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In the title compound, [Co(NO2)3(C17H25N3O6)]·H2O or [CoIII(NO2)3(pybox)]·H2O, where pybox is 2,6-bis­[(4R)-(+)-4-iso­propyl-4,5-di­hydro-1,3-oxazol-2-yl]­pyridine, the coord­ination geometry is distorted octahedral. This is the first reported complexation of the pybox mol­ecule to a CoIII atom. The pybox ligand exhibits tridentate coordination to CoIII in a 1:1 ratio and the nitro anions occupy the remaining meridional positions of the octahedron. Molecules are linked, via solvent water mol­ecules, into O—H...O—N hydrogen-bonded chains.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680301643X/bt6314sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680301643X/bt6314Isup2.hkl
Contains datablock I

CCDC reference: 221666

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.067
  • wR factor = 0.153
  • Data-to-parameter ratio = 16.1

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
RINTA_01 Alert C The value of Rint is greater than 0.10 Rint given 0.102 General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.47 From the CIF: _reflns_number_total 4948 Count of symmetry unique reflns 2955 Completeness (_total/calc) 167.45% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1993 Fraction of Friedel pairs measured 0.674 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: COLLECT (Nonius BV, 1997-2002); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXTL (Sheldrick, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
[Co(NO2)3(C17H25N3O6)]·H2OF(000) = 1072
Mr = 516.36Dx = 1.523 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 2747 reflections
a = 6.7185 (3) Åθ = 2.6–27.5°
b = 16.5766 (8) ŵ = 0.82 mm1
c = 20.2149 (10) ÅT = 150 K
V = 2251.33 (19) Å3Needle, colourless
Z = 40.10 × 0.04 × 0.03 mm
Data collection top
Nonius KappaCCD
diffractometer
4948 independent reflections
Radiation source: fine-focus sealed tube3621 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.102
Detector resolution: 9 pixels mm-1θmax = 27.5°, θmin = 3.2°
φ scans, and ω scans with κ offsetsh = 88
Absorption correction: multi-scan
(DENZO-SMN; Otwinowski & Minor, 1997)
k = 2121
Tmin = 0.922, Tmax = 0.976l = 2626
9702 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)] = 0.067H-atom parameters constrained
wR(F2) = 0.153 w = 1/[σ2(Fo2) + 0.7005P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.001
4948 reflectionsΔρmax = 0.71 e Å3
308 parametersΔρmin = 0.71 e Å3
