Download citation
Download citation
link to html
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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806047982/ci2219sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806047982/ci2219Isup2.hkl
Contains datablock I

CCDC reference: 629627

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](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

Computing details top

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).

(I) top
Crystal data top
[Co(C7H7N2O4)(H2O)4](Cl)(OH)·2H2OF(000) = 416
Mr = 402.63Dx = 1.671 Mg m3
Monoclinic, P21/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybCell parameters from 6016 reflections
a = 5.245 (4) Åθ = 3.1–27.5°
b = 11.744 (7) ŵ = 1.29 mm1
c = 13.030 (7) ÅT = 295 K
β = 94.45 (3)°Prism, pink
V = 800.2 (9) Å30.34 × 0.24 × 0.18 mm
Z = 2
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
1920 independent reflections
Radiation source: fine-focus sealed tube1506 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.075
ω scanθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 66
Tmin = 0.393, Tmax = 0.801k = 1415
7919 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.072Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.201H 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 parametersΔρmax = 0.84 e Å3
10 restraintsΔρmin = 0.69 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.56872 (18)0.25000.41343 (8)0.0267 (3)
Cl10.9011 (8)0.0651 (4)0.0027 (3)0.0649 (10)0.50
O10.3119 (7)0.3832 (3)0.3690 (3)0.0348 (9)
O20.5627 (7)0.5373 (3)0.3703 (3)0.0334 (8)
O30.798 (3)0.1706 (13)0.0110 (12)0.095 (4)0.50
O1w0.7157 (14)0.25000.2723 (5)0.0480 (15)
H1w10.716 (14)0.1909 (4)0.2345 (16)0.058*
O2w0.3890 (11)0.25000.5509 (4)0.0336 (12)
H2w10.323 (9)0.3091 (4)0.576 (4)0.040*
O3w0.8437 (7)0.1265 (3)0.4707 (3)0.0355 (9)
H3w10.793 (9)0.061 (2)0.451 (5)0.043*
H3w21.003 (3)0.133 (4)0.462 (5)0.043*
O4w0.6020 (15)0.0797 (6)0.1334 (5)0.0795 (18)
H4w10.725 (13)0.051 (7)0.103 (6)0.095*
H4w20.529 (16)0.131 (6)0.095 (6)0.095*
N10.2093 (8)0.6581 (4)0.2497 (3)0.0302 (9)
C10.3605 (9)0.4833 (4)0.3440 (4)0.0270 (10)
C20.1499 (10)0.5405 (5)0.2759 (4)0.0338 (12)
H2a0.11970.49690.21290.041*
H2b0.00660.53960.31100.041*
C30.1098 (14)0.75000.2904 (6)0.0313 (15)
H30.00990.75000.33940.038*
C40.3799 (11)0.6928 (5)0.1812 (4)0.0377 (12)
H40.47730.64590.14200.045*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0233 (5)0.0231 (5)0.0340 (5)0.0000.0032 (4)0.000
Cl10.058 (2)0.073 (3)0.064 (2)0.0039 (19)0.0004 (17)0.0052 (19)
