Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807042614/bv2063sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807042614/bv2063Isup2.hkl |
CCDC reference: 663566
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- Disorder in solvent or counterion
- R factor = 0.048
- wR factor = 0.101
- Data-to-parameter ratio = 14.3
checkCIF/PLATON results
No syntax errors found
Alert level C ABSTM02_ALERT_3_C The ratio of Tmax/Tmin expected RT(exp) is > 1.10 Absorption corrections should be applied. Tmin and Tmax expected: 0.770 0.888 RT(exp) = 1.153 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT057_ALERT_3_C Correction for Absorption Required RT(exp) ... 1.16 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O9 PLAT480_ALERT_4_C Long H...A H-Bond Reported H3B .. O9 .. 2.63 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H9C .. O2 .. 2.61 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 H4 O2
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 6
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 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 3 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Salicylhydrazide (15.2 mg, 0.1 mmol) was dissolved in a mixed solvent (20 ml) of DMF and methanol (1:1), then ZnSO4.7H2O (28.7 mg, 0.1 mmol) was added, stired for 10 min and filtered. Colourless single crystals suitable for X-ray diffraction analysis were obtained by slow diffusion of the filtrate for one week,.
Except the water H atoms, all the H atoms were located at the ideal positions with C–H = 0.93 Å (aromatic), N–H = 0.86 Å (imine) and 0.90 Å (amine), O–H = 0.82 Å(phenol); and Uiso(H) = 1.2Ueq(C) for aromatic H atoms, Uiso(H) = 1.2Ueq(N) for H atoms bonded to N atoms and Uiso(H) = 1.2Ueq(O) for hydroxyl H atoms. The water H atoms were located from the difference maps and refined with the constraints of O–H = 0.82 (1) Å, H–H = 1.35 (1) Å, and the Uiso values of these two H atoms were set 1.5 times of Ueq value of water O9 atom. The water O atom was disordered over two positions with occupancies of 0.589 (3):0.411 (3).
The molecular self-assembly of supramolecular architectures has received much attention during recent decades (Tao et al., 2000). The structures and properties of such systems depend on the coordination and geometric preferences of both the central metal ions and the bridging building blocks, as well as on the influence of weaker non-covalent interactions, such as hydrogen bonds and π-π stacking interactions. In this paper, we report the synthesis and crystal structure of the title compound, (I), [ZnSO4(C7H8N2O2)2].H2O, (Fig.1) a novel ZnII complex formed by the ligand salicylhydrazide. The ZnII ion is situated in a tetragonal-pyramidal enviroment consisting of two O atoms and two N atoms from two ligands in the basal plane,and an O atom from the sulfate anion in the apical position. Intermolecular O—H···O hydrogen bonds (Table 1) result in a two-dimensional network.
