Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807028073/xu2267sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807028073/xu2267Isup2.hkl |
CCDC reference: 654748
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.003 Å
- R factor = 0.022
- wR factor = 0.055
- Data-to-parameter ratio = 17.2
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - Cl1 .. 7.28 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - N2 .. 5.39 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - N3 .. 8.34 su
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 28.30 From the CIF: _reflns_number_total 4821 Count of symmetry unique reflns 2700 Completeness (_total/calc) 178.56% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 2121 Fraction of Friedel pairs measured 0.786 Are heavy atom types Z>Si present yes PLAT033_ALERT_2_G Flack Parameter Value Deviates 2 * su from zero. 0.03 PLAT794_ALERT_5_G Check Predicted Bond Valency for Co1 (2) 1.70 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 0 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 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For related structures, see: Zhong et al. (2006); Liu et al. (2004); Fu et al. (2006); Zhong et al. (2007).
A methanol solution (5 ml) of 1,10-phenanthroline (0.5 mmol) was added to an aqueous solution (10 ml) of cobalt dichloride (1.0 mmol) with stirring. The mixture was stirred continuously for 2 h at room temperature, and then filtered. Slow evaporation of the solution gave single crystals of the title compound.
H atoms were placed in calculated positions with C—H = 0.93 Å and refined in riding mode with Uiso(H) = 1.2Ueq(C).
Herein, we report a polymorph of the title complex. This complex was determined with monoclinic P 21/c space group by Zhong et al. (2006). The corresponding six-coordinate complex with water and carbonate anion have been reported (Liu et al., 2004; Fu et al., 2006; Zhong et al., 2007).
In the present structure, the CoII ion is located in a distorted octahedral geometry (Fig. 1) and coordinated by four N atoms from two 1,10-phenanthroline ligands and two Cl- anions. The average Co—Cl bond distance of 2.168 (2) Å and Co—N bond distance of 2.4138 (5) Å (Table 1) are somewhat shorter than those found in the reported monoclinic structure [average 2.326 (2) Å and 2.4435 (8) Å].
The molecules are linked into a two-dimensional framework (Fig. 2) via weak intermolecular C—H···Cl hydrogen bonding (Table 2). But in the reported monoclinic structure, the molecules are linked into a three-dimensional framework by C—H···Cl hydrogen bonding and the π-π stacking.
For related structures, see: Zhong et al. (2006); Liu et al. (2004); Fu et al. (2006); Zhong et al. (2007).
Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); 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, 1999); software used to prepare material for publication: SHELXTL.
Fig. 1. The molecular structure of the title compound, displacement ellipsoids are drawn at the 30% probability. | |
Fig. 2. The unit cell packing diagram. |
[CoCl2(C12H8N2)2] | F(000) = 996 |
Mr = 490.24 | Dx = 1.564 Mg m−3 |
Orthorhombic, Pna21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2c -2n | Cell parameters from 5332 reflections |
a = 21.2371 (14) Å | θ = 2.5–28.2° |
b = 7.7364 (5) Å | µ = 1.10 mm−1 |
c = 12.6733 (9) Å | T = 273 K |
V = 2082.2 (2) Å3 | Block, red |
Z = 4 | 0.43 × 0.21 × 0.13 mm |
Bruker CCD area-detector diffractometer | 4821 independent reflections |
Radiation source: fine-focus sealed tube | 4496 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.012 |
φ and ω scans | θmax = 28.3°, θmin = 2.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1990) | h = −8→28 |
Tmin = 0.649, Tmax = 0.870 | k = −9→10 |
8974 measured reflections | l = −15→16 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.022 | H-atom parameters constrained |
wR(F2) = 0.055 | w = 1/[σ2(Fo2) + (0.0247P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.003 |
4821 reflections | Δρmax = 0.20 e Å−3 |
280 parameters | Δρmin = −0.15 e Å−3 |
1 restraint | Absolute structure: Flack (1983), with 2121 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.028 (9) |
[CoCl2(C12H8N2)2] | V = 2082.2 (2) Å3 |
Mr = 490.24 | Z = 4 |
Orthorhombic, Pna21 | Mo Kα radiation |
a = 21.2371 (14) Å | µ = 1.10 mm−1 |
b = 7.7364 (5) Å | T = 273 K |
c = 12.6733 (9) Å | 0.43 × 0.21 × 0.13 mm |
Bruker CCD area-detector diffractometer | 4821 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1990) | 4496 reflections with I > 2σ(I) |
Tmin = 0.649, Tmax = 0.870 | Rint = 0.012 |
8974 measured reflections |
R[F2 > 2σ(F2)] = 0.022 | H-atom parameters constrained |
wR(F2) = 0.055 | Δρmax = 0.20 e Å−3 |
S = 1.02 | Δρmin = −0.15 e Å−3 |
4821 reflections | Absolute structure: Flack (1983), with 2121 Friedel pairs |
280 parameters | Absolute structure parameter: 0.028 (9) |
1 restraint |
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. |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.836180 (9) | 0.68890 (3) | 0.71778 (2) | 0.03249 (6) | |
Cl2 | 0.92419 (2) | 0.85110 (6) | 0.64460 (4) | 0.04752 (11) | |
Cl1 | 0.81796 (2) | 0.51066 (6) | 0.56653 (4) | 0.04825 (11) | |
C11 | 0.70676 (7) | 0.8328 (2) | 0.71241 (17) | 0.0357 (3) | |
N4 | 0.85782 (7) | 0.82299 (17) | 0.86690 (12) | 0.0360 (3) | |
N3 | 0.90037 (6) | 0.51456 (18) | 0.79647 (11) | 0.0344 (3) | |
N2 | 0.76570 (6) | 0.87682 (19) | 0.68047 (11) | 0.0369 (3) | |
