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In each of [N,N,N′,N′-tetra­kis(2-pyridyl­methyl)­ethane-1,2-diamine-κ6N]zinc(II) bis(perchlorate) 0.67-hydrate, [Zn(C26H28N6)](ClO4)2·0.67H2O, (I), [N,N,N′-tris­(2-pyridylmethyl)-N′-(2-quinolyl­methyl)­ethane-1,2-diamine-κ6N]zinc(II) bis(perchlorate), [Zn(C30H30N6)](ClO4)2, (II), and [N,N′-bis­(2-pyri­dyl­methyl)-N,N′-bis­(2-quinolyl­methyl)­ethane-1,2-diamine-κ6N]zinc(II) bis(perchlorate) monohydrate, [Zn(C34H32N6)](ClO4)2·H2O, (III), the Zn atom is coordinated to all six N atoms of the ligand. Compound (I) has one complex cation in a general position and one on a twofold axis. The coordination environments are inter­mediate between a regular octa­hedron and a penta­gonal bipyramid which lacks one equatorial bond; complexes (II) and (III) are shown to be closer to the latter description. The quinolyl groups are in equatorial positions and the deviation from octa­hedral geometry increases with the number of these groups. This study demonstrates the systematic changes in the geometry at the central Zn atom as the overlap between the ligands increases.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270108007014/ga3084sup1.cif
Contains datablocks global, I, II, III

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270108007014/ga3084Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270108007014/ga3084IIsup3.hkl
Contains datablock II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270108007014/ga3084IIIsup4.hkl
Contains datablock III

CCDC references: 690167; 690168; 690169

Comment top

Ligands based on N,N,N',N'-tetrakis(2-pyridylmethyl)ethane-1,2-diamine (tpen) are potentially hexadentate, but some metal atoms such as chromium(III) also form complexes in which only five or four N atoms are coordinated (Eriksen et al., 1999). Recently, this type of hexadentate ligand, with all four of the pyridyl groups replaced by quinonyl groups, has attracted interest as a fluorescent sensor for zinc(II) (Mikata et al., 2005). This work reports the structures of three zinc(II) complexes with the tpen ligand and with ligands in which an intermediate number of pyridyl groups have been replaced by quinonyl groups (see scheme). The three zinc(II) complexes with the tpen ligand, (I), the qtpen ligand, (II) [qtpen is N-mono(2-quinolmethyl)-N,N',N'-tris(2-pyridylmethyl)ethane-1,2-diamine], and the bqpben ligand, (III) [bqpben is N,N'-bis(2-quinolmethyl)-N,N',-bis(2-pyridylmethyl)ethane-1,2-diamine], have all been isolated as perchlorate salts. In each of the three cations, all six N atoms are coordinated to ZnII.

Compound (I), [Zn(tpen)](ClO4)2·0.67H2O (Fig 1), crystallizes with one complex cation in a general position and with one on a twofold rotation axis. The perchlorate ions and the water molecule are all in general positions. The structure is very similar to that of [Zn(tpen)](ClO4)2·0.67CH3OH, (IV) (Mikata et al., 2005), which differs from (I) only in the solvate molecule being methanol. For compounds (II), [Zn(qtpen)](ClO4)2 (Fig 2), and (III), [Zn(bqbpen)](ClO4)2·H2O (Fig 3), the coordination around ZnII is very similar to that in [Zn(tpen)]2+, with the quinonyl groups in the equatorial positions. Both sp3 N atoms have the S configuration for the crystal studied. There is an intramolecular C—H..π bond involving atom H3 of an axial pyridine group and the phenyl ring of the equatorial quinonyl group in (II).

The coordination polyhedron around the ZnII centres is irregular (Tables 4 and 5) and is closer to being a pentagonal bipyramid, with N3—Zn1—N6 as the axis and with one equatorial bond lacking, than it is to being a regular octahedron. The two possibilities were compared by constructing an observed polyhedron with unit bond lengths and calculating the r.m.s. values, δoct, of the deviations of the positions, δ, from those of an ideal octahedron with bond angles all 90° and those, δpbp, of an ideal pentagonal bipyramid with eight bond angles of 90°, three of 72° and one of 144°. These calculations gave δoct = 0.191 (38) and 0.185 (18) Å and δpbp = 0.172 (7) and 0.151 (8) Å for the two [Zn(tpen)]2+ cations in (I), δoct = 0.198 (24) Å and δpbp = 0.133 (4) Å for the [Zn(qtpen)]2+ cation in (II), and δoct = 0.217 (32) Å and δpbp = 0.102 (3) Å for the [Zn(bqbpen)]2+ cation in (III).

Another aspect of the introduction of quinonyl groups in the equatorial plane is an increase of the N4—Zn—N5 angle from 119.5 (1) and 121.0 (1)° in [Zn(tpen)]2+, to 125.04 (1)° in [Zn(qtpen)]2+ and 129.8 (1)° in [Zn(bqbpen)]2+. This distortion is accompanied by a twisting of the equatorial aromatic groups out of the plane defined by the ZnII atom and the four equatorial N atoms. The twist angle is in the range 8.2 (2)–10.7 (3)° for the pyridine rings in the two [Zn(tpen)]2+ cations and is 14.6 (2)° in (II). The quinoline ring systems are twisted even more, by 22.0 (2)° in (II), and by 23.5 (2) and 25.8 (2)° in (III). The Zn—N bond lengths vary between 2.082 (3) and 2.236 (3) Å in the four complex cations. The variation of the Zn—N bond lengths from ZnII to the N atoms of the ethane-1,2-diamine part of the ligands behaves normally, but the bond lengths to the aromatic ligands are much more irregular, particularly when the ligand with four quinonyl groups, (IV) (Mikata et al., 2005) is included in the comparisons. This last complex, (IV), also exhibits overcrowding of the axial quinonyl groups, resulting in very long bonds to the axial N atoms of the ligands of 2.401 (2) and 2.371 (2) Å, compared with an average of 2.138 (1) Å here for (II) and (III). Generally, the bond lengths to the axial N atoms decrease as the number of equatorial quinonyl groups increases. This general observation is more specific when the correlation between the lengths deq and dax is considered (Fig. 4): for a given cation in a general position, the longest axial bond is paired with that of the closest equatorial aromatic system. This almost linear correlation, shown in Fig. 4 (gradient −0.823, regression coefficient −0.964 for eight points), may be explained by the interaction between an H atom of the axial pyridyl group and the π-system of the closest equatorial aromatic system. For the cations in special positions, there are two aromatic systems which are equally close and the points for these lie below the regression line.

In compound (I), the Zn and Cl atoms and the water molecules pack in layers perpendicular to the b axis at y = ±1/4. Within the layers, the cations form zigzag chains parallel to the (101) direction (Fig. 5). The two independent cations are linked by C—H···π hydrogen bonds and the cation which is in a general position is hydrogen-bonded to a symmetry-related cation. These hydrogen bonds link the cations into infinite chains, and these chains are separated by perchlorate ions and water molecules. In the layer at y = ±3/4, the chains are displaced by c/2 so that they are above the perchlorate ions of the neighbouring layer. The packing interactions are hydrogen bonds of the O—H···O(perchlorate) and C—H···π types (Table 1).

In (II), the cations lie in layers parallel to the (101) plane; intermolecular C—H···π hydrogen bonds link pairs of cations (Fig. 6). The dimers are close-packed within these layers and are almost superimposed on those of the neighbouring layer. The perchlorate ions are located between the layers so that the packing utilizes C—H···O and C—H···π interactions (Table 2).

In (III), the cations pack alternately up the 21 screw axes parallel to b at (0, y, 1/4) and (1/2, y, 3/4), giving close-packed columns with the perchlorate ions and water molecules in the spaces between these columns (Fig. 7). The axial Zn—N bonds are parallel to b, resulting in open channels parallel to the b axis. C—H···π bonds link the cation columns along the 21 axis. The C—H···π, O—H···O(perchlorate) and C—H···O interactions are listed in Table 3.

In a large proportion of their salts, perchlorate anions tend to be disordered, which results in large apparent displacement parameters. Here, in ccompounds (I) and (II) [Should this be (III)?], which are both hydrates, the water molecules are hydrogen-bonded to two perchlorate ions, ensuring the anions are ordered. In the anhydrous compound, (III) [Should this be (II)?], one of the perchlorate ions (Cl1) was so disordered that it was modelled as two interpenetrating regular tetrahedra, but even then the U3/U1 value was unrealistically high.

Experimental top

Caution: Perchlorate salts and ethanolic solutions of perchlorate salts are potentially explosive, and should be handled accordingly.

For [Zn(tpen)](ClO4)2·2H2O, a solution of zinc perchlorate hexahydrate (0.896 g, 2.4 mmol) in absolute ethanol (15 ml) was added slowly to a solution of tpen (1 g, 2.4 mmol) in absolute ethanol (10 ml). The mixture was stirred for 30 min at 333 K and then cooled to room temperature. The white crystals which formed were filtered off and washed with ethanol (5 ml) (yield 1.49 g, 92%). The crystals were recrystallized from a mixture of water and ethanol (1:1 v/v). Analysis, found: C 45.36, H 3.94, N 12.09, Cl 9.51%; calculated for {[C26H28N6Zn](ClO4)2}3·2H2O: C 44.56, H 4.22, N 11.99, Cl 10.18%.

For [Zn(qtpen](ClO4)2, a solution of zinc perchlorate hexahydrate (0.785 g, 2.11 mmol) in absolute ethanol (12 ml) was added slowly to a solution of qtpen (1 g, 2.11 mmol) in absolute ethanol (12 ml), which was heated to 323 K. The mixture was cooled to room temperature and the white crystals which formed were filtered off and washed with ice-cold ethanol (4 ml) (yield 1.4 g, 94%). The crystals were dissolved in boiling water, filtered and cooled to room temperature (yield 1.3 g, 85%). Analysis, found: C 48.83, H 3.79, N 11.37, Cl 9.43%; calculated for [C30H30N6Zn](ClO4)2: C 44.77, H 4.09, N 11.37, Cl 9.60%.

For [Zn(bqbpen)](ClO4)2·H2O, a solution of zinc perchlorate hexahydrate (0.524 g, 1.4 mmol) in absolute ethanol (10 ml) was added slowly to a solution of bqbppen (0.74 g, 1.4 mmol) in absolute ethanol (12 ml), which was heated to 333 K. The mixture was cooled to room temperature and the white crystals which formed were filtered off and washed with ethanol (5 ml) (yield 1 g, 90%). The crystals were dissolved in boiling water, filtered and cooled to room temperature. Analysis, found: C 51.17, H 4.03, N 10.47, Cl 8.73%; calculated for [C34H32N6Zn](ClO4)2·H2O: C 50.60, H 4.25, N 10.41, Cl 8.79%.

Refinement top

Water-bound H atoms were refined isotropically [Range of O—H distances?]. [Contradicts CIF data tables - O-bound H atoms in (I), (II) and (III) are constrained] Carbon-bound H atoms were fixed in calculated positions, with C—H = 0.95 Å and Uiso(H) = 1.2Ueq(C). In (II), one of the perchlorate groups is disordered and was modelled as two interpenetrating regular tetrahedra with a common Cl—O distance and combined occupancy factors of unity for the two tetrahedra. For (III), a Rogers parameter (Rogers, 1981) refined to 0.93 (2), defining the cation as chiral with the Δ configuration in the crystal studied.

Computing details top

For all compounds, data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SIR97 (Altomare et al., 1997) and KRYSTAL (Hazell, 1995); program(s) used to refine structure: ORFLS (Busing et al., 1962; modified) and KRYSTAL (Hazell, 1995); molecular graphics: ORTEPIII (Burnett and Johnson, 1996), KRYSTAL (Hazell, 1995) and PLATON (Spek, 2003); software used to prepare material for publication: KRYSTAL (Hazell, 1995).

