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The tris­(methyl­pyridyl)­amine (tpa, C18H18N4) ligand in the title complex, [CoCl(tpa)(H2O)](ClO4)2·H2O, is bound to the CoIII centre in a tripodal fashion through the four N-donor atoms, allowing the chloro and aqua ligands to occupy the remaining cis sites in the octahedral coordination geometry. The chloro ligand is coordinated trans to the tertiary amine N atom of the tpa ligand. A solvent water mol­ecule is hydrogen bonded to the aqua ligand. The metal-ligand bond lengths are typical for CoIII complexes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804011341/hb6039sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804011341/hb6039Isup2.hkl
Contains datablock I

CCDC reference: 242043

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.004 Å
  • Disorder in solvent or counterion
  • R factor = 0.037
  • wR factor = 0.108
  • Data-to-parameter ratio = 15.5

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT214_ALERT_2_A Atom O9' (Anion/Solvent) ADP max/min Ratio 7.30 prolat PLAT761_ALERT_1_A CIF Contains no X-H Bonds ...................... ? PLAT762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ?
Alert level B PLAT417_ALERT_2_B Short Inter D-H..H-D H1W .. H10B .. 1.63 Ang.
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 .... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.61 Ratio PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl3 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl2 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 27.00 Perc. PLAT355_ALERT_3_C Long O-H Bond (0.82A) O1 - H10B ... 1.01 Ang. PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 33.10 Deg. O8 -CL3 -O9' 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 37.50 Deg. O6 -CL3 -O8' 1.555 1.555 1.555
3 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 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 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

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

(I) top
Crystal data top
[CoCl(C18H18N4)(H2O)](ClO4)2·H2OF(000) = 1264
Mr = 619.68Dx = 1.661 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 1006 reflections
a = 11.882 (2) Åθ = 2.7–27.4°
b = 16.367 (3) ŵ = 1.08 mm1
c = 12.744 (3) ÅT = 150 K
β = 90.353 (3)°Block, purple
V = 2478.5 (9) Å30.49 × 0.38 × 0.19 mm
Z = 4
Data collection top
Bruker SMART1000 CCD
diffractometer
5830 independent reflections
Radiation source: fine-focus sealed tube4486 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ω scansθmax = 28.0°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1515