O10.0265 (19)0.0286 (19)0.048 (2)0.0019 (15)0.0024 (16)0.0061 (16)
O20.031 (2)0.0255 (18)0.043 (2)0.0001 (15)0.0008 (15)0.0015 (16)
O30.079 (9)0.090 (10)0.117 (11)0.002 (8)0.018 (8)0.010 (8)
O1w0.059 (4)0.043 (3)0.044 (3)0.0000.015 (3)0.000
O2w0.036 (3)0.022 (2)0.043 (3)0.0000.007 (2)0.000
O3w0.0286 (19)0.033 (2)0.044 (2)0.0019 (15)0.0002 (16)0.0072 (17)
O4w0.102 (5)0.069 (4)0.068 (4)0.010 (4)0.011 (3)0.008 (3)
N10.029 (2)0.026 (2)0.036 (2)0.0028 (18)0.0007 (17)0.0002 (18)
C10.026 (2)0.024 (2)0.032 (2)0.0023 (19)0.0057 (19)0.003 (2)
C20.026 (3)0.029 (3)0.045 (3)0.010 (2)0.002 (2)0.005 (2)
C30.027 (4)0.027 (3)0.039 (4)0.0000.001 (3)0.000
C40.041 (3)0.035 (3)0.038 (3)0.002 (2)0.008 (2)0.000 (2)
Geometric parameters (Å, º) top
Co1—O12.115 (4)O4w—H4w10.85 (1)
Co1—O1i2.115 (4)O4w—H4w20.85 (1)
Co1—O1w2.048 (6)N1—C31.327 (6)
Co1—O2w2.088 (6)N1—C41.374 (7)
Co1—O3w2.139 (4)N1—C21.462 (7)
Co1—O3wi2.139 (4)C1—C21.519 (7)
O1—C11.251 (6)C2—H2A0.97
O2—C11.260 (6)C2—H2B0.97
O1w—H1w10.85 (1)C3—N1ii1.327 (6)
O2w—H2w10.85 (1)C3—H30.93
O3w—H3w10.85 (1)C4—C4ii1.342 (11)
O3w—H3w20.85 (1)C4—H40.93
O1—Co1—O1i95.4 (2)H3w1—O3w—H3w2109.2 (18)
O1—Co1—O1w91.7 (2)H4w1—O4w—H4w2109.3 (18)
O1—Co1—O2w85.1 (2)C3—N1—C4108.3 (5)
O1—Co1—O3w174.2 (2)C3—N1—C2125.2 (5)
O1—Co1—O3wi89.6 (2)C4—N1—C2126.5 (5)
O1w—Co1—O1i91.7 (2)O1—C1—O2125.9 (5)
O2w—Co1—O1i85.1 (2)O1—C1—C2114.5 (4)
O1i—Co1—O3w89.6 (2)O2—C1—C2119.6 (4)
O1i—Co1—O3wi174.2 (2)N1—C2—C1113.3 (4)
O1w—Co1—O2w175.3 (3)N1—C2—H2A108.9
O1w—Co1—O3w91.3 (2)C1—C2—H2A108.9
O2w—Co1—O3w92.2 (2)N1—C2—H2B108.9
O1w—Co1—O3wi91.3 (2)C1—C2—H2B108.9
O2w—Co1—O3wi92.2 (2)H2A—C2—H2B107.7
O3w—Co1—O3wi85.4 (2)N1ii—C3—N1108.8 (7)
C1—O1—Co1128.9 (3)N1ii—C3—H3125.6
Co1—O1w—H1w1122 (3)N1—C3—H3125.6
Co1—O2w—H2w1124 (2)C4ii—C4—N1107.3 (3)
Co1—O3w—H3w1109 (4)C4ii—C4—H4126.4
Co1—O3w—H3w2122 (4)N1—C4—H4126.4
O1w—Co1—O1—C163.2 (5)C4—N1—C2—C173.8 (7)
O2w—Co1—O1—C1120.3 (5)O1—C1—C2—N1178.8 (4)
O1i—Co1—O1—C1155.1 (4)O2—C1—C2—N11.1 (7)
O3wi—Co1—O1—C128.1 (5)C4—N1—C3—N1ii0.5 (8)
O3w—Co1—O1—C158.1 (17)C2—N1—C3—N1ii179.2 (4)
Co1—O1—C1—O224.4 (8)C3—N1—C4—C4ii0.3 (5)
Co1—O1—C1—C2155.7 (4)C2—N1—C4—C4ii179.0 (4)
C3—N1—C2—C1104.6 (7)
Symmetry codes: (i) x, y+1/2, z; (ii) x, y+3/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O4w0.85 (1)1.92 (3)2.731 (8)160 (7)
O3w—H3w2···O1iii0.85 (1)2.11 (3)2.881 (6)150 (5)
O3w—H3w1···O2i0.85 (1)1.92 (3)2.700 (5)152 (6)
O4w—H4w1···Cl10.85 (1)2.15 (5)2.945 (8)156 (10)
O4w—H4w2···O3iv0.85 (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.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds