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The title compound, [Ni(C7H5O2)2], exhibits a mononuclear structure in which the central NiII atom is located on an inversion centre and is coordinated by four O atoms from two salicylaldehyde ligands in a distorted square-planar geometry. The complex was obtained by the reaction of salicylaldehyde and nickel(II) nitrate hexahydrate in ethanol, using 3-amino-1,2-propanediol as a growth-directing reagent.
Supporting information
CCDC reference: 1179630
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.046
- wR factor = 0.100
- Data-to-parameter ratio = 13.8
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT230_ALERT_2_B Hirshfeld Test Diff for O2 - C7 .. 9.23 su
Alert level C
REFLT03_ALERT_3_C Reflection count < 95% complete
From the CIF: _diffrn_reflns_theta_max 27.04
From the CIF: _diffrn_reflns_theta_full 27.04
From the CIF: _reflns_number_total 1224
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 1338
Completeness (_total/calc) 91.48%
PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.92
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - O2 .. 9.85 su
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 1
O1 -NI1 -O1 -C1 0.00 0.00 3.666 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 6
O2 -NI1 -O2 -C7 4.00 0.00 3.666 1.555 1.555 1.555
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
9 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 ALERT type 2 Indicator that the structure model may be wrong or deficient
2 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: XSCANS (Siemens, 1990); cell refinement: XSCANS; data reduction: SHELXTL-Plus (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus; software used to prepare material for publication: SHELXL97.
Bis(2-formylphenolato-
κ2O,
O')nickel(II)
top
Crystal data top
[Ni(C7H5O2)2] | F(000) = 308 |
Mr = 300.93 | Dx = 1.644 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 25 reflections |
a = 12.934 (3) Å | θ = 6.5–15° |
b = 5.827 (1) Å | µ = 1.60 mm−1 |
c = 8.108 (2) Å | T = 293 K |
β = 95.67 (3)° | Block, red |
V = 608.1 (2) Å3 | 0.24 × 0.21 × 0.16 mm |
Z = 2 | |
Data collection top
Siemens R3m diffractometer | 856 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.033 |
Graphite monochromator | θmax = 27.0°, θmin = 3.2° |
ω scans | h = −16→7 |
Absorption correction: ψ scan (Kopfmann & Huber, 1968) | k = −5→7 |
Tmin = 0.688, Tmax = 0.774 | l = −10→9 |
2151 measured reflections | 2 standard reflections every 200 reflections |
1224 independent reflections | intensity decay: none |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.046 | H-atom parameters constrained |
wR(F2) = 0.100 | w = 1/[σ2(Fo2) + (0.0158P)2 + 1.3629P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.032 |
1224 reflections | Δρmax = 0.51 e Å−3 |
89 parameters | Δρmin = −0.39 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.001 |
Special details top
Experimental. IR data (ν, cm-1): 3303 (s), 1619 (versus), 1529 (s),
1448 (s), 1329 (m), 1219 (m), 1145 (w), 1117 (w), 902
(w), 812 (s), 754 (s), 497 (w), 463 (w). CH elemental analysis,
calculated for NiC14H10O4: C 55.88, H 3.35%; found: C 55.96, H 3.29%. |
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 | 0.5000 | 0.5000 | 0.5000 | 0.0271 (3) | |
O1 | 0.59652 (19) | 0.6554 (4) | 0.6382 (3) | 0.0350 (7) | |
