catena-Poly[[(N,N-dimethyl­formamide-κO)(nitrato-κO)silver(I)]-μ-1,2-bis­(diphenyl­phosphino)ethane-κ²P:P′] at 100 and 293 K: temperature effects on the volume of the solvent pocket

In the title chain compound, [Ag(NO₃)(C₃H₇NO)(C₂₆H₂₄P₂)]_n, the bis­(diphenyl­phosphino)ethane (dppe) components lie across centres of inversion. The dppe units link the Ag⁺ ions into chains along [100]. A nitrate anion is coordinated to the Ag atom, together with one mol­ecule of N,N-dimethyl­formamide (DMF) solvent. At room temperature, the coordinated DMF shows a long Ag—O distance [2.620 (3) Å] and relatively large thermal motion, while at 100 K the Ag—O distance is shorter [2.5588 (19) Å] and the thermal motion is similar to that of the rest of the complex. The behaviour of the DMF mol­ecule is related to the size of the solvent pocket, viz. 146 ų at 293 K and 131 ų at 100 K.

S1. Comment

Bis(diphenylphosphano)ethane (dppe) is a versatile ligand, forming complexes in which a bridging motif is frequently encountered. In complexes with a reduced number of ligands, the result is the formation of a polymeric chain. Silver(I) is a particular example where diphosphine-bridged coordination polymers are common (Zhang et al., 2003; Aslanidis et al., 2004; Cingolani et al., 2006; Bao et al., 2005).

The structure of the title compound, (I), at 293 K is polymeric, with dppe ligands bridging between Ag centres to generate a chain. There are two half dppe ligands in the asymmetric unit, with the remaining parts generated by crystallographic centres of inversion at the midpoints of the C—C bond of the ethane moiety. The polymeric chains extend parallel to the crystallographic a axis (Fig. 2).

The Ag atom in (I) has a distorted tetrahedral geometry (Fig. 1), made up of atoms P1 and P2 of the two half dppe ligands, atom O1 of the coordinating nitrate ligand and atom O11 of the DMF molecule. The bond distances and angles in (I) at 293 K (Table 1) are close to the average values observed in similar Ag complexes found in the Cambridge Structural Database (Version 5.27, August 2006; Allen, 2002), where the average Ag—P distance for Ag(dppe) complexes is 2.464 (6) Å (67 observations) and that for Ag(NO₃) is 2.498 (9) Å (188 observations). The nitrate ligand shows a fairly long Ag1···O2 contact but with an acute N1—O2···Ag1 angle. This interaction forces the P1—Ag—P2 angle to open considerably. The other angles around the Ag are close to the ideal value of 109.47 °.

[Five instances of dppm in the previous two paragraphs have been changed to dppe. Please check this is correct.]

The large thermal motion of the DMF solvate at room temperature prompted us to investigate the solid-state behaviour at low temperature. The single-crystal X-ray experiment at 100 K showed a slight reduction in the cell volume of 2.87%, corresponding to 42.19 (10) ų, with decreases in the lengths of all three cell axes compared with the 293 K experiment. The b axis shows a much greater decrease (1.71%) than the a or c axes (0.80 and 0.68%, respectively). The resulting structure (Fig. 3) is very similar to that at 293 K. The distances and angles are very similar for the nitrate and dppe ligands and their bonds to the Ag centre. However, the DMF molecule not only presents anisotropic displacement parameters similar to the other ligand atoms, but also a much shorter Ag—O11 distance in the low-temperature study.

The volume of the solvent pocket was calculated using PLATON (Spek, 2003). At 293 K, one void was found per asymmetric unit, with a volume of 146 ų; the centroid has coordinates (0.197, 0.844, 0.034), 3.67 Šfrom atom C123, corresponding to the location of the DMF molecule (Fig. 4a). At 100 K, the volume of the void was found to be 132 ų, a decrease of 9.59%; the centroid has coordinates (0.197, 0.845, 0.034), 3.54 Šfrom atom C123. The volume of the DMF molecule in the solid state is about 119.7 ų (Baburin & Blatov, 2004). At 293 K, the solvent pocket is much larger (26 ų) than the solvent, allowing greater motion. At 100 K, the cell-volume reduction is due largely to the reduction of the solvent pocket, restricting the motion of the DMF molecule. Concomitantly, the DMF molecule forms a shorter and stronger bond to the Ag centre.

Related literature

For related literature, see: Allen (2002); Aslanidis et al. (2004); Baburin & Blatov (2004); Bao et al. (2005); Cingolani et al. (2006); Spek (2003); Zhang et al. (2003).

S2. Experimental

The [Ag(dppe)]NO₃ polymer was synthesized by the addition of dppe (71 mg, 0.18 mmol) in methanol (5 ml) to silver nitrate (31 mg, 0.18 mmol) in water (5 ml) with stirring at room temperature. After 1 h, the yellow precipitate which formed was collected, washed with methanol and allowed to dry. The product was dissolved in a small quantity of warm DMF (0.5 ml). The colourless solution was filtered on a Celite column and then allowed to evaporate in a desiccator at 277 K. After one week, colourless crystals of the title compound formed (m.p. above 523 K). IR (KBr, ν, cm^-1): 3440 (s), 3066 (w), 3046 (w), 2926 (w), 1657 (vs), 1435 (s), 1385 (vs), 1303 (s), 1097 (m), 735 (m), 696 (s), 509 (m).

S3. Refinement

All H atoms were located in difference maps and were then placed in idealized positions and treated as riding atoms, with C—H distances of 0.93 (aromatic and aldehyde), 0.97 (CH₂) or 0.96 Å (CH₃) at 293 K, and 0.95, 0.99 and 0.98 Å, respectively, at 100 K, with U_iso(H) = kU_eq(C), where k = 1.5 for the methyl groups and 1.2 for all other H atoms.

Computing details

For both compounds, data collection: APEX2, BIS and COSMO (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT and SADABS (Bruker, 2006); program(s) used to solve structure: SHELXTL (Bruker, 2006); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures

	Fig. 1. A view of (I) at 293 K, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level and H atoms are shown as small spheres of arbitrary radii. The symmetry-generated part of the polymer is shown in grey, with phenyl groups represented as lines. [Symmetry codes: (i) 1 - x, 1 - y, 1 - z; (ii) -x, 1 - y, 1 - z.]
	Fig. 2. A view of the polymeric chain of (I). The vertical direction is parallel to the b axis and the horizontal direction is parallel to the a axis. The phenyl groups are represented as lines.
	Fig. 3. A view of (I) at 100 K, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level and H atoms are shown as small spheres of arbitrary radii. The symmetry-generated part of the polymer is shown in grey, with phenyl groups represented as lines. [Symmetry codes: (i) 1 - x, 1 - y, 1 - z; (ii) -x, 1 - y, 1 - z.]
	Fig. 4. Stereoviews of the solvent pocket calculated by PLATON (Spek, 2003) at (a) 293 K and (b) 100 K. The vertical direction is parallel to the b axis and the horizontal direction is parallel to the a axis.

