Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802021669/ob6193sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802021669/ob6193Isup2.hkl |
CCDC reference: 202305
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.041
- wR factor = 0.112
- Data-to-parameter ratio = 10.6
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_354 Alert C Short O-H Bond (0.82A) OW3 - H3A = 0.69 Ang. PLAT_354 Alert C Short O-H Bond (0.82A) OW6 - H6A = 0.71 Ang. General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C14 H20 N2 Ni2 O15 Atom count from _chemical_formula_moiety:C14 H18 N2 Ni2 O15
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check
The title compound, (I), was prepared by mixing hot ethanol–water (3:2, v/v, 25 ml) solutions of nickel iodide (0.157 g, 0.5 mmol) and dipicolinic acid (0.077 g, 0.5 mmol), which were stirred at 353 K for 30 min. 1,10-Phenanthroline (0.090 g, 0.5 mmol) was added and the resulting mixture stirred for 1.5 h and then filtered. After allowing the solution to stand for 1 month, light-green single crystals formed.
The water H atoms were refined, while the remaining H atoms were located geometrically. The O—H bond lengths are in the range 0.64 (6)–0.96 (11) Å.
Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens, 1994); data reduction: SMART; program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
Fig. 1. The molecular structure of (I), showing 10% displacement ellipsoids for non-H atoms. |
[Ni2(C7H3NO4)2(H2O)5]·2H2O | F(000) = 1176 |
Mr = 573.74 | Dx = 1.754 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 8.3399 (2) Å | Cell parameters from 4506 reflections |
b = 27.2748 (6) Å | θ = 1.5–25.0° |
c = 9.6593 (1) Å | µ = 1.81 mm−1 |
β = 98.588 (1)° | T = 293 K |
V = 2172.56 (7) Å3 | Prism, green |
Z = 4 | 0.48 × 0.36 × 0.34 mm |
Siemens SMART CCD diffractometer | 3767 independent reflections |
Radiation source: fine-focus sealed tube | 3290 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.5° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −8→9 |
Tmin = 0.408, Tmax = 0.540 | k = −32→20 |
6851 measured reflections | l = −11→10 |
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)] = 0.041 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.112 | w = 1/[σ2(Fo2) + (0.0544P)2 + 7.4039P] where P = (Fo2 + 2Fc2)/3 |
S = 0.95 | (Δ/σ)max = 0.006 |
3767 reflections | Δρmax = 0.46 e Å−3 |
355 parameters | Δρmin = −0.48 e Å−3 |
