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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 CoII 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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806002315/wn6409sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806002315/wn6409Isup2.hkl
Contains datablock I

CCDC reference: 601265

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

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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

Computing details top

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 top
Crystal data top
[Co(SO4)(C12H8N2)2]·C2H6O2F(000) = 1188
Mr = 577.47Dx = 1.559 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 18.500 (2) ÅCell parameters from 4704 reflections
b = 11.8612 (12) Åθ = 3.2–28.0°
c = 12.8230 (14) ŵ = 0.83 mm1
β = 119.052 (2)°T = 293 K
V = 2459.8 (5) Å3Block, red
Z = 40.61 × 0.46 × 0.41 mm
Data collection top
Bruker SMART CCD 1K area-detector
diffractometer
3065 independent reflections
Radiation source: fine-focus sealed tube2656 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
φ and ω scansθmax = 28.3°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 2411
Tmin = 0.630, Tmax = 0.726k = 1515
8438 measured reflectionsl = 1417
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0624P)2 + 0.6033P]
where P = (Fo2 + 2Fc2)/3
3065 reflections(Δ/σ)max = 0.001
191 parametersΔρmax = 0.55 e Å3
10 restraintsΔρmin = 0.52 e Å3
Special details top

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 (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.50000.69577 (3)0.25000.03100 (12)
S10.50000.46760 (5)0.25000.03093 (15)
O10.55314 (8)0.54535 (12)0.34866 (12)0.0482 (3)
O20.55007 (10)0.39789 (14)0.21717 (17)0.0601 (4)
N10.59299 (9)0.80396 (12)0.37837 (13)0.0349 (3)
N20.58130 (9)0.71550 (12)0.17796 (13)0.0343 (3)
C10.60063 (13)0.84350 (17)0.48050 (17)0.0451 (4)
H1A0.55840.82930.49840.054*
C20.66924 (15)0.90543 (18)0.56193 (19)0.0522 (5)
H2B0.67230.93110.63250.063*
C30.73142 (14)0.92798 (16)0.53748 (18)0.0474 (5)
H3A0.77710.96950.59100.057*
C40.72630 (11)0.88829 (15)0.43090 (16)0.0381 (4)
C50.78880 (12)0.90643 (17)0.39792 (19)0.0464 (5)
H5A0.83570.94750.44860.056*
C60.78163 (11)0.86568 (18)0.29550 (18)0.0473 (5)
H6A0.82300.88010.27590.057*
C70.71101 (11)0.80035 (15)0.21625 (17)0.0386 (4)
C80.70114 (12)0.7523 (2)0.11033 (19)0.0509 (5)
H8A0.74120.76360.08740.061*
C90.63306 (14)0.68935 (19)0.04106 (19)0.0502 (5)
H9A0.62560.65850.03010.060*
C100.57440 (12)0.67154 (17)0.07811 (17)0.0422 (4)
H10A0.52860.62710.03100.051*
C110.65563 (10)0.82575 (14)0.35436 (15)0.0317 (3)
C120.64855 (10)0.77977 (14)0.24615 (15)0.0313 (3)
C130.5282 (3)0.0910 (3)0.2291 (5)0.1123 (14)
H13A0.58080.07160.29750.135*
H13B0.51300.02720.17520.135*
O30.5449 (14)0.1735 (6)0.1748 (18)0.090 (6)0.30
H30.56010.22920.21800.135*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 (Å2) top
U11U22U33U12U13U23
Co10.02739 (18)0.03238 (19)0.03370 (19)0.0000.01521 (14)0.000
S10.0249 (3)0.0314 (3)0.0374 (3)0.0000.0158 (2)0.000
O10.0435 (7)0.0404 (7)0.0390 (7)0.0012 (6)0.0030 (6)0.0001 (6)
O20.0584 (10)0.0516 (8)0.0925 (13)0.0091 (7)0.0542 (9)0.0042 (8)
N10.0370 (8)0.0346 (7)0.0353 (8)0.0032 (6)0.0193 (6)0.0026 (5)
N20.0306 (7)0.0372 (7)0.0355 (7)0.0022 (6)0.0163 (6)0.0049 (6)
C10.0549 (12)0.0455 (10)0.0430 (10)0.0073 (9)0.0302 (9)0.0088 (8)
C20.0657 (14)0.0519 (11)0.0383 (10)0.0056 (10)0.0247 (10)0.0116 (9)
C30.0501 (11)0.0428 (10)0.0375 (10)0.0086 (8)0.0120 (8)0.0069 (8)
C40.0353 (9)0.0347 (8)0.0362 (9)0.0036 (7)0.0110 (7)0.0006 (7)
C50.0309 (9)0.0489 (11)0.0483 (11)0.0100 (8)0.0105 (8)0.0011 (8)
C60.0317 (9)0.0574 (12)0.0532 (11)0.0067 (8)0.0211 (8)0.0031 (10)
C70.0324 (9)0.0438 (10)0.0412 (9)0.0000 (7)0.0192 (7)0.0038 (7)
C80.0460 (11)0.0669 (14)0.0525 (11)0.0036 (10)0.0338 (9)0.0020 (10)
C90.0557 (12)0.0605 (13)0.0429 (11)0.0001 (9)0.0308 (10)0.0086 (9)
C100.0398 (10)0.0486 (10)0.0389 (9)0.0041 (8)0.0197 (8)0.0090 (8)
C110.0312 (8)0.0300 (7)0.0314 (8)0.0000 (6)0.0131 (6)0.0017 (6)
C120.0282 (7)0.0311 (7)0.0338 (8)0.0013 (6)0.0145 (6)0.0019 (6)
C130.148 (4)0.0546 (17)0.191 (4)0.0155 (19)0.126 (4)0.005 (2)
O30.177 (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) top
Co1—N2i2.1261 (15)C3—H3A0.930
Co1—N22.1261 (15)C4—C111.406 (2)
Co1—O1i2.1313 (14)C4—C51.427 (3)
Co1—O12.1313 (14)C5—C61.344 (3)
Co1—N12.1368 (15)C5—H5A0.930
Co1—N1i2.1368 (14)C6—C71.432 (3)
Co1—S12.7064 (7)C6—H6A0.930
S1—O2i1.4483 (14)C7—C81.400 (3)
S1—O21.4483 (14)C7—C121.404 (2)
S1—O11.4865 (14)C8—C91.359 (3)
S1—O1i1.4865 (13)C8—H8A0.930
N1—C11.332 (2)C9—C101.396 (3)
N1—C111.361 (2)C9—H9A0.930
N2—C101.330 (2)C10—H10A0.930
N2—C121.355 (2)C11—C121.436 (2)
C1—C21.398 (3)C13—O31.320 (6)
C1—H1A0.930C13—C13i1.386 (7)
C2—C31.358 (3)C13—H13A0.970
C2—H2B0.930C13—H13B0.970
C3—C41.405 (3)O3—H30.820
N2i—Co1—N2167.36 (8)C3—C2—C1119.66 (19)
N2i—Co1—O1i97.49 (6)C3—C2—H2B120.2
N2—Co1—O1i93.09 (6)C1—C2—H2B120.2
N2i—Co1—O193.09 (6)C2—C3—C4119.62 (18)
N2—Co1—O197.49 (6)C2—C3—H3A120.2
O1i—Co1—O166.32 (7)C4—C3—H3A120.2
N2i—Co1—N194.24 (6)C3—C4—C11117.17 (18)
N2—Co1—N178.10 (6)C3—C4—C5123.80 (17)
O1i—Co1—N1157.94 (5)C11—C4—C5119.03 (17)
O1—Co1—N194.52 (5)C6—C5—C4121.70 (17)
N2i—Co1—N1i78.10 (6)C6—C5—H5A119.2
N2—Co1—N1i94.24 (6)C4—C5—H5A119.2
O1i—Co1—N1i94.52 (5)C5—C6—C7120.74 (18)
O1—Co1—N1i157.94 (6)C5—C6—H6A119.6
N1—Co1—N1i106.18 (8)C7—C6—H6A119.6
N2i—Co1—S196.32 (4)C8—C7—C12117.19 (16)
N2—Co1—S196.32 (4)C8—C7—C6123.55 (17)
O1i—Co1—S133.16 (3)C12—C7—C6119.24 (18)
O1—Co1—S133.16 (3)C9—C8—C7120.03 (17)
N1—Co1—S1126.91 (4)C9—C8—H8A120.0
N1i—Co1—S1126.91 (4)C7—C8—H8A120.0
O2i—S1—O2110.38 (14)C8—C9—C10119.18 (19)
O2i—S1—O1111.02 (10)C8—C9—H9A120.4
O2—S1—O1110.46 (9)C10—C9—H9A120.4
O2i—S1—O1i110.46 (9)N2—C10—C9122.77 (18)
O2—S1—O1i111.03 (10)N2—C10—H10A118.6
O1—S1—O1i103.31 (11)C9—C10—H10A118.6
O2i—S1—Co1124.81 (7)N1—C11—C4123.21 (16)
O2—S1—Co1124.81 (7)N1—C11—C12117.28 (15)
O1—S1—Co151.66 (5)C4—C11—C12119.50 (16)
O1i—S1—Co151.66 (5)N2—C12—C7122.74 (16)
S1—O1—Co195.18 (6)N2—C12—C11117.47 (14)
C1—N1—C11117.39 (16)C7—C12—C11119.77 (15)
C1—N1—Co1129.06 (13)O3—C13—C13i128.1 (6)
C11—N1—Co1113.28 (11)O3—C13—H13A105.3
C10—N2—C12118.07 (15)C13i—C13—H13A105.3
C10—N2—Co1128.15 (12)O3—C13—H13B105.3
C12—N2—Co1113.77 (11)C13i—C13—H13B105.3
N1—C1—C2122.94 (18)H13A—C13—H13B106.0
N1—C1—H1A118.5C13—O3—H3109.5
C2—C1—H1A118.5
O3—C13—C13i—O3i40 (3)
Symmetry code: (i) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O20.822.012.709 (8)143
 

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