The title compound, {[Co(C8H4O5)(C12H8N2)]·H2O}n, is isostructural with its manganese analog [Skakle, Foreman & Plater (2001). Acta Cryst. E57, m373–m375]. The asymmetric unit consists of one Co atom, one 1,10-phenanthroline ligand bound in a bidentate manner, one hydroxyisophthalate ligand and one water molecule. The Co coordination is completed by two further O atoms from two symmetry-related hydroxyisophthalate ligands, giving a grossly distorted octahedral geometry.
Supporting information
CCDC reference: 238670
Key indicators
- Single-crystal X-ray study
- T = 130 K
- Mean (C-C) = 0.002 Å
- R factor = 0.034
- wR factor = 0.089
- Data-to-parameter ratio = 15.7
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT128_ALERT_4_C Non-standard setting of Space group P2/c .... P2/n
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 3
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens,1994); data reduction: XPREP in SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Poly[[[(1,10-phenanthroline-
κ2N,
N')cobalt(II)]-µ
3-5-hydroxyisophthalato-
κ4O,
O':
O'':
O''']
monohydrate]
top
Crystal data top
[Co(C8H4O5)(C12H8N2)]·H2O | F(000) = 892 |
Mr = 437.26 | Dx = 1.697 Mg m−3 |
Monoclinic, P2/n | Mo Kα radiation, λ = 0.71073 Å |
a = 8.5218 (10) Å | Cell parameters from 4790 reflections |
b = 12.044 (1) Å | θ = 1.7–28.3° |
c = 17.028 (2) Å | µ = 1.05 mm−1 |
β = 101.599 (5)° | T = 130 K |
V = 1712.0 (3) Å3 | Prism, red |
Z = 4 | 0.40 × 0.30 × 0.20 mm |
Data collection top
Siemens SMART CCD area-detector diffractometer | 4248 independent reflections |
Radiation source: fine-focus sealed tube | 4069 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
ω scans | θmax = 28.3°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.734, Tmax = 0.811 | k = −16→16 |
13723 measured reflections | l = −13→22 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.034 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.089 | w = 1/[σ2(Fo2) + (0.0522P)2 + 1.0992P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.002 |
4248 reflections | Δρmax = 0.57 e Å−3 |
270 parameters | Δρmin = −0.64 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00015 (3) |
Special details top
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 of F2 >
σ(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 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.94458 (2) | 0.707696 (16) | 0.836120 (12) | 0.01029 (8) | |
OW1 | 1.03872 (16) | 0.40105 (11) | 0.85694 (10) | 0.0236 (3) | |
O1 | 1.04286 (14) | 0.61031 (10) | 0.94143 (7) | 0.0191 (3) | |
O2 | 1.20135 (14) | 0.72981 (10) | 0.89943 (7) | 0.0180 (2) | |
O3 | 1.28121 (14) | 0.35010 (9) | 1.16517 (7) | 0.0149 (2) | |
O4 | 1.48499 (14) | 0.41534 (9) | 1.25678 (7) | 0.0155 (2) | |