0 restraints | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0071 (5) |
[Ni2(C7H3NO4)2(H2O)5]·2H2O | V = 2172.56 (7) Å3 |
Mr = 573.74 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 8.3399 (2) Å | µ = 1.81 mm−1 |
b = 27.2748 (6) Å | T = 293 K |
c = 9.6593 (1) Å | 0.48 × 0.36 × 0.34 mm |
β = 98.588 (1)° |
Siemens SMART CCD diffractometer | 3767 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 3290 reflections with I > 2σ(I) |
Tmin = 0.408, Tmax = 0.540 | Rint = 0.025 |
6851 measured reflections |
R[F2 > 2σ(F2)] = 0.041 | 0 restraints |
wR(F2) = 0.112 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.95 | Δρmax = 0.46 e Å−3 |
3767 reflections | Δρmin = −0.48 e Å−3 |
355 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. The structure was solved by direct methods and successive Fourier difference syntheses. 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 | 0.74912 (6) | 0.385914 (18) | 0.51306 (5) | 0.02552 (17) | |
Ni2 | 0.24141 (6) | 0.399483 (19) | 0.05945 (5) | 0.02580 (17) | |
OW1 | 0.2130 (5) | 0.46641 (15) | −0.0325 (4) | 0.0483 (10) | |
OW2 | 0.4400 (5) | 0.38333 (16) | −0.0326 (4) | 0.0508 (10) | |
OW3 | 0.0302 (4) | 0.41302 (15) | 0.1516 (3) | 0.0321 (7) | |
OW4 | 0.2869 (5) | 0.33558 (12) | 0.1715 (4) | 0.0349 (7) | |
OW5 | 0.0875 (4) | 0.36823 (14) | −0.1021 (3) | 0.0356 (7) | |
O11 | 0.9224 (4) | 0.42057 (11) | 0.6722 (3) | 0.0328 (7) | |
O12 | 1.0030 (4) | 0.49495 (11) | 0.7516 (3) | 0.0370 (7) | |
O13 | 0.3890 (3) | 0.43885 (11) | 0.2061 (3) | 0.0329 (7) | |
O14 | 0.5481 (3) | 0.38539 (11) | 0.3407 (3) | 0.0332 (7) | |
O21 | 0.6047 (4) | 0.37444 (11) | 0.6703 (3) | 0.0371 (7) | |
O22 | 0.4881 (4) | 0.31394 (13) | 0.7756 (4) | 0.0504 (9) | |
O23 | 1.0599 (4) | 0.30114 (13) | 0.3180 (4) | 0.0502 (9) | |
O24 | 0.9261 (4) | 0.36633 (10) | 0.3808 (3) | 0.0321 (7) | |
N1 | 0.7172 (4) | 0.45640 (12) | 0.4715 (3) | 0.0242 (7) | |
N2 | 0.7671 (4) | 0.31468 (12) | 0.5394 (3) | 0.0257 (7) | |
C11 | 0.8086 (4) | 0.48965 (14) | 0.5471 (4) | 0.0238 (8) | |
C12 | 0.7963 (5) | 0.53905 (15) | 0.5146 (4) | 0.0278 (9) | |
H12A | 0.8614 | 0.5620 | 0.5675 | 0.033* | |
C13 | 0.6841 (5) | 0.55339 (16) | 0.4007 (5) | 0.0325 (9) | |
H13A | 0.6747 | 0.5863 | 0.3754 | 0.039* | |
C14 | 0.5865 (5) | 0.51883 (16) | 0.3251 (4) | 0.0302 (9) | |
H14A | 0.5102 | 0.5280 | 0.2493 | 0.036* | |
C15 | 0.6051 (5) | 0.47005 (15) | 0.3647 (4) | 0.0256 (8) | |
