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The title compound, [ZnBr2(C15H26N2)], when synthesized starting from Zn0, is obtained in two polymorphic forms, one belonging to space group P212121 and one to P1. The present contribution deals with the triclinic phase, which is isostructural with the orthorhombic form but presents a larger metal–metal intermolecular separation; the Zn...Zn distance is 7.4715 (6) Å for the triclinic polymorph as opposed to 6.534 Å for the orthorhombic polymorph.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270103001483/gd1241sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270103001483/gd1241Isup2.hkl
Contains datablock I

CCDC reference: 207992

Comment top

The correlation between the tetrahedral coordination of the CuII ion in type 1 blue copper proteins and some unique spectroscopic features reported for these proteins is a well established fact (Krishnan, 1978; Colman et al., 1978; Solomon et al., 1992; Holland & Tolman, 2000). Well studied examples are the intense absorption observed in electronic spectra near 600 nm (ε 5000 M−1 cm−1) and the small Cu hyperfine splitting observed in EPR spectra (A// < 70 × 10−4 cm−1), which is reduced to less than half the value observed in common CuII coordination complexes.

In this context, numerous CuII complexes containing sparteine as a ligand have been synthesized, with the hope of accurately modeling spectroscopic and structural features of the catalytic center of these proteins (Boschmann et al., 1974; Choi et al., 1975; Kim et al., 2001). For the X-ray-characterized complexes, the expected distorted tetrahedral geometry has been observed in most cases, although the spectroscopic characteristics of these complexes did not always fit correctly with those of the proteins (Childers et al., 1975; Lopez et al., 1998; Choi et al., 1995; Lee et al., 2000).

During the course of our work dealing with this class of compounds, we prepared by direct synthesis a series of complexes with the general formula M(SP)X2 where SP is the naturally occurring (-)-sparteine ligand, X = Cl or Br, and M = CuII or ZnII. The CuII complexes are intended to be used for modeling the active site of type 1 blue copper proteins (structurally and spectroscopically), while the ZnII complexes are used as diluting agents for measuring the hyperfine, and eventually the super-hyperfine, coupling by electron paramagnetic resonance (EPR) on powdered samples. To validate the EPR, isostructurality between Cu and Zn complexes has first to be established by X-ray diffraction. In the case of X = Br, both metals yielded two isomorphous polymorphic crystalline phases, one in space group P1 and one in P212121, when a direct synthesis was used, i.e. using metallic copper or zinc as a starting material (see experimental section). The Zn complex here described, (I), corresponds to the triclinic polymorph of Zn(SP)Br2. The orthorhombic phase, which is synthesized using zinc(II) bromide as a starting material, was reported very recently by Lee et al. (2002).

The molecular structure of (I) is, within the experimental s.u. values, identical (Fig. 1) to that of the reported orthorhombic phase: the r.m.s. deviation between the two structures is 0.0362 Å (excluding H atoms). The largest observed deviation for the fit, 0.082 Å, arises from the Br atoms.

In contrast, the symmetry change induces dramatic differences for the packing structures. The orthorhombic phase is stabilized through two intermolecular contacts involving both the Br atoms and the methylene or methine H atoms belonging to the SP ligands of symmetry-related molecules: Zn—Br1···H15Bi [contact = 2.910 Å, angle = 156.0°; (i) 1/2 − x, 1 − y, −1/2 + z] and Zn—Br2···H7ii (contact = 2.933 Å, angle = 160.0°; (ii) 1/2 − x, −y, −1/2 + z). The Br···H separations are then 0.14 and 0.12 Å shorter than the van der Waals distance. This arrangement generates layers of connected molecules, with the layers normal to the a axis of the orthorhombic cell (Fig. 2).

In the case of (I), the only operators available for connecting molecules are axis translations. A single short Br···H contact is observed (Table 1), which corresponds to a relatively weak interaction, with a difference from the van der Waals distance of 0.06 Å; the resulting network of interconnected molecules is one dimensional (Fig. 3). In spite of these weak contacts, the packing index (Spek, 2003) is lowered from 0.683 for the orthorhombic phase to 0.681 for (I). This more efficient packing for (I) is confirmed by the analysis of the intermolecular H···H contacts. The shortest contact observed for the orthorhombic phase is H3A···H11Bi = 2.403 Å [(i) 1 + x, y, z], i.e. a separation equal to the van der Waals distance. However, for (I), the shortest H···H separation is 2.317 Å (Table 1), which corresponds to an actual H···H contact (Fig. 3).

