Aqua­bis(1,2-ethanediamine-κ²N,N′)hydroxidocobalt(III) naphthalene-1,5-disulfonate monohydrate

The Co^III atom in the title compound, [Co(C₂H₈N₂)₂(OH)(H₂O)](C₁₀H₆O₆S₂)·H₂O, exhibits an octa­hedral coordination geometry, with the hydroxide and water ligands occupying cis sites. Adjacent cations are linked into linear chains through hydrogen-bonded OH...OH₂ units. The Co^III atom lies on a twofold rotation axis and the naphthalene-1,5-disulfonate dianion lies on a centre of inversion.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.005 Å
• Disorder in main residue
• R factor = 0.040
• wR factor = 0.105
• Data-to-parameter ratio = 15.5

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT395_ALERT_2_B Deviating  X-O-Y  Angle from 120 Deg for   <O1W'     162.00 Deg.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.98
PLAT301_ALERT_3_C Main Residue  Disorder .........................       4.00 Perc.
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........        O1W
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          1
            O1  -CO1 -N1  -C1      9.10  1.70   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          8
            N2  -CO1 -N2  -C2    115.71  0.19   2.655   1.555   1.555   1.555
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          5

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   4 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: SHELXL97 and publCIF (Westrip, 2007).

Aquabis(1,2-ethanediamine-κ²N,N')hydroxidocobalt(III) naphthalene-1,5-disulfonate monohydrate

Crystal data

[Co(C2H8N2)2(OH)(H2O)](C10H6O6S2)·H2O	F(000) = 1080
Mr = 518.45	Dx = 1.607 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 2369 reflections
a = 21.017 (2) Å	θ = 3.0–26.9°
b = 11.0917 (8) Å	µ = 1.05 mm^−1
c = 9.2140 (7) Å	T = 293 K
β = 94.002 (1)°	Block, orange
V = 2142.7 (3) Å^3	0.41 × 0.33 × 0.28 mm
Z = 4

Data collection

Bruker SMART CCD area-detector diffractometer	2336 independent reflections
Radiation source: fine-focus sealed tube	1714 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.047
φ and ω scans	θmax = 27.0°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −26→26
Tmin = 0.673, Tmax = 0.758	k = −14→14
8917 measured reflections	l = −11→11

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)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.105	H-atom parameters constrained
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0493P)^2 + 2.9275P] where P = (Fo^2 + 2Fc^2)/3
2336 reflections	(Δ/σ)max = 0.001
151 parameters	Δρmax = 0.46 e Å^−3
15 restraints	Δρmin = −0.36 e Å^−3

