Literature DB >> 21201571

Poly[aqua-[μ(2)-1,1'-(butane-1,4-di-yl)diimidazole](μ(2)-naphthalene-1,4-dicarboxyl-ato)nickel(II)].

Xian-Zhi Zou1.   

Abstract

In the title compound, [Ni(C(12)H(6)O(4))(C(10)H(14)N(4))(H(2)O)](n), the coordination polyhedron around each Ni(II) atom is a distorted cis-NiN(2)O(4) octa-hedron. The naphthalene-1,4-dicarboxyl-ate and 1,1'-(butane-1,4-di-yl)diimidazole ligands bridge the Ni centres to form a two-dimensional (4,4)-network, and O-H⋯O hydrogen bonds complete the structure.

Entities:  

Year:  2008        PMID： 21201571      PMCID： PMC2960619          DOI： 10.1107/S1600536808024008

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


Related literature

For general background, see: Batten & Robson (1998 ▶). For a related structure, see: Ma et al., (2003 ▶).

Experimental

Crystal data

[Ni(C12H6O4)(C10H14N4)(H2O)] M = 481.15 Monoclinic, a = 12.4213 (12) Å b = 13.2543 (13) Å c = 13.4328 (13) Å β = 107.361 (2)° V = 2110.8 (4) Å3 Z = 4 Mo Kα radiation μ = 0.96 mm−1 T = 293 (2) K 0.19 × 0.17 × 0.15 mm

Data collection

Bruker APEX CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 1998 ▶) T min = 0.827, T max = 0.866 11720 measured reflections 4157 independent reflections 2982 reflections with I > 2σ(I) R int = 0.063

