Bis(ethyl­enedi­ammonium) μ-ethyl­enedi­aminetetra­acetato-1κ³O,N,O′:2κ³O′′,N′,O′′′-bis­[tri­oxidomolybdate(VI)] tetra­hydrate

The title compound, (C₂H₁₀N₂)₂[(C₁₀H₁₂N₂O₈)(MoO₃)₂]·4H₂O, which crystallizes in the monoclinic C2/c space group, was obtained by mixing molybdenum oxide, ethyl­enedi­amine and ethyl­enedi­amine­tetra­acetic acid (H₄edta) in a 2:4:1 ratio. The complex anion contains two MoO₃ units bridged by an edta⁴⁻ anion. The midpoint of the central C—C bond of the edta⁴⁻ anion is located on a crystallographic inversion centre. The independent Mo atom is tridentately coordin­ated by a nitro­gen atom and two carboxyl­ate groups of the edta⁴⁻ ligand, together with the three oxo ligands, producing a distorted octa­hedral coordination environment. In the three-dimensional supra­molecular crystal structure, the dinuclear anions, the organo­ammonium counter-ions and the solvent water mol­ecules are linked by N—H...O_w, N—H...O_edta and O—H...O hydrogen bonds.

Computing details

Bis(ethylenediammonium) µ-ethylenediaminetetraacetato-1κ³O,N,O':2κ³O'',N',O'''-bis[trioxidomolybdate(VI)] tetrahydrate

Crystal data

(C2H10N2)2[Mo2(C10H12N2O8)O6]·4H2O	F(000) = 1576
Mr = 772.40	Dx = 1.853 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 22.5897 (14) Å	Cell parameters from 9873 reflections
b = 7.5100 (4) Å	θ = 2.9–27.5°
c = 16.3743 (10) Å	µ = 1.00 mm^−1
β = 94.716 (2)°	T = 150 K
V = 2768.5 (3) Å^3	Block, colourless
Z = 4	0.17 × 0.17 × 0.13 mm

Data collection

Bruker APEXII CCD diffractometer	2946 reflections with I > 2σ(I)
φ and ω scans	Rint = 0.032
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	θmax = 27.5°, θmin = 1.8°
Tmin = 0.691, Tmax = 0.746	h = −29→29
24031 measured reflections	k = −9→9
3192 independent reflections	l = −20→21

