Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807048684/cv2311sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807048684/cv2311Isup2.hkl |
CCDC reference: 667222
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.005 Å
- R factor = 0.044
- wR factor = 0.108
- Data-to-parameter ratio = 15.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.60 Ratio
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Ni1 (2) 2.06
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
Nickel chloride hexahydrate (5 mmol, 1189 mg) in absolute ethanol (15 ml) was added dropwise to an absolute ethanol solution (20 ml) of P-dimethylaminobenzaldehyde (10 mmol, 1492 mg). The mixture was heated under reflux with stirring for 4 h. The solution was kept at room temperature for three weeks, after which large green block-shaped crystals of the title complex suitable for X-ray diffraction analysis were obtained.
All H-atoms were positioned geometrically (C—H 0.93–0.96 Å, O—H 0.85 Å) and refined using a riding model, with Uiso = 1.2–1.5Ueq(parent atom).
Nickel is vital for organism as a trace element. It often acts as a component or secondary factor of enzyme. In the last two decades, biological inorganic chemistry of nickel has became one of the hottest fields and the coordination chemistry of nickel has made a great progress (Jiang et al., 2003). We report here the synthesis and crystal structure of the title compound, a new nickel(II) complex.
The title complex (Fig.1) consists of cations [Ni(C9H11NO)2(H2O)3Cl]+ and non-coordinating chloride anions. The NiII ion is six-coordinated by one Cl atom, two O atoms of 4-dimethylaminobenzaldehyde molecules and three water molecules in a distorted octahedral geometry.
In the crystal, the intermolecular O—H···Cl hydrogen bonds (Table 1) link cations and anions into two-dimensional sheets parallel to ab plane with the up and down protruding ligands.
For general background, see: Jiang et al. (2003).
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL (Sheldrick, 1997b).
Fig. 1. The structure of the title complex, showing 30% probability displacement ellipsoids and the atom-numbering scheme. |
[NiCl(C9H11NO)2(H2O)3]Cl | F(000) = 1008 |
Mr = 482.03 | Dx = 1.454 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 3371 reflections |
a = 11.632 (3) Å | θ = 2.1–27.5° |
b = 7.5534 (19) Å | µ = 1.15 mm−1 |
c = 25.704 (6) Å | T = 298 K |
β = 102.87 (3)° | Block, green |
V = 2201.6 (9) Å3 | 0.38 × 0.19 × 0.16 mm |
Z = 4 |
Siemens SMART CCD area-detector diffractometer | 3861 independent reflections |
Radiation source: fine-focus sealed tube | 2471 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.097 |
φ and ω scans | θmax = 25.0°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→13 |
Tmin = 0.668, Tmax = 0.837 | k = −8→8 |
9852 measured reflections | l = −30→30 |
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)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.109 | H-atom parameters constrained |