C23 | 0.91076 (7) | 0.7581 (2) | 0.91265 (14) | 0.0344 (3) | |
C12 | 0.69965 (8) | 0.6750 (2) | 0.77073 (14) | 0.0365 (4) | |
N1 | 0.75226 (6) | 0.58222 (18) | 0.79065 (12) | 0.0379 (3) | |
C22 | 0.83464 (9) | 0.9694 (3) | 0.90508 (17) | 0.0466 (5) | |
H22 | 0.7976 | 1.0128 | 0.8763 | 0.056* | |
C19 | 0.94340 (9) | 0.8446 (2) | 0.99313 (14) | 0.0411 (4) | |
C7 | 0.65355 (9) | 0.9379 (3) | 0.69216 (16) | 0.0493 (5) | |
C10 | 0.77303 (10) | 1.0268 (2) | 0.63089 (17) | 0.0484 (5) | |
H10 | 0.8132 | 1.0587 | 0.6092 | 0.058* | |
C24 | 0.93201 (7) | 0.5905 (2) | 0.87816 (13) | 0.0335 (3) | |
C15 | 0.99882 (10) | 0.3426 (3) | 0.89786 (19) | 0.0527 (5) | |
H15 | 1.0315 | 0.2841 | 0.9312 | 0.063* | |
C4 | 0.63959 (9) | 0.6242 (3) | 0.80633 (17) | 0.0504 (5) | |
C6 | 0.59281 (9) | 0.8773 (3) | 0.7262 (2) | 0.0653 (6) | |
H6 | 0.5572 | 0.9427 | 0.7107 | 0.078* | |
C21 | 0.86354 (11) | 1.0611 (3) | 0.98676 (17) | 0.0550 (5) | |
H21 | 0.8452 | 1.1618 | 1.0126 | 0.066* | |
C9 | 0.72273 (13) | 1.1385 (3) | 0.61005 (19) | 0.0627 (6) | |
H9 | 0.7296 | 1.2427 | 0.5753 | 0.075* | |
C2 | 0.68866 (13) | 0.3801 (3) | 0.8858 (2) | 0.0669 (7) | |
H2 | 0.6863 | 0.2785 | 0.9248 | 0.080* | |
C13 | 0.91756 (8) | 0.3573 (2) | 0.76871 (15) | 0.0418 (4) | |
H13 | 0.8963 | 0.3043 | 0.7133 | 0.050* | |
C8 | 0.66375 (11) | 1.0931 (3) | 0.6412 (2) | 0.0639 (6) | |
H8 | 0.6301 | 1.1670 | 0.6282 | 0.077* | |
C20 | 0.91877 (11) | 1.0023 (3) | 1.02858 (16) | 0.0510 (5) | |
H20 | 0.9398 | 1.0660 | 1.0799 | 0.061* | |
C16 | 0.98266 (8) | 0.5114 (3) | 0.92949 (15) | 0.0418 (4) | |
C5 | 0.58623 (9) | 0.7304 (4) | 0.7792 (2) | 0.0667 (7) | |
H5 | 0.5461 | 0.6951 | 0.7993 | 0.080* | |
C14 | 0.96628 (10) | 0.2657 (3) | 0.81833 (16) | 0.0505 (5) | |
H14 | 0.9762 | 0.1539 | 0.7971 | 0.061* | |
C1 | 0.74660 (11) | 0.4377 (3) | 0.84612 (17) | 0.0537 (5) | |
H1 | 0.7824 | 0.3720 | 0.8592 | 0.064* | |
C3 | 0.63605 (12) | 0.4745 (3) | 0.8664 (2) | 0.0683 (7) | |
H3 | 0.5975 | 0.4389 | 0.8935 | 0.082* | |
C18 | 0.99832 (9) | 0.7653 (3) | 1.03787 (16) | 0.0500 (5) | |
H18 | 1.0221 | 0.8262 | 1.0870 | 0.060* | |
C17 | 1.01607 (9) | 0.6046 (3) | 1.01017 (17) | 0.0521 (5) | |
H17 | 1.0503 | 0.5532 | 1.0435 | 0.063* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.02694 (9) | 0.03490 (11) | 0.03564 (11) | −0.00102 (7) | −0.00133 (10) | 0.00495 (11) |
Cl2 | 0.0369 (2) | 0.0532 (3) | 0.0524 (3) | −0.01210 (18) | 0.0080 (2) | 0.0052 (2) |
Cl1 | 0.0511 (2) | 0.0495 (3) | 0.0442 (2) | −0.0074 (2) | −0.0059 (2) | −0.0020 (2) |
C11 | 0.0306 (7) | 0.0412 (8) | 0.0354 (8) | 0.0027 (6) | −0.0049 (8) | −0.0030 (8) |
N4 | 0.0356 (7) | 0.0363 (8) | 0.0363 (8) | 0.0000 (6) | −0.0002 (6) | −0.0007 (6) |
N3 | 0.0340 (7) | 0.0355 (7) | 0.0336 (7) | 0.0000 (5) | 0.0012 (6) | 0.0005 (6) |