2 restraintsAbsolute structure: Flack (1983); 2017 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.02 (3)
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
Co10.72694 (9)0.13797 (4)0.77949 (3)0.02465 (19)
O10.4723 (6)0.0247 (2)0.89840 (18)0.0355 (9)
O21.0154 (6)0.0784 (3)0.61241 (17)0.0352 (9)
O30.3666 (7)0.0876 (3)0.7214 (3)0.0555 (12)
O40.4164 (6)0.2136 (2)0.7134 (2)0.0435 (10)
O50.8068 (6)0.3004 (2)0.77423 (19)0.0412 (10)
O60.6007 (7)0.2694 (3)0.85087 (19)0.0410 (10)
O71.0786 (7)0.1856 (3)0.8416 (2)0.0539 (13)
O81.0434 (8)0.0589 (3)0.8380 (3)0.0598 (14)
N10.5900 (7)0.0909 (3)0.8551 (2)0.0278 (10)
N20.7368 (7)0.0273 (3)0.75423 (18)0.0263 (9)
N30.8723 (6)0.1487 (3)0.69513 (19)0.0250 (9)
N40.9814 (7)0.1274 (3)0.8245 (2)0.0307 (10)
N50.7125 (7)0.2486 (3)0.8041 (2)0.0300 (10)
N60.4726 (6)0.1471 (3)0.73255 (19)0.0294 (10)
C10.5074 (8)0.1164 (3)0.9199 (2)0.0297 (12)
H1A0.41140.16170.91310.036*
C20.3938 (9)0.0408 (4)0.9414 (3)0.0342 (13)
H2A0.41880.02860.98860.041*
H2B0.24890.04780.93470.041*
C30.5661 (8)0.0138 (3)0.8502 (2)0.0273 (11)
C40.6529 (8)0.0278 (3)0.7933 (2)0.0274 (11)
C50.6561 (8)0.1091 (3)0.7761 (3)0.0350 (12)
H5A0.58920.14810.80240.042*
C60.7588 (8)0.1315 (3)0.7202 (3)0.0372 (11)
H6A0.76560.18680.70830.045*
C70.8533 (9)0.0736 (4)0.6807 (3)0.0339 (13)
H7A0.92670.08900.64260.041*
C80.8364 (8)0.0066 (3)0.6989 (3)0.0299 (12)
C90.9108 (8)0.0800 (4)0.6680 (2)0.0290 (12)
C101.0855 (9)0.1628 (4)0.6038 (3)0.0340 (13)
H10A1.06180.18160.55800.041*
H10B1.22950.16710.61360.041*
C110.9619 (8)0.2133 (3)0.6538 (3)0.0288 (12)
H11A1.05400.24640.68160.035*
C120.6738 (8)0.1436 (4)0.9676 (2)0.0326 (12)
H12A0.76250.18120.94260.039*
C130.8029 (9)0.0734 (4)0.9917 (3)0.0436 (15)
H13A0.91660.09451.01670.065*
H13B0.85120.04260.95360.065*
H13C0.72360.03811.02030.065*
C140.5855 (10)0.1907 (4)1.0242 (3)0.0437 (15)
H14A0.68840.20091.05750.066*
H14B0.47700.15951.04420.066*
H14C0.53350.24211.00780.066*
C150.8066 (8)0.2685 (3)0.6219 (3)0.0358 (13)
H15A0.71970.28950.65820.043*
C160.6732 (9)0.2259 (5)0.5730 (3)0.0504 (18)
H16A0.62030.17660.59320.076*
H16B0.74990.21200.53340.076*
H16C0.56280.26150.56070.076*
C170.9122 (11)0.3412 (4)0.5909 (3)0.0554 (19)
H17A0.81450.37490.56790.083*
H17B1.01240.32220.55930.083*
H17C0.97710.37280.62570.083*
O1W0.6804 (11)0.4392 (4)0.8881 (3)0.095 (2)
H1W0.7150.4710.8580.114*
H2W0.6680.3930.8710.114*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0240 (3)0.0252 (3)0.0248 (3)0.0001 (3)0.0008 (3)0.0002 (3)
O10.036 (2)0.031 (2)0.040 (2)0.0048 (17)0.0065 (17)0.0071 (18)
