Bis[μ-3-(1H-pyrazol-1-yl)benzonitrile-κN:N']bis-[perchloratosilver(I)].

In the title centrosymmetric complex, [Ag(2)(ClO(4))(2)(C(10)H(7)N(3))(2)], the unique Ag(I) ion is coordinated by an N atom from a carbonitrile group, an N atom from a symmetry-related pyrazole group and an O atom of a perchlorate ligand to form a distorted T-shaped environment. Two 3-(1H-pyrazol-1-yl)benzonitrile ligands each bridge two Ag(I) ions to form a dinuclear complex. In the crystal structure, there are weak Ag⋯O inter-actions within the range 2.70-3.01 Å linking dimeric units into layers approximately parallel to (100). The O atoms of the perchlorate ligand are disordered over two sites with occupancies of 0.570 (11) and 0.430 (11), respectively.

Related literature

For background information, see: Antonioli et al. (2006 ▶); Bourlier et al. (2007 ▶); Niu et al. (2007 ▶); Sumby & Hardie (2005 ▶).

Experimental

Crystal data

[Ag2(ClO4)2(C10H7N3)2]

M = 753.02

Monoclinic,

a = 7.8522 (13) Å

b = 10.6086 (17) Å

c = 15.322 (2) Å

β = 101.100 (2)°

V = 1252.5 (3) Å3

Z = 2

Mo Kα radiation

μ = 1.83 mm−1

T = 173 (2) K

0.51 × 0.47 × 0.36 mm

Data collection

Siemens SMART CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.455, T max = 0.558 (expected range = 0.421–0.517)

7721 measured reflections

2833 independent reflections

2180 reflections with I > 2σ(I)

R int = 0.021

Refinement

R[F 2 > 2σ(F 2)] = 0.042

wR(F 2) = 0.114

S = 0.96

2833 reflections

209 parameters

74 restraints

H-atom parameters constrained

Δρmax = 0.75 e Å−3

Δρmin = −0.59 e Å−3

Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1994 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶) and PLATON (Spek, 2003 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808030602/lh2676sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808030602/lh2676Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Ag2(ClO4)2(C10H7N3)2]	F(000) = 736
Mr = 753.02	Dx = 1.997 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 3269 reflections
a = 7.8522 (13) Å	θ = 2.7–27.5°
b = 10.6086 (17) Å	µ = 1.84 mm−1
c = 15.322 (2) Å	T = 173 K
β = 101.100 (2)°	Prism, colourless
V = 1252.5 (3) Å3	0.51 × 0.47 × 0.36 mm
Z = 2

Siemens SMART CCD diffractometer	2833 independent reflections
Radiation source: fine-focus sealed tube	2180 reflections with I > 2σ(I)
graphite	Rint = 0.021
φ and ω scans	θmax = 27.5°, θmin = 2.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→10
Tmin = 0.455, Tmax = 0.558	k = −13→9
7721 measured reflections	l = −17→19

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)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.114	H-atom parameters constrained
S = 0.96	w = 1/[σ2(Fo2) + (0.0532P)2 + 1.7339P] where P = (Fo2 + 2Fc2)/3
2833 reflections	(Δ/σ)max < 0.001
209 parameters	Δρmax = 0.75 e Å−3
74 restraints	Δρmin = −0.59 e Å−3