Refinement

R[F 2 > 2σ(F 2)] = 0.049 wR(F 2) = 0.097 S = 1.05 4157 reflections 297 parameters 3 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.54 e Å−3 Δρmin = −0.40 e Å−3 Data collection: SMART (Bruker, 1998 ▶); cell refinement: SAINT (Bruker, 1998 ▶); 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/S1600536808024008/hb2770sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808024008/hb2770Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ni(C12H6O4)(C10H14N4)(H2O)]F000 = 1000
Mr = 481.15Dx = 1.514 Mg m−3
Monoclinic, P21/nMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 4157 reflections
a = 12.4213 (12) Åθ = 1.9–26.1º
b = 13.2543 (13) ŵ = 0.96 mm−1
c = 13.4328 (13) ÅT = 293 (2) K
β = 107.361 (2)ºBlock, green
V = 2110.8 (4) Å30.19 × 0.17 × 0.15 mm
Z = 4
Bruker APEX CCD diffractometer4157 independent reflections
Radiation source: fine-focus sealed tube2982 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.063
T = 293(2) Kθmax = 26.1º
ω scansθmin = 2.0º
Absorption correction: multi-scan(SADABS; Bruker, 1998)h = −9→15
Tmin = 0.827, Tmax = 0.866k = −16→14
11720 measured reflectionsl = −16→16
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.049H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.097  w = 1/[σ2(Fo2) + (0.0253P)2] where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max < 0.001
4157 reflectionsΔρmax = 0.54 e Å−3
297 parametersΔρmin = −0.40 e Å−3
3 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
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
C10.2969 (3)0.1196 (2)0.2222 (3)0.0208 (8)
C20.2145 (3)0.1584 (2)0.2758 (2)0.0190 (8)
C30.2114 (3)0.2586 (2)0.2946 (3)0.0264 (9)
H30.25830.30190.27210.032*
C40.1392 (3)0.2986 (2)0.3472 (3)0.0238 (8)
H40.13990.36770.35970.029*
C50.0674 (3)0.2376 (2)0.3805 (2)0.0203 (8)
C6−0.0034 (3)0.2829 (2)0.4420 (3)0.0218 (8)
C70.0636 (3)0.1328 (2)0.3576 (2)0.0180 (7)
C80.1382 (3)0.0919 (2)0.3055 (2)0.0172 (7)
C90.1306 (3)−0.0118 (2)0.2806 (3)0.0256 (8)
H90.1795−0.03930.24730.031*
C100.0536 (3)−0.0723 (3)0.3042 (3)0.0281 (9)
H100.0497−0.14040.28680.034*
C11−0.0196 (3)−0.0320 (3)0.3546 (3)0.0312 (9)
H11−0.0722−0.07380.37060.037*
C12−0.0157 (3)0.0664 (2)0.3806 (3)0.0257 (8)
H12−0.06570.09140.41410.031*
C130.1710 (3)0.2460 (3)−0.1581 (3)0.0335 (10)
H130.16440.1937−0.20560.040*
C140.1151 (4)0.3340 (3)−0.1787 (3)0.0430 (11)
H140.06440.3537−0.24180.052*
C150.2219 (3)0.3312 (3)−0.0198 (3)0.0310 (9)
H150.25810.35100.04840.037*
C160.1118 (3)0.4914 (2)−0.0714 (3)0.0274 (9)
H16A0.12680.50240.00290.033*
H16B0.03110.4976−0.10390.033*
C170.1715 (3)0.5711 (2)−0.1149 (3)0.0296 (9)
H17A0.14980.5648−0.19030.036*
H17B0.25230.5605−0.08820.036*
C180.1434 (3)0.6771 (2)−0.0863 (3)0.0293 (9)
H18A0.06220.6862−0.10830.035*
H18B0.17050.6855−0.01120.035*
C190.1971 (3)0.7560 (2)−0.1379 (3)0.0293 (9)
H19A0.27540.7381−0.12770.035*
H19B0.15900.7559−0.21230.035*
C200.1050 (3)0.9021 (3)−0.0704 (3)0.0395 (11)
H200.03530.8734−0.07490.047*
C210.2746 (3)0.9270 (2)−0.0777 (3)0.0238 (8)
H210.34360.9163−0.08980.029*
N40.2477 (2)1.01080 (19)−0.0399 (2)0.0212 (7)
C230.1402 (3)0.9948 (3)−0.0365 (3)0.0378 (10)