N2 | 0.0342 (7) | 0.0376 (8) | 0.0390 (8) | −0.0024 (6) | −0.0049 (6) | 0.0078 (6) |
C23 | 0.0350 (8) | 0.0353 (9) | 0.0328 (9) | −0.0035 (7) | 0.0024 (7) | 0.0020 (7) |
C12 | 0.0314 (8) | 0.0449 (10) | 0.0333 (9) | −0.0058 (6) | 0.0013 (7) | −0.0038 (7) |
N1 | 0.0361 (7) | 0.0384 (8) | 0.0391 (8) | −0.0052 (6) | 0.0000 (6) | 0.0075 (6) |
C22 | 0.0472 (10) | 0.0444 (11) | 0.0483 (12) | 0.0092 (8) | 0.0040 (9) | −0.0037 (9) |
C19 | 0.0457 (10) | 0.0451 (10) | 0.0323 (9) | −0.0117 (8) | −0.0020 (7) | 0.0031 (8) |
C7 | 0.0411 (9) | 0.0571 (12) | 0.0497 (13) | 0.0139 (8) | −0.0093 (8) | −0.0115 (9) |
C10 | 0.0540 (11) | 0.0422 (10) | 0.0490 (12) | −0.0047 (8) | −0.0059 (9) | 0.0122 (9) |
C24 | 0.0293 (7) | 0.0391 (9) | 0.0321 (9) | −0.0019 (6) | 0.0001 (6) | 0.0030 (7) |
C15 | 0.0498 (11) | 0.0555 (12) | 0.0527 (13) | 0.0194 (9) | −0.0034 (10) | 0.0087 (10) |
C4 | 0.0380 (9) | 0.0663 (13) | 0.0469 (11) | −0.0157 (9) | 0.0096 (9) | −0.0109 (10) |
C6 | 0.0345 (9) | 0.0851 (15) | 0.0764 (16) | 0.0168 (9) | −0.0009 (12) | −0.0137 (17) |
C21 | 0.0740 (14) | 0.0408 (11) | 0.0501 (12) | 0.0028 (10) | 0.0056 (11) | −0.0091 (9) |
C9 | 0.0804 (16) | 0.0418 (11) | 0.0659 (15) | 0.0045 (11) | −0.0179 (12) | 0.0141 (10) |
C2 | 0.0836 (17) | 0.0579 (14) | 0.0592 (15) | −0.0278 (12) | 0.0075 (13) | 0.0191 (12) |
C13 | 0.0454 (10) | 0.0406 (9) | 0.0394 (10) | 0.0034 (7) | 0.0009 (8) | 0.0006 (8) |
C8 | 0.0679 (15) | 0.0544 (13) | 0.0695 (15) | 0.0256 (10) | −0.0208 (13) | 0.0012 (12) |
C20 | 0.0676 (13) | 0.0447 (11) | 0.0408 (11) | −0.0100 (9) | −0.0028 (9) | −0.0059 (8) |
C16 | 0.0364 (9) | 0.0499 (11) | 0.0391 (10) | 0.0018 (7) | −0.0022 (7) | 0.0040 (8) |
C5 | 0.0284 (10) | 0.0954 (18) | 0.0762 (17) | −0.0009 (10) | 0.0113 (9) | −0.0159 (15) |
C14 | 0.0606 (12) | 0.0438 (10) | 0.0471 (12) | 0.0153 (9) | 0.0029 (10) | 0.0015 (9) |
C1 | 0.0614 (12) | 0.0493 (11) | 0.0504 (12) | −0.0080 (10) | −0.0044 (10) | 0.0154 (9) |
C3 | 0.0603 (14) | 0.0819 (17) | 0.0627 (15) | −0.0322 (13) | 0.0154 (12) | 0.0036 (13) |
C18 | 0.0473 (10) | 0.0597 (12) | 0.0428 (11) | −0.0119 (9) | −0.0148 (9) | 0.0023 (9) |
C17 | 0.0403 (10) | 0.0709 (15) | 0.0450 (12) | −0.0009 (9) | −0.0140 (8) | 0.0051 (10) |
Co1—N1 | 2.1703 (14) | C24—C16 | 1.398 (2) |
Co1—N2 | 2.1395 (14) | C15—C14 | 1.359 (3) |
Co1—N3 | 2.1615 (14) | C15—C16 | 1.409 (3) |
Co1—N4 | 2.2043 (15) | C15—H15 | 0.9300 |
Co1—Cl1 | 2.3928 (6) | C4—C3 | 1.388 (3) |
Co1—Cl2 | 2.4348 (5) | C4—C5 | 1.441 (3) |
C11—N2 | 1.359 (2) | C6—C5 | 1.327 (4) |
C11—C7 | 1.416 (2) | C6—H6 | 0.9300 |
C11—C12 | 1.435 (2) | C21—C20 | 1.365 (3) |
N4—C22 | 1.326 (2) | C21—H21 | 0.9300 |
N4—C23 | 1.361 (2) | C9—C8 | 1.360 (4) |
N3—C13 | 1.318 (2) | C9—H9 | 0.9300 |
N3—C24 | 1.367 (2) | C2—C3 | 1.357 (4) |
N2—C10 | 1.328 (2) | C2—C1 | 1.402 (3) |
C23—C19 | 1.403 (2) | C2—H2 | 0.9300 |
C23—C24 | 1.441 (2) | C13—C14 | 1.403 (3) |
C12—N1 | 1.352 (2) | C13—H13 | 0.9300 |
C12—C4 | 1.409 (2) | C8—H8 | 0.9300 |
N1—C1 | 1.326 (2) | C20—H20 | 0.9300 |
C22—C21 | 1.397 (3) | C16—C17 | 1.438 (3) |
C22—H22 | 0.9300 | C5—H5 | 0.9300 |
C19—C20 | 1.401 (3) | C14—H14 | 0.9300 |
C19—C18 | 1.435 (3) | C1—H1 | 0.9300 |
C7—C8 | 1.380 (3) | C3—H3 | 0.9300 |
C7—C6 | 1.439 (3) | C18—C17 | 1.346 (3) |
C10—C9 | 1.400 (3) | C18—H18 | 0.9300 |
C10—H10 | 0.9300 | C17—H17 | 0.9300 |
N2—Co1—N3 | 165.28 (5) | C16—C24—C23 | 119.57 (15) |
N2—Co1—N1 | 77.17 (5) | C14—C15—C16 | 119.53 (18) |
N3—Co1—N1 | 94.83 (5) | C14—C15—H15 | 120.2 |
N2—Co1—N4 | 90.89 (5) | C16—C15—H15 | 120.2 |
N3—Co1—N4 | 76.51 (5) | C3—C4—C12 | 117.2 (2) |
N1—Co1—N4 | 89.16 (6) | C3—C4—C5 | 124.3 (2) |
N2—Co1—Cl1 | 95.82 (4) | C12—C4—C5 | 118.4 (2) |
N3—Co1—Cl1 | 96.43 (4) | C5—C6—C7 | 121.67 (18) |
N1—Co1—Cl1 | 89.37 (4) | C5—C6—H6 | 119.2 |
N4—Co1—Cl1 | 172.63 (4) | C7—C6—H6 | 119.2 |
N2—Co1—Cl2 | 95.89 (4) | C20—C21—C22 | 119.74 (19) |
N3—Co1—Cl2 | 90.76 (4) | C20—C21—H21 | 120.1 |
N1—Co1—Cl2 | 171.28 (4) | C22—C21—H21 | 120.1 |
N4—Co1—Cl2 | 85.64 (4) | C8—C9—C10 | 119.2 (2) |
Cl1—Co1—Cl2 | 96.66 (2) | C8—C9—H9 | 120.4 |
N2—C11—C7 | 122.52 (17) | C10—C9—H9 | 120.4 |
N2—C11—C12 | 117.60 (14) | C3—C2—C1 | 119.1 (2) |
C7—C11—C12 | 119.86 (16) | C3—C2—H2 | 120.4 |
C22—N4—C23 | 117.78 (16) | C1—C2—H2 | 120.4 |
C22—N4—Co1 | 129.59 (13) | N3—C13—C14 | 123.42 (18) |
C23—N4—Co1 | 111.34 (11) | N3—C13—H13 | 118.3 |
C13—N3—C24 | 117.56 (15) | C14—C13—H13 | 118.3 |
C13—N3—Co1 | 128.87 (13) | C9—C8—C7 | 120.35 (19) |
C24—N3—Co1 | 113.04 (11) | C9—C8—H8 | 119.8 |
C10—N2—C11 | 117.87 (15) | C7—C8—H8 | 119.8 |
C10—N2—Co1 | 128.02 (12) | C21—C20—C19 | 119.10 (18) |
C11—N2—Co1 | 114.11 (11) | C21—C20—H20 | 120.4 |
N4—C23—C19 | 122.83 (15) | C19—C20—H20 | 120.4 |
N4—C23—C24 | 117.47 (15) | C24—C16—C15 | 117.42 (18) |
C19—C23—C24 | 119.67 (15) | C24—C16—C17 | 119.43 (18) |
N1—C12—C4 | 122.70 (17) | C15—C16—C17 | 123.14 (19) |
N1—C12—C11 | 117.45 (14) | C6—C5—C4 | 121.75 (18) |
C4—C12—C11 | 119.85 (17) | C6—C5—H5 | 119.1 |
C1—N1—C12 | 118.15 (16) | C4—C5—H5 | 119.1 |
C1—N1—Co1 | 128.36 (13) | C15—C14—C13 | 119.11 (19) |
C12—N1—Co1 | 113.41 (11) | C15—C14—H14 | 120.4 |
N4—C22—C21 | 122.74 (19) | C13—C14—H14 | 120.4 |
N4—C22—H22 | 118.6 | N1—C1—C2 | 122.5 (2) |
C21—C22—H22 | 118.6 | N1—C1—H1 | 118.7 |
C20—C19—C23 | 117.63 (17) | C2—C1—H1 | 118.7 |
C20—C19—C18 | 123.31 (18) | C2—C3—C4 | 120.2 (2) |
C23—C19—C18 | 119.01 (17) | C2—C3—H3 | 119.9 |
C8—C7—C11 | 117.33 (18) | C4—C3—H3 | 119.9 |
C8—C7—C6 | 124.36 (19) | C17—C18—C19 | 121.32 (17) |
