In the crystal structure of the title compound, [Co(C7H7N2O4)(H2O)4]Cl(OH)·2H2O, the cations form a polycationic chain that propagates along the b axis of the monoclinic unit cell. The CoIII atom and two coordinated water molecules lie on special positions of site symmetry m. The C7H7N2O4 anion displays crystallographic mirror symmetry. The chloride and hydroxide anions are disordered and they interact, along with the uncoordinated water molecule, with the polycationic chain to form a three-dimensional, hydrogen-bonded network.
Supporting information
CCDC reference: 629627
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.008 Å
- H-atom completeness 96%
- Disorder in solvent or counterion
- R factor = 0.072
- wR factor = 0.201
- Data-to-parameter ratio = 14.4
checkCIF/PLATON results
No syntax errors found
Alert level B
ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
Tmin and Tmax reported: 0.393 0.801
Tmin(prime) and Tmax expected: 0.638 0.792
RR(prime) = 0.609
Please check that your absorption correction is appropriate.
PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.60
PLAT731_ALERT_1_B Bond Calc 0.85(7), Rep 0.850(10) ...... 7.00 su-Ra
O4W -H4W1 1.555 1.555
PLAT731_ALERT_1_B Bond Calc 0.86(7), Rep 0.850(10) ...... 7.00 su-Ra
O4W -H4W2 1.555 1.555
PLAT732_ALERT_1_B Angle Calc 109(8), Rep 109.3(18) ...... 4.44 su-Ra
H4W1 -O4W -H4W2 1.555 1.555 1.555
PLAT735_ALERT_1_B D-H Calc 0.85(7), Rep 0.850(10) ...... 7.00 su-Ra
O4W -H5# 1.555 1.555
PLAT735_ALERT_1_B D-H Calc 0.86(7), Rep 0.850(10) ...... 7.00 su-Ra
O4W -H6# 1.555 1.555
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 33.00 Perc.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8
PLAT417_ALERT_2_C Short Inter D-H..H-D H1W1 .. H4W2 .. 2.12 Ang.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 5
O3W -CO1 -O1 -C1 58.10 1.70 1.555 1.555 1.555 1.555
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Ra
O2W -H2W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Ra
O3W -H3W1 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 109(5), Rep 109.2(18) ...... 2.78 su-Ra
H3W1 -O3W -H3W2 1.555 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Ra
O3W -H3# 1.555 1.555
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C7 H20 Cl1 Co1 N2 O11
Atom count from _chemical_formula_moiety:
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C7 H20 Cl1 Co1 N2 O11
Atom count from the _atom_site data: C7 H19 Cl1 Co1 N2 O11
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
From the CIF: _cell_formula_units_Z 2
From the CIF: _chemical_formula_sum C7 H20 Cl Co N2 O11
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 14.00 14.00 0.00
H 40.00 38.00 2.00
Cl 2.00 2.00 0.00
Co 2.00 2.00 0.00
N 4.00 4.00 0.00
O 22.00 22.00 0.00
0 ALERT level A = In general: serious problem
7 ALERT level B = Potentially serious problem
13 ALERT level C = Check and explain
4 ALERT level G = General alerts; check
16 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2006).
Crystal data top
