[μ-N,N′-Bis(diphenyl­phosphinometh­yl)benzene-1,4-diamine-κ2P:P′]bis­[(2,2′-bipyridine-κ2N,N′)silver(I)] bis­(per­chlorate) acetone disolvate

Gui, L.-C.; Ni, Q.-L.; Jiang, X.-F.; Zeng, J.-Q.; Wang, X.-J.

doi:10.1107/S1600536809014871

metal-organic compounds

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 65| Part 5| May 2009| Pages m589-m590

doi:10.1107/S1600536809014871

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[μ-N,N′-Bis(diphenylphosphinomethyl)benzene-1,4-diamine-κ²P:P′]bis[(2,2′-bipyridine-κ²N,N′)silver(I)] bis(perchlorate) acetone disolvate

Liu-Cheng Gui,^a ^* Qing-Ling Ni,^a Xuan-Feng Jiang,^a Jian-Qiang Zeng ^a and Xiu-Jian Wang ^a

^aSchool of Chemistry and Chemical Engineering, Guangxi Normal University, Guilin 541004, People's Republic of China
^*Correspondence e-mail: guiliucheng@yahoo.com.cn

(Received 14 April 2009; accepted 22 April 2009; online 30 April 2009)

The title complex, [Ag₂(C₁₀H₈N₂)₂(C₃₂H₃₀N₂P₂)](ClO₄)₂·2CH₃COCH₃, is a centrosymmetric dimer with pairs of Ag^I atoms bridged by N,N′-bis(diphenylphosphinomethyl)benzene-1,4-diamine ligands. In addition, each Ag^I atom is coordinated by one chelating 2,2′-bipyridine ligand, giving a distorted trigonal coordination environment.

Related literature

Diphosphine ligands effectively stabilize low-valent d¹⁰ metals complexes due to their electronic and steric characteristics, see: Meijboom et al. (2009 ); Ogasawara et al. (2000 ). Adducts of chelating polypyridyl ligands such as 2,2′-bipyridine and 1,10-phenanthroline (phen) always exhibit strong ligand–metal charge-transfer (LMCT) or metal–ligand charge-transfer (MLCT) absorption bands in the visible spectrum, see: Armaroli (2001 ). For a series of Ag^I and Cu^I complexes containing both diphosphine and chelating polypyridyl ligands which exhibit interesting photoluminescent properties at low temperature or even at room temperature, see: Wang et al. (2008 ). For the synthesis of N,N-bis[(diphenylphosphino)methyl]-benzene-1,4-diamine, see: Durran et al. (2000 ); Hellmann et al. (1962 ). For related structures, see: Effendy et al. (2007 ); Zhang et al. (2003 ).

Experimental

Crystal data

[Ag₂(C₁₀H₈N₂)₂(C₃₂H₃₀N₂P₂)](ClO₄)₂·2C₃H₆O
M_r = 1347.68
Monoclinic, P 2₁ /c
a = 10.6372 (13) Å
b = 15.8958 (19) Å
c = 16.6684 (19) Å
β = 91.432 (3)°
V = 2817.5 (6) Å³
Z = 2
Mo Kα radiation
μ = 0.91 mm⁻¹
T = 173 K
0.38 × 0.24 × 0.20 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1998 ) T_min = 0.657, T_max = 0.833
14114 measured reflections
6120 independent reflections
3944 reflections with I > 2σ(I)
R_int = 0.044

Refinement

R[F² > 2σ(F²)] = 0.046
wR(F²) = 0.132
S = 1.05
6120 reflections
361 parameters
H-atom parameters constrained
Δρ_max = 1.02 e Å⁻³
Δρ_min = −0.68 e Å⁻³

