Poly[[{μ3-tris­[2-(4-phenyl-1,2,3-triazol-1-yl)eth­yl]amine}silver(I)] hexa­fluorido­phosphate]

Ohi, H.; Shimizu, M.; Obata, M.; Funabiki, T.; Yano, S.

doi:10.1107/S1600536808028298

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 10| October 2008| Pages m1256-m1257

doi:10.1107/S1600536808028298

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Poly[[{μ₃-tris[2-(4-phenyl-1,2,3-triazol-1-yl)ethyl]amine}silver(I)] hexafluoridophosphate]

Hiromi Ohi,^a Mayumi Shimizu,^b Makoto Obata,^b Takuzo Funabiki ^c and Shigenobu Yano ^a ^*

^aEndowed Research Section, Photomedical Science, Innovative Collaboration Center, Kyoto University, Kyoto-daigaku Katsura, Nishikyo-ku, Kyoto 615-8520, Japan, ^bGraduate School of Humanities and Sciences, Nara Women's University, Kitauoyanishimachi, Nara 630-8506, Japan, and ^cDepartment of Molecular Chemistry and Biochemistry, Factory of Science and Engineering, Doshisha University, Kyotanabe, Kyoto 610-0321, Japan
^*Correspondence e-mail: yano@icc.kyoto-u.ac.jp

(Received 1 September 2008; accepted 4 September 2008; online 13 September 2008)

The title compound, {[Ag(L)]PF₆)_n {L is tris[2-(4-phenyl-1,2,3-triazol-1-yl)ethyl]amine, C₃₀H₃₀N₁₀}, consists of alternating two-dimensional cationic layers of [Ag(L)]⁺ and anionic PF₆⁻ layers. Each Ag^I atom is three coordinated in a T-shaped geometry by three N atoms from three ligands. Each ligand links three Ag^I atoms, generating a two-dimensional network structure with two different metallacycles, A and B. In A, eight coordination units from four ligands connect four Ag^I atoms, forming a 48-membered ring. In B, four coordination units from two ligands link two Ag^I atoms, forming a 24-membered ring. Each B ring is surrounded by four A rings, and each A ring has four A and four B rings as neighbours. This cationic layer thus generates a 4.8² topology network, with each Ag^I centre and ligand acting as a three-connected topological node.

Related literature

For related literature, see: Newkome et al. (1999 ); Robin & Fromm (2006 ); Ohi et al. (2004 , 2005 ); Obata et al. (2008 ).

Experimental

Crystal data

[Ag(C₃₀H₃₀N₁₀)]PF₆
M_r = 783.47
Monoclinic, P 2₁ /n
a = 14.893 (3) Å
b = 14.935 (3) Å
c = 15.735 (3) Å
β = 112.646 (5)°
V = 3230.2 (12) Å³
Z = 4
Mo Kα radiation
μ = 0.75 mm⁻¹
T = 193.1 K
0.30 × 0.15 × 0.05 mm

Data collection

Rigaku Mercury diffractometer
Absorption correction: multi-scan (Jacobson, 1998 ) T_min = 0.776, T_max = 0.963
31971 measured reflections
7326 independent reflections
4647 reflections with F² > 2σ(F²)
R_int = 0.075

Refinement

R[F² > 2σ(F²)] = 0.054
wR(F²) = 0.055
S = 1.03
7326 reflections
463 parameters
All H-atom parameters refined
Δρ_max = 3.48 e Å⁻³
Δρ_min = −2.33 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Ag1—N4	2.208 (2)
Ag1—N7ⁱ	2.210 (3)
Ag1—N10ⁱⁱ	2.268 (2)

N4—Ag1—N7ⁱ	132.43 (10)
N4—Ag1—N10ⁱⁱ	114.02 (10)
N7ⁱ—Ag1—N10ⁱⁱ	113.51 (10)
Symmetry codes: (i) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) $[x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: CrystalClear (Rigaku/MSC & Rigaku, 2006 ); cell refinement: CrystalClear; data reduction: CrystalStructure; program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003 ); molecular graphics: ORTEPIII (Burnett & Johnson, 1996 ); software used to prepare material for publication: CrystalStructure (Rigaku/MSC & Rigaku, 2006).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808028298/bt2780sup1.cif

Structure factors: contains datablocks I, I. DOI: 10.1107/S1600536808028298/bt2780Isup2.hkl

checkCIF report

Comment top

Coordination polymer complexes have attracted much attention due to their various intriguing framework topologies and their unique properties such as magnetism, physical gas adsorption, ion-exchange, heterogeneous catalysis, and so on (Newkome et al., 1999; Robin et al., 2006). We have recently demonstrated that a C₃ symmetric tripodal tripyridine ligand consisting of a 1,3,5-triethylbenzene spacer can be adopted in coordination polymer chemistry to give one- and/or two-dimensional coordination polymer complexes with a variety of network topology (Ohi et al., 2004, 2005). In this study, we synthesized a new C₃ symmetric lingad (L) consisting of triethylamine as the spacer and three 1,2,3-triazole groups as the metal binding site by using Huisgen reaction and used this ligand to synthesize a new Ag^I complex, [[Ag^I(L)](PF₆)]_n (I). We report here the crystal structure of Ag^I complex.

In the title compound (I), the asymmetric unit contained one ligand molecular, one Ag^I ion, and one PF₆^- counterion. No solvent molecules were incorporated in the structure. As shown in Fig. 1, each Ag^I ion features a T-shaped coordination geometry, being coordinated by three nitrogen atoms from three ligands [Ag—N: 2.208 (2)–2.268 (2) Å; N—Ag—N: 113.51 (10)–132.43 (10)°], and each ligand links three Ag^I atoms to generate a two-dimensional network structure with two different metallacycles A and B. In A, eight coordination moieties from four ligands connected four Ag^I atoms to form a 48-membered ring. In B, four coordination moieties from two ligands link two Ag^I atoms to form 24-membered ring. Each B ring is surrounded by four A rings, and each A ring neighbors upon four A and four B rings. Thus, this sheet generates a rare 4.8² topology network with each Ag^I center and lingad acting as a three-connected topological node (Fig. 2a). The two-dimensional polymer sheets are stacked alternate arranging cationic two-dimensional layers of [Ag^I(L)]⁺ and anionic (PF₆^-) layers to form laminated structure (Fig. 2b), where no specific interaction is probably between the sheets.

Related literature top

For related literature, see: Newkome et al. (1999); Robin et al. (2006); Ohi et al. (2004, 2005); Obata et al. (2008).

Experimental top

The ligand tris((4-phenyl-1,2,3-triazole-1-yl)ethyl)amine) (L) was synthesized by using Huisgen reaction, which is known as cycloaddition of azide and acetylene derivatives to give 1,2,3-triazole unit (Obata et al., 2008). The title coordination complex, (I), was synthesized according to the following method. An acetone/CHCl₃ (v/v = 1/1, 5 ml) solution of Ag^IPF₆ (50.6 mg, 2.0 x 10 ^-4 mol) was added slowly to an acetone/CHCl₃ (v/v = 1/1, 45 ml) solution of L (104.6 mg, 2.0 x 10 ^-4 mol). After the mixture was stirred for 1 day under dark, the precipitate was collected by filtration to give white powder. This powder was dissolved in CH₃CN and insoluble materials were removed by filtration. The filtrate was concentrated under reduced pressure to give white powder (98.6 mg, yield 64%). Single crystals suitable for X-ray crystallographic analysis were obtained by recrystallization from CH₃CN/CHCl₃ (v/v = 2/1)/Et₂O. Anal. Calcd. for C₃₀H₃₀AgF₆N₁₀P: C 45.99, H 3.86, N 17.88. Found: C 46.17, H 4.00, N 17.80.

