Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807037695/hb2500sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807037695/hb2500Isup2.hkl |
CCDC reference: 660062
Key indicators
- Single-crystal X-ray study
- T = 290 K
- Mean (C-C) = 0.005 Å
- R factor = 0.034
- wR factor = 0.071
- Data-to-parameter ratio = 17.1
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) 500 Ang. PLAT230_ALERT_2_C Hirshfeld Test Diff for O2 - N3 .. 6.85 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cu1 - O4 .. 6.17 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cu1 - O1_a .. 6.97 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O4 PLAT420_ALERT_2_C D-H Without Acceptor N2 - H12 ... ? PLAT431_ALERT_2_C Short Inter HL..A Contact Br1 .. O3 .. 3.20 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Br2 .. O2 .. 3.18 Ang.
Alert level G PLAT793_ALERT_1_G Check the Absolute Configuration of N2 = ... R PLAT794_ALERT_5_G Check Predicted Bond Valency for Cu1 (2) 2.21
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 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 1 ALERT type 5 Informative message, check
For related literature, see: Solomon et al. (1996); Collman, Zhong, Zhang & Costanzo (2001); Collman, Zhong, Zeng & Costanzo (2001); Xu et al. (2005).
For related literature, see: Gavrilova & Bosnich (2004); Yang et al. (2006).
2,4-Dibromo-6-((pyridine-2-ylmethylamino)methyl)phenol (0.372 g, 1 mmol) was added to a methanol solution (20 ml) of Cu(NO3)2.3H2O (0.241 g, 1 mmol) with stirring. The resulting solution was left to stand at room temperature and green crystals of (I) were obtained after several days.
All H atoms on C atoms were poisitioned geometrically and refined as riding atoms, with C—H = 0.93 Å and Uiso = 1.2Ueq (C). The H atom bonded to N atom was located in a difference Fourier map and refined freely.
The synthesis and characterization of binuclear copper(II) compounds have received increasing interest in bio-inorganic chemistry (Solomon et al., 1996) and catalysis (Collman, Zhong, Zhang & Costanzo, 2001; Collman, Zhong, Zeng & Costanzo, 2001). It is well known that the phenolate anion is a good bridging ligand for the construction of binuclear transition metal compounds (Gavrilova & Bosnich 2004; Yang et al., 2006). Modification of the phenolate anion in its ortho position can lead to the formation of stable binuclear compounds through chelation (Xu, et al., 2005). The structure of a new binuclear complex [Cu2(dmp)2(NO3)2], (I), where dmp is 2,4-dibromo-6-((pyridine-2-ylmethylamino)methyl)phenol, is presented here.
As shown in Fig. 1, the title compound, [Cu2(C13H11Br2N2O)(NO3)2], contains a binuclear copper(II) unit bridged by two phenolate O atoms with a Cu···Cu distance of 3.207 (4) Å. Each CuII atom is chelated by one dmp ligand and is also coordinated by a nitrate O atom. Finally, the trigonal-bipyramidal coordination environment is completed by bond to the phenolate O atom from another dmp ligand. The axial positions of the trigonal-bipyramid are occupied by one phenolate O atom and one pyridine N atom with the O—Cu—N angle being 171.25 (10)°.
For related literature, see: Solomon et al. (1996); Collman, Zhong, Zhang & Costanzo (2001); Collman, Zhong, Zeng & Costanzo (2001); Xu et al. (2005).
For related literature, see: Gavrilova & Bosnich (2004); Yang et al. (2006).
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.