(I_293K) catena-Poly[[(N,N-dimethylformamide-κO)(nitrato-κ²O:O')silver(I)]- µ-1,2-bis(diphenylphosphino)ethane-κ²P:P']

Crystal data

[Ag(NO3)(C3H7NO)(C26H24P2)]	Z = 2
Mr = 641.37	F(000) = 656
Triclinic, P1	Dx = 1.453 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 11.1758 (3) Å	Cell parameters from 5132 reflections
b = 12.1731 (3) Å	θ = 2.7–22.6°
c = 13.0499 (3) Å	µ = 0.83 mm^−1
α = 112.201 (1)°	T = 293 K
β = 102.200 (1)°	Block, colourless
γ = 106.856 (1)°	0.26 × 0.15 × 0.08 mm
V = 1466.34 (7) Å^3

Data collection

Bruker APEXII CCD area-detector diffractometer	5657 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.053
ϕ and ω scans	θmax = 30.0°, θmin = 3.0°
Absorption correction: numerical Bruker APEX2 routines (using XPREP and SADABS) were used to perform the Gaussian face-indexed numerical absorption correction.	h = −15→15
Tmin = 0.898, Tmax = 0.951	k = −17→17
35945 measured reflections	l = −18→18
8523 independent reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.111	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0474P)^2 + 0.249P] where P = (Fo^2 + 2Fc^2)/3
8523 reflections	(Δ/σ)max = 0.001
345 parameters	Δρmax = 0.66 e Å^−3
0 restraints	Δρmin = −0.53 e Å^−3

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 (Ų)

	x	y	z	Uiso*/Ueq
Ag1	0.20328 (2)	0.48532 (2)	0.32426 (2)	0.04324 (9)
C1	0.4526 (3)	0.4340 (3)	0.4903 (2)	0.0398 (6)
H1A	0.4137	0.4472	0.5513	0.048*
H1B	0.5028	0.3822	0.4960	0.048*
C2	0.0473 (3)	0.5716 (3)	0.5326 (2)	0.0360 (6)
H2A	0.1229	0.5861	0.5963	0.043*
H2B	0.0008	0.6226	0.5680	0.043*
C11	−0.0824 (6)	0.2728 (5)	0.0573 (6)	0.1110 (19)
H11	−0.0543	0.3374	0.0354	0.133*
C12	−0.2331 (6)	0.0654 (6)	0.0094 (6)	0.138 (3)
H12A	−0.2027	−0.0001	−0.0282	0.207*
H12B	−0.3293	0.0282	−0.0188	0.207*
H12C	−0.1979	0.0982	0.0939	0.207*
C13	−0.2639 (7)	0.1504 (8)	−0.1316 (5)	0.168 (4)
H13A	−0.3563	0.1279	−0.1397	0.251*
H13B	−0.2565	0.0818	−0.1939	0.251*
H13C	−0.2297	0.2295	−0.1366	0.251*
C111	0.4067 (3)	0.3073 (3)	0.2404 (3)	0.0399 (6)
C112	0.3728 (4)	0.3189 (4)	0.1386 (3)	0.0614 (10)
H112	0.3033	0.3439	0.1209	0.074*
C113	0.4423 (6)	0.2931 (5)	0.0619 (4)	0.0887 (15)
H113	0.4184	0.3001	−0.0074	0.106*
C114	0.5439 (6)	0.2583 (5)	0.0875 (5)	0.0958 (16)
H114	0.5911	0.2437	0.0365	0.115*
C115	0.5790 (5)	0.2440 (5)	0.1868 (4)	0.0946 (16)
H115	0.6482	0.2179	0.2026	0.113*
C116	0.5101 (4)	0.2689 (4)	0.2640 (3)	0.0672 (11)
H116	0.5336	0.2597	0.3321	0.081*
C121	0.2222 (3)	0.1916 (3)	0.3316 (3)	0.0394 (6)
C122	0.1049 (3)	0.1090 (3)	0.2327 (3)	0.0564 (9)
H122	0.0792	0.1342	0.1757	0.068*
C123	0.0265 (4)	−0.0101 (4)	0.2188 (4)	0.0699 (11)
H123	−0.0508	−0.0653	0.1516	0.084*
C124	0.0612 (4)	−0.0479 (4)	0.3029 (4)	0.0739 (12)
H124	0.0062	−0.1275	0.2935	0.089*
C125	0.1758 (4)	0.0306 (4)	0.4003 (4)	0.0697 (11)
H125	0.1993	0.0044	0.4570	0.084*
C126	0.2575 (4)	0.1500 (3)	0.4148 (3)	0.0558 (9)
H126	0.3365	0.2027	0.4808	0.067*
C212	−0.0386 (3)	0.6225 (3)	0.3368 (3)	0.0377 (6)
C213	−0.0492 (3)	0.5888 (3)	0.2212 (3)	0.0488 (8)
H213	0.0185	0.5716	0.1964	0.059*
C214	−0.1599 (4)	0.5802 (4)	0.1405 (3)	0.0619 (10)
H214	−0.1660	0.5580	0.0626	0.074*
C215	−0.2595 (4)	0.6047 (4)	0.1773 (4)	0.0658 (10)
H215	−0.3350	0.5966	0.1234	0.079*
C216	−0.2491 (4)	0.6410 (4)	0.2923 (4)	0.0675 (11)
H216	−0.3157	0.6606	0.3173	0.081*
C217	−0.1400 (3)	0.6486 (4)	0.3713 (3)	0.0580 (9)
H217	−0.1345	0.6718	0.4493	0.070*
C221	0.2169 (3)	0.7977 (3)	0.5331 (3)	0.0385 (6)
C222	0.1783 (4)	0.8781 (3)	0.6147 (3)	0.0592 (9)
H222	0.0942	0.8450	0.6186	0.071*
C223	0.2640 (4)	1.0068 (4)	0.6900 (4)	0.0730 (11)
H223	0.2366	1.0601	0.7435	0.088*
C224	0.3880 (4)	1.0561 (4)	0.6868 (4)	0.0703 (11)
H224	0.4455	1.1427	0.7382	0.084*
C225	0.4281 (4)	0.9776 (4)	0.6072 (4)	0.0648 (10)
H225	0.5129	1.0113	0.6047	0.078*
C226	0.3429 (3)	0.8483 (3)	0.5307 (3)	0.0495 (8)
H226	0.3710	0.7955	0.4775	0.059*
N1	0.3609 (3)	0.6073 (3)	0.2012 (2)	0.0482 (6)
N11	−0.1875 (4)	0.1686 (4)	−0.0182 (3)	0.0810 (11)
O1	0.2362 (2)	0.5401 (3)	0.1655 (2)	0.0607 (6)
O2	0.4305 (3)	0.6486 (3)	0.3063 (2)	0.0673 (7)
O3	0.4117 (3)	0.6270 (3)	0.1312 (2)	0.0755 (8)
O11	−0.0171 (4)	0.2934 (3)	0.1551 (4)	0.1368 (18)
P1	0.31895 (7)	0.34780 (7)	0.34372 (6)	0.03427 (16)
P2	0.10879 (7)	0.62630 (7)	0.43386 (6)	0.03282 (16)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ag1	0.04467 (14)	0.04584 (15)	0.04727 (15)	0.02378 (11)	0.01886 (11)	0.02454 (12)
C1	0.0448 (16)	0.0408 (17)	0.0291 (14)	0.0153 (13)	0.0086 (12)	0.0162 (13)
C2	0.0406 (15)	0.0329 (15)	0.0344 (15)	0.0123 (12)	0.0131 (12)	0.0179 (13)
C11	0.107 (4)	0.073 (4)	0.118 (5)	0.042 (3)	0.002 (4)	0.028 (3)
C12	0.109 (5)	0.083 (4)	0.164 (7)	0.030 (4)	0.030 (4)	0.019 (4)
C13	0.157 (6)	0.247 (9)	0.063 (3)	0.148 (7)	−0.003 (4)	0.013 (4)
C111	0.0463 (16)	0.0325 (16)	0.0339 (15)	0.0148 (13)	0.0152 (13)	0.0095 (13)
C112	0.097 (3)	0.062 (2)	0.051 (2)	0.049 (2)	0.036 (2)	0.0341 (19)
C113	0.160 (5)	0.087 (3)	0.067 (3)	0.073 (4)	0.073 (3)	0.049 (3)
C114	0.122 (4)	0.092 (4)	0.098 (4)	0.053 (3)	0.084 (4)	0.038 (3)
C115	0.070 (3)	0.123 (4)	0.081 (3)	0.056 (3)	0.040 (3)	0.018 (3)
C116	0.061 (2)	0.095 (3)	0.043 (2)	0.047 (2)	0.0164 (17)	0.020 (2)
C121	0.0430 (16)	0.0366 (16)	0.0428 (17)	0.0201 (13)	0.0185 (13)	0.0184 (14)
C122	0.0464 (18)	0.043 (2)	0.067 (2)	0.0098 (15)	0.0072 (17)	0.0270 (18)
C123	0.050 (2)	0.046 (2)	0.087 (3)	0.0059 (17)	0.008 (2)	0.025 (2)
C124	0.072 (3)	0.046 (2)	0.109 (4)	0.019 (2)	0.036 (3)	0.044 (3)
C125	0.082 (3)	0.057 (2)	0.083 (3)	0.027 (2)	0.029 (2)	0.048 (2)
C126	0.067 (2)	0.045 (2)	0.050 (2)	0.0173 (17)	0.0152 (17)	0.0245 (17)
C212	0.0374 (15)	0.0352 (16)	0.0423 (16)	0.0141 (13)	0.0124 (13)	0.0218 (14)
C213	0.0566 (19)	0.055 (2)	0.0407 (18)	0.0281 (17)	0.0179 (15)	0.0242 (16)
C214	0.072 (2)	0.065 (2)	0.0404 (19)	0.027 (2)	0.0066 (17)	0.0252 (18)
C215	0.049 (2)	0.078 (3)	0.068 (3)	0.027 (2)	0.0036 (18)	0.042 (2)
C216	0.052 (2)	0.101 (3)	0.079 (3)	0.049 (2)	0.030 (2)	0.054 (3)
C217	0.058 (2)	0.085 (3)	0.054 (2)	0.043 (2)	0.0264 (17)	0.040 (2)
C221	0.0382 (15)	0.0329 (15)	0.0434 (17)	0.0108 (12)	0.0118 (13)	0.0215 (14)
C222	0.053 (2)	0.0389 (19)	0.070 (2)	0.0101 (16)	0.0268 (18)	0.0149 (18)
C223	0.078 (3)	0.037 (2)	0.073 (3)	0.0099 (19)	0.028 (2)	0.0056 (19)
C224	0.063 (2)	0.041 (2)	0.067 (3)	−0.0037 (18)	0.004 (2)	0.015 (2)
C225	0.0454 (19)	0.060 (2)	0.070 (3)	−0.0014 (17)	0.0126 (18)	0.033 (2)
C226	0.0435 (17)	0.049 (2)	0.0511 (19)	0.0128 (15)	0.0140 (15)	0.0249 (17)
N1	0.0622 (18)	0.0435 (16)	0.0460 (16)	0.0226 (14)	0.0255 (14)	0.0240 (14)
N11	0.072 (2)	0.067 (2)	0.065 (2)	0.040 (2)	−0.0035 (18)	−0.0014 (19)
O1	0.0484 (14)	0.0806 (18)	0.0566 (15)	0.0214 (13)	0.0196 (12)	0.0390 (14)
O2	0.0658 (16)	0.0789 (19)	0.0440 (14)	0.0177 (14)	0.0151 (12)	0.0275 (14)
O3	0.0828 (19)	0.0754 (19)	0.0569 (16)	0.0090 (15)	0.0363 (15)	0.0315 (15)
O11	0.122 (3)	0.063 (2)	0.123 (3)	0.007 (2)	−0.062 (3)	0.025 (2)
P1	0.0364 (4)	0.0328 (4)	0.0325 (4)	0.0152 (3)	0.0111 (3)	0.0143 (3)
P2	0.0337 (4)	0.0320 (4)	0.0366 (4)	0.0131 (3)	0.0134 (3)	0.0198 (3)

