Aqua-chlorido{6,6'-dimeth-oxy-2,2'-[ethane-1,2-diylbis(nitrilo-dimethyl-idyne)]diphenolato-κO,N,N',O}cobalt(III) monohydrate.

The title compound, [Co(C(18)H(18)N(2)O(4))Cl(H(2)O)]·H(2)O, contains a distorted octa-hedral cobalt(III) complex with a 6,6'-dimeth-oxy-2,2'-[ethane-1,2-diylbis(nitrilo-dimethyl-idyne)]diphenolate ligand, a chloride and an aqua ligand, and also a disordered water solvent mol-ecule (half-occupancy). The Co(III) ion is coordinated in an N(2)O(3)Cl manner. Weak O-H⋯O hydrogen bonds may help to stabilize the crystal packing.

Related literature

For related literature, see: Aurangzeb et al. (1994 ▶); Hulme et al. (1997 ▶); Li et al. (2008 ▶); Fei & Fang (2008 ▶); Wang et al. (1979 ▶); Xia et al. (2007 ▶); Zhang & Janiak (2001 ▶).

Experimental

Crystal data

[Co(C18H18N2O4)Cl(H2O)]·H2O

M = 456.76

Trigonal,

a = 26.490 (2) Å

c = 15.6234 (17) Å

V = 9494.5 (14) Å3

Z = 18

Mo Kα radiation

μ = 0.98 mm−1

T = 293 K

0.15 × 0.13 × 0.09 mm

Data collection

Bruker APEXII CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ▶) T min = 0.868, T max = 0.917

13737 measured reflections

4116 independent reflections

2834 reflections with I > 2σ(I)

R int = 0.062

Refinement

R[F 2 > 2σ(F 2)] = 0.074

wR(F 2) = 0.259

S = 1.03

4116 reflections

274 parameters

H-atom parameters constrained

Δρmax = 1.55 e Å−3

Δρmin = −1.03 e Å−3

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP (Sheldrick, 1998 ▶); software used to prepare material for publication: XP.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809011167/hg2491sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809011167/hg2491Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Co(C18H18N2O4)Cl(H2O)]·H2O	Dx = 1.438 Mg m−3Dm = 1.438 Mg m−3Dm measured by not measured
Mr = 456.76	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3	Cell parameters from 5356 reflections
Hall symbol: -R 3	θ = 2.7–26.9°
a = 26.490 (2) Å	µ = 0.98 mm−1
c = 15.6234 (17) Å	T = 293 K
V = 9494.5 (14) Å3	Block, orange
Z = 18	0.15 × 0.13 × 0.09 mm
F(000) = 4248

Bruker APEXII CCD area-detector diffractometer	4116 independent reflections
Radiation source: fine-focus sealed tube	2834 reflections with I > 2σ(I)
graphite	Rint = 0.062
φ and ω scans	θmax = 26.2°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −28→32
Tmin = 0.868, Tmax = 0.917	k = −32→25
13737 measured reflections	l = −19→12

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.074	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.259	H-atom parameters constrained
S = 1.03	w = 1/[σ2(Fo2) + (0.1835P)2] where P = (Fo2 + 2Fc2)/3
4116 reflections	(Δ/σ)max = 0.001
274 parameters	Δρmax = 1.55 e Å−3
0 restraints	Δρmin = −1.03 e Å−3

