Layered (ethyl­ene­di­amine-[kappa]²N,N')cobalt(II) molybdate(VI)

The structure of poly­[[(ethyl­enedi­amine-[kappa]²N,N')­cobalt(II)]-[mu]-tetra­oxo­molyb­dato(VI)], [Co(C₂H₈N₂)MoO₄]_n or [CoMoO₄(C₂H₈N₂)]_n, is composed of puckered layers constructed from MoO₄ tetrahedra and CoN₂O₄ octahedra, with the ethyl­enedi­amine ligand coordinated to the Co atom in a cis fashion. Each pair of cobalt sites forms a binu­clear edge-sharing unit through a {Co₂O₂} interaction. The binuclear octahedral units are interconnected through the bridging MoO₄ tetrahedra into a layer structure.

Computing details

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1987); cell refinement: TEXSAN (Molecular Structure Corporation, 1987); data reduction: TEXRAY in TEXSAN; program(s) used to solve structure: SHELXS86 (Sheldrick, 1990a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1990b); software used to prepare material for publication: SHELXL97.

Polymeric [ethylenediamine-cobalt(II)] molybdate(VI)

Crystal data

C2H8CoMoN2O4	F(000) = 540
Mr = 278.97	Dx = 2.670 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ybc	Cell parameters from 300 reflections
a = 10.3955 (6) Å	θ = 10–25°
b = 9.7127 (8) Å	µ = 4.15 mm^−1
c = 7.1234 (4) Å	T = 293 K
β = 105.236 (6)°	Plate, violet
V = 693.96 (8) Å^3	0.12 × 0.10 × 0.08 mm
Z = 4

Data collection

Rigaku AFC-5R diffractometer	1461 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.038
Graphite monochromator	θmax = 27.5°, θmin = 2.9°
ω–2θ scans	h = −13→13
Absorption correction: ψ scan (North et al., 1968)	k = −12→0
Tmin = 0.614, Tmax = 0.716	l = 0→9
6370 measured reflections	3 standard reflections every 150 reflections
1590 independent reflections	intensity decay: 0.2%

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)] = 0.023	Hydrogen site location: difference Fourier map
wR(F^2) = 0.054	H-atom parameters not refined
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0304P)^2] where P = (Fo^2 + 2Fc^2)/3
1590 reflections	(Δ/σ)max = 0.002
91 parameters	Δρmax = 0.82 e Å^−3
0 restraints	Δρmin = −0.67 e Å^−3

Special details

Experimental. crystal coated in epoxy glue

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
Mo	0.34406 (2)	0.395709 (19)	0.29607 (3)	0.01601 (8)
Co	0.37886 (3)	0.02788 (3)	0.31572 (4)	0.01677 (10)
O1	0.42317 (19)	0.23468 (17)	0.3482 (3)	0.0234 (4)
O2	0.1778 (2)	0.3679 (2)	0.1793 (3)	0.0316 (4)
O3	0.3554 (2)	0.48648 (19)	0.5138 (2)	0.0280 (4)
O4	0.41481 (18)	0.48974 (17)	0.1294 (2)	0.0192 (4)
N1	0.3273 (2)	−0.1844 (2)	0.3113 (3)	0.0238 (4)
H1A	0.3388	−0.2254	0.2029	0.080*
H1B	0.3796	−0.2283	0.4154	0.080*
N2	0.1685 (2)	0.0530 (2)	0.2656 (3)	0.0236 (4)
H2A	0.1461	0.1232	0.1812	0.050*
H2B	0.1591	0.0827	0.3790	0.050*
C1	0.1865 (3)	−0.1933 (3)	0.3148 (4)	0.0306 (6)
H1C	0.1866	−0.1786	0.4447	0.050*
H1D	0.1499	−0.2762	0.2692	0.050*
C2	0.1064 (3)	−0.0794 (3)	0.1919 (4)	0.0284 (6)
H2C	0.1066	−0.0911	0.0582	0.050*
H2D	0.0158	−0.0817	0.2003	0.050*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo	0.01930 (13)	0.01660 (12)	0.01333 (12)	0.00156 (7)	0.00642 (8)	0.00213 (6)
Co	0.01892 (18)	0.01729 (16)	0.01453 (16)	−0.00028 (13)	0.00513 (13)	−0.00016 (11)
O1	0.0290 (10)	0.0171 (8)	0.0241 (8)	0.0004 (8)	0.0067 (7)	0.0011 (7)
O2	0.0234 (10)	0.0424 (11)	0.0279 (10)	−0.0030 (9)	0.0048 (8)	0.0071 (9)
O3	0.0402 (12)	0.0291 (9)	0.0178 (8)	0.0064 (9)	0.0134 (8)	0.0005 (7)
O4	0.0226 (9)	0.0201 (8)	0.0160 (8)	−0.0023 (7)	0.0071 (7)	0.0004 (6)
N1	0.0294 (12)	0.0212 (9)	0.0210 (10)	−0.0010 (10)	0.0069 (9)	0.0002 (8)
N2	0.0231 (11)	0.0263 (11)	0.0209 (10)	0.0033 (10)	0.0050 (8)	−0.0005 (9)
C1	0.0336 (15)	0.0289 (13)	0.0308 (14)	−0.0062 (13)	0.0114 (12)	0.0039 (11)
C2	0.0213 (13)	0.0342 (13)	0.0284 (13)	−0.0031 (12)	0.0040 (10)	0.0001 (11)

