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Acta Cryst. (2009). E65, m1601    [ doi:10.1107/S1600536809048144 ]

[2-(Tetrazol-1-yl)acetato-[kappa]O]tris(triphenylphosphine-[kappa]P)silver(I) monohydrate

J. Zhao, Z.-Z. Hu, X.-G. Zheng and S. W. Ng

Abstract top

The AgI atom in the title compound, [Ag(C3H3N4O2)(C18H15P)3]·H2O, exists in a distorted tetrahedral environment. The uncoordinated water molecule forms only one hydrogen bond to the uncoordinated carbonyl O atom.

Related literature top

For the crystal structure of silver tetrazol-1-yl-acetate, see: Dong et al. (2008).

Experimental top

Silver tetrazol-1-yl-acetate (0.024 g, 0.1 mmol) (Dong et al., 2008) and triphenylphosphine (0.079 g, 0.3 mmol) were dissolved in 10 ml dichloromethane. The solution was filtered and set aside for the growth of crystals.

Refinement top

All phenyl rings were refined as rigid hexagons of 1.39 Å sides as there was a slight spead of C—C distances. C-bound H atoms were placed in calculated positions (C—H = 0.93 and 0.97 Å) and were included in the refinement in the riding model approximation, with Uiso(H) = 1.2Ueq(C). The water H atoms were placed in chemically sensible positions (O—H = 0.84 Å) on the basis of hydrogen bonding interactions; the water molecule forms only one hydrogen bond.

A large difference of the components of the anisotropic displacement parameters along the Ag1—P1 and Ag1—P2 bonds was noted. However, there was no contamination of these parameters with other (unresolved) effects such as (substitutional) disorder, model or data errors and/or over-refinement. Neither was the P atoms wrongly assigned, and the multi-scan absorption was adequate.

Computing details top

Data collection: CrystalClear (Rigaku, 2002); cell refinement: CrystalClear (Rigaku, 2002); data reduction: CrystalClear (Rigaku, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2009).

