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The title complex, [Ni(C9H7O5)2(H2O)4], a neutral mononuclear molecule, consists of an NiII ion, a 3-carboxyphenoxyacetate (3-CPOAH-) ligand and four coordinated water molecules. The NiII atom, located on a symmetry center, has octahedral coordination involving two oxoacetate O atoms of two 3-CPOAH- ligands and four water molecules. Intermolecular hydrogen bonds form a supramolecular network structure.
Supporting information
CCDC reference: 222737
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.034
- wR factor = 0.084
- Data-to-parameter ratio = 14.4
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96
| Author Response: ... the "_diffrn_reflns_theta_full" is 27.49
|
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - O1W = 5.18 su
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.21
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1
C18 H22 Ni O14
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: RAPID-AUTO (Rigaku Corporation, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97.
Tetraaqua[(3-carboxyphenoxy)acetato]nickel(II)
top
Crystal data top
[Ni(C9H7O5)2(H2O)4] | Z = 1 |
Mr = 521.07 | F(000) = 270 |
Triclinic, P1 | Dx = 1.682 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 4.9412 (10) Å | Cell parameters from 5791 reflections |
b = 5.7963 (12) Å | θ = 3.4–27.5° |
c = 18.362 (4) Å | µ = 1.02 mm−1 |
α = 96.94 (3)° | T = 293 K |
β = 94.82 (3)° | Prism, green |
γ = 97.91 (3)° | 0.32 × 0.30 × 0.30 mm |
V = 514.36 (18) Å3 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 2294 independent reflections |
Radiation source: fine-focus sealed tube | 2076 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.014 |
Detector resolution: 10.000 pixels mm-1 | θmax = 27.5°, θmin = 3.4° |
ω scans | h = −5→6 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −7→7 |
Tmin = 0.721, Tmax = 0.735 | l = −23→22 |
3641 measured reflections | |
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)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.084 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0498P)2 + 0.1735P] where P = (Fo2 + 2Fc2)/3 |
2294 reflections | (Δ/σ)max < 0.001 |
159 parameters | Δρmax = 0.42 e Å−3 |
0 restraints | Δρmin = −0.40 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 | 1.5000 | 1.0000 | 0.5000 | 0.02405 (12) | |
O1W | 1.2304 (3) | 0.7002 (2) | 0.49699 (8) | 0.0322 (3) | |
H11A | 1.2628 | 0.6392 | 0.5342 | 0.048* | |
O2W | 1.7319 (3) | 0.8164 (2) | 0.42990 (8) | 0.0313 (3) | |
H12A | 1.6502 | 0.6831 | 0.4163 | 0.047* | |
O1 | 1.2548 (3) | 1.0770 (2) | 0.41237 (8) | 0.0318 (3) | |
O2 | 1.5293 (3) | 1.3674 (2) | 0.37313 (8) | 0.0329 (3) | |
O3 | 0.8983 (3) | 1.0266 (3) | 0.29526 (8) | 0.0343 (3) | |
O4 | 0.6974 (4) | 1.4407 (3) | 0.07318 (10) | 0.0536 (5) | |
O5 | 0.2958 (4) | 1.2462 (4) | 0.01941 (10) | 0.0586 (5) | |
