catena-Poly[aqua­silver(I)-μ-4,4′-bipyridine] catena-poly[[aqua­(naphthalene-1,4-dicarboxyl­ato)silver(I)]-μ-4,4′-bipyridine] polyhydrate

Ye, L.; Wu, Y.

doi:10.1107/S1600536805026802

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catena-Poly[aquasilver(I)-μ-4,4′-bipyridine] catena-poly[[aqua(naphthalene-1,4-dicarboxylato)silver(I)]-μ-4,4′-bipyridine] polyhydrate

L. Ye and Y. Wu

The title complex, {[Ag(C₁₀H₈N₂)(H₂O)][Ag(C₁₀H₈N₂)(C₁₂H₆O₄)(H₂O)]·H₂O}_n, consists of cationic complex chains, anionic complex chains and solvent water molecules. In the cationic chain, the Ag atom adopts a trigonal coordination geometry, while the Ag atom in the anionic chain assumes a square-planar coordination geometry.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805026802/xu6029sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805026802/xu6029Isup2.hkl Contains datablock I

CCDC reference: 287758

checkCIF report

Key indicators

Single-crystal X-ray study
T = 294 K
Mean (C-C) = 0.004 Å
R factor = 0.037
wR factor = 0.096
Data-to-parameter ratio = 14.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N4
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C13
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C21
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       3.23
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       3.21
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          7

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

The photoluminescent property of polynuclear d¹⁰ metal complexes has attracted extensive interest (Chen & Liu, 2002). Recently, a series of polynuclear d¹⁰ metal complexes with 1,4-benzenedicarboxylates have been investigated (Yaghi et al., 2003). We present here the structure of a similar Ag^I complex, (I), incorporating the naphthalenedicarboxylate (NDC) ligand (Vodak et al., 2001).

The structure of (I) consists of 4,4'-bipyridine-bridged cationic complex chains, anionic complex chains and solvent water molecules. A segment of the polymeric structure of (I) is shown in Fig. 1. Within the cationic chain, atom Ag1 adopts a distorted trigonal coordination geometry, defined by two N donors from two 4,4'-bipyridine ligands and one water molecule, while in the anionic chain, atom Ag2 has a distorted square-planar coordination geometry, formed by two N donors from two 4,4'-bipyridine, one water molecule and one O atom of the NDC ligand.

The Ag1—O2W, Ag2—O3 and Ag2—O3W distances (Table 1) are much shorter than the sum of the van der Waals radii (Reference for van der Waals data?) and imply a bonding interaction between the Ag and O atoms, but these bonding interactions are weak, because the bond distances are much longer than the sum of the covalent radii (Ma et al., 2005). The average Ag—N bond distance of 2.164 (2) Å agrees with that found in a reported Ag^I complex with 4,4'-bipyridine (Sun et al., 2003).

The nearest Ag1···Ag2 separation between neighbouring polymeric chains is 3.3978 (8) Å, which is identical to the sum of the van der Waals radii of Ag atoms, and implies a weak interaction between the Ag atoms of neighbouring chains. The centroid-to-centroid separations of 3.548 (2) Å between parallel N2-pyridine and N2(−x, 1 − y, 1 − z)-pyridine rings, and 3.559 (2) Å between nearly parallel N2-pyridine and N3-pyridine rings, suggest the existence of π–π stacking. Extensive hydrogen bonding occurs in the crystal structure of (I) (Table 2).

Experimental top

A mixture of AgNO₃ (0.170 g, 1 mmol), H₂NDC (0.108 g, 0.5 mmol) and NaOH (0.04 g, 1 mmol) in water (10 ml) was stirred for 10 min at room temperature. 4,4'-Bipyridine (0.090 g, 0.5 mmol) was then added to the mixture. After stirring for a further 10 min, a white precipitate was collected and dissolved in 14 M ammonia (10 ml). Single crystals of (I) were obtained by slow evaporation at room temperature (yield 55%, based on Ag). Analysis, calculated for C₃₂H₂₈Ag₂N₄O₇: C 48.22, H 3.52, N 7.03%; found: C 48.35, H 3.44, N 7.18%.