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level.
[2-(Tetrazol-1-yl)acetato-κO]tris(triphenylphosphine- κP)silver(I) monohydrate top
Crystal data top
[Ag(C3H3N4O2)(C18H15P)3]·H2OF(000) = 2144
Mr = 1039.79Dx = 1.374 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 8961 reflections
a = 13.613 (4) Åθ = 2.1–27.5°
b = 23.017 (6) ŵ = 0.55 mm−1
c = 16.115 (4) ÅT = 293 K
β = 95.590 (3)°Block, colorless
V = 5025 (2) Å30.40 × 0.20 × 0.20 mm
Z = 4
Data collection top
Rigaku Mercury CCD
diffractometer		11514 independent reflections
Radiation source: fine-focus sealed tube9437 reflections with I > 2σ(I)
graphiteRint = 0.038
ω scanθmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2002)		h = −16→17
Tmin = 0.811, Tmax = 0.899k = −29→26
38977 measured reflectionsl = −20→20
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)] = 0.053Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.139H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.065P)2 + 3.6165P]
where P = (Fo2 + 2Fc2)/3
11514 reflections(Δ/σ)max = 0.001
505 parametersΔρmax = 0.64 e Å−3
6 restraintsΔρmin = −0.55 e Å−3
Crystal data top
[Ag(C3H3N4O2)(C18H15P)3]·H2OV = 5025 (2) Å3
Mr = 1039.79Z = 4
Monoclinic, P21/nMo Kα radiation
a = 13.613 (4) ŵ = 0.55 mm−1
b = 23.017 (6) ÅT = 293 K
c = 16.115 (4) Å0.40 × 0.20 × 0.20 mm
β = 95.590 (3)°
Data collection top
Rigaku Mercury CCD
diffractometer		11514 independent reflections
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2002)		9437 reflections with I > 2σ(I)
Tmin = 0.811, Tmax = 0.899Rint = 0.038
38977 measured reflectionsθmax = 27.5°
Refinement top
R[F2 > 2σ(F2)] = 0.053H-atom parameters constrained
wR(F2) = 0.139Δρmax = 0.64 e Å−3
S = 1.06Δρmin = −0.55 e Å−3
11514 reflectionsAbsolute structure: ?
505 parametersFlack parameter: ?
6 restraintsRogers parameter: ?
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ag10.599944 (17)0.636548 (11)0.735961 (14)0.03902 (9)
P10.72965 (6)0.67625 (4)0.84989 (5)0.0411 (2)
P20.63570 (6)0.65042 (4)0.58575 (5)0.03453 (18)
P30.43100 (6)0.65097 (4)0.78029 (5)0.03721 (19)
O10.6750 (2)0.54428 (11)0.75165 (16)0.0564 (7)
O20.5471 (2)0.50271 (14)0.8047 (2)0.0695 (8)
O1W0.3908 (6)0.4246 (4)0.7697 (6)0.267 (4)
H1W10.42730.45410.77180.401*
H1W20.38360.41220.72040.401*
N10.7978 (2)0.45528 (13)0.7941 (2)0.0510 (7)
N20.8329 (3)0.42544 (19)0.7329 (2)0.0766 (11)
N30.9236 (3)0.4415 (2)0.7300 (3)0.0852 (13)
N40.9487 (3)0.4813 (2)0.7895 (3)0.0849 (12)
C10.84036 (14)0.70195 (11)0.80516 (14)0.0445 (8)
C20.8852 (2)0.66286 (10)0.75500 (16)0.0631 (11)
H20.86050.62530.74770.076*
C30.9670 (2)0.67986 (15)0.71568 (16)0.0797 (15)
H30.99710.65370.68210.096*
C41.00398 (16)0.73593 (16)0.72653 (17)0.0792 (16)
H41.05870.74730.70020.095*
C50.95910 (19)0.77502 (12)0.77669 (18)0.0720 (13)
H50.98380.81250.78390.086*
C60.87729 (18)0.75802 (10)0.81600 (15)0.0551 (9)
H60.84730.78420.84960.066*
C70.77831 (16)0.62218 (10)0.92662 (13)0.0448 (8)
C80.71101 (14)0.58444 (12)0.95758 (16)0.0613 (10)