Geometric parameters (Å, º)

Mo—O2	1.731 (2)	N1—H1A	0.90
Mo—O1	1.7607 (17)	N1—H1B	0.90
Mo—O3	1.7606 (17)	N2—C2	1.472 (3)
Mo—O4	1.8007 (16)	N2—H2A	0.90
Co—O1	2.0601 (17)	N2—H2B	0.89
Co—O3^i	2.1048 (17)	C1—C2	1.517 (4)
Co—O4^ii	2.1095 (18)	C1—H1C	0.94
Co—N1	2.129 (2)	C1—H1D	0.91
Co—N2	2.135 (2)	C2—H2C	0.96
Co—O4^iii	2.1735 (16)	C2—H2D	0.96
N1—C1	1.472 (4)
O2—Mo—O1	108.36 (9)	Co^iv—O4—Co^i	95.50 (7)
O2—Mo—O3	109.18 (10)	C1—N1—Co	107.69 (17)
O1—Mo—O3	109.85 (8)	C1—N1—H1A	110.1
O2—Mo—O4	106.94 (8)	Co—N1—H1A	110.4
O1—Mo—O4	109.92 (8)	C1—N1—H1B	110.2
O3—Mo—O4	112.47 (8)	Co—N1—H1B	110.5
O1—Co—O3^i	98.16 (7)	H1A—N1—H1B	107.9
O1—Co—O4^ii	87.94 (7)	C2—N2—Co	107.10 (16)
O3^i—Co—O4^ii	90.96 (7)	C2—N2—H2A	114.3
O1—Co—N1	173.76 (8)	Co—N2—H2A	105.8
O3^i—Co—N1	87.69 (8)	C2—N2—H2B	117.8
O4^ii—Co—N1	94.16 (8)	Co—N2—H2B	103.8
O1—Co—N2	95.54 (8)	H2A—N2—H2B	106.9
O3^i—Co—N2	89.90 (8)	N1—C1—C2	110.2 (2)
O4^ii—Co—N2	176.27 (8)	N1—C1—H1C	105.4
N1—Co—N2	82.25 (9)	C2—C1—H1C	108.5
O1—Co—O4^iii	89.33 (7)	N1—C1—H1D	111.6
O3^i—Co—O4^iii	171.11 (7)	C2—C1—H1D	108.8
O4^ii—Co—O4^iii	84.50 (7)	H1C—C1—H1D	112.2
N1—Co—O4^iii	85.03 (7)	N2—C2—C1	107.9 (2)
N2—Co—O4^iii	94.16 (7)	N2—C2—H2C	110.0
Mo—O1—Co	139.83 (11)	C1—C2—H2C	110.0
Mo—O3—Co^iii	146.09 (10)	N2—C2—H2D	110.1
Mo—O4—Co^iv	122.58 (9)	C1—C2—H2D	110.2
Mo—O4—Co^i	130.40 (9)	H2C—C2—H2D	108.5

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O1^ii	0.90	2.62	3.192 (3)	122
N1—H1B···O1^v	0.90	2.29	3.089 (3)	148
N2—H2A···O2	0.90	2.40	3.127 (3)	138
N2—H2B···O2^iii	0.89	2.15	3.022 (3)	167

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