Di­aqua­bis(μ-4-hydroxy­benzene­carboxyl­ato-κ²O,O′)­disilver(I)(Ag—Ag) tetrahydrate

The title complex, [Ag₂(C₇H₅O₃)₂(H₂O)₂]·4H₂O, is a centrosymmetric bis­(carboxyl­ato-κ²O,O′)-bridged binuclear dimer with a strong Ag—Ag interaction. Each Ag^I atom has a four-coordinate square-planar geometry, in which it is bonded to two carboxyl­ate O atoms, one water O atom and the other Ag^I atom. All the coordinated and uncoordinated water mol­ecules are disordered; they form a cluster around the dimer through intermolecular hydrogen-bond networks, linking the complex mol­ecules to each other.

Key indicators

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.025
• wR factor = 0.065
• Data-to-parameter ratio = 16.7

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D       H42    ..  H62     ..       2.03 Ang.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Ag1    -   O4      ..       6.76 su
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.32
PLAT725_ALERT_1_C D-H     Calc     0.90713, Rep     0.92000 Dev...       0.01 Ang.
              O5   -H51     1.555   1.555
PLAT725_ALERT_1_C D-H     Calc     0.91559, Rep     0.93000 Dev...       0.01 Ang.
              O5   -H53     1.555   1.555
PLAT726_ALERT_1_C H...A   Calc     2.13936, Rep     2.15000 Dev...       0.01 Ang.
              H63  -O6      1.555   2.655

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

   4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 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
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: RAPID-AUTO (Rigaku, 2003); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2004) and CRYSTALS (Watkin et al., 1996); program(s) used to solve structure: SIR97 (Altomare et al., 1999) and DIRDIF99 (Beurskens et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: CrystalStructure.

Diaquabis(µ-4-hydroxybenzenecarboxylato-κ²O,O')disilver(I)(Ag—Ag) tetrahydrate

Crystal data

[Ag2(C7H5O3)2(H2O)2]·4H2O	Z = 1
Mr = 598.06	F(000) = 296
Triclinic, P1	Dx = 2.085 Mg m^−3
Hall symbol: -p_1	Mo Kα radiation, λ = 0.71075 Å
a = 6.635 (5) Å	Cell parameters from 4290 reflections
b = 9.239 (7) Å	θ = 3.3–27.5°
c = 9.359 (8) Å	µ = 2.11 mm^−1
α = 115.53 (3)°	T = 296 K
β = 107.51 (2)°	Prism, colorless
γ = 95.60 (2)°	0.30 × 0.10 × 0.10 mm
V = 476.2 (7) Å^3

Data collection

Rigaku R-AXIS RAPID diffractometer	2149 independent reflections
Radiation source: fine-focus sealed tube	1950 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.012
Detector resolution: 10.00 pixels mm^-1	θmax = 27.5°, θmin = 3.3°
ω scans	h = −8→8
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −11→11
Tmin = 0.590, Tmax = 0.810	l = −12→11
4695 measured 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)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.065	H-atom parameters constrained
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0336P)^2 + 0.2921P] where P = (Fo^2 + 2Fc^2)/3
2149 reflections	(Δ/σ)max < 0.001
129 parameters	Δρmax = 0.96 e Å^−3
45 restraints	Δρmin = −0.83 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	Occ. (<1)
Ag1	0.48279 (4)	0.33905 (2)	0.47207 (3)	0.05192 (10)
O1	0.2306 (3)	0.3855 (2)	0.5845 (2)	0.0350 (4)
O2	0.3108 (3)	0.6588 (2)	0.6712 (2)	0.0373 (4)
O3	−0.3923 (3)	0.6256 (2)	0.9909 (2)	0.0375 (4)
H31	−0.4054	0.7206	1.0217	0.045*	0.50
H32	−0.4223	0.5468	1.0065	0.045*	0.50
O4	0.3802 (3)	0.0273 (2)	0.3684 (3)	0.0493 (5)
H41	0.2363	0.0193	0.3640	0.074*	0.50
H42	0.4132	−0.0101	0.2736	0.074*
H43	0.4567	0.0043	0.4534	0.074*	0.50
O5	−0.0250 (3)	0.0622 (2)	0.3852 (3)	0.0456 (4)
H51	0.0200	0.1743	0.4526	0.068*
H52	0.1073	0.0493	0.3665	0.068*	0.50
H53	−0.0036	0.0398	0.4741	0.068*	0.50
O6	0.5561 (3)	−0.0597 (2)	0.1205 (3)	0.0484 (5)
H61	0.5326	−0.1725	0.0592	0.073*	0.50
H62	0.6842	−0.0031	0.2152	0.073*
H63	0.5561	0.0316	0.1033	0.073*	0.50
C1	0.0514 (3)	0.5535 (3)	0.7508 (3)	0.0265 (4)
C2	−0.0743 (4)	0.4195 (3)	0.7454 (3)	0.0299 (4)
H2	−0.0568	0.3135	0.6887	0.036*
C3	−0.2251 (4)	0.4422 (3)	0.8234 (3)	0.0300 (4)
H3	−0.3096	0.3518	0.8175	0.036*
C4	−0.2490 (3)	0.6008 (3)	0.9104 (3)	0.0279 (4)
C5	−0.1249 (4)	0.7351 (3)	0.9166 (3)	0.0339 (5)
H5	−0.1418	0.8412	0.9737	0.041*
C6	0.0237 (4)	0.7106 (3)	0.8376 (3)	0.0316 (5)
H6	0.1068	0.8011	0.8427	0.038*
C7	0.2105 (3)	0.5312 (3)	0.6626 (3)	0.0283 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ag1	0.06155 (16)	0.03772 (13)	0.07920 (19)	0.01621 (10)	0.05755 (14)	0.02659 (12)
O1	0.0310 (8)	0.0349 (8)	0.0410 (9)	0.0076 (7)	0.0227 (7)	0.0141 (7)
O2	0.0368 (8)	0.0389 (9)	0.0476 (10)	0.0096 (7)	0.0297 (8)	0.0216 (8)
O3	0.0437 (9)	0.0360 (9)	0.0542 (10)	0.0170 (8)	0.0384 (8)	0.0256 (8)
O4	0.0562 (11)	0.0444 (11)	0.0615 (12)	0.0195 (9)	0.0367 (10)	0.0270 (10)
O5	0.0470 (10)	0.0382 (10)	0.0533 (11)	0.0084 (8)	0.0238 (9)	0.0212 (9)
O6	0.0483 (10)	0.0387 (10)	0.0510 (11)	0.0074 (8)	0.0257 (9)	0.0121 (9)
C1	0.0222 (9)	0.0335 (11)	0.0265 (10)	0.0064 (8)	0.0126 (8)	0.0150 (9)
C2	0.0302 (10)	0.0305 (11)	0.0336 (11)	0.0095 (9)	0.0175 (9)	0.0157 (9)
C3	0.0301 (10)	0.0305 (11)	0.0360 (11)	0.0060 (9)	0.0184 (9)	0.0182 (9)
C4	0.0254 (9)	0.0345 (11)	0.0302 (10)	0.0088 (9)	0.0160 (8)	0.0173 (9)
C5	0.0378 (12)	0.0286 (11)	0.0430 (13)	0.0103 (9)	0.0257 (10)	0.0168 (10)
C6	0.0303 (10)	0.0304 (11)	0.0383 (12)	0.0046 (9)	0.0190 (9)	0.0170 (10)
C7	0.0225 (9)	0.0375 (11)	0.0270 (10)	0.0079 (9)	0.0123 (8)	0.0156 (9)