Computing details top

Data collection: CrystalClear (Rigaku/MSC & Rigaku, 2006); cell refinement: CrystalClear (Rigaku/MSC & Rigaku, 2006); data reduction: CrystalStructure (Rigaku/MSC & Rigaku, 2006); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: ORTEP-3 (Burnett & Johnson, 1996); software used to prepare material for publication: CrystalStructure (Rigaku/MSC & Rigaku, 2006).

Figures top

	Fig. 1. The coordination geometry of the Ag^I atom and the ligated mode of L in the title compound. Displacement ellipsoids are drawn at the 50% probability level. H atoms omitted for clarity.
	Fig. 2. (a) Two-dimensional 4.8² topology network with 24-membered and 48-membered metallacycles. (b). Three-dimensional packing diagram, showing the alternate arrangement of cationic layers (black) and anionic layers (pink).

Poly[[{µ₃-tris[2-(4-phenyl-1,2,3-triazol-1-yl)ethyl]amine}silver(I)] hexafluoridophosphate] top

Crystal data top

[Ag(C₃₀H₃₀N₁₀)]PF₆	F(000) = 1584.00
M_r = 783.47	D_x = 1.611 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2yn	Cell parameters from 9566 reflections
a = 14.893 (3) Å	θ = 4.0–27.5°
b = 14.935 (3) Å	µ = 0.75 mm⁻¹
c = 15.735 (3) Å	T = 193 K
β = 112.646 (5)°	Platelet, colourless
V = 3230.2 (12) Å³	0.30 × 0.15 × 0.05 mm
Z = 4

Data collection top

Rigaku Mercury diffractometer	4647 reflections with F² > 2σ(F²)
Detector resolution: 7.31 pixels mm^-1	R_int = 0.075
ω scans	θ_max = 27.5°
Absorption correction: multi-scan (Jacobson, 1998)	h = −19→16
T_min = 0.776, T_max = 0.963	k = −19→19
31971 measured reflections	l = −20→20
7326 independent reflections

Refinement top

Refinement on F²	0 restraints
R[F² > 2σ(F²)] = 0.054	All H-atom parameters refined
wR(F²) = 0.055	w = 1/[1.0000σ(F_o²)]/(4F_o²)
S = 1.03	(Δ/σ)_max < 0.001
7326 reflections	Δρ_max = 3.48 e Å⁻³
463 parameters	Δρ_min = −2.33 e Å⁻³

Crystal data top

[Ag(C₃₀H₃₀N₁₀)]PF₆	V = 3230.2 (12) Å³
M_r = 783.47	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 14.893 (3) Å	µ = 0.75 mm⁻¹
b = 14.935 (3) Å	T = 193 K
c = 15.735 (3) Å	0.30 × 0.15 × 0.05 mm
β = 112.646 (5)°

Data collection top

Rigaku Mercury diffractometer	7326 independent reflections
Absorption correction: multi-scan (Jacobson, 1998)	4647 reflections with F² > 2σ(F²)
T_min = 0.776, T_max = 0.963	R_int = 0.075
31971 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.054	0 restraints
wR(F²) = 0.055	All H-atom parameters refined
S = 1.03	Δρ_max = 3.48 e Å⁻³
7326 reflections	Δρ_min = −2.33 e Å⁻³
463 parameters

Special details top

Experimental. The ligand tris((4-phenyl-1,2,3-triazole-1-yl)ethyl)amine) (L) was synthesized by using Huisgen reaction, which is known as cycloaddition of azide and acetylene derivatives to give 1,2,3-triazole unit. The conversion of tris(2-chloroethyl)amine (2.21 g, 10.9 mmol) into tris(2-azidoethyl)amine was achieved by addition of 3 mole equivalents of sodium azide to tris(2-chloroethyl)amine in dimethylformamide under stirring at 80 °C. To the THF (100 ml) and water (100 ml) solution of crude tris(2-azidoethyl)amine obtained and phenylacethylene (2.57 g, 25.2 mmol) was added 1 M sodium ascorbate (aq) (0.9 ml) and 7.5 wt% CuSO₄ (aq) (2.5 ml) and the mixture was stirred at 50 °C for 1 day. After concentration under reduced pressure, the resulting residue was then suspended in CHCl₃, to which an aqueous solution of NH₃ was successively added. After washing the organic layer with the NH₃ aqueous solution, the organic layer was dried over anhydrous Na₂SO₄ and concentrated by evaporation. The resulting residue was purified by silica gel column chromatography (eluent; from CHCl₃ to ethyl acetate). The organic materials having R_f = 0.21 (eluent; ethyl acetate) were collected (1.73 g, yield 37%). ¹H NMR (CDCl₃, 400 MHz): δ 3.33 (dt, 6H, J = 4.8, 2.4 Hz, N—CH₂CH₂–), 4.10 (dt, 6H, J = 4.8, 2.4 Hz, N—CH₂CH₂–), 6.80 (s, 3H, triazole-H), 7.00 (t, 6H, J = 7.6 Hz Ar-3H, 5H), 7.18 (tt, 3H, J = 7.6, 1.2 Hz, Ar-4H), 7.27 (d, 3H, J = 7.6 Hz, Ar-2H or 6H), 7.28 (d, 3H, J = 7.6 Hz, Ar-2H or 6H). HRMS (FAB, pos): m/z = 531.2729 calcd for [L + H]⁺, C₃₀H₃₁N₁₀, 531.2733.