Fig. 1. A view of the molecular structure of (I). Displacement ellipsoids are drawn at the 30% probability level (arbitrary spheres for the H atoms). Symmetry code: (i) 2 - x, -y, 1 - z. |
[Cu2(C13H11Br2N2O)2(NO3)2] | F(000) = 964 |
Mr = 993.22 | Dx = 2.075 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: -P 2yn | Cell parameters from 11121 reflections |
a = 10.385 (5) Å | θ = 3.0–27.5° |
b = 11.252 (5) Å | µ = 6.42 mm−1 |
c = 14.074 (5) Å | T = 290 K |
β = 104.810 (5)° | Block, green |
V = 1589.9 (12) Å3 | 0.24 × 0.16 × 0.13 mm |
Z = 2 |
Rigaku R-AXIS RAPID diffractometer | 3629 independent reflections |
Radiation source: rotating anode | 2707 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.054 |
Detector resolution: 10.0 pixels mm-1 | θmax = 27.5°, θmin = 3° |
ω scans | h = −13→13 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −14→14 |
Tmin = 0.30, Tmax = 0.43 | l = −15→18 |
14979 measured reflections |
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: difmap and geom |
wR(F2) = 0.071 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0224P)2 + 0.8145P] where P = (Fo2 + 2Fc2)/3 |
3629 reflections | (Δ/σ)max = 0.007 |
212 parameters | Δρmax = 0.48 e Å−3 |
0 restraints | Δρmin = −0.49 e Å−3 |
[Cu2(C13H11Br2N2O)2(NO3)2] | V = 1589.9 (12) Å3 |
Mr = 993.22 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.385 (5) Å | µ = 6.42 mm−1 |
b = 11.252 (5) Å | T = 290 K |
c = 14.074 (5) Å | 0.24 × 0.16 × 0.13 mm |
β = 104.810 (5)° |
Rigaku R-AXIS RAPID diffractometer | 3629 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 2707 reflections with I > 2σ(I) |
Tmin = 0.30, Tmax = 0.43 | Rint = 0.054 |
14979 measured reflections |
R[F2 > 2σ(F2)] = 0.035 | 0 restraints |
wR(F2) = 0.071 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | Δρmax = 0.48 e Å−3 |
3629 reflections | Δρmin = −0.49 e Å−3 |
212 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 | ||
Cu1 | 0.93487 (4) | 0.01290 (3) | 0.38420 (3) | 0.03277 (11) | |
C1 | 0.9741 (4) | 0.2204 (3) | 0.2616 (3) | 0.0414 (8) | |
H1 | 0.9214 | 0.2636 | 0.2936 | 0.050* | |
C2 | 1.0259 (4) | 0.2770 (3) | 0.1930 (3) | 0.0461 (9) | |
H2 | 1.0085 | 0.3570 | 0.1789 | 0.055* | |
C3 | 1.1040 (4) | 0.2130 (3) | 0.1454 (3) | 0.0444 (9) | |
H3 | 1.1398 | 0.2492 | 0.0986 | 0.053* | |
C4 | 1.1286 (4) | 0.0938 (3) | 0.1685 (3) | 0.0432 (9) | |
H4 | 1.1806 | 0.0489 | 0.1370 | 0.052* | |
C5 | 1.0746 (3) | 0.0432 (3) | 0.2387 (2) | 0.0340 (7) | |
C6 | 1.1035 (4) | −0.0829 (3) | 0.2745 (3) | 0.0416 (8) | |