Finally, the metal–metal separations are significantly affected by the symmetry. The observed distances are Zn···Zni = 6.534 Å [(i) 1/2 + x, 1/2 − y, −z] in the orthorhombic case versus Zn···Znii = 7.4715 (6) Å [(ii) 1 + x, y, z] for (I). This difference of ca 1 Å is unimportant for the ZnII-based compounds but essential for the corresponding CuII-based compounds that are intended for modeling. Considering that the metal centers should be magnetically isolated in the native proteins, the triclinic phase seems to be a more suitable magnetic model than the orthorhombic one.

Experimental top

Equimolar amounts of zinc (0.123 g), CBr4 (0.626 g) and (-)sparteine (0.433 ml) were mixed in DMSO (5.376 ml). The mixture was heated at 333 K for 30 min and then filtered. The first drop of crystals was collected after 2 days (0.219 g, yield 25.3%, m.p. 566 K). These crystals exhibited a characteristic hexagonal plate habit and were identified as (I). Further crystallization produced small quantities of the orthorhombic polymorph, which can be distinguished from (I) on the basis of its quite isotropic block habit.

Refinement top

H atoms were treated as riding atoms with C—H distances 0.97 Å (CH2) or 0.98 Å (CH).

Computing details top

Data collection: XSCANS 2.21 (Siemens, 1996); cell refinement: XSCANS 2.21 (Siemens, 1996); data reduction: XSCANS 2.21 (Siemens, 1996); program(s) used to solve structure: SHELXTL-Plus (Sheldrick, 1998); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1998) and Mercury 1.1 (CCDC, 2002); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. The structure of (I) with displacement ellipsoids at the 40% probability level. The numbering scheme is identical to that adopted by Lee et al. (2002) for the orthorhombic phase.
[Figure 2] Fig. 2. One layer of interconnected Zn(SP)Br2 molecules in the packing structure of the orthorhombic polymorph, viewed down the a axis. Nine molecules are represented. The capped sticks representation of the bottom molecule is given with the numbering scheme for non-C atoms, and H atoms not involved in the network have been omitted for clarity. For the remaining molecules, Br1, Br2, H7 and H15B atoms that connect molecules are represented as van der Waals radii spheres (CCDC, 2002), making obvious the two-dimensional character of the network.
[Figure 3] Fig. 3. The packing structure for (I) viewed down the a axis. As in Fig. 2, nine molecules are represented, one of which (bottom left) includes labels for non-C atoms. The retained H atoms are those that give short non-bonding H···H intermolecular contacts. For the remaining molecules, Br2 and H8A atoms that connect molecules are represented as van der Waals radii spheres (CCDC, 2002), while dotted lines join H atoms that are participating in the H···H contacts network (see Table 1).
dibromo[(6R,7S,8S,14S)-1,3,4,7,7a,8,9,10,11,13,14,14a-dodecahydro-7,14- methano-2H,6H-dipyrido[1,2 − a;1',2'-e][1,5]diazocine-κ2N,N']zinc(II) top
Crystal data top
[ZnBr2(C15H26N2)]Z = 1
Mr = 459.57F(000) = 230
Triclinic, P1Dx = 1.766 Mg m3
