REPORT WRITING

Report Writing



Report Writing

Introduction

In the title compound, (C3H5N2)[Co(C4H5NO4)2], the cation and anion are located on a twofold rotation axis and inversion center, respectively. Intermolecular N—HO hydrogen bonds link the cations and anions into layers parallel to the ab plane. The crystal packing also exhibits weak C—HO hydrogen bonds, including bifurcated hydrogen bonds, and C=Op interactions.

Experiment

Chemicals were readily available from commercial sources and were used as received without further purification. To a 10 ml of solution containing imidazole (0.14 g, 2 mmol) in a flask with constant stirring, added dropwise Co(CH3COO)2.3H2O (0.23 g, 1 mmol) in 5 ml of aqueous solution and 5 ml aqueous solution containing iminodiacetic acid (0.27 g, 2 mmol) was added dropwise. The mixture was stirred for 3 h, and then filtered. The dark-red filtrate was left to stand at room temperature, and after three weeks, dark-red crystals of the title compound were formed.

Refinement

H atoms attached to C atoms of (I) were placed in geometrically idealized positions and refined withUiso(H)=1.2Ueq(C). H atoms attached to N1 and N2 in (I) were located from difference Fourier maps, with fixed bond lengths, and refined using a riding model, with Uiso(H) = 1.2Ueq(N).

Crystal data

(C3H5N2)[Co(C4H5NO4)2]

F(000) = 800

Mr = 390.20

Dx = 1.716 Mg m-3

Orthorhombic, Pcca

Mo Ka radiation, ? = 0.71073 Å

Hall symbol: -P 2a 2ac

Cell parameters from 2958 reflections

a = 16.889 (3) Å

? = 2.4-27.0°

b = 5.2906 (10) Å

µ = 1.19 mm-1

c = 16.901 (3) Å

T = 298 K

V = 1510.2 (5) Å3

Block, red

Z = 4

0.20 × 0.20 × 0.20 mm

Special details

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 ofF2 > s(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 ar

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

x

y

z

Uiso*/Ueq

Co1

0.0000

1.0000

0.0000

0.02108 (14)

O1

-0.06498 (8)

1.0888 (2)

0.08656 (8)

0.0305 (3)

O2

-0.10143 (10)

0.9556 (3)

0.20572 (10)

0.0502 (5)

O3

0.07296 (7)

1.2495 (2)

0.03073 (9)

0.0306 (3)

O4

0.17666 (11)

1.3151 (3)

0.10704 (14)

0.0775 (7)

N1

0.05329 (8)

0.7739 (3)

0.07205 (9)

0.0240 (3)

H1

0.0644

0.6440

0.0521

0.029*

C1

-0.06105 (12)

0.9354 (4)

0.14545 (12)

0.0319 (4)

C2

-0.00355 (11)

0.7182 (4)

0.13637 (12)

0.0315 (5)

H2A

0.0249

0.6926

0.1856

0.038*

H2B

-0.0324

0.5644

0.1242

0.038*

C3

0.12727 (11)

0.8972 (4)

0.09931 (13)

0.0327 (4)

H3A

0.1724

0.8161

0.0744

0.039*

H3B

0.1324

0.8764

0.1561

0.039*

C4

0.12754 (12)

1.1751 (4)

0.07933 (13)

0.0369 (5)

N2

0.20741 (11)

0.3528 (4)

0.31139 (13)

0.0526 (5)

H2

0.1749

0.2389

0.2952

0.063*

C5

0.2500

0.5000

0.2661 (2)

0.0461 (9)

H5

0.2500

0.5000

0.2110

0.055*

C6

0.22287 (19)

0.4090 (8)

0.38741 (18)

0.0811 (11)

H6

0.1999

0.3346

0.4317

0.097*

Atomic displacement parameters (Å2)

U11

U22

U33

U12

U13

U23

Co1

0.0249 (2)

0.0181 (2)

0.0202 (2)

0.00274 (13)

-0.00159 (13)

-0.00175 (12)

O1

0.0359 (7)

0.0297 (7)

0.0259 (7)

0.0101 (6)

0.0047 (6)

-0.0001 (6)

O2

0.0550 (10)

0.0629 (11)

0.0325 (9)

0.0263 (8)

0.0165 (8)

0.0112 (8)

O3

0.0323 (7)

0.0210 (6)

0.0385 (8)

-0.0005 (5)

-0.0086 (6)

-0.0013 (6)

O4

0.0655 (12)

0.0340 (9)

0.1330 (19)

-0.0079 (9)

-0.0602 (12)

-0.0013 (10)

N1

0.0288 (8)

0.0187 (7)

0.0246 (8)

0.0051 (6)

-0.0019 (6)

-0.0030 (6)

C1

0.0334 (10)

0.0351 (10)

0.0271 (11)

0.0056 (9)

0.0021 (9)

0.0002 (8)

C2

0.0376 (11)

0.0297 (10)

0.0273 (11)

0.0068 (8)

0.0025 (8)

0.0064 (8)

C3

0.0301 (10)

0.0306 (10)

0.0374 (11)

0.0032 (8)

-0.0084 (9)

-0.0001 (9)

C4

0.0345 (10)

0.0269 (10)

0.0492 (13)

0.0013 (8)

-0.0115 (9)

-0.0061 (9)

N2

0.0418 (11)

0.0547 (13)

0.0613 (14)

-0.0206 (10)

-0.0043 (10)

-0.0035 (10)

C5

0.0403 (19)

0.057 (2)

0.041 (2)

-0.0004 (15)

0.000

0.000

C6

0.074 (2)

0.122 (3)

0.0467 (18)

-0.048 (2)

0.0007 (15)

0.0132 (18)

Geometric parameters (Å, °)

Co1—O3i

1.8790 (12)

C1—C2

1.512 (3)

Co1—O3

1.8790 (12)

C2—H2A

0.9700

Co1—O1

1.8882 (13)

C2—H2B

0.9700

Co1—O1i

1.8882 (13)

C3—C4

1.508 (3)

Co1—N1i

1.9299 (14)

C3—H3A

0.9700

Co1—N1

1.9299 (14)

C3—H3B

0.9700

O1—C1

1.286 (2)

N2—C5

1.308 (3)

O2—C1

1.230 (2)

N2—C6

1.344 (4)

O3—C4

1.296 (2)

N2—H2

0.8599

O4—C4

1.207 (3)

C5—N2ii

1.308 (3)

N1—C2

1.480 (2)

C5—H5

0.9300

N1—C3

1.483 (2)

C6—C6ii

1.329 (6)

N1—H1

0.7879

C6—H6

0.9300

O3i—Co1—O3

180.00 (9)

O1—C1—C2

115.72 (17)

O3i—Co1—O1

90.44 (6)

N1—C2—C1

109.88 (16)

O3—Co1—O1

89.56 (6)

N1—C2—H2A

109.7

O3i—Co1—O1i

89.56 (6)

C1—C2—H2A

109.7

O3—Co1—O1i

90.44 (6)

N1—C2—H2B

109.7

O1—Co1—O1i

180.0

C1—C2—H2B

109.7

O3i—Co1—N1i

87.43 (6)

H2A—C2—H2B

108.2

O3—Co1—N1i

92.57 (6)

N1—C3—C4

111.22 (15)

O1—Co1—N1i

93.65 (6)

N1—C3—H3A

109.4

O1i—Co1—N1i

86.35 (6)

C4—C3—H3A

109.4

O3i—Co1—N1

92.57 (6)

N1—C3—H3B

109.4

O3—Co1—N1

87.43 (6)

C4—C3—H3B

109.4

O1—Co1—N1

86.35 (6)

H3A—C3—H3B

108.0

O1i—Co1—N1

93.65 (6)

O4—C4—O3

123.3 (2)

N1i—Co1—N1

180.00 (7)

O4—C4—C3

120.91 (19)

C1—O1—Co1

114.38 (12)

O3—C4—C3

115.83 (16)

C4—O3—Co1

115.36 (12)

C5—N2—C6

108.8 (2)

C2—N1—C3

113.95 (15)

C5—N2—H2

125.6

C2—N1—Co1

106.52 (11)

C6—N2—H2

125.6

C3—N1—Co1

108.42 (11)

N2ii—C5—N2

108.3 (3)

C2—N1—H1

107.2

N2ii—C5—H5

125.9

C3—N1—H1

108.4

N2—C5—H5

125.9

Co1—N1—H1

112.5

C6ii—C6—N2

107.09 (15)

O2—C1—O1

123.87 (19)

C6ii—C6—H6

126.5

O2—C1—C2

120.40 (18)

N2—C6—H6

126.5

O3i—Co1—O1—C1

77.41 (15)

O1i—Co1—N1—C3

80.29 (12)

O3—Co1—O1—C1

-102.59 (15)

Co1—O1—C1—O2

-176.80 (17)

N1i—Co1—O1—C1

164.87 (14)

Co1—O1—C1—C2

2.0 (2)

N1—Co1—O1—C1

-15.13 (14)

C3—N1—C2—C1

92.47 (19)

O1—Co1—O3—C4

90.08 (15)

Co1—N1—C2—C1

-27.03 (19)

O1i—Co1—O3—C4

-89.92 (15)

O2—C1—C2—N1

-163.64 (19)

N1i—Co1—O3—C4

-176.29 (15)

O1—C1—C2—N1

17.5 (3)

N1—Co1—O3—C4

3.71 (15)

C2—N1—C3—C4

-104.50 (19)

O3i—Co1—N1—C2

-66.96 (12)

Co1—N1—C3—C4

13.92 (19)

O3—Co1—N1—C2

113.04 (12)

Co1—O3—C4—O4

-176.8 (2)

O1—Co1—N1—C2

23.32 (12)

Co1—O3—C4—C3

3.9 (2)

O1i—Co1—N1—C2

-156.68 (12)

N1—C3—C4—O4

168.6 (2)

O3i—Co1—N1—C3

170.01 (12)

N1—C3—C4—O3

-12.2 (3)

O3—Co1—N1—C3

-9.99 (12)

C6—N2—C5—N2ii

0.4 (2)

O1—Co1—N1—C3

-99.71 (12)

C5—N2—C6—C6ii

-1.2 (5)

Symmetry codes: (i) -x, -y+2, -z; (ii) -x+1/2, ...