The 1:1 adduct of cobalt(II) terephthalate with N,N-di­methyl­form­amide

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:O-μ₄-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.

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

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Computing details

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:O-µ₄-terephthalato- κ⁴O:O':O'':O''']

Crystal data

[Co(C8H4O4)(C3H7NO)]	F(000) = 604
Mr = 296.14	Dx = 1.591 Mg m^−3
Orthorhombic, Imma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -I 2b 2	Cell parameters from 4989 reflections
a = 19.258 (1) Å	θ = 2.5–28.1°
b = 7.2459 (4) Å	µ = 1.40 mm^−1
c = 8.8593 (5) Å	T = 295 K
V = 1236.3 (1) Å^3	Prism, pink
Z = 4	0.39 × 0.38 × 0.33 mm

Data collection

Bruker APEX area-detector diffractometer	789 independent reflections
Radiation source: fine-focus sealed tube	781 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.019
φ and ω scans	θmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −24→24
Tmin = 0.536, Tmax = 0.629	k = −9→9
6527 measured reflections	l = −11→11

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.093	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.064P)^2 + 1.9208P] where P = (Fo^2 + 2Fc^2)/3
789 reflections	(Δ/σ)max = 0.001
63 parameters	Δρmax = 0.69 e Å^−3
3 restraints	Δρmin = −0.78 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Co1	0.5000	0.5000	0.5000	0.0164 (2)
O1	0.4221 (1)	0.5959 (2)	0.3647 (2)	0.0346 (4)
O2	0.5000	0.7500	0.6379 (3)	0.0273 (6)
N1	0.5000	0.7500	0.8946 (4)	0.049 (1)
C1	0.3943 (1)	0.7500	0.3467 (3)	0.0263 (6)
C2	0.3194 (2)	0.7500	0.2961 (4)	0.0295 (6)
C3	0.2842 (1)	0.5864 (3)	0.2736 (4)	0.0536 (8)
C4	0.5269 (4)	0.7500	0.7581 (7)	0.033 (1)	0.50
C5	0.5297 (6)	0.7500	1.0370 (9)	0.072 (4)	0.50
C6	0.4261 (5)	0.7500	0.8993 (11)	0.086 (4)	0.50
H3	0.3067	0.4748	0.2905	0.064*
H4	0.5752	0.7500	0.7556	0.039*	0.50
H5a	0.5770	0.7909	1.0300	0.108*	0.25
H5b	0.5285	0.6273	1.0778	0.108*	0.25
H5c	0.5042	0.8317	1.1017	0.108*	0.25
H6a	0.4108	0.7025	0.9948	0.129*	0.25
H6b	0.4084	0.6737	0.8195	0.129*	0.25
H6c	0.4094	0.8738	0.8867	0.129*	0.25

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0121 (3)	0.0171 (3)	0.0200 (3)	0.000	0.000	0.0011 (2)
O1	0.0257 (7)	0.0282 (8)	0.0499 (9)	0.0034 (6)	−0.0197 (7)	−0.0004 (7)
O2	0.043 (2)	0.019 (1)	0.020 (1)	0.000	0.000	0.000
N1	0.090 (4)	0.036 (2)	0.022 (2)	0.000	0.000	0.000
C1	0.020 (1)	0.028 (1)	0.031 (1)	0.000	−0.0111 (11)	0.000
C2	0.022 (1)	0.026 (1)	0.041 (2)	0.000	−0.0145 (11)	0.000
C3	0.031 (1)	0.024 (1)	0.106 (2)	0.003 (1)	−0.033 (2)	0.003 (1)
C4	0.046 (3)	0.022 (2)	0.030 (3)	0.000	−0.009 (2)	0.000
C5	0.13 (1)	0.052 (5)	0.032 (3)	0.000	−0.019 (5)	0.000
C6	0.15 (1)	0.069 (7)	0.040 (5)	0.000	0.030 (6)	0.000

Geometric parameters (Å, º)

