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The crystal structure of a CoII complex with 1,4-di­aza­cyclo­heptane (DACH) functionalized by two additional pyridine donor pendants, [CoCl(L)](ClO4), where L = 1,4-bis­(pyridyl-2-yl­methyl)-DACH (C17H22N4), has been determined by X-ray diffraction analysis. In the mononuclear complex, the CoII center is pentacoordinated by the four nitro­gen donors of the ligand and one axial chloride anion, resulting in a coordination sphere intermediate between ideal square-pyramidal and trigonal bipyramidal. It forms a one-dimensional linear structure through intermolecular C—H...Cl and C—H...O hydrogen-bonding interactions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680201293X/ww6033sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680201293X/ww6033Isup2.hkl
Contains datablock I

CCDC reference: 193722

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.049
  • wR factor = 0.091
  • Data-to-parameter ratio = 14.1

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








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: XP (Bruker, 1998); software used to prepare material for publication: SHELXL97.

[1,4-Bis(pyridyl-2-ylmethyl)-1,4-diazacycloheptane]chlorocobalt(II) perchlorate top
Crystal data top
[CoCl(C17H22N4)](ClO4)F(000) = 980
Mr = 476.22Dx = 1.570 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 12.286 (4) ÅCell parameters from 8012 reflections
b = 7.300 (2) Åθ = 1.7–25.0°
c = 22.573 (7) ŵ = 1.15 mm1
β = 95.731 (6)°T = 293 K
V = 2014.5 (10) Å3Prism, purple
Z = 40.30 × 0.25 × 0.20 mm
Data collection top
Bruker SMART 1000
diffractometer
1824 reflections with I > 2.0σ(I)
ω scansRint = 0.084
Absorption correction: multi-scan
[SAINT (Bruker 1998) and SADABS (Sheldrick, 1997)]
θmax = 25.0°
Tmin = 0.725, Tmax = 0.803h = 1314
8055 measured reflectionsk = 78
3555 independent reflectionsl = 1926
Refinement top
Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.049 w = 1/[σ2(Fo2) + (0.0188P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.091(Δ/σ)max < 0.001
S = 0.98Δρmax = 0.52 e Å3
3555 reflectionsΔρmin = 0.51 e Å3
253 parameters
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. Full-MATRIX