Tmin = 0.628, Tmax = 0.815k = 2121
23833 measured reflectionsl = 1616
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)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.0669P)2 + 0.0165P]
where P = (Fo2 + 2Fc2)/3
5830 reflections(Δ/σ)max = 0.001
377 parametersΔρmax = 0.51 e Å3
0 restraintsΔρmin = 0.37 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)
Co10.76235 (2)0.141385 (16)0.28829 (2)0.02811 (10)
Cl10.76105 (5)0.21723 (3)0.43276 (4)0.03919 (14)
O10.72365 (16)0.23648 (10)0.20614 (13)0.0379 (4)
H10A0.769 (3)0.274 (2)0.208 (2)0.053 (9)*
H10B0.646 (3)0.258 (2)0.222 (2)0.069 (9)*
N10.91744 (15)0.16105 (11)0.25322 (13)0.0310 (4)
N20.80345 (14)0.04209 (10)0.35953 (13)0.0274 (4)
N30.60598 (15)0.10924 (12)0.29796 (15)0.0370 (4)
N40.75999 (16)0.07759 (11)0.15897 (13)0.0333 (4)
C10.99880 (19)0.18744 (13)0.31829 (17)0.0347 (5)
H10.98060.20030.38890.042*
C21.1081 (2)0.19627 (15)0.2851 (2)0.0439 (6)
H21.16470.21510.33220.053*
C31.1346 (2)0.17756 (17)0.1828 (2)0.0519 (7)
H31.20980.18330.15870.062*
C41.0510 (2)0.15042 (16)0.1154 (2)0.0489 (6)
H41.06780.13770.04440.059*
C50.9430 (2)0.14211 (14)0.15277 (17)0.0377 (5)
C60.8448 (2)0.11486 (16)0.08704 (17)0.0424 (6)
H6A0.81140.16210.04960.051*
H6B0.86950.07430.03440.051*
C70.82774 (17)0.03308 (14)0.46247 (16)0.0320 (4)
H70.82870.07980.50680.038*
C80.8512 (2)0.04268 (15)0.50443 (17)0.0392 (5)
H80.86890.04800.57690.047*
C90.8489 (2)0.11088 (16)0.44056 (19)0.0438 (6)
H90.86390.16350.46880.053*
C100.8248 (2)0.10161 (14)0.33548 (18)0.0418 (5)
H100.82200.14770.29030.050*
C110.80455 (18)0.02385 (13)0.29681 (16)0.0316 (4)
C120.7888 (2)0.00943 (14)0.18251 (17)0.0408 (5)
H12A0.72780.04520.15590.049*
H12B0.85880.02420.14530.049*
C130.5422 (2)0.11014 (17)0.3842 (2)0.0487 (6)
H130.57130.13340.44710.058*
C140.4348 (2)0.0779 (2)0.3834 (3)0.0735 (10)
H140.39040.07910.44510.088*
C150.3927 (3)0.0441 (3)0.2928 (3)0.0826 (11)
H150.31900.02170.29120.099*
C160.4587 (3)0.0431 (2)0.2039 (3)0.0729 (10)
H160.43120.01910.14090.088*
C170.5649 (2)0.07712 (16)0.2074 (2)0.0468 (6)
C180.6428 (2)0.08390 (16)0.11659 (19)0.0452 (6)
H18A0.63200.13690.08050.054*
H18B0.62810.03940.06570.054*
Cl20.89613 (5)0.41897 (3)0.28661 (4)0.03749 (14)
O20.97740 (14)0.38819 (12)0.35987 (13)0.0495 (4)
O30.93851 (17)0.49084 (11)0.23601 (14)0.0545 (5)
O40.79298 (16)0.43535 (15)0.33940 (16)0.0664 (6)
O50.8773 (2)0.35792 (12)0.20633 (15)0.0609 (6)
Cl30.37223 (6)0.18579 (4)0.95830 (6)0.05160 (17)
O60.3363 (4)0.1915 (3)0.8534 (3)0.0918 (16)0.66
O70.3282 (5)0.1121 (2)1.0049 (3)0.0906 (14)0.66
