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

Zhong, H.; Zeng, X.-R.; Liu, Y.-Q.; Luo, Q.-Y.

doi:10.1107/S1600536806041122

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

H. Zhong, X.-R. Zeng, Y.-Q. Liu and Q.-Y. Luo

The Co(II) ion in the title compound, [CoCl(phen)₂(H₂O)]Cl·C(NH₂)₂S [phen = 1,10-phenanthroline, (C₁₂H₈N₂)], has a distorted octahedral coordination formed by one Cl atom, one water molecule, and four N atoms of two phen ligands. Ions and molecules are linked into a three-dimensional framework by N—H

S, N—H

Cl and O—H

Cl hydrogen bonds. The supramolecular network structure is consolidated by π–π stacking interactions and hydrogen bonds.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806041122/hk2146sup1.cif Contains datablocks I, aa
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806041122/hk2146Isup2.hkl Contains datablock I

CCDC reference: 1195260

checkCIF report

Key indicators

Single-crystal X-ray study
T = 273 K
Mean (C-C) = 0.008 Å
R factor = 0.048
wR factor = 0.181
Data-to-parameter ratio = 16.1

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.98
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        C25
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          7
PLAT420_ALERT_2_C D-H Without Acceptor       N6     -   H6B    ...          ?

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

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

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: APEX2; software used to prepare material for publication: APEX2.

(I) top

Crystal data top

[CoCl(C₁₂H₈N₂)₂(H₂O)]Cl·(NH₂)₂CS	Z = 2
M_r = 584.38	F(000) = 598
Triclinic, P1	D_x = 1.536 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.8147 (9) Å	Cell parameters from 2467 reflections
b = 11.3517 (11) Å	θ = 2.6–25.0°
c = 12.8454 (12) Å	µ = 1.01 mm⁻¹
α = 64.223 (1)°	T = 273 K
β = 86.947 (1)°	Block, pink
γ = 78.748 (1)°	0.21 × 0.20 × 0.09 mm
V = 1263.2 (2) Å³

Data collection top

Bruker APEX-II area-detector diffractometer	5320 independent reflections
Radiation source: fine-focus sealed tube	3160 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.030
φ and ω scans	θ_max = 26.9°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −12→12
T_min = 0.815, T_max = 0.915	k = −14→14
8804 measured reflections	l = −16→15

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.048	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.181	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	w = 1/[σ²(F_o²) + (0.101P)² + 0.010P] where P = (F_o² + 2F_c²)/3
5320 reflections	(Δ/σ)_max < 0.001
330 parameters	Δρ_max = 1.17 e Å⁻³
0 restraints	Δρ_min = −0.80 e Å⁻³

