Retracted: Aqua­chloro­bis(1,10-phenanthroline)cobalt(II) chloride thio­acetamide solvate

The Co atom in the cation of the title complex, [CoCl(C₁₂H₈N₂)₂(H₂O)]Cl·H₂NC(CH₃)S, exists within a distorted octa­hedral coordination geometry defined by a Cl atom, the O atom of a water mol­ecule, and four N atoms from two 1,10-phenanthroline ligands. Mol­ecules are linked into a three-dimensional framework primarily by O—H...Cl hydrogen bonds and π–π stacking inter­actions.

Key indicators

• Single-crystal X-ray study
• T = 273 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.048
• wR factor = 0.164
• Data-to-parameter ratio = 15.4

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT362_ALERT_2_B Short  C(sp3)-C(sp2) Bond  C25    -   C26    ...       1.23 Ang.

Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.96
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000)         400 Deg.
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        C25
PLAT245_ALERT_2_C U(iso) H1A     Smaller than U(eq) O1      by ...       0.01 AngSq
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          8
PLAT354_ALERT_3_C Short   O-H Bond (0.82A)   O1     -   H1A    ...       0.66 Ang.
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety        C26
PLAT420_ALERT_2_C D-H Without Acceptor       N5     -   H5B    ...          ?
PLAT432_ALERT_2_C Short Inter X...Y Contact  S1     ..  C26     ..       3.28 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H24    ..  CL1     ..       2.92 Ang.

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

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

---

Computing details

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: SHELXL97.

Aquachlorobis(1,10-phenanthroline)cobalt(II) chloride thioacetamide solvate

Crystal data

[CoCl(C12H8N2)2(H2O)]Cl·C2H5NS	Z = 2
Mr = 583.38	F(000) = 598
Triclinic, P1	Dx = 1.543 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.785 (3) Å	Cell parameters from 3178 reflections
b = 11.350 (3) Å	θ = 2.7–25.9°
c = 12.799 (4) Å	µ = 1.01 mm^−1
α = 64.382 (4)°	T = 273 K
β = 86.963 (4)°	Block, pink
γ = 78.633 (4)°	0.42 × 0.27 × 0.17 mm
V = 1255.7 (6) Å^3

Data collection

Bruker APEX-II area-detector diffractometer	5128 independent reflections
Radiation source: fine-focus sealed tube	3284 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.027
φ and ω scans	θmax = 26.7°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→12
Tmin = 0.724, Tmax = 0.846	k = −14→14
8636 measured reflections	l = −15→16