Data collection: SMART (Bruker, 1998 ); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809014871/at2766sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809014871/at2766Isup2.hkl

checkCIF report

Comment top

There has been great interest in d¹⁰ metals complexes containing diphosphine and polypyridyl ligands because of two main reasons: the first is diphosphine ligands effectively stabilize low-valent d¹⁰ metals complexes due to their electronic and steric characteristics (Meijboom et al., 2009; Ogasawara et al., 2000), and the other is the chelating polypyridyl ligands such as 2,2'-bipyridine and 1,10-phenanthroline (phen) are present of low-energy orbitals, the adducts always exhibit strong Ligand-metal charge-transfer (LMCT) or Metal-ligand charge-transfer (MLCT) absorption bands in the visible spectrum (Armaroli, 2001). In the past, we have obtained a series of Ag^I and Cu(I) complexes containing both diphosphine and chelating polypyridyl ligands, from which we found that these complexes all exhibit interesting photoluminescent properties at low temperature or even at room temperature (Wang et al., 2008). Here we report the crystal and molecular structure of[Ag₂(C₁₀H₈N₂)₂(C₃₂H₃₀N₂P₂)](ClO₄)₂.2CH₃COCH₃, (I). This work complements and extends our structural characterization of d¹⁰ metals complexes containing diphosphine and polypyridyl ligands.

Related literature top

Diphosphine ligands effectively stabilize low-valent d¹⁰ metals complexes due to their electronic and steric characteristics, see: Meijboom et al. (2009); Ogasawara et al. (2000). Adducts of chelating polypyridyl ligands such as 2,2'-bipyridine and 1,10-phenanthroline (phen) always exhibit strong ligand–metal charge-transfer (LMCT) or metal–ligand charge-transfer (MLCT) absorption bands in the visible spectrum, see: Armaroli (2001). For a series of Ag^I and Cu(I) complexes containing both diphosphine and chelating polypyridyl ligands which exhibit interesting photoluminescent properties at low temperature or even at room temperature, see: Wang et al. (2008). For the synthesis of N,N-bis[(diphenylphosphino)methyl]-benzene-1,4-diamine, see: Durran et al. (2000); Hellmann et al. (1962). For related structures, see: Effendy et al. (2007); Zhang et al. (2003).

Experimental top

The synthesis of (I) was carried out by the reaction of AgClO₄.H₂O (0.045 g, 0.2 mmol), 2,2'-bipyridine (0.032 g, 0.2 mmol) and N,N-bis[(diphenylphosphino)methyl]-benzene-1,4-diamine (0.0504 g, 0.1 mmol, synthesized according to literature (Durran, et al., 2000; Hellmann et al., 1962) in acetonitrile-acetone (7 ml with a ratio of 4: 3) solution, the resulting orange red solution was allowed to stir for 0.5 h at room temperature.Then by slow diffusion of diethyl ether into the solution, block red crystals were formed suitable for X-ray diffraction analysis.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

Fig. 1. View of (I), showing 30% probability displacement ellipsoids and atom-numbering scheme for the contents of the asymmetric unit. [Symmetry code: (i) -x, y + 1/2, -z + 1/2]

[µ-N,N'-Bis(diphenylphosphinomethyl)benzene-1,4-diamine- κ²P:P']bis[(2,2'-bipyridine-κ²N,N')silver(I)] bis(perchlorate) acetone disolvate top

Crystal data top

[Ag₂(C₁₀H₈N₂)₂(C₃₂H₃₀N₂P₂)](ClO₄)₂·2C₃H₆O	F(000) = 1372
M_r = 1347.68	D_x = 1.589 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 3856 reflections
a = 10.6372 (13) Å	θ = 2.3–25.9°
b = 15.8958 (19) Å	µ = 0.91 mm⁻¹
c = 16.6684 (19) Å	T = 173 K
β = 91.432 (3)°	Block, red
V = 2817.5 (6) Å³	0.38 × 0.24 × 0.20 mm
Z = 2

Data collection top

Bruker SMART CCD area-detector diffractometer	6120 independent reflections
Radiation source: fine-focus sealed tube	3944 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.044
ω scans	θ_max = 27.1°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1998)	h = −6→13
T_min = 0.657, T_max = 0.833	k = −19→20
14114 measured reflections	l = −21→18

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.132	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0655P)²] where P = (F_o² + 2F_c²)/3
6120 reflections	(Δ/σ)_max < 0.001
361 parameters	Δρ_max = 1.02 e Å⁻³
0 restraints	Δρ_min = −0.68 e Å⁻³

