Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807024671/cf2103sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807024671/cf2103Isup2.hkl |
CCDC reference: 654810
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.005 Å
- R factor = 0.040
- wR factor = 0.085
- Data-to-parameter ratio = 10.7
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT223_ALERT_4_B Large Solvent/Anion H Ueq(max)/Ueq(min) ... 4.52 Ratio
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 13 PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.62 Ratio PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 43 C11 -N11 -CU1 -N11 22.00 5.00 1.555 1.555 1.555 3.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 44 N12 -N11 -CU1 -N11 -155.00 5.00 1.555 1.555 1.555 3.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 57 C31 -N31 -CU1 -N31 1.00 0.00 1.555 1.555 1.555 3.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 58 N32 -N31 -CU1 -N31 17.00 0.00 1.555 1.555 1.555 3.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 71 C21 -N21 -CU1 -N21 -1.50 0.40 1.555 1.555 1.555 3.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 72 N22 -N21 -CU1 -N21 163.16 0.15 1.555 1.555 1.555 3.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 Cl
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Cu1 (1) 1.25
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 12 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 10 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For related literature, see: Allen et al. (1987); Astley et al. (1993); Kitajima et al. (1990); Martini et al. (2002); Orpen et al. (1989); Qiu et al. (1994).
The title compound was prepared by the previously published procedure (Martini et al., 2002) using copper(II) chloride dihydrate and tris(1-pyrazolyl)methane as starting materials and a reaction time of 24 h. Suitable crystals for X-ray study were obtained by vapour diffusion of diethyl ether into a methanol solution of (I) at 278 K. Anal. Cal. for CuC22H28N12Cl2O: C, 42.1; H, 4.5; N, 26.8. Found: C, 42.4; H, 4.0; N, 28.4%. IR (KBr pellet): 3092.0 [s, ν (C–H)], 1630.2 and 1518.4 [s, ν (C?C), ν (N?C), HC(pz)3]. EPR (90 K): g = 2.0732; aCu = 168; aN = 12.5. FAB+—MS, m/z: 626 [M]+, 611 [M – O]+, 561 [M – pz]+, 528 [M – 2pz +Cl]+, 493 [M – 2pz]+. FAB-–MS, m/z: 35 [Cl]-–.
All H atoms were located in a difference map and refined freely, giving C—H = 0.86 (3)–0.99 (4)° and O—H = 0.76 (4) Å.
Copper complexes of tripodal N3-donor ligands are of significance from a bioinorganic point of view since, for example, the N3–1igand coordination can mimic some spectroscopic features of blue copper proteins (Kitajima et al., 1990; Qiu et al., 1994). Compared with the enormous number of synthetic and structural studies of poly(1-pyrazolyl)borate Cu(II) comp1exes, only a few studies have been reported on the analogous poly(1-pyrazolyl)methane derivatives (Astley et al., 1993; Martini et al., 2002). We describe here a copper(II) complex containing tris(1-pyrazolyl)methane ligands, (I).
The structure of (I) (Fig. 1) consists of discrete centrosymmetric octahedral mononuclear CuII species with two tris(1-pyrazolyl)methane ligands, Cl- counter-ions, and methanol of crystallization. The bonding parameters are similar to those of the analogous complexes [Cu{HC(pz)3}2](NO3)2 and [Cu{HC(pz)3}2](ClO4)2 (Martini et al., 2002).
The Cu—N distances are close to those for [Cu{HC(pz)3}2](ClO4)2 (Martini et al., 2002). Two short Cu—N distances, approximately 2.0 Å, and one long, approximately 2.4 Å, are observed in both cases, consistent with Jahn-Teller distortion. All other bond lengths are normal (Allen et al., 1987; Orpen et al., 1989).
For related literature, see: Allen et al. (1987); Astley et al. (1993); Kitajima et al. (1990); Martini et al. (2002); Orpen et al. (1989); Qiu et al. (1994).
