In the title compound, catena-poly[[bis(1,10-phenanthroline)cadmium(II)]-μ-tetraoxomolybdato], {[CdMoO4(C12H8N2)2]·H2O}n, the CdII ion has a distorted octahedral geometry, defined by four N atoms of two chelating phen (phenanthroline) ligands and two O atoms from two MoO4 tetrahedra. The MoVI atom has a distorted tetrahedral geometry, defined by two terminal O atoms and two bridging (to Cd) O atoms. The compound exhibits a one-dimensional corrugated chain structure, and is further extended into a three-dimensional inorganic–organic hybrid compound via hydrogen-bonding and weaker π–π bonding interactions.
Supporting information
CCDC reference: 277352
Key indicators
- Single-crystal X-ray study
- T = 283 K
- Mean (C-C) = 0.007 Å
- R factor = 0.038
- wR factor = 0.128
- Data-to-parameter ratio = 15.9
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.08 Ratio
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mo2
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 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
2 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXL97.
catena-poly[[bis(1,10-phenanthroline)cadmium(II)]-µ-tetraoxomolybdato]
top
Crystal data top
[CdMoO4(C12H8N2)2]·H2O | F(000) = 1280 |
Mr = 650.76 | Dx = 1.923 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 20706 reflections |
a = 13.901 (3) Å | θ = 3.0–27.5° |
b = 15.370 (3) Å | µ = 1.55 mm−1 |
c = 10.742 (2) Å | T = 283 K |
β = 101.61 (3)° | Block, colorless |
V = 2248.2 (8) Å3 | 0.34 × 0.28 × 0.26 mm |
Z = 4 | |
Data collection top
Rigaku R-AXIS RAPID IP diffractometer | 5060 independent reflections |
Radiation source: Rotation anode | 4251 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
Detector resolution: 0.01 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
oscillation scans | h = −18→16 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −19→19 |
Tmin = 0.611, Tmax = 0.668 | l = −13→13 |
20706 measured reflections | |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.128 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.09P)2] where P = (Fo2 + 2Fc2)/3 |
5060 reflections | (Δ/σ)max = 0.001 |
318 parameters | Δρmax = 0.60 e Å−3 |
2 restraints | Δρmin = −0.98 e Å−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 | |
Cd1 | 0.76417 (2) | 0.143867 (18) | 0.34358 (3) | 0.01603 (12) | |
Mo2 | 0.82708 (3) | 0.13525 (2) | 0.00745 (3) | 0.01740 (12) | |
O1 | 0.8087 (3) | 0.1648 (2) | 0.1595 (3) | 0.0310 (7) | |
O1W | 0.8486 (3) | −0.1171 (2) | −0.0445 (4) | 0.0370 (9) | |
H1 | 0.8260 | −0.0656 | −0.0554 | 0.033 (15)* | |
H2 | 0.9070 | −0.1237 | −0.0556 | 0.06 (2)* | |
O2 | 0.7852 (3) | 0.2810 (2) | 0.3980 (3) | 0.0311 (7) | |
O3 | 0.9512 (3) | 0.1171 (3) | 0.0171 (3) | 0.0397 (9) | |
O4 | 0.7590 (3) | 0.0418 (2) | −0.0429 (3) | 0.0358 (8) | |
N1 | 0.7861 (2) | −0.0096 (2) | 0.3265 (3) | 0.0193 (7) | |
N2 | 0.8821 (3) | 0.0934 (2) | 0.5203 (3) | 0.0202 (7) | |
N3 | 0.5991 (3) | 0.1374 (3) | 0.2297 (4) | 0.0270 (9) | |
N4 | 0.6499 (3) | 0.1313 (3) | 0.4899 (3) | 0.0231 (8) | |
C1 | 0.5720 (4) | 0.1421 (4) | 0.1033 (5) | 0.0401 (14) | |
H1A | 0.6207 | 0.1496 | 0.0563 | 0.048* | |
C2 | 0.4761 (5) | 0.1364 (5) | 0.0384 (5) | 0.0533 (19) | |
H2A | 0.4615 | 0.1406 | −0.0498 | 0.064* | |
C3 | 0.4030 (4) | 0.1246 (4) | 0.1035 (5) | 0.0391 (13) | |
H3A | 0.3381 | 0.1195 | 0.0604 | 0.047* | |
C4 | 0.4265 (3) | 0.1201 (3) | 0.2371 (4) | 0.0289 (10) | |
C5 | 0.3543 (4) | 0.1096 (4) | 0.3127 (5) | 0.0372 (12) | |
H5A | 0.2885 | 0.1045 | 0.2734 | 0.045* | |
C6 | 0.3796 (4) | 0.1071 (4) | 0.4398 (5) | 0.0421 (13) | |
H6A | 0.3309 | 0.1000 | 0.4870 | 0.051* | |
C7 | 0.4796 (4) | 0.1149 (4) | 0.5047 (5) | 0.0311 (10) | |
C8 | 0.5098 (4) | 0.1132 (4) | 0.6391 (5) | 0.0404 (13) | |
H8A | 0.4633 | 0.1064 | 0.6896 | 0.048* | |
C9 | 0.6048 (4) | 0.1215 (4) | 0.6932 (5) | 0.0416 (14) | |
H9A | 0.6246 | 0.1209 | 0.7812 | 0.050* | |
C10 | 0.6743 (4) | 0.1310 (4) | 0.6156 (5) | 0.0328 (11) | |
H10A | 0.7401 | 0.1374 | 0.6541 | 0.039* | |
C11 | 0.5261 (3) | 0.1267 (3) | 0.2964 (4) | 0.0203 (8) | |
C12 | 0.5540 (3) | 0.1243 (3) | 0.4342 (4) | 0.0207 (9) | |
C13 | 0.9275 (3) | 0.1434 (3) | 0.6154 (4) | 0.0238 (9) | |
H13A | 0.9270 | 0.2033 | 0.6034 | 0.029* | |
C14 | 0.9756 (3) | 0.1102 (3) | 0.7320 (4) | 0.0257 (9) | |
H14A | 1.0064 | 0.1475 | 0.7960 | 0.031* | |
C15 | 0.9773 (3) | 0.0227 (3) | 0.7515 (4) | 0.0246 (9) | |
H15A | 1.0076 | −0.0002 | 0.8297 | 0.030* | |
C16 | 0.9325 (3) | −0.0330 (3) | 0.6516 (4) | 0.0200 (8) | |
C17 | 0.9345 (4) | −0.1262 (3) | 0.6628 (4) | 0.0255 (10) | |
H17A | 0.9644 | −0.1514 | 0.7395 | 0.031* | |
C18 | 0.8940 (3) | −0.1777 (3) | 0.5651 (4) | 0.0259 (9) | |
H18A | 0.8989 | −0.2378 | 0.5735 | 0.031* | |
C19 | 0.8430 (3) | −0.1399 (3) | 0.4469 (4) | 0.0213 (9) | |
C20 | 0.7995 (3) | −0.1906 (3) | 0.3418 (4) | 0.0255 (9) | |
H20A | 0.8026 | −0.2510 | 0.3465 | 0.031* | |
C21 | 0.7527 (4) | −0.1507 (3) | 0.2330 (4) | 0.0275 (10) | |
