The crystal structure of the title compound, (C2H10N2)[Zn(H2O)6]>(SO4)2, comprises ZnII complex cations, sulfate anions and diprotonated ethane-1,2-diamine (DAE). The ZnII atom is located on an inversion centre and is coordinated by six water molecules in an octahedral geometry. The DAE dication is located on another inversion centre. Hydrogen bonding occurs between anions and cations but not between DAE and ZnII complex cations.
Supporting information
CCDC reference: 277813
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.024
- wR factor = 0.064
- Data-to-parameter ratio = 13.9
checkCIF/PLATON results
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Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 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
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
Ethane-1,2-diaminium hexaaquazinc(II) sulfate
top
Crystal data top
(C2H10N2)[Zn(H2O)6](SO4)2 | F(000) = 444 |
Mr = 427.71 | Dx = 1.895 Mg m−3 |
Monoclinic, P21/n | Melting point: not measured K |
Hall symbol: -P 2yn | Mo Kα radiation, λ = 0.71073 Å |
a = 8.1827 (6) Å | Cell parameters from 1676 reflections |
b = 7.0914 (5) Å | θ = 1.6–28.2° |
c = 13.1674 (9) Å | µ = 1.99 mm−1 |
β = 101.154 (1)° | T = 293 K |
V = 749.63 (9) Å3 | Platelet, colorless |
Z = 2 | 0.17 × 0.05 × 0.03 mm |
Data collection top
Nonius KappaCCD diffractometer | 1308 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.023 |
Graphite monochromator | θmax = 25.2°, θmin = 2.7° |
Detector resolution: 9 pixels mm-1 | h = −9→9 |
φ and ω scans | k = −8→5 |
3753 measured reflections | l = −15→15 |
1352 independent 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)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.064 | H-atom parameters constrained |
S = 1.14 | w = 1/[σ2(Fo2) + (0.0267P)2 + 0.7365P] where P = (Fo2 + 2Fc2)/3 |
1352 reflections | (Δ/σ)max = 0.001 |
97 parameters | Δρmax = 0.55 e Å−3 |
0 restraints | Δρmin = −0.42 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 | |
Zn | 0.5000 | 0.0000 | 0.5000 | 0.01070 (13) | |
S | 0.00803 (6) | 0.06362 (7) | 0.71577 (4) | 0.01111 (14) | |
O1 | 0.56222 (16) | 0.1414 (2) | 0.64194 (10) | 0.0147 (3) | |
H3 | 0.5128 | 0.2583 | 0.6460 | 0.022* | |
H4 | 0.6719 | 0.1666 | 0.6623 | 0.022* | |
O2 | 0.26596 (16) | −0.0685 (2) | 0.53179 (10) | 0.0140 (3) | |
H5 | 0.1843 | −0.0341 | 0.4825 | 0.021* | |
H6 | 0.2264 | −0.0123 | 0.5834 | 0.021* | |
O3 | 0.38732 (16) | 0.24721 (19) | 0.43211 (10) | 0.0145 (3) | |
H7 | 0.3120 | 0.2147 | 0.3852 | 0.022* | |
H8 | 0.4506 | 0.3225 | 0.4039 | 0.022* | |
O4 | −0.10587 (16) | 0.22731 (19) | 0.70232 (11) | 0.0148 (3) | |
O5 | 0.03920 (18) | −0.00057 (18) | 0.82442 (11) | 0.0144 (3) | |
O6 | 0.16802 (17) | 0.1184 (2) | 0.68848 (10) | 0.0153 (3) | |
O7 | −0.07003 (17) | −0.0897 (2) | 0.64620 (11) | 0.0143 (3) | |
N1 | 0.0632 (2) | 0.5440 (2) | 0.64290 (13) | 0.0140 (4) | |
H1A | 0.1606 | 0.5483 | 0.6829 | 0.021* | |
H1B | 0.0153 | 0.6589 | 0.6476 | 0.021* | |
H1C | 0.0061 | 0.4653 | 0.6629 | 0.021* | |
C2 | 0.0849 (2) | 0.5002 (3) | 0.53602 (15) | 0.0140 (4) | |
H2A | 0.1372 | 0.3777 | 0.5346 | 0.021* | |