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Cu(C10H10N6)2]Cl2·2CH4O | F(000) = 646 |
Mr = 627.00 | Dx = 1.458 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71069 Å |
a = 8.5069 (13) Å | Cell parameters from 829 reflections |
b = 10.4307 (16) Å | θ = 2.5–22.6° |
c = 16.101 (3) Å | µ = 1.00 mm−1 |
β = 91.574 (8)° | T = 150 K |
V = 1428.1 (4) Å3 | Block, blue |
Z = 2 | 0.10 × 0.08 × 0.06 mm |
Bruker SMART CCD area-detector diffractometer | 2497 independent reflections |
Radiation source: fine-focus sealed tube | 1871 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.058 |
φ and ω scans | θmax = 25.3°, θmin = 3.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | h = −9→8 |
Tmin = 0.907, Tmax = 0.943 | k = −12→8 |
6690 measured reflections | l = −19→19 |
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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.085 | All H-atom parameters refined |
S = 0.97 | w = 1/[σ2(Fo2) + (0.0365P)2] where P = (Fo2 + 2Fc2)/3 |
2497 reflections | (Δ/σ)max = 0.001 |
234 parameters | Δρmax = 0.33 e Å−3 |
0 restraints | Δρmin = −0.34 e Å−3 |
[Cu(C10H10N6)2]Cl2·2CH4O | V = 1428.1 (4) Å3 |
Mr = 627.00 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 8.5069 (13) Å | µ = 1.00 mm−1 |
b = 10.4307 (16) Å | T = 150 K |
c = 16.101 (3) Å | 0.10 × 0.08 × 0.06 mm |
β = 91.574 (8)° |
Bruker SMART CCD area-detector diffractometer | 2497 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | 1871 reflections with I > 2σ(I) |
Tmin = 0.907, Tmax = 0.943 | Rint = 0.058 |
6690 measured reflections |
R[F2 > 2σ(F2)] = 0.040 | 0 restraints |
wR(F2) = 0.085 | All H-atom parameters refined |
S = 0.97 | Δρmax = 0.33 e Å−3 |
2497 reflections | Δρmin = −0.34 e Å−3 |
234 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 | ||
C1 | 0.1681 (4) | 0.2505 (3) | −0.05452 (19) | 0.0131 (7) | |
C10 | −0.0476 (7) | 0.3472 (4) | 0.2225 (3) | 0.0405 (11) | |
C11 | 0.2292 (4) | −0.0536 (3) | −0.1423 (2) | 0.0181 (8) | |
C12 | 0.3208 (4) | 0.1382 (3) | −0.16536 (19) | 0.0173 (8) | |
C13 | 0.3323 (4) | 0.0143 (3) | −0.1904 (2) | 0.0198 (8) | |
C21 | 0.2827 (4) | 0.1359 (3) | 0.1412 (2) | 0.0169 (7) | |
C22 | 0.3558 (4) | 0.2975 (3) | 0.0643 (2) | 0.0163 (7) | |
C23 | 0.3904 (4) | 0.2372 (3) | 0.1373 (2) | 0.0200 (8) | |
C31 | −0.2408 (4) | 0.2123 (3) | −0.0468 (2) | 0.0183 (8) | |
C32 | −0.0855 (4) | 0.3708 (3) | −0.0796 (2) | 0.0182 (8) | |
C33 | −0.2401 (4) | 0.3394 (3) | −0.0739 (2) | 0.0209 (8) | |
N11 | 0.1550 (3) | 0.0229 (2) | −0.09019 (15) | 0.0142 (6) | |