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: Crystal Structure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.

Figures top

Fig. 1. A segment of the polymeric Ag^I complex chains, with 50% probability displacement ellipsoids (arbitrary spheres for H atoms) [symmetry code: (A) x, −1 + y, z]. The dashed line indicates the weak van der Waals interaction between Ag atoms of neighbouring chains.

catena-Poly[aquasilver(I)-µ-4,4'-bipyridine] catena-poly[[aqua(naphthalene-1,4-dicarboxylato)silver(I)]-µ-4,4'-bipyridine] polyhydrate top

Crystal data top

[Ag(C₁₀H₈N₂)(H₂O)][Ag(C₁₀H₈N₂)(C₁₂H₆O₄)(H₂O)]·H₂O	Z = 2
M_r = 796.32	F(000) = 796
Triclinic, P1	D_x = 1.846 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.5977 (19) Å	Cell parameters from 10623 reflections
b = 11.444 (2) Å	θ = 3.1–27.4°
c = 14.018 (3) Å	µ = 1.43 mm⁻¹
α = 78.50 (3)°	T = 294 K
β = 71.77 (3)°	Block, colourless
γ = 86.82 (3)°	0.50 × 0.33 × 0.24 mm
V = 1433.0 (6) Å³

Data collection top

Rigaku R-AXIS RAPID diffractometer	6361 independent reflections
Radiation source: rotating anode	4888 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.036
ω scans	θ_max = 27.4°, θ_min = 3.1°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −12→11
T_min = 0.506, T_max = 0.710	k = −14→14
13653 measured reflections	l = −18→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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.096	H atoms treated by a mixture of independent and constrained refinement
S = 1.10	w = 1/[σ²(F_o²) + (0.0401P)² + 0.6543P] where P = (F_o² + 2F_c²)/3
6361 reflections	(Δ/σ)_max = 0.001
430 parameters	Δρ_max = 1.19 e Å⁻³
2 restraints	Δρ_min = −0.97 e Å⁻³

Crystal data top

[Ag(C₁₀H₈N₂)(H₂O)][Ag(C₁₀H₈N₂)(C₁₂H₆O₄)(H₂O)]·H₂O	γ = 86.82 (3)°
M_r = 796.32	V = 1433.0 (6) Å³
Triclinic, P1	Z = 2
a = 9.5977 (19) Å	Mo Kα radiation
b = 11.444 (2) Å	µ = 1.43 mm⁻¹
c = 14.018 (3) Å	T = 294 K
α = 78.50 (3)°	0.50 × 0.33 × 0.24 mm
β = 71.77 (3)°