Figures top
[Figure 1] Fig. 1. A view of (I) showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level. Most H atoms have been omitted for clarity. The perclorate Cl3 atom is drawn at (1 − x, 1 + y, 3/2 − z) to avoid overlap. Intramolecular C—H···π and O—H···O hydrogen bonds are represented by dashed lines. [Symmetry code: (i) 1 − x, y, 1/2 − z; (ii) x, 1 − y, −1/2 + z.]
[Figure 2] Fig. 2. A view of (II) showing the atom-labelling scheme; atoms Cl1 and Cl1' are superimposed. Displacement ellipsoids are shown at the 50% probability levels. Most H atoms have been omitted for clarity. The intramolecular C—H···π bond is represented by a dashed line.
[Figure 3] Fig. 3. A view of (III), showing the atom-labelling scheme. Perchlorate groups are drawn at (x − 1, y, z). Displacement ellipsoids are drawn at the 50% probability level. H atoms have been omitted for clarity.
[Figure 4] Fig. 4. The correlation between equatorial and axial Zn—N bond lengths for which the distance between an H atom of an axial pyridyl group and the closest equatorial aromatic π-system is lowest. Filled circles: this work; filled squares: compound (IV), [Zn(tpen)]2+ (Mikata et al., 2005). Points for the cations in special positions are shown as open circles for (I) and squares for (IV).
[Figure 5] Fig. 5. A packing diagram for (I), showing the slice (y = 0 to 1/2) perpendicular to the b axis. Intermolecular C—H···π bonds are shown as dashed lines. H atoms have been omitted, except for those of the water molecule and those of the C—H···π bonds.
[Figure 6] Fig. 6. Packing diagram for (II), showing the slice (0, y, 0) to (1/2, y, 1/2) parallel to {1 0 1}. Intermolecular C—H···π bonds are shown as dashed lines. H atoms have been omitted except for those of the C—H···π bonds.
[Figure 7] Fig. 7. Unit-cell contents of (III), viewed down the b axis. H atoms have been omitted for clarity except for those of the water molecule.
(I) [N,N,N',N'-tetrakis(2-pyridylmethyl)ethane-1,2-diamine-κ6N]zinc(II) diperchlorate 0.67-hydrate top
Crystal data top
[Zn(C26H28N6)](ClO4)2·0.67H2OF(000) = 4328.0
Mr = 700.86Dx = 1.603 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 8192 reflections
a = 41.064 (3) Åθ = 1.8–29.8°
b = 9.3590 (7) ŵ = 1.09 mm1
c = 23.785 (2) ÅT = 120 K
β = 107.625 (2)°Block, colourless
V = 8711.9 (12) Å30.41 × 0.26 × 0.08 mm
Z = 12
Data collection top
Siemens SMART CCD area-detector
diffractometer
10019 independent reflections
Radiation source: x-ray tube6179 reflections with I > 2.5σ(I)
Graphite monochromatorRint = 0.063
ω rotation scans with narrow framesθmax = 27.5°, θmin = 1.8°
Absorption correction: integration
(XPREP; Siemens, 1995)
h = 5454
Tmin = 0.681, Tmax = 0.919k = 1213
41218 measured reflectionsl = 3124
Refinement top
Refinement on F0 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.037H-atom parameters constrained
wR(F2) = 0.038 w = 1/{[σcs(F2) + B + (1 + A)F2]1/2-|F|}2
where A = 0.03 and B = 0.5
S = 0.99(Δ/σ)max = 0.003
6179 reflectionsΔρmax = 0.55 (4) e Å3
591 parametersΔρmin = 0.35 (4) e Å3
Crystal data top
[Zn(C26H28N6)](ClO4)2·0.67H2OV = 8711.9 (12) Å3
Mr = 700.86Z = 12
Monoclinic, C2/cMo Kα radiation
a = 41.064 (3) ŵ = 1.09 mm1
b = 9.3590 (7) ÅT = 120 K
c = 23.785 (2) Å0.41 × 0.26 × 0.08 mm
β = 107.625 (2)°
Data collection top
Siemens SMART CCD area-detector
diffractometer
10019 independent reflections
Absorption correction: integration
(XPREP; Siemens, 1995)
6179 reflections with I > 2.5σ(I)
Tmin = 0.681, Tmax = 0.919Rint = 0.063
41218 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0370 restraints
wR(F2) = 0.038H-atom parameters constrained
S = 0.99Δρmax = 0.55 (4) e Å3
6179 reflectionsΔρmin = 0.35 (4) e Å3
591 parameters
Special details top