Geometric parameters (Å, º)

Ag1—O1	2.469 (2)	C121—P1	1.821 (3)
Ag1—O2	2.851 (3)	C122—C123	1.378 (5)
Ag1—O11	2.620 (3)	C122—H122	0.9300
Ag1—P1	2.4445 (7)	C123—C124	1.368 (6)
Ag1—P2	2.4372 (7)	C123—H123	0.9300
C1—C1^i	1.536 (6)	C124—C125	1.361 (6)
C1—P1	1.832 (3)	C124—H124	0.9300
C1—H1A	0.9700	C125—C126	1.390 (5)
C1—H1B	0.9700	C125—H125	0.9300
C2—C2^ii	1.520 (5)	C126—H126	0.9300
C2—P2	1.826 (3)	C212—C213	1.374 (4)
C2—H2A	0.9700	C212—C217	1.381 (4)
C2—H2B	0.9700	C212—P2	1.830 (3)
C11—O11	1.218 (6)	C213—C214	1.392 (4)
C11—N11	1.289 (6)	C213—H213	0.9300
C11—H11	0.9300	C214—C215	1.368 (5)
C12—N11	1.421 (7)	C214—H214	0.9300
C12—H12A	0.9600	C215—C216	1.362 (5)
C12—H12B	0.9600	C215—H215	0.9300
C12—H12C	0.9600	C216—C217	1.374 (5)
C13—N11	1.440 (6)	C216—H216	0.9300
C13—H13A	0.9600	C217—H217	0.9300
C13—H13B	0.9600	C221—C226	1.376 (4)
C13—H13C	0.9600	C221—C222	1.388 (5)
C111—C112	1.374 (4)	C221—P2	1.824 (3)
C111—C116	1.387 (4)	C222—C223	1.381 (5)
C111—P1	1.833 (3)	C222—H222	0.9300
C112—C113	1.391 (5)	C223—C224	1.357 (6)
C112—H112	0.9300	C223—H223	0.9300
C113—C114	1.343 (7)	C224—C225	1.375 (6)
C113—H113	0.9300	C224—H224	0.9300
C114—C115	1.364 (7)	C225—C226	1.387 (5)
C114—H114	0.9300	C225—H225	0.9300
C115—C116	1.390 (5)	C226—H226	0.9300
C115—H115	0.9300	N1—O3	1.232 (3)
C116—H116	0.9300	N1—O2	1.242 (3)
C121—C122	1.391 (4)	N1—O1	1.267 (4)
C121—C126	1.393 (4)
P2—Ag1—P1	140.92 (2)	C125—C124—C123	120.2 (4)
P2—Ag1—O1	107.16 (6)	C125—C124—H124	119.9
P1—Ag1—O1	110.04 (6)	C123—C124—H124	119.9
P2—Ag1—O11	100.02 (11)	C124—C125—C126	120.0 (4)
P1—Ag1—O11	95.27 (8)	C124—C125—H125	120.0
O1—Ag1—O11	84.19 (12)	C126—C125—H125	120.0
P2—Ag1—O2	106.76 (6)	C125—C126—C121	120.6 (3)
P1—Ag1—O2	90.21 (6)	C125—C126—H126	119.7
O1—Ag1—O2	47.17 (7)	C121—C126—H126	119.7
O11—Ag1—O2	129.27 (12)	C213—C212—C217	118.3 (3)
N1—O2—Ag1	87.55 (19)	C213—C212—P2	117.2 (2)
C1^i—C1—P1	110.1 (2)	C217—C212—P2	124.5 (2)
C1^i—C1—H1A	109.6	C212—C213—C214	121.0 (3)
P1—C1—H1A	109.6	C212—C213—H213	119.5
C1^i—C1—H1B	109.6	C214—C213—H213	119.5
P1—C1—H1B	109.6	C215—C214—C213	119.2 (3)
H1A—C1—H1B	108.2	C215—C214—H214	120.4
C2^ii—C2—P2	111.9 (3)	C213—C214—H214	120.4
C2^ii—C2—H2A	109.2	C216—C215—C214	120.5 (3)
P2—C2—H2A	109.2	C216—C215—H215	119.7
C2^ii—C2—H2B	109.2	C214—C215—H215	119.7
P2—C2—H2B	109.2	C215—C216—C217	120.0 (3)
H2A—C2—H2B	107.9	C215—C216—H216	120.0
O11—C11—N11	125.3 (6)	C217—C216—H216	120.0
O11—C11—H11	117.4	C216—C217—C212	121.0 (3)
N11—C11—H11	117.4	C216—C217—H217	119.5
N11—C12—H12A	109.5	C212—C217—H217	119.5
N11—C12—H12B	109.5	C226—C221—C222	118.7 (3)
H12A—C12—H12B	109.5	C226—C221—P2	119.2 (2)
N11—C12—H12C	109.5	C222—C221—P2	122.1 (2)
H12A—C12—H12C	109.5	C223—C222—C221	120.4 (3)
H12B—C12—H12C	109.5	C223—C222—H222	119.8
N11—C13—H13A	109.5	C221—C222—H222	119.8
N11—C13—H13B	109.5	C224—C223—C222	120.6 (4)
H13A—C13—H13B	109.5	C224—C223—H223	119.7
N11—C13—H13C	109.5	C222—C223—H223	119.7
H13A—C13—H13C	109.5	C223—C224—C225	119.7 (4)
H13B—C13—H13C	109.5	C223—C224—H224	120.1
C112—C111—C116	118.6 (3)	C225—C224—H224	120.1
C112—C111—P1	119.7 (2)	C224—C225—C226	120.3 (3)
C116—C111—P1	121.6 (2)	C224—C225—H225	119.8
C111—C112—C113	120.1 (4)	C226—C225—H225	119.8
C111—C112—H112	119.9	C221—C226—C225	120.3 (3)
C113—C112—H112	119.9	C221—C226—H226	119.9
C114—C113—C112	120.3 (4)	C225—C226—H226	119.9
C114—C113—H113	119.9	O3—N1—O2	121.2 (3)
C112—C113—H113	119.9	O3—N1—O1	120.1 (3)
C113—C114—C115	121.2 (4)	O2—N1—O1	118.6 (3)
