Download citation
Download citation
link to html
The asymmetric unit of the title polymer, poly[copper(II)-μ6-benzene-1,3,5-tricarboxyl­ato-tri-μ3-hydroxo], [Cu3(C9H3O6)(OH)3]n, contains two independent CuII atoms, one located in a general position assuming a pyramidal coordination geometry, and the other located on an inversion center assuming a square-planar geometry. The benzene­tricarboxyl­ate and hydroxo groups bridge the CuII atoms to form a three-dimensional polymeric structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805025687/xu6033sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805025687/xu6033Isup2.hkl
Contains datablock I

CCDC reference: 284007

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.023
  • wR factor = 0.065
  • Data-to-parameter ratio = 9.9

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O1 - H1A ... ?
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.376 0.630 Tmin(prime) and Tmax expected: 0.435 0.630 RR(prime) = 0.864 Please check that your absorption correction is appropriate. PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.84 PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.90 PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT213_ALERT_2_C Atom O5 has ADP max/min Ratio ............. 3.10 prolat PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 3.53 PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ ! PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

poly[copper(II)-µ6-benzene-1,3,5-tricarboxylato-tri-µ3-hydroxo] top
Crystal data top
[Cu3(C9H3O6)(OH)3]F(000) = 438
Mr = 448.76Dx = 2.701 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 1551 reflections
a = 3.6100 (11) Åθ = 2.4–24.9°
b = 14.110 (4) ŵ = 5.78 mm1
c = 10.915 (3) ÅT = 293 K
β = 97.060 (4)°Block, blue
V = 551.8 (3) Å30.14 × 0.12 × 0.08 mm
Z = 2
Data collection top
Bruker APEX-II CCD area-detector
diffractometer
1020 independent reflections
Radiation source: Rigaku rotating anode generator914 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
φ and ω scansθmax = 25.0°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 43
Tmin = 0.376, Tmax = 0.630k = 1616
2985 measured reflectionsl = 912
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)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.065H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0412P)2 + 0.6748P]
where P = (Fo2 + 2Fc2)/3
1020 reflections(Δ/σ)max = 0.001
103 parametersΔρmax = 0.75 e Å3
0 restraintsΔρmin = 0.38 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
Cu10.45911 (12)0.37002 (3)0.72375 (4)0.01567 (16)
Cu20.00000.50000.50000.01400 (18)
O10.5038 (9)0.25000.6393 (3)0.0180 (8)
H1A0.33010.25000.57080.022*
O20.0155 (6)0.40055 (16)0.6144 (2)0.0153 (5)
H2A0.08730.34930.57630.018*
O30.3654 (8)0.57695 (16)0.6082 (2)0.0224 (6)
O40.4998 (7)0.49913 (16)0.7876 (2)0.0196 (6)
O50.8104 (7)0.32981 (16)0.8645 (2)0.0232 (6)
C10.4745 (9)0.5724 (2)0.7232 (3)0.0137 (7)
C20.5867 (8)0.6643 (2)0.7871 (3)0.0112 (7)
C30.4985 (12)0.75000.7273 (4)0.0120 (9)
H30.37990.75000.64670.014*
C40.8953 (13)0.25000.9117 (4)0.0119 (10)
