Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807033557/pv2015sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807033557/pv2015Isup2.hkl |
CCDC reference: 660137
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (C-C) = 0.007 Å
- Disorder in solvent or counterion
- R factor = 0.048
- wR factor = 0.136
- Data-to-parameter ratio = 11.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for B1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for B2 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 29.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 7
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 99
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For related literature, see: Şerb et al. (2007); Sheldrick (1997); Sigman et al. (1979); Tomislav (2006); Xu et al. (2005).
A aqueous solution (15 ml) of Cu(BF4)2 (23.7 mg, 0.1 mmol) was added to the methanol solution (20 ml) of 1,10-phenanthroline (39.6 mg, 0.2 mmol) and stirred for a further 1 h. The solution was kept at room temperature and blue crystals were formed after a week (yield 35%).
The H atoms were placed in caculated positions with C—H = 0.93 Å and O—H = 0.85 Å and were included in the refinement with Uiso(H) = 1.2Ueq(C/O). One of the BF4 anions was found to be disordered oversites F1 - F4 and F1' - F4'. The site occupancies of F-atoms were determined using an isotropic model and the B—F distances were fixed at 1.36 (1) Å for both the anions in the subsequent refinement cycles.
Copper(II) coordination compounds have been investigated frequently, not only because of their interesting magnetic superexchange interactions, but also because of their relevance for bioinorganic model systems in copper enzymes (Sigman et al., 1979). Here, the synthesis and crystal structure of the title bis(tetrafluoridoborate) complex, are reported.
The crystal structure of (I) consists of copper(II) complex cations and bis(tetrafluoridoborate) anions, as shown in Fig. 1. The CuII atom assumes a CuN4O trigonal-bipyramidal coordination geometry formed by two N,N'-bidentate bpy ligands and one equatorial oxygen atom (Fig. 1). The Cu—N bond lengths are in the range 1.982 (3)–2.124 (3) Å, while the Cu—O bond distance is 2.035 (4) Å (Table 1). The Cu—N bond lengths in (I) are in agreement with those in previously characterized Cu—N bonds in [Cu(bpy)2]I or [Cu(phen)2]II(Tomislav, 2006; Xu et al., 2005; Şerb et al., 2007). The bite angles in (I) are smaller than 90 °, which is due to the rigid geometry of the bidentate bpy ligand.