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F². R-factor (gt) are based on F. The threshold expression of F² > 2.0 σ(F²) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ag(1)	0.45614 (2)	0.23636 (2)	0.47433 (2)	0.02556 (7)
P(1)	0.72081 (8)	0.21389 (8)	0.19893 (9)	0.0300 (3)
F(1)	0.78327 (16)	0.23364 (19)	0.13875 (17)	0.0552 (8)
F(2)	0.65821 (18)	0.19439 (16)	0.25993 (18)	0.0492 (9)
F(3)	0.7415 (2)	0.31311 (17)	0.2382 (2)	0.0583 (10)
F(4)	0.81644 (17)	0.17994 (18)	0.28073 (17)	0.0477 (8)
F(5)	0.70048 (18)	0.11394 (16)	0.15986 (17)	0.0475 (8)
F(6)	0.62526 (17)	0.2473 (2)	0.11681 (17)	0.0628 (9)
N(1)	0.0406 (2)	0.4073 (2)	0.3528 (2)	0.0209 (9)
N(2)	0.2601 (2)	0.4507 (2)	0.4393 (2)	0.0264 (10)
N(3)	0.2869 (2)	0.3656 (2)	0.4548 (2)	0.0249 (10)
N(4)	0.3631 (2)	0.3565 (2)	0.4315 (2)	0.0223 (9)
N(5)	−0.0085 (2)	0.5197 (2)	0.1746 (2)	0.0258 (10)
N(6)	−0.0277 (2)	0.5971 (2)	0.1282 (2)	0.0303 (10)
N(7)	0.0412 (2)	0.6093 (2)	0.0966 (2)	0.0242 (9)
N(8)	0.0859 (2)	0.2467 (2)	0.26377 (19)	0.0231 (9)
N(9)	0.0191 (2)	0.2593 (2)	0.1787 (2)	0.0265 (9)
N(10)	0.06704 (19)	0.2581 (2)	0.1214 (2)	0.0214 (8)
C(1)	0.1011 (2)	0.4214 (2)	0.4501 (2)	0.0245 (11)
C(2)	0.1823 (3)	0.4872 (2)	0.4670 (3)	0.0290 (13)
C(3)	0.3162 (3)	0.4970 (2)	0.4061 (2)	0.0258 (12)
C(4)	0.3837 (2)	0.4368 (2)	0.4008 (2)	0.0196 (10)
C(5)	0.4644 (2)	0.4490 (2)	0.3710 (2)	0.0216 (11)
C(6)	0.5077 (3)	0.3770 (2)	0.3441 (3)	0.0320 (13)
C(7)	0.5821 (3)	0.3898 (2)	0.3148 (3)	0.0355 (13)
C(8)	0.6151 (3)	0.4762 (2)	0.3095 (3)	0.0339 (13)
C(9)	0.5733 (3)	0.5481 (2)	0.3355 (3)	0.0334 (13)
C(10)	0.4994 (2)	0.5343 (2)	0.3659 (2)	0.0262 (12)
C(11)	−0.0307 (2)	0.4794 (2)	0.3191 (2)	0.0275 (12)
C(12)	−0.0760 (3)	0.4862 (2)	0.2144 (2)	0.0292 (12)
C(13)	0.0726 (3)	0.4829 (2)	0.1727 (2)	0.0289 (12)
C(14)	0.1058 (2)	0.5395 (2)	0.1229 (2)	0.0213 (11)
C(15)	0.1908 (3)	0.5339 (2)	0.0964 (3)	0.0260 (12)
C(16)	0.2701 (3)	0.4828 (2)	0.1481 (3)	0.0338 (13)
C(17)	0.3512 (3)	0.4771 (3)	0.1237 (3)	0.0435 (15)
C(18)	0.3528 (3)	0.5245 (3)	0.0501 (3)	0.0378 (14)
C(19)	0.2756 (3)	0.5757 (2)	−0.0014 (3)	0.0373 (14)
C(20)	0.1933 (3)	0.5808 (2)	0.0213 (3)	0.0330 (13)
C(21)	−0.0095 (2)	0.3209 (2)	0.3415 (2)	0.0264 (12)
C(22)	0.0557 (2)	0.2428 (2)	0.3421 (2)	0.0305 (11)
C(23)	0.1756 (2)	0.2375 (2)	0.2625 (2)	0.0246 (10)
C(24)	0.1642 (2)	0.2460 (2)	0.1730 (2)	0.0186 (9)
C(25)	0.2370 (2)	0.2422 (2)	0.1313 (2)	0.0229 (10)
C(26)	0.3333 (2)	0.2192 (2)	0.1856 (2)	0.0300 (12)
C(27)	0.4044 (2)	0.2207 (2)	0.1484 (2)	0.0348 (13)
C(28)	0.3802 (2)	0.2411 (3)	0.0577 (3)	0.0398 (13)
C(29)	0.2856 (3)	0.2615 (3)	0.0021 (2)	0.0463 (14)
C(30)	0.2140 (2)	0.2632 (3)	0.0378 (2)	0.0371 (12)
H(1)	0.0609	0.4411	0.4809	0.031*
H(2)	0.1300	0.3657	0.4752	0.031*
H(3)	0.2097	0.5019	0.5306	0.035*
H(4)	0.1560	0.5396	0.4320	0.035*
H(5)	0.3109	0.5585	0.3894	0.030*
H(6)	0.4843	0.3180	0.3456	0.038*
H(7)	0.6119	0.3401	0.2984	0.043*
H(8)	0.6660	0.4853	0.2882	0.042*
H(9)	0.5956	0.6070	0.3318	0.039*
H(10)	0.4713	0.5841	0.3842	0.032*
H(11)	−0.0812	0.4703	0.3410	0.033*
H(12)	0.0015	0.5343	0.3426	0.033*
H(13)	−0.1302	0.5256	0.1973	0.034*
H(14)	−0.0975	0.4283	0.1902	0.035*
H(15)	0.1018	0.4283	0.2008	0.034*
H(16)	0.2699	0.4520	0.2009	0.042*
H(17)	0.4051	0.4408	0.1587	0.051*
H(18)	0.4077	0.5204	0.0335	0.046*
H(19)	0.2777	0.6090	−0.0521	0.046*
H(20)	0.1390	0.6162	−0.0148	0.038*
H(21)	−0.0344	0.3136	0.3883	0.033*
H(22)	−0.0618	0.3215	0.2829	0.033*
H(23)	0.0215	0.1885	0.3391	0.038*
H(24)	0.1117	0.2447	0.3979	0.038*
H(25)	0.2345	0.2270	0.3140	0.029*
H(26)	0.3498	0.2023	0.2480	0.033*
H(27)	0.4700	0.2075	0.1866	0.041*
H(28)	0.4292	0.2411	0.0330	0.049*
H(29)	0.2695	0.2747	−0.0612	0.056*
H(30)	0.1488	0.2782	−0.0003	0.043*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ag(1)	0.02591 (16)	0.01924 (15)	0.02906 (17)	0.00118 (17)	0.00786 (13)	−0.00264 (17)
P(1)	0.0251 (6)	0.0333 (7)	0.0370 (7)	0.0018 (5)	0.0179 (5)	−0.0044 (5)
F(1)	0.0571 (16)	0.0648 (18)	0.0679 (18)	0.0167 (16)	0.0508 (15)	0.0146 (17)
F(2)	0.0509 (16)	0.0533 (17)	0.066 (2)	−0.0082 (13)	0.0474 (15)	−0.0081 (14)
F(3)	0.059 (2)	0.0343 (16)	0.100 (2)	−0.0089 (14)	0.0517 (19)	−0.0210 (15)
F(4)	0.0291 (15)	0.0657 (19)	0.0396 (16)	−0.0025 (13)	0.0036 (13)	−0.0018 (13)
F(5)	0.0530 (17)	0.0392 (16)	0.0500 (17)	−0.0004 (13)	0.0195 (14)	−0.0172 (13)
F(6)	0.0385 (14)	0.073 (2)	0.0681 (18)	0.0214 (17)	0.0110 (13)	0.0161 (18)
N(1)	0.0190 (18)	0.0246 (19)	0.0191 (18)	0.0041 (14)	0.0073 (15)	0.0046 (14)
N(2)	0.0191 (19)	0.027 (2)	0.032 (2)	0.0078 (15)	0.0085 (17)	−0.0015 (16)
N(3)	0.025 (2)	0.0202 (19)	0.028 (2)	0.0007 (15)	0.0092 (17)	−0.0004 (15)
N(4)	0.0207 (18)	0.0194 (18)	0.027 (2)	−0.0013 (14)	0.0091 (16)	−0.0030 (15)
N(5)	0.027 (2)	0.024 (2)	0.024 (2)	−0.0012 (16)	0.0073 (17)	0.0025 (16)
N(6)	0.033 (2)	0.028 (2)	0.027 (2)	0.0027 (17)	0.0082 (18)	0.0069 (16)
N(7)	0.029 (2)	0.0230 (19)	0.0200 (19)	0.0010 (15)	0.0080 (16)	0.0034 (15)
N(8)	0.0319 (18)	0.0146 (19)	0.0206 (17)	0.0029 (15)	0.0076 (15)	0.0042 (15)
N(9)	0.0206 (16)	0.0262 (19)	0.0275 (18)	−0.0016 (16)	0.0035 (14)	0.0025 (17)
N(10)	0.0153 (15)	0.0141 (17)	0.0324 (18)	−0.0031 (14)	0.0065 (14)	−0.0005 (15)
C(1)	0.023 (2)	0.036 (2)	0.019 (2)	0.0077 (19)	0.0132 (19)	0.0000 (19)
C(2)	0.026 (2)	0.037 (2)	0.026 (2)	0.009 (2)	0.012 (2)	−0.002 (2)
C(3)	0.029 (2)	0.021 (2)	0.025 (2)	−0.0017 (18)	0.008 (2)	0.0042 (18)
C(4)	0.020 (2)	0.016 (2)	0.019 (2)	0.0022 (16)	0.0027 (18)	0.0006 (16)
C(5)	0.022 (2)	0.017 (2)	0.024 (2)	0.0005 (17)	0.0068 (19)	−0.0013 (17)
C(6)	0.033 (2)	0.023 (2)	0.039 (2)	−0.0044 (19)	0.012 (2)	−0.004 (2)
C(7)	0.028 (2)	0.034 (2)	0.045 (3)	0.003 (2)	0.015 (2)	−0.006 (2)
C(8)	0.024 (2)	0.041 (2)	0.040 (2)	−0.004 (2)	0.016 (2)	0.001 (2)
C(9)	0.028 (2)	0.026 (2)	0.044 (2)	−0.007 (2)	0.011 (2)	−0.002 (2)
C(10)	0.026 (2)	0.022 (2)	0.033 (2)	0.0018 (18)	0.013 (2)	0.0001 (19)
C(11)	0.023 (2)	0.030 (2)	0.029 (2)	0.0057 (19)	0.0093 (19)	0.0033 (19)
C(12)	0.026 (2)	0.034 (2)	0.026 (2)	0.0013 (19)	0.009 (2)	0.003 (2)
C(13)	0.034 (2)	0.020 (2)	0.031 (2)	0.0055 (19)	0.010 (2)	0.0060 (19)
C(14)	0.028 (2)	0.016 (2)	0.016 (2)	−0.0004 (18)	0.0034 (19)	−0.0009 (16)
C(15)	0.030 (2)	0.020 (2)	0.025 (2)	−0.0051 (19)	0.006 (2)	−0.0044 (18)
C(16)	0.037 (2)	0.032 (2)	0.035 (2)	−0.002 (2)	0.018 (2)	0.007 (2)
C(17)	0.037 (2)	0.048 (3)	0.042 (3)	0.010 (2)	0.012 (2)	0.009 (2)
C(18)	0.029 (2)	0.046 (3)	0.040 (2)	0.002 (2)	0.014 (2)	−0.000 (2)
C(19)	0.049 (3)	0.031 (2)	0.036 (2)	−0.006 (2)	0.020 (2)	0.003 (2)
C(20)	0.040 (2)	0.026 (2)	0.029 (2)	0.000 (2)	0.009 (2)	0.006 (2)
C(21)	0.025 (2)	0.031 (2)	0.026 (2)	0.0000 (19)	0.0136 (19)	0.0095 (19)
C(22)	0.041 (2)	0.027 (2)	0.028 (2)	−0.001 (2)	0.018 (2)	0.004 (2)
C(23)	0.020 (2)	0.029 (2)	0.024 (2)	0.004 (2)	0.0074 (17)	0.003 (2)
C(24)	0.0205 (19)	0.009 (2)	0.0212 (19)	−0.0041 (16)	0.0022 (16)	−0.0047 (16)
C(25)	0.0212 (19)	0.021 (2)	0.023 (2)	−0.0004 (18)	0.0052 (16)	−0.0066 (19)
C(26)	0.026 (2)	0.026 (2)	0.030 (2)	0.0029 (19)	0.003 (2)	0.0026 (19)
C(27)	0.020 (2)	0.041 (2)	0.040 (2)	0.005 (2)	0.008 (2)	−0.005 (2)
C(28)	0.030 (2)	0.051 (3)	0.042 (2)	−0.004 (2)	0.019 (2)	−0.011 (2)
C(29)	0.039 (2)	0.072 (3)	0.029 (2)	−0.006 (2)	0.014 (2)	0.002 (2)
C(30)	0.025 (2)	0.058 (2)	0.024 (2)	−0.005 (2)	0.0050 (18)	0.003 (2)