Crystal data top

[Ag₂(C₁₀H₈N₂)₂(C₃₂H₃₀N₂P₂)](ClO₄)₂·2C₃H₆O	V = 2817.5 (6) Å³
M_r = 1347.68	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 10.6372 (13) Å	µ = 0.91 mm⁻¹
b = 15.8958 (19) Å	T = 173 K
c = 16.6684 (19) Å	0.38 × 0.24 × 0.20 mm
β = 91.432 (3)°

Data collection top

Bruker SMART CCD area-detector diffractometer	6120 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1998)	3944 reflections with I > 2σ(I)
T_min = 0.657, T_max = 0.833	R_int = 0.044
14114 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.046	0 restraints
wR(F²) = 0.132	H-atom parameters constrained
S = 1.05	Δρ_max = 1.02 e Å⁻³
6120 reflections	Δρ_min = −0.68 e Å⁻³
361 parameters

Special details top

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	U_iso*/U_eq
Ag1	0.21755 (3)	0.40337 (2)	0.14606 (2)	0.03172 (13)
Cl1	0.48508 (14)	0.89672 (9)	0.20183 (10)	0.0534 (4)
P1	0.06386 (11)	0.32350 (7)	0.20844 (6)	0.0217 (2)
O1	0.5433 (6)	0.8587 (4)	0.2698 (4)	0.124 (2)
O2	0.5382 (5)	0.8626 (4)	0.1311 (4)	0.120 (2)
O3	0.5114 (4)	0.9841 (3)	0.2031 (3)	0.0788 (14)
O4	0.3559 (4)	0.8806 (3)	0.2030 (3)	0.0819 (15)
O5	−0.2686 (4)	0.1981 (3)	0.0953 (3)	0.0705 (13)
N1	−0.0972 (4)	0.3598 (2)	0.0811 (2)	0.0304 (9)
H1A	−0.1320	0.3197	0.0517	0.037*
N2	0.2913 (4)	0.4064 (2)	0.0167 (2)	0.0300 (8)
N3	0.3101 (3)	0.5301 (2)	0.1275 (2)	0.0265 (8)
C1	−0.0460 (4)	0.4297 (3)	0.0420 (2)	0.0231 (9)
C2	−0.0201 (4)	0.5056 (3)	0.0812 (2)	0.0256 (10)
H2A	−0.0332	0.5102	0.1372	0.031*
C3	−0.0246 (4)	0.4255 (3)	−0.0395 (2)	0.0259 (10)
H3A	−0.0407	0.3744	−0.0674	0.031*
C4	−0.0954 (4)	0.3509 (3)	0.1662 (2)	0.0280 (10)
H4A	−0.1557	0.3065	0.1810	0.034*
H4B	−0.1235	0.4043	0.1905	0.034*
C5	0.0783 (4)	0.2100 (3)	0.1927 (2)	0.0243 (9)
C6	−0.0183 (5)	0.1549 (3)	0.2088 (2)	0.0297 (10)
H6A	−0.0961	0.1757	0.2274	0.036*
C7	−0.0017 (5)	0.0684 (3)	0.1979 (3)	0.0354 (12)
H7A	−0.0685	0.0307	0.2086	0.042*
C8	0.1110 (5)	0.0380 (3)	0.1719 (3)	0.0375 (12)
H8A	0.1212	−0.0205	0.1628	0.045*
C9	0.2093 (5)	0.0925 (3)	0.1589 (3)	0.0372 (12)
H9A	0.2884	0.0710	0.1431	0.045*
C10	0.1934 (5)	0.1786 (3)	0.1686 (3)	0.0320 (11)
H10A	0.2610	0.2160	0.1589	0.038*
C11	0.0445 (4)	0.3334 (2)	0.3160 (2)	0.0229 (9)