For related literature, see: Tao et al. (2000).
Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: PLATON (Spek, 2003).
Fig. 1. Molecular structure of (I), showing the atom-numbering scheme. | |
Fig. 2. Part of the crystal structure of (I), showing the formation of the two-dimensional network. |
[Zn(SO4)(C7H8N2O2)2]·H2O | Z = 2 |
Mr = 483.75 | F(000) = 496 |
Triclinic, P1 | Dx = 1.723 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.2028 (6) Å | Cell parameters from 2048 reflections |
b = 8.8006 (7) Å | θ = 2.5–25.1° |
c = 15.6983 (13) Å | µ = 1.49 mm−1 |
α = 101.930 (1)° | T = 293 K |
β = 95.491 (2)° | Plate, colourless |
γ = 104.210 (1)° | 0.20 × 0.15 × 0.08 mm |
V = 932.50 (13) Å3 |
Bruker SMART APEX CCD area-detector diffractometer | 2757 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.078 |
Graphite monochromator | θmax = 27.0°, θmin = 2.5° |
0.3° wide ω exposures scans | h = −9→9 |
8372 measured reflections | k = −11→11 |
3978 independent reflections | l = −18→19 |
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)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.101 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.92 | w = 1/[σ2(Fo2) + (0.0377P)2] where P = (Fo2 + 2Fc2)/3 |
3978 reflections | (Δ/σ)max = 0.012 |
278 parameters | Δρmax = 0.58 e Å−3 |
6 restraints | Δρmin = −0.51 e Å−3 |
[Zn(SO4)(C7H8N2O2)2]·H2O | γ = 104.210 (1)° |
Mr = 483.75 | V = 932.50 (13) Å3 |
Triclinic, P1 | Z = 2 |
a = 7.2028 (6) Å | Mo Kα radiation |
b = 8.8006 (7) Å | µ = 1.49 mm−1 |
c = 15.6983 (13) Å | T = 293 K |
α = 101.930 (1)° | 0.20 × 0.15 × 0.08 mm |
β = 95.491 (2)° |
Bruker SMART APEX CCD area-detector diffractometer | 2757 reflections with I > 2σ(I) |
8372 measured reflections | Rint = 0.078 |
3978 independent reflections |
R[F2 > 2σ(F2)] = 0.048 | 6 restraints |
wR(F2) = 0.101 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.92 | Δρmax = 0.58 e Å−3 |
3978 reflections | Δρmin = −0.51 e Å−3 |
278 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 | Occ. (<1) | |
Zn1 | 0.13536 (4) | 0.88473 (3) | 0.314727 (19) | 0.03306 (9) | |
C1 | 0.3139 (4) | 1.2506 (3) | 0.18144 (15) | 0.0286 (6) | |
C2 | 0.4106 (4) | 1.4158 (3) | 0.20697 (16) | 0.0298 (6) | |
C3 | 0.4111 (4) | 1.5095 (3) | 0.14579 (17) | 0.0436 (8) | |
H3A | 0.4734 | 1.6194 | 0.1627 | 0.052* | |
C4 | 0.3203 (4) | 1.4411 (3) | 0.06052 (18) | 0.0466 (8) | |
H4A | 0.3225 | 1.5050 | 0.0201 | 0.056* | |
C5 | 0.2259 (4) | 1.2786 (3) | 0.03429 (18) | 0.0452 (8) | |
H5A | 0.1641 | 1.2327 | −0.0234 | 0.054* | |