C16 | 0.9206 (5) | 0.46704 (15) | 0.6667 (4) | 0.0267 (9) | |
C17 | 0.5067 (5) | 0.42768 (15) | 0.2971 (4) | 0.0268 (9) | |
C21 | 0.6694 (5) | 0.29280 (16) | 0.6186 (4) | 0.0306 (9) | |
C22 | 0.6629 (6) | 0.24249 (17) | 0.6269 (5) | 0.0404 (11) | |
H22A | 0.5934 | 0.2273 | 0.6803 | 0.048* | |
C23 | 0.7615 (6) | 0.21515 (17) | 0.5543 (5) | 0.0440 (12) | |
H23A | 0.7591 | 0.1811 | 0.5587 | 0.053* | |
C24 | 0.8641 (6) | 0.23820 (16) | 0.4750 (5) | 0.0386 (11) | |
H24A | 0.9325 | 0.2200 | 0.4269 | 0.046* | |
C25 | 0.8630 (5) | 0.28856 (15) | 0.4686 (4) | 0.0284 (9) | |
C26 | 0.5781 (5) | 0.32963 (17) | 0.6936 (5) | 0.0347 (10) | |
C27 | 0.9586 (5) | 0.32060 (16) | 0.3826 (4) | 0.0326 (10) | |
OW7 | 0.7388 (5) | 0.42951 (15) | −0.0584 (5) | 0.0465 (9) | |
OW6 | 0.1585 (6) | 0.29215 (16) | −0.2533 (6) | 0.0650 (13) | |
H5B | 0.118 (6) | 0.345 (2) | −0.129 (5) | 0.037 (16)* | |
H7B | 0.734 (6) | 0.4161 (19) | −0.136 (6) | 0.042 (15)* | |
H4B | 0.223 (8) | 0.331 (2) | 0.222 (6) | 0.06 (2)* | |
H4A | 0.362 (8) | 0.343 (2) | 0.230 (7) | 0.07 (2)* | |
H6A | 0.244 (9) | 0.290 (3) | −0.252 (8) | 0.08 (3)* | |
H5A | 0.048 (10) | 0.386 (3) | −0.162 (9) | 0.10 (3)* | |
H3B | 0.007 (7) | 0.398 (2) | 0.215 (7) | 0.06 (2)* | |
H1B | 0.145 (8) | 0.476 (2) | −0.091 (7) | 0.06 (2)* | |
H3A | 0.029 (6) | 0.437 (2) | 0.173 (5) | 0.033 (17)* | |
H7A | 0.811 (8) | 0.418 (2) | −0.007 (7) | 0.07 (2)* | |
H2A | 0.451 (8) | 0.361 (3) | −0.085 (7) | 0.08 (2)* | |
H1A | 0.236 (7) | 0.487 (2) | −0.004 (6) | 0.04 (2)* | |
H2B | 0.516 (9) | 0.402 (3) | −0.031 (7) | 0.08 (2)* | |
H6B | 0.173 (12) | 0.269 (4) | −0.177 (11) | 0.15 (4)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0264 (3) | 0.0247 (3) | 0.0251 (3) | 0.0023 (2) | 0.0024 (2) | 0.0010 (2) |
Ni2 | 0.0253 (3) | 0.0276 (3) | 0.0236 (3) | −0.0008 (2) | 0.0006 (2) | 0.0000 (2) |
OW1 | 0.065 (3) | 0.031 (2) | 0.039 (2) | −0.0036 (19) | −0.0217 (18) | 0.0065 (17) |
OW2 | 0.042 (2) | 0.052 (2) | 0.064 (3) | −0.0163 (18) | 0.0296 (18) | −0.023 (2) |
OW3 | 0.0359 (18) | 0.030 (2) | 0.0312 (18) | 0.0011 (14) | 0.0078 (13) | −0.0010 (16) |
OW4 | 0.0348 (18) | 0.0327 (17) | 0.0384 (18) | 0.0025 (14) | 0.0091 (16) | 0.0068 (14) |
OW5 | 0.0427 (19) | 0.0293 (18) | 0.0318 (18) | 0.0002 (15) | −0.0045 (14) | −0.0051 (15) |
O11 | 0.0365 (16) | 0.0279 (16) | 0.0299 (15) | 0.0021 (13) | −0.0078 (13) | 0.0018 (12) |