N12 | 0.2121 (3) | 0.1422 (2) | −0.10577 (15) | 0.0135 (6) | |
N21 | 0.1868 (3) | 0.1328 (2) | 0.07567 (16) | 0.0154 (6) | |
N22 | 0.2318 (3) | 0.2345 (2) | 0.02865 (16) | 0.0139 (6) | |
N31 | −0.0963 (3) | 0.1681 (2) | −0.03537 (16) | 0.0143 (6) | |
N32 | 0.0001 (3) | 0.2665 (2) | −0.05655 (16) | 0.0141 (6) | |
O10 | −0.0946 (3) | 0.3534 (2) | 0.13793 (16) | 0.0265 (6) | |
Cl1 | 0.38445 (10) | 0.47169 (6) | −0.14522 (5) | 0.0183 (2) | |
Cu1 | 0.0000 | 0.0000 | 0.0000 | 0.01293 (17) | |
H1 | 0.214 (3) | 0.329 (3) | −0.0776 (17) | 0.008 (7)* | |
H10 | −0.170 (5) | 0.390 (3) | 0.132 (2) | 0.031 (13)* | |
H10A | −0.138 (8) | 0.321 (6) | 0.254 (4) | 0.14 (3)* | |
H10B | −0.018 (5) | 0.434 (4) | 0.243 (3) | 0.050 (12)* | |
H10C | 0.036 (7) | 0.293 (5) | 0.229 (3) | 0.11 (2)* | |
H11 | 0.205 (4) | −0.141 (3) | −0.1439 (19) | 0.021 (9)* | |
H12 | 0.366 (4) | 0.207 (3) | −0.181 (2) | 0.020 (9)* | |
H13 | 0.396 (4) | −0.016 (3) | −0.2311 (19) | 0.015 (9)* | |
H21 | 0.280 (4) | 0.074 (3) | 0.185 (2) | 0.021 (9)* | |
H22 | 0.397 (4) | 0.370 (3) | 0.0392 (18) | 0.017 (8)* | |
H23 | 0.468 (4) | 0.258 (3) | 0.173 (2) | 0.029 (10)* | |
H31 | −0.331 (4) | 0.159 (3) | −0.038 (2) | 0.029 (10)* | |
H32 | −0.027 (4) | 0.444 (3) | −0.0968 (18) | 0.010 (8)* | |
H33 | −0.334 (4) | 0.391 (3) | −0.0892 (19) | 0.023 (9)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.013 (2) | 0.0095 (15) | 0.0171 (17) | −0.0023 (13) | 0.0011 (14) | 0.0012 (13) |
C10 | 0.041 (3) | 0.040 (2) | 0.040 (3) | 0.008 (2) | −0.015 (2) | −0.006 (2) |
C11 | 0.018 (2) | 0.0151 (16) | 0.0214 (19) | 0.0027 (14) | 0.0051 (15) | −0.0027 (14) |
C12 | 0.018 (2) | 0.0179 (17) | 0.0165 (18) | 0.0002 (14) | 0.0068 (15) | 0.0042 (13) |
C13 | 0.020 (2) | 0.0203 (17) | 0.0194 (18) | 0.0031 (15) | 0.0116 (16) | −0.0001 (15) |
C21 | 0.018 (2) | 0.0168 (16) | 0.0159 (18) | −0.0037 (14) | 0.0023 (15) | 0.0014 (13) |
C22 | 0.015 (2) | 0.0128 (16) | 0.0215 (18) | −0.0038 (14) | 0.0059 (15) | −0.0021 (13) |
C23 | 0.017 (2) | 0.0245 (17) | 0.0189 (19) | −0.0029 (15) | −0.0024 (16) | −0.0042 (15) |
C31 | 0.014 (2) | 0.0191 (16) | 0.0220 (19) | 0.0024 (15) | 0.0014 (15) | −0.0013 (14) |
C32 | 0.028 (2) | 0.0092 (15) | 0.0175 (17) | 0.0017 (14) | 0.0008 (15) | 0.0029 (13) |
C33 | 0.016 (2) | 0.0179 (16) | 0.029 (2) | 0.0073 (15) | 0.0013 (16) | 0.0046 (15) |
N11 | 0.0165 (17) | 0.0097 (12) | 0.0166 (14) | −0.0024 (11) | 0.0029 (12) | 0.0037 (10) |
N12 | 0.0163 (17) | 0.0104 (12) | 0.0140 (14) | −0.0027 (11) | 0.0043 (12) | 0.0015 (10) |
N21 | 0.0144 (17) | 0.0157 (13) | 0.0160 (14) | −0.0033 (11) | 0.0015 (12) | 0.0017 (11) |