Hall symbol: P 1Melting point: 566 K
a = 7.4715 (6) ÅMo Kα radiation, λ = 0.71073 Å
b = 7.7082 (7) ÅCell parameters from 84 reflections
c = 9.1435 (6) Åθ = 5.0–13.0°
α = 97.429 (6)°µ = 6.04 mm1
β = 112.808 (5)°T = 296 K
γ = 110.666 (6)°Prism, colorless
V = 432.02 (7) Å30.60 × 0.24 × 0.16 mm
Data collection top
Bruker P4
diffractometer
4244 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.048
Graphite monochromatorθmax = 30.0°, θmin = 2.5°
2θ/ω scansh = 910
Absorption correction: ψ-scan
XSCANS 2.21 (Siemens, 1996)
k = 1010
Tmin = 0.254, Tmax = 0.381l = 1212
4908 measured reflections3 standard reflections every 97 reflections
4908 independent reflections intensity decay: 1%
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.040 w = 1/[σ2(Fo2) + (0.0364P)2 + 0.6283P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.097(Δ/σ)max < 0.001
S = 1.04Δρmax = 0.53 e Å3
4908 reflectionsΔρmin = 0.77 e Å3
182 parametersExtinction correction: SHELXL97, Fc* = kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
3 restraintsExtinction coefficient: 0.0083 (17)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983); 2436 Friedel pairs
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.016 (13)
Crystal data top
[ZnBr2(C15H26N2)]γ = 110.666 (6)°
Mr = 459.57V = 432.02 (7) Å3
Triclinic, P1Z = 1
a = 7.4715 (6) ÅMo Kα radiation
b = 7.7082 (7) ŵ = 6.04 mm1
c = 9.1435 (6) ÅT = 296 K
α = 97.429 (6)°0.60 × 0.24 × 0.16 mm
β = 112.808 (5)°
Data collection top
Bruker P4
diffractometer
4244 reflections with I > 2σ(I)
Absorption correction: ψ-scan
XSCANS 2.21 (Siemens, 1996)
Rint = 0.048
Tmin = 0.254, Tmax = 0.3813 standard reflections every 97 reflections
4908 measured reflections intensity decay: 1%
4908 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.040H-atom parameters constrained
wR(F2) = 0.097Δρmax = 0.53 e Å3
S = 1.04Δρmin = 0.77 e Å3
4908 reflectionsAbsolute structure: Flack (1983); 2436 Friedel pairs
182 parametersAbsolute structure parameter: 0.016 (13)
3 restraints
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
xyzUiso*/Ueq
Zn10.64020 (6)0.60790 (6)0.13464 (5)0.03135 (13)
Br10.94293 (9)0.90078 (8)0.19208 (8)0.05669 (18)
Br20.31099 (9)0.57007 (9)0.07858 (7)0.05857 (18)
N10.7406 (6)0.3888 (5)0.1528 (5)0.0310 (7)
C20.7964 (10)0.3414 (8)0.0173 (7)0.0465 (12)
H2A0.85680.24880.03620.056*
H2B0.90560.45890.02040.056*
C30.6019 (11)0.2570 (9)0.1510 (7)0.0509 (13)
H3A0.64300.22340.23520.061*
H3B0.55010.35440.17420.061*
C40.4189 (11)0.0749 (9)0.1623 (7)0.0585 (16)
H4A0.28990.03510.26710.070*
H4B0.46050.03100.15950.070*
C50.3705 (8)0.1160 (7)0.0182 (6)0.0412 (11)
H5A0.26760.00450.01930.049*
H5B0.30500.20530.03220.049*
C60.5745 (7)0.2039 (6)0.1488 (6)0.0330 (9)
H6A0.63620.11030.15780.040*
C70.5350 (8)0.2371 (7)0.3007 (6)0.0350 (9)
H7A0.42970.11220.29370.042*
C80.9051 (7)0.4956 (7)0.4687 (6)0.0366 (10)
H8A1.04350.53500.56750.044*
N90.6050 (6)0.5912 (5)0.3492 (4)0.0282 (7)
C100.5210 (8)0.7348 (7)0.3770 (6)0.0387 (10)
H10A0.37320.68510.29010.046*
H10B0.60580.85520.36490.046*
C110.5246 (10)0.7812 (9)0.5452 (7)0.0511 (13)
H11A0.47590.88140.55440.061*
H11B0.42630.66550.55380.061*
C120.7514 (11)0.8511 (10)0.6861 (7)0.0550 (15)
H12A0.75040.87200.79260.066*
H12B0.84780.97340.68450.066*
C130.8302 (9)0.6960 (9)0.6631 (6)0.0452 (13)
H13A0.73980.57770.67430.054*
H13B0.97710.74160.75040.054*
C140.8245 (7)0.6492 (6)0.4918 (5)0.0315 (8)
H14A0.92450.76950.48780.038*
C150.9415 (7)0.4698 (7)0.3149 (6)0.0374 (10)
H15A1.03990.59550.31980.045*
H15B1.01090.38400.31920.045*
C160.4477 (7)0.3884 (6)0.3169 (5)0.0322 (9)
H16A0.31640.35250.21490.039*
H16B0.41040.38520.40740.039*
C170.7462 (9)0.2974 (7)0.4580 (6)0.0408 (10)
H17A0.80190.20210.45140.049*
H17B0.72330.30760.55550.049*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0304 (3)0.0336 (3)0.0299 (2)0.0126 (2)0.0142 (2)0.0132 (2)
Br10.0473 (3)0.0442 (3)0.0787 (4)0.0112 (2)0.0343 (3)0.0297 (3)
Br20.0509 (3)0.0706 (4)0.0441 (3)0.0325 (3)0.0055 (2)0.0242 (3)
N10.0305 (17)0.0320 (18)0.0334 (18)0.0116 (15)0.0196 (15)0.0106 (15)
C20.057 (3)0.048 (3)0.056 (3)0.027 (3)0.043 (3)0.020 (2)
C30.069 (4)0.051 (3)0.043 (3)0.021 (3)0.040 (3)0.014 (2)
C40.070 (4)0.049 (3)0.042 (3)0.009 (3)0.032 (3)0.000 (2)
C50.039 (2)0.034 (2)0.032 (2)0.0028 (19)0.0141 (19)0.0004 (18)
C60.037 (2)0.028 (2)0.041 (2)0.0143 (17)0.0235 (19)0.0094 (17)
C70.037 (2)0.033 (2)0.036 (2)0.0103 (18)0.0216 (19)0.0135 (18)
C80.030 (2)0.045 (3)0.031 (2)0.018 (2)0.0086 (17)0.0164 (19)
N90.0254 (16)0.0323 (18)0.0232 (15)0.0118 (14)0.0092 (13)0.0071 (13)
C100.035 (2)0.040 (3)0.037 (2)0.018 (2)0.0152 (19)0.0048 (19)
C110.054 (3)0.058 (3)0.044 (3)0.026 (3)0.027 (3)0.005 (2)
C120.062 (4)0.056 (4)0.033 (2)0.021 (3)0.018 (2)0.001 (2)
C130.040 (3)0.052 (3)0.025 (2)0.011 (2)0.0095 (19)0.003 (2)
C140.0234 (18)0.034 (2)0.0262 (18)0.0062 (16)0.0075 (15)0.0075 (16)
C150.027 (2)0.044 (3)0.044 (2)0.0180 (19)0.0156 (18)0.016 (2)
C160.0245 (19)0.036 (2)0.030 (2)0.0067 (17)0.0148 (16)0.0072 (17)
C170.049 (3)0.040 (2)0.039 (2)0.021 (2)0.021 (2)0.022 (2)
Geometric parameters (Å, º) top
Zn1—N12.077 (4)C8—C141.532 (7)
Zn1—N92.092 (3)C8—C151.534 (7)
Zn1—Br22.3590 (7)C8—H8A0.9800
Zn1—Br12.3784 (7)N9—C101.492 (6)
N1—C151.488 (6)N9—C161.492 (6)
N1—C21.494 (6)N9—C141.504 (5)
N1—C61.508 (6)C10—C111.521 (7)
C2—C31.498 (9)C10—H10A0.9700
C2—H2A0.9700C10—H10B0.9700
C2—H2B0.9700C11—C121.518 (9)
C3—C41.533 (8)C11—H11A0.9700
C3—H3A0.9700C11—H11B0.9700
C3—H3B0.9700C12—C131.532 (9)
C4—C51.520 (7)C12—H12A0.9700
C4—H4A0.9700C12—H12B0.9700
C4—H4B0.9700C13—C141.542 (6)
C5—C61.521 (7)C13—H13A0.9700
C5—H5A0.9700C13—H13B0.9700
C5—H5B0.9700C14—H14A0.9800
C6—C71.537 (6)C15—H15A0.9700
C6—H6A0.9800C15—H15B0.9700
C7—C171.525 (7)C16—H16A0.9700
C7—C161.541 (7)C16—H16B0.9700
C7—H7A0.9800C17—H17A0.9700
C8—C171.531 (7)C17—H17B0.9700
Br2···H8Ai2.986H5A···H13Biii2.317
H3A···H17Bii2.319H10B···H17Aiv2.390
N1—Zn1—N988.66 (14)C10—N9—C16111.5 (3)
N1—Zn1—Br2124.28 (11)C10—N9—C14110.6 (3)
N9—Zn1—Br2108.51 (10)C16—N9—C14112.5 (3)
N1—Zn1—Br1107.81 (10)C10—N9—Zn1105.3 (3)
N9—Zn1—Br1110.88 (10)C16—N9—Zn1108.5 (2)
Br2—Zn1—Br1113.69 (3)C14—N9—Zn1108.1 (2)
C15—N1—C2108.0 (4)N9—C10—C11115.6 (4)
C15—N1—C6110.0 (3)N9—C10—H10A108.4
C2—N1—C6108.7 (4)C11—C10—H10A108.4
