Literature DB >> 21201049

A novel double-chain silver(I) coordination polymer: catena-poly[[[μ-aqua-aqua-disilver(I)]-bis-(μ(3)-5-methyl-pyrazine-2-carboxyl-ato)] dihydrate].

Bin Zhai1, Xiangfei Zhang, Maotian Xu.   

Abstract

In the title silver(I) coordination polymer, {[Ag(2)(C(6)H(5)N(2)O(2))(2)(H(2)O)(2)]·2H(2)O}(n), the [Ag(2)(μ(2)-H(2)O)(H(2)O)] cores are extended by anti-parallel 5-methyl-pyrazine-2-carboxyl-ate (L) ligands, forming a novel double-chain structure. Both Ag(+) cations show a distorted square-pyramidal coordination. Ag1 is bonded to two water molecules, one L N atom, one N atom and one carboxylate O atom from a neighbouring L, whereas Ag2 is surrounded by two L N atoms, two L carboxylate O atoms and one bridging water molecule. O-H⋯O hydrogen-bonding inter-actions involving water clusters and carboxyl-ate O atoms link the mol-ecules into a three-dimensional supra-molecular architecture, which is further consolidated by weak C-H⋯O inter-actions and π-π stacking inter-actions [centroid-centroid distance 3.643 (5) Å].

Entities:  

Year:  2008        PMID： 21201049      PMCID： PMC2959376          DOI： 10.1107/S160053680802984X

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


Related literature

For related literature, see: Ciurtin et al. (2001 ▶, 2003 ▶); Dong et al. (2000 ▶); Garribba et al. (2006 ▶); Liu et al. (2007 ▶); Ptasiewicz-Bak & Leciejewicz (2000 ▶); Shang et al. (2007 ▶); Tanase et al. (2006 ▶); Etter (1990 ▶).

Experimental

Crystal data

[Ag2(C6H5N2O2)2(H2O)2]·2H2O M = 562.04 Triclinic, a = 6.9481 (5) Å b = 10.1827 (8) Å c = 13.483 (1) Å α = 107.503 (1)° β = 100.185 (1)° γ = 103.164 (1)° V = 854.4 (1) Å3 Z = 2 Mo Kα radiation μ = 2.34 mm−1 T = 293 (2) K 0.24 × 0.20 × 0.16 mm

Data collection

Bruker APEX CCD area-detector diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.581, T max = 0.698 4422 measured reflections 2982 independent reflections 2518 reflections with I > 2σ(I) R int = 0.014

Refinement

R[F 2 > 2σ(F 2)] = 0.027 wR(F 2) = 0.071 S = 1.07 2982 reflections 236 parameters H-atom parameters constrained Δρmax = 0.39 e Å−3 Δρmin = −0.51 e Å−3 Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT (Bruker, 2003 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg & Putz, 2005 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053680802984X/kj2095sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S160053680802984X/kj2095Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ag2(C6H5N2O2)2(H2O)2]·2H2OZ = 2
Mr = 562.04F(000) = 552
Triclinic, P1Dx = 2.185 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.9481 (5) ÅCell parameters from 2098 reflections
b = 10.1827 (8) Åθ = 3.1–27.8°
c = 13.483 (1) ŵ = 2.34 mm−1
α = 107.503 (1)°T = 293 K
β = 100.185 (1)°Block, colourless
γ = 103.164 (1)°0.24 × 0.20 × 0.16 mm
V = 854.4 (1) Å3
Bruker APEX CCD area-detector diffractometer2982 independent reflections
Radiation source: fine-focus sealed tube2518 reflections with I > 2σ(I)
graphiteRint = 0.014
φ and ω scansθmax = 25.0°, θmin = 1.6°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)h = −8→7
Tmin = 0.581, Tmax = 0.698k = −12→12
4422 measured reflectionsl = −7→16
Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.027w = 1/[σ2(Fo2) + (0.0298P)2 + 0.2298P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.071(Δ/σ)max = 0.001
S = 1.07Δρmax = 0.39 e Å−3
2982 reflectionsΔρmin = −0.51 e Å−3
236 parameters
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.
xyzUiso*/Ueq
Ag10.51241 (5)0.71236 (3)0.76748 (2)0.04603 (12)
Ag20.92839 (4)0.50359 (3)1.21079 (2)0.04547 (11)
O10.6620 (4)0.2358 (3)0.8569 (2)0.0435 (6)
O20.8186 (4)0.2942 (3)1.0300 (2)0.0440 (6)
O30.2277 (4)0.2659 (3)0.5098 (2)0.0475 (7)
O40.3568 (4)0.4346 (3)0.6721 (2)0.0508 (7)
O50.1848 (4)0.7679 (3)0.7910 (2)0.0525 (7)
H5A0.14040.82060.76000.079*
H5B0.18490.78660.85680.079*
O60.7016 (5)0.9584 (3)0.7828 (3)0.0646 (9)
H6A0.80650.96400.75820.097*
H6B0.67531.03730.80910.097*
O70.9786 (4)0.0754 (3)0.3171 (2)0.0489 (7)
H7A0.87160.01250.31420.073*
H7B1.04550.13520.37980.073*
O80.3319 (4)0.1221 (3)0.6643 (3)0.0627 (8)
H8A0.43390.15760.71960.094*
H8B0.30650.17660.63010.094*
N10.6624 (4)0.6564 (3)0.9057 (2)0.0309 (6)
N20.8050 (4)0.5719 (3)1.0748 (2)0.0282 (6)
N30.3601 (4)0.6478 (3)0.5860 (2)0.0315 (6)
N40.1450 (4)0.5712 (3)0.3731 (2)0.0325 (6)
C10.6657 (5)0.5205 (3)0.8899 (3)0.0283 (7)
H10.61780.45310.82010.034*
C20.7365 (4)0.4767 (3)0.9722 (3)0.0268 (7)
C30.8019 (5)0.7062 (4)1.0902 (3)0.0327 (8)
H30.84840.77341.16010.039*
C40.7324 (5)0.7511 (4)1.0068 (3)0.0308 (7)
C50.7297 (6)0.9034 (4)1.0286 (3)0.0481 (10)
H5A'0.64570.90940.96630.072*
H5B'0.67480.93391.08920.072*
H5C'0.86680.96491.04420.072*
C60.7382 (5)0.3213 (4)0.9515 (3)0.0301 (7)
C70.3370 (5)0.7465 (4)0.5428 (3)0.0348 (8)
H70.39630.84360.58520.042*
C80.2759 (5)0.5087 (4)0.5229 (3)0.0290 (7)
C90.1744 (5)0.4725 (4)0.4164 (3)0.0323 (7)
H90.12420.37550.37270.039*
C100.2270 (5)0.7099 (4)0.4361 (3)0.0325 (8)