Geometric parameters (Å, º) top

Ag(1)—N(4)	2.208 (2)	C(17)—C(18)	1.365 (7)
Ag(1)—N(7)ⁱ	2.210 (3)	C(18)—C(19)	1.359 (5)
Ag(1)—N(10)ⁱⁱ	2.268 (2)	C(19)—C(20)	1.405 (8)
P(1)—F(1)	1.590 (3)	C(21)—C(22)	1.516 (5)
P(1)—F(2)	1.601 (3)	C(23)—C(24)	1.359 (5)
P(1)—F(3)	1.590 (2)	C(24)—C(25)	1.468 (6)
P(1)—F(4)	1.591 (2)	C(25)—C(26)	1.401 (4)
P(1)—F(5)	1.598 (2)	C(25)—C(30)	1.410 (5)
P(1)—F(6)	1.590 (2)	C(26)—C(27)	1.395 (7)
N(1)—C(1)	1.462 (4)	C(27)—C(28)	1.365 (6)
N(1)—C(11)	1.462 (4)	C(28)—C(29)	1.376 (5)
N(1)—C(21)	1.466 (4)	C(29)—C(30)	1.385 (7)
N(2)—N(3)	1.327 (4)	C(1)—H(1)	0.950
N(2)—C(2)	1.489 (6)	C(1)—H(2)	0.950
N(2)—C(3)	1.336 (6)	C(2)—H(3)	0.950
N(3)—N(4)	1.327 (5)	C(2)—H(4)	0.950
N(4)—C(4)	1.372 (5)	C(3)—H(5)	0.950
N(5)—N(6)	1.338 (4)	C(6)—H(6)	0.950
N(5)—C(12)	1.463 (6)	C(7)—H(7)	0.950
N(5)—C(13)	1.337 (6)	C(8)—H(8)	0.950
N(6)—N(7)	1.314 (6)	C(9)—H(9)	0.950
N(7)—C(14)	1.370 (4)	C(10)—H(10)	0.950
N(8)—N(9)	1.339 (3)	C(11)—H(11)	0.950
N(8)—C(22)	1.466 (5)	C(11)—H(12)	0.950
N(8)—C(23)	1.350 (5)	C(12)—H(13)	0.950
N(9)—N(10)	1.349 (5)	C(12)—H(14)	0.950
N(10)—C(24)	1.372 (3)	C(13)—H(15)	0.950
C(1)—C(2)	1.501 (5)	C(16)—H(16)	0.950
C(3)—C(4)	1.375 (6)	C(17)—H(17)	0.950
C(4)—C(5)	1.460 (6)	C(18)—H(18)	0.950
C(5)—C(6)	1.402 (6)	C(19)—H(19)	0.950
C(5)—C(10)	1.390 (5)	C(20)—H(20)	0.950
C(6)—C(7)	1.368 (7)	C(21)—H(21)	0.950
C(7)—C(8)	1.394 (6)	C(21)—H(22)	0.950
C(8)—C(9)	1.381 (6)	C(22)—H(23)	0.950
C(9)—C(10)	1.374 (7)	C(22)—H(24)	0.950
C(11)—C(12)	1.524 (5)	C(23)—H(25)	0.950
C(13)—C(14)	1.368 (6)	C(26)—H(26)	0.950
C(14)—C(15)	1.479 (7)	C(27)—H(27)	0.950
C(15)—C(16)	1.379 (5)	C(28)—H(28)	0.950
C(15)—C(20)	1.386 (6)	C(29)—H(29)	0.950
C(16)—C(17)	1.404 (8)	C(30)—H(30)	0.950