C113—C114—H114	119.4	C11—N11—C12	119.7 (5)
C115—C114—H114	119.4	C11—N11—C13	123.2 (6)
C114—C115—C116	119.1 (4)	C12—N11—C13	117.1 (5)
C114—C115—H115	120.4	N1—O1—Ag1	105.46 (18)
C116—C115—H115	120.4	C11—O11—Ag1	133.3 (4)
C111—C116—C115	120.6 (4)	C121—P1—C1	104.52 (13)
C111—C116—H116	119.7	C121—P1—C111	103.83 (13)
C115—C116—H116	119.7	C1—P1—C111	103.70 (14)
C122—C121—C126	118.1 (3)	C121—P1—Ag1	118.39 (9)
C122—C121—P1	117.5 (2)	C1—P1—Ag1	109.55 (10)
C126—C121—P1	124.4 (3)	C111—P1—Ag1	115.39 (10)
C123—C122—C121	120.4 (3)	C221—P2—C2	102.71 (13)
C123—C122—H122	119.8	C221—P2—C212	105.98 (13)
C121—C122—H122	119.8	C2—P2—C212	104.35 (13)
C124—C123—C122	120.7 (4)	C221—P2—Ag1	118.94 (10)
C124—C123—H123	119.7	C2—P2—Ag1	110.86 (9)
C122—C123—H123	119.7	C212—P2—Ag1	112.63 (10)
C116—C111—C112—C113	−0.5 (6)	C1^i—C1—P1—C121	177.0 (3)
P1—C111—C112—C113	177.6 (3)	C1^i—C1—P1—C111	68.5 (3)
C111—C112—C113—C114	−0.8 (7)	C1^i—C1—P1—Ag1	−55.2 (3)
C112—C113—C114—C115	1.8 (8)	C112—C111—P1—C121	111.6 (3)
C113—C114—C115—C116	−1.5 (8)	C116—C111—P1—C121	−70.4 (3)
C112—C111—C116—C115	0.7 (6)	C112—C111—P1—C1	−139.3 (3)
P1—C111—C116—C115	−177.3 (3)	C116—C111—P1—C1	38.6 (3)
C114—C115—C116—C111	0.2 (7)	C112—C111—P1—Ag1	−19.6 (3)
C126—C121—C122—C123	0.2 (5)	C116—C111—P1—Ag1	158.4 (3)
P1—C121—C122—C123	−179.4 (3)	P2—Ag1—P1—C121	74.25 (12)
C121—C122—C123—C124	1.3 (6)	O1—Ag1—P1—C121	−124.47 (13)
C122—C123—C124—C125	−1.7 (7)	O11—Ag1—P1—C121	−38.74 (16)
C123—C124—C125—C126	0.4 (7)	P2—Ag1—P1—C1	−45.37 (11)
C124—C125—C126—C121	1.1 (6)	O1—Ag1—P1—C1	115.91 (12)
C122—C121—C126—C125	−1.4 (5)	O11—Ag1—P1—C1	−158.36 (15)
P1—C121—C126—C125	178.2 (3)	P2—Ag1—P1—C111	−161.89 (11)
C217—C212—C213—C214	−0.5 (5)	O1—Ag1—P1—C111	−0.61 (13)
P2—C212—C213—C214	178.3 (3)	O11—Ag1—P1—C111	85.11 (16)
C212—C213—C214—C215	−0.5 (6)	C226—C221—P2—C2	132.7 (2)
C213—C214—C215—C216	1.9 (6)	C222—C221—P2—C2	−44.7 (3)
C214—C215—C216—C217	−2.3 (7)	C226—C221—P2—C212	−118.1 (2)
C215—C216—C217—C212	1.3 (6)	C222—C221—P2—C212	64.5 (3)
C213—C212—C217—C216	0.1 (5)	C226—C221—P2—Ag1	9.9 (3)
P2—C212—C217—C216	−178.6 (3)	C222—C221—P2—Ag1	−167.5 (2)
C226—C221—C222—C223	1.3 (5)	C2^ii—C2—P2—C221	179.8 (3)
P2—C221—C222—C223	178.7 (3)	C2^ii—C2—P2—C212	69.3 (3)
C221—C222—C223—C224	−1.0 (7)	C2^ii—C2—P2—Ag1	−52.2 (3)
C222—C223—C224—C225	0.5 (7)	C213—C212—P2—C221	106.7 (3)
C223—C224—C225—C226	−0.2 (6)	C217—C212—P2—C221	−74.6 (3)
C222—C221—C226—C225	−1.0 (5)	C213—C212—P2—C2	−145.3 (2)
P2—C221—C226—C225	−178.5 (3)	C217—C212—P2—C2	33.4 (3)
C224—C225—C226—C221	0.5 (5)	C213—C212—P2—Ag1	−25.0 (3)
O11—C11—N11—C12	−1.5 (9)	C217—C212—P2—Ag1	153.7 (3)
O11—C11—N11—C13	178.0 (6)	P1—Ag1—P2—C221	88.20 (11)
O3—N1—O1—Ag1	165.4 (2)	O1—Ag1—P2—C221	−73.40 (12)
O2—N1—O1—Ag1	−12.1 (3)	O11—Ag1—P2—C221	−160.37 (14)
P2—Ag1—O1—N1	103.49 (19)	P1—Ag1—P2—C2	−30.47 (11)
P1—Ag1—O1—N1	−64.3 (2)	O1—Ag1—P2—C2	167.93 (11)
O11—Ag1—O1—N1	−157.8 (2)	O11—Ag1—P2—C2	80.96 (13)
N11—C11—O11—Ag1	176.8 (4)	P1—Ag1—P2—C212	−146.96 (10)
P2—Ag1—O11—C11	88.5 (6)	O1—Ag1—P2—C212	51.44 (12)
P1—Ag1—O11—C11	−127.6 (6)	O11—Ag1—P2—C212	−35.53 (14)
O1—Ag1—O11—C11	−17.9 (6)	O3—N1—O2—Ag1	−167.4 (3)
C122—C121—P1—C1	174.0 (3)	O1—N1—O2—Ag1	10.1 (3)
C126—C121—P1—C1	−5.6 (3)	P2—Ag1—O2—N1	−104.29 (18)
C122—C121—P1—C111	−77.6 (3)	P1—Ag1—O2—N1	111.44 (18)
C126—C121—P1—C111	102.8 (3)	O1—Ag1—O2—N1	−6.19 (17)
C122—C121—P1—Ag1	51.8 (3)	O11—Ag1—O2—N1	14.5 (2)
C126—C121—P1—Ag1	−127.8 (3)