C51.1199 (12)0.25001.0361 (4)0.0116 (9)
C61.2220 (9)0.3358 (2)1.0946 (3)0.0118 (7)
H61.16190.39291.05430.014*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0229 (3)0.0076 (2)0.0134 (3)0.00080 (16)0.01023 (17)0.00014 (15)
Cu20.0194 (3)0.0103 (3)0.0100 (3)0.0020 (2)0.0076 (2)0.0016 (2)
O10.0235 (19)0.0099 (16)0.0177 (18)0.0000.0092 (14)0.000
O20.0204 (13)0.0091 (11)0.0139 (12)0.0042 (10)0.0079 (9)0.0018 (9)
O30.0384 (16)0.0136 (12)0.0120 (12)0.0084 (11)0.0102 (11)0.0005 (9)
O40.0341 (15)0.0085 (11)0.0130 (12)0.0008 (10)0.0094 (10)0.0000 (9)
O50.0378 (16)0.0083 (12)0.0185 (13)0.0009 (11)0.0170 (11)0.0035 (10)
C10.0135 (16)0.0127 (17)0.0133 (17)0.0003 (13)0.0041 (13)0.0030 (13)
C20.0128 (16)0.0068 (16)0.0128 (17)0.0007 (12)0.0031 (13)0.0016 (12)
C30.013 (2)0.014 (2)0.007 (2)0.0000.0054 (17)0.000
C40.015 (2)0.009 (2)0.012 (2)0.0000.0011 (18)0.000
C50.010 (2)0.013 (2)0.011 (2)0.0000.0031 (17)0.000
C60.0140 (16)0.0085 (15)0.0122 (16)0.0013 (12)0.0016 (13)0.0016 (12)
Geometric parameters (Å, º) top
Cu1—O11.9444 (18)O4—C11.247 (4)
Cu1—O21.925 (2)O5—C41.260 (3)
Cu1—O2i2.496 (3)C1—C21.505 (4)
Cu1—O41.950 (2)C2—C31.392 (4)
Cu1—O51.953 (2)C2—C6iv1.387 (5)
Cu2—O21.875 (2)C3—C2v1.392 (4)
Cu2—O2ii1.875 (2)C3—H30.9300
Cu2—O31.983 (2)C4—O5iii1.260 (3)
Cu2—O3ii1.983 (2)C4—C51.494 (6)
O1—Cu1iii1.9444 (18)C5—C61.397 (4)
O1—H1A0.9148C5—C6iii1.397 (4)
O2—H2A0.8923C6—C2iv1.387 (5)
O3—C11.270 (4)C6—H60.9300
O1—Cu1—O2i78.76 (11)C1—O3—Cu2131.6 (2)
O2—Cu1—O2i108.80 (10)C1—O4—Cu1125.2 (2)
O4—Cu1—O2i88.86 (10)C4—O5—Cu1133.1 (2)
O5—Cu1—O2i86.75 (10)O4—C1—O3126.2 (3)
O2—Cu1—O190.70 (12)O4—C1—C2117.2 (3)
O2—Cu1—O491.88 (10)O3—C1—C2116.6 (3)
O1—Cu1—O4167.52 (13)C3—C2—C6iv119.8 (3)
O2—Cu1—O5164.44 (11)C3—C2—C1119.9 (3)
O1—Cu1—O592.09 (12)C6iv—C2—C1120.3 (3)
O4—Cu1—O588.68 (10)C2v—C3—C2120.5 (4)
O2—Cu2—O2ii180.000 (1)C2v—C3—H3119.8
O2—Cu2—O392.85 (10)C2—C3—H3119.8
O2ii—Cu2—O387.15 (10)O5iii—C4—O5126.7 (4)
O2—Cu2—O3ii87.15 (10)O5iii—C4—C5116.7 (2)
O2ii—Cu2—O3ii92.85 (10)O5—C4—C5116.7 (2)
O3—Cu2—O3ii180.00 (11)C6—C5—C6iii120.2 (4)
Cu1—O1—Cu1iii121.13 (18)C6—C5—C4119.9 (2)
Cu1—O1—H1A107.4C6iii—C5—C4119.9 (2)
Cu1iii—O1—H1A107.4C2iv—C6—C5119.8 (3)
Cu2—O2—Cu1122.34 (12)C2iv—C6—H6120.1
Cu2—O2—H2A108.6C5—C6—H6120.1
Cu1—O2—H2A112.0
O2—Cu1—O1—Cu1iii115.72 (19)Cu2—O3—C1—O431.6 (5)
O4—Cu1—O1—Cu1iii142.3 (4)Cu2—O3—C1—C2148.9 (2)
O5—Cu1—O1—Cu1iii49.0 (2)O4—C1—C2—C3167.6 (4)
O3—Cu2—O2—Cu132.05 (15)O3—C1—C2—C312.9 (5)
O3ii—Cu2—O2—Cu1147.95 (15)O4—C1—C2—C6iv12.5 (5)
O1—Cu1—O2—Cu2112.75 (16)O3—C1—C2—C6iv167.0 (3)
O4—Cu1—O2—Cu255.04 (15)C6iv—C2—C3—C2v2.8 (7)
O5—Cu1—O2—Cu2146.9 (3)C1—C2—C3—C2v177.3 (3)
O2—Cu1—O4—C147.6 (3)Cu1—O5—C4—O5iii12.9 (8)
O1—Cu1—O4—C154.3 (6)Cu1—O5—C4—C5167.2 (3)
O5—Cu1—O4—C1148.0 (3)O5iii—C4—C5—C6179.5 (4)
O2—Cu1—O5—C471.4 (6)O5—C4—C5—C60.5 (6)
O1—Cu1—O5—C428.8 (4)O5iii—C4—C5—C6iii0.5 (6)
O4—Cu1—O5—C4163.7 (4)O5—C4—C5—C6iii179.5 (4)
Cu1—O4—C1—O311.0 (5)C6iii—C5—C6—C2iv2.4 (7)
Cu1—O4—C1—C2168.4 (2)C4—C5—C6—C2iv176.6 (4)
Symmetry codes: (i) x+1, y, z; (ii) x, y+1, z+1; (iii) x, y+1/2, z; (iv) x+2, y+1, z+2; (v) x, y+3/2, z.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds