Literature DB >> 22346891

The chain structure of [Ni(C(4)H(2)O(4))(C(12)H(8)N(2))(H(2)O)](n) with different types of fumarate bridging.

Anna Uhrinová1, Juraj Kuchár, Juraj Cernák.   

Abstract

Using modified solvothermal conditions (longer cooling time), beside previously characterized dark-green crystals of [Ni(C(4)H(2)O(4))(C(12)n class="Species">H(8)N(2))] (main product), a few light-green crystals of the polymeric title compound, catena-poly[[aqua-(1,10-phenanthroline-κ(2)N,N')nickel(II)]-μ-fumarato-κ(2)O:O'-[aqua-(1,10-phenanthroline-κ(2)N,N')nickel(II)]-μ-fumarato-κ(4)O,O':O'',O'''], [Ni(C(4)H(2)O(4))(C(12)H(8)N(2))(H(2)O)](n) were isolated. Its crystal structure is made up from zigzag chains, propagating in [001], in which the Ni(2+) ions are linked alternatively by μ(2)-fumarato and bis-chelating fumarato bridging ligands. The Ni(2+) ion is coordinated in a deformed octa-hedral geometry by one chelating 1,10-phenanthroline ligand, one aqua ligand in a cis position with regard to both N-donor atoms and by two different fumarato ligands, each residing with its central C=C bond on an inversion centre, occupying the remaining coordination sites in a fac fashion. The chains thus formed are linked by O-H⋯O hydrogen bonds and π-π inter-actions between the aromatic rings of the phenanthroline ligands with a shortest ring centroid separation of 3.4787 (10) Å.

Entities:  

Year:  2012        PMID： 22346891      PMCID： PMC3274842          DOI： 10.1107/S1600536811054614

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


Related literature

For Ni2+ complexes containing both n class="Chemical">fum and phen ligands (fum = fumarato, phen = 1,10-phenanthroline), see: Černák et al. (2009 ▶) for [Ni(fum)(phen)] with a two-dimensional structure and Ma et al. (2003 ▶) for [Ni2(phen)4(fum)(H2O)2]fum·16H2O with an ionic structure containing a dinuclear complex cation. For an Ni2+ complex, [Ni2(fum)2(py)6]·2py (py = pyridine), exhibiting a one-dimensional structure with the same type of fumarato bridging ligands, see: Mori et al. (2004 ▶); Marsh et al. (2005 ▶).

Experimental

Crystal data

[Ni(C4H2O4)(C12n class="Species">H8N2)(H2O)] M = 370.99 Triclinic, a = 7.8998 (4) Å b = 9.8238 (5) Å c = 11.3815 (8) Å α = 68.677 (6)° β = 70.141 (6)° γ = 89.655 (5)° V = 766.89 (8) Å3 Z = 2 Mo Kα radiation μ = 1.29 mm−1 T = 173 K 0.46 × 0.27 × 0.12 mm

Data collection

Oxford Diffraction Xcalibur Sapphire2 diffractometer Absorption correction: analytical [Clark & Reid (1995 ▶) in CrysAlis PRO (Oxford Diffraction, 2009 ▶)] T min = 0.658, T max = 0.866 12619 measured reflections 3173 independent reflections 2972 reflections with I > 2σ(I) R int = 0.022