Geometric parameters (Å, º)

Ag1—O2^i	2.190 (2)	O5—H53	0.9160
Ag1—O1	2.214 (2)	O6—H61	0.9163
Ag1—O4	2.552 (3)	O6—H62	0.9176
Ag1—Ag1^i	2.761 (2)	O6—H63	0.9241
O1—C7	1.269 (3)	C1—C6	1.388 (3)
O2—C7	1.254 (3)	C1—C2	1.397 (3)
O2—Ag1^i	2.190 (2)	C1—C7	1.503 (3)
O3—C4	1.360 (3)	C2—C3	1.388 (3)
O3—H31	0.820	C2—H2	0.930
O3—H32	0.8185	C3—C4	1.390 (3)
O4—H41	0.9370	C3—H3	0.930
O4—H42	0.9071	C4—C5	1.389 (3)
O4—H43	0.9269	C5—C6	1.381 (3)
O5—H51	0.9066	C5—H5	0.930
O5—H52	0.9540	C6—H6	0.930
O2^i—Ag1—O1	162.24 (7)	H62—O6—H63	91.1
O2^i—Ag1—O4	98.58 (7)	C6—C1—C2	118.4 (2)
O1—Ag1—O4	93.51 (7)	C6—C1—C7	119.6 (2)
O2^i—Ag1—Ag1^i	81.79 (5)	C2—C1—C7	121.9 (2)
O1—Ag1—Ag1^i	83.75 (5)	C3—C2—C1	120.9 (2)
O4—Ag1—Ag1^i	168.31 (5)	C3—C2—H2	119.5
C7—O1—Ag1	121.30 (15)	C1—C2—H2	119.5
C7—O2—Ag1^i	125.23 (15)	C2—C3—C4	119.6 (2)
C4—O3—H31	109.5	C2—C3—H3	120.2
C4—O3—H32	109.8	C4—C3—H3	120.2
H31—O3—H32	139.7	O3—C4—C5	119.8 (2)
Ag1—O4—H41	96.2	O3—C4—C3	120.2 (2)
Ag1—O4—H42	99.5	C5—C4—C3	120.0 (2)
H41—O4—H42	123.1	C6—C5—C4	119.8 (2)
Ag1—O4—H43	110.6	C6—C5—H5	120.1
H41—O4—H43	107.6	C4—C5—H5	120.1
H42—O4—H43	116.8	C5—C6—C1	121.2 (2)
H51—O5—H52	96.5	C5—C6—H6	119.4
H51—O5—H53	95.0	C1—C6—H6	119.4
H52—O5—H53	100.7	O2—C7—O1	125.5 (2)
H61—O6—H62	116.5	O2—C7—C1	116.9 (2)
H61—O6—H63	139.6	O1—C7—C1	117.6 (2)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H31···O6^ii	0.82	1.92	2.729 (4)	171
O3—H32···O3^iii	0.82	1.93	2.701 (3)	157
O4—H41···O5	0.94	1.86	2.782 (4)	166
O4—H42···O6	0.91	1.87	2.756 (4)	165
O4—H43···O4^iv	0.93	1.86	2.777 (4)	177
O5—H51···O1	0.92	1.91	2.754 (2)	155
O5—H52···O4	0.95	1.84	2.782 (4)	169
O5—H53···O5^v	0.93	1.90	2.793 (4)	165
O6—H61···O3^vi	0.91	1.87	2.729 (4)	157
O6—H62···O5^vii	0.92	1.92	2.823 (3)	164
O6—H63···O6^viii	0.93	2.15	2.858 (4)	133

Symmetry codes: (ii) x−1, y+1, z+1; (iii) −x−1, −y+1, −z+2; (iv) −x+1, −y, −z+1; (v) −x, −y, −z+1; (vi) x+1, y−1, z−1; (vii) x+1, y, z; (viii) −x+1, −y, −z.