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The monoclinic unit cell of the title compound, [CuBr(C3H4N2)4]Br, emulates an orthorhombic cell as its β angle is close to 90°; the crystal structure is twinned with approximately equal contributions of the two components. The Cu atom is five-coordinate in a square-pyramidal geometry. The cation interacts with the bromide anion through hydrogen bonds, which give rise to a layer structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804019609/ci6419sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804019609/ci6419Isup2.hkl
Contains datablock I

CCDC reference: 251618

Key indicators

  • Single-crystal X-ray study
  • T = 113 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.053
  • wR factor = 0.168
  • Data-to-parameter ratio = 16.0

checkCIF/PLATON results

No syntax errors found



Alert level A ABSTM02_ALERT_3_A The ratio of expected to reported Tmax/Tmin(RR) is > 2.00 Tmin and Tmax reported: 0.337 0.653 Tmin and Tmax expected: 0.073 0.650 RR = 4.565 Please check that your absorption correction is appropriate.
Author Response: The transmission factors were given by SADABS. The range is large because of the twinned nature of the crystal. The monoclinic data emulated orthorhombic data. Also, any value of \m*2r led to an even larger range of transmission factors.
PLAT060_ALERT_3_A Ratio Tmax/Tmin (Exp-to-Rep) (too) Large .......       4.44
Author Response: See above response.

Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Br1 - Cu1 .. 19.89 su
Alert level C PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
2 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Bromotetrakis(1H-imidazole-κN3)copper(II) bromide top
Crystal data top
[CuBr(C3H4N2)4]BrF(000) = 972
Mr = 495.69Dx = 1.987 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 7789 reflections
a = 8.9625 (3) Åθ = 2.7–26.4°
b = 13.2140 (5) ŵ = 6.15 mm1
c = 13.9889 (5) ÅT = 113 K
β = 90.052 (1)°Plate, blue
V = 1656.7 (1) Å30.48 × 0.38 × 0.07 mm
Z = 4
Data collection top
Siemens P4/CCD area-detector
diffractometer
3343 independent reflections
Radiation source: fine-focus sealed tube3081 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
φ and ω scansθmax = 26.4°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 1111
Tmin = 0.337, Tmax = 0.653k = 1614
14285 measured reflectionsl = 1717
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.053Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.168H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.1271P)2 + 5.3184P]
where P = (Fo2 + 2Fc2)/3
3343 reflections(Δ/σ)max < 0.001
209 parametersΔρmax = 2.30 e Å3
103 restraintsΔρmin = 2.23 e Å3
Special details top

