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The title compound, [Zn(C2H3O2)(C6H18N4)][B5O6(OH)4], contains mixed-ligand [Zn(CH3COO)(teta)]+ complex cations (teta is triethyl­ene­tetramine) and penta­borate [B5O6(OH)4]- anions. The [B5O6(OH)4]- anions are connected to one another through hydrogen bonds, forming a three-dimensional supra­molecular network, in which the [Zn(CH3COO)(teta)]+ cations are located.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270109024445/fn3025sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270109024445/fn3025Isup2.hkl
Contains datablock I

CCDC reference: 746046

Comment top

Borate materials have attracted a great deal of attention in the past because of their rich structural chemistry and potential applications in mineralogy and industry (Christ & Clark, 1977; Becker, 1998; Burns, 1995; Grice et al., 1999; Chen et al., 1995). Borate materials with various alkali metals, alkaline earth metals, main group metals, rare earths and transition metals have been widely explored. In contrast, less work has been carried out on organic borates. To date, only a few organic amines have been successfully introduced into borate systems, such as [NH3CH2CH2NH3][B6O9(OH)2] (Li et al., 2006), [H3N(C6H10)NH3][B4O5(OH)4] and [H3N(C6H10)NH3][B5O8(OH)] (Wang et al., 2004) and [C6H13N2][B5O6(OH)4] (Liu et al., 2008), or metals coordinated by amines, such as [Cu(en)2][B7O13H3]n (en is ethylenediamine; Sung et al., 2000), [Mn(C10H18N6)][B5O6(OH)4]2 (Zhang et al., 2004), [Ni(C4H10N2)(C2H8N2)2][B5O6(OH)4]2 (Liu et al., 2006) and [Zn(dien)2][B5O6(OH)4]2 and [B5O7(OH)3Zn(tren)] [dien is diethylenetriamine and tren is tris(2-aminoethyl)amine; Wang et al., 2005]. However, borates involving organic acids are extremely rare (Tombul et al., 2007). We describe here the synthesis and crystal structure of the title novel metallo-organically templated borate, [Zn(CH3COO)(teta)][B5O6(OH)4] (teta is triethylenetetramine), (I), in which the [Zn(CH3COO)(teta)]+ complex cation contains both organic amine and organic acid ligands.

The asymmetric unit of (I) consists of a [Zn(CH3COO)(teta)]+ cation and a [B5O6(OH)4]- polyborate anion (Fig. 1). In the [Zn(CH3COO)(teta)]+ metal complex cation, the Zn centre is coordinated by four N atoms from teta and one carboxylate O atom, forming a square pyramid with an O atom as the vertex. The Zn—N bond lengths are in the range 2.049 (19)–2.207 (2) Å and the N—Zn—N angles are between 80.46 (8) and 157.06 (8) °. The Zn—O bond length is 2.0020 (16) Å . The second O atom of the carboxylate group is equally disordered over three positions (see Experimental).

The [B5O6(OH)4]- borate polyanion is formed by two [B3O3] rings linked by a common BO4 tetrahedron. Each ring is composed of two BO3 triangles and a slightly distorted common BO4 tetrahedron. The terminal O atoms are protonated. The trigonally coordinated B atoms have B—O distances in the range 1.344 (2)–1.381 (2) Å and the tetrahedral B atoms have longer B—O distances in the range 1.453 (2)–1.483 (2) Å. The O—B—O angles of the BO3 triangles lie in the range 115.20 (15)–123.64 (16) ° and those of the BO4 tetrahedra range from 107.71 (13) to 111.59 (13) °.

Extensive hydrogen-bond interactions are important in the formation and stability of low-dimensional structures (Chang et al., 2001; Dalrymple & Shimizu, 2007).The overall sheet-like structure of (I) is formed by extensive multipoint hydrogen bonding involving the [B5O6(OH)4]- borate polyanions. The [B5O6(OH)4]- polyanions and the templating [Zn(CH3COO)(teta)]+ cations are further connected by hydrogen bonds to form a three-dimensional supramolecular network [N1—H1F···O3, N2—H2A···O7, N3—H3D···O10 and N4—H4A···O2; N···O = 3.054 (3)–3.125 (3) Å; Table 2]. The [Zn(CH3COO)(teta)]+ cations are located in the free space of the network and interact with the inorganic framework by extensive hydrogen bonding (Fig. 2 and Table 2).