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Co10.71601 (6)0.08481 (10)0.12858 (3)0.0377 (2)
Cl10.57118 (11)0.1043 (2)0.11242 (6)0.0593 (5)
N10.8334 (3)0.0968 (6)0.16527 (18)0.0455 (12)
N20.8308 (4)0.1252 (7)0.0667 (2)0.0517 (13)
N30.6526 (3)0.3100 (5)0.07533 (17)0.0375 (11)
N40.6773 (3)0.2652 (6)0.19271 (18)0.0350 (11)
C10.8229 (5)0.2110 (8)0.2108 (2)0.0510 (16)
H1A0.76270.19920.23250.061*
C20.8989 (6)0.3452 (8)0.2263 (3)0.0653 (19)
H2A0.89180.42090.25880.078*
C30.9854 (6)0.3655 (10)0.1929 (3)0.081 (2)
H3A1.03600.45860.20170.097*
C40.9972 (5)0.2494 (10)0.1468 (3)0.073 (2)
H4A1.05630.26080.12440.087*
C50.9205 (5)0.1155 (8)0.1341 (2)0.0493 (15)
C60.9304 (5)0.0198 (10)0.0853 (3)0.091 (2)
H6A0.98850.10520.09820.109*
H6B0.95230.04510.05100.109*
C70.7783 (5)0.0542 (9)0.0101 (3)0.081 (2)
H7A0.74410.06220.01750.097*
H7B0.83440.03140.01640.097*
C80.6940 (5)0.1783 (9)0.0207 (2)0.076 (2)
H8A0.73170.28150.03640.092*
H8B0.65760.11250.05430.092*
C90.6082 (4)0.2520 (7)0.0152 (2)0.0547 (17)
H9A0.57290.35590.00550.066*
H9B0.55310.15860.01860.066*
C100.8525 (5)0.3238 (9)0.0655 (2)0.0639 (18)
H10A0.88050.35600.02820.077*
H10B0.90750.35570.09770.077*
C110.7473 (4)0.4322 (7)0.0720 (2)0.0498 (15)
H11A0.75730.50630.10780.060*
H11B0.73300.51400.03830.060*
C120.5692 (4)0.3939 (7)0.1087 (2)0.0459 (14)
H12A0.50120.32670.10110.055*
H12B0.55630.51890.09520.055*
C130.6037 (4)0.3938 (8)0.1733 (2)0.0398 (14)
C140.5629 (5)0.5135 (7)0.2127 (3)0.0585 (18)
H14A0.51280.60290.19880.070*
C150.5964 (6)0.5011 (9)0.2726 (3)0.073 (2)
H15A0.56920.58140.29950.087*
C160.6705 (5)0.3684 (9)0.2919 (3)0.0644 (19)
H16A0.69400.35690.33220.077*
C170.7095 (4)0.2535 (8)0.2513 (2)0.0487 (16)
H17A0.76000.16400.26460.058*
Cl20.21085 (14)0.3375 (2)0.10627 (7)0.0605 (5)
O10.3004 (4)0.2932 (9)0.0800 (3)0.175 (3)
O20.1706 (5)0.1890 (9)0.1328 (2)0.188 (3)
O30.1335 (4)0.3822 (8)0.0588 (2)0.154 (2)
O40.2312 (6)0.4729 (10)0.1436 (3)0.232 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0405 (5)0.0358 (5)0.0374 (4)0.0037 (4)0.0072 (3)0.0017 (4)
Cl10.0605 (10)0.0487 (11)0.0693 (10)0.0147 (9)0.0090 (8)0.0008 (8)
N10.049 (3)0.042 (3)0.046 (3)0.003 (3)0.009 (2)0.004 (3)
N20.053 (3)0.051 (4)0.052 (3)0.009 (3)0.014 (3)0.006 (3)
N30.042 (3)0.038 (3)0.032 (3)0.000 (2)0.002 (2)0.006 (2)
N40.033 (3)0.040 (3)0.031 (3)0.001 (2)0.001 (2)0.006 (2)
C10.058 (4)0.051 (4)0.044 (4)0.001 (4)0.005 (3)0.002 (3)
C20.071 (5)0.053 (5)0.066 (5)0.003 (4)0.023 (4)0.012 (3)
C30.060 (5)0.079 (6)0.099 (6)0.024 (4)0.016 (4)0.004 (5)
C40.044 (4)0.086 (6)0.088 (6)0.018 (4)0.010 (4)0.004 (4)
C50.045 (4)0.048 (5)0.056 (4)0.007 (4)0.011 (3)0.007 (3)
C60.069 (5)0.109 (7)0.099 (6)0.038 (5)0.032 (4)0.035 (5)
C70.088 (5)0.083 (6)0.076 (5)0.002 (5)0.032 (4)0.024 (4)
C80.092 (6)0.102 (6)0.034 (4)0.016 (5)0.002 (4)0.022 (4)
C90.067 (5)0.056 (4)0.038 (4)0.000 (3)0.011 (3)0.003 (3)
C100.055 (4)0.073 (5)0.064 (4)0.012 (4)0.009 (3)0.004 (4)
C110.068 (4)0.035 (4)0.046 (4)0.010 (4)0.003 (3)0.013 (3)
C120.051 (4)0.029 (4)0.055 (4)0.005 (3)0.006 (3)0.003 (3)
C130.038 (3)0.037 (4)0.045 (4)0.005 (3)0.009 (3)0.000 (3)
C140.072 (5)0.040 (4)0.069 (5)0.006 (3)0.032 (4)0.002 (3)
C150.108 (6)0.055 (5)0.064 (5)0.004 (4)0.051 (5)0.017 (4)
C160.078 (5)0.073 (6)0.045 (4)0.019 (4)0.017 (4)0.009 (4)