H80.64470.58620.93750.074*
C90.7429 (2)0.54412 (12)1.01856 (17)0.0757 (13)
H90.69780.51891.03930.091*
C100.8420 (2)0.54154 (11)1.04857 (16)0.0742 (13)
H100.86330.51461.08940.089*
C110.90932 (15)0.57928 (12)1.01761 (16)0.0645 (11)
H110.97570.57761.03770.077*
C120.87747 (15)0.61960 (11)0.95663 (15)0.0538 (9)
H120.92250.64490.93590.065*
C130.69582 (17)0.73678 (9)0.91528 (12)0.0425 (7)
C140.64237 (17)0.78217 (11)0.87600 (11)0.0513 (9)
H140.62660.78150.81850.062*
C150.61245 (18)0.82861 (10)0.92259 (16)0.0617 (10)
H150.57670.85900.89630.074*
C160.6360 (2)0.82967 (10)1.00846 (16)0.0655 (11)
H160.61600.86081.03960.079*
C170.6895 (2)0.78428 (12)1.04775 (10)0.0660 (11)
H170.70520.78501.10520.079*
C180.71937 (18)0.73784 (10)1.00116 (12)0.0540 (9)
H180.75510.70751.02740.065*
C190.54054 (14)0.61888 (11)0.51130 (15)0.0410 (7)
C200.56112 (16)0.57351 (15)0.4588 (2)0.114 (3)
H200.62570.56050.45760.137*
C210.4852 (2)0.54751 (15)0.4079 (2)0.140 (3)
H210.49900.51720.37280.168*
C220.38870 (19)0.56688 (14)0.4097 (2)0.0758 (13)
H220.33790.54950.37560.091*
C230.36812 (13)0.61224 (14)0.46219 (19)0.0696 (12)
H230.30360.62520.46330.083*
C240.44404 (16)0.63825 (12)0.51302 (17)0.0608 (11)
H240.43030.66860.54820.073*
C250.64115 (17)0.72619 (8)0.55331 (13)0.0376 (7)
C260.60325 (17)0.74622 (10)0.47532 (12)0.0481 (8)
H260.56970.72090.43750.058*
C270.6155 (2)0.80408 (11)0.45384 (14)0.0607 (10)
H270.59010.81750.40170.073*
C280.6656 (2)0.84190 (8)0.5104 (2)0.0786 (14)
H280.67380.88060.49600.094*
C290.7035 (2)0.82187 (10)0.58835 (17)0.0884 (16)
H290.73710.84720.62620.106*
C300.6913 (2)0.76401 (11)0.60982 (12)0.0614 (11)
H300.71670.75060.66200.074*
C310.74926 (14)0.62037 (10)0.55056 (14)0.0395 (7)
C320.79144 (18)0.64384 (10)0.48291 (15)0.0627 (11)
H320.76390.67660.45620.075*
C330.87483 (19)0.61828 (13)0.45522 (16)0.0728 (13)
H330.90310.63400.41000.087*
C340.91602 (16)0.56926 (12)0.49519 (17)0.0644 (11)
H340.97180.55220.47670.077*
C350.87383 (18)0.54580 (10)0.56285 (16)0.0617 (10)
H350.90140.51300.58960.074*
C360.79045 (17)0.57135 (10)0.59053 (13)0.0485 (8)
H360.76220.55570.63580.058*
C370.32834 (15)0.60244 (11)0.74617 (15)0.0423 (7)
C380.24374 (18)0.59950 (13)0.78783 (15)0.0623 (11)
H380.23890.62170.83550.075*
C390.16630 (15)0.56336 (14)0.7583 (2)0.0726 (13)
H390.10970.56140.78620.087*
C400.1735 (2)0.53015 (13)0.6871 (2)0.0822 (15)
H400.12170.50600.66730.099*
C410.2581 (2)0.53309 (14)0.64542 (18)0.0932 (17)
H410.26290.51090.59780.112*
C420.33550 (18)0.56923 (13)0.67497 (16)0.0685 (12)
H420.39210.57120.64710.082*
C430.43479 (18)0.64740 (10)0.89372 (10)0.0437 (8)
C440.4426 (2)0.69731 (9)0.94247 (15)0.0633 (11)
H440.43790.73370.91730.076*
C450.4573 (2)0.69284 (11)1.02880 (14)0.0846 (17)
H450.46250.72621.06140.102*
C460.4643 (2)0.63845 (14)1.06639 (10)0.0809 (16)
H460.47410.63551.12420.097*
C470.4565 (2)0.58853 (11)1.01765 (15)0.0673 (12)
H470.46110.55211.04280.081*
C480.44175 (19)0.59300 (9)0.93131 (14)0.0544 (9)
H480.43650.55960.89870.065*
C490.38348 (17)0.72416 (8)0.75446 (15)0.0419 (7)
C500.29639 (17)0.74544 (11)0.78129 (17)0.0632 (11)
H500.25880.72210.81320.076*
C510.26542 (18)0.80157 (12)0.76044 (19)0.0775 (14)
H510.20720.81580.77840.093*
C520.3215 (2)0.83642 (9)0.7128 (2)0.0777 (14)
H520.30080.87400.69880.093*
C530.4086 (2)0.81515 (10)0.68593 (18)0.0726 (12)
H530.44620.83850.65400.087*
C540.43960 (16)0.75902 (11)0.70678 (15)0.0541 (9)
H540.49790.74480.68880.065*
C550.6329 (3)0.50491 (16)0.7867 (2)0.0462 (8)
C560.6954 (3)0.45096 (17)0.8125 (3)0.0581 (10)
H56A0.69400.44480.87200.070*
H56B0.66560.41730.78400.070*
C570.8694 (4)0.4888 (2)0.8271 (3)0.0757 (13)
H570.86410.51430.87110.091*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ag10.03652 (14)0.04310 (16)0.03750 (14)0.00269 (10)0.00390 (9)0.00264 (10)
P10.0354 (4)0.0509 (5)0.0357 (4)−0.0027 (4)−0.0027 (3)−0.0002 (4)
P20.0310 (4)0.0413 (5)0.0313 (4)−0.0004 (3)0.0032 (3)−0.0013 (3)
P30.0334 (4)0.0447 (5)0.0342 (4)−0.0020 (3)0.0066 (3)0.0015 (3)
O10.0673 (17)0.0433 (15)0.0611 (16)0.0095 (12)0.0191 (13)0.0133 (12)
O20.0553 (17)0.069 (2)0.087 (2)0.0087 (14)0.0180 (15)0.0076 (16)
O1W0.250 (7)0.252 (8)0.285 (8)−0.105 (6)−0.045 (6)0.096 (6)
N10.0535 (18)0.0413 (17)0.0586 (18)0.0103 (14)0.0069 (14)0.0084 (14)
N20.068 (2)0.088 (3)0.075 (2)0.010 (2)0.0119 (19)−0.022 (2)
N30.060 (2)0.111 (4)0.086 (3)0.017 (2)0.015 (2)−0.007 (3)
N40.057 (2)0.093 (3)0.104 (3)0.005 (2)0.006 (2)−0.001 (3)
C10.0352 (16)0.066 (2)0.0310 (15)−0.0001 (15)−0.0027 (13)0.0012 (15)
C20.057 (2)0.082 (3)0.051 (2)0.001 (2)0.0082 (18)−0.008 (2)
C30.059 (3)0.132 (5)0.050 (2)0.012 (3)0.015 (2)0.000 (3)
C40.045 (2)0.143 (5)0.050 (2)−0.002 (3)0.0074 (18)0.026 (3)
C50.055 (2)0.098 (4)0.062 (3)−0.023 (2)0.000 (2)0.023 (2)
C60.050 (2)0.070 (3)0.0447 (19)−0.0103 (18)−0.0005 (16)0.0071 (18)
C70.0456 (18)0.049 (2)0.0388 (17)−0.0014 (15)−0.0008 (14)−0.0041 (14)
C80.056 (2)0.070 (3)0.057 (2)−0.008 (2)0.0052 (18)0.009 (2)
C90.090 (3)0.073 (3)0.065 (3)−0.022 (3)0.012 (2)0.017 (2)
C100.100 (4)0.063 (3)0.057 (2)0.004 (3)−0.002 (2)0.017 (2)
C110.066 (3)0.064 (3)0.059 (2)0.008 (2)−0.017 (2)0.005 (2)
C120.047 (2)0.058 (2)0.054 (2)−0.0012 (17)−0.0085 (16)0.0022 (18)
C130.0351 (16)0.053 (2)0.0387 (16)−0.0029 (14)0.0009 (13)0.0011 (14)
C140.0386 (18)0.064 (2)0.051 (2)0.0021 (16)0.0020 (15)0.0049 (17)
C150.048 (2)0.060 (3)0.079 (3)0.0116 (18)0.0122 (19)0.006 (2)
C160.066 (3)0.063 (3)0.071 (3)−0.001 (2)0.027 (2)−0.012 (2)
C170.080 (3)0.072 (3)0.048 (2)0.000 (2)0.011 (2)−0.009 (2)
C180.059 (2)0.061 (3)0.0411 (18)0.0051 (18)−0.0004 (16)0.0005 (17)
C190.0357 (16)0.0454 (19)0.0411 (17)−0.0010 (13)−0.0001 (13)−0.0018 (14)
C200.058 (3)0.129 (5)0.146 (5)0.026 (3)−0.032 (3)−0.095 (4)
C210.083 (4)0.142 (6)0.181 (7)0.031 (4)−0.058 (4)−0.116 (6)
C220.065 (3)0.078 (3)0.078 (3)−0.010 (2)−0.026 (2)−0.016 (3)
C230.0359 (19)0.098 (4)0.073 (3)−0.003 (2)−0.0028 (18)−0.003 (3)
C240.0374 (19)0.075 (3)0.068 (3)0.0053 (18)−0.0028 (17)−0.019 (2)
C250.0378 (16)0.0366 (17)0.0392 (16)0.0006 (13)0.0078 (13)−0.0010 (13)