Data collection top

Rigaku R-AXIS RAPID diffractometer	6361 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	4888 reflections with I > 2σ(I)
T_min = 0.506, T_max = 0.710	R_int = 0.036
13653 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	2 restraints
wR(F²) = 0.096	H atoms treated by a mixture of independent and constrained refinement
S = 1.10	Δρ_max = 1.19 e Å⁻³
6361 reflections	Δρ_min = −0.97 e Å⁻³
430 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
C1	0.1398 (4)	0.9279 (3)	0.6035 (3)	0.0474 (9)
H1	0.2274	0.9676	0.5914	0.057*
C2	0.1445 (3)	0.8071 (3)	0.5985 (3)	0.0458 (9)
H2	0.2344	0.7688	0.5813	0.055*
C3	0.0162 (3)	0.7440 (2)	0.6189 (2)	0.0265 (6)
C4	0.0172 (3)	0.6139 (2)	0.6193 (2)	0.0261 (6)
C5	0.1488 (3)	0.5513 (3)	0.5949 (3)	0.0398 (8)
H5	0.2382	0.5912	0.5747	0.048*
C6	0.1447 (4)	0.4286 (3)	0.6010 (3)	0.0424 (8)
H6	0.2331	0.3880	0.5854	0.051*
C7	−0.1036 (4)	0.4262 (3)	0.6493 (3)	0.0408 (8)
H7	−0.1912	0.3843	0.6670	0.049*
C8	−0.1109 (3)	0.5480 (3)	0.6470 (3)	0.0373 (7)
H8	−0.2015	0.5854	0.6640	0.045*
C9	−0.1118 (4)	0.8083 (3)	0.6400 (3)	0.0465 (9)
H9	−0.2010	0.7708	0.6526	0.056*
C10	−0.1088 (4)	0.9289 (3)	0.6427 (3)	0.0447 (9)
H10	−0.1972	0.9695	0.6576	0.054*
C11	0.0809 (4)	0.9459 (3)	0.8643 (3)	0.0512 (10)
H11	0.1695	0.9859	0.8482	0.061*
C12	0.0828 (4)	0.8243 (3)	0.8657 (3)	0.0492 (10)
H12	0.1723	0.7853	0.8498	0.059*
C13	−0.0446 (3)	0.7600 (2)	0.8898 (2)	0.0285 (6)
C14	−0.1731 (4)	0.8254 (3)	0.9153 (4)	0.0576 (11)
H14	−0.2636	0.7875	0.9343	0.069*
C15	−0.1665 (4)	0.9470 (3)	0.9123 (4)	0.0591 (11)
H15	−0.2542	0.9882	0.9305	0.071*
C16	−0.0471 (3)	0.6311 (2)	0.8877 (2)	0.0270 (6)
C17	−0.1771 (3)	0.5671 (3)	0.9122 (3)	0.0352 (7)
H17	−0.2669	0.6052	0.9314	0.042*
C18	−0.1730 (4)	0.4465 (3)	0.9081 (3)	0.0381 (7)
H18	−0.2614	0.4061	0.9248	0.046*
C19	0.0823 (3)	0.5667 (3)	0.8594 (3)	0.0359 (7)
H036	0.1721	0.6052	0.8423	0.043*
C20	0.0793 (4)	0.4471 (3)	0.8565 (3)	0.0377 (7)
H20	0.1676	0.4070	0.8368	0.045*
N1	0.0145 (3)	0.9890 (2)	0.6251 (2)	0.0322 (6)
N2	0.0202 (3)	0.3661 (2)	0.6280 (2)	0.0312 (6)
N3	−0.0489 (3)	0.3859 (2)	0.8816 (2)	0.0325 (6)
N4	−0.0430 (3)	1.0072 (2)	0.8853 (2)	0.0362 (6)
O1W	0.5048 (4)	0.8595 (3)	0.1276 (2)	0.0622 (8)
O2W	0.2573 (3)	0.2058 (2)	0.7862 (2)	0.0468 (6)
O3W	−0.2916 (3)	0.1788 (2)	0.6767 (3)	0.0516 (7)
Ag1	−0.03558 (3)	0.19760 (2)	0.87674 (2)	0.04809 (10)
Ag2	0.01754 (3)	0.176703 (19)	0.62945 (2)	0.04427 (10)