The interligand dihedral angle of 67.3 (3) ° in (I) is much lower than that found in [Cu(bpy)2]I cited above (87.5 (11) °). The structure is stabilized by O—H···F type hydrogen bonds between the CuII complex and tetrafluoridoborate anion.
For related literature, see: Şerb et al. (2007); Sheldrick (1997); Sigman et al. (1979); Tomislav (2006); Xu et al. (2005).
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Fig. 1. A view of complex (I), showing 30% probability displacement ellipsoids and the atom-numbering scheme. |
[Cu(C10H8N2)2(H2O)](BF4)2 | F(000) = 1140 |
Mr = 567.54 | Dx = 1.624 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2544 reflections |
a = 9.0961 (16) Å | θ = 2.3–23.3° |
b = 13.571 (2) Å | µ = 1.03 mm−1 |
c = 19.338 (3) Å | T = 294 K |
β = 103.507 (3)° | Block, blue |
V = 2321.1 (6) Å3 | 0.24 × 0.20 × 0.16 mm |
Z = 4 |
Bruker SMART CCD area-detector diffractometer | 4090 independent reflections |
Radiation source: fine-focus sealed tube | 2549 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
φ and ω scans | θmax = 25.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −10→10 |
Tmin = 0.780, Tmax = 0.853 | k = −16→12 |
11615 measured reflections | l = −18→22 |
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)] = 0.048 | H-atom parameters constrained |
wR(F2) = 0.136 | w = 1/[σ2(Fo2) + (0.0615P)2 + 1.4025P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.003 |
4090 reflections | Δρmax = 0.46 e Å−3 |
363 parameters | Δρmin = −0.37 e Å−3 |
99 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0078 (8) |
[Cu(C10H8N2)2(H2O)](BF4)2 | V = 2321.1 (6) Å3 |
Mr = 567.54 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 9.0961 (16) Å | µ = 1.03 mm−1 |
b = 13.571 (2) Å | T = 294 K |
c = 19.338 (3) Å | 0.24 × 0.20 × 0.16 mm |
β = 103.507 (3)° |
Bruker SMART CCD area-detector diffractometer | 4090 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 2549 reflections with I > 2σ(I) |
Tmin = 0.780, Tmax = 0.853 | Rint = 0.049 |
11615 measured reflections |
R[F2 > 2σ(F2)] = 0.048 | 99 restraints |
wR(F2) = 0.136 | H-atom parameters constrained |
S = 1.02 | Δρmax = 0.46 e Å−3 |
4090 reflections | Δρmin = −0.37 e Å−3 |
363 parameters |
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 | Occ. (<1) | |
Cu1 | 0.94520 (6) | 0.73629 (4) | 0.86050 (3) | 0.0429 (2) | |
O1 | 0.9400 (4) | 0.5864 (3) | 0.86045 (18) | 0.0758 (11) | |
H1A | 0.8685 | 0.5616 | 0.8775 | 0.091* | |
H1B | 1.0214 | 0.5516 | 0.8665 | 0.091* | |
N1 | 1.0849 (4) | 0.7371 (2) | 0.79494 (19) | 0.0451 (9) | |
N2 | 0.8180 (4) | 0.8221 (2) | 0.77547 (17) | 0.0419 (9) | |
N3 | 0.8064 (4) | 0.7459 (2) | 0.92541 (18) | 0.0398 (8) | |
N4 | 1.0677 (4) | 0.8328 (2) | 0.93734 (18) | 0.0432 (9) | |
C1 | 1.2179 (5) | 0.6899 (4) | 0.8075 (3) | 0.0615 (14) | |
H1 | 1.2488 | 0.6553 | 0.8499 | 0.074* | |
C2 | 1.3106 (6) | 0.6902 (4) | 0.7609 (3) | 0.0652 (14) | |
H2 | 1.4019 | 0.6563 | 0.7714 | 0.078* | |
C3 | 1.2659 (6) | 0.7414 (4) | 0.6989 (3) | 0.0596 (13) | |
H3 | 1.3271 | 0.7438 | 0.6666 | 0.072* | |
C4 | 1.1294 (6) | 0.7893 (3) | 0.6849 (2) | 0.0532 (12) | |
H4 | 1.0975 | 0.8242 | 0.6427 | 0.064* | |
C5 | 1.0392 (5) | 0.7859 (3) | 0.7329 (2) | 0.0384 (10) | |
C6 | 0.8878 (5) | 0.8317 (3) | 0.7217 (2) | 0.0389 (10) | |
C7 | 0.8180 (6) | 0.8806 (3) | 0.6600 (2) | 0.0500 (12) | |
H7 | 0.8680 | 0.8880 | 0.6235 | 0.060* | |
C8 | 0.6743 (6) | 0.9182 (3) | 0.6525 (3) | 0.0589 (13) | |
H8 | 0.6255 | 0.9498 | 0.6108 | 0.071* | |
C9 | 0.6046 (6) | 0.9080 (3) | 0.7084 (3) | 0.0587 (13) | |
H9 | 0.5079 | 0.9329 | 0.7050 | 0.070* | |
C10 | 0.6803 (5) | 0.8605 (3) | 0.7689 (2) | 0.0500 (12) | |
H10 | 0.6339 | 0.8549 | 0.8067 | 0.060* | |
C11 | 0.6722 (5) | 0.7006 (3) | 0.9144 (2) | 0.0514 (12) | |
H11 | 0.6407 | 0.6623 | 0.8738 | 0.062* | |
C12 | 0.5795 (5) | 0.7083 (4) | 0.9609 (3) | 0.0583 (13) | |
H12 | 0.4875 | 0.6753 | 0.9520 | 0.070* | |
C13 | 0.6240 (6) | 0.7651 (3) | 1.0202 (3) | 0.0568 (13) | |
H13 | 0.5616 | 0.7725 | 1.0517 | 0.068* | |
C14 | 0.7635 (5) | 0.8118 (3) | 1.0329 (2) | 0.0510 (12) | |
H14 | 0.7967 | 0.8499 | 1.0735 | 0.061* | |
C15 | 0.8525 (5) | 0.8009 (3) | 0.9845 (2) | 0.0384 (10) | |
C16 | 1.0044 (5) | 0.8465 (3) | 0.9928 (2) | 0.0401 (10) | |
C17 | 1.0767 (6) | 0.8993 (3) | 1.0525 (2) | 0.0536 (12) | |
H17 | 1.0308 | 0.9078 | 1.0903 | 0.064* | |
C18 | 1.2169 (6) | 0.9387 (4) | 1.0551 (3) | 0.0678 (15) | |
H18 | 1.2679 | 0.9736 | 1.0949 | 0.081* | |
C19 | 1.2808 (6) | 0.9257 (4) | 0.9976 (3) | 0.0685 (15) | |
H19 | 1.3755 | 0.9520 | 0.9983 | 0.082* | |
C20 | 1.2037 (5) | 0.8736 (3) | 0.9395 (3) | 0.0550 (12) | |
H20 | 1.2465 | 0.8665 | 0.9005 | 0.066* | |
B1 | 0.6694 (6) | 0.5485 (4) | 0.6935 (3) | 0.0659 (17) | |
F1 | 0.8178 (9) | 0.5433 (9) | 0.6902 (8) | 0.104 (4) | 0.595 (11) |
F2 | 0.5891 (10) | 0.4695 (7) | 0.6616 (5) | 0.122 (4) | 0.595 (11) |
F3 | 0.5912 (11) | 0.6298 (8) | 0.6588 (6) | 0.148 (4) | 0.595 (11) |
F4 | 0.6459 (12) | 0.5574 (8) | 0.7600 (4) | 0.084 (3) | 0.595 (11) |
F1' | 0.8079 (12) | 0.5843 (11) | 0.6883 (9) | 0.077 (4) | 0.405 (11) |
