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The title compound, [Co2(CH3O)2(C4H5N3)4](BF4)2, consists of a discrete dimeric CoII complex. The asymmetric unit consists of one pyrimidin-2-amine ligand, which occupies a general position, and one methanolate group, as well as one CoII cation and one tetrafluoroborate anion, which are located in special positions. The CoII cation lies on a twofold rotation axis, whereas the tetrafluoroborate anion and the methanolate group lie on mirror planes. The N atoms of the pyrimidin-2-amine ligand are involved in intermolecular hydrogen bonding. From this arrangement, large channels are formed, which elongate in the direction of the crystallographic c axis.
Supporting information
CCDC reference: 608602
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- R factor = 0.064
- wR factor = 0.207
- Data-to-parameter ratio = 23.3
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - O1 .. 5.35 su
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for B1
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.23
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10
PLAT602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure !
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 3
N1 -CO1 -O1 -C5 -164.40 0.90 2.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 6
N1 -CO1 -O1 -CO1 52.10 1.10 2.555 1.555 1.555 5.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 7
O1 -CO1 -N1 -C1 -116.10 1.00 5.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 11
O1 -CO1 -N1 -C4 66.40 1.10 5.555 1.555 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 1.365(14), Rep 1.365(6) ...... 2.33 su-Rat
B1 -F2 1.555 1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.20 Ratio
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
14 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
4 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
1 ALERT type 3 Indicator that the structure quality may be low
7 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Di-µ
2-methanolato-bis[tetrakis(pyrimidin-2-amine-
κN1)cobalt(II)]
bis(tetrafluoroborate)
top
Crystal data top
[Co2(CH3O)2(C4H5N3)4](BF4)2 | F(000) = 740 |
Mr = 733.99 | Dx = 1.140 Mg m−3 |
Monoclinic, C2/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2y | Cell parameters from 1625 reflections |
a = 16.338 (6) Å | θ = 2.9–26.4° |
b = 14.704 (2) Å | µ = 0.84 mm−1 |
c = 12.040 (4) Å | T = 293 K |
β = 132.34 (1)° | Block, red |
V = 2138.0 (11) Å3 | 0.32 × 0.28 × 0.20 mm |
Z = 2 | |
Data collection top
Bruker APEX area-detector diffractometer | 2541 independent reflections |
Radiation source: fine-focus sealed tube | 2010 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
φ and ω scans | θmax = 27.5°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = 0→21 |