O80.3396 (7)0.2502 (3)1.0185 (6)0.151 (3)0.66
O90.4900 (3)0.1824 (5)0.9560 (4)0.1174 (19)0.66
O6'0.2535 (5)0.1727 (5)0.9626 (6)0.079 (2)0.34
O7'0.4353 (8)0.1197 (5)0.9464 (7)0.086 (3)0.34
O8'0.3748 (10)0.2408 (8)0.8641 (12)0.161 (6)0.34
O9'0.3934 (11)0.2327 (9)1.0456 (13)0.185 (9)0.34
O1W0.5220 (3)0.2960 (2)0.2008 (3)0.1023 (10)
H1W0.5515 (18)0.3224 (13)0.2633 (18)0.017 (5)*
H2W0.473 (2)0.3377 (17)0.176 (2)0.046 (8)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.03459 (17)0.02559 (16)0.02406 (15)0.00125 (11)0.00645 (11)0.00190 (10)
Cl10.0489 (3)0.0346 (3)0.0340 (3)0.0022 (2)0.0026 (2)0.0113 (2)
O10.0440 (10)0.0291 (8)0.0404 (9)0.0020 (8)0.0105 (7)0.0021 (7)
N10.0410 (10)0.0261 (9)0.0258 (9)0.0004 (7)0.0025 (7)0.0051 (7)
N20.0305 (9)0.0282 (9)0.0233 (8)0.0016 (7)0.0035 (7)0.0019 (7)
N30.0338 (10)0.0344 (10)0.0428 (11)0.0012 (8)0.0075 (8)0.0073 (8)
N40.0461 (11)0.0308 (9)0.0230 (8)0.0030 (8)0.0085 (7)0.0009 (7)
C10.0402 (12)0.0291 (11)0.0345 (11)0.0009 (9)0.0059 (9)0.0067 (9)
C20.0427 (13)0.0391 (13)0.0498 (14)0.0054 (10)0.0062 (11)0.0160 (11)
C30.0461 (14)0.0492 (15)0.0605 (17)0.0009 (12)0.0130 (12)0.0206 (13)
C40.0585 (16)0.0479 (15)0.0405 (14)0.0031 (12)0.0125 (12)0.0124 (11)
C50.0510 (14)0.0341 (12)0.0279 (11)0.0021 (10)0.0002 (10)0.0086 (9)
C60.0606 (15)0.0445 (13)0.0221 (10)0.0039 (12)0.0016 (10)0.0041 (9)
C70.0353 (11)0.0370 (11)0.0236 (10)0.0031 (9)0.0012 (8)0.0016 (8)
C80.0461 (13)0.0455 (13)0.0261 (10)0.0011 (11)0.0039 (9)0.0074 (10)
C90.0549 (15)0.0372 (13)0.0393 (13)0.0044 (11)0.0027 (11)0.0119 (10)
C100.0581 (15)0.0295 (12)0.0377 (12)0.0040 (11)0.0031 (11)0.0002 (10)
C110.0391 (11)0.0296 (11)0.0261 (10)0.0011 (9)0.0040 (8)0.0007 (8)
C120.0664 (16)0.0297 (11)0.0263 (11)0.0084 (11)0.0073 (10)0.0015 (9)
C130.0378 (13)0.0504 (15)0.0580 (16)0.0021 (11)0.0003 (11)0.0133 (13)
C140.0431 (16)0.090 (2)0.087 (2)0.0149 (16)0.0102 (16)0.022 (2)
C150.0416 (16)0.103 (3)0.103 (3)0.0212 (18)0.0038 (17)0.029 (2)
C160.0526 (17)0.085 (2)0.080 (2)0.0129 (16)0.0264 (16)0.0253 (19)
C170.0425 (13)0.0463 (14)0.0514 (15)0.0013 (11)0.0186 (11)0.0109 (11)
C180.0528 (14)0.0462 (14)0.0363 (12)0.0025 (11)0.0204 (11)0.0074 (10)
Cl20.0482 (3)0.0345 (3)0.0297 (3)0.0005 (2)0.0058 (2)0.0033 (2)
O20.0476 (10)0.0636 (12)0.0373 (9)0.0044 (9)0.0052 (8)0.0137 (8)
O30.0837 (14)0.0342 (9)0.0455 (10)0.0076 (9)0.0105 (9)0.0079 (8)
O40.0532 (12)0.0882 (16)0.0578 (12)0.0258 (11)0.0064 (9)0.0149 (11)
O50.0884 (15)0.0494 (11)0.0447 (11)0.0273 (10)0.0015 (10)0.0081 (8)
Cl30.0486 (4)0.0467 (4)0.0595 (4)0.0054 (3)0.0089 (3)0.0025 (3)
