Redetermination of diaqua­bis(vanillinato-κ²O,O′)cobalt(II)

The structure of the title complex, [Co(C₈H₇O₃)₂(H₂O)₂], has been redetermined in the space group C2/c. The original report [Xiao, Lan, Zhang & Jiang (2002). Guangxi Shifan Daxue Xuebao Ziran Kexueban (J. Guangxi Normal Univ.), 20, 81–83] declared the space group to be Cc. The mol­ecule lies on a twofold axis; the vanillinate anion chelates to the Co^II atom through the meth­oxy and hydr­oxy groups. The Co—O_meth­oxy bond is longer than the Co—O_hydr­oxy bond by 0.2673 (18) Å.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C)= 0.003 Å
• R factor = 0.032
• wR factor = 0.084
• Data-to-parameter ratio = 17.2

checkCIF/PLATON results

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Computing details

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: averaging the coordinates of the published Cc structure (Xiao et al., 2002); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

diaquabis(vanillinato-κ²O,O')cobalt(II)

Crystal data

[Co(C8H7O3)2(H2O)2]	F(000) = 820
Mr = 397.23	Dx = 1.527 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 6807 reflections
a = 22.270 (2) Å	θ = 3.2–26.0°
b = 10.4487 (12) Å	µ = 1.03 mm^−1
c = 7.7771 (9) Å	T = 295 K
β = 107.249 (12)°	Prism, red
V = 1728.3 (3) Å^3	0.40 × 0.38 × 0.30 mm
Z = 4

Data collection

Rigaku R-AXIS RAPID diffractometer	1973 independent reflections
Radiation source: fine-focus sealed tube	1798 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.024
Detector resolution: 10.00 pixels mm^-1	θmax = 27.5°, θmin = 1.9°
ω scans	h = −27→28
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −13→13
Tmin = 0.672, Tmax = 0.738	l = −10→10
7677 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.084	H-atom parameters constrained
S = 1.09	w = 1/[σ^2(Fo^2) + (0.0446P)^2 + 1.1767P] where P = (Fo^2 + 2Fc^2)/3
1973 reflections	(Δ/σ)max < 0.001
115 parameters	Δρmax = 0.29 e Å^−3
0 restraints	Δρmin = −0.24 e Å^−3

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. 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 (Ų)

	x	y	z	Uiso*/Ueq
Co	0.5000	0.15843 (3)	0.2500	0.03372 (12)
O1	0.82098 (6)	0.41801 (17)	0.7983 (2)	0.0611 (4)
O2	0.43973 (6)	0.02273 (13)	0.2910 (2)	0.0496 (3)
H2A	0.4035	0.0479	0.2937	0.074*
H2B	0.4518	−0.0479	0.3541	0.074*
O3	0.57272 (6)	0.30852 (14)	0.24496 (17)	0.0452 (3)
O4	0.54453 (6)	0.19436 (12)	0.50848 (16)	0.0377 (3)
C3	0.61787 (8)	0.31481 (16)	0.4107 (2)	0.0349 (4)
C1	0.71767 (8)	0.36917 (18)	0.6190 (3)	0.0401 (4)
C2	0.67556 (9)	0.37263 (17)	0.4449 (2)	0.0385 (4)
H2	0.6866	0.4140	0.3529	0.046*
C4	0.59947 (8)	0.25106 (16)	0.5472 (2)	0.0343 (4)
C5	0.64209 (9)	0.25060 (19)	0.7208 (2)	0.0417 (4)
H5	0.6311	0.2108	0.8142	0.050*
C6	0.70003 (9)	0.30838 (19)	0.7547 (3)	0.0439 (4)
H6	0.7278	0.3065	0.8707	0.053*
C7	0.78041 (9)	0.4211 (2)	0.6527 (3)	0.0498 (5)
H7	0.7905	0.4593	0.5569	0.060*
C8	0.58407 (14)	0.3723 (3)	0.0982 (3)	0.0782 (9)
H8A	0.5488	0.3606	−0.0071	0.117*
H8B	0.6212	0.3379	0.0769	0.117*
H8C	0.5900	0.4620	0.1248	0.117*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co	0.02859 (18)	0.03306 (19)	0.03686 (19)	0.000	0.00565 (13)	0.000
O1	0.0355 (7)	0.0744 (11)	0.0694 (10)	−0.0115 (7)	0.0094 (7)	−0.0162 (8)
O2	0.0303 (6)	0.0434 (7)	0.0730 (9)	0.0000 (5)	0.0119 (6)	0.0151 (7)
O3	0.0464 (7)	0.0498 (8)	0.0351 (6)	−0.0143 (6)	0.0053 (5)	0.0055 (6)
O4	0.0330 (6)	0.0411 (7)	0.0382 (6)	−0.0069 (5)	0.0093 (5)	0.0029 (5)
C3	0.0368 (9)	0.0315 (8)	0.0348 (8)	−0.0026 (7)	0.0082 (7)	−0.0018 (6)
C1	0.0348 (9)	0.0369 (9)	0.0477 (10)	−0.0048 (7)	0.0110 (7)	−0.0074 (7)
C2	0.0403 (9)	0.0363 (9)	0.0410 (9)	−0.0064 (7)	0.0153 (7)	−0.0018 (7)
C4	0.0337 (8)	0.0305 (8)	0.0387 (8)	−0.0022 (6)	0.0111 (7)	−0.0022 (7)
C5	0.0446 (10)	0.0440 (10)	0.0353 (9)	−0.0085 (8)	0.0099 (7)	0.0006 (7)
C6	0.0392 (10)	0.0467 (10)	0.0401 (9)	−0.0049 (8)	0.0029 (8)	−0.0024 (8)
C7	0.0392 (10)	0.0513 (11)	0.0602 (12)	−0.0086 (9)	0.0170 (9)	−0.0106 (10)
C8	0.0832 (18)	0.101 (2)	0.0418 (12)	−0.0365 (16)	0.0056 (11)	0.0200 (13)

