In the title coordination polymer, [Mn(HIDC)(H
2O)]
n (HIDC
2− is the 1
H-imidazole-4,5-dicarboxylate dianion, C
5H
2N
2O
4), each Mn
II atom is in an octahedral coordination by one N atom and four carboxylate O atoms from three HIDC
2− anions, and one water molecule. The Mn
II atoms are linked by HIDC
2− anions into a layer structure. A three-dimensional coordination network is formed by O—H
N and O—H
O hydrogen bonding.
Supporting information
CCDC reference: 262274
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.022
- wR factor = 0.049
- Data-to-parameter ratio = 12.4
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT199_ALERT_1_C Check the Reported cell_measurement_temperature 293
PLAT200_ALERT_1_C Check the Reported cell_ambient_temperature .... 293
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.18 Ratio
Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 27.48
From the CIF: _reflns_number_total 1534
Count of symmetry unique reflns 885
Completeness (_total/calc) 173.33%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 649
Fraction of Friedel pairs measured 0.733
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
2 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
2 ALERT type 4 Improvement, methodology, query or suggestion
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: ORTEPII (Johnson, 1976); software used to prepare material for publication: Please provide missing information.
Poly[aquamanganese(II)-µ
3-1
H-imidazole-4,5-dicarboxylato]
top
Crystal data top
[Mn(C5H2N2O4)(H2O)] | F(000) = 226 |
Mr = 227.04 | Dx = 2.089 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 3428 reflections |
a = 7.0561 (14) Å | θ = 3.0–27.5° |
b = 7.5531 (15) Å | µ = 1.82 mm−1 |
c = 7.6261 (15) Å | T = 293 K |
β = 117.36 (3)° | Prism, colourless |
V = 360.97 (16) Å3 | 0.32 × 0.24 × 0.11 mm |
Z = 2 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 1534 independent reflections |
Radiation source: fine-focus sealed tube | 1456 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
Detector resolution: 10 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω scans | h = −9→9 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −9→9 |
Tmin = 0.594, Tmax = 0.825 | l = −9→9 |
3525 measured reflections | |
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)] = 0.022 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.049 | w = 1/[σ2(Fo2) + (0.0256P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max < 0.001 |
1534 reflections | Δρmax = 0.26 e Å−3 |
124 parameters | Δρmin = −0.22 e Å−3 |
4 restraints | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.013 (17) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mn1 | 0.28813 (4) | 0.74557 (3) | 0.16233 (4) | 0.01539 (9) | |
