Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802001629/bt6105sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802001629/bt6105Isup2.hkl |
CCDC reference: 180763
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.038
- wR factor = 0.104
- Data-to-parameter ratio = 25.8
checkCIF results
No syntax errors foundGLOBAL _publ field problems
Alert Level A:
PUBL_002 Alert A The contact author's address is missing, _publ_contact_author_address. ADDSYM reports no extra symmetry
Alert Level C:
WEIGH_01 Alert C Extra text has been found in the _refine_ls_weighting_scheme field. This should be in the _refine_ls_weighting_details field. Weighting scheme given as calc w = 1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.931 Weighting scheme identified as calc General Notes
ABSTM_02 The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.687 0.881 Tmin' and Tmax expected: 0.627 0.696 RR' = 0.865 Please check that your absorption correction is appropriate.
1 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: SDP (Enraf-Nonius, 1985); cell refinement: SDP; data reduction: XCAD4 in SDP; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXL97.
[CuBr2(C4H6N2)4] | F(000) = 550 |
Mr = 551.79 | Dx = 1.626 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 8.2657 (9) Å | Cell parameters from 78 reflections |
b = 12.053 (1) Å | θ = 10.0–17.5° |
c = 11.338 (1) Å | µ = 4.53 mm−1 |
β = 94.06 (1)° | T = 293 K |
V = 1126.73 (18) Å3 | Block, blue |
Z = 2 | 0.1 × 0.1 × 0.08 mm |
Enraf-Nonius CAD-4 diffractometer | 2136 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.039 |
Graphite monochromator | θmax = 30.1°, θmin = 2.5° |
ω scans | h = 0→11 |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998) | k = −16→6 |
Tmin = 0.687, Tmax = 0.881 | l = −15→15 |
5129 measured reflections | 3 standard reflections every 240 min |
3300 independent reflections | intensity decay: none |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.104 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | Calculated w = 1/[σ2(Fo2) + (0.0461P)2 + 0.9319P] where P = (Fo2 + 2Fc2)/3 |
3300 reflections | (Δ/σ)max = 0.001 |
128 parameters | Δρmax = 1.23 e Å−3 |
0 restraints | Δρmin = −0.95 e Å−3 |
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 | 0.5000 | 0.5000 | 0.5000 | 0.04036 (16) | |
Br1 | 0.33099 (4) | 0.53646 (3) | 0.74605 (4) | 0.05020 (13) | |
N1 | 0.7068 (3) | 0.4539 (2) | 0.5916 (2) | 0.0372 (5) | |
C1 | 0.8428 (4) | 0.5093 (3) | 0.6033 (3) | 0.0417 (7) | |
H1 | 0.8607 | 0.5764 | 0.5659 | 0.050* | |
N2 | 0.9530 (3) | 0.4576 (2) | 0.6757 (3) | 0.0437 (6) | |