Geometric parameters (Å, º)

Co—O2^i	2.0415 (13)	C3—C4	1.413 (2)
Co—O2	2.0415 (13)	C1—C6	1.384 (3)
Co—O3	2.2631 (13)	C1—C2	1.400 (3)
Co—O3^i	2.2631 (13)	C1—C7	1.448 (3)
Co—O4	1.9958 (12)	C2—H2	0.9300
Co—O4^i	1.9958 (12)	C4—C5	1.401 (2)
O1—C7	1.222 (3)	C5—C6	1.377 (3)
O2—H2A	0.8555	C5—H5	0.9300
O2—H2B	0.8826	C6—H6	0.9300
O3—C3	1.382 (2)	C7—H7	0.9300
O3—C8	1.408 (3)	C8—H8A	0.9600
O4—C4	1.311 (2)	C8—H8B	0.9600
C3—C2	1.372 (2)	C8—H8C	0.9600
O2—Co—O2^i	92.02 (8)	C6—C1—C2	119.26 (17)
O2—Co—O3	172.33 (5)	C6—C1—C7	120.70 (18)
O2—Co—O3^i	88.37 (6)	C2—C1—C7	119.91 (18)
O2^i—Co—O3	88.37 (6)	C3—C2—C1	119.74 (17)
O2—Co—O4	97.28 (5)	C3—C2—H2	120.1
O3—Co—O3^i	92.27 (8)	C1—C2—H2	120.1
O3—Co—O4	75.09 (5)	O4—C4—C5	122.62 (16)
O4—Co—O4^i	158.32 (8)	O4—C4—C3	119.93 (15)
O4—Co—O2^i	97.74 (6)	C5—C4—C3	117.45 (16)
O4^i—Co—O2^i	97.28 (5)	C6—C5—C4	120.74 (17)
O4^i—Co—O2	97.74 (6)	C6—C5—H5	119.6
O4^i—Co—O3	89.81 (5)	C4—C5—H5	119.6
O4—Co—O3^i	89.81 (5)	C5—C6—C1	121.12 (17)
O4^i—Co—O3^i	75.09 (5)	C5—C6—H6	119.4
O2^i—Co—O3^i	172.33 (5)	C1—C6—H6	119.4
Co—O2—H2A	117.3	O1—C7—C1	124.5 (2)
Co—O2—H2B	124.2	O1—C7—H7	117.7
H2A—O2—H2B	112.1	C1—C7—H7	117.7
C3—O3—C8	118.55 (16)	O3—C8—H8A	109.5
C3—O3—Co	110.08 (10)	O3—C8—H8B	109.5
C8—O3—Co	130.07 (13)	H8A—C8—H8B	109.5
C4—O4—Co	117.87 (11)	O3—C8—H8C	109.5
C2—C3—O3	125.61 (16)	H8A—C8—H8C	109.5
C2—C3—C4	121.69 (16)	H8B—C8—H8C	109.5
O3—C3—C4	112.68 (15)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2A···O1^ii	0.85	1.88	2.733 (2)	173
O2—H2B···O4^iii	0.88	1.85	2.7158 (19)	165

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