Bis(1,10-phenanthroline-κ²N,N′)(sulfato-κ²O,O′)cobalt(II) 1,2-ethanediol solvate

In the title compound, [Co(SO₄)(C₁₂H₈N₂)₂]·C₂H₆O₂, a twofold rotation axis passes through the Co and S atoms, and through the mid-point of the solvent C—C bond. The coordination environment of the Co^II centre is a distorted CoN₄O₂ octa­hedron, with four N atoms from two chelating 1,10-phenanthroline ligands and two O atoms from a bidentate sulfate ligand. The two chelating N₂C₂ groups are oriented at 70.16 (6)° to each other. Inter­molecular O—H...O hydrogen bonds help to stabilize the structure.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.004 Å
• H-atom completeness 94%
• Disorder in solvent or counterion
• R factor = 0.036
• wR factor = 0.107
• Data-to-parameter ratio = 16.0

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact  O2     ..  O3"     ..       2.76 Ang.

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.98
PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size .......       0.61 mm
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         S1
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for        O3'
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for         O3
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      25.00 Perc.
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........         O3
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........        O3'
PLAT366_ALERT_2_C Short? C(sp?)-C(sp?) Bond  C13    -   C13_b  ...       1.38 Ang.

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C26 H22 Co1 N4 O6 S1
            Atom count from the _atom_site data:  C26 H20.6 Co1 N4 O6 S1
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    4
           From the CIF: _chemical_formula_sum  C26 H22 Co N4 O6 S
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C        104.00    104.00    0.00
           H         88.00     82.40    5.60
           Co         4.00      4.00    0.00
           N         16.00     16.00    0.00
           O         24.00     24.00    0.00
           S          4.00      4.00    0.00

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

   7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   7 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
   5 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Bis(1,10-phenanthroline-κ²N,N')(sulfato-κ²O,O')cobalt(II) 1,2-ethenediol solvate

Crystal data

[Co(SO4)(C12H8N2)2]·C2H6O2	F(000) = 1188
Mr = 577.47	Dx = 1.559 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 18.500 (2) Å	Cell parameters from 4704 reflections
b = 11.8612 (12) Å	θ = 3.2–28.0°
c = 12.8230 (14) Å	µ = 0.83 mm^−1
β = 119.052 (2)°	T = 293 K
V = 2459.8 (5) Å^3	Block, red
Z = 4	0.61 × 0.46 × 0.41 mm

Data collection

Bruker SMART CCD 1K area-detector diffractometer	3065 independent reflections
Radiation source: fine-focus sealed tube	2656 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.052
φ and ω scans	θmax = 28.3°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −24→11
Tmin = 0.630, Tmax = 0.726	k = −15→15
8438 measured reflections	l = −14→17

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)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.107	H-atom parameters constrained
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0624P)^2 + 0.6033P] where P = (Fo^2 + 2Fc^2)/3
3065 reflections	(Δ/σ)max = 0.001
191 parameters	Δρmax = 0.55 e Å^−3
10 restraints	Δρmin = −0.52 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	Occ. (<1)
Co1	0.5000	0.69577 (3)	0.2500	0.03100 (12)
S1	0.5000	0.46760 (5)	0.2500	0.03093 (15)
O1	0.55314 (8)	0.54535 (12)	0.34866 (12)	0.0482 (3)
O2	0.55007 (10)	0.39789 (14)	0.21717 (17)	0.0601 (4)
N1	0.59299 (9)	0.80396 (12)	0.37837 (13)	0.0349 (3)
N2	0.58130 (9)	0.71550 (12)	0.17796 (13)	0.0343 (3)
C1	0.60063 (13)	0.84350 (17)	0.48050 (17)	0.0451 (4)
H1A	0.5584	0.8293	0.4984	0.054*
C2	0.66924 (15)	0.90543 (18)	0.56193 (19)	0.0522 (5)
H2B	0.6723	0.9311	0.6325	0.063*
C3	0.73142 (14)	0.92798 (16)	0.53748 (18)	0.0474 (5)
H3A	0.7771	0.9695	0.5910	0.057*
C4	0.72630 (11)	0.88829 (15)	0.43090 (16)	0.0381 (4)
C5	0.78880 (12)	0.90643 (17)	0.39792 (19)	0.0464 (5)
H5A	0.8357	0.9475	0.4486	0.056*
C6	0.78163 (11)	0.86568 (18)	0.29550 (18)	0.0473 (5)
H6A	0.8230	0.8801	0.2759	0.057*
C7	0.71101 (11)	0.80035 (15)	0.21625 (17)	0.0386 (4)
C8	0.70114 (12)	0.7523 (2)	0.11033 (19)	0.0509 (5)
H8A	0.7412	0.7636	0.0874	0.061*
C9	0.63306 (14)	0.68935 (19)	0.04106 (19)	0.0502 (5)
H9A	0.6256	0.6585	−0.0301	0.060*
C10	0.57440 (12)	0.67154 (17)	0.07811 (17)	0.0422 (4)
H10A	0.5286	0.6271	0.0310	0.051*
C11	0.65563 (10)	0.82575 (14)	0.35436 (15)	0.0317 (3)
C12	0.64855 (10)	0.77977 (14)	0.24615 (15)	0.0313 (3)
C13	0.5282 (3)	0.0910 (3)	0.2291 (5)	0.1123 (14)
H13A	0.5808	0.0716	0.2975	0.135*
H13B	0.5130	0.0272	0.1752	0.135*
O3	0.5449 (14)	0.1735 (6)	0.1748 (18)	0.090 (6)	0.30
H3	0.5601	0.2292	0.2180	0.135*	0.30
O3"	0.5836 (6)	0.1698 (6)	0.2460 (15)	0.078 (3)	0.40
O3'	0.563 (2)	0.1794 (8)	0.208 (4)	0.127 (12)	0.30