C110.1903 (6)0.8224 (4)0.3919 (3)0.0446 (9)
H11A0.04620.81160.37390.067*
H11B0.23890.81170.32840.067*
H11C0.26230.91640.44510.067*
C120.2901 (5)0.3943 (4)0.5726 (3)0.0337 (8)
U11U22U33U12U13U23
Ag10.0615 (2)0.04191 (18)0.02887 (17)0.01567 (14)−0.00615 (14)0.01461 (14)
Ag20.0587 (2)0.04844 (19)0.02474 (17)0.01533 (15)−0.00451 (14)0.01602 (14)
O10.0578 (16)0.0322 (13)0.0318 (14)0.0159 (12)0.0002 (12)0.0042 (12)
O20.0594 (16)0.0437 (15)0.0361 (15)0.0211 (13)0.0066 (13)0.0235 (13)
O30.0637 (17)0.0331 (15)0.0403 (15)0.0112 (13)0.0052 (14)0.0129 (13)
O40.0679 (17)0.0483 (16)0.0298 (15)0.0125 (13)−0.0072 (13)0.0203 (13)
O50.0775 (19)0.0463 (16)0.0371 (15)0.0244 (14)0.0124 (14)0.0168 (13)
O60.085 (2)0.0323 (15)0.085 (2)0.0153 (14)0.0464 (19)0.0196 (16)
O70.0594 (16)0.0432 (15)0.0392 (16)0.0134 (13)0.0068 (13)0.0128 (13)
O80.0576 (17)0.0515 (17)0.076 (2)0.0076 (14)−0.0009 (16)0.0351 (17)
N10.0363 (15)0.0281 (15)0.0233 (15)0.0079 (12)−0.0021 (12)0.0093 (12)
N20.0315 (14)0.0321 (15)0.0185 (14)0.0094 (12)0.0025 (12)0.0078 (12)
N30.0347 (15)0.0332 (16)0.0236 (15)0.0097 (12)0.0001 (12)0.0107 (13)
N40.0339 (15)0.0387 (17)0.0248 (15)0.0108 (13)0.0034 (12)0.0137 (13)
C10.0310 (17)0.0273 (17)0.0220 (17)0.0086 (14)0.0012 (14)0.0054 (14)
C20.0208 (15)0.0322 (18)0.0238 (17)0.0060 (13)0.0006 (13)0.0097 (15)
C30.0385 (18)0.0325 (18)0.0203 (17)0.0102 (15)0.0018 (15)0.0036 (15)
C40.0318 (17)0.0305 (18)0.0285 (18)0.0096 (14)0.0031 (15)0.0109 (15)
C50.073 (3)0.0265 (19)0.036 (2)0.0127 (18)0.001 (2)0.0071 (17)
C60.0303 (17)0.0310 (18)0.033 (2)0.0109 (14)0.0105 (15)0.0143 (16)
C70.0382 (19)0.0315 (18)0.0309 (19)0.0081 (15)0.0041 (16)0.0105 (16)
C80.0245 (16)0.0384 (19)0.0276 (18)0.0127 (14)0.0065 (14)0.0143 (16)
C90.0357 (18)0.0324 (18)0.0274 (18)0.0125 (15)0.0046 (15)0.0093 (15)
C100.0319 (17)0.040 (2)0.0323 (19)0.0138 (15)0.0096 (15)0.0196 (17)
C110.057 (2)0.042 (2)0.039 (2)0.0143 (18)0.0074 (19)0.0222 (19)
C120.0296 (17)0.037 (2)0.037 (2)0.0119 (15)0.0048 (15)0.0170 (17)
Ag1—N12.260 (3)N2—C21.353 (4)
Ag1—N32.311 (3)N3—C71.330 (4)
Ag1—O62.478 (3)N3—C81.339 (4)
Ag1—O52.517 (3)N4—C101.335 (4)
Ag1—O42.598 (3)N4—C91.340 (4)
Ag2—N4i2.233 (3)N4—Ag2iii2.233 (3)
Ag2—N22.250 (3)C1—C21.369 (4)
Ag2—O22.558 (3)C1—H10.9300
Ag2—O5ii2.688 (3)C2—C61.525 (4)
Ag2—O4ii2.809 (3)C3—C41.387 (5)
O1—C61.244 (4)C3—H30.9300
O2—C61.244 (4)C4—C51.495 (5)
O3—C121.249 (4)C5—H5A'0.9600
O4—C121.243 (4)C5—H5B'0.9600
O5—H5A0.8500C5—H5C'0.9600
O5—H5B0.8500C7—C101.396 (5)
O6—H6A0.8500C7—H70.9300
O6—H6B0.8500C8—C91.378 (5)
O7—H7A0.8501C8—C121.521 (5)
O7—H7B0.8501C9—H90.9300
O8—H8A0.8499C10—C111.491 (5)
O8—H8B0.8499C11—H11A0.9600
N1—C41.336 (4)C11—H11B0.9600
N1—C11.342 (4)C11—H11C0.9600
N2—C31.326 (4)
N1—Ag1—N3149.97 (10)N2—C2—C6118.5 (3)
N1—Ag1—O6110.25 (10)C1—C2—C6121.6 (3)
N3—Ag1—O692.51 (10)N2—C3—C4123.0 (3)
N1—Ag1—O5111.71 (9)N2—C3—H3118.5
N3—Ag1—O583.98 (9)C4—C3—H3118.5
O6—Ag1—O595.92 (9)N1—C4—C3119.7 (3)
N1—Ag1—O484.35 (9)N1—C4—C5119.3 (3)