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

	x	y	z	U_iso*/U_eq
C1	0.1929 (5)	−0.0629 (5)	0.1418 (4)	0.0563 (13)
H1	0.2796	−0.0711	0.1100	0.068*
C2	0.0953 (5)	−0.1286 (6)	0.1268 (5)	0.0667 (15)
H2	0.1170	−0.1781	0.0844	0.080*
C3	−0.0305 (5)	−0.1208 (6)	0.1732 (5)	0.0608 (14)
H3	−0.0962	−0.1644	0.1633	0.073*
C4	−0.0607 (4)	−0.0448 (5)	0.2376 (4)	0.0470 (11)
C5	0.0421 (4)	0.0187 (4)	0.2489 (3)	0.0408 (10)
C6	0.0161 (4)	0.0952 (4)	0.3148 (3)	0.0388 (10)
C7	−0.1899 (5)	−0.0359 (5)	0.2944 (4)	0.0549 (12)
H7	−0.2595	−0.0761	0.2852	0.066*
C8	−0.2111 (4)	0.0310 (5)	0.3619 (4)	0.0521 (12)
H8	−0.2933	0.0320	0.4013	0.063*
C9	−0.1082 (4)	0.1004 (4)	0.3732 (4)	0.0425 (10)
C10	−0.1259 (5)	0.1722 (5)	0.4391 (4)	0.0494 (11)
H10	−0.2063	0.1764	0.4801	0.059*
C11	−0.0239 (5)	0.2358 (5)	0.4427 (4)	0.0513 (12)
H11	−0.0350	0.2859	0.4848	0.062*
C12	0.0980 (5)	0.2260 (5)	0.3829 (4)	0.0462 (11)
H12	0.1673	0.2692	0.3873	0.055*
C13	0.1201 (5)	0.3156 (5)	−0.0115 (4)	0.0489 (11)
H13	0.0853	0.2408	−0.0010	0.059*
C14	0.0788 (5)	0.4323 (6)	−0.1095 (4)	0.0581 (14)
H14	0.0164	0.4355	−0.1631	0.070*
C15	0.1292 (5)	0.5427 (5)	−0.1278 (4)	0.0599 (14)
H15	0.1032	0.6210	−0.1948	0.072*
C16	0.2210 (5)	0.5379 (5)	−0.0450 (4)	0.0491 (12)
C17	0.2583 (4)	0.4167 (4)	0.0522 (4)	0.0409 (10)
C18	0.3521 (4)	0.4038 (4)	0.1399 (4)	0.0381 (9)
C19	0.2773 (5)	0.6491 (5)	−0.0554 (5)	0.0622 (14)
H19	0.2540	0.7303	−0.1201	0.075*
C20	0.3649 (6)	0.6371 (5)	0.0288 (5)	0.0638 (15)
H20	0.3993	0.7112	0.0211	0.077*
C21	0.4051 (4)	0.5146 (5)	0.1282 (4)	0.0489 (11)
C22	0.4974 (5)	0.4981 (5)	0.2164 (5)	0.0584 (13)
H22	0.5368	0.5684	0.2115	0.070*
C23	0.5271 (5)	0.3763 (6)	0.3089 (5)	0.0590 (13)
H23	0.5858	0.3638	0.3687	0.071*
C24	0.4706 (4)	0.2709 (5)	0.3146 (4)	0.0466 (11)
H24	0.4936	0.1887	0.3783	0.056*
C25	0.2482 (12)	0.4413 (11)	0.5281 (8)	0.127 (3)
Cl1	0.42462 (11)	−0.05267 (12)	0.38482 (9)	0.0500 (3)
Cl2	0.37942 (13)	0.18632 (13)	0.85438 (11)	0.0586 (4)
Co1	0.29819 (5)	0.12891 (6)	0.22383 (5)	0.0369 (2)
N1	0.1673 (4)	0.0111 (4)	0.2000 (3)	0.0437 (9)
N2	0.1187 (3)	0.1579 (3)	0.3204 (3)	0.0386 (8)
N3	0.3846 (3)	0.2829 (3)	0.2324 (3)	0.0376 (8)
N4	0.2074 (3)	0.3056 (3)	0.0685 (3)	0.0396 (8)
N5	0.1724 (9)	0.4020 (8)	0.6134 (7)	0.171 (4)
H5A	0.2093	0.3500	0.6812	0.206*
H5B	0.0836	0.4272	0.6043	0.206*
N6	0.3857 (10)	0.3916 (14)	0.5588 (10)	0.247 (7)
H6A	0.4106	0.3399	0.6298	0.296*
H6B	0.4473	0.4119	0.5070	0.296*
O1	0.4540 (3)	0.0967 (4)	0.1127 (3)	0.0489 (8)
H1A	0.4233	0.1352	0.0456	0.073*
S1	0.1732 (3)	0.5482 (3)	0.3936 (2)	0.1518 (11)
H1B	0.510 (5)	0.019 (5)	0.148 (4)	0.052 (15)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.053 (3)	0.072 (4)	0.060 (3)	−0.019 (3)	0.012 (2)	−0.042 (3)
C2	0.066 (3)	0.085 (4)	0.082 (4)	−0.031 (3)	0.018 (3)	−0.061 (4)
C3	0.063 (3)	0.069 (4)	0.068 (3)	−0.030 (3)	0.007 (3)	−0.039 (3)
C4	0.043 (2)	0.053 (3)	0.046 (3)	−0.015 (2)	0.001 (2)	−0.019 (2)
C5	0.039 (2)	0.043 (3)	0.035 (2)	−0.0072 (19)	0.0002 (18)	−0.0124 (19)
C6	0.037 (2)	0.038 (2)	0.034 (2)	−0.0057 (18)	−0.0026 (17)	−0.0086 (18)
C7	0.040 (2)	0.061 (3)	0.063 (3)	−0.013 (2)	−0.006 (2)	−0.024 (3)
C8	0.034 (2)	0.056 (3)	0.052 (3)	−0.007 (2)	0.004 (2)	−0.011 (2)
C9	0.038 (2)	0.039 (3)	0.038 (2)	−0.0016 (19)	−0.0020 (19)	−0.0075 (19)
C10	0.045 (3)	0.049 (3)	0.042 (2)	−0.001 (2)	0.004 (2)	−0.012 (2)
C11	0.061 (3)	0.050 (3)	0.041 (2)	0.005 (2)	0.001 (2)	−0.024 (2)
C12	0.048 (2)	0.045 (3)	0.043 (2)	−0.003 (2)	−0.001 (2)	−0.019 (2)
C13	0.049 (3)	0.051 (3)	0.045 (3)	−0.002 (2)	−0.008 (2)	−0.021 (2)
C14	0.056 (3)	0.070 (4)	0.041 (3)	0.010 (3)	−0.011 (2)	−0.024 (3)
C15	0.066 (3)	0.050 (3)	0.038 (2)	0.011 (3)	−0.001 (2)	−0.004 (2)
C16	0.048 (3)	0.042 (3)	0.041 (2)	0.004 (2)	0.009 (2)	−0.009 (2)
C17	0.039 (2)	0.037 (2)	0.039 (2)	−0.0019 (19)	0.0067 (18)	−0.0112 (19)
C18	0.034 (2)	0.037 (2)	0.044 (2)	−0.0072 (18)	0.0035 (18)	−0.019 (2)
C19	0.065 (3)	0.035 (3)	0.067 (3)	−0.001 (2)	0.013 (3)	−0.009 (2)
C20	0.068 (3)	0.041 (3)	0.081 (4)	−0.017 (3)	0.023 (3)	−0.024 (3)
C21	0.042 (2)	0.041 (3)	0.062 (3)	−0.010 (2)	0.013 (2)	−0.020 (2)
C22	0.049 (3)	0.056 (3)	0.085 (4)	−0.019 (2)	0.009 (3)	−0.042 (3)
C23	0.049 (3)	0.070 (4)	0.072 (3)	−0.006 (3)	−0.010 (2)	−0.044 (3)
C24	0.047 (3)	0.047 (3)	0.048 (3)	−0.006 (2)	−0.009 (2)	−0.023 (2)
C25	0.138 (8)	0.156 (9)	0.093 (6)	−0.011 (7)	0.032 (6)	−0.070 (6)
Cl1	0.0509 (7)	0.0503 (7)	0.0393 (6)	−0.0054 (5)	−0.0022 (5)	−0.0122 (5)
Cl2	0.0631 (8)	0.0576 (8)	0.0594 (7)	−0.0054 (6)	−0.0027 (6)	−0.0313 (6)
Co1	0.0375 (3)	0.0368 (4)	0.0359 (3)	−0.0087 (2)	0.0023 (2)	−0.0147 (3)
N1	0.0409 (19)	0.050 (2)	0.043 (2)	−0.0121 (17)	0.0048 (16)	−0.0213 (18)
N2	0.0386 (18)	0.040 (2)	0.0325 (18)	−0.0066 (15)	0.0041 (14)	−0.0124 (16)
N3	0.0371 (18)	0.037 (2)	0.0389 (19)	−0.0069 (15)	0.0011 (15)	−0.0165 (16)
N4	0.0417 (19)	0.039 (2)	0.0367 (18)	−0.0060 (16)	0.0020 (15)	−0.0154 (16)
N5	0.149 (7)	0.146 (8)	0.139 (8)	0.002 (6)	−0.018 (6)	0.001 (6)
N6	0.158 (8)	0.46 (2)	0.240 (12)	−0.087 (11)	0.092 (9)	−0.260 (14)
O1	0.0492 (18)	0.047 (2)	0.0443 (17)	−0.0011 (16)	0.0056 (15)	−0.0182 (17)
S1	0.187 (3)	0.150 (2)	0.1045 (18)	0.002 (2)	0.0128 (17)	−0.0575 (17)