O60.091 (3)0.101 (3)0.083 (3)0.033 (3)0.055 (2)0.048 (3)
O70.176 (5)0.0472 (19)0.0486 (19)0.031 (2)0.012 (2)0.0030 (16)
O80.230 (8)0.046 (2)0.180 (6)0.012 (4)0.130 (6)0.001 (3)
O90.052 (2)0.222 (6)0.077 (3)0.030 (3)0.018 (2)0.026 (4)
O6'0.052 (4)0.098 (6)0.088 (5)0.027 (4)0.023 (3)0.024 (4)
O7'0.087 (6)0.078 (5)0.092 (6)0.044 (4)0.032 (5)0.020 (5)
O8'0.127 (10)0.124 (10)0.233 (15)0.051 (8)0.064 (9)0.111 (10)
O9'0.158 (11)0.160 (13)0.236 (15)0.018 (8)0.134 (11)0.144 (11)
O1W0.0770 (18)0.119 (3)0.111 (2)0.0354 (18)0.0010 (17)0.000 (2)
Geometric parameters (Å, º) top
Co1—N21.9232 (17)C8—C91.382 (4)
Co1—N11.9260 (19)C9—C101.376 (3)
Co1—O11.9298 (16)C10—C111.385 (3)
Co1—N31.9357 (19)C11—C121.486 (3)
Co1—N41.9510 (18)C13—C141.380 (4)
Co1—Cl12.2207 (7)C14—C151.372 (5)
N1—C11.341 (3)C15—C161.382 (5)
N1—C51.353 (3)C16—C171.379 (4)
N2—C111.343 (3)C17—C181.491 (4)
N2—C71.350 (2)Cl2—O41.4272 (19)
N3—C131.339 (3)Cl2—O21.4307 (17)
N3—C171.357 (3)Cl2—O31.4342 (18)
N4—C181.494 (3)Cl2—O51.4466 (19)
N4—C121.495 (3)Cl3—O7'1.326 (7)
N4—C61.496 (3)Cl3—O81.361 (5)
C1—C21.376 (3)Cl3—O9'1.374 (10)
C2—C31.378 (4)Cl3—O91.401 (4)
C3—C41.383 (4)Cl3—O61.405 (4)
C4—C51.379 (4)Cl3—O6'1.429 (6)
C5—C61.500 (3)Cl3—O71.444 (4)
C7—C81.378 (3)Cl3—O8'1.501 (11)
N2—Co1—N190.59 (7)C10—C11—C12121.0 (2)
N2—Co1—O1175.31 (7)C11—C12—N4112.04 (17)
N1—Co1—O187.96 (8)N3—C13—C14121.2 (3)
N2—Co1—N388.93 (8)C15—C14—C13119.5 (3)
N1—Co1—N3168.62 (8)C14—C15—C16119.3 (3)
O1—Co1—N391.61 (8)C17—C16—C15119.5 (3)
N2—Co1—N487.07 (7)N3—C17—C16120.5 (3)
N1—Co1—N484.39 (8)N3—C17—C18114.2 (2)
O1—Co1—N488.35 (7)C16—C17—C18125.3 (3)
N3—Co1—N484.23 (8)C17—C18—N4107.25 (19)
N2—Co1—Cl194.82 (5)O4—Cl2—O2109.67 (11)
N1—Co1—Cl196.35 (6)O4—Cl2—O3111.28 (13)
O1—Co1—Cl189.78 (5)O2—Cl2—O3110.17 (12)
N3—Co1—Cl195.02 (6)O4—Cl2—O5109.48 (14)
N4—Co1—Cl1177.96 (6)O2—Cl2—O5108.61 (13)
C1—N1—C5119.6 (2)O3—Cl2—O5107.57 (11)
C1—N1—Co1126.68 (15)O7'—Cl3—O8149.3 (5)
C5—N1—Co1113.69 (15)O7'—Cl3—O9'116.6 (6)
C11—N2—C7119.20 (18)O8—Cl3—O9'33.1 (6)
C11—N2—Co1113.67 (13)O7'—Cl3—O953.1 (4)
C7—N2—Co1127.11 (15)O8—Cl3—O9109.3 (4)
C13—N3—C17120.0 (2)O9'—Cl3—O982.0 (6)
C13—N3—Co1126.71 (16)O7'—Cl3—O696.6 (4)
C17—N3—Co1113.07 (17)O8—Cl3—O6113.5 (4)
C18—N4—C12110.49 (19)O9'—Cl3—O6141.9 (7)
C18—N4—C6112.33 (18)O9—Cl3—O6106.3 (3)
C12—N4—C6110.93 (19)O7'—Cl3—O6'116.2 (6)
C18—N4—Co1106.08 (14)O8—Cl3—O6'79.0 (4)
C12—N4—Co1109.77 (13)O9'—Cl3—O6'103.2 (7)
C6—N4—Co1107.04 (13)O9—Cl3—O6'169.1 (4)
N1—C1—C2121.4 (2)O6—Cl3—O6'75.6 (4)
C1—C2—C3119.3 (2)O7'—Cl3—O764.6 (5)
C2—C3—C4119.4 (2)O8—Cl3—O7108.1 (3)