H6A | 1.1081 | −0.1336 | 0.2198 | 0.050* | |
H6B | 1.1891 | −0.0858 | 0.3225 | 0.050* | |
C7 | 1.0454 (3) | −0.2280 (3) | 0.3883 (2) | 0.0352 (8) | |
H7A | 1.1168 | −0.2020 | 0.4432 | 0.042* | |
H7B | 1.0793 | −0.2915 | 0.3547 | 0.042* | |
C8 | 0.9315 (3) | −0.2731 (3) | 0.4252 (2) | 0.0314 (7) | |
C9 | 0.8915 (4) | −0.3920 (3) | 0.4112 (2) | 0.0374 (8) | |
H9 | 0.9362 | −0.4439 | 0.3794 | 0.045* | |
C10 | 0.7862 (4) | −0.4316 (3) | 0.4448 (2) | 0.0377 (8) | |
C11 | 0.7165 (4) | −0.3581 (3) | 0.4914 (3) | 0.0394 (8) | |
H11 | 0.6448 | −0.3865 | 0.5131 | 0.047* | |
C12 | 0.7563 (3) | −0.2396 (3) | 0.5055 (2) | 0.0344 (7) | |
C13 | 0.8643 (3) | −0.1944 (3) | 0.4740 (2) | 0.0314 (7) | |
N1 | 0.9972 (3) | 0.1047 (2) | 0.2840 (2) | 0.0343 (6) | |
N2 | 1.0003 (3) | −0.1265 (2) | 0.3190 (2) | 0.0326 (6) | |
N3 | 0.6808 (3) | 0.0902 (3) | 0.3379 (2) | 0.0450 (7) | |
O1 | 0.9028 (2) | −0.08086 (17) | 0.49007 (15) | 0.0322 (5) | |
O2 | 0.7906 (3) | 0.13349 (19) | 0.38969 (19) | 0.0425 (6) | |
O3 | 0.5783 (3) | 0.1497 (3) | 0.3244 (2) | 0.0759 (9) | |
O4 | 0.6836 (3) | −0.0106 (2) | 0.3020 (2) | 0.0554 (7) | |
Br1 | 0.65460 (4) | −0.13772 (4) | 0.56476 (3) | 0.05240 (12) | |
Br2 | 0.73308 (4) | −0.59426 (3) | 0.42370 (3) | 0.04830 (12) | |
H12 | 0.925 (4) | −0.148 (3) | 0.276 (3) | 0.063 (13)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0386 (2) | 0.02697 (19) | 0.0346 (2) | 0.00306 (17) | 0.01283 (18) | −0.00048 (15) |
C1 | 0.045 (2) | 0.0328 (17) | 0.046 (2) | 0.0052 (17) | 0.0120 (17) | 0.0002 (15) |
C2 | 0.050 (2) | 0.0345 (18) | 0.053 (2) | −0.0009 (17) | 0.0119 (19) | 0.0097 (16) |
C3 | 0.046 (2) | 0.0450 (19) | 0.045 (2) | −0.0064 (18) | 0.0167 (18) | 0.0034 (16) |
C4 | 0.048 (2) | 0.0435 (19) | 0.042 (2) | −0.0010 (18) | 0.0188 (18) | −0.0030 (15) |
C5 | 0.0352 (19) | 0.0360 (17) | 0.0312 (19) | −0.0010 (15) | 0.0090 (15) | −0.0030 (13) |
C6 | 0.045 (2) | 0.0329 (17) | 0.051 (2) | 0.0065 (16) | 0.0208 (18) | 0.0013 (15) |
C7 | 0.041 (2) | 0.0278 (15) | 0.036 (2) | 0.0064 (15) | 0.0079 (15) | 0.0016 (13) |
C8 | 0.0329 (18) | 0.0285 (15) | 0.0303 (18) | 0.0021 (14) | 0.0034 (14) | 0.0039 (12) |
C9 | 0.043 (2) | 0.0276 (16) | 0.039 (2) | 0.0022 (16) | 0.0068 (16) | −0.0019 (14) |
C10 | 0.047 (2) | 0.0260 (15) | 0.0346 (19) | −0.0049 (16) | 0.0008 (16) | 0.0031 (13) |
C11 | 0.040 (2) | 0.0364 (18) | 0.038 (2) | −0.0081 (16) | 0.0044 (16) | 0.0049 (14) |
C12 | 0.0349 (19) | 0.0359 (17) | 0.0319 (19) | 0.0042 (15) | 0.0074 (15) | −0.0014 (13) |
C13 | 0.0328 (18) | 0.0306 (16) | 0.0273 (18) | 0.0009 (14) | 0.0015 (14) | 0.0005 (12) |
N1 | 0.0351 (16) | 0.0331 (14) | 0.0340 (16) | 0.0030 (13) | 0.0073 (12) | −0.0016 (11) |
N2 | 0.0336 (16) | 0.0290 (13) | 0.0352 (17) | 0.0028 (13) | 0.0090 (13) | −0.0009 (11) |
N3 | 0.048 (2) | 0.0483 (18) | 0.0425 (19) | 0.0085 (17) | 0.0188 (16) | 0.0103 (14) |
O1 | 0.0383 (13) | 0.0278 (10) | 0.0305 (12) | −0.0039 (10) | 0.0091 (10) | −0.0040 (9) |
O2 | 0.0408 (14) | 0.0330 (12) | 0.0528 (17) | 0.0040 (11) | 0.0107 (12) | −0.0054 (10) |
O3 | 0.0446 (17) | 0.101 (2) | 0.086 (2) | 0.0342 (18) | 0.0253 (17) | 0.0162 (18) |
O4 | 0.0572 (18) | 0.0503 (15) | 0.0514 (17) | −0.0076 (14) | 0.0007 (14) | 0.0011 (12) |
Br1 | 0.0483 (2) | 0.0566 (2) | 0.0579 (3) | −0.00440 (19) | 0.02369 (19) | −0.01596 (18) |
Br2 | 0.0671 (3) | 0.02887 (17) | 0.0439 (2) | −0.00976 (17) | 0.00495 (19) | 0.00350 (14) |
Cu1—O1 | 1.923 (2) | C7—C8 | 1.497 (4) |
Cu1—N1 | 1.985 (3) | C7—H7A | 0.9700 |
Cu1—N2 | 2.021 (3) | C7—H7B | 0.9700 |
Cu1—O2 | 2.038 (2) | C8—C9 | 1.399 (4) |
Cu1—O1i | 2.243 (2) | C8—C13 | 1.410 (4) |
C1—N1 | 1.347 (4) | C9—C10 | 1.371 (5) |
C1—C2 | 1.375 (5) | C9—H9 | 0.9300 |
C1—H1 | 0.9300 | C10—C11 | 1.372 (5) |
C2—C3 | 1.379 (5) | C10—Br2 | 1.913 (3) |
C2—H2 | 0.9300 | C11—C12 | 1.396 (4) |
C3—C4 | 1.387 (5) | C11—H11 | 0.9300 |
C3—H3 | 0.9300 | C12—C13 | 1.402 (4) |
C4—C5 | 1.378 (5) | C12—Br1 | 1.891 (3) |
C4—H4 | 0.9300 | C13—O1 | 1.341 (3) |
C5—N1 | 1.339 (4) | N2—H12 | 0.90 (4) |
C5—C6 | 1.509 (4) | N3—O3 | 1.230 (4) |
C6—N2 | 1.457 (4) | N3—O4 | 1.245 (4) |
C6—H6A | 0.9700 | N3—O2 | 1.282 (4) |
C6—H6B | 0.9700 | O1—Cu1i | 2.243 (2) |
C7—N2 | 1.497 (4) | ||
O1—Cu1—N1 | 171.25 (10) | H7A—C7—H7B | 108.2 |
O1—Cu1—N2 | 94.09 (10) | C9—C8—C13 | 120.2 (3) |
N1—Cu1—N2 | 82.67 (11) | C9—C8—C7 | 120.5 (3) |
O1—Cu1—O2 | 93.51 (10) | C13—C8—C7 | 119.3 (3) |
N1—Cu1—O2 | 93.27 (11) | C10—C9—C8 | 119.7 (3) |
N2—Cu1—O2 | 150.47 (12) | C10—C9—H9 | 120.1 |
O1—Cu1—O1i | 79.63 (9) | C8—C9—H9 | 120.1 |
N1—Cu1—O1i | 93.86 (10) | C9—C10—C11 | 122.3 (3) |
N2—Cu1—O1i | 110.53 (11) | C9—C10—Br2 | 118.8 (3) |
O2—Cu1—O1i | 98.90 (9) | C11—C10—Br2 | 119.0 (3) |
N1—C1—C2 | 122.3 (3) | C10—C11—C12 | 118.1 (3) |
N1—C1—H1 | 118.9 | C10—C11—H11 | 121.0 |
C2—C1—H1 | 118.9 | C12—C11—H11 | 121.0 |
C1—C2—C3 | 118.9 (3) | C11—C12—C13 | 122.2 (3) |
C1—C2—H2 | 120.6 | C11—C12—Br1 | 117.6 (3) |
C3—C2—H2 | 120.6 | C13—C12—Br1 | 120.1 (2) |
C2—C3—C4 | 119.1 (3) | O1—C13—C12 | 121.4 (3) |
C2—C3—H3 | 120.4 | O1—C13—C8 | 121.1 (3) |
C4—C3—H3 | 120.4 | C12—C13—C8 | 117.5 (3) |
C5—C4—C3 | 118.9 (3) | C5—N1—C1 | 118.7 (3) |
C5—C4—H4 | 120.6 | C5—N1—Cu1 | 114.4 (2) |
C3—C4—H4 | 120.6 | C1—N1—Cu1 | 126.8 (2) |
N1—C5—C4 | 122.1 (3) | C6—N2—C7 | 113.3 (3) |
N1—C5—C6 | 114.8 (3) | C6—N2—Cu1 | 107.64 (19) |
C4—C5—C6 | 123.1 (3) | C7—N2—Cu1 | 112.4 (2) |
N2—C6—C5 | 110.8 (3) | C6—N2—H12 | 114 (3) |
N2—C6—H6A | 109.5 | C7—N2—H12 | 108 (3) |
C5—C6—H6A | 109.5 | Cu1—N2—H12 | 100 (2) |
N2—C6—H6B | 109.5 | O3—N3—O4 | 122.8 (4) |
C5—C6—H6B | 109.5 | O3—N3—O2 | 119.3 (3) |
H6A—C6—H6B | 108.1 | O4—N3—O2 | 117.9 (3) |
N2—C7—C8 | 110.0 (3) | C13—O1—Cu1 | 119.73 (19) |
N2—C7—H7A | 109.7 | C13—O1—Cu1i | 126.11 (18) |
C8—C7—H7A | 109.7 | Cu1—O1—Cu1i | 100.37 (9) |
N2—C7—H7B | 109.7 | N3—O2—Cu1 | 106.3 (2) |
C8—C7—H7B | 109.7 | ||
N1—C1—C2—C3 | 0.0 (6) | O1i—Cu1—N1—C5 | 96.5 (2) |
C1—C2—C3—C4 | −0.3 (6) | N2—Cu1—N1—C1 | 169.3 (3) |
C2—C3—C4—C5 | −0.4 (5) | O2—Cu1—N1—C1 | 18.7 (3) |
C3—C4—C5—N1 | 1.3 (5) | O1i—Cu1—N1—C1 | −80.5 (3) |
C3—C4—C5—C6 | −175.3 (3) | C5—C6—N2—C7 | −158.1 (3) |
N1—C5—C6—N2 | 24.0 (4) | C5—C6—N2—Cu1 | −33.1 (3) |
C4—C5—C6—N2 | −159.2 (3) | C8—C7—N2—C6 | −176.0 (3) |
N2—C7—C8—C9 | 122.3 (3) | C8—C7—N2—Cu1 | 61.6 (3) |
N2—C7—C8—C13 | −57.5 (4) | O1—Cu1—N2—C6 | −146.0 (2) |
C13—C8—C9—C10 | 0.4 (5) | N1—Cu1—N2—C6 | 25.8 (2) |
C7—C8—C9—C10 | −179.4 (3) | O2—Cu1—N2—C6 | 109.5 (3) |
C8—C9—C10—C11 | 0.6 (5) | O1i—Cu1—N2—C6 | −65.6 (2) |
C8—C9—C10—Br2 | 179.5 (2) | O1—Cu1—N2—C7 | −20.5 (2) |
C9—C10—C11—C12 | −0.6 (5) | N1—Cu1—N2—C7 | 151.3 (2) |
Br2—C10—C11—C12 | −179.6 (2) | O2—Cu1—N2—C7 | −125.1 (2) |
C10—C11—C12—C13 | −0.3 (5) | O1i—Cu1—N2—C7 | 59.9 (2) |
C10—C11—C12—Br1 | 177.3 (3) | C12—C13—O1—Cu1 | −132.0 (3) |
C11—C12—C13—O1 | −178.5 (3) | C8—C13—O1—Cu1 | 48.3 (4) |
Br1—C12—C13—O1 | 3.9 (4) | C12—C13—O1—Cu1i | 95.7 (3) |
C11—C12—C13—C8 | 1.2 (5) | C8—C13—O1—Cu1i | −84.0 (3) |
Br1—C12—C13—C8 | −176.4 (2) | N2—Cu1—O1—C13 | −32.5 (2) |
C9—C8—C13—O1 | 178.5 (3) | O2—Cu1—O1—C13 | 119.0 (2) |
C7—C8—C13—O1 | −1.7 (4) | O1i—Cu1—O1—C13 | −142.6 (3) |
C9—C8—C13—C12 | −1.2 (5) | N2—Cu1—O1—Cu1i | 110.14 (11) |
C7—C8—C13—C12 | 178.6 (3) | O2—Cu1—O1—Cu1i | −98.42 (10) |
C4—C5—N1—C1 | −1.5 (5) | O1i—Cu1—O1—Cu1i | 0.0 |
C6—C5—N1—C1 | 175.3 (3) | O3—N3—O2—Cu1 | −175.6 (3) |
C4—C5—N1—Cu1 | −178.7 (3) | O4—N3—O2—Cu1 | 3.1 (3) |
C6—C5—N1—Cu1 | −1.9 (4) | O1—Cu1—O2—N3 | −84.6 (2) |
C2—C1—N1—C5 | 0.9 (5) | N1—Cu1—O2—N3 | 101.0 (2) |
C2—C1—N1—Cu1 | 177.7 (3) | N2—Cu1—O2—N3 | 20.1 (3) |
N2—Cu1—N1—C5 | −13.7 (2) | O1i—Cu1—O2—N3 | −164.6 (2) |
O2—Cu1—N1—C5 | −164.4 (2) |
Symmetry code: (i) −x+2, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Cu2(C13H11Br2N2O)2(NO3)2] |
Mr | 993.22 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 290 |
a, b, c (Å) | 10.385 (5), 11.252 (5), 14.074 (5) |
β (°) | 104.810 (5) |
V (Å3) | 1589.9 (12) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 6.42 |
Crystal size (mm) | 0.24 × 0.16 × 0.13 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.30, 0.43 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14979, 3629, 2707 |
Rint | 0.054 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.035, 0.071, 1.05 |
No. of reflections | 3629 |
No. of parameters | 212 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.48, −0.49 |
Computer programs: PROCESS-AUTO (Rigaku, 1998), PROCESS-AUTO, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1990), SHELXL97.
Cu1—O1 | 1.923 (2) | Cu1—O2 | 2.038 (2) |
Cu1—N1 | 1.985 (3) | Cu1—O1i | 2.243 (2) |
Cu1—N2 | 2.021 (3) |
Symmetry code: (i) −x+2, −y, −z+1. |
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The synthesis and characterization of binuclear copper(II) compounds have received increasing interest in bio-inorganic chemistry (Solomon et al., 1996) and catalysis (Collman, Zhong, Zhang & Costanzo, 2001; Collman, Zhong, Zeng & Costanzo, 2001). It is well known that the phenolate anion is a good bridging ligand for the construction of binuclear transition metal compounds (Gavrilova & Bosnich 2004; Yang et al., 2006). Modification of the phenolate anion in its ortho position can lead to the formation of stable binuclear compounds through chelation (Xu, et al., 2005). The structure of a new binuclear complex [Cu2(dmp)2(NO3)2], (I), where dmp is 2,4-dibromo-6-((pyridine-2-ylmethylamino)methyl)phenol, is presented here.
As shown in Fig. 1, the title compound, [Cu2(C13H11Br2N2O)(NO3)2], contains a binuclear copper(II) unit bridged by two phenolate O atoms with a Cu···Cu distance of 3.207 (4) Å. Each CuII atom is chelated by one dmp ligand and is also coordinated by a nitrate O atom. Finally, the trigonal-bipyramidal coordination environment is completed by bond to the phenolate O atom from another dmp ligand. The axial positions of the trigonal-bipyramid are occupied by one phenolate O atom and one pyridine N atom with the O—Cu—N angle being 171.25 (10)°.