Geometric parameters (Å, º) top

C1—N1	1.332 (6)	C16—C19	1.426 (7)
C1—C2	1.391 (7)	C17—N4	1.375 (6)
C1—H1	0.9300	C17—C18	1.432 (6)
C2—C3	1.347 (7)	C18—N3	1.359 (5)
C2—H2	0.9300	C18—C21	1.399 (6)
C3—C4	1.418 (7)	C19—C20	1.362 (7)
C3—H3	0.9300	C19—H19	0.9300
C4—C5	1.397 (6)	C20—C21	1.419 (7)
C4—C7	1.437 (6)	C20—H20	0.9300
C5—N1	1.354 (5)	C21—C22	1.414 (7)
C5—C6	1.437 (6)	C22—C23	1.363 (7)
C6—N2	1.364 (5)	C22—H22	0.9300
C6—C9	1.402 (6)	C23—C24	1.387 (7)
C7—C8	1.365 (7)	C23—H23	0.9300
C7—H7	0.9300	C24—N3	1.331 (5)
C8—C9	1.444 (7)	C24—H24	0.9300
C8—H8	0.9300	C25—N5	1.253 (10)
C9—C10	1.393 (6)	C25—N6	1.364 (13)
C10—C11	1.357 (7)	C25—S1	1.721 (10)
C10—H10	0.9300	Cl1—Co1	2.3733 (12)
C11—C12	1.399 (6)	Co1—O1	2.124 (3)
C11—H11	0.9300	Co1—N3	2.131 (3)
C12—N2	1.319 (5)	Co1—N1	2.145 (4)
C12—H12	0.9300	Co1—N2	2.156 (3)
C13—N4	1.326 (5)	Co1—N4	2.193 (3)
C13—C14	1.378 (6)	N5—H5A	0.8600
C13—H13	0.9300	N5—H5B	0.8600
C14—C15	1.358 (7)	N6—H6A	0.8600
C14—H14	0.9300	N6—H6B	0.8600
C15—C16	1.408 (7)	O1—H1A	0.8300
C15—H15	0.9300	O1—H1B	0.88 (6)
C16—C17	1.394 (6)

