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The crystal structure of the title compound, [Zn(C4H10N4)3](ClO4)2, has been precisely determined at ca 110 K. The organometallic cation, which is located on a \overline 3 axis, is characterized by an approximate octahedral geometry, with each of the ligands occupying two coordination sites around the metal.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805004757/ci6528sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805004757/ci6528Isup2.hkl
Contains datablock I

CCDC reference: 269414

Key indicators

  • Single-crystal X-ray study
  • T = 110 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.035
  • wR factor = 0.090
  • Data-to-parameter ratio = 15.7

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 27.48 From the CIF: _reflns_number_total 893 From the CIF: _diffrn_reflns_limit_ max hkl 12. 10. 18. From the CIF: _diffrn_reflns_limit_ min hkl -12. -10. -18. TEST1: Expected hkl limits for theta max Calculated maximum hkl 12. 12. 19. Calculated minimum hkl -12. -12. -19.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1999); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and Mercury (Bruno et al., 2002); software used to prepare material for publication: SHELXL97.

Tris(biacetyl dihydrazone-κ2N,N')zinc(II) bis(perchlorate) top
Crystal data top
[Zn(C4H10N4)3](ClO4)2Dx = 1.700 Mg m3
Mr = 606.75Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3c1Cell parameters from 1664 reflections
Hall symbol: -P 3 2"cθ = 2.5–27.5°
a = 9.4496 (4) ŵ = 1.33 mm1
c = 15.3237 (4) ÅT = 110 K
V = 1185.01 (8) Å3Needle, light yellow
Z = 20.35 × 0.10 × 0.10 mm
F(000) = 628
Data collection top
Nonius KappaCCD
diffractometer
893 independent reflections
Radiation source: fine-focus sealed tube705 reflections with I > 2σ(I)'
Graphite monochromatorRint = 0.035
Detector resolution: 56 microns pixels mm-1θmax = 27.5°, θmin = 2.5°
φ and ω scansh = 1212
Absorption correction: multi-scan
(Blessing, 1995)
k = 1010
Tmin = 0.654, Tmax = 0.879l = 1818
6818 measured reflections
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)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.090H-atom parameters constrained
S = 0.98 w = 1/[σ2(Fo2) + (0.0348P)2 + 2.7971P]
where P = (Fo2 + 2Fc2)/3
893 reflections(Δ/σ)max = 0.001
57 parametersΔρmax = 0.36 e Å3
0 restraintsΔρmin = 0.42 e Å3
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.

The metal cation is located on a 3 bar axis, while the perchlorate anion is located on a 3 axis of rotation.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Zn10.00000.00000.25000.0108 (2)
N20.2321 (3)0.1259 (3)0.08856 (12)0.0166 (5)
H2A0.34030.18150.06970.033 (9)*
H2B0.18300.19440.08010.033 (9)*
N30.2168 (3)0.0698 (2)0.17354 (13)0.0127 (5)
C40.3231 (3)0.0379 (3)0.20537 (15)0.0128 (5)
C50.4754 (3)0.0701 (3)0.15924 (18)0.0191 (6)
H5A0.45530.05730.09620.029*
H5B0.50840.00750.17940.029*
H5C0.56270.18180.17180.029*
Cl60.33330.66670.07464 (6)0.0156 (2)
O70.2608 (3)0.5007 (2)0.04370 (12)0.0295 (5)
O80.33330.66670.16832 (19)0.0192 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0124 (4)0.0120.0077 (3)0.0060.0000.000
N20.0182 (11)0.0221 (12)0.0094 (10)0.0100 (10)0.0036 (8)0.0053 (8)
N30.0139 (11)0.0141 (10)0.0083 (10)0.0057 (8)0.0018 (8)0.0016 (7)
C40.0132 (13)0.0092 (11)0.0142 (12)0.0041 (10)0.0010 (9)0.0016 (9)
C50.0160 (13)0.0172 (14)0.0229 (14)0.0075 (12)0.0051 (10)0.0016 (11)
Cl60.0175 (5)0.0210.0093 (5)0.0110.0000.000
O70.0348 (13)0.0251 (11)0.0253 (11)0.0124 (10)0.0036 (9)0.0135 (8)
O80.0253 (16)0.0250.0070 (14)0.0120.0000.000
Geometric parameters (Å, º) top
Zn1—N3i2.158 (2)C4—C51.492 (3)
Zn1—N3ii2.158 (2)C4—C4ii1.502 (5)
Zn1—N3iii2.158 (2)C5—H5A0.98
Zn1—N32.158 (2)C5—H5B0.98
Zn1—N3iv2.158 (2)C5—H5C0.98
Zn1—N3v2.158 (2)Cl6—O81.435 (3)
N2—N31.386 (3)Cl6—O7vi1.441 (2)
N2—H2A0.93Cl6—O7vii1.442 (2)
N2—H2B0.98Cl6—O71.442 (2)
N3—C41.281 (3)
N3i—Zn1—N3ii93.31 (7)C4—N3—N2120.3 (2)
N3i—Zn1—N3iii93.31 (7)C4—N3—Zn1117.25 (16)
N3ii—Zn1—N3iii93.31 (7)N2—N3—Zn1121.89 (16)
N3i—Zn1—N3102.24 (11)N3—C4—C5124.2 (2)
N3ii—Zn1—N374.33 (11)N3—C4—C4ii115.54 (14)
N3iii—Zn1—N3160.52 (11)C5—C4—C4ii120.31 (14)
N3i—Zn1—N3iv160.52 (11)C4—C5—H5A109.5
N3ii—Zn1—N3iv102.24 (11)C4—C5—H5B109.5
N3iii—Zn1—N3iv74.33 (11)H5A—C5—H5B109.5
N3—Zn1—N3iv93.30 (7)C4—C5—H5C109.5
N3i—Zn1—N3v74.33 (11)H5A—C5—H5C109.5
N3ii—Zn1—N3v160.52 (11)H5B—C5—H5C109.5
N3iii—Zn1—N3v102.24 (11)O8—Cl6—O7vi109.21 (9)
N3—Zn1—N3v93.30 (7)O8—Cl6—O7vii109.20 (9)
N3iv—Zn1—N3v93.30 (7)O7vi—Cl6—O7vii109.76 (9)
N3—N2—H2A112.5O8—Cl6—O7109.20 (9)
N3—N2—H2B112.7O7vi—Cl6—O7109.75 (9)
H2A—N2—H2B109.7O7vii—Cl6—O7109.71 (9)
N3i—Zn1—N3—C491.09 (19)N3iii—Zn1—N3—N2120.11 (18)
N3ii—Zn1—N3—C41.07 (14)N3iv—Zn1—N3—N270.49 (15)
N3iii—Zn1—N3—C451.11 (18)N3v—Zn1—N3—N223.01 (18)
N3iv—Zn1—N3—C4100.7 (2)N2—N3—C4—C55.4 (4)
N3v—Zn1—N3—C4165.77 (19)Zn1—N3—C4—C5176.80 (19)
N3i—Zn1—N3—N297.69 (19)N2—N3—C4—C4ii174.1 (2)
N3ii—Zn1—N3—N2172.3 (2)Zn1—N3—C4—C4ii2.7 (3)
Symmetry codes: (i) y, x, z+1/2; (ii) xy, y, z+1/2; (iii) x, x+y, z+1/2; (iv) x+y, x, z; (v) y, xy, z; (vi) x+y, x+1, z; (vii) y+1, xy+1, z.
 

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