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)] = 0.048	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.164	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ^2(Fo^2) + (0.1P)^2 + 0.801P] where P = (Fo^2 + 2Fc^2)/3
5128 reflections	(Δ/σ)max = 0.001
333 parameters	Δρmax = 0.52 e Å^−3
0 restraints	Δρmin = −0.79 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
Co1	0.79790 (5)	0.62976 (5)	0.72374 (4)	0.0369 (2)
S1	0.6707 (4)	1.0492 (3)	−0.1071 (2)	0.1581 (12)
Cl1	0.92467 (12)	0.44852 (11)	0.88470 (9)	0.0496 (3)
Cl2	0.87927 (13)	0.68594 (12)	0.35484 (11)	0.0581 (3)
O1	0.9540 (4)	0.5967 (4)	0.6137 (3)	0.0485 (8)
N1	0.6674 (4)	0.5128 (4)	0.6991 (3)	0.0429 (8)
N2	0.6186 (3)	0.6587 (3)	0.8204 (3)	0.0384 (8)
N3	0.7073 (3)	0.8060 (3)	0.5690 (3)	0.0396 (8)
N4	0.8837 (3)	0.7833 (3)	0.7321 (3)	0.0402 (8)
N5	0.8843 (12)	0.8925 (15)	0.0586 (11)	0.249 (7)
H5A	0.9112	0.8427	0.1298	0.299*
H5B	0.9448	0.9134	0.0058	0.299*
C1	0.6932 (5)	0.4393 (5)	0.6407 (4)	0.0572 (12)
H1	0.7795	0.4324	0.6075	0.069*
C2	0.5956 (6)	0.3716 (6)	0.6270 (5)	0.0668 (14)
H2	0.6175	0.3210	0.5853	0.080*
C3	0.4704 (5)	0.3798 (5)	0.6740 (4)	0.0602 (13)
H3	0.4047	0.3362	0.6639	0.072*
C4	0.4389 (5)	0.4540 (4)	0.7382 (4)	0.0469 (10)
C5	0.5425 (4)	0.5190 (4)	0.7491 (3)	0.0406 (9)
C6	0.5167 (4)	0.5958 (4)	0.8145 (3)	0.0395 (9)
C7	0.3107 (5)	0.4629 (5)	0.7953 (4)	0.0543 (12)
H7	0.2412	0.4220	0.7868	0.065*
C8	0.2888 (5)	0.5310 (5)	0.8623 (4)	0.0512 (11)
H8	0.2063	0.5327	0.9017	0.061*
C9	0.3918 (4)	0.5999 (4)	0.8724 (3)	0.0428 (10)
C10	0.3742 (5)	0.6727 (5)	0.9393 (4)	0.0500 (11)
H10	0.2935	0.6771	0.9803	0.060*
C11	0.4758 (5)	0.7361 (5)	0.9432 (4)	0.0510 (11)
H11	0.4645	0.7858	0.9859	0.061*
C12	0.5974 (5)	0.7269 (4)	0.8832 (4)	0.0468 (10)
H12	0.6665	0.7705	0.8875	0.056*
C13	0.6204 (5)	0.8156 (5)	0.4886 (4)	0.0485 (11)
H13	0.5862	0.7406	0.4990	0.058*
C14	0.5779 (5)	0.9328 (5)	0.3892 (4)	0.0580 (13)
H14	0.5154	0.9362	0.3353	0.070*
C15	0.6291 (5)	1.0420 (5)	0.3725 (4)	0.0612 (14)
H15	0.6032	1.1204	0.3056	0.073*
C16	0.7209 (5)	1.0376 (4)	0.4552 (4)	0.0495 (11)
C17	0.7584 (4)	0.9164 (4)	0.5520 (3)	0.0397 (9)
C18	0.8515 (4)	0.9042 (4)	0.6396 (3)	0.0392 (9)
C19	0.7780 (6)	1.1492 (5)	0.4449 (5)	0.0629 (14)
H19	0.7546	1.2302	0.3800	0.076*
C20	0.8653 (6)	1.1376 (5)	0.5286 (5)	0.0641 (15)
H20	0.9005	1.2113	0.5206	0.077*
C21	0.9045 (5)	1.0154 (4)	0.6282 (4)	0.0491 (11)
C22	0.9967 (5)	0.9986 (5)	0.7166 (5)	0.0593 (13)
H22	1.0359	1.0689	0.7122	0.071*
C23	1.0271 (5)	0.8765 (5)	0.8089 (5)	0.0613 (13)
H23	1.0871	0.8637	0.8685	0.074*
C24	0.9702 (5)	0.7720 (5)	0.8150 (4)	0.0484 (11)
H24	0.9928	0.6903	0.8793	0.058*
C25	0.7428 (12)	0.9391 (11)	0.0291 (9)	0.127 (3)
C26	0.6708 (10)	0.9001 (8)	0.1147 (8)	0.132 (3)
