The title compound, (H
3O)
4[Co(H
2O)
6)][Co(C
11H
14N
2O
8)]
2[Mo
8O
26]·6H
2O, features two anionic cobalt complexes and an octamolybdate ion (site symmetry
), three cationic hydronium and one hexaaquacobalt(II) ions (site symmetry
), and six isolated water molecules, forming an inorganic–organic hybrid. These cationic and anionic components together with isolated water molecules are linked together to form a three-dimensional framework connected by various hydrogen bonds.
Supporting information
CCDC reference: 624001
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.006 Å
- R factor = 0.029
- wR factor = 0.087
- Data-to-parameter ratio = 14.0
checkCIF/PLATON results
No syntax errors found
Alert level A
DIFF020_ALERT_1_A _diffrn_standards_interval_count and
_diffrn_standards_interval_time are missing. Number of measurements
between standards or time (min) between standards.
DIFF022_ALERT_1_A _diffrn_standards_decay_% is missing
Percentage decrease in standards intensity.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Co2
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O23
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O24
2 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 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
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Bergerhoff et al., 1996).; software used to prepare material for publication: SHELXTL.
Tetrahydronium hexaaquacobalt(II)
bis{[propane-1,3-diyldiamine-
N,
N,
N',
N'-tetraacetato]cobalt(III)} octamolybdate hexahydrate
top
Crystal data top
(H3O)4[Co(H2O)6)][Co(C11H14N2O8)]2[Mo8O26]·6H2O | Z = 1 |
Mr = 2257.08 | F(000) = 1105 |
Triclinic, P1 | Dx = 2.423 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 8.3925 (4) Å | Cell parameters from 4689 reflections |
b = 10.7997 (6) Å | θ = 1.2–27.5° |
c = 17.4788 (10) Å | µ = 2.48 mm−1 |
α = 89.8891 (8)° | T = 296 K |
β = 85.1910 (7)° | Block, violet |
γ = 78.4996 (8)° | 0.27 × 0.24 × 0.22 mm |
V = 1546.76 (14) Å3 | |
Data collection top
Bruker SMART APEX-II diffractometer | 6031 independent reflections |
Radiation source: fine-focus sealed tube | 5022 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
ω scans | θmax = 26.1°, θmin = 1.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −10→10 |
Tmin = 0.520, Tmax = 0.590 | k = −13→13 |
8404 measured reflections | l = −20→21 |
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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.087 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.047P)2] where P = (Fo2 + 2Fc2)/3 |