O1	0.5124 (3)	0.2715 (2)	0.0258 (2)	0.0572 (7)
O2	0.6040 (5)	0.0954 (3)	0.0659 (2)	0.0891 (12)
O3	0.3257 (3)	0.1651 (2)	0.58441 (18)	0.0451 (6)
O4	0.5394 (3)	0.2597 (3)	0.54520 (19)	0.0514 (6)
C21	0.5497 (4)	0.1911 (3)	0.0880 (3)	0.0376 (7)
C22	0.5208 (3)	0.2063 (3)	0.1980 (2)	0.0305 (6)
C23	0.5048 (3)	0.1035 (3)	0.2722 (3)	0.0342 (7)
H23	0.5147	0.0299	0.2523	0.041*
C24	0.4740 (3)	0.1069 (3)	0.3770 (2)	0.0314 (6)
H24	0.4573	0.0358	0.4248	0.038*
C25	0.4684 (3)	0.2129 (3)	0.4095 (2)	0.0286 (6)
C26	0.4417 (3)	0.2131 (3)	0.5223 (2)	0.0297 (6)
C27	0.4912 (3)	0.3228 (2)	0.3338 (2)	0.0266 (6)
C28	0.5114 (3)	0.3202 (2)	0.2292 (2)	0.0285 (6)
C29	0.5239 (3)	0.4317 (3)	0.1592 (3)	0.0369 (7)
H29	0.5351	0.4322	0.0908	0.044*
C30	0.5197 (4)	0.5376 (3)	0.1914 (3)	0.0428 (8)
H30	0.5274	0.6090	0.1447	0.051*
C31	0.5039 (4)	0.5401 (3)	0.2944 (3)	0.0412 (8)
H31	0.5038	0.6127	0.3147	0.049*
C32	0.4888 (3)	0.4365 (3)	0.3641 (3)	0.0351 (7)
H32	0.4768	0.4389	0.4321	0.042*
HW11	0.474 (5)	0.841 (4)	0.081 (4)	0.077 (16)*
HW12	0.520 (4)	0.928 (3)	0.103 (3)	0.032 (10)*
HW21	0.287 (5)	0.190 (4)	0.729 (4)	0.061 (14)*
HW22	0.318 (5)	0.184 (4)	0.817 (3)	0.056 (14)*
HW31	−0.342 (6)	0.188 (5)	0.636 (4)	0.12 (2)*
HW32	−0.342 (5)	0.163 (4)	0.737 (3)	0.057 (14)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0323 (17)	0.0240 (16)	0.082 (3)	−0.0072 (14)	−0.0064 (17)	−0.0163 (16)
C2	0.0243 (16)	0.0291 (16)	0.082 (3)	0.0004 (13)	−0.0067 (16)	−0.0229 (17)
C3	0.0310 (15)	0.0178 (13)	0.0313 (16)	0.0013 (11)	−0.0097 (12)	−0.0064 (11)
C4	0.0327 (15)	0.0176 (12)	0.0297 (15)	0.0031 (11)	−0.0112 (12)	−0.0068 (11)
C5	0.0289 (16)	0.0217 (14)	0.067 (2)	0.0030 (12)	−0.0086 (15)	−0.0154 (14)
C6	0.0330 (17)	0.0262 (16)	0.062 (2)	0.0052 (14)	−0.0043 (15)	−0.0141 (15)
C7	0.0366 (18)	0.0233 (15)	0.064 (2)	−0.0029 (13)	−0.0162 (16)	−0.0098 (15)
C8	0.0292 (16)	0.0229 (14)	0.062 (2)	0.0045 (12)	−0.0148 (15)	−0.0117 (14)
C9	0.0316 (17)	0.0240 (15)	0.087 (3)	0.0008 (13)	−0.0188 (17)	−0.0163 (16)
C10	0.0365 (18)	0.0196 (14)	0.080 (3)	0.0076 (13)	−0.0189 (17)	−0.0152 (16)
C11	0.042 (2)	0.0238 (16)	0.090 (3)	−0.0050 (15)	−0.0209 (19)	−0.0138 (17)
C12	0.0335 (18)	0.0196 (15)	0.094 (3)	0.0054 (13)	−0.0170 (18)	−0.0170 (17)
C13	0.0337 (16)	0.0193 (13)	0.0335 (16)	0.0017 (12)	−0.0097 (12)	−0.0085 (11)
C14	0.0339 (18)	0.0242 (16)	0.105 (3)	0.0004 (14)	−0.0017 (19)	−0.0225 (19)