F2' | 0.6878 (18) | 0.4499 (7) | 0.7132 (8) | 0.131 (5) | 0.405 (11) |
F3' | 0.5836 (10) | 0.5514 (11) | 0.6293 (4) | 0.095 (4) | 0.405 (11) |
F4' | 0.633 (2) | 0.5993 (11) | 0.7463 (8) | 0.101 (5) | 0.405 (11) |
B2 | 0.2352 (6) | 0.5935 (4) | 0.0273 (2) | 0.0459 (13) | |
F5 | 0.0851 (3) | 0.6057 (2) | 0.02780 (15) | 0.0775 (9) | |
F6 | 0.3119 (4) | 0.6801 (2) | 0.04648 (19) | 0.0944 (11) | |
F7 | 0.2497 (4) | 0.5678 (3) | −0.03890 (15) | 0.0938 (11) | |
F8 | 0.2977 (4) | 0.5252 (3) | 0.07647 (19) | 0.1033 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0414 (3) | 0.0536 (4) | 0.0386 (3) | −0.0004 (3) | 0.0190 (2) | 0.0054 (3) |
O1 | 0.070 (2) | 0.072 (2) | 0.090 (3) | −0.0009 (19) | 0.028 (2) | 0.006 (2) |
N1 | 0.042 (2) | 0.053 (2) | 0.044 (2) | 0.0051 (18) | 0.0161 (17) | 0.0097 (18) |
N2 | 0.044 (2) | 0.047 (2) | 0.035 (2) | −0.0001 (17) | 0.0100 (17) | 0.0040 (16) |
N3 | 0.040 (2) | 0.048 (2) | 0.0344 (19) | −0.0024 (16) | 0.0143 (15) | 0.0015 (16) |
N4 | 0.039 (2) | 0.043 (2) | 0.048 (2) | −0.0009 (16) | 0.0099 (18) | 0.0100 (17) |
C1 | 0.050 (3) | 0.082 (4) | 0.056 (3) | 0.012 (3) | 0.020 (3) | 0.018 (3) |
C2 | 0.047 (3) | 0.086 (4) | 0.070 (4) | 0.008 (3) | 0.028 (3) | 0.002 (3) |
C3 | 0.053 (3) | 0.078 (4) | 0.056 (3) | −0.012 (3) | 0.030 (2) | −0.011 (3) |
C4 | 0.062 (3) | 0.065 (3) | 0.039 (3) | −0.015 (3) | 0.024 (2) | 0.002 (2) |
C5 | 0.045 (3) | 0.040 (2) | 0.032 (2) | −0.0089 (19) | 0.0120 (19) | −0.0009 (18) |
C6 | 0.047 (3) | 0.036 (2) | 0.035 (2) | −0.0085 (19) | 0.012 (2) | 0.0006 (19) |
C7 | 0.062 (3) | 0.051 (3) | 0.039 (3) | −0.008 (2) | 0.016 (2) | 0.005 (2) |
C8 | 0.066 (4) | 0.056 (3) | 0.048 (3) | 0.000 (3) | −0.001 (3) | 0.016 (2) |
C9 | 0.055 (3) | 0.050 (3) | 0.066 (3) | 0.009 (2) | 0.004 (3) | 0.006 (3) |
C10 | 0.047 (3) | 0.057 (3) | 0.047 (3) | 0.007 (2) | 0.012 (2) | 0.003 (2) |
C11 | 0.046 (3) | 0.064 (3) | 0.048 (3) | −0.011 (2) | 0.020 (2) | −0.005 (2) |
C12 | 0.044 (3) | 0.072 (3) | 0.063 (3) | −0.010 (2) | 0.022 (2) | 0.005 (3) |
C13 | 0.058 (3) | 0.066 (3) | 0.057 (3) | 0.007 (3) | 0.035 (3) | 0.007 (3) |
C14 | 0.063 (3) | 0.054 (3) | 0.040 (3) | 0.003 (2) | 0.020 (2) | 0.003 (2) |
C15 | 0.048 (3) | 0.036 (2) | 0.033 (2) | 0.0040 (19) | 0.014 (2) | 0.0077 (19) |
C16 | 0.047 (3) | 0.030 (2) | 0.041 (3) | 0.0017 (19) | 0.005 (2) | 0.0058 (19) |
C17 | 0.065 (3) | 0.043 (3) | 0.048 (3) | 0.005 (2) | 0.002 (2) | 0.002 (2) |
C18 | 0.068 (4) | 0.049 (3) | 0.075 (4) | −0.008 (3) | −0.005 (3) | −0.007 (3) |