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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ag1	0.76740 (6)	0.39146 (4)	0.86430 (3)	0.07794 (19)
N1	1.0182 (5)	0.3203 (4)	0.9364 (2)	0.0701 (10)
N2	1.0408 (5)	0.2463 (4)	1.0104 (2)	0.0651 (9)
N3	0.4622 (7)	0.5000 (5)	1.1304 (3)	0.0911 (14)
Cl1	0.84901 (17)	0.60883 (10)	0.70970 (7)	0.0661 (3)
O1	0.7551 (17)	0.6867 (11)	0.7615 (9)	0.135 (6)	0.570 (11)
O2	0.7442 (18)	0.5787 (12)	0.6285 (7)	0.202 (8)	0.570 (11)
O3	0.9945 (14)	0.6862 (10)	0.6941 (9)	0.176 (6)	0.570 (11)
O4	0.9186 (10)	0.5048 (6)	0.7585 (5)	0.086 (3)	0.570 (11)
O1'	0.720 (2)	0.5094 (13)	0.7054 (9)	0.183 (8)	0.430 (11)
O2'	0.8668 (17)	0.6337 (11)	0.6228 (5)	0.107 (5)	0.430 (11)
O3'	1.0098 (17)	0.5589 (15)	0.7614 (8)	0.179 (9)	0.430 (11)
O4'	0.7999 (18)	0.7139 (10)	0.7552 (7)	0.085 (4)	0.430 (11)
C1	1.1968 (7)	0.1905 (5)	1.0250 (3)	0.0783 (13)
H1	1.2412	0.1350	1.0726	0.094*
C2	1.2802 (7)	0.2279 (6)	0.9589 (4)	0.0815 (14)
H2	1.3928	0.2041	0.9510	0.098*
C3	1.1662 (7)	0.3073 (5)	0.9066 (3)	0.0782 (14)
H3	1.1897	0.3484	0.8551	0.094*
C4	0.9047 (6)	0.2323 (4)	1.0594 (3)	0.0628 (11)
C5	0.8791 (8)	0.1159 (5)	1.0957 (3)	0.0760 (13)
H5	0.9520	0.0468	1.0885	0.091*
C6	0.7462 (8)	0.1014 (5)	1.1426 (4)	0.0865 (17)
H6	0.7288	0.0219	1.1681	0.104*
C7	0.6402 (8)	0.2000 (6)	1.1527 (3)	0.0802 (15)
H7	0.5488	0.1893	1.1846	0.096*
C8	0.6672 (7)	0.3159 (5)	1.1158 (3)	0.0674 (11)
C9	0.8030 (6)	0.3330 (4)	1.0700 (3)	0.0626 (10)
H9	0.8240	0.4133	1.0468	0.075*
C10	0.5544 (8)	0.4191 (6)	1.1244 (3)	0.0762 (14)

	U11	U22	U33	U12	U13	U23
Ag1	0.0955 (3)	0.0756 (3)	0.0665 (3)	−0.0075 (2)	0.0251 (2)	0.00463 (17)
N1	0.086 (3)	0.074 (2)	0.0521 (19)	−0.016 (2)	0.0166 (18)	0.0037 (17)
N2	0.083 (3)	0.063 (2)	0.0512 (19)	−0.0112 (19)	0.0176 (18)	−0.0030 (16)
N3	0.103 (4)	0.095 (3)	0.084 (3)	−0.004 (3)	0.039 (3)	0.000 (3)
Cl1	0.0891 (8)	0.0551 (6)	0.0545 (6)	−0.0027 (5)	0.0151 (5)	0.0009 (4)
O1	0.158 (10)	0.110 (9)	0.157 (10)	0.023 (7)	0.079 (8)	0.002 (7)
O2	0.254 (15)	0.164 (11)	0.138 (11)	0.034 (10)	−0.087 (11)	−0.050 (9)
O3	0.217 (12)	0.148 (9)	0.187 (12)	−0.070 (8)	0.100 (10)	0.013 (8)
O4	0.096 (4)	0.076 (4)	0.096 (4)	0.022 (3)	0.042 (3)	0.038 (3)
O1'	0.246 (15)	0.191 (13)	0.128 (11)	−0.158 (12)	0.079 (10)	−0.058 (9)
O2'	0.145 (10)	0.127 (9)	0.063 (6)	0.017 (7)	0.052 (7)	0.033 (6)
O3'	0.164 (13)	0.198 (15)	0.135 (11)	0.075 (11)	−0.069 (10)	−0.072 (10)
O4'	0.125 (9)	0.069 (6)	0.058 (5)	0.016 (6)	0.007 (5)	−0.009 (4)
C1	0.091 (4)	0.077 (3)	0.067 (3)	0.000 (3)	0.016 (3)	0.002 (2)
C2	0.082 (3)	0.092 (4)	0.075 (3)	−0.010 (3)	0.026 (3)	−0.016 (3)
C3	0.094 (4)	0.087 (3)	0.059 (3)	−0.025 (3)	0.028 (3)	−0.008 (2)
C4	0.080 (3)	0.063 (3)	0.045 (2)	−0.016 (2)	0.0128 (19)	−0.0027 (18)
C5	0.101 (4)	0.066 (3)	0.061 (3)	−0.011 (3)	0.016 (3)	0.005 (2)
C6	0.115 (5)	0.075 (4)	0.071 (3)	−0.025 (3)	0.021 (3)	0.019 (3)
C7	0.093 (4)	0.091 (4)	0.058 (3)	−0.024 (3)	0.021 (2)	0.011 (2)
C8	0.078 (3)	0.076 (3)	0.048 (2)	−0.014 (2)	0.014 (2)	0.000 (2)
C9	0.084 (3)	0.058 (2)	0.047 (2)	−0.015 (2)	0.016 (2)	0.0004 (18)
C10	0.087 (3)	0.088 (4)	0.058 (3)	−0.016 (3)	0.025 (2)	0.001 (2)