Related literature top

For related literature, see: Becker (1998); Burns (1995); Chen et al. (1995); Christ & Clark (1977); Grice et al. (1999); Li et al. (2006); Liu et al. (2006, 2008); Sung et al. (2000); Tombul et al. (2007); Wang et al. (2004, 2005); Zhang et al. (2004).

Experimental top

A mixture of Zn(CH3COO)2.H2O (1.1120 g), H3BO3 (1.2291 g) and H2O (50 ml) was placed in a beaker and stirred at 363 K until the solution had evaporated to 2–3 ml, then teta (1 ml) was added and thorough mixing was carried out. The resulting viscous milky liquid was sealed in a Teflon-lined autoclave, heated at 453 K for 7 d and then cooled to room temperature. Colourless transparent block-like crystals of (I) were obtained, and these were washed with deionized water and dried at ambient temperature.

Refinement top

All H atoms were placed at calculated positions and were included in the refinement in the riding-model approximation, with hydroxyl O—H = 0.84Å, imine N—H = 0.93Å, amine N—H = 0.92Å, methylene C—H = 0.99Å and methyl C—H = 0.98Å, and with Uiso(H) = 1.5Ueq(O), 1.2Ueq(N), 1.2Ueq(C) or 1.5Ueq(methyl C).

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of (I), showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 45% probability level and H atoms are shown as small spheres of arbitrary radii. The O12 atom is disordered over three positions that refined to a ratio of 0.22 (2):0.37 (4):0.41 (4).
[Figure 2] Fig. 2. View of the [Zn(CH3COO)(teta)]+ cations in the inorganic borate network, along the c axis. Dashed lines indicate hydrogen bonds.
acetato[N,N'-bis(2-aminoethyl)ethane-1,2-diamine]zinc(II) 4,4',6,6'-tetrahydroxy-2,2'-spirobi[cyclotriboroxane](1-) top
Crystal data top
[Zn(C2H3O2)(C6H18N4)](B5H4O10)Z = 2
Mr = 488.74F(000) = 504
Triclinic, P1Dx = 1.558 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.7778 (18) ÅCell parameters from 8475 reflections
b = 10.260 (2) Åθ = 3.0–27.5°
c = 12.882 (3) ŵ = 1.24 mm1
α = 69.08 (3)°T = 295 K
β = 87.10 (3)°Block-like, colourless
γ = 74.26 (3)°0.57 × 0.41 × 0.27 mm
V = 1041.6 (4) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
4703 independent reflections
Radiation source: fine-focus sealed tube3988 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
ω scansθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 1011
Tmin = 0.538, Tmax = 0.730k = 1213
10240 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.080H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0381P)2 + 0.3178P]
where P = (Fo2 + 2Fc2)/3
4703 reflections(Δ/σ)max = 0.001
284 parametersΔρmax = 0.28 e Å3
1 restraintΔρmin = 0.24 e Å3
Crystal data top
[Zn(C2H3O2)(C6H18N4)](B5H4O10)γ = 74.26 (3)°
Mr = 488.74V = 1041.6 (4) Å3
Triclinic, P1Z = 2
a = 8.7778 (18) ÅMo Kα radiation
b = 10.260 (2) ŵ = 1.24 mm1
c = 12.882 (3) ÅT = 295 K
α = 69.08 (3)°0.57 × 0.41 × 0.27 mm
β = 87.10 (3)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
4703 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