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.02739 (18)	0.03238 (19)	0.03370 (19)	0.000	0.01521 (14)	0.000
S1	0.0249 (3)	0.0314 (3)	0.0374 (3)	0.000	0.0158 (2)	0.000
O1	0.0435 (7)	0.0404 (7)	0.0390 (7)	0.0012 (6)	0.0030 (6)	0.0001 (6)
O2	0.0584 (10)	0.0516 (8)	0.0925 (13)	0.0091 (7)	0.0542 (9)	−0.0042 (8)
N1	0.0370 (8)	0.0346 (7)	0.0353 (8)	−0.0032 (6)	0.0193 (6)	−0.0026 (5)
N2	0.0306 (7)	0.0372 (7)	0.0355 (7)	−0.0022 (6)	0.0163 (6)	−0.0049 (6)
C1	0.0549 (12)	0.0455 (10)	0.0430 (10)	−0.0073 (9)	0.0302 (9)	−0.0088 (8)
C2	0.0657 (14)	0.0519 (11)	0.0383 (10)	−0.0056 (10)	0.0247 (10)	−0.0116 (9)
C3	0.0501 (11)	0.0428 (10)	0.0375 (10)	−0.0086 (8)	0.0120 (8)	−0.0069 (8)
C4	0.0353 (9)	0.0347 (8)	0.0362 (9)	−0.0036 (7)	0.0110 (7)	0.0006 (7)
C5	0.0309 (9)	0.0489 (11)	0.0483 (11)	−0.0100 (8)	0.0105 (8)	0.0011 (8)
C6	0.0317 (9)	0.0574 (12)	0.0532 (11)	−0.0067 (8)	0.0211 (8)	0.0031 (10)
C7	0.0324 (9)	0.0438 (10)	0.0412 (9)	0.0000 (7)	0.0192 (7)	0.0038 (7)
C8	0.0460 (11)	0.0669 (14)	0.0525 (11)	−0.0036 (10)	0.0338 (9)	−0.0020 (10)
C9	0.0557 (12)	0.0605 (13)	0.0429 (11)	−0.0001 (9)	0.0308 (10)	−0.0086 (9)
C10	0.0398 (10)	0.0486 (10)	0.0389 (9)	−0.0041 (8)	0.0197 (8)	−0.0090 (8)
C11	0.0312 (8)	0.0300 (7)	0.0314 (8)	0.0000 (6)	0.0131 (6)	0.0017 (6)
C12	0.0282 (7)	0.0311 (7)	0.0338 (8)	0.0013 (6)	0.0145 (6)	0.0019 (6)
C13	0.148 (4)	0.0546 (17)	0.191 (4)	0.0155 (19)	0.126 (4)	0.005 (2)
O3	0.177 (16)	0.046 (5)	0.099 (8)	0.030 (6)	0.108 (10)	0.006 (5)
O3"	0.068 (4)	0.042 (3)	0.138 (9)	0.020 (3)	0.061 (4)	0.023 (4)
O3'	0.15 (2)	0.112 (13)	0.20 (3)	0.024 (11)	0.15 (2)	0.052 (12)

Geometric parameters (Å, º)