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Co1	0.73792 (3)	0.12280 (3)	0.59262 (4)	0.0357 (3)
Cl1	0.62851 (7)	0.08016 (8)	0.61355 (10)	0.0637 (5)
O1	0.5945 (14)	0.144 (3)	0.478 (3)	0.057 (16)	0.15 (3)
H1C	0.6127	0.1636	0.4355	0.068*	0.15 (3)
H1D	0.6144	0.1305	0.5014	0.068*	0.15 (3)
O8	0.5817 (6)	0.1059 (11)	0.4435 (11)	0.058 (7)	0.35 (3)
H8E	0.5971	0.1406	0.4241	0.069*	0.35 (3)
H8D	0.5990	0.1068	0.4887	0.069*	0.35 (3)
O2	0.7381 (4)	0.2826 (4)	0.3172 (5)	0.055 (2)	0.50
H2C	0.7532	0.2773	0.2735	0.066*	0.25
H2D	0.7539	0.3193	0.3258	0.066*	0.50
H2B	0.7012	0.2675	0.3109	0.066*	0.25
O3	0.74870 (15)	0.07928 (14)	0.6768 (2)	0.0349 (8)
O4	0.76146 (16)	0.18833 (15)	0.6619 (2)	0.0404 (8)
O5	0.77398 (18)	0.04171 (17)	0.8092 (2)	0.0481 (9)
O6	0.78604 (19)	0.25833 (17)	0.7866 (3)	0.0552 (10)
O7	0.83443 (14)	0.15912 (15)	0.5522 (2)	0.0401 (8)
H7C	0.8552	0.1539	0.5881	0.048*
H7D	0.8499	0.1958	0.5434	0.048*
N1	0.71890 (18)	0.06087 (19)	0.5088 (2)	0.0376 (9)
N2	0.73614 (19)	0.1675 (2)	0.4961 (3)	0.0422 (10)
C1	0.7312 (2)	−0.0054 (2)	0.5961 (3)	0.0417 (12)
C2	0.7457 (2)	0.0273 (2)	0.6710 (3)	0.0352 (10)
C3	0.7579 (3)	0.0050 (2)	0.7421 (3)	0.0429 (12)
C4	0.7545 (3)	−0.0489 (3)	0.7403 (4)	0.0608 (17)
H4	0.7633	−0.0628	0.7894	0.073*
C5	0.7387 (4)	−0.0815 (3)	0.6683 (5)	0.074 (2)
H5	0.7354	−0.1181	0.6685	0.088*
C6	0.7280 (3)	−0.0612 (3)	0.5979 (5)	0.0592 (16)
H6	0.7182	−0.0835	0.5482	0.071*
C7	0.7192 (2)	0.0129 (2)	0.5214 (3)	0.0399 (11)
H7	0.7102	−0.0118	0.4745	0.048*
C8	0.7796 (3)	0.0185 (4)	0.8876 (4)	0.070 (2)
H8A	0.7445	−0.0177	0.8988	0.104*
H8B	0.7861	0.0456	0.9329	0.104*
H8C	0.8120	0.0118	0.8844	0.104*
C9	0.7448 (2)	0.2507 (3)	0.5713 (4)	0.0462 (12)
C10	0.7583 (2)	0.2354 (2)	0.6479 (3)	0.0406 (12)
C11	0.7708 (3)	0.2746 (2)	0.7164 (4)	0.0473 (13)
C12	0.7685 (3)	0.3254 (3)	0.7061 (5)	0.0666 (18)
H12	0.7766	0.3503	0.7525	0.080*
C13	0.7547 (4)	0.3394 (3)	0.6299 (6)	0.079 (2)
H13	0.7527	0.3733	0.6243	0.095*
C14	0.7439 (3)	0.3038 (3)	0.5620 (5)	0.0635 (17)
H14	0.7358	0.3140	0.5089	0.076*
C15	0.8063 (3)	0.2980 (3)	0.8565 (4)	0.0628 (18)
H15A	0.8427	0.3318	0.8415	0.094*
H15B	0.8117	0.2795	0.9056	0.094*
H15C	0.7781	0.3096	0.8695	0.094*
C16	0.7376 (3)	0.2170 (3)	0.4987 (4)	0.0477 (13)
H16	0.7334	0.2317	0.4468	0.057*
C17	0.7351 (3)	0.1387 (3)	0.4155 (3)	0.0537 (15)
H17A	0.7745	0.1508	0.3975	0.064*
H17B	0.7166	0.1496	0.3712	0.064*
C18	0.7020 (3)	0.0749 (3)	0.4289 (3)	0.0537 (14)
H18A	0.6606	0.0613	0.4294	0.064*
H18B	0.7099	0.0555	0.3824	0.064*

	U11	U22	U33	U12	U13	U23
Co1	0.0441 (5)	0.0379 (4)	0.0280 (4)	0.0226 (3)	−0.0021 (3)	−0.0013 (2)
Cl1	0.0478 (9)	0.0909 (12)	0.0596 (10)	0.0402 (9)	0.0133 (7)	0.0135 (8)
O1	0.053 (18)	0.08 (3)	0.05 (2)	0.04 (2)	0.001 (14)	0.02 (2)
O8	0.054 (8)	0.079 (15)	0.050 (9)	0.041 (9)	0.001 (6)	0.023 (9)
O2	0.059 (5)	0.064 (5)	0.038 (4)	0.028 (4)	−0.016 (3)	−0.006 (4)
O3	0.048 (2)	0.0316 (17)	0.0316 (16)	0.0247 (16)	−0.0040 (14)	−0.0019 (13)
O4	0.055 (2)	0.0358 (19)	0.0366 (18)	0.0271 (17)	−0.0075 (15)	−0.0045 (14)
O5	0.067 (3)	0.050 (2)	0.0366 (19)	0.036 (2)	−0.0030 (17)	0.0073 (16)
O6	0.070 (3)	0.041 (2)	0.052 (2)	0.025 (2)	−0.0006 (19)	−0.0114 (17)
O7	0.039 (2)	0.0397 (19)	0.0370 (19)	0.0165 (16)	−0.0023 (14)	0.0003 (14)
N1	0.035 (2)	0.044 (2)	0.031 (2)	0.0166 (19)	−0.0035 (16)	−0.0091 (17)
N2	0.043 (2)	0.052 (3)	0.033 (2)	0.025 (2)	−0.0031 (18)	0.0039 (18)
C1	0.040 (3)	0.033 (3)	0.051 (3)	0.018 (2)	−0.001 (2)	−0.009 (2)
C2	0.032 (2)	0.033 (2)	0.043 (3)	0.018 (2)	0.0029 (19)	0.0007 (19)
C3	0.052 (3)	0.040 (3)	0.041 (3)	0.027 (3)	0.004 (2)	0.008 (2)
C4	0.083 (5)	0.048 (4)	0.063 (4)	0.041 (4)	−0.004 (3)	0.008 (3)
C5	0.100 (6)	0.042 (4)	0.091 (6)	0.044 (4)	−0.014 (4)	−0.005 (3)
C6	0.072 (4)	0.038 (3)	0.070 (4)	0.029 (3)	−0.002 (3)	−0.013 (3)
C7	0.035 (3)	0.037 (3)	0.041 (3)	0.014 (2)	−0.004 (2)	−0.015 (2)
C8	0.096 (5)	0.088 (5)	0.038 (3)	0.056 (5)	0.000 (3)	0.018 (3)
C9	0.044 (3)	0.047 (3)	0.055 (3)	0.028 (3)	−0.001 (2)	0.007 (2)
C10	0.040 (3)	0.035 (3)	0.052 (3)	0.021 (2)	0.004 (2)	0.002 (2)
C11	0.047 (3)	0.038 (3)	0.057 (3)	0.021 (3)	0.002 (2)	−0.005 (2)
C12	0.082 (5)	0.046 (4)	0.080 (5)	0.039 (4)	−0.002 (4)	−0.011 (3)
C13	0.093 (6)	0.051 (4)	0.108 (6)	0.047 (4)	−0.005 (5)	0.003 (4)
C14	0.068 (4)	0.055 (4)	0.079 (4)	0.040 (3)	−0.003 (3)	0.008 (3)
C15	0.060 (4)	0.053 (4)	0.056 (4)	0.014 (3)	0.002 (3)	−0.023 (3)
C16	0.047 (3)	0.053 (3)	0.046 (3)	0.026 (3)	−0.005 (2)	0.013 (2)
C17	0.064 (4)	0.063 (4)	0.029 (3)	0.028 (3)	−0.005 (2)	−0.001 (2)
C18	0.062 (4)	0.066 (4)	0.033 (3)	0.032 (3)	−0.008 (2)	−0.009 (3)