N22 | 0.0144 (16) | 0.0096 (12) | 0.0180 (15) | −0.0020 (11) | 0.0035 (12) | 0.0028 (11) |
N31 | 0.0098 (17) | 0.0117 (12) | 0.0216 (15) | −0.0038 (11) | 0.0041 (12) | 0.0020 (11) |
N32 | 0.0119 (17) | 0.0114 (12) | 0.0191 (15) | 0.0014 (11) | 0.0029 (12) | 0.0013 (11) |
O10 | 0.0262 (18) | 0.0226 (13) | 0.0306 (15) | 0.0054 (12) | −0.0027 (13) | −0.0015 (11) |
Cl1 | 0.0164 (5) | 0.0161 (4) | 0.0225 (4) | −0.0028 (3) | 0.0027 (4) | 0.0023 (3) |
Cu1 | 0.0121 (3) | 0.0095 (3) | 0.0174 (3) | 0.0000 (2) | 0.0042 (2) | 0.0027 (2) |
C1—N32 | 1.438 (4) | C22—H22 | 0.93 (3) |
C1—N22 | 1.440 (4) | C23—H23 | 0.89 (4) |
C1—N12 | 1.454 (4) | C31—N31 | 1.321 (4) |
C1—H1 | 0.99 (3) | C31—C33 | 1.396 (4) |
C10—O10 | 1.411 (5) | C31—H31 | 0.96 (3) |
C10—H10A | 0.98 (7) | C32—N32 | 1.355 (4) |
C10—H10B | 0.99 (4) | C32—C33 | 1.361 (5) |
C10—H10C | 0.91 (6) | C32—H32 | 0.96 (3) |
C11—N11 | 1.329 (4) | C33—H33 | 0.98 (3) |
C11—C13 | 1.382 (5) | N11—N12 | 1.362 (3) |
C11—H11 | 0.93 (3) | N11—Cu1 | 2.002 (3) |
C12—N12 | 1.352 (4) | N21—N22 | 1.364 (3) |
C12—C13 | 1.358 (4) | N21—Cu1 | 2.413 (2) |
C12—H12 | 0.86 (3) | N31—N32 | 1.363 (3) |
C13—H13 | 0.92 (3) | N31—Cu1 | 2.011 (2) |
C21—N21 | 1.316 (4) | O10—H10 | 0.76 (4) |
C21—C23 | 1.401 (4) | Cu1—N11i | 2.002 (3) |
C21—H21 | 0.95 (3) | Cu1—N31i | 2.011 (2) |
C22—N22 | 1.357 (4) | Cu1—N21i | 2.413 (2) |
C22—C23 | 1.357 (5) | ||
N32—C1—N22 | 112.5 (3) | C32—C33—H33 | 128.9 (18) |
N32—C1—N12 | 110.4 (2) | C31—C33—H33 | 125.7 (18) |
N22—C1—N12 | 110.0 (2) | C11—N11—N12 | 104.7 (2) |
N32—C1—H1 | 107.5 (17) | C11—N11—Cu1 | 136.0 (2) |
N22—C1—H1 | 107.7 (16) | N12—N11—Cu1 | 119.17 (18) |
N12—C1—H1 | 108.6 (16) | C12—N12—N11 | 110.9 (2) |
O10—C10—H10A | 108 (4) | C12—N12—C1 | 128.2 (2) |
O10—C10—H10B | 110 (2) | N11—N12—C1 | 120.5 (2) |
H10A—C10—H10B | 106 (4) | C21—N21—N22 | 104.4 (2) |
O10—C10—H10C | 110 (4) | C21—N21—Cu1 | 143.5 (2) |
H10A—C10—H10C | 113 (5) | N22—N21—Cu1 | 110.92 (18) |
H10B—C10—H10C | 109 (4) | C22—N22—N21 | 111.6 (3) |
N11—C11—C13 | 111.5 (3) | C22—N22—C1 | 127.3 (3) |
N11—C11—H11 | 120 (2) | N21—N22—C1 | 120.1 (2) |
C13—C11—H11 | 129 (2) | C31—N31—N32 | 105.5 (2) |
N12—C12—C13 | 107.3 (3) | C31—N31—Cu1 | 135.5 (2) |
N12—C12—H12 | 121 (2) | N32—N31—Cu1 | 118.98 (19) |
C13—C12—H12 | 132 (2) | C32—N32—N31 | 110.5 (3) |
C12—C13—C11 | 105.6 (3) | C32—N32—C1 | 128.8 (3) |
C12—C13—H13 | 126.0 (19) | N31—N32—C1 | 120.7 (2) |
C11—C13—H13 | 128.4 (19) | C10—O10—H10 | 112 (3) |
N21—C21—C23 | 111.9 (3) | N11—Cu1—N11i | 180.00 (14) |