C260.0472 (19)0.049 (2)0.0476 (19)−0.0015 (15)−0.0001 (15)0.0076 (16)
C270.058 (2)0.057 (3)0.068 (3)0.0069 (19)0.0126 (19)0.024 (2)
C280.094 (4)0.046 (3)0.099 (4)−0.002 (2)0.028 (3)0.014 (2)
C290.128 (5)0.053 (3)0.083 (3)−0.033 (3)0.006 (3)−0.014 (3)
C300.080 (3)0.051 (2)0.051 (2)−0.017 (2)0.0000 (19)−0.0073 (18)
C310.0297 (14)0.049 (2)0.0399 (16)0.0007 (13)0.0025 (12)−0.0042 (14)
C320.049 (2)0.077 (3)0.065 (3)0.0173 (19)0.0231 (19)0.024 (2)
C330.051 (2)0.092 (4)0.081 (3)0.014 (2)0.035 (2)0.019 (3)
C340.045 (2)0.075 (3)0.076 (3)0.0121 (19)0.0194 (19)−0.002 (2)
C350.056 (2)0.058 (3)0.072 (3)0.0178 (19)0.012 (2)0.006 (2)
C360.0493 (19)0.050 (2)0.0469 (19)0.0073 (16)0.0108 (15)0.0024 (16)
C370.0399 (17)0.045 (2)0.0423 (17)−0.0017 (14)0.0040 (13)0.0015 (14)
C380.044 (2)0.076 (3)0.068 (3)−0.0125 (19)0.0167 (18)−0.009 (2)
C390.042 (2)0.079 (3)0.096 (3)−0.014 (2)0.008 (2)0.008 (3)
C400.063 (3)0.072 (3)0.107 (4)−0.017 (2)−0.014 (3)−0.014 (3)
C410.086 (4)0.089 (4)0.103 (4)−0.022 (3)−0.001 (3)−0.043 (3)
C420.063 (3)0.073 (3)0.071 (3)−0.008 (2)0.014 (2)−0.019 (2)
C430.0335 (16)0.062 (2)0.0363 (16)−0.0066 (14)0.0085 (13)−0.0013 (15)
C440.075 (3)0.069 (3)0.048 (2)−0.025 (2)0.0131 (19)−0.0057 (19)
C450.104 (4)0.109 (4)0.043 (2)−0.046 (3)0.016 (2)−0.015 (2)
C460.083 (3)0.123 (5)0.036 (2)−0.028 (3)0.007 (2)0.005 (2)
C470.061 (2)0.095 (4)0.047 (2)0.005 (2)0.0117 (18)0.021 (2)
C480.053 (2)0.066 (3)0.0447 (19)0.0034 (18)0.0112 (16)0.0062 (17)
C490.0404 (17)0.045 (2)0.0404 (17)0.0014 (14)0.0017 (13)0.0002 (14)
C500.054 (2)0.057 (3)0.080 (3)0.0036 (19)0.016 (2)0.000 (2)
C510.071 (3)0.068 (3)0.093 (3)0.026 (2)0.006 (3)−0.011 (3)
C520.100 (4)0.048 (3)0.080 (3)0.019 (2)−0.014 (3)0.001 (2)
C530.087 (3)0.055 (3)0.075 (3)0.003 (2)0.007 (2)0.020 (2)
C540.056 (2)0.055 (2)0.052 (2)−0.0014 (17)0.0054 (17)0.0058 (17)
C550.053 (2)0.0399 (19)0.0466 (19)0.0054 (15)0.0078 (15)−0.0007 (15)
C560.058 (2)0.047 (2)0.072 (3)0.0082 (17)0.0182 (19)0.0155 (19)
C570.068 (3)0.075 (3)0.084 (3)0.001 (2)0.007 (2)−0.020 (3)
Geometric parameters (Å, °) top
Ag1—O12.360 (3)C22—H220.9300
Ag1—P12.587 (1)C23—C241.3900
Ag1—P22.535 (1)C23—H230.9300
Ag1—P32.496 (1)C24—H240.9300
P1—C11.8309 (19)C25—C261.3900
P1—C71.832 (2)C25—C301.3900
P1—C131.8325 (19)C26—C271.3900
P2—C251.8243 (19)C26—H260.9300
P2—C191.8280 (19)C27—C281.3900
P2—C311.8330 (17)C27—H270.9300
P3—C431.8255 (19)C28—C291.3900
P3—C371.831 (2)C28—H280.9300
P3—C491.838 (2)C29—C301.3900
O1—C551.238 (4)C29—H290.9300
O2—C551.232 (4)C30—H300.9300
O1W—H1W10.8401C31—C321.3900
O1W—H1W20.8400C31—C361.3900
N1—C571.314 (6)C32—C331.3900
N1—N21.328 (5)C32—H320.9300
N1—C561.457 (5)C33—C341.3900
N2—N31.294 (6)C33—H330.9300
N3—N41.345 (6)C34—C351.3900
N4—C571.299 (6)C34—H340.9300
C1—C21.3900C35—C361.3900
C1—C61.3900C35—H350.9300
C2—C31.3900C36—H360.9300
C2—H20.9300C37—C381.3900
C3—C41.3900C37—C421.3900
C3—H30.9300C38—C391.3900
C4—C51.3900C38—H380.9300
C4—H40.9300C39—C401.3900
C5—C61.3900C39—H390.9300
