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The title compound, [Cu3(C4H6N2O2)2(C5H5N)7](ClO4)2, is a trinuclear CuII complex bridged by two glyoximate groups. The central Cu and the pyridine N atom bonded to it lie on a twofold axis. The geometry around each Cu atom is a distorted square pyramid.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680301331X/ob6252sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680301331X/ob6252Isup2.hkl
Contains datablock I

CCDC reference: 221632

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.051
  • wR factor = 0.082
  • Data-to-parameter ratio = 22.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SMART (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
[Cu3(C4H6N2O2)2(C5H5N)7](ClO4)2F(000) = 2396
Mr = 1171.47Dx = 1.541 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3680 reflections
a = 24.615 (5) Åθ = 2.6–25.2°
b = 8.3158 (17) ŵ = 1.43 mm1
c = 25.469 (5) ÅT = 293 K
β = 104.48 (3)°Prism, black
V = 5047.7 (19) Å30.25 × 0.2 × 0.15 mm
Z = 4
Data collection top
Bruker CCD area-detector
diffractometer
7370 independent reflections
Radiation source: fine-focus sealed tube2919 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.061
Detector resolution: 15×15 microns pixels mm-1θmax = 30°, θmin = 2.7°
φ and ω scansh = 3434
Absorption correction: multi-scan
(SADABS; Bruker, 1999)
k = 1011
Tmin = 0.717, Tmax = 0.807l = 3534
19837 measured reflections
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)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.082H-atom parameters constrained
S = 1.07 w = {exp[1.50(sinθ/λ)2]}/[σ2(Fo2) + (0.001P)2]
where P = (Fo2 + 2Fc2)/3
7345 reflections(Δ/σ)max = 0.003
322 parametersΔρmax = 0.53 e Å3
0 restraintsΔρmin = 0.64 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.50000.27798 (8)0.25000.03695 (17)
Cu20.411147 (18)0.19183 (6)0.124310 (18)0.04841 (15)
Cl10.66856 (6)0.0917 (2)0.14861 (6)0.0784 (4)
O10.38765 (9)0.3306 (3)0.17468 (9)0.0488 (7)
O20.51937 (10)0.3049 (3)0.37100 (9)0.0565 (8)
O30.6535 (4)0.0183 (8)0.1751 (3)0.319 (5)
O40.6309 (3)0.1904 (10)0.1414 (3)0.318 (5)
O50.6745 (4)0.0386 (10)0.1057 (3)0.325 (5)
O60.7129 (3)0.1487 (11)0.1680 (3)0.351 (6)
N10.35001 (14)0.3280 (4)0.05632 (13)0.0604 (10)
N20.43487 (14)0.0347 (4)0.07239 (13)0.0530 (9)
N30.36047 (13)0.0113 (4)0.14329 (13)0.0538 (9)
N40.50000.0226 (5)0.25000.0425 (11)
N50.41851 (11)0.3259 (3)0.22596 (11)0.0379 (7)
N60.48431 (12)0.3182 (4)0.32218 (11)0.0409 (8)
C10.30521 (19)0.3961 (6)0.06513 (17)0.0693 (14)
H1A0.29720.37670.09830.083*
C20.2694 (2)0.4935 (7)0.0294 (2)0.0868 (17)
H2A0.23890.54130.03860.104*
C30.2793 (2)0.5184 (7)0.0192 (2)0.1012 (19)
H3A0.25510.58180.04490.121*
C40.3248 (3)0.4500 (8)0.0304 (2)0.116 (2)
H4A0.33240.46440.06400.139*
C50.3597 (2)0.3583 (7)0.0092 (2)0.0930 (18)
H5A0.39200.31560.00190.112*
C60.39805 (18)0.0334 (6)0.03109 (17)0.0700 (14)
H6A0.36120.00380.02250.084*
C70.4116 (2)0.1542 (7)0.00087 (19)0.103 (2)
H7A0.38490.19470.02870.124*
C80.4644 (3)0.2155 (7)0.0143 (2)0.121 (2)
H8A0.47400.30160.00490.146*
C90.5029 (2)0.1487 (7)0.0562 (2)0.1011 (19)
H9A0.53960.18680.06580.121*
C100.48668 (18)0.0237 (6)0.08408 (16)0.0653 (13)
H10A0.51330.02220.11260.078*
C110.37271 (19)0.1439 (6)0.14398 (18)0.0719 (14)
H11A0.40530.17450.13440.086*
C120.3401 (2)0.2620 (6)0.1580 (2)0.0924 (17)
H12A0.35050.36960.15810.111*
C130.2924 (2)0.2185 (8)0.1715 (2)0.0977 (19)
H13A0.26910.29600.18070.117*
C140.2790 (2)0.0605 (8)0.1716 (2)0.0938 (18)
H14A0.24630.02790.18050.113*
C150.31472 (19)0.0511 (6)0.15829 (17)0.0744 (15)
H15A0.30620.15960.16000.089*
C160.53702 (16)0.0623 (5)0.23080 (16)0.0533 (11)
H16A0.56360.00690.21760.064*
C170.5376 (2)0.2240 (6)0.2298 (2)0.0902 (17)
H17A0.56350.27870.21530.108*
C180.50000.3055 (9)0.25000.133 (4)
H18A0.50000.41740.25000.160*
C190.33500 (14)0.4091 (5)0.25580 (15)0.0645 (13)
H19A0.31710.40530.21770.097*
H19B0.33210.51590.26920.097*
H19C0.31690.33470.27470.097*
C200.39531 (15)0.3646 (4)0.26476 (14)0.0412 (9)
C210.43287 (16)0.3603 (4)0.31935 (14)0.0424 (10)
C220.41269 (16)0.3983 (5)0.36877 (14)0.0725 (15)
H22A0.44330.38890.40050.109*
H22B0.38360.32420.37140.109*
H22C0.39820.50600.36620.109*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0374 (4)0.0344 (4)0.0440 (4)0.0000.0196 (3)0.000
Cu20.0424 (3)0.0548 (4)0.0500 (3)0.0053 (3)0.0153 (2)0.0088 (3)
Cl10.0512 (8)0.1039 (13)0.0805 (10)0.0003 (8)0.0175 (7)0.0048 (9)
O10.0427 (15)0.057 (2)0.0445 (15)0.0061 (13)0.0061 (12)0.0030 (14)
O20.0584 (17)0.074 (2)0.0394 (15)0.0223 (16)0.0167 (13)0.0078 (15)
O30.477 (12)0.167 (6)0.441 (10)0.016 (7)0.357 (10)0.067 (7)
O40.187 (6)0.296 (10)0.466 (12)0.161 (7)0.072 (7)0.055 (8)
O50.403 (12)0.421 (12)0.222 (7)0.057 (9)0.213 (8)0.111 (7)
O60.144 (5)0.531 (14)0.299 (9)0.156 (7)0.096 (5)0.046 (9)
N10.058 (2)0.068 (3)0.057 (2)0.004 (2)0.0182 (18)0.004 (2)
N20.044 (2)0.065 (3)0.050 (2)0.0082 (19)0.0133 (17)0.0110 (19)
N30.052 (2)0.053 (3)0.061 (2)0.0047 (19)0.0228 (18)0.003 (2)
N40.043 (3)0.035 (3)0.053 (3)0.0000.018 (2)0.000
N50.0408 (18)0.033 (2)0.0443 (18)0.0030 (14)0.0191 (15)0.0013 (16)
N60.0481 (19)0.037 (2)0.0421 (18)0.0060 (16)0.0199 (15)0.0045 (16)
C10.063 (3)0.092 (4)0.049 (3)0.009 (3)0.006 (2)0.006 (3)
C20.070 (4)0.107 (5)0.075 (4)0.015 (3)0.004 (3)0.004 (4)
C30.106 (5)0.105 (5)0.079 (4)0.012 (4)0.003 (4)0.013 (4)
C40.146 (6)0.130 (6)0.081 (4)0.015 (5)0.046 (4)0.043 (4)
C50.090 (4)0.117 (5)0.085 (4)0.023 (4)0.046 (3)0.028 (4)
C60.053 (3)0.090 (4)0.064 (3)0.004 (3)0.010 (2)0.031 (3)
C70.090 (4)0.124 (6)0.081 (4)0.013 (4)0.006 (3)0.059 (4)
C80.128 (5)0.121 (6)0.105 (5)0.031 (5)0.011 (4)0.067 (4)
C90.083 (4)0.121 (5)0.095 (4)0.038 (4)0.013 (3)0.034 (4)
C100.053 (3)0.082 (4)0.060 (3)0.005 (3)0.011 (2)0.016 (3)
C110.077 (3)0.060 (4)0.083 (4)0.008 (3)0.027 (3)0.001 (3)
C120.111 (5)0.057 (4)0.114 (4)0.016 (3)0.036 (4)0.000 (3)
C130.096 (5)0.082 (5)0.118 (5)0.038 (4)0.032 (4)0.018 (4)
C140.080 (4)0.096 (5)0.121 (5)0.020 (4)0.056 (3)0.015 (4)
C150.070 (3)0.069 (4)0.097 (4)0.010 (3)0.046 (3)0.003 (3)
C160.055 (3)0.043 (3)0.068 (3)0.000 (2)0.027 (2)0.002 (2)
C170.098 (4)0.050 (4)0.136 (5)0.015 (3)0.054 (3)0.010 (4)
C180.145 (8)0.032 (5)0.255 (11)0.0000.110 (8)0.000
C190.046 (3)0.081 (4)0.072 (3)0.013 (2)0.025 (2)0.001 (3)
C200.040 (2)0.039 (3)0.049 (2)0.0060 (18)0.0216 (19)0.005 (2)
C210.052 (2)0.038 (2)0.047 (2)0.0072 (19)0.028 (2)0.007 (2)
C220.077 (3)0.101 (4)0.050 (3)0.038 (3)0.037 (2)0.012 (3)
Geometric parameters (Å, º) top
Cu1—N51.986 (3)C11—C121.371 (6)
Cu1—N5i1.986 (3)C12—C131.354 (6)
Cu1—N61.999 (3)C13—C141.355 (7)
Cu1—N6i1.999 (3)C14—C151.377 (6)
Cu1—N42.124 (4)C16—C171.345 (6)
Cu2—O11.919 (2)C17—C181.349 (6)
Cu2—O2i1.929 (2)C18—C17i1.349 (6)
Cu2—N22.045 (3)C19—C201.491 (4)
Cu2—N32.085 (3)C20—C211.465 (4)
Cu2—N12.290 (3)C21—C221.498 (4)
Cl1—O61.179 (5)C1—H1A0.9300
Cl1—O41.217 (5)C2—H2A0.9300
Cl1—O51.221 (5)C3—H3A0.9300
Cl1—O31.247 (5)C4—H4A0.9300
O1—N51.337 (3)C5—H5A0.9300
O2—N61.329 (3)C6—H6A0.9300
O2—Cu2i1.929 (2)C7—H7A0.9300
N1—C51.305 (5)C8—H8A0.9300
N1—C11.308 (5)C9—H9A0.9300
N2—C101.327 (4)C10—H10A0.9300
N2—C61.331 (4)C11—H11A0.9300
N3—C151.319 (4)C12—H12A0.9300
N3—C111.324 (5)C13—H13A0.9300
N4—C16i1.338 (4)C14—H14A0.9300
N4—C161.338 (4)C15—H15A0.9300
N5—C201.300 (4)C16—H16A0.9300
N6—C211.298 (4)C17—H17A0.9300
C1—C21.363 (6)C18—H18A0.9300
C2—C31.335 (6)C19—H19A0.9600
C3—C41.348 (7)C19—H19B0.9600
C4—C51.380 (6)C19—H19C0.9600
C6—C71.357 (6)C22—H22A0.9600
C7—C81.360 (6)C22—H22B0.9600
C8—C91.355 (6)C22—H22C0.9600
C9—C101.374 (6)
N5—Cu1—N5i156.84 (17)C13—C14—C15118.9 (5)
N5—Cu1—N680.65 (12)N3—C15—C14123.1 (5)
N5i—Cu1—N695.48 (12)N4—C16—C17123.1 (4)
N5—Cu1—N6i95.48 (12)C16—C17—C18118.9 (5)
N5i—Cu1—N6i80.65 (12)C17i—C18—C17119.7 (7)
N6—Cu1—N6i160.75 (17)N5—C20—C21115.0 (3)
N5—Cu1—N4101.58 (8)N5—C20—C19123.7 (3)
N5i—Cu1—N4101.58 (8)C21—C20—C19121.3 (3)
N6—Cu1—N499.62 (9)N6—C21—C20115.8 (3)
N6i—Cu1—N499.62 (9)N6—C21—C22122.3 (3)
O1—Cu2—O2i94.37 (11)C20—C21—C22121.9 (3)
O1—Cu2—N2177.23 (12)N1—C1—H1A117.5
O2i—Cu2—N287.69 (12)C2—C1—H1A117.5
O1—Cu2—N388.86 (12)C3—C2—H2A120.8
O2i—Cu2—N3155.43 (12)C1—C2—H2A120.8
N2—Cu2—N388.50 (13)C2—C3—H3A120.6
O1—Cu2—N187.55 (12)C4—C3—H3A120.6
O2i—Cu2—N1102.16 (12)C3—C4—H4A120.7
N2—Cu2—N193.84 (13)C5—C4—H4A120.7
N3—Cu2—N1102.32 (13)N1—C5—H5A118.2
O6—Cl1—O4112.5 (6)C4—C5—H5A118.2
O6—Cl1—O5102.3 (5)N2—C6—H6A118.4
O4—Cl1—O5111.5 (5)C7—C6—H6A118.4
O6—Cl1—O3116.0 (6)C6—C7—H7A120.3
O4—Cl1—O3104.9 (5)C8—C7—H7A120.3
O5—Cl1—O3109.7 (5)C9—C8—H8A120.7
N5—O1—Cu2116.30 (19)C7—C8—H8A120.7
N6—O2—Cu2i117.17 (19)C8—C9—H9A120.6
C5—N1—C1115.5 (4)C10—C9—H9A120.6
C5—N1—Cu2123.6 (3)N2—C10—H10A118.4
C1—N1—Cu2120.5 (3)C9—C10—H10A118.4
C10—N2—C6116.6 (4)N3—C11—H11A118.1
C10—N2—Cu2120.2 (3)C12—C11—H11A118.1
C6—N2—Cu2122.3 (3)C13—C12—H12A120.8
C15—N3—C11116.7 (4)C11—C12—H12A120.8
C15—N3—Cu2119.4 (3)C12—C13—H13A120.4
C11—N3—Cu2123.9 (3)C14—C13—H13A120.4
C16i—N4—C16116.3 (5)C13—C14—H14A120.6
C16i—N4—Cu1121.9 (2)C15—C14—H14A120.6
C16—N4—Cu1121.9 (2)N3—C15—H15A118.5
C20—N5—O1119.0 (3)C14—C15—H15A118.5
C20—N5—Cu1114.7 (2)N4—C16—H16A118.5
O1—N5—Cu1126.18 (19)C17—C16—H16A118.5
C21—N6—O2118.1 (3)C16—C17—H17A120.5
C21—N6—Cu1113.8 (2)C18—C17—H17A120.5
O2—N6—Cu1128.1 (2)C17—C18—H18A120.2
N1—C1—C2125.0 (5)C17i—C18—H18A120.2
C3—C2—C1118.3 (5)C20—C19—H19A109.5
C2—C3—C4118.9 (6)C20—C19—H19B109.5
C3—C4—C5118.5 (5)H19A—C19—H19B109.5
N1—C5—C4123.7 (5)C20—C19—H19C109.5
N2—C6—C7123.3 (4)H19A—C19—H19C109.5
C6—C7—C8119.3 (5)H19B—C19—H19C109.5
C9—C8—C7118.7 (5)C21—C22—H22A109.5
C8—C9—C10118.8 (5)C21—C22—H22B109.5
N2—C10—C9123.2 (4)H22A—C22—H22B109.5
N3—C11—C12123.8 (5)C21—C22—H22C109.5
C13—C12—C11118.4 (5)H22A—C22—H22C109.5
C12—C13—C14119.1 (5)H22B—C22—H22C109.5
Symmetry code: (i) x+1, y, z+1/2.
 

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