Co1—N2^i	2.1261 (15)	C3—H3A	0.930
Co1—N2	2.1261 (15)	C4—C11	1.406 (2)
Co1—O1^i	2.1313 (14)	C4—C5	1.427 (3)
Co1—O1	2.1313 (14)	C5—C6	1.344 (3)
Co1—N1	2.1368 (15)	C5—H5A	0.930
Co1—N1^i	2.1368 (14)	C6—C7	1.432 (3)
Co1—S1	2.7064 (7)	C6—H6A	0.930
S1—O2^i	1.4483 (14)	C7—C8	1.400 (3)
S1—O2	1.4483 (14)	C7—C12	1.404 (2)
S1—O1	1.4865 (14)	C8—C9	1.359 (3)
S1—O1^i	1.4865 (13)	C8—H8A	0.930
N1—C1	1.332 (2)	C9—C10	1.396 (3)
N1—C11	1.361 (2)	C9—H9A	0.930
N2—C10	1.330 (2)	C10—H10A	0.930
N2—C12	1.355 (2)	C11—C12	1.436 (2)
C1—C2	1.398 (3)	C13—O3	1.320 (6)
C1—H1A	0.930	C13—C13^i	1.386 (7)
C2—C3	1.358 (3)	C13—H13A	0.970
C2—H2B	0.930	C13—H13B	0.970
C3—C4	1.405 (3)	O3—H3	0.820
N2^i—Co1—N2	167.36 (8)	C3—C2—C1	119.66 (19)
N2^i—Co1—O1^i	97.49 (6)	C3—C2—H2B	120.2
N2—Co1—O1^i	93.09 (6)	C1—C2—H2B	120.2
N2^i—Co1—O1	93.09 (6)	C2—C3—C4	119.62 (18)
N2—Co1—O1	97.49 (6)	C2—C3—H3A	120.2
O1^i—Co1—O1	66.32 (7)	C4—C3—H3A	120.2
N2^i—Co1—N1	94.24 (6)	C3—C4—C11	117.17 (18)
N2—Co1—N1	78.10 (6)	C3—C4—C5	123.80 (17)
O1^i—Co1—N1	157.94 (5)	C11—C4—C5	119.03 (17)
O1—Co1—N1	94.52 (5)	C6—C5—C4	121.70 (17)
N2^i—Co1—N1^i	78.10 (6)	C6—C5—H5A	119.2
N2—Co1—N1^i	94.24 (6)	C4—C5—H5A	119.2
O1^i—Co1—N1^i	94.52 (5)	C5—C6—C7	120.74 (18)
O1—Co1—N1^i	157.94 (6)	C5—C6—H6A	119.6
N1—Co1—N1^i	106.18 (8)	C7—C6—H6A	119.6
N2^i—Co1—S1	96.32 (4)	C8—C7—C12	117.19 (16)
N2—Co1—S1	96.32 (4)	C8—C7—C6	123.55 (17)
O1^i—Co1—S1	33.16 (3)	C12—C7—C6	119.24 (18)
O1—Co1—S1	33.16 (3)	C9—C8—C7	120.03 (17)
N1—Co1—S1	126.91 (4)	C9—C8—H8A	120.0
N1^i—Co1—S1	126.91 (4)	C7—C8—H8A	120.0
O2^i—S1—O2	110.38 (14)	C8—C9—C10	119.18 (19)
O2^i—S1—O1	111.02 (10)	C8—C9—H9A	120.4
O2—S1—O1	110.46 (9)	C10—C9—H9A	120.4
O2^i—S1—O1^i	110.46 (9)	N2—C10—C9	122.77 (18)
O2—S1—O1^i	111.03 (10)	N2—C10—H10A	118.6
O1—S1—O1^i	103.31 (11)	C9—C10—H10A	118.6
O2^i—S1—Co1	124.81 (7)	N1—C11—C4	123.21 (16)
O2—S1—Co1	124.81 (7)	N1—C11—C12	117.28 (15)
O1—S1—Co1	51.66 (5)	C4—C11—C12	119.50 (16)
O1^i—S1—Co1	51.66 (5)	N2—C12—C7	122.74 (16)
S1—O1—Co1	95.18 (6)	N2—C12—C11	117.47 (14)
C1—N1—C11	117.39 (16)	C7—C12—C11	119.77 (15)
C1—N1—Co1	129.06 (13)	O3—C13—C13^i	128.1 (6)
C11—N1—Co1	113.28 (11)	O3—C13—H13A	105.3
C10—N2—C12	118.07 (15)	C13^i—C13—H13A	105.3
C10—N2—Co1	128.15 (12)	O3—C13—H13B	105.3
C12—N2—Co1	113.77 (11)	C13^i—C13—H13B	105.3
N1—C1—C2	122.94 (18)	H13A—C13—H13B	106.0
N1—C1—H1A	118.5	C13—O3—H3	109.5
C2—C1—H1A	118.5
O3—C13—C13^i—O3^i	−40 (3)

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
O3—H3···O2	0.82	2.01	2.709 (8)	143