3988 reflections with I > 2σ(I)
Tmin = 0.538, Tmax = 0.730Rint = 0.018
10240 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0311 restraint
wR(F2) = 0.080H-atom parameters constrained
S = 1.04Δρmax = 0.28 e Å3
4703 reflectionsΔρmin = 0.24 e Å3
284 parameters
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
xyzUiso*/UeqOcc. (<1)
Zn10.47591 (3)0.39003 (2)0.350305 (18)0.04313 (9)
C10.1771 (3)0.2654 (3)0.6031 (2)0.0708 (7)
H1B0.11620.19880.60180.106*
H1C0.10420.35890.59810.106*
H1D0.24230.22440.67270.106*
C20.2816 (3)0.2868 (3)0.50683 (18)0.0568 (6)
C30.2488 (4)0.5959 (3)0.1623 (3)0.0779 (8)
H3B0.21190.69290.10350.093*
H3C0.15590.55750.18670.093*
C40.3658 (4)0.4975 (3)0.11786 (19)0.0682 (7)
H4B0.31610.48720.05500.082*
H4C0.45630.53850.09010.082*
C50.5621 (3)0.2575 (3)0.1824 (2)0.0641 (6)
H5A0.64490.30870.15420.077*
H5B0.53460.22350.12480.077*
C60.6231 (3)0.1301 (3)0.2882 (2)0.0690 (7)
H6A0.54380.07400.31240.083*
H6B0.72200.06540.27460.083*
C70.8104 (3)0.2086 (3)0.3724 (2)0.0641 (7)
H7A0.84170.24310.29450.077*
H7B0.89050.11750.41430.077*
C80.8042 (3)0.3203 (3)0.4231 (2)0.0709 (8)
H8B0.78600.28100.50350.085*
H8C0.90650.34530.41500.085*
N10.3239 (2)0.6074 (2)0.25698 (17)0.0606 (5)
H1E0.24810.63790.30150.073*
H1F0.38350.67280.23220.073*
N20.4221 (2)0.35553 (19)0.20610 (14)0.0509 (4)
H2A0.34040.31070.22080.061*
N30.6537 (2)0.1813 (2)0.37538 (15)0.0555 (5)
H3D0.64310.11440.44470.067*
N40.6745 (2)0.4519 (2)0.36706 (14)0.0544 (5)
H4A0.70390.50280.29820.065*
H4D0.65340.51090.40850.065*
O10.09555 (18)0.54868 (13)0.13616 (11)0.0498 (4)
H1A0.03010.58110.09550.075*
O20.29160 (16)0.34529 (13)0.13194 (10)0.0456 (3)
O30.50676 (18)0.15544 (15)0.13021 (13)0.0585 (4)
H3A0.55520.07030.09070.088*
O40.11629 (13)0.32734 (11)0.01583 (9)0.0317 (3)
O50.33931 (14)0.12480 (12)0.02258 (9)0.0332 (3)
O60.08432 (15)0.08712 (12)0.06758 (9)0.0348 (3)
O70.22590 (14)0.14987 (12)0.19056 (9)0.0331 (3)
O80.0341 (2)0.10567 (19)0.14699 (12)0.0655 (5)
H8A0.06210.08130.07980.098*
O90.1077 (2)0.04509 (15)0.26163 (11)0.0527 (4)
O100.2170 (2)0.02584 (17)0.38478 (11)0.0574 (4)
H10A0.24750.09550.38730.086*
O110.3670 (2)0.36977 (18)0.49334 (13)0.0627 (4)
O12A0.275 (4)0.261 (4)0.422 (3)0.0827 (18)0.22
O12B0.252 (3)0.255 (2)0.4256 (15)0.0827 (18)0.37
O12C0.3153 (10)0.1835 (7)0.4675 (5)0.0827 (18)0.40
B10.1642 (2)0.4062 (2)0.08186 (16)0.0328 (4)
B20.3790 (3)0.2040 (2)0.07763 (17)0.0374 (4)
B30.1909 (2)0.17166 (19)0.07556 (15)0.0289 (4)
B40.1852 (3)0.0462 (2)0.27743 (16)0.0376 (4)
B50.0522 (3)0.0197 (2)0.15673 (17)0.0395 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.05178 (15)0.04918 (14)0.03022 (12)0.02143 (10)0.00767 (9)0.01131 (9)
C10.0847 (18)0.0874 (18)0.0548 (14)0.0532 (15)0.0293 (13)0.0236 (13)
C20.0679 (14)0.0746 (15)0.0402 (11)0.0370 (12)0.0132 (10)0.0232 (10)
C30.0707 (17)0.0708 (17)0.0738 (18)0.0147 (14)0.0208 (14)0.0043 (14)
C40.094 (2)0.0737 (16)0.0379 (12)0.0390 (15)0.0124 (12)0.0072 (11)
C50.0814 (17)0.0749 (16)0.0536 (14)0.0330 (14)0.0148 (12)0.0365 (12)
