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The title compound, [Zn(C
11H
7O
3)
2(H
2O)
2], is a mononuclear zinc(II) complex, with the Zn atom on a twofold rotation axis, coordinated by two O atoms from two water molecules and two O atoms from two 3-hydroxynaphthalene-2-carboxylate ligands, in a distorted tetrahedral geometry. The crystal structure is stabilized by O—H
O hydrogen bonds, forming a two-dimensional network.
Supporting information
CCDC reference: 255402
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.015 Å
- R factor = 0.057
- wR factor = 0.158
- Data-to-parameter ratio = 8.4
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT034_ALERT_1_C No Flack Parameter Given. Z .GT. Si, NonCentro . ?
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15
Alert level G
REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may
be needed to determine absolute structure
From the CIF: _diffrn_reflns_theta_max 26.01
From the CIF: _reflns_number_total 1180
Count of symmetry unique reflns 1179
Completeness (_total/calc) 100.08%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 1
Fraction of Friedel pairs measured 0.001
Are heavy atom types Z>Si present yes
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
0 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
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SHELXTL-Plus (Siemens, 1990); cell refinement: SHELXTL-Plus; data reduction: SHELXTL-Plus; 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: SHELXL97.
Diaquabis(3-hydroxynaphthalene-2-carboxylato-
κO)zinc(II)
top
Crystal data top
[Zn(C11H7O3)2(H2O)2] | F(000) = 488 |
Mr = 475.73 | Dx = 1.459 Mg m−3 |
Monoclinic, C2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C 2y | Cell parameters from 25 reflections |
a = 15.597 (9) Å | θ = 7.5–15.0° |
b = 5.509 (4) Å | µ = 1.18 mm−1 |
c = 12.648 (7) Å | T = 293 K |
β = 95.06 (2)° | Block, pale yellow |
V = 1082.5 (12) Å3 | 0.52 × 0.20 × 0.18 mm |
Z = 2 | |
Data collection top
Siemens R3m diffractometer | 879 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.089 |
Graphite monochromator | θmax = 26.0°, θmin = 2.6° |
ω scans | h = 0→19 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→6 |
Tmin = 0.579, Tmax = 0.816 | l = −15→15 |
1227 measured reflections | 2 standard reflections every 200 reflections |
1180 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)] = 0.057 | H-atom parameters constrained |
wR(F2) = 0.158 | w = 1/[σ2(Fo2) + (0.0945P)2 + 0.6786P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max < 0.001 |
1180 reflections | Δρmax = 0.41 e Å−3 |
141 parameters | Δρmin = −0.54 e Å−3 |
0 restraints | Absolute structure: Flack (1983), no Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.00 (4) |
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 | |
Zn1 | 1.0000 | −0.00352 (19) | 0.0000 | 0.0620 (5) | |
O1W | 0.9212 (4) | −0.2331 (12) | −0.0830 (5) | 0.0801 (19) | |
H1W | 0.9342 | −0.3585 | −0.1131 | 0.120* | |
H2W | 0.8658 | −0.2215 | −0.0841 | 0.120* | |
O1 | 1.0213 (3) | 0.3351 (12) | 0.1460 (5) | 0.0741 (17) | |
O2 | 0.9037 (4) | 0.1548 (12) | 0.0702 (5) | 0.0720 (16) | |
O3 | 0.7527 (3) | 0.3442 (14) | 0.0815 (4) | 0.0767 (18) | |
H3 | 0.7893 | 0.2520 | 0.0616 | 0.115* | |
C1 | 0.9181 (5) | 0.6652 (18) | 0.2578 (7) | 0.065 (2) | |
H1 | 0.9772 | 0.6603 | 0.2762 | 0.078* | |
C2 | 0.8826 (4) | 0.503 (3) | 0.1831 (5) | 0.0533 (15) | |
C3 | 0.7912 (4) | 0.507 (3) | 0.1561 (5) | 0.0587 (16) | |
C4 | 0.7391 (5) | 0.6730 (18) | 0.2027 (7) | 0.067 (2) | |
H4 | 0.6800 | 0.6741 | 0.1850 | 0.081* | |
C5 | 0.7258 (6) | 1.020 (3) | 0.3275 (6) | 0.079 (3) | |
H5 | 0.6666 | 1.0252 | 0.3103 | 0.095* | |
C6 | 0.7643 (8) | 1.186 (2) | 0.4010 (7) | 0.091 (3) | |
H6 | 0.7307 | 1.3025 | 0.4309 | 0.110* | |
C7 | 0.8549 (8) | 1.177 (2) | 0.4304 (8) | 0.094 (3) | |
H7 | 0.8796 | 1.2834 | 0.4817 | 0.112* | |
C8 | 0.9051 (7) | 1.014 (4) | 0.3833 (7) | 0.089 (3) | |
H8 | 0.9644 | 1.0142 | 0.4001 | 0.107* | |
C9 | 0.8677 (6) | 0.8405 (18) | 0.3081 (7) | 0.066 (2) | |
C10 | 0.7774 (6) | 0.8408 (18) | 0.2778 (6) | 0.065 (2) | |
C11 | 0.9396 (5) | 0.3217 (16) | 0.1319 (6) | 0.0578 (19) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.0516 (7) | 0.0452 (7) | 0.0903 (9) | 0.000 | 0.0115 (5) | 0.000 |
O1W | 0.056 (3) | 0.062 (4) | 0.122 (5) | 0.002 (3) | 0.000 (3) | −0.035 (4) |
O1 | 0.054 (3) | 0.059 (4) | 0.109 (5) | 0.007 (3) | 0.012 (3) | 0.008 (4) |
O2 | 0.073 (3) | 0.051 (3) | 0.095 (4) | 0.001 (3) | 0.020 (3) | −0.012 (4) |
O3 | 0.058 (3) | 0.077 (4) | 0.094 (4) | 0.007 (3) | 0.003 (3) | −0.029 (4) |
C1 | 0.060 (4) | 0.064 (6) | 0.070 (5) | −0.005 (5) | 0.000 (4) | 0.007 (5) |
C2 | 0.055 (3) | 0.049 (3) | 0.056 (4) | 0.007 (9) | 0.006 (3) | 0.008 (7) |
C3 | 0.062 (4) | 0.049 (4) | 0.065 (4) | 0.007 (8) | 0.006 (3) | −0.003 (8) |
C4 | 0.063 (5) | 0.061 (5) | 0.077 (5) | 0.003 (5) | 0.003 (4) | −0.001 (5) |
C5 | 0.101 (6) | 0.066 (7) | 0.072 (5) | 0.027 (9) | 0.013 (4) | −0.010 (8) |
C6 | 0.142 (10) | 0.060 (7) | 0.074 (6) | 0.012 (8) | 0.024 (6) | −0.004 (6) |
C7 | 0.138 (10) | 0.064 (6) | 0.081 (7) | −0.011 (8) | 0.020 (7) | −0.011 (6) |
C8 | 0.112 (7) | 0.076 (6) | 0.079 (5) | −0.010 (12) | 0.008 (5) | −0.025 (9) |
C9 | 0.081 (6) | 0.051 (5) | 0.067 (5) | −0.006 (5) | 0.008 (4) | −0.005 (5) |
C10 | 0.082 (6) | 0.054 (5) | 0.058 (5) | 0.009 (5) | 0.006 (4) | 0.001 (5) |
C11 | 0.064 (5) | 0.041 (4) | 0.070 (5) | 0.004 (4) | 0.009 (4) | 0.008 (4) |
Geometric parameters (Å, º) top
Zn1—O1W | 1.996 (6) | C2—C11 | 1.518 (15) |
Zn1—O1Wi | 1.996 (6) | C3—C4 | 1.389 (14) |
Zn1—O2i | 2.010 (6) | C4—C10 | 1.418 (12) |
Zn1—O2 | 2.010 (6) | C4—H4 | 0.93 |
O1W—H1W | 0.82 | C5—C6 | 1.400 (17) |
O1W—H2W | 0.87 | C5—C10 | 1.452 (15) |
O1—C11 | 1.273 (9) | C5—H5 | 0.93 |
O2—C11 | 1.300 (10) | C6—C7 | 1.429 (14) |
O3—C3 | 1.399 (14) | C6—H6 | 0.93 |
O3—H3 | 0.82 | C7—C8 | 1.367 (18) |
C1—C2 | 1.382 (15) | C7—H7 | 0.93 |
C1—C9 | 1.430 (13) | C8—C9 | 1.434 (17) |
C1—H1 | 0.93 | C8—H8 | 0.93 |
C2—C3 | 1.436 (9) | C9—C10 | 1.426 (13) |
| | | |
O1W—Zn1—O1Wi | 101.3 (4) | C10—C4—H4 | 120.5 |
O1W—Zn1—O2i | 119.5 (2) | C6—C5—C10 | 120.7 (9) |
O1Wi—Zn1—O2i | 93.3 (2) | C6—C5—H5 | 119.7 |
O1W—Zn1—O2 | 93.3 (2) | C10—C5—H5 | 119.7 |
O1Wi—Zn1—O2 | 119.5 (2) | C5—C6—C7 | 120.5 (10) |
O2i—Zn1—O2 | 128.6 (4) | C5—C6—H6 | 119.7 |
Zn1—O1W—H1W | 127.6 | C7—C6—H6 | 119.7 |
Zn1—O1W—H2W | 121.9 | C8—C7—C6 | 120.0 (10) |
H1W—O1W—H2W | 109.9 | C8—C7—H7 | 120.0 |
C11—O2—Zn1 | 105.9 (5) | C6—C7—H7 | 120.0 |
C3—O3—H3 | 109.5 | C7—C8—C9 | 120.9 (10) |
C2—C1—C9 | 122.6 (8) | C7—C8—H8 | 119.6 |
C2—C1—H1 | 118.7 | C9—C8—H8 | 119.6 |
C9—C1—H1 | 118.7 | C10—C9—C1 | 116.8 (8) |
C1—C2—C3 | 118.8 (11) | C10—C9—C8 | 120.8 (9) |
C1—C2—C11 | 120.2 (6) | C1—C9—C8 | 122.4 (9) |
C3—C2—C11 | 121.0 (11) | C4—C10—C9 | 121.8 (8) |
C4—C3—O3 | 118.4 (6) | C4—C10—C5 | 121.1 (9) |
C4—C3—C2 | 121.0 (11) | C9—C10—C5 | 117.1 (9) |
O3—C3—C2 | 120.6 (10) | O1—C11—O2 | 119.8 (8) |
C3—C4—C10 | 119.1 (8) | O1—C11—C2 | 121.2 (8) |
C3—C4—H4 | 120.5 | O2—C11—C2 | 118.9 (7) |
| | | |
O1W—Zn1—O2—C11 | −179.8 (5) | C7—C8—C9—C10 | 2.3 (19) |
O1Wi—Zn1—O2—C11 | 75.1 (6) | C7—C8—C9—C1 | −179.5 (10) |
O2i—Zn1—O2—C11 | −47.3 (5) | C3—C4—C10—C9 | −1.2 (14) |
C9—C1—C2—C3 | −1.1 (15) | C3—C4—C10—C5 | 179.0 (10) |
C9—C1—C2—C11 | 179.6 (8) | C1—C9—C10—C4 | 1.0 (13) |
C1—C2—C3—C4 | 0.9 (16) | C8—C9—C10—C4 | 179.3 (11) |
C11—C2—C3—C4 | −179.9 (10) | C1—C9—C10—C5 | −179.3 (9) |
C1—C2—C3—O3 | −179.4 (10) | C8—C9—C10—C5 | −0.9 (16) |
C11—C2—C3—O3 | −0.2 (16) | C6—C5—C10—C4 | −179.6 (10) |
O3—C3—C4—C10 | −179.4 (9) | C6—C5—C10—C9 | 0.6 (16) |
C2—C3—C4—C10 | 0.3 (16) | Zn1—O2—C11—O1 | −7.8 (9) |
C10—C5—C6—C7 | −1.6 (18) | Zn1—O2—C11—C2 | 170.1 (7) |
C5—C6—C7—C8 | 2.9 (18) | C1—C2—C11—O1 | −9.1 (14) |
C6—C7—C8—C9 | −3.2 (19) | C3—C2—C11—O1 | 171.7 (10) |
C2—C1—C9—C10 | 0.2 (13) | C1—C2—C11—O2 | 173.0 (8) |
C2—C1—C9—C8 | −178.1 (11) | C3—C2—C11—O2 | −6.2 (14) |
Symmetry code: (i) −x+2, y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W···O1ii | 0.82 | 1.89 | 2.688 (9) | 165 |
O1W—H2W···O3iii | 0.87 | 1.89 | 2.747 (8) | 173 |
O3—H3···O2 | 0.82 | 1.86 | 2.591 (8) | 148 |
Symmetry codes: (ii) −x+2, y−1, −z; (iii) −x+3/2, y−1/2, −z. |
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