Poly[aqua-μ-1H-1,2,3-benzotriazole-μ-nitrato-nitratodisilver(I)]

A unique and stable silver benzotriazole complex, [Ag₂(NO₃)₂(C₆H₃N₃)(H₂O)]_n, is reported in which the benzotriazole is coordinated to the silver as a neutral donor ligand, bridging two silver atoms. Weakly bound nitrate anions and H₂O complete the coordination environment. The structure is built upon a chain of alternating units [–Ag-HBZT-Ag-(NO₃)₂-H₂O–] where the three available bonding sites of the HBZT (1H-1,2,3-benzotriazole) ligand are fully occupied: two N atoms of the azine component are bound to silver and the third retains the original hydrogen.

Key indicators

• Single-crystal X-ray study
• T = 294 K
• Mean [sigma](C-C) = 0.012 Å
• R factor = 0.037
• wR factor = 0.078
• Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
            Tmin and Tmax reported:      0.796     0.974
            Tmin and Tmax expected:      0.515     0.934
            RR =      1.481
            Please check that your absorption correction is appropriate.
PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large .......       1.50
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.96
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         12

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           27.46
           From the CIF: _reflns_number_total               2264
           Count of symmetry unique reflns         1375
           Completeness (_total/calc)            164.65%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured       889
           Fraction of Friedel pairs measured     0.647
           Are heavy atom types Z>Si present        yes

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

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

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Computing details

Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and MaterialsStudio (Accelrys Inc., 2002); software used to prepare material for publication: SHELXTL and MaterialsStudio.

Poly[aqua-µ-1H-1,2,3-benzotriazole-µ-nitrato-nitratodisilver(I)]

Crystal data

[Ag2(NO3)2(C6H3N3)(H2O)]	F(000) = 904
Mr = 474.89	Dx = 2.728 Mg m^−3
Orthorhombic, Pna21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2n	Cell parameters from 5272 reflections
a = 7.0503 (3) Å	θ = 1.0–27.5°
b = 10.9102 (5) Å	µ = 3.43 mm^−1
c = 15.0341 (6) Å	T = 294 K
V = 1156.43 (9) Å^3	Rod, white
Z = 4	0.20 × 0.20 × 0.02 mm

Data collection

Nonius KappaCCD diffractometer	2264 independent reflections
Radiation source: fine-focus sealed tube	1546 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.066
Detector resolution: 9 pixels mm^-1	θmax = 27.5°, θmin = 4.5°
CCD scans	h = −7→9
Absorption correction: multi-scan (SORTAV; Blessing, 1995)	k = −12→14
Tmin = 0.796, Tmax = 0.974	l = −15→19
8772 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.037	H-atom parameters constrained
wR(F^2) = 0.078	w = 1/[σ^2(Fo^2) + (0.0331P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.97	(Δ/σ)max = 0.001
2264 reflections	Δρmax = 0.61 e Å^−3
181 parameters	Δρmin = −0.78 e Å^−3
1 restraint	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.07 (5)