N1—C1—C2	122.7 (4)	C16—C19—H19	119.8
N1—C1—H1	118.7	C19—C20—C21	121.7 (5)
C2—C1—H1	118.7	C19—C20—H20	119.1
C3—C2—C1	120.3 (5)	C21—C20—H20	119.1
C3—C2—H2	119.8	C18—C21—C22	117.9 (4)
C1—C2—H2	119.8	C18—C21—C20	118.9 (4)
C2—C3—C4	118.6 (4)	C22—C21—C20	123.2 (5)
C2—C3—H3	120.7	C23—C22—C21	118.2 (4)
C4—C3—H3	120.7	C23—C22—H22	120.9
C5—C4—C3	117.9 (4)	C21—C22—H22	120.9
C5—C4—C7	119.7 (4)	C22—C23—C24	120.7 (5)
C3—C4—C7	122.3 (4)	C22—C23—H23	119.6
N1—C5—C4	122.5 (4)	C24—C23—H23	119.6
N1—C5—C6	118.0 (4)	N3—C24—C23	122.5 (4)
C4—C5—C6	119.5 (4)	N3—C24—H24	118.8
N2—C6—C9	122.2 (4)	C23—C24—H24	118.8
N2—C6—C5	117.1 (4)	N5—C25—N6	111.9 (10)
C9—C6—C5	120.7 (4)	N5—C25—S1	119.5 (9)
C8—C7—C4	120.4 (4)	N6—C25—S1	128.6 (9)
C8—C7—H7	119.8	O1—Co1—N3	92.49 (13)
C4—C7—H7	119.8	O1—Co1—N1	94.99 (13)
C7—C8—C9	121.2 (4)	N3—Co1—N1	166.10 (13)
C7—C8—H8	119.4	O1—Co1—N2	171.40 (13)
C9—C8—H8	119.4	N3—Co1—N2	94.03 (13)
C10—C9—C6	118.2 (4)	N1—Co1—N2	77.51 (13)
C10—C9—C8	123.4 (4)	O1—Co1—N4	85.18 (13)
C6—C9—C8	118.3 (4)	N3—Co1—N4	77.09 (13)
C11—C10—C9	118.9 (4)	N1—Co1—N4	91.87 (13)
C11—C10—H10	120.5	N2—Co1—N4	90.80 (12)
C9—C10—H10	120.5	O1—Co1—Cl1	89.78 (10)
C10—C11—C12	119.9 (4)	N3—Co1—Cl1	97.59 (9)
C10—C11—H11	120.0	N1—Co1—Cl1	94.14 (10)
C12—C11—H11	120.0	N2—Co1—Cl1	94.92 (9)
N2—C12—C11	122.7 (4)	N4—Co1—Cl1	172.47 (9)
N2—C12—H12	118.6	C1—N1—C5	117.9 (4)
C11—C12—H12	118.6	C1—N1—Co1	128.2 (3)
N4—C13—C14	122.7 (5)	C5—N1—Co1	113.8 (3)
N4—C13—H13	118.6	C12—N2—C6	117.9 (4)
C14—C13—H13	118.6	C12—N2—Co1	128.5 (3)
C15—C14—C13	119.9 (5)	C6—N2—Co1	113.6 (3)
C15—C14—H14	120.0	C24—N3—C18	117.9 (4)
C13—C14—H14	120.0	C24—N3—Co1	127.0 (3)
C14—C15—C16	119.7 (4)	C18—N3—Co1	115.0 (3)
C14—C15—H15	120.2	C13—N4—C17	118.2 (4)
C16—C15—H15	120.2	C13—N4—Co1	129.0 (3)
C17—C16—C15	117.3 (5)	C17—N4—Co1	112.6 (3)
C17—C16—C19	118.9 (5)	C25—N5—H5A	120.0
C15—C16—C19	123.8 (5)	C25—N5—H5B	120.0
N4—C17—C16	122.1 (4)	H5A—N5—H5B	120.0
N4—C17—C18	117.3 (4)	C25—N6—H6A	120.0
C16—C17—C18	120.6 (4)	C25—N6—H6B	120.0
N3—C18—C21	122.8 (4)	H6A—N6—H6B	120.0
N3—C18—C17	117.7 (4)	Co1—O1—H1A	109.5
C21—C18—C17	119.5 (4)	Co1—O1—H1B	112 (3)
C20—C19—C16	120.4 (5)	H1A—O1—H1B	129.2
C20—C19—H19	119.8

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1B···Cl2ⁱ	0.88 (5)	2.39 (5)	3.165 (4)	148 (4)
O1—H1A···Cl2ⁱⁱ	0.82	2.31	3.100 (3)	162
N6—H6A···Cl2	0.86	2.68	3.491 (12)	157
N5—H5B···S1ⁱⁱⁱ	0.86	2.48	3.328 (9)	168
N5—H5A···Cl2	0.86	2.60	3.441 (8)	165

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

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