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The title compound, [Zn(C10H12N2O)2(ClO4)2], crystallizes as mononuclear mol­ecules with distorted octa­hedral ZnII coordination. 3-Dimethyl­amino-l-(2-pyrid­yl)prop-2-enone ions are coordinated to ZnII as bidentate ligands, while the perchlorate ions are monodentate. The Zn atom lies on a centre of symmetry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805020623/hk6010sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805020623/hk6010Isup2.hkl
Contains datablock I

CCDC reference: 282380

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.004 Å
  • Disorder in main residue
  • R factor = 0.034
  • wR factor = 0.101
  • Data-to-parameter ratio = 11.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.97 PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cl1 PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc. PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C5 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 3 N2 -ZN1 -N2 -C6 5.00 0.00 2.755 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 10 N2 -ZN1 -N2 -C10 13.00 0.00 2.755 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 27 O1 -ZN1 -O1 -C1 12.00 0.00 2.755 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 52 O2' -ZN1 -O2 -CL1 -102.00 8.00 2.755 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 54 O2 -ZN1 -O2 -CL1 12.00 0.00 2.755 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 63 O2' -ZN1 -O2' -CL1 10.00 0.00 2.755 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 65 O2 -ZN1 -O2' -CL1 102.00 8.00 2.755 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 13.40 Deg. O2 -CL1 -O2' 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 14 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 9 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Bis[3-dimethylamino-l-(2-pyridyl)prop-2-enonato]diperchloratozinc(II) top
Crystal data top
[Zn(C10H12N2O)2(ClO4)2]Z = 1
Mr = 616.70F(000) = 316
Triclinic, P1Dx = 1.680 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.5449 (19) ÅCell parameters from 2384 reflections
b = 9.187 (2) Åθ = 2.4–27.0°
c = 9.5884 (19) ŵ = 1.29 mm1
α = 79.358 (3)°T = 298 K
β = 78.130 (2)°Block, pink
γ = 70.887 (3)°0.52 × 0.34 × 0.31 mm
V = 609.6 (2) Å3
Data collection top
Bruker SMART CCD area-detecter
diffractometer
2166 independent reflections
Radiation source: fine-focus sealed tube1988 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
Detector resolution: 0 pixels mm-1θmax = 25.3°, θmin = 2.2°
φ and ω scansh = 69
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 911
Tmin = 0.554, Tmax = 0.691l = 1011
3200 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.034H-atom parameters constrained
wR(F2) = 0.101 w = 1/[σ2(Fo2) + (0.0539P)2 + 0.1968P]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max = 0.025
2166 reflectionsΔρmax = 0.30 e Å3
182 parametersΔρmin = 0.38 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.027 (4)
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*/UeqOcc. (<1)
Zn11.00000.00000.00000.0506 (2)
Cl10.69651 (8)0.26114 (7)0.22739 (7)0.0457 (2)
O10.7526 (2)0.0668 (2)0.13509 (18)0.0465 (4)
O20.884 (3)0.193 (5)0.199 (2)0.056 (4)0.62 (13)
O2'0.888 (5)0.155 (6)0.202 (3)0.054 (6)0.38 (13)
O30.6116 (4)0.3714 (3)0.1287 (3)0.0884 (8)
O40.5911 (4)0.1544 (3)0.2070 (3)0.0830 (8)
O50.7109 (4)0.3346 (3)0.3713 (3)0.0940 (9)
N10.2965 (3)0.1831 (2)0.4474 (2)0.0405 (5)
N21.0404 (3)0.1798 (2)0.0742 (2)0.0363 (4)
C10.7333 (3)0.1793 (2)0.2008 (2)0.0344 (5)
C20.5813 (3)0.2303 (3)0.3085 (2)0.0378 (5)
C30.4440 (3)0.1558 (3)0.3458 (2)0.0362 (5)
C40.1579 (4)0.0975 (3)0.4713 (3)0.0506 (6)
C50.2575 (5)0.3017 (4)0.5411 (3)0.0665 (8)
C60.8902 (3)0.2538 (3)0.1638 (2)0.0342 (5)
C70.8890 (4)0.3834 (3)0.2177 (3)0.0438 (6)
C81.0480 (4)0.4350 (3)0.1798 (3)0.0473 (6)
C91.2021 (4)0.3570 (3)0.0899 (3)0.0444 (6)
C101.1939 (3)0.2305 (3)0.0381 (3)0.0425 (5)
H2A0.57290.31360.35450.045*
H3A0.45770.07670.29270.043*
H4A0.14680.04880.56900.076*
H4B0.03670.16790.45310.076*
H4C0.19910.01950.40760.076*
H5A0.24260.40130.48430.100*
H5B0.14290.30340.60760.100*
H5C0.36130.27840.59330.100*
H7A0.78330.43540.27840.053*
H8A1.05010.52200.21530.057*
H9A1.31030.38950.06440.053*
H10A1.29760.17810.02380.051*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.0449 (3)0.0562 (3)0.0583 (3)0.0268 (2)0.01984 (19)0.0357 (2)
Cl10.0418 (4)0.0443 (4)0.0538 (4)0.0178 (3)0.0010 (3)0.0138 (3)
O10.0410 (9)0.0529 (10)0.0518 (10)0.0242 (8)0.0156 (7)0.0284 (8)
O20.043 (5)0.058 (9)0.065 (4)0.020 (5)0.002 (3)0.005 (4)
O2'0.056 (7)0.048 (12)0.043 (6)0.000 (6)0.000 (4)0.004 (5)
O30.0844 (17)0.0648 (14)0.116 (2)0.0251 (12)0.0240 (15)0.0510 (14)
O40.0749 (15)0.0907 (17)0.1056 (19)0.0536 (14)0.0058 (13)0.0364 (15)
O50.0899 (17)0.107 (2)0.0693 (16)0.0239 (15)0.0158 (13)0.0211 (14)
N10.0349 (10)0.0445 (11)0.0394 (10)0.0115 (8)0.0037 (8)0.0098 (8)
N20.0332 (9)0.0386 (10)0.0385 (10)0.0138 (8)0.0016 (7)0.0113 (8)
C10.0348 (11)0.0336 (11)0.0344 (11)0.0097 (9)0.0010 (9)0.0094 (8)
C20.0366 (12)0.0384 (12)0.0382 (12)0.0109 (9)0.0024 (9)0.0145 (9)
C30.0353 (11)0.0343 (12)0.0356 (11)0.0066 (9)0.0020 (9)0.0077 (9)
C40.0408 (13)0.0543 (15)0.0536 (15)0.0188 (12)0.0038 (11)0.0037 (12)
C50.0574 (17)0.082 (2)0.0634 (18)0.0263 (15)0.0204 (14)0.0412 (16)
C60.0355 (11)0.0358 (11)0.0316 (10)0.0116 (9)0.0023 (8)0.0065 (8)
C70.0468 (13)0.0418 (13)0.0451 (13)0.0153 (11)0.0014 (10)0.0174 (10)
C80.0542 (15)0.0443 (14)0.0521 (14)0.0238 (12)0.0077 (12)0.0117 (11)
C90.0418 (13)0.0499 (14)0.0487 (13)0.0245 (11)0.0090 (10)0.0025 (11)
C100.0349 (12)0.0478 (14)0.0442 (13)0.0149 (10)0.0012 (10)0.0080 (10)
Geometric parameters (Å, º) top
Zn1—O1i2.0216 (16)C7—C81.388 (4)
Zn1—O12.0216 (16)C7—H7A0.9300
Zn1—N2i2.0448 (19)C1—O11.261 (3)
Zn1—N22.0448 (19)C1—C21.393 (3)
Zn1—O2'i2.32 (3)C1—C61.505 (3)
Zn1—O2'2.32 (3)C2—C31.375 (3)
Zn1—O22.44 (3)C2—H2A0.9300
Zn1—O2i2.44 (3)C10—C91.369 (4)
Cl1—O21.41 (2)C10—H10A0.9300
Cl1—O41.417 (2)C8—C91.371 (4)
Cl1—O31.418 (2)C8—H8A0.9300
Cl1—O51.419 (2)C3—H3A0.9300
Cl1—O2'1.49 (3)C9—H9A0.9300
N1—C31.308 (3)C5—H5C0.9600
N1—C51.457 (3)C5—H5B0.9600
N1—C41.463 (3)C5—H5A0.9600
