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The crystal structure of the title compound, {[Co(N3)2(C7H6N2)2]·2H2O}n, consists of a di-μ-azido-bridged [Co(N3)2]n chain that propagates along the c axis of the orthorhombic unit cell, together with uncoordinated water molecules. Adjacent Co—N—Co—N rhombi are coplanar; the metal atom lies on a special position of 2/m site symmetry and the azide groups on special positions of site symmetry 2. The heterocycle lies on a mirror plane. The heterocycles are positioned above and below the rhombi so that the geometry of Co is an all-trans octahedral. The chain motif is consolidated by hydrogen bonding with the uncoordinated water molecules, which lie on mirror planes.
Supporting information
CCDC reference: 620750
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.006 Å
- R factor = 0.035
- wR factor = 0.095
- Data-to-parameter ratio = 11.4
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 2.60 Ratio
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N2
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Ra
O1W -H1O 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.850(10) ...... 3.00 su-Ra
N5 -H5N 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.86(3), Rep 0.850(10) ...... 3.00 su-Ra
N5 -H5N 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Ra
O1W -H1O 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.93(3), Rep 1.940(10) ...... 3.00 su-Ra
H5N -O1W 1.555 1.555
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
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: X-SEED (Barbour, 2001); software used to prepare material for publication: SHELXL97.
catena-Poly[[[bis(1
H-benzimidazole-
κN3)cobalt(II)]di-µ-azido] dihydrate]
top
Crystal data top
[Co(N3)2(C7H6N2)2]·2H2O | F(000) = 852 |
Mr = 415.30 | Dx = 1.557 Mg m−3 |
Orthorhombic, Ibam | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -I 2 2c | Cell parameters from 1412 reflections |
a = 17.112 (2) Å | θ = 1.8–26.4° |
b = 15.361 (2) Å | µ = 1.00 mm−1 |
c = 6.738 (1) Å | T = 295 K |
V = 1771.1 (4) Å3 | Column, pink |
Z = 4 | 0.16 × 0.12 × 0.08 mm |
Data collection top
Bruker SMART area-detector diffractometer | 993 independent reflections |
Radiation source: fine-focus sealed tube | 702 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.058 |
φ and ω scans | θmax = 26.4°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −18→21 |
Tmin = 0.856, Tmax = 0.924 | k = −9→19 |
4780 measured reflections | l = −8→8 |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.095 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.045P)2 + 1.8594P] where P = (Fo2 + 2Fc2)/3 |
993 reflections | (Δ/σ)max = 0.001 |
87 parameters | Δρmax = 0.26 e Å−3 |
2 restraints | Δρmin = −0.51 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.5000 | 0.5000 | 0.5000 | 0.0207 (2) | |
O1w | 0.3363 (3) | 0.0929 (3) | 0.5000 | 0.068 (1) | |
N1 | 0.4179 (2) | 0.5000 | 0.2500 | 0.027 (1) | |
N2 | 0.3487 (2) | 0.5000 | 0.2500 | 0.031 (1) | |
N3 | 0.2809 (2) | 0.5000 | 0.2500 | 0.068 (1) | |
N4 | 0.4944 (2) | 0.3636 (2) | 0.5000 | 0.026 (1) | |
N5 | 0.4388 (2) | 0.2331 (2) | 0.5000 | 0.036 (1) | |
C1 | 0.5530 (3) | 0.3008 (2) | 0.5000 | 0.028 (1) | |
C2 | 0.6341 (2) | 0.3085 (3) | 0.5000 | 0.037 (1) | |
C3 | 0.6771 (3) | 0.2323 (3) | 0.5000 | 0.051 (1) | |
C4 | 0.6416 (3) | 0.1499 (3) | 0.5000 | 0.054 (1) | |
C5 | 0.5622 (3) | 0.1417 (3) | 0.5000 | 0.049 (1) | |
C6 | 0.5183 (2) | 0.2173 (3) | 0.5000 | 0.033 (1) | |
C7 | 0.4283 (2) | 0.3202 (3) | 0.5000 | 0.032 (1) | |