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.022	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.060	H-atom parameters constrained
S = 1.06	w = 1/[σ^2(Fo^2) + (0.0247P)^2 + 9.3382P] where P = (Fo^2 + 2Fc^2)/3
3192 reflections	(Δ/σ)max = 0.001
189 parameters	Δρmax = 0.67 e Å^−3
0 restraints	Δρmin = −1.06 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Mo1	0.34131 (2)	0.30046 (2)	0.43898 (2)	0.01140 (6)
O2	0.38304 (7)	0.07064 (19)	0.38526 (10)	0.0184 (3)
O3	0.34930 (6)	0.3750 (2)	0.31149 (9)	0.0153 (3)
O5	0.32695 (7)	0.5278 (2)	0.45742 (9)	0.0167 (3)
O6	0.27328 (7)	0.1984 (2)	0.41260 (10)	0.0192 (3)
O7	0.36649 (7)	0.2195 (2)	0.53376 (10)	0.0199 (3)
O8	0.46292 (8)	−0.0988 (2)	0.38094 (12)	0.0305 (4)
O9	0.40393 (8)	0.4592 (3)	0.21238 (10)	0.0313 (4)
N1	0.44444 (7)	0.3699 (2)	0.42662 (10)	0.0110 (3)
N2	0.68095 (9)	−0.1480 (2)	0.31790 (11)	0.0180 (4)
H2C	0.682765	−0.194661	0.266874	0.022*
H2D	0.644495	−0.169814	0.335592	0.022*
H2E	0.709362	−0.199255	0.352923	0.022*
N3	0.68986 (8)	0.3285 (2)	0.39152 (11)	0.0166 (4)
H3C	0.662370	0.374203	0.353458	0.020*
H3D	0.726961	0.352136	0.376498	0.020*
H3E	0.685339	0.379149	0.441115	0.020*
C1	0.43883 (10)	0.0440 (3)	0.39471 (13)	0.0165 (4)
C2	0.46667 (9)	0.4795 (3)	0.49874 (12)	0.0136 (4)
H2A	0.458550	0.415662	0.549512	0.016*
H2B	0.444417	0.593202	0.497625	0.016*
C3	0.44903 (9)	0.4682 (3)	0.34868 (12)	0.0158 (4)
H3A	0.486764	0.435686	0.325738	0.019*
H3B	0.450105	0.597629	0.360192	0.019*
C4	0.68156 (10)	0.1326 (3)	0.39721 (13)	0.0181 (4)
H4A	0.640934	0.106237	0.412324	0.022*
H4B	0.710243	0.083077	0.440266	0.022*
C5	0.39759 (10)	0.4287 (3)	0.28535 (13)	0.0159 (4)
C6	0.47677 (9)	0.1985 (3)	0.42775 (15)	0.0184 (4)
H6A	0.492092	0.171560	0.484797	0.022*
H6B	0.511335	0.210675	0.394705	0.022*
C7	0.69112 (12)	0.0470 (3)	0.31517 (13)	0.0225 (5)
H7A	0.663501	0.100557	0.271922	0.027*
H7B	0.732207	0.070407	0.301180	0.027*
O1	0.30869 (7)	−0.2039 (2)	0.34909 (9)	0.0180 (3)
H1A	0.317459	−0.290614	0.383210	0.027*
H1B	0.333866	−0.120160	0.364109	0.027*
O10	0.56206 (14)	−0.0882 (7)	0.30040 (19)	0.1003 (14)
H10A	0.533675	−0.115649	0.330976	0.151*
H10B	0.549760	−0.103261	0.249098	0.151*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.01159 (9)	0.01140 (9)	0.01128 (9)	−0.00124 (6)	0.00129 (6)	−0.00028 (6)
O2	0.0146 (7)	0.0131 (7)	0.0272 (8)	−0.0018 (6)	−0.0006 (6)	−0.0051 (6)
O3	0.0139 (7)	0.0207 (7)	0.0113 (7)	−0.0022 (6)	−0.0005 (5)	0.0000 (6)
O5	0.0197 (8)	0.0149 (7)	0.0157 (7)	0.0013 (6)	0.0031 (6)	−0.0022 (6)
O6	0.0142 (7)	0.0206 (8)	0.0229 (8)	−0.0029 (6)	0.0024 (6)	−0.0023 (6)
O7	0.0201 (8)	0.0226 (8)	0.0172 (7)	−0.0033 (6)	0.0021 (6)	0.0059 (6)
O8	0.0238 (9)	0.0153 (8)	0.0507 (12)	0.0053 (7)	−0.0067 (8)	−0.0107 (8)
O9	0.0263 (9)	0.0548 (12)	0.0123 (7)	−0.0165 (8)	−0.0016 (7)	0.0047 (8)
N1	0.0129 (8)	0.0100 (7)	0.0097 (7)	−0.0009 (6)	−0.0016 (6)	−0.0013 (6)
N2	0.0225 (9)	0.0163 (9)	0.0152 (8)	0.0008 (7)	0.0019 (7)	0.0001 (7)
N3	0.0183 (9)	0.0176 (9)	0.0137 (8)	0.0017 (7)	−0.0007 (7)	−0.0025 (7)
C1	0.0174 (10)	0.0132 (9)	0.0185 (10)	0.0003 (8)	−0.0018 (8)	−0.0013 (8)
C2	0.0133 (10)	0.0156 (9)	0.0115 (9)	−0.0025 (7)	−0.0017 (7)	−0.0027 (7)
C3	0.0150 (10)	0.0198 (10)	0.0125 (9)	−0.0062 (8)	0.0001 (7)	0.0020 (8)
C4	0.0234 (11)	0.0170 (10)	0.0138 (9)	0.0003 (8)	0.0019 (8)	−0.0002 (8)
C5	0.0190 (10)	0.0160 (10)	0.0125 (9)	−0.0031 (8)	−0.0002 (8)	0.0000 (8)
C6	0.0130 (10)	0.0141 (10)	0.0273 (11)	0.0015 (8)	−0.0038 (8)	−0.0038 (8)
C7	0.0376 (13)	0.0159 (10)	0.0138 (10)	−0.0012 (9)	0.0013 (9)	−0.0001 (8)
O1	0.0207 (8)	0.0152 (7)	0.0175 (7)	−0.0052 (6)	−0.0025 (6)	0.0023 (6)
O10	0.0533 (18)	0.200 (4)	0.0469 (16)	0.015 (2)	0.0000 (14)	0.007 (2)

Geometric parameters (Å, º)