C15	0.044 (2)	0.0260 (17)	0.099 (3)	0.0039 (16)	−0.004 (2)	−0.0228 (19)
C16	0.0337 (15)	0.0184 (13)	0.0297 (15)	−0.0027 (11)	−0.0088 (12)	−0.0072 (11)
C17	0.0330 (16)	0.0255 (15)	0.0463 (19)	0.0000 (12)	−0.0067 (14)	−0.0136 (13)
C18	0.0395 (18)	0.0251 (15)	0.050 (2)	−0.0058 (13)	−0.0100 (15)	−0.0124 (14)
C19	0.0327 (16)	0.0240 (15)	0.050 (2)	0.0032 (12)	−0.0100 (14)	−0.0101 (13)
C20	0.0325 (16)	0.0258 (15)	0.053 (2)	0.0059 (13)	−0.0098 (14)	−0.0116 (14)
N1	0.0363 (14)	0.0177 (11)	0.0425 (16)	0.0014 (10)	−0.0109 (11)	−0.0078 (10)
N2	0.0403 (15)	0.0150 (11)	0.0394 (15)	−0.0011 (10)	−0.0117 (11)	−0.0084 (10)
N3	0.0441 (15)	0.0172 (11)	0.0362 (14)	0.0007 (11)	−0.0107 (11)	−0.0080 (10)
N4	0.0486 (16)	0.0195 (12)	0.0393 (16)	0.0005 (11)	−0.0090 (12)	−0.0102 (11)
O1W	0.088 (2)	0.059 (2)	0.0488 (18)	0.0077 (17)	−0.0305 (16)	−0.0190 (16)
O2W	0.0450 (15)	0.0451 (14)	0.0469 (17)	0.0050 (12)	−0.0074 (13)	−0.0127 (12)
O3W	0.0456 (16)	0.0458 (15)	0.063 (2)	0.0062 (12)	−0.0166 (15)	−0.0110 (14)
Ag1	0.0744 (2)	0.01665 (13)	0.05871 (19)	0.00243 (12)	−0.02580 (15)	−0.01176 (11)
Ag2	0.0643 (2)	0.01553 (12)	0.05526 (18)	0.00064 (11)	−0.01922 (14)	−0.01095 (10)
O1	0.0739 (18)	0.0570 (17)	0.0455 (16)	−0.0009 (14)	−0.0240 (14)	−0.0113 (13)
O2	0.155 (3)	0.067 (2)	0.0521 (19)	0.040 (2)	−0.033 (2)	−0.0346 (16)
O3	0.0425 (13)	0.0452 (13)	0.0428 (14)	−0.0094 (11)	−0.0017 (11)	−0.0131 (11)
O4	0.0455 (14)	0.0735 (18)	0.0429 (15)	−0.0087 (13)	−0.0175 (11)	−0.0197 (13)
C21	0.0388 (18)	0.0411 (18)	0.0354 (18)	−0.0016 (14)	−0.0116 (14)	−0.0123 (14)
C22	0.0276 (15)	0.0315 (15)	0.0340 (17)	0.0029 (12)	−0.0092 (12)	−0.0109 (12)
C23	0.0351 (16)	0.0268 (14)	0.0464 (19)	0.0054 (13)	−0.0151 (14)	−0.0177 (13)
C24	0.0373 (16)	0.0217 (13)	0.0365 (17)	0.0022 (12)	−0.0139 (13)	−0.0050 (12)
C25	0.0236 (14)	0.0277 (14)	0.0364 (17)	−0.0001 (11)	−0.0098 (12)	−0.0092 (12)
C26	0.0280 (15)	0.0258 (14)	0.0343 (17)	0.0057 (12)	−0.0066 (12)	−0.0095 (12)
C27	0.0200 (13)	0.0243 (13)	0.0370 (17)	0.0002 (11)	−0.0088 (11)	−0.0090 (12)
C28	0.0196 (13)	0.0279 (14)	0.0384 (18)	0.0013 (11)	−0.0075 (12)	−0.0095 (12)
C29	0.0350 (16)	0.0326 (16)	0.0408 (19)	0.0015 (13)	−0.0107 (14)	−0.0035 (13)
C30	0.0393 (18)	0.0267 (15)	0.058 (2)	−0.0009 (14)	−0.0128 (16)	−0.0005 (14)
C31	0.0382 (18)	0.0228 (14)	0.064 (2)	0.0009 (13)	−0.0152 (16)	−0.0119 (15)
C32	0.0299 (16)	0.0324 (16)	0.048 (2)	0.0021 (13)	−0.0133 (14)	−0.0180 (14)