H230.09731.0419−0.01370.045*
N10.2384 (2)0.2446 (2)−0.0581 (2)0.0224 (7)
N20.1476 (2)0.38862 (19)−0.0887 (2)0.0232 (7)
N30.1920 (2)0.8579 (2)−0.0970 (2)0.0240 (7)
O1−0.05860 (18)0.36339 (16)0.40707 (17)0.0227 (5)
O20.3062 (2)0.17401 (16)0.14730 (18)0.0266 (6)
O1W0.4733 (2)0.04150 (17)0.12115 (19)0.0208 (6)
O3−0.00731 (19)0.24467 (16)0.52507 (17)0.0265 (6)
O40.35191 (19)0.04171 (16)0.25344 (18)0.0257 (6)
Ni10.35134 (4)0.13565 (3)0.01819 (3)0.02231 (14)
HW120.495 (2)−0.0135 (16)0.107 (2)0.020 (10)*
HW110.440 (3)0.034 (2)0.166 (2)0.053 (15)*
U11U22U33U12U13U23
C10.023 (2)0.0180 (19)0.0236 (19)−0.0040 (15)0.0094 (15)−0.0067 (15)
C20.025 (2)0.0174 (19)0.0172 (18)0.0032 (14)0.0099 (15)0.0011 (14)
C30.034 (2)0.0166 (19)0.037 (2)−0.0033 (16)0.0226 (18)0.0027 (16)
C40.033 (2)0.0108 (18)0.033 (2)0.0005 (15)0.0184 (18)−0.0043 (15)
C50.024 (2)0.0201 (19)0.0198 (19)0.0018 (15)0.0110 (15)0.0017 (15)
C60.023 (2)0.0178 (19)0.028 (2)−0.0063 (15)0.0133 (17)−0.0083 (16)
C70.0207 (18)0.0162 (18)0.0187 (17)0.0009 (14)0.0085 (14)0.0007 (14)
C80.0238 (19)0.0136 (17)0.0162 (17)0.0012 (14)0.0088 (15)0.0009 (13)
C90.030 (2)0.021 (2)0.030 (2)0.0018 (16)0.0157 (17)−0.0013 (16)
C100.034 (2)0.0147 (19)0.039 (2)−0.0018 (16)0.0167 (19)−0.0041 (16)
C110.037 (2)0.022 (2)0.041 (2)−0.0094 (17)0.021 (2)−0.0018 (17)
C120.030 (2)0.025 (2)0.028 (2)−0.0024 (16)0.0182 (17)−0.0027 (16)
C130.047 (3)0.023 (2)0.029 (2)0.0090 (18)0.0076 (19)−0.0050 (17)
C140.057 (3)0.035 (2)0.026 (2)0.019 (2)−0.004 (2)0.0003 (18)
C150.035 (2)0.024 (2)0.027 (2)0.0056 (17)−0.0011 (18)−0.0046 (16)
C160.027 (2)0.019 (2)0.037 (2)0.0056 (15)0.0124 (18)−0.0005 (16)
C170.030 (2)0.020 (2)0.039 (2)0.0018 (16)0.0105 (18)−0.0001 (17)
C180.029 (2)0.020 (2)0.039 (2)0.0005 (16)0.0105 (18)0.0004 (17)
C190.033 (2)0.020 (2)0.036 (2)−0.0053 (16)0.0123 (18)−0.0043 (17)
C200.025 (2)0.025 (2)0.074 (3)−0.0038 (17)0.023 (2)−0.005 (2)
C210.019 (2)0.024 (2)0.031 (2)−0.0005 (15)0.0100 (16)0.0025 (16)
N40.0213 (17)0.0140 (15)0.0293 (17)−0.0003 (12)0.0092 (13)−0.0001 (13)
C230.025 (2)0.023 (2)0.071 (3)−0.0001 (17)0.023 (2)−0.011 (2)
N10.0244 (17)0.0182 (16)0.0264 (17)0.0042 (12)0.0104 (14)0.0006 (13)
N20.0265 (17)0.0127 (16)0.0304 (17)0.0036 (12)0.0086 (14)0.0024 (12)
N30.0238 (17)0.0149 (16)0.0341 (17)−0.0021 (13)0.0099 (14)−0.0015 (13)
O10.0282 (14)0.0136 (12)0.0333 (14)0.0018 (10)0.0196 (11)0.0008 (11)
O20.0385 (16)0.0226 (14)0.0284 (14)0.0093 (11)0.0246 (12)0.0068 (11)
O1W0.0230 (15)0.0157 (14)0.0277 (15)0.0028 (11)0.0138 (12)−0.0024 (11)
O30.0388 (16)0.0215 (13)0.0276 (14)0.0028 (11)0.0226 (12)0.0014 (11)
O40.0309 (15)0.0202 (14)0.0316 (14)0.0091 (11)0.0178 (12)0.0062 (11)
Ni10.0259 (3)0.0180 (2)0.0269 (3)0.0016 (2)0.0137 (2)0.0008 (2)
C1—O41.240 (4)C16—C171.505 (5)
C1—O21.270 (4)C16—H16A0.9700
C1—C21.508 (4)C16—H16B0.9700
C2—C31.356 (4)C17—C181.525 (4)
C2—C81.434 (4)C17—H17A0.9700
C3—C41.400 (4)C17—H17B0.9700
C3—H30.9300C18—C191.515 (4)
C4—C51.375 (4)C18—H18A0.9700
C4—H40.9300C18—H18B0.9700
C5—C71.420 (4)C19—N31.466 (4)
C5—C61.500 (4)C19—H19A0.9700
C6—O31.240 (4)C19—H19B0.9700
C6—O11.279 (4)C20—C231.338 (5)