O5 | 1.70698 (14) | 0.72769 (10) | 1.11247 (7) | 0.0165 (2) | |
H5A | 1.7694 | 0.7047 | 1.1522 | 0.025* | |
N1 | 0.87222 (16) | 0.84353 (11) | 0.89923 (8) | 0.0122 (3) | |
N2 | 0.98605 (16) | 0.84364 (11) | 0.76536 (8) | 0.0116 (3) | |
C1 | 0.8110 (2) | 0.83948 (14) | 0.96494 (10) | 0.0159 (3) | |
H1A | 0.7962 | 0.7707 | 0.9871 | 0.019* | |
C2 | 0.7678 (2) | 0.93565 (14) | 1.00198 (10) | 0.0186 (3) | |
H2A | 0.7239 | 0.9300 | 1.0476 | 0.022* | |
C3 | 0.7905 (2) | 1.03836 (14) | 0.97075 (11) | 0.0185 (3) | |
H3A | 0.7643 | 1.1026 | 0.9956 | 0.022* | |
C4 | 0.85406 (19) | 1.04505 (13) | 0.90044 (10) | 0.0146 (3) | |
C5 | 0.89154 (18) | 0.94411 (13) | 0.86711 (9) | 0.0118 (3) | |
C6 | 0.95709 (18) | 0.94439 (13) | 0.79567 (9) | 0.0118 (3) | |
C7 | 1.0520 (2) | 0.84146 (14) | 0.70115 (10) | 0.0155 (3) | |
H7A | 1.0743 | 0.7731 | 0.6805 | 0.019* | |
C8 | 1.0894 (2) | 0.93823 (15) | 0.66328 (10) | 0.0204 (3) | |
H8A | 1.1357 | 0.9334 | 0.6184 | 0.024* | |
C9 | 1.0575 (2) | 1.04046 (14) | 0.69254 (11) | 0.0192 (3) | |
H9A | 1.0810 | 1.1052 | 0.6674 | 0.023* | |
C10 | 0.98880 (19) | 1.04567 (13) | 0.76109 (10) | 0.0154 (3) | |
C11 | 0.8854 (2) | 1.14753 (13) | 0.86362 (11) | 0.0181 (3) | |
H11A | 0.8611 | 1.2146 | 0.8855 | 0.022* | |
C12 | 0.9505 (2) | 1.14755 (13) | 0.79687 (10) | 0.0176 (3) | |
H12A | 0.9706 | 1.2148 | 0.7740 | 0.021* | |
C13 | 1.31081 (18) | 0.62554 (13) | 1.01747 (9) | 0.0121 (3) | |
C14 | 1.29223 (18) | 0.53605 (13) | 1.06673 (9) | 0.0128 (3) | |
H14A | 1.1998 | 0.4930 | 1.0557 | 0.015* | |
C15 | 1.41352 (19) | 0.51145 (13) | 1.13284 (9) | 0.0128 (3) | |
C16 | 1.55351 (18) | 0.57484 (14) | 1.14841 (10) | 0.0145 (3) | |
H16A | 1.6340 | 0.5583 | 1.1924 | 0.017* | |
C17 | 1.57282 (19) | 0.66263 (13) | 1.09826 (10) | 0.0137 (3) | |
C18 | 1.45144 (19) | 0.68846 (13) | 1.03276 (10) | 0.0133 (3) | |
H18A | 1.4641 | 0.7474 | 0.9993 | 0.016* | |
C19 | 1.17867 (19) | 0.65672 (13) | 0.94844 (9) | 0.0130 (3) | |
C20 | 1.39047 (18) | 0.41902 (13) | 1.18856 (9) | 0.0127 (3) | |
HW1B | 1.039 (4) | 0.431 (2) | 0.8957 (19) | 0.044 (9)* | |
HW1A | 1.031 (4) | 0.452 (3) | 0.820 (2) | 0.072 (11)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.01242 (12) | 0.00818 (12) | 0.00967 (12) | −0.00059 (7) | 0.00076 (8) | 0.00004 (7) |
OW1 | 0.0237 (6) | 0.0151 (6) | 0.0314 (8) | 0.0027 (5) | 0.0044 (6) | −0.0021 (6) |
O1 | 0.0145 (5) | 0.0200 (6) | 0.0200 (6) | −0.0039 (4) | −0.0029 (5) | 0.0066 (5) |
O2 | 0.0179 (6) | 0.0204 (6) | 0.0144 (6) | −0.0021 (5) | 0.0004 (5) | 0.0060 (5) |
O3 | 0.0143 (5) | 0.0133 (5) | 0.0168 (6) | −0.0035 (4) | 0.0024 (4) | 0.0002 (4) |
O4 | 0.0175 (5) | 0.0125 (5) | 0.0145 (5) | −0.0028 (4) | −0.0016 (4) | 0.0045 (4) |
O5 | 0.0123 (5) | 0.0160 (5) | 0.0193 (6) | −0.0040 (4) | −0.0011 (4) | 0.0047 (5) |
N1 | 0.0133 (6) | 0.0107 (6) | 0.0124 (6) | −0.0013 (5) | 0.0020 (5) | −0.0013 (5) |
N2 | 0.0134 (6) | 0.0098 (6) | 0.0114 (6) | −0.0010 (5) | 0.0016 (5) | 0.0004 (5) |
C1 | 0.0201 (8) | 0.0141 (7) | 0.0148 (7) | −0.0018 (6) | 0.0064 (6) | −0.0003 (6) |
C2 | 0.0222 (8) | 0.0197 (8) | 0.0159 (8) | 0.0001 (6) | 0.0082 (6) | −0.0032 (6) |
C3 | 0.0205 (8) | 0.0163 (8) | 0.0196 (8) | 0.0014 (6) | 0.0061 (7) | −0.0054 (6) |
C4 | 0.0147 (7) | 0.0119 (7) | 0.0163 (8) | −0.0001 (6) | 0.0011 (6) | −0.0025 (6) |
C5 | 0.0122 (7) | 0.0108 (7) | 0.0117 (7) | −0.0011 (5) | 0.0007 (5) | −0.0005 (5) |
C6 | 0.0125 (7) | 0.0106 (7) | 0.0115 (7) | −0.0007 (5) | 0.0008 (5) | 0.0007 (5) |
C7 | 0.0186 (8) | 0.0156 (7) | 0.0135 (7) | −0.0008 (6) | 0.0059 (6) | −0.0015 (6) |
C8 | 0.0264 (9) | 0.0212 (9) | 0.0158 (8) | −0.0036 (7) | 0.0099 (7) | 0.0006 (6) |
C9 | 0.0246 (8) | 0.0156 (8) | 0.0180 (8) | −0.0028 (6) | 0.0058 (7) | 0.0048 (6) |
C10 | 0.0162 (7) | 0.0131 (7) | 0.0161 (8) | −0.0015 (6) | 0.0013 (6) | 0.0019 (6) |
C11 | 0.0220 (8) | 0.0092 (7) | 0.0220 (8) | 0.0003 (6) | 0.0020 (7) | −0.0026 (6) |
C12 | 0.0215 (8) | 0.0097 (7) | 0.0204 (8) | −0.0010 (6) | 0.0013 (7) | 0.0015 (6) |
C13 | 0.0118 (7) | 0.0128 (7) | 0.0113 (7) | 0.0007 (5) | 0.0019 (5) | −0.0002 (6) |
C14 | 0.0129 (7) | 0.0126 (7) | 0.0129 (7) | −0.0008 (5) | 0.0027 (6) | −0.0003 (6) |
C15 | 0.0141 (7) | 0.0117 (7) | 0.0125 (7) | −0.0002 (5) | 0.0022 (6) | 0.0018 (6) |
C16 | 0.0124 (7) | 0.0148 (7) | 0.0149 (7) | −0.0006 (5) | −0.0006 (6) | 0.0024 (6) |
C17 | 0.0126 (7) | 0.0121 (7) | 0.0162 (7) | −0.0023 (5) | 0.0027 (6) | −0.0003 (6) |
C18 | 0.0133 (7) | 0.0131 (7) | 0.0139 (7) | −0.0002 (6) | 0.0038 (6) | 0.0025 (6) |
C19 | 0.0149 (7) | 0.0120 (7) | 0.0118 (7) | 0.0012 (5) | 0.0016 (6) | −0.0005 (5) |
C20 | 0.0131 (7) | 0.0113 (7) | 0.0135 (7) | 0.0002 (5) | 0.0020 (6) | 0.0015 (6) |
Geometric parameters (Å, º) top
Co1—O3i | 2.0421 (12) | C4—C5 | 1.405 (2) |
Co1—O4ii | 2.0801 (11) | C4—C11 | 1.434 (2) |
Co1—N2 | 2.1044 (13) | C5—C6 | 1.437 (2) |
Co1—N1 | 2.1161 (13) | C6—C10 | 1.404 (2) |
Co1—O1 | 2.1654 (12) | C7—C8 | 1.399 (2) |
Co1—O2 | 2.2523 (13) | C7—H7A | 0.9300 |
OW1—HW1B | 0.75 (3) | C8—C9 | 1.376 (2) |
OW1—HW1A | 0.87 (4) | C8—H8A | 0.9300 |
O1—C19 | 1.269 (2) | C9—C10 | 1.409 (2) |
O2—C19 | 1.254 (2) | C9—H9A | 0.9300 |
O3—C20 | 1.2512 (19) | C10—C12 | 1.436 (2) |
O3—Co1i | 2.0421 (12) | C11—C12 | 1.361 (3) |
O4—C20 | 1.2743 (19) | C11—H11A | 0.9300 |
O4—Co1iii | 2.0801 (11) | C12—H12A | 0.9300 |
O5—C17 | 1.3669 (19) | C13—C14 | 1.394 (2) |
O5—H5A | 0.8200 | C13—C18 | 1.397 (2) |
N1—C1 | 1.327 (2) | C13—C19 | 1.503 (2) |
N1—C5 | 1.353 (2) | C14—C15 | 1.398 (2) |
N2—C7 | 1.326 (2) | C14—H14A | 0.9300 |
N2—C6 | 1.360 (2) | C15—C16 | 1.396 (2) |
