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In the crystal structure of [Co2(C10H2O8)(C3H7NO)2]n, the tetra-anion uses seven of its eight O atoms to interact with eight CoII atoms, as one of these seven binds to two metal atoms simultaneously. Four of the eight Co atoms are crystallograpically equivalent and exist in a tetrahedral environment; the other four, which belong to another equivalent set, are each also coordinated by two di­methyl­form­amide mol­ecules in an octahedral environment.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804021944/bt6512sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804021944/bt6512Isup2.hkl
Contains datablock I

CCDC reference: 252760

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.011 Å
  • R factor = 0.055
  • wR factor = 0.149
  • Data-to-parameter ratio = 11.5

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.87 Ratio
Author Response: This refers to the methyl groups of DMF. There is probably some disorder, but the disorder is not treated.
PLAT222_ALERT_3_A Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       7.75 Ratio
Author Response: Same as above.

Alert level B ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.522 0.887 Tmin' and Tmax expected: 0.710 0.884 RR' = 0.733 Please check that your absorption correction is appropriate. PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.72 PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors for N2
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.56 Ratio
Author Response: This refers to the methyl groups of DMF. There is probably some disorder, but the disorder is not treated.
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors  for         N1
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         11
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .      38.00 A   3  

Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 3163 Count of symmetry unique reflns 2254 Completeness (_total/calc) 140.33% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 909 Fraction of Friedel pairs measured 0.403 Are heavy atom types Z>Si present yes
2 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 1 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.