6031 reflections | (Δ/σ)max < 0.001 |
430 parameters | Δρmax = 0.73 e Å−3 |
0 restraints | Δρmin = −0.96 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 | |
Co1 | 0.04594 (6) | 0.33634 (5) | 0.16373 (3) | 0.01804 (13) | |
Co2 | 0.5000 | 0.5000 | 0.0000 | 0.02386 (19) | |
Mo1 | 0.69729 (4) | 0.02773 (3) | 0.515690 (19) | 0.01560 (9) | |
Mo2 | 0.19066 (4) | 0.28854 (3) | 0.53252 (2) | 0.01885 (10) | |
Mo3 | 0.40833 (4) | 0.10508 (3) | 0.65123 (2) | 0.01947 (10) | |
Mo4 | 0.48455 (4) | 0.20774 (3) | 0.39794 (2) | 0.01828 (10) | |
O1 | 0.5004 (4) | 0.2191 (3) | 0.30136 (18) | 0.0308 (7) | |
O2 | 0.2606 (3) | 0.2802 (3) | 0.42526 (16) | 0.0212 (6) | |
O3 | −0.0082 (4) | 0.3608 (3) | 0.53525 (18) | 0.0297 (7) | |
O4 | 0.2908 (4) | 0.4047 (3) | 0.55714 (18) | 0.0279 (7) | |
O5 | 0.1997 (3) | 0.1983 (3) | 0.62803 (16) | 0.0231 (6) | |
O6 | 0.5041 (4) | 0.2241 (3) | 0.67155 (19) | 0.0313 (7) | |
O7 | 0.3571 (4) | 0.0453 (3) | 0.73736 (17) | 0.0317 (7) | |
O8 | 0.4443 (3) | 0.1264 (2) | 0.51961 (15) | 0.0174 (6) | |
O9 | 0.6072 (3) | −0.0219 (2) | 0.61540 (16) | 0.0190 (6) | |
O10 | 0.5722 (4) | 0.3247 (3) | 0.43050 (18) | 0.0269 (7) | |
O11 | 0.6744 (3) | 0.0630 (2) | 0.40840 (15) | 0.0179 (6) | |
O12 | 0.7756 (3) | 0.1511 (3) | 0.54436 (18) | 0.0254 (7) | |
O13 | 0.8613 (3) | −0.1008 (2) | 0.50450 (17) | 0.0212 (6) | |
O14 | −0.1471 (4) | 0.3062 (3) | 0.12559 (17) | 0.0246 (7) | |
O15 | 0.1707 (4) | 0.2390 (3) | 0.07959 (17) | 0.0266 (7) | |
O16 | 0.2406 (3) | 0.3685 (3) | 0.19773 (17) | 0.0257 (7) | |
O17 | 0.0272 (4) | 0.4914 (3) | 0.10866 (17) | 0.0265 (7) | |
O18 | 0.3348 (4) | 0.4953 (3) | 0.2733 (2) | 0.0395 (8) | |
O19 | −0.2856 (4) | 0.1551 (3) | 0.1072 (2) | 0.0398 (9) | |
O21 | −0.1086 (4) | 0.6900 (3) | 0.1128 (2) | 0.0435 (9) | |
O22 | 0.3397 (4) | 0.0547 (3) | 0.05458 (19) | 0.0404 (9) | |
O23 | 0.3634 (4) | 0.5801 (3) | 0.4212 (2) | 0.0466 (9) | |
H1 | 0.2996 | 0.6348 | 0.3972 | 0.056* | |
H2 | 0.4334 | 0.6150 | 0.4405 | 0.056* | |
H3 | 0.3085 | 0.5493 | 0.4568 | 0.056* | |
O24 | 0.6229 (5) | 0.8908 (4) | 0.1033 (2) | 0.0595 (12) | |
H4 | 0.7028 | 0.8237 | 0.1085 | 0.071* | |
H5 | 0.6269 | 0.9510 | 0.1389 | 0.071* | |
H6 | 0.6290 | 0.9082 | 0.0520 | 0.071* | |
O25 | 0.0824 (7) | 0.8690 (5) | 0.0637 (3) | 0.0909 (18) | |
H7 | 0.1408 | 0.8538 | 0.0217 | 0.109* | |
H8 | 0.0249 | 0.8145 | 0.0584 | 0.109* | |
O26 | 0.3327 (7) | 0.7692 (4) | 0.1605 (3) | 0.0802 (16) | |
H9 | 0.3357 | 0.8325 | 0.1315 | 0.096* | |
H10 | 0.3646 | 0.7829 | 0.2041 | 0.096* | |
O27 | 0.4867 (4) | 0.5321 (3) | 0.11809 (18) | 0.0391 (8) | |