H10 | 0.3133 | 1.3507 | −0.0070 | 0.088* | |
C1 | 1.3135 (4) | 1.2225 (3) | 0.36852 (10) | 0.0253 (4) | |
C2 | 1.1051 (4) | 1.2272 (3) | 0.30301 (11) | 0.0302 (4) | |
H2A | 1.0214 | 1.3690 | 0.3102 | 0.036* | |
H2B | 1.1971 | 1.2287 | 0.2584 | 0.036* | |
C3 | 0.7030 (4) | 1.0007 (4) | 0.23570 (11) | 0.0309 (4) | |
C4 | 0.4999 (5) | 0.8061 (4) | 0.22945 (13) | 0.0388 (5) | |
H4 | 0.5025 | 0.7013 | 0.2640 | 0.047* | |
C5 | 0.2924 (5) | 0.7685 (4) | 0.17125 (14) | 0.0461 (6) | |
H5 | 0.1552 | 0.6393 | 0.1675 | 0.055* | |
C6 | 0.2881 (5) | 0.9216 (4) | 0.11891 (13) | 0.0417 (5) | |
H6 | 0.1491 | 0.8959 | 0.0801 | 0.050* | |
C7 | 0.4925 (4) | 1.1126 (4) | 0.12507 (11) | 0.0347 (4) | |
C8 | 0.7013 (4) | 1.1546 (4) | 0.18354 (11) | 0.0337 (4) | |
H8 | 0.8375 | 1.2845 | 0.1874 | 0.040* | |
C9 | 0.4992 (4) | 1.2794 (4) | 0.06947 (12) | 0.0388 (5) | |
H12B | 1.820 (6) | 0.877 (5) | 0.4068 (16) | 0.052 (9)* | |
H11B | 1.084 (7) | 0.718 (6) | 0.4918 (18) | 0.064 (10)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.02022 (17) | 0.02399 (18) | 0.02660 (19) | −0.00224 (11) | −0.00345 (12) | 0.00844 (12) |
O1W | 0.0247 (7) | 0.0296 (7) | 0.0408 (9) | −0.0026 (5) | −0.0050 (6) | 0.0120 (6) |
O2W | 0.0290 (7) | 0.0290 (7) | 0.0346 (8) | −0.0034 (5) | 0.0043 (6) | 0.0067 (6) |
O1 | 0.0256 (7) | 0.0373 (7) | 0.0314 (7) | −0.0034 (5) | −0.0056 (5) | 0.0155 (6) |
O2 | 0.0308 (7) | 0.0322 (7) | 0.0328 (8) | −0.0053 (5) | −0.0025 (6) | 0.0085 (6) |
O3 | 0.0285 (7) | 0.0417 (8) | 0.0303 (7) | −0.0054 (6) | −0.0073 (5) | 0.0150 (6) |
O4 | 0.0461 (9) | 0.0661 (11) | 0.0452 (10) | −0.0081 (8) | −0.0139 (8) | 0.0256 (8) |
O5 | 0.0494 (10) | 0.0783 (13) | 0.0444 (10) | −0.0061 (9) | −0.0207 (8) | 0.0290 (9) |
C1 | 0.0247 (8) | 0.0273 (8) | 0.0238 (9) | 0.0039 (7) | −0.0006 (7) | 0.0049 (7) |
C2 | 0.0264 (9) | 0.0341 (10) | 0.0298 (10) | −0.0008 (7) | −0.0029 (7) | 0.0133 (8) |
C3 | 0.0253 (9) | 0.0404 (10) | 0.0255 (10) | 0.0018 (8) | −0.0029 (7) | 0.0063 (8) |
C4 | 0.0373 (11) | 0.0407 (11) | 0.0358 (11) | −0.0026 (9) | −0.0047 (9) | 0.0105 (9) |
C5 | 0.0402 (12) | 0.0471 (13) | 0.0437 (13) | −0.0119 (10) | −0.0102 (10) | 0.0075 (10) |
C6 | 0.0349 (11) | 0.0524 (13) | 0.0330 (11) | −0.0010 (9) | −0.0102 (9) | 0.0039 (9) |
C7 | 0.0314 (10) | 0.0467 (12) | 0.0253 (10) | 0.0046 (8) | −0.0020 (8) | 0.0072 (8) |
C8 | 0.0284 (9) | 0.0418 (11) | 0.0292 (10) | −0.0010 (8) | −0.0029 (8) | 0.0098 (8) |
C9 | 0.0339 (11) | 0.0535 (13) | 0.0282 (11) | 0.0045 (9) | −0.0041 (8) | 0.0096 (9) |
Geometric parameters (Å, º) top
Ni1—O1W | 2.0311 (15) | O5—H10 | 0.8200 |
Ni1—O1Wi | 2.0311 (15) | C1—C2 | 1.522 (2) |
Ni1—O1i | 2.0617 (14) | C2—H2A | 0.9700 |
Ni1—O1 | 2.0617 (14) | C2—H2B | 0.9700 |
Ni1—O2Wi | 2.0870 (16) | C3—C8 | 1.386 (3) |
Ni1—O2W | 2.0870 (16) | C3—C4 | 1.389 (3) |
O1W—H11A | 0.8200 | C4—C5 | 1.392 (3) |
O1W—H11B | 0.74 (3) | C4—H4 | 0.9300 |