C170.053 (4)0.051 (4)0.041 (4)0.003 (3)0.001 (3)0.004 (3)
Cl20.0609 (12)0.0631 (13)0.0587 (12)0.0005 (10)0.0121 (10)0.0009 (9)
O10.074 (4)0.221 (8)0.238 (6)0.014 (4)0.047 (4)0.083 (5)
O20.189 (6)0.217 (7)0.144 (5)0.105 (5)0.046 (4)0.115 (5)
O30.110 (4)0.197 (7)0.149 (5)0.005 (4)0.015 (4)0.091 (5)
O40.354 (10)0.182 (7)0.162 (6)0.054 (7)0.037 (6)0.131 (6)
Geometric parameters (Å, º) top
Co1—N42.048 (4)C7—H7A0.9700
Co1—N12.070 (4)C7—H7B0.9700
Co1—N22.102 (4)C8—C91.492 (7)
Co1—N32.137 (4)C8—H8A0.9700
Co1—Cl12.253 (2)C8—H8B0.9700
N1—C11.341 (6)C9—H9A0.9700
N1—C51.344 (6)C9—H9B0.9700
N2—C71.468 (7)C10—C111.535 (6)
N2—C61.471 (6)C10—H10A0.9700
N2—C101.475 (6)C10—H10B0.9700
N3—C121.465 (5)C11—H11A0.9700
N3—C91.474 (5)C11—H11B0.9700
N3—C111.474 (5)C12—C131.477 (6)
N4—C171.345 (5)C12—H12A0.9700
N4—C131.347 (6)C12—H12B0.9700
C1—C21.374 (7)C13—C141.376 (6)
C1—H1A0.9300C14—C151.377 (7)
C2—C31.370 (7)C14—H14A0.9300
C2—H2A0.9300C15—C161.370 (7)
C3—C41.360 (7)C15—H15A0.9300
C3—H3A0.9300C16—C171.363 (7)
C4—C51.368 (7)C16—H16A0.9300
C4—H4A0.9300C17—H17A0.9300
C5—C61.493 (7)Cl2—O41.307 (5)
C6—H6A0.9700Cl2—O11.339 (5)
C6—H6B0.9700Cl2—O21.355 (5)
C7—C81.494 (7)Cl2—O31.397 (5)
N4—Co1—N1109.30 (17)C8—C7—H7B108.6
N4—Co1—N2126.72 (18)H7A—C7—H7B107.6
N1—Co1—N282.45 (17)C9—C8—C7117.5 (5)
N4—Co1—N378.79 (16)C9—C8—H8A107.9
N1—Co1—N3156.62 (17)C7—C8—H8A107.9
N2—Co1—N375.50 (17)C9—C8—H8B107.9
N4—Co1—Cl1105.86 (11)C7—C8—H8B107.9
N1—Co1—Cl1100.36 (13)H8A—C8—H8B107.2
N2—Co1—Cl1123.36 (15)N3—C9—C8112.7 (4)
N3—Co1—Cl198.21 (12)N3—C9—H9A109.0
C1—N1—C5118.8 (5)C8—C9—H9A109.0
C1—N1—Co1126.1 (4)N3—C9—H9B109.0
C5—N1—Co1114.5 (4)C8—C9—H9B109.0
C7—N2—C6110.2 (5)H9A—C9—H9B107.8
C7—N2—C10113.3 (5)N2—C10—C11110.5 (5)
C6—N2—C10111.9 (5)N2—C10—H10A109.6
C7—N2—Co1105.3 (3)C11—C10—H10A109.6
C6—N2—Co1109.4 (3)N2—C10—H10B109.6
C10—N2—Co1106.5 (3)C11—C10—H10B109.6
C12—N3—C9112.3 (4)H10A—C10—H10B108.1
C12—N3—C11111.7 (4)N3—C11—C10111.7 (4)
C9—N3—C11110.4 (4)N3—C11—H11A109.3
C12—N3—Co1105.5 (3)C10—C11—H11A109.3
C9—N3—Co1112.2 (3)N3—C11—H11B109.3
C11—N3—Co1104.4 (3)C10—C11—H11B109.3
C17—N4—C13119.1 (4)H11A—C11—H11B107.9
C17—N4—Co1126.1 (4)N3—C12—C13111.1 (4)
C13—N4—Co1114.4 (3)N3—C12—H12A109.4
N1—C1—C2121.5 (5)C13—C12—H12A109.4
N1—C1—H1A119.2N3—C12—H12B109.4
C2—C1—H1A119.2C13—C12—H12B109.4
C3—C2—C1118.8 (6)H12A—C12—H12B108.0
C3—C2—H2A120.6N4—C13—C14120.5 (5)
C1—C2—H2A120.6N4—C13—C12116.0 (5)
C4—C3—C2120.1 (6)C14—C13—C12123.4 (6)
C4—C3—H3A120.0C15—C14—C13120.0 (6)
C2—C3—H3A120.0C15—C14—H14A120.0
C3—C4—C5118.8 (6)C13—C14—H14A120.0
C3—C4—H4A120.6C16—C15—C14118.9 (6)
C5—C4—H4A120.6C16—C15—H15A120.6
N1—C5—C4122.0 (6)C14—C15—H15A120.6
N1—C5—C6116.5 (5)C17—C16—C15119.2 (6)
C4—C5—C6121.5 (6)C17—C16—H16A120.4
N2—C6—C5115.4 (5)C15—C16—H16A120.4
N2—C6—H6A108.4N4—C17—C16122.2 (6)
C5—C6—H6A108.4N4—C17—H17A118.9
N2—C6—H6B108.4C16—C17—H17A118.9
C5—C6—H6B108.4O4—Cl2—O1110.8 (4)
H6A—C6—H6B107.5O4—Cl2—O2112.0 (4)
N2—C7—C8114.5 (5)O1—Cl2—O2110.7 (4)
N2—C7—H7A108.6O4—Cl2—O3112.9 (5)
C8—C7—H7A108.6O1—Cl2—O3104.1 (4)
N2—C7—H7B108.6O2—Cl2—O3106.0 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C12—H12B···Cl1i0.972.783.664 (5)151
C17—H17A···O4ii0.932.493.164 (9)129
Symmetry codes: (i) x, y+1, z; (ii) x+1, y1/2, z+1/2.
 

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