Refinement

R[F 2 > 2σ(F 2)] = 0.022 wR(F 2) = 0.057 S = 1.04 3173 reflections 217 parameters H-atom parameters constrained Δρmax = 0.33 e Å−3 Δρmin = −0.25 e Å−3 Data collection: CrysAlis PRO (Oxford Diffraction, 2009 ▶); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Crystal Impact, 2009 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811054614/wm2574sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811054614/wm2574Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ni(C4H2O4)(C12H8N2)(H2O)]Z = 2
Mr = 370.99F(000) = 380
Triclinic, P1Dx = 1.607 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.8998 (4) ÅCell parameters from 9394 reflections
b = 9.8238 (5) Åθ = 3.3–29.4°
c = 11.3815 (8) ŵ = 1.29 mm−1
α = 68.677 (6)°T = 173 K
β = 70.141 (6)°Prism, light-green
γ = 89.655 (5)°0.46 × 0.27 × 0.12 mm
V = 766.89 (8) Å3
Oxford Diffraction Xcalibur Sapphire2 diffractometer3173 independent reflections
Radiation source: Enhance (Mo) X-ray Source2972 reflections with I > 2σ(I)
graphiteRint = 0.022
Detector resolution: 8.3438 pixels mm-1θmax = 26.5°, θmin = 3.3°
ω scansh = −9→9
Absorption correction: analytical [Clark & Reid (1995) in CrysAlis PRO (Oxford Diffraction, 2009)]k = −12→12
Tmin = 0.658, Tmax = 0.866l = −14→14
12619 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.022Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.057H-atom parameters constrained
S = 1.04w = 1/[σ2(Fo2) + (0.0268P)2 + 0.3218P] where P = (Fo2 + 2Fc2)/3
3173 reflections(Δ/σ)max = 0.001
217 parametersΔρmax = 0.33 e Å−3
0 restraintsΔρmin = −0.24 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.
xyzUiso*/Ueq
Ni10.83574 (2)0.255869 (19)0.208342 (18)0.02046 (7)
O11.05052 (14)0.37310 (12)0.20856 (11)0.0254 (2)
H1O10.99460.42260.25390.038*
H2O11.10600.43100.12680.038*
O20.77961 (14)0.43278 (11)0.05893 (11)0.0246 (2)
O30.60066 (15)0.22129 (11)0.15882 (11)0.0256 (2)
O40.65578 (15)0.30773 (12)0.35633 (11)0.0297 (2)
O50.82308 (16)0.48624 (13)0.36300 (12)0.0351 (3)
N10.85113 (17)0.05252 (14)0.34101 (12)0.0240 (3)
N21.02443 (17)0.18287 (13)0.07328 (12)0.0215 (3)
C10.7599 (2)−0.01127 (18)0.47314 (16)0.0311 (4)
H10.67070.03850.51530.037*
C20.7899 (3)−0.1492 (2)0.55307 (17)0.0373 (4)
H20.7221−0.19160.64760.045*
C30.9174 (3)−0.22201 (19)0.49376 (18)0.0370 (4)
H30.9389−0.31550.54690.044*
C41.1536 (3)−0.22521 (19)0.28194 (19)0.0375 (4)
H41.1810−0.31870.33000.045*
C51.2444 (2)−0.15787 (19)0.14727 (19)0.0351 (4)