Tmin = 0.775, Tmax = 0.850 | k = 0→19 |
2626 measured reflections | l = −15→11 |
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)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.207 | H-atom parameters constrained |
S = 1.11 | w = 1/[σ2(Fo2) + (0.1252P)2 + 2.7158P] where P = (Fo2 + 2Fc2)/3 |
2541 reflections | (Δ/σ)max = 0.003 |
109 parameters | Δρmax = 0.86 e Å−3 |
0 restraints | Δρmin = −0.60 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 | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.0000 | 0.10015 (4) | 0.0000 | 0.0410 (3) | |
O1 | 0.0973 (3) | 0.0000 | 0.1198 (4) | 0.0508 (9) | |
C5 | 0.2121 (5) | 0.0000 | 0.2001 (8) | 0.0722 (18) | |
H5A | 0.2415 | −0.0600 | 0.2379 | 0.108* | 0.50 |
H5B | 0.2495 | 0.0419 | 0.2825 | 0.108* | 0.50 |
H5C | 0.2230 | 0.0180 | 0.1342 | 0.108* | 0.50 |
N1 | 0.1166 (3) | 0.1969 (2) | 0.1248 (4) | 0.0580 (9) | |
N2 | 0.1491 (4) | 0.1670 (3) | 0.3384 (5) | 0.0886 (16) | |
H2A | 0.0904 | 0.1295 | 0.2879 | 0.133* | |
H2B | 0.1843 | 0.1797 | 0.4346 | 0.133* | |
N3 | 0.2423 (4) | 0.2852 (3) | 0.3459 (5) | 0.0798 (13) | |
C1 | 0.1687 (4) | 0.2155 (3) | 0.2684 (5) | 0.0615 (11) | |
C2 | 0.2640 (5) | 0.3337 (4) | 0.2768 (6) | 0.0862 (17) | |
H2 | 0.3130 | 0.3823 | 0.3280 | 0.103* | |
C3 | 0.2181 (6) | 0.3164 (4) | 0.1337 (7) | 0.0940 (19) | |
H3 | 0.2383 | 0.3493 | 0.0895 | 0.113* | |
C4 | 0.1409 (5) | 0.2485 (3) | 0.0580 (6) | 0.0744 (14) | |
H4 | 0.1042 | 0.2378 | −0.0421 | 0.089* | |
B1 | 0.0628 (4) | 0.0000 | 0.7771 (5) | 0.0281 (9) | |
F1 | −0.0454 (5) | 0.0000 | 0.6403 (6) | 0.1115 (17) | |
F2 | 0.1392 (6) | 0.0000 | 0.7634 (9) | 0.121 (2) | |
F3 | 0.0765 (3) | 0.0786 (2) | 0.8565 (4) | 0.0821 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0441 (4) | 0.0311 (4) | 0.0335 (4) | 0.000 | 0.0203 (3) | 0.000 |
O1 | 0.0439 (19) | 0.047 (2) | 0.0447 (19) | 0.000 | 0.0230 (16) | 0.000 |
C5 | 0.050 (3) | 0.069 (4) | 0.070 (4) | 0.000 | 0.030 (3) | 0.000 |
N1 | 0.069 (2) | 0.0437 (17) | 0.0520 (18) | −0.0099 (16) | 0.0369 (17) | −0.0050 (14) |
N2 | 0.110 (3) | 0.086 (3) | 0.063 (2) | −0.057 (3) | 0.056 (3) | −0.025 (2) |
N3 | 0.096 (3) | 0.072 (3) | 0.066 (2) | −0.041 (2) | 0.053 (2) | −0.024 (2) |
C1 | 0.070 (3) | 0.052 (2) | 0.055 (2) | −0.019 (2) | 0.039 (2) | −0.0125 (19) |
C2 | 0.103 (4) | 0.072 (3) | 0.082 (3) | −0.041 (3) | 0.062 (3) | −0.017 (3) |
C3 | 0.132 (5) | 0.080 (4) | 0.092 (4) | −0.045 (4) | 0.085 (4) | −0.017 (3) |
C4 | 0.098 (4) | 0.057 (3) | 0.066 (3) | −0.019 (3) | 0.054 (3) | −0.004 (2) |
B1 | 0.042 (2) | 0.0159 (18) | 0.044 (2) | 0.000 | 0.036 (2) | 0.000 |
F1 | 0.114 (4) | 0.097 (4) | 0.094 (3) | 0.000 | 0.058 (3) | 0.000 |
F2 | 0.174 (6) | 0.071 (3) | 0.229 (7) | 0.000 | 0.181 (6) | 0.000 |