N21—C21—H21 | 123 (2) | N11—Cu1—N31 | 87.82 (10) |
C23—C21—H21 | 125 (2) | N11i—Cu1—N31 | 92.18 (10) |
N22—C22—C23 | 106.8 (3) | N11—Cu1—N31i | 92.18 (10) |
N22—C22—H22 | 120.5 (19) | N11i—Cu1—N31i | 87.82 (10) |
C23—C22—H22 | 132.6 (19) | N31—Cu1—N31i | 180.00 (15) |
C22—C23—C21 | 105.2 (3) | N11—Cu1—N21 | 81.95 (9) |
C22—C23—H23 | 126 (2) | N11i—Cu1—N21 | 98.05 (9) |
C21—C23—H23 | 129 (2) | N31—Cu1—N21 | 84.24 (9) |
N31—C31—C33 | 111.3 (3) | N31i—Cu1—N21 | 95.76 (9) |
N31—C31—H31 | 121 (2) | N11—Cu1—N21i | 98.05 (9) |
C33—C31—H31 | 127 (2) | N11i—Cu1—N21i | 81.95 (9) |
N32—C32—C33 | 107.6 (3) | N31—Cu1—N21i | 95.76 (9) |
N32—C32—H32 | 116.0 (18) | N31i—Cu1—N21i | 84.24 (9) |
C33—C32—H32 | 136.4 (18) | N21—Cu1—N21i | 180.00 (14) |
C32—C33—C31 | 105.2 (3) | ||
N12—C12—C13—C11 | −1.2 (4) | C31—N31—N32—C1 | −177.7 (3) |
N11—C11—C13—C12 | 0.6 (4) | Cu1—N31—N32—C1 | 0.6 (3) |
N22—C22—C23—C21 | 1.0 (4) | N22—C1—N32—C32 | 114.0 (3) |
N21—C21—C23—C22 | −0.2 (4) | N12—C1—N32—C32 | −122.7 (3) |
N32—C32—C33—C31 | −0.2 (4) | N22—C1—N32—N31 | −67.7 (3) |
N31—C31—C33—C32 | 0.8 (4) | N12—C1—N32—N31 | 55.6 (3) |
C13—C11—N11—N12 | 0.2 (4) | C11—N11—Cu1—N11i | 22 (5) |
C13—C11—N11—Cu1 | −177.0 (2) | N12—N11—Cu1—N11i | −155 (5) |
C13—C12—N12—N11 | 1.4 (4) | C11—N11—Cu1—N31 | −145.0 (3) |
C13—C12—N12—C1 | 174.0 (3) | N12—N11—Cu1—N31 | 38.1 (2) |
C11—N11—N12—C12 | −1.0 (3) | C11—N11—Cu1—N31i | 35.0 (3) |
Cu1—N11—N12—C12 | 176.8 (2) | N12—N11—Cu1—N31i | −141.9 (2) |
C11—N11—N12—C1 | −174.2 (3) | C11—N11—Cu1—N21 | 130.5 (3) |
Cu1—N11—N12—C1 | 3.5 (4) | N12—N11—Cu1—N21 | −46.4 (2) |
N32—C1—N12—C12 | 129.8 (3) | C11—N11—Cu1—N21i | −49.5 (3) |
N22—C1—N12—C12 | −105.5 (3) | N12—N11—Cu1—N21i | 133.6 (2) |
N32—C1—N12—N11 | −58.3 (3) | C31—N31—Cu1—N11 | 137.2 (3) |
N22—C1—N12—N11 | 66.4 (3) | N32—N31—Cu1—N11 | −40.4 (2) |
C23—C21—N21—N22 | −0.6 (3) | C31—N31—Cu1—N11i | −42.8 (3) |
C23—C21—N21—Cu1 | 164.7 (3) | N32—N31—Cu1—N11i | 139.6 (2) |
C23—C22—N22—N21 | −1.4 (4) | C31—N31—Cu1—N31i | −14 (25) |
C23—C22—N22—C1 | −169.9 (3) | N32—N31—Cu1—N31i | 169 (25) |
C21—N21—N22—C22 | 1.2 (3) | C31—N31—Cu1—N21 | −140.7 (3) |
Cu1—N21—N22—C22 | −169.5 (2) | N32—N31—Cu1—N21 | 41.7 (2) |
C21—N21—N22—C1 | 170.6 (3) | C31—N31—Cu1—N21i | 39.3 (3) |
Cu1—N21—N22—C1 | 0.0 (3) | N32—N31—Cu1—N21i | −138.3 (2) |
N32—C1—N22—C22 | −131.0 (3) | C21—N21—Cu1—N11 | −118.9 (4) |
N12—C1—N22—C22 | 105.5 (3) | N22—N21—Cu1—N11 | 45.76 (19) |
N32—C1—N22—N21 | 61.4 (3) | C21—N21—Cu1—N11i | 61.1 (4) |
N12—C1—N22—N21 | −62.1 (4) | N22—N21—Cu1—N11i | −134.24 (19) |
C33—C31—N31—N32 | −1.0 (4) | C21—N21—Cu1—N31 | 152.5 (4) |