O20.039 (2)0.038 (2)0.0282 (19)0.0024 (18)0.0045 (17)0.0029 (17)
O30.044 (3)0.039 (3)0.084 (3)0.010 (2)0.031 (3)0.008 (2)
O40.039 (2)0.032 (2)0.059 (3)0.0048 (17)0.011 (2)0.002 (2)
O50.044 (2)0.033 (2)0.046 (2)0.0069 (17)0.008 (2)0.0034 (19)
O60.052 (3)0.033 (2)0.038 (2)0.0011 (19)0.008 (2)0.0075 (18)
O70.046 (3)0.040 (3)0.075 (3)0.006 (2)0.027 (3)0.002 (2)
O80.047 (3)0.042 (3)0.090 (4)0.011 (2)0.034 (3)0.001 (3)
N10.024 (2)0.029 (3)0.030 (2)0.0017 (18)0.0034 (18)0.0005 (19)
N20.020 (2)0.032 (2)0.0263 (18)0.002 (2)0.0026 (18)0.0021 (17)
N30.021 (2)0.029 (2)0.0249 (18)0.0016 (19)0.0005 (16)0.0011 (19)
N40.027 (2)0.036 (3)0.029 (2)0.004 (2)0.0030 (17)0.000 (2)
N50.028 (2)0.032 (2)0.030 (2)0.006 (2)0.0012 (18)0.0002 (19)
N60.033 (2)0.028 (2)0.027 (2)0.001 (2)0.0028 (17)0.001 (2)
C10.027 (3)0.039 (3)0.024 (2)0.005 (2)0.006 (2)0.004 (2)
C20.027 (3)0.041 (3)0.034 (3)0.002 (2)0.006 (2)0.004 (2)
C30.019 (3)0.032 (3)0.030 (3)0.000 (2)0.001 (2)0.004 (2)
C40.026 (3)0.028 (3)0.028 (3)0.003 (2)0.005 (2)0.004 (2)
C50.036 (3)0.027 (3)0.041 (3)0.004 (2)0.003 (3)0.003 (3)
C60.042 (3)0.025 (3)0.044 (3)0.003 (3)0.003 (3)0.007 (3)
C70.034 (3)0.036 (3)0.032 (3)0.004 (2)0.001 (2)0.008 (2)
C80.026 (3)0.035 (3)0.028 (2)0.002 (2)0.001 (2)0.004 (2)
C90.025 (3)0.038 (3)0.024 (2)0.000 (2)0.001 (2)0.003 (2)
C100.029 (3)0.041 (4)0.031 (3)0.003 (2)0.004 (2)0.003 (2)
C110.025 (3)0.034 (3)0.028 (3)0.001 (2)0.002 (2)0.003 (2)
C120.034 (3)0.038 (3)0.026 (2)0.002 (3)0.0020 (19)0.003 (3)
C130.036 (4)0.058 (4)0.036 (3)0.009 (3)0.008 (3)0.004 (3)
C140.052 (4)0.049 (4)0.030 (3)0.006 (3)0.002 (3)0.001 (3)
C150.034 (3)0.038 (3)0.036 (3)0.005 (2)0.006 (2)0.010 (2)
C160.029 (4)0.081 (5)0.041 (3)0.007 (3)0.007 (3)0.008 (3)
C170.060 (5)0.047 (4)0.059 (4)0.013 (3)0.023 (3)0.024 (3)
O1W0.098 (6)0.081 (5)0.106 (5)0.029 (4)0.041 (4)0.024 (4)
Geometric parameters (Å, º) top
Co1—N51.903 (5)C6—C71.400 (8)
Co1—N21.905 (4)C6—H6A0.9500
Co1—N41.945 (5)C7—C81.384 (8)
Co1—N11.946 (4)C7—H7A0.9500
Co1—N61.960 (4)C8—C91.457 (8)
Co1—N31.973 (4)C10—C111.553 (8)
O1—C31.325 (6)C10—H10A0.9900
O1—C21.487 (7)C10—H10B0.9900
O2—C91.326 (6)C11—C151.531 (7)
O2—C101.486 (7)C11—H11A1.0000
O3—N61.236 (6)C12—C141.506 (8)
O4—N61.228 (6)C12—C131.532 (8)
O5—N51.225 (6)C12—H12A1.0000
O6—N51.256 (6)C13—H13A0.9800
O7—N41.214 (6)C13—H13B0.9800
O8—N41.240 (6)C13—H13C0.9800
N1—C31.293 (7)C14—H14A0.9800
N1—C11.485 (6)C14—H14B0.9800
N2—C41.333 (6)C14—H14C0.9800
N2—C81.347 (6)C15—C161.509 (9)
N3—C91.290 (7)C15—C171.531 (9)
N3—C111.486 (7)C15—H15A1.0000
C1—C21.530 (8)C16—H16A0.9800
