Literature DB >> 21201859

catena-Poly[[silver(I)-μ-[N-(4-pyridyl-meth-yl)pyridine-4-carboxamide-κN:N']] nitrate monohydrate].

Abstract

The title coordination polymer, {[Ag(C(12)H(11)N(3)O)]NO(3)·H(2)O}(n), has a polycationic chain motif in which the Ag atom is bridged by the heterocyclic ligand; the Ag atom shows linear coordination. If the two long Ag⋯O(nitrate) inter-actions [2.794 (6) and 2.867 (5) Å] are regarded as bonds, the compound adopts a three-dimensional network structure. The water mol-ecule consolidates the network structure by forming hydrogen bonds, one to the polycationic chain and one to the nitrate anion.

Entities: CellLine Chemical Disease Species

Year: 2008 PMID： 21201859 PMCID： PMC2960773 DOI： 10.1107/S1600536807049082

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For the structure of the hydrated disilver oxalate adduct of the heterocyclic ligand, see Tong et al. (2002 ▶).

Experimental

Crystal data

[Ag(C12H11N3O)]NO3·H2O M = 401.13 Orthorhombic, a = 12.912 (7) Å b = 9.021 (5) Å c = 24.52 (1) Å V = 2856 (3) Å3 Z = 8 Mo Kα radiation μ = 1.45 mm−1 T = 295 (2) K 0.6 × 0.4 × 0.2 mm

Data collection

Rigaku Mercury diffractometer Absorption correction: multi-scan (Jacobson, 1998 ▶) T min = 0.50, T max = 0.75 25888 measured reflections 3249 independent reflections 2433 reflections with I > 2σ(I) R int = 0.047

Refinement

R[F 2 > 2σ(F 2)] = 0.053 wR(F 2) = 0.141 S = 1.06 3249 reflections 211 parameters 3 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.91 e Å−3 Δρmin = −0.75 e Å−3 Data collection: CrystalClear (Rigaku/MSC, 2005 ▶); cell refinement: CrystalClear ; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2008 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807049082/bg2109sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807049082/bg2109Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Ag(C₁₂H₁₁N₃O)]NO₃·H₂O	F₀₀₀ = 1600
M_r = 401.13	D_x = 1.879 Mg m⁻³
Orthorhombic, Pbca	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 5655 reflections
a = 12.912 (7) Å	θ = 3.2–27.5º
b = 9.021 (5) Å	µ = 1.45 mm⁻¹
c = 24.52 (1) Å	T = 295 (2) K
V = 2856 (3) Å³	Column, colourless
Z = 8	0.6 × 0.4 × 0.2 mm

Rigaku Mercury diffractometer	3249 independent reflections
Radiation source: medium-focus sealed tube	2433 reflections with I > 2σ(I)
Monochromator: graphite	R_int = 0.047
T = 295(2) K	θ_max = 27.5º
ω scans	θ_min = 3.2º
Absorption correction: multi-scan(Jacobson, 1998)	h = −16→16
T_min = 0.50, T_max = 0.75	k = −11→11
25888 measured reflections	l = −30→31

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.053	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.141	w = 1/[σ²(F_o²) + (0.0589P)² + 5.5451P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max = 0.001
3249 reflections	Δρ_max = 0.91 e Å⁻³
211 parameters	Δρ_min = −0.75 e Å⁻³
3 restraints	Extinction correction: none
Primary atom site location: structure-invariant direct methods

