Literature DB >> 21578566

catena-Poly[[[aqua-silver(I)]-μ-1,1'-(butane-1,4-di-yl)di-1H-imidazole-κN:N] hemi(biphenyl-4,4'-dicarboxyl-ate) dihydrate].

Zheyu Zhang1.   

Abstract

In the title compound, {[Ag(C(10)H(14)N(4))(H(2)O)](C(14)H(8)O(4))(0.5)·2H(2)O}(n), the Ag(I) ion is three-coordinated by two N atoms from two independent 1,1'-(butane-1,4-di-yl)di-1H-imidazole (BBI) ligands and one water O atom in a distorted T-shaped coordination geometry. The biphenyl-4,4'-dicarboxyl-ate (BPDC) dianions do not coordinate to Ag(I) ions but act as counter-ions. The Ag(I) ions are linked by BBI ligands, forming a zigzag chain. These chains are linked into a two-dimensional supra-molecular architecture by O-H⋯O hydrogen-bonding inter-actions between water mol-ecules and carboxyl-ate O atoms of the BPDC dianions.

Entities:  

Year:  2009        PMID： 21578566      PMCID： PMC2971936          DOI： 10.1107/S1600536809045826

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


Related literature

For general background to the design and construction of metal-organic frameworks, see: Kitagawa et al. (2004 ▶); Ma et al. (2009 ▶); Li et al. (2005 ▶). For a related structure, see: Ma et al. (2005 ▶).

Experimental

Crystal data

[Ag(C10H14N4)(H2O)](C14H8O4)0.5·2H2O M = 472.27 Triclinic, a = 9.7685 (6) Å b = 10.0659 (6) Å c = 10.9224 (7) Å α = 80.190 (1)° β = 68.898 (1)° γ = 74.775 (1)° V = 963.36 (10) Å3 Z = 2 Mo Kα radiation μ = 1.08 mm−1 T = 293 K 0.23 × 0.16 × 0.14 mm

Data collection

Bruker APEX CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.81, T max = 0.86 5289 measured reflections 3569 independent reflections 3422 reflections with I > 2σ(I) R int = 0.011

