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The tris­(methyl­pyridyl)­amine (tpa, C18H18N4) ligand in the title complex, [Co(tpa)Cl2]ClO4·0.5H2O, is bound to the CoIII centre in a tripodal fashion through the four N-donor atoms, allowing the two chloro ligands to occupy the remaining cis sites in the octahedral coordination sphere. Half a solvent water mol­ecule is disordered over two sites. The metal-ligand bond lengths are typical for CoIII complexes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803014545/tk6111sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803014545/tk6111Isup2.hkl
Contains datablock I

CCDC reference: 221637

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.002 Å
  • Disorder in solvent or counterion
  • R factor = 0.025
  • wR factor = 0.074
  • Data-to-parameter ratio = 26.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ......................... 7.00 Perc.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: SMART (Bruker, 1995); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).

(I) top
Crystal data top
[CoCl2(C18H18N4)]ClO4·0.5H20F(000) = 1072
Mr = 527.64Dx = 1.669 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 172 reflections
a = 10.2642 (14) Åθ = 2.0–33.0°
b = 15.166 (2) ŵ = 1.24 mm1
c = 14.2695 (19) ÅT = 150 K
β = 109.001 (3)°Prism, purple
V = 2100.2 (5) Å30.50 × 0.30 × 0.10 mm
Z = 4
Data collection top
Bruker CCD
diffractometer
7781 independent reflections
Radiation source: fine-focus sealed tube6722 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
φ and ω scansθmax = 33.0°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1515
Tmin = 0.577, Tmax = 0.886k = 2323
31017 measured reflectionsl = 2121
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)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.074H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0426P)2 + 0.434P]
where P = (Fo2 + 2Fc2)/3
7781 reflections(Δ/σ)max < 0.001
289 parametersΔρmax = 0.51 e Å3
0 restraintsΔρmin = 0.41 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
O10.20457 (10)0.32163 (6)0.46979 (7)0.0307 (2)
O20.32278 (11)0.40702 (7)0.55322 (8)0.0345 (2)
O30.08170 (11)0.41913 (7)0.59653 (8)0.0420 (3)
O40.22488 (12)0.47548 (8)0.44473 (8)0.0412 (3)
OWA0.0048 (8)0.5265 (5)0.1789 (7)0.088 (2)0.25
OWB0.0005 (12)0.6162 (7)0.1742 (8)0.121 (3)0.25
C10.20480 (14)0.47534 (9)0.07732 (9)0.0281 (2)
H10.14980.43900.02520.034*
C20.20330 (17)0.56605 (10)0.06390 (11)0.0380 (3)
H20.14840.59130.00290.046*
C30.28221 (17)0.61954 (9)0.13991 (12)0.0374 (3)
H30.28110.68180.13190.045*
C40.36292 (15)0.58119 (8)0.22795 (10)0.0294 (2)
H40.41810.61660.28100.035*
C50.36164 (12)0.49015 (7)0.23714 (8)0.02076 (19)
C60.44529 (11)0.44078 (7)0.32785 (8)0.02020 (19)
H6A0.53590.42410.32260.024*
H6B0.46060.47750.38780.024*
C70.00996 (11)0.28716 (8)0.15453 (8)0.0218 (2)
H70.01220.26310.09260.026*
C80.12999 (12)0.28903 (8)0.17903 (9)0.0256 (2)
H80.21380.26740.13380.031*
C90.12680 (12)0.32276 (8)0.27030 (9)0.0246 (2)