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
Co1	0.5000	0.37103 (5)	0.2500	0.02094 (17)
S1	0.38767 (4)	0.25322 (7)	−0.27412 (9)	0.0290 (2)
O1	0.52879 (10)	0.48891 (18)	0.3903 (2)	0.0267 (5)
H1	0.4996	0.5004	0.4476	0.040*	0.75
H11	0.5374	0.5553	0.3500	0.040*	0.75
O2	0.40458 (11)	0.3452 (2)	−0.1658 (3)	0.0413 (6)
O3	0.42854 (10)	0.2566 (2)	−0.3945 (3)	0.0398 (6)
O4	0.38309 (11)	0.1339 (2)	−0.2130 (3)	0.0389 (6)
O1w	0.5003 (11)	0.0029 (6)	0.2811 (13)	0.046 (5)	0.297 (7)
O1w'	0.4866 (8)	0.0018 (13)	0.4204 (19)	0.072 (6)	0.203 (7)
H1w	0.4768	−0.0176	0.3370	0.109*
N1	0.46598 (12)	0.2485 (2)	0.1142 (3)	0.0273 (6)
H1n1	0.4635	0.2767	0.0283	0.033*
H1n2	0.4908	0.1879	0.1167	0.033*
N2	0.41488 (11)	0.3747 (2)	0.3204 (3)	0.0265 (6)
H2n1	0.4144	0.3351	0.3993	0.032*
H2n2	0.4042	0.4471	0.3370	0.032*
C1	0.40192 (15)	0.2108 (3)	0.1540 (4)	0.0337 (8)
H1A	0.4055	0.1494	0.2290	0.040*
H1B	0.3775	0.1782	0.0698	0.040*
C2	0.36968 (15)	0.3209 (3)	0.2088 (3)	0.0318 (7)
H2A	0.3601	0.3775	0.1300	0.038*
H2B	0.3302	0.2991	0.2507	0.038*
C3	0.30995 (14)	0.2943 (3)	−0.3500 (3)	0.0279 (7)
C4	0.28212 (15)	0.3937 (3)	−0.2970 (4)	0.0361 (8)
H4	0.3020	0.4340	−0.2177	0.043*
C5	0.22401 (16)	0.4365 (3)	−0.3598 (4)	0.0404 (9)
H5	0.2057	0.5052	−0.3226	0.048*
C6	0.19402 (15)	0.3779 (3)	−0.4753 (4)	0.0332 (7)
H6	0.1558	0.4081	−0.5176	0.040*
C7	0.22017 (14)	0.2721 (3)	−0.5312 (3)	0.0252 (6)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0228 (3)	0.0232 (3)	0.0168 (3)	0.000	0.0010 (2)	0.000
S1	0.0253 (4)	0.0324 (5)	0.0283 (4)	−0.0062 (3)	−0.0051 (3)	0.0074 (3)
O1	0.0326 (12)	0.0272 (11)	0.0210 (11)	−0.0017 (9)	0.0073 (9)	−0.0045 (9)
O2	0.0425 (14)	0.0395 (14)	0.0390 (14)	−0.0075 (11)	−0.0183 (11)	0.0012 (11)
O3	0.0262 (12)	0.0555 (16)	0.0376 (13)	−0.0017 (11)	0.0013 (10)	0.0146 (11)
O4	0.0380 (13)	0.0352 (13)	0.0424 (14)	−0.0065 (11)	−0.0059 (11)	0.0149 (11)
O1W	0.042 (4)	0.028 (4)	0.066 (11)	−0.004 (5)	−0.003 (8)	−0.005 (4)
O1W'	0.078 (8)	0.049 (7)	0.087 (10)	−0.036 (6)	−0.023 (7)	0.006 (7)
N1	0.0329 (14)	0.0282 (14)	0.0204 (13)	0.0008 (11)	−0.0007 (11)	−0.0031 (11)
N2	0.0273 (13)	0.0304 (14)	0.0220 (13)	0.0019 (11)	0.0028 (10)	0.0034 (11)
C1	0.0342 (18)	0.0325 (18)	0.0335 (18)	−0.0107 (14)	−0.0032 (14)	0.0002 (14)
C2	0.0266 (16)	0.0384 (19)	0.0300 (17)	−0.0039 (14)	−0.0006 (13)	0.0019 (14)
C3	0.0214 (15)	0.0332 (17)	0.0286 (16)	−0.0031 (13)	−0.0001 (12)	0.0013 (13)
C4	0.0315 (17)	0.039 (2)	0.0370 (19)	−0.0044 (15)	−0.0031 (14)	−0.0126 (15)
C5	0.0352 (19)	0.0330 (19)	0.053 (2)	0.0065 (15)	0.0004 (16)	−0.0139 (17)
C6	0.0237 (16)	0.0360 (19)	0.0395 (19)	0.0032 (14)	−0.0012 (13)	−0.0027 (15)
C7	0.0221 (15)	0.0262 (16)	0.0273 (16)	−0.0022 (12)	0.0027 (12)	−0.0001 (12)

Geometric parameters (Å, º)