C5—H50.9300C40—C411.3900
C6—H60.9300C40—H400.9300
C7—C81.3900C41—C421.3900
C7—C121.3900C41—H410.9300
C8—C91.3900C42—H420.9300
C8—H80.9300C43—C441.3900
C9—C101.3900C43—C481.3900
C9—H90.9300C44—C451.3900
C10—C111.3900C44—H440.9300
C10—H100.9300C45—C461.3900
C11—C121.3900C45—H450.9300
C11—H110.9300C46—C471.3900
C12—H120.9300C46—H460.9300
C13—C141.3900C47—C481.3900
C13—C181.3900C47—H470.9300
C14—C151.3900C48—H480.9300
C14—H140.9300C49—C501.3900
C15—C161.3900C49—C541.3900
C15—H150.9300C50—C511.3900
C16—C171.3900C50—H500.9300
C16—H160.9300C51—C521.3900
C17—C181.3900C51—H510.9300
C17—H170.9300C52—C531.3900
C18—H180.9300C52—H520.9300
C19—C201.3900C53—C541.3900
C19—C241.3900C53—H530.9300
C20—C211.3900C54—H540.9300
C20—H200.9300C55—C561.540 (5)
C21—C221.3900C56—H56A0.9700
C21—H210.9300C56—H56B0.9700
C22—C231.3900C57—H570.9300
O1—Ag1—P189.04 (8)C19—C24—H24120.0
O1—Ag1—P295.40 (6)C26—C25—C30120.0
O1—Ag1—P3119.38 (7)C26—C25—P2123.67 (13)
P1—Ag1—P2116.87 (3)C30—C25—P2116.23 (13)
P1—Ag1—P3109.52 (3)C27—C26—C25120.0
P2—Ag1—P3121.63 (3)C27—C26—H26120.0
C1—P1—C7103.17 (11)C25—C26—H26120.0
C1—P1—C13104.08 (12)C28—C27—C26120.0
C7—P1—C13102.88 (11)C28—C27—H27120.0
C1—P1—Ag1111.46 (8)C26—C27—H27120.0
C7—P1—Ag1114.58 (9)C27—C28—C29120.0
C13—P1—Ag1118.97 (8)C27—C28—H28120.0
C25—P2—C19103.75 (12)C29—C28—H28120.0
C25—P2—C31102.30 (11)C28—C29—C30120.0
C19—P2—C31102.25 (11)C28—C29—H29120.0
C25—P2—Ag1114.26 (8)C30—C29—H29120.0
C19—P2—Ag1112.76 (9)C29—C30—C25120.0
C31—P2—Ag1119.60 (8)C29—C30—H30120.0
C43—P3—C37102.68 (11)C25—C30—H30120.0
C43—P3—C49104.07 (12)C32—C31—C36120.0
C37—P3—C49104.46 (12)C32—C31—P2121.42 (13)
C43—P3—Ag1110.10 (9)C36—C31—P2118.50 (13)
C37—P3—Ag1122.03 (9)C33—C32—C31120.0
C49—P3—Ag1111.77 (8)C33—C32—H32120.0
C55—O1—Ag1119.5 (2)C31—C32—H32120.0
H1W1—O1W—H1W2109.0C32—C33—C34120.0
C57—N1—N2107.3 (4)C32—C33—H33120.0
C57—N1—C56130.2 (4)C34—C33—H33120.0
N2—N1—C56122.5 (4)C35—C34—C33120.0
N3—N2—N1107.0 (4)C35—C34—H34120.0
N2—N3—N4110.3 (4)C33—C34—H34120.0
C57—N4—N3104.9 (4)C34—C35—C36120.0
C2—C1—C6120.0C34—C35—H35120.0
C2—C1—P1116.43 (14)C36—C35—H35120.0
C6—C1—P1123.51 (14)C35—C36—C31120.0
C1—C2—C3120.0C35—C36—H36120.0
C1—C2—H2120.0C31—C36—H36120.0
C3—C2—H2120.0C38—C37—C42120.0
C4—C3—C2120.0C38—C37—P3121.91 (14)
C4—C3—H3120.0C42—C37—P3118.06 (14)
C2—C3—H3120.0C37—C38—C39120.0
C3—C4—C5120.0C37—C38—H38120.0
C3—C4—H4120.0C39—C38—H38120.0
C5—C4—H4120.0C40—C39—C38120.0
C6—C5—C4120.0C40—C39—H39120.0
C6—C5—H5120.0C38—C39—H39120.0
C4—C5—H5120.0C39—C40—C41120.0
C5—C6—C1120.0C39—C40—H40120.0
C5—C6—H6120.0C41—C40—H40120.0
C1—C6—H6120.0C42—C41—C40120.0
C8—C7—C12120.0C42—C41—H41120.0
C8—C7—P1117.33 (14)C40—C41—H41120.0
C12—C7—P1122.61 (14)C41—C42—C37120.0
C9—C8—C7120.0C41—C42—H42120.0
C9—C8—H8120.0C37—C42—H42120.0
C7—C8—H8120.0C44—C43—C48120.0
C10—C9—C8120.0C44—C43—P3121.45 (14)
C10—C9—H9120.0C48—C43—P3118.10 (14)
C8—C9—H9120.0C45—C44—C43120.0
C11—C10—C9120.0C45—C44—H44120.0
C11—C10—H10120.0C43—C44—H44120.0
C9—C10—H10120.0C44—C45—C46120.0