F(1)···N(3)ⁱⁱⁱ	3.271 (4)	N(10)···H(20)^ix	3.433
F(1)···N(9)^iv	3.343 (3)	C(4)···H(10)^vii	3.253
F(1)···C(9)^v	3.427 (5)	C(7)···H(3)^vii	3.513
F(1)···C(19)^vi	3.477 (5)	C(8)···H(3)^vii	2.863
F(2)···N(6)ⁱ	3.409 (5)	C(9)···H(3)^vii	3.195
F(2)···C(7)	3.362 (5)	C(11)···H(1)^xiii	3.550
F(2)···C(12)ⁱ	3.421 (5)	C(12)···H(19)^ix	3.414
F(2)···C(27)	3.523 (4)	C(12)···H(20)^ix	3.289
F(3)···C(7)	3.256 (6)	C(13)···H(20)^ix	3.502
F(3)···C(8)	3.516 (5)	C(19)···H(13)^ix	3.368
F(3)···C(21)^iv	3.430 (4)	C(19)···H(14)^ix	3.131
F(4)···C(9)^v	3.498 (5)	C(20)···H(13)^ix	3.572
F(4)···C(21)^iv	3.188 (4)	C(20)···H(14)^ix	3.079
F(4)···C(22)^iv	3.445 (4)	C(21)···H(28)^viii	3.591
F(5)···C(1)ⁱⁱⁱ	3.099 (4)	C(28)···H(21)ⁱⁱⁱ	3.465
F(5)···C(2)ⁱⁱⁱ	3.307 (5)	H(1)···F(5)^viii	2.901
F(5)···C(8)^v	3.316 (5)	H(1)···F(6)^viii	3.440
F(5)···C(9)^v	3.484 (5)	H(1)···C(11)^xiii	3.550
F(5)···C(11)ⁱ	3.345 (5)	H(1)···H(1)^xiii	2.754
F(6)···C(1)ⁱⁱⁱ	3.554 (4)	H(1)···H(11)^xiii	3.006
F(6)···C(27)	3.533 (5)	H(1)···H(12)^xiii	3.271
F(6)···C(28)	3.403 (4)	H(2)···P(1)^viii	3.460
N(2)···C(9)^vii	3.456 (4)	H(2)···F(1)^viii	3.084
N(3)···F(1)^viii	3.271 (4)	H(2)···F(5)^viii	2.700
N(3)···C(9)^vii	3.405 (4)	H(2)···F(6)^viii	2.818
N(4)···C(10)^vii	3.463 (4)	H(3)···F(5)^viii	2.714
N(5)···C(20)^ix	3.578 (4)	H(3)···C(7)^vii	3.513
N(6)···F(2)^x	3.409 (5)	H(3)···C(8)^vii	2.863
N(9)···F(1)^xi	3.343 (3)	H(3)···C(9)^vii	3.195
C(1)···F(5)^viii	3.099 (4)	H(3)···H(8)^vii	2.744
C(1)···F(6)^viii	3.554 (4)	H(3)···H(9)^vii	3.303
C(2)···F(5)^viii	3.307 (5)	H(3)···H(11)^xiii	3.300
C(4)···C(10)^vii	3.431 (5)	H(7)···P(1)	3.254
C(7)···F(2)	3.362 (5)	H(7)···F(2)	2.429
C(7)···F(3)	3.256 (6)	H(7)···F(3)	2.489
C(8)···F(3)	3.516 (5)	H(7)···F(6)	3.251
C(8)···F(5)^xii	3.316 (5)	H(8)···F(3)	3.030
C(9)···F(1)^xii	3.427 (5)	H(8)···F(4)^xii	3.148
C(9)···F(4)^xii	3.498 (5)	H(8)···F(5)^xii	2.657
C(9)···F(5)^xii	3.484 (5)	H(8)···H(3)^vii	2.744
C(9)···N(2)^vii	3.456 (4)	H(8)···H(11)^iv	3.536
C(9)···N(3)^vii	3.405 (4)	H(9)···P(1)^xii	3.358
C(10)···N(4)^vii	3.463 (4)	H(9)···F(1)^xii	2.530
C(10)···C(4)^vii	3.431 (5)	H(9)···F(4)^xii	2.797
C(11)···F(5)^x	3.345 (5)	H(9)···F(5)^xii	2.990
C(12)···F(2)^x	3.421 (5)	H(9)···N(2)^vii	3.517
C(12)···C(20)^ix	3.582 (5)	H(9)···N(3)^vii	3.159
C(19)···F(1)^vi	3.477 (5)	H(9)···N(4)^vii	3.576
C(20)···N(5)^ix	3.578 (4)	H(9)···H(3)^vii	3.303
C(20)···C(12)^ix	3.582 (5)	H(10)···Ag(1)^vii	3.386
C(21)···F(3)^xi	3.430 (4)	H(10)···N(3)^vii	3.595
C(21)···F(4)^xi	3.188 (4)	H(10)···N(4)^vii	3.127
C(22)···F(4)^xi	3.445 (4)	H(10)···C(4)^vii	3.253
C(27)···F(2)	3.523 (4)	H(11)···F(3)^xi	3.437
C(27)···F(6)	3.533 (5)	H(11)···F(5)^x	2.782
C(28)···F(6)	3.403 (4)	H(11)···H(1)^xiii	3.006
Ag(1)···H(10)^vii	3.386	H(11)···H(3)^xiii	3.300
P(1)···H(2)ⁱⁱⁱ	3.460	H(11)···H(8)^xi	3.536
P(1)···H(7)	3.254	H(12)···F(2)^x	3.320
P(1)···H(9)^v	3.358	H(12)···F(5)^x	3.221
P(1)···H(19)^vi	3.519	H(12)···H(1)^xiii	3.271
P(1)···H(22)^iv	3.394	H(13)···F(2)^x	2.682
P(1)···H(29)ⁱⁱ	3.564	H(13)···F(5)^x	3.114
F(1)···H(2)ⁱⁱⁱ	3.084	H(13)···C(19)^ix	3.368
F(1)···H(9)^v	2.530	H(13)···C(20)^ix	3.572
F(1)···H(14)^iv	3.340	H(13)···H(19)^ix	3.198
F(1)···H(19)^vi	2.694	H(13)···H(20)^ix	3.530
F(1)···H(20)^vi	3.451	H(14)···F(1)^xi	3.340
F(1)···H(22)^iv	2.857	H(14)···F(3)^xi	3.267
F(2)···H(7)	2.429	H(14)···C(19)^ix	3.131
F(2)···H(12)ⁱ	3.320	H(14)···C(20)^ix	3.079
F(2)···H(13)ⁱ	2.682	H(14)···H(19)^ix	2.783
F(2)···H(27)	2.595	H(14)···H(20)^ix	2.670
F(2)···H(29)ⁱⁱ	2.700	H(18)···H(18)^vi	3.360
F(3)···H(7)	2.489	H(19)···P(1)^vi	3.519
F(3)···H(8)	3.030	H(19)···F(1)^vi	2.694
F(3)···H(11)^iv	3.437	H(19)···F(3)^vi	3.062
F(3)···H(14)^iv	3.267	H(19)···F(6)^vi	2.978
F(3)···H(19)^vi	3.062	H(19)···C(12)^ix	3.414
F(3)···H(21)^iv	3.263	H(19)···H(13)^ix	3.198
F(3)···H(22)^iv	2.740	H(19)···H(14)^ix	2.783
F(3)···H(29)ⁱⁱ	3.293	H(20)···F(1)^vi	3.451
F(4)···H(8)^v	3.148	H(20)···N(5)^ix	3.234
F(4)···H(9)^v	2.797	H(20)···N(9)^ix	3.312
F(4)···H(21)^iv	2.981	H(20)···N(10)^ix	3.433
F(4)···H(22)^iv	2.777	H(20)···C(12)^ix	3.289
F(4)···H(23)^iv	2.833	H(20)···C(13)^ix	3.502
F(4)···H(29)ⁱⁱ	2.912	H(20)···H(13)^ix	3.530
F(5)···H(1)ⁱⁱⁱ	2.901	H(20)···H(14)^ix	2.670
F(5)···H(2)ⁱⁱⁱ	2.700	H(21)···F(3)^xi	3.263
F(5)···H(3)ⁱⁱⁱ	2.714	H(21)···F(4)^xi	2.981
F(5)···H(8)^v	2.657	H(21)···F(6)^viii	3.582
F(5)···H(9)^v	2.990	H(21)···C(28)^viii	3.465
F(5)···H(11)ⁱ	2.782	H(21)···H(28)^viii	2.664
F(5)···H(12)ⁱ	3.221	H(21)···H(29)^viii	3.563
F(5)···H(13)ⁱ	3.114	H(22)···P(1)^xi	3.394
F(6)···H(1)ⁱⁱⁱ	3.440	H(22)···F(1)^xi	2.857
F(6)···H(2)ⁱⁱⁱ	2.818	H(22)···F(3)^xi	2.740
F(6)···H(7)	3.251	H(22)···F(4)^xi	2.777
F(6)···H(19)^vi	2.978	H(23)···F(4)^xi	2.833
F(6)···H(21)ⁱⁱⁱ	3.582	H(24)···F(6)^viii	3.374
F(6)···H(24)ⁱⁱⁱ	3.374	H(27)···F(2)	2.595
F(6)···H(27)	2.977	H(27)···F(6)	2.977
F(6)···H(28)	2.703	H(28)···F(6)	2.703
N(2)···H(9)^vii	3.517	H(28)···C(21)ⁱⁱⁱ	3.591
N(3)···H(9)^vii	3.159	H(28)···H(21)ⁱⁱⁱ	2.664
N(3)···H(10)^vii	3.595	H(29)···P(1)^xiv	3.564
N(4)···H(9)^vii	3.576	H(29)···F(2)^xiv	2.700
N(4)···H(10)^vii	3.127	H(29)···F(3)^xiv	3.293
N(5)···H(20)^ix	3.234	H(29)···F(4)^xiv	2.912
N(6)···H(30)^ix	2.825	H(29)···H(21)ⁱⁱⁱ	3.563
N(7)···H(30)^ix	3.136	H(30)···N(6)^ix	2.825
N(9)···H(20)^ix	3.312	H(30)···N(7)^ix	3.136

N(4)—Ag(1)—N(7)ⁱ	132.43 (10)	C(23)—C(24)—C(25)	129.9 (2)
N(4)—Ag(1)—N(10)ⁱⁱ	114.02 (10)	C(24)—C(25)—C(26)	119.7 (3)
N(7)ⁱ—Ag(1)—N(10)ⁱⁱ	113.51 (10)	C(24)—C(25)—C(30)	122.2 (3)
F(1)—P(1)—F(2)	179.70 (15)	C(26)—C(25)—C(30)	118.1 (4)
F(1)—P(1)—F(3)	89.34 (18)	C(25)—C(26)—C(27)	120.3 (3)
F(1)—P(1)—F(4)	89.67 (14)	C(26)—C(27)—C(28)	120.3 (3)
F(1)—P(1)—F(5)	90.68 (16)	C(27)—C(28)—C(29)	120.6 (4)
F(1)—P(1)—F(6)	90.20 (15)	C(28)—C(29)—C(30)	120.4 (4)
F(2)—P(1)—F(3)	90.39 (17)	C(25)—C(30)—C(29)	120.2 (3)
F(2)—P(1)—F(4)	90.20 (15)	N(1)—C(1)—H(1)	108.9
F(2)—P(1)—F(5)	89.59 (15)	N(1)—C(1)—H(2)	107.9
F(2)—P(1)—F(6)	89.93 (14)	C(2)—C(1)—H(1)	109.2
F(3)—P(1)—F(4)	90.18 (14)	C(2)—C(1)—H(2)	107.1
F(3)—P(1)—F(5)	179.69 (15)	H(1)—C(1)—H(2)	109.5
F(3)—P(1)—F(6)	90.13 (15)	N(2)—C(2)—H(3)	109.0
F(4)—P(1)—F(5)	89.51 (13)	N(2)—C(2)—H(4)	109.0
F(4)—P(1)—F(6)	179.66 (16)	C(1)—C(2)—H(3)	109.2
F(5)—P(1)—F(6)	90.17 (14)	C(1)—C(2)—H(4)	108.3
C(1)—N(1)—C(11)	110.0 (3)	H(3)—C(2)—H(4)	109.5
C(1)—N(1)—C(21)	109.5 (3)	N(2)—C(3)—H(5)	127.7
C(11)—N(1)—C(21)	109.9 (2)	C(4)—C(3)—H(5)	126.8
N(3)—N(2)—C(2)	120.7 (3)	C(5)—C(6)—H(6)	119.2
N(3)—N(2)—C(3)	112.2 (3)	C(7)—C(6)—H(6)	119.4
C(2)—N(2)—C(3)	126.8 (3)	C(6)—C(7)—H(7)	120.3
N(2)—N(3)—N(4)	106.0 (3)	C(8)—C(7)—H(7)	119.7
Ag(1)—N(4)—N(3)	120.1 (2)	C(7)—C(8)—H(8)	120.1
Ag(1)—N(4)—C(4)	128.3 (2)	C(9)—C(8)—H(8)	120.4
N(3)—N(4)—C(4)	109.8 (3)	C(8)—C(9)—H(9)	119.5
N(6)—N(5)—C(12)	119.4 (3)	C(10)—C(9)—H(9)	120.5
N(6)—N(5)—C(13)	110.4 (3)	C(5)—C(10)—H(10)	118.8
C(12)—N(5)—C(13)	130.1 (3)	C(9)—C(10)—H(10)	119.5
N(5)—N(6)—N(7)	106.9 (3)	N(1)—C(11)—H(11)	109.2
Ag(1)^x—N(7)—N(6)	118.6 (2)	N(1)—C(11)—H(12)	107.9
Ag(1)^x—N(7)—C(14)	131.2 (3)	C(12)—C(11)—H(11)	108.6
N(6)—N(7)—C(14)	110.0 (3)	C(12)—C(11)—H(12)	108.0
N(9)—N(8)—C(22)	119.7 (3)	H(11)—C(11)—H(12)	109.5
N(9)—N(8)—C(23)	111.0 (3)	N(5)—C(12)—H(13)	108.4
C(22)—N(8)—C(23)	129.3 (2)	N(5)—C(12)—H(14)	108.7
N(8)—N(9)—N(10)	106.6 (2)	C(11)—C(12)—H(13)	108.8
Ag(1)^xiv—N(10)—N(9)	108.43 (17)	C(11)—C(12)—H(14)	108.2
Ag(1)^xiv—N(10)—C(24)	142.8 (2)	H(13)—C(12)—H(14)	109.5
N(9)—N(10)—C(24)	108.4 (2)	N(5)—C(13)—H(15)	126.8
N(1)—C(1)—C(2)	114.2 (3)	C(14)—C(13)—H(15)	126.5
N(2)—C(2)—C(1)	111.9 (3)	C(15)—C(16)—H(16)	119.6
N(2)—C(3)—C(4)	105.5 (3)	C(17)—C(16)—H(16)	120.2
N(4)—C(4)—C(3)	106.4 (4)	C(16)—C(17)—H(17)	120.0
N(4)—C(4)—C(5)	123.0 (3)	C(18)—C(17)—H(17)	120.1
C(3)—C(4)—C(5)	130.5 (3)	C(17)—C(18)—H(18)	119.8
C(4)—C(5)—C(6)	122.2 (3)	C(19)—C(18)—H(18)	119.5
C(4)—C(5)—C(10)	120.4 (3)	C(18)—C(19)—H(19)	120.1
C(6)—C(5)—C(10)	117.3 (4)	C(20)—C(19)—H(19)	119.9
C(5)—C(6)—C(7)	121.4 (4)	C(15)—C(20)—H(20)	119.7
C(6)—C(7)—C(8)	120.0 (4)	C(19)—C(20)—H(20)	120.2
C(7)—C(8)—C(9)	119.5 (4)	N(1)—C(21)—H(21)	109.8
C(8)—C(9)—C(10)	120.0 (4)	N(1)—C(21)—H(22)	107.4
C(5)—C(10)—C(9)	121.7 (4)	C(22)—C(21)—H(21)	110.3
N(1)—C(11)—C(12)	113.5 (3)	C(22)—C(21)—H(22)	107.3
N(5)—C(12)—C(11)	113.2 (3)	H(21)—C(21)—H(22)	109.5
N(5)—C(13)—C(14)	106.7 (3)	N(8)—C(22)—H(23)	109.0
N(7)—C(14)—C(13)	106.0 (4)	N(8)—C(22)—H(24)	109.4
N(7)—C(14)—C(15)	122.4 (3)	C(21)—C(22)—H(23)	109.0
C(13)—C(14)—C(15)	131.6 (3)	C(21)—C(22)—H(24)	108.3
C(14)—C(15)—C(16)	119.7 (4)	H(23)—C(22)—H(24)	109.5
C(14)—C(15)—C(20)	121.2 (3)	N(8)—C(23)—H(25)	126.8
C(16)—C(15)—C(20)	119.0 (4)	C(24)—C(23)—H(25)	127.2
C(15)—C(16)—C(17)	120.2 (4)	C(25)—C(26)—H(26)	119.6
C(16)—C(17)—C(18)	119.9 (4)	C(27)—C(26)—H(26)	120.1
C(17)—C(18)—C(19)	120.7 (5)	C(26)—C(27)—H(27)	119.6
C(18)—C(19)—C(20)	120.0 (4)	C(28)—C(27)—H(27)	120.1
C(15)—C(20)—C(19)	120.1 (3)	C(27)—C(28)—H(28)	119.5
N(1)—C(21)—C(22)	112.4 (3)	C(29)—C(28)—H(28)	120.0
N(8)—C(22)—C(21)	111.5 (3)	C(28)—C(29)—H(29)	119.8
N(8)—C(23)—C(24)	106.1 (2)	C(30)—C(29)—H(29)	119.8
N(10)—C(24)—C(23)	107.9 (3)	C(25)—C(30)—H(30)	119.3
N(10)—C(24)—C(25)	122.2 (3)	C(29)—C(30)—H(30)	120.5