S = 0.96 | w = 1/[σ2(Fo2) + (0.095P)2 + 4.2002P] where P = (Fo2 + 2Fc2)/3 |
3861 reflections | (Δ/σ)max = 0.001 |
253 parameters | Δρmax = 0.53 e Å−3 |
0 restraints | Δρmin = −0.44 e Å−3 |
[NiCl(C9H11NO)2(H2O)3]Cl | V = 2201.6 (9) Å3 |
Mr = 482.03 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 11.632 (3) Å | µ = 1.15 mm−1 |
b = 7.5534 (19) Å | T = 298 K |
c = 25.704 (6) Å | 0.38 × 0.19 × 0.16 mm |
β = 102.87 (3)° |
Siemens SMART CCD area-detector diffractometer | 3861 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2471 reflections with I > 2σ(I) |
Tmin = 0.668, Tmax = 0.837 | Rint = 0.097 |
9852 measured reflections |
R[F2 > 2σ(F2)] = 0.044 | 0 restraints |
wR(F2) = 0.109 | H-atom parameters constrained |
S = 0.96 | Δρmax = 0.53 e Å−3 |
3861 reflections | Δρmin = −0.44 e Å−3 |
253 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 | ||
Ni1 | 0.31610 (4) | 0.73333 (6) | 0.514421 (19) | 0.02885 (16) | |
Cl1 | 0.52350 (7) | 0.76902 (13) | 0.54060 (4) | 0.0355 (3) | |
Cl2 | 0.09692 (8) | 0.27614 (14) | 0.47263 (4) | 0.0420 (3) | |
N1 | 0.3676 (3) | 0.8312 (5) | 0.19083 (13) | 0.0357 (9) | |
N2 | 0.3835 (3) | 0.6733 (5) | 0.84909 (13) | 0.0414 (9) | |
O1 | 0.3131 (2) | 0.7215 (4) | 0.43276 (10) | 0.0409 (7) | |
O2 | 0.3021 (2) | 0.7448 (3) | 0.59345 (10) | 0.0356 (7) | |
O3 | 0.2972 (2) | 1.0016 (3) | 0.51083 (10) | 0.0415 (8) | |
H19 | 0.3510 | 1.0577 | 0.5002 | 0.062* | |
H20 | 0.2326 | 1.0483 | 0.4946 | 0.062* | |
O4 | 0.3347 (2) | 0.4651 (3) | 0.52158 (10) | 0.0350 (7) | |
H21 | 0.3830 | 0.4208 | 0.5048 | 0.053* | |
H22 | 0.2718 | 0.4068 | 0.5097 | 0.053* | |
O5 | 0.1378 (2) | 0.6939 (4) | 0.49070 (10) | 0.0405 (7) | |
H23 | 0.1152 | 0.5896 | 0.4811 | 0.061* | |
H24 | 0.0857 | 0.7427 | 0.5044 | 0.061* | |
C1 | 0.3864 (3) | 0.7913 (5) | 0.41131 (16) | 0.0369 (10) | |
H1 | 0.4523 | 0.8416 | 0.4336 | 0.044* | |
C2 | 0.3790 (3) | 0.8017 (5) | 0.35487 (15) | 0.0318 (10) | |
C3 | 0.4687 (3) | 0.8831 (5) | 0.33590 (16) | 0.0364 (10) | |
H3A | 0.5328 | 0.9302 | 0.3601 | 0.044* | |
C4 | 0.4649 (3) | 0.8958 (5) | 0.28259 (16) | 0.0347 (10) | |
H4A | 0.5259 | 0.9536 | 0.2715 | 0.042* | |
C5 | 0.3717 (3) | 0.8239 (5) | 0.24395 (16) | 0.0307 (9) | |
C6 | 0.2794 (3) | 0.7441 (5) | 0.26374 (16) | 0.0375 (11) | |
H6 | 0.2139 | 0.6993 | 0.2398 | 0.045* | |
C7 | 0.2852 (3) | 0.7321 (5) | 0.31661 (16) | 0.0368 (10) | |
H7 | 0.2244 | 0.6752 | 0.3281 | 0.044* | |
C8 | 0.4634 (3) | 0.9121 (6) | 0.17189 (16) | 0.0485 (12) | |
H8A | 0.4644 | 1.0371 | 0.1787 | 0.073* | |
H8B | 0.4524 | 0.8921 | 0.1342 | 0.073* | |
H8C | 0.5368 | 0.8608 | 0.1901 | 0.073* | |
C9 | 0.2689 (4) | 0.7645 (6) | 0.15098 (15) | 0.0533 (13) | |
H9A | 0.2579 | 0.6410 | 0.1573 | 0.080* | |
H9B | 0.2847 | 0.7795 | 0.1161 | 0.080* | |
H9C | 0.1989 | 0.8287 | 0.1531 | 0.080* | |
C10 | 0.3730 (3) | 0.6683 (5) | 0.62962 (15) | 0.0350 (10) | |
H10 | 0.4313 | 0.6008 | 0.6195 | 0.042* | |
C11 | 0.3740 (3) | 0.6735 (5) | 0.68512 (15) | 0.0294 (9) | |
C12 | 0.2921 (3) | 0.7697 (5) | 0.70616 (15) | 0.0331 (10) | |