C19 | 0.049 (3) | 0.052 (3) | 0.097 (5) | −0.011 (2) | 0.001 (3) | 0.007 (3) |
C20 | 0.043 (3) | 0.055 (3) | 0.067 (3) | −0.008 (2) | 0.013 (3) | 0.008 (3) |
B1 | 0.069 (5) | 0.082 (5) | 0.052 (4) | 0.006 (4) | 0.024 (4) | 0.015 (4) |
F1 | 0.073 (5) | 0.133 (8) | 0.113 (6) | 0.009 (4) | 0.031 (4) | −0.023 (6) |
F2 | 0.109 (6) | 0.148 (7) | 0.121 (7) | −0.030 (5) | 0.048 (5) | −0.068 (5) |
F3 | 0.161 (7) | 0.160 (8) | 0.134 (7) | 0.027 (6) | 0.057 (5) | 0.061 (6) |
F4 | 0.080 (5) | 0.124 (7) | 0.052 (4) | −0.020 (5) | 0.023 (3) | −0.001 (4) |
F1' | 0.073 (7) | 0.109 (9) | 0.061 (6) | −0.009 (5) | 0.036 (5) | 0.009 (6) |
F2' | 0.159 (9) | 0.102 (7) | 0.150 (9) | 0.033 (6) | 0.072 (7) | 0.056 (6) |
F3' | 0.070 (6) | 0.139 (9) | 0.061 (6) | −0.016 (6) | −0.018 (4) | 0.010 (5) |
F4' | 0.085 (7) | 0.103 (8) | 0.122 (9) | 0.016 (6) | 0.039 (7) | −0.043 (7) |
B2 | 0.051 (3) | 0.053 (3) | 0.037 (3) | −0.007 (3) | 0.017 (3) | −0.001 (3) |
F5 | 0.0545 (19) | 0.113 (2) | 0.068 (2) | −0.0087 (16) | 0.0209 (15) | −0.0189 (17) |
F6 | 0.095 (2) | 0.080 (2) | 0.120 (3) | −0.0336 (19) | 0.049 (2) | −0.020 (2) |
F7 | 0.082 (2) | 0.152 (3) | 0.0515 (19) | 0.003 (2) | 0.0243 (17) | −0.0254 (19) |
F8 | 0.103 (3) | 0.102 (3) | 0.099 (3) | 0.004 (2) | 0.014 (2) | 0.049 (2) |
Cu1—N3 | 1.982 (3) | C10—H10 | 0.9300 |
Cu1—N1 | 1.993 (3) | C11—C12 | 1.372 (6) |
Cu1—O1 | 2.035 (4) | C11—H11 | 0.9300 |
Cu1—N4 | 2.095 (4) | C12—C13 | 1.362 (7) |
Cu1—N2 | 2.124 (3) | C12—H12 | 0.9300 |
O1—H1A | 0.8635 | C13—C14 | 1.389 (6) |
O1—H1B | 0.8629 | C13—H13 | 0.9300 |
N1—C1 | 1.340 (6) | C14—C15 | 1.381 (6) |
N1—C5 | 1.347 (5) | C14—H14 | 0.9300 |
N2—C10 | 1.335 (5) | C15—C16 | 1.488 (6) |
N2—C6 | 1.345 (5) | C16—C17 | 1.387 (6) |
N3—C11 | 1.339 (5) | C17—C18 | 1.373 (7) |
N3—C15 | 1.347 (5) | C17—H17 | 0.9300 |
N4—C16 | 1.344 (5) | C18—C19 | 1.380 (7) |
N4—C20 | 1.347 (5) | C18—H18 | 0.9300 |
C1—C2 | 1.371 (6) | C19—C20 | 1.374 (7) |
C1—H1 | 0.9300 | C19—H19 | 0.9300 |
C2—C3 | 1.362 (7) | C20—H20 | 0.9300 |
C2—H2 | 0.9300 | B1—F3' | 1.304 (7) |
C3—C4 | 1.372 (7) | B1—F4' | 1.339 (9) |
C3—H3 | 0.9300 | B1—F4 | 1.359 (8) |
C4—C5 | 1.376 (6) | B1—F2 | 1.361 (7) |
C4—H4 | 0.9300 | B1—F1 | 1.368 (8) |
C5—C6 | 1.480 (6) | B1—F1' | 1.375 (9) |
C6—C7 | 1.383 (6) | B1—F2' | 1.391 (8) |
C7—C8 | 1.379 (6) | B1—F3 | 1.397 (7) |
C7—H7 | 0.9300 | B2—F8 | 1.355 (5) |
C8—C9 | 1.381 (7) | B2—F7 | 1.363 (5) |
C8—H8 | 0.9300 | B2—F6 | 1.373 (5) |
C9—C10 | 1.372 (6) | B2—F5 | 1.378 (5) |
C9—H9 | 0.9300 | ||
N3—Cu1—N1 | 175.88 (14) | C13—C12—H12 | 120.4 |
