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In the title complex, [Co(C3H4N2)4(H2O)2](C8H4O4), the octahedrally coordinated Co atom lies on a center of symmetry and is bonded by four imidazole and two water molecules. The terephthalate anion also lies on a center of symmetry but does not coordinate to the Co atom. Hydrogen bonding leads to a three-dimensional structure.
Supporting information
CCDC reference: 251604
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.044
- wR factor = 0.133
- Data-to-parameter ratio = 9.9
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98
PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.91
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 8
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.43
PLAT738_ALERT_1_C D-H..A Calc 175(2), Rep 175(5) ...... 2.50 su-Rat
N2 -H2A -O1 1.555 1.555 1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.23 Ratio
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
7 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
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
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1994); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1994); software used to prepare material for publication: SHELXS97.
Diaquatetrakis(1
H-imidazole-
κN3)cobalt(II) terephthalate
top
Crystal data top
[Co(C3H4N2)4(H2O)2](C8H4O4) | F(000) = 1100 |
Mr = 531.40 | Dx = 1.487 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 82 reflections |
a = 22.2830 (7) Å | θ = 2.1–25.1° |
b = 7.6818 (3) Å | µ = 0.78 mm−1 |
c = 16.1127 (3) Å | T = 293 K |
β = 120.630 (2)° | Prism, purple |
V = 2373.25 (12) Å3 | 0.32 × 0.21 × 0.06 mm |
Z = 4 | |
Data collection top
Siemens SMART CCD diffractometer | 2071 independent reflections |
Radiation source: fine-focus sealed tube | 1731 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
ω scans | θmax = 25.1°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −12→25 |
Tmin = 0.736, Tmax = 0.950 | k = −8→9 |
3377 measured reflections | l = −19→17 |
Refinement top
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)] = 0.044 | All H-atom parameters refined |
wR(F2) = 0.133 | w = 1/[σ2(Fo2) + (0.0643P)2 + 7.3403P] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | (Δ/σ)max < 0.001 |
2071 reflections | Δρmax = 0.40 e Å−3 |
209 parameters | Δρmin = −0.34 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0019 (4) |
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 | Uiso*/Ueq | |