C6 | 0.2246 (4) | 1.1852 (3) | 0.09485 (16) | 0.0374 (7) | |
H6A | 0.1621 | 1.0754 | 0.0771 | 0.045* | |
C7 | 0.2938 (4) | 1.1418 (3) | 0.24223 (15) | 0.0284 (6) | |
C8 | −0.1049 (4) | 0.3849 (3) | 0.21322 (16) | 0.0293 (6) | |
C9 | −0.1469 (4) | 0.2470 (3) | 0.24732 (16) | 0.0316 (7) | |
C10 | −0.2507 (4) | 0.1002 (3) | 0.19232 (18) | 0.0404 (8) | |
H10A | −0.2821 | 0.0095 | 0.2154 | 0.049* | |
C11 | −0.3077 (4) | 0.0858 (3) | 0.10502 (19) | 0.0434 (8) | |
H11A | −0.3756 | −0.0142 | 0.0689 | 0.052* | |
C12 | −0.2645 (4) | 0.2206 (3) | 0.06998 (18) | 0.0452 (8) | |
H12A | −0.3025 | 0.2117 | 0.0104 | 0.054* | |
C13 | −0.1651 (4) | 0.3667 (3) | 0.12426 (17) | 0.0386 (7) | |
H13A | −0.1370 | 0.4569 | 0.1007 | 0.046* | |
C14 | 0.0002 (4) | 0.5478 (2) | 0.26454 (15) | 0.0281 (6) | |
N1 | 0.3799 (3) | 1.1983 (2) | 0.32565 (12) | 0.0316 (6) | |
H1A | 0.4540 | 1.2952 | 0.3437 | 0.038* | |
N2 | 0.3466 (3) | 1.0954 (2) | 0.38360 (12) | 0.0299 (5) | |
H2A | 0.3047 | 1.1433 | 0.4316 | 0.036* | |
H2B | 0.4567 | 1.0719 | 0.4011 | 0.036* | |
N3 | 0.0868 (3) | 0.5710 (2) | 0.34653 (13) | 0.0361 (6) | |
H3B | 0.0820 | 0.4914 | 0.3709 | 0.043* | |
N4 | 0.1867 (3) | 0.7301 (2) | 0.39233 (14) | 0.0371 (6) | |
H4B | 0.3146 | 0.7397 | 0.4030 | 0.044* | |
H4C | 0.1446 | 0.7549 | 0.4442 | 0.044* | |
O1 | 0.1941 (3) | 0.99810 (18) | 0.21592 (10) | 0.0369 (5) | |
O2 | 0.5027 (3) | 1.48017 (18) | 0.29031 (11) | 0.0441 (6) | |
H2C | 0.5256 | 1.5787 | 0.3009 | 0.066* | |
O3 | 0.0069 (3) | 0.66568 (18) | 0.23094 (11) | 0.0434 (5) | |
O4 | −0.0854 (3) | 0.26218 (19) | 0.33444 (11) | 0.0471 (6) | |
H4D | −0.0849 | 0.1733 | 0.3428 | 0.071* | |
O5 | −0.0905 (3) | 0.95954 (19) | 0.35224 (11) | 0.0407 (5) | |
O6 | −0.4187 (3) | 0.7940 (2) | 0.33021 (12) | 0.0438 (5) | |
O7 | −0.1873 (3) | 0.78945 (19) | 0.45077 (11) | 0.0414 (5) | |
O8 | −0.3047 (2) | 1.02338 (19) | 0.45151 (11) | 0.0403 (5) | |
S1 | −0.25252 (9) | 0.88909 (6) | 0.39720 (4) | 0.02728 (16) | |
O9' | −0.2612 (6) | 0.4713 (4) | 0.4754 (2) | 0.0685 (12) | 0.589 (3) |
H9A | −0.235 (3) | 0.5609 (9) | 0.4650 (14) | 0.103* | 0.589 (3) |
H9B | −0.2009 (19) | 0.4211 (16) | 0.4438 (14) | 0.103* | 0.589 (3) |
O9 | −0.3556 (8) | 0.4900 (6) | 0.5003 (3) | 0.0685 (12) | 0.411 (3) |
H9C | −0.359 (3) | 0.5274 (19) | 0.4567 (8) | 0.103* | 0.411 (3) |
H9D | −0.4656 (14) | 0.478 (4) | 0.5129 (13) | 0.103* | 0.411 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.03925 (18) | 0.01937 (13) | 0.04079 (17) | 0.00402 (12) | 0.00967 (14) | 0.01088 (12) |
C1 | 0.0320 (14) | 0.0254 (11) | 0.0308 (13) | 0.0077 (10) | 0.0100 (11) | 0.0096 (10) |
C2 | 0.0326 (14) | 0.0254 (11) | 0.0325 (13) | 0.0060 (10) | 0.0080 (11) | 0.0101 (10) |