Refinement. Sfls: F calc weight full matrix

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Zn10.669763 (9)0.24994 (4)0.59094 (2)0.0202 (2)
Zn20.5000000.29968 (6)0.250000.0198 (3)
Cl10.67788 (2)0.73073 (8)0.71405 (4)0.0229 (5)
Cl20.65166 (2)0.72043 (10)0.37534 (4)0.0340 (6)
Cl30.50834 (2)0.18391 (9)0.60638 (4)0.0237 (5)
O10.67150 (7)0.5941 (3)0.7357 (1)0.041 (2)
O20.68619 (6)0.8302 (3)0.7628 (1)0.038 (2)
O30.70622 (7)0.7204 (3)0.6908 (1)0.042 (2)
O40.64802 (7)0.7790 (3)0.6701 (1)0.043 (2)
O50.64101 (10)0.8245 (4)0.4101 (2)0.083 (3)
O60.67075 (10)0.6158 (4)0.4146 (1)0.079 (3)
O70.67339 (9)0.7924 (4)0.3491 (2)0.083 (3)
O80.62397 (9)0.6672 (4)0.3322 (2)0.099 (3)
O90.52684 (10)0.0782 (3)0.5876 (2)0.090 (4)
O100.47742 (8)0.2089 (4)0.5588 (1)0.066 (2)
O110.49856 (7)0.1390 (3)0.6557 (1)0.047 (2)
O120.52683 (6)0.3153 (3)0.6170 (1)0.037 (2)
O130.67950 (9)0.3237 (3)0.3802 (1)0.070 (3)
N10.70714 (6)0.2480 (3)0.6789 (1)0.022 (2)
N20.63440 (7)0.2006 (3)0.6401 (1)0.022 (2)
N30.69408 (7)0.0359 (3)0.5919 (1)0.023 (2)
N40.71103 (7)0.3500 (3)0.5728 (1)0.021 (2)
N50.62857 (7)0.1795 (3)0.5215 (1)0.024 (2)
N60.64201 (7)0.4533 (3)0.5839 (1)0.022 (2)
N70.53684 (7)0.4778 (3)0.2745 (1)0.026 (2)
N80.54605 (7)0.1897 (3)0.2613 (1)0.022 (2)
N90.50799 (7)0.3136 (3)0.3445 (1)0.022 (2)
C10.68679 (8)0.2502 (4)0.7206 (1)0.026 (2)
C20.65616 (9)0.1520 (4)0.6990 (2)0.025 (2)
C30.68734 (9)0.0610 (4)0.5482 (2)0.028 (2)
C40.70974 (10)0.1679 (4)0.5452 (2)0.034 (3)
C50.74100 (10)0.1735 (4)0.5879 (2)0.036 (3)
C60.74845 (9)0.0753 (4)0.6334 (2)0.029 (2)
C70.72385 (9)0.0251 (3)0.6352 (2)0.024 (2)
C80.72962 (9)0.1215 (4)0.6873 (2)0.034 (2)
C90.71683 (9)0.3664 (4)0.5206 (2)0.025 (2)
C100.74628 (9)0.4261 (4)0.5151 (2)0.028 (2)
C110.77120 (9)0.4707 (4)0.5657 (2)0.028 (2)
C120.76535 (8)0.4556 (4)0.6193 (2)0.025 (2)
C130.73520 (8)0.3954 (3)0.6218 (2)0.022 (2)
C140.72656 (8)0.3807 (3)0.6789 (2)0.023 (2)
C150.62333 (9)0.1965 (4)0.4633 (2)0.029 (2)
C160.59540 (9)0.1404 (4)0.4216 (2)0.029 (2)
C170.57175 (9)0.0648 (4)0.4400 (2)0.030 (2)
C180.57622 (9)0.0506 (3)0.4995 (2)0.026 (2)
C190.60513 (8)0.1087 (3)0.5396 (2)0.021 (2)
C200.61315 (9)0.0846 (4)0.6056 (2)0.028 (2)
C210.64351 (8)0.5609 (4)0.5472 (2)0.026 (2)
C220.61850 (9)0.6630 (4)0.5286 (2)0.027 (2)
C230.59037 (9)0.6551 (4)0.5490 (2)0.027 (2)
C240.58833 (8)0.5447 (4)0.5867 (2)0.025 (2)
C250.61449 (8)0.4460 (3)0.6031 (1)0.021 (2)
C260.61381 (9)0.3276 (4)0.6455 (2)0.028 (2)
C270.51785 (10)0.6051 (4)0.2461 (2)0.034 (2)
C280.55232 (9)0.0490 (4)0.2699 (2)0.025 (2)
C290.58431 (9)0.0096 (4)0.2788 (2)0.033 (2)
C300.61089 (10)0.0805 (4)0.2795 (2)0.040 (3)
C310.60482 (9)0.2250 (4)0.2706 (2)0.036 (3)
C320.57228 (9)0.2768 (4)0.2613 (1)0.025 (2)
C330.56386 (9)0.4335 (4)0.2490 (2)0.031 (2)
C340.49215 (8)0.2348 (4)0.3758 (2)0.026 (2)
C350.49819 (9)0.2522 (4)0.4356 (2)0.030 (2)
C360.52075 (10)0.3562 (4)0.4645 (2)0.033 (2)
C370.53750 (10)0.4362 (4)0.4331 (2)0.031 (2)
C380.53074 (9)0.4111 (3)0.3733 (2)0.024 (2)
C390.55044 (10)0.4926 (4)0.3396 (2)0.031 (2)
H1310.674490.41130.38480.100*
H1320.684750.29740.34940.100*
H1a0.679110.34490.72350.031*
H1b0.700610.21900.75830.031*
H2a0.663770.05720.69610.031*
H2b0.643260.15420.72610.031*
H30.666090.05540.51790.034*
H40.703750.23650.51430.041*
H50.757290.24400.58610.043*
H60.770010.07650.66300.035*
H8a0.726410.06700.71880.041*
H8b0.752570.15440.69760.041*
H90.699830.33530.48590.030*
H100.749500.43660.47740.033*
H110.791980.51110.56330.034*
H120.782000.48650.65440.030*
H14a0.747110.37820.71090.028*
H14b0.713180.46020.68330.028*
H150.639560.24920.45050.035*
H160.592440.15360.38080.035*
H170.552550.02280.41200.035*
H180.559720.00160.51290.031*
H20a0.592310.08010.61510.033*
H20b0.625050.00330.61570.033*
H210.662900.56660.53340.031*
H220.620450.73690.50240.033*
H230.572700.72440.53740.033*
H240.569200.53720.60110.030*
H26a0.622440.36380.68450.034*
H26b0.590770.29820.63840.034*
H27a0.514350.60800.20480.041*
H27b0.528020.69200.26350.041*
H280.533920.01260.26990.030*
H290.587890.10960.28440.039*
H300.633270.04350.28600.048*
H310.622980.28820.27100.043*
H33a0.583810.48890.26600.037*
H33b0.556170.44860.20750.037*
H340.476180.16430.35580.031*
H350.486960.19340.45650.036*
H360.524710.37260.50550.040*
H370.553460.50760.45230.037*
H39a0.550070.59100.34920.037*
H39b0.573360.45910.35180.037*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0177 (2)0.0188 (2)0.0225 (2)0.0002 (2)0.0036 (2)0.0001 (2)
Zn20.0251 (3)0.0150 (3)0.0184 (3)0.00000.0052 (2)0.0000
Cl10.0232 (4)0.0160 (4)0.0287 (5)0.0033 (3)0.0066 (4)0.0012 (4)
Cl20.0298 (5)0.0363 (6)0.0357 (6)0.0027 (4)0.0095 (4)0.0016 (4)
Cl30.0272 (5)0.0200 (4)0.0271 (5)0.0035 (4)0.0128 (4)0.0017 (4)
O10.057 (2)0.020 (1)0.059 (2)0.002 (1)0.034 (2)0.008 (1)
O20.036 (2)0.034 (2)0.036 (2)0.002 (1)0.000 (1)0.014 (1)
O30.043 (2)0.037 (2)0.057 (2)0.006 (1)0.031 (1)0.010 (1)
O40.042 (2)0.037 (2)0.037 (2)0.010 (1)0.006 (1)0.004 (1)
O50.115 (3)0.075 (3)0.074 (3)0.037 (2)0.054 (2)0.003 (2)
O60.111 (3)0.060 (2)0.057 (2)0.035 (2)0.012 (2)0.015 (2)
O70.071 (2)0.113 (3)0.071 (3)0.034 (2)0.033 (2)0.006 (2)
O80.066 (2)0.064 (2)0.129 (4)0.025 (2)0.027 (2)0.017 (2)
O90.125 (3)0.037 (2)0.153 (4)0.000 (2)0.109 (3)0.015 (2)
O100.057 (2)0.077 (2)0.048 (2)0.027 (2)0.011 (2)0.017 (2)
O110.072 (2)0.044 (2)0.032 (2)0.028 (2)0.028 (2)0.006 (1)
O120.042 (2)0.030 (1)0.042 (2)0.016 (1)0.018 (1)0.003 (1)
O130.108 (3)0.052 (2)0.041 (2)0.012 (2)0.011 (2)0.007 (2)
N10.023 (1)0.016 (1)0.026 (2)0.002 (1)0.003 (1)0.000 (1)
N20.022 (1)0.020 (1)0.023 (2)0.002 (1)0.004 (1)0.006 (1)
N30.022 (2)0.017 (1)0.028 (2)0.003 (1)0.008 (1)0.004 (1)
N40.019 (1)0.018 (1)0.025 (2)0.002 (1)0.004 (1)0.002 (1)
N50.021 (1)0.025 (2)0.025 (2)0.002 (1)0.005 (1)0.001 (1)
N60.019 (1)0.019 (1)0.026 (2)0.001 (1)0.006 (1)0.002 (1)
N70.038 (2)0.019 (2)0.019 (2)0.005 (1)0.007 (1)0.001 (1)
N80.024 (2)0.022 (1)0.017 (2)0.002 (1)0.005 (1)0.000 (1)
N90.028 (2)0.020 (1)0.018 (2)0.000 (1)0.006 (1)0.001 (1)
C10.028 (2)0.023 (2)0.023 (2)0.000 (2)0.003 (1)0.004 (2)
C20.029 (2)0.022 (2)0.023 (2)0.001 (2)0.005 (2)0.007 (2)
C30.030 (2)0.023 (2)0.036 (2)0.010 (2)0.017 (2)0.006 (2)
C40.051 (3)0.015 (2)0.047 (3)0.009 (2)0.031 (2)0.006 (2)
C50.046 (2)0.016 (2)0.058 (3)0.007 (2)0.034 (2)0.007 (2)
C60.027 (2)0.021 (2)0.043 (3)0.004 (2)0.016 (2)0.012 (2)
C70.024 (2)0.015 (2)0.033 (2)0.001 (1)0.011 (2)0.004 (2)
C80.034 (2)0.024 (2)0.038 (3)0.010 (2)0.001 (2)0.000 (2)
C90.029 (2)0.023 (2)0.024 (2)0.000 (2)0.007 (2)0.002 (2)
C100.032 (2)0.024 (2)0.032 (2)0.001 (2)0.015 (2)0.001 (2)
C110.022 (2)0.024 (2)0.041 (3)0.000 (2)0.011 (2)0.003 (2)
C120.020 (2)0.021 (2)0.031 (2)0.001 (1)0.005 (2)0.001 (2)
C130.021 (2)0.015 (2)0.028 (2)0.005 (1)0.005 (2)0.001 (1)
C140.020 (2)0.020 (2)0.028 (2)0.001 (1)0.004 (2)0.006 (2)
C150.028 (2)0.030 (2)0.029 (2)0.002 (2)0.009 (2)0.000 (2)
C160.025 (2)0.035 (2)0.023 (2)0.001 (2)0.002 (2)0.004 (2)
C170.023 (2)0.026 (2)0.032 (2)0.004 (2)0.001 (2)0.006 (2)
C180.025 (2)0.019 (2)0.032 (2)0.004 (1)0.007 (2)0.002 (2)
C190.020 (2)0.017 (2)0.025 (2)0.002 (1)0.003 (2)0.001 (1)
C200.026 (2)0.023 (2)0.031 (2)0.006 (2)0.005 (2)0.004 (2)
C210.023 (2)0.023 (2)0.033 (2)0.003 (2)0.008 (2)0.002 (2)
C220.030 (2)0.019 (2)0.029 (2)0.003 (2)0.002 (2)0.006 (2)
C230.024 (2)0.019 (2)0.033 (2)0.004 (1)0.001 (2)0.001 (2)
C240.022 (2)0.024 (2)0.030 (2)0.001 (1)0.007 (2)0.003 (2)
C250.021 (2)0.018 (2)0.022 (2)0.002 (1)0.004 (2)0.003 (1)
C260.028 (2)0.026 (2)0.034 (2)0.004 (2)0.015 (2)0.006 (2)
C270.057 (3)0.013 (2)0.029 (2)0.007 (2)0.009 (2)0.002 (2)
C280.027 (2)0.022 (2)0.025 (2)0.004 (2)0.006 (2)0.004 (2)
C290.032 (2)0.030 (2)0.037 (2)0.005 (2)0.012 (2)0.007 (2)
C300.029 (2)0.048 (3)0.046 (3)0.002 (2)0.017 (2)0.015 (2)
C310.030 (2)0.041 (3)0.041 (2)0.009 (2)0.017 (2)0.012 (2)
C320.032 (2)0.026 (2)0.019 (2)0.007 (2)0.011 (2)0.005 (1)
C330.035 (2)0.032 (2)0.026 (2)0.013 (2)0.010 (2)0.001 (2)
C340.028 (2)0.024 (2)0.026 (2)0.002 (2)0.008 (2)0.001 (2)
C350.035 (2)0.033 (2)0.027 (2)0.005 (2)0.015 (2)0.005 (2)
C360.048 (2)0.031 (2)0.020 (2)0.005 (2)0.010 (2)0.004 (2)
C370.041 (2)0.025 (2)0.023 (2)0.002 (2)0.004 (2)0.004 (2)
C380.032 (2)0.019 (2)0.019 (2)0.004 (2)0.004 (2)0.000 (1)
C390.042 (2)0.023 (2)0.026 (2)0.010 (2)0.009 (2)0.007 (2)
Geometric parameters (Å, º) top
Zn1—N12.188 (3)C21—C221.374 (5)