H51.3352−0.20460.10260.042*
C61.2939 (2)0.05748 (19)−0.07064 (18)0.0321 (4)
H61.38500.0156−0.12090.039*
C71.2463 (2)0.19111 (18)−0.13455 (16)0.0311 (4)
H71.30510.2431−0.22940.037*
C81.1105 (2)0.25035 (17)−0.05917 (15)0.0263 (3)
H81.07860.3429−0.10480.032*
C91.0168 (2)−0.15825 (17)0.35373 (17)0.0291 (3)
C100.9774 (2)−0.01967 (16)0.28145 (15)0.0228 (3)
C111.2066 (2)−0.01704 (17)0.07015 (17)0.0271 (3)
C121.0727 (2)0.05085 (16)0.13778 (15)0.0221 (3)
C130.6336 (2)0.35570 (16)0.08395 (14)0.0219 (3)
C140.4973 (2)0.42762 (17)0.02642 (16)0.0249 (3)
H140.40640.36450.03400.030*
C150.6762 (2)0.41233 (16)0.39247 (15)0.0247 (3)
C160.5037 (2)0.44635 (18)0.47800 (16)0.0280 (3)
H160.40000.38930.49870.034*
U11U22U33U12U13U23
Ni10.01891 (11)0.02183 (11)0.01896 (10)0.00744 (7)−0.00459 (8)−0.00816 (8)
O10.0204 (6)0.0307 (6)0.0219 (5)0.0058 (4)−0.0051 (4)−0.0091 (4)
O20.0189 (6)0.0254 (5)0.0260 (5)0.0056 (4)−0.0082 (5)−0.0062 (4)
O30.0252 (6)0.0218 (5)0.0281 (6)0.0065 (4)−0.0082 (5)−0.0093 (4)
O40.0258 (6)0.0322 (6)0.0296 (6)0.0048 (5)−0.0008 (5)−0.0186 (5)
O50.0254 (6)0.0413 (7)0.0394 (7)0.0038 (5)−0.0029 (5)−0.0247 (6)
N10.0222 (7)0.0256 (6)0.0207 (6)0.0043 (5)−0.0059 (5)−0.0068 (5)
N20.0209 (7)0.0216 (6)0.0208 (6)0.0059 (5)−0.0059 (5)−0.0082 (5)
C10.0282 (9)0.0358 (9)0.0236 (8)0.0030 (7)−0.0054 (7)−0.0088 (7)
C20.0402 (11)0.0378 (9)0.0226 (8)−0.0031 (8)−0.0091 (8)−0.0011 (7)
C30.0461 (11)0.0285 (8)0.0326 (9)0.0039 (8)−0.0212 (9)−0.0012 (7)
C40.0444 (11)0.0270 (8)0.0482 (11)0.0179 (8)−0.0262 (9)−0.0139 (8)
C50.0329 (10)0.0330 (9)0.0480 (10)0.0185 (7)−0.0175 (8)−0.0226 (8)
C60.0255 (9)0.0365 (9)0.0368 (9)0.0070 (7)−0.0043 (7)−0.0233 (8)
C70.0297 (9)0.0340 (9)0.0235 (8)0.0004 (7)−0.0006 (7)−0.0126 (7)
C80.0288 (9)0.0247 (7)0.0224 (7)0.0040 (6)−0.0069 (7)−0.0079 (6)
C90.0323 (9)0.0249 (7)0.0327 (8)0.0061 (7)−0.0182 (7)−0.0078 (7)
C100.0219 (8)0.0222 (7)0.0249 (7)0.0043 (6)−0.0104 (6)−0.0080 (6)
C110.0233 (8)0.0280 (8)0.0348 (8)0.0077 (6)−0.0108 (7)−0.0172 (7)
C120.0201 (8)0.0226 (7)0.0257 (7)0.0049 (6)−0.0090 (6)−0.0111 (6)
C130.0202 (8)0.0246 (7)0.0204 (7)0.0080 (6)−0.0047 (6)−0.0106 (6)
C140.0177 (8)0.0291 (7)0.0283 (8)0.0061 (6)−0.0079 (6)−0.0119 (6)
C150.0263 (8)0.0258 (7)0.0193 (7)0.0080 (6)−0.0049 (6)−0.0090 (6)
C160.0223 (8)0.0322 (8)0.0260 (8)0.0036 (6)−0.0016 (7)−0.0140 (7)
Ni1—O42.0263 (10)C3—H30.9500
Ni1—N12.0527 (12)C4—C51.350 (3)
Ni1—O12.0576 (11)C4—C91.432 (2)
Ni1—N22.0811 (12)C4—H40.9500
Ni1—O22.1124 (10)C5—C111.436 (2)
Ni1—O32.1771 (11)C5—H50.9500
O1—H1O10.8500C6—C71.371 (2)
O1—H2O10.8500C6—C111.408 (2)
O2—C131.2711 (18)C6—H60.9500
O3—C131.2540 (18)C7—C81.398 (2)
O4—C151.2671 (18)C7—H70.9500
O5—C151.2470 (19)C8—H80.9500
N1—C11.326 (2)C9—C101.408 (2)
N1—C101.3563 (19)C10—C121.438 (2)
N2—C81.3253 (19)C11—C121.403 (2)
N2—C121.3631 (19)C13—C141.490 (2)
C1—C21.402 (2)C14—C14i1.322 (3)
C1—H10.9500C14—H140.9127
C2—C31.365 (3)C15—C161.498 (2)
C2—H20.9500C16—C16ii1.315 (3)
C3—C91.407 (2)C16—H160.9056
O4—Ni1—N193.22 (5)C5—C4—C9121.22 (15)
O4—Ni1—O192.07 (4)C5—C4—H4119.4
N1—Ni1—O198.29 (5)C9—C4—H4119.4
O4—Ni1—N2173.69 (5)C4—C5—C11121.40 (15)
N1—Ni1—N280.59 (5)C4—C5—H5119.3
O1—Ni1—N287.68 (5)C11—C5—H5119.3
O4—Ni1—O290.64 (4)C7—C6—C11119.38 (14)
N1—Ni1—O2165.34 (5)C7—C6—H6120.3
O1—Ni1—O295.70 (4)C11—C6—H6120.3
N2—Ni1—O295.66 (4)C6—C7—C8119.52 (15)
O4—Ni1—O384.64 (4)C6—C7—H7120.2
N1—Ni1—O3104.64 (5)C8—C7—H7120.2
O1—Ni1—O3156.97 (4)N2—C8—C7122.79 (14)
N2—Ni1—O398.02 (4)N2—C8—H8118.6
O2—Ni1—O361.64 (4)C7—C8—H8118.6
O4—Ni1—C1384.46 (5)C3—C9—C10116.94 (15)
N1—Ni1—C13135.31 (5)C3—C9—C4124.20 (15)
O1—Ni1—C13126.36 (5)C10—C9—C4118.86 (15)
N2—Ni1—C13100.76 (5)N1—C10—C9122.99 (14)
O2—Ni1—C1331.19 (4)N1—C10—C12117.23 (13)
O3—Ni1—C1330.68 (4)C9—C10—C12119.78 (14)
Ni1—O1—H1O1100.8C12—C11—C6117.24 (14)
Ni1—O1—H2O1106.0C12—C11—C5118.60 (15)
H1O1—O1—H2O1109.3C6—C11—C5124.15 (15)
C13—O2—Ni189.42 (8)N2—C12—C11123.04 (14)
C13—O3—Ni186.97 (9)N2—C12—C10116.83 (13)
C15—O4—Ni1127.93 (10)C11—C12—C10120.13 (13)
C1—N1—C10118.30 (13)O3—C13—O2121.07 (13)
C1—N1—Ni1128.64 (11)O3—C13—C14119.63 (13)
C10—N1—Ni1113.02 (10)O2—C13—C14119.28 (13)
C8—N2—C12118.02 (13)O3—C13—Ni162.35 (8)
C8—N2—Ni1129.72 (10)O2—C13—Ni159.39 (7)
C12—N2—Ni1112.00 (10)C14—C13—Ni1170.01 (10)
N1—C1—C2122.60 (16)C14i—C14—C13122.62 (18)
N1—C1—H1118.7C14i—C14—H14122.2
C2—C1—H1118.7C13—C14—H14115.2
C3—C2—C1119.33 (16)O5—C15—O4126.05 (14)
C3—C2—H2120.3O5—C15—C16119.26 (13)
C1—C2—H2120.3O4—C15—C16114.68 (14)
C2—C3—C9119.83 (15)C16ii—C16—C15123.7 (2)
C2—C3—H3120.1C16ii—C16—H16119.5
C9—C3—H3120.1C15—C16—H16116.8
O4—Ni1—O2—C13−78.18 (8)C2—C3—C9—C4179.82 (16)
N1—Ni1—O2—C1327.1 (2)C5—C4—C9—C3−179.90 (17)
O1—Ni1—O2—C13−170.32 (8)C5—C4—C9—C100.0 (2)
N2—Ni1—O2—C13101.46 (8)C1—N1—C10—C9−0.6 (2)
O3—Ni1—O2—C135.38 (8)Ni1—N1—C10—C9177.36 (12)
O4—Ni1—O3—C1388.17 (9)C1—N1—C10—C12179.14 (14)