C5—C4—C3118.9 (2)O9'—Cl3—O7101.5 (8)
N1—C5—C4121.3 (2)O9—Cl3—O7109.9 (3)
N1—C5—C6114.7 (2)O6—Cl3—O7109.8 (2)
C4—C5—C6124.0 (2)O6'—Cl3—O759.9 (4)
N4—C6—C5107.67 (17)O7'—Cl3—O8'112.6 (7)
N2—C7—C8121.1 (2)O8—Cl3—O8'89.6 (6)
C7—C8—C9119.7 (2)O9'—Cl3—O8'107.9 (10)
C10—C9—C8119.2 (2)O9—Cl3—O8'89.0 (5)
C9—C10—C11118.8 (2)O6—Cl3—O8'37.5 (7)
N2—C11—C10121.9 (2)O6'—Cl3—O8'98.4 (6)
N2—C11—C12117.00 (18)O7—Cl3—O8'147.1 (7)
N2—Co1—N1—C175.13 (18)C2—C3—C4—C50.5 (4)
O1—Co1—N1—C1109.33 (18)C1—N1—C5—C40.9 (3)
N3—Co1—N1—C1162.6 (4)Co1—N1—C5—C4178.26 (18)
N4—Co1—N1—C1162.13 (18)C1—N1—C5—C6178.88 (19)
Cl1—Co1—N1—C119.79 (18)Co1—N1—C5—C63.7 (2)
N2—Co1—N1—C5102.04 (15)C3—C4—C5—N10.9 (4)
O1—Co1—N1—C573.50 (15)C3—C4—C5—C6178.8 (2)
N3—Co1—N1—C514.5 (5)C18—N4—C6—C5153.12 (19)
N4—Co1—N1—C515.04 (15)C12—N4—C6—C582.7 (2)
Cl1—Co1—N1—C5163.05 (14)Co1—N4—C6—C537.1 (2)
N1—Co1—N2—C1188.70 (15)N1—C5—C6—N427.4 (3)
N3—Co1—N2—C1179.94 (15)C4—C5—C6—N4154.7 (2)
N4—Co1—N2—C114.35 (15)C11—N2—C7—C81.4 (3)
Cl1—Co1—N2—C11174.89 (14)Co1—N2—C7—C8177.08 (16)
N1—Co1—N2—C792.76 (17)N2—C7—C8—C90.6 (3)
N3—Co1—N2—C798.61 (17)C7—C8—C9—C100.9 (4)
N4—Co1—N2—C7177.11 (17)C8—C9—C10—C110.6 (4)
Cl1—Co1—N2—C73.66 (17)C7—N2—C11—C103.1 (3)
N2—Co1—N3—C1373.8 (2)Co1—N2—C11—C10175.60 (18)
N1—Co1—N3—C13161.5 (3)C7—N2—C11—C12173.92 (19)
O1—Co1—N3—C13110.9 (2)Co1—N2—C11—C127.4 (3)
N4—Co1—N3—C13161.0 (2)C9—C10—C11—N22.7 (4)
Cl1—Co1—N3—C1320.9 (2)C9—C10—C11—C12174.2 (2)
N2—Co1—N3—C17100.69 (18)N2—C11—C12—N47.0 (3)
N1—Co1—N3—C1713.0 (5)C10—C11—C12—N4175.9 (2)
O1—Co1—N3—C1774.65 (18)C18—N4—C12—C11113.5 (2)
N4—Co1—N3—C1713.53 (18)C6—N4—C12—C11121.3 (2)
Cl1—Co1—N3—C17164.57 (17)Co1—N4—C12—C113.2 (2)
N2—Co1—N4—C18119.78 (15)C17—N3—C13—C140.8 (4)
N1—Co1—N4—C18149.34 (15)Co1—N3—C13—C14173.3 (2)
O1—Co1—N4—C1861.23 (15)N3—C13—C14—C150.2 (5)
N3—Co1—N4—C1830.56 (15)C13—C14—C15—C160.0 (6)
N2—Co1—N4—C120.39 (16)C14—C15—C16—C171.0 (6)
N1—Co1—N4—C1291.27 (16)C13—N3—C17—C161.9 (4)
O1—Co1—N4—C12179.39 (16)Co1—N3—C17—C16173.0 (2)
N3—Co1—N4—C1288.83 (16)C13—N3—C17—C18177.1 (2)
N2—Co1—N4—C6120.09 (14)Co1—N3—C17—C188.0 (3)
N1—Co1—N4—C629.21 (14)C15—C16—C17—N32.0 (5)
O1—Co1—N4—C658.90 (15)C15—C16—C17—C18176.9 (3)
N3—Co1—N4—C6150.69 (15)N3—C17—C18—N432.8 (3)
C5—N1—C1—C20.4 (3)C16—C17—C18—N4148.2 (3)
Co1—N1—C1—C2177.44 (16)C12—N4—C18—C1777.9 (2)
N1—C1—C2—C30.0 (3)C6—N4—C18—C17157.66 (19)
C1—C2—C3—C40.1 (4)Co1—N4—C18—C1741.0 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H10A···O50.82 (3)1.88 (3)2.699 (3)177 (3)
O1—H10B···O1W1.02 (3)1.61 (3)2.587 (3)159 (3)
 

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