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

(I_100K) catena-Poly[[(N,N-dimethylformamide-κO)(nitrato-κ²O:O')silver(I)]- µ-1,2-bis(diphenylphosphino)ethane-κ²P:P']

Crystal data

[Ag(NO3)(C3H7NO)(C26H24P2)]	Z = 2
Mr = 641.37	F(000) = 656
Triclinic, P1	Dx = 1.496 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 11.0869 (3) Å	Cell parameters from 9993 reflections
b = 11.9653 (4) Å	θ = 2.8–29.7°
c = 12.9618 (4) Å	µ = 0.86 mm^−1
α = 112.322 (2)°	T = 100 K
β = 102.410 (2)°	Block, colourless
γ = 106.216 (2)°	0.22 × 0.15 × 0.06 mm
V = 1424.15 (9) Å^3

Data collection

Bruker APEXII CCD area-detector diffractometer	7005 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.042
ϕ and ω scans	θmax = 30.0°, θmin = 3.0°
Absorption correction: numerical Bruker APEX2 routines (using XPREP and SADABS) were used to perform the Gaussian face-indexed numerical absorption correction.	h = −15→15
Tmin = 0.900, Tmax = 0.958	k = −16→16
36255 measured reflections	l = −18→18
8237 independent reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.034	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.081	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0342P)^2 + 1.2423P] where P = (Fo^2 + 2Fc^2)/3
8237 reflections	(Δ/σ)max = 0.001
345 parameters	Δρmax = 1.60 e Å^−3
0 restraints	Δρmin = −0.63 e Å^−3

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 (Ų)