O2W—H12A | 0.8200 | C5—C6 | 1.386 (3) |
O2W—H12B | 0.72 (3) | C5—H5 | 0.9300 |
O1—C1 | 1.257 (2) | C6—C7 | 1.379 (3) |
O2—C1 | 1.254 (2) | C6—H6 | 0.9300 |
O3—C3 | 1.376 (2) | C7—C8 | 1.399 (3) |
O3—C2 | 1.423 (2) | C7—C9 | 1.488 (3) |
O4—C9 | 1.249 (3) | C8—H8 | 0.9300 |
O5—C9 | 1.281 (3) | | |
| | | |
O1W—Ni1—O1Wi | 180.00 (9) | O3—C2—C1 | 110.16 (15) |
O1W—Ni1—O1i | 92.72 (6) | O3—C2—H2A | 109.6 |
O1Wi—Ni1—O1i | 87.28 (6) | C1—C2—H2A | 109.6 |
O1W—Ni1—O1 | 87.28 (6) | O3—C2—H2B | 109.6 |
O1Wi—Ni1—O1 | 92.72 (6) | C1—C2—H2B | 109.6 |
O1i—Ni1—O1 | 180.000 (1) | H2A—C2—H2B | 108.1 |
O1W—Ni1—O2Wi | 90.77 (6) | O3—C3—C8 | 123.84 (18) |
O1Wi—Ni1—O2Wi | 89.23 (6) | O3—C3—C4 | 116.08 (18) |
O1i—Ni1—O2Wi | 92.05 (6) | C8—C3—C4 | 120.08 (18) |
O1—Ni1—O2Wi | 87.95 (6) | C3—C4—C5 | 119.7 (2) |
O1W—Ni1—O2W | 89.23 (6) | C3—C4—H4 | 120.1 |
O1Wi—Ni1—O2W | 90.77 (6) | C5—C4—H4 | 120.1 |
O1i—Ni1—O2W | 87.95 (6) | C6—C5—C4 | 120.7 (2) |
O1—Ni1—O2W | 92.05 (6) | C6—C5—H5 | 119.7 |
O2Wi—Ni1—O2W | 180.00 (7) | C4—C5—H5 | 119.7 |
Ni1—O1W—H11A | 109.5 | C7—C6—C5 | 119.13 (19) |
Ni1—O1W—H11B | 114 (3) | C7—C6—H6 | 120.4 |
H11A—O1W—H11B | 111.6 | C5—C6—H6 | 120.4 |
Ni1—O2W—H12A | 109.5 | C6—C7—C8 | 121.0 (2) |
Ni1—O2W—H12B | 121 (2) | C6—C7—C9 | 121.05 (18) |
H12A—O2W—H12B | 121.7 | C8—C7—C9 | 117.93 (19) |
C1—O1—Ni1 | 128.35 (12) | C3—C8—C7 | 119.32 (19) |
C3—O3—C2 | 116.68 (15) | C3—C8—H8 | 120.3 |
C9—O5—H10 | 109.5 | C7—C8—H8 | 120.3 |
O2—C1—O1 | 126.43 (17) | O4—C9—O5 | 123.6 (2) |
O2—C1—C2 | 115.63 (16) | O4—C9—C7 | 119.79 (18) |
O1—C1—C2 | 117.94 (16) | O5—C9—C7 | 116.6 (2) |
| | | |
O1W—Ni1—O1—C1 | −162.87 (17) | C3—C4—C5—C6 | 0.8 (4) |
O1Wi—Ni1—O1—C1 | 17.13 (17) | C4—C5—C6—C7 | 0.0 (4) |
O2Wi—Ni1—O1—C1 | 106.26 (17) | C5—C6—C7—C8 | −0.6 (4) |
O2W—Ni1—O1—C1 | −73.74 (17) | C5—C6—C7—C9 | 178.9 (2) |
Ni1—O1—C1—O2 | −6.7 (3) | O3—C3—C8—C7 | −179.84 (19) |
Ni1—O1—C1—C2 | 173.47 (13) | C4—C3—C8—C7 | 0.4 (3) |
C3—O3—C2—C1 | −176.67 (16) | C6—C7—C8—C3 | 0.4 (3) |
O2—C1—C2—O3 | 168.14 (17) | C9—C7—C8—C3 | −179.13 (19) |
O1—C1—C2—O3 | −12.0 (3) | C6—C7—C9—O4 | −174.6 (2) |
C2—O3—C3—C8 | 1.2 (3) | C8—C7—C9—O4 | 4.9 (3) |
C2—O3—C3—C4 | −179.02 (19) | C6—C7—C9—O5 | 5.1 (3) |
O3—C3—C4—C5 | 179.2 (2) | C8—C7—C9—O5 | −175.3 (2) |
C8—C3—C4—C5 | −1.0 (4) | | |
Symmetry code: (i) −x+3, −y+2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H11A···O2i | 0.82 | 1.92 | 2.670 (2) | 152 |
O2W—H12A···O2ii | 0.82 | 1.90 | 2.704 (2) | 167 |
O5—H10···O4iii | 0.82 | 1.82 | 2.631 (3) | 171 |
O2W—H12B···O1iv | 0.72 (3) | 2.29 (3) | 2.871 (2) | 140 (3) |
O2W—H12B···O3iv | 0.72 (3) | 2.36 (3) | 3.011 (2) | 152 (3) |
O1W—H11B···O2Wv | 0.74 (3) | 2.18 (3) | 2.861 (2) | 153 (3) |
Symmetry codes: (i) −x+3, −y+2, −z+1; (ii) x, y−1, z; (iii) −x+1, −y+3, −z; (iv) x+1, y, z; (v) x−1, y, z. |
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