H90.20810.32440.28820.029*
C100.00312 (12)0.35395 (8)0.33473 (8)0.0219 (2)
H100.00190.37690.39780.026*
C110.11301 (11)0.35112 (7)0.30552 (7)0.01754 (17)
C120.24698 (11)0.38819 (7)0.36834 (8)0.01968 (19)
H12A0.26590.36840.43760.024*
H12B0.24110.45340.36740.024*
C130.25924 (13)0.12200 (8)0.21771 (9)0.0248 (2)
H130.20720.12080.14910.030*
C140.27840 (16)0.04450 (8)0.27235 (10)0.0327 (3)
H140.24180.00950.24110.039*
C150.35140 (16)0.04679 (8)0.37271 (10)0.0324 (3)
H150.36500.00570.41110.039*
C160.40455 (14)0.12635 (8)0.41688 (9)0.0263 (2)
H160.45290.12950.48600.032*
C170.38559 (12)0.20120 (7)0.35812 (8)0.01956 (19)
C180.44851 (12)0.28888 (7)0.39647 (8)0.02108 (19)
H18A0.45140.29670.46600.025*
H18B0.54400.29170.39470.025*
N10.28262 (10)0.43799 (6)0.16269 (7)0.01991 (17)
N20.11016 (9)0.31880 (6)0.21676 (7)0.01685 (15)
N30.31309 (10)0.19884 (6)0.26012 (7)0.01822 (16)
N40.36372 (9)0.36015 (6)0.33316 (6)0.01649 (15)
Cl10.20281 (3)0.266105 (19)0.041265 (19)0.02402 (6)
Cl20.50300 (3)0.302188 (18)0.18381 (2)0.02212 (6)
Cl30.20722 (3)0.406110 (17)0.516501 (19)0.02069 (5)
Co10.290232 (14)0.313712 (9)0.197717 (10)0.01524 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0341 (5)0.0295 (5)0.0297 (4)0.0027 (4)0.0120 (4)0.0110 (4)
O20.0422 (5)0.0298 (5)0.0427 (5)0.0058 (4)0.0290 (5)0.0107 (4)
O30.0351 (5)0.0355 (5)0.0398 (6)0.0011 (4)0.0094 (4)0.0058 (4)
O40.0470 (6)0.0376 (6)0.0388 (5)0.0000 (5)0.0136 (5)0.0188 (4)
OWA0.086 (5)0.065 (4)0.135 (7)0.022 (4)0.064 (5)0.011 (4)
OWB0.135 (8)0.115 (8)0.130 (8)0.037 (7)0.068 (7)0.024 (6)
C10.0328 (6)0.0262 (6)0.0243 (5)0.0020 (5)0.0079 (4)0.0063 (4)
C20.0481 (8)0.0280 (6)0.0366 (7)0.0053 (6)0.0119 (6)0.0149 (5)
C30.0518 (9)0.0195 (5)0.0443 (8)0.0021 (5)0.0205 (7)0.0094 (5)
C40.0394 (7)0.0177 (5)0.0350 (6)0.0050 (5)0.0176 (5)0.0003 (4)
C50.0244 (5)0.0166 (4)0.0243 (5)0.0031 (4)0.0120 (4)0.0005 (4)
C60.0212 (5)0.0173 (4)0.0222 (5)0.0050 (4)0.0071 (4)0.0029 (4)
C70.0203 (5)0.0226 (5)0.0214 (5)0.0010 (4)0.0054 (4)0.0037 (4)
C80.0196 (5)0.0273 (5)0.0287 (6)0.0013 (4)0.0063 (4)0.0035 (4)
C90.0202 (5)0.0262 (5)0.0297 (6)0.0019 (4)0.0114 (4)0.0010 (4)
C100.0228 (5)0.0231 (5)0.0225 (5)0.0024 (4)0.0109 (4)0.0002 (4)
C110.0203 (4)0.0157 (4)0.0177 (4)0.0008 (3)0.0077 (3)0.0001 (3)
C120.0224 (5)0.0199 (5)0.0189 (4)0.0032 (4)0.0096 (4)0.0050 (4)
C130.0340 (6)0.0178 (5)0.0236 (5)0.0041 (4)0.0108 (4)0.0041 (4)
C140.0511 (8)0.0162 (5)0.0337 (6)0.0049 (5)0.0176 (6)0.0028 (4)
C150.0516 (8)0.0180 (5)0.0323 (6)0.0023 (5)0.0199 (6)0.0048 (4)
C160.0375 (6)0.0208 (5)0.0223 (5)0.0049 (4)0.0121 (5)0.0043 (4)
C170.0244 (5)0.0178 (4)0.0176 (4)0.0019 (4)0.0084 (4)0.0001 (3)
C180.0241 (5)0.0189 (5)0.0171 (4)0.0005 (4)0.0024 (4)0.0001 (4)
N10.0225 (4)0.0182 (4)0.0203 (4)0.0005 (3)0.0087 (3)0.0023 (3)
N20.0191 (4)0.0152 (4)0.0166 (4)0.0007 (3)0.0062 (3)0.0009 (3)
N30.0225 (4)0.0152 (4)0.0183 (4)0.0004 (3)0.0086 (3)0.0014 (3)
N40.0188 (4)0.0146 (4)0.0164 (4)0.0016 (3)0.0060 (3)0.0010 (3)