N2—C61.340 (3)C4—H4C0.9600
N2—C101.344 (3)C4—H4B0.9600
C7—C61.380 (3)C4—H4A0.9600
O1i—Zn1—O1180.00 (11)C6—N2—Zn1113.31 (14)
O1i—Zn1—N2i80.22 (7)C10—N2—Zn1126.96 (16)
O1—Zn1—N2i99.78 (7)C6—C7—C8118.9 (2)
O1i—Zn1—N299.78 (7)C6—C7—H7A120.5
O1—Zn1—N280.22 (7)C8—C7—H7A120.5
N2i—Zn1—N2180.0O1—C1—C2123.3 (2)
O1i—Zn1—O2'i95.6 (7)O1—C1—C6116.80 (18)
O1—Zn1—O2'i84.4 (7)C2—C1—C6119.82 (19)
N2i—Zn1—O2'i93.1 (16)N2—C6—C7121.0 (2)
N2—Zn1—O2'i86.9 (16)N2—C6—C1113.84 (18)
O1i—Zn1—O2'84.4 (7)C7—C6—C1125.1 (2)
O1—Zn1—O2'95.6 (7)C1—O1—Zn1115.54 (14)
N2i—Zn1—O2'86.9 (16)C3—C2—C1119.1 (2)
N2—Zn1—O2'93.1 (16)C3—C2—H2A120.5
O2'i—Zn1—O2'180.000 (2)C1—C2—H2A120.5
O1i—Zn1—O286.4 (6)N2—C10—C9122.0 (2)
O1—Zn1—O293.6 (6)N2—C10—H10A119.0
N2i—Zn1—O294.7 (8)C9—C10—H10A119.0
N2—Zn1—O285.3 (8)C9—C8—C7119.6 (2)
O2'i—Zn1—O2172.1 (12)C9—C8—H8A120.2
O2'—Zn1—O27.9 (12)C7—C8—H8A120.2
O1i—Zn1—O2i93.6 (6)N1—C3—C2127.6 (2)
O1—Zn1—O2i86.4 (6)N1—C3—H3A116.2
N2i—Zn1—O2i85.3 (8)C2—C3—H3A116.2
N2—Zn1—O2i94.7 (8)C10—C9—C8118.8 (2)
O2'i—Zn1—O2i7.9 (12)C10—C9—H9A120.6
O2'—Zn1—O2i172.1 (12)C8—C9—H9A120.6
O2—Zn1—O2i180.0 (18)N1—C5—H5C109.5
O2—Cl1—O4113.8 (14)N1—C5—H5B109.5
O2—Cl1—O3104.6 (14)H5C—C5—H5B109.5
O4—Cl1—O3109.54 (16)N1—C5—H5A109.5
O2—Cl1—O5106.2 (8)H5C—C5—H5A109.5
O4—Cl1—O5111.11 (18)H5B—C5—H5A109.5
O3—Cl1—O5111.39 (18)N1—C4—H4C109.5
O2—Cl1—O2'13.4 (19)N1—C4—H4B109.5
O4—Cl1—O2'101 (2)H4C—C4—H4B109.5
O3—Cl1—O2'114.6 (18)N1—C4—H4A109.5
O5—Cl1—O2'108.6 (12)H4C—C4—H4A109.5
C3—N1—C5122.6 (2)H4B—C4—H4A109.5
C3—N1—C4121.5 (2)Cl1—O2—Zn1128.9 (11)
C5—N1—C4115.9 (2)Cl1—O2'—Zn1132.5 (16)
C6—N2—C10119.7 (2)
O1i—Zn1—N2—C6176.96 (15)O1—C1—C2—C30.3 (4)
O1—Zn1—N2—C63.04 (15)C6—C1—C2—C3176.8 (2)
N2i—Zn1—N2—C649 (100)C6—N2—C10—C90.3 (3)
O2'i—Zn1—N2—C687.8 (8)Zn1—N2—C10—C9177.01 (17)
O2'—Zn1—N2—C692.2 (8)C6—C7—C8—C90.2 (4)
O2—Zn1—N2—C691.4 (5)C5—N1—C3—C21.0 (4)
O2i—Zn1—N2—C688.6 (5)C4—N1—C3—C2177.7 (2)
O1i—Zn1—N2—C100.5 (2)C1—C2—C3—N1177.0 (2)
O1—Zn1—N2—C10179.5 (2)N2—C10—C9—C80.8 (4)
N2i—Zn1—N2—C10133 (100)C7—C8—C9—C100.8 (4)
O2'i—Zn1—N2—C1094.7 (8)O4—Cl1—O2—Zn143 (3)
O2'—Zn1—N2—C1085.3 (8)O3—Cl1—O2—Zn176 (3)
O2—Zn1—N2—C1086.0 (5)O5—Cl1—O2—Zn1166.1 (19)
O2i—Zn1—N2—C1094.0 (5)O2'—Cl1—O2—Zn164 (7)
C10—N2—C6—C71.3 (3)O1i—Zn1—O2—Cl1153 (3)
Zn1—N2—C6—C7176.35 (17)O1—Zn1—O2—Cl127 (3)
C10—N2—C6—C1176.9 (2)N2i—Zn1—O2—Cl173 (3)
Zn1—N2—C6—C15.4 (2)N2—Zn1—O2—Cl1107 (3)
C8—C7—C6—N21.2 (4)O2'i—Zn1—O2—Cl1102 (8)
C8—C7—C6—C1176.7 (2)O2'—Zn1—O2—Cl178 (8)
O1—C1—C6—N26.0 (3)O2i—Zn1—O2—Cl1121 (100)
C2—C1—C6—N2170.7 (2)O2—Cl1—O2'—Zn195 (8)
O1—C1—C6—C7175.9 (2)O4—Cl1—O2'—Zn167 (5)
C2—C1—C6—C77.4 (3)O3—Cl1—O2'—Zn151 (5)
C2—C1—O1—Zn1173.20 (17)O5—Cl1—O2'—Zn1176 (4)
C6—C1—O1—Zn13.4 (3)O1i—Zn1—O2'—Cl1177 (5)
O1i—Zn1—O1—C1121 (100)O1—Zn1—O2'—Cl13 (5)
N2i—Zn1—O1—C1179.65 (17)N2i—Zn1—O2'—Cl197 (5)
N2—Zn1—O1—C10.35 (17)N2—Zn1—O2'—Cl183 (5)
O2'i—Zn1—O1—C187.4 (16)O2'i—Zn1—O2'—Cl196 (100)
O2'—Zn1—O1—C192.6 (16)O2—Zn1—O2'—Cl178 (8)
O2—Zn1—O1—C185.0 (8)O2i—Zn1—O2'—Cl1102 (8)
O2i—Zn1—O1—C195.0 (8)
Symmetry code: (i) x+2, y, z.
 

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