Co1—O1	1.908 (2)	N2—H2N1	0.850
Co1—O1^i	1.908 (2)	N2—H2N2	0.850
Co1—N1	1.949 (2)	C1—C2	1.501 (4)
Co1—N1^i	1.949 (2)	C1—H1A	0.970
Co1—N2	1.946 (2)	C1—H1B	0.970
Co1—N2^i	1.946 (2)	C2—H2A	0.970
S1—O4	1.444 (2)	C2—H2B	0.970
S1—O3	1.450 (2)	C3—C4	1.355 (4)
S1—O2	1.454 (2)	C3—C7^ii	1.430 (4)
S1—C3	1.790 (3)	C4—C5	1.397 (5)
O1—H1	0.85	C4—H4	0.930
O1—H11	0.85	C5—C6	1.363 (4)
O1W—H1W	0.77	C5—H5	0.930
O1W'—H1W	0.81	C6—C7	1.408 (4)
N1—C1	1.480 (4)	C6—H6	0.930
N1—H1N1	0.850	C7—C7^ii	1.429 (6)
N1—H1N2	0.850	C7—C3^ii	1.430 (4)
N2—C2	1.477 (4)
O1—Co1—O1^i	93.5 (1)	H2N1—N2—H2N2	108.3
O1—Co1—N1	176.3 (1)	N1—C1—C2	107.0 (2)
O1^i—Co1—N1	87.6 (1)	N1—C1—H1A	110.3
O1—Co1—N2	90.9 (1)	C2—C1—H1A	110.3
O1^i—Co1—N2	87.5 (1)	N1—C1—H1B	110.3
N1—Co1—N1^i	91.6 (2)	C2—C1—H1B	110.3
N1—Co1—N2	85.6 (1)	H1A—C1—H1B	108.6
N1—Co1—N2^i	96.0 (1)	N2—C2—C1	106.2 (2)
N2—Co1—N2^i	177.6 (2)	N2—C2—H2A	110.5
O4—S1—O3	112.41 (15)	C1—C2—H2A	110.5
O4—S1—O2	113.26 (14)	N2—C2—H2B	110.5
O3—S1—O2	112.19 (15)	C1—C2—H2B	110.5
O4—S1—C3	107.56 (14)	H2A—C2—H2B	108.7
O3—S1—C3	105.53 (14)	C4—C3—C7^ii	121.1 (3)
O2—S1—C3	105.20 (14)	C4—C3—S1	118.1 (2)
Co1—O1—H1	108.40 (16)	C7^ii—C3—S1	120.7 (2)
Co1—O1—H11	111.37 (16)	C3—C4—C5	120.9 (3)
H1—O1—H11	109.1 (2)	C3—C4—H4	119.6
C1—N1—Co1	109.73 (19)	C5—C4—H4	119.6
C1—N1—H1N1	109.7	C6—C5—C4	120.3 (3)
Co1—N1—H1N1	109.7	C6—C5—H5	119.8
C1—N1—H1N2	109.7	C4—C5—H5	119.8
Co1—N1—H1N2	109.7	C5—C6—C7	120.8 (3)
H1N1—N1—H1N2	108.2	C5—C6—H6	119.6
C2—N2—Co1	108.71 (18)	C7—C6—H6	119.6
C2—N2—H2N1	109.9	C6—C7—C7^ii	119.5 (3)
Co1—N2—H2N1	109.9	C6—C7—C3^ii	123.1 (3)
C2—N2—H2N2	109.9	C7^ii—C7—C3^ii	117.4 (3)
Co1—N2—H2N2	109.9
O1—Co1—N1—C1	9.1 (17)	O4—S1—C3—C4	120.0 (3)
O1^i—Co1—N1—C1	−97.6 (2)	O3—S1—C3—C4	−119.8 (3)
N2—Co1—N1—C1	−9.9 (2)	O2—S1—C3—C4	−1.0 (3)
N2^i—Co1—N1—C1	171.8 (2)	O4—S1—C3—C7^ii	−63.5 (3)
N1^i—Co1—N1—C1	86.0 (2)	O3—S1—C3—C7^ii	56.7 (3)
O1—Co1—N2—C2	162.40 (19)	O2—S1—C3—C7^ii	175.5 (2)
O1^i—Co1—N2—C2	68.97 (19)	C7^ii—C3—C4—C5	−2.0 (5)
N2^i—Co1—N2—C2	115.71 (19)	S1—C3—C4—C5	174.5 (3)
N1—Co1—N2—C2	−18.8 (2)	C3—C4—C5—C6	0.6 (6)
N1^i—Co1—N2—C2	−109.9 (2)	C4—C5—C6—C7	1.4 (5)
Co1—N1—C1—C2	36.0 (3)	C5—C6—C7—C7^ii	−1.9 (6)
Co1—N2—C2—C1	42.9 (3)	C5—C6—C7—C3^ii	178.6 (3)
N1—C1—C2—N2	−51.1 (3)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O1^iii	0.85	1.65	2.439 (4)	154
O1—H11···O3^iv	0.85	2.24	2.961 (3)	144
N1—H1N1···O2	0.85	2.24	3.001 (3)	150
N1—H1N2···O1W^i	0.85	2.26	2.960 (9)	140
N1—H1N2···O1W'^i	0.85	2.15	2.94 (1)	154
N2—H2N1···O3^v	0.85	2.09	2.932 (3)	169
N2—H2N2···O2^vi	0.85	2.30	3.118 (4)	160

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