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The solvothermal reaction of cobalt(II) nitrate and terephthalic acid in N,N-di­methyl­form­amide (DMF) yields the polymeric title compound, poly­[cobalt(II)-μ2-N,N-di­methyl­form­amide-κ2O:O4-terephthalato- κ4O:O′:O′′:O′′′], [Co(C8H4O4)(C3H7NO)]n. In the crystal structure, both the Co atom and the terephthalate group occupy special positions of 2/m site symmetry. The DMF ligand is located on a mirror plane with the N atom on a special position of site symmetry mm2. The octahedral coordination polyhedron around the Co atom has two opposite sites that are occupied by the O atoms of DMF mol­ecules; the other sites are occupied by the carboxyl O atoms of four different terephthalate groups. The compound adopts an open framework structure having channels in which the disordered DMF mol­ecules reside.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804023384/bt6522sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804023384/bt6522Isup2.hkl
Contains datablock I

CCDC reference: 252945

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.032
  • wR factor = 0.093
  • Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . C4 PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . C5 PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . C6 PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . H4 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.27 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.31 Ratio PLAT301_ALERT_3_C Main Residue Disorder ......................... 15.00 Perc.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 6 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 2 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, 2002); cell refinement: SAINT (Bruker, 2002); 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.

poly[cobalt(II)-µ2-N,N-dimethylformamide-κ2O:O4-terephthalato- κ4O:O':O'':O'''] top
Crystal data top
[Co(C8H4O4)(C3H7NO)]F(000) = 604
Mr = 296.14Dx = 1.591 Mg m3
Orthorhombic, ImmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -I 2b 2Cell parameters from 4989 reflections
a = 19.258 (1) Åθ = 2.5–28.1°
b = 7.2459 (4) ŵ = 1.40 mm1
c = 8.8593 (5) ÅT = 295 K
V = 1236.3 (1) Å3Prism, pink
Z = 40.39 × 0.38 × 0.33 mm
Data collection top
Bruker APEX area-detector
diffractometer
789 independent reflections
Radiation source: fine-focus sealed tube781 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
φ and ω scansθmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 2424
Tmin = 0.536, Tmax = 0.629k = 99
6527 measured reflectionsl = 1111
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.093H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.064P)2 + 1.9208P]
where P = (Fo2 + 2Fc2)/3
789 reflections(Δ/σ)max = 0.001
63 parametersΔρmax = 0.69 e Å3
3 restraintsΔρmin = 0.78 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.50000.50000.50000.0164 (2)
O10.4221 (1)0.5959 (2)0.3647 (2)0.0346 (4)
O20.50000.75000.6379 (3)0.0273 (6)
N10.50000.75000.8946 (4)0.049 (1)
C10.3943 (1)0.75000.3467 (3)0.0263 (6)