H11 | 0.4394 | 0.6072 | 0.1297 | 0.047* | |
H12 | 0.4458 | 0.5000 | 0.1590 | 0.047* | |
O28 | 0.4798 (4) | 0.3098 (3) | 0.0211 (2) | 0.0393 (8) | |
H13 | 0.3858 | 0.3085 | 0.0425 | 0.047* | |
H14 | 0.5507 | 0.2661 | 0.0512 | 0.047* | |
O29 | 0.7476 (4) | 0.4464 (3) | −0.0004 (2) | 0.0410 (9) | |
H15 | 0.8293 | 0.4626 | −0.0332 | 0.049* | |
H16 | 0.7791 | 0.4059 | 0.0376 | 0.049* | |
O30 | 0.8890 (5) | 0.1640 (4) | 0.7026 (2) | 0.0623 (12) | |
H17 | 0.9798 | 0.1670 | 0.6769 | 0.075* | |
H18 | 0.8982 | 0.1716 | 0.7505 | 0.075* | |
N1 | 0.0620 (4) | 0.1746 (3) | 0.21526 (19) | 0.0196 (7) | |
N2 | −0.0713 (4) | 0.4418 (3) | 0.2491 (2) | 0.0214 (7) | |
C1 | −0.1781 (6) | 0.1957 (4) | 0.1376 (3) | 0.0271 (10) | |
C2 | −0.0766 (5) | 0.1157 (4) | 0.1939 (3) | 0.0279 (10) | |
H2A | −0.1455 | 0.1052 | 0.2398 | 0.033* | |
H2B | −0.0330 | 0.0326 | 0.1713 | 0.033* | |
C3 | −0.0864 (5) | 0.2632 (4) | 0.3420 (3) | 0.0291 (10) | |
H3A | −0.0561 | 0.2933 | 0.3898 | 0.035* | |
H3B | −0.1615 | 0.2073 | 0.3550 | 0.035* | |
C4 | 0.0652 (5) | 0.1857 (4) | 0.3003 (2) | 0.0250 (9) | |
H4A | 0.1575 | 0.2226 | 0.3107 | 0.030* | |
H4B | 0.0832 | 0.1013 | 0.3213 | 0.030* | |
C5 | −0.1789 (5) | 0.3768 (4) | 0.3011 (3) | 0.0260 (10) | |
H5A | −0.2578 | 0.3490 | 0.2711 | 0.031* | |
H5B | −0.2388 | 0.4373 | 0.3394 | 0.031* | |
C6 | 0.0523 (5) | 0.4886 (4) | 0.2923 (3) | 0.0279 (10) | |
H6A | 0.0507 | 0.4547 | 0.3437 | 0.034* | |
H6B | 0.0235 | 0.5800 | 0.2968 | 0.034* | |
C7 | 0.2229 (5) | 0.4501 (4) | 0.2525 (3) | 0.0252 (9) | |
C8 | 0.2218 (5) | 0.0995 (4) | 0.1828 (2) | 0.0247 (9) | |
H8A | 0.2230 | 0.0100 | 0.1887 | 0.030* | |
H8B | 0.3093 | 0.1203 | 0.2100 | 0.030* | |
C9 | 0.2466 (5) | 0.1293 (4) | 0.0990 (3) | 0.0249 (9) | |
C10 | −0.1740 (5) | 0.5487 (4) | 0.2111 (3) | 0.0283 (10) | |
H10A | −0.2033 | 0.6210 | 0.2460 | 0.034* | |
H10B | −0.2736 | 0.5246 | 0.1979 | 0.034* | |
C11 | −0.0808 (5) | 0.5835 (4) | 0.1398 (3) | 0.0274 (10) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0193 (3) | 0.0170 (3) | 0.0172 (3) | −0.0022 (2) | −0.0014 (2) | 0.0011 (2) |
Co2 | 0.0194 (4) | 0.0251 (4) | 0.0276 (5) | −0.0058 (3) | −0.0019 (3) | 0.0060 (3) |
Mo1 | 0.01363 (17) | 0.01452 (17) | 0.01933 (19) | −0.00442 (13) | −0.00146 (13) | −0.00156 (13) |
Mo2 | 0.01759 (18) | 0.01522 (18) | 0.0231 (2) | −0.00253 (13) | 0.00009 (14) | −0.00241 (14) |
Mo3 | 0.02203 (19) | 0.01846 (19) | 0.01716 (19) | −0.00294 (14) | 0.00022 (14) | −0.00343 (14) |
Mo4 | 0.01878 (18) | 0.01522 (18) | 0.0205 (2) | −0.00307 (13) | −0.00042 (14) | 0.00178 (14) |
O1 | 0.0345 (18) | 0.0290 (17) | 0.0275 (18) | −0.0030 (14) | −0.0025 (14) | 0.0057 (13) |
O2 | 0.0194 (14) | 0.0200 (14) | 0.0233 (16) | −0.0005 (11) | −0.0046 (12) | 0.0023 (12) |
O3 | 0.0219 (16) | 0.0259 (16) | 0.039 (2) | 0.0001 (13) | 0.0017 (14) | −0.0048 (14) |
O4 | 0.0280 (17) | 0.0232 (16) | 0.0341 (18) | −0.0090 (13) | −0.0027 (14) | −0.0031 (13) |
O5 | 0.0218 (15) | 0.0244 (15) | 0.0213 (16) | −0.0018 (12) | 0.0017 (12) | 0.0008 (12) |
O6 | 0.0324 (17) | 0.0265 (17) | 0.0366 (19) | −0.0088 (14) | −0.0054 (15) | −0.0089 (14) |
O7 | 0.0397 (19) | 0.0341 (18) | 0.0192 (16) | −0.0048 (15) | 0.0032 (14) | −0.0001 (13) |
O8 | 0.0150 (13) | 0.0181 (14) | 0.0196 (15) | −0.0036 (11) | −0.0028 (11) | −0.0027 (11) |
O9 | 0.0192 (14) | 0.0198 (14) | 0.0187 (15) | −0.0045 (11) | −0.0039 (11) | 0.0000 (11) |
O10 | 0.0257 (16) | 0.0208 (15) | 0.0345 (19) | −0.0068 (12) | 0.0002 (14) | 0.0001 (13) |
O11 | 0.0167 (13) | 0.0189 (14) | 0.0174 (15) | −0.0039 (11) | 0.0029 (11) | −0.0002 (11) |
O12 | 0.0204 (15) | 0.0215 (15) | 0.0366 (18) | −0.0089 (12) | −0.0050 (13) | −0.0021 (13) |
O13 | 0.0190 (14) | 0.0168 (14) | 0.0275 (16) | −0.0028 (11) | −0.0014 (12) | −0.0008 (12) |
O14 | 0.0268 (16) | 0.0222 (15) | 0.0270 (17) | −0.0065 (12) | −0.0113 (13) | 0.0045 (12) |
O15 | 0.0329 (17) | 0.0220 (15) | 0.0213 (16) | 0.0018 (13) | 0.0004 (13) | 0.0005 (12) |
O16 | 0.0221 (15) | 0.0279 (16) | 0.0269 (17) | −0.0042 (12) | −0.0028 (13) | −0.0031 (13) |
O17 | 0.0302 (16) | 0.0209 (15) | 0.0263 (17) | −0.0017 (13) | 0.0014 (13) | 0.0070 (12) |
O18 | 0.0329 (19) | 0.046 (2) | 0.044 (2) | −0.0183 (16) | −0.0058 (16) | −0.0035 (17) |
O19 | 0.044 (2) | 0.0350 (19) | 0.049 (2) | −0.0188 (16) | −0.0300 (18) | 0.0098 (16) |
O21 | 0.044 (2) | 0.0231 (17) | 0.057 (2) | 0.0047 (15) | 0.0036 (18) | 0.0170 (16) |
O22 | 0.044 (2) | 0.0335 (19) | 0.034 (2) | 0.0098 (16) | 0.0072 (16) | −0.0027 (15) |
O23 | 0.040 (2) | 0.046 (2) | 0.056 (2) | −0.0108 (17) | −0.0058 (18) | 0.0028 (18) |
O24 | 0.065 (3) | 0.057 (3) | 0.047 (3) | 0.015 (2) | −0.012 (2) | −0.007 (2) |
O25 | 0.110 (4) | 0.074 (3) | 0.095 (4) | −0.053 (3) | 0.040 (3) | −0.030 (3) |
O26 | 0.133 (5) | 0.047 (3) | 0.054 (3) | −0.015 (3) | 0.026 (3) | −0.008 (2) |
O27 | 0.0385 (19) | 0.049 (2) | 0.0261 (18) | −0.0029 (16) | 0.0024 (15) | 0.0061 (15) |
O28 | 0.0306 (18) | 0.0308 (18) | 0.058 (2) | −0.0090 (15) | −0.0058 (17) | 0.0155 (16) |
O29 | 0.0218 (17) | 0.063 (2) | 0.037 (2) | −0.0073 (16) | −0.0021 (15) | 0.0240 (17) |
O30 | 0.050 (2) | 0.096 (3) | 0.042 (2) | −0.024 (2) | 0.008 (2) | −0.001 (2) |
N1 | 0.0220 (17) | 0.0214 (18) | 0.0149 (17) | −0.0023 (14) | −0.0041 (14) | 0.0010 (13) |
N2 | 0.0187 (17) | 0.0223 (18) | 0.0235 (19) | −0.0057 (14) | 0.0008 (15) | −0.0029 (14) |
C1 | 0.030 (2) | 0.023 (2) | 0.027 (2) | −0.0028 (18) | −0.0030 (19) | −0.0022 (18) |
C2 | 0.032 (2) | 0.024 (2) | 0.031 (3) | −0.0119 (19) | −0.009 (2) | 0.0036 (19) |
C3 | 0.031 (2) | 0.035 (3) | 0.023 (2) | −0.011 (2) | 0.0013 (19) | 0.0076 (19) |
C4 | 0.028 (2) | 0.027 (2) | 0.020 (2) | −0.0040 (18) | −0.0049 (18) | 0.0019 (18) |
C5 | 0.025 (2) | 0.025 (2) | 0.027 (2) | −0.0060 (18) | 0.0036 (18) | −0.0020 (18) |
C6 | 0.030 (2) | 0.028 (2) | 0.027 (2) | −0.0083 (19) | −0.0006 (19) | −0.0073 (19) |
C7 | 0.025 (2) | 0.026 (2) | 0.028 (2) | −0.0121 (18) | −0.0070 (19) | 0.0074 (19) |
C8 | 0.025 (2) | 0.019 (2) | 0.025 (2) | 0.0068 (17) | −0.0013 (18) | 0.0024 (17) |
C9 | 0.025 (2) | 0.023 (2) | 0.025 (2) | −0.0011 (18) | −0.0008 (18) | −0.0025 (18) |
C10 | 0.026 (2) | 0.022 (2) | 0.034 (3) | 0.0012 (18) | 0.0024 (19) | −0.0004 (19) |
C11 | 0.023 (2) | 0.020 (2) | 0.038 (3) | −0.0028 (17) | −0.004 (2) | 0.0025 (19) |
Geometric parameters (Å, º) top
Co1—O16 | 1.879 (3) | O23—H1 | 0.8501 |
Co1—O14 | 1.889 (3) | O23—H2 | 0.8501 |
Co1—O17 | 1.915 (3) | O23—H3 | 0.8501 |
Co1—O15 | 1.917 (3) | O24—H4 | 0.8943 |
Co1—N1 | 1.949 (3) | O24—H5 | 0.9070 |
Co1—N2 | 1.951 (3) | O24—H6 | 0.9153 |
Co2—O29 | 2.042 (3) | O25—H7 | 0.8447 |
Co2—O29i | 2.042 (3) | O25—H8 | 0.8420 |
Co2—O27i | 2.084 (3) | O26—H9 | 0.8540 |
Co2—O27 | 2.084 (3) | O26—H10 | 0.8507 |
Co2—O28i | 2.123 (3) | O27—H11 | 0.8457 |
Co2—O28 | 2.123 (3) | O27—H12 | 0.8690 |
Mo1—O12 | 1.693 (3) | O28—H13 | 0.8471 |
Mo1—O13 | 1.747 (3) | O28—H14 | 0.8918 |
Mo1—O11 | 1.931 (3) | O29—H15 | 0.9003 |
Mo1—O9 | 1.958 (3) | O29—H16 | 0.8277 |
Mo1—O8 | 2.173 (3) | O30—H17 | 0.8580 |
Mo1—O8ii | 2.341 (3) | O30—H18 | 0.8526 |
Mo2—O3 | 1.693 (3) | N1—C8 | 1.490 (5) |
Mo2—O4 | 1.717 (3) | N1—C4 | 1.494 (5) |
Mo2—O2 | 1.914 (3) | N1—C2 | 1.506 (5) |
Mo2—O5 | 1.931 (3) | N2—C10 | 1.487 (5) |
Mo2—O13ii | 2.264 (3) | N2—C6 | 1.498 (5) |
Mo2—O8 | 2.466 (3) | N2—C5 | 1.499 (5) |
Mo3—O7 | 1.693 (3) | C1—C2 | 1.511 (6) |
Mo3—O6 | 1.699 (3) | C2—H2A | 0.9700 |
Mo3—O5 | 1.913 (3) | C2—H2B | 0.9700 |
Mo3—O9 | 1.993 (3) | C3—C4 | 1.508 (6) |
Mo3—O8 | 2.312 (3) | C3—C5 | 1.526 (6) |
Mo3—O11ii | 2.344 (3) | C3—H3A | 0.9700 |
Mo4—O1 | 1.688 (3) | C3—H3B | 0.9700 |
Mo4—O10 | 1.704 (3) | C4—H4A | 0.9700 |
Mo4—O2 | 1.907 (3) | C4—H4B | 0.9700 |
Mo4—O11 | 2.017 (3) | C5—H5A | 0.9700 |
Mo4—O9ii | 2.307 (3) | C5—H5B | 0.9700 |