O12 | 0.0397 (17) | 0.0295 (16) | 0.0360 (16) | 0.0047 (13) | −0.0136 (13) | −0.0043 (13) |
O13 | 0.0308 (15) | 0.0310 (16) | 0.0328 (16) | 0.0019 (12) | −0.0090 (13) | −0.0011 (12) |
O14 | 0.0313 (15) | 0.0304 (16) | 0.0346 (16) | −0.0010 (12) | −0.0065 (13) | 0.0009 (13) |
O21 | 0.0405 (17) | 0.0335 (17) | 0.0404 (18) | 0.0071 (14) | 0.0157 (14) | 0.0035 (13) |
O22 | 0.054 (2) | 0.049 (2) | 0.057 (2) | −0.0085 (17) | 0.0369 (18) | −0.0081 (17) |
O23 | 0.053 (2) | 0.0402 (19) | 0.066 (2) | 0.0022 (16) | 0.0393 (19) | −0.0013 (17) |
O24 | 0.0356 (16) | 0.0265 (16) | 0.0369 (16) | −0.0014 (12) | 0.0137 (13) | 0.0011 (13) |
N1 | 0.0210 (16) | 0.0245 (17) | 0.0261 (17) | 0.0049 (13) | 0.0003 (13) | 0.0044 (13) |
N2 | 0.0261 (17) | 0.0230 (17) | 0.0278 (18) | −0.0005 (13) | 0.0037 (14) | 0.0017 (13) |
C11 | 0.0179 (18) | 0.028 (2) | 0.026 (2) | −0.0004 (15) | 0.0042 (15) | −0.0044 (16) |
C12 | 0.026 (2) | 0.028 (2) | 0.029 (2) | 0.0006 (16) | 0.0017 (16) | −0.0034 (17) |
C13 | 0.031 (2) | 0.023 (2) | 0.042 (3) | 0.0028 (17) | 0.0022 (18) | 0.0059 (18) |
C14 | 0.024 (2) | 0.036 (2) | 0.030 (2) | 0.0041 (17) | −0.0004 (17) | 0.0027 (18) |
C15 | 0.0234 (19) | 0.032 (2) | 0.0214 (19) | 0.0009 (16) | 0.0024 (15) | −0.0003 (16) |
C16 | 0.026 (2) | 0.032 (2) | 0.022 (2) | 0.0034 (17) | 0.0019 (16) | −0.0017 (16) |
C17 | 0.023 (2) | 0.033 (2) | 0.023 (2) | 0.0016 (17) | 0.0009 (16) | 0.0000 (17) |
C21 | 0.029 (2) | 0.037 (2) | 0.028 (2) | −0.0041 (18) | 0.0081 (17) | 0.0008 (18) |
C22 | 0.048 (3) | 0.036 (3) | 0.040 (3) | −0.009 (2) | 0.017 (2) | 0.004 (2) |
C23 | 0.062 (3) | 0.026 (2) | 0.048 (3) | −0.003 (2) | 0.019 (2) | 0.002 (2) |
C24 | 0.044 (3) | 0.030 (2) | 0.045 (3) | 0.005 (2) | 0.018 (2) | −0.001 (2) |
C25 | 0.029 (2) | 0.029 (2) | 0.028 (2) | 0.0014 (17) | 0.0081 (17) | −0.0016 (17) |
C26 | 0.032 (2) | 0.040 (3) | 0.033 (2) | 0.0007 (19) | 0.0089 (19) | −0.0006 (19) |
C27 | 0.034 (2) | 0.037 (3) | 0.028 (2) | −0.0044 (19) | 0.0085 (18) | 0.0015 (18) |
OW7 | 0.038 (2) | 0.055 (2) | 0.047 (2) | −0.0005 (17) | 0.0054 (17) | −0.0086 (19) |
OW6 | 0.057 (3) | 0.043 (2) | 0.100 (4) | −0.004 (2) | 0.030 (3) | −0.016 (2) |
Ni1—N2 | 1.962 (3) | O23—C27 | 1.242 (5) |
Ni1—N1 | 1.974 (3) | O24—C27 | 1.276 (5) |
Ni1—O21 | 2.098 (3) | N1—C11 | 1.330 (5) |
Ni1—O24 | 2.159 (3) | N1—C15 | 1.337 (5) |
Ni1—O11 | 2.164 (3) | N2—C25 | 1.334 (5) |
Ni1—O14 | 2.179 (3) | N2—C21 | 1.339 (5) |