Ag1—N3i	2.154 (6)	Cl1—O3	1.463 (7)
Ag1—N1	2.198 (4)	C1—C2	1.367 (7)
Ag1—O4	2.495 (6)	C1—H1	0.9500
Ag1—O4'ii	2.609 (6)	C2—C3	1.370 (8)
N1—C3	1.335 (7)	C2—H2	0.9500
N1—N2	1.362 (5)	C3—H3	0.9500
N2—C1	1.340 (7)	C4—C9	1.362 (7)
N2—C4	1.428 (6)	C4—C5	1.384 (6)
N3—C10	1.137 (7)	C5—C6	1.385 (8)
N3—Ag1i	2.154 (6)	C5—H5	0.9500
Cl1—O4	1.385 (5)	C6—C7	1.364 (8)
Cl1—O2	1.390 (6)	C6—H6	0.9500
Cl1—O2'	1.391 (6)	C7—C8	1.387 (7)
Cl1—O4'	1.407 (7)	C7—H7	0.9500
Cl1—O1	1.442 (7)	C8—C9	1.396 (6)
Cl1—O1'	1.453 (7)	C8—C10	1.430 (8)
Cl1—O3'	1.455 (7)	C9—H9	0.9500
N3i—Ag1—N1	147.16 (17)	O4'—Cl1—O3	86.2 (8)
N3i—Ag1—O4	105.89 (19)	O1—Cl1—O3	105.4 (6)
N1—Ag1—O4	89.96 (19)	O1'—Cl1—O3	163.3 (7)
N1—Ag1—O4'ii	98.4 (19)	O3'—Cl1—O3	70.7 (9)
N3i—Ag1—O4'ii	110.8 (19)	Cl1—O4—Ag1	123.1 (4)
C3—N1—N2	104.1 (4)	N2—C1—C2	107.5 (5)
C3—N1—Ag1	128.2 (3)	N2—C1—H1	126.2
N2—N1—Ag1	125.2 (3)	C2—C1—H1	126.2
C1—N2—N1	111.2 (4)	C1—C2—C3	105.1 (5)
C1—N2—C4	128.2 (4)	C1—C2—H2	127.5
N1—N2—C4	120.5 (4)	C3—C2—H2	127.5
C10—N3—Ag1i	163.0 (5)	N1—C3—C2	112.1 (5)
O4—Cl1—O2	113.8 (6)	N1—C3—H3	123.9
O4—Cl1—O2'	124.4 (6)	C2—C3—H3	123.9
O2—Cl1—O2'	48.6 (6)	C9—C4—C5	121.2 (4)
O4—Cl1—O4'	118.8 (6)	C9—C4—N2	119.8 (4)
O2—Cl1—O4'	117.0 (8)	C5—C4—N2	119.0 (5)
O2'—Cl1—O4'	114.3 (6)	C4—C5—C6	119.3 (5)
O4—Cl1—O1	110.5 (6)	C4—C5—H5	120.3
O2—Cl1—O1	110.3 (7)	C6—C5—H5	120.3
O2'—Cl1—O1	125.1 (8)	C7—C6—C5	120.7 (5)
O4—Cl1—O1'	69.2 (7)	C7—C6—H6	119.6
O2—Cl1—O1'	60.4 (7)	C5—C6—H6	119.6