H1o | 0.312 (2) | 0.080 (3) | 0.395 (4) | 0.11 (2)* | |
H5n | 0.403 (2) | 0.194 (2) | 0.5000 | 0.07 (2)* | |
H2 | 0.6583 | 0.3627 | 0.5000 | 0.044* | |
H3 | 0.7313 | 0.2357 | 0.5000 | 0.062* | |
H4 | 0.6726 | 0.1002 | 0.5000 | 0.065* | |
H5 | 0.5385 | 0.0872 | 0.5000 | 0.058* | |
H7 | 0.3794 | 0.3467 | 0.5000 | 0.039* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0206 (4) | 0.0200 (3) | 0.0215 (4) | −0.0009 (4) | 0.000 | 0.000 |
O1w | 0.081 (3) | 0.068 (3) | 0.055 (3) | −0.046 (2) | 0.000 | 0.000 |
N1 | 0.022 (2) | 0.033 (2) | 0.026 (2) | 0.000 | 0.000 | 0.003 (2) |
N2 | 0.030 (2) | 0.037 (2) | 0.025 (2) | 0.000 | 0.000 | −0.009 (2) |
N3 | 0.022 (2) | 0.110 (4) | 0.071 (3) | 0.000 | 0.000 | −0.041 (3) |
N4 | 0.028 (2) | 0.023 (2) | 0.027 (2) | −0.002 (2) | 0.000 | 0.000 |
N5 | 0.041 (2) | 0.031 (2) | 0.035 (2) | −0.012 (2) | 0.000 | 0.000 |
C1 | 0.043 (2) | 0.020 (2) | 0.020 (2) | 0.002 (2) | 0.000 | 0.000 |
C2 | 0.032 (2) | 0.035 (2) | 0.042 (3) | 0.006 (2) | 0.000 | 0.000 |
C3 | 0.047 (3) | 0.053 (3) | 0.054 (3) | 0.019 (3) | 0.000 | 0.000 |
C4 | 0.071 (4) | 0.034 (3) | 0.057 (3) | 0.027 (3) | 0.000 | 0.000 |
C5 | 0.077 (4) | 0.025 (2) | 0.044 (3) | 0.003 (2) | 0.000 | 0.000 |
C6 | 0.045 (3) | 0.026 (2) | 0.027 (2) | −0.004 (2) | 0.000 | 0.000 |
C7 | 0.036 (3) | 0.029 (2) | 0.032 (2) | −0.002 (2) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
Co1—N1 | 2.193 (2) | C1—C6 | 1.412 (5) |
Co1—N1i | 2.193 (2) | C2—C3 | 1.383 (6) |
Co1—N1ii | 2.193 (2) | C3—C4 | 1.403 (7) |
Co1—N1iii | 2.193 (2) | C4—C5 | 1.364 (7) |
Co1—N4 | 2.098 (3) | C5—C6 | 1.384 (6) |
Co1—N4ii | 2.098 (3) | O1w—H1o | 0.84 (1) |
N1—N2 | 1.185 (4) | N5—H5n | 0.85 (1) |
N2—N3 | 1.160 (4) | C2—H2 | 0.93 |
N4—C7 | 1.312 (5) | C3—H3 | 0.93 |
N4—C1 | 1.392 (5) | C4—H4 | 0.93 |
N5—C7 | 1.351 (5) | C5—H5 | 0.93 |
N5—C6 | 1.382 (6) | C7—H7 | 0.93 |
C1—C2 | 1.392 (6) | | |
| | | |
N1—Co1—N1i | 79.7 (1) | C5—C4—C3 | 121.0 (5) |
N1—Co1—N1ii | 180 | C4—C5—C6 | 117.5 (5) |
N1—Co1—N1iii | 100.4 (1) | N5—C6—C5 | 132.9 (4) |
N1—Co1—N4 | 88.3 (1) | N5—C6—C1 | 104.8 (4) |
N1—Co1—N4ii | 91.7 (1) | C5—C6—C1 | 122.3 (4) |
N4—Co1—N4ii | 180 | N4—C7—N5 | 112.8 (4) |
N2—N1—Co1 | 129.8 (1) | C7—N5—H5n | 127 (4) |
N2—N1—Co1iv | 129.8 (1) | C6—N5—H5n | 125 (4) |
Co1—N1—Co1iv | 100.4 (1) | C3—C2—H2 | 121.4 |
N3—N2—N1 | 180 | C1—C2—H2 | 121.4 |
C7—N4—C1 | 105.6 (3) | C2—C3—H3 | 118.9 |
C7—N4—Co1 | 123.1 (3) | C4—C3—H3 | 118.9 |
C1—N4—Co1 | 131.2 (3) | C5—C4—H4 | 119.5 |
C7—N5—C6 | 107.7 (4) | C3—C4—H4 | 119.5 |
N4—C1—C2 | 131.3 (4) | C4—C5—H5 | 121.2 |
N4—C1—C6 | 109.0 (4) | C6—C5—H5 | 121.2 |
C2—C1—C6 | 119.8 (4) | N4—C7—H7 | 123.6 |
C3—C2—C1 | 117.3 (4) | N5—C7—H7 | 123.6 |
C2—C3—C4 | 122.2 (5) | | |
| | | |
N4ii—Co1—N1—N2 | −92.03 (7) | N1—Co1—N4—C7 | −50.2 (1) |
N4—Co1—N1—N2 | 87.97 (7) | N1ii—Co1—N4—C7 | 129.8 (1) |
N1iii—Co1—N1—N2 | 0 | N1iii—Co1—N4—C7 | 50.2 (1) |
N1i—Co1—N1—N2 | 180.0 | N1i—Co1—N4—C7 | −129.8 (1) |
N4ii—Co1—N1—Co1iv | 87.97 (7) | N1—Co1—N4—C1 | 129.8 (1) |
N4—Co1—N1—Co1iv | −92.03 (7) | N1ii—Co1—N4—C1 | −50.2 (1) |
N1iii—Co1—N1—Co1iv | 180 | N1iii—Co1—N4—C1 | −129.8 (1) |
N1i—Co1—N1—Co1iv | 0 | N1i—Co1—N4—C1 | 50.2 (1) |
Symmetry codes: (i) −x+1, −y+1, z; (ii) −x+1, −y+1, −z+1; (iii) x, y, −z+1; (iv) x, −y+1, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N5—H5n···O1w | 0.85 (1) | 1.94 (1) | 2.777 (5) | 171 (5) |
O1w—H1o···N3v | 0.84 (1) | 2.24 (2) | 2.983 (4) | 148 (4) |
Symmetry code: (v) −x+1/2, −y+1/2, −z+1/2. |
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