Co1—O3	1.863 (3)	C2—C3	1.370 (7)
Co1—O4	1.868 (3)	C3—C4	1.385 (8)
Co1—N2	1.932 (4)	C4—C5	1.350 (9)
Co1—N1	1.957 (4)	C4—H4	0.9300
Co1—O7	2.324 (3)	C5—C6	1.315 (10)
Co1—Cl1	2.5513 (17)	C5—H5	0.9300
O1—H1C	0.8381	C6—H6	0.9300
O1—H1D	0.8514	C7—H7	0.9300
O1—H8E	0.8596	C8—H8A	0.9600
O1—H8D	1.0649	C8—H8B	0.9600
O8—H1D	1.1965	C8—H8C	0.9600
O8—H8E	0.8530	C9—C10	1.367 (8)
O8—H8D	0.8360	C9—C16	1.396 (8)
O2—H2C	0.8374	C9—C14	1.426 (8)
O2—H2D	0.8561	C10—C11	1.411 (8)
O2—H2B	0.8563	C11—C12	1.385 (9)
O3—C2	1.342 (6)	C12—C13	1.350 (11)
O4—C10	1.309 (6)	C12—H12	0.9300
O5—C3	1.347 (7)	C13—C14	1.352 (10)
O5—C8	1.412 (7)	C13—H13	0.9300
O6—C11	1.314 (7)	C14—H14	0.9300
O6—C15	1.422 (7)	C15—H15A	0.9600
O7—H7C	0.8439	C15—H15B	0.9600
O7—H7D	0.8561	C15—H15C	0.9600
N1—C7	1.290 (7)	C16—H16	0.9300
N1—C18	1.436 (7)	C17—C18	1.480 (9)
N2—C16	1.294 (8)	C17—H17A	0.9700
N2—C17	1.465 (7)	C17—H17B	0.9700
C1—C7	1.362 (7)	C18—H18A	0.9700
C1—C2	1.391 (7)	C18—H18B	0.9700
C1—C6	1.438 (8)
O3—Co1—O4	94.76 (14)	C6—C5—C4	119.7 (6)
O3—Co1—N2	171.32 (17)	C6—C5—H5	120.1
O4—Co1—N2	88.92 (18)	C4—C5—H5	120.1
O3—Co1—N1	90.48 (16)	C5—C6—C1	121.5 (6)
O4—Co1—N1	172.92 (17)	C5—C6—H6	119.3
N2—Co1—N1	85.24 (18)	C1—C6—H6	119.3
O3—Co1—O7	88.31 (14)	N1—C7—C1	126.8 (5)
O4—Co1—O7	89.17 (15)	N1—C7—H7	116.6
N2—Co1—O7	83.87 (16)	C1—C7—H7	116.6
N1—Co1—O7	86.23 (15)	O5—C8—H8A	109.5
O3—Co1—Cl1	97.31 (12)	O5—C8—H8B	109.5
O4—Co1—Cl1	96.58 (13)	H8A—C8—H8B	109.5
N2—Co1—Cl1	90.05 (14)	O5—C8—H8C	109.5
N1—Co1—Cl1	87.44 (13)	H8A—C8—H8C	109.5
O7—Co1—Cl1	171.56 (10)	H8B—C8—H8C	109.5
H1C—O1—H1D	108.1	C10—C9—C16	119.6 (5)
H1C—O1—H8E	39.0	C10—C9—C14	121.2 (6)
H1D—O1—H8E	105.8	C16—C9—C14	118.9 (5)
H1C—O1—H8D	113.4	O4—C10—C9	125.4 (5)
H1D—O1—H8D	33.5	O4—C10—C11	118.2 (5)
H8E—O1—H8D	89.9	C9—C10—C11	116.4 (5)
H1C—O8—H1D	65.3	O6—C11—C12	125.9 (6)
H1C—O8—H8E	16.5	O6—C11—C10	112.8 (5)
H1D—O8—H8E	81.6	C12—C11—C10	121.2 (6)
H1C—O8—H8D	91.9	C13—C12—C11	121.3 (6)
H1D—O8—H8D	26.9	C13—C12—H12	119.4
H8E—O8—H8D	108.1	C11—C12—H12	119.4
H2C—O2—H2D	108.4	C12—C13—C14	119.5 (6)
H2C—O2—H2B	111.0	C12—C13—H13	120.2
H2D—O2—H2B	110.1	C14—C13—H13	120.2
C2—O3—Co1	129.7 (3)	C13—C14—C9	120.3 (7)
C10—O4—Co1	129.6 (3)	C13—C14—H14	119.8
C3—O5—C8	115.2 (5)	C9—C14—H14	119.8
C11—O6—C15	117.5 (5)	O6—C15—H15A	109.5
Co1—O7—H7C	115.1	O6—C15—H15B	109.5
Co1—O7—H7D	108.4	H15A—C15—H15B	109.5
H7C—O7—H7D	108.2	O6—C15—H15C	109.5
C7—N1—C18	122.9 (4)	H15A—C15—H15C	109.5
C7—N1—Co1	126.7 (3)	H15B—C15—H15C	109.5
C18—N1—Co1	110.4 (4)	N2—C16—C9	126.8 (5)
C16—N2—C17	122.5 (5)	N2—C16—H16	116.6
C16—N2—Co1	126.9 (4)	C9—C16—H16	116.6
C17—N2—Co1	110.6 (4)	N2—C17—C18	108.7 (5)
C7—C1—C2	122.6 (5)	N2—C17—H17A	110.0
C7—C1—C6	118.7 (5)	C18—C17—H17A	110.0
C2—C1—C6	118.7 (5)	N2—C17—H17B	110.0
O3—C2—C3	118.8 (4)	C18—C17—H17B	110.0
O3—C2—C1	123.6 (5)	H17A—C17—H17B	108.3
C3—C2—C1	117.6 (5)	N1—C18—C17	109.6 (5)
O5—C3—C2	112.2 (4)	N1—C18—H18A	109.7
O5—C3—C4	126.4 (5)	C17—C18—H18A	109.7
C2—C3—C4	121.4 (5)	N1—C18—H18B	109.7
C5—C4—C3	121.0 (6)	C17—C18—H18B	109.7
C5—C4—H4	119.5	H18A—C18—H18B	108.2
C3—C4—H4	119.5

