Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801019171/br6030sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801019171/br6030Isup2.hkl |
CCDC reference: 177184
Key indicators
- Single-crystal X-ray study
- T = 301 K
- Mean (C-C) = 0.008 Å
- R factor = 0.038
- wR factor = 0.095
- Data-to-parameter ratio = 17.1
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_213 Alert C Atom C23 has ADP max/min Ratio ........... 4.00 prolate PLAT_420 Alert C D-H Without Acceptor N3 - H3A ? General Notes
ABSTY_01 Extra text has been found in the _exptl_absorpt_correction_type field, which should be only a single keyword. A literature citation should be included in the _exptl_absorpt_process_details field.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check
Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1993); cell refinement: SHELXL97 (Sheldrick, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97; molecular graphics: PLATON (Spek, 2000); software used to prepare material for publication: SHELXL97.
[CuZnBr2(C17H16N2O2)(CH3)2(C5H11N)] | Z = 4 |
Mr = 682.25 | Dx = 1.736 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 10.659 (2) Å | θ = 1.9–26.0° |
b = 14.550 (1) Å | µ = 4.82 mm−1 |
c = 16.992 (3) Å | T = 301 K |
β = 97.91 (2)° | Prism, light green |
V = 2610.2 (7) Å3 | 0.35 × 0.30 × 0.25 mm |
Enraf-Nonius CAD-4 diffractometer | Rint = 0.041 |
ω/2θ scans | θmax = 26.0° |
Absorption correction: empirical (using intensity measurements) via ψ scans (Fair, 1990) | h = −13→6 |
Tmin = 0.202, Tmax = 0.300 | k = −17→0 |
8583 measured reflections | l = −20→20 |
5111 independent reflections | 3 standard reflections every 120 min |
3403 reflections with I > 2σ(I) | intensity decay: 1.2% |
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)] = 0.038 | H-atom parameters constrained |
wR(F2) = 0.095 | w = 1/[σ2(Fo2) + (0.0506P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max = 0.0001 |
5111 reflections | Δρmax = 0.82 e Å−3 |
299 parameters | Δρmin = −0.50 e Å−3 |
2 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0028 (3) |
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 | ||
Cu | 0.26737 (5) | 0.24855 (3) | 0.38658 (3) | 0.03827 (17) | |
Zn | 0.01432 (5) | 0.33604 (4) | 0.31450 (4) | 0.04724 (18) | |
Br1 | −0.15362 (5) | 0.37698 (4) | 0.38186 (5) | 0.0752 (2) | |