Zn1—N22.173 (3)C22—C231.384 (5)
Zn1—N32.236 (3)C23—C241.387 (5)
Zn1—N42.092 (3)C24—C251.380 (4)
Zn1—N52.082 (3)C25—C261.504 (5)
Zn1—N62.199 (3)C27—C27i1.532 (8)
Zn2—N72.208 (3)C28—C291.380 (5)
Zn2—N7i2.208 (3)C29—C301.376 (5)
Zn2—N82.097 (3)C30—C311.380 (5)
Zn2—N8i2.097 (3)C31—C321.375 (5)
Zn2—N92.175 (3)C32—C331.515 (5)
Zn2—N9i2.175 (3)C34—C351.377 (5)
Cl1—O11.432 (2)C35—C361.376 (5)
Cl1—O21.446 (2)C36—C371.380 (5)
Cl1—O31.435 (2)C37—C381.384 (5)
Cl1—O41.423 (2)C38—C391.507 (5)
Cl2—O51.430 (3)O13—H1310.860
Cl2—O61.415 (3)O13—H1320.860
Cl2—O71.406 (3)C1—H1a0.950
Cl2—O81.374 (3)C1—H1b0.950
Cl3—O91.401 (3)C2—H2b0.950
Cl3—O101.441 (3)C2—H2a0.950
Cl3—O111.414 (3)C3—H30.950
Cl3—O121.428 (2)C4—H40.950
N1—C141.476 (4)C5—H50.950
N1—C81.477 (4)C6—H60.950
N1—C11.478 (4)C8—H8a0.950
N2—C201.476 (4)C8—H8b0.950
N2—C21.486 (4)C9—H90.950
N2—C261.487 (4)C10—H100.950
N3—C71.343 (4)C11—H110.950
N3—C31.343 (4)C12—H120.950
N4—C91.342 (4)C14—H14a0.950
N4—C131.351 (4)C14—H14b0.950
N5—C191.342 (4)C15—H150.950
N5—C151.345 (4)C16—H160.950
N6—C251.342 (4)C17—H170.950
N6—C211.347 (4)C18—H180.950
N7—C271.471 (4)C20—H20a0.950
N7—C331.477 (5)C20—H20b0.950
N7—C391.485 (4)C21—H210.950
N8—C281.345 (4)C22—H220.950
N8—C321.350 (4)C23—H230.950
N9—C381.337 (4)C24—H240.950
N9—C341.346 (4)C26—H26a0.950
C1—C21.516 (4)C26—H26b0.950
C3—C41.376 (5)C27—H27a0.950
C4—C51.375 (5)C27—H27b0.950
C5—C61.382 (5)C28—H280.950
C6—C71.390 (4)C29—H290.950
C7—C81.492 (5)C30—H300.950
C9—C101.375 (5)C31—H310.950
C10—C111.387 (5)C33—H33b0.950
C11—C121.375 (5)C33—H33a0.950
C12—C131.378 (4)C34—H340.950
C13—C141.510 (5)C35—H350.950
C15—C161.373 (5)C36—H360.950
C16—C171.376 (5)C37—H370.950
C17—C181.375 (5)C39—H39a0.950
C18—C191.389 (4)C39—H39b0.950
C19—C201.521 (5)
N1—Zn1—N282.7 (1)N6—C25—C26117.0 (3)
N1—Zn1—N378.5 (1)C24—C25—C26120.7 (3)
N1—Zn1—N479.8 (1)N2—C26—C25113.9 (3)
N1—Zn1—N5157.3 (1)N7—C27—C27i109.8 (3)
N1—Zn1—N6106.1 (1)N8—C28—C29122.9 (3)
N2—Zn1—N3100.0 (1)C28—C29—C30118.2 (3)
N2—Zn1—N4157.1 (1)C29—C30—C31119.6 (3)
N2—Zn1—N581.1 (1)C30—C31—C32119.4 (3)
N2—Zn1—N679.0 (1)N8—C32—C31121.6 (3)
N3—Zn1—N490.9 (1)N8—C32—C33116.7 (3)
N3—Zn1—N588.7 (1)C31—C32—C33121.7 (3)
N3—Zn1—N6175.0 (1)N7—C33—C32110.4 (3)
N4—Zn1—N5119.5 (1)N9—C34—C35122.6 (3)
N4—Zn1—N691.7 (1)C34—C35—C36119.0 (3)
N5—Zn1—N686.3 (1)C35—C36—C37118.9 (3)
N7—Zn2—N7i81.9 (1)C36—C37—C38119.1 (3)
N7—Zn2—N879.5 (1)N9—C38—C37122.3 (3)
N7i—Zn2—N8i79.5 (1)N9—C38—C39118.5 (3)
N7—Zn2—N8i157.5 (1)C37—C38—C39119.2 (3)
N7i—Zn2—N8157.5 (1)N7—C39—C38114.5 (3)
N7—Zn2—N978.7 (1)H131—O13—H132120.7
N7i—Zn2—N9i78.7 (1)H1a—C1—H1b109.5
N7i—Zn2—N996.0 (1)N1—C1—H1a109.3
N7—Zn2—N9i96.0 (1)C2—C1—H1a109.3
N8—Zn2—N8i121.2 (1)N1—C1—H1b109.3
N8—Zn2—N992.8 (1)C2—C1—H1b109.3
N8i—Zn2—N9i92.8 (1)H2a—C2—H2b109.5
N8—Zn2—N9i90.6 (1)N2—C2—H2b109.5
N8i—Zn2—N990.6 (1)C1—C2—H2b109.5
N9—Zn2—N9i173.1 (1)N2—C2—H2a109.5
Zn1—N1—C1105.4 (2)C1—C2—H2a109.5
Zn1—N1—C8111.4 (2)N3—C3—H3118.4
Zn1—N1—C14102.5 (2)C4—C3—H3118.4
Zn1—N2—C20103.6 (2)C5—C4—H4120.7
Zn1—N2—C2105.3 (2)C3—C4—H4120.7
Zn1—N3—C7112.0 (2)C4—C5—H5120.4
Zn1—N2—C26111.5 (2)C6—C5—H5120.3
Zn1—N3—C3127.6 (2)C5—C6—H6120.6
Zn1—N4—C9128.6 (2)C7—C6—H6120.5
Zn1—N4—C13113.1 (2)H8a—C8—H8b109.5
Zn1—N5—C15128.2 (2)N1—C8—H8a107.8
Zn1—N5—C19113.0 (2)C7—C8—H8a107.9
Zn1—N6—C25113.6 (2)N1—C8—H8b107.8
Zn1—N6—C21124.9 (2)C7—C8—H8b107.8
Zn2—N7—C27105.3 (2)N4—C9—H9118.6
Zn2—N7—C33102.7 (2)C10—C9—H9118.6
Zn2—N7—C39110.9 (2)C9—C10—H10120.7
Zn2—N8—C28128.6 (2)C11—C10—H10120.7
Zn2—N8—C32113.1 (2)C12—C11—H11120.5
Zn2—N9—C34126.2 (2)C10—C11—H11120.5
Zn2—N9—C38115.7 (2)C11—C12—H12120.2
O1—Cl1—O2108.1 (2)C13—C12—H12120.2
O1—Cl1—O3109.7 (2)H14a—C14—H14b109.5
O1—Cl1—O4109.7 (2)N1—C14—H14a109.2
O2—Cl1—O3109.3 (2)C13—C14—H14a109.2
O2—Cl1—O4109.1 (1)N1—C14—H14b109.2
O3—Cl1—O4110.9 (2)C13—C14—H14b109.2
O5—Cl2—O6107.2 (2)N5—C15—H15118.8
O5—Cl2—O7106.1 (2)C16—C15—H15118.8
O5—Cl2—O8110.5 (2)C15—C16—H16120.6
O6—Cl2—O7109.0 (2)C17—C16—H16120.6
O6—Cl2—O8114.2 (2)C18—C17—H17120.3
O7—Cl2—O8109.6 (3)C16—C17—H17120.4
O9—Cl3—O10107.4 (2)C17—C18—H18120.4
O9—Cl3—O11111.9 (2)C19—C18—H18120.4
O9—Cl3—O12110.7 (2)H20a—C20—H20b109.5
O10—Cl3—O11107.2 (2)N2—C20—H20a108.9
O10—Cl3—O12107.1 (2)C19—C20—H20a108.9
O11—Cl3—O12112.3 (2)N2—C20—H20b108.9
C8—N1—C14111.0 (3)C19—C20—H20b108.9
C1—N1—C14113.8 (3)N6—C21—H21118.2
C1—N1—C8112.2 (3)C22—C21—H21118.2
C2—N2—C20112.6 (3)C21—C22—H22120.9
C20—N2—C26112.3 (3)C23—C22—H22120.9
C2—N2—C26111.1 (3)C22—C23—H23120.4
C3—N3—C7118.0 (3)C24—C23—H23120.4
C9—N4—C13118.2 (3)C25—C24—H24120.4
C15—N5—C19118.8 (3)C23—C24—H24120.5
C21—N6—C25117.8 (3)H26a—C26—H26b109.5
C27—N7—C33113.5 (3)N2—C26—H26a108.4
C27—N7—C39112.5 (3)C25—C26—H26a108.4
C33—N7—C39111.3 (3)N2—C26—H26b108.3
C28—N8—C32118.3 (3)C25—C26—H26b108.3
C34—N9—C38118.1 (3)H27a—C27—H27b109.4
N1—C1—C2110.1 (3)N7—C27—H27a113.1
N2—C2—C1109.5 (3)C27i—C27—H27a105.9
N3—C3—C4123.1 (3)N7—C27—H27b113.1
C3—C4—C5118.6 (3)C27i—C27—H27b105.0
C4—C5—C6119.3 (3)N8—C28—H28118.6
C5—C6—C7118.9 (3)C29—C28—H28118.6
N3—C7—C6121.9 (3)C30—C29—H29120.9
N3—C7—C8118.1 (3)C28—C29—H29120.9
C6—C7—C8120.0 (3)C29—C30—H30120.2
N1—C8—C7115.9 (3)C31—C30—H30120.2
N4—C9—C10122.9 (3)C32—C31—H31120.3
C9—C10—C11118.6 (3)C30—C31—H31120.3
C10—C11—C12118.9 (3)H33a—C33—H33b109.5
C11—C12—C13119.6 (3)N7—C33—H33b109.3
N4—C13—C12121.8 (3)C32—C33—H33b109.3
N4—C13—C14115.8 (3)N7—C33—H33a109.3
C12—C13—C14122.4 (3)C32—C33—H33a109.2
N1—C14—C13110.6 (3)N9—C34—H34118.7
N5—C15—C16122.4 (3)C35—C34—H34118.7
C15—C16—C17118.9 (4)C36—C35—H35120.5
C16—C17—C18119.3 (3)C34—C35—H35120.5
C17—C18—C19119.2 (3)C35—C36—H36120.5
N5—C19—C18121.3 (3)C37—C36—H36120.6
N5—C19—C20116.9 (3)C36—C37—H37120.4
C18—C19—C20121.6 (3)C38—C37—H37120.4
N2—C20—C19111.8 (3)H39a—C39—H39b109.5
N6—C21—C22123.5 (3)N7—C39—H39a108.2
C21—C22—C23118.1 (3)C38—C39—H39a108.2
C22—C23—C24119.1 (3)N7—C39—H39b108.2
C23—C24—C25119.1 (3)C38—C39—H39b108.2
N6—C25—C24122.3 (3)
Symmetry code: (i) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O13—H131···O60.862.062.907 (5)167
O13—H132···O2ii0.862.403.227 (4)162
C1—H1a···O10.952.383.320 (5)169
C9—H9···O130.952.403.250 (5)149
C12—H12···O2iii0.952.483.134 (5)126
C14—H14b···O30.952.463.321 (4)150
C20—H20a···O90.952.573.439 (6)153
C20—H20b···O4iv0.952.443.355 (5)160
C26—H26b···O120.952.523.430 (5)160
C27—H27a···O12ii0.952.413.287 (5)154
C33—H33a···O80.952.533.440 (6)160
C35—H35···O100.952.583.315 (5)134
C10—H10···Cg3v0.952.703.546 (5)148
C16—H16···Cg80.952.523.454 (5)167
Symmetry codes: (ii) x, y+1, z1/2; (iii) x+3/2, y1/2, z+3/2; (iv) x, y1, z; (v) x+3/2, y+1/2, z+1.
(II) [N,N,N'-tris(2-pyridylmethyl)-N'-(2-quinolmethyl)ethane-1,2-diamine-κ6N]- diperchlorate top
Crystal data top
[Zn(C30H30N6)](ClO4)2F(000) = 1520
Mr = 738.91Dx = 1.620 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 7829 reflections
a = 13.231 (2) Åθ = 1.9–29.7°
b = 15.147 (2) ŵ = 1.05 mm1
c = 15.167 (2) ÅT = 120 K
β = 94.634 (3)°Block, colourless
V = 3029.5 (7) Å30.60 × 0.42 × 0.28 mm
Z = 4
Data collection top
Siemens SMART CCD area-detector
diffractometer
6946 independent reflections
Radiation source: x-ray tube4838 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.026
ω rotation scans with narrow framesθmax = 27.5°, θmin = 1.9°
Absorption correction: integration
(XPREP; Siemens, 1995
h = 1717
Tmin = 0.596, Tmax = 0.778k = 1919
25310 measured reflectionsl = 1919
Refinement top
Refinement on F0 restraints
Least-squares matrix: full78 constraints
R[F2 > 2σ(F2)] = 0.030H-atom parameters constrained
wR(F2) = 0.035 w = 1/{[σcs(F2) + B (1 + A)F2]1/2-|F|}2
where A = 0.03 and B = 5.7
S = 1.00(Δ/σ)max = 0.001
4838 reflectionsΔρmax = 1.43 (7) e Å3
402 parametersΔρmin = 1.18 (7) e Å3
Crystal data top
[Zn(C30H30N6)](ClO4)2V = 3029.5 (7) Å3
Mr = 738.91Z = 4
Monoclinic, P21/nMo Kα radiation
a = 13.231 (2) ŵ = 1.05 mm1
b = 15.147 (2) ÅT = 120 K
c = 15.167 (2) Å0.60 × 0.42 × 0.28 mm
β = 94.634 (3)°
Data collection top
Siemens SMART CCD area-detector
diffractometer
6946 independent reflections
Absorption correction: integration
(XPREP; Siemens, 1995
4838 reflections with I > 3σ(I)
Tmin = 0.596, Tmax = 0.778Rint = 0.026
25310 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.035H-atom parameters constrained
S = 1.00Δρmax = 1.43 (7) e Å3
4838 reflectionsΔρmin = 1.18 (7) e Å3
402 parameters
Special details top