C3 | 0.0506 (18) | 0.0314 (12) | 0.0536 (16) | 0.0083 (12) | 0.0144 (14) | 0.0211 (12) |
C4 | 0.0535 (18) | 0.0486 (14) | 0.0452 (15) | 0.0132 (13) | 0.0067 (14) | 0.0290 (12) |
C5 | 0.0493 (17) | 0.0499 (15) | 0.0371 (15) | 0.0132 (14) | 0.0041 (14) | 0.0131 (13) |
C6 | 0.0407 (16) | 0.0332 (12) | 0.0384 (14) | 0.0078 (12) | 0.0085 (13) | 0.0102 (11) |
C7 | 0.0285 (13) | 0.0235 (11) | 0.0334 (13) | 0.0058 (10) | 0.0089 (11) | 0.0072 (10) |
C8 | 0.0269 (13) | 0.0216 (11) | 0.0383 (14) | 0.0058 (10) | 0.0042 (11) | 0.0058 (10) |
C9 | 0.0333 (14) | 0.0225 (11) | 0.0375 (14) | 0.0072 (11) | 0.0006 (12) | 0.0064 (10) |
C10 | 0.0390 (16) | 0.0250 (12) | 0.0528 (16) | 0.0033 (12) | 0.0002 (14) | 0.0091 (12) |
C11 | 0.0413 (16) | 0.0254 (13) | 0.0523 (17) | 0.0062 (12) | −0.0048 (14) | −0.0063 (13) |
C12 | 0.0490 (18) | 0.0399 (14) | 0.0398 (16) | 0.0083 (14) | −0.0060 (14) | 0.0045 (13) |
C13 | 0.0451 (17) | 0.0301 (12) | 0.0384 (15) | 0.0070 (12) | 0.0000 (13) | 0.0103 (11) |
C14 | 0.0314 (13) | 0.0191 (10) | 0.0344 (13) | 0.0061 (10) | 0.0075 (11) | 0.0076 (10) |
N1 | 0.0387 (12) | 0.0190 (9) | 0.0330 (11) | −0.0013 (9) | 0.0033 (10) | 0.0094 (8) |
N2 | 0.0347 (11) | 0.0276 (9) | 0.0311 (10) | 0.0079 (9) | 0.0082 (9) | 0.0144 (8) |
N3 | 0.0470 (13) | 0.0181 (9) | 0.0401 (12) | 0.0059 (9) | −0.0039 (11) | 0.0083 (9) |
N4 | 0.0423 (13) | 0.0186 (9) | 0.0418 (12) | 0.0058 (9) | −0.0080 (11) | −0.0020 (9) |
O1 | 0.0485 (11) | 0.0223 (8) | 0.0329 (9) | −0.0027 (8) | 0.0042 (9) | 0.0069 (7) |
O2 | 0.0637 (13) | 0.0206 (8) | 0.0398 (10) | −0.0020 (9) | 0.0017 (10) | 0.0083 (8) |
O3 | 0.0654 (13) | 0.0218 (8) | 0.0363 (10) | 0.0002 (9) | −0.0027 (9) | 0.0108 (7) |
O4 | 0.0676 (13) | 0.0212 (8) | 0.0474 (11) | 0.0032 (9) | −0.0051 (10) | 0.0141 (8) |
O5 | 0.0403 (10) | 0.0380 (8) | 0.0565 (10) | 0.0153 (8) | 0.0240 (9) | 0.0259 (8) |
O6 | 0.0394 (11) | 0.0298 (9) | 0.0507 (11) | 0.0004 (8) | −0.0059 (9) | 0.0009 (9) |
O7 | 0.0475 (11) | 0.0395 (8) | 0.0477 (10) | 0.0167 (8) | 0.0143 (9) | 0.0244 (8) |
O8 | 0.0418 (10) | 0.0385 (9) | 0.0399 (10) | 0.0200 (8) | 0.0024 (9) | −0.0013 (8) |
S1 | 0.0293 (3) | 0.0204 (3) | 0.0324 (3) | 0.0048 (2) | 0.0054 (3) | 0.0090 (2) |
O9' | 0.089 (3) | 0.0608 (14) | 0.0756 (19) | 0.0311 (19) | 0.029 (2) | 0.0403 (14) |
O9 | 0.089 (3) | 0.0608 (14) | 0.0756 (19) | 0.0311 (19) | 0.029 (2) | 0.0403 (14) |
Zn1—O5 | 1.9937 (19) | C11—H11A | 0.9300 |
Zn1—O1 | 2.0343 (16) | C12—C13 | 1.367 (3) |
Zn1—O3 | 2.0361 (15) | C12—H12A | 0.9300 |
Zn1—N4 | 2.079 (2) | C13—H13A | 0.9300 |
Zn1—N2 | 2.0962 (17) | C14—O3 | 1.250 (3) |
C1—C6 | 1.386 (3) | C14—N3 | 1.328 (3) |
C1—C2 | 1.403 (3) | N1—N2 | 1.407 (2) |
C1—C7 | 1.478 (3) | N1—H1A | 0.8600 |
C2—O2 | 1.348 (3) | N2—H2A | 0.9000 |
C2—C3 | 1.389 (3) | N2—H2B | 0.9000 |