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	0.65513 (8)	0.66622 (6)	0.53586 (4)	0.04770 (19)
Ag2	0.95983 (9)	1.01065 (6)	0.71697 (6)	0.0565 (2)
N1	0.5737 (8)	0.3924 (7)	0.5988 (4)	0.0312 (16)
N2	0.6346 (8)	0.4607 (5)	0.5334 (5)	0.0338 (13)
N3	0.6890 (8)	0.3859 (6)	0.4668 (4)	0.0296 (15)
H3	0.7328	0.4107	0.4165	0.035*
N4	0.4117 (10)	0.7011 (8)	0.3688 (5)	0.0402 (19)
N5	0.8769 (8)	0.7329 (7)	0.7079 (5)	0.0336 (15)
O7	0.6637 (7)	0.9934 (5)	0.8128 (4)	0.0385 (13)
O1	0.4419 (8)	0.7701 (6)	0.4357 (4)	0.0540 (17)
O2	0.4781 (8)	0.5969 (6)	0.3682 (4)	0.0459 (16)
O3	0.3164 (10)	0.7397 (7)	0.3059 (4)	0.0653 (19)
O4	0.8194 (7)	0.7907 (6)	0.6390 (4)	0.0471 (16)
O5	0.8513 (7)	0.6208 (5)	0.7142 (4)	0.0438 (13)
O6	0.9612 (8)	0.7931 (6)	0.7661 (4)	0.0468 (15)
C1	0.5906 (10)	0.2720 (8)	0.5754 (6)	0.0263 (18)
C2	0.5482 (10)	0.1638 (8)	0.6213 (5)	0.0326 (19)
H2	0.4959	0.1653	0.6781	0.039*
C3	0.5873 (11)	0.0553 (8)	0.5787 (6)	0.039 (2)
H3A	0.5623	−0.0182	0.6079	0.047*
C4	0.6638 (10)	0.0520 (9)	0.4926 (6)	0.037 (2)
H4	0.6868	−0.0236	0.4662	0.045*
C5	0.7060 (10)	0.1574 (8)	0.4460 (5)	0.0334 (19)
H5A	0.7581	0.1549	0.3892	0.040*
C6	0.6660 (10)	0.2682 (8)	0.4890 (5)	0.0281 (18)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ag1	0.0586 (4)	0.0413 (4)	0.0433 (3)	−0.0064 (3)	0.0005 (4)	−0.0007 (4)
Ag2	0.0822 (5)	0.0516 (5)	0.0356 (3)	−0.0179 (4)	0.0150 (4)	0.0025 (4)
N1	0.031 (3)	0.037 (5)	0.026 (4)	−0.001 (3)	0.001 (3)	0.002 (3)
N2	0.029 (3)	0.042 (4)	0.031 (3)	0.002 (3)	0.001 (3)	0.002 (4)
N3	0.032 (3)	0.036 (4)	0.021 (3)	0.001 (3)	0.002 (3)	0.002 (3)
N4	0.042 (4)	0.041 (6)	0.038 (4)	0.004 (4)	0.007 (3)	0.007 (4)
N5	0.036 (3)	0.033 (5)	0.031 (4)	0.007 (3)	0.001 (3)	0.003 (4)
O7	0.044 (3)	0.038 (4)	0.033 (3)	0.000 (2)	−0.008 (2)	0.006 (3)
O1	0.057 (4)	0.054 (5)	0.052 (4)	0.007 (3)	0.001 (3)	−0.019 (3)
O2	0.063 (4)	0.035 (4)	0.040 (4)	0.012 (3)	0.003 (3)	−0.003 (3)
O3	0.079 (4)	0.078 (6)	0.038 (3)	0.038 (4)	−0.005 (3)	0.007 (4)
O4	0.054 (4)	0.049 (4)	0.038 (3)	−0.003 (3)	−0.010 (3)	0.004 (3)
O5	0.051 (3)	0.032 (4)	0.049 (3)	0.007 (2)	−0.006 (4)	−0.001 (3)
O6	0.047 (3)	0.054 (4)	0.039 (3)	−0.005 (3)	−0.008 (3)	−0.003 (3)
C1	0.020 (4)	0.035 (6)	0.024 (4)	−0.002 (3)	0.000 (3)	0.003 (4)
C2	0.027 (4)	0.038 (6)	0.033 (4)	−0.008 (4)	−0.001 (3)	0.015 (4)
C3	0.037 (5)	0.032 (6)	0.047 (5)	−0.001 (4)	−0.002 (4)	0.006 (5)
C4	0.030 (5)	0.044 (6)	0.038 (5)	0.004 (4)	−0.002 (4)	−0.005 (4)
C5	0.030 (4)	0.047 (6)	0.023 (4)	−0.002 (4)	−0.001 (3)	0.004 (4)
C6	0.026 (4)	0.031 (5)	0.027 (4)	0.004 (4)	0.000 (3)	−0.001 (4)

Geometric parameters (Å, º)