O2 | 0.5863 (2) | 0.2513 (6) | 0.4748 (4) | 0.0498 (8) | |
C1 | 0.6926 (3) | 0.5964 (7) | 0.6854 (4) | 0.0262 (8) | |
C2 | 0.7539 (3) | 0.7484 (7) | 0.7893 (4) | 0.0308 (9) | |
H2A | 0.7238 | 0.8890 | 0.8236 | 0.080* | |
C3 | 0.8556 (3) | 0.6964 (7) | 0.8423 (5) | 0.0366 (10) | |
H3A | 0.8966 | 0.8047 | 0.9098 | 0.080* | |
C4 | 0.9002 (3) | 0.4889 (9) | 0.7996 (5) | 0.0422 (10) | |
H4A | 0.9702 | 0.4506 | 0.8405 | 0.080* | |
C5 | 0.8416 (3) | 0.3405 (7) | 0.6985 (5) | 0.0352 (9) | |
H5A | 0.8719 | 0.1996 | 0.6652 | 0.080* | |
C6 | 0.7382 (3) | 0.3889 (7) | 0.6413 (4) | 0.0267 (8) | |
C7 | 0.6810 (3) | 0.2239 (7) | 0.5388 (4) | 0.0281 (8) | |
H7A | 0.7156 | 0.0833 | 0.5163 | 0.080* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0302 (4) | 0.0197 (4) | 0.0305 (4) | 0.0036 (4) | −0.0010 (2) | −0.0069 (4) |
O1 | 0.0361 (15) | 0.0270 (15) | 0.0399 (15) | 0.0058 (12) | −0.0058 (12) | −0.0146 (12) |
O2 | 0.059 (2) | 0.0371 (18) | 0.0535 (19) | 0.0057 (16) | 0.0049 (15) | −0.0079 (15) |
C1 | 0.0324 (19) | 0.0227 (18) | 0.0236 (18) | −0.0026 (17) | 0.0031 (15) | 0.0016 (15) |
C2 | 0.043 (2) | 0.023 (2) | 0.0259 (18) | −0.0032 (18) | 0.0017 (16) | 0.0019 (16) |
C3 | 0.043 (2) | 0.032 (2) | 0.033 (2) | −0.012 (2) | −0.0021 (17) | 0.0004 (18) |
C4 | 0.0356 (19) | 0.045 (3) | 0.045 (2) | −0.001 (2) | −0.0029 (16) | 0.005 (2) |
C5 | 0.039 (2) | 0.033 (2) | 0.033 (2) | 0.0038 (19) | 0.0014 (17) | 0.0009 (18) |
C6 | 0.0337 (19) | 0.024 (2) | 0.0229 (17) | 0.0011 (17) | 0.0049 (15) | 0.0015 (16) |
C7 | 0.034 (2) | 0.021 (2) | 0.0293 (19) | 0.0053 (16) | 0.0028 (16) | −0.0022 (15) |
Geometric parameters (Å, º) top
Ni1—O1i | 1.832 (2) | C2—H2A | 0.9600 |
Ni1—O1 | 1.832 (2) | C3—C4 | 1.397 (6) |
Ni1—O2 | 1.853 (3) | C3—H3A | 0.9600 |
Ni1—O2i | 1.853 (3) | C4—C5 | 1.368 (6) |
O1—C1 | 1.310 (4) | C4—H4A | 0.9601 |
O2—C7 | 1.292 (5) | C5—C6 | 1.401 (5) |
C1—C6 | 1.407 (6) | C5—H5A | 0.9600 |
C1—C2 | 1.412 (5) | C6—C7 | 1.428 (5) |
C2—C3 | 1.377 (6) | C7—H7A | 0.9600 |
| | | |
O1i—Ni1—O1 | 180.0 | C2—C3—H3A | 119.3 |
O1i—Ni1—O2 | 85.83 (12) | C4—C3—H3A | 119.5 |
O1—Ni1—O2 | 94.17 (12) | C5—C4—C3 | 118.6 (4) |
O1i—Ni1—O2i | 94.17 (12) | C5—C4—H4A | 120.5 |
O1—Ni1—O2i | 85.83 (12) | C3—C4—H4A | 120.9 |
O2—Ni1—O2i | 180.0 | C4—C5—C6 | 121.7 (4) |
C1—O1—Ni1 | 128.2 (2) | C4—C5—H5A | 119.5 |
C7—O2—Ni1 | 127.6 (3) | C6—C5—H5A | 118.8 |
O1—C1—C6 | 124.1 (3) | C5—C6—C1 | 120.0 (4) |
O1—C1—C2 | 118.1 (4) | C5—C6—C7 | 118.7 (4) |
C6—C1—C2 | 117.8 (3) | C1—C6—C7 | 121.3 (3) |
C3—C2—C1 | 120.8 (4) | O2—C7—C6 | 124.5 (4) |
C3—C2—H2A | 120.0 | O2—C7—H7A | 118.0 |
C1—C2—H2A | 119.2 | C6—C7—H7A | 117.4 |
C2—C3—C4 | 121.2 (4) | | |
| | | |
O1i—Ni1—O1—C1 | 1 (100) | C2—C3—C4—C5 | 2.3 (6) |
O2—Ni1—O1—C1 | 3.1 (3) | C3—C4—C5—C6 | −1.8 (6) |
O2i—Ni1—O1—C1 | −176.9 (3) | C4—C5—C6—C1 | 1.1 (6) |
O1i—Ni1—O2—C7 | 179.0 (3) | C4—C5—C6—C7 | −178.7 (4) |
O1—Ni1—O2—C7 | −1.0 (3) | O1—C1—C6—C5 | −179.7 (4) |
O2i—Ni1—O2—C7 | 38 (100) | C2—C1—C6—C5 | −0.8 (5) |
Ni1—O1—C1—C6 | −3.1 (5) | O1—C1—C6—C7 | 0.1 (5) |
Ni1—O1—C1—C2 | 178.0 (2) | C2—C1—C6—C7 | 179.0 (3) |
O1—C1—C2—C3 | −179.7 (3) | Ni1—O2—C7—C6 | −1.3 (6) |
C6—C1—C2—C3 | 1.4 (5) | C5—C6—C7—O2 | −178.1 (4) |
C1—C2—C3—C4 | −2.1 (6) | C1—C6—C7—O2 | 2.2 (6) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
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