C3—C4 | 1.374 (3) | N3—N4 | 1.409 (2) |
C3—H3A | 0.9300 | N3—H3B | 0.8600 |
C4—C5 | 1.380 (3) | N4—H4B | 0.9000 |
C4—H4A | 0.9300 | N4—H4C | 0.9000 |
C5—C6 | 1.379 (4) | O2—H2C | 0.8200 |
C5—H5A | 0.9300 | O4—H4D | 0.8200 |
C6—H6A | 0.9300 | O5—S1 | 1.4928 (18) |
C7—O1 | 1.252 (2) | O6—S1 | 1.4634 (17) |
C7—N1 | 1.331 (3) | O7—S1 | 1.4588 (17) |
C8—C13 | 1.386 (3) | O8—S1 | 1.4585 (17) |
C8—C9 | 1.404 (3) | O9'—H9A | 0.819 (9) |
C8—C14 | 1.466 (3) | O9'—H9B | 0.821 (9) |
C9—O4 | 1.365 (3) | O9'—H9C | 1.011 (18) |
C9—C10 | 1.384 (3) | O9—H9A | 1.191 (19) |
C10—C11 | 1.363 (4) | O9—H9C | 0.819 (9) |
C10—H10A | 0.9300 | O9—H9D | 0.822 (9) |
C11—C12 | 1.388 (4) | ||
O5—Zn1—O1 | 101.24 (7) | C13—C12—H12A | 120.5 |
O5—Zn1—O3 | 102.77 (8) | C11—C12—H12A | 120.5 |
O1—Zn1—O3 | 93.86 (6) | C12—C13—C8 | 122.3 (2) |
O5—Zn1—N4 | 107.05 (8) | C12—C13—H13A | 118.9 |
O1—Zn1—N4 | 151.69 (9) | C8—C13—H13A | 118.9 |
O3—Zn1—N4 | 78.90 (7) | O3—C14—N3 | 119.87 (19) |
O5—Zn1—N2 | 95.68 (7) | O3—C14—C8 | 119.7 (2) |
O1—Zn1—N2 | 79.12 (7) | N3—C14—C8 | 120.5 (2) |
O3—Zn1—N2 | 161.25 (8) | C7—N1—N2 | 118.25 (17) |
N4—Zn1—N2 | 99.01 (7) | C7—N1—H1A | 120.9 |
C6—C1—C2 | 118.6 (2) | N2—N1—H1A | 120.9 |
C6—C1—C7 | 117.3 (2) | N1—N2—Zn1 | 107.10 (12) |
C2—C1—C7 | 124.0 (2) | N1—N2—H2A | 110.3 |
O2—C2—C3 | 121.3 (2) | Zn1—N2—H2A | 110.3 |
O2—C2—C1 | 119.2 (2) | N1—N2—H2B | 110.3 |
C3—C2—C1 | 119.5 (2) | Zn1—N2—H2B | 110.3 |
C4—C3—C2 | 120.5 (2) | H2A—N2—H2B | 108.6 |
C4—C3—H3A | 119.7 | C14—N3—N4 | 117.91 (18) |
C2—C3—H3A | 119.7 | C14—N3—H3B | 121.0 |
C3—C4—C5 | 120.7 (2) | N4—N3—H3B | 121.0 |
C3—C4—H4A | 119.7 | N3—N4—Zn1 | 108.09 (14) |
C5—C4—H4A | 119.7 | N3—N4—H4B | 110.1 |
C6—C5—C4 | 119.0 (2) | Zn1—N4—H4B | 110.1 |
C6—C5—H5A | 120.5 | N3—N4—H4C | 110.1 |
C4—C5—H5A | 120.5 | Zn1—N4—H4C | 110.1 |
C5—C6—C1 | 121.7 (2) | H4B—N4—H4C | 108.4 |
C5—C6—H6A | 119.1 | C7—O1—Zn1 | 113.80 (15) |
C1—C6—H6A | 119.1 | C2—O2—H2C | 109.5 |
O1—C7—N1 | 120.1 (2) | C14—O3—Zn1 | 114.63 (14) |
O1—C7—C1 | 120.3 (2) | C9—O4—H4D | 109.5 |
N1—C7—C1 | 119.53 (19) | S1—O5—Zn1 | 132.28 (10) |
C13—C8—C9 | 118.0 (2) | O8—S1—O7 | 111.27 (10) |
C13—C8—C14 | 117.1 (2) | O8—S1—O6 | 109.20 (11) |
C9—C8—C14 | 124.9 (2) | O7—S1—O6 | 111.30 (10) |
O4—C9—C10 | 121.8 (2) | O8—S1—O5 | 107.26 (10) |
O4—C9—C8 | 118.82 (19) | O7—S1—O5 | 108.94 (11) |
C10—C9—C8 | 119.4 (2) | O6—S1—O5 | 108.75 (11) |
C11—C10—C9 | 121.3 (2) | H9A—O9'—H9B | 104.5 (15) |
C11—C10—H10A | 119.4 | H9A—O9'—H9C | 54.7 (17) |
C9—C10—H10A | 119.4 | H9B—O9'—H9C | 127.7 (18) |
C10—C11—C12 | 120.0 (2) | H9A—O9—H9C | 46.1 (16) |
C10—C11—H11A | 120.0 | H9A—O9—H9D | 146 (2) |
C12—C11—H11A | 120.0 | H9C—O9—H9D | 104.3 (15) |
C13—C12—C11 | 119.0 (2) | ||
C6—C1—C2—O2 | −178.1 (2) | C7—N1—N2—Zn1 | −6.3 (3) |