C60.0727 (16)0.0531 (14)0.0873 (19)0.0224 (12)0.0250 (14)0.0312 (13)
C70.0469 (12)0.0741 (16)0.0479 (13)0.0123 (11)0.0034 (10)0.0023 (11)
C80.0585 (14)0.105 (2)0.0423 (13)0.0367 (14)0.0054 (11)0.0057 (13)
N10.0673 (13)0.0516 (11)0.0573 (12)0.0164 (9)0.0119 (10)0.0137 (9)
N20.0629 (11)0.0570 (10)0.0402 (9)0.0321 (9)0.0040 (8)0.0145 (8)
N30.0561 (11)0.0501 (10)0.0452 (10)0.0172 (8)0.0106 (8)0.0017 (8)
N40.0685 (12)0.0705 (12)0.0317 (9)0.0397 (10)0.0092 (8)0.0127 (8)
O10.0584 (9)0.0290 (6)0.0390 (7)0.0022 (6)0.0219 (6)0.0019 (5)
O20.0542 (8)0.0292 (6)0.0338 (7)0.0007 (6)0.0203 (6)0.0004 (5)
O30.0614 (9)0.0342 (7)0.0520 (9)0.0041 (6)0.0341 (7)0.0007 (6)
O40.0361 (6)0.0234 (5)0.0291 (6)0.0051 (5)0.0102 (5)0.0049 (4)
O50.0367 (6)0.0246 (5)0.0302 (6)0.0040 (5)0.0107 (5)0.0046 (4)
O60.0450 (7)0.0334 (6)0.0275 (6)0.0184 (5)0.0060 (5)0.0074 (5)
O70.0416 (7)0.0324 (6)0.0248 (6)0.0144 (5)0.0058 (5)0.0072 (4)
O80.1065 (14)0.0759 (11)0.0381 (8)0.0690 (10)0.0191 (9)0.0178 (8)
O90.0865 (11)0.0504 (8)0.0276 (7)0.0418 (8)0.0099 (7)0.0051 (6)
O100.0852 (11)0.0619 (9)0.0249 (7)0.0351 (9)0.0012 (7)0.0039 (6)
O110.0790 (11)0.0727 (10)0.0506 (9)0.0443 (9)0.0298 (8)0.0248 (8)
O12A0.125 (6)0.113 (4)0.050 (3)0.079 (4)0.028 (3)0.044 (2)
O12B0.125 (6)0.113 (4)0.050 (3)0.079 (4)0.028 (3)0.044 (2)
O12C0.125 (6)0.113 (4)0.050 (3)0.079 (4)0.028 (3)0.044 (2)
B10.0382 (10)0.0263 (9)0.0276 (9)0.0062 (8)0.0073 (8)0.0051 (7)
B20.0418 (11)0.0286 (9)0.0341 (10)0.0053 (8)0.0118 (8)0.0064 (8)
B30.0342 (9)0.0246 (8)0.0254 (9)0.0089 (7)0.0073 (7)0.0061 (6)
B40.0463 (11)0.0349 (10)0.0272 (9)0.0124 (9)0.0054 (8)0.0055 (7)
B50.0536 (12)0.0384 (11)0.0313 (10)0.0229 (9)0.0136 (9)0.0120 (8)
Geometric parameters (Å, º) top
Zn1—O112.0020 (16)C7—H7B0.9900
Zn1—N42.0549 (19)C8—N41.481 (3)
Zn1—N22.1090 (18)C8—H8B0.9900
Zn1—N12.198 (2)C8—H8C0.9900
Zn1—N32.207 (2)N1—H1E0.9200
Zn1—O12A2.44 (2)N1—H1F0.9200
C1—C21.493 (3)N2—H2A0.9300
C1—H1B0.9800N3—H3D0.9300
C1—H1C0.9800N4—H4A0.9200
C1—H1D0.9800N4—H4D0.9200
C2—O12A1.22 (3)O1—B11.350 (2)
C2—O111.242 (3)O1—H1A0.8400
C2—O12B1.259 (19)O2—B11.376 (2)
C2—O12C1.290 (6)O2—B21.381 (2)
C3—N11.471 (4)O3—B21.351 (2)
C3—C41.481 (4)O3—H3A0.8400
C3—H3B0.9900O4—B11.349 (2)
C3—H3C0.9900O4—B31.476 (2)
C4—N21.464 (3)O5—B21.344 (2)
C4—H4B0.9900O5—B31.483 (2)
C4—H4C0.9900O6—B51.355 (2)
C5—N21.458 (3)O6—B31.467 (2)
C5—C61.508 (4)O7—B41.351 (2)
C5—H5A0.9900O7—B31.453 (2)
C5—H5B0.9900O8—B51.349 (3)
C6—N31.462 (3)O8—H8A0.8400
C6—H6A0.9900O9—B51.370 (3)
C6—H6B0.9900O9—B41.371 (3)
C7—N31.473 (3)O10—B41.354 (2)
C7—C81.496 (4)O10—H10A0.8400
C7—H7A0.9900
O11—Zn1—N4105.65 (8)N4—C8—H8B109.7
O11—Zn1—N2132.06 (7)C7—C8—H8B109.7
N4—Zn1—N2122.28 (8)N4—C8—H8C109.7
O11—Zn1—N195.43 (8)C7—C8—H8C109.7
N4—Zn1—N197.20 (8)H8B—C8—H8C108.2
N2—Zn1—N180.78 (8)C3—N1—Zn1106.70 (16)
O11—Zn1—N3106.94 (8)C3—N1—H1E110.4
N4—Zn1—N381.88 (8)Zn1—N1—H1E110.4
N2—Zn1—N380.46 (8)C3—N1—H1F110.4
N1—Zn1—N3157.06 (8)Zn1—N1—H1F110.4
O11—Zn1—O12A52.7 (8)H1E—N1—H1F108.6
N4—Zn1—O12A153.3 (8)C5—N2—C4115.5 (2)
N2—Zn1—O12A80.7 (8)C5—N2—Zn1108.01 (14)
N1—Zn1—O12A100.2 (10)C4—N2—Zn1107.75 (14)
N3—Zn1—O12A89.7 (10)C5—N2—H2A108.5
C2—C1—H1B109.5C4—N2—H2A108.5
C2—C1—H1C109.5Zn1—N2—H2A108.5
H1B—C1—H1C109.5C6—N3—C7113.9 (2)
C2—C1—H1D109.5C6—N3—Zn1107.72 (15)
H1B—C1—H1D109.5C7—N3—Zn1106.71 (15)
H1C—C1—H1D109.5C6—N3—H3D109.5
O12A—C2—O11109.4 (11)C7—N3—H3D109.5
O11—C2—O12B118.7 (6)Zn1—N3—H3D109.5
O11—C2—O12C122.0 (4)C8—N4—Zn1108.74 (15)
O12A—C2—C1129.5 (13)C8—N4—H4A109.9
O11—C2—C1119.1 (2)Zn1—N4—H4A109.9
O12B—C2—C1119.4 (8)C8—N4—H4D109.9
O12C—C2—C1114.8 (4)Zn1—N4—H4D109.9
N1—C3—C4108.9 (2)H4A—N4—H4D108.3
N1—C3—H3B109.9B1—O1—H1A109.5
C4—C3—H3B109.9B1—O2—B2119.50 (14)
N1—C3—H3C109.9B2—O3—H3A109.5
C4—C3—H3C109.9B1—O4—B3123.88 (13)
H3B—C3—H3C108.3B2—O5—B3123.93 (14)
N2—C4—C3109.4 (2)B5—O6—B3122.65 (15)
N2—C4—H4B109.8B4—O7—B3122.58 (15)
C3—C4—H4B109.8B5—O8—H8A109.5
N2—C4—H4C109.8B5—O9—B4119.42 (15)
C3—C4—H4C109.8B4—O10—H10A109.5
H4B—C4—H4C108.2C2—O11—Zn1109.38 (15)
N2—C5—C6108.7 (2)C2—O12A—Zn187.8 (14)
N2—C5—H5A110.0O4—B1—O1123.64 (16)
C6—C5—H5A110.0O4—B1—O2121.14 (15)
N2—C5—H5B110.0O1—B1—O2115.20 (15)
C6—C5—H5B110.0O5—B2—O3123.72 (17)
H5A—C5—H5B108.3O5—B2—O2120.72 (16)
N3—C6—C5109.85 (19)O3—B2—O2115.52 (16)
N3—C6—H6A109.7O7—B3—O6111.59 (13)
C5—C6—H6A109.7O7—B3—O4108.49 (14)
N3—C6—H6B109.7O6—B3—O4109.59 (14)
C5—C6—H6B109.7O7—B3—O5109.93 (14)
H6A—C6—H6B108.2O6—B3—O5107.71 (13)
N3—C7—C8109.6 (2)O4—B3—O5109.51 (13)
N3—C7—H7A109.7O7—B4—O10122.83 (18)
C8—C7—H7A109.7O7—B4—O9121.46 (17)
N3—C7—H7B109.7O10—B4—O9115.72 (16)
C8—C7—H7B109.7O8—B5—O6122.21 (18)
H7A—C7—H7B108.2O8—B5—O9117.05 (16)
N4—C8—C7109.72 (19)O6—B5—O9120.74 (18)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O4i0.841.872.703 (2)174
O3—H3A···O5ii0.841.852.692 (3)171
O8—H8A···O6iii0.841.942.751 (2)162
N1—H1F···O3iv0.922.213.112 (3)165
N2—H2A···O70.932.303.125 (3)148
N3—H3D···O10v0.932.343.116 (3)141
N4—H4A···O2iv0.922.163.054 (3)164
N4—H4D···O11vi0.922.022.939 (4)173
O10—H10A···O12a0.841.982.799 (2)164
O10—H10A···O12b0.841.882.682 (2)159
O10—H10A···O12c0.841.802.565 (2)149
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z; (iii) x, y, z; (iv) x+1, y+1, z; (v) x+1, y, z+1; (vi) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Zn(C2H3O2)(C6H18N4)](B5H4O10)
Mr488.74
Crystal system, space groupTriclinic, P1
Temperature (K)295
a, b, c (Å)8.7778 (18), 10.260 (2), 12.882 (3)
α, β, γ (°)69.08 (3), 87.10 (3), 74.26 (3)
V3)1041.6 (4)
Z2
Radiation typeMo Kα
µ (mm1)1.24
Crystal size (mm)0.57 × 0.41 × 0.27
Data collection
DiffractometerRigaku R-AXIS RAPID
diffractometer
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.538, 0.730
No. of measured, independent and
observed [I > 2σ(I)] reflections
10240, 4703, 3988
Rint0.018
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.031, 0.080, 1.04
No. of reflections4703
No. of parameters284
No. of restraints1
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.28, 0.24

Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEPII (Johnson, 1976).

Selected geometric parameters (Å, º) top
Zn1—O112.0020 (16)O4—B31.476 (2)
Zn1—N42.0549 (19)O5—B21.344 (2)
Zn1—N22.1090 (18)O5—B31.483 (2)
Zn1—N12.198 (2)O6—B51.355 (2)
Zn1—N32.207 (2)O6—B31.467 (2)
Zn1—O12A2.44 (2)O7—B41.351 (2)
O1—B11.350 (2)O7—B31.453 (2)
O2—B11.376 (2)O9—B51.370 (3)
O2—B21.381 (2)O9—B41.371 (3)
O3—B21.351 (2)O10—B41.354 (2)
O4—B11.349 (2)
O11—Zn1—N4105.65 (8)O1—B1—O2115.20 (15)
O11—Zn1—N2132.06 (7)O5—B2—O3123.72 (17)
N4—Zn1—N2122.28 (8)O5—B2—O2120.72 (16)
O11—Zn1—N195.43 (8)O3—B2—O2115.52 (16)
N4—Zn1—N197.20 (8)O7—B3—O6111.59 (13)
N2—Zn1—N180.78 (8)O7—B3—O4108.49 (14)
O11—Zn1—N3106.94 (8)O6—B3—O4109.59 (14)
N4—Zn1—N381.88 (8)O7—B3—O5109.93 (14)
N2—Zn1—N380.46 (8)O6—B3—O5107.71 (13)
N1—Zn1—N3157.06 (8)O4—B3—O5109.51 (13)
O11—Zn1—O12A52.7 (8)O7—B4—O10122.83 (18)
N4—Zn1—O12A153.3 (8)O7—B4—O9121.46 (17)
N2—Zn1—O12A80.7 (8)O10—B4—O9115.72 (16)
N1—Zn1—O12A100.2 (10)O8—B5—O6122.21 (18)
N3—Zn1—O12A89.7 (10)O8—B5—O9117.05 (16)
O4—B1—O1123.64 (16)O6—B5—O9120.74 (18)
O4—B1—O2121.14 (15)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O4i0.841.872.703 (2)174
O3—H3A···O5ii0.841.852.692 (3)171
O8—H8A···O6iii0.841.942.751 (2)162
N1—H1F···O3iv0.922.213.112 (3)165
N2—H2A···O70.932.303.125 (3)148
N3—H3D···O10v0.932.343.116 (3)141
N4—H4A···O2iv0.922.163.054 (3)164
N4—H4D···O11vi0.922.022.939 (4)173
O10—H10A···O12a0.841.982.799 (2)164
O10—H10A···O12b0.841.882.682 (2)159
O10—H10A···O12c0.841.802.565 (2)149
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z; (iii) x, y, z; (iv) x+1, y+1, z; (v) x+1, y, z+1; (vi) x+1, y+1, z+1.
 

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