C10—C11—C12120.0C44—C45—H45120.0
C10—C11—H11120.0C46—C45—H45120.0
C12—C11—H11120.0C47—C46—C45120.0
C11—C12—C7120.0C47—C46—H46120.0
C11—C12—H12120.0C45—C46—H46120.0
C7—C12—H12120.0C48—C47—C46120.0
C14—C13—C18120.0C48—C47—H47120.0
C14—C13—P1117.34 (13)C46—C47—H47120.0
C18—C13—P1122.64 (13)C47—C48—C43120.0
C15—C14—C13120.0C47—C48—H48120.0
C15—C14—H14120.0C43—C48—H48120.0
C13—C14—H14120.0C50—C49—C54120.0
C16—C15—C14120.0C50—C49—P3123.00 (14)
C16—C15—H15120.0C54—C49—P3117.00 (14)
C14—C15—H15120.0C49—C50—C51120.0
C15—C16—C17120.0C49—C50—H50120.0
C15—C16—H16120.0C51—C50—H50120.0
C17—C16—H16120.0C52—C51—C50120.0
C16—C17—C18120.0C52—C51—H51120.0
C16—C17—H17120.0C50—C51—H51120.0
C18—C17—H17120.0C51—C52—C53120.0
C17—C18—C13120.0C51—C52—H52120.0
C17—C18—H18120.0C53—C52—H52120.0
C13—C18—H18120.0C52—C53—C54120.0
C20—C19—C24120.0C52—C53—H53120.0
C20—C19—P2121.75 (14)C54—C53—H53120.0
C24—C19—P2118.05 (14)C53—C54—C49120.0
C21—C20—C19120.0C53—C54—H54120.0
C21—C20—H20120.0C49—C54—H54120.0
C19—C20—H20120.0O2—C55—O1129.1 (4)
C20—C21—C22120.0O2—C55—C56114.5 (3)
C20—C21—H21120.0O1—C55—C56116.4 (3)
C22—C21—H21120.0N1—C56—C55113.9 (3)
C21—C22—C23120.0N1—C56—H56A108.8
C21—C22—H22120.0C55—C56—H56A108.8
C23—C22—H22120.0N1—C56—H56B108.8
C22—C23—C24120.0C55—C56—H56B108.8
C22—C23—H23120.0H56A—C56—H56B107.7
C24—C23—H23120.0N4—C57—N1110.6 (4)
C23—C24—C19120.0N4—C57—H57124.7
C23—C24—H24120.0N1—C57—H57124.7
O1—Ag1—P1—C188.43 (11)C20—C21—C22—C230.0
P3—Ag1—P1—C1−150.59 (10)C21—C22—C23—C240.0
P2—Ag1—P1—C1−7.14 (10)C22—C23—C24—C190.0
O1—Ag1—P1—C7−28.24 (11)C20—C19—C24—C230.0
P3—Ag1—P1—C792.73 (10)P2—C19—C24—C23−174.9 (2)
P2—Ag1—P1—C7−123.82 (9)C19—P2—C25—C26−17.68 (18)
O1—Ag1—P1—C13−150.48 (11)C31—P2—C25—C2688.40 (17)
P3—Ag1—P1—C13−29.50 (10)Ag1—P2—C25—C26−140.85 (13)
P2—Ag1—P1—C13113.95 (10)C19—P2—C25—C30165.90 (15)
O1—Ag1—P2—C25−155.08 (11)C31—P2—C25—C30−88.02 (16)
P3—Ag1—P2—C2575.35 (9)Ag1—P2—C25—C3042.73 (15)
P1—Ag1—P2—C25−63.41 (9)C30—C25—C26—C270.0
O1—Ag1—P2—C1986.78 (12)P2—C25—C26—C27−176.29 (19)
P3—Ag1—P2—C19−42.80 (10)C25—C26—C27—C280.0
P1—Ag1—P2—C19178.44 (9)C26—C27—C28—C290.0
O1—Ag1—P2—C31−33.42 (12)C27—C28—C29—C300.0
P3—Ag1—P2—C31−163.00 (10)C28—C29—C30—C250.0
P1—Ag1—P2—C3158.24 (11)C26—C25—C30—C290.0
O1—Ag1—P3—C4369.53 (12)P2—C25—C30—C29176.56 (18)
P2—Ag1—P3—C43−172.19 (9)C25—P2—C31—C32−27.63 (17)
P1—Ag1—P3—C43−30.79 (9)C19—P2—C31—C3279.60 (18)
O1—Ag1—P3—C37−50.78 (14)Ag1—P2—C31—C32−155.04 (13)
P2—Ag1—P3—C3767.50 (12)C25—P2—C31—C36155.51 (15)
P1—Ag1—P3—C37−151.10 (11)C19—P2—C31—C36−97.26 (17)
O1—Ag1—P3—C49−175.32 (12)Ag1—P2—C31—C3628.09 (18)
P2—Ag1—P3—C49−57.04 (10)C36—C31—C32—C330.0
P1—Ag1—P3—C4984.35 (10)P2—C31—C32—C33−176.81 (19)
P3—Ag1—O1—C55−4.7 (3)C31—C32—C33—C340.0
P2—Ag1—O1—C55−135.9 (3)C32—C33—C34—C350.0
P1—Ag1—O1—C55107.2 (3)C33—C34—C35—C360.0
C57—N1—N2—N3−0.3 (5)C34—C35—C36—C310.0
C56—N1—N2—N3176.3 (4)C32—C31—C36—C350.0
N1—N2—N3—N40.7 (6)P2—C31—C36—C35176.91 (19)
N2—N3—N4—C57−0.8 (6)C43—P3—C37—C3837.41 (19)
C7—P1—C1—C269.95 (15)C49—P3—C37—C38−70.97 (19)