Co1 | 0.2500 | 0.2500 | 0.0000 | 0.0271 (3) | |
O1 | 0.43317 (13) | 0.2038 (4) | 0.48940 (16) | 0.0451 (7) | |
O2 | 0.34304 (11) | 0.2279 (3) | 0.51061 (16) | 0.0342 (6) | |
O3 | 0.26104 (14) | −0.0168 (3) | 0.04451 (18) | 0.0355 (6) | |
H3B | 0.290 (3) | −0.079 (6) | 0.035 (3) | 0.061 (14)* | |
H3A | 0.225 (3) | −0.067 (6) | 0.025 (3) | 0.053 (14)* | |
N1 | 0.28202 (14) | 0.3254 (4) | 0.14525 (19) | 0.0340 (7) | |
N2 | 0.33941 (17) | 0.3117 (5) | 0.3035 (2) | 0.0439 (8) | |
H2A | 0.367 (3) | 0.273 (6) | 0.361 (4) | 0.059 (14)* | |
N3 | 0.35697 (14) | 0.2638 (4) | 0.0368 (2) | 0.0322 (6) | |
N4 | 0.45348 (17) | 0.2477 (4) | 0.0325 (3) | 0.0432 (8) | |
H4A | 0.482 (3) | 0.219 (6) | 0.021 (3) | 0.054 (14)* | |
C1 | 0.40699 (17) | 0.2092 (5) | 0.5423 (2) | 0.0317 (8) | |
C2 | 0.45557 (17) | 0.1930 (5) | 0.6499 (2) | 0.0322 (7) | |
C3 | 0.52687 (19) | 0.1916 (6) | 0.6903 (3) | 0.0452 (10) | |
H3 | 0.546 (2) | 0.187 (6) | 0.646 (3) | 0.059 (12)* | |
C4 | 0.42895 (19) | 0.1923 (6) | 0.7113 (3) | 0.0429 (9) | |
H4 | 0.383 (2) | 0.197 (6) | 0.686 (3) | 0.057 (13)* | |
C5 | 0.2747 (2) | 0.4798 (6) | 0.1818 (3) | 0.0463 (10) | |
H5 | 0.247 (2) | 0.568 (6) | 0.138 (3) | 0.056 (12)* | |
C6 | 0.3097 (2) | 0.4710 (6) | 0.2788 (3) | 0.0535 (11) | |
H6 | 0.316 (3) | 0.557 (7) | 0.327 (4) | 0.072 (14)* | |
C7 | 0.3216 (2) | 0.2291 (5) | 0.2216 (3) | 0.0385 (9) | |
H7 | 0.3335 (18) | 0.113 (5) | 0.222 (3) | 0.035 (10)* | |
C8 | 0.4080 (2) | 0.3610 (6) | 0.1101 (3) | 0.0513 (11) | |
H8 | 0.402 (2) | 0.421 (5) | 0.152 (3) | 0.045 (11)* | |
C9 | 0.4675 (2) | 0.3507 (7) | 0.1081 (3) | 0.0586 (12) | |
H9 | 0.509 (3) | 0.392 (6) | 0.147 (3) | 0.065 (14)* | |
C10 | 0.38695 (19) | 0.1997 (5) | −0.0085 (3) | 0.0397 (8) | |
H10 | 0.364 (2) | 0.127 (6) | −0.066 (3) | 0.057 (12)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0230 (4) | 0.0364 (4) | 0.0225 (4) | 0.0010 (2) | 0.0120 (3) | −0.0007 (2) |
O1 | 0.0288 (12) | 0.083 (2) | 0.0247 (12) | 0.0018 (13) | 0.0148 (10) | 0.0070 (12) |
O2 | 0.0214 (12) | 0.0497 (15) | 0.0294 (12) | −0.0003 (10) | 0.0115 (10) | 0.0032 (10) |
O3 | 0.0301 (14) | 0.0372 (14) | 0.0404 (14) | 0.0009 (12) | 0.0188 (12) | 0.0000 (11) |
N1 | 0.0310 (15) | 0.0455 (17) | 0.0256 (14) | 0.0044 (13) | 0.0145 (12) | −0.0005 (13) |
N2 | 0.0386 (17) | 0.065 (2) | 0.0209 (15) | −0.0003 (16) | 0.0103 (13) | 0.0010 (15) |
N3 | 0.0252 (14) | 0.0396 (16) | 0.0310 (14) | −0.0001 (11) | 0.0136 (12) | −0.0012 (12) |
N4 | 0.0295 (17) | 0.061 (2) | 0.0484 (19) | 0.0017 (14) | 0.0264 (15) | −0.0011 (16) |