	x	y	z	U_iso*/U_eq
Ag1	0.16581 (3)	0.61149 (5)	0.002207 (15)	0.05996 (18)
O1	0.1859 (3)	0.1438 (4)	0.23653 (13)	0.0598 (9)
O2	0.3756 (4)	0.6914 (6)	0.00374 (16)	0.0905 (14)
O3	0.5035 (4)	0.7095 (7)	−0.0481 (2)	0.1077 (17)
O4	0.3682 (5)	0.8329 (7)	−0.0644 (2)	0.118 (2)
O1W	0.5539 (3)	0.2042 (5)	0.17401 (17)	0.0660 (10)
H1W1	0.608 (3)	0.189 (8)	0.193 (2)	0.10 (2)*
H1W2	0.562 (8)	0.176 (10)	0.1412 (13)	0.15 (4)*
N1	0.1990 (3)	0.4795 (4)	0.07408 (14)	0.0448 (8)
N2	0.3572 (3)	0.1578 (4)	0.22161 (14)	0.0458 (9)
H2N	0.408 (3)	0.198 (5)	0.2048 (19)	0.061 (16)*
N3	0.3656 (3)	0.2837 (4)	0.42466 (15)	0.0470 (9)
N4	0.4163 (3)	0.7500 (4)	−0.03557 (16)	0.0469 (9)
C1	0.1231 (4)	0.4240 (6)	0.1046 (2)	0.0567 (12)
H1	0.0551	0.4506	0.0967	0.068*
C2	0.1412 (4)	0.3281 (6)	0.14763 (19)	0.0528 (12)
H2	0.0859	0.2895	0.1674	0.063*
C3	0.2413 (3)	0.2900 (4)	0.16112 (14)	0.0377 (9)
C4	0.3201 (4)	0.3498 (6)	0.1298 (2)	0.0524 (12)
H4	0.3890	0.3279	0.1376	0.063*
C5	0.2952 (4)	0.4425 (6)	0.08692 (19)	0.0513 (11)
H5	0.3489	0.4809	0.0659	0.062*
C6	0.2592 (4)	0.1894 (5)	0.20953 (15)	0.0417 (9)
C7	0.3844 (4)	0.0665 (5)	0.26853 (17)	0.0487 (11)
H7A	0.4547	0.0307	0.2639	0.058*
H7B	0.3390	−0.0191	0.2694	0.058*
C8	0.3770 (3)	0.1465 (4)	0.32274 (16)	0.0379 (9)
C9	0.3479 (4)	0.2929 (5)	0.32757 (19)	0.0474 (11)
H9A	0.3325	0.3486	0.2967	0.057*
C10	0.3418 (4)	0.3559 (5)	0.3786 (2)	0.0515 (12)
H10	0.3201	0.4540	0.3812	0.062*
C11	0.3960 (4)	0.1419 (5)	0.41994 (18)	0.0514 (11)
H11	0.4134	0.0895	0.4513	0.062*
C12	0.4021 (4)	0.0715 (5)	0.37027 (17)	0.0482 (11)
H12	0.4233	−0.0270	0.3686	0.058*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ag1	0.0659 (3)	0.0671 (3)	0.0469 (3)	0.00106 (19)	−0.01097 (16)	0.01944 (19)
O1	0.065 (2)	0.074 (2)	0.0410 (18)	−0.0126 (18)	0.0093 (16)	0.0097 (17)
O2	0.111 (4)	0.103 (4)	0.058 (3)	−0.013 (3)	0.013 (2)	0.026 (2)
O3	0.076 (3)	0.171 (5)	0.076 (3)	0.009 (3)	0.003 (2)	−0.016 (3)
O4	0.130 (4)	0.135 (5)	0.089 (4)	0.049 (4)	0.001 (3)	0.050 (3)
O1W	0.056 (2)	0.087 (3)	0.055 (2)	0.005 (2)	−0.0059 (19)	0.011 (2)
N1	0.052 (2)	0.048 (2)	0.0343 (18)	0.0005 (18)	−0.0060 (16)	0.0031 (16)
N2	0.058 (2)	0.047 (2)	0.0318 (18)	0.0024 (19)	0.0050 (17)	0.0092 (16)
N3	0.053 (2)	0.049 (2)	0.0394 (19)	−0.0026 (18)	−0.0003 (17)	−0.0094 (17)
N4	0.053 (2)	0.048 (2)	0.041 (2)	−0.0017 (19)	0.0040 (18)	0.0014 (17)
C1	0.047 (3)	0.071 (3)	0.052 (3)	0.001 (2)	−0.008 (2)	0.014 (2)
C2	0.046 (2)	0.071 (3)	0.041 (2)	−0.011 (2)	−0.0001 (19)	0.006 (2)
C3	0.049 (2)	0.037 (2)	0.0265 (17)	−0.0034 (19)	0.0008 (17)	−0.0015 (15)
C4	0.043 (2)	0.063 (3)	0.051 (3)	0.007 (2)	0.005 (2)	0.018 (2)
C5	0.045 (2)	0.059 (3)	0.049 (3)	0.005 (2)	0.007 (2)	0.022 (2)
C6	0.056 (3)	0.043 (2)	0.0255 (18)	−0.004 (2)	0.0057 (18)	−0.0009 (16)
C7	0.071 (3)	0.043 (2)	0.032 (2)	0.008 (2)	−0.001 (2)	0.0033 (18)
C8	0.043 (2)	0.037 (2)	0.0333 (19)	−0.0026 (18)	−0.0003 (17)	−0.0010 (16)
C9	0.057 (3)	0.041 (2)	0.044 (2)	0.005 (2)	−0.009 (2)	−0.0001 (19)
C10	0.057 (3)	0.043 (2)	0.054 (3)	0.006 (2)	−0.006 (2)	−0.009 (2)
C11	0.073 (3)	0.046 (3)	0.035 (2)	0.001 (2)	−0.005 (2)	−0.0004 (19)
C12	0.069 (3)	0.037 (2)	0.039 (2)	0.004 (2)	0.002 (2)	0.0023 (18)