Bis(N,N-dimethylformamide)-1,2,4,5-benzenedicarboxylatodicobalt(II) top
Crystal data top
[Co2(C10H2O8)(C3H7NO)2]F(000) = 1040
Mr = 514.17Dx = 1.748 Mg m3
Monoclinic, CcMo Kα radiation, λ = 0.71073 Å
Hall symbol: C -2ycCell parameters from 826 reflections
a = 10.789 (3) Åθ = 2.3–19.6°
b = 15.420 (4) ŵ = 1.76 mm1
c = 11.742 (3) ÅT = 295 K
β = 90.555 (4)°Plate, purple
V = 1953.4 (8) Å30.19 × 0.16 × 0.07 mm
Z = 4
Data collection top
Bruker SMART APEX area-detector
diffractometer
3163 independent reflections
Radiation source: fine-focus sealed tube2580 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.058
φ and ω scanθmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1013
Tmin = 0.522, Tmax = 0.887k = 1820
5502 measured reflectionsl = 1514
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.055H-atom parameters constrained
wR(F2) = 0.149 w = 1/[σ2(Fo2) + (0.063P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
3163 reflectionsΔρmax = 0.63 e Å3
275 parametersΔρmin = 0.60 e Å3
26 restraintsAbsolute structure: Flack (1983), 975 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.17 (3)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Co10.50000 (9)0.61278 (6)0.50000 (9)0.0188 (3)
Co20.63640 (11)0.49490 (6)0.31152 (10)0.0156 (3)
O10.6788 (5)0.5805 (4)0.4349 (5)0.0203 (12)
O20.8263 (8)0.6258 (5)0.3224 (6)0.052 (2)
O30.6003 (6)0.6060 (4)0.6542 (5)0.0257 (14)
O40.7732 (6)0.5785 (4)0.7469 (5)0.0254 (14)
O50.9186 (6)0.8785 (4)0.8371 (5)0.0315 (16)
O61.0570 (6)0.9212 (4)0.7086 (5)0.0272 (14)
O70.9426 (6)0.9864 (3)0.5144 (5)0.0234 (13)
O81.0544 (6)0.9014 (4)0.4011 (5)0.0295 (15)
O90.3380 (7)0.6418 (5)0.5873 (6)0.0371 (17)
O100.5323 (7)0.7437 (4)0.4912 (7)0.0439 (19)
N10.2127 (8)0.6114 (6)0.7328 (8)0.043 (2)
N20.4572 (9)0.8710 (5)0.5527 (7)0.037 (2)
C10.7709 (8)0.6325 (5)0.4096 (6)0.0175 (17)
C20.7130 (8)0.6213 (5)0.6702 (6)0.0173 (16)
C30.9620 (9)0.8802 (5)0.7392 (7)0.0214 (18)
C40.9778 (7)0.9122 (5)0.4799 (6)0.0157 (17)
C50.8079 (8)0.6989 (5)0.4960 (7)0.0197 (17)
C60.7842 (7)0.6920 (5)0.6127 (6)0.0155 (16)
C70.8319 (8)0.7539 (5)0.6879 (7)0.0197 (17)
H70.81710.74810.76540.024*
C80.9010 (8)0.8240 (5)0.6496 (7)0.0206 (17)
C90.9208 (7)0.8338 (5)0.5317 (6)0.0157 (16)
C100.8774 (7)0.7693 (5)0.4592 (6)0.0168 (16)
H100.89570.77340.38220.020*
C110.3097 (9)0.5992 (6)0.6718 (8)0.033 (2)
H110.36270.55450.69350.039*
C120.1287 (16)0.6840 (11)0.7066 (14)0.089 (5)
H12a0.10100.70980.77630.133*
H12b0.05850.66300.66410.133*
H12c0.17180.72660.66250.133*
C130.1835 (12)0.5614 (10)0.8294 (11)0.061 (4)
H13a0.11080.52730.81380.091*
H13b0.16830.59910.89280.091*
H13c0.25170.52360.84750.091*
C140.4525 (12)0.7985 (8)0.4948 (11)0.054 (3)
H140.38080.78820.45240.064*
C150.5563 (19)0.8841 (12)0.6271 (15)0.103 (6)
H15a0.55240.84270.68800.155*
H15b0.55240.94170.65770.155*
H15c0.63270.87680.58690.155*
C160.3500 (16)0.9272 (11)0.5451 (15)0.088 (5)
H16a0.37010.97750.50080.132*
H16b0.32620.94480.62020.132*
H16c0.28270.89660.50930.132*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0236 (6)0.0142 (6)0.0187 (5)0.0004 (5)0.0021 (4)0.0011 (5)
Co20.0178 (5)0.0122 (5)0.0166 (5)0.0015 (5)0.0000 (4)0.0010 (4)