Refinement

R[F 2 > 2σ(F 2)] = 0.023 wR(F 2) = 0.058 S = 1.06 3569 reflections 267 parameters 9 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.36 e Å−3 Δρmin = −0.42 e Å−3 Data collection: SMART (Bruker, 2002 ▶); cell refinement: SAINT (Bruker, 2002 ▶); 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 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809045826/ci2938sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809045826/ci2938Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ag(C10H14N4)(H2O)](C14H8O4)0.5·2H2OZ = 2
Mr = 472.27F(000) = 482
Triclinic, P1Dx = 1.628 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.7685 (6) ÅCell parameters from 3658 reflections
b = 10.0659 (6) Åθ = 2.0–25.7°
c = 10.9224 (7) ŵ = 1.08 mm−1
α = 80.190 (1)°T = 293 K
β = 68.898 (1)°Block, colourless
γ = 74.775 (1)°0.23 × 0.16 × 0.14 mm
V = 963.36 (10) Å3
Bruker APEX CCD area-detector diffractometer3569 independent reflections
Radiation source: fine-focus sealed tube3422 reflections with I > 2σ(I)
graphiteRint = 0.011
φ and ω scansθmax = 25.7°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −11→11
Tmin = 0.81, Tmax = 0.86k = −12→11
5289 measured reflectionsl = −12→13
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.058H atoms treated by a mixture of independent and constrained refinement
S = 1.06w = 1/[σ2(Fo2) + (0.0296P)2 + 0.5838P] where P = (Fo2 + 2Fc2)/3
3569 reflections(Δ/σ)max = 0.003
267 parametersΔρmax = 0.36 e Å−3
9 restraintsΔρmin = −0.41 e Å−3
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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*/UeqOcc. (<1)
Ag10.956725 (17)0.248290 (16)0.414393 (15)0.03644 (7)
C11.1776 (2)0.4373 (2)0.3910 (2)0.0390 (5)
H11.17380.41400.47810.047*
C21.2573 (2)0.5253 (2)0.3053 (2)0.0390 (5)
H21.31740.57310.32190.047*
C31.1389 (2)0.4463 (2)0.2074 (2)0.0325 (4)
H31.10420.43150.14310.039*
C41.2955 (2)0.6107 (2)0.0650 (2)0.0372 (5)
H4A1.26050.70830.07850.045*0.855 (8)
H4B1.25930.5933−0.00140.045*0.855 (8)
H4C1.32030.68960.08320.045*0.145 (8)
H4D1.22210.64280.02090.045*0.145 (8)
C51.4677 (3)0.5751 (3)0.0147 (3)0.0374 (9)0.855 (8)
H5A1.50360.6338−0.06470.045*0.855 (8)
H5B1.50380.59420.08040.045*0.855 (8)
C5A1.4372 (14)0.5180 (14)−0.0276 (12)0.024 (4)*0.145 (8)
H5C1.41220.4341−0.03720.029*0.145 (8)
H5D1.46860.5669−0.11410.029*0.145 (8)
C60.5360 (2)0.0327 (2)0.93096 (18)0.0289 (4)
H6A0.45800.08040.89370.035*
H6B0.58760.10040.93700.035*
C70.6471 (2)−0.0754 (2)0.84084 (19)0.0305 (4)
H7A0.7307−0.11570.87310.037*