H26A	0.5740	0.9341	0.0913	0.197*
H26B	0.6944	0.9313	0.1689	0.197*
H26C	0.6878	0.8046	0.1506	0.197*
H1A	0.941 (5)	0.623 (5)	0.557 (4)	0.037 (16)*
H1B	1.015 (6)	0.516 (6)	0.644 (4)	0.071 (17)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0382 (3)	0.0377 (3)	0.0374 (3)	−0.0082 (2)	0.0001 (2)	−0.0182 (2)
S1	0.206 (3)	0.153 (2)	0.1071 (18)	0.005 (2)	0.0059 (18)	−0.0649 (18)
Cl1	0.0525 (7)	0.0491 (6)	0.0406 (6)	−0.0052 (5)	−0.0043 (4)	−0.0144 (5)
Cl2	0.0629 (8)	0.0593 (7)	0.0599 (7)	−0.0061 (6)	−0.0036 (5)	−0.0346 (6)
O1	0.053 (2)	0.049 (2)	0.042 (2)	−0.0028 (16)	0.0045 (16)	−0.0212 (17)
N1	0.044 (2)	0.045 (2)	0.045 (2)	−0.0116 (15)	0.0035 (15)	−0.0237 (17)
N2	0.0420 (19)	0.0370 (18)	0.0365 (17)	−0.0057 (14)	0.0003 (14)	−0.0169 (15)
N3	0.0394 (19)	0.043 (2)	0.0386 (18)	−0.0050 (15)	0.0009 (14)	−0.0205 (16)
N4	0.0392 (19)	0.0417 (19)	0.0425 (19)	−0.0055 (14)	−0.0022 (14)	−0.0213 (16)
N5	0.184 (10)	0.45 (2)	0.250 (13)	−0.104 (13)	0.100 (10)	−0.270 (15)
C1	0.056 (3)	0.073 (3)	0.063 (3)	−0.018 (2)	0.013 (2)	−0.048 (3)
C2	0.071 (4)	0.076 (4)	0.084 (4)	−0.029 (3)	0.015 (3)	−0.058 (3)
C3	0.064 (3)	0.071 (3)	0.070 (3)	−0.028 (3)	0.004 (2)	−0.047 (3)
C4	0.047 (3)	0.045 (3)	0.049 (2)	−0.0150 (19)	−0.0014 (19)	−0.019 (2)
C5	0.042 (2)	0.040 (2)	0.040 (2)	−0.0094 (18)	−0.0027 (17)	−0.0159 (18)
C6	0.044 (2)	0.036 (2)	0.034 (2)	−0.0029 (17)	−0.0047 (16)	−0.0108 (17)
C7	0.044 (3)	0.059 (3)	0.060 (3)	−0.015 (2)	−0.003 (2)	−0.023 (2)
C8	0.037 (2)	0.053 (3)	0.053 (3)	−0.008 (2)	−0.0008 (19)	−0.013 (2)
C9	0.038 (2)	0.041 (2)	0.039 (2)	−0.0001 (17)	−0.0011 (17)	−0.0108 (18)
C10	0.046 (3)	0.052 (3)	0.044 (2)	0.000 (2)	0.0031 (19)	−0.018 (2)
C11	0.061 (3)	0.048 (3)	0.044 (2)	0.001 (2)	0.001 (2)	−0.023 (2)
C12	0.051 (3)	0.048 (3)	0.046 (2)	−0.008 (2)	−0.0020 (19)	−0.025 (2)
C13	0.045 (3)	0.053 (3)	0.050 (3)	−0.004 (2)	−0.0098 (19)	−0.025 (2)
C14	0.055 (3)	0.070 (3)	0.046 (3)	0.007 (2)	−0.013 (2)	−0.028 (3)
C15	0.062 (3)	0.058 (3)	0.043 (3)	0.012 (2)	−0.002 (2)	−0.012 (2)
C16	0.052 (3)	0.045 (3)	0.040 (2)	0.002 (2)	0.0035 (19)	−0.013 (2)
C17	0.038 (2)	0.036 (2)	0.042 (2)	−0.0017 (17)	0.0041 (17)	−0.0174 (18)
C18	0.040 (2)	0.038 (2)	0.044 (2)	−0.0083 (17)	0.0047 (17)	−0.0205 (19)
C19	0.068 (3)	0.039 (3)	0.067 (3)	−0.007 (2)	0.013 (3)	−0.011 (2)
C20	0.067 (3)	0.041 (3)	0.085 (4)	−0.017 (2)	0.022 (3)	−0.027 (3)
C21	0.050 (3)	0.042 (2)	0.060 (3)	−0.012 (2)	0.012 (2)	−0.027 (2)
C22	0.054 (3)	0.059 (3)	0.086 (4)	−0.018 (2)	0.007 (3)	−0.049 (3)
C23	0.049 (3)	0.073 (4)	0.078 (3)	−0.007 (2)	−0.011 (2)	−0.047 (3)
C24	0.048 (3)	0.051 (3)	0.052 (3)	−0.007 (2)	−0.008 (2)	−0.028 (2)
C25	0.143 (8)	0.140 (8)	0.103 (6)	0.015 (7)	0.011 (6)	−0.076 (6)
C26	0.146 (8)	0.095 (6)	0.113 (7)	−0.002 (6)	−0.029 (6)	−0.013 (5)

Geometric parameters (Å, º)

Co1—Cl1	2.3695 (12)	C8—C9	1.434 (6)
Co1—O1	2.112 (3)	C8—H8	0.9300
Co1—N1	2.137 (4)	C9—C10	1.409 (6)
Co1—N2	2.147 (3)	C10—C11	1.351 (7)
Co1—N3	2.184 (3)	C10—H10	0.9300
Co1—N4	2.122 (4)	C11—C12	1.393 (6)
S1—C25	1.731 (10)	C11—H11	0.9300
O1—H1A	0.67 (4)	C12—H12	0.9300
O1—H1B	0.92 (6)	C13—C14	1.391 (7)
N1—C1	1.325 (6)	C13—H13	0.9300
N1—C5	1.352 (5)	C14—C15	1.355 (7)
N2—C12	1.320 (5)	C14—H14	0.9300
N2—C6	1.359 (5)	C15—C16	1.403 (7)
N3—C13	1.324 (5)	C15—H15	0.9300
N3—C17	1.367 (5)	C16—C17	1.392 (6)
N4—C24	1.339 (5)	C16—C19	1.434 (7)
N4—C18	1.360 (5)	C17—C18	1.424 (6)
N5—C25	1.391 (13)	C18—C21	1.406 (6)
N5—H5A	0.8600	C19—C20	1.351 (8)
N5—H5B	0.8600	C19—H19	0.9300
C1—C2	1.398 (7)	C20—C21	1.417 (7)
C1—H1	0.9300	C20—H20	0.9300
C2—C3	1.340 (7)	C21—C22	1.409 (7)
C2—H2	0.9300	C22—C23	1.365 (7)
C3—C4	1.395 (6)	C22—H22	0.9300
C3—H3	0.9300	C23—C24	1.378 (7)
C4—C5	1.411 (6)	C23—H23	0.9300
C4—C7	1.427 (6)	C24—H24	0.9300
C5—C6	1.431 (6)	C25—C26	1.230 (11)
C6—C9	1.399 (6)	C26—H26A	0.9600
C7—C8	1.366 (7)	C26—H26B	0.9600
C7—H7	0.9300	C26—H26C	0.9600
Cl1—Co1—O1	89.46 (12)	C6—C9—C10	117.3 (4)
Cl1—Co1—N1	94.22 (10)	C6—C9—C8	119.7 (4)
Cl1—Co1—N2	94.85 (9)	C10—C9—C8	123.1 (4)
Cl1—Co1—N3	172.38 (9)	C11—C10—C9	119.3 (4)
Cl1—Co1—N4	97.79 (10)	C11—C10—H10	120.3
O1—Co1—N1	94.89 (13)	C9—C10—H10	120.3
O1—Co1—N2	171.61 (14)	C10—C11—C12	119.9 (4)
O1—Co1—N3	85.52 (14)	C10—C11—H11	120.0
O1—Co1—N4	92.47 (13)	C12—C11—H11	120.0
N1—Co1—N2	77.65 (13)	N2—C12—C11	122.7 (4)
N1—Co1—N3	91.92 (13)	N2—C12—H12	118.7
N1—Co1—N4	165.97 (13)	C11—C12—H12	118.7
N2—Co1—N3	90.87 (12)	N3—C13—C14	123.0 (5)
N2—Co1—N4	94.07 (13)	N3—C13—H13	118.5
N3—Co1—N4	76.74 (13)	C14—C13—H13	118.5
Co1—O1—H1A	121 (4)	C15—C14—C13	118.8 (4)
Co1—O1—H1B	117 (3)	C15—C14—H14	120.6
H1A—O1—H1B	114 (6)	C13—C14—H14	120.6
C1—N1—C5	117.9 (4)	C14—C15—C16	120.6 (4)
C1—N1—Co1	128.3 (3)	C14—C15—H15	119.7
C5—N1—Co1	113.9 (3)	C16—C15—H15	119.7
C12—N2—C6	118.1 (4)	C17—C16—C15	116.9 (5)
C12—N2—Co1	128.7 (3)	C17—C16—C19	119.1 (4)
C6—N2—Co1	113.3 (3)	C15—C16—C19	124.0 (4)
C13—N3—C17	118.0 (4)	N3—C17—C16	122.7 (4)
C13—N3—Co1	128.8 (3)	N3—C17—C18	117.2 (3)
C17—N3—Co1	113.1 (3)	C16—C17—C18	120.2 (4)
C24—N4—C18	117.4 (4)	N4—C18—C21	123.0 (4)
C24—N4—Co1	127.1 (3)	N4—C18—C17	117.4 (4)
C18—N4—Co1	115.3 (3)	C21—C18—C17	119.7 (4)
C25—N5—H5A	120.0	C20—C19—C16	120.6 (5)
C25—N5—H5B	120.0	C20—C19—H19	119.7
H5A—N5—H5B	120.0	C16—C19—H19	119.7
N1—C1—C2	122.5 (4)	C19—C20—C21	121.4 (5)
N1—C1—H1	118.7	C19—C20—H20	119.3
C2—C1—H1	118.7	C21—C20—H20	119.3
C3—C2—C1	119.9 (5)	C18—C21—C22	117.7 (4)
C3—C2—H2	120.0	C18—C21—C20	119.1 (5)
C1—C2—H2	120.0	C22—C21—C20	123.2 (5)
C2—C3—C4	119.8 (5)	C23—C22—C21	118.3 (5)
C2—C3—H3	120.1	C23—C22—H22	120.8
C4—C3—H3	120.1	C21—C22—H22	120.8
C3—C4—C5	117.2 (4)	C22—C23—C24	120.9 (5)
C3—C4—C7	123.3 (4)	C22—C23—H23	119.6
C5—C4—C7	119.4 (4)	C24—C23—H23	119.6
N1—C5—C4	122.6 (4)	N4—C24—C23	122.7 (4)
N1—C5—C6	117.6 (4)	N4—C24—H24	118.7
C4—C5—C6	119.8 (4)	C23—C24—H24	118.7
N2—C6—C9	122.7 (4)	C26—C25—N5	111.7 (11)
N2—C6—C5	117.6 (4)	C26—C25—S1	122.0 (9)
C9—C6—C5	119.7 (4)	N5—C25—S1	126.2 (10)
C8—C7—C4	120.7 (4)	C25—C26—H26A	109.5
C8—C7—H7	119.7	C25—C26—H26B	109.5
C4—C7—H7	119.7	H26A—C26—H26B	109.5
C7—C8—C9	120.6 (4)	C25—C26—H26C	109.5
C7—C8—H8	119.7	H26A—C26—H26C	109.5
C9—C8—H8	119.7	H26B—C26—H26C	109.5

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C24—H24···Cl1	0.93	2.92	3.499 (5)	122
O1—H1A···Cl2	0.67 (4)	2.44 (5)	3.098 (4)	171 (5)
N5—H5A···Cl2	0.86	2.69	3.494 (13)	156
O1—H1B···Cl2^i	0.92 (6)	2.31 (6)	3.163 (4)	153 (5)

Symmetry code: (i) −x+2, −y+1, −z+1.