metal-organic compounds
catena-Poly[[[(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-κ4N)nickel(II)]-μ-oxido-[dioxidotungstate(VI)]-μ-oxido] tetrahydrate]
aDepartment of Biology and Chemistry, Hunan University of Science and Engineering, Yongzhou Hunan 425100, People's Republic of China
*Correspondence e-mail: ouguangchuan@yahoo.com.cn
In the title compound, {[NiWO4(C16H36N4)]·4H2O}n, the NiII ion lies on an inversion center and is octahedrally coordinated by four N atoms of the tetradentate macrocyclic 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane (L) ligand in the equatorial plane and two O atoms of [WO4]2− anions in axial positions. Each [WO4]2− anion bridges two adjacent [NiL]2+ cations, forming a chain along [001]. The chains are further connected via N—H⋯O, O—H⋯O and C—H⋯O hydrogen-bonding interactions, generating a three-dimensional structure.
Experimental
Crystal data
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Refinement
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Data collection: SMART (Bruker, 1999); cell SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus; 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.
Supporting information
10.1107/S1600536812034538/pv2574sup1.cif
contains datablocks I, global. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536812034538/pv2574Isup2.hkl
A glass tube was charged with an aqueous solution of K2WO4 (0.033 g, 0.1 mmol) in water (20 ml), and a mixture of methanol and H2O (1/1, 20 ml) was gently added as an upper layer. A solution of NiL (ClO4)2 (0.054 g, 0.1 mmol) (L = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane) in methanol (20 ml) was added carefully as a third layer, and then the tube was sealed. After several weeks, yellow prism-shaped crystals were obtained.
The H atoms bound to N and C atoms were positioned geometrically and refined using the riding model with N—H = 0.93 Å and C—H = 0.98 to 1.00 Å. The hydrogen atoms of the water molecules were located from a difference Fourier map and were constrained at distances O—H = 0.86 (2) Å. Uiso(H) were set to 1.5 × Ueq(methyl C) and 1.2 × Ueq(the rest of the parent atoms).
Data collection: SMART (Bruker, 1999); cell
SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus (Bruker, 1999); 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 (Sheldrick, 2008).Fig. 1. The molecular structure of the title complex, with atom labels and 50% probability displacement ellipsoids for non-H atoms. Symmetry codes for the generated atoms: A: 2 - x, 2 - y, 1 - z; B: 2 - x, 2 - y, 2 - z. | |
Fig. 2. A view of the hydrogen bonds (dotted lines) in the crystal structure of the title compound. H atoms non-participating in hydrogen- bonding were omitted for clarity. | |
Fig. 3. Hydrogen bonding (dashed lines) in the title compound. Symmetry codes for the generated atoms: A: 1 - x, 1 - y, 1 - z; B: -1 + x, y, z; C: - x, 1 - y, 1 - z. |
[NiWO4(C16H36N4)]·4H2O | Z = 2 |
Mr = 663.11 | F(000) = 668 |
Triclinic, P1 | Dx = 1.737 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.8402 (14) Å | Cell parameters from 3766 reflections |
b = 11.7653 (18) Å | θ = 1.9–27.1° |
c = 13.931 (2) Å | µ = 5.32 mm−1 |
α = 107.163 (2)° | T = 173 K |
β = 102.529 (3)° | Prism, yellow |
γ = 104.984 (3)° | 0.31 × 0.11 × 0.02 mm |
V = 1268.1 (3) Å3 |
Bruker SMART CCD area-detector diffractometer | 5397 independent reflections |
Radiation source: fine-focus sealed tube | 4330 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
ϕ and ω scans | θmax = 27.1°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→4 |
Tmin = 0.289, Tmax = 0.901 | k = −14→15 |
7631 measured reflections | l = −17→17 |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.096 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0498P)2] where P = (Fo2 + 2Fc2)/3 |
5397 reflections | (Δ/σ)max = 0.001 |
304 parameters | Δρmax = 2.33 e Å−3 |
13 restraints | Δρmin = −1.48 e Å−3 |
[NiWO4(C16H36N4)]·4H2O | γ = 104.984 (3)° |
Mr = 663.11 | V = 1268.1 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 8.8402 (14) Å | Mo Kα radiation |
b = 11.7653 (18) Å | µ = 5.32 mm−1 |
c = 13.931 (2) Å | T = 173 K |
α = 107.163 (2)° | 0.31 × 0.11 × 0.02 mm |
β = 102.529 (3)° |
Bruker SMART CCD area-detector diffractometer | 5397 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 4330 reflections with I > 2σ(I) |
Tmin = 0.289, Tmax = 0.901 | Rint = 0.030 |
7631 measured reflections |
R[F2 > 2σ(F2)] = 0.038 | 13 restraints |
wR(F2) = 0.096 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | Δρmax = 2.33 e Å−3 |
5397 reflections | Δρmin = −1.48 e Å−3 |
304 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. |
x | y | z | Uiso*/Ueq | ||
W1 | 0.86432 (3) | 0.90496 (2) | 0.70182 (2) | 0.01423 (9) | |
O4 | 0.9085 (5) | 0.9844 (4) | 0.8399 (3) | 0.0187 (9) | |
O1 | 0.9900 (5) | 0.9988 (4) | 0.6505 (3) | 0.0201 (10) | |
O3 | 0.6535 (5) | 0.8719 (4) | 0.6342 (4) | 0.0231 (10) | |
O2 | 0.9049 (6) | 0.7611 (4) | 0.6806 (4) | 0.0258 (11) | |
Ni1 | 1.0000 | 1.0000 | 1.0000 | 0.0130 (2) | |
Ni2 | 1.0000 | 1.0000 | 0.5000 | 0.0139 (2) | |
N1 | 0.9427 (7) | 1.1622 (5) | 1.0653 (4) | 0.0170 (11) | |
H1C | 0.9860 | 1.1842 | 1.1380 | 0.020* | |
N2 | 1.2351 (6) | 1.1000 (5) | 1.0097 (4) | 0.0158 (11) | |
H2C | 1.3028 | 1.1227 | 1.0785 | 0.019* | |
N4 | 0.7426 (6) | 0.9212 (5) | 0.4386 (4) | 0.0183 (11) | |
H4D | 0.7043 | 0.9048 | 0.4920 | 0.022* | |
N3 | 1.0343 (7) | 0.8257 (5) | 0.4733 (4) | 0.0195 (12) | |
H3A | 1.0258 | 0.8088 | 0.5334 | 0.023* | |
C6 | 1.0127 (9) | 1.2828 (6) | 1.0490 (5) | 0.0219 (15) | |
C11 | 0.6783 (9) | 0.7997 (7) | 0.3458 (6) | 0.0298 (17) | |
H11 | 0.7226 | 0.8148 | 0.2887 | 0.036* | |
C5 | 1.1979 (9) | 1.3084 (6) | 1.0670 (6) | 0.0264 (16) | |
H5A | 1.2466 | 1.3084 | 1.1380 | 0.032* | |
H5B | 1.2477 | 1.3953 | 1.0694 | 0.032* | |
C9 | 1.2125 (8) | 0.8541 (7) | 0.4833 (6) | 0.0271 (16) | |
H9A | 1.2321 | 0.8652 | 0.4188 | 0.033* | |
H9B | 1.2474 | 0.7833 | 0.4922 | 0.033* | |
C10 | 0.6896 (9) | 1.0242 (7) | 0.4200 (6) | 0.0295 (17) | |
H10A | 0.5698 | 1.0036 | 0.4095 | 0.035* | |
H10B | 0.7109 | 1.0349 | 0.3558 | 0.035* | |
C14 | 0.9159 (9) | 0.7086 (6) | 0.3836 (6) | 0.0266 (16) | |
C16 | 0.9464 (10) | 0.7001 (7) | 0.2778 (6) | 0.0359 (19) | |
H16A | 0.9446 | 0.7773 | 0.2649 | 0.054* | |
H16B | 0.8597 | 0.6263 | 0.2204 | 0.054* | |
H16C | 1.0543 | 0.6912 | 0.2805 | 0.054* | |
C13 | 0.7386 (9) | 0.7023 (6) | 0.3763 (6) | 0.0313 (18) | |
H13A | 0.6640 | 0.6175 | 0.3245 | 0.038* | |
H13B | 0.7252 | 0.7078 | 0.4461 | 0.038* | |
C15 | 0.9397 (11) | 0.5905 (7) | 0.4055 (7) | 0.041 (2) | |
H15A | 0.8627 | 0.5129 | 0.3469 | 0.061* | |
H15B | 0.9180 | 0.5911 | 0.4717 | 0.061* | |
H15C | 1.0533 | 0.5934 | 0.4117 | 0.061* | |
C12 | 0.4873 (10) | 0.7496 (8) | 0.3017 (7) | 0.045 (2) | |
H12A | 0.4416 | 0.7344 | 0.3568 | 0.068* | |
H12B | 0.4495 | 0.6701 | 0.2403 | 0.068* | |
H12C | 0.4499 | 0.8125 | 0.2803 | 0.068* | |
C3 | 1.2531 (9) | 1.2195 (6) | 0.9881 (6) | 0.0256 (16) | |
H3 | 1.1785 | 1.1969 | 0.9150 | 0.031* | |
C8 | 0.9959 (10) | 1.3946 (6) | 1.1322 (6) | 0.0283 (16) | |
H8A | 0.8787 | 1.3813 | 1.1227 | 0.042* | |
H8B | 1.0477 | 1.4736 | 1.1233 | 0.042* | |
H8C | 1.0506 | 1.4000 | 1.2034 | 0.042* | |
C7 | 0.9231 (9) | 1.2735 (7) | 0.9384 (6) | 0.0298 (17) | |
H7A | 0.9179 | 1.1950 | 0.8854 | 0.045* | |
H7B | 0.9832 | 1.3464 | 0.9246 | 0.045* | |
H7C | 0.8109 | 1.2731 | 0.9343 | 0.045* | |
C4 | 1.4286 (10) | 1.2865 (8) | 0.9937 (8) | 0.051 (3) | |
H4A | 1.5007 | 1.3220 | 1.0674 | 0.077* | |
H4B | 1.4304 | 1.3550 | 0.9671 | 0.077* | |
H4C | 1.4677 | 1.2257 | 0.9504 | 0.077* | |
C1 | 0.7623 (8) | 1.1146 (6) | 1.0442 (5) | 0.0213 (14) | |
H1A | 0.7047 | 1.1009 | 0.9702 | 0.026* | |
H1B | 0.7301 | 1.1780 | 1.0919 | 0.026* | |
C2 | 1.2872 (8) | 1.0076 (6) | 0.9384 (5) | 0.0188 (14) | |
H2A | 1.4084 | 1.0407 | 0.9539 | 0.023* | |
H2B | 1.2336 | 0.9936 | 0.8636 | 0.023* | |
O2W | 0.3988 (7) | 0.6388 (5) | 0.5720 (5) | 0.0422 (14) | |
H2WA | 0.389 (10) | 0.589 (5) | 0.510 (3) | 0.051* | |
H2WB | 0.458 (9) | 0.714 (3) | 0.582 (5) | 0.051* | |
O4W | 0.5200 (7) | 0.9166 (6) | 0.8089 (4) | 0.0441 (15) | |
H4WB | 0.461 (7) | 0.842 (3) | 0.797 (4) | 0.053* | |
H4WA | 0.564 (9) | 0.915 (6) | 0.759 (5) | 0.053* | |
O1W | 0.6501 (8) | 0.5326 (5) | 0.6291 (5) | 0.0447 (15) | |
H1WA | 0.729 (5) | 0.599 (5) | 0.639 (7) | 0.054* | |
H1WB | 0.560 (4) | 0.547 (7) | 0.617 (7) | 0.054* | |
O3W | 0.2150 (7) | 0.7401 (6) | 0.6956 (5) | 0.0504 (17) | |
H3WA | 0.109 (3) | 0.714 (8) | 0.681 (5) | 0.061* | |
H3WB | 0.234 (7) | 0.706 (8) | 0.638 (3) | 0.061* |
U11 | U22 | U33 | U12 | U13 | U23 | |
W1 | 0.01641 (14) | 0.01438 (14) | 0.01496 (14) | 0.00471 (10) | 0.00913 (10) | 0.00725 (10) |
O4 | 0.021 (2) | 0.019 (2) | 0.017 (2) | 0.0070 (19) | 0.0074 (19) | 0.0073 (19) |
O1 | 0.014 (2) | 0.023 (2) | 0.021 (3) | 0.0006 (19) | 0.0067 (19) | 0.010 (2) |
O3 | 0.015 (2) | 0.028 (3) | 0.022 (3) | 0.003 (2) | 0.007 (2) | 0.004 (2) |
O2 | 0.029 (3) | 0.018 (2) | 0.034 (3) | 0.012 (2) | 0.010 (2) | 0.011 (2) |
Ni1 | 0.0154 (6) | 0.0136 (5) | 0.0142 (6) | 0.0060 (4) | 0.0092 (5) | 0.0070 (4) |
Ni2 | 0.0161 (6) | 0.0127 (5) | 0.0161 (6) | 0.0038 (4) | 0.0092 (5) | 0.0077 (4) |
N1 | 0.027 (3) | 0.016 (3) | 0.019 (3) | 0.011 (2) | 0.016 (2) | 0.012 (2) |
N2 | 0.020 (3) | 0.016 (3) | 0.017 (3) | 0.008 (2) | 0.009 (2) | 0.011 (2) |
N4 | 0.019 (3) | 0.021 (3) | 0.018 (3) | 0.006 (2) | 0.008 (2) | 0.010 (2) |
N3 | 0.023 (3) | 0.021 (3) | 0.021 (3) | 0.010 (2) | 0.010 (2) | 0.012 (2) |
C6 | 0.039 (4) | 0.015 (3) | 0.021 (4) | 0.016 (3) | 0.017 (3) | 0.010 (3) |
C11 | 0.020 (4) | 0.031 (4) | 0.029 (4) | −0.001 (3) | 0.007 (3) | 0.008 (3) |
C5 | 0.036 (4) | 0.016 (3) | 0.032 (4) | 0.008 (3) | 0.022 (3) | 0.010 (3) |
C9 | 0.024 (4) | 0.038 (4) | 0.030 (4) | 0.020 (3) | 0.013 (3) | 0.017 (3) |
C10 | 0.026 (4) | 0.032 (4) | 0.045 (5) | 0.015 (3) | 0.019 (4) | 0.023 (4) |
C14 | 0.042 (5) | 0.015 (3) | 0.024 (4) | 0.007 (3) | 0.020 (3) | 0.007 (3) |
C16 | 0.047 (5) | 0.029 (4) | 0.028 (4) | 0.010 (4) | 0.018 (4) | 0.005 (3) |
C13 | 0.042 (5) | 0.013 (3) | 0.029 (4) | −0.004 (3) | 0.012 (4) | 0.004 (3) |
C15 | 0.059 (6) | 0.018 (4) | 0.046 (5) | 0.013 (4) | 0.024 (4) | 0.010 (4) |
C12 | 0.038 (5) | 0.032 (5) | 0.045 (5) | 0.002 (4) | 0.001 (4) | 0.004 (4) |
C3 | 0.028 (4) | 0.017 (3) | 0.041 (5) | 0.009 (3) | 0.024 (3) | 0.015 (3) |
C8 | 0.044 (5) | 0.019 (4) | 0.032 (4) | 0.017 (3) | 0.021 (4) | 0.011 (3) |
C7 | 0.044 (5) | 0.032 (4) | 0.027 (4) | 0.021 (4) | 0.016 (4) | 0.020 (3) |
C4 | 0.039 (5) | 0.029 (5) | 0.098 (8) | 0.008 (4) | 0.041 (5) | 0.032 (5) |
C1 | 0.024 (4) | 0.021 (3) | 0.025 (4) | 0.012 (3) | 0.013 (3) | 0.010 (3) |
C2 | 0.016 (3) | 0.019 (3) | 0.025 (4) | 0.007 (3) | 0.015 (3) | 0.006 (3) |
O2W | 0.031 (3) | 0.029 (3) | 0.055 (4) | 0.001 (3) | 0.020 (3) | 0.003 (3) |
O4W | 0.027 (3) | 0.071 (4) | 0.029 (3) | 0.012 (3) | 0.015 (3) | 0.012 (3) |
O1W | 0.041 (3) | 0.027 (3) | 0.048 (4) | −0.003 (3) | 0.000 (3) | 0.011 (3) |
O3W | 0.032 (3) | 0.044 (4) | 0.060 (4) | 0.007 (3) | 0.025 (3) | −0.005 (3) |
W1—O1 | 1.772 (4) | C10—H10A | 0.9900 |
W1—O2 | 1.773 (4) | C10—H10B | 0.9900 |
W1—O4 | 1.775 (4) | C14—C13 | 1.529 (10) |
W1—O3 | 1.778 (4) | C14—C16 | 1.534 (9) |
O4—Ni1 | 2.135 (4) | C14—C15 | 1.563 (9) |
O1—Ni2 | 2.121 (4) | C16—H16A | 0.9800 |
Ni1—N2 | 2.059 (5) | C16—H16B | 0.9800 |
Ni1—N2i | 2.059 (5) | C16—H16C | 0.9800 |
Ni1—N1i | 2.098 (5) | C13—H13A | 0.9900 |
Ni1—N1 | 2.098 (5) | C13—H13B | 0.9900 |
Ni1—O4i | 2.135 (4) | C15—H15A | 0.9800 |
Ni2—N3ii | 2.087 (5) | C15—H15B | 0.9800 |
Ni2—N3 | 2.087 (5) | C15—H15C | 0.9800 |
Ni2—N4ii | 2.089 (5) | C12—H12A | 0.9800 |
Ni2—N4 | 2.089 (5) | C12—H12B | 0.9800 |
Ni2—O1ii | 2.121 (4) | C12—H12C | 0.9800 |
N1—C1 | 1.477 (8) | C3—C4 | 1.521 (10) |
N1—C6 | 1.498 (8) | C3—H3 | 1.0000 |
N1—H1C | 0.9300 | C8—H8A | 0.9800 |
N2—C2 | 1.484 (7) | C8—H8B | 0.9800 |
N2—C3 | 1.499 (8) | C8—H8C | 0.9800 |
N2—H2C | 0.9300 | C7—H7A | 0.9800 |
N4—C10 | 1.478 (8) | C7—H7B | 0.9800 |
N4—C11 | 1.486 (8) | C7—H7C | 0.9800 |
N4—H4D | 0.9300 | C4—H4A | 0.9800 |
N3—C9 | 1.490 (8) | C4—H4B | 0.9800 |
N3—C14 | 1.492 (8) | C4—H4C | 0.9800 |
N3—H3A | 0.9300 | C1—C2i | 1.498 (8) |
C6—C7 | 1.530 (9) | C1—H1A | 0.9900 |
C6—C5 | 1.535 (10) | C1—H1B | 0.9900 |
C6—C8 | 1.539 (9) | C2—C1i | 1.498 (8) |
C11—C13 | 1.511 (10) | C2—H2A | 0.9900 |
C11—C12 | 1.548 (10) | C2—H2B | 0.9900 |
C11—H11 | 1.0000 | O2W—H2WA | 0.85 (2) |
C5—C3 | 1.536 (9) | O2W—H2WB | 0.86 (2) |
C5—H5A | 0.9900 | O4W—H4WB | 0.845 (19) |
C5—H5B | 0.9900 | O4W—H4WA | 0.86 (2) |
C9—C10ii | 1.526 (10) | O1W—H1WA | 0.86 (2) |
C9—H9A | 0.9900 | O1W—H1WB | 0.85 (2) |
C9—H9B | 0.9900 | O3W—H3WA | 0.87 (2) |
C10—C9ii | 1.526 (10) | O3W—H3WB | 0.863 (19) |
O1—W1—O2 | 108.7 (2) | N3—C9—H9A | 110.2 |
O1—W1—O4 | 110.9 (2) | C10ii—C9—H9A | 110.2 |
O2—W1—O4 | 108.7 (2) | N3—C9—H9B | 110.2 |
O1—W1—O3 | 108.9 (2) | C10ii—C9—H9B | 110.2 |
O2—W1—O3 | 109.7 (2) | H9A—C9—H9B | 108.5 |
O4—W1—O3 | 109.9 (2) | N4—C10—C9ii | 108.0 (6) |
W1—O4—Ni1 | 151.1 (2) | N4—C10—H10A | 110.1 |
W1—O1—Ni2 | 137.9 (2) | C9ii—C10—H10A | 110.1 |
N2—Ni1—N2i | 180.000 (1) | N4—C10—H10B | 110.1 |
N2—Ni1—N1i | 85.46 (19) | C9ii—C10—H10B | 110.1 |
N2i—Ni1—N1i | 94.5 (2) | H10A—C10—H10B | 108.4 |
N2—Ni1—N1 | 94.5 (2) | N3—C14—C13 | 109.8 (5) |
N2i—Ni1—N1 | 85.46 (19) | N3—C14—C16 | 112.3 (6) |
N1i—Ni1—N1 | 180.000 (3) | C13—C14—C16 | 110.8 (6) |
N2—Ni1—O4 | 90.57 (18) | N3—C14—C15 | 108.7 (6) |
N2i—Ni1—O4 | 89.43 (18) | C13—C14—C15 | 108.1 (6) |
N1i—Ni1—O4 | 85.20 (18) | C16—C14—C15 | 106.9 (6) |
N1—Ni1—O4 | 94.80 (18) | C14—C16—H16A | 109.5 |
N2—Ni1—O4i | 89.43 (18) | C14—C16—H16B | 109.5 |
N2i—Ni1—O4i | 90.57 (18) | H16A—C16—H16B | 109.5 |
N1i—Ni1—O4i | 94.80 (18) | C14—C16—H16C | 109.5 |
N1—Ni1—O4i | 85.20 (18) | H16A—C16—H16C | 109.5 |
O4—Ni1—O4i | 180.000 (2) | H16B—C16—H16C | 109.5 |
N3ii—Ni2—N3 | 180.000 (2) | C11—C13—C14 | 118.9 (6) |
N3ii—Ni2—N4ii | 94.6 (2) | C11—C13—H13A | 107.6 |
N3—Ni2—N4ii | 85.4 (2) | C14—C13—H13A | 107.6 |
N3ii—Ni2—N4 | 85.4 (2) | C11—C13—H13B | 107.6 |
N3—Ni2—N4 | 94.6 (2) | C14—C13—H13B | 107.6 |
N4ii—Ni2—N4 | 180.000 (1) | H13A—C13—H13B | 107.0 |
N3ii—Ni2—O1ii | 86.13 (19) | C14—C15—H15A | 109.5 |
N3—Ni2—O1ii | 93.87 (19) | C14—C15—H15B | 109.5 |
N4ii—Ni2—O1ii | 90.23 (18) | H15A—C15—H15B | 109.5 |
N4—Ni2—O1ii | 89.77 (18) | C14—C15—H15C | 109.5 |
N3ii—Ni2—O1 | 93.87 (19) | H15A—C15—H15C | 109.5 |
N3—Ni2—O1 | 86.13 (19) | H15B—C15—H15C | 109.5 |
N4ii—Ni2—O1 | 89.77 (18) | C11—C12—H12A | 109.5 |
N4—Ni2—O1 | 90.23 (18) | C11—C12—H12B | 109.5 |
O1ii—Ni2—O1 | 180.000 (2) | H12A—C12—H12B | 109.5 |
C1—N1—C6 | 116.7 (5) | C11—C12—H12C | 109.5 |
C1—N1—Ni1 | 104.6 (4) | H12A—C12—H12C | 109.5 |
C6—N1—Ni1 | 122.1 (4) | H12B—C12—H12C | 109.5 |
C1—N1—H1C | 103.7 | N2—C3—C4 | 112.5 (6) |
C6—N1—H1C | 103.7 | N2—C3—C5 | 109.4 (5) |
Ni1—N1—H1C | 103.7 | C4—C3—C5 | 110.3 (6) |
C2—N2—C3 | 113.8 (5) | N2—C3—H3 | 108.2 |
C2—N2—Ni1 | 105.4 (4) | C4—C3—H3 | 108.2 |
C3—N2—Ni1 | 115.3 (4) | C5—C3—H3 | 108.2 |
C2—N2—H2C | 107.3 | C6—C8—H8A | 109.5 |
C3—N2—H2C | 107.3 | C6—C8—H8B | 109.5 |
Ni1—N2—H2C | 107.3 | H8A—C8—H8B | 109.5 |
C10—N4—C11 | 115.2 (5) | C6—C8—H8C | 109.5 |
C10—N4—Ni2 | 104.7 (4) | H8A—C8—H8C | 109.5 |
C11—N4—Ni2 | 114.5 (4) | H8B—C8—H8C | 109.5 |
C10—N4—H4D | 107.3 | C6—C7—H7A | 109.5 |
C11—N4—H4D | 107.3 | C6—C7—H7B | 109.5 |
Ni2—N4—H4D | 107.3 | H7A—C7—H7B | 109.5 |
C9—N3—C14 | 116.5 (5) | C6—C7—H7C | 109.5 |
C9—N3—Ni2 | 104.7 (4) | H7A—C7—H7C | 109.5 |
C14—N3—Ni2 | 121.3 (4) | H7B—C7—H7C | 109.5 |
C9—N3—H3A | 104.1 | C3—C4—H4A | 109.5 |
C14—N3—H3A | 104.1 | C3—C4—H4B | 109.5 |
Ni2—N3—H3A | 104.1 | H4A—C4—H4B | 109.5 |
N1—C6—C7 | 110.9 (6) | C3—C4—H4C | 109.5 |
N1—C6—C5 | 107.7 (5) | H4A—C4—H4C | 109.5 |
C7—C6—C5 | 111.8 (6) | H4B—C4—H4C | 109.5 |
N1—C6—C8 | 110.2 (5) | N1—C1—C2i | 109.7 (5) |
C7—C6—C8 | 108.9 (5) | N1—C1—H1A | 109.7 |
C5—C6—C8 | 107.4 (6) | C2i—C1—H1A | 109.7 |
N4—C11—C13 | 109.7 (6) | N1—C1—H1B | 109.7 |
N4—C11—C12 | 111.8 (6) | C2i—C1—H1B | 109.7 |
C13—C11—C12 | 110.3 (6) | H1A—C1—H1B | 108.2 |
N4—C11—H11 | 108.3 | N2—C2—C1i | 108.5 (5) |
C13—C11—H11 | 108.3 | N2—C2—H2A | 110.0 |
C12—C11—H11 | 108.3 | C1i—C2—H2A | 110.0 |
C6—C5—C3 | 119.3 (6) | N2—C2—H2B | 110.0 |
C6—C5—H5A | 107.5 | C1i—C2—H2B | 110.0 |
C3—C5—H5A | 107.5 | H2A—C2—H2B | 108.4 |
C6—C5—H5B | 107.5 | H2WA—O2W—H2WB | 109 (3) |
C3—C5—H5B | 107.5 | H4WB—O4W—H4WA | 109 (3) |
H5A—C5—H5B | 107.0 | H3WA—O3W—H3WB | 107 (3) |
N3—C9—C10ii | 107.7 (5) | ||
O1—W1—O4—Ni1 | −113.9 (5) | N4ii—Ni2—N3—C14 | −149.8 (5) |
O2—W1—O4—Ni1 | 5.5 (6) | N4—Ni2—N3—C14 | 30.2 (5) |
O3—W1—O4—Ni1 | 125.6 (5) | O1ii—Ni2—N3—C14 | −59.9 (5) |
O2—W1—O1—Ni2 | 73.4 (4) | O1—Ni2—N3—C14 | 120.1 (5) |
O4—W1—O1—Ni2 | −167.2 (3) | C1—N1—C6—C7 | −53.1 (7) |
O3—W1—O1—Ni2 | −46.1 (4) | Ni1—N1—C6—C7 | 77.3 (6) |
W1—O4—Ni1—N2 | 87.9 (5) | C1—N1—C6—C5 | −175.7 (5) |
W1—O4—Ni1—N2i | −92.1 (5) | Ni1—N1—C6—C5 | −45.2 (7) |
W1—O4—Ni1—N1i | 2.5 (5) | C1—N1—C6—C8 | 67.5 (7) |
W1—O4—Ni1—N1 | −177.5 (5) | Ni1—N1—C6—C8 | −162.1 (5) |
W1—O1—Ni2—N3ii | 117.7 (4) | C10—N4—C11—C13 | −178.8 (5) |
W1—O1—Ni2—N3 | −62.3 (4) | Ni2—N4—C11—C13 | 59.7 (6) |
W1—O1—Ni2—N4ii | −147.8 (4) | C10—N4—C11—C12 | −56.2 (8) |
W1—O1—Ni2—N4 | 32.2 (4) | Ni2—N4—C11—C12 | −177.7 (5) |
N2—Ni1—N1—C1 | 167.3 (4) | N1—C6—C5—C3 | 67.8 (7) |
N2i—Ni1—N1—C1 | −12.7 (4) | C7—C6—C5—C3 | −54.3 (8) |
O4—Ni1—N1—C1 | 76.4 (4) | C8—C6—C5—C3 | −173.6 (6) |
O4i—Ni1—N1—C1 | −103.6 (4) | C14—N3—C9—C10ii | −179.4 (5) |
N2—Ni1—N1—C6 | 32.0 (5) | Ni2—N3—C9—C10ii | 43.7 (6) |
N2i—Ni1—N1—C6 | −148.0 (5) | C11—N4—C10—C9ii | −171.2 (5) |
O4—Ni1—N1—C6 | −58.9 (5) | Ni2—N4—C10—C9ii | −44.5 (6) |
O4i—Ni1—N1—C6 | 121.1 (5) | C9—N3—C14—C13 | −172.9 (5) |
N1i—Ni1—N2—C2 | 16.8 (4) | Ni2—N3—C14—C13 | −43.5 (7) |
N1—Ni1—N2—C2 | −163.2 (4) | C9—N3—C14—C16 | −49.2 (8) |
O4—Ni1—N2—C2 | −68.4 (4) | Ni2—N3—C14—C16 | 80.2 (7) |
O4i—Ni1—N2—C2 | 111.6 (4) | C9—N3—C14—C15 | 69.0 (7) |
N1i—Ni1—N2—C3 | 143.2 (5) | Ni2—N3—C14—C15 | −161.6 (5) |
N1—Ni1—N2—C3 | −36.8 (5) | N4—C11—C13—C14 | −78.2 (8) |
O4—Ni1—N2—C3 | 58.0 (4) | C12—C11—C13—C14 | 158.4 (6) |
O4i—Ni1—N2—C3 | −122.0 (4) | N3—C14—C13—C11 | 66.9 (8) |
N3ii—Ni2—N4—C10 | 16.1 (4) | C16—C14—C13—C11 | −57.8 (8) |
N3—Ni2—N4—C10 | −163.9 (4) | C15—C14—C13—C11 | −174.6 (6) |
O1ii—Ni2—N4—C10 | −70.1 (4) | C2—N2—C3—C4 | −56.5 (8) |
O1—Ni2—N4—C10 | 109.9 (4) | Ni1—N2—C3—C4 | −178.5 (5) |
N3ii—Ni2—N4—C11 | 143.2 (5) | C2—N2—C3—C5 | −179.3 (5) |
N3—Ni2—N4—C11 | −36.8 (5) | Ni1—N2—C3—C5 | 58.7 (7) |
O1ii—Ni2—N4—C11 | 57.1 (4) | C6—C5—C3—N2 | −77.9 (8) |
O1—Ni2—N4—C11 | −122.9 (4) | C6—C5—C3—C4 | 157.9 (6) |
N4ii—Ni2—N3—C9 | −15.4 (4) | C6—N1—C1—C2i | 178.6 (5) |
N4—Ni2—N3—C9 | 164.6 (4) | Ni1—N1—C1—C2i | 40.5 (6) |
O1ii—Ni2—N3—C9 | 74.5 (4) | C3—N2—C2—C1i | −170.8 (6) |
O1—Ni2—N3—C9 | −105.5 (4) | Ni1—N2—C2—C1i | −43.5 (6) |
Symmetry codes: (i) −x+2, −y+2, −z+2; (ii) −x+2, −y+2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···O2i | 0.93 | 2.32 | 3.253 (7) | 180 |
N2—H2C···O4Wi | 0.93 | 2.21 | 3.040 (8) | 149 |
O4W—H4WB···O3W | 0.85 (2) | 2.12 (5) | 2.720 (8) | 128 (6) |
O4W—H4WA···O3 | 0.86 (2) | 2.05 (3) | 2.900 (7) | 168 (6) |
O2W—H2WA···O1Wiii | 0.85 (2) | 1.94 (2) | 2.790 (8) | 175 (7) |
O3W—H3WA···O2iv | 0.87 (2) | 2.01 (5) | 2.784 (7) | 148 (8) |
O1W—H1WA···O2 | 0.86 (2) | 1.95 (2) | 2.801 (7) | 172 (8) |
O2W—H2WB···O3 | 0.86 (2) | 1.99 (3) | 2.811 (7) | 160 (8) |
O3W—H3WB···O2W | 0.86 (2) | 2.08 (4) | 2.834 (8) | 145 (6) |
O1W—H1WB···O2W | 0.85 (2) | 2.10 (4) | 2.895 (9) | 157 (7) |
C16—H16A···O1ii | 0.98 | 2.40 | 3.241 (9) | 144 |
Symmetry codes: (i) −x+2, −y+2, −z+2; (ii) −x+2, −y+2, −z+1; (iii) −x+1, −y+1, −z+1; (iv) x−1, y, z. |
Experimental details
Crystal data | |
Chemical formula | [NiWO4(C16H36N4)]·4H2O |
Mr | 663.11 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 173 |
a, b, c (Å) | 8.8402 (14), 11.7653 (18), 13.931 (2) |
α, β, γ (°) | 107.163 (2), 102.529 (3), 104.984 (3) |