C33—C31—N31—Cu1 | −178.9 (2) | N22—N21—Cu1—N31 | −42.85 (19) |
C33—C32—N32—N31 | −0.5 (4) | C21—N21—Cu1—N31i | −27.5 (4) |
C33—C32—N32—C1 | 178.0 (3) | N22—N21—Cu1—N31i | 137.15 (19) |
C31—N31—N32—C32 | 0.9 (3) | C21—N21—Cu1—N21i | −1.5 (4) |
Cu1—N31—N32—C32 | 179.2 (2) | N22—N21—Cu1—N21i | 163.16 (15) |
Symmetry code: (i) −x, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | [Cu(C10H10N6)2]Cl2·2CH4O |
Mr | 627.00 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 150 |
a, b, c (Å) | 8.5069 (13), 10.4307 (16), 16.101 (3) |
β (°) | 91.574 (8) |
V (Å3) | 1428.1 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.00 |
Crystal size (mm) | 0.10 × 0.08 × 0.06 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2003) |
Tmin, Tmax | 0.907, 0.943 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6690, 2497, 1871 |
Rint | 0.058 |
(sin θ/λ)max (Å−1) | 0.601 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.085, 0.97 |
No. of reflections | 2497 |
No. of parameters | 234 |
H-atom treatment | All H-atom parameters refined |
Δρmax, Δρmin (e Å−3) | 0.33, −0.34 |
Computer programs: SMART (Bruker, 2000), SMART, SAINT (Bruker, 2000), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997), WinGX (Farrugia, 1999).
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Copper complexes of tripodal N3-donor ligands are of significance from a bioinorganic point of view since, for example, the N3–1igand coordination can mimic some spectroscopic features of blue copper proteins (Kitajima et al., 1990; Qiu et al., 1994). Compared with the enormous number of synthetic and structural studies of poly(1-pyrazolyl)borate Cu(II) comp1exes, only a few studies have been reported on the analogous poly(1-pyrazolyl)methane derivatives (Astley et al., 1993; Martini et al., 2002). We describe here a copper(II) complex containing tris(1-pyrazolyl)methane ligands, (I).
The structure of (I) (Fig. 1) consists of discrete centrosymmetric octahedral mononuclear CuII species with two tris(1-pyrazolyl)methane ligands, Cl- counter-ions, and methanol of crystallization. The bonding parameters are similar to those of the analogous complexes [Cu{HC(pz)3}2](NO3)2 and [Cu{HC(pz)3}2](ClO4)2 (Martini et al., 2002).
The Cu—N distances are close to those for [Cu{HC(pz)3}2](ClO4)2 (Martini et al., 2002). Two short Cu—N distances, approximately 2.0 Å, and one long, approximately 2.4 Å, are observed in both cases, consistent with Jahn-Teller distortion. All other bond lengths are normal (Allen et al., 1987; Orpen et al., 1989).