H12 | 0.2340 | 0.8344 | 0.6832 | 0.040* | |
C13 | 0.2954 (3) | 0.7707 (5) | 0.75929 (15) | 0.0367 (10) | |
H13 | 0.2395 | 0.8364 | 0.7718 | 0.044* | |
C14 | 0.3813 (3) | 0.6748 (5) | 0.79631 (16) | 0.0311 (10) | |
C15 | 0.4646 (3) | 0.5804 (5) | 0.77481 (16) | 0.0361 (11) | |
H15 | 0.5240 | 0.5172 | 0.7975 | 0.043* | |
C16 | 0.4592 (3) | 0.5804 (5) | 0.72124 (16) | 0.0347 (10) | |
H16 | 0.5149 | 0.5154 | 0.7084 | 0.042* | |
C17 | 0.4703 (4) | 0.5718 (7) | 0.88665 (16) | 0.0621 (15) | |
H17A | 0.4611 | 0.4482 | 0.8779 | 0.093* | |
H17B | 0.4593 | 0.5905 | 0.9221 | 0.093* | |
H17C | 0.5481 | 0.6094 | 0.8847 | 0.093* | |
C18 | 0.3019 (4) | 0.7759 (7) | 0.87143 (18) | 0.0772 (18) | |
H18A | 0.3198 | 0.8995 | 0.8695 | 0.116* | |
H18B | 0.3087 | 0.7427 | 0.9080 | 0.116* | |
H18C | 0.2230 | 0.7539 | 0.8517 | 0.116* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0264 (3) | 0.0323 (3) | 0.0302 (3) | 0.0008 (2) | 0.01120 (19) | 0.0021 (3) |
Cl1 | 0.0274 (5) | 0.0439 (6) | 0.0374 (6) | −0.0022 (4) | 0.0115 (4) | 0.0000 (5) |
Cl2 | 0.0311 (5) | 0.0508 (7) | 0.0459 (6) | −0.0013 (5) | 0.0125 (4) | −0.0062 (6) |
N1 | 0.0366 (18) | 0.042 (2) | 0.027 (2) | −0.0032 (16) | 0.0047 (15) | 0.0023 (18) |
N2 | 0.053 (2) | 0.047 (2) | 0.024 (2) | 0.0080 (18) | 0.0071 (16) | −0.0006 (19) |
O1 | 0.0411 (15) | 0.0500 (19) | 0.0353 (17) | −0.0068 (14) | 0.0161 (13) | 0.0011 (16) |
O2 | 0.0388 (15) | 0.0413 (18) | 0.0298 (15) | 0.0024 (13) | 0.0142 (12) | 0.0023 (15) |
O3 | 0.0348 (15) | 0.0335 (16) | 0.059 (2) | 0.0025 (12) | 0.0169 (14) | 0.0110 (15) |
O4 | 0.0301 (13) | 0.0331 (16) | 0.0445 (18) | −0.0011 (12) | 0.0138 (12) | −0.0081 (14) |
O5 | 0.0260 (13) | 0.0481 (18) | 0.0500 (18) | 0.0022 (13) | 0.0143 (12) | 0.0012 (16) |
C1 | 0.037 (2) | 0.036 (3) | 0.038 (3) | 0.0002 (19) | 0.0095 (18) | −0.005 (2) |
C2 | 0.033 (2) | 0.035 (2) | 0.029 (2) | −0.0019 (18) | 0.0107 (17) | 0.001 (2) |
C3 | 0.034 (2) | 0.044 (3) | 0.030 (3) | −0.0075 (19) | 0.0048 (18) | −0.006 (2) |
C4 | 0.030 (2) | 0.041 (3) | 0.035 (3) | −0.0075 (18) | 0.0122 (18) | −0.001 (2) |
C5 | 0.029 (2) | 0.030 (2) | 0.034 (3) | 0.0000 (17) | 0.0077 (17) | 0.002 (2) |
C6 | 0.032 (2) | 0.044 (3) | 0.035 (3) | −0.0097 (19) | 0.0033 (17) | 0.000 (2) |
C7 | 0.032 (2) | 0.039 (3) | 0.041 (3) | −0.0062 (18) | 0.0112 (17) | 0.004 (2) |
C8 | 0.052 (3) | 0.063 (3) | 0.034 (3) | −0.010 (2) | 0.018 (2) | −0.001 (3) |
C9 | 0.051 (3) | 0.074 (4) | 0.032 (3) | −0.010 (2) | 0.003 (2) | −0.005 (3) |
C10 | 0.035 (2) | 0.037 (3) | 0.036 (3) | −0.0008 (19) | 0.0148 (19) | 0.002 (2) |
C11 | 0.029 (2) | 0.032 (2) | 0.028 (2) | −0.0009 (17) | 0.0066 (17) | 0.003 (2) |
C12 | 0.0303 (19) | 0.039 (3) | 0.029 (2) | 0.0022 (18) | 0.0040 (16) | 0.005 (2) |
C13 | 0.032 (2) | 0.042 (3) | 0.037 (3) | 0.0103 (19) | 0.0115 (17) | 0.005 (2) |
C14 | 0.034 (2) | 0.027 (2) | 0.031 (3) | −0.0046 (18) | 0.0052 (18) | 0.000 (2) |
C15 | 0.033 (2) | 0.038 (3) | 0.034 (3) | 0.0075 (19) | 0.0024 (18) | −0.001 (2) |