Ni2—OW1 | 2.028 (4) | C11—C12 | 1.384 (6) |
Ni2—O13 | 2.038 (3) | C11—C16 | 1.505 (5) |
Ni2—OW2 | 2.041 (4) | C12—C13 | 1.390 (6) |
Ni2—OW5 | 2.052 (3) | C12—H12A | 0.9300 |
Ni2—OW4 | 2.057 (3) | C13—C14 | 1.381 (6) |
Ni2—OW3 | 2.121 (3) | C13—H13A | 0.9300 |
OW1—H1B | 0.79 (7) | C14—C15 | 1.387 (6) |
OW1—H1A | 0.64 (6) | C14—H14A | 0.9300 |
OW2—H2A | 0.80 (7) | C15—C17 | 1.509 (6) |
OW2—H2B | 0.81 (7) | C21—C22 | 1.376 (6) |
OW3—H3B | 0.78 (6) | C21—C26 | 1.509 (6) |
OW3—H3A | 0.69 (6) | C22—C23 | 1.377 (7) |
OW4—H4B | 0.78 (7) | C22—H22A | 0.9300 |
OW4—H4A | 0.81 (7) | C23—C24 | 1.382 (6) |
OW5—H5B | 0.74 (6) | C23—H23A | 0.9300 |
OW5—H5A | 0.79 (9) | C24—C25 | 1.375 (6) |
O11—C16 | 1.268 (5) | C24—H24A | 0.9300 |
O12—C16 | 1.248 (5) | C25—C27 | 1.512 (6) |
O13—C17 | 1.253 (5) | OW7—H7B | 0.83 (6) |
O14—C17 | 1.258 (5) | OW7—H7A | 0.79 (7) |
O21—C26 | 1.268 (5) | OW6—H6A | 0.72 (8) |
O22—C26 | 1.246 (5) | OW6—H6B | 0.96 (11) |
N2—Ni1—N1 | 174.93 (13) | C11—N1—C15 | 120.7 (3) |
N2—Ni1—O21 | 78.42 (13) | C11—N1—Ni1 | 120.2 (3) |
N1—Ni1—O21 | 102.59 (13) | C15—N1—Ni1 | 119.0 (3) |
N2—Ni1—O24 | 77.65 (12) | C25—N2—C21 | 121.2 (4) |
N1—Ni1—O24 | 101.77 (12) | C25—N2—Ni1 | 120.2 (3) |
O21—Ni1—O24 | 155.33 (12) | C21—N2—Ni1 | 118.3 (3) |
N2—Ni1—O11 | 108.08 (12) | N1—C11—C12 | 121.5 (4) |
N1—Ni1—O11 | 76.97 (12) | N1—C11—C16 | 112.4 (3) |
O21—Ni1—O11 | 86.87 (12) | C12—C11—C16 | 126.1 (4) |
O24—Ni1—O11 | 94.90 (12) | C11—C12—C13 | 118.2 (4) |
N2—Ni1—O14 | 97.34 (12) | C11—C12—H12A | 120.9 |
N1—Ni1—O14 | 77.64 (12) | C13—C12—H12A | 120.9 |
O21—Ni1—O14 | 95.34 (12) | C14—C13—C12 | 120.0 (4) |
O24—Ni1—O14 | 93.56 (12) | C14—C13—H13A | 120.0 |
O11—Ni1—O14 | 154.38 (11) | C12—C13—H13A | 120.0 |
OW1—Ni2—O13 | 81.33 (15) | C13—C14—C15 | 118.4 (4) |
OW1—Ni2—OW2 | 93.01 (18) | C13—C14—H14A | 120.8 |
O13—Ni2—OW2 | 88.37 (15) | C15—C14—H14A | 120.8 |
OW1—Ni2—OW5 | 91.25 (17) | N1—C15—C14 | 121.1 (4) |
O13—Ni2—OW5 | 172.58 (14) | N1—C15—C17 | 113.2 (3) |
OW2—Ni2—OW5 | 92.01 (16) | C14—C15—C17 | 125.7 (4) |
OW1—Ni2—OW4 | 173.37 (16) | O12—C16—O11 | 125.4 (4) |
O13—Ni2—OW4 | 92.05 (13) | O12—C16—C11 | 118.2 (4) |
OW2—Ni2—OW4 | 87.05 (16) | O11—C16—C11 | 116.4 (3) |
OW5—Ni2—OW4 | 95.37 (15) | O13—C17—O14 | 127.2 (4) |
OW1—Ni2—OW3 | 88.70 (17) | O13—C17—C15 | 115.8 (4) |
O13—Ni2—OW3 | 93.99 (13) | O14—C17—C15 | 116.9 (3) |
OW2—Ni2—OW3 | 177.27 (16) | N2—C21—C22 | 120.7 (4) |
