metal-organic compounds
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
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804021944/bt6512sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804021944/bt6512Isup2.hkl |
CCDC reference: 252760
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 = 514.17 | Dx = 1.748 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C -2yc | Cell parameters from 826 reflections |
a = 10.789 (3) Å | θ = 2.3–19.6° |
b = 15.420 (4) Å | µ = 1.76 mm−1 |
c = 11.742 (3) Å | T = 295 K |
β = 90.555 (4)° | Plate, purple |
V = 1953.4 (8) Å3 | 0.19 × 0.16 × 0.07 mm |
Z = 4 |
Data collection top
Bruker SMART APEX area-detector diffractometer | 3163 independent reflections |
Radiation source: fine-focus sealed tube | 2580 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.058 |
φ and ω scan | θmax = 27.5°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −10→13 |
Tmin = 0.522, Tmax = 0.887 | k = −18→20 |
5502 measured reflections | l = −15→14 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.055 | H-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 reflections | Δρmax = 0.63 e Å−3 |
275 parameters | Δρmin = −0.60 e Å−3 |
26 restraints | Absolute structure: Flack (1983), 975 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.17 (3) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Co1 | 0.50000 (9) | 0.61278 (6) | 0.50000 (9) | 0.0188 (3) | |
Co2 | 0.63640 (11) | 0.49490 (6) | 0.31152 (10) | 0.0156 (3) | |
O1 | 0.6788 (5) | 0.5805 (4) | 0.4349 (5) | 0.0203 (12) | |
O2 | 0.8263 (8) | 0.6258 (5) | 0.3224 (6) | 0.052 (2) | |
O3 | 0.6003 (6) | 0.6060 (4) | 0.6542 (5) | 0.0257 (14) | |
O4 | 0.7732 (6) | 0.5785 (4) | 0.7469 (5) | 0.0254 (14) | |
O5 | 0.9186 (6) | 0.8785 (4) | 0.8371 (5) | 0.0315 (16) | |
O6 | 1.0570 (6) | 0.9212 (4) | 0.7086 (5) | 0.0272 (14) | |
O7 | 0.9426 (6) | 0.9864 (3) | 0.5144 (5) | 0.0234 (13) | |
O8 | 1.0544 (6) | 0.9014 (4) | 0.4011 (5) | 0.0295 (15) | |
O9 | 0.3380 (7) | 0.6418 (5) | 0.5873 (6) | 0.0371 (17) | |
O10 | 0.5323 (7) | 0.7437 (4) | 0.4912 (7) | 0.0439 (19) | |
N1 | 0.2127 (8) | 0.6114 (6) | 0.7328 (8) | 0.043 (2) | |
N2 | 0.4572 (9) | 0.8710 (5) | 0.5527 (7) | 0.037 (2) | |
C1 | 0.7709 (8) | 0.6325 (5) | 0.4096 (6) | 0.0175 (17) | |
C2 | 0.7130 (8) | 0.6213 (5) | 0.6702 (6) | 0.0173 (16) | |
C3 | 0.9620 (9) | 0.8802 (5) | 0.7392 (7) | 0.0214 (18) | |
C4 | 0.9778 (7) | 0.9122 (5) | 0.4799 (6) | 0.0157 (17) | |