C1—C2 | 1.403 (2) | C15—C20 | 1.501 (2) |
C1—H1A | 0.9300 | C16—C17 | 1.390 (2) |
C2—C3 | 1.375 (2) | C16—H16A | 0.9300 |
C2—H2A | 0.9300 | C17—C18 | 1.395 (2) |
C3—C4 | 1.412 (2) | C18—H18A | 0.9300 |
C3—H3A | 0.9300 | | |
| | | |
O3i—Co1—O4ii | 91.66 (5) | C10—C6—C5 | 119.82 (14) |
O3i—Co1—N2 | 121.69 (5) | N2—C7—C8 | 122.47 (15) |
O4ii—Co1—N2 | 96.52 (5) | N2—C7—H7A | 118.8 |
O3i—Co1—N1 | 84.19 (5) | C8—C7—H7A | 118.8 |
O4ii—Co1—N1 | 169.67 (5) | C9—C8—C7 | 119.92 (16) |
N2—Co1—N1 | 77.81 (5) | C9—C8—H8A | 120.0 |
O3i—Co1—O1 | 91.78 (5) | C7—C8—H8A | 120.0 |
O4ii—Co1—O1 | 93.73 (5) | C8—C9—C10 | 119.02 (15) |
N2—Co1—O1 | 144.49 (5) | C8—C9—H9A | 120.5 |
N1—Co1—O1 | 95.85 (5) | C10—C9—H9A | 120.5 |
O3i—Co1—O2 | 150.24 (5) | C6—C10—C9 | 117.12 (15) |
O4ii—Co1—O2 | 97.08 (5) | C6—C10—C12 | 119.01 (15) |
N2—Co1—O2 | 85.59 (5) | C9—C10—C12 | 123.86 (15) |
N1—Co1—O2 | 91.13 (5) | C12—C11—C4 | 120.55 (15) |
O1—Co1—O2 | 59.39 (4) | C12—C11—H11A | 119.7 |
HW1B—OW1—HW1A | 106 (3) | C4—C11—H11A | 119.7 |
C19—O1—Co1 | 91.89 (9) | C11—C12—C10 | 121.29 (15) |
C19—O2—Co1 | 88.32 (10) | C11—C12—H12A | 119.4 |
C20—O3—Co1i | 150.32 (11) | C10—C12—H12A | 119.4 |
C20—O4—Co1iii | 117.39 (10) | C14—C13—C18 | 120.27 (14) |
C17—O5—H5A | 109.5 | C14—C13—C19 | 120.39 (14) |
C1—N1—C5 | 118.31 (14) | C18—C13—C19 | 119.33 (14) |
C1—N1—Co1 | 127.14 (11) | C13—C14—C15 | 119.55 (14) |
C5—N1—Co1 | 114.55 (10) | C13—C14—H14A | 120.2 |
C7—N2—C6 | 118.01 (13) | C15—C14—H14A | 120.2 |
C7—N2—Co1 | 127.18 (11) | C16—C15—C14 | 120.14 (14) |
C6—N2—Co1 | 114.37 (10) | C16—C15—C20 | 120.07 (14) |
N1—C1—C2 | 122.13 (15) | C14—C15—C20 | 119.77 (14) |
N1—C1—H1A | 118.9 | C17—C16—C15 | 120.11 (15) |
C2—C1—H1A | 118.9 | C17—C16—H16A | 119.9 |
C3—C2—C1 | 119.92 (15) | C15—C16—H16A | 119.9 |
C3—C2—H2A | 120.0 | O5—C17—C16 | 121.71 (14) |
C1—C2—H2A | 120.0 | O5—C17—C18 | 118.23 (14) |
C2—C3—C4 | 119.13 (15) | C16—C17—C18 | 120.04 (14) |
C2—C3—H3A | 120.4 | C17—C18—C13 | 119.88 (14) |
C4—C3—H3A | 120.4 | C17—C18—H18A | 120.1 |
C5—C4—C3 | 116.75 (15) | C13—C18—H18A | 120.1 |
C5—C4—C11 | 119.39 (15) | O2—C19—O1 | 120.40 (15) |
C3—C4—C11 | 123.84 (15) | O2—C19—C13 | 120.28 (14) |
N1—C5—C4 | 123.74 (14) | O1—C19—C13 | 119.29 (14) |
N1—C5—C6 | 116.36 (13) | O3—C20—O4 | 124.09 (14) |
C4—C5—C6 | 119.90 (14) | O3—C20—C15 | 118.32 (14) |
N2—C6—C10 | 123.43 (14) | O4—C20—C15 | 117.58 (14) |
N2—C6—C5 | 116.75 (13) | | |
Symmetry codes: (i) −x+2, −y+1, −z+2; (ii) x−1/2, −y+1, z−1/2; (iii) x+1/2, −y+1, z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···OW1iv | 0.82 | 2.10 | 2.6302 (18) | 122 |
OW1—HW1B···O1 | 0.75 (3) | 2.30 (3) | 2.8988 (19) | 138 (3) |
OW1—HW1A···O4ii | 0.87 (4) | 1.92 (4) | 2.7740 (19) | 165 (3) |
Symmetry codes: (ii) x−1/2, −y+1, z−1/2; (iv) −x+3, −y+1, −z+2. |