H21A | 0.7251 | −0.1835 | 0.1619 | 0.033* | |
C22 | 0.7467 (3) | −0.0597 (3) | 0.2294 (4) | 0.0255 (9) | |
H22A | 0.7135 | −0.0333 | 0.1553 | 0.031* | |
C23 | 0.8361 (3) | −0.0493 (3) | 0.4343 (4) | 0.0171 (8) | |
C24 | 0.8839 (3) | 0.0061 (3) | 0.5375 (3) | 0.0179 (8) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.01486 (18) | 0.01847 (18) | 0.01448 (18) | −0.00094 (10) | 0.00224 (13) | 0.00115 (9) |
Mo2 | 0.0183 (2) | 0.0188 (2) | 0.0151 (2) | 0.00222 (13) | 0.00338 (15) | 0.00207 (12) |
O1 | 0.0364 (19) | 0.038 (2) | 0.0217 (15) | −0.0043 (15) | 0.0137 (15) | −0.0014 (14) |
O1W | 0.0269 (19) | 0.0237 (18) | 0.061 (2) | −0.0020 (14) | 0.0114 (18) | −0.0060 (17) |
O2 | 0.042 (2) | 0.0235 (18) | 0.0242 (15) | −0.0046 (14) | −0.0011 (15) | −0.0039 (12) |
O3 | 0.0205 (18) | 0.068 (3) | 0.0305 (18) | 0.0115 (17) | 0.0055 (15) | 0.0092 (17) |
O4 | 0.044 (2) | 0.0235 (18) | 0.0374 (18) | −0.0037 (15) | 0.0028 (16) | −0.0012 (14) |
N1 | 0.0166 (17) | 0.0222 (18) | 0.0185 (15) | 0.0010 (13) | 0.0023 (14) | 0.0024 (13) |
N2 | 0.0186 (18) | 0.0215 (19) | 0.0196 (16) | 0.0017 (14) | 0.0015 (14) | 0.0007 (13) |
N3 | 0.018 (2) | 0.046 (3) | 0.0178 (18) | −0.0001 (16) | 0.0062 (16) | 0.0005 (15) |
N4 | 0.0178 (19) | 0.033 (2) | 0.0192 (18) | −0.0013 (14) | 0.0051 (15) | −0.0004 (14) |
C1 | 0.021 (3) | 0.081 (5) | 0.018 (2) | 0.000 (2) | 0.002 (2) | 0.002 (2) |
C2 | 0.031 (3) | 0.106 (6) | 0.021 (3) | −0.004 (3) | 0.000 (3) | 0.002 (3) |
C3 | 0.016 (2) | 0.071 (4) | 0.027 (3) | −0.003 (2) | −0.005 (2) | −0.001 (2) |
C4 | 0.019 (2) | 0.039 (3) | 0.027 (2) | −0.0043 (19) | 0.001 (2) | −0.0024 (19) |
C5 | 0.010 (2) | 0.060 (4) | 0.039 (3) | −0.003 (2) | 0.000 (2) | 0.003 (2) |
C6 | 0.022 (3) | 0.068 (4) | 0.040 (3) | −0.003 (2) | 0.016 (2) | 0.003 (3) |
C7 | 0.022 (2) | 0.046 (3) | 0.027 (2) | −0.001 (2) | 0.009 (2) | 0.001 (2) |
C8 | 0.033 (3) | 0.063 (4) | 0.028 (3) | 0.000 (3) | 0.016 (2) | 0.002 (2) |
C9 | 0.032 (3) | 0.080 (4) | 0.013 (2) | −0.005 (3) | 0.006 (2) | −0.001 (2) |
C10 | 0.020 (2) | 0.053 (3) | 0.025 (2) | −0.001 (2) | 0.005 (2) | −0.002 (2) |
C11 | 0.016 (2) | 0.026 (2) | 0.019 (2) | −0.0022 (16) | 0.0049 (17) | 0.0003 (15) |
C12 | 0.017 (2) | 0.023 (2) | 0.022 (2) | −0.0020 (16) | 0.0050 (18) | −0.0019 (16) |
C13 | 0.020 (2) | 0.019 (2) | 0.029 (2) | 0.0008 (16) | −0.0019 (19) | −0.0019 (16) |
C14 | 0.023 (2) | 0.031 (3) | 0.021 (2) | −0.0025 (18) | −0.0005 (18) | −0.0051 (17) |
C15 | 0.027 (2) | 0.028 (2) | 0.0176 (18) | 0.0018 (18) | 0.0031 (18) | 0.0021 (16) |