C1 | 0.0277 (17) | 0.043 (2) | 0.0223 (16) | −0.0014 (14) | 0.0114 (14) | 0.0023 (13) |
C2 | 0.0277 (17) | 0.0433 (19) | 0.0237 (16) | 0.0029 (14) | 0.0117 (14) | 0.0025 (14) |
C3 | 0.0325 (19) | 0.080 (3) | 0.0260 (17) | 0.0054 (19) | 0.0169 (15) | 0.0044 (18) |
C4 | 0.0217 (17) | 0.076 (3) | 0.0303 (18) | −0.0046 (18) | 0.0125 (15) | −0.0024 (18) |
C5 | 0.050 (2) | 0.053 (2) | 0.0336 (19) | 0.0073 (19) | 0.0198 (18) | −0.0045 (18) |
C6 | 0.057 (3) | 0.066 (3) | 0.0323 (19) | 0.005 (2) | 0.0186 (18) | −0.011 (2) |
C7 | 0.0354 (19) | 0.050 (2) | 0.0262 (17) | 0.0057 (17) | 0.0131 (15) | 0.0026 (16) |
C8 | 0.040 (2) | 0.064 (3) | 0.055 (2) | −0.0109 (19) | 0.029 (2) | −0.023 (2) |
C9 | 0.031 (2) | 0.079 (3) | 0.062 (3) | −0.012 (2) | 0.022 (2) | −0.021 (2) |
C10 | 0.0298 (18) | 0.055 (2) | 0.0370 (19) | 0.0003 (17) | 0.0192 (16) | −0.0026 (17) |
Geometric parameters (Å, º) top
Co1—O3 | 2.144 (3) | N4—C10 | 1.331 (5) |
Co1—O3i | 2.144 (3) | N4—C9 | 1.349 (6) |
Co1—N3i | 2.146 (3) | N4—O1iv | 2.743 (4) |
Co1—N3 | 2.146 (3) | N4—H4A | 0.79 (5) |
Co1—N1 | 2.149 (3) | C1—C2 | 1.511 (4) |
Co1—N1i | 2.149 (3) | C2—C3 | 1.376 (5) |
O1—C1 | 1.254 (4) | C2—C4 | 1.389 (5) |
O1—N2 | 2.765 (4) | C3—C4v | 1.375 (5) |
O2—C1 | 1.253 (4) | C3—H3 | 1.00 (5) |
O3—O2ii | 2.699 (3) | C4—C3v | 1.375 (5) |
O3—O2iii | 2.813 (4) | C4—H4 | 0.89 (5) |
O3—H3B | 0.88 (5) | C5—C6 | 1.346 (5) |
O3—H3A | 0.80 (5) | C5—H5 | 0.95 (5) |
N1—C7 | 1.316 (5) | C6—H6 | 0.97 (5) |
N1—C5 | 1.370 (5) | C7—H7 | 0.93 (4) |
N2—C7 | 1.330 (5) | C8—C9 | 1.345 (6) |
N2—C6 | 1.351 (6) | C8—H8 | 0.88 (4) |
N2—H2A | 0.86 (5) | C9—H9 | 0.87 (5) |
N3—C10 | 1.311 (5) | C10—H10 | 0.97 (5) |
N3—C8 | 1.371 (5) | | |
| | | |
O3—Co1—N3i | 88.11 (11) | C10—N4—O1iv | 140.1 (3) |
O3i—Co1—N3i | 91.89 (11) | C9—N4—O1iv | 112.5 (3) |
O3—Co1—N3 | 91.89 (11) | C10—N4—H4A | 130 (3) |
O3i—Co1—N3 | 88.11 (11) | C9—N4—H4A | 123 (3) |
O3—Co1—N1 | 88.59 (11) | O2—C1—O1 | 123.6 (3) |
O3i—Co1—N1 | 91.41 (11) | O2—C1—C2 | 118.5 (3) |
N3i—Co1—N1 | 91.13 (10) | O1—C1—C2 | 117.9 (3) |
N3—Co1—N1 | 88.87 (10) | C3—C2—C4 | 118.2 (3) |
O3—Co1—N1i | 91.41 (11) | C3—C2—C1 | 121.5 (3) |
O3i—Co1—N1i | 88.59 (11) | C4—C2—C1 | 120.1 (3) |
N3i—Co1—N1i | 88.87 (10) | C4v—C3—C2 | 121.4 (3) |
N3—Co1—N1i | 91.13 (10) | C4v—C3—H3 | 120 (3) |
C1—O1—H2A | 110.8 (15) | C2—C3—H3 | 118 (3) |
C1—O1—N2 | 111.7 (2) | C3v—C4—C2 | 120.4 (3) |
Co1—O3—O2ii | 118.74 (12) | C3v—C4—H4 | 121 (3) |
Co1—O3—O2iii | 128.70 (12) | C2—C4—H4 | 119 (3) |