C15—N1—Zn1105.6 (3)N9—C10—H10B108.4
C2—N1—Zn1111.5 (3)C11—C10—H10B108.4
C6—N1—Zn1112.9 (3)H10A—C10—H10B107.5
N1—C2—C3111.5 (5)C12—C11—C10110.5 (5)
N1—C2—H2A109.3C12—C11—H11A109.5
C3—C2—H2A109.3C10—C11—H11A109.5
N1—C2—H2B109.3C12—C11—H11B109.5
C3—C2—H2B109.3C10—C11—H11B109.5
H2A—C2—H2B108.0H11A—C11—H11B108.1
C2—C3—C4112.1 (5)C11—C12—C13108.7 (5)
C2—C3—H3A109.2C11—C12—H12A110.0
C4—C3—H3A109.2C13—C12—H12A110.0
C2—C3—H3B109.2C11—C12—H12B110.0
C4—C3—H3B109.2C13—C12—H12B110.0
H3A—C3—H3B107.9H12A—C12—H12B108.3
C5—C4—C3110.5 (4)C12—C13—C14112.2 (4)
C5—C4—H4A109.6C12—C13—H13A109.2
C3—C4—H4A109.6C14—C13—H13A109.2
C5—C4—H4B109.6C12—C13—H13B109.2
C3—C4—H4B109.6C14—C13—H13B109.2
H4A—C4—H4B108.1H13A—C13—H13B107.9
C4—C5—C6111.5 (5)N9—C14—C8110.7 (3)
C4—C5—H5A109.3N9—C14—C13112.5 (4)
C6—C5—H5A109.3C8—C14—C13112.5 (4)
C4—C5—H5B109.3N9—C14—H14A106.9
C6—C5—H5B109.3C8—C14—H14A106.9
H5A—C5—H5B108.0C13—C14—H14A106.9
N1—C6—C5110.7 (4)N1—C15—C8114.4 (4)
N1—C6—C7111.1 (3)N1—C15—H15A108.7
C5—C6—C7114.2 (4)C8—C15—H15A108.7
N1—C6—H6A106.8N1—C15—H15B108.7
C5—C6—H6A106.8C8—C15—H15B108.7
C7—C6—H6A106.8H15A—C15—H15B107.6
C17—C7—C6108.4 (4)N9—C16—C7113.3 (3)
C17—C7—C16109.1 (4)N9—C16—H16A108.9
C6—C7—C16115.8 (4)C7—C16—H16A108.9
C17—C7—H7A107.7N9—C16—H16B108.9
C6—C7—H7A107.7C7—C16—H16B108.9
C16—C7—H7A107.7H16A—C16—H16B107.7
C17—C8—C14110.3 (4)C7—C17—C8106.6 (4)
C17—C8—C15108.3 (4)C7—C17—H17A110.4
C14—C8—C15114.7 (4)C8—C17—H17A110.4
C17—C8—H8A107.8C7—C17—H17B110.4
C14—C8—H8A107.8C8—C17—H17B110.4
C15—C8—H8A107.8H17A—C17—H17B108.6
N9—Zn1—N1—C1561.8 (3)Br2—Zn1—N9—C14170.5 (2)
Br2—Zn1—N1—C15173.4 (2)Br1—Zn1—N9—C1444.9 (3)
Br1—Zn1—N1—C1549.7 (3)C16—N9—C10—C1174.6 (5)
N9—Zn1—N1—C2178.8 (3)C14—N9—C10—C1151.5 (5)
Br2—Zn1—N1—C269.6 (4)Zn1—N9—C10—C11168.0 (4)
Br1—Zn1—N1—C267.3 (3)N9—C10—C11—C1255.6 (7)
N9—Zn1—N1—C658.4 (3)C10—C11—C12—C1355.8 (7)
Br2—Zn1—N1—C653.2 (3)C11—C12—C13—C1456.8 (6)
Br1—Zn1—N1—C6170.0 (2)C10—N9—C14—C8176.6 (4)
C15—N1—C2—C3179.5 (4)C16—N9—C14—C851.1 (4)
C6—N1—C2—C360.2 (6)Zn1—N9—C14—C868.7 (4)
Zn1—N1—C2—C364.9 (5)C10—N9—C14—C1349.7 (5)
N1—C2—C3—C456.7 (7)C16—N9—C14—C1375.7 (5)
C2—C3—C4—C551.6 (7)Zn1—N9—C14—C13164.5 (3)
C3—C4—C5—C651.9 (7)C17—C8—C14—N958.9 (5)
C15—N1—C6—C5178.4 (4)C15—C8—C14—N963.6 (5)
C2—N1—C6—C560.3 (5)C17—C8—C14—C1367.9 (5)
Zn1—N1—C6—C564.0 (4)C15—C8—C14—C13169.6 (4)
C15—N1—C6—C753.7 (5)C12—C13—C14—N954.7 (5)
C2—N1—C6—C7171.7 (4)C12—C13—C14—C8179.5 (4)
Zn1—N1—C6—C764.0 (4)C2—N1—C15—C8170.7 (4)
C4—C5—C6—N157.4 (5)C6—N1—C15—C852.2 (5)
C4—C5—C6—C7176.3 (4)Zn1—N1—C15—C869.9 (4)
N1—C6—C7—C1762.0 (5)C17—C8—C15—N157.3 (5)
C5—C6—C7—C17172.0 (4)C14—C8—C15—N166.3 (5)
N1—C6—C7—C1661.0 (5)C10—N9—C16—C7175.6 (4)
C5—C6—C7—C1665.0 (5)C14—N9—C16—C750.7 (5)
N1—Zn1—N9—C10178.1 (3)Zn1—N9—C16—C768.9 (4)
Br2—Zn1—N9—C1052.2 (3)C17—C7—C16—N956.4 (5)
Br1—Zn1—N9—C1073.3 (3)C6—C7—C16—N966.2 (5)
N1—Zn1—N9—C1658.6 (3)C6—C7—C17—C865.4 (5)
Br2—Zn1—N9—C1667.3 (3)C16—C7—C17—C861.6 (5)
Br1—Zn1—N9—C16167.2 (2)C14—C8—C17—C764.2 (5)
N1—Zn1—N9—C1463.6 (3)C15—C8—C17—C762.0 (5)
Symmetry codes: (i) x1, y, z1; (ii) x, y, z1; (iii) x1, y1, z1; (iv) x, y+1, z.