H2 | 1.0500 | 0.4802 | 0.6948 | 0.052* | |
C2 | 0.8843 (4) | 0.3628 (3) | 0.7139 (3) | 0.0455 (8) | |
C3 | 0.7326 (4) | 0.3607 (3) | 0.6611 (3) | 0.0462 (8) | |
H3 | 0.6569 | 0.3048 | 0.6703 | 0.055* | |
C4 | 0.9701 (6) | 0.2856 (4) | 0.8006 (5) | 0.0749 (14) | |
H4A | 1.0730 | 0.3169 | 0.8276 | 0.112* | 0.30 (6) |
H4B | 0.9870 | 0.2156 | 0.7631 | 0.112* | 0.30 (6) |
H4C | 0.9055 | 0.2748 | 0.8668 | 0.112* | 0.30 (6) |
H4D | 0.9040 | 0.2213 | 0.8107 | 0.112* | 0.70 (6) |
H4E | 0.9900 | 0.3226 | 0.8752 | 0.112* | 0.70 (6) |
H4F | 1.0715 | 0.2634 | 0.7715 | 0.112* | 0.70 (6) |
N3 | 0.5728 (3) | 0.6598 (2) | 0.5063 (2) | 0.0370 (6) | |
C11 | 0.5418 (4) | 0.7306 (3) | 0.5884 (3) | 0.0453 (8) | |
H11 | 0.4841 | 0.7140 | 0.6537 | 0.054* | |
N4 | 0.6040 (4) | 0.8307 (2) | 0.5666 (3) | 0.0480 (7) | |
H4 | 0.5966 | 0.8891 | 0.6095 | 0.058* | |
C12 | 0.6810 (4) | 0.8234 (3) | 0.4644 (3) | 0.0439 (8) | |
C13 | 0.6608 (4) | 0.7183 (3) | 0.4280 (3) | 0.0420 (7) | |
H13 | 0.7003 | 0.6890 | 0.3598 | 0.050* | |
C14 | 0.7616 (6) | 0.9219 (4) | 0.4144 (4) | 0.0701 (12) | |
H14A | 0.8702 | 0.9026 | 0.3973 | 0.105* | 0.57 (6) |
H14B | 0.7648 | 0.9815 | 0.4707 | 0.105* | 0.57 (6) |
H14C | 0.7018 | 0.9449 | 0.3429 | 0.105* | 0.57 (6) |
H14D | 0.6876 | 0.9834 | 0.4099 | 0.105* | 0.43 (6) |
H14E | 0.7931 | 0.9045 | 0.3366 | 0.105* | 0.43 (6) |
H14F | 0.8561 | 0.9411 | 0.4643 | 0.105* | 0.43 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0383 (3) | 0.0265 (3) | 0.0536 (3) | −0.0072 (2) | −0.0157 (2) | 0.0029 (2) |
Br1 | 0.04270 (19) | 0.0413 (2) | 0.0652 (2) | −0.00560 (14) | −0.00567 (15) | 0.01207 (16) |
N1 | 0.0358 (12) | 0.0335 (14) | 0.0412 (14) | −0.0046 (11) | −0.0055 (10) | 0.0006 (11) |
C1 | 0.0377 (16) | 0.0383 (17) | 0.0487 (18) | −0.0029 (13) | −0.0003 (13) | 0.0029 (14) |
N2 | 0.0295 (12) | 0.0441 (16) | 0.0563 (17) | −0.0034 (11) | −0.0046 (11) | −0.0008 (13) |
C2 | 0.0378 (16) | 0.0401 (18) | 0.057 (2) | −0.0005 (13) | −0.0094 (14) | 0.0030 (15) |
C3 | 0.0389 (17) | 0.0377 (17) | 0.060 (2) | −0.0076 (13) | −0.0094 (15) | 0.0073 (15) |
C4 | 0.058 (3) | 0.063 (3) | 0.099 (4) | −0.005 (2) | −0.029 (2) | 0.026 (2) |
N3 | 0.0367 (13) | 0.0301 (13) | 0.0427 (15) | −0.0071 (10) | −0.0072 (11) | −0.0002 (11) |
C11 | 0.051 (2) | 0.0389 (18) | 0.0470 (19) | −0.0088 (15) | 0.0070 (15) | −0.0018 (14) |
N4 | 0.0564 (18) | 0.0332 (15) | 0.0542 (18) | −0.0072 (13) | 0.0028 (14) | −0.0083 (13) |
C12 | 0.0436 (17) | 0.0371 (17) | 0.0495 (19) | −0.0079 (14) | −0.0074 (14) | 0.0060 (14) |