C5 | 0.8079 (8) | 0.6989 (5) | 0.4960 (7) | 0.0197 (17) | |
C6 | 0.7842 (7) | 0.6920 (5) | 0.6127 (6) | 0.0155 (16) | |
C7 | 0.8319 (8) | 0.7539 (5) | 0.6879 (7) | 0.0197 (17) | |
H7 | 0.8171 | 0.7481 | 0.7654 | 0.024* | |
C8 | 0.9010 (8) | 0.8240 (5) | 0.6496 (7) | 0.0206 (17) | |
C9 | 0.9208 (7) | 0.8338 (5) | 0.5317 (6) | 0.0157 (16) | |
C10 | 0.8774 (7) | 0.7693 (5) | 0.4592 (6) | 0.0168 (16) | |
H10 | 0.8957 | 0.7734 | 0.3822 | 0.020* | |
C11 | 0.3097 (9) | 0.5992 (6) | 0.6718 (8) | 0.033 (2) | |
H11 | 0.3627 | 0.5545 | 0.6935 | 0.039* | |
C12 | 0.1287 (16) | 0.6840 (11) | 0.7066 (14) | 0.089 (5) | |
H12a | 0.1010 | 0.7098 | 0.7763 | 0.133* | |
H12b | 0.0585 | 0.6630 | 0.6641 | 0.133* | |
H12c | 0.1718 | 0.7266 | 0.6625 | 0.133* | |
C13 | 0.1835 (12) | 0.5614 (10) | 0.8294 (11) | 0.061 (4) | |
H13a | 0.1108 | 0.5273 | 0.8138 | 0.091* | |
H13b | 0.1683 | 0.5991 | 0.8928 | 0.091* | |
H13c | 0.2517 | 0.5236 | 0.8475 | 0.091* | |
C14 | 0.4525 (12) | 0.7985 (8) | 0.4948 (11) | 0.054 (3) | |
H14 | 0.3808 | 0.7882 | 0.4524 | 0.064* | |
C15 | 0.5563 (19) | 0.8841 (12) | 0.6271 (15) | 0.103 (6) | |
H15a | 0.5524 | 0.8427 | 0.6880 | 0.155* | |
H15b | 0.5524 | 0.9417 | 0.6577 | 0.155* | |
H15c | 0.6327 | 0.8768 | 0.5869 | 0.155* | |
C16 | 0.3500 (16) | 0.9272 (11) | 0.5451 (15) | 0.088 (5) | |
H16a | 0.3701 | 0.9775 | 0.5008 | 0.132* | |
H16b | 0.3262 | 0.9448 | 0.6202 | 0.132* | |
H16c | 0.2827 | 0.8966 | 0.5093 | 0.132* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0236 (6) | 0.0142 (6) | 0.0187 (5) | 0.0004 (5) | 0.0021 (4) | −0.0011 (5) |
Co2 | 0.0178 (5) | 0.0122 (5) | 0.0166 (5) | 0.0015 (5) | 0.0000 (4) | −0.0010 (4) |
O1 | 0.024 (3) | 0.015 (3) | 0.022 (3) | −0.004 (2) | 0.000 (2) | −0.004 (2) |
O2 | 0.072 (6) | 0.055 (5) | 0.029 (4) | −0.035 (4) | 0.029 (4) | −0.021 (3) |
O3 | 0.030 (4) | 0.028 (3) | 0.020 (3) | −0.014 (3) | 0.000 (2) | 0.001 (2) |
O4 | 0.025 (3) | 0.021 (3) | 0.031 (3) | −0.007 (3) | 0.005 (3) | 0.009 (3) |
O5 | 0.033 (4) | 0.037 (4) | 0.025 (3) | −0.011 (3) | 0.002 (3) | −0.011 (3) |
O6 | 0.033 (4) | 0.027 (3) | 0.021 (3) | −0.008 (3) | −0.003 (3) | 0.001 (3) |
O7 | 0.030 (4) | 0.014 (3) | 0.026 (3) | −0.004 (2) | 0.004 (3) | 0.002 (2) |
O8 | 0.043 (4) | 0.016 (3) | 0.030 (3) | −0.006 (3) | 0.011 (3) | 0.000 (3) |
O9 | 0.039 (4) | 0.032 (4) | 0.040 (4) | 0.009 (3) | 0.008 (3) | 0.000 (3) |
O10 | 0.047 (5) | 0.019 (3) | 0.066 (5) | 0.004 (3) | 0.013 (4) | 0.000 (3) |