OW5—Ni2—OW3 | 85.82 (14) | N2—C21—C26 | 111.8 (4) |
OW4—Ni2—OW3 | 91.50 (15) | C22—C21—C26 | 127.5 (4) |
Ni2—OW1—H1B | 130 (5) | C21—C22—C23 | 118.6 (4) |
Ni2—OW1—H1A | 126 (6) | C21—C22—H22A | 120.7 |
H1B—OW1—H1A | 99 (7) | C23—C22—H22A | 120.7 |
Ni2—OW2—H2A | 128 (5) | C22—C23—C24 | 120.1 (4) |
Ni2—OW2—H2B | 123 (5) | C22—C23—H23A | 119.9 |
H2A—OW2—H2B | 109 (7) | C24—C23—H23A | 119.9 |
Ni2—OW3—H3B | 124 (4) | C25—C24—C23 | 118.6 (4) |
Ni2—OW3—H3A | 110 (4) | C25—C24—H24A | 120.7 |
H3B—OW3—H3A | 103 (6) | C23—C24—H24A | 120.7 |
Ni2—OW4—H4B | 112 (5) | N2—C25—C24 | 120.8 (4) |
Ni2—OW4—H4A | 103 (5) | N2—C25—C27 | 112.2 (4) |
H4B—OW4—H4A | 98 (6) | C24—C25—C27 | 127.0 (4) |
Ni2—OW5—H5B | 115 (4) | O22—C26—O21 | 125.6 (4) |
Ni2—OW5—H5A | 116 (6) | O22—C26—C21 | 118.1 (4) |
H5B—OW5—H5A | 113 (7) | O21—C26—C21 | 116.3 (4) |
C16—O11—Ni1 | 113.8 (2) | O23—C27—O24 | 124.7 (4) |
C17—O13—Ni2 | 133.4 (3) | O23—C27—C25 | 118.9 (4) |
C17—O14—Ni1 | 113.0 (2) | O24—C27—C25 | 116.4 (4) |
C26—O21—Ni1 | 114.0 (3) | H7B—OW7—H7A | 109 (6) |
C27—O24—Ni1 | 113.3 (3) | H6A—OW6—H6B | 85 (8) |
D—H···A | D—H | H···A | D···A | D—H···A |
OW2—H2B···OW7 | 0.81 (7) | 2.06 (7) | 2.837 (5) | 161 (7) |
OW5—H5B···OW6 | 0.74 (6) | 1.94 (6) | 2.655 (6) | 162 (6) |
OW2—H2A···O22i | 0.80 (7) | 1.92 (7) | 2.720 (5) | 173 (7) |
OW6—H6A···O22i | 0.72 (8) | 2.12 (8) | 2.785 (6) | 156 (8) |
OW1—H1B···O12ii | 0.79 (7) | 1.85 (7) | 2.633 (5) | 171 (7) |
OW5—H5A···O11ii | 0.79 (9) | 2.01 (9) | 2.790 (5) | 169 (8) |
Symmetry codes: (i) x, y, z−1; (ii) x−1, y, z−1. |
Experimental details
Crystal data | |
Chemical formula | [Ni2(C7H3NO4)2(H2O)5]·2H2O |
Mr | 573.74 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 8.3399 (2), 27.2748 (6), 9.6593 (1) |
β (°) | 98.588 (1) |
V (Å3) | 2172.56 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.81 |
Crystal size (mm) | 0.48 × 0.36 × 0.34 |
Data collection | |
Diffractometer | Siemens SMART CCD diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.408, 0.540 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6851, 3767, 3290 |
Rint | 0.025 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.041, 0.112, 0.95 |
No. of reflections | 3767 |
No. of parameters | 355 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.46, −0.48 |
Computer programs: SMART (Siemens, 1996), SMART and SAINT (Siemens, 1994), SMART, SHELXTL (Siemens, 1994), SHELXTL, SHELXL97 (Sheldrick, 1997).
