In the title coordination polymer, [Ni(C8H4O4)(C4H10N2)]n, the Ni(II) atom is situated on a C2 axis and is six-coordinated by two N atoms from two piperazine (pip) molecules, four O atoms from two bidentate and chelating terephthalate (tp) anions, forming a distorted octahedron. Both pip and tp molecules, which are centrosymmetric, bridge adjacent Ni(II) atoms, forming a three-dimensional network.
Supporting information
CCDC reference: 642968
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C)= 0.003 Å
- R factor = 0.027
- wR factor = 0.075
- Data-to-parameter ratio = 22.1
checkCIF/PLATON results
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Data collection: Collect Software (Nonius, 1998); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR2002 (Burla et al., 2003); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP for Windows (Farrugia, 1997) and
CaRIne Crystallography (Boudias & Monceau, 1989); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).
Crystal data top
C12H14N2NiO4 | F(000) = 640 |
Mr = 308.96 | Dx = 1.621 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 2043 reflections |
a = 19.110 (9) Å | θ = 0.4–26.7° |
b = 6.814 (4) Å | µ = 1.54 mm−1 |
c = 10.319 (5) Å | T = 298 K |
β = 109.61 (1)° | Plate, green |
V = 1265.8 (11) Å3 | 0.15 × 0.11 × 0.07 mm |
Z = 4 | |
Data collection top
Nonius Model? Diffractometer | 1919 independent reflections |
Radiation source: fine-focus sealed tube | 1682 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.051 |
CCD scans | θmax = 30.5°, θmin = 3.2° |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | h = 1→27 |
Tmin = 0.80, Tmax = 0.90 | k = 0→9 |
14181 measured reflections | l = −14→13 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.075 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0247P)2 + 1.5176P] where P = (Fo2 + 2Fc2)/3 |
1919 reflections | (Δ/σ)max < 0.001 |
87 parameters | Δρmax = 0.38 e Å−3 |
0 restraints | Δρmin = −0.49 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni1 | 0.0000 | 0.15182 (4) | 0.7500 | 0.01553 (10) | |
N2 | −0.00287 (8) | 0.3333 (2) | 0.90851 (14) | 0.0173 (3) | |
H2 | −0.0234 | 0.2565 | 0.9583 | 0.021* | |
O4 | −0.11030 (7) | 0.0922 (2) | 0.71243 (14) | 0.0270 (3) | |
O5 | −0.05640 (7) | −0.07574 (19) | 0.59159 (13) | 0.0242 (3) | |
C3 | −0.18409 (9) | −0.1479 (2) | 0.55928 (18) | 0.0195 (3) | |
C6 | −0.11281 (9) | −0.0383 (2) | 0.62415 (17) | 0.0190 (3) | |
C7 | 0.06797 (10) | 0.3998 (3) | 1.01166 (18) | 0.0226 (4) | |
H7A | 0.0924 | 0.4912 | 0.9687 | 0.027* | |
H7B | 0.1006 | 0.2878 | 1.0436 | 0.027* | |
C8 | −0.05515 (10) | 0.5016 (3) | 0.86644 (17) | 0.0206 (3) | |
H8A | −0.1023 | 0.4555 | 0.8033 | 0.025* | |
H8B | −0.0354 | 0.5971 | 0.8182 | 0.025* | |
C9 | −0.20301 (10) | −0.2158 (3) | 0.42510 (18) | 0.0232 (4) | |
H9 | −0.1717 | −0.1919 | 0.3747 | 0.028* | |
C10 | −0.23155 (10) | −0.1809 (3) | 0.63395 (19) | 0.0252 (4) | |
H10 | −0.2194 | −0.1337 | 0.7234 | 0.030* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.01490 (15) | 0.01485 (16) | 0.01648 (16) | 0.000 | 0.00483 (11) | 0.000 |
N2 | 0.0192 (7) | 0.0173 (7) | 0.0151 (7) | −0.0004 (5) | 0.0055 (5) | −0.0016 (5) |
O4 | 0.0208 (6) | 0.0305 (7) | 0.0312 (7) | −0.0080 (5) | 0.0106 (5) | −0.0149 (6) |
O5 | 0.0188 (6) | 0.0248 (7) | 0.0295 (7) | −0.0037 (5) | 0.0090 (5) | −0.0099 (5) |
C3 | 0.0165 (8) | 0.0196 (8) | 0.0218 (8) | −0.0024 (6) | 0.0056 (6) | −0.0035 (6) |
C6 | 0.0174 (8) | 0.0197 (8) | 0.0192 (8) | −0.0042 (6) | 0.0053 (6) | −0.0030 (6) |
C7 | 0.0183 (8) | 0.0261 (9) | 0.0218 (8) | 0.0005 (7) | 0.0046 (7) | −0.0055 (7) |
C8 | 0.0216 (8) | 0.0207 (8) | 0.0166 (7) | 0.0010 (7) | 0.0028 (7) | −0.0020 (6) |
C9 | 0.0203 (8) | 0.0281 (9) | 0.0240 (8) | −0.0064 (7) | 0.0112 (7) | −0.0044 (7) |
C10 | 0.0223 (8) | 0.0337 (10) | 0.0201 (9) | −0.0074 (7) | 0.0079 (7) | −0.0085 (7) |
Geometric parameters (Å, º) top
Ni1—O4i | 2.0519 (16) | C3—C10 | 1.391 (2) |
Ni1—O4 | 2.0519 (16) | C3—C6 | 1.500 (2) |
Ni1—N2 | 2.0659 (16) | C7—C8ii | 1.517 (2) |
Ni1—O5 | 2.2484 (15) | C7—H7A | 0.9700 |
Ni1—C6 | 2.4765 (19) | C7—H7B | 0.9700 |
N2—C7 | 1.484 (2) | C8—H8A | 0.9700 |
N2—C8 | 1.487 (2) | C8—H8B | 0.9700 |
N2—H2 | 0.9100 | C9—C10iii | 1.385 (3) |
O4—C6 | 1.262 (2) | C9—H9 | 0.9300 |
O5—C6 | 1.258 (2) | C10—H10 | 0.9300 |
C3—C9 | 1.388 (2) | | |
| | | |
O4i—Ni1—O4 | 157.15 (8) | C10—C3—C6 | 119.77 (16) |
O4i—Ni1—N2 | 105.52 (6) | O5—C6—O4 | 120.47 (15) |
O4—Ni1—N2 | 88.26 (6) | O5—C6—C3 | 120.74 (15) |
N2—Ni1—N2i | 106.46 (9) | O4—C6—C3 | 118.79 (15) |
O4i—Ni1—O5 | 102.25 (6) | O5—C6—Ni1 | 64.72 (9) |
O4—Ni1—O5 | 60.97 (5) | O4—C6—Ni1 | 55.78 (9) |
N2—Ni1—O5 | 148.74 (5) | C3—C6—Ni1 | 174.23 (12) |
N2—Ni1—O5i | 88.33 (7) | N2—C7—C8ii | 111.57 (15) |
O5—Ni1—O5i | 92.80 (8) | N2—C7—H7A | 109.3 |
O4i—Ni1—C6 | 130.83 (6) | C8ii—C7—H7A | 109.3 |
O4—Ni1—C6 | 30.58 (5) | N2—C7—H7B | 109.3 |
N2—Ni1—C6 | 118.59 (6) | C8ii—C7—H7B | 109.3 |
N2i—Ni1—C6 | 98.49 (6) | H7A—C7—H7B | 108.0 |
O5—Ni1—C6 | 30.40 (5) | N2—C8—C7ii | 112.29 (14) |
O5i—Ni1—C6 | 98.11 (6) | N2—C8—H8A | 109.1 |
C6—Ni1—C6i | 116.92 (9) | C7ii—C8—H8A | 109.1 |
C7—N2—C8 | 109.62 (13) | N2—C8—H8B | 109.1 |
C7—N2—Ni1 | 119.36 (11) | C7ii—C8—H8B | 109.1 |
C8—N2—Ni1 | 115.11 (10) | H8A—C8—H8B | 107.9 |
C7—N2—H2 | 103.5 | C10iii—C9—C3 | 120.18 (16) |
C8—N2—H2 | 103.5 | C10iii—C9—H9 | 119.9 |
Ni1—N2—H2 | 103.5 | C3—C9—H9 | 119.9 |
C6—O4—Ni1 | 93.65 (10) | C9iii—C10—C3 | 119.90 (16) |
C6—O5—Ni1 | 84.87 (10) | C9iii—C10—H10 | 120.0 |
C9—C3—C10 | 119.91 (16) | C3—C10—H10 | 120.0 |
C9—C3—C6 | 120.33 (15) | | |
Symmetry codes: (i) −x, y, −z+3/2; (ii) −x, −y+1, −z+2; (iii) −x−1/2, −y−1/2, −z+1. |