N1 | 0.034 (5) | 0.054 (6) | 0.042 (5) | 0.009 (4) | 0.011 (4) | −0.001 (4) |
N2 | 0.049 (6) | 0.021 (4) | 0.042 (5) | 0.014 (4) | 0.002 (4) | −0.005 (4) |
C1 | 0.027 (5) | 0.008 (4) | 0.018 (4) | 0.000 (3) | 0.001 (3) | 0.000 (3) |
C2 | 0.025 (5) | 0.014 (4) | 0.013 (4) | −0.002 (3) | 0.000 (3) | −0.005 (3) |
C3 | 0.030 (5) | 0.014 (4) | 0.020 (4) | −0.003 (4) | −0.008 (3) | 0.001 (3) |
C4 | 0.017 (5) | 0.018 (4) | 0.012 (4) | −0.002 (3) | −0.005 (3) | −0.004 (3) |
C5 | 0.025 (5) | 0.016 (4) | 0.018 (4) | −0.007 (3) | 0.000 (3) | −0.001 (3) |
C6 | 0.018 (4) | 0.008 (4) | 0.020 (4) | −0.002 (3) | 0.000 (3) | 0.002 (3) |
C7 | 0.029 (5) | 0.014 (4) | 0.016 (4) | −0.012 (3) | 0.005 (3) | 0.000 (3) |
C8 | 0.025 (5) | 0.015 (4) | 0.022 (4) | 0.000 (3) | −0.002 (3) | 0.000 (3) |
C9 | 0.016 (4) | 0.014 (4) | 0.017 (4) | −0.005 (3) | 0.000 (3) | −0.002 (3) |
C10 | 0.018 (4) | 0.017 (4) | 0.015 (4) | −0.006 (3) | 0.002 (3) | 0.001 (3) |
C11 | 0.032 (6) | 0.028 (5) | 0.038 (5) | 0.008 (4) | 0.004 (4) | −0.005 (4) |
C12 | 0.079 (8) | 0.102 (9) | 0.085 (8) | 0.030 (7) | 0.014 (7) | 0.000 (7) |
C13 | 0.052 (7) | 0.075 (7) | 0.056 (6) | −0.005 (6) | 0.017 (5) | −0.007 (6) |
C14 | 0.055 (8) | 0.043 (7) | 0.063 (8) | 0.007 (6) | 0.009 (6) | 0.000 (6) |
C15 | 0.100 (9) | 0.119 (10) | 0.091 (9) | −0.005 (8) | −0.007 (8) | −0.009 (8) |
C16 | 0.094 (9) | 0.084 (8) | 0.086 (8) | 0.029 (7) | 0.015 (7) | 0.012 (7) |
Geometric parameters (Å, º) top
Co1—O1 | 2.140 (6) | C1—C5 | 1.493 (10) |
Co1—O3 | 2.104 (6) | C2—C6 | 1.499 (11) |
Co1—O5i | 2.102 (6) | C3—C8 | 1.510 (11) |
Co1—O7ii | 2.052 (5) | C4—C9 | 1.490 (11) |
Co1—O9 | 2.083 (7) | C5—C10 | 1.391 (11) |
Co1—O10 | 2.051 (7) | C5—C6 | 1.401 (11) |
Co2—O1 | 2.010 (5) | C6—C7 | 1.394 (11) |
Co2—O4iii | 2.015 (6) | C7—C8 | 1.390 (11) |
Co2—O6i | 1.961 (6) | C7—H7 | 0.9300 |
Co2—O8ii | 1.996 (6) | C8—C9 | 1.411 (11) |
O1—C1 | 1.312 (10) | C9—C10 | 1.388 (10) |
O2—C1 | 1.195 (10) | C10—H10 | 0.9300 |
O3—C2 | 1.250 (10) | C11—H11 | 0.9300 |
O4—C2 | 1.287 (9) | C12—H12a | 0.9600 |
O5—C3 | 1.246 (11) | C12—H12b | 0.9600 |
O6—C3 | 1.259 (11) | C12—H12c | 0.9600 |
O7—C4 | 1.273 (10) | C13—H13a | 0.9600 |
O8—C4 | 1.258 (11) | C13—H13b | 0.9600 |
O9—C11 | 1.231 (12) | C13—H13c | 0.9600 |
O10—C14 | 1.207 (13) | C14—H14 | 0.9300 |
N1—C11 | 1.288 (13) | C15—H15a | 0.9600 |
N1—C13 | 1.411 (16) | C15—H15b | 0.9600 |
N1—C12 | 1.470 (17) | C15—H15c | 0.9600 |