Refinement. Sfls: F calc weight full matrix

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zn10.67198 (2)0.11561 (2)0.83858 (2)0.0157 (1)
Cl10.2116 (2)0.0433 (1)0.5866 (1)0.0266 (2)0.294 (9)
O10.2147 (7)0.0109 (5)0.6631 (4)0.0399 (6)0.294
O20.2772 (8)0.1166 (5)0.6029 (7)0.0632 (10)0.294
O30.1111 (4)0.0737 (7)0.5658 (7)0.0563 (10)0.294
O40.2436 (9)0.0063 (6)0.5145 (4)0.0615 (9)0.294
Cl1'0.2100 (1)0.0434 (1)0.5853 (1)0.0266 (2)0.706
O1'0.2310 (3)0.0208 (2)0.6525 (2)0.0431 (6)0.706
O2'0.2278 (5)0.1290 (1)0.6213 (2)0.0697 (12)0.706
O3'0.1071 (1)0.0362 (4)0.5515 (2)0.0574 (11)0.706
O4'0.2741 (3)0.0290 (3)0.5160 (2)0.0507 (9)0.706
Cl20.39008 (5)0.31530 (4)0.53154 (4)0.0214 (3)
O50.4330 (2)0.3127 (2)0.6212 (1)0.046 (1)
O60.4700 (1)0.3226 (1)0.4729 (1)0.036 (1)
O70.3345 (2)0.2347 (1)0.5125 (1)0.030 (1)
O80.3222 (2)0.3887 (1)0.5180 (2)0.041 (1)
N10.7250 (2)0.2502 (1)0.8678 (1)0.019 (1)
N20.6726 (2)0.1639 (1)0.6998 (1)0.020 (1)
N30.5283 (2)0.1819 (1)0.8551 (1)0.021 (1)
N40.7129 (2)0.1115 (1)0.9807 (1)0.019 (1)
N50.5916 (2)0.0141 (1)0.7643 (1)0.018 (1)
N60.8150 (2)0.0660 (1)0.8061 (1)0.019 (1)
C10.7563 (2)0.2863 (2)0.7838 (2)0.023 (1)
C20.6802 (2)0.2614 (2)0.7070 (2)0.023 (1)
C30.4341 (2)0.1490 (2)0.8376 (2)0.025 (1)
C40.3474 (2)0.1974 (2)0.8460 (2)0.028 (1)
C50.3574 (2)0.2838 (2)0.8747 (2)0.029 (1)
C60.4532 (2)0.3189 (2)0.8924 (2)0.025 (1)
C70.5378 (2)0.2662 (2)0.8819 (2)0.021 (1)
C80.6431 (2)0.3023 (2)0.9037 (2)0.023 (1)
C90.6830 (2)0.0557 (2)1.0427 (2)0.022 (1)
C100.7189 (2)0.0604 (2)1.1306 (2)0.023 (1)
C110.7866 (2)0.1269 (2)1.1568 (2)0.023 (1)
C120.8161 (2)0.1857 (2)1.0945 (2)0.023 (1)
C130.7786 (2)0.1764 (2)1.0066 (2)0.019 (1)
C140.8101 (2)0.2387 (2)0.9358 (2)0.021 (1)
C150.5645 (2)0.0669 (2)0.7956 (2)0.019 (1)
C160.4904 (2)0.1203 (2)0.7492 (2)0.021 (1)
C170.4502 (2)0.0902 (2)0.6649 (2)0.024 (1)
C180.4819 (2)0.0120 (2)0.6328 (2)0.023 (1)
C190.5515 (2)0.0405 (2)0.6854 (2)0.020 (1)
C200.5765 (2)0.1326 (2)0.6552 (2)0.023 (1)
C210.8826 (2)0.0224 (2)0.8616 (2)0.022 (1)
C220.9733 (2)0.0086 (2)0.8355 (2)0.026 (1)
C230.9966 (2)0.0062 (2)0.7492 (2)0.028 (1)
C240.9274 (2)0.0493 (2)0.6920 (2)0.025 (1)
C250.8369 (2)0.0786 (2)0.7221 (2)0.020 (1)
C260.7599 (2)0.1246 (2)0.6587 (2)0.024 (1)
C270.4600 (2)0.1999 (2)0.7885 (2)0.026 (1)
C280.5042 (2)0.2259 (2)0.8691 (2)0.027 (1)
C290.5825 (2)0.1756 (2)0.9121 (2)0.026 (1)
C300.6127 (2)0.0976 (2)0.8765 (2)0.023 (1)
H1a0.82110.26320.77330.028*
H1b0.76030.34880.78820.028*
H2a0.61570.28520.71700.027*
H2b0.70200.28480.65360.027*
H30.42720.08940.81840.030*
H40.28220.17200.83260.034*
H50.29910.31880.88190.035*
H60.46150.37840.91180.030*
H8a0.64540.36050.88050.028*
H8b0.65540.30430.96620.028*
H90.63490.01111.02520.026*
H100.69760.01891.17220.028*
H110.81240.13181.21690.028*
H120.86170.23231.11140.027*
H14a0.82800.29430.96160.026*
H14b0.86680.21480.90940.026*
H170.40130.12480.63090.029*
H180.45740.00740.57550.028*
H20a0.58190.13200.59310.027*
H20b0.52350.17160.66850.027*
H210.86690.01260.92090.027*
H221.01910.03950.87600.032*
H231.05950.01310.73000.033*
H240.94120.05890.63220.030*
H26a0.79370.17060.63010.028*
H26b0.73450.08270.61590.028*
H270.40880.23550.75880.031*
H280.48160.27830.89600.033*
H290.61510.19580.96640.032*
H300.66580.06410.90620.027*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0164 (1)0.0161 (1)0.0146 (1)0.0007 (1)0.0007 (1)0.0002 (1)
Cl10.0301 (2)0.0212 (2)0.0297 (2)0.0026 (1)0.0098 (1)0.0053 (1)
O10.0290 (7)0.0488 (6)0.0433 (3)0.0041 (5)0.0108 (4)0.0247 (4)
O20.0828 (12)0.0511 (7)0.0546 (11)0.0367 (10)0.0012 (7)0.0095 (5)
O30.0346 (2)0.0852 (16)0.0520 (7)0.0196 (6)0.0201 (3)0.0437 (9)
O40.0930 (13)0.0489 (8)0.0463 (4)0.0185 (8)0.0289 (6)0.0058 (5)
Cl1'0.0301 (2)0.0212 (2)0.0297 (2)0.0026 (1)0.0098 (1)0.0053 (1)
O1'0.0353 (9)0.0453 (4)0.0505 (4)0.0087 (4)0.0147 (4)0.0276 (4)
O2'0.1189 (19)0.0294 (2)0.0626 (8)0.0135 (5)0.0176 (9)0.0092 (3)
O3'0.0336 (2)0.0949 (17)0.0437 (7)0.0137 (4)0.0027 (3)0.0389 (8)
O4'0.0517 (7)0.0644 (13)0.0393 (4)0.0241 (8)0.0236 (5)0.0147 (6)
Cl20.0239 (3)0.0223 (3)0.0177 (3)0.0006 (3)0.0005 (2)0.0024 (2)
O50.070 (2)0.044 (1)0.021 (1)0.017 (1)0.012 (1)0.004 (1)
O60.023 (1)0.049 (1)0.038 (1)0.003 (1)0.008 (1)0.009 (1)
O70.032 (1)0.028 (1)0.029 (1)0.007 (1)0.004 (1)0.004 (1)
O80.044 (1)0.030 (1)0.051 (1)0.013 (1)0.015 (1)0.012 (1)
N10.019 (1)0.019 (1)0.018 (1)0.001 (1)0.000 (1)0.001 (1)
N20.020 (1)0.022 (1)0.017 (1)0.001 (1)0.001 (1)0.003 (1)
N30.019 (1)0.023 (1)0.021 (1)0.001 (1)0.003 (1)0.000 (1)
N40.022 (1)0.019 (1)0.017 (1)0.000 (1)0.001 (1)0.001 (1)
N50.019 (1)0.019 (1)0.017 (1)0.000 (1)0.001 (1)0.001 (1)
N60.020 (1)0.019 (1)0.018 (1)0.000 (1)0.002 (1)0.000 (1)
C10.025 (1)0.020 (1)0.025 (1)0.004 (1)0.003 (1)0.004 (1)
C20.026 (1)0.022 (1)0.021 (1)0.001 (1)0.002 (1)0.006 (1)
C30.021 (1)0.030 (1)0.024 (1)0.003 (1)0.003 (1)0.000 (1)
C40.020 (1)0.039 (2)0.025 (1)0.001 (1)0.003 (1)0.008 (1)
C50.025 (1)0.034 (2)0.028 (1)0.010 (1)0.009 (1)0.014 (1)
C60.030 (1)0.023 (1)0.022 (1)0.006 (1)0.008 (1)0.008 (1)
C70.025 (1)0.021 (1)0.016 (1)0.001 (1)0.004 (1)0.003 (1)
C80.027 (1)0.019 (1)0.024 (1)0.001 (1)0.002 (1)0.002 (1)
C90.025 (1)0.020 (1)0.021 (1)0.003 (1)0.005 (1)0.003 (1)
C100.027 (1)0.022 (1)0.020 (1)0.003 (1)0.006 (1)0.001 (1)
C110.025 (1)0.026 (1)0.019 (1)0.005 (1)0.001 (1)0.002 (1)
C120.021 (1)0.023 (1)0.024 (1)0.002 (1)0.001 (1)0.004 (1)
C130.017 (1)0.019 (1)0.020 (1)0.002 (1)0.001 (1)0.001 (1)
C140.020 (1)0.021 (1)0.023 (1)0.004 (1)0.002 (1)0.001 (1)
C150.021 (1)0.017 (1)0.019 (1)0.001 (1)0.005 (1)0.003 (1)
C160.020 (1)0.020 (1)0.024 (1)0.000 (1)0.005 (1)0.005 (1)
C170.021 (1)0.026 (1)0.026 (1)0.001 (1)0.001 (1)0.007 (1)
C180.022 (1)0.030 (1)0.018 (1)0.002 (1)0.003 (1)0.002 (1)
C190.020 (1)0.023 (1)0.018 (1)0.000 (1)0.002 (1)0.001 (1)
C200.023 (1)0.025 (1)0.019 (1)0.001 (1)0.003 (1)0.004 (1)
C210.026 (1)0.021 (1)0.020 (1)0.000 (1)0.000 (1)0.001 (1)
C220.026 (1)0.021 (1)0.031 (1)0.006 (1)0.002 (1)0.002 (1)
C230.026 (1)0.024 (1)0.034 (2)0.005 (1)0.009 (1)0.000 (1)
C240.030 (1)0.020 (1)0.026 (1)0.000 (1)0.009 (1)0.000 (1)
C250.023 (1)0.017 (1)0.021 (1)0.003 (1)0.003 (1)0.002 (1)
C260.024 (1)0.028 (1)0.019 (1)0.000 (1)0.005 (1)0.002 (1)
C270.026 (1)0.021 (1)0.030 (1)0.003 (1)0.005 (1)0.007 (1)
C280.036 (2)0.017 (1)0.031 (1)0.001 (1)0.011 (1)0.002 (1)
C290.038 (2)0.021 (1)0.021 (1)0.004 (1)0.004 (1)0.000 (1)
C300.028 (1)0.019 (1)0.021 (1)0.001 (1)0.002 (1)0.003 (1)
Geometric parameters (Å, º) top
Zn1—N12.189 (2)C15—C301.415 (4)
Zn1—N22.229 (2)C16—C271.416 (4)
Zn1—N32.182 (2)C16—C171.419 (4)
Zn1—N42.181 (2)C17—C181.360 (4)
Zn1—N52.138 (2)C18—C191.412 (4)
Zn1—N62.131 (2)C19—C201.514 (4)