Br2 | −0.00582 (7) | 0.36447 (4) | 0.17715 (4) | 0.0739 (2) | |
O1 | 0.0950 (3) | 0.2132 (2) | 0.3395 (2) | 0.0439 (8) | |
O2 | 0.1876 (3) | 0.36854 (19) | 0.3681 (2) | 0.0503 (9) | |
N1 | 0.3244 (3) | 0.1197 (2) | 0.3859 (2) | 0.0388 (9) | |
N2 | 0.4351 (3) | 0.3058 (2) | 0.4167 (2) | 0.0410 (9) | |
N3 | 0.2296 (4) | 0.2350 (3) | 0.5169 (2) | 0.0461 (10) | |
C1 | 0.0476 (4) | 0.1310 (3) | 0.3183 (3) | 0.0398 (10) | |
C2 | −0.0823 (4) | 0.1221 (3) | 0.2899 (3) | 0.0497 (12) | |
C3 | −0.1330 (5) | 0.0379 (4) | 0.2681 (3) | 0.0566 (14) | |
C4 | −0.0566 (5) | −0.0409 (4) | 0.2730 (3) | 0.0555 (13) | |
C5 | 0.0677 (5) | −0.0326 (3) | 0.3005 (3) | 0.0482 (12) | |
C6 | 0.1237 (4) | 0.0526 (3) | 0.3246 (3) | 0.0389 (10) | |
C7 | 0.2559 (4) | 0.0517 (3) | 0.3563 (3) | 0.0415 (11) | |
C8 | 0.4517 (4) | 0.0936 (3) | 0.4248 (3) | 0.0493 (12) | |
C9 | 0.5573 (4) | 0.1582 (3) | 0.4087 (3) | 0.0473 (12) | |
C10 | 0.5457 (4) | 0.2494 (3) | 0.4512 (3) | 0.0511 (12) | |
C11 | 0.5604 (5) | 0.1715 (4) | 0.3206 (3) | 0.0622 (15) | |
C12 | 0.6831 (5) | 0.1151 (4) | 0.4470 (4) | 0.0740 (18) | |
C13 | 0.4578 (4) | 0.3915 (3) | 0.4117 (3) | 0.0462 (11) | |
C14 | 0.3697 (4) | 0.4651 (3) | 0.3890 (3) | 0.0419 (11) | |
C15 | 0.4205 (5) | 0.5544 (3) | 0.3877 (3) | 0.0536 (13) | |
C16 | 0.3435 (6) | 0.6291 (3) | 0.3688 (4) | 0.0608 (15) | |
C17 | 0.2155 (6) | 0.6153 (3) | 0.3519 (4) | 0.0603 (15) | |
C18 | 0.1621 (5) | 0.5290 (3) | 0.3520 (4) | 0.0577 (14) | |
C19 | 0.2400 (4) | 0.4528 (3) | 0.3702 (3) | 0.0451 (11) | |
C20 | 0.2374 (6) | 0.3087 (5) | 0.5729 (4) | 0.0799 (19) | |
C21 | 0.1109 (7) | 0.3402 (6) | 0.5845 (5) | 0.110 (3) | |
C22 | 0.0399 (6) | 0.2659 (5) | 0.6135 (4) | 0.0709 (18) | |
C23 | 0.0281 (6) | 0.1957 (7) | 0.5528 (5) | 0.114 (3) | |
C24 | 0.1556 (6) | 0.1621 (4) | 0.5433 (4) | 0.0756 (17) | |
H2 | −0.1352 | 0.1749 | 0.2860 | 0.060* | |
H3 | −0.2209 | 0.0329 | 0.2493 | 0.068* | |
H3A | 0.3079 | 0.2094 | 0.5359 | 0.055* | |
H4 | −0.0918 | −0.0991 | 0.2573 | 0.067* | |
H5 | 0.1194 | −0.0860 | 0.3038 | 0.058* | |
H7 | 0.2978 | −0.0058 | 0.3553 | 0.050* | |
H8A | 0.4713 | 0.0312 | 0.4068 | 0.059* | |
H8B | 0.4503 | 0.0907 | 0.4828 | 0.059* | |
H10A | 0.5387 | 0.2370 | 0.5077 | 0.061* | |
H10B | 0.6240 | 0.2854 | 0.4493 | 0.061* | |