Co1—O1	2.042 (1)	N1—C6	1.423 (9)
Co1—O1^i	2.042 (1)	C1—O1^v	1.249 (2)
Co1—O1^ii	2.042 (1)	C1—C2	1.510 (4)
Co1—O1^iii	2.042 (1)	C2—C3	1.380 (3)
Co1—O2	2.185 (2)	C2—C3^v	1.380 (3)
Co1—O2^ii	2.185 (2)	C3—C3^vi	1.382 (4)
O1—C1	1.249 (2)	C3—H3	0.93
O2—C4	1.184 (7)	C4—H4	0.93
O2—C4^iv	1.184 (7)	C5—H5a	0.96
N1—C4^iv	1.316 (6)	C5—H5b	0.96
N1—C4	1.316 (6)	C5—H5c	0.96
N1—C5	1.385 (7)	C6—H6a	0.96
N1—C5^iv	1.385 (7)	C6—H6b	0.96
N1—C6^iv	1.423 (9)	C6—H6c	0.96
O1—Co1—O1^i	85.5 (1)	C4—N1—C5	132.4 (6)
O1—Co1—O2	92.6 (1)	C4—N1—C6	114.9 (6)
O1—Co1—O1^ii	180	C5—N1—C6	112.7 (7)
O1—Co1—O1^iii	94.6 (1)	O1^v—C1—O1	126.8 (3)
O1—Co1—O2^ii	87.4 (1)	O1^v—C1—C2	116.6 (1)
O1^i—Co1—O1^ii	94.6 (1)	O1—C1—C2	116.6 (1)
O1^i—Co1—O1^iii	180	C3—C2—C3^v	118.4 (3)
O1^i—Co1—O2	87.4 (1)	C3—C2—C1	120.8 (1)
O1^i—Co1—O2^ii	92.6 (1)	C3^v—C2—C1	120.8 (1)
O1^ii—Co1—O1^iii	85.5 (1)	C3^vi—C3—C2	120.8 (1)
O1^ii—Co1—O2	87.4 (1)	C3^vi—C3—H3	119.6
O1^ii—Co1—O2^ii	92.6 (1)	C2—C3—H3	119.6
O1^iii—Co1—O2	92.6 (1)	O2—C4—N1	130.8 (6)
O1^iii—Co1—O2^ii	87.4 (1)	O2—C4—H4	114.6
O2^ii—Co1—O2	180	N1—C4—H4	114.6
C1—O1—Co1	134.0 (2)	N1—C5—H5a	109.5
C4—O2—Co1	120.2 (1)	N1—C5—H5b	109.5
C4^iv—O2—Co1	120.2 (1)	N1—C5—H5c	109.5
C4—O2—Co1^iv	120.2 (1)	N1—C6—H6a	109.5
C4^iv—O2—Co1^iv	120.2 (1)	N1—C6—H6b	109.5
Co1—O2—Co1^iv	112.0 (1)	N1—C6—H6c	109.5
O1^iii—Co1—O1—C1	−80.4 (3)	Co1—O1—C1—O1^v	29.3 (5)
O1^i—Co1—O1—C1	99.6 (3)	Co1—O1—C1—C2	−151.4 (2)
O2^ii—Co1—O1—C1	−167.6 (3)	O1^v—C1—C2—C3	−179.8 (3)
O2—Co1—O1—C1	12.4 (3)	O1—C1—C2—C3	0.9 (5)
O1^iii—Co1—O2—C4	−102.2 (4)	O1^v—C1—C2—C3^v	−0.9 (5)
O1—Co1—O2—C4	163.1 (4)	O1—C1—C2—C3^v	179.8 (3)
O1^ii—Co1—O2—C4	−16.9 (4)	C3^v—C2—C3—C3^vi	1.5 (8)
O1^i—Co1—O2—C4	77.8 (4)	C1—C2—C3—C3^vi	−179.6 (4)
O1^iii—Co1—O2—C4^iv	−163.1 (4)	C4^iv—O2—C4—N1	0.0
O1—Co1—O2—C4^iv	102.2 (4)	Co1—O2—C4—N1	−106.4 (2)
O1^ii—Co1—O2—C4^iv	−77.8 (4)	Co1^iv—O2—C4—N1	106.4 (2)
O1^i—Co1—O2—C4^iv	16.9 (4)	C4^iv—N1—C4—O2	0.0
O1^iii—Co1—O2—Co1^iv	47.34 (5)	C5—N1—C4—O2	180
O1—Co1—O2—Co1^iv	−47.34 (5)	C6^iv—N1—C4—O2	180
O1^ii—Co1—O2—Co1^iv	132.7 (1)	C6—N1—C4—O2	0
O1^i—Co1—O2—Co1^iv	−132.7 (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.