	x	y	z	Uiso*/Ueq
Ag1	0.201247 (16)	0.484687 (16)	0.321223 (14)	0.01572 (5)
C1	0.4526 (2)	0.4334 (2)	0.49036 (18)	0.0147 (4)
H1A	0.4119	0.4476	0.5527	0.018*
H1B	0.5043	0.3794	0.497	0.018*
C2	0.0477 (2)	0.5729 (2)	0.53449 (18)	0.0143 (4)
H2A	0.1253	0.5862	0.5991	0.017*
H2B	0	0.6259	0.5717	0.017*
C11	−0.0818 (3)	0.2733 (3)	0.0535 (3)	0.0327 (6)
H11	−0.0555	0.3384	0.0285	0.039*
C12	−0.2360 (3)	0.0593 (3)	0.0105 (3)	0.0360 (6)
H12A	−0.2214	−0.0169	−0.0399	0.054*
H12B	−0.3321	0.0337	−0.0021	0.054*
H12C	−0.1846	0.0906	0.0947	0.054*
C13	−0.2687 (3)	0.1429 (3)	−0.1375 (2)	0.0445 (8)
H13A	−0.2274	0.2197	−0.1481	0.067*
H13B	−0.3614	0.1307	−0.1428	0.067*
H13C	−0.2691	0.0643	−0.2002	0.067*
C111	0.4105 (2)	0.3049 (2)	0.24057 (19)	0.0150 (4)
C112	0.3802 (3)	0.3203 (2)	0.1384 (2)	0.0217 (5)
H112	0.3097	0.348	0.1198	0.026*
C113	0.4532 (3)	0.2950 (3)	0.0630 (2)	0.0314 (6)
H113	0.4319	0.3049	−0.0072	0.038*
C114	0.5560 (3)	0.2557 (3)	0.0902 (3)	0.0347 (6)
H114	0.607	0.2411	0.04	0.042*
C115	0.5851 (3)	0.2372 (3)	0.1902 (2)	0.0331 (6)
H115	0.6549	0.2083	0.2076	0.04*
C116	0.5124 (2)	0.2611 (3)	0.2653 (2)	0.0255 (5)
H116	0.532	0.2476	0.3336	0.031*
C121	0.2216 (2)	0.1881 (2)	0.32879 (19)	0.0150 (4)
C122	0.1042 (2)	0.1043 (2)	0.2264 (2)	0.0190 (4)
H122	0.0799	0.1308	0.1674	0.023*
C123	0.0236 (2)	−0.0169 (2)	0.2112 (2)	0.0247 (5)
H123	−0.0543	−0.0739	0.1408	0.03*
C124	0.0562 (2)	−0.0553 (2)	0.2985 (2)	0.0247 (5)
H124	−0.0002	−0.1377	0.2884	0.03*
C125	0.1707 (2)	0.0264 (2)	0.3998 (2)	0.0235 (5)
H125	0.1924	0.0003	0.4597	0.028*
C126	0.2548 (2)	0.1471 (2)	0.4149 (2)	0.0193 (4)
H126	0.3348	0.2015	0.4837	0.023*
C211	−0.0406 (2)	0.6240 (2)	0.33620 (19)	0.0144 (4)
C212	−0.0508 (2)	0.5891 (2)	0.21807 (19)	0.0175 (4)
H212	0.0198	0.5727	0.193	0.021*
C213	−0.1638 (2)	0.5782 (2)	0.1368 (2)	0.0216 (5)
H213	−0.1702	0.5544	0.0564	0.026*
C214	−0.2671 (2)	0.6019 (2)	0.1729 (2)	0.0219 (5)
H214	−0.345	0.5927	0.1169	0.026*
C215	−0.2567 (2)	0.6390 (2)	0.2903 (2)	0.0234 (5)
H215	−0.3266	0.6573	0.3153	0.028*
C216	−0.1444 (2)	0.6496 (2)	0.3718 (2)	0.0200 (4)
H216	−0.1381	0.6743	0.4523	0.024*
C221	0.2144 (2)	0.8015 (2)	0.53434 (19)	0.0146 (4)
C222	0.1735 (2)	0.8831 (2)	0.6167 (2)	0.0208 (4)
H222	0.0871	0.8484	0.6202	0.025*
C223	0.2585 (3)	1.0147 (2)	0.6932 (2)	0.0248 (5)
H223	0.23	1.0695	0.7486	0.03*
C224	0.3849 (2)	1.0660 (2)	0.6890 (2)	0.0247 (5)
H224	0.4428	1.1559	0.7413	0.03*
C225	0.4267 (2)	0.9859 (2)	0.6083 (2)	0.0232 (5)
H225	0.5136	1.0212	0.606	0.028*
C226	0.3424 (2)	0.8545 (2)	0.5306 (2)	0.0188 (4)
H226	0.3714	0.8005	0.4751	0.023*
N1	0.35962 (19)	0.60651 (18)	0.19860 (17)	0.0172 (4)
N11	−0.1915 (2)	0.1639 (2)	−0.02095 (19)	0.0278 (5)
O1	0.23316 (16)	0.54134 (17)	0.16375 (14)	0.0220 (3)
O2	0.43074 (17)	0.65141 (17)	0.30621 (14)	0.0233 (3)
O3	0.41026 (18)	0.62281 (17)	0.12625 (15)	0.0258 (4)
O11	−0.0126 (2)	0.29565 (19)	0.15202 (19)	0.0446 (6)
P1	0.31958 (5)	0.34638 (5)	0.34195 (5)	0.01304 (10)
P2	0.10820 (5)	0.62830 (5)	0.43420 (5)	0.01235 (10)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ag1	0.01650 (8)	0.01643 (8)	0.01691 (8)	0.00821 (6)	0.00695 (6)	0.00877 (7)
C1	0.0174 (10)	0.0149 (10)	0.0102 (9)	0.0051 (8)	0.0038 (8)	0.0061 (8)
C2	0.0177 (10)	0.0122 (9)	0.0135 (10)	0.0043 (8)	0.0058 (8)	0.0075 (8)
C11	0.0308 (13)	0.0204 (12)	0.0383 (15)	0.0116 (11)	0.0029 (12)	0.0099 (11)
C12	0.0311 (14)	0.0217 (13)	0.0368 (16)	0.0069 (11)	0.0053 (12)	0.0025 (12)
C13	0.0420 (17)	0.057 (2)	0.0217 (14)	0.0326 (16)	0.0011 (12)	0.0026 (14)
C111	0.0173 (10)	0.0110 (9)	0.0135 (10)	0.0044 (8)	0.0062 (8)	0.0031 (8)
C112	0.0326 (12)	0.0179 (11)	0.0195 (11)	0.0145 (10)	0.0119 (10)	0.0091 (9)
C113	0.0560 (18)	0.0263 (13)	0.0261 (13)	0.0216 (13)	0.0264 (13)	0.0161 (11)
C114	0.0385 (15)	0.0314 (14)	0.0371 (15)	0.0141 (12)	0.0291 (13)	0.0103 (12)
C115	0.0222 (12)	0.0400 (16)	0.0301 (14)	0.0183 (12)	0.0093 (11)	0.0057 (12)
C116	0.0239 (12)	0.0337 (14)	0.0166 (11)	0.0167 (11)	0.0047 (9)	0.0074 (10)
C121	0.0172 (10)	0.0133 (9)	0.0159 (10)	0.0066 (8)	0.0078 (8)	0.0070 (8)
C122	0.0186 (10)	0.0182 (11)	0.0193 (11)	0.0069 (9)	0.0054 (9)	0.0089 (9)
C123	0.0192 (11)	0.0183 (11)	0.0297 (13)	0.0051 (9)	0.0033 (10)	0.0092 (10)
C124	0.0241 (11)	0.0154 (11)	0.0360 (14)	0.0067 (9)	0.0116 (10)	0.0139 (10)
C125	0.0297 (12)	0.0199 (11)	0.0266 (12)	0.0108 (10)	0.0115 (10)	0.0149 (10)
C126	0.0233 (11)	0.0177 (11)	0.0167 (10)	0.0088 (9)	0.0060 (9)	0.0081 (9)
C211	0.0154 (9)	0.0121 (9)	0.0164 (10)	0.0051 (8)	0.0050 (8)	0.0082 (8)
C212	0.0214 (10)	0.0167 (10)	0.0164 (10)	0.0093 (9)	0.0075 (8)	0.0084 (9)
C213	0.0265 (12)	0.0213 (11)	0.0132 (10)	0.0088 (9)	0.0036 (9)	0.0068 (9)
C214	0.0188 (10)	0.0230 (12)	0.0207 (11)	0.0078 (9)	0.0006 (9)	0.0109 (10)
C215	0.0182 (11)	0.0311 (13)	0.0257 (12)	0.0145 (10)	0.0085 (9)	0.0144 (11)
C216	0.0216 (11)	0.0269 (12)	0.0161 (10)	0.0134 (9)	0.0080 (9)	0.0114 (9)
C221	0.0144 (9)	0.0141 (9)	0.0158 (10)	0.0047 (8)	0.0042 (8)	0.0089 (8)
C222	0.0184 (10)	0.0163 (10)	0.0249 (12)	0.0044 (8)	0.0082 (9)	0.0085 (9)
C223	0.0263 (12)	0.0168 (11)	0.0253 (12)	0.0068 (9)	0.0094 (10)	0.0052 (10)
C224	0.0230 (11)	0.0176 (11)	0.0228 (12)	0.0009 (9)	0.0004 (9)	0.0085 (10)
C225	0.0182 (10)	0.0223 (12)	0.0234 (12)	0.0008 (9)	0.0043 (9)	0.0121 (10)
C226	0.0162 (10)	0.0205 (11)	0.0193 (11)	0.0046 (8)	0.0054 (8)	0.0116 (9)
N1	0.0216 (9)	0.0153 (9)	0.0175 (9)	0.0086 (7)	0.0093 (7)	0.0083 (7)
N11	0.0257 (10)	0.0257 (11)	0.0211 (10)	0.0136 (9)	0.0007 (8)	0.0023 (9)
O1	0.0168 (8)	0.0302 (9)	0.0205 (8)	0.0074 (7)	0.0073 (6)	0.0145 (7)
O2	0.0235 (8)	0.0275 (9)	0.0152 (8)	0.0068 (7)	0.0050 (6)	0.0100 (7)
O3	0.0293 (9)	0.0252 (9)	0.0180 (8)	0.0026 (7)	0.0127 (7)	0.0093 (7)
O11	0.0385 (11)	0.0210 (9)	0.0428 (12)	0.0020 (8)	−0.0183 (9)	0.0093 (9)
P1	0.0142 (2)	0.0127 (2)	0.0119 (2)	0.0054 (2)	0.00441 (19)	0.0056 (2)
P2	0.0130 (2)	0.0128 (2)	0.0134 (2)	0.00524 (19)	0.00531 (19)	0.0078 (2)

Geometric parameters (Å, º)

Ag1—O1	2.4451 (16)	C121—P1	1.823 (2)
Ag1—O2	2.8573 (17)	C122—C123	1.387 (3)
Ag1—O11	2.5588 (19)	C122—H122	0.95
Ag1—P1	2.4354 (5)	C123—C124	1.390 (3)
Ag1—P2	2.4268 (6)	C123—H123	0.95
C1—C1^i	1.535 (4)	C124—C125	1.381 (3)
C1—P1	1.834 (2)	C124—H124	0.95
C1—H1A	0.99	C125—C126	1.396 (3)
C1—H1B	0.99	C125—H125	0.95
C2—C2^ii	1.529 (4)	C126—H126	0.95
C2—P2	1.834 (2)	C211—C212	1.395 (3)
C2—H2A	0.99	C211—C216	1.396 (3)
C2—H2B	0.99	C211—P2	1.828 (2)
C11—O11	1.223 (3)	C212—C213	1.390 (3)
C11—N11	1.331 (3)	C212—H212	0.95
C11—H11	0.95	C213—C214	1.387 (3)
C12—N11	1.451 (4)	C213—H213	0.95
C12—H12A	0.98	C214—C215	1.381 (3)
C12—H12B	0.98	C214—H214	0.95
C12—H12C	0.98	C215—C216	1.389 (3)
C13—N11	1.454 (3)	C215—H215	0.95
C13—H13A	0.98	C216—H216	0.95
C13—H13B	0.98	C221—C222	1.401 (3)
C13—H13C	0.98	C221—C226	1.402 (3)
C111—C112	1.389 (3)	C221—P2	1.818 (2)
C111—C116	1.398 (3)	C222—C223	1.391 (3)
C111—P1	1.829 (2)	C222—H222	0.95
C112—C113	1.398 (3)	C223—C224	1.386 (4)
C112—H112	0.95	C223—H223	0.95
C113—C114	1.377 (4)	C224—C225	1.386 (4)
C113—H113	0.95	C224—H224	0.95
C114—C115	1.382 (4)	C225—C226	1.390 (3)
C114—H114	0.95	C225—H225	0.95
C115—C116	1.391 (3)	C226—H226	0.95
C115—H115	0.95	N1—O3	1.240 (2)
C116—H116	0.95	N1—O2	1.256 (2)
C121—C126	1.401 (3)	N1—O1	1.276 (2)
C121—C122	1.407 (3)
P2—Ag1—P1	139.863 (18)	C125—C124—H124	120
P2—Ag1—O1	107.38 (4)	C123—C124—H124	120
P1—Ag1—O1	110.53 (4)	C124—C125—C126	120.4 (2)
P2—Ag1—O11	101.31 (6)	C124—C125—H125	119.8
P1—Ag1—O11	95.67 (5)	C126—C125—H125	119.8
O1—Ag1—O11	83.44 (7)	C125—C126—C121	120.2 (2)
P2—Ag1—O2	106.37 (4)	C125—C126—H126	119.9
P1—Ag1—O2	89.91 (4)	C121—C126—H126	119.9
O1—Ag1—O2	47.74 (5)	C212—C211—C216	119.07 (19)
O11—Ag1—O2	128.93 (7)	C212—C211—P2	116.91 (16)
C1^i—C1—P1	109.73 (17)	C216—C211—P2	123.99 (16)
C1^i—C1—H1A	109.7	C213—C212—C211	120.3 (2)
P1—C1—H1A	109.7	C213—C212—H212	119.8
C1^i—C1—H1B	109.7	C211—C212—H212	119.8
P1—C1—H1B	109.7	C214—C213—C212	120.0 (2)
H1A—C1—H1B	108.2	C214—C213—H213	120
C2^ii—C2—P2	110.53 (18)	C212—C213—H213	120
C2^ii—C2—H2A	109.5	C215—C214—C213	120.1 (2)
P2—C2—H2A	109.5	C215—C214—H214	120
C2^ii—C2—H2B	109.5	C213—C214—H214	120
P2—C2—H2B	109.5	C214—C215—C216	120.2 (2)
H2A—C2—H2B	108.1	C214—C215—H215	119.9
O11—C11—N11	124.4 (3)	C216—C215—H215	119.9
O11—C11—H11	117.8	C215—C216—C211	120.3 (2)
N11—C11—H11	117.8	C215—C216—H216	119.8
N11—C12—H12A	109.5	C211—C216—H216	119.8
N11—C12—H12B	109.5	C222—C221—C226	119.0 (2)
H12A—C12—H12B	109.5	C222—C221—P2	122.03 (16)
N11—C12—H12C	109.5	C226—C221—P2	118.94 (17)
H12A—C12—H12C	109.5	C223—C222—C221	120.3 (2)
H12B—C12—H12C	109.5	C223—C222—H222	119.8
N11—C13—H13A	109.5	C221—C222—H222	119.8
N11—C13—H13B	109.5	C224—C223—C222	120.2 (2)
H13A—C13—H13B	109.5	C224—C223—H223	119.9
N11—C13—H13C	109.5	C222—C223—H223	119.9
H13A—C13—H13C	109.5	C225—C224—C223	119.9 (2)
H13B—C13—H13C	109.5	C225—C224—H224	120
C112—C111—C116	119.3 (2)	C223—C224—H224	120
C112—C111—P1	119.33 (16)	C224—C225—C226	120.5 (2)
C116—C111—P1	121.36 (17)	C224—C225—H225	119.7
C111—C112—C113	120.0 (2)	C226—C225—H225	119.7
C111—C112—H112	120	C225—C226—C221	120.0 (2)
C113—C112—H112	120	C225—C226—H226	120
C114—C113—C112	120.1 (2)	C221—C226—H226	120
C114—C113—H113	119.9	O3—N1—O2	121.31 (19)
C112—C113—H113	119.9	O3—N1—O1	119.94 (18)
C113—C114—C115	120.4 (2)	O2—N1—O1	118.74 (18)
C113—C114—H114	119.8	N1—O2—Ag1	86.18 (12)
C115—C114—H114	119.8	C11—N11—C12	120.7 (2)
C114—C115—C116	120.0 (2)	C11—N11—C13	121.6 (3)
C114—C115—H115	120	C12—N11—C13	117.6 (2)
C116—C115—H115	120	N1—O1—Ag1	105.41 (12)
C115—C116—C111	120.2 (2)	C11—O11—Ag1	135.48 (19)
C115—C116—H116	119.9	C121—P1—C111	103.80 (9)
C111—C116—H116	119.9	C121—P1—C1	104.77 (9)
C126—C121—C122	118.8 (2)	C111—P1—C1	103.17 (10)
C126—C121—P1	124.05 (17)	C121—P1—Ag1	117.53 (7)
C122—C121—P1	117.15 (16)	C111—P1—Ag1	116.35 (7)
C123—C122—C121	120.3 (2)	C1—P1—Ag1	109.70 (7)
C123—C122—H122	119.8	C221—P2—C211	106.06 (9)
C121—C122—H122	119.8	C221—P2—C2	102.30 (9)
C122—C123—C124	120.3 (2)	C211—P2—C2	104.56 (10)
C122—C123—H123	119.8	C221—P2—Ag1	119.87 (7)
C124—C123—H123	119.8	C211—P2—Ag1	111.50 (7)
C125—C124—C123	119.9 (2)	C2—P2—Ag1	111.17 (7)
C116—C111—C112—C113	−1.4 (4)	C112—C111—P1—C121	113.25 (19)
P1—C111—C112—C113	176.95 (19)	C116—C111—P1—C121	−68.4 (2)
C111—C112—C113—C114	−0.5 (4)	C112—C111—P1—C1	−137.66 (18)
C112—C113—C114—C115	1.9 (4)	C116—C111—P1—C1	40.7 (2)
C113—C114—C115—C116	−1.3 (4)	C112—C111—P1—Ag1	−17.5 (2)
C114—C115—C116—C111	−0.6 (4)	C116—C111—P1—Ag1	160.84 (17)
C112—C111—C116—C115	2.0 (4)	C1^i—C1—P1—C121	177.02 (19)
P1—C111—C116—C115	−176.4 (2)	C1^i—C1—P1—C111	68.7 (2)
C126—C121—C122—C123	−0.3 (3)	C1^i—C1—P1—Ag1	−56.0 (2)
P1—C121—C122—C123	−179.09 (18)	P2—Ag1—P1—C121	75.71 (8)
C121—C122—C123—C124	1.7 (4)	O1—Ag1—P1—C121	−124.43 (9)
C122—C123—C124—C125	−1.2 (4)	O11—Ag1—P1—C121	−39.34 (10)
C123—C124—C125—C126	−0.6 (4)	P2—Ag1—P1—C111	−160.34 (8)
C124—C125—C126—C121	1.9 (4)	O1—Ag1—P1—C111	−0.48 (9)
C122—C121—C126—C125	−1.4 (3)	O11—Ag1—P1—C111	84.61 (10)
P1—C121—C126—C125	177.23 (18)	P2—Ag1—P1—C1	−43.76 (8)
C216—C211—C212—C213	−0.9 (3)	O1—Ag1—P1—C1	116.09 (8)
P2—C211—C212—C213	177.25 (17)	O11—Ag1—P1—C1	−158.81 (9)
C211—C212—C213—C214	0.0 (3)	C222—C221—P2—C211	64.2 (2)
C212—C213—C214—C215	1.3 (4)	C226—C221—P2—C211	−117.10 (17)
C213—C214—C215—C216	−1.5 (4)	C222—C221—P2—C2	−45.1 (2)
C214—C215—C216—C211	0.6 (4)	C226—C221—P2—C2	133.60 (17)
C212—C211—C216—C215	0.6 (3)	C222—C221—P2—Ag1	−168.57 (15)
P2—C211—C216—C215	−177.38 (18)	C226—C221—P2—Ag1	10.14 (19)
C226—C221—C222—C223	0.2 (3)	C212—C211—P2—C221	107.02 (17)
P2—C221—C222—C223	178.90 (18)	C216—C211—P2—C221	−74.9 (2)
C221—C222—C223—C224	−0.3 (4)	C212—C211—P2—C2	−145.30 (16)
C222—C223—C224—C225	0.0 (4)	C216—C211—P2—C2	32.8 (2)
C223—C224—C225—C226	0.5 (4)	C212—C211—P2—Ag1	−25.08 (18)
C224—C225—C226—C221	−0.6 (3)	C216—C211—P2—Ag1	152.98 (17)
C222—C221—C226—C225	0.2 (3)	C2^ii—C2—P2—C221	178.81 (19)
P2—C221—C226—C225	−178.50 (17)	C2^ii—C2—P2—C211	68.4 (2)
O11—C11—N11—C12	−1.2 (4)	C2^ii—C2—P2—Ag1	−52.1 (2)
O11—C11—N11—C13	−179.3 (3)	P1—Ag1—P2—C221	87.60 (8)
O3—N1—O1—Ag1	163.48 (16)	O1—Ag1—P2—C221	−72.65 (9)
O2—N1—O1—Ag1	−15.5 (2)	O11—Ag1—P2—C221	−159.24 (9)
P2—Ag1—O1—N1	104.58 (12)	P1—Ag1—P2—C211	−147.72 (7)
P1—Ag1—O1—N1	−61.97 (13)	O1—Ag1—P2—C211	52.03 (8)
O11—Ag1—O1—N1	−155.58 (14)	O11—Ag1—P2—C211	−34.55 (9)
N11—C11—O11—Ag1	179.59 (19)	P1—Ag1—P2—C2	−31.47 (8)
P2—Ag1—O11—C11	86.9 (3)	O1—Ag1—P2—C2	168.29 (8)
P1—Ag1—O11—C11	−129.6 (3)	O11—Ag1—P2—C2	81.70 (9)
O1—Ag1—O11—C11	−19.6 (3)	O3—N1—O2—Ag1	−166.20 (18)
C126—C121—P1—C111	103.80 (19)	O1—N1—O2—Ag1	12.76 (18)
C122—C121—P1—C111	−77.53 (18)	P2—Ag1—O2—N1	−106.69 (11)
C126—C121—P1—C1	−4.1 (2)	P1—Ag1—O2—N1	110.53 (11)
C122—C121—P1—C1	174.57 (17)	O1—Ag1—O2—N1	−7.85 (11)
C126—C121—P1—Ag1	−126.14 (17)	O11—Ag1—O2—N1	13.32 (15)
C122—C121—P1—Ag1	52.53 (18)

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