O10.024 (3)0.015 (3)0.022 (3)0.004 (2)0.000 (2)0.004 (2)
O20.072 (6)0.055 (5)0.029 (4)0.035 (4)0.029 (4)0.021 (3)
O30.030 (4)0.028 (3)0.020 (3)0.014 (3)0.000 (2)0.001 (2)
O40.025 (3)0.021 (3)0.031 (3)0.007 (3)0.005 (3)0.009 (3)
O50.033 (4)0.037 (4)0.025 (3)0.011 (3)0.002 (3)0.011 (3)
O60.033 (4)0.027 (3)0.021 (3)0.008 (3)0.003 (3)0.001 (3)
O70.030 (4)0.014 (3)0.026 (3)0.004 (2)0.004 (3)0.002 (2)
O80.043 (4)0.016 (3)0.030 (3)0.006 (3)0.011 (3)0.000 (3)
O90.039 (4)0.032 (4)0.040 (4)0.009 (3)0.008 (3)0.000 (3)
O100.047 (5)0.019 (3)0.066 (5)0.004 (3)0.013 (4)0.000 (3)
N10.034 (5)0.054 (6)0.042 (5)0.009 (4)0.011 (4)0.001 (4)
N20.049 (6)0.021 (4)0.042 (5)0.014 (4)0.002 (4)0.005 (4)
C10.027 (5)0.008 (4)0.018 (4)0.000 (3)0.001 (3)0.000 (3)
C20.025 (5)0.014 (4)0.013 (4)0.002 (3)0.000 (3)0.005 (3)
C30.030 (5)0.014 (4)0.020 (4)0.003 (4)0.008 (3)0.001 (3)
C40.017 (5)0.018 (4)0.012 (4)0.002 (3)0.005 (3)0.004 (3)
C50.025 (5)0.016 (4)0.018 (4)0.007 (3)0.000 (3)0.001 (3)
C60.018 (4)0.008 (4)0.020 (4)0.002 (3)0.000 (3)0.002 (3)
C70.029 (5)0.014 (4)0.016 (4)0.012 (3)0.005 (3)0.000 (3)
C80.025 (5)0.015 (4)0.022 (4)0.000 (3)0.002 (3)0.000 (3)
C90.016 (4)0.014 (4)0.017 (4)0.005 (3)0.000 (3)0.002 (3)
C100.018 (4)0.017 (4)0.015 (4)0.006 (3)0.002 (3)0.001 (3)
C110.032 (6)0.028 (5)0.038 (5)0.008 (4)0.004 (4)0.005 (4)
C120.079 (8)0.102 (9)0.085 (8)0.030 (7)0.014 (7)0.000 (7)
C130.052 (7)0.075 (7)0.056 (6)0.005 (6)0.017 (5)0.007 (6)
C140.055 (8)0.043 (7)0.063 (8)0.007 (6)0.009 (6)0.000 (6)
C150.100 (9)0.119 (10)0.091 (9)0.005 (8)0.007 (8)0.009 (8)
C160.094 (9)0.084 (8)0.086 (8)0.029 (7)0.015 (7)0.012 (7)
Geometric parameters (Å, º) top
Co1—O12.140 (6)C1—C51.493 (10)
Co1—O32.104 (6)C2—C61.499 (11)
Co1—O5i2.102 (6)C3—C81.510 (11)
Co1—O7ii2.052 (5)C4—C91.490 (11)
Co1—O92.083 (7)C5—C101.391 (11)
Co1—O102.051 (7)C5—C61.401 (11)
Co2—O12.010 (5)C6—C71.394 (11)
Co2—O4iii2.015 (6)C7—C81.390 (11)
Co2—O6i1.961 (6)C7—H70.9300
Co2—O8ii1.996 (6)C8—C91.411 (11)
O1—C11.312 (10)C9—C101.388 (10)
O2—C11.195 (10)C10—H100.9300
O3—C21.250 (10)C11—H110.9300
O4—C21.287 (9)C12—H12a0.9600
O5—C31.246 (11)C12—H12b0.9600
O6—C31.259 (11)C12—H12c0.9600
O7—C41.273 (10)C13—H13a0.9600
O8—C41.258 (11)C13—H13b0.9600
O9—C111.231 (12)C13—H13c0.9600
O10—C141.207 (13)C14—H140.9300
N1—C111.288 (13)C15—H15a0.9600
N1—C131.411 (16)C15—H15b0.9600
N1—C121.470 (17)C15—H15c0.9600
N2—C141.309 (14)C16—H16a0.9600
N2—C151.39 (2)C16—H16b0.9600
N2—C161.447 (17)C16—H16c0.9600
O1—Co1—O380.7 (2)O7—C4—C9118.3 (7)
O1—Co1—O5i93.4 (2)C10—C5—C6117.8 (7)
O1—Co1—O7ii94.7 (2)C10—C5—C1117.8 (7)
O1—Co1—O9171.4 (3)C6—C5—C1124.3 (7)
O1—Co1—O1093.3 (3)C7—C6—C5119.9 (7)
O3—Co1—O5i173.7 (3)C7—C6—C2113.6 (7)
O3—Co1—O7ii92.0 (2)C5—C6—C2126.5 (7)
O3—Co1—O990.8 (3)C8—C7—C6121.5 (7)
O3—Co1—O1090.3 (3)C8—C7—H7119.2
O5i—Co1—O7ii90.7 (3)C6—C7—H7119.2
O5i—Co1—O995.1 (3)C7—C8—C9119.1 (7)
O5i—Co1—O1087.8 (3)C7—C8—C3117.0 (7)
O7ii—Co1—O984.7 (3)C9—C8—C3123.6 (7)
O7ii—Co1—O10171.9 (3)C10—C9—C8118.2 (7)
O9—Co1—O1087.5 (3)C10—C9—C4118.0 (7)
O1—Co2—O4iii118.6 (2)C8—C9—C4123.7 (7)
O1—Co2—O6i96.1 (2)C9—C10—C5123.2 (7)