[Co(C7H7N2O4)(H2O)4](Cl)(OH)·2H2O | F(000) = 416 |
Mr = 402.63 | Dx = 1.671 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yb | Cell parameters from 6016 reflections |
a = 5.245 (4) Å | θ = 3.1–27.5° |
b = 11.744 (7) Å | µ = 1.29 mm−1 |
c = 13.030 (7) Å | T = 295 K |
β = 94.45 (3)° | Prism, pink |
V = 800.2 (9) Å3 | 0.34 × 0.24 × 0.18 mm |
Z = 2 | |
Data collection top
Rigaku R-AXIS RAPID IP diffractometer | 1920 independent reflections |
Radiation source: fine-focus sealed tube | 1506 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.075 |
ω scan | θmax = 27.5°, θmin = 3.1° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −6→6 |
Tmin = 0.393, Tmax = 0.801 | k = −14→15 |
7919 measured reflections | l = −16→16 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.072 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.201 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.13 | w = 1/[σ2(Fo2) + (0.079P)2 + 3.1848P] where P = (Fo2 + 2Fc2)/3 |
1920 reflections | (Δ/σ)max = 0.001 |
133 parameters | Δρmax = 0.84 e Å−3 |
10 restraints | Δρmin = −0.69 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.56872 (18) | 0.2500 | 0.41343 (8) | 0.0267 (3) | |
Cl1 | 0.9011 (8) | −0.0651 (4) | 0.0027 (3) | 0.0649 (10) | 0.50 |
O1 | 0.3119 (7) | 0.3832 (3) | 0.3690 (3) | 0.0348 (9) | |
O2 | 0.5627 (7) | 0.5373 (3) | 0.3703 (3) | 0.0334 (8) | |
O3 | 0.798 (3) | −0.1706 (13) | 0.0110 (12) | 0.095 (4) | 0.50 |
O1w | 0.7157 (14) | 0.2500 | 0.2723 (5) | 0.0480 (15) | |
H1w1 | 0.716 (14) | 0.1909 (4) | 0.2345 (16) | 0.058* | |
O2w | 0.3890 (11) | 0.2500 | 0.5509 (4) | 0.0336 (12) | |
H2w1 | 0.323 (9) | 0.3091 (4) | 0.576 (4) | 0.040* | |
O3w | 0.8437 (7) | 0.1265 (3) | 0.4707 (3) | 0.0355 (9) | |
H3w1 | 0.793 (9) | 0.061 (2) | 0.451 (5) | 0.043* | |
H3w2 | 1.003 (3) | 0.133 (4) | 0.462 (5) | 0.043* | |
O4w | 0.6020 (15) | 0.0797 (6) | 0.1334 (5) | 0.0795 (18) | |
H4w1 | 0.725 (13) | 0.051 (7) | 0.103 (6) | 0.095* | |
H4w2 | 0.529 (16) | 0.131 (6) | 0.095 (6) | 0.095* | |
N1 | 0.2093 (8) | 0.6581 (4) | 0.2497 (3) | 0.0302 (9) | |
C1 | 0.3605 (9) | 0.4833 (4) | 0.3440 (4) | 0.0270 (10) | |
C2 | 0.1499 (10) | 0.5405 (5) | 0.2759 (4) | 0.0338 (12) | |
H2a | 0.1197 | 0.4969 | 0.2129 | 0.041* | |
H2b | −0.0066 | 0.5396 | 0.3110 | 0.041* | |
C3 | 0.1098 (14) | 0.7500 | 0.2904 (6) | 0.0313 (15) | |
H3 | −0.0099 | 0.7500 | 0.3394 | 0.038* | |
C4 | 0.3799 (11) | 0.6928 (5) | 0.1812 (4) | 0.0377 (12) | |
H4 | 0.4773 | 0.6459 | 0.1420 | 0.045* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0233 (5) | 0.0231 (5) | 0.0340 (5) | 0.000 | 0.0032 (4) | 0.000 |
Cl1 | 0.058 (2) | 0.073 (3) | 0.064 (2) | 0.0039 (19) | 0.0004 (17) | −0.0052 (19) |
O1 | 0.0265 (19) | 0.0286 (19) | 0.048 (2) | 0.0019 (15) | −0.0024 (16) | 0.0061 (16) |
O2 | 0.031 (2) | 0.0255 (18) | 0.043 (2) | −0.0001 (15) | 0.0008 (15) | −0.0015 (16) |
O3 | 0.079 (9) | 0.090 (10) | 0.117 (11) | −0.002 (8) | 0.018 (8) | −0.010 (8) |
O1w | 0.059 (4) | 0.043 (3) | 0.044 (3) | 0.000 | 0.015 (3) | 0.000 |