C12	−0.0679 (4)	0.3110 (3)	0.3519 (3)	0.0284 (10)
H12A	−0.1358	0.2891	0.3202	0.034*
C13	−0.0799 (5)	0.3207 (3)	0.4338 (3)	0.0330 (11)
H13A	−0.1567	0.3059	0.4581	0.040*
C14	0.0169 (6)	0.3513 (3)	0.4800 (3)	0.0411 (13)
H14A	0.0074	0.3579	0.5362	0.049*
C15	0.1292 (5)	0.3730 (3)	0.4454 (3)	0.0414 (13)
H15A	0.1972	0.3937	0.4777	0.050*
C16	0.1419 (4)	0.3644 (3)	0.3634 (3)	0.0294 (10)
H16A	0.2186	0.3800	0.3395	0.035*
C17	0.2814 (5)	0.3429 (3)	−0.0352 (3)	0.0375 (12)
H17A	0.2563	0.2892	−0.0164	0.045*
C18	0.3065 (5)	0.3529 (4)	−0.1160 (3)	0.0444 (13)
H18A	0.2973	0.3070	−0.1521	0.053*
C19	0.3447 (5)	0.4298 (4)	−0.1426 (3)	0.0447 (14)
H19A	0.3631	0.4378	−0.1975	0.054*
C20	0.3565 (4)	0.4960 (3)	−0.0888 (3)	0.0355 (11)
H20A	0.3844	0.5497	−0.1060	0.043*
C21	0.3265 (4)	0.4821 (3)	−0.0092 (3)	0.0284 (10)
C22	0.3353 (4)	0.5508 (3)	0.0512 (3)	0.0258 (10)
C23	0.3680 (4)	0.6325 (3)	0.0318 (3)	0.0365 (12)
H23A	0.3830	0.6474	−0.0224	0.044*
C24	0.3788 (5)	0.6924 (3)	0.0920 (3)	0.0443 (13)
H24A	0.4035	0.7483	0.0799	0.053*
C25	0.3534 (5)	0.6699 (3)	0.1697 (3)	0.0402 (12)
H25A	0.3601	0.7097	0.2120	0.048*
C26	0.3187 (4)	0.5892 (3)	0.1843 (3)	0.0327 (11)
H26A	0.2994	0.5740	0.2377	0.039*
C27	−0.4843 (6)	0.1744 (5)	0.0964 (5)	0.087 (2)
H27A	−0.4852	0.2307	0.1203	0.131*
H27B	−0.5191	0.1338	0.1342	0.131*
H27C	−0.5352	0.1743	0.0466	0.131*
C28	−0.3312 (7)	0.0678 (4)	0.0406 (4)	0.075 (2)
H28A	−0.2411	0.0606	0.0318	0.112*
H28B	−0.3773	0.0651	−0.0110	0.112*
H28C	−0.3607	0.0229	0.0758	0.112*
C29	−0.3534 (6)	0.1507 (4)	0.0787 (3)	0.0477 (14)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ag1	0.0352 (2)	0.0282 (2)	0.0323 (2)	−0.00696 (17)	0.01181 (15)	0.00382 (16)
Cl1	0.0401 (8)	0.0428 (8)	0.0772 (10)	−0.0068 (6)	0.0019 (7)	−0.0166 (7)
P1	0.0262 (6)	0.0194 (5)	0.0198 (5)	−0.0024 (5)	0.0046 (5)	0.0026 (4)
O1	0.097 (5)	0.105 (4)	0.169 (6)	−0.012 (4)	−0.061 (5)	0.038 (4)
O2	0.073 (4)	0.116 (4)	0.173 (6)	−0.027 (3)	0.036 (4)	−0.097 (4)
O3	0.089 (4)	0.056 (3)	0.092 (3)	−0.036 (3)	0.017 (3)	−0.023 (2)
O4	0.035 (2)	0.070 (3)	0.142 (5)	−0.010 (2)	0.009 (3)	−0.023 (3)
O5	0.057 (3)	0.086 (3)	0.069 (3)	−0.019 (3)	0.002 (2)	−0.014 (2)