O2ii—O3—O2iii | 92.95 (10) | C6—C5—N1 | 109.3 (4) |
Co1—O3—H3B | 116 (3) | C6—C5—H5 | 133 (3) |
O2iii—O3—H3B | 97 (3) | N1—C5—H5 | 118 (3) |
Co1—O3—H3A | 114 (3) | C5—C6—N2 | 107.1 (4) |
O2ii—O3—H3A | 106 (3) | C5—C6—H6 | 131 (3) |
H3B—O3—H3A | 111 (5) | N2—C6—H6 | 122 (3) |
C7—N1—C5 | 104.7 (3) | N1—C7—N2 | 112.3 (4) |
C7—N1—Co1 | 124.0 (3) | N1—C7—H7 | 126 (2) |
C5—N1—Co1 | 130.9 (2) | N2—C7—H7 | 121 (2) |
C7—N2—C6 | 106.6 (3) | C9—C8—N3 | 110.0 (4) |
C7—N2—O1 | 127.6 (3) | C9—C8—H8 | 126 (3) |
C6—N2—O1 | 125.3 (3) | N3—C8—H8 | 124 (3) |
C7—N2—H2A | 126 (3) | C8—C9—N4 | 106.2 (4) |
C6—N2—H2A | 127 (3) | C8—C9—H9 | 131 (3) |
C10—N3—C8 | 104.5 (3) | N4—C9—H9 | 123 (3) |
C10—N3—Co1 | 129.6 (2) | N3—C10—N4 | 112.0 (4) |
C8—N3—Co1 | 125.6 (2) | N3—C10—H10 | 125 (3) |
C10—N4—C9 | 107.3 (3) | N4—C10—H10 | 123 (3) |
| | | |
N3i—Co1—O3—O2ii | 143.19 (14) | C1—C2—C3—C4v | 174.2 (4) |
N1i—Co1—O3—O2ii | 54.37 (14) | C3—C2—C4—C3v | 0.5 (6) |
N3—Co1—O3—O2iii | −157.78 (15) | C1—C2—C4—C3v | −174.8 (4) |
N1—Co1—O3—O2iii | 113.40 (16) | C7—N1—C5—C6 | −0.4 (5) |
O3i—Co1—N1—C7 | −153.8 (3) | Co1—N1—C5—C6 | −173.4 (3) |
N3i—Co1—N1—C7 | 114.3 (3) | N1—C5—C6—N2 | 0.3 (5) |
O3—Co1—N1—C5 | −162.0 (3) | C7—N2—C6—C5 | −0.1 (5) |
N3—Co1—N1—C5 | 106.1 (3) | O1—N2—C6—C5 | 172.2 (3) |
C1—O1—N2—C7 | −128.5 (4) | C5—N1—C7—N2 | 0.4 (4) |
C1—O1—N2—C6 | 60.8 (4) | Co1—N1—C7—N2 | 174.0 (2) |
O3—Co1—N3—C10 | 75.1 (3) | C6—N2—C7—N1 | −0.2 (5) |
O3i—Co1—N3—C10 | −104.9 (3) | O1—N2—C7—N1 | −172.3 (2) |
N1—Co1—N3—C10 | 163.7 (3) | C10—N3—C8—C9 | −1.0 (5) |
O3i—Co1—N3—C8 | 67.6 (3) | Co1—N3—C8—C9 | −175.0 (3) |
N1i—Co1—N3—C8 | 156.2 (3) | N3—C8—C9—N4 | 0.5 (6) |
N2—O1—C1—C2 | −166.7 (3) | C10—N4—C9—C8 | 0.2 (5) |
O2—C1—C2—C3 | −172.7 (4) | O1iv—N4—C9—C8 | 179.9 (3) |
O1—C1—C2—C3 | 7.1 (6) | C8—N3—C10—N4 | 1.1 (5) |
O2—C1—C2—C4 | 2.4 (5) | Co1—N3—C10—N4 | 174.8 (2) |
O1—C1—C2—C4 | −177.8 (4) | C9—N4—C10—N3 | −0.8 (5) |
C4—C2—C3—C4v | −1.0 (6) | O1iv—N4—C10—N3 | 179.5 (3) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z; (ii) x, −y, z−1/2; (iii) −x+1/2, y−1/2, −z+1/2; (iv) −x+1, y, −z+1/2; (v) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2A···O1 | 0.86 (5) | 1.91 (5) | 2.765 (4) | 175 (5) |
N4—H4A···O1iv | 0.79 (5) | 1.97 (5) | 2.743 (4) | 165 (5) |
O3—H3B···O2ii | 0.88 (5) | 1.82 (5) | 2.699 (3) | 174 (4) |
O3—H3A···O2iii | 0.80 (5) | 2.05 (5) | 2.813 (4) | 159 (5) |
Symmetry codes: (ii) x, −y, z−1/2; (iii) −x+1/2, y−1/2, −z+1/2; (iv) −x+1, y, −z+1/2. |
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