N3—Cu1—O1 | 92.77 (14) | C11—C12—H12 | 120.4 |
N1—Cu1—O1 | 91.35 (14) | C12—C13—C14 | 119.1 (4) |
N3—Cu1—N4 | 79.72 (14) | C12—C13—H13 | 120.4 |
N1—Cu1—N4 | 97.76 (14) | C14—C13—H13 | 120.4 |
O1—Cu1—N4 | 129.30 (13) | C15—C14—C13 | 119.2 (4) |
N3—Cu1—N2 | 98.15 (14) | C15—C14—H14 | 120.4 |
N1—Cu1—N2 | 79.47 (14) | C13—C14—H14 | 120.4 |
O1—Cu1—N2 | 122.65 (14) | N3—C15—C14 | 121.2 (4) |
N4—Cu1—N2 | 108.05 (13) | N3—C15—C16 | 114.8 (4) |
Cu1—O1—H1A | 114.1 | C14—C15—C16 | 124.0 (4) |
Cu1—O1—H1B | 121.9 | N4—C16—C17 | 121.9 (4) |
H1A—O1—H1B | 115.8 | N4—C16—C15 | 114.6 (4) |
C1—N1—C5 | 118.3 (4) | C17—C16—C15 | 123.5 (4) |
C1—N1—Cu1 | 124.3 (3) | C18—C17—C16 | 119.1 (5) |
C5—N1—Cu1 | 117.3 (3) | C18—C17—H17 | 120.4 |
C10—N2—C6 | 119.3 (4) | C16—C17—H17 | 120.4 |
C10—N2—Cu1 | 128.2 (3) | C17—C18—C19 | 118.9 (5) |
C6—N2—Cu1 | 112.4 (3) | C17—C18—H18 | 120.5 |
C11—N3—C15 | 118.8 (4) | C19—C18—H18 | 120.5 |
C11—N3—Cu1 | 124.1 (3) | C20—C19—C18 | 119.6 (5) |
C15—N3—Cu1 | 117.1 (3) | C20—C19—H19 | 120.2 |
C16—N4—C20 | 118.7 (4) | C18—C19—H19 | 120.2 |
C16—N4—Cu1 | 113.4 (3) | N4—C20—C19 | 121.8 (5) |
C20—N4—Cu1 | 127.7 (3) | N4—C20—H20 | 119.1 |
N1—C1—C2 | 123.1 (5) | C19—C20—H20 | 119.1 |
N1—C1—H1 | 118.4 | F3'—B1—F4' | 120.7 (10) |
C2—C1—H1 | 118.4 | F3'—B1—F4 | 135.1 (8) |
C3—C2—C1 | 118.5 (5) | F3'—B1—F2 | 57.0 (6) |
C3—C2—H2 | 120.7 | F4'—B1—F2 | 123.2 (9) |
C1—C2—H2 | 120.7 | F4—B1—F2 | 108.2 (7) |
C2—C3—C4 | 119.0 (4) | F3'—B1—F1 | 109.6 (9) |
C2—C3—H3 | 120.5 | F4'—B1—F1 | 119.1 (11) |
C4—C3—H3 | 120.5 | F4—B1—F1 | 115.1 (9) |
C3—C4—C5 | 120.5 (4) | F2—B1—F1 | 111.7 (7) |
C3—C4—H4 | 119.8 | F3'—B1—F1' | 105.9 (9) |
C5—C4—H4 | 119.8 | F4'—B1—F1' | 105.6 (12) |
N1—C5—C4 | 120.5 (4) | F4—B1—F1' | 112.8 (9) |
N1—C5—C6 | 114.9 (4) | F2—B1—F1' | 130.5 (9) |
C4—C5—C6 | 124.6 (4) | F3'—B1—F2' | 107.4 (9) |
N2—C6—C7 | 120.6 (4) | F4'—B1—F2' | 108.7 (9) |
N2—C6—C5 | 115.9 (4) | F4—B1—F2' | 82.0 (7) |
C7—C6—C5 | 123.5 (4) | F2—B1—F2' | 52.0 (6) |
C8—C7—C6 | 120.0 (4) | F1—B1—F2' | 84.6 (7) |
C8—C7—H7 | 120.0 | F1'—B1—F2' | 107.9 (9) |
C6—C7—H7 | 120.0 | F3'—B1—F3 | 52.7 (6) |
C7—C8—C9 | 118.6 (4) | F4'—B1—F3 | 76.6 (8) |
C7—C8—H8 | 120.7 | F4—B1—F3 | 102.0 (7) |
C9—C8—H8 | 120.7 | F2—B1—F3 | 104.2 (7) |
C10—C9—C8 | 118.9 (5) | F1—B1—F3 | 114.6 (8) |
C10—C9—H9 | 120.6 | F1'—B1—F3 | 93.4 (8) |
C8—C9—H9 | 120.6 | F2'—B1—F3 | 155.1 (9) |
N2—C10—C9 | 122.6 (4) | F8—B2—F7 | 111.5 (4) |
N2—C10—H10 | 118.7 | F8—B2—F6 | 107.0 (4) |
C9—C10—H10 | 118.7 | F7—B2—F6 | 108.6 (4) |
N3—C11—C12 | 122.5 (4) | F8—B2—F5 | 109.4 (4) |
N3—C11—H11 | 118.7 | F7—B2—F5 | 110.5 (4) |
C12—C11—H11 | 118.7 | F6—B2—F5 | 109.7 (4) |
C13—C12—C11 | 119.2 (4) | ||
O1—Cu1—N1—C1 | −55.2 (4) | Cu1—N2—C6—C7 | 176.4 (3) |
N4—Cu1—N1—C1 | 74.8 (4) | C10—N2—C6—C5 | −179.2 (4) |
N2—Cu1—N1—C1 | −178.2 (4) | Cu1—N2—C6—C5 | −2.7 (4) |
O1—Cu1—N1—C5 | 122.5 (3) | N1—C5—C6—N2 | 2.4 (5) |
N4—Cu1—N1—C5 | −107.5 (3) | C4—C5—C6—N2 | −178.8 (4) |
N2—Cu1—N1—C5 | −0.5 (3) | N1—C5—C6—C7 | −176.6 (4) |
N3—Cu1—N2—C10 | −5.5 (4) | C4—C5—C6—C7 | 2.2 (7) |
N1—Cu1—N2—C10 | 177.9 (4) | N2—C6—C7—C8 | −1.3 (6) |
O1—Cu1—N2—C10 | 93.1 (4) | C5—C6—C7—C8 | 177.6 (4) |
N4—Cu1—N2—C10 | −87.3 (4) | C6—C7—C8—C9 | 1.5 (7) |
N3—Cu1—N2—C6 | 178.3 (3) | C7—C8—C9—C10 | −0.3 (7) |
N1—Cu1—N2—C6 | 1.8 (3) | C6—N2—C10—C9 | 1.5 (6) |
O1—Cu1—N2—C6 | −83.0 (3) | Cu1—N2—C10—C9 | −174.4 (3) |
N4—Cu1—N2—C6 | 96.6 (3) | C8—C9—C10—N2 | −1.3 (7) |
O1—Cu1—N3—C11 | −52.2 (4) | C15—N3—C11—C12 | 0.4 (7) |
N4—Cu1—N3—C11 | 178.4 (4) | Cu1—N3—C11—C12 | 179.5 (3) |
N2—Cu1—N3—C11 | 71.4 (4) | N3—C11—C12—C13 | 0.7 (7) |
O1—Cu1—N3—C15 | 127.0 (3) | C11—C12—C13—C14 | −1.5 (7) |
N4—Cu1—N3—C15 | −2.5 (3) | C12—C13—C14—C15 | 1.2 (7) |
N2—Cu1—N3—C15 | −109.5 (3) | C11—N3—C15—C14 | −0.7 (6) |
N3—Cu1—N4—C16 | 5.4 (3) | Cu1—N3—C15—C14 | −179.9 (3) |
N1—Cu1—N4—C16 | −177.9 (3) | C11—N3—C15—C16 | 178.7 (4) |
O1—Cu1—N4—C16 | −79.8 (3) | Cu1—N3—C15—C16 | −0.5 (4) |
N2—Cu1—N4—C16 | 100.7 (3) | C13—C14—C15—N3 | −0.1 (6) |
N3—Cu1—N4—C20 | 179.4 (4) | C13—C14—C15—C16 | −179.4 (4) |
N1—Cu1—N4—C20 | −3.9 (4) | C20—N4—C16—C17 | −1.6 (6) |
O1—Cu1—N4—C20 | 94.3 (4) | Cu1—N4—C16—C17 | 173.0 (3) |
N2—Cu1—N4—C20 | −85.3 (4) | C20—N4—C16—C15 | 178.3 (4) |
C5—N1—C1—C2 | 1.1 (7) | Cu1—N4—C16—C15 | −7.1 (4) |
Cu1—N1—C1—C2 | 178.8 (4) | N3—C15—C16—N4 | 5.2 (5) |
N1—C1—C2—C3 | 0.3 (8) | C14—C15—C16—N4 | −175.4 (4) |
C1—C2—C3—C4 | −1.0 (8) | N3—C15—C16—C17 | −174.8 (4) |
C2—C3—C4—C5 | 0.2 (7) | C14—C15—C16—C17 | 4.5 (6) |
C1—N1—C5—C4 | −1.9 (6) | N4—C16—C17—C18 | 0.1 (6) |
Cu1—N1—C5—C4 | −179.7 (3) | C15—C16—C17—C18 | −179.9 (4) |
C1—N1—C5—C6 | 177.0 (4) | C16—C17—C18—C19 | 0.9 (7) |
Cu1—N1—C5—C6 | −0.8 (5) | C17—C18—C19—C20 | −0.2 (8) |
C3—C4—C5—N1 | 1.2 (7) | C16—N4—C20—C19 | 2.3 (6) |
C3—C4—C5—C6 | −177.5 (4) | Cu1—N4—C20—C19 | −171.4 (3) |
C10—N2—C6—C7 | −0.2 (6) | C18—C19—C20—N4 | −1.4 (7) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···F8i | 0.86 | 2.26 | 3.113 (4) | 171 |
O1—H1B···F7ii | 0.86 | 2.44 | 3.038 (4) | 127 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1, y, z+1. |
Experimental details
Crystal data | |
Chemical formula | [Cu(C10H8N2)2(H2O)](BF4)2 |
Mr | 567.54 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 294 |
a, b, c (Å) | 9.0961 (16), 13.571 (2), 19.338 (3) |
β (°) | 103.507 (3) |
V (Å3) | 2321.1 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.03 |
Crystal size (mm) | 0.24 × 0.20 × 0.16 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.780, 0.853 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11615, 4090, 2549 |
Rint | 0.049 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.048, 0.136, 1.02 |
No. of reflections | 4090 |
No. of parameters | 363 |
No. of restraints | 99 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.46, −0.37 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXTL (Bruker, 2000), SHELXTL.
Cu1—N3 | 1.982 (3) | Cu1—N4 | 2.095 (4) |
Cu1—N1 | 1.993 (3) | Cu1—N2 | 2.124 (3) |
Cu1—O1 | 2.035 (4) | ||
N3—Cu1—N4 | 79.72 (14) | N1—Cu1—N2 | 79.47 (14) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···F8i | 0.864 | 2.257 | 3.113 (4) | 171.1 |
O1—H1B···F7ii | 0.863 | 2.436 | 3.038 (4) | 127.3 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1, y, z+1. |
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Copper(II) coordination compounds have been investigated frequently, not only because of their interesting magnetic superexchange interactions, but also because of their relevance for bioinorganic model systems in copper enzymes (Sigman et al., 1979). Here, the synthesis and crystal structure of the title bis(tetrafluoridoborate) complex, are reported.
The crystal structure of (I) consists of copper(II) complex cations and bis(tetrafluoridoborate) anions, as shown in Fig. 1. The CuII atom assumes a CuN4O trigonal-bipyramidal coordination geometry formed by two N,N'-bidentate bpy ligands and one equatorial oxygen atom (Fig. 1). The Cu—N bond lengths are in the range 1.982 (3)–2.124 (3) Å, while the Cu—O bond distance is 2.035 (4) Å (Table 1). The Cu—N bond lengths in (I) are in agreement with those in previously characterized Cu—N bonds in [Cu(bpy)2]I or [Cu(phen)2]II(Tomislav, 2006; Xu et al., 2005; Şerb et al., 2007). The bite angles in (I) are smaller than 90 °, which is due to the rigid geometry of the bidentate bpy ligand.
The interligand dihedral angle of 67.3 (3) ° in (I) is much lower than that found in [Cu(bpy)2]I cited above (87.5 (11) °). The structure is stabilized by O—H···F type hydrogen bonds between the CuII complex and tetrafluoridoborate anion.