C20.3194 (2)0.75000.2961 (4)0.0295 (6)
C30.2842 (1)0.5864 (3)0.2736 (4)0.0536 (8)
C40.5269 (4)0.75000.7581 (7)0.033 (1)0.50
C50.5297 (6)0.75001.0370 (9)0.072 (4)0.50
C60.4261 (5)0.75000.8993 (11)0.086 (4)0.50
H30.30670.47480.29050.064*
H40.57520.75000.75560.039*0.50
H5a0.57700.79091.03000.108*0.25
H5b0.52850.62731.07780.108*0.25
H5c0.50420.83171.10170.108*0.25
H6a0.41080.70250.99480.129*0.25
H6b0.40840.67370.81950.129*0.25
H6c0.40940.87380.88670.129*0.25
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0121 (3)0.0171 (3)0.0200 (3)0.0000.0000.0011 (2)
O10.0257 (7)0.0282 (8)0.0499 (9)0.0034 (6)0.0197 (7)0.0004 (7)
O20.043 (2)0.019 (1)0.020 (1)0.0000.0000.000
N10.090 (4)0.036 (2)0.022 (2)0.0000.0000.000
C10.020 (1)0.028 (1)0.031 (1)0.0000.0111 (11)0.000
C20.022 (1)0.026 (1)0.041 (2)0.0000.0145 (11)0.000
C30.031 (1)0.024 (1)0.106 (2)0.003 (1)0.033 (2)0.003 (1)
C40.046 (3)0.022 (2)0.030 (3)0.0000.009 (2)0.000
C50.13 (1)0.052 (5)0.032 (3)0.0000.019 (5)0.000
C60.15 (1)0.069 (7)0.040 (5)0.0000.030 (6)0.000
Geometric parameters (Å, º) top
Co1—O12.042 (1)N1—C61.423 (9)
Co1—O1i2.042 (1)C1—O1v1.249 (2)
Co1—O1ii2.042 (1)C1—C21.510 (4)
Co1—O1iii2.042 (1)C2—C31.380 (3)
Co1—O22.185 (2)C2—C3v1.380 (3)
Co1—O2ii2.185 (2)C3—C3vi1.382 (4)
O1—C11.249 (2)C3—H30.93
O2—C41.184 (7)C4—H40.93
O2—C4iv1.184 (7)C5—H5a0.96
N1—C4iv1.316 (6)C5—H5b0.96
N1—C41.316 (6)C5—H5c0.96
N1—C51.385 (7)C6—H6a0.96
N1—C5iv1.385 (7)C6—H6b0.96
N1—C6iv1.423 (9)C6—H6c0.96
O1—Co1—O1i85.5 (1)C4—N1—C5132.4 (6)
O1—Co1—O292.6 (1)C4—N1—C6114.9 (6)
O1—Co1—O1ii180C5—N1—C6112.7 (7)
O1—Co1—O1iii94.6 (1)O1v—C1—O1126.8 (3)
O1—Co1—O2ii87.4 (1)O1v—C1—C2116.6 (1)
O1i—Co1—O1ii94.6 (1)O1—C1—C2116.6 (1)
O1i—Co1—O1iii180C3—C2—C3v118.4 (3)
O1i—Co1—O287.4 (1)C3—C2—C1120.8 (1)
O1i—Co1—O2ii92.6 (1)C3v—C2—C1120.8 (1)
O1ii—Co1—O1iii85.5 (1)C3vi—C3—C2120.8 (1)
O1ii—Co1—O287.4 (1)C3vi—C3—H3119.6
O1ii—Co1—O2ii92.6 (1)C2—C3—H3119.6
O1iii—Co1—O292.6 (1)O2—C4—N1130.8 (6)
O1iii—Co1—O2ii87.4 (1)O2—C4—H4114.6
O2ii—Co1—O2180N1—C4—H4114.6
C1—O1—Co1134.0 (2)N1—C5—H5a109.5
C4—O2—Co1120.2 (1)N1—C5—H5b109.5
C4iv—O2—Co1120.2 (1)N1—C5—H5c109.5
C4—O2—Co1iv120.2 (1)N1—C6—H6a109.5
C4iv—O2—Co1iv120.2 (1)N1—C6—H6b109.5
Co1—O2—Co1iv112.0 (1)N1—C6—H6c109.5
O1iii—Co1—O1—C180.4 (3)Co1—O1—C1—O1v29.3 (5)
O1i—Co1—O1—C199.6 (3)Co1—O1—C1—C2151.4 (2)
O2ii—Co1—O1—C1167.6 (3)O1v—C1—C2—C3179.8 (3)
O2—Co1—O1—C112.4 (3)O1—C1—C2—C30.9 (5)
O1iii—Co1—O2—C4102.2 (4)O1v—C1—C2—C3v0.9 (5)
O1—Co1—O2—C4163.1 (4)O1—C1—C2—C3v179.8 (3)
O1ii—Co1—O2—C416.9 (4)C3v—C2—C3—C3vi1.5 (8)
O1i—Co1—O2—C477.8 (4)C1—C2—C3—C3vi179.6 (4)
O1iii—Co1—O2—C4iv163.1 (4)C4iv—O2—C4—N10.0
O1—Co1—O2—C4iv102.2 (4)Co1—O2—C4—N1106.4 (2)
O1ii—Co1—O2—C4iv77.8 (4)Co1iv—O2—C4—N1106.4 (2)
O1i—Co1—O2—C4iv16.9 (4)C4iv—N1—C4—O20.0
O1iii—Co1—O2—Co1iv47.34 (5)C5—N1—C4—O2180
O1—Co1—O2—Co1iv47.34 (5)C6iv—N1—C4—O2180
O1ii—Co1—O2—Co1iv132.7 (1)C6—N1—C4—O20
O1i—Co1—O2—Co1iv132.7 (1)
Symmetry codes: (i) x, y+1, z+1; (ii) x+1, y+1, z+1; (iii) x+1, y, z; (iv) x+1, y+3/2, z; (v) x, y+3/2, z; (vi) x+1/2, y, z+1/2.
 

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