C16 | 0.031 (2) | 0.035 (2) | 0.040 (3) | 0.0023 (18) | 0.0136 (18) | 0.000 (2) |
C17 | 0.077 (3) | 0.072 (4) | 0.032 (3) | 0.018 (3) | 0.000 (2) | 0.006 (3) |
C18 | 0.089 (4) | 0.111 (5) | 0.036 (3) | 0.032 (4) | 0.023 (3) | 0.000 (3) |
Ni1—O3 | 2.038 (3) | C5—C6 | 1.420 (5) |
Ni1—O4 | 2.042 (3) | C6—C7 | 1.349 (5) |
Ni1—O5 | 2.049 (2) | C6—H6 | 0.9300 |
Ni1—O2 | 2.075 (3) | C7—H7 | 0.9300 |
Ni1—O1 | 2.094 (3) | C8—H8A | 0.9600 |
Ni1—Cl1 | 2.3712 (11) | C8—H8B | 0.9600 |
N1—C5 | 1.357 (5) | C8—H8C | 0.9600 |
N1—C8 | 1.447 (5) | C9—H9A | 0.9600 |
N1—C9 | 1.448 (4) | C9—H9B | 0.9600 |
N2—C14 | 1.351 (5) | C9—H9C | 0.9600 |
N2—C18 | 1.439 (5) | C10—C11 | 1.425 (5) |
N2—C17 | 1.451 (5) | C10—H10 | 0.9300 |
O1—C1 | 1.232 (4) | C11—C16 | 1.389 (5) |
O2—C10 | 1.240 (4) | C11—C12 | 1.399 (5) |
O3—H19 | 0.8500 | C12—C13 | 1.357 (5) |
O3—H20 | 0.8500 | C12—H12 | 0.9300 |
O4—H21 | 0.8500 | C13—C14 | 1.416 (5) |
O4—H22 | 0.8501 | C13—H13 | 0.9300 |
O5—H23 | 0.8500 | C14—C15 | 1.411 (5) |
O5—H24 | 0.8499 | C15—C16 | 1.364 (5) |
C1—C2 | 1.436 (5) | C15—H15 | 0.9300 |
C1—H1 | 0.9300 | C16—H16 | 0.9300 |
C2—C3 | 1.390 (5) | C17—H17A | 0.9600 |
C2—C7 | 1.398 (5) | C17—H17B | 0.9600 |
C3—C4 | 1.365 (5) | C17—H17C | 0.9600 |
C3—H3A | 0.9300 | C18—H18A | 0.9600 |
C4—C5 | 1.406 (5) | C18—H18B | 0.9600 |
C4—H4A | 0.9300 | C18—H18C | 0.9600 |
O3—Ni1—O4 | 177.40 (10) | C5—C6—H6 | 119.4 |
O3—Ni1—O5 | 92.24 (10) | C6—C7—C2 | 122.7 (4) |
O4—Ni1—O5 | 87.84 (10) | C6—C7—H7 | 118.7 |
O3—Ni1—O2 | 88.37 (11) | C2—C7—H7 | 118.7 |
O4—Ni1—O2 | 89.02 (10) | N1—C8—H8A | 109.5 |
O5—Ni1—O2 | 90.15 (10) | N1—C8—H8B | 109.5 |
O3—Ni1—O1 | 91.12 (11) | H8A—C8—H8B | 109.5 |
O4—Ni1—O1 | 91.48 (10) | N1—C8—H8C | 109.5 |
O5—Ni1—O1 | 84.59 (10) | H8A—C8—H8C | 109.5 |
O2—Ni1—O1 | 174.70 (10) | H8B—C8—H8C | 109.5 |
O3—Ni1—Cl1 | 89.57 (7) | N1—C9—H9A | 109.5 |
O4—Ni1—Cl1 | 90.39 (7) | N1—C9—H9B | 109.5 |
O5—Ni1—Cl1 | 177.98 (8) | H9A—C9—H9B | 109.5 |
O2—Ni1—Cl1 | 90.79 (8) | N1—C9—H9C | 109.5 |
O1—Ni1—Cl1 | 94.48 (8) | H9A—C9—H9C | 109.5 |
C5—N1—C8 | 119.9 (3) | H9B—C9—H9C | 109.5 |
C5—N1—C9 | 122.8 (3) | O2—C10—C11 | 126.4 (4) |
C8—N1—C9 | 117.2 (3) | O2—C10—H10 | 116.8 |
C14—N2—C18 | 122.0 (3) | C11—C10—H10 | 116.8 |
C14—N2—C17 | 121.8 (4) | C16—C11—C12 | 116.8 (3) |
C18—N2—C17 | 116.2 (4) | C16—C11—C10 | 120.0 (4) |
C1—O1—Ni1 | 124.9 (3) | C12—C11—C10 | 123.2 (3) |
C10—O2—Ni1 | 122.1 (2) | C13—C12—C11 | 121.5 (3) |
Ni1—O3—H19 | 115.5 | C13—C12—H12 | 119.3 |
Ni1—O3—H20 | 120.7 | C11—C12—H12 | 119.3 |
H19—O3—H20 | 105.6 | C12—C13—C14 | 122.1 (4) |
Ni1—O4—H21 | 114.4 | C12—C13—H13 | 119.0 |
Ni1—O4—H22 | 114.6 | C14—C13—H13 | 119.0 |
H21—O4—H22 | 103.1 | N2—C14—C15 | 121.9 (4) |
Ni1—O5—H23 | 116.6 | N2—C14—C13 | 122.1 (4) |
Ni1—O5—H24 | 125.6 | C15—C14—C13 | 116.0 (4) |
H23—O5—H24 | 108.6 | C16—C15—C14 | 120.9 (4) |
O1—C1—C2 | 125.7 (4) | C16—C15—H15 | 119.5 |
O1—C1—H1 | 117.2 | C14—C15—H15 | 119.5 |
C2—C1—H1 | 117.2 | C15—C16—C11 | 122.7 (4) |
C3—C2—C7 | 116.6 (4) | C15—C16—H16 | 118.7 |