Cl1—O11.419 (2)C21—C221.376 (4)
Cl1—O21.419 (1)C22—C231.386 (4)
Cl1—O31.419 (1)C23—C241.375 (4)
Cl1—O41.419 (1)C24—C251.388 (4)
Cl1'—O1'1.419 (2)C25—C261.514 (4)
Cl1'—O2'1.419 (1)C27—C281.370 (4)
Cl1'—O3'1.419 (1)C28—C291.404 (4)
Cl1'—O4'1.419 (1)C29—C301.371 (4)
Cl2—O51.432 (2)C1—H1a0.95
Cl2—O61.439 (2)C1—H1b0.95
Cl2—O71.442 (2)C2—H2a0.95
Cl2—O81.433 (2)C2—H2b0.95
N1—C11.476 (3)C3—H30.95
N1—C81.480 (3)C4—H40.95
N1—C141.474 (3)C5—H50.95
N2—C21.484 (3)C6—H60.95
N2—C201.469 (3)C8—H8a0.95
N2—C261.480 (3)C8—H8b0.95
N3—C31.349 (3)C9—H90.95
N3—C71.342 (3)C10—H100.95
N4—C91.347 (3)C11—H110.95
N4—C131.349 (3)C12—H120.95
N5—C151.374 (3)C14—H14a0.95
N5—C191.331 (3)C14—H14b0.95
N6—C211.349 (3)C17—H170.95
N6—C251.343 (3)C18—H180.95
C1—C21.525 (4)C20—H20a0.95
C3—C41.377 (4)C20—H20b0.95
C4—C51.382 (4)C21—H210.95
C5—C61.381 (4)C22—H220.95
C6—C71.394 (4)C23—H230.95
C7—C81.508 (4)C24—H240.95
C9—C101.380 (4)C26—H26a0.95
C10—C111.384 (4)C26—H26b0.95
C11—C121.378 (4)C27—H270.95
C12—C131.392 (3)C28—H280.95
C13—C141.514 (4)C29—H290.95
C15—C161.415 (4)C30—H300.95
N1—Zn1—N281.96 (8)N5—C19—C18122.2 (2)
N1—Zn1—N379.40 (8)N5—C19—C20117.9 (2)
N1—Zn1—N477.10 (8)C18—C19—C20119.8 (2)
N1—Zn1—N5156.04 (8)N2—C20—C19111.1 (2)
N1—Zn1—N695.70 (8)N6—C21—C22122.5 (2)
N2—Zn1—N391.57 (8)C21—C22—C23118.8 (2)
N2—Zn1—N4157.43 (8)C22—C23—C24119.1 (2)
N2—Zn1—N577.16 (8)C23—C24—C25119.4 (2)
N2—Zn1—N680.01 (8)N6—C25—C24121.6 (2)
N3—Zn1—N492.77 (8)N6—C25—C26118.8 (2)
N3—Zn1—N589.47 (8)C24—C25—C26119.5 (2)
N3—Zn1—N6170.83 (8)N2—C26—C25115.2 (2)
N4—Zn1—N5125.00 (8)C16—C27—C28120.4 (2)
N4—Zn1—N693.69 (8)C27—C28—C29120.2 (2)
N5—Zn1—N692.16 (8)C28—C29—C30120.9 (2)
Zn1—N1—C1106.2 (1)C15—C30—C29119.9 (2)
Zn1—N1—C8109.8 (2)H1a—C1—H1b109.4
Zn1—N1—C14104.3 (1)N1—C1—H1b109.1
Zn1—N2—C2105.2 (1)C2—C1—H1b109.2
Zn1—N2—C20105.1 (1)N1—C1—H1a109.1
Zn1—N2—C26109.2 (1)C2—C1—H1a109.2
Zn1—N3—C3127.3 (2)H2a—C2—H2b109.4
Zn1—N3—C7114.3 (2)N2—C2—H2a109.4
Zn1—N4—C9130.2 (2)C1—C2—H2a109.4
Zn1—N4—C13111.7 (2)N2—C2—H2b109.4
Zn1—N5—C15126.3 (2)C1—C2—H2b109.3
Zn1—N5—C19113.8 (2)N3—C3—H3118.4
Zn1—N6—C21125.8 (2)C4—C3—H3118.3
Zn1—N6—C25115.6 (2)C3—C4—H4120.9
O1—Cl1—O2109.47 (2)C5—C4—H4120.8
O1—Cl1—O3109.47 (2)C6—C5—H5120.3
O1—Cl1—O4109.47 (2)C4—C5—H5120.4
O2—Cl1—O3109.47 (1)C5—C6—H6120.4
O2—Cl1—O4109.47 (1)C7—C6—H6120.3
O3—Cl1—O4109.47 (6)H8a—C8—H8b109.4
O1'—Cl1'—O2'109.47 (2)N1—C8—H8b108.2
O1'—Cl1'—O3'109.47 (2)C7—C8—H8b108.2
O1'—Cl1'—O4'109.47 (2)N1—C8—H8a108.2
O2'—Cl1'—O3'109.47 (1)C7—C8—H8a108.2
O2'—Cl1'—O4'109.47 (1)N4—C9—H9118.5
O3'—Cl1'—O4'109.47 (6)C10—C9—H9118.5
O5—Cl2—O6109.5 (1)C9—C10—H10120.6
O5—Cl2—O7108.8 (1)C11—C10—H10120.7
O5—Cl2—O8110.7 (1)C12—C11—H11120.5
O6—Cl2—O7109.3 (1)C10—C11—H11120.5
O6—Cl2—O8109.6 (1)C11—C12—H12120.3
O7—Cl2—O8108.9 (1)C13—C12—H12120.2
C1—N1—C8112.6 (2)H14a—C14—H14b109.4
C1—N1—C14113.3 (2)N1—C14—H14a109.6
C8—N1—C14110.3 (2)C13—C14—H14a109.6
C2—N2—C20113.9 (2)N1—C14—H14b109.5
C2—N2—C26112.4 (2)C13—C14—H14b109.4
C20—N2—C26110.6 (2)C18—C17—H17120.1
C3—N3—C7118.3 (2)C16—C17—H17120.0
C9—N4—C13118.2 (2)C17—C18—H18120.2
C15—N5—C19118.9 (2)C19—C18—H18120.1
C21—N6—C25118.6 (2)H20a—C20—H20b109.4
N1—C1—C2110.7 (2)N2—C20—H20a109.2
N2—C2—C1109.9 (2)C19—C20—H20a109.0
N3—C3—C4123.3 (3)N2—C20—H20b109.1
C3—C4—C5118.3 (3)C19—C20—H20b109.0
C4—C5—C6119.3 (3)N6—C21—H21118.7
C5—C6—C7119.3 (3)C22—C21—H21118.8
N3—C7—C6121.5 (2)C21—C22—H22120.4
N3—C7—C8118.3 (2)C23—C22—H22120.8
C6—C7—C8120.2 (2)C24—C23—H23120.5
N1—C8—C7114.6 (2)C22—C23—H23120.5
N4—C9—C10123.0 (2)C23—C24—H24120.4
C9—C10—C11118.6 (2)C25—C24—H24120.2
C10—C11—C12119.1 (2)H26a—C26—H26b109.3
C11—C12—C13119.5 (2)N2—C26—H26b108.2
N4—C13—C12121.6 (2)C25—C26—H26b108.0
N4—C13—C14117.2 (2)N2—C26—H26a108.1
C12—C13—C14121.2 (2)C25—C26—H26a108.0
N1—C14—C13109.3 (2)C28—C27—H27119.7
N5—C15—C16121.9 (2)C16—C27—H27119.9
N5—C15—C30118.8 (2)C27—C28—H28119.8
C16—C15—C30119.3 (2)C29—C28—H28120.0
C15—C16—C27119.1 (2)C30—C29—H29119.5
C15—C16—C17117.3 (2)C28—C29—H29119.6
C17—C16—C27123.6 (2)C29—C30—H30120.1
C16—C17—C18119.9 (2)C15—C30—H30120.0
C17—C18—C19119.6 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C5—H5···O1i0.952.513.194 (4)129
C17—H17···O70.952.553.448 (3)157
C18—H18···O40.952.543.209 (3)128
C20—H20a···O7ii0.952.553.276 (3)134
C21—H21···O8iii0.952.493.266 (3)139
C27—H27···O50.952.433.053 (3)123
C3—H3···Cg50.952.853.639 (3)141
C29—H29···Cg3iv0.952.793.538 (3)136
Symmetry codes: (i) x+1/2, y+1/2, z+3/2; (ii) x+1, y, z+1; (iii) x+1/2, y1/2, z+1/2; (iv) x+1, y, z+2.
(III) [N,N'-bis(2-pyridylmethyl)-N,N'-bis(2-quinolmethyl)ethane-1,2-diamine-κ6N]- zinc(II) diperchlorate monohydrate top
Crystal data top
[Zn(C34H32N6)](ClO4)2·H2OF(000) = 1664
Mr = 806.99Dx = 1.573 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 8135 reflections
a = 11.891 (3) Åθ = 1.9–29.7°
b = 12.022 (3) ŵ = 0.94 mm1
c = 23.838 (5) ÅT = 120 K
V = 3407.8 (14) Å3Block, colourless
Z = 40.54 × 0.38 × 0.30 mm
Data collection top
Siemens SMART CCD area-detector
diffractometer
7803 independent reflections
Radiation source: x-ray tube6872 reflections with I > 2.5σ(I)
Graphite monochromatorRint = 0.064
ω rotation scans with narrow framesθmax = 27.5°, θmin = 1.9°
Absorption correction: integration
(XPREP; Siemens, 1995)
h = 1515
Tmin = 0.664, Tmax = 0.774k = 1515
28487 measured reflectionsl = 2430
Refinement top
Refinement on F0 constraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.033 w = 1/{[σcs(F2) + B + (1 + A)F2]1/2-|F|}2
where A = 0.03 and B = 0.51
wR(F2) = 0.038(Δ/σ)max = 0.006
S = 1.00Δρmax = 1.15 (9) e Å3
6872 reflectionsΔρmin = 0.59 (9) e Å3
470 parametersAbsolute structure: Rogers factor refined for 2959 Bijvoet pairs where both members have I > 3σ(I)
For the crystal studied, N1 and N2 have the S configuration
0 restraintsRogers parameter: 0.93 (2)
Crystal data top
[Zn(C34H32N6)](ClO4)2·H2OV = 3407.8 (14) Å3
Mr = 806.99Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 11.891 (3) ŵ = 0.94 mm1
b = 12.022 (3) ÅT = 120 K
c = 23.838 (5) Å0.54 × 0.38 × 0.30 mm
Data collection top
Siemens SMART CCD area-detector
diffractometer
7803 independent reflections
Absorption correction: integration
(XPREP; Siemens, 1995)
6872 reflections with I > 2.5σ(I)
Tmin = 0.664, Tmax = 0.774Rint = 0.064
28487 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.033H-atom parameters constrained
wR(F2) = 0.038Δρmax = 1.15 (9) e Å3
S = 1.00Δρmin = 0.59 (9) e Å3
6872 reflectionsAbsolute structure: Rogers factor refined for 2959 Bijvoet pairs where both members have I > 3σ(I)
For the crystal studied, N1 and N2 have the S configuration
470 parametersRogers parameter: 0.93 (2)
0 restraints
Special details top

Refinement. Sfls: F calc weight full matrix

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Zn10.34767 (3)0.90694 (3)0.64272 (1)0.0220 (1)
Cl10.01330 (7)0.18957 (6)0.53900 (3)0.0296 (4)
Cl20.14471 (9)0.66346 (8)0.63062 (3)0.0469 (5)
O10.0131 (2)0.1406 (2)0.5940 (1)0.039 (1)
O20.1191 (2)0.1693 (2)0.5115 (1)0.042 (1)
O30.0035 (3)0.3083 (2)0.5441 (1)0.069 (2)
O40.0760 (2)0.1426 (2)0.5066 (1)0.046 (1)
O50.0618 (2)0.6516 (3)0.6743 (1)0.063 (2)
O60.1735 (4)0.5589 (2)0.6069 (1)0.094 (3)
O70.2457 (3)0.7122 (4)0.6558 (1)0.090 (3)
O80.1056 (3)0.7368 (2)0.5880 (1)0.058 (2)
O90.0754 (3)0.4863 (3)0.6044 (2)0.098 (3)
N10.3494 (2)0.9623 (2)0.5545 (1)0.028 (1)
N20.1809 (2)0.8480 (2)0.6149 (1)0.028 (1)
N30.2940 (2)1.0734 (2)0.6553 (1)0.024 (1)
N40.5234 (2)0.9624 (2)0.6291 (1)0.026 (1)
N50.2633 (2)0.8509 (2)0.7207 (1)0.023 (1)
N60.3915 (2)0.7409 (2)0.6222 (1)0.028 (1)
C10.2576 (3)0.9044 (3)0.5244 (1)0.036 (2)
C20.1546 (3)0.9019 (3)0.5610 (1)0.032 (1)
C30.2599 (2)1.1198 (2)0.7036 (1)0.027 (2)
C40.2200 (3)1.2268 (3)0.7072 (1)0.032 (2)
C50.2135 (3)1.2883 (2)0.6580 (1)0.033 (2)
C60.2484 (3)1.2431 (2)0.6081 (1)0.028 (2)
C70.2897 (2)1.1339 (2)0.6079 (1)0.024 (1)
C80.3347 (3)1.0855 (3)0.5542 (1)0.030 (1)
C90.6073 (3)0.9875 (2)0.6674 (1)0.025 (1)
C100.7217 (3)0.9980 (2)0.6511 (1)0.033 (2)
C110.7477 (3)0.9877 (3)0.5936 (2)0.045 (2)
C120.6637 (3)0.9702 (3)0.5564 (1)0.042 (2)
C130.5524 (3)0.9570 (3)0.5751 (1)0.030 (2)
C140.4617 (3)0.9317 (3)0.5328 (1)0.034 (2)
C150.3089 (2)0.8255 (2)0.7719 (1)0.024 (1)
C160.2416 (3)0.8177 (2)0.8211 (1)0.030 (2)
C170.1250 (3)0.8307 (3)0.8149 (1)0.039 (2)
C180.0797 (3)0.8480 (3)0.7630 (1)0.038 (2)
C190.1510 (3)0.8586 (2)0.7165 (1)0.028 (1)
C200.1025 (3)0.8815 (2)0.6596 (1)0.030 (2)
C210.4961 (3)0.6962 (3)0.6216 (1)0.034 (2)
C220.5174 (3)0.5904 (3)0.6021 (1)0.039 (2)
C230.4290 (4)0.5278 (3)0.5829 (1)0.046 (2)
C240.3210 (3)0.5700 (3)0.5840 (1)0.038 (2)
C250.3041 (3)0.6785 (3)0.6048 (1)0.031 (2)
C260.1870 (3)0.7247 (2)0.6101 (1)0.033 (2)
C270.2937 (3)0.7944 (3)0.8728 (1)0.036 (2)
C280.4064 (3)0.7766 (3)0.8756 (1)0.036 (2)
C290.4729 (3)0.7802 (2)0.8269 (1)0.032 (2)
C300.4256 (3)0.8045 (2)0.7763 (1)0.028 (2)
C310.8035 (3)1.0221 (3)0.6929 (2)0.038 (2)
C320.7733 (3)1.0346 (3)0.7475 (1)0.036 (2)
C330.6599 (3)1.0269 (2)0.7630 (1)0.033 (2)
C340.5787 (3)1.0049 (2)0.7241 (1)0.027 (2)
H910.03300.42630.58830.100*
H920.01170.52660.62050.100*
H1a0.24110.94280.49060.043*
H1b0.28010.83040.51590.043*
H2a0.09680.86130.54250.039*
H2b0.12980.97580.56760.039*
H30.26351.07650.73690.032*
H40.19771.25770.74210.038*
H50.18471.36210.65890.039*
H60.24451.28490.57430.033*
H8a0.40591.11840.54690.036*
H8b0.28411.10400.52480.036*
H110.82330.99290.58120.054*
H120.68000.96680.51750.050*
H14a0.46270.85430.52470.041*
H14b0.47600.97260.49950.041*
H170.07750.82750.84690.046*
H180.00050.85280.75840.045*
H20a0.08760.95890.65630.037*
H20b0.03430.84110.65550.037*
H210.55720.73960.63510.041*
H220.59170.56140.60190.047*
H230.44210.45490.56890.055*
H240.25930.52690.57090.046*
H26a0.15350.69340.64270.040*
H26b0.14540.70280.57790.040*
H270.24970.79100.90610.043*
H280.44070.76170.91080.043*
H290.55120.76550.82930.038*
H300.47150.80750.74370.033*
H310.88021.02960.68260.046*
H320.82901.04860.77510.043*
H330.63921.03710.80110.040*
H340.50221.00130.73530.032*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0254 (1)0.0231 (1)0.0175 (1)0.0017 (1)0.0007 (1)0.0002 (1)
Cl10.0334 (4)0.0305 (4)0.0249 (3)0.0062 (3)0.0065 (3)0.0009 (3)
Cl20.0551 (5)0.0530 (5)0.0326 (4)0.0194 (5)0.0010 (4)0.0058 (3)
O10.043 (1)0.050 (1)0.023 (1)0.004 (1)0.002 (1)0.002 (1)
O20.035 (1)0.054 (1)0.038 (1)0.009 (1)0.014 (1)0.008 (1)
O30.097 (2)0.028 (1)0.083 (2)0.004 (1)0.040 (2)0.002 (1)
O40.039 (1)0.071 (2)0.027 (1)0.015 (1)0.004 (1)0.010 (1)
O50.049 (2)0.080 (2)0.059 (2)0.012 (1)0.007 (1)0.018 (2)
O60.176 (4)0.045 (2)0.060 (2)0.027 (2)0.033 (2)0.002 (1)
O70.056 (2)0.148 (4)0.065 (2)0.017 (2)0.004 (2)0.006 (2)
O80.073 (2)0.052 (2)0.049 (2)0.014 (1)0.004 (1)0.005 (1)
O90.084 (3)0.069 (2)0.142 (4)0.001 (2)0.023 (3)0.002 (2)
N10.036 (1)0.030 (1)0.019 (1)0.004 (1)0.001 (1)0.001 (1)
N20.031 (1)0.027 (1)0.025 (1)0.001 (1)0.007 (1)0.002 (1)
N30.025 (1)0.027 (1)0.020 (1)0.002 (1)0.003 (1)0.001 (1)
N40.031 (1)0.027 (1)0.019 (1)0.005 (1)0.003 (1)0.001 (1)
N50.026 (1)0.020 (1)0.023 (1)0.001 (1)0.001 (1)0.001 (1)
N60.036 (1)0.029 (1)0.020 (1)0.007 (1)0.001 (1)0.002 (1)
C10.053 (2)0.034 (2)0.021 (1)0.003 (2)0.012 (1)0.001 (1)
C20.036 (2)0.033 (1)0.028 (1)0.004 (2)0.013 (1)0.003 (1)
C30.028 (2)0.027 (2)0.025 (1)0.003 (1)0.004 (1)0.001 (1)
C40.032 (2)0.031 (2)0.033 (2)0.000 (1)0.007 (1)0.005 (1)
C50.033 (2)0.023 (1)0.041 (2)0.001 (1)0.001 (1)0.002 (1)
C60.027 (2)0.026 (1)0.030 (2)0.003 (1)0.005 (1)0.005 (1)
C70.023 (2)0.023 (1)0.026 (1)0.000 (1)0.003 (1)0.001 (1)
C80.039 (2)0.031 (1)0.021 (1)0.002 (2)0.000 (1)0.002 (1)
C90.031 (2)0.023 (1)0.021 (1)0.001 (1)0.001 (1)0.001 (1)
C100.035 (2)0.030 (2)0.034 (2)0.001 (1)0.003 (1)0.005 (1)
C110.033 (2)0.057 (2)0.043 (2)0.003 (2)0.017 (2)0.008 (2)
C120.044 (2)0.055 (2)0.027 (2)0.000 (2)0.018 (2)0.000 (1)
C130.039 (2)0.030 (2)0.022 (1)0.005 (1)0.006 (1)0.001 (1)
C140.047 (2)0.038 (2)0.017 (1)0.011 (1)0.002 (1)0.000 (1)
C150.032 (2)0.018 (1)0.021 (1)0.000 (1)0.002 (1)0.000 (1)
C160.042 (2)0.024 (1)0.025 (1)0.003 (1)0.006 (1)0.001 (1)
C170.036 (2)0.047 (2)0.033 (2)0.002 (1)0.015 (1)0.003 (1)
C180.026 (2)0.043 (2)0.044 (2)0.001 (1)0.007 (1)0.005 (2)
C190.029 (1)0.023 (1)0.031 (1)0.001 (1)0.001 (1)0.001 (1)
C200.028 (2)0.029 (2)0.035 (2)0.001 (1)0.005 (1)0.003 (1)
C210.038 (2)0.038 (2)0.027 (1)0.014 (2)0.004 (1)0.001 (1)
C220.047 (2)0.040 (2)0.031 (2)0.018 (2)0.006 (1)0.000 (2)
C230.075 (3)0.035 (2)0.027 (2)0.020 (2)0.004 (2)0.007 (1)
C240.058 (2)0.033 (2)0.023 (1)0.010 (1)0.014 (1)0.005 (1)
C250.046 (2)0.028 (1)0.018 (1)0.005 (1)0.010 (1)0.003 (1)
C260.043 (2)0.025 (1)0.032 (2)0.001 (1)0.012 (1)0.003 (1)
C270.054 (2)0.036 (2)0.019 (2)0.004 (2)0.005 (1)0.001 (1)
C280.055 (2)0.031 (2)0.022 (2)0.005 (2)0.009 (1)0.001 (1)
C290.037 (2)0.029 (2)0.029 (2)0.005 (1)0.007 (1)0.000 (1)
C300.033 (2)0.027 (1)0.024 (1)0.000 (1)0.000 (1)0.000 (1)
C310.028 (2)0.035 (2)0.051 (2)0.001 (1)0.002 (2)0.006 (2)
C320.038 (2)0.031 (2)0.040 (2)0.005 (1)0.013 (2)0.004 (1)
C330.044 (2)0.028 (1)0.028 (1)0.003 (2)0.003 (2)0.001 (1)
C340.031 (2)0.027 (1)0.023 (1)0.002 (1)0.001 (1)0.002 (1)
Geometric parameters (Å, º) top
Zn1—N12.205 (2)C22—C231.371 (5)
Zn1—N22.208 (2)C23—C241.382 (5)
Zn1—N32.122 (2)C24—C251.410 (4)
Zn1—N42.217 (3)C25—C261.505 (5)
Zn1—N52.217 (2)C27—C161.407 (4)
Zn1—N62.121 (2)C28—C271.359 (5)
Cl1—O11.437 (2)C29—C281.405 (5)
Cl1—O21.440 (2)C30—C291.364 (4)
Cl1—O31.447 (3)C31—C101.422 (5)
Cl1—O41.429 (2)C32—C311.357 (5)
Cl2—O51.441 (3)C33—C321.401 (5)
Cl2—O61.421 (3)C34—C331.365 (4)
Cl2—O81.423 (3)O9—H910.96
Cl2—O71.465 (3)O9—H920.98
N1—C11.481 (4)C2—H2b0.95
N1—C81.492 (4)C2—H2a0.95
N1—C141.478 (4)C1—H1b0.95
N2—C21.474 (4)C1—H1a0.95
N2—C201.473 (4)C30—H300.95
N2—C261.489 (4)C29—H290.95
N3—C31.342 (4)C28—H280.95
N3—C71.346 (4)C27—H270.95
N4—C91.385 (4)C17—H170.95
N4—C131.336 (4)C18—H180.95
N5—C151.371 (4)C20—H20a0.95
N5—C191.343 (4)C20—H20b0.95
N6—C211.355 (4)C21—H210.95
N6—C251.347 (4)C22—H220.95
C1—C21.504 (5)C23—H230.95
C3—C41.374 (4)C24—H240.95
C4—C51.388 (4)C26—H26a0.95
C5—C61.374 (4)C26—H26b0.95
C6—C71.401 (4)C34—H340.95
C7—C81.505 (4)C33—H330.95
C9—C101.420 (4)C32—H320.95
C9—C341.410 (4)C31—H310.95
C10—C111.411 (5)C11—H110.95
C11—C121.352 (5)C12—H120.95
C12—C131.404 (5)C14—H14b0.95
C13—C141.507 (4)C14—H14a0.95
C15—C301.415 (4)C3—H30.95
C15—C161.423 (4)C4—H40.95
C16—C171.404 (5)C5—H50.95
C17—C181.366 (5)C6—H60.95
C18—C191.401 (4)C8—H8b0.95
C19—C201.499 (4)C8—H8a0.95
C21—C221.378 (5)
N1—Zn1—N279.6 (1)C9—C10—C31118.8 (3)
N1—Zn1—N381.57 (9)C31—C10—C11123.3 (3)
N1—Zn1—N476.18 (9)C10—C11—C12119.3 (3)
N1—Zn1—N5153.5 (1)C11—C12—C13120.4 (3)
N1—Zn1—N693.57 (9)C12—C13—C14119.1 (3)
N2—Zn1—N394.32 (9)C30—C15—C16118.7 (3)
N2—Zn1—N4154.04 (9)C15—C16—C17117.5 (3)
N2—Zn1—N575.40 (9)C27—C16—C17123.3 (3)
N2—Zn1—N681.3 (1)C15—C16—C27119.2 (3)
N3—Zn1—N491.16 (9)C16—C17—C18120.1 (3)
N3—Zn1—N591.81 (8)C17—C18—C19119.5 (3)
N3—Zn1—N6174.03 (9)C18—C19—C20120.0 (3)
N4—Zn1—N5129.82 (8)C21—C22—C23118.6 (3)
N4—Zn1—N691.04 (9)C22—C23—C24120.3 (3)
N5—Zn1—N691.04 (9)C23—C24—C25118.6 (3)
Zn1—N1—C1108.3 (2)C24—C25—C26120.2 (3)
Zn1—N1—C280.9 (1)C28—C27—C16120.5 (3)
Zn1—N1—C8107.7 (2)C29—C28—C27120.6 (3)
Zn1—N1—C1379.2 (1)C30—C29—C28120.4 (3)
Zn1—N1—C14105.5 (2)C15—C30—C29120.5 (3)
Zn1—N2—C180.8 (1)C32—C31—C10120.9 (3)
Zn1—N2—C2108.2 (2)C33—C32—C31120.0 (3)
Zn1—N2—C26107.4 (2)C34—C33—C32121.0 (3)
Zn1—N2—C1979.5 (1)C9—C34—C33120.7 (3)
Zn1—N2—C20105.3 (2)H91—O9—H9297.0
Zn1—N3—C3127.2 (2)H2a—C2—H2b109.5
Zn1—N3—C4155.8 (1)N2—C2—H2b109.4
Zn1—N3—C6143.7 (1)C1—C2—H2b109.4
Zn1—N3—C7113.7 (2)N2—C2—H2a109.3
Zn1—N3—C881.8 (1)C1—C2—H2a109.3
Zn1—N4—C9130.5 (2)H1a—C1—H1b109.5
Zn1—N4—C12140.3 (1)N1—C1—H1b109.6
Zn1—N4—C10158.0 (1)C2—C1—H1b109.6
Zn1—N4—C1478.9 (1)N1—C1—H1a109.6
Zn1—N4—C34100.6 (1)C2—C1—H1a109.5
Zn1—N5—C19111.5 (2)C29—C30—H30119.7
Zn1—N5—C15129.5 (2)C15—C30—H30119.8
Zn1—N5—C18140.1 (1)C30—C29—H29119.8
Zn1—N5—C3099.7 (1)C28—C29—H29119.8
Zn1—N5—C2078.9 (1)C27—C28—H28119.7
Zn1—N5—C16156.9 (1)C29—C28—H28119.6
Zn1—N6—C21127.0 (2)C28—C27—H27119.7
Zn1—N4—C13111.7 (2)C16—C27—H27119.8
Zn1—N6—C22155.6 (2)C18—C17—H17120.0
Zn1—N6—C24143.9 (1)C16—C17—H17119.9
Zn1—N6—C25113.9 (2)C17—C18—H18120.2
Zn1—N6—C2681.9 (1)C19—C18—H18120.2
O1—Cl1—O2110.4 (2)H20a—C20—H20b109.5
O1—Cl1—O3109.1 (2)N2—C20—H20a109.1
O1—Cl1—O4109.2 (1)C19—C20—H20a109.1
O2—Cl1—O3109.0 (2)N2—C20—H20b109.0
O2—Cl1—O4109.7 (1)C19—C20—H20b109.0
O3—Cl1—O4109.4 (2)N6—C21—H21118.7
O5—Cl2—O6111.4 (2)C22—C21—H21118.7
O5—Cl2—O7107.7 (2)C23—C22—H22120.7
O5—Cl2—O8110.7 (2)C21—C22—H22120.7
O6—Cl2—O7108.6 (3)C22—C23—H23119.8
O6—Cl2—O8110.0 (2)C24—C23—H23119.9
O7—Cl2—O8108.2 (2)C23—C24—H24120.7
C1—N1—C8112.2 (2)C25—C24—H24120.7
C1—N1—C14112.3 (2)H26a—C26—H26b109.5
C14—N1—C8110.5 (2)N2—C26—H26a108.1
C2—N2—C20112.1 (2)C25—C26—H26a108.2
C2—N2—C26112.5 (2)N2—C26—H26b108.2
C20—N2—C26111.0 (2)C25—C26—H26b108.1
C3—N3—C7119.0 (2)C33—C34—H34119.7
C9—N4—C13117.3 (3)C9—C34—H34119.6
C15—N5—C19118.4 (2)C34—C33—H33119.5
C21—N6—C25119.0 (3)C32—C33—H33119.6
N1—C1—C2109.2 (2)C31—C32—H32120.0
N1—C8—C7114.9 (2)C33—C32—H32120.0
N1—C14—C13111.3 (2)C32—C31—H31119.5
N2—C2—C1109.9 (2)C10—C31—H31119.6
N2—C20—C19111.2 (2)C12—C11—H11120.4
N2—C26—C25114.7 (3)C10—C11—H11120.3
N3—C3—C4123.1 (3)C11—C12—H12119.8
N3—C7—C6121.1 (3)C13—C12—H12119.8
N3—C7—C8119.5 (2)H14a—C14—H14b109.4
N4—C9—C10122.1 (3)N1—C14—H14b109.1
N4—C9—C34119.3 (3)C13—C14—H14b109.0
N4—C13—C12122.9 (3)N1—C14—H14a109.0
N4—C13—C14118.0 (3)C13—C14—H14a109.0
N5—C15—C16121.8 (3)N3—C3—H3118.4
N5—C15—C30119.5 (3)C4—C3—H3118.5
N5—C19—C18122.4 (3)C3—C4—H4121.1
N5—C19—C20117.6 (3)C5—C4—H4121.1
N6—C21—C22122.6 (3)C6—C5—H5119.9
N6—C25—C24120.9 (3)C4—C5—H5119.9
N6—C25—C26118.9 (3)C5—C6—H6120.7
C3—C4—C5117.8 (3)C7—C6—H6120.6
C4—C5—C6120.2 (3)H8a—C8—H8b109.4
C5—C6—C7118.7 (3)N1—C8—H8b108.1
C6—C7—C8119.3 (3)C7—C8—H8b108.1
C34—C9—C10118.6 (3)N1—C8—H8a108.1
C9—C10—C11117.8 (3)C7—C8—H8a108.1
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H91···O30.961.802.716 (5)158
O9—H92···O50.982.163.064 (5)153
O9—H92···O60.982.263.086 (6)142
C1—H1a···O6i0.952.543.265 (4)134
C2—H2b···O4ii0.952.563.306 (4)136
C4—H4···O7iii0.952.563.285 (3)133
C5—H5···O9ii0.952.373.162 (5)141
C8—H8b···O4ii0.952.553.350 (4)141
C20—H20b···O50.952.593.403 (4)144
C21—H21···O7iv0.952.423.183 (5)137
C23—H23···O2v0.952.543.318 (4)140
C24—H24···O90.952.383.127 (5)135
C28—H28···O4vi0.952.563.277 (4)132
C29—H29···Cg3vii0.952.553.479 (4)166
C33—H33···Cg9viii0.952.633.544 (3)161
Symmetry codes: (i) x+1/2, y+3/2, z+1; (ii) x, y+1, z; (iii) x, y+1/2, z+3/2; (iv) x+1, y, z; (v) x+1/2, y+1/2, z+1; (vi) x+1/2, y+1, z+1/2; (vii) x+1, y1/2, z+3/2; (viii) x+1, y+1/2, z+3/2.

