2 (6)C235—C236—C231—P2−175.8 (4)
P3—Ag—O1—C1−107.4 (4)C221—P2—C231—C23216.0 (5)
P2—Ag—O1—C1139.5 (4)C211—P2—C231—C232−92.4 (5)
P1—Ag—O1—C16.4 (5)Ag—P2—C231—C232138.4 (4)
O2—Ag—O1—C16.4 (4)C221—P2—C231—C236−167.5 (4)
P3—Ag—O2—C259.9 (4)C211—P2—C231—C23684.0 (4)
P2—Ag—O2—C2−75.5 (5)Ag—P2—C231—C236−45.1 (5)
P1—Ag—O2—C2169.7 (5)C122—C121—C126—C1251.3 (8)
O1—Ag—O2—C2−10.3 (4)P1—C121—C126—C125−175.3 (4)
C321—P3—C331—C336−0.2 (5)C314—C313—C312—C3111.2 (9)
C311—P3—C331—C336109.6 (5)C316—C311—C312—C313−0.1 (8)
Ag—P3—C331—C336−126.8 (4)P3—C311—C312—C313−176.4 (4)
C321—P3—C331—C332176.6 (4)C111—C116—C115—C1140.0 (9)
C311—P3—C331—C332−73.6 (4)C322—C321—C326—C325−0.8 (9)
Ag—P3—C331—C33250.0 (4)P3—C321—C326—C325−174.7 (5)
C211—P2—C221—C226164.5 (4)C324—C325—C326—C3210.9 (10)
C231—P2—C221—C22659.0 (5)C5—C6—C7—C110.2 (11)
Ag—P2—C221—C226−72.2 (4)C5—C6—C7—Br7−173.9 (5)
C211—P2—C221—C222−20.4 (5)O1—C1—C7—C6173.6 (6)
C231—P2—C221—C222−125.8 (4)C2—C1—C7—C6−5.3 (10)
Ag—P2—C221—C222102.9 (4)O1—C1—C7—Br7−2.2 (7)
C131—P1—C121—C126−156.8 (4)C2—C1—C7—Br7178.9 (4)
C111—P1—C121—C12695.9 (5)C231—C236—C235—C234−1.3 (8)
Ag—P1—C121—C126−31.5 (5)C233—C234—C235—C2360.3 (9)
C131—P1—C121—C12226.8 (5)C235—C234—C233—C2321.1 (9)
C111—P1—C121—C122−80.5 (5)C131—C132—C133—C1340.5 (9)
Ag—P1—C121—C122152.1 (4)C121—C126—C125—C124−0.2 (8)
C131—P1—C111—C116−111.3 (5)C123—C124—C125—C126−0.6 (9)
C121—P1—C111—C116−4.7 (5)C214—C215—C216—C2110.8 (10)
Ag—P1—C111—C116121.0 (4)C212—C211—C216—C215−0.7 (9)
C131—P1—C111—C11273.4 (5)P2—C211—C216—C215−178.8 (5)
C121—P1—C111—C112−180.0 (4)C224—C225—C226—C221−2.4 (9)
Ag—P1—C111—C112−54.3 (5)C222—C221—C226—C2253.6 (8)
C221—P2—C211—C212118.0 (4)P2—C221—C226—C225178.8 (4)
C231—P2—C211—C212−135.3 (4)C326—C325—C324—C323−0.5 (11)
Ag—P2—C211—C212−1.4 (5)C116—C115—C114—C113−0.3 (9)
C221—P2—C211—C216−63.9 (5)C112—C113—C114—C1151.0 (9)
C231—P2—C211—C21642.7 (5)C212—C213—C214—C2151.2 (10)
Ag—P2—C211—C216176.7 (4)C216—C215—C214—C213−1.0 (11)
C112—C111—C116—C115−0.5 (8)C312—C311—C316—C315−0.6 (8)
P1—C111—C116—C115−175.8 (4)P3—C311—C316—C315175.4 (4)
Ag—O2—C2—C3−160.9 (4)C314—C315—C316—C3110.4 (9)
Ag—O2—C2—C112.9 (7)C132—C133—C134—C1351.6 (10)
O1—C1—C2—O2−6.1 (7)C136—C135—C134—C133−1.6 (9)
C7—C1—C2—O2172.9 (5)C5—C4—C3—C2−10.0 (11)
O1—C1—C2—C3167.6 (5)C5—C4—C3—Br3173.3 (5)
C7—C1—C2—C3−13.4 (8)O2—C2—C3—C4−163.7 (6)
C334—C333—C332—C331−0.3 (8)C1—C2—C3—C422.9 (10)
C336—C331—C332—C333−1.5 (8)O2—C2—C3—Br313.0 (7)
P3—C331—C332—C333−178.6 (4)C1—C2—C3—Br3−160.4 (4)
C126—C121—C122—C123−1.6 (8)C132—C131—C136—C1352.7 (9)
P1—C121—C122—C123174.8 (4)P1—C131—C136—C135−177.5 (4)
C222—C223—C224—C2251.6 (9)C134—C135—C136—C131−0.6 (9)
C226—C225—C224—C223−0.2 (9)C312—C313—C314—C315−1.5 (9)
C331—P3—C321—C322110.9 (5)C316—C315—C314—C3130.6 (9)
C311—P3—C321—C3222.6 (6)C325—C324—C323—C322−0.1 (10)
Ag—P3—C321—C322−123.3 (4)C321—C322—C323—C3240.3 (9)
C331—P3—C321—C326−75.3 (5)C234—C233—C232—C231−1.5 (9)
C311—P3—C321—C326176.4 (5)C236—C231—C232—C2330.5 (9)
Ag—P3—C321—C32650.4 (5)P2—C231—C232—C233176.9 (4)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NG2535).

References

  • Brandenburg, K. & Putz, H. (2006). DIAMOND Crystal Impact GbR, Bonn, Germany.
  • Bruker (1998). SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Bruker (2004). SAINT-Plus Bruker AXS Inc., Madison, Wisconsin, USA.
  • Bruker (2005). APEX2 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. [PubMed]
  • Dean, P. A. W., Scudder, M., Craig, D. & Dance, I. (2001). CrystEngComm, 3, 84–90.
  • Hill, T. N. & Steyl, G. (2008). Acta Cryst. E64, m1580–m1581. [PMC free article] [PubMed]
  • Roodt, A., Otto, S. & Steyl, G. (2003). Coord. Chem. Rev.245, 121–137.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Steyl, G. (2006). Acta Cryst. E62, m650–m652.
  • Steyl, G. (2007). Acta Cryst. E63, m2613–m2614.
  • Steyl, G. & Hill, T. N. (2009). Acta Cryst. E65, m233. [PMC free article] [PubMed]
  • Steyl, G. & Roodt, A. (2006). S. Afr. J. Chem.59, 21–27.

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