C7—C121.421 (4)C20—N31.368 (4)
C7—C81.424 (4)C20—H200.9300
C8—C91.412 (4)C21—N41.306 (4)
C9—C101.356 (4)C21—N31.341 (4)
C9—H90.9300C21—H210.9300
C10—C111.392 (5)N4—C231.367 (4)
C10—H100.9300N4—Ni1i2.099 (3)
C11—C121.347 (4)C23—H230.9300
C11—H110.9300O1—Ni1ii2.116 (2)
C12—H120.9300O1W—HW120.819 (16)
C13—C141.343 (5)O1W—HW110.83 (4)
C13—N11.355 (4)O3—Ni1ii2.347 (2)
C13—H130.9300Ni1—O1W2.125 (2)
C14—N21.363 (4)Ni1—O22.040 (2)
C14—H140.9300Ni1—O1iii2.116 (2)
C15—N11.299 (4)Ni1—O3iii2.347 (2)
C15—N21.334 (4)Ni1—N12.060 (3)
C15—H150.9300Ni1—N4iv2.099 (3)
C16—N21.472 (4)
O4—C1—O2124.8 (3)H17A—C17—H17B107.9
O4—C1—C2120.4 (3)C19—C18—C17110.8 (3)
O2—C1—C2114.8 (3)C19—C18—H18A109.5
C3—C2—C8119.5 (3)C17—C18—H18A109.5
C3—C2—C1118.9 (3)C19—C18—H18B109.5
C8—C2—C1121.5 (3)C17—C18—H18B109.5
C2—C3—C4121.6 (3)H18A—C18—H18B108.1
C2—C3—H3119.2N3—C19—C18113.0 (3)
C4—C3—H3119.2N3—C19—H19A109.0
C5—C4—C3121.1 (3)C18—C19—H19A109.0
C5—C4—H4119.5N3—C19—H19B109.0
C3—C4—H4119.5C18—C19—H19B109.0
C4—C5—C7119.2 (3)H19A—C19—H19B107.8
C4—C5—C6119.1 (3)C23—C20—N3106.2 (3)
C7—C5—C6121.7 (3)C23—C20—H20126.9
O3—C6—O1120.7 (3)N3—C20—H20126.9
O3—C6—C5121.2 (3)N4—C21—N3112.7 (3)
O1—C6—C5118.1 (3)N4—C21—H21123.6
C5—C7—C12122.5 (3)N3—C21—H21123.6
C5—C7—C8119.6 (3)C21—N4—C23104.3 (3)
C12—C7—C8117.8 (3)C21—N4—Ni1i128.0 (2)
C9—C8—C7118.6 (3)C23—N4—Ni1i127.4 (2)
C9—C8—C2122.4 (3)C20—C23—N4110.8 (3)
C7—C8—C2118.9 (3)C20—C23—H23124.6
C10—C9—C8121.5 (3)N4—C23—H23124.6
C10—C9—H9119.2C15—N1—C13104.8 (3)
C8—C9—H9119.2C15—N1—Ni1126.0 (2)
C9—C10—C11119.7 (3)C13—N1—Ni1129.1 (2)
C9—C10—H10120.2C15—N2—C14105.8 (3)
C11—C10—H10120.2C15—N2—C16126.7 (3)
C12—C11—C10121.3 (3)C14—N2—C16127.5 (3)
C12—C11—H11119.4C21—N3—C20106.0 (3)
C10—C11—H11119.4C21—N3—C19125.8 (3)
C11—C12—C7121.1 (3)C20—N3—C19128.1 (3)
C11—C12—H12119.5C6—O1—Ni1ii94.87 (19)
C7—C12—H12119.5C1—O2—Ni1130.1 (2)
C14—C13—N1110.2 (3)Ni1—O1W—HW12126 (2)
C14—C13—H13124.9Ni1—O1W—HW1197 (3)
N1—C13—H13124.9HW12—O1W—HW11110 (2)
C13—C14—N2106.3 (3)C6—O3—Ni1ii85.3 (2)
C13—C14—H14126.9O2—Ni1—N185.93 (10)
N2—C14—H14126.9O2—Ni1—N4iv102.65 (10)
N1—C15—N2112.9 (3)N1—Ni1—N4iv96.70 (11)
N1—C15—H15123.6O2—Ni1—O1iii159.34 (9)
N2—C15—H15123.6N1—Ni1—O1iii94.01 (10)
N2—C16—C17112.4 (3)N4iv—Ni1—O1iii97.87 (10)
N2—C16—H16A109.1O2—Ni1—O1W85.20 (9)
C17—C16—H16A109.1N1—Ni1—O1W169.33 (10)
N2—C16—H16B109.1N4iv—Ni1—O1W91.03 (10)
C17—C16—H16B109.1O1iii—Ni1—O1W92.20 (9)
H16A—C16—H16B107.9O2—Ni1—O3iii100.97 (9)
C16—C17—C18111.9 (3)N1—Ni1—O3iii86.35 (10)
C16—C17—H17A109.2N4iv—Ni1—O3iii156.33 (9)
C18—C17—H17A109.2O1iii—Ni1—O3iii58.47 (8)
C16—C17—H17B109.2O1W—Ni1—O3iii89.53 (8)
C18—C17—H17B109.2
D—H···AD—HH···AD···AD—H···A
O1W—HW12···O1v0.819 (16)1.847 (18)2.661 (3)172 (3)
O1W—HW11···O40.83 (4)1.83 (4)2.651 (3)169 (3)
Table 1

Selected bond lengths (Å)

Ni1—O1W2.125 (2)
Ni1—O22.040 (2)
Ni1—O1i2.116 (2)
Ni1—O3i2.347 (2)
Ni1—N12.060 (3)
Ni1—N4ii2.099 (3)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1W—HW12⋯O1iii0.819 (16)1.847 (18)2.661 (3)172 (3)
O1W—HW11⋯O40.83 (4)1.83 (4)2.651 (3)169 (3)

Symmetry code: (iii) .

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