C16 | 0.018 (2) | 0.027 (2) | 0.0159 (17) | 0.0026 (16) | 0.0061 (17) | 0.0045 (15) |
C17 | 0.030 (3) | 0.027 (2) | 0.018 (2) | 0.0046 (18) | 0.0009 (19) | 0.0065 (16) |
C18 | 0.028 (2) | 0.021 (2) | 0.027 (2) | 0.0033 (18) | 0.0028 (19) | 0.0065 (17) |
C19 | 0.023 (2) | 0.026 (2) | 0.0168 (19) | 0.0005 (16) | 0.0089 (18) | 0.0040 (15) |
C20 | 0.029 (2) | 0.019 (2) | 0.028 (2) | 0.0016 (18) | 0.0046 (19) | 0.0010 (17) |
C21 | 0.034 (3) | 0.027 (2) | 0.021 (2) | −0.0033 (19) | 0.005 (2) | −0.0037 (16) |
C22 | 0.030 (2) | 0.025 (2) | 0.0197 (19) | 0.0011 (18) | 0.0003 (18) | 0.0033 (16) |
C23 | 0.0137 (19) | 0.024 (2) | 0.0160 (18) | 0.0016 (15) | 0.0080 (16) | 0.0020 (15) |
C24 | 0.0141 (19) | 0.026 (2) | 0.0146 (17) | 0.0008 (15) | 0.0052 (16) | 0.0020 (15) |
Geometric parameters (Å, º) top
Cd1—O2 | 2.191 (3) | C6—C7 | 1.429 (7) |
Cd1—O1 | 2.211 (3) | C6—H6A | 0.9300 |
Cd1—N2 | 2.374 (4) | C7—C12 | 1.407 (6) |
Cd1—N3 | 2.375 (4) | C7—C8 | 1.420 (7) |
Cd1—N1 | 2.390 (4) | C8—C9 | 1.338 (8) |
Cd1—N4 | 2.457 (4) | C8—H8A | 0.9300 |
Mo2—O3 | 1.730 (3) | C9—C10 | 1.404 (7) |
Mo2—O4 | 1.746 (3) | C9—H9A | 0.9300 |
Mo2—O2i | 1.762 (3) | C10—H10A | 0.9300 |
Mo2—O1 | 1.763 (3) | C11—C12 | 1.453 (6) |
O1W—H1 | 0.8501 | C13—C14 | 1.393 (7) |
O1W—H2 | 0.8500 | C13—H13A | 0.9300 |
O2—Mo2ii | 1.762 (3) | C14—C15 | 1.360 (7) |
N1—C22 | 1.323 (5) | C14—H14A | 0.9300 |
N1—C23 | 1.368 (5) | C15—C16 | 1.416 (6) |
N2—C13 | 1.332 (6) | C15—H15A | 0.9300 |
N2—C24 | 1.354 (6) | C16—C24 | 1.409 (5) |
N3—C1 | 1.337 (6) | C16—C17 | 1.437 (6) |
N3—C11 | 1.364 (6) | C17—C18 | 1.344 (7) |
N4—C10 | 1.325 (6) | C17—H17A | 0.9300 |
N4—C12 | 1.351 (6) | C18—C19 | 1.446 (6) |
C1—C2 | 1.376 (8) | C18—H18A | 0.9300 |
C1—H1A | 0.9300 | C19—C23 | 1.400 (6) |
C2—C3 | 1.357 (8) | C19—C20 | 1.405 (6) |
C2—H2A | 0.9300 | C20—C21 | 1.364 (6) |
C3—C4 | 1.408 (7) | C20—H20A | 0.9300 |
C3—H3A | 0.9300 | C21—C22 | 1.401 (6) |
C4—C11 | 1.406 (7) | C21—H21A | 0.9300 |
C4—C5 | 1.422 (7) | C22—H22A | 0.9300 |
C5—C6 | 1.340 (8) | C23—C24 | 1.449 (5) |
C5—H5A | 0.9300 | | |
| | | |
O2—Cd1—O1 | 92.98 (13) | C12—C7—C8 | 116.8 (4) |
O2—Cd1—N2 | 93.89 (12) | C12—C7—C6 | 119.6 (4) |
O1—Cd1—N2 | 119.36 (13) | C8—C7—C6 | 123.5 (4) |
O2—Cd1—N3 | 103.91 (13) | C9—C8—C7 | 120.2 (5) |
O1—Cd1—N3 | 87.75 (13) | C9—C8—H8A | 119.9 |
N2—Cd1—N3 | 146.91 (13) | C7—C8—H8A | 119.9 |
O2—Cd1—N1 | 163.27 (12) | C8—C9—C10 | 119.3 (5) |
O1—Cd1—N1 | 90.70 (12) | C8—C9—H9A | 120.4 |