H2B | 0.1563 | 0.5939 | 0.5132 | 0.021* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn | 0.01208 (19) | 0.0104 (2) | 0.00916 (19) | 0.00001 (11) | 0.00080 (13) | −0.00012 (11) |
S | 0.0121 (2) | 0.0100 (3) | 0.0103 (3) | −0.00005 (18) | −0.00027 (18) | −0.00053 (18) |
O1 | 0.0147 (7) | 0.0141 (7) | 0.0138 (7) | 0.0007 (6) | −0.0012 (5) | −0.0028 (6) |
O2 | 0.0136 (7) | 0.0163 (7) | 0.0116 (7) | −0.0006 (6) | 0.0011 (5) | 0.0001 (6) |
O3 | 0.0163 (7) | 0.0136 (7) | 0.0126 (7) | −0.0016 (6) | 0.0001 (5) | 0.0014 (5) |
O4 | 0.0147 (7) | 0.0109 (7) | 0.0177 (7) | 0.0017 (6) | 0.0004 (5) | 0.0003 (6) |
O5 | 0.0189 (8) | 0.0129 (8) | 0.0106 (7) | −0.0002 (5) | 0.0008 (6) | 0.0011 (5) |
O6 | 0.0156 (7) | 0.0158 (7) | 0.0140 (7) | −0.0013 (6) | 0.0018 (5) | −0.0012 (6) |
O7 | 0.0155 (7) | 0.0113 (7) | 0.0143 (7) | 0.0001 (6) | −0.0016 (6) | −0.0026 (6) |
N1 | 0.0159 (8) | 0.0112 (8) | 0.0133 (8) | −0.0011 (7) | −0.0010 (7) | 0.0001 (7) |
C2 | 0.0140 (11) | 0.0144 (11) | 0.0125 (10) | −0.0003 (7) | −0.0006 (9) | 0.0001 (7) |
Geometric parameters (Å, º) top
Zn—O2 | 2.0950 (13) | O2—H5 | 0.8713 |
Zn—O2i | 2.0950 (13) | O2—H6 | 0.9010 |
Zn—O1 | 2.0953 (13) | O3—H7 | 0.8171 |
Zn—O1i | 2.0953 (13) | O3—H8 | 0.8750 |
Zn—O3i | 2.0985 (13) | N1—C2 | 1.485 (3) |
Zn—O3 | 2.0985 (14) | N1—H1A | 0.8666 |
S—O6 | 1.4752 (14) | N1—H1B | 0.9112 |
S—O5 | 1.4758 (14) | N1—H1C | 0.8048 |
S—O4 | 1.4777 (14) | C2—C2ii | 1.524 (4) |
S—O7 | 1.4843 (14) | C2—H2A | 0.9700 |
O1—H3 | 0.9282 | C2—H2B | 0.9700 |
O1—H4 | 0.9031 | | |
| | | |
O2—Zn—O2i | 180.0 | Zn—O1—H3 | 116.4 |
O2—Zn—O1 | 90.38 (5) | Zn—O1—H4 | 114.5 |
O2i—Zn—O1 | 89.62 (5) | H3—O1—H4 | 103.1 |
O2—Zn—O1i | 89.62 (5) | Zn—O2—H5 | 112.7 |
O2i—Zn—O1i | 90.38 (5) | Zn—O2—H6 | 121.6 |
O1—Zn—O1i | 180.0 | H5—O2—H6 | 95.8 |
O2—Zn—O3i | 93.69 (5) | Zn—O3—H7 | 106.9 |
O2i—Zn—O3i | 86.31 (5) | Zn—O3—H8 | 116.3 |
O1—Zn—O3i | 90.52 (5) | H7—O3—H8 | 105.8 |
O1i—Zn—O3i | 89.48 (5) | C2—N1—H1A | 108.6 |
O2—Zn—O3 | 86.31 (5) | C2—N1—H1B | 112.6 |
O2i—Zn—O3 | 93.69 (5) | H1A—N1—H1B | 106.5 |
O1—Zn—O3 | 89.48 (5) | C2—N1—H1C | 110.4 |
O1i—Zn—O3 | 90.52 (5) | H1A—N1—H1C | 110.4 |
O3i—Zn—O3 | 180.00 (7) | H1B—N1—H1C | 108.2 |
O6—S—O5 | 108.81 (8) | N1—C2—C2ii | 109.2 (2) |
O6—S—O4 | 109.43 (8) | N1—C2—H2A | 109.8 |
O5—S—O4 | 110.19 (8) | C2ii—C2—H2A | 109.8 |
O6—S—O7 | 109.81 (8) | N1—C2—H2B | 109.8 |
O5—S—O7 | 110.20 (8) | C2ii—C2—H2B | 109.8 |
O4—S—O7 | 108.39 (8) | H2A—C2—H2B | 108.3 |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H3···O5iii | 0.93 | 1.82 | 2.7335 (19) | 167 |
O1—H4···O4iv | 0.90 | 1.84 | 2.7466 (19) | 178 |
O2—H5···O7v | 0.87 | 1.98 | 2.8052 (19) | 159 |
O2—H6···O6 | 0.90 | 1.80 | 2.701 (2) | 173 |
O3—H7···O7v | 0.82 | 2.14 | 2.8312 (19) | 143 |
O3—H8···O5vi | 0.87 | 1.87 | 2.7322 (19) | 167 |
N1—H1A···O6iii | 0.87 | 2.04 | 2.856 (2) | 156 |
N1—H1A···O5iii | 0.87 | 2.50 | 3.214 (2) | 140 |
N1—H1B···O7vii | 0.91 | 1.91 | 2.820 (2) | 173 |
N1—H1C···O4 | 0.80 | 2.03 | 2.826 (2) | 168 |
Symmetry codes: (iii) −x+1/2, y+1/2, −z+3/2; (iv) x+1, y, z; (v) −x, −y, −z+1; (vi) x+1/2, −y+1/2, z−1/2; (vii) x, y+1, z. |