C13—P1—C1—C2177.09 (13)Ag1—P3—C37—C38161.20 (13)
Ag1—P1—C1—C2−53.49 (14)C43—P3—C37—C42−144.53 (17)
C7—P1—C1—C6−113.02 (17)C49—P3—C37—C42107.09 (18)
C13—P1—C1—C6−5.89 (17)Ag1—P3—C37—C42−20.7 (2)
Ag1—P1—C1—C6123.54 (13)C42—C37—C38—C390.0
C6—C1—C2—C30.0P3—C37—C38—C39178.0 (2)
P1—C1—C2—C3177.14 (17)C37—C38—C39—C400.0
C1—C2—C3—C40.0C38—C39—C40—C410.0
C2—C3—C4—C50.0C39—C40—C41—C420.0
C3—C4—C5—C60.0C40—C41—C42—C370.0
C4—C5—C6—C10.0C38—C37—C42—C410.0
C2—C1—C6—C50.0P3—C37—C42—C41−178.1 (2)
P1—C1—C6—C5−176.93 (19)C37—P3—C43—C44−133.54 (16)
C1—P1—C7—C8−164.93 (15)C49—P3—C43—C44−24.87 (18)
C13—P1—C7—C887.03 (16)Ag1—P3—C43—C4495.06 (15)
Ag1—P1—C7—C8−43.59 (16)C37—P3—C43—C4854.13 (17)
C1—P1—C7—C1217.90 (18)C49—P3—C43—C48162.80 (14)
C13—P1—C7—C12−90.15 (17)Ag1—P3—C43—C48−77.27 (14)
Ag1—P1—C7—C12139.24 (13)C48—C43—C44—C450.0
C12—C7—C8—C90.0P3—C43—C44—C45−172.2 (2)
P1—C7—C8—C9−177.26 (19)C43—C44—C45—C460.0
C7—C8—C9—C100.0C44—C45—C46—C470.0
C8—C9—C10—C110.0C45—C46—C47—C480.0
C9—C10—C11—C120.0C46—C47—C48—C430.0
C10—C11—C12—C70.0C44—C43—C48—C470.0
C8—C7—C12—C110.0P3—C43—C48—C47172.45 (19)
P1—C7—C12—C11177.1 (2)C43—P3—C49—C50−53.29 (18)
C1—P1—C13—C1482.03 (16)C37—P3—C49—C5054.06 (17)
C7—P1—C13—C14−170.62 (14)Ag1—P3—C49—C50−172.09 (13)
Ag1—P1—C13—C14−42.71 (16)C43—P3—C49—C54125.82 (16)
C1—P1—C13—C18−99.60 (16)C37—P3—C49—C54−126.83 (15)
C7—P1—C13—C187.75 (17)Ag1—P3—C49—C547.02 (17)
Ag1—P1—C13—C18135.65 (12)C54—C49—C50—C510.0
C18—C13—C14—C150.0P3—C49—C50—C51179.1 (2)
P1—C13—C14—C15178.41 (18)C49—C50—C51—C520.0
C13—C14—C15—C160.0C50—C51—C52—C530.0
C14—C15—C16—C170.0C51—C52—C53—C540.0
C15—C16—C17—C180.0C52—C53—C54—C490.0
C16—C17—C18—C130.0C50—C49—C54—C530.0
C14—C13—C18—C170.0P3—C49—C54—C53−179.14 (19)
P1—C13—C18—C17−178.32 (19)Ag1—O1—C55—O212.9 (6)
C25—P2—C19—C20119.2 (2)Ag1—O1—C55—C56−166.5 (3)
C31—P2—C19—C2013.0 (2)C57—N1—C56—C5568.5 (6)
Ag1—P2—C19—C20−116.69 (18)N2—N1—C56—C55−107.2 (4)
C25—P2—C19—C24−66.1 (2)O2—C55—C56—N1−177.5 (3)
C31—P2—C19—C24−172.18 (18)O1—C55—C56—N12.1 (5)
Ag1—P2—C19—C2458.1 (2)N3—N4—C57—N10.6 (6)
C24—C19—C20—C210.0N2—N1—C57—N4−0.2 (6)
P2—C19—C20—C21174.7 (2)C56—N1—C57—N4−176.5 (4)
C19—C20—C21—C220.0
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O20.842.012.800 (8)157
Table 1
Selected geometric parameters (Å) top
Ag1—O12.360 (3)Ag1—P22.535 (1)
Ag1—P12.587 (1)Ag1—P32.496 (1)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O20.842.012.800 (8)157
Acknowledgements top

We thank the Important Project of Hubei Provincial Education Office (Z20091301), the Natural Science Foundation of Hubei Province of China (2008CDB030) and the University of Malaya for supporting this study.

references
References top

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.

Dong, W.-W., Zhao, J. & Xu, L. (2008). J. Solid State Chem. 181, 1149–1154.

Rigaku (2002). CrystalClear. Rigaku Corporation, Tokyo, Japan.

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

Westrip, S. P. (2009). publCIF. In preparation.