[1,4-Bis­(pyridyl-2-yl­methyl)-1,4-di­aza­cyclo­heptane]­chloro­cobalt(II) perchlorate

The crystal structure of a Co^II 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 Co^II 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.

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

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Computing details

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

Crystal data

[CoCl(C17H22N4)](ClO4)	F(000) = 980
Mr = 476.22	Dx = 1.570 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 12.286 (4) Å	Cell parameters from 8012 reflections
b = 7.300 (2) Å	θ = 1.7–25.0°
c = 22.573 (7) Å	µ = 1.15 mm^−1
β = 95.731 (6)°	T = 293 K
V = 2014.5 (10) Å^3	Prism, purple
Z = 4	0.30 × 0.25 × 0.20 mm

Data collection

Bruker SMART 1000 diffractometer	1824 reflections with I > 2.0σ(I)
ω scans	Rint = 0.084
Absorption correction: multi-scan [SAINT (Bruker 1998) and SADABS (Sheldrick, 1997)]	θmax = 25.0°
Tmin = 0.725, Tmax = 0.803	h = −13→14
8055 measured reflections	k = −7→8
3555 independent reflections	l = −19→26

Refinement

Refinement on F^2	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.049	w = 1/[σ^2(Fo^2) + (0.0188P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.091	(Δ/σ)max < 0.001
S = 0.98	Δρmax = 0.52 e Å^−3
3555 reflections	Δρmin = −0.51 e Å^−3
253 parameters