C11—C7—C6 | 118.3 (2) | C17—C18—H18 | 119.3 |
N2—C10—C9 | 122.6 (2) | C19—C18—H18 | 119.3 |
N2—C10—H10 | 118.7 | C18—C17—C16 | 120.67 (18) |
C9—C10—H10 | 118.7 | C18—C17—H17 | 119.7 |
N3—C24—C16 | 122.87 (16) | C16—C17—H17 | 119.7 |
N3—C24—C23 | 117.55 (14) |
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H2···Cl1i | 0.93 | 2.74 | 3.665 (2) | 171 |
C9—H9···Cl1ii | 0.93 | 2.80 | 3.561 (3) | 140 |
Symmetry codes: (i) −x+3/2, y−1/2, z+1/2; (ii) x, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | [CoCl2(C12H8N2)2] |
Mr | 490.24 |
Crystal system, space group | Orthorhombic, Pna21 |
Temperature (K) | 273 |
a, b, c (Å) | 21.2371 (14), 7.7364 (5), 12.6733 (9) |
V (Å3) | 2082.2 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.10 |
Crystal size (mm) | 0.43 × 0.21 × 0.13 |
Data collection | |
Diffractometer | Bruker CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1990) |
Tmin, Tmax | 0.649, 0.870 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8974, 4821, 4496 |
Rint | 0.012 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.022, 0.055, 1.02 |
No. of reflections | 4821 |
No. of parameters | 280 |
No. of restraints | 1 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.20, −0.15 |
Absolute structure | Flack (1983), with 2121 Friedel pairs |
Absolute structure parameter | 0.028 (9) |
Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1999), SHELXTL.
Co1—N1 | 2.1703 (14) | Co1—N4 | 2.2043 (15) |
Co1—N2 | 2.1395 (14) | Co1—Cl1 | 2.3928 (6) |
Co1—N3 | 2.1615 (14) | Co1—Cl2 | 2.4348 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H2···Cl1i | 0.93 | 2.74 | 3.665 (2) | 171 |
C9—H9···Cl1ii | 0.93 | 2.80 | 3.561 (3) | 140 |
Symmetry codes: (i) −x+3/2, y−1/2, z+1/2; (ii) x, y+1, z. |
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Herein, we report a polymorph of the title complex. This complex was determined with monoclinic P 21/c space group by Zhong et al. (2006). The corresponding six-coordinate complex with water and carbonate anion have been reported (Liu et al., 2004; Fu et al., 2006; Zhong et al., 2007).
In the present structure, the CoII ion is located in a distorted octahedral geometry (Fig. 1) and coordinated by four N atoms from two 1,10-phenanthroline ligands and two Cl- anions. The average Co—Cl bond distance of 2.168 (2) Å and Co—N bond distance of 2.4138 (5) Å (Table 1) are somewhat shorter than those found in the reported monoclinic structure [average 2.326 (2) Å and 2.4435 (8) Å].
The molecules are linked into a two-dimensional framework (Fig. 2) via weak intermolecular C—H···Cl hydrogen bonding (Table 2). But in the reported monoclinic structure, the molecules are linked into a three-dimensional framework by C—H···Cl hydrogen bonding and the π-π stacking.