C1—C121.544 (7)C16—H16B0.9800
C1—H1A1.0000C16—H16C0.9800
C2—H2A0.9900C17—H17A0.9800
C2—H2B0.9900C17—H17B0.9800
C3—C41.462 (7)C17—H17C0.9800
C4—C51.392 (7)O1W—H1W0.8400
C5—C61.375 (8)O1W—H2W0.8400
C5—H5A0.9500
N5—Co1—N2179.0 (2)C8—C7—C6117.9 (5)
N5—Co1—N490.5 (2)C8—C7—H7A121.0
N2—Co1—N490.5 (2)C6—C7—H7A121.0
N5—Co1—N199.03 (18)N2—C8—C7120.5 (5)
N2—Co1—N180.86 (18)N2—C8—C9108.2 (5)
N4—Co1—N190.71 (19)C7—C8—C9131.3 (5)
N5—Co1—N690.45 (19)N3—C9—O2118.9 (5)
N2—Co1—N688.55 (19)N3—C9—C8119.1 (5)
N4—Co1—N6178.8 (2)O2—C9—C8122.0 (5)
N1—Co1—N689.92 (18)O2—C10—C11105.2 (4)
N5—Co1—N399.43 (19)O2—C10—H10A110.7
N2—Co1—N380.69 (18)C11—C10—H10A110.7
N4—Co1—N388.70 (17)O2—C10—H10B110.7
N1—Co1—N3161.53 (18)C11—C10—H10B110.7
N6—Co1—N390.37 (16)H10A—C10—H10B108.8
C3—O1—C2104.3 (4)N3—C11—C15113.1 (4)
C9—O2—C10104.4 (4)N3—C11—C10101.2 (4)
C3—N1—C1107.6 (4)C15—C11—C10114.4 (4)
C3—N1—Co1113.3 (3)N3—C11—H11A109.3
C1—N1—Co1139.1 (4)C15—C11—H11A109.3
C4—N2—C8121.7 (5)C10—C11—H11A109.3
C4—N2—Co1119.1 (3)C14—C12—C13112.0 (4)
C8—N2—Co1119.1 (4)C14—C12—C1109.9 (5)
C9—N3—C11108.4 (4)C13—C12—C1112.7 (5)
C9—N3—Co1112.7 (4)C14—C12—H12A107.3
C11—N3—Co1138.7 (3)C13—C12—H12A107.3
O7—N4—O8118.9 (5)C1—C12—H12A107.3
O7—N4—Co1122.3 (4)C12—C13—H13A109.5
O8—N4—Co1118.7 (4)C12—C13—H13B109.5
O5—N5—O6119.2 (5)H13A—C13—H13B109.5
O5—N5—Co1121.3 (4)C12—C13—H13C109.5
O6—N5—Co1119.5 (4)H13A—C13—H13C109.5
O4—N6—O3118.7 (4)H13B—C13—H13C109.5
O4—N6—Co1119.3 (4)C12—C14—H14A109.5
O3—N6—Co1121.9 (4)C12—C14—H14B109.5
N1—C1—C2101.8 (4)H14A—C14—H14B109.5
N1—C1—C12111.4 (4)C12—C14—H14C109.5
C2—C1—C12115.1 (4)H14A—C14—H14C109.5
N1—C1—H1A109.4H14B—C14—H14C109.5
C2—C1—H1A109.4C16—C15—C11113.6 (5)
C12—C1—H1A109.4C16—C15—C17112.0 (5)
O1—C2—C1104.8 (4)C11—C15—C17109.1 (5)
O1—C2—H2A110.8C16—C15—H15A107.3
C1—C2—H2A110.8C11—C15—H15A107.3
O1—C2—H2B110.8C17—C15—H15A107.3
C1—C2—H2B110.8C15—C16—H16A109.5
H2A—C2—H2B108.9C15—C16—H16B109.5
N1—C3—O1118.7 (5)H16A—C16—H16B109.5
N1—C3—C4118.5 (5)C15—C16—H16C109.5
O1—C3—C4122.8 (5)H16A—C16—H16C109.5
N2—C4—C5120.7 (5)H16B—C16—H16C109.5
N2—C4—C3108.1 (4)C15—C17—H17A109.5
C5—C4—C3131.2 (5)C15—C17—H17B109.5
C6—C5—C4118.3 (5)H17A—C17—H17B109.5
C6—C5—H5A120.9C15—C17—H17C109.5
C4—C5—H5A120.9H17A—C17—H17C109.5
C5—C6—C7120.8 (5)H17B—C17—H17C109.5
C5—C6—H6A119.6H1W—O1W—H2W107
C7—C6—H6A119.6
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H2W···O60.842.142.962 (8)165
O1W—H1W···O3i0.842.573.326 (10)150
Symmetry code: (i) x+1, y+1/2, z+3/2.
 

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