N1	0.038 (2)	0.029 (2)	0.0236 (19)	−0.0080 (18)	−0.0099 (17)	0.0009 (16)
N2	0.027 (2)	0.029 (2)	0.034 (2)	−0.0056 (17)	0.0079 (17)	−0.0015 (17)
N3	0.0234 (19)	0.029 (2)	0.0273 (19)	−0.0006 (16)	−0.0018 (16)	0.0013 (16)
C1	0.020 (2)	0.022 (2)	0.027 (2)	0.0009 (18)	−0.0072 (18)	0.0053 (17)
C2	0.026 (2)	0.031 (2)	0.019 (2)	0.002 (2)	−0.0001 (18)	0.0013 (18)
C3	0.032 (3)	0.023 (2)	0.022 (2)	0.0005 (19)	−0.007 (2)	−0.0028 (17)
C4	0.030 (3)	0.026 (2)	0.027 (2)	0.000 (2)	−0.002 (2)	0.0050 (19)
C5	0.033 (3)	0.022 (2)	0.019 (2)	0.0010 (19)	0.0032 (19)	0.0021 (17)
C6	0.034 (3)	0.030 (3)	0.025 (2)	−0.005 (2)	0.000 (2)	−0.0024 (19)
C7	0.054 (3)	0.026 (2)	0.026 (2)	−0.010 (2)	−0.005 (2)	0.0019 (19)
C8	0.060 (4)	0.021 (2)	0.031 (2)	0.001 (2)	0.004 (2)	−0.001 (2)
C9	0.042 (3)	0.034 (3)	0.036 (3)	0.015 (2)	0.004 (2)	0.001 (2)
C10	0.035 (3)	0.028 (3)	0.033 (2)	0.002 (2)	0.004 (2)	0.002 (2)
C11	0.033 (3)	0.012 (2)	0.025 (2)	0.0045 (18)	0.0110 (19)	0.0015 (17)
C12	0.029 (3)	0.028 (2)	0.028 (2)	−0.003 (2)	0.002 (2)	−0.0022 (19)
C13	0.041 (3)	0.035 (3)	0.023 (2)	−0.003 (2)	0.007 (2)	0.000 (2)
C14	0.065 (4)	0.035 (3)	0.023 (2)	0.008 (3)	0.001 (3)	−0.002 (2)
C15	0.050 (3)	0.046 (3)	0.027 (2)	0.001 (3)	−0.010 (2)	−0.002 (2)
C16	0.030 (3)	0.029 (2)	0.029 (2)	−0.004 (2)	0.000 (2)	0.003 (2)
C17	0.037 (3)	0.041 (3)	0.035 (3)	−0.006 (2)	0.002 (2)	−0.005 (2)
C18	0.042 (3)	0.056 (4)	0.035 (3)	−0.004 (3)	0.005 (2)	−0.013 (3)
C19	0.034 (3)	0.075 (4)	0.026 (3)	0.009 (3)	0.003 (2)	0.007 (3)
C20	0.028 (3)	0.045 (3)	0.034 (3)	0.000 (2)	0.004 (2)	0.008 (2)
C21	0.022 (2)	0.032 (3)	0.031 (2)	−0.002 (2)	0.0059 (19)	0.007 (2)
C22	0.017 (2)	0.030 (2)	0.030 (2)	−0.0009 (19)	−0.0068 (18)	0.0070 (19)
C23	0.031 (3)	0.039 (3)	0.039 (3)	−0.010 (2)	−0.013 (2)	0.012 (2)
C24	0.044 (3)	0.029 (3)	0.059 (3)	−0.006 (2)	−0.014 (3)	0.007 (2)
C25	0.034 (3)	0.032 (3)	0.054 (3)	0.000 (2)	−0.001 (3)	−0.002 (2)
C26	0.027 (2)	0.034 (3)	0.036 (3)	−0.002 (2)	0.006 (2)	−0.003 (2)
C27	0.057 (5)	0.088 (5)	0.119 (6)	0.012 (4)	0.033 (4)	0.029 (5)
C28	0.081 (5)	0.057 (4)	0.088 (5)	−0.012 (4)	0.024 (4)	−0.003 (4)
C29	0.047 (4)	0.051 (3)	0.045 (3)	−0.006 (3)	0.005 (3)	0.010 (3)

