catena-Poly[[[tetra­aqua­cobalt(III)]-μ-1H-imidazole-1,3-diyldiacetato-κ²O:O′] chloride hydroxide dihydrate]

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 Co^III 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.

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

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Computing details

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)

Crystal data

[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) Å^3	0.34 × 0.24 × 0.18 mm
Z = 2

Data collection

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

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)] = 0.072	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.201	H atoms treated by a mixture of independent and constrained refinement
S = 1.13	w = 1/[σ^2(Fo^2) + (0.079P)^2 + 3.1848P] where P = (Fo^2 + 2Fc^2)/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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Co1—O1	2.115 (4)	O4w—H4w1	0.85 (1)
Co1—O1^i	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—O3w^i	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—N1^ii	1.327 (6)
O2w—H2w1	0.85 (1)	C3—H3	0.93
O3w—H3w1	0.85 (1)	C4—C4^ii	1.342 (11)
O3w—H3w2	0.85 (1)	C4—H4	0.93
O1—Co1—O1^i	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—O3w^i	89.6 (2)	C4—N1—C2	126.5 (5)
O1w—Co1—O1^i	91.7 (2)	O1—C1—O2	125.9 (5)
O2w—Co1—O1^i	85.1 (2)	O1—C1—C2	114.5 (4)
O1^i—Co1—O3w	89.6 (2)	O2—C1—C2	119.6 (4)
O1^i—Co1—O3w^i	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—O3w^i	91.3 (2)	C1—C2—H2B	108.9
O2w—Co1—O3w^i	92.2 (2)	H2A—C2—H2B	107.7
O3w—Co1—O3w^i	85.4 (2)	N1^ii—C3—N1	108.8 (7)
C1—O1—Co1	128.9 (3)	N1^ii—C3—H3	125.6
Co1—O1w—H1w1	122 (3)	N1—C3—H3	125.6
Co1—O2w—H2w1	124 (2)	C4^ii—C4—N1	107.3 (3)
Co1—O3w—H3w1	109 (4)	C4^ii—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)
O1^i—Co1—O1—C1	−155.1 (4)	O2—C1—C2—N1	−1.1 (7)
O3w^i—Co1—O1—C1	28.1 (5)	C4—N1—C3—N1^ii	0.5 (8)
O3w—Co1—O1—C1	58.1 (17)	C2—N1—C3—N1^ii	179.2 (4)
Co1—O1—C1—O2	−24.4 (8)	C3—N1—C4—C4^ii	−0.3 (5)
Co1—O1—C1—C2	155.7 (4)	C2—N1—C4—C4^ii	−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)

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···O1^iii	0.85 (1)	2.11 (3)	2.881 (6)	150 (5)
O3w—H3w1···O2^i	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···O3^iv	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.