Mo1—O2	2.1858 (15)	N3—C4	1.487 (3)
Mo1—O3	2.1831 (14)	C1—C6	1.516 (3)
Mo1—O5	1.7686 (15)	C2—C2^i	1.534 (4)
Mo1—O6	1.7397 (15)	C2—H2A	0.9900
Mo1—O7	1.7195 (16)	C2—H2B	0.9900
Mo1—N1	2.4121 (17)	C3—H3A	0.9900
O2—C1	1.273 (3)	C3—H3B	0.9900
O3—C5	1.270 (3)	C3—C5	1.521 (3)
O8—C1	1.232 (3)	C4—H4A	0.9900
O9—C5	1.236 (3)	C4—H4B	0.9900
N1—C2	1.492 (2)	C4—C7	1.521 (3)
N1—C3	1.485 (3)	C6—H6A	0.9900
N1—C6	1.479 (3)	C6—H6B	0.9900
N2—H2C	0.9100	C7—H7A	0.9900
N2—H2D	0.9100	C7—H7B	0.9900
N2—H2E	0.9100	O1—H1A	0.8703
N2—C7	1.484 (3)	O1—H1B	0.8697
N3—H3C	0.9100	O10—H10A	0.8701
N3—H3D	0.9100	O10—H10B	0.8702
N3—H3E	0.9100
O2—Mo1—N1	71.68 (6)	O8—C1—C6	119.11 (19)
O3—Mo1—O2	75.25 (6)	N1—C2—C2^i	113.4 (2)
O3—Mo1—N1	73.02 (5)	N1—C2—H2A	108.9
O5—Mo1—O2	157.26 (6)	N1—C2—H2B	108.9
O5—Mo1—O3	86.93 (6)	C2^i—C2—H2A	108.9
O5—Mo1—N1	89.85 (6)	C2^i—C2—H2B	108.9
O6—Mo1—O2	87.34 (6)	H2A—C2—H2B	107.7
O6—Mo1—O3	90.94 (7)	N1—C3—H3A	109.1
O6—Mo1—O5	107.27 (7)	N1—C3—H3B	109.1
O6—Mo1—N1	156.07 (6)	N1—C3—C5	112.68 (16)
O7—Mo1—O2	87.85 (7)	H3A—C3—H3B	107.8
O7—Mo1—O3	155.03 (7)	C5—C3—H3A	109.1
O7—Mo1—O5	103.83 (7)	C5—C3—H3B	109.1
O7—Mo1—O6	106.75 (7)	N3—C4—H4A	109.8
O7—Mo1—N1	84.38 (7)	N3—C4—H4B	109.8
C1—O2—Mo1	122.03 (13)	N3—C4—C7	109.60 (17)
C5—O3—Mo1	123.00 (13)	H4A—C4—H4B	108.2
C2—N1—Mo1	108.51 (11)	C7—C4—H4A	109.8
C3—N1—Mo1	108.40 (12)	C7—C4—H4B	109.8
C3—N1—C2	111.30 (15)	O3—C5—C3	117.47 (18)
C6—N1—Mo1	106.85 (12)	O9—C5—O3	123.7 (2)
C6—N1—C2	109.66 (16)	O9—C5—C3	118.68 (19)
C6—N1—C3	111.95 (16)	N1—C6—C1	113.43 (17)
H2C—N2—H2D	109.5	N1—C6—H6A	108.9
H2C—N2—H2E	109.5	N1—C6—H6B	108.9
H2D—N2—H2E	109.5	C1—C6—H6A	108.9
C7—N2—H2C	109.5	C1—C6—H6B	108.9
C7—N2—H2D	109.5	H6A—C6—H6B	107.7
C7—N2—H2E	109.5	N2—C7—C4	110.94 (18)
H3C—N3—H3D	109.5	N2—C7—H7A	109.5
H3C—N3—H3E	109.5	N2—C7—H7B	109.5
H3D—N3—H3E	109.5	C4—C7—H7A	109.5
C4—N3—H3C	109.5	C4—C7—H7B	109.5
C4—N3—H3D	109.5	H7A—C7—H7B	108.0
C4—N3—H3E	109.5	H1A—O1—H1B	104.5
O2—C1—C6	116.65 (18)	H10A—O10—H10B	109.4
O8—C1—O2	124.2 (2)
Mo1—O2—C1—O8	164.21 (18)	N1—C3—C5—O3	24.0 (3)
Mo1—O2—C1—C6	−13.7 (3)	N1—C3—C5—O9	−159.7 (2)
Mo1—O3—C5—O9	174.61 (18)	N3—C4—C7—N2	−177.90 (18)
Mo1—O3—C5—C3	−9.3 (3)	C2—N1—C3—C5	−143.96 (17)
Mo1—N1—C2—C2^i	175.59 (18)	C2—N1—C6—C1	145.79 (18)
Mo1—N1—C3—C5	−24.7 (2)	C3—N1—C2—C2^i	−65.2 (3)
Mo1—N1—C6—C1	28.4 (2)	C3—N1—C6—C1	−90.2 (2)
O2—C1—C6—N1	−13.0 (3)	C6—N1—C2—C2^i	59.2 (3)
O8—C1—C6—N1	169.0 (2)	C6—N1—C3—C5	92.9 (2)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2C···O1^ii	0.91	1.93	2.795 (2)	159
N2—H2D···O10	0.91	2.00	2.715 (4)	134
N2—H2D···O7^iii	0.91	2.21	2.786 (2)	121
N2—H2E···O6^iv	0.91	1.84	2.748 (2)	172
N3—H3C···O9^ii	0.91	1.88	2.785 (3)	170
N3—H3D···O1^v	0.91	1.98	2.838 (2)	156
N3—H3E···O5^i	0.91	1.84	2.753 (2)	177
O1—H1A···O5^vi	0.87	1.83	2.694 (2)	173
O1—H1B···O2	0.87	1.83	2.694 (2)	173
O10—H10A···O8	0.87	1.86	2.692 (4)	160
O10—H10B···O8^ii	0.87	2.13	2.978 (4)	166

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