Cl10.02860 (13)0.02813 (13)0.01611 (11)0.00402 (10)0.00835 (9)0.00495 (9)
Cl20.02044 (11)0.02485 (12)0.02337 (12)0.00111 (9)0.01027 (9)0.00005 (9)
Cl30.02264 (11)0.02028 (11)0.01913 (11)0.00037 (9)0.00676 (9)0.00005 (8)
Co10.01774 (7)0.01438 (7)0.01429 (6)0.00091 (4)0.00615 (5)0.00102 (4)
Geometric parameters (Å, º) top
O1—Cl31.4485 (9)C10—H100.9500
O2—Cl31.4445 (10)C11—N21.3495 (13)
O3—Cl31.4300 (10)C11—C121.4859 (15)
O4—Cl31.4379 (10)C12—N41.5035 (14)
C1—N11.3450 (15)C12—H12A0.9900
C1—C21.3884 (19)C12—H12B0.9900
C1—H10.9500C13—N31.3460 (14)
C2—C31.385 (2)C13—C141.3886 (17)
C2—H20.9500C13—H130.9500
C3—C41.388 (2)C14—C151.384 (2)
C3—H30.9500C14—H140.9500
C4—C51.3874 (16)C15—C161.3881 (18)
C4—H40.9500C15—H150.9500
C5—N11.3605 (14)C16—C171.3868 (15)
C5—C61.4998 (16)C16—H160.9500
C6—N41.4977 (14)C17—N31.3538 (14)
C6—H6A0.9900C17—C181.5015 (15)
C6—H6B0.9900C18—N41.4933 (14)
C7—N21.3513 (14)C18—H18A0.9900
C7—C81.3862 (16)C18—H18B0.9900
C7—H70.9500Co1—N11.9450 (10)
C8—C91.3896 (17)Co1—N21.9553 (9)
C8—H80.9500Co1—N31.9357 (9)
C9—C101.3858 (17)Co1—N41.9624 (9)
C9—H90.9500Co1—Cl12.2374 (4)
C10—C111.3856 (15)Co1—Cl22.2630 (4)
N1—C1—C2121.25 (13)C16—C15—H15120.3
N1—C1—H1119.4C17—C16—C15118.68 (11)
C2—C1—H1119.4C17—C16—H16120.7
C3—C2—C1119.66 (13)C15—C16—H16120.7
C3—C2—H2120.2N3—C17—C16121.64 (10)
C1—C2—H2120.2N3—C17—C18115.24 (9)
C2—C3—C4119.21 (12)C16—C17—C18123.06 (10)
C2—C3—H3120.4N4—C18—C17108.89 (9)
C4—C3—H3120.4N4—C18—H18A109.9
C5—C4—C3118.78 (13)C17—C18—H18A109.9
C5—C4—H4120.6N4—C18—H18B109.9
C3—C4—H4120.6C17—C18—H18B109.9
N1—C5—C4121.76 (11)H18A—C18—H18B108.3
N1—C5—C6114.33 (9)C1—N1—C5119.32 (10)
C4—C5—C6123.91 (11)C1—N1—Co1127.09 (8)
N4—C6—C5106.19 (8)C5—N1—Co1113.50 (7)
N4—C6—H6A110.5C11—N2—C7118.82 (9)
C5—C6—H6A110.5C11—N2—Co1114.34 (7)
N4—C6—H6B110.5C7—N2—Co1126.59 (8)
C5—C6—H6B110.5C13—N3—C17119.64 (10)
H6A—C6—H6B108.7C13—N3—Co1126.99 (8)
N2—C7—C8121.51 (10)C17—N3—Co1113.26 (7)
N2—C7—H7119.2C18—N4—C6113.35 (8)
C8—C7—H7119.2C18—N4—C12111.93 (8)
C7—C8—C9119.49 (11)C6—N4—C12107.79 (8)
C7—C8—H8120.3C18—N4—Co1107.30 (6)
C9—C8—H8120.3C6—N4—Co1106.57 (6)
C10—C9—C8118.96 (11)C12—N4—Co1109.74 (6)
C10—C9—H9120.5O3—Cl3—O4109.85 (7)
C8—C9—H9120.5O3—Cl3—O2109.99 (7)
C11—C10—C9118.81 (10)O4—Cl3—O2108.87 (7)
C11—C10—H10120.6O3—Cl3—O1110.04 (6)
C9—C10—H10120.6O4—Cl3—O1109.65 (7)
N2—C11—C10122.39 (10)O2—Cl3—O1108.42 (6)
N2—C11—C12115.89 (9)N3—Co1—N1168.26 (4)
C10—C11—C12121.64 (9)N3—Co1—N287.14 (4)
C11—C12—N4111.91 (8)N1—Co1—N292.11 (4)
C11—C12—H12A109.2N3—Co1—N485.40 (4)
N4—C12—H12A109.2N1—Co1—N482.86 (4)
C11—C12—H12B109.2N2—Co1—N485.79 (4)
N4—C12—H12B109.2N3—Co1—Cl196.76 (3)
H12A—C12—H12B107.9N1—Co1—Cl194.98 (3)
N3—C13—C14121.19 (11)N2—Co1—Cl193.51 (3)
N3—C13—H13119.4N4—Co1—Cl1177.70 (3)
C14—C13—H13119.4N3—Co1—Cl289.71 (3)
C15—C14—C13119.34 (12)N1—Co1—Cl290.66 (3)
C15—C14—H14120.3N2—Co1—Cl2176.47 (3)
C13—C14—H14120.3N4—Co1—Cl292.38 (3)
C14—C15—C16119.47 (11)Cl1—Co1—Cl288.429 (13)
C14—C15—H15120.3
 

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