N(4)—Ag(1)—N(7)ⁱ—N(6)ⁱ	104.7 (2)	Ag(1)^xiv—N(10)—C(24)—C(23)	−170.2 (3)
N(4)—Ag(1)—N(7)ⁱ—C(14)ⁱ	−68.5 (3)	Ag(1)^xiv—N(10)—C(24)—C(25)	8.7 (5)
N(7)ⁱ—Ag(1)—N(4)—N(3)	96.6 (2)	N(9)—N(10)—C(24)—C(23)	1.4 (3)
N(7)ⁱ—Ag(1)—N(4)—C(4)	−100.5 (3)	N(9)—N(10)—C(24)—C(25)	−179.6 (3)
N(4)—Ag(1)—N(10)ⁱⁱ—N(9)ⁱⁱ	66.5 (2)	N(1)—C(1)—C(2)—N(2)	−70.9 (4)
N(4)—Ag(1)—N(10)ⁱⁱ—C(24)ⁱⁱ	−105.2 (3)	N(2)—C(3)—C(4)—N(4)	0.2 (3)
N(10)ⁱⁱ—Ag(1)—N(4)—N(3)	−80.8 (2)	N(2)—C(3)—C(4)—C(5)	−178.9 (3)
N(10)ⁱⁱ—Ag(1)—N(4)—C(4)	82.1 (3)	N(4)—C(4)—C(5)—C(6)	20.4 (5)
N(7)ⁱ—Ag(1)—N(10)ⁱⁱ—N(9)ⁱⁱ	−111.4 (2)	N(4)—C(4)—C(5)—C(10)	−161.5 (3)
N(7)ⁱ—Ag(1)—N(10)ⁱⁱ—C(24)ⁱⁱ	76.9 (4)	C(3)—C(4)—C(5)—C(6)	−160.5 (3)
N(10)ⁱⁱ—Ag(1)—N(7)ⁱ—N(6)ⁱ	−77.9 (2)	C(3)—C(4)—C(5)—C(10)	17.6 (5)
N(10)ⁱⁱ—Ag(1)—N(7)ⁱ—C(14)ⁱ	108.9 (3)	C(4)—C(5)—C(6)—C(7)	178.8 (3)
C(1)—N(1)—C(11)—C(12)	162.9 (3)	C(4)—C(5)—C(10)—C(9)	−178.0 (3)
C(11)—N(1)—C(1)—C(2)	−80.9 (4)	C(6)—C(5)—C(10)—C(9)	0.2 (4)
C(1)—N(1)—C(21)—C(22)	−79.6 (4)	C(10)—C(5)—C(6)—C(7)	0.6 (5)
C(21)—N(1)—C(1)—C(2)	158.2 (3)	C(5)—C(6)—C(7)—C(8)	−1.3 (5)
C(11)—N(1)—C(21)—C(22)	159.5 (3)	C(6)—C(7)—C(8)—C(9)	1.1 (5)
C(21)—N(1)—C(11)—C(12)	−76.5 (4)	C(7)—C(8)—C(9)—C(10)	−0.3 (5)
N(3)—N(2)—C(2)—C(1)	−39.0 (4)	C(8)—C(9)—C(10)—C(5)	−0.3 (5)
C(2)—N(2)—N(3)—N(4)	−173.8 (2)	N(1)—C(11)—C(12)—N(5)	−71.1 (4)
N(3)—N(2)—C(3)—C(4)	−0.4 (4)	N(5)—C(13)—C(14)—N(7)	−0.0 (3)
C(3)—N(2)—N(3)—N(4)	0.4 (3)	N(5)—C(13)—C(14)—C(15)	−179.0 (3)
C(2)—N(2)—C(3)—C(4)	173.3 (3)	N(7)—C(14)—C(15)—C(16)	157.3 (3)
C(3)—N(2)—C(2)—C(1)	147.8 (3)	N(7)—C(14)—C(15)—C(20)	−21.3 (5)
N(2)—N(3)—N(4)—Ag(1)	165.6 (2)	C(13)—C(14)—C(15)—C(16)	−23.9 (6)
N(2)—N(3)—N(4)—C(4)	−0.2 (3)	C(13)—C(14)—C(15)—C(20)	157.5 (4)
Ag(1)—N(4)—C(4)—C(3)	−164.4 (2)	C(14)—C(15)—C(16)—C(17)	−180.0 (3)
Ag(1)—N(4)—C(4)—C(5)	14.9 (4)	C(14)—C(15)—C(20)—C(19)	178.9 (3)
N(3)—N(4)—C(4)—C(3)	−0.0 (3)	C(16)—C(15)—C(20)—C(19)	0.2 (5)
N(3)—N(4)—C(4)—C(5)	179.2 (3)	C(20)—C(15)—C(16)—C(17)	−1.3 (6)
N(6)—N(5)—C(12)—C(11)	−117.3 (3)	C(15)—C(16)—C(17)—C(18)	2.1 (6)
C(12)—N(5)—N(6)—N(7)	−177.2 (2)	C(16)—C(17)—C(18)—C(19)	−1.7 (6)
N(6)—N(5)—C(13)—C(14)	−0.1 (3)	C(17)—C(18)—C(19)—C(20)	0.6 (6)
C(13)—N(5)—N(6)—N(7)	0.1 (3)	C(18)—C(19)—C(20)—C(15)	0.2 (5)
C(12)—N(5)—C(13)—C(14)	176.9 (3)	N(1)—C(21)—C(22)—N(8)	−63.9 (3)
C(13)—N(5)—C(12)—C(11)	66.0 (5)	N(8)—C(23)—C(24)—N(10)	−1.4 (4)
N(5)—N(6)—N(7)—Ag(1)^x	−174.7 (2)	N(8)—C(23)—C(24)—C(25)	179.7 (3)
N(5)—N(6)—N(7)—C(14)	−0.1 (3)	N(10)—C(24)—C(25)—C(26)	−172.5 (3)
Ag(1)^x—N(7)—C(14)—C(13)	173.7 (2)	N(10)—C(24)—C(25)—C(30)	9.1 (5)
Ag(1)^x—N(7)—C(14)—C(15)	−7.2 (5)	C(23)—C(24)—C(25)—C(26)	6.2 (6)
N(6)—N(7)—C(14)—C(13)	0.1 (3)	C(23)—C(24)—C(25)—C(30)	−172.2 (4)
N(6)—N(7)—C(14)—C(15)	179.2 (3)	C(24)—C(25)—C(26)—C(27)	−176.0 (3)
N(9)—N(8)—C(22)—C(21)	−49.6 (4)	C(24)—C(25)—C(30)—C(29)	177.9 (4)
C(22)—N(8)—N(9)—N(10)	−178.8 (2)	C(26)—C(25)—C(30)—C(29)	−0.5 (6)
N(9)—N(8)—C(23)—C(24)	0.9 (4)	C(30)—C(25)—C(26)—C(27)	2.4 (5)
C(23)—N(8)—N(9)—N(10)	−0.0 (3)	C(25)—C(26)—C(27)—C(28)	−2.5 (6)
C(22)—N(8)—C(23)—C(24)	179.5 (3)	C(26)—C(27)—C(28)—C(29)	0.7 (6)
C(23)—N(8)—C(22)—C(21)	131.9 (3)	C(27)—C(28)—C(29)—C(30)	1.3 (7)
N(8)—N(9)—N(10)—Ag(1)^xiv	173.8 (2)	C(28)—C(29)—C(30)—C(25)	−1.3 (7)
N(8)—N(9)—N(10)—C(24)	−0.9 (3)

Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) x+1/2, −y+1/2, z+1/2; (iii) x+1/2, −y+1/2, z−1/2; (iv) x+1, y, z; (v) −x+3/2, y−1/2, −z+1/2; (vi) −x+1, −y+1, −z; (vii) −x+1, −y+1, −z+1; (viii) x−1/2, −y+1/2, z+1/2; (ix) −x, −y+1, −z; (x) −x+1/2, y+1/2, −z+1/2; (xi) x−1, y, z; (xii) −x+3/2, y+1/2, −z+1/2; (xiii) −x, −y+1, −z+1; (xiv) x−1/2, −y+1/2, z−1/2.

Experimental details

Crystal data
Chemical formula	[Ag(C₃₀H₃₀N₁₀)]PF₆
M_r	783.47
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	193
a, b, c (Å)	14.893 (3), 14.935 (3), 15.735 (3)
β (°)	112.646 (5)
V (Å³)	3230.2 (12)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	0.75
Crystal size (mm)	0.30 × 0.15 × 0.05

Data collection
Diffractometer	Rigaku Mercury diffractometer
Absorption correction	Multi-scan (Jacobson, 1998)
T_min, T_max	0.776, 0.963
No. of measured, independent and observed [F² > 2σ(F²)] reflections	31971, 7326, 4647
R_int	0.075
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.054, 0.055, 1.03
No. of reflections	7326
No. of parameters	463
H-atom treatment	All H-atom parameters refined
Δρ_max, Δρ_min (e Å⁻³)	3.48, −2.33

Computer programs: CrystalClear (Rigaku/MSC & Rigaku, 2006), CrystalStructure (Rigaku/MSC & Rigaku, 2006), SIR97 (Altomare et al., 1999), CRYSTALS (Betteridge et al., 2003), ORTEP-3 (Burnett & Johnson, 1996).

Selected geometric parameters (Å, º) top

Ag(1)—N(4)	2.208 (2)	Ag(1)—N(10)ⁱⁱ	2.268 (2)
Ag(1)—N(7)ⁱ	2.210 (3)

N(4)—Ag(1)—N(7)ⁱ	132.43 (10)	N(7)ⁱ—Ag(1)—N(10)ⁱⁱ	113.51 (10)
N(4)—Ag(1)—N(10)ⁱⁱ	114.02 (10)

Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) x+1/2, −y+1/2, z+1/2.

Acknowledgements

This work was financially supported in part by Grants-in-Aid for Scientific Research (Nos. 19350031 and 19614009) from the Ministry of Education, Culture, Sport, Science and Technology (MEXT) of the Japanese Government, the Japan–German exchange program supported by the Japan Society for the Promotion of Science (JSPS), Nara Women's University Intramural Grant for Project Research, and grants from Osaka Gas, San-EiGen, and REI Medical Foundation for Chemical Research. The authors thank Professors Yuji Mikata, Takanori Nishioka, Akio Toshimitsu, Isamu Kinoshita and Michael Gottschaldt for valuable contributions.

References

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