O1—Co2—O8ii101.1 (2)C9—C10—H10118.4
O4iii—Co2—O6i117.1 (3)C5—C10—H10118.4
O4iii—Co2—O8ii97.1 (3)O9—C11—N1125.5 (9)
O6i—Co2—O8ii127.4 (3)O9—C11—H11117.3
C1—O1—Co2113.9 (5)N1—C11—H11117.3
C1—O1—Co1128.8 (5)N1—C12—H12a109.5
Co2—O1—Co1102.1 (2)N1—C12—H12b109.5
C2—O3—Co1127.7 (5)H12a—C12—H12b109.5
C2—O4—Co2iv100.6 (5)N1—C12—H12c109.5
C3—O5—Co1v132.9 (6)H12a—C12—H12c109.5
C3—O6—Co2v120.5 (6)H12b—C12—H12c109.5
C4—O7—Co1vi137.4 (6)N1—C13—H13a109.5
C4—O8—Co2vi126.2 (5)N1—C13—H13b109.5
C11—O9—Co1119.9 (6)H13a—C13—H13b109.5
C14—O10—Co1124.5 (8)N1—C13—H13c109.5
C11—N1—C13123.8 (10)H13a—C13—H13c109.5
C11—N1—C12119.8 (10)H13b—C13—H13c109.5
C13—N1—C12116.3 (11)O10—C14—N2126.3 (13)
C14—N2—C15118.4 (12)O10—C14—H14116.9
C14—N2—C16116.9 (11)N2—C14—H14116.9
C15—N2—C16124.2 (13)N2—C15—H15a109.5
O2—C1—O1121.8 (7)N2—C15—H15b109.5
O2—C1—C5120.6 (8)H15a—C15—H15b109.5
O1—C1—C5117.6 (7)N2—C15—H15c109.5
O3—C2—O4119.5 (7)H15a—C15—H15c109.5
O3—C2—C6124.9 (7)H15b—C15—H15c109.5
O4—C2—C6115.4 (7)N2—C16—H16a109.5
O5—C3—O6126.0 (7)N2—C16—H16b109.5
O5—C3—C8117.7 (8)H16a—C16—H16b109.5
O6—C3—C8116.1 (8)N2—C16—H16c109.5
O8—C4—O7123.6 (8)H16a—C16—H16c109.5
O8—C4—C9118.0 (7)H16b—C16—H16c109.5
O6i—Co2—O1—C173.5 (5)Co1vi—O7—C4—O815.5 (12)
O8ii—Co2—O1—C1156.4 (5)Co1vi—O7—C4—C9167.5 (5)
O4iii—Co2—O1—C151.9 (6)O2—C1—C5—C1021.0 (12)
O6i—Co2—O1—Co169.2 (3)O1—C1—C5—C10161.3 (7)
O8ii—Co2—O1—Co160.9 (3)O2—C1—C5—C6154.6 (9)
O4iii—Co2—O1—Co1165.4 (2)O1—C1—C5—C623.1 (12)
O10—Co1—O1—C14.1 (7)C10—C5—C6—C71.1 (12)
O7ii—Co1—O1—C1177.0 (6)C1—C5—C6—C7174.5 (8)
O5i—Co1—O1—C192.1 (6)C10—C5—C6—C2179.3 (8)
O3—Co1—O1—C185.7 (6)C1—C5—C6—C23.7 (13)
O10—Co1—O1—Co2130.7 (3)O3—C2—C6—C7117.4 (9)
O7ii—Co1—O1—Co248.3 (3)O4—C2—C6—C757.5 (10)
O5i—Co1—O1—Co242.7 (3)O3—C2—C6—C564.3 (12)
O3—Co1—O1—Co2139.5 (3)O4—C2—C6—C5120.8 (9)
O10—Co1—O3—C264.0 (7)C5—C6—C7—C81.3 (13)
O7ii—Co1—O3—C2123.7 (7)C2—C6—C7—C8179.7 (8)
O9—Co1—O3—C2151.6 (7)C6—C7—C8—C91.5 (13)
O1—Co1—O3—C229.2 (7)C6—C7—C8—C3172.2 (8)
O10—Co1—O9—C11136.7 (8)O5—C3—C8—C721.6 (12)
O7ii—Co1—O9—C1145.5 (7)O6—C3—C8—C7154.7 (8)
O5i—Co1—O9—C11135.8 (7)O5—C3—C8—C9164.9 (8)
O3—Co1—O9—C1146.4 (8)O6—C3—C8—C918.7 (12)
O9—Co1—O10—C1425.3 (10)C7—C8—C9—C104.4 (12)
O5i—Co1—O10—C1469.9 (10)C3—C8—C9—C10168.9 (8)
O3—Co1—O10—C14116.1 (10)C7—C8—C9—C4171.1 (8)
O1—Co1—O10—C14163.3 (10)C3—C8—C9—C415.6 (13)
Co2—O1—C1—O22.9 (11)O8—C4—C9—C1045.5 (10)
Co1—O1—C1—O2133.5 (8)O7—C4—C9—C10131.7 (8)
Co2—O1—C1—C5179.4 (5)O8—C4—C9—C8139.0 (8)
Co1—O1—C1—C548.8 (9)O7—C4—C9—C843.9 (11)
Co1—O3—C2—O4147.2 (6)C8—C9—C10—C54.7 (12)
Co1—O3—C2—C638.1 (11)C4—C9—C10—C5171.1 (8)
Co2iv—O4—C2—O32.5 (8)C6—C5—C10—C91.9 (13)
Co2iv—O4—C2—C6172.8 (5)C1—C5—C10—C9177.9 (7)
Co1v—O5—C3—O631.1 (14)Co1—O9—C11—N1179.6 (8)
Co1v—O5—C3—C8144.8 (6)C13—N1—C11—O9179.8 (11)
Co2v—O6—C3—O59.8 (13)C12—N1—C11—O93.2 (17)
Co2v—O6—C3—C8174.2 (5)Co1—O10—C14—N2136.9 (11)
Co2vi—O8—C4—O70.7 (11)C15—N2—C14—O107 (2)
Co2vi—O8—C4—C9176.3 (5)C16—N2—C14—O10179.6 (13)
Symmetry codes: (i) x1/2, y+3/2, z1/2; (ii) x1/2, y1/2, z; (iii) x, y+1, z1/2; (iv) x, y+1, z+1/2; (v) x+1/2, y+3/2, z+1/2; (vi) x+1/2, y+1/2, z.
 

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