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Co1	0.71601 (6)	0.08481 (10)	0.12858 (3)	0.0377 (2)
Cl1	0.57118 (11)	−0.1043 (2)	0.11242 (6)	0.0593 (5)
N1	0.8334 (3)	−0.0968 (6)	0.16527 (18)	0.0455 (12)
N2	0.8308 (4)	0.1252 (7)	0.0667 (2)	0.0517 (13)
N3	0.6526 (3)	0.3100 (5)	0.07533 (17)	0.0375 (11)
N4	0.6773 (3)	0.2652 (6)	0.19271 (18)	0.0350 (11)
C1	0.8229 (5)	−0.2110 (8)	0.2108 (2)	0.0510 (16)
H1A	0.7627	−0.1992	0.2325	0.061*
C2	0.8989 (6)	−0.3452 (8)	0.2263 (3)	0.0653 (19)
H2A	0.8918	−0.4209	0.2588	0.078*
C3	0.9854 (6)	−0.3655 (10)	0.1929 (3)	0.081 (2)
H3A	1.0360	−0.4586	0.2017	0.097*
C4	0.9972 (5)	−0.2494 (10)	0.1468 (3)	0.073 (2)
H4A	1.0563	−0.2608	0.1244	0.087*
C5	0.9205 (5)	−0.1155 (8)	0.1341 (2)	0.0493 (15)
C6	0.9304 (5)	0.0198 (10)	0.0853 (3)	0.091 (2)
H6A	0.9885	0.1052	0.0982	0.109*
H6B	0.9523	−0.0451	0.0510	0.109*
C7	0.7783 (5)	0.0542 (9)	0.0101 (3)	0.081 (2)
H7A	0.7441	−0.0622	0.0175	0.097*
H7B	0.8344	0.0314	−0.0164	0.097*
C8	0.6940 (5)	0.1783 (9)	−0.0207 (2)	0.076 (2)
H8A	0.7317	0.2815	−0.0364	0.092*
H8B	0.6576	0.1125	−0.0543	0.092*
C9	0.6082 (4)	0.2520 (7)	0.0152 (2)	0.0547 (17)
H9A	0.5729	0.3559	−0.0055	0.066*
H9B	0.5531	0.1586	0.0186	0.066*
C10	0.8525 (5)	0.3238 (9)	0.0655 (2)	0.0639 (18)
H10A	0.8805	0.3560	0.0282	0.077*
H10B	0.9075	0.3557	0.0977	0.077*
C11	0.7473 (4)	0.4322 (7)	0.0720 (2)	0.0498 (15)
H11A	0.7573	0.5063	0.1078	0.060*
H11B	0.7330	0.5140	0.0383	0.060*
C12	0.5692 (4)	0.3939 (7)	0.1087 (2)	0.0459 (14)
H12A	0.5012	0.3267	0.1011	0.055*
H12B	0.5563	0.5189	0.0952	0.055*
C13	0.6037 (4)	0.3938 (8)	0.1733 (2)	0.0398 (14)
C14	0.5629 (5)	0.5135 (7)	0.2127 (3)	0.0585 (18)
H14A	0.5128	0.6029	0.1988	0.070*
C15	0.5964 (6)	0.5011 (9)	0.2726 (3)	0.073 (2)
H15A	0.5692	0.5814	0.2995	0.087*
C16	0.6705 (5)	0.3684 (9)	0.2919 (3)	0.0644 (19)
H16A	0.6940	0.3569	0.3322	0.077*
C17	0.7095 (4)	0.2535 (8)	0.2513 (2)	0.0487 (16)
H17A	0.7600	0.1640	0.2646	0.058*
Cl2	0.21085 (14)	0.3375 (2)	0.10627 (7)	0.0605 (5)
O1	0.3004 (4)	0.2932 (9)	0.0800 (3)	0.175 (3)