C3—C2—C1 | 119.8 (4) | C11—C16—H16 | 118.7 |
C7—C2—C1 | 123.5 (3) | N2—C17—H17A | 109.5 |
C4—C3—C2 | 121.7 (4) | N2—C17—H17B | 109.5 |
C4—C3—H3A | 119.2 | H17A—C17—H17B | 109.5 |
C2—C3—H3A | 119.2 | N2—C17—H17C | 109.5 |
C3—C4—C5 | 122.0 (4) | H17A—C17—H17C | 109.5 |
C3—C4—H4A | 119.0 | H17B—C17—H17C | 109.5 |
C5—C4—H4A | 119.0 | N2—C18—H18A | 109.5 |
N1—C5—C4 | 122.9 (3) | N2—C18—H18B | 109.5 |
N1—C5—C6 | 121.2 (3) | H18A—C18—H18B | 109.5 |
C4—C5—C6 | 115.9 (4) | N2—C18—H18C | 109.5 |
C7—C6—C5 | 121.1 (3) | H18A—C18—H18C | 109.5 |
C7—C6—H6 | 119.4 | H18B—C18—H18C | 109.5 |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H19···Cl1i | 0.85 | 2.37 | 3.214 (3) | 171 |
O3—H20···Cl2ii | 0.85 | 2.32 | 3.110 (3) | 155 |
O4—H21···Cl1iii | 0.85 | 2.27 | 3.095 (3) | 163 |
O5—H24···Cl2iv | 0.85 | 2.33 | 3.088 (3) | 149 |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) x, y+1, z; (iii) −x+1, −y+1, −z+1; (iv) −x, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [NiCl(C9H11NO)2(H2O)3]Cl |
Mr | 482.03 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 298 |
a, b, c (Å) | 11.632 (3), 7.5534 (19), 25.704 (6) |
β (°) | 102.87 (3) |
V (Å3) | 2201.6 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.15 |
Crystal size (mm) | 0.38 × 0.19 × 0.16 |
Data collection | |
Diffractometer | Siemens SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.668, 0.837 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 9852, 3861, 2471 |
Rint | 0.097 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.044, 0.109, 0.96 |
No. of reflections | 3861 |
No. of parameters | 253 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.53, −0.44 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b).
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H19···Cl1i | 0.85 | 2.37 | 3.214 (3) | 170.9 |
O3—H20···Cl2ii | 0.85 | 2.32 | 3.110 (3) | 155.1 |
O4—H21···Cl1iii | 0.85 | 2.27 | 3.095 (3) | 162.8 |
O5—H24···Cl2iv | 0.85 | 2.33 | 3.088 (3) | 148.5 |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) x, y+1, z; (iii) −x+1, −y+1, −z+1; (iv) −x, −y+1, −z+1. |
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Nickel is vital for organism as a trace element. It often acts as a component or secondary factor of enzyme. In the last two decades, biological inorganic chemistry of nickel has became one of the hottest fields and the coordination chemistry of nickel has made a great progress (Jiang et al., 2003). We report here the synthesis and crystal structure of the title compound, a new nickel(II) complex.
The title complex (Fig.1) consists of cations [Ni(C9H11NO)2(H2O)3Cl]+ and non-coordinating chloride anions. The NiII ion is six-coordinated by one Cl atom, two O atoms of 4-dimethylaminobenzaldehyde molecules and three water molecules in a distorted octahedral geometry.
In the crystal, the intermolecular O—H···Cl hydrogen bonds (Table 1) link cations and anions into two-dimensional sheets parallel to ab plane with the up and down protruding ligands.