C7—C1—C2—O2 | 4.5 (4) | O5—Zn1—N2—N1 | −91.44 (15) |
C6—C1—C2—C3 | 1.3 (4) | O1—Zn1—N2—N1 | 8.95 (14) |
C7—C1—C2—C3 | −176.1 (2) | O3—Zn1—N2—N1 | 78.3 (3) |
O2—C2—C3—C4 | 178.4 (3) | N4—Zn1—N2—N1 | 160.26 (15) |
C1—C2—C3—C4 | −1.0 (4) | O3—C14—N3—N4 | −1.0 (4) |
C2—C3—C4—C5 | 0.5 (5) | C8—C14—N3—N4 | 179.5 (2) |
C3—C4—C5—C6 | −0.3 (5) | C14—N3—N4—Zn1 | 6.2 (3) |
C4—C5—C6—C1 | 0.6 (4) | O5—Zn1—N4—N3 | 93.69 (16) |
C2—C1—C6—C5 | −1.1 (4) | O1—Zn1—N4—N3 | −83.7 (2) |
C7—C1—C6—C5 | 176.4 (3) | O3—Zn1—N4—N3 | −6.42 (15) |
C6—C1—C7—O1 | −2.4 (4) | N2—Zn1—N4—N3 | −167.49 (16) |
C2—C1—C7—O1 | 175.1 (2) | N1—C7—O1—Zn1 | 11.9 (3) |
C6—C1—C7—N1 | 178.8 (2) | C1—C7—O1—Zn1 | −166.91 (18) |
C2—C1—C7—N1 | −3.8 (4) | O5—Zn1—O1—C7 | 82.16 (18) |
C13—C8—C9—O4 | 178.8 (2) | O3—Zn1—O1—C7 | −173.99 (18) |
C14—C8—C9—O4 | −0.6 (4) | N4—Zn1—O1—C7 | −100.4 (2) |
C13—C8—C9—C10 | −1.9 (4) | N2—Zn1—O1—C7 | −11.53 (18) |
C14—C8—C9—C10 | 178.7 (3) | N3—C14—O3—Zn1 | −5.2 (3) |
O4—C9—C10—C11 | −178.6 (3) | C8—C14—O3—Zn1 | 174.31 (18) |
C8—C9—C10—C11 | 2.1 (4) | O5—Zn1—O3—C14 | −98.63 (19) |
C9—C10—C11—C12 | −1.0 (4) | O1—Zn1—O3—C14 | 158.93 (19) |
C10—C11—C12—C13 | −0.2 (4) | N4—Zn1—O3—C14 | 6.55 (19) |
C11—C12—C13—C8 | 0.4 (4) | N2—Zn1—O3—C14 | 91.9 (3) |
C9—C8—C13—C12 | 0.7 (4) | O1—Zn1—O5—S1 | 155.47 (13) |
C14—C8—C13—C12 | −179.9 (3) | O3—Zn1—O5—S1 | 58.85 (15) |
C13—C8—C14—O3 | 10.4 (4) | N4—Zn1—O5—S1 | −23.28 (16) |
C9—C8—C14—O3 | −170.2 (2) | N2—Zn1—O5—S1 | −124.53 (14) |
C13—C8—C14—N3 | −170.1 (2) | Zn1—O5—S1—O8 | 147.72 (13) |
C9—C8—C14—N3 | 9.3 (4) | Zn1—O5—S1—O7 | 27.17 (17) |
O1—C7—N1—N2 | −3.5 (4) | Zn1—O5—S1—O6 | −94.30 (15) |
C1—C7—N1—N2 | 175.4 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O2 | 0.86 | 1.95 | 2.613 (2) | 133 |
N2—H2A···O7i | 0.90 | 2.14 | 3.026 (3) | 169 |
N2—H2B···O8ii | 0.90 | 2.00 | 2.898 (3) | 175 |
N3—H3B···O4 | 0.86 | 2.01 | 2.655 (2) | 131 |
N3—H3B···O9′iii | 0.86 | 2.54 | 3.085 (4) | 122 |
N3—H3B···O9iii | 0.86 | 2.63 | 3.158 (6) | 120 |
N4—H4B···O6ii | 0.90 | 2.33 | 3.053 (3) | 137 |
N4—H4C···O8i | 0.90 | 2.24 | 2.817 (2) | 121 |
N4—H4C···O7 | 0.90 | 2.49 | 3.056 (3) | 121 |
O2—H2C···O6iv | 0.82 | 1.79 | 2.606 (2) | 177 |
O4—H4D···O5v | 0.82 | 1.91 | 2.727 (2) | 175 |
O9′—H9A···O7 | 0.82 (1) | 2.02 (1) | 2.833 (4) | 173 (2) |
O9′—H9B···O4 | 0.82 (1) | 2.33 (1) | 3.144 (4) | 169 (2) |
O9—H9C···O7 | 0.82 (1) | 2.36 (1) | 2.912 (5) | 125 (1) |
O9—H9C···O2vi | 0.82 (1) | 2.61 (1) | 3.333 (6) | 147 (1) |
O9—H9D···O9vii | 0.82 (1) | 1.39 (2) | 2.130 (11) | 147 (3) |
Symmetry codes: (i) −x, −y+2, −z+1; (ii) x+1, y, z; (iii) −x, −y+1, −z+1; (iv) x+1, y+1, z; (v) x, y−1, z; (vi) x−1, y−1, z; (vii) −x−1, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Zn(SO4)(C7H8N2O2)2]·H2O |