N3—Ag1—O467.85 (9)C3—C4—C5120.9 (3)
O6—Ag1—O4154.82 (9)C4—C5—H5A'109.5
O5—Ag1—O497.40 (9)C4—C5—H5B'109.5
N4i—Ag2—N2146.43 (10)H5A'—C5—H5B'109.5
N4i—Ag2—O2138.04 (9)C4—C5—H5C'109.5
N2—Ag2—O269.03 (9)H5A'—C5—H5C'109.5
C6—O2—Ag2114.8 (2)H5B'—C5—H5C'109.5
C12—O4—Ag1114.3 (2)O2—C6—O1127.0 (3)
Ag1—O5—H5A119.7O2—C6—C2116.9 (3)
Ag1—O5—H5B108.3O1—C6—C2116.1 (3)
H5A—O5—H5B116.9N3—C7—C10122.5 (3)
Ag1—O6—H6A115.2N3—C7—H7118.8
Ag1—O6—H6B128.7C10—C7—H7118.8
H6A—O6—H6B116.2N3—C8—C9119.8 (3)
H7A—O7—H7B115.7N3—C8—C12118.5 (3)
H8A—O8—H8B117.8C9—C8—C12121.7 (3)
C4—N1—C1117.3 (3)N4—C9—C8122.8 (3)
C4—N1—Ag1122.3 (2)N4—C9—H9118.6
C1—N1—Ag1120.1 (2)C8—C9—H9118.6
C3—N2—C2117.1 (3)N4—C10—C7119.7 (3)
C3—N2—Ag2122.3 (2)N4—C10—C11118.8 (3)
C2—N2—Ag2120.5 (2)C7—C10—C11121.4 (3)
C7—N3—C8117.7 (3)C10—C11—H11A109.5
C7—N3—Ag1121.3 (2)C10—C11—H11B109.5
C8—N3—Ag1120.7 (2)H11A—C11—H11B109.5
C10—N4—C9117.4 (3)C10—C11—H11C109.5
C10—N4—Ag2iii121.7 (2)H11A—C11—H11C109.5
C9—N4—Ag2iii120.3 (2)H11B—C11—H11C109.5
N1—C1—C2122.9 (3)O4—C12—O3125.0 (3)
N1—C1—H1118.6O4—C12—C8118.0 (3)
C2—C1—H1118.6O3—C12—C8116.9 (3)
N2—C2—C1119.9 (3)
N4i—Ag2—O2—C6−159.0 (2)Ag2—N2—C3—C4177.9 (2)
N2—Ag2—O2—C6−3.8 (2)C1—N1—C4—C3−0.9 (5)
N1—Ag1—O4—C12−162.1 (3)Ag1—N1—C4—C3172.7 (2)
N3—Ag1—O4—C126.3 (2)C1—N1—C4—C5−179.3 (3)
O6—Ag1—O4—C12−34.7 (4)Ag1—N1—C4—C5−5.7 (4)
O5—Ag1—O4—C1286.7 (2)N2—C3—C4—N10.8 (5)
N3—Ag1—N1—C4178.7 (2)N2—C3—C4—C5179.2 (3)
O6—Ag1—N1—C441.6 (3)Ag2—O2—C6—O1−175.6 (3)
O5—Ag1—N1—C4−63.7 (3)Ag2—O2—C6—C25.9 (3)
O4—Ag1—N1—C4−159.5 (3)N2—C2—C6—O2−5.7 (4)
N3—Ag1—N1—C1−7.9 (4)C1—C2—C6—O2175.1 (3)
O6—Ag1—N1—C1−144.9 (2)N2—C2—C6—O1175.7 (3)
O5—Ag1—N1—C1109.7 (2)C1—C2—C6—O1−3.6 (4)
O4—Ag1—N1—C114.0 (2)C8—N3—C7—C101.0 (5)
N4i—Ag2—N2—C3−27.5 (3)Ag1—N3—C7—C10−173.2 (2)
O2—Ag2—N2—C3−177.1 (3)C7—N3—C8—C91.7 (5)
N4i—Ag2—N2—C2150.2 (2)Ag1—N3—C8—C9175.9 (2)
O2—Ag2—N2—C20.6 (2)C7—N3—C8—C12−176.5 (3)
N1—Ag1—N3—C7−164.1 (2)Ag1—N3—C8—C12−2.3 (4)
O6—Ag1—N3—C7−23.9 (3)C10—N4—C9—C83.1 (5)
O5—Ag1—N3—C771.8 (3)Ag2iii—N4—C9—C8−167.9 (2)
O4—Ag1—N3—C7172.4 (3)N3—C8—C9—N4−3.9 (5)
N1—Ag1—N3—C821.9 (3)C12—C8—C9—N4174.3 (3)
O6—Ag1—N3—C8162.1 (2)C9—N4—C10—C7−0.4 (5)
O5—Ag1—N3—C8−102.2 (2)Ag2iii—N4—C10—C7170.5 (2)
O4—Ag1—N3—C8−1.7 (2)C9—N4—C10—C11−177.6 (3)
C4—N1—C1—C20.1 (5)Ag2iii—N4—C10—C11−6.7 (4)
Ag1—N1—C1—C2−173.6 (2)N3—C7—C10—N4−1.6 (5)
C3—N2—C2—C1−0.8 (4)N3—C7—C10—C11175.4 (3)
Ag2—N2—C2—C1−178.7 (2)Ag1—O4—C12—O3172.6 (3)
C3—N2—C2—C6179.9 (3)Ag1—O4—C12—C8−9.6 (4)
Ag2—N2—C2—C62.1 (4)N3—C8—C12—O48.6 (5)
N1—C1—C2—N20.7 (5)C9—C8—C12—O4−169.5 (3)
N1—C1—C2—C6180.0 (3)N3—C8—C12—O3−173.4 (3)
C2—N2—C3—C40.1 (5)C9—C8—C12—O38.4 (5)
D—H···AD—HH···AD···AD—H···A
C1—H1···O40.932.383.061 (4)130
O5—H5B···O2ii0.851.942.675 (4)144
O5—H5A···O7iv0.851.912.756 (4)175
O6—H6A···O7v0.852.002.828 (4)166
O6—H6B···O1vi0.851.962.794 (4)168
O7—H7A···O8vii0.851.862.698 (4)168
O7—H7B···O3viii0.851.872.712 (4)171
O8—H8A···O10.852.022.867 (4)176
O8—H8B···O30.852.132.965 (4)166
O8—H8B···O40.852.443.116 (4)137
Table 1

Selected bond lengths (Å)

Ag1—N12.260 (3)
Ag1—N32.311 (3)
Ag1—O62.478 (3)
Ag1—O52.517 (3)
Ag1—O42.598 (3)
Ag2—N4i2.233 (3)
Ag2—N22.250 (3)
Ag2—O22.558 (3)
Ag2—O5ii2.688 (3)
Ag2—O4ii2.809 (3)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C1—H1⋯O40.932.383.061 (4)130
O5—H5B⋯O2ii0.851.942.675 (4)144
O5—H5A⋯O7iii0.851.912.756 (4)175
O6—H6A⋯O7iv0.852.002.828 (4)166
O6—H6B⋯O1v0.851.962.794 (4)168
O7—H7A⋯O8vi0.851.862.698 (4)168
O7—H7B⋯O3vii0.851.872.712 (4)171
O8—H8A⋯O10.852.022.867 (4)176
O8—H8B⋯O30.852.132.965 (4)166
O8—H8B⋯O40.852.443.116 (4)137

Symmetry codes: (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) .

  2 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Metal-containing ligands for mixed-metal polymers: novel Cu(II)-Ag(I) mixed-metal coordination polymers generated from [Cu(2-methylpyrazine-5-carboxylate)2(H2O)].3H2O and silver(I) salts.

Authors:  Y B Dong; M D Smith; H C zur Loye
Journal:  Inorg Chem       Date:  2000-05-01       Impact factor: 5.165
  2 in total

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