N1 | 0.1831 (3) | 0.6125 (3) | 0.3638 (3) | 0.0191 (4) | |
N2 | 0.0594 (3) | 0.5519 (3) | 0.5732 (3) | 0.0215 (4) | |
O1 | 0.5815 (3) | 0.6474 (2) | 0.4159 (3) | 0.0231 (4) | |
O2 | 0.7245 (2) | 0.5010 (2) | 0.6994 (2) | 0.0193 (3) | |
O3 | 0.5465 (3) | 0.3925 (2) | 0.9622 (2) | 0.0297 (4) | |
O4 | 0.2724 (3) | 0.5204 (2) | 0.9794 (2) | 0.0204 (3) | |
O1W | −0.0375 (3) | 0.7794 (2) | −0.0537 (3) | 0.0305 (5) | |
C1 | 0.0107 (4) | 0.5991 (3) | 0.3880 (4) | 0.0226 (5) | |
C2 | 0.5667 (3) | 0.5713 (3) | 0.5535 (3) | 0.0160 (4) | |
C3 | 0.3512 (3) | 0.5645 (3) | 0.5426 (3) | 0.0154 (4) | |
C4 | 0.2763 (3) | 0.5269 (3) | 0.6752 (3) | 0.0176 (5) | |
C5 | 0.3747 (4) | 0.4762 (3) | 0.8882 (3) | 0.0179 (5) | |
H1 | −0.1272 | 0.6196 | 0.2892 | 0.027* | |
H2 | −0.0297 | 0.5394 | 0.6202 | 0.026* | |
H3 | −0.133 (4) | 0.839 (4) | −0.042 (5) | 0.046* | |
H4 | −0.098 (4) | 0.688 (3) | −0.122 (4) | 0.046* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.01473 (13) | 0.01772 (14) | 0.01484 (13) | −0.00036 (16) | 0.00778 (10) | −0.00005 (17) |
N1 | 0.0140 (9) | 0.0256 (10) | 0.0175 (9) | 0.0000 (8) | 0.0071 (8) | 0.0016 (8) |
N2 | 0.0143 (9) | 0.0292 (10) | 0.0245 (10) | 0.0027 (8) | 0.0119 (8) | 0.0040 (9) |
O1 | 0.0155 (8) | 0.0320 (9) | 0.0245 (8) | 0.0004 (7) | 0.0115 (7) | 0.0065 (7) |
O2 | 0.0125 (7) | 0.0224 (8) | 0.0206 (8) | 0.0022 (6) | 0.0057 (6) | 0.0063 (7) |
O3 | 0.0310 (9) | 0.0408 (10) | 0.0200 (9) | 0.0167 (8) | 0.0142 (8) | 0.0043 (8) |
O4 | 0.0240 (8) | 0.0212 (8) | 0.0242 (8) | −0.0009 (7) | 0.0181 (7) | −0.0026 (7) |
O1W | 0.0209 (8) | 0.0260 (12) | 0.0340 (9) | 0.0064 (8) | 0.0037 (7) | −0.0092 (8) |
C1 | 0.0141 (10) | 0.0291 (13) | 0.0239 (12) | 0.0027 (10) | 0.0081 (9) | 0.0052 (10) |
C2 | 0.0156 (10) | 0.0159 (10) | 0.0176 (10) | −0.0007 (9) | 0.0085 (9) | −0.0021 (9) |
C3 | 0.0133 (10) | 0.0164 (10) | 0.0158 (10) | 0.0013 (9) | 0.0060 (8) | −0.0002 (9) |
C4 | 0.0149 (10) | 0.0189 (11) | 0.0211 (11) | 0.0017 (9) | 0.0101 (9) | 0.0003 (9) |
C5 | 0.0201 (10) | 0.0165 (11) | 0.0191 (10) | −0.0015 (9) | 0.0108 (9) | −0.0022 (9) |
Geometric parameters (Å, º) top
Mn1—N1 | 2.228 (2) | N2—C1 | 1.340 (3) |
Mn1—O1 | 2.2125 (18) | N2—C4 | 1.374 (3) |
Mn1—O2i | 2.2197 (16) | N2—H2 | 0.8600 |
Mn1—O3i | 2.1246 (18) | O2—Mn1iii | 2.2197 (16) |
Mn1—O4ii | 2.1700 (16) | O3—Mn1iii | 2.1246 (18) |
Mn1—O1W | 2.1399 (18) | O4—Mn1iv | 2.1700 (16) |
O1—C2 | 1.242 (3) | O1W—H3 | 0.85 (3) |
O2—C2 | 1.273 (3) | O1W—H4 | 0.85 (3) |
O3—C5 | 1.248 (3) | C1—H1 | 0.9300 |
O4—C5 | 1.256 (3) | C2—C3 | 1.485 (3) |
N1—C1 | 1.315 (3) | C3—C4 | 1.370 (3) |
N1—C3 | 1.382 (3) | C4—C5 | 1.493 (3) |
| | | |
O1—Mn1—N1 | 73.76 (7) | O1—C2—O2 | 123.5 (2) |
O1—Mn1—O2i | 95.83 (7) | O1—C2—C3 | 116.72 (19) |
O2i—Mn1—N1 | 88.03 (7) | O2—C2—C3 | 119.75 (19) |
O3i—Mn1—N1 | 165.64 (7) | O3—C5—O4 | 124.7 (2) |
O3i—Mn1—O1 | 94.61 (7) | O3—C5—C4 | 119.4 (2) |
O3i—Mn1—O2i | 84.76 (7) | O4—C5—C4 | 115.8 (2) |
O3i—Mn1—O4ii | 89.90 (7) | C1—N1—Mn1 | 138.91 (16) |
O3i—Mn1—O1W | 102.08 (8) | C1—N1—C3 | 105.7 (2) |
O4ii—Mn1—N1 | 98.91 (7) | C1—N2—C4 | 108.3 (2) |
O4ii—Mn1—O1 | 92.88 (7) | C1—N2—H2 | 125.9 |
O4ii—Mn1—O2i | 170.11 (6) | C2—O1—Mn1 | 119.05 (14) |
O1W—Mn1—N1 | 90.29 (8) | C2—O2—Mn1iii | 124.61 (14) |
O1W—Mn1—O1 | 162.79 (7) | C3—N1—Mn1 | 113.05 (15) |
O1W—Mn1—O2i | 89.92 (6) | C3—C4—N2 | 105.10 (19) |
O1W—Mn1—O4ii | 83.05 (7) | C3—C4—C5 | 135.41 (19) |
Mn1—O1W—H3 | 127 (2) | C4—N2—H2 | 125.9 |
Mn1—O1W—H4 | 116 (2) | C4—C3—N1 | 109.61 (19) |
N1—C1—N2 | 111.3 (2) | C4—C3—C2 | 134.31 (19) |
N1—C1—H1 | 124.4 | C5—O3—Mn1iii | 132.91 (16) |
N1—C3—C2 | 116.03 (19) | C5—O4—Mn1iv | 133.77 (14) |
N2—C1—H1 | 124.4 | H3—O1W—H4 | 107 (2) |
N2—C4—C5 | 119.4 (2) | | |
| | | |
Mn1—N1—C1—N2 | −158.03 (19) | O2i—Mn1—O1—C2 | 84.34 (18) |
Mn1—N1—C3—C2 | −13.2 (2) | O2—C2—C3—N1 | −167.9 (2) |
Mn1—N1—C3—C4 | 164.48 (15) | O2—C2—C3—C4 | 15.2 (4) |
Mn1—O1—C2—O2 | 175.53 (16) | O3i—Mn1—N1—C1 | 130.7 (3) |
Mn1—O1—C2—C3 | −4.5 (3) | O3i—Mn1—N1—C3 | −28.7 (4) |
Mn1iii—O2—C2—O1 | −140.18 (18) | O3i—Mn1—O1—C2 | 169.52 (17) |
Mn1iii—O2—C2—C3 | 39.8 (3) | O4ii—Mn1—N1—C1 | −102.0 (3) |
Mn1iii—O3—C5—O4 | 161.83 (17) | O4ii—Mn1—N1—C3 | 98.55 (16) |
Mn1iii—O3—C5—C4 | −16.9 (3) | O4ii—Mn1—O1—C2 | −100.34 (18) |
Mn1iv—O4—C5—O3 | 86.1 (3) | O1W—Mn1—N1—C1 | −19.0 (3) |
Mn1iv—O4—C5—C4 | −95.1 (2) | O1W—Mn1—N1—C3 | −178.44 (16) |
N1—Mn1—O1—C2 | −1.90 (16) | O1W—Mn1—O1—C2 | −24.6 (4) |
N1—C3—C4—N2 | 0.4 (3) | C1—N1—C3—C2 | −179.26 (19) |
N1—C3—C4—C5 | −177.0 (2) | C1—N1—C3—C4 | −1.6 (3) |
N2—C4—C5—O3 | 153.9 (2) | C1—N2—C4—C3 | 1.1 (3) |
N2—C4—C5—O4 | −24.9 (3) | C1—N2—C4—C5 | 178.9 (2) |
O1—Mn1—N1—C1 | 167.5 (3) | C2—C3—C4—N2 | 177.4 (2) |
O1—Mn1—N1—C3 | 8.13 (15) | C2—C3—C4—C5 | 0.0 (5) |
O1—C2—C3—N1 | 12.1 (3) | C3—N1—C1—N2 | 2.3 (3) |
O1—C2—C3—C4 | −164.8 (3) | C3—C4—C5—O3 | −29.0 (4) |
O2i—Mn1—N1—C1 | 70.9 (2) | C3—C4—C5—O4 | 152.2 (3) |
O2i—Mn1—N1—C3 | −88.53 (16) | C4—N2—C1—N1 | −2.2 (3) |
Symmetry codes: (i) −x+1, y+1/2, −z+1; (ii) x, y, z−1; (iii) −x+1, y−1/2, −z+1; (iv) x, y, z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···O1v | 0.86 | 2.59 | 3.101 (3) | 119 |
N2—H2···O2v | 0.86 | 2.10 | 2.958 (3) | 173 |
O1W—H4···O2vi | 0.85 (3) | 1.96 (3) | 2.808 (2) | 171 (3) |
O1W—H3···O4vii | 0.85 (3) | 1.87 (3) | 2.692 (2) | 162 (3) |
Symmetry codes: (v) x−1, y, z; (vi) x−1, y, z−1; (vii) −x, y+1/2, −z+1. |