Ag1—N3ⁱ	2.162 (4)	C2—C3	1.377 (6)
Ag1—N1	2.170 (4)	C2—H2	0.9300
Ag1—O2	2.803 (6)	C3—C4	1.385 (6)
Ag1—O3ⁱⁱ	2.874 (6)	C3—C6	1.512 (5)
O1—C6	1.226 (5)	C4—C5	1.381 (6)
O2—N4	1.219 (5)	C4—H4	0.9300
O3—N4	1.223 (6)	C5—H5	0.9300
O4—N4	1.202 (6)	C7—C8	1.516 (6)
O1W—H1W1	0.85 (4)	C7—H7A	0.9700
O1W—H1W2	0.85 (4)	C7—H7B	0.9700
N1—C5	1.325 (6)	C8—C9	1.378 (6)
N1—C1	1.331 (6)	C8—C12	1.386 (6)
N2—C6	1.330 (6)	C9—C10	1.377 (6)
N2—C7	1.458 (5)	C9—H9A	0.9300
N2—H2N	0.86 (4)	C10—H10	0.9300
N3—C10	1.340 (6)	C11—C12	1.376 (6)
N3—C11	1.343 (6)	C11—H11	0.9300
C1—C2	1.385 (7)	C12—H12	0.9300
C1—H1	0.9300

N3ⁱ—Ag1—N1	172.52 (14)	C5—C4—H4	120.4
N3ⁱ—Ag1—O2	94.61 (13)	C3—C4—H4	120.4
N1—Ag1—O2	86.53 (14)	N1—C5—C4	123.5 (4)
N3ⁱ—Ag1—O3ⁱⁱ	87.80 (15)	N1—C5—H5	118.3
N1—Ag1—O3ⁱⁱ	97.73 (15)	C4—C5—H5	118.3
O2—Ag1—O3ⁱⁱ	123.69 (16)	O1—C6—N2	122.8 (4)
N4—O2—Ag1	121.2 (4)	O1—C6—C3	120.5 (4)
H1W1—O1W—H1W2	111 (8)	N2—C6—C3	116.7 (4)
C5—N1—C1	117.5 (4)	N2—C7—C8	114.0 (4)
C5—N1—Ag1	121.1 (3)	N2—C7—H7A	108.7
C1—N1—Ag1	121.2 (3)	C8—C7—H7A	108.7
C6—N2—C7	121.8 (4)	N2—C7—H7B	108.7
C6—N2—H2N	122 (4)	C8—C7—H7B	108.7
C7—N2—H2N	116 (4)	H7A—C7—H7B	107.6
C10—N3—C11	117.2 (4)	C9—C8—C12	117.4 (4)
C10—N3—Ag1ⁱⁱⁱ	119.1 (3)	C9—C8—C7	123.3 (4)
C11—N3—Ag1ⁱⁱⁱ	123.2 (3)	C12—C8—C7	119.3 (4)
O4—N4—O2	120.8 (5)	C10—C9—C8	119.3 (4)
O4—N4—O3	120.9 (5)	C10—C9—H9A	120.4
O2—N4—O3	117.8 (5)	C8—C9—H9A	120.4
N1—C1—C2	122.6 (5)	N3—C10—C9	123.5 (4)
N1—C1—H1	118.7	N3—C10—H10	118.2
C2—C1—H1	118.7	C9—C10—H10	118.2
C3—C2—C1	119.8 (4)	N3—C11—C12	122.2 (4)
C3—C2—H2	120.1	N3—C11—H11	118.9
C1—C2—H2	120.1	C12—C11—H11	118.9
C2—C3—C4	117.4 (4)	C11—C12—C8	120.3 (4)
C2—C3—C6	118.8 (4)	C11—C12—H12	119.8
C4—C3—C6	123.8 (4)	C8—C12—H12	119.8
C5—C4—C3	119.1 (4)

N3ⁱ—Ag1—O2—N4	−7.1 (5)	C7—N2—C6—O1	−0.4 (7)
N1—Ag1—O2—N4	165.5 (5)	C7—N2—C6—C3	177.7 (4)
O3ⁱⁱ—Ag1—O2—N4	−97.5 (4)	C2—C3—C6—O1	−0.7 (6)
O2—Ag1—N1—C5	−17.8 (4)	C4—C3—C6—O1	177.8 (4)
O3ⁱⁱ—Ag1—N1—C5	−141.4 (4)	C2—C3—C6—N2	−178.8 (4)
O2—Ag1—N1—C1	167.1 (4)	C4—C3—C6—N2	−0.3 (6)
O3ⁱⁱ—Ag1—N1—C1	43.5 (4)	C6—N2—C7—C8	−76.5 (6)
Ag1—O2—N4—O4	33.5 (7)	N2—C7—C8—C9	−0.5 (7)
Ag1—O2—N4—O3	−138.7 (4)	N2—C7—C8—C12	−179.3 (4)
C5—N1—C1—C2	−1.5 (8)	C12—C8—C9—C10	−2.1 (7)
Ag1—N1—C1—C2	173.8 (4)	C7—C8—C9—C10	179.1 (4)
N1—C1—C2—C3	1.7 (8)	C11—N3—C10—C9	−0.6 (7)
C1—C2—C3—C4	−0.7 (7)	Ag1ⁱⁱⁱ—N3—C10—C9	−172.5 (4)
C1—C2—C3—C6	177.9 (4)	C8—C9—C10—N3	1.9 (7)
C2—C3—C4—C5	−0.5 (7)	C10—N3—C11—C12	−0.5 (7)
C6—C3—C4—C5	−179.0 (4)	Ag1ⁱⁱⁱ—N3—C11—C12	171.1 (4)
C1—N1—C5—C4	0.2 (8)	N3—C11—C12—C8	0.2 (8)
Ag1—N1—C5—C4	−175.1 (4)	C9—C8—C12—C11	1.1 (7)
C3—C4—C5—N1	0.8 (8)	C7—C8—C12—C11	180.0 (5)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···O1W	0.86 (4)	2.04 (2)	2.827 (6)	154 (5)
O1W—H1W1···O1^iv	0.85 (4)	2.05 (3)	2.831 (5)	154 (7)
O1W—H1W2···O4^v	0.85 (4)	2.09 (4)	2.888 (7)	157 (9)

Table 1

Selected bond lengths (Å)

Ag1—N3ⁱ	2.162 (4)
Ag1—N1	2.170 (4)
Ag1—O2	2.803 (6)
Ag1—O3ⁱⁱ	2.874 (6)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2N⋯O1W	0.86 (4)	2.04 (2)	2.827 (6)	154 (5)
O1W—H1W1⋯O1ⁱⁱⁱ	0.85 (4)	2.05 (3)	2.831 (5)	154 (7)
O1W—H1W2⋯O4^iv	0.85 (4)	2.09 (4)	2.888 (7)	157 (9)

Symmetry codes: (iii) ; (iv) .

1 in total

1. Pseudo-polyrotaxane and beta-sheet layer-based three-dimensional coordination polymers constructed with silver salts and flexible pyridyl-type ligands.

Authors: Ming-Liang Tong; Yin-Miao Wu; Jie Ru; Xiao-Ming Chen; Ho-Chol Chang; Susumu Kitagawa
Journal: Inorg Chem Date: 2002-09-23 Impact factor: 5.165

1 in total