Experimental details

Crystal data
Chemical formula[ZnBr2(C15H26N2)]
Mr459.57
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)7.4715 (6), 7.7082 (7), 9.1435 (6)
α, β, γ (°)97.429 (6), 112.808 (5), 110.666 (6)
V3)432.02 (7)
Z1
Radiation typeMo Kα
µ (mm1)6.04
Crystal size (mm)0.60 × 0.24 × 0.16
Data collection
DiffractometerBruker P4
diffractometer
Absorption correctionψ-scan
XSCANS 2.21 (Siemens, 1996)
Tmin, Tmax0.254, 0.381
No. of measured, independent and
observed [I > 2σ(I)] reflections
4908, 4908, 4244
Rint0.048
(sin θ/λ)max1)0.703
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.040, 0.097, 1.04
No. of reflections4908
No. of parameters182
No. of restraints3
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.53, 0.77
Absolute structureFlack (1983); 2436 Friedel pairs
Absolute structure parameter0.016 (13)

Computer programs: XSCANS 2.21 (Siemens, 1996), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1998) and Mercury 1.1 (CCDC, 2002).

Selected interatomic distances (Å) top
Br2···H8Ai2.986H5A···H13Biii2.317
H3A···H17Bii2.319H10B···H17Aiv2.390
Symmetry codes: (i) x1, y, z1; (ii) x, y, z1; (iii) x1, y1, z1; (iv) x, y+1, z.
 

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