Experimental. When the data were reduced by SADABS (Bruker, 2001), the dimensionless µ*2r was set as zero; other values led to a great number of non-positive definite atoms.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Br10.54815 (9)0.40315 (6)0.37801 (7)0.0253 (2)
Br20.05553 (8)0.08885 (6)0.37512 (7)0.0250 (2)
Cu10.29988 (8)0.28022 (5)0.37666 (6)0.0077 (2)
N10.1367 (5)0.3852 (4)0.3802 (5)0.0089 (9)
N20.0863 (6)0.4543 (4)0.3737 (6)0.0177 (11)
H2n0.18390.46100.37190.021*
N30.2914 (7)0.2709 (4)0.5192 (4)0.0114 (11)
N40.3162 (8)0.3116 (5)0.6703 (4)0.0164 (14)
H4n0.34380.34450.72210.020*
N50.4071 (5)0.1460 (4)0.3724 (5)0.0085 (9)
N60.5929 (6)0.0365 (4)0.3700 (6)0.0136 (11)
H6n0.68380.01160.36720.016*
N70.2896 (7)0.2802 (4)0.2342 (4)0.0097 (11)
N80.3224 (8)0.3165 (5)0.0823 (4)0.0158 (15)
H8n0.35610.34580.03010.019*
C10.1511 (7)0.4874 (4)0.3834 (6)0.0168 (13)
H10.24290.52300.38800.020*
C20.0142 (6)0.5307 (5)0.3790 (6)0.0172 (13)
H20.00720.60110.37960.021*
C30.0102 (6)0.3659 (5)0.3719 (6)0.0134 (12)
H30.05350.30060.36570.016*
C40.2194 (10)0.2016 (6)0.5746 (5)0.0139 (15)
H40.16440.14550.55080.017*
C50.2375 (10)0.2243 (6)0.6688 (5)0.0176 (17)
H50.20240.18680.72220.021*
C60.3456 (9)0.3402 (6)0.5798 (4)0.0132 (14)
H60.39680.40020.56180.016*
C70.3495 (7)0.0508 (4)0.3751 (7)0.0149 (11)
H70.24630.03460.37740.018*
C80.4637 (6)0.0183 (5)0.3741 (7)0.0164 (12)
H80.45480.08990.37580.020*
C90.5564 (6)0.1362 (4)0.3711 (6)0.0108 (11)
H90.62560.19060.37090.013*
C100.2057 (11)0.2169 (6)0.1801 (4)0.0152 (15)
H100.14360.16490.20480.018*
C110.2227 (10)0.2382 (6)0.0862 (4)0.0159 (17)
H110.17520.20560.03380.019*
C120.3598 (9)0.3406 (6)0.1728 (4)0.0114 (14)
H120.42670.39330.19040.014*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br10.0234 (4)0.0266 (4)0.0259 (4)0.0024 (3)0.0002 (5)0.0018 (4)
Br20.0223 (4)0.0298 (5)0.0228 (4)0.0027 (3)0.0003 (5)0.0010 (4)
Cu10.0101 (3)0.0073 (4)0.0055 (3)0.0033 (2)0.0000 (5)0.0002 (3)
N10.0118 (19)0.007 (2)0.008 (2)0.0012 (16)0.001 (3)0.002 (2)
N20.011 (2)0.019 (3)0.023 (3)0.0049 (19)0.002 (4)0.005 (3)
N30.012 (3)0.011 (3)0.0111 (19)0.002 (2)0.001 (2)0.0011 (18)
N40.010 (3)0.030 (4)0.009 (2)0.001 (3)0.005 (3)0.003 (2)
N50.009 (2)0.013 (2)0.004 (2)0.0040 (16)0.002 (3)0.000 (2)
N60.011 (2)0.010 (3)0.020 (3)0.0065 (18)0.004 (3)0.002 (3)
N70.009 (3)0.009 (3)0.0121 (19)0.002 (2)0.002 (2)0.0008 (18)
N80.018 (4)0.020 (4)0.010 (2)0.006 (3)0.002 (3)0.002 (2)
C10.018 (3)0.011 (3)0.022 (4)0.002 (2)0.003 (4)0.001 (3)
C20.027 (3)0.006 (3)0.019 (3)0.006 (2)0.002 (4)0.003 (3)
C30.014 (2)0.008 (3)0.018 (3)0.0031 (19)0.006 (4)0.004 (3)
C40.014 (4)0.019 (4)0.009 (3)0.003 (3)0.001 (3)0.004 (2)
C50.012 (4)0.031 (4)0.010 (3)0.000 (3)0.000 (3)0.000 (3)
C60.007 (3)0.021 (4)0.011 (3)0.001 (3)0.002 (3)0.006 (2)
C70.009 (2)0.013 (2)0.022 (3)0.004 (2)0.005 (4)0.002 (4)
C80.016 (3)0.006 (2)0.027 (3)0.003 (2)0.003 (4)0.001 (3)
C90.015 (2)0.005 (2)0.012 (3)0.0011 (19)0.001 (4)0.000 (3)
C100.018 (4)0.017 (4)0.010 (3)0.001 (3)0.001 (3)0.002 (2)
C110.024 (4)0.015 (4)0.009 (3)0.007 (3)0.003 (3)0.005 (3)
C120.014 (4)0.014 (4)0.007 (2)0.004 (3)0.001 (3)0.001 (2)
Geometric parameters (Å, º) top
Br1—Cu12.755 (1)N7—C101.355 (7)