N1—Ni1—O3—C13−179.90 (8)Ni1—N1—C10—C12−2.93 (16)
O1—Ni1—O3—C135.53 (15)C3—C9—C10—N10.4 (2)
N2—Ni1—O3—C13−97.59 (9)C4—C9—C10—N1−179.51 (14)
O2—Ni1—O3—C13−5.46 (8)C3—C9—C10—C12−179.28 (14)
N1—Ni1—O4—C15117.90 (13)C4—C9—C10—C120.8 (2)
O1—Ni1—O4—C1519.47 (13)C7—C6—C11—C120.4 (2)
O2—Ni1—O4—C15−76.25 (13)C7—C6—C11—C5179.43 (15)
O3—Ni1—O4—C15−137.69 (13)C4—C5—C11—C120.3 (2)
C13—Ni1—O4—C15−106.87 (13)C4—C5—C11—C6−178.73 (17)
O4—Ni1—N1—C13.18 (14)C8—N2—C12—C11−0.9 (2)
O1—Ni1—N1—C195.75 (14)Ni1—N2—C12—C11−175.67 (11)
N2—Ni1—N1—C1−178.02 (14)C8—N2—C12—C10179.84 (13)
O2—Ni1—N1—C1−101.8 (2)Ni1—N2—C12—C105.10 (16)
O3—Ni1—N1—C1−82.11 (14)C6—C11—C12—N20.4 (2)
C13—Ni1—N1—C1−82.18 (15)C5—C11—C12—N2−178.66 (14)
O4—Ni1—N1—C10−174.48 (10)C6—C11—C12—C10179.62 (14)
O1—Ni1—N1—C10−81.92 (10)C5—C11—C12—C100.6 (2)
N2—Ni1—N1—C104.31 (10)N1—C10—C12—N2−1.5 (2)
O2—Ni1—N1—C1080.5 (2)C9—C10—C12—N2178.18 (13)
O3—Ni1—N1—C10100.22 (10)N1—C10—C12—C11179.20 (13)
C13—Ni1—N1—C10100.15 (11)C9—C10—C12—C11−1.1 (2)
N1—Ni1—N2—C8−179.04 (14)Ni1—O3—C13—O29.36 (13)
O1—Ni1—N2—C8−80.24 (14)Ni1—O3—C13—C14−168.84 (12)
O2—Ni1—N2—C815.26 (14)Ni1—O2—C13—O3−9.63 (14)
O3—Ni1—N2—C877.35 (14)Ni1—O2—C13—C14168.57 (12)
C13—Ni1—N2—C846.36 (14)O4—Ni1—C13—O3−88.83 (8)
N1—Ni1—N2—C12−5.08 (10)N1—Ni1—C13—O30.14 (11)
O1—Ni1—N2—C1293.73 (10)O1—Ni1—C13—O3−177.32 (7)
O2—Ni1—N2—C12−170.78 (10)N2—Ni1—C13—O387.59 (9)
O3—Ni1—N2—C12−108.69 (10)O2—Ni1—C13—O3170.69 (13)
C13—Ni1—N2—C12−139.67 (10)O4—Ni1—C13—O2100.48 (8)
C10—N1—C1—C20.4 (2)N1—Ni1—C13—O2−170.55 (8)
Ni1—N1—C1—C2−177.15 (12)O1—Ni1—C13—O211.99 (10)
N1—C1—C2—C3−0.1 (3)N2—Ni1—C13—O2−83.10 (8)
C1—C2—C3—C90.0 (3)O3—Ni1—C13—O2−170.69 (13)
C9—C4—C5—C11−0.6 (3)O3—C13—C14—C14i164.10 (18)
C11—C6—C7—C8−0.7 (2)O2—C13—C14—C14i−14.1 (3)
C12—N2—C8—C70.6 (2)Ni1—O4—C15—O5−15.4 (2)
Ni1—N2—C8—C7174.28 (11)Ni1—O4—C15—C16164.36 (10)
C6—C7—C8—N20.2 (2)O5—C15—C16—C16ii1.9 (3)
C2—C3—C9—C10−0.1 (2)O4—C15—C16—C16ii−177.9 (2)
D—H···AD—HH···AD···AD—H···A
O1—H1O1···O50.851.782.6085 (15)163
O1—H2O1···O2iii0.851.932.7820 (15)177
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1—H1O1⋯O50.851.782.6085 (15)163
O1—H2O1⋯O2i0.851.932.7820 (15)177

Symmetry code: (i) .

  2 in total

1.  Space group P1: an update.

Authors:  Richard E Marsh
Journal:  Acta Crystallogr B       Date:  2005-05-13

2.  A short history of SHELX.

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

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