V (Å3) | 1268.1 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 5.32 |
Crystal size (mm) | 0.31 × 0.11 × 0.02 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.289, 0.901 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7631, 5397, 4330 |
Rint | 0.030 |
(sin θ/λ)max (Å−1) | 0.642 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.096, 1.02 |
No. of reflections | 5397 |
No. of parameters | 304 |
No. of restraints | 13 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 2.33, −1.48 |
Computer programs: SMART (Bruker, 1999), SAINT-Plus (Bruker, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···O2i | 0.93 | 2.32 | 3.253 (7) | 179.7 |
N2—H2C···O4Wi | 0.93 | 2.21 | 3.040 (8) | 149.0 |
O4W—H4WB···O3W | 0.845 (19) | 2.12 (5) | 2.720 (8) | 128 (6) |
O4W—H4WA···O3 | 0.86 (2) | 2.05 (3) | 2.900 (7) | 168 (6) |
O2W—H2WA···O1Wii | 0.85 (2) | 1.94 (2) | 2.790 (8) | 175 (7) |
O3W—H3WA···O2iii | 0.87 (2) | 2.01 (5) | 2.784 (7) | 148 (8) |
O1W—H1WA···O2 | 0.86 (2) | 1.95 (2) | 2.801 (7) | 172 (8) |
O2W—H2WB···O3 | 0.86 (2) | 1.99 (3) | 2.811 (7) | 160 (8) |
O3W—H3WB···O2W | 0.863 (19) | 2.08 (4) | 2.834 (8) | 145 (6) |
O1W—H1WB···O2W | 0.85 (2) | 2.10 (4) | 2.895 (9) | 157 (7) |
C16—H16A···O1iv | 0.98 | 2.40 | 3.241 (9) | 143.8 |
Symmetry codes: (i) −x+2, −y+2, −z+2; (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z; (iv) −x+2, −y+2, −z+1. |
Acknowledgements
The authors thank the Science and Technology Planning Project of Hunan Province (2012 F J3050, 2012 N K3067), the Construct Program of the Key Discipline in Hunan Province (2011–76) and the Science and Technology Innovative Research Team in Higher Educational Institutions of Hunan Province (2012–318) for financial support.
References
Bruker (1999). SMART and SAINT-Plus. Bruker AXS Inc, Madison, Wisconsin, USA. Google Scholar
Ou, G. C., Zou, L. S. & Yuan, Z. H. (2011). Z. Kristallogr. New Cryst. Struct. 226, 543–544. CAS Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
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Continuing our research (Ou et al., 2011), we now report the crystal structure of the title complex. The asymmetric unit of the title complex contains one cation [NiL]2+, one anion [WO4]2-, and four water molecules of hydration. Each NiII ion displays a distorted octahedral coordination geometry by coordination with four nitrogen atoms of L in in the equatorial plane, and two oxygen atoms of [WO4]2- anions in the axial positions. Each [WO4]2- anion bridges two adjacent [NiL]2+ cations to form a one-dimensional chain. The one-dimensional chains are further connected through O···O (2.720 (8)–2.900 (8) Å) and N···O (3.040 (8) and 3.253 (7) Å) hydrogen bonding interactions between the oxygen atoms of [WO4]2- anions, free water molecules and the secondary amine of [NiL]2+, forming a three-dimensional supramolecular structure (Tab. 2, Figs. 2, 3).