Ag1—N2	2.247 (6)	N4—O1	1.274 (9)
Ag1—O4	2.365 (6)	N5—O5	1.239 (8)
Ag1—O1	2.411 (6)	N5—O6	1.246 (9)
Ag2—N1^i	2.218 (7)	N5—O4	1.278 (8)
Ag2—O6	2.486 (7)	O2—Ag2^iv	2.500 (6)
Ag2—O2^ii	2.500 (6)	C1—C2	1.400 (11)
Ag2—O7	2.544 (5)	C1—C6	1.404 (9)
N1—N2	1.307 (9)	C2—C3	1.374 (12)
N1—C1	1.365 (10)	C2—H2	0.9300
N1—Ag2^iii	2.218 (6)	C3—C4	1.403 (10)
N2—N3	1.348 (9)	C3—H3A	0.9300
N3—C6	1.337 (11)	C4—C5	1.379 (11)
N3—H3	0.8600	C4—H4	0.9300
N4—O2	1.229 (9)	C5—C6	1.399 (11)
N4—O3	1.235 (9)	C5—H5A	0.9300
N2—Ag1—O4	128.0 (2)	O6—N5—O4	117.4 (7)
N2—Ag1—O1	114.8 (2)	N4—O1—Ag1	108.6 (5)
O4—Ag1—O1	116.4 (2)	N4—O2—Ag2^iv	114.9 (5)
N1^i—Ag2—O6	133.8 (2)	N5—O4—Ag1	113.8 (5)
N1^i—Ag2—O2^ii	119.0 (2)	N5—O6—Ag2	107.0 (5)
O6—Ag2—O2^ii	95.1 (2)	N1—C1—C2	131.7 (7)
N1^i—Ag2—O7	141.8 (2)	N1—C1—C6	107.5 (8)
O6—Ag2—O7	76.35 (19)	C2—C1—C6	120.8 (9)
O2^ii—Ag2—O7	69.89 (18)	C3—C2—C1	117.0 (8)
N2—N1—C1	109.0 (6)	C3—C2—H2	121.5
N2—N1—Ag2^iii	116.7 (5)	C1—C2—H2	121.5
C1—N1—Ag2^iii	134.2 (5)	C2—C3—C4	121.9 (9)
N1—N2—N3	107.9 (6)	C2—C3—H3A	119.0
N1—N2—Ag1	125.3 (6)	C4—C3—H3A	119.0
N3—N2—Ag1	126.7 (5)	C5—C4—C3	122.1 (9)
C6—N3—N2	111.2 (6)	C5—C4—H4	119.0
C6—N3—H3	124.4	C3—C4—H4	119.0
N2—N3—H3	124.4	C4—C5—C6	116.2 (7)
O2—N4—O3	121.1 (8)	C4—C5—H5A	121.9
O2—N4—O1	119.2 (7)	C6—C5—H5A	121.9
O3—N4—O1	119.6 (8)	N3—C6—C5	133.6 (7)
O5—N5—O6	122.4 (7)	N3—C6—C1	104.4 (7)
O5—N5—O4	120.2 (7)	C5—C6—C1	122.0 (9)
C1—N1—N2—N3	0.8 (8)	O4—N5—O6—Ag2	2.7 (7)
Ag2^iii—N1—N2—N3	−177.0 (4)	N1^i—Ag2—O6—N5	−60.4 (6)
C1—N1—N2—Ag1	−176.8 (4)	O2^ii—Ag2—O6—N5	160.1 (5)
Ag2^iii—N1—N2—Ag1	5.3 (7)	O7—Ag2—O6—N5	92.3 (5)
O4—Ag1—N2—N1	55.9 (6)	N2—N1—C1—C2	179.1 (7)
O1—Ag1—N2—N1	−113.1 (6)	Ag2^iii—N1—C1—C2	−3.6 (12)
O4—Ag1—N2—N3	−121.3 (5)	N2—N1—C1—C6	−0.5 (8)
O1—Ag1—N2—N3	69.7 (5)	Ag2^iii—N1—C1—C6	176.8 (5)
N1—N2—N3—C6	−0.8 (8)	N1—C1—C2—C3	−178.3 (7)
Ag1—N2—N3—C6	176.7 (5)	C6—C1—C2—C3	1.3 (10)
O2—N4—O1—Ag1	5.1 (9)	C1—C2—C3—C4	−0.9 (11)
O3—N4—O1—Ag1	−175.0 (6)	C2—C3—C4—C5	0.6 (11)
N2—Ag1—O1—N4	−29.8 (6)	C3—C4—C5—C6	−0.8 (10)
O4—Ag1—O1—N4	159.9 (5)	N2—N3—C6—C5	−177.4 (8)
O3—N4—O2—Ag2^iv	27.0 (9)	N2—N3—C6—C1	0.5 (7)
O1—N4—O2—Ag2^iv	−153.1 (5)	C4—C5—C6—N3	178.8 (7)
O5—N5—O4—Ag1	2.8 (8)	C4—C5—C6—C1	1.2 (10)
O6—N5—O4—Ag1	−178.5 (5)	N1—C1—C6—N3	0.0 (7)
N2—Ag1—O4—N5	−11.5 (6)	C2—C1—C6—N3	−179.7 (7)
O1—Ag1—O4—N5	157.3 (4)	N1—C1—C6—C5	178.2 (7)
O5—N5—O6—Ag2	−178.7 (5)	C2—C1—C6—C5	−1.5 (10)

Symmetry codes: (i) x+1/2, −y+3/2, z; (ii) −x+3/2, y+1/2, z+1/2; (iii) x−1/2, −y+3/2, z; (iv) −x+3/2, y−1/2, z−1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N3—H3···O7^iv	0.86	1.94	2.795 (8)	170

Symmetry code: (iv) −x+3/2, y−1/2, z−1/2.