Geometric parameters (Å, º) top

Ag1—N3	2.267 (3)	C11—C16	1.378 (6)
Ag1—N2	2.314 (4)	C11—C12	1.397 (6)
Ag1—P1	2.3348 (11)	C12—C13	1.383 (6)
Cl1—O4	1.398 (4)	C12—H12A	0.9500
Cl1—O1	1.413 (6)	C13—C14	1.361 (7)
Cl1—O3	1.416 (4)	C13—H13A	0.9500
Cl1—O2	1.428 (5)	C14—C15	1.383 (7)
P1—C11	1.817 (4)	C14—H14A	0.9500
P1—C5	1.830 (4)	C15—C16	1.383 (6)
P1—C4	1.870 (4)	C15—H15A	0.9500
O5—C29	1.203 (6)	C16—H16A	0.9500
N1—C1	1.404 (5)	C17—C18	1.388 (7)
N1—C4	1.425 (5)	C17—H17A	0.9500
N1—H1A	0.8800	C18—C19	1.365 (8)
N2—C17	1.331 (6)	C18—H18A	0.9500
N2—C21	1.336 (5)	C19—C20	1.386 (7)
N3—C26	1.335 (5)	C19—H19A	0.9500
N3—C22	1.346 (5)	C20—C21	1.390 (6)
C1—C3	1.384 (6)	C20—H20A	0.9500
C1—C2	1.397 (6)	C21—C22	1.487 (6)
C2—C3ⁱ	1.387 (6)	C22—C23	1.386 (6)
C2—H2A	0.9500	C23—C24	1.387 (7)
C3—C2ⁱ	1.387 (6)	C23—H23A	0.9500
C3—H3A	0.9500	C24—C25	1.376 (7)
C4—H4A	0.9900	C24—H24A	0.9500
C4—H4B	0.9900	C25—C26	1.358 (6)
C5—C6	1.383 (6)	C25—H25A	0.9500
C5—C10	1.390 (6)	C26—H26A	0.9500
C6—C7	1.397 (6)	C27—C29	1.480 (8)
C6—H6A	0.9500	C27—H27A	0.9800
C7—C8	1.372 (7)	C27—H27B	0.9800
C7—H7A	0.9500	C27—H27C	0.9800
C8—C9	1.379 (7)	C28—C29	1.484 (8)
C8—H8A	0.9500	C28—H28A	0.9800
C9—C10	1.390 (6)	C28—H28B	0.9800
C9—H9A	0.9500	C28—H28C	0.9800
C10—H10A	0.9500