O2w | 0.036 (3) | 0.022 (2) | 0.043 (3) | 0.000 | 0.007 (2) | 0.000 |
O3w | 0.0286 (19) | 0.033 (2) | 0.044 (2) | −0.0019 (15) | 0.0002 (16) | −0.0072 (17) |
O4w | 0.102 (5) | 0.069 (4) | 0.068 (4) | −0.010 (4) | 0.011 (3) | −0.008 (3) |
N1 | 0.029 (2) | 0.026 (2) | 0.036 (2) | 0.0028 (18) | −0.0007 (17) | 0.0002 (18) |
C1 | 0.026 (2) | 0.024 (2) | 0.032 (2) | 0.0023 (19) | 0.0057 (19) | −0.003 (2) |
C2 | 0.026 (3) | 0.029 (3) | 0.045 (3) | −0.010 (2) | −0.002 (2) | 0.005 (2) |
C3 | 0.027 (4) | 0.027 (3) | 0.039 (4) | 0.000 | 0.001 (3) | 0.000 |
C4 | 0.041 (3) | 0.035 (3) | 0.038 (3) | 0.002 (2) | 0.008 (2) | 0.000 (2) |
Geometric parameters (Å, º) top
Co1—O1 | 2.115 (4) | O4w—H4w1 | 0.85 (1) |
Co1—O1i | 2.115 (4) | O4w—H4w2 | 0.85 (1) |
Co1—O1w | 2.048 (6) | N1—C3 | 1.327 (6) |
Co1—O2w | 2.088 (6) | N1—C4 | 1.374 (7) |
Co1—O3w | 2.139 (4) | N1—C2 | 1.462 (7) |
Co1—O3wi | 2.139 (4) | C1—C2 | 1.519 (7) |
O1—C1 | 1.251 (6) | C2—H2A | 0.97 |
O2—C1 | 1.260 (6) | C2—H2B | 0.97 |
O1w—H1w1 | 0.85 (1) | C3—N1ii | 1.327 (6) |
O2w—H2w1 | 0.85 (1) | C3—H3 | 0.93 |
O3w—H3w1 | 0.85 (1) | C4—C4ii | 1.342 (11) |
O3w—H3w2 | 0.85 (1) | C4—H4 | 0.93 |
| | | |
O1—Co1—O1i | 95.4 (2) | H3w1—O3w—H3w2 | 109.2 (18) |
O1—Co1—O1w | 91.7 (2) | H4w1—O4w—H4w2 | 109.3 (18) |
O1—Co1—O2w | 85.1 (2) | C3—N1—C4 | 108.3 (5) |
O1—Co1—O3w | 174.2 (2) | C3—N1—C2 | 125.2 (5) |
O1—Co1—O3wi | 89.6 (2) | C4—N1—C2 | 126.5 (5) |
O1w—Co1—O1i | 91.7 (2) | O1—C1—O2 | 125.9 (5) |
O2w—Co1—O1i | 85.1 (2) | O1—C1—C2 | 114.5 (4) |
O1i—Co1—O3w | 89.6 (2) | O2—C1—C2 | 119.6 (4) |
O1i—Co1—O3wi | 174.2 (2) | N1—C2—C1 | 113.3 (4) |
O1w—Co1—O2w | 175.3 (3) | N1—C2—H2A | 108.9 |
O1w—Co1—O3w | 91.3 (2) | C1—C2—H2A | 108.9 |
O2w—Co1—O3w | 92.2 (2) | N1—C2—H2B | 108.9 |
O1w—Co1—O3wi | 91.3 (2) | C1—C2—H2B | 108.9 |
O2w—Co1—O3wi | 92.2 (2) | H2A—C2—H2B | 107.7 |
O3w—Co1—O3wi | 85.4 (2) | N1ii—C3—N1 | 108.8 (7) |
C1—O1—Co1 | 128.9 (3) | N1ii—C3—H3 | 125.6 |
Co1—O1w—H1w1 | 122 (3) | N1—C3—H3 | 125.6 |
Co1—O2w—H2w1 | 124 (2) | C4ii—C4—N1 | 107.3 (3) |
Co1—O3w—H3w1 | 109 (4) | C4ii—C4—H4 | 126.4 |
Co1—O3w—H3w2 | 122 (4) | N1—C4—H4 | 126.4 |
| | | |
O1w—Co1—O1—C1 | −63.2 (5) | C4—N1—C2—C1 | 73.8 (7) |
O2w—Co1—O1—C1 | 120.3 (5) | O1—C1—C2—N1 | 178.8 (4) |
O1i—Co1—O1—C1 | −155.1 (4) | O2—C1—C2—N1 | −1.1 (7) |
O3wi—Co1—O1—C1 | 28.1 (5) | C4—N1—C3—N1ii | 0.5 (8) |
O3w—Co1—O1—C1 | 58.1 (17) | C2—N1—C3—N1ii | 179.2 (4) |
Co1—O1—C1—O2 | −24.4 (8) | C3—N1—C4—C4ii | −0.3 (5) |
Co1—O1—C1—C2 | 155.7 (4) | C2—N1—C4—C4ii | −179.0 (4) |
C3—N1—C2—C1 | −104.6 (7) | | |
Symmetry codes: (i) x, −y+1/2, z; (ii) x, −y+3/2, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O4w | 0.85 (1) | 1.92 (3) | 2.731 (8) | 160 (7) |
O3w—H3w2···O1iii | 0.85 (1) | 2.11 (3) | 2.881 (6) | 150 (5) |
O3w—H3w1···O2i | 0.85 (1) | 1.92 (3) | 2.700 (5) | 152 (6) |
O4w—H4w1···Cl1 | 0.85 (1) | 2.15 (5) | 2.945 (8) | 156 (10) |
O4w—H4w2···O3iv | 0.85 (1) | 2.17 (6) | 2.91 (2) | 145 (10) |
Symmetry codes: (i) x, −y+1/2, z; (iii) x+1, −y+1/2, z; (iv) −x+1, −y, −z. |