H11A | 0.6292 | 0.2138 | 0.3127 | 0.093* | |
H11B | 0.4795 | 0.1972 | 0.2960 | 0.093* | |
H11C | 0.5747 | 0.1121 | 0.2961 | 0.093* | |
H12A | 0.6809 | 0.1063 | 0.5040 | 0.111* | |
H12B | 0.7534 | 0.1561 | 0.4394 | 0.111* | |
H12C | 0.6950 | 0.0556 | 0.4221 | 0.111* | |
H13 | 0.5440 | 0.4091 | 0.4246 | 0.055* | |
H15 | 0.5094 | 0.5630 | 0.4001 | 0.064* | |
H16 | 0.3783 | 0.6891 | 0.3674 | 0.073* | |
H17 | 0.1618 | 0.6670 | 0.3399 | 0.072* | |
H18 | 0.0730 | 0.5216 | 0.3396 | 0.069* | |
H20A | 0.2853 | 0.3603 | 0.5535 | 0.096* | |
H20B | 0.2836 | 0.2877 | 0.6243 | 0.096* | |
H21A | 0.1182 | 0.3915 | 0.6231 | 0.131* | |
H21B | 0.0656 | 0.3631 | 0.5335 | 0.131* | |
H22A | −0.0449 | 0.2876 | 0.6229 | 0.085* | |
H22B | 0.0850 | 0.2415 | 0.6640 | 0.085* | |
H23A | −0.0137 | 0.2214 | 0.5019 | 0.137* | |
H23B | −0.0242 | 0.1444 | 0.5683 | 0.137* | |
H24A | 0.1979 | 0.1380 | 0.5947 | 0.091* | |
H24B | 0.1486 | 0.1114 | 0.5042 | 0.091* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu | 0.0297 (3) | 0.0407 (3) | 0.0443 (4) | 0.0001 (2) | 0.0046 (2) | −0.0009 (2) |
Zn | 0.0340 (3) | 0.0443 (3) | 0.0619 (4) | 0.0070 (3) | 0.0013 (2) | 0.0004 (2) |
Br1 | 0.0455 (3) | 0.0798 (4) | 0.1035 (6) | 0.0111 (3) | 0.0218 (3) | 0.0125 (3) |
Br2 | 0.0931 (5) | 0.0632 (4) | 0.0622 (5) | 0.0123 (3) | −0.0005 (3) | −0.0106 (3) |
O1 | 0.0313 (15) | 0.0399 (15) | 0.059 (2) | 0.0017 (14) | 0.0007 (14) | −0.0028 (13) |
O2 | 0.0344 (16) | 0.0371 (16) | 0.078 (3) | 0.0007 (15) | 0.0019 (16) | −0.0028 (13) |
N1 | 0.0310 (18) | 0.043 (2) | 0.042 (2) | 0.0041 (17) | 0.0059 (16) | 0.0032 (15) |
N2 | 0.0322 (18) | 0.048 (2) | 0.043 (3) | −0.0035 (17) | 0.0057 (17) | −0.0022 (15) |
N3 | 0.048 (2) | 0.058 (2) | 0.036 (2) | −0.0090 (18) | 0.0206 (19) | −0.0080 (18) |
C1 | 0.038 (2) | 0.046 (2) | 0.036 (3) | 0.0027 (19) | 0.007 (2) | −0.0064 (19) |
C2 | 0.033 (2) | 0.055 (3) | 0.060 (4) | 0.001 (2) | 0.005 (2) | −0.004 (2) |
C3 | 0.042 (3) | 0.063 (3) | 0.065 (4) | −0.002 (3) | 0.008 (2) | −0.015 (2) |
C4 | 0.057 (3) | 0.050 (3) | 0.059 (4) | −0.004 (2) | 0.009 (3) | −0.017 (2) |
C5 | 0.056 (3) | 0.044 (2) | 0.045 (3) | 0.003 (2) | 0.009 (2) | −0.004 (2) |
C6 | 0.041 (2) | 0.043 (2) | 0.033 (3) | 0.0041 (19) | 0.006 (2) | −0.0019 (19) |
C7 | 0.047 (2) | 0.040 (2) | 0.038 (3) | 0.0016 (19) | 0.006 (2) | 0.003 (2) |
C8 | 0.041 (3) | 0.055 (3) | 0.049 (3) | 0.003 (2) | −0.003 (2) | 0.008 (2) |
C9 | 0.031 (2) | 0.062 (3) | 0.048 (3) | −0.001 (2) | 0.001 (2) | 0.008 (2) |
C10 | 0.034 (2) | 0.065 (3) | 0.052 (3) | −0.001 (2) | −0.005 (2) | −0.004 (2) |
C11 | 0.044 (3) | 0.088 (4) | 0.057 (4) | −0.003 (3) | 0.014 (3) | 0.011 (3) |
C12 | 0.039 (3) | 0.087 (4) | 0.093 (5) | 0.006 (3) | −0.001 (3) | 0.016 (3) |
C13 | 0.033 (2) | 0.062 (3) | 0.044 (3) | −0.006 (2) | 0.007 (2) | −0.009 (2) |
C14 | 0.042 (2) | 0.047 (2) | 0.038 (3) | −0.005 (2) | 0.011 (2) | −0.010 (2) |
C15 | 0.058 (3) | 0.060 (3) | 0.043 (3) | −0.004 (2) | 0.007 (2) | −0.016 (3) |
C16 | 0.085 (4) | 0.044 (3) | 0.053 (4) | −0.008 (2) | 0.009 (3) | −0.015 (3) |
C17 | 0.073 (4) | 0.042 (3) | 0.066 (4) | −0.005 (2) | 0.008 (3) | 0.002 (2) |
C18 | 0.055 (3) | 0.042 (3) | 0.076 (4) | −0.005 (2) | 0.009 (3) | 0.002 (2) |
C19 | 0.046 (3) | 0.041 (2) | 0.049 (3) | −0.003 (2) | 0.008 (2) | −0.003 (2) |
C20 | 0.078 (4) | 0.099 (5) | 0.062 (5) | −0.020 (4) | 0.008 (3) | −0.004 (4) |
C21 | 0.099 (6) | 0.126 (7) | 0.100 (7) | −0.043 (5) | 0.001 (5) | 0.053 (5) |
C22 | 0.053 (3) | 0.113 (5) | 0.055 (4) | 0.014 (4) | 0.034 (3) | 0.032 (3) |
C23 | 0.055 (4) | 0.186 (9) | 0.102 (7) | 0.081 (7) | 0.012 (4) | −0.012 (5) |
C24 | 0.085 (4) | 0.090 (4) | 0.055 (4) | 0.006 (3) | 0.022 (3) | −0.011 (4) |
Cu—Zn | 3.0800 (9) | C11—H11B | 0.98 |
Cu—O1 | 1.969 (3) | C11—H11C | 0.98 |
Cu—O2 | 1.948 (3) | C12—H12A | 0.98 |
Cu—N1 | 1.972 (3) | C12—H12B | 0.98 |
Cu—N2 | 1.975 (3) | C12—H12C | 0.98 |
Cu—N3 | 2.312 (4) | C13—N2 | 1.274 (6) |
Zn—Br1 | 2.3309 (9) | C13—C14 | 1.442 (6) |
Zn—Br2 | 2.3508 (10) | C13—H13 | 0.95 |
Zn—O1 | 2.003 (3) | C14—C19 | 1.388 (6) |
Zn—O2 | 2.001 (3) | C14—C15 | 1.409 (6) |
N3—H3A | 0.9375 | C15—C16 | 1.373 (7) |
C1—O1 | 1.328 (5) | C15—H15 | 0.95 |
C1—C2 | 1.409 (6) | C16—C17 | 1.370 (8) |
C1—C6 | 1.395 (6) | C16—H16 | 0.95 |
C2—C3 | 1.369 (7) | C17—C18 | 1.379 (7) |
C2—H2 | 0.95 | C17—H17 | 0.95 |
C3—C4 | 1.402 (7) | C18—C19 | 1.394 (6) |
C3—H3 | 0.95 | C18—H18 | 0.95 |
C4—C5 | 1.348 (7) | C19—O2 | 1.346 (5) |
C4—H4 | 0.95 | C20—N3 | 1.428 (7) |
C5—C6 | 1.411 (6) | C20—C21 | 1.463 (9) |
C5—H5 | 0.95 | C20—H20A | 0.99 |
C6—C7 | 1.438 (6) | C20—H20B | 0.99 |
C7—N1 | 1.290 (5) | C21—C22 | 1.445 (9) |
C7—H7 | 0.95 | C21—H21A | 0.99 |
C8—N1 | 1.475 (5) | C21—H21B | 0.99 |
C8—C9 | 1.520 (7) | C22—C23 | 1.444 (10) |
C8—H8A | 0.99 | C22—H22A | 0.99 |
C8—H8B | 0.99 | C22—H22B | 0.99 |
C9—C11 | 1.514 (8) | C23—C24 | 1.474 (10) |
C9—C10 | 1.524 (7) | C23—H23A | 0.99 |
C9—C12 | 1.541 (6) | C23—H23B | 0.99 |
C10—N2 | 1.488 (6) | C24—N3 | 1.431 (7) |
C10—H10A | 0.99 | C24—H24A | 0.99 |
C10—H10B | 0.99 | C24—H24B | 0.99 |
C11—H11A | 0.98 | ||
O2—Cu—O1 | 78.84 (12) | C11—C9—C10 | 111.8 (4) |
O2—Cu—N1 | 168.33 (15) | C8—C9—C10 | 110.0 (4) |
O1—Cu—N1 | 91.17 (13) | C11—C9—C12 | 109.5 (4) |
O2—Cu—N2 | 91.32 (14) | C8—C9—C12 | 107.2 (4) |
O1—Cu—N2 | 167.54 (15) | C10—C9—C12 | 106.1 (4) |
N1—Cu—N2 | 97.70 (15) | N2—C10—C9 | 113.9 (4) |
O2—Cu—N3 | 95.80 (15) | N2—C13—C14 | 128.5 (4) |
O1—Cu—N3 | 95.22 (14) | C19—C14—C15 | 119.2 (4) |
N1—Cu—N3 | 91.07 (15) | C19—C14—C13 | 123.9 (4) |
N2—Cu—N3 | 93.34 (15) | C15—C14—C13 | 116.9 (4) |
O2—Cu—Zn | 39.37 (9) | C16—C15—C14 | 121.0 (5) |
O1—Cu—Zn | 39.55 (9) | C17—C16—C15 | 118.7 (5) |
N1—Cu—Zn | 130.12 (10) | C16—C17—C18 | 122.2 (5) |
N2—Cu—Zn | 129.85 (11) | C17—C18—C19 | 119.4 (5) |
Cu—O2—Zn | 102.50 (13) | O2—C19—C14 | 121.3 (4) |
O2—Zn—O1 | 76.80 (12) | O2—C19—C18 | 119.2 (4) |
O2—Zn—Br1 | 116.05 (11) | C14—C19—C18 | 119.5 (4) |
O1—Zn—Br1 | 117.39 (10) | N3—C20—C21 | 110.8 (5) |
O2—Zn—Br2 | 111.29 (12) | C22—C21—C20 | 110.3 (6) |
O1—Zn—Br2 | 110.22 (10) | C21—C22—C23 | 106.5 (6) |
Br1—Zn—Br2 | 118.11 (4) | C22—C23—C24 | 108.8 (6) |
O2—Zn—Cu | 38.13 (8) | N3—C24—C23 | 110.2 (5) |
O1—Zn—Cu | 38.75 (8) | N3—Cu—Zn | 99.08 (10) |
Br1—Zn—Cu | 126.87 (3) | C7—N1—C8 | 114.4 (4) |
Br2—Zn—Cu | 115.01 (3) | C7—N1—Cu | 125.0 (3) |
O1—C1—C2 | 119.7 (4) | C8—N1—Cu | 120.5 (3) |
O1—C1—C6 | 121.4 (4) | C13—N2—C10 | 114.7 (4) |
C2—C1—C6 | 118.9 (4) | C13—N2—Cu | 124.6 (3) |
C3—C2—C1 | 120.6 (4) | C10—N2—Cu | 120.6 (3) |
C2—C3—C4 | 120.7 (4) | C24—N3—C20 | 109.3 (5) |
C5—C4—C3 | 118.9 (5) | C24—N3—Cu | 122.7 (3) |
C4—C5—C6 | 122.3 (5) | C20—N3—Cu | 124.9 (4) |
C1—C6—C5 | 118.6 (4) | C1—O1—Cu | 130.1 (3) |
C1—C6—C7 | 124.4 (4) | C1—O1—Zn | 127.6 (3) |
C5—C6—C7 | 117.0 (4) | Cu—O1—Zn | 101.70 (13) |
N1—C7—C6 | 127.7 (4) | C19—O2—Cu | 130.0 (3) |
N1—C8—C9 | 114.8 (4) | C19—O2—Zn | 125.5 (3) |
C11—C9—C8 | 112.0 (4) |
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