N3—Ag1—N2	72.30 (12)	C13—C12—C11	119.7 (4)
N3—Ag1—P1	148.80 (9)	C13—C12—H12A	120.1
N2—Ag1—P1	133.15 (9)	C11—C12—H12A	120.1
O4—Cl1—O1	108.8 (4)	C14—C13—C12	120.7 (5)
O4—Cl1—O3	111.9 (3)	C14—C13—H13A	119.6
O1—Cl1—O3	109.0 (3)	C12—C13—H13A	119.6
O4—Cl1—O2	110.5 (3)	C13—C14—C15	120.2 (4)
O1—Cl1—O2	109.0 (4)	C13—C14—H14A	119.9
O3—Cl1—O2	107.6 (3)	C15—C14—H14A	119.9
C11—P1—C5	103.83 (17)	C14—C15—C16	119.6 (5)
C11—P1—C4	103.2 (2)	C14—C15—H15A	120.2
C5—P1—C4	104.8 (2)	C16—C15—H15A	120.2
C11—P1—Ag1	119.36 (15)	C11—C16—C15	120.7 (4)
C5—P1—Ag1	114.18 (14)	C11—C16—H16A	119.6
C4—P1—Ag1	110.07 (14)	C15—C16—H16A	119.6
C1—N1—C4	123.0 (4)	N2—C17—C18	122.0 (5)
C1—N1—H1A	118.5	N2—C17—H17A	119.0
C4—N1—H1A	118.5	C18—C17—H17A	119.0
C17—N2—C21	119.4 (4)	C19—C18—C17	118.9 (5)
C17—N2—Ag1	124.5 (3)	C19—C18—H18A	120.6
C21—N2—Ag1	115.1 (3)	C17—C18—H18A	120.6
C26—N3—C22	119.1 (4)	C18—C19—C20	119.5 (4)
C26—N3—Ag1	123.4 (3)	C18—C19—H19A	120.2
C22—N3—Ag1	116.3 (3)	C20—C19—H19A	120.2
C3—C1—C2	117.7 (4)	C19—C20—C21	118.5 (5)
C3—C1—N1	119.6 (4)	C19—C20—H20A	120.7
C2—C1—N1	122.7 (4)	C21—C20—H20A	120.7
C3ⁱ—C2—C1	120.9 (4)	N2—C21—C20	121.6 (4)
C3ⁱ—C2—H2A	119.5	N2—C21—C22	117.1 (4)
C1—C2—H2A	119.5	C20—C21—C22	121.2 (4)
C1—C3—C2ⁱ	121.4 (4)	N3—C22—C23	120.4 (4)
C1—C3—H3A	119.3	N3—C22—C21	116.7 (4)
C2ⁱ—C3—H3A	119.3	C23—C22—C21	122.8 (4)
N1—C4—P1	112.8 (3)	C22—C23—C24	119.4 (4)
N1—C4—H4A	109.0	C22—C23—H23A	120.3
P1—C4—H4A	109.0	C24—C23—H23A	120.3
N1—C4—H4B	109.0	C25—C24—C23	119.2 (5)
P1—C4—H4B	109.0	C25—C24—H24A	120.4
H4A—C4—H4B	107.8	C23—C24—H24A	120.4
C6—C5—C10	119.5 (4)	C26—C25—C24	118.4 (5)
C6—C5—P1	122.1 (3)	C26—C25—H25A	120.8
C10—C5—P1	118.3 (3)	C24—C25—H25A	120.8
C5—C6—C7	120.1 (4)	N3—C26—C25	123.4 (4)
C5—C6—H6A	120.0	N3—C26—H26A	118.3
C7—C6—H6A	120.0	C25—C26—H26A	118.3
C8—C7—C6	120.1 (5)	C29—C27—H27A	109.5
C8—C7—H7A	120.0	C29—C27—H27B	109.5
C6—C7—H7A	120.0	H27A—C27—H27B	109.5
C7—C8—C9	120.1 (4)	C29—C27—H27C	109.5
C7—C8—H8A	120.0	H27A—C27—H27C	109.5
C9—C8—H8A	120.0	H27B—C27—H27C	109.5
C8—C9—C10	120.3 (5)	C29—C28—H28A	109.5
C8—C9—H9A	119.9	C29—C28—H28B	109.5
C10—C9—H9A	119.9	H28A—C28—H28B	109.5
C9—C10—C5	119.9 (4)	C29—C28—H28C	109.5
C9—C10—H10A	120.0	H28A—C28—H28C	109.5
C5—C10—H10A	120.0	H28B—C28—H28C	109.5
C16—C11—C12	119.0 (4)	O5—C29—C27	119.9 (6)
C16—C11—P1	119.6 (3)	O5—C29—C28	122.0 (6)
C12—C11—P1	121.3 (3)	C27—C29—C28	118.2 (6)

Symmetry code: (i) −x, −y+1, −z.

Experimental details

Crystal data
Chemical formula	[Ag₂(C₁₀H₈N₂)₂(C₃₂H₃₀N₂P₂)](ClO₄)₂·2C₃H₆O
M_r	1347.68
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	173
a, b, c (Å)	10.6372 (13), 15.8958 (19), 16.6684 (19)
β (°)	91.432 (3)
V (Å³)	2817.5 (6)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.91
Crystal size (mm)	0.38 × 0.24 × 0.20

Data collection
Diffractometer	Bruker SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1998)
T_min, T_max	0.657, 0.833
No. of measured, independent and observed [I > 2σ(I)] reflections	14114, 6120, 3944
R_int	0.044
(sin θ/λ)_max (Å⁻¹)	0.640

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.046, 0.132, 1.05
No. of reflections	6120
No. of parameters	361
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.02, −0.68

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Acknowledgements

This work was supported by the Programme for Excellent Talents in Guangxi Higher Education Institutions of China.

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