C13 | 0.0491 (19) | 0.0389 (18) | 0.0377 (17) | −0.0058 (14) | 0.0007 (14) | −0.0004 (13) |
C14 | 0.081 (3) | 0.054 (2) | 0.075 (3) | −0.026 (2) | 0.003 (2) | 0.018 (2) |
Cu1—N1i | 2.014 (3) | C4—H4E | 0.9600 |
Cu1—N1 | 2.014 (3) | C4—H4F | 0.9600 |
Cu1—N3 | 2.017 (2) | N3—C11 | 1.302 (4) |
Cu1—N3i | 2.017 (2) | N3—C13 | 1.381 (4) |
N1—C1 | 1.306 (4) | C11—N4 | 1.341 (4) |
N1—C3 | 1.381 (4) | C11—H11 | 0.9300 |
C1—N2 | 1.337 (4) | N4—C12 | 1.364 (5) |
C1—H1 | 0.9300 | N4—H4 | 0.8600 |
N2—C2 | 1.360 (5) | C12—C13 | 1.339 (5) |
N2—H2 | 0.8600 | C12—C14 | 1.493 (5) |
C2—C3 | 1.351 (4) | C13—H13 | 0.9300 |
C2—C4 | 1.495 (5) | C14—H14A | 0.9600 |
C3—H3 | 0.9300 | C14—H14B | 0.9600 |
C4—H4A | 0.9600 | C14—H14C | 0.9600 |
C4—H4B | 0.9600 | C14—H14D | 0.9600 |
C4—H4C | 0.9600 | C14—H14E | 0.9600 |
C4—H4D | 0.9600 | C14—H14F | 0.9600 |
N1i—Cu1—N1 | 180.0 | H4C—C4—H4F | 141.1 |
N1i—Cu1—N3 | 89.70 (10) | H4D—C4—H4F | 109.5 |
N1—Cu1—N3 | 90.30 (10) | H4E—C4—H4F | 109.5 |
N1i—Cu1—N3i | 90.30 (10) | C11—N3—C13 | 105.3 (3) |
N1—Cu1—N3i | 89.70 (10) | C11—N3—Cu1 | 125.3 (2) |
N3—Cu1—N3i | 180.0 | C13—N3—Cu1 | 129.4 (2) |
C1—N1—C3 | 105.1 (3) | N3—C11—N4 | 111.1 (3) |
C1—N1—Cu1 | 127.2 (2) | N3—C11—H11 | 124.4 |
C3—N1—Cu1 | 127.6 (2) | N4—C11—H11 | 124.4 |
N1—C1—N2 | 111.6 (3) | C11—N4—C12 | 107.8 (3) |
N1—C1—H1 | 124.2 | C11—N4—H4 | 126.1 |
N2—C1—H1 | 124.2 | C12—N4—H4 | 126.1 |
C1—N2—C2 | 107.8 (3) | C13—C12—N4 | 105.5 (3) |
C1—N2—H2 | 126.1 | C13—C12—C14 | 133.2 (4) |
C2—N2—H2 | 126.1 | N4—C12—C14 | 121.3 (3) |
C3—C2—N2 | 105.7 (3) | C12—C13—N3 | 110.2 (3) |
C3—C2—C4 | 131.4 (4) | C12—C13—H13 | 124.9 |
N2—C2—C4 | 122.9 (3) | N3—C13—H13 | 124.9 |
C2—C3—N1 | 109.8 (3) | C12—C14—H14A | 109.5 |
C2—C3—H3 | 125.1 | C12—C14—H14B | 109.5 |
N1—C3—H3 | 125.1 | H14A—C14—H14B | 109.5 |
C2—C4—H4A | 109.5 | C12—C14—H14C | 109.5 |
C2—C4—H4B | 109.5 | H14A—C14—H14C | 109.5 |
H4A—C4—H4B | 109.5 | H14B—C14—H14C | 109.5 |
C2—C4—H4C | 109.5 | C12—C14—H14D | 109.5 |
H4A—C4—H4C | 109.5 | H14A—C14—H14D | 141.1 |
H4B—C4—H4C | 109.5 | H14B—C14—H14D | 56.3 |
C2—C4—H4D | 109.5 | H14C—C14—H14D | 56.3 |
H4A—C4—H4D | 141.1 | C12—C14—H14E | 109.5 |
H4B—C4—H4D | 56.3 | H14A—C14—H14E | 56.3 |
H4C—C4—H4D | 56.3 | H14B—C14—H14E | 141.1 |
C2—C4—H4E | 109.5 | H14C—C14—H14E | 56.3 |
H4A—C4—H4E | 56.3 | H14D—C14—H14E | 109.5 |
H4B—C4—H4E | 141.1 | C12—C14—H14F | 109.5 |
H4C—C4—H4E | 56.3 | H14A—C14—H14F | 56.3 |
H4D—C4—H4E | 109.5 | H14B—C14—H14F | 56.3 |
C2—C4—H4F | 109.5 | H14C—C14—H14F | 141.1 |
H4A—C4—H4F | 56.3 | H14D—C14—H14F | 109.5 |
H4B—C4—H4F | 56.3 | H14E—C14—H14F | 109.5 |
Symmetry code: (i) −x+1, −y+1, −z+1. |