O2	0.1706 (5)	0.1890 (9)	0.1328 (2)	0.188 (3)
O3	0.1335 (4)	0.3822 (8)	0.0588 (2)	0.154 (2)
O4	0.2312 (6)	0.4729 (10)	0.1436 (3)	0.232 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0405 (5)	0.0358 (5)	0.0374 (4)	0.0037 (4)	0.0072 (3)	0.0017 (4)
Cl1	0.0605 (10)	0.0487 (11)	0.0693 (10)	−0.0147 (9)	0.0090 (8)	0.0008 (8)
N1	0.049 (3)	0.042 (3)	0.046 (3)	0.003 (3)	0.009 (2)	0.004 (3)
N2	0.053 (3)	0.051 (4)	0.052 (3)	0.009 (3)	0.014 (3)	0.006 (3)
N3	0.042 (3)	0.038 (3)	0.032 (3)	0.000 (2)	−0.002 (2)	−0.006 (2)
N4	0.033 (3)	0.040 (3)	0.031 (3)	0.001 (2)	−0.001 (2)	0.006 (2)
C1	0.058 (4)	0.051 (4)	0.044 (4)	0.001 (4)	0.005 (3)	0.002 (3)
C2	0.071 (5)	0.053 (5)	0.066 (5)	0.003 (4)	−0.023 (4)	0.012 (3)
C3	0.060 (5)	0.079 (6)	0.099 (6)	0.024 (4)	−0.016 (4)	0.004 (5)
C4	0.044 (4)	0.086 (6)	0.088 (6)	0.018 (4)	0.010 (4)	−0.004 (4)
C5	0.045 (4)	0.048 (5)	0.056 (4)	0.007 (4)	0.011 (3)	−0.007 (3)
C6	0.069 (5)	0.109 (7)	0.099 (6)	0.038 (5)	0.032 (4)	0.035 (5)
C7	0.088 (5)	0.083 (6)	0.076 (5)	−0.002 (5)	0.032 (4)	−0.024 (4)
C8	0.092 (6)	0.102 (6)	0.034 (4)	−0.016 (5)	0.002 (4)	−0.022 (4)
C9	0.067 (5)	0.056 (4)	0.038 (4)	0.000 (3)	−0.011 (3)	−0.003 (3)
C10	0.055 (4)	0.073 (5)	0.064 (4)	−0.012 (4)	0.009 (3)	−0.004 (4)
C11	0.068 (4)	0.035 (4)	0.046 (4)	−0.010 (4)	0.003 (3)	0.013 (3)
C12	0.051 (4)	0.029 (4)	0.055 (4)	0.005 (3)	−0.006 (3)	0.003 (3)
C13	0.038 (3)	0.037 (4)	0.045 (4)	−0.005 (3)	0.009 (3)	0.000 (3)
C14	0.072 (5)	0.040 (4)	0.069 (5)	0.006 (3)	0.032 (4)	0.002 (3)
C15	0.108 (6)	0.055 (5)	0.064 (5)	−0.004 (4)	0.051 (5)	−0.017 (4)
C16	0.078 (5)	0.073 (6)	0.045 (4)	−0.019 (4)	0.017 (4)	−0.009 (4)
C17	0.053 (4)	0.051 (4)	0.041 (4)	−0.003 (3)	0.001 (3)	0.004 (3)
Cl2	0.0609 (12)	0.0631 (13)	0.0587 (12)	0.0005 (10)	0.0121 (10)	0.0009 (9)
O1	0.074 (4)	0.221 (8)	0.238 (6)	0.014 (4)	0.047 (4)	−0.083 (5)
O2	0.189 (6)	0.217 (7)	0.144 (5)	−0.105 (5)	−0.046 (4)	0.115 (5)
O3	0.110 (4)	0.197 (7)	0.149 (5)	0.005 (4)	−0.015 (4)	0.091 (5)
O4	0.354 (10)	0.182 (7)	0.162 (6)	−0.054 (7)	0.037 (6)	−0.131 (6)

Geometric parameters (Å, º)

Co1—N4	2.048 (4)	C7—H7A	0.9700
Co1—N1	2.070 (4)	C7—H7B	0.9700
Co1—N2	2.102 (4)	C8—C9	1.492 (7)
Co1—N3	2.137 (4)	C8—H8A	0.9700
Co1—Cl1	2.253 (2)	C8—H8B	0.9700
N1—C1	1.341 (6)	C9—H9A	0.9700
N1—C5	1.344 (6)	C9—H9B	0.9700
N2—C7	1.468 (7)	C10—C11	1.535 (6)
N2—C6	1.471 (6)	C10—H10A	0.9700
N2—C10	1.475 (6)	C10—H10B	0.9700
N3—C12	1.465 (5)	C11—H11A	0.9700
N3—C9	1.474 (5)	C11—H11B	0.9700
N3—C11	1.474 (5)	C12—C13	1.477 (6)
N4—C17	1.345 (5)	C12—H12A	0.9700
N4—C13	1.347 (6)	C12—H12B	0.9700
C1—C2	1.374 (7)	C13—C14	1.376 (6)
C1—H1A	0.9300	C14—C15	1.377 (7)
C2—C3	1.370 (7)	C14—H14A	0.9300
C2—H2A	0.9300	C15—C16	1.370 (7)
C3—C4	1.360 (7)	C15—H15A	0.9300
C3—H3A	0.9300	C16—C17	1.363 (7)
C4—C5	1.368 (7)	C16—H16A	0.9300
C4—H4A	0.9300	C17—H17A	0.9300
C5—C6	1.493 (7)	Cl2—O4	1.307 (5)
C6—H6A	0.9700	Cl2—O1	1.339 (5)
C6—H6B	0.9700	Cl2—O2	1.355 (5)
C7—C8	1.494 (7)	Cl2—O3	1.397 (5)
N4—Co1—N1	109.30 (17)	C8—C7—H7B	108.6
N4—Co1—N2	126.72 (18)	H7A—C7—H7B	107.6
N1—Co1—N2	82.45 (17)	C9—C8—C7	117.5 (5)
N4—Co1—N3	78.79 (16)	C9—C8—H8A	107.9
N1—Co1—N3	156.62 (17)	C7—C8—H8A	107.9
N2—Co1—N3	75.50 (17)	C9—C8—H8B	107.9
N4—Co1—Cl1	105.86 (11)	C7—C8—H8B	107.9
N1—Co1—Cl1	100.36 (13)	H8A—C8—H8B	107.2
N2—Co1—Cl1	123.36 (15)	N3—C9—C8	112.7 (4)
N3—Co1—Cl1	98.21 (12)	N3—C9—H9A	109.0
C1—N1—C5	118.8 (5)	C8—C9—H9A	109.0
C1—N1—Co1	126.1 (4)	N3—C9—H9B	109.0
C5—N1—Co1	114.5 (4)	C8—C9—H9B	109.0
C7—N2—C6	110.2 (5)	H9A—C9—H9B	107.8
C7—N2—C10	113.3 (5)	N2—C10—C11	110.5 (5)
C6—N2—C10	111.9 (5)	N2—C10—H10A	109.6
C7—N2—Co1	105.3 (3)	C11—C10—H10A	109.6
C6—N2—Co1	109.4 (3)	N2—C10—H10B	109.6
C10—N2—Co1	106.5 (3)	C11—C10—H10B	109.6
C12—N3—C9	112.3 (4)	H10A—C10—H10B	108.1
C12—N3—C11	111.7 (4)	N3—C11—C10	111.7 (4)
C9—N3—C11	110.4 (4)	N3—C11—H11A	109.3
C12—N3—Co1	105.5 (3)	C10—C11—H11A	109.3
C9—N3—Co1	112.2 (3)	N3—C11—H11B	109.3
C11—N3—Co1	104.4 (3)	C10—C11—H11B	109.3
C17—N4—C13	119.1 (4)	H11A—C11—H11B	107.9
C17—N4—Co1	126.1 (4)	N3—C12—C13	111.1 (4)
C13—N4—Co1	114.4 (3)	N3—C12—H12A	109.4
N1—C1—C2	121.5 (5)	C13—C12—H12A	109.4
N1—C1—H1A	119.2	N3—C12—H12B	109.4
C2—C1—H1A	119.2	C13—C12—H12B	109.4
C3—C2—C1	118.8 (6)	H12A—C12—H12B	108.0
C3—C2—H2A	120.6	N4—C13—C14	120.5 (5)
C1—C2—H2A	120.6	N4—C13—C12	116.0 (5)
C4—C3—C2	120.1 (6)	C14—C13—C12	123.4 (6)
C4—C3—H3A	120.0	C15—C14—C13	120.0 (6)
C2—C3—H3A	120.0	C15—C14—H14A	120.0
C3—C4—C5	118.8 (6)	C13—C14—H14A	120.0
C3—C4—H4A	120.6	C16—C15—C14	118.9 (6)
C5—C4—H4A	120.6	C16—C15—H15A	120.6
N1—C5—C4	122.0 (6)	C14—C15—H15A	120.6
N1—C5—C6	116.5 (5)	C17—C16—C15	119.2 (6)
C4—C5—C6	121.5 (6)	C17—C16—H16A	120.4
N2—C6—C5	115.4 (5)	C15—C16—H16A	120.4
N2—C6—H6A	108.4	N4—C17—C16	122.2 (6)
C5—C6—H6A	108.4	N4—C17—H17A	118.9
N2—C6—H6B	108.4	C16—C17—H17A	118.9
C5—C6—H6B	108.4	O4—Cl2—O1	110.8 (4)
H6A—C6—H6B	107.5	O4—Cl2—O2	112.0 (4)
N2—C7—C8	114.5 (5)	O1—Cl2—O2	110.7 (4)
N2—C7—H7A	108.6	O4—Cl2—O3	112.9 (5)
C8—C7—H7A	108.6	O1—Cl2—O3	104.1 (4)
N2—C7—H7B	108.6	O2—Cl2—O3	106.0 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C12—H12B···Cl1^i	0.97	2.78	3.664 (5)	151
C17—H17A···O4^ii	0.93	2.49	3.164 (9)	129

Symmetry codes: (i) x, y+1, z; (ii) −x+1, y−1/2, −z+1/2.