H7B0.5982−0.14860.84330.037*
C80.7895 (2)0.0778 (2)0.6596 (2)0.0318 (4)
H80.82110.11760.71270.038*
C90.7547 (2)0.0266 (2)0.4916 (2)0.0357 (5)
H90.75880.02480.40550.043*
C100.6817 (2)−0.0505 (2)0.5973 (2)0.0344 (4)
H100.6266−0.11320.59750.041*
C110.4496 (2)0.46334 (19)0.55623 (18)0.0242 (4)
C120.4568 (2)0.3221 (2)0.5596 (2)0.0327 (4)
H120.52560.27280.48970.039*
C130.3640 (2)0.2543 (2)0.6645 (2)0.0326 (4)
H130.37160.16030.66410.039*
C140.2594 (2)0.32470 (19)0.77048 (18)0.0261 (4)
C150.2498 (2)0.4651 (2)0.7673 (2)0.0321 (4)
H150.17970.51430.83670.038*
C160.3426 (2)0.5328 (2)0.6629 (2)0.0318 (4)
H160.33370.62700.66340.038*
C170.1584 (2)0.2522 (2)0.88668 (19)0.0288 (4)
N11.10255 (19)0.38726 (19)0.32976 (17)0.0341 (4)
N21.23205 (18)0.53009 (17)0.18881 (17)0.0315 (4)
N30.82188 (19)0.10780 (18)0.53071 (16)0.0323 (4)
N40.70506 (18)−0.01762 (17)0.70361 (15)0.0286 (3)
O10.17403 (16)0.12310 (14)0.88583 (15)0.0355 (3)
O20.06563 (18)0.32386 (16)0.97662 (15)0.0418 (4)
O2W0.08819 (17)0.93824 (16)0.11184 (15)0.0354 (3)
O3W0.64273 (19)0.13798 (18)0.20741 (18)0.0471 (4)
O1W0.91632 (17)0.19506 (16)0.20090 (14)0.0353 (3)
H2A0.128 (3)0.984 (3)0.040 (2)0.053*
H2B0.014 (2)0.908 (3)0.115 (3)0.053*
H3A0.715 (3)0.175 (2)0.202 (3)0.053*
H3B0.677 (3)0.0563 (19)0.180 (3)0.053*
H1B0.957 (3)0.243 (2)0.130 (2)0.053*
H1A0.958 (3)0.1105 (17)0.201 (3)0.053*
U11U22U33U12U13U23
Ag10.03500 (10)0.03866 (11)0.03170 (10)−0.01681 (7)−0.00289 (7)0.00291 (7)
C10.0356 (11)0.0507 (13)0.0313 (11)−0.0134 (10)−0.0098 (9)−0.0015 (9)
C20.0344 (11)0.0456 (12)0.0412 (12)−0.0159 (9)−0.0118 (9)−0.0049 (10)
C30.0277 (10)0.0364 (11)0.0306 (10)−0.0102 (8)−0.0044 (8)−0.0021 (8)
C40.0315 (11)0.0308 (11)0.0403 (12)−0.0079 (9)−0.0050 (9)0.0070 (9)
C50.0313 (14)0.0285 (15)0.0442 (15)−0.0113 (10)−0.0033 (11)0.0055 (11)
C60.0295 (10)0.0319 (10)0.0240 (10)−0.0112 (8)−0.0062 (8)0.0027 (8)
C70.0319 (10)0.0327 (10)0.0246 (9)−0.0115 (8)−0.0073 (8)0.0056 (8)
C80.0316 (10)0.0382 (11)0.0260 (9)−0.0151 (9)−0.0069 (8)0.0019 (8)
C90.0406 (12)0.0438 (12)0.0240 (10)−0.0168 (10)−0.0085 (8)0.0003 (8)
C100.0391 (11)0.0371 (11)0.0292 (10)−0.0153 (9)−0.0101 (9)−0.0008 (8)
C110.0232 (9)0.0249 (9)0.0243 (9)−0.0071 (7)−0.0078 (7)0.0009 (7)
C120.0358 (11)0.0256 (10)0.0285 (10)−0.0083 (8)0.0004 (8)−0.0030 (8)
C130.0384 (11)0.0230 (9)0.0322 (10)−0.0106 (8)−0.0050 (9)−0.0003 (8)
C140.0241 (9)0.0294 (10)0.0258 (9)−0.0093 (7)−0.0094 (7)0.0031 (7)
C150.0302 (10)0.0300 (10)0.0299 (10)−0.0076 (8)−0.0011 (8)−0.0046 (8)
C160.0331 (10)0.0228 (9)0.0336 (10)−0.0090 (8)−0.0016 (8)−0.0036 (8)