N2—C14 | 1.309 (14) | C16—H16a | 0.9600 |
N2—C15 | 1.39 (2) | C16—H16b | 0.9600 |
N2—C16 | 1.447 (17) | C16—H16c | 0.9600 |
O1—Co1—O3 | 80.7 (2) | O7—C4—C9 | 118.3 (7) |
O1—Co1—O5i | 93.4 (2) | C10—C5—C6 | 117.8 (7) |
O1—Co1—O7ii | 94.7 (2) | C10—C5—C1 | 117.8 (7) |
O1—Co1—O9 | 171.4 (3) | C6—C5—C1 | 124.3 (7) |
O1—Co1—O10 | 93.3 (3) | C7—C6—C5 | 119.9 (7) |
O3—Co1—O5i | 173.7 (3) | C7—C6—C2 | 113.6 (7) |
O3—Co1—O7ii | 92.0 (2) | C5—C6—C2 | 126.5 (7) |
O3—Co1—O9 | 90.8 (3) | C8—C7—C6 | 121.5 (7) |
O3—Co1—O10 | 90.3 (3) | C8—C7—H7 | 119.2 |
O5i—Co1—O7ii | 90.7 (3) | C6—C7—H7 | 119.2 |
O5i—Co1—O9 | 95.1 (3) | C7—C8—C9 | 119.1 (7) |
O5i—Co1—O10 | 87.8 (3) | C7—C8—C3 | 117.0 (7) |
O7ii—Co1—O9 | 84.7 (3) | C9—C8—C3 | 123.6 (7) |
O7ii—Co1—O10 | 171.9 (3) | C10—C9—C8 | 118.2 (7) |
O9—Co1—O10 | 87.5 (3) | C10—C9—C4 | 118.0 (7) |
O1—Co2—O4iii | 118.6 (2) | C8—C9—C4 | 123.7 (7) |
O1—Co2—O6i | 96.1 (2) | C9—C10—C5 | 123.2 (7) |
O1—Co2—O8ii | 101.1 (2) | C9—C10—H10 | 118.4 |
O4iii—Co2—O6i | 117.1 (3) | C5—C10—H10 | 118.4 |
O4iii—Co2—O8ii | 97.1 (3) | O9—C11—N1 | 125.5 (9) |
O6i—Co2—O8ii | 127.4 (3) | O9—C11—H11 | 117.3 |
C1—O1—Co2 | 113.9 (5) | N1—C11—H11 | 117.3 |
C1—O1—Co1 | 128.8 (5) | N1—C12—H12a | 109.5 |
Co2—O1—Co1 | 102.1 (2) | N1—C12—H12b | 109.5 |
C2—O3—Co1 | 127.7 (5) | H12a—C12—H12b | 109.5 |
C2—O4—Co2iv | 100.6 (5) | N1—C12—H12c | 109.5 |
C3—O5—Co1v | 132.9 (6) | H12a—C12—H12c | 109.5 |
C3—O6—Co2v | 120.5 (6) | H12b—C12—H12c | 109.5 |
C4—O7—Co1vi | 137.4 (6) | N1—C13—H13a | 109.5 |
C4—O8—Co2vi | 126.2 (5) | N1—C13—H13b | 109.5 |
C11—O9—Co1 | 119.9 (6) | H13a—C13—H13b | 109.5 |
C14—O10—Co1 | 124.5 (8) | N1—C13—H13c | 109.5 |
C11—N1—C13 | 123.8 (10) | H13a—C13—H13c | 109.5 |
C11—N1—C12 | 119.8 (10) | H13b—C13—H13c | 109.5 |
C13—N1—C12 | 116.3 (11) | O10—C14—N2 | 126.3 (13) |
C14—N2—C15 | 118.4 (12) | O10—C14—H14 | 116.9 |
C14—N2—C16 | 116.9 (11) | N2—C14—H14 | 116.9 |
C15—N2—C16 | 124.2 (13) | N2—C15—H15a | 109.5 |
O2—C1—O1 | 121.8 (7) | N2—C15—H15b | 109.5 |
O2—C1—C5 | 120.6 (8) | H15a—C15—H15b | 109.5 |
O1—C1—C5 | 117.6 (7) | N2—C15—H15c | 109.5 |
O3—C2—O4 | 119.5 (7) | H15a—C15—H15c | 109.5 |
O3—C2—C6 | 124.9 (7) | H15b—C15—H15c | 109.5 |
O4—C2—C6 | 115.4 (7) | N2—C16—H16a | 109.5 |
O5—C3—O6 | 126.0 (7) | N2—C16—H16b | 109.5 |
O5—C3—C8 | 117.7 (8) | H16a—C16—H16b | 109.5 |
O6—C3—C8 | 116.1 (8) | N2—C16—H16c | 109.5 |
O8—C4—O7 | 123.6 (8) | H16a—C16—H16c | 109.5 |