Ni1—N2 | 1.962 (3) | Ni2—OW1 | 2.028 (4) |
Ni1—N1 | 1.974 (3) | Ni2—O13 | 2.038 (3) |
Ni1—O21 | 2.098 (3) | Ni2—OW2 | 2.041 (4) |
Ni1—O24 | 2.159 (3) | Ni2—OW5 | 2.052 (3) |
Ni1—O11 | 2.164 (3) | Ni2—OW4 | 2.057 (3) |
Ni1—O14 | 2.179 (3) | Ni2—OW3 | 2.121 (3) |
N2—Ni1—N1 | 174.93 (13) | OW2—Ni2—OW5 | 92.01 (16) |
N2—Ni1—O21 | 78.42 (13) | OW1—Ni2—OW4 | 173.37 (16) |
N1—Ni1—O21 | 102.59 (13) | O13—Ni2—OW4 | 92.05 (13) |
N2—Ni1—O24 | 77.65 (12) | OW2—Ni2—OW4 | 87.05 (16) |
N1—Ni1—O24 | 101.77 (12) | OW5—Ni2—OW4 | 95.37 (15) |
O21—Ni1—O24 | 155.33 (12) | OW1—Ni2—OW3 | 88.70 (17) |
N2—Ni1—O11 | 108.08 (12) | O13—Ni2—OW3 | 93.99 (13) |
N1—Ni1—O11 | 76.97 (12) | OW2—Ni2—OW3 | 177.27 (16) |
O21—Ni1—O11 | 86.87 (12) | OW5—Ni2—OW3 | 85.82 (14) |
O24—Ni1—O11 | 94.90 (12) | OW4—Ni2—OW3 | 91.50 (15) |
N2—Ni1—O14 | 97.34 (12) | C16—O11—Ni1 | 113.8 (2) |
N1—Ni1—O14 | 77.64 (12) | C17—O13—Ni2 | 133.4 (3) |
O21—Ni1—O14 | 95.34 (12) | C17—O14—Ni1 | 113.0 (2) |
O24—Ni1—O14 | 93.56 (12) | C26—O21—Ni1 | 114.0 (3) |
O11—Ni1—O14 | 154.38 (11) | C27—O24—Ni1 | 113.3 (3) |
OW1—Ni2—O13 | 81.33 (15) | C11—N1—Ni1 | 120.2 (3) |
OW1—Ni2—OW2 | 93.01 (18) | C15—N1—Ni1 | 119.0 (3) |
O13—Ni2—OW2 | 88.37 (15) | C25—N2—Ni1 | 120.2 (3) |
OW1—Ni2—OW5 | 91.25 (17) | C21—N2—Ni1 | 118.3 (3) |
O13—Ni2—OW5 | 172.58 (14) |
D—H···A | D—H | H···A | D···A | D—H···A |
OW2—H2B···OW7 | 0.81 (7) | 2.06 (7) | 2.837 (5) | 161 (7) |
OW5—H5B···OW6 | 0.74 (6) | 1.94 (6) | 2.655 (6) | 162 (6) |
OW2—H2A···O22i | 0.80 (7) | 1.92 (7) | 2.720 (5) | 173 (7) |
OW6—H6A···O22i | 0.72 (8) | 2.12 (8) | 2.785 (6) | 156 (8) |
OW1—H1B···O12ii | 0.79 (7) | 1.85 (7) | 2.633 (5) | 171 (7) |
OW5—H5A···O11ii | 0.79 (9) | 2.01 (9) | 2.790 (5) | 169 (8) |
Symmetry codes: (i) x, y, z−1; (ii) x−1, y, z−1. |
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The complexation of metal ions by dipicolinic acid (pyridine-2,6-dicarboxylic acid) has been extensively studied (Alain et al., 1992; Laine et al., 1995a,b). Owing to its unique ability of the ligand to form stable chelates with various coordination modes and its biological activity, many crystal structures have been determined. In these complexes, dipicolinic acid acts as a tridentate ligand by coordination of the N atom and one O atom from each carboxylate group. Dipicolinic acid is thus a multi-chelating ligand capable of forming monomeric or polymeric complexes (Guerriero et al., 1987; Kjell et al., 1993). We report here the synthesis and crystal structure of a dinuclear nickel dipicolinate compound, (I) (Khalil et al., 1998).
In title compound, (I), the Ni1 atom is octahedrally coordinated by two tridentate dipicolinate ligands via their carboxylate and nitrilo donors. Nevertheless, the Ni—N and Ni—O bond lengths in the two ligands are different: Ni1—N1 = 1.974 (3) Å and Ni1—N2 = 1.962 (3) Å, Ni1—O11 and Ni1—O14 = 2.164 (3) and 2.179 (3) Å, while Ni1—O24 and Ni1—O21 = 2.159 (3) and 2.098 (3) Å, respectively. The planes defining the rings are orthogonal to each other. The Ni2 atom is octahedrally coordinated by five H2O molecules together with one O atom from one dipicolinate coordinated to Ni1, leading to the dinuclear nickel structure. Furthermore, there are two solvated water molecules in an asymmetric unit (Fig. 1 and Table 2).