C170.0274 (9)0.0318 (10)0.0291 (10)−0.0123 (8)−0.0097 (8)0.0017 (8)
N10.0312 (9)0.0382 (10)0.0312 (9)−0.0133 (8)−0.0053 (7)−0.0005 (7)
N20.0249 (8)0.0299 (9)0.0352 (9)−0.0075 (7)−0.0049 (7)−0.0002 (7)
N30.0327 (9)0.0370 (9)0.0256 (8)−0.0137 (7)−0.0062 (7)0.0032 (7)
N40.0294 (8)0.0310 (8)0.0237 (8)−0.0104 (7)−0.0062 (6)0.0020 (6)
O10.0360 (8)0.0283 (7)0.0378 (8)−0.0146 (6)−0.0038 (6)0.0019 (6)
O20.0445 (9)0.0343 (8)0.0333 (8)−0.0135 (7)0.0052 (7)−0.0010 (6)
O2W0.0375 (8)0.0371 (8)0.0352 (8)−0.0129 (6)−0.0157 (7)0.0029 (6)
O3W0.0394 (9)0.0453 (10)0.0573 (10)−0.0110 (8)−0.0152 (8)−0.0052 (8)
O1W0.0397 (8)0.0319 (8)0.0295 (7)−0.0129 (6)−0.0030 (6)−0.0007 (6)
Ag1—N12.1209 (17)C7—H7B0.97
Ag1—N32.1237 (16)C8—N31.326 (3)
Ag1—O1W2.6611 (12)C8—N41.344 (3)
C1—C21.350 (3)C8—H80.93
C1—N11.378 (3)C9—C101.355 (3)
C1—H10.93C9—N31.372 (3)
C2—N21.371 (3)C9—H90.93
C2—H20.93C10—N41.368 (3)
C3—N11.328 (3)C10—H100.93
C3—N21.338 (3)C11—C161.399 (3)
C3—H30.93C11—C121.400 (3)
C4—N21.469 (3)C11—C11iii1.492 (4)
C4—C51.531 (3)C12—C131.382 (3)
C4—C5A1.564 (13)C12—H120.93
C4—H4A0.97C13—C141.391 (3)
C4—H4B0.97C13—H130.93
C4—H4C0.96C14—C151.387 (3)
C4—H4D0.96C14—C171.509 (3)
C5—C5i1.518 (5)C15—C161.379 (3)
C5—H5A0.97C15—H150.93
C5—H5B0.97C16—H160.93
C5A—C5Ai1.49 (3)C17—O21.251 (2)
C5A—H5C0.97C17—O11.269 (2)
C5A—H5D0.97O2W—H2A0.857 (16)
C6—C71.519 (3)O2W—H2B0.842 (16)
C6—C6ii1.531 (4)O3W—H3A0.865 (16)
C6—H6A0.97O3W—H3B0.864 (16)
C6—H6B0.97O1W—H1B0.863 (16)
C7—N41.473 (2)O1W—H1A0.842 (16)
C7—H7A0.97
N1—Ag1—N3169.34 (7)N4—C7—H7B109.1
C2—C1—N1109.61 (19)C6—C7—H7B109.1
C2—C1—H1125.2H7A—C7—H7B107.8
N1—C1—H1125.2N3—C8—N4111.21 (18)
C1—C2—N2106.38 (19)N3—C8—H8124.4
C1—C2—H2126.8N4—C8—H8124.4
N2—C2—H2126.8C10—C9—N3109.77 (18)
N1—C3—N2111.13 (19)C10—C9—H9125.1
N1—C3—H3124.4N3—C9—H9125.1
N2—C3—H3124.4C9—C10—N4106.30 (18)
N2—C4—C5112.46 (18)C9—C10—H10126.9
N2—C4—C5A110.1 (5)N4—C10—H10126.9
N2—C4—H4A109.1C16—C11—C12116.87 (17)
C5—C4—H4A109.1C16—C11—C11iii121.5 (2)
C5A—C4—H4A136.1C12—C11—C11iii121.6 (2)
N2—C4—H4B109.1C13—C12—C11121.43 (18)
C5—C4—H4B109.1C13—C12—H12119.3
C5A—C4—H4B76.9C11—C12—H12119.3
H4A—C4—H4B107.8C12—C13—C14120.93 (18)
N2—C4—H4C109.8C12—C13—H13119.5
C5—C4—H4C77.1C14—C13—H13119.5
C5A—C4—H4C110.9C15—C14—C13118.11 (17)
H4B—C4—H4C134.0C15—C14—C17120.18 (17)
N2—C4—H4D109.4C13—C14—C17121.72 (17)
C5—C4—H4D132.7C16—C15—C14121.05 (18)
C5A—C4—H4D108.3C16—C15—H15119.5
H4A—C4—H4D75.9C14—C15—H15119.5
H4C—C4—H4D108.3C15—C16—C11121.60 (18)
C5i—C5—C4112.6 (3)C15—C16—H16119.2
C5i—C5—H5A109.1C11—C16—H16119.2
C4—C5—H5A109.1O2—C17—O1124.92 (18)
C5i—C5—H5B109.1O2—C17—C14117.50 (17)
C4—C5—H5B109.1O1—C17—C14117.59 (17)
H5A—C5—H5B107.8C3—N1—C1105.41 (17)
C5Ai—C5A—C4110.4 (13)C3—N1—Ag1127.40 (15)
C5Ai—C5A—H5C109.6C1—N1—Ag1127.18 (15)
C4—C5A—H5C109.6C3—N2—C2107.47 (17)
C5Ai—C5A—H5D109.6C3—N2—C4125.54 (19)
C4—C5A—H5D109.6C2—N2—C4126.99 (18)
H5C—C5A—H5D108.1C8—N3—C9105.46 (17)
C7—C6—C6ii111.4 (2)C8—N3—Ag1125.56 (14)
C7—C6—H6A109.4C9—N3—Ag1128.95 (14)
C6ii—C6—H6A109.4C8—N4—C10107.26 (16)
C7—C6—H6B109.4C8—N4—C7126.55 (17)
C6ii—C6—H6B109.4C10—N4—C7126.19 (17)
H6A—C6—H6B108.0H2A—O2W—H2B116 (2)
N4—C7—C6112.45 (16)H3A—O3W—H3B111 (2)
N4—C7—H7A109.1H1B—O1W—H1A114 (2)
C6—C7—H7A109.1
N1—C1—C2—N2−0.1 (3)C2—C1—N1—Ag1−178.88 (15)
N2—C4—C5—C5i61.3 (4)N3—Ag1—N1—C3177.4 (3)
C5A—C4—C5—C5i−32.3 (8)N3—Ag1—N1—C1−3.9 (5)
N2—C4—C5A—C5Ai−68.5 (14)N1—C3—N2—C2−0.1 (2)
C5—C4—C5A—C5Ai32.3 (9)N1—C3—N2—C4179.42 (18)
C6ii—C6—C7—N4173.50 (19)C1—C2—N2—C30.1 (2)
N3—C9—C10—N4−0.6 (3)C1—C2—N2—C4−179.36 (19)
C16—C11—C12—C13−1.0 (3)C5—C4—N2—C3−121.4 (2)
C11iii—C11—C12—C13179.5 (2)C5A—C4—N2—C3−82.8 (6)
C11—C12—C13—C140.2 (3)C5—C4—N2—C258.1 (3)
C12—C13—C14—C150.7 (3)C5A—C4—N2—C296.6 (6)
C12—C13—C14—C17−179.23 (19)N4—C8—N3—C9−0.2 (2)
C13—C14—C15—C16−0.8 (3)N4—C8—N3—Ag1−178.33 (13)
C17—C14—C15—C16179.08 (19)C10—C9—N3—C80.5 (3)
C14—C15—C16—C110.1 (3)C10—C9—N3—Ag1178.52 (15)
C12—C11—C16—C150.8 (3)N1—Ag1—N3—C812.2 (5)
C11iii—C11—C16—C15−179.6 (2)N1—Ag1—N3—C9−165.4 (3)
C15—C14—C17—O21.4 (3)N3—C8—N4—C10−0.1 (2)
C13—C14—C17—O2−178.69 (19)N3—C8—N4—C7−179.62 (18)
C15—C14—C17—O1−178.55 (18)C9—C10—N4—C80.4 (2)
C13—C14—C17—O11.3 (3)C9—C10—N4—C7179.93 (19)
N2—C3—N1—C10.0 (2)C6—C7—N4—C864.4 (3)
N2—C3—N1—Ag1178.97 (13)C6—C7—N4—C10−115.0 (2)
C2—C1—N1—C30.1 (3)
D—H···AD—HH···AD···AD—H···A
O2W—H2A···O1iv0.86 (2)1.99 (2)2.833 (2)166 (3)
O2W—H2B···O1v0.84 (2)1.95 (2)2.779 (2)169 (3)
O3W—H3B···O1vi0.86 (2)2.05 (2)2.877 (2)160 (2)
O3W—H3A···O1W0.86 (2)2.02 (2)2.852 (2)161 (2)
O1W—H1A···O2Wvii0.84 (2)2.03 (2)2.802 (2)153 (2)
Table 1

Selected bond lengths (Å)

Ag1—N12.1209 (17)
Ag1—O1W 2.6611 (12)
Ag1—N32.1237 (16)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O2W—H2A⋯O1i 0.86 (2)1.99 (2)2.833 (2)166 (3)
O2W—H2B⋯O1ii 0.84 (2)1.95 (2)2.779 (2)169 (3)
O3W—H3B⋯O1iii 0.86 (2)2.05 (2)2.877 (2)160 (2)
O3W—H3A⋯O1W 0.86 (2)2.02 (2)2.852 (2)161 (2)
O1W—H1A⋯O2W iv 0.84 (2)2.03 (2)2.802 (2)153 (2)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) .

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