O2'—Cl1—O1'	106.9 (6)	C6—C7—C8	119.3 (5)
O4'—Cl1—O1'	110.1 (7)	C6—C7—H7	120.4
O1—Cl1—O1'	90.9 (9)	C8—C7—H7	120.4
O2—Cl1—O3'	134.9 (8)	C7—C8—C9	120.8 (5)
O2'—Cl1—O3'	110.7 (7)	C7—C8—C10	119.7 (5)
O4'—Cl1—O3'	108.1 (6)	C9—C8—C10	119.5 (4)
O1—Cl1—O3'	113.0 (8)	C4—C9—C8	118.7 (4)
O1'—Cl1—O3'	106.5 (7)	C4—C9—H9	120.7
O4—Cl1—O3	107.2 (6)	C8—C9—H9	120.7
O2—Cl1—O3	109.2 (7)	N3—C10—C8	178.7 (6)
O2'—Cl1—O3	60.8 (6)
N3i—Ag1—N1—C3	−142.6 (4)	N2—C1—C2—C3	0.2 (6)
O4—Ag1—N1—C3	−22.4 (5)	N2—N1—C3—C2	0.2 (6)
N3i—Ag1—N1—N2	58.4 (5)	Ag1—N1—C3—C2	−162.3 (4)
O4—Ag1—N1—N2	178.6 (4)	C1—C2—C3—N1	−0.2 (6)
C3—N1—N2—C1	0.0 (5)	C1—N2—C4—C9	144.8 (5)
Ag1—N1—N2—C1	163.1 (3)	N1—N2—C4—C9	−38.0 (6)
C3—N1—N2—C4	−177.7 (4)	C1—N2—C4—C5	−34.9 (7)
Ag1—N1—N2—C4	−14.5 (5)	N1—N2—C4—C5	142.3 (4)
O2—Cl1—O4—Ag1	−88.2 (10)	C9—C4—C5—C6	0.9 (7)
O2'—Cl1—O4—Ag1	−143.1 (8)	N2—C4—C5—C6	−179.4 (5)
O4'—Cl1—O4—Ag1	55.7 (10)	C4—C5—C6—C7	0.5 (8)
O1—Cl1—O4—Ag1	36.5 (9)	C5—C6—C7—C8	−0.4 (8)
O1'—Cl1—O4—Ag1	−46.4 (7)	C6—C7—C8—C9	−1.1 (8)
O3'—Cl1—O4—Ag1	138.0 (15)	C6—C7—C8—C10	178.7 (5)
O3—Cl1—O4—Ag1	150.9 (7)	C5—C4—C9—C8	−2.3 (7)
N3i—Ag1—O4—Cl1	−5.6 (7)	N2—C4—C9—C8	177.9 (4)
N1—Ag1—O4—Cl1	−156.5 (6)	C7—C8—C9—C4	2.4 (7)
N1—N2—C1—C2	−0.2 (6)	C10—C8—C9—C4	−177.4 (4)
C4—N2—C1—C2	177.3 (4)

Ag1—N3i	2.154 (6)
Ag1—N1	2.198 (4)
Ag1—O4	2.495 (6)
Ag1—O4′ii	2.609 (6)

N3i—Ag1—N1	147.16 (17)
N3i—Ag1—O4	105.89 (19)
N1—Ag1—O4	89.96 (19)
N1—Ag1—O4′ii	98.4 (19)
N3i—Ag1—O4′ii	110.8 (19)

Symmetry codes: (i) ; (ii) .