Cu1—N12.016 (5)N8—C121.349 (6)
Cu1—N32.000 (6)N8—C111.368 (7)
Cu1—N52.018 (5)N8—H8n0.88
Cu1—N71.995 (6)C1—C21.355 (6)
N1—C31.346 (6)C1—H10.95
N1—C11.357 (6)C2—H20.95
N2—C31.353 (6)C3—H30.95
N2—C21.355 (6)C4—C51.361 (7)
N2—H2n0.88C4—H40.95
N3—C61.339 (7)C5—H50.95
N3—C41.362 (7)C6—H60.95
N4—C61.347 (6)C7—C81.371 (6)
N4—C51.352 (7)C7—H70.95
N4—H4n0.88C8—H80.95
N5—C91.344 (6)C9—H90.95
N5—C71.361 (6)C10—C111.353 (7)
N6—C91.357 (6)C10—H100.95
N6—C81.367 (6)C11—H110.95
N6—H6n0.88C12—H120.95
N7—C121.331 (7)
N1—Cu1—N389.4 (3)C2—C1—H1125.3
N1—Cu1—N5162.0 (2)N1—C1—H1125.3
N1—Cu1—N789.5 (3)C1—C2—N2106.8 (5)
N1—Cu1—Br1100.4 (1)C1—C2—H2126.6
N3—Cu1—N589.6 (3)N2—C2—H2126.6
N3—Cu1—N7174.0 (2)N1—C3—N2109.1 (5)
N3—Cu1—Br193.5 (2)N1—C3—H3125.4
N5—Cu1—N789.6 (3)N2—C3—H3125.4
N5—Cu1—Br197.7 (1)C5—C4—N3110.2 (6)
N7—Cu1—Br192.5 (2)C5—C4—H4124.9
C3—N1—C1106.5 (5)N3—C4—H4124.9
C3—N1—Cu1125.2 (4)N4—C5—C4105.3 (6)
C1—N1—Cu1128.1 (4)N4—C5—H5127.3
C3—N2—C2108.0 (5)C4—C5—H5127.3
C3—N2—H2n126.0N3—C6—N4109.3 (6)
C2—N2—H2n126.0N3—C6—H6125.3
C6—N3—C4105.8 (6)N4—C6—H6125.3
C6—N3—Cu1125.1 (4)N5—C7—C8109.4 (5)
C4—N3—Cu1128.8 (4)N5—C7—H7125.3
C6—N4—C5109.2 (6)C8—C7—H7125.3
C6—N4—H4n125.4N6—C8—C7106.2 (5)
C5—N4—H4n125.4N6—C8—H8126.9
C9—N5—C7106.8 (5)C7—C8—H8126.9
C9—N5—Cu1124.0 (4)N5—C9—N6109.5 (5)
C7—N5—Cu1129.1 (4)N5—C9—H9125.3
C9—N6—C8108.0 (5)N6—C9—H9125.3
C9—N6—H6n126.0C11—C10—N7110.6 (6)
C8—N6—H6n126.0C11—C10—H10124.7
C12—N7—C10105.8 (6)N7—C10—H10124.7
C12—N7—Cu1128.5 (4)C10—C11—N8105.7 (6)
C10—N7—Cu1125.7 (4)C10—C11—H11127.2
C12—N8—C11107.6 (5)N8—C11—H11127.2
C12—N8—H8n126.2N7—C12—N8110.3 (6)
C11—N8—H8n126.2N7—C12—H12124.9
C2—C1—N1109.4 (5)N8—C12—H12124.9
N7—Cu1—N1—C381.2 (8)C3—N1—C1—C21.2 (10)
N3—Cu1—N1—C392.9 (8)Cu1—N1—C1—C2176.3 (6)
N5—Cu1—N1—C35.9 (13)N1—C1—C2—N20.5 (10)
Br1—Cu1—N1—C3173.6 (7)C3—N2—C2—C11.9 (10)
N7—Cu1—N1—C193.1 (7)C1—N1—C3—N22.4 (11)
N3—Cu1—N1—C192.7 (7)Cu1—N1—C3—N2177.7 (6)
N5—Cu1—N1—C1179.8 (8)C2—N2—C3—N12.7 (11)
Br1—Cu1—N1—C10.7 (8)C6—N3—C4—C54.0 (10)
N1—Cu1—N3—C674.6 (6)Cu1—N3—C4—C5177.9 (7)
N5—Cu1—N3—C6123.5 (6)C6—N4—C5—C40.5 (11)
Br1—Cu1—N3—C625.8 (6)N3—C4—C5—N42.8 (11)
N1—Cu1—N3—C498.2 (7)C4—N3—C6—N43.7 (10)
N5—Cu1—N3—C463.8 (7)Cu1—N3—C6—N4177.8 (6)
Br1—Cu1—N3—C4161.5 (7)C5—N4—C6—N32.1 (11)
N7—Cu1—N5—C992.5 (7)C9—N5—C7—C80.9 (10)
N3—Cu1—N5—C993.5 (7)Cu1—N5—C7—C8177.7 (6)
N1—Cu1—N5—C9179.5 (8)C9—N6—C8—C71.5 (10)
Br1—Cu1—N5—C90.0 (7)N5—C7—C8—N60.4 (10)
N7—Cu1—N5—C791.1 (8)C7—N5—C9—N61.8 (11)
N3—Cu1—N5—C782.9 (8)Cu1—N5—C9—N6178.9 (5)
N1—Cu1—N5—C74.1 (13)C8—N6—C9—N52.1 (11)
Br1—Cu1—N5—C7176.4 (7)C12—N7—C10—C110.4 (10)
N1—Cu1—N7—C1286.5 (7)Cu1—N7—C10—C11179.0 (7)
N5—Cu1—N7—C12111.6 (7)N7—C10—C11—N80.9 (12)
Br1—Cu1—N7—C1213.9 (7)C12—N8—C11—C101.0 (11)
N1—Cu1—N7—C1092.9 (7)C10—N7—C12—N80.2 (9)
N5—Cu1—N7—C1069.1 (7)Cu1—N7—C12—N8179.7 (6)
Br1—Cu1—N7—C10166.7 (6)C11—N8—C12—N70.8 (11)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2n···Br1i0.882.523.346 (6)156
N4—H4n···Br2ii0.882.483.355 (6)170
N6—H6n···Br2iii0.882.553.227 (5)134
N8—H8n···Br2iv0.882.463.341 (6)174
Symmetry codes: (i) x1, y, z; (ii) x+1/2, y+1/2, z+1/2; (iii) x+1, y, z; (iv) x+1/2, y+1/2, z1/2.
 

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