F3 | 0.101 (2) | 0.0579 (16) | 0.103 (2) | 0.0020 (15) | 0.075 (2) | −0.0080 (15) |
Geometric parameters (Å, º) top
Co1—O1i | 1.920 (2) | N2—H2A | 0.8999 |
Co1—O1 | 1.920 (2) | N2—H2B | 0.9000 |
Co1—N1 | 2.014 (3) | N3—C2 | 1.313 (7) |
Co1—N1ii | 2.014 (3) | N3—C1 | 1.362 (6) |
Co1—Co1i | 2.9452 (13) | C2—C3 | 1.362 (8) |
O1—C5 | 1.418 (8) | C2—H2 | 0.9300 |
O1—Co1i | 1.920 (2) | C3—C4 | 1.367 (7) |
C5—H5A | 0.9600 | C3—H3 | 0.9300 |
C5—H5B | 0.9600 | C4—H4 | 0.9300 |
C5—H5C | 0.9600 | B1—F2 | 1.365 (6) |
N1—C1 | 1.344 (5) | B1—F1 | 1.384 (7) |
N1—C4 | 1.345 (6) | B1—F3 | 1.419 (4) |
N2—C1 | 1.297 (6) | B1—F3iii | 1.419 (4) |
| | | |
O1i—Co1—O1 | 79.86 (17) | C1—N2—H2A | 121.0 |
O1i—Co1—N1 | 172.23 (15) | C1—N2—H2B | 120.0 |
O1—Co1—N1 | 95.33 (14) | H2A—N2—H2B | 117.5 |
O1i—Co1—N1ii | 95.33 (14) | C2—N3—C1 | 117.7 (4) |
O1—Co1—N1ii | 172.23 (15) | N2—C1—N1 | 120.3 (4) |
N1—Co1—N1ii | 90.1 (2) | N2—C1—N3 | 117.2 (4) |
O1i—Co1—Co1i | 39.93 (8) | N1—C1—N3 | 122.5 (4) |
O1—Co1—Co1i | 39.93 (8) | N3—C2—C3 | 123.1 (5) |
N1—Co1—Co1i | 134.96 (11) | N3—C2—H2 | 118.5 |
N1ii—Co1—Co1i | 134.96 (11) | C3—C2—H2 | 118.5 |
C5—O1—Co1i | 123.92 (19) | C2—C3—C4 | 117.1 (5) |
C5—O1—Co1 | 123.92 (19) | C2—C3—H3 | 121.5 |
Co1i—O1—Co1 | 100.14 (17) | C4—C3—H3 | 121.5 |
O1—C5—H5A | 109.5 | N1—C4—C3 | 121.6 (5) |
O1—C5—H5B | 109.5 | N1—C4—H4 | 119.2 |
H5A—C5—H5B | 109.5 | C3—C4—H4 | 119.2 |
O1—C5—H5C | 109.5 | F2—B1—F1 | 113.3 (5) |
H5A—C5—H5C | 109.5 | F2—B1—F3 | 109.9 (3) |
H5B—C5—H5C | 109.5 | F1—B1—F3 | 107.3 (3) |
C1—N1—C4 | 117.9 (4) | F2—B1—F3iii | 109.9 (3) |
C1—N1—Co1 | 124.4 (3) | F1—B1—F3iii | 107.3 (3) |
C4—N1—Co1 | 117.7 (3) | F3—B1—F3iii | 109.1 (4) |
| | | |
O1i—Co1—O1—C5 | 143.5 (5) | Co1i—Co1—N1—C4 | 112.1 (4) |
N1—Co1—O1—C5 | −30.4 (5) | C4—N1—C1—N2 | −179.2 (5) |
N1ii—Co1—O1—C5 | −164.4 (9) | Co1—N1—C1—N2 | 3.3 (7) |
Co1i—Co1—O1—C5 | 143.5 (5) | C4—N1—C1—N3 | 1.5 (8) |
N1—Co1—O1—Co1i | −173.85 (16) | Co1—N1—C1—N3 | −176.0 (4) |
N1ii—Co1—O1—Co1i | 52.1 (11) | C2—N3—C1—N2 | 179.0 (6) |
O1i—Co1—N1—C1 | −116.1 (10) | C2—N3—C1—N1 | −1.7 (8) |
O1—Co1—N1—C1 | −64.8 (4) | C1—N3—C2—C3 | −1.3 (10) |
N1ii—Co1—N1—C1 | 109.6 (4) | N3—C2—C3—C4 | 4.2 (11) |
Co1i—Co1—N1—C1 | −70.4 (4) | C1—N1—C4—C3 | 1.7 (8) |
O1i—Co1—N1—C4 | 66.4 (11) | Co1—N1—C4—C3 | 179.3 (5) |
O1—Co1—N1—C4 | 117.7 (4) | C2—C3—C4—N1 | −4.4 (10) |
N1ii—Co1—N1—C4 | −67.9 (4) | | |
Symmetry codes: (i) −x, −y, −z; (ii) −x, y, −z; (iii) x, −y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2B···N3iv | 0.90 | 2.10 | 3.001 (6) | 176 |
N2—H2A···F3v | 0.90 | 2.15 | 3.022 (6) | 163 |
N2—H2A···F1vi | 0.90 | 2.40 | 3.091 (6) | 134 |
Symmetry codes: (iv) −x+1/2, −y+1/2, −z+1; (v) −x, y, −z+1; (vi) −x, −y, −z+1. |
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