N2—Cd1—N1 | 70.17 (12) | C10—C9—H9A | 120.4 |
N3—Cd1—N1 | 92.54 (13) | N4—C10—C9 | 122.7 (5) |
O2—Cd1—N4 | 88.48 (12) | N4—C10—H10A | 118.7 |
O1—Cd1—N4 | 156.46 (13) | C9—C10—H10A | 118.7 |
N2—Cd1—N4 | 83.91 (12) | N3—C11—C4 | 122.7 (4) |
N3—Cd1—N4 | 69.15 (13) | N3—C11—C12 | 117.6 (4) |
N1—Cd1—N4 | 94.61 (12) | C4—C11—C12 | 119.7 (4) |
O3—Mo2—O4 | 110.96 (19) | N4—C12—C7 | 122.4 (4) |
O3—Mo2—O2i | 110.48 (17) | N4—C12—C11 | 119.1 (4) |
O4—Mo2—O2i | 108.00 (16) | C7—C12—C11 | 118.5 (4) |
O3—Mo2—O1 | 108.39 (17) | N2—C13—C14 | 123.1 (4) |
O4—Mo2—O1 | 109.16 (17) | N2—C13—H13A | 118.4 |
O2i—Mo2—O1 | 109.84 (16) | C14—C13—H13A | 118.4 |
Mo2—O1—Cd1 | 155.5 (2) | C15—C14—C13 | 119.4 (4) |
H1—O1W—H2 | 115.4 | C15—C14—H14A | 120.3 |
Mo2ii—O2—Cd1 | 152.79 (19) | C13—C14—H14A | 120.3 |
C22—N1—C23 | 117.8 (4) | C14—C15—C16 | 119.4 (4) |
C22—N1—Cd1 | 126.6 (3) | C14—C15—H15A | 120.3 |
C23—N1—Cd1 | 115.2 (3) | C16—C15—H15A | 120.3 |
C13—N2—C24 | 118.3 (4) | C24—C16—C15 | 117.5 (4) |
C13—N2—Cd1 | 124.7 (3) | C24—C16—C17 | 119.7 (4) |
C24—N2—Cd1 | 115.1 (3) | C15—C16—C17 | 122.8 (4) |
C1—N3—C11 | 116.9 (4) | C18—C17—C16 | 121.6 (4) |
C1—N3—Cd1 | 124.5 (3) | C18—C17—H17A | 119.2 |
C11—N3—Cd1 | 118.6 (3) | C16—C17—H17A | 119.2 |
C10—N4—C12 | 118.6 (4) | C17—C18—C19 | 120.2 (4) |
C10—N4—Cd1 | 125.9 (3) | C17—C18—H18A | 119.9 |
C12—N4—Cd1 | 115.5 (3) | C19—C18—H18A | 119.9 |
N3—C1—C2 | 123.9 (5) | C23—C19—C20 | 117.6 (4) |
N3—C1—H1A | 118.1 | C23—C19—C18 | 119.8 (4) |
C2—C1—H1A | 118.1 | C20—C19—C18 | 122.5 (4) |
C3—C2—C1 | 119.8 (5) | C21—C20—C19 | 119.5 (4) |
C3—C2—H2A | 120.1 | C21—C20—H20A | 120.2 |
C1—C2—H2A | 120.1 | C19—C20—H20A | 120.2 |
C2—C3—C4 | 119.2 (5) | C20—C21—C22 | 119.2 (4) |
C2—C3—H3A | 120.4 | C20—C21—H21A | 120.4 |
C4—C3—H3A | 120.4 | C22—C21—H21A | 120.4 |
C11—C4—C3 | 117.6 (4) | N1—C22—C21 | 123.2 (4) |
C11—C4—C5 | 119.6 (4) | N1—C22—H22A | 118.4 |
C3—C4—C5 | 122.8 (5) | C21—C22—H22A | 118.4 |
C6—C5—C4 | 120.9 (5) | N1—C23—C19 | 122.6 (4) |
C6—C5—H5A | 119.5 | N1—C23—C24 | 117.5 (4) |
C4—C5—H5A | 119.5 | C19—C23—C24 | 119.8 (4) |
C5—C6—C7 | 121.6 (5) | N2—C24—C16 | 122.2 (4) |
C5—C6—H6A | 119.2 | N2—C24—C23 | 119.0 (4) |
C7—C6—H6A | 119.2 | C16—C24—C23 | 118.7 (4) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) x, −y+1/2, z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1···O4 | 0.85 | 1.91 | 2.743 (5) | 165 |
O1W—H2···O3iii | 0.85 | 1.93 | 2.739 (6) | 158 |
Symmetry code: (iii) −x+2, −y, −z. |