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7D···O3i	0.86	2.44	2.883 (5)	113
O7—H7D···O5i	0.86	2.22	3.078 (5)	178
O7—H7C···O6i	0.84	2.58	3.033 (6)	115
O7—H7C···O4i	0.84	1.95	2.798 (5)	178
O2—H2D···O2ii	0.86	2.01	2.861 (9)	178
O2—H2C···O8ii	0.84	2.13	2.868 (19)	147
O2—H2C···O1ii	0.84	1.72	2.56 (3)	175
O8—H8E···O2iii	0.85	2.04	2.868 (19)	163
O8—H8D···Cl1	0.84	2.34	3.147 (12)	163
O1—H1D···Cl1	0.85	2.34	3.11 (3)	150

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7D⋯O3i	0.86	2.44	2.883 (5)	113
O7—H7D⋯O5i	0.86	2.22	3.078 (5)	178
O7—H7C⋯O6i	0.84	2.58	3.033 (6)	115
O7—H7C⋯O4i	0.84	1.95	2.798 (5)	178
O2—H2D⋯O2ii	0.86	2.01	2.861 (9)	178
O2—H2C⋯O8ii	0.84	2.13	2.868 (19)	147
O2—H2C⋯O1ii	0.84	1.72	2.56 (3)	175
O8—H8E⋯O2iii	0.85	2.04	2.868 (19)	163
O8—H8D⋯Cl1	0.84	2.34	3.147 (12)	163
O1—H1D⋯Cl1	0.85	2.34	3.11 (3)	150

Symmetry codes: (i) ; (ii) ; (iii) .