Mr | 483.75 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 7.2028 (6), 8.8006 (7), 15.6983 (13) |
α, β, γ (°) | 101.930 (1), 95.491 (2), 104.210 (1) |
V (Å3) | 932.50 (13) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.49 |
Crystal size (mm) | 0.20 × 0.15 × 0.08 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD area-detector |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8372, 3978, 2757 |
Rint | 0.078 |
(sin θ/λ)max (Å−1) | 0.639 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.048, 0.101, 0.92 |
No. of reflections | 3978 |
No. of parameters | 278 |
No. of restraints | 6 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.58, −0.51 |
Computer programs: SMART (Bruker, 2001), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 2003).
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O2 | 0.86 | 1.95 | 2.613 (2) | 132.6 |
N2—H2A···O7i | 0.90 | 2.14 | 3.026 (3) | 168.9 |
N2—H2B···O8ii | 0.90 | 2.00 | 2.898 (3) | 174.6 |
N3—H3B···O4 | 0.86 | 2.01 | 2.655 (2) | 130.8 |
N3—H3B···O9'iii | 0.86 | 2.54 | 3.085 (4) | 122.0 |
N3—H3B···O9iii | 0.86 | 2.63 | 3.158 (6) | 120.4 |
N4—H4B···O6ii | 0.90 | 2.33 | 3.053 (3) | 137.4 |
N4—H4C···O8i | 0.90 | 2.24 | 2.817 (2) | 121.3 |
N4—H4C···O7 | 0.90 | 2.49 | 3.056 (3) | 121.2 |
O2—H2C···O6iv | 0.82 | 1.79 | 2.606 (2) | 176.7 |
O4—H4D···O5v | 0.82 | 1.91 | 2.727 (2) | 175.4 |
O9'—H9A···O7 | 0.819 (9) | 2.018 (8) | 2.833 (4) | 173 (2) |
O9'—H9B···O4 | 0.821 (9) | 2.334 (11) | 3.144 (4) | 168.8 (18) |
O9—H9C···O7 | 0.819 (9) | 2.360 (14) | 2.912 (5) | 125.3 (13) |
O9—H9C···O2vi | 0.819 (9) | 2.614 (11) | 3.333 (6) | 147.3 (14) |
O9—H9D···O9vii | 0.822 (9) | 1.39 (2) | 2.130 (11) | 147 (3) |
Symmetry codes: (i) −x, −y+2, −z+1; (ii) x+1, y, z; (iii) −x, −y+1, −z+1; (iv) x+1, y+1, z; (v) x, y−1, z; (vi) x−1, y−1, z; (vii) −x−1, −y+1, −z+1. |
The molecular self-assembly of supramolecular architectures has received much attention during recent decades (Tao et al., 2000). The structures and properties of such systems depend on the coordination and geometric preferences of both the central metal ions and the bridging building blocks, as well as on the influence of weaker non-covalent interactions, such as hydrogen bonds and π-π stacking interactions. In this paper, we report the synthesis and crystal structure of the title compound, (I), [ZnSO4(C7H8N2O2)2].H2O, (Fig.1) a novel ZnII complex formed by the ligand salicylhydrazide. The ZnII ion is situated in a tetragonal-pyramidal enviroment consisting of two O atoms and two N atoms from two ligands in the basal plane,and an O atom from the sulfate anion in the apical position. Intermolecular O—H···O hydrogen bonds (Table 1) result in a two-dimensional network.