Geometric parameters (Å, º) top

Ag1—N3	2.165 (2)	C16—C17	1.394 (4)
Ag1—N4ⁱ	2.163 (2)	C16—C19	1.396 (4)
Ag1—O2W	2.696 (3)	C17—C18	1.391 (4)
Ag2—N1ⁱ	2.163 (2)	C17—H17	0.9300
Ag2—N2	2.166 (2)	C18—N3	1.331 (4)
Ag2—O3	2.826 (3)	C18—H18	0.9300
Ag2—O3W	2.831 (3)	C19—C20	1.380 (4)
C1—N1	1.338 (4)	C19—H036	0.9300
C1—C2	1.396 (4)	C20—N3	1.362 (4)
C1—H1	0.9300	C20—H20	0.9300
C2—C3	1.384 (4)	O1W—HW11	0.86 (5)
C2—H2	0.9300	O1W—HW12	0.79 (4)
C3—C9	1.378 (4)	O2W—HW21	0.82 (4)
C3—C4	1.488 (4)	O2W—HW22	0.82 (4)
C4—C8	1.385 (4)	O3W—HW31	0.84 (6)
C4—C5	1.397 (4)	O3W—HW32	0.82 (4)
C5—C6	1.392 (4)	O1—C21	1.254 (4)
C5—H5	0.9300	O2—C21	1.239 (4)
C6—N2	1.336 (4)	O3—C26	1.253 (4)
C6—H6	0.9300	O4—C26	1.256 (4)
C7—N2	1.320 (4)	C21—C22	1.524 (4)
C7—C8	1.387 (4)	C22—C23	1.386 (4)
C7—H7	0.9300	C22—C28	1.445 (4)
C8—H8	0.9300	C23—C24	1.413 (4)
C9—C10	1.390 (4)	C23—H23	0.9300
C9—H9	0.9300	C24—C25	1.372 (4)
C10—N1	1.332 (4)	C24—H24	0.9300
C10—H10	0.9300	C25—C27	1.452 (4)
C11—N4	1.328 (5)	C25—C26	1.521 (4)
C11—C12	1.387 (4)	C27—C28	1.424 (4)
C11—H11	0.9300	C27—C32	1.444 (4)
C12—C13	1.375 (4)	C28—C29	1.431 (4)
C12—H12	0.9300	C29—C30	1.370 (5)
C13—C14	1.391 (4)	C29—H29	0.9300
C13—C16	1.483 (4)	C30—C31	1.409 (5)
C14—C15	1.389 (5)	C30—H30	0.9300
C14—H14	0.9300	C31—C32	1.361 (5)
C15—N4	1.314 (5)	C31—H31	0.9300
C15—H15	0.9300	C32—H32	0.9300