O8—C4—C9 | 118.0 (7) | H16b—C16—H16c | 109.5 |
O6i—Co2—O1—C1 | −73.5 (5) | Co1vi—O7—C4—O8 | −15.5 (12) |
O8ii—Co2—O1—C1 | 156.4 (5) | Co1vi—O7—C4—C9 | 167.5 (5) |
O4iii—Co2—O1—C1 | 51.9 (6) | O2—C1—C5—C10 | 21.0 (12) |
O6i—Co2—O1—Co1 | 69.2 (3) | O1—C1—C5—C10 | −161.3 (7) |
O8ii—Co2—O1—Co1 | −60.9 (3) | O2—C1—C5—C6 | −154.6 (9) |
O4iii—Co2—O1—Co1 | −165.4 (2) | O1—C1—C5—C6 | 23.1 (12) |
O10—Co1—O1—C1 | 4.1 (7) | C10—C5—C6—C7 | −1.1 (12) |
O7ii—Co1—O1—C1 | −177.0 (6) | C1—C5—C6—C7 | 174.5 (8) |
O5i—Co1—O1—C1 | 92.1 (6) | C10—C5—C6—C2 | −179.3 (8) |
O3—Co1—O1—C1 | −85.7 (6) | C1—C5—C6—C2 | −3.7 (13) |
O10—Co1—O1—Co2 | −130.7 (3) | O3—C2—C6—C7 | 117.4 (9) |
O7ii—Co1—O1—Co2 | 48.3 (3) | O4—C2—C6—C7 | −57.5 (10) |
O5i—Co1—O1—Co2 | −42.7 (3) | O3—C2—C6—C5 | −64.3 (12) |
O3—Co1—O1—Co2 | 139.5 (3) | O4—C2—C6—C5 | 120.8 (9) |
O10—Co1—O3—C2 | −64.0 (7) | C5—C6—C7—C8 | 1.3 (13) |
O7ii—Co1—O3—C2 | 123.7 (7) | C2—C6—C7—C8 | 179.7 (8) |
O9—Co1—O3—C2 | −151.6 (7) | C6—C7—C8—C9 | 1.5 (13) |
O1—Co1—O3—C2 | 29.2 (7) | C6—C7—C8—C3 | −172.2 (8) |
O10—Co1—O9—C11 | −136.7 (8) | O5—C3—C8—C7 | −21.6 (12) |
O7ii—Co1—O9—C11 | 45.5 (7) | O6—C3—C8—C7 | 154.7 (8) |
O5i—Co1—O9—C11 | 135.8 (7) | O5—C3—C8—C9 | 164.9 (8) |
O3—Co1—O9—C11 | −46.4 (8) | O6—C3—C8—C9 | −18.7 (12) |
O9—Co1—O10—C14 | −25.3 (10) | C7—C8—C9—C10 | −4.4 (12) |
O5i—Co1—O10—C14 | 69.9 (10) | C3—C8—C9—C10 | 168.9 (8) |
O3—Co1—O10—C14 | −116.1 (10) | C7—C8—C9—C4 | 171.1 (8) |
O1—Co1—O10—C14 | 163.3 (10) | C3—C8—C9—C4 | −15.6 (13) |
Co2—O1—C1—O2 | −2.9 (11) | O8—C4—C9—C10 | −45.5 (10) |
Co1—O1—C1—O2 | −133.5 (8) | O7—C4—C9—C10 | 131.7 (8) |
Co2—O1—C1—C5 | 179.4 (5) | O8—C4—C9—C8 | 139.0 (8) |
Co1—O1—C1—C5 | 48.8 (9) | O7—C4—C9—C8 | −43.9 (11) |
Co1—O3—C2—O4 | −147.2 (6) | C8—C9—C10—C5 | 4.7 (12) |
Co1—O3—C2—C6 | 38.1 (11) | C4—C9—C10—C5 | −171.1 (8) |
Co2iv—O4—C2—O3 | −2.5 (8) | C6—C5—C10—C9 | −1.9 (13) |
Co2iv—O4—C2—C6 | 172.8 (5) | C1—C5—C10—C9 | −177.9 (7) |
Co1v—O5—C3—O6 | −31.1 (14) | Co1—O9—C11—N1 | 179.6 (8) |
Co1v—O5—C3—C8 | 144.8 (6) | C13—N1—C11—O9 | −179.8 (11) |
Co2v—O6—C3—O5 | −9.8 (13) | C12—N1—C11—O9 | −3.2 (17) |
Co2v—O6—C3—C8 | 174.2 (5) | Co1—O10—C14—N2 | 136.9 (11) |
Co2vi—O8—C4—O7 | −0.7 (11) | C15—N2—C14—O10 | −7 (2) |
Co2vi—O8—C4—C9 | 176.3 (5) | C16—N2—C14—O10 | −179.6 (13) |
Symmetry codes: (i) x−1/2, −y+3/2, z−1/2; (ii) x−1/2, y−1/2, z; (iii) x, −y+1, z−1/2; (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. |