Experimental details

(I)(II)(III)
Crystal data
Chemical formula[Zn(C26H28N6)](ClO4)2·0.67H2O[Zn(C30H30N6)](ClO4)2[Zn(C34H32N6)](ClO4)2·H2O
Mr700.86738.91806.99
Crystal system, space groupMonoclinic, C2/cMonoclinic, P21/nOrthorhombic, P212121
Temperature (K)120120120
a, b, c (Å)41.064 (3), 9.3590 (7), 23.785 (2)13.231 (2), 15.147 (2), 15.167 (2)11.891 (3), 12.022 (3), 23.838 (5)
α, β, γ (°)90, 107.625 (2), 9090, 94.634 (3), 9090, 90, 90
V3)8711.9 (12)3029.5 (7)3407.8 (14)
Z1244
Radiation typeMo KαMo KαMo Kα
µ (mm1)1.091.050.94
Crystal size (mm)0.41 × 0.26 × 0.080.60 × 0.42 × 0.280.54 × 0.38 × 0.30
Data collection
DiffractometerSiemens SMART CCD area-detector
diffractometer
Siemens SMART CCD area-detector
diffractometer
Siemens SMART CCD area-detector
diffractometer
Absorption correctionIntegration
(XPREP; Siemens, 1995)
Integration
(XPREP; Siemens, 1995
Integration
(XPREP; Siemens, 1995)
Tmin, Tmax0.681, 0.9190.596, 0.7780.664, 0.774
No. of measured, independent and
observed reflections
41218, 10019, 6179 [I > 2.5σ(I)]25310, 6946, 4838 [I > 3σ(I)]28487, 7803, 6872 [I > 2.5σ(I)]
Rint0.0630.0260.064
(sin θ/λ)max1)0.6500.6500.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.038, 0.99 0.030, 0.035, 1.00 0.033, 0.038, 1.00
No. of reflections617948386872
No. of parameters591402470
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.55 (4), 0.35 (4)1.43 (7), 1.18 (7)1.15 (9), 0.59 (9)
Absolute structure??Rogers factor refined for 2959 Bijvoet pairs where both members have I > 3σ(I)

For the crystal studied, N1 and N2 have the S configuration

Rogers parameter??0.93 (2)

Computer programs: SMART (Siemens, 1995), SAINT (Siemens, 1995), SIR97 (Altomare et al., 1997) and KRYSTAL (Hazell, 1995), ORFLS (Busing et al., 1962; modified) and KRYSTAL (Hazell, 1995), ORTEPIII (Burnett and Johnson, 1996), KRYSTAL (Hazell, 1995) and PLATON (Spek, 2003), KRYSTAL (Hazell, 1995).

Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
O13—H131···O60.862.062.907 (5)167
O13—H132···O2i0.862.403.227 (4)162
C1—H1a···O10.952.383.320 (5)169
C9—H9···O130.952.403.250 (5)149
C12—H12···O2ii0.952.483.134 (5)126
C14—H14b···O30.952.463.321 (4)150
C20—H20a···O90.952.573.439 (6)153
C20—H20b···O4iii0.952.443.355 (5)160
C26—H26b···O120.952.523.430 (5)160
C27—H27a···O12i0.952.413.287 (5)154
C33—H33a···O80.952.533.440 (6)160
C35—H35···O100.952.583.315 (5)134
C10—H10···Cg3iv0.952.703.546 (5)148
C16—H16···Cg80.952.523.454 (5)167
Symmetry codes: (i) x, y+1, z1/2; (ii) x+3/2, y1/2, z+3/2; (iii) x, y1, z; (iv) x+3/2, y+1/2, z+1.
Hydrogen-bond geometry (Å, º) for (II) top
D—H···AD—HH···AD···AD—H···A
C5—H5···O1'i0.952.513.194 (4)129
C17—H17···O70.952.553.448 (3)157
C18—H18···O4'0.952.543.209 (3)128
C20—H20a···O7ii0.952.553.276 (3)134
C21—H21···O8iii0.952.493.266 (3)139
C27—H27···O50.952.433.053 (3)123
C3—H3···Cg50.952.853.639 (3)141
C29—H29···Cg3iv0.952.793.538 (3)136
Symmetry codes: (i) x+1/2, y+1/2, z+3/2; (ii) x+1, y, z+1; (iii) x+1/2, y1/2, z+1/2; (iv) x+1, y, z+2.
Hydrogen-bond geometry (Å, º) for (III) top
D—H···AD—HH···AD···AD—H···A
O9—H91···O30.961.802.716 (5)158
O9—H92···O50.982.163.064 (5)153
O9—H92···O60.982.263.086 (6)142
C1—H1a···O6i0.952.543.265 (4)134
C2—H2b···O4ii0.952.563.306 (4)136
C4—H4···O7iii0.952.563.285 (3)133
C5—H5···O9ii0.952.373.162 (5)141
C8—H8b···O4ii0.952.553.350 (4)141
C20—H20b···O50.952.593.403 (4)144
C21—H21···O7iv0.952.423.183 (5)137
C23—H23···O2v0.952.543.318 (4)140
C24—H24···O90.952.383.127 (5)135
C28—H28···O4vi0.952.563.277 (4)132
C29—H29···Cg3vii0.952.553.479 (4)166
C33—H33···Cg9viii0.952.633.544 (3)161
Symmetry codes: (i) x+1/2, y+3/2, z+1; (ii) x, y+1, z; (iii) x, y+1/2, z+3/2; (iv) x+1, y, z; (v) x+1/2, y+1/2, z+1; (vi) x+1/2, y+1, z+1/2; (vii) x+1, y1/2, z+3/2; (viii) x+1, y+1/2, z+3/2.
Comparison of Zn—N distances (Å) for complexes with tpen, (I), qtpen, (II), and bqbpen, (III) top
Bond(I)a(I)b(II)(III)
Zn—N12.188 (3)2.208 (3)2.189 (2)2.205 (2)
Zn—N22.173 (3)2.208 (3)2.229 (2)2.208 (2)
Zn—N32.236 (3)2.175 (3)2.181 (2)2.122 (2)
Zn—N42.092 (3)2.097 (3)2.180 (2)2.217 (3)
Zn—N52.082 (3)2.097 (3)2.137 (2)2.217 (2)
Zn—N62.199 (3)2.175 (3)2.129 (2)2.121 (2)
Notes: (a) molecule 1; (b) molecule 2.
Comparison of N—Zn—N angles (°) for complexes with tpen, (I), qtpen, (II), and bqbpen, (III) top
Angle(I)a(I)b(II)(III)
N1—Zn—N282.7 (1)81.9 (2)81.96 (7)79.6 (1)
N1—Zn—N378.5 (1)78.8 (1)79.37 (7)81.57 (9)
N1—Zn—N479.8 (1)79.5 (1)77.09 (7)76.18 (9)
N1—Zn—N5157.3 (1)157.5 (1)156.00 (7)153.5 (1)
N1—Zn—N6106.1 (1)96.0 (1)95.72 (7)93.57 (9)
N2—Zn—N3100.0 (1)96.0 (1)91.55 (7)94.32 (9)
N2—Zn—N4157.1 (1)157.5 (1)157.42 (7)154.04 (9)
N2—Zn—N581.1 (1)79.5 (1)77.14 (7)75.40 (9)
N2—Zn—N679.0 (1)78.7 (1)80.03 (7)81.3 (1)
N3—Zn—N490.9 (1)92.8 (1)92.76 (7)91.81 (8)
N3—Zn—N588.7 (1)90.6 (1)89.48 (7)91.16 (9)
N3—Zn—N6185.0 (1)c173.1 (1)170.82 (7)174.03 (9)
N4—Zn—N5119.5 (1)121.2 (1)125.04 (7)129.82 (8)
N4—Zn—N691.7 (1)90.6 (1)93.68 (7)91.04 (9)
N5—Zn—N686.3 (1)92.8 (1)92.16 (7)91.04 (9)
Notes: (a) molecule 1; (b) molecule 2; (c) angle defined as <180° for bonds bent toward the ethanediamine moiety.
 

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