N1—C1—C2	122.8 (3)	C10—N1—C1	116.8 (3)
N1—C1—H1	118.6	C10—N1—Ag2ⁱⁱ	122.9 (2)
C2—C1—H1	118.6	C1—N1—Ag2ⁱⁱ	120.3 (2)
C3—C2—C1	120.4 (3)	C7—N2—C6	117.0 (3)
C3—C2—H2	119.8	C7—N2—Ag2	120.4 (2)
C1—C2—H2	119.8	C6—N2—Ag2	122.5 (2)
C9—C3—C2	116.1 (3)	C18—N3—C20	117.3 (3)
C9—C3—C4	122.2 (3)	C18—N3—Ag1	125.0 (2)
C2—C3—C4	121.6 (3)	C20—N3—Ag1	117.7 (2)
C8—C4—C5	116.7 (3)	C15—N4—C11	117.3 (3)
C8—C4—C3	122.2 (3)	C15—N4—Ag1ⁱⁱ	122.8 (2)
C5—C4—C3	121.1 (3)	C11—N4—Ag1ⁱⁱ	119.8 (2)
C6—C5—C4	119.3 (3)	HW11—O1W—HW12	97 (4)
C6—C5—H5	120.4	HW21—O2W—HW22	110 (4)
C4—C5—H5	120.4	HW31—O3W—HW32	113 (5)
N2—C6—C5	123.4 (3)	N4ⁱ—Ag1—N3	173.93 (10)
N2—C6—H6	118.3	N4ⁱ—Ag1—O2W	92.09 (11)
C5—C6—H6	118.3	N3—Ag1—O2W	93.44 (10)
N2—C7—C8	123.9 (3)	N1ⁱ—Ag2—N2	177.87 (10)
N2—C7—H7	118.0	N1ⁱ—Ag2—O3	88.98 (10)
C8—C7—H7	118.0	N2—Ag2—O3	91.27 (9)
C4—C8—C7	119.7 (3)	N1ⁱ—Ag2—O3W	88.93 (10)
C4—C8—H8	120.1	N2—Ag2—O3W	90.84 (10)
C7—C8—H8	120.1	O3—Ag2—O3W	177.79 (8)
C3—C9—C10	120.6 (3)	O2—C21—O1	123.1 (3)
C3—C9—H9	119.7	O2—C21—C22	117.1 (3)
C10—C9—H9	119.7	O1—C21—C22	119.7 (3)
N1—C10—C9	123.3 (3)	C23—C22—C28	118.4 (3)
N1—C10—H10	118.4	C23—C22—C21	117.3 (3)
C9—C10—H10	118.4	C28—C22—C21	124.3 (3)
N4—C11—C12	122.2 (3)	C22—C23—C24	122.2 (3)
N4—C11—H11	118.9	C22—C23—H23	118.9
C12—C11—H11	118.9	C24—C23—H23	118.9
C13—C12—C11	121.6 (3)	C25—C24—C23	121.2 (3)
C13—C12—H12	119.2	C25—C24—H24	119.4
C11—C12—H12	119.2	C23—C24—H24	119.4
C12—C13—C14	115.0 (3)	C24—C25—C27	118.4 (3)
C12—C13—C16	123.3 (3)	C24—C25—C26	119.9 (3)
C14—C13—C16	121.7 (3)	C27—C25—C26	121.7 (2)
C15—C14—C13	120.2 (3)	O3—C26—O4	125.7 (3)
C15—C14—H14	119.9	O3—C26—C25	117.3 (3)
C13—C14—H14	119.9	O4—C26—C25	117.0 (3)
N4—C15—C14	123.5 (3)	C28—C27—C32	119.0 (3)
N4—C15—H15	118.2	C28—C27—C25	120.5 (2)
C14—C15—H15	118.2	C32—C27—C25	120.5 (3)
C17—C16—C19	115.9 (3)	C27—C28—C29	118.0 (3)
C17—C16—C13	122.6 (3)	C27—C28—C22	119.0 (3)
C19—C16—C13	121.4 (3)	C29—C28—C22	123.0 (3)
C18—C17—C16	120.2 (3)	C30—C29—C28	121.0 (3)
C18—C17—H17	119.9	C30—C29—H29	119.5
C16—C17—H17	119.9	C28—C29—H29	119.5
N3—C18—C17	123.3 (3)	C29—C30—C31	121.0 (3)
N3—C18—H18	118.3	C29—C30—H30	119.5
C17—C18—H18	118.3	C31—C30—H30	119.5
C20—C19—C16	121.2 (3)	C32—C31—C30	120.1 (3)
C20—C19—H036	119.4	C32—C31—H31	119.9
C16—C19—H036	119.4	C30—C31—H31	119.9
N3—C20—C19	122.0 (3)	C31—C32—C27	120.8 (3)
N3—C20—H20	119.0	C31—C32—H32	119.6
C19—C20—H20	119.0	C27—C32—H32	119.6

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—HW11···O1ⁱⁱⁱ	0.86 (5)	2.14 (5)	2.904 (4)	148 (4)
O1W—HW12···O2ⁱⁱ	0.79 (4)	2.03 (4)	2.790 (5)	162 (4)
O2W—HW21···O3	0.82 (4)	2.02 (5)	2.825 (4)	170 (4)
O2W—HW22···O1W^iv	0.82 (4)	2.09 (4)	2.900 (5)	171 (4)
O3W—HW31···O4^v	0.84 (6)	1.99 (6)	2.812 (4)	163 (6)
O3W—HW32···O1W^vi	0.82 (4)	2.03 (4)	2.831 (5)	166 (4)

Symmetry codes: (ii) x, y+1, z; (iii) −x+1, −y+1, −z; (iv) −x+1, −y+1, −z+1; (v) x−1, y, z; (vi) −x, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	[Ag(C₁₀H₈N₂)(H₂O)][Ag(C₁₀H₈N₂)(C₁₂H₆O₄)(H₂O)]·H₂O
M_r	796.32
Crystal system, space group	Triclinic, P1
Temperature (K)	294
a, b, c (Å)	9.5977 (19), 11.444 (2), 14.018 (3)
α, β, γ (°)	78.50 (3), 71.77 (3), 86.82 (3)
V (Å³)	1433.0 (6)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.43
Crystal size (mm)	0.50 × 0.33 × 0.24

Data collection
Diffractometer	Rigaku R-AXIS RAPID diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.506, 0.710
No. of measured, independent and observed [I > 2σ(I)] reflections	13653, 6361, 4888
R_int	0.036
(sin θ/λ)_max (Å⁻¹)	0.647

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.096, 1.10
No. of reflections	6361
No. of parameters	430
No. of restraints	2
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.19, −0.97

Computer programs: PROCESS-AUTO (Rigaku, 1998), PROCESS-AUTO, Crystal Structure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1990), SHELXL97.

Selected bond lengths (Å) top

Ag1—N3	2.165 (2)	Ag2—N2	2.166 (2)
Ag1—N4ⁱ	2.163 (2)	Ag2—O3	2.826 (3)
Ag1—O2W	2.696 (3)	Ag2—O3W	2.831 (3)
Ag2—N1ⁱ	2.163 (2)

Symmetry code: (i) x, y−1, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—HW11···O1ⁱⁱ	0.86 (5)	2.14 (5)	2.904 (4)	148 (4)
O1W—HW12···O2ⁱⁱⁱ	0.79 (4)	2.03 (4)	2.790 (5)	162 (4)
O2W—HW21···O3	0.82 (4)	2.02 (5)	2.825 (4)	170 (4)
O2W—HW22···O1W^iv	0.82 (4)	2.09 (4)	2.900 (5)	171 (4)
O3W—HW31···O4^v	0.84 (6)	1.99 (6)	2.812 (4)	163 (6)
O3W—HW32···O1W^vi	0.82 (4)	2.03 (4)	2.831 (5)	166 (4)

Symmetry codes: (ii) −x+1, −y+1, −z; (iii) x, y+1, z; (iv) −x+1, −y+1, −z+1; (v) x−1, y, z; (vi) −x, −y+1, −z+1.

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