Mo4—O8 | 2.323 (3) | C6—C7 | 1.518 (6) |
O14—C1 | 1.284 (5) | C6—H6A | 0.9700 |
O15—C9 | 1.287 (5) | C6—H6B | 0.9700 |
O16—C7 | 1.282 (5) | C8—C9 | 1.506 (6) |
O17—C11 | 1.291 (5) | C8—H8A | 0.9700 |
O18—C7 | 1.222 (5) | C8—H8B | 0.9700 |
O19—C1 | 1.235 (5) | C10—C11 | 1.503 (6) |
O21—C11 | 1.229 (5) | C10—H10A | 0.9700 |
O22—C9 | 1.229 (5) | C10—H10B | 0.9700 |
| | | |
O16—Co1—O14 | 177.70 (13) | Mo3—O8—Mo2 | 86.57 (9) |
O16—Co1—O17 | 87.64 (13) | Mo4—O8—Mo2 | 85.37 (9) |
O14—Co1—O17 | 90.66 (13) | Mo1ii—O8—Mo2 | 91.47 (10) |
O16—Co1—O15 | 89.20 (13) | Mo1—O9—Mo3 | 109.63 (13) |
O14—Co1—O15 | 89.33 (14) | Mo1—O9—Mo4ii | 109.82 (12) |
O17—Co1—O15 | 93.04 (13) | Mo3—O9—Mo4ii | 104.71 (12) |
O16—Co1—N1 | 94.41 (14) | Mo1—O11—Mo4 | 109.67 (12) |
O14—Co1—N1 | 87.24 (13) | Mo1—O11—Mo3ii | 109.97 (12) |
O17—Co1—N1 | 177.15 (13) | Mo4—O11—Mo3ii | 102.63 (12) |
O15—Co1—N1 | 85.00 (13) | Mo1—O13—Mo2ii | 117.74 (14) |
O16—Co1—N2 | 87.90 (14) | C1—O14—Co1 | 115.9 (3) |
O14—Co1—N2 | 93.50 (14) | C9—O15—Co1 | 113.6 (3) |
O17—Co1—N2 | 85.02 (14) | C7—O16—Co1 | 115.4 (3) |
O15—Co1—N2 | 176.58 (14) | C11—O17—Co1 | 114.3 (3) |
N1—Co1—N2 | 97.03 (15) | H1—O23—H2 | 109.4 |
O29—Co2—O29i | 180.0 (2) | H1—O23—H3 | 109.5 |
O29—Co2—O27i | 90.87 (13) | H2—O23—H3 | 109.5 |
O29i—Co2—O27i | 89.13 (13) | H4—O24—H5 | 109.9 |
O29—Co2—O27 | 89.13 (13) | H4—O24—H6 | 105.1 |
O29i—Co2—O27 | 90.87 (13) | H5—O24—H6 | 120.9 |
O27i—Co2—O27 | 180.000 (1) | H7—O25—H8 | 97.0 |
O29—Co2—O28i | 90.89 (14) | H9—O26—H10 | 110.2 |
O29i—Co2—O28i | 89.11 (14) | Co2—O27—H11 | 111.0 |
O27i—Co2—O28i | 89.23 (14) | Co2—O27—H12 | 136.4 |
O27—Co2—O28i | 90.77 (14) | H11—O27—H12 | 94.4 |
O29—Co2—O28 | 89.11 (14) | Co2—O28—H13 | 109.3 |
O29i—Co2—O28 | 90.89 (14) | Co2—O28—H14 | 116.5 |
O27i—Co2—O28 | 90.77 (14) | H13—O28—H14 | 106.0 |
O27—Co2—O28 | 89.23 (14) | Co2—O29—H15 | 131.6 |
O28i—Co2—O28 | 180.0 | Co2—O29—H16 | 114.5 |
O12—Mo1—O13 | 105.99 (14) | H15—O29—H16 | 113.8 |
O12—Mo1—O11 | 101.93 (13) | H17—O30—H18 | 110.1 |
O13—Mo1—O11 | 98.13 (12) | C8—N1—C4 | 108.7 (3) |
O12—Mo1—O9 | 99.39 (13) | C8—N1—C2 | 110.9 (3) |
O13—Mo1—O9 | 96.15 (13) | C4—N1—C2 | 112.0 (3) |
O11—Mo1—O9 | 149.88 (11) | C8—N1—Co1 | 103.8 (2) |
O12—Mo1—O8 | 97.00 (12) | C4—N1—Co1 | 113.1 (3) |
O13—Mo1—O8 | 156.91 (12) | C2—N1—Co1 | 108.1 (2) |
O11—Mo1—O8 | 78.83 (11) | C10—N2—C6 | 110.2 (3) |
O9—Mo1—O8 | 77.66 (11) | C10—N2—C5 | 109.3 (3) |
O12—Mo1—O8ii | 172.56 (12) | C6—N2—C5 | 111.4 (3) |
O13—Mo1—O8ii | 81.29 (12) | C10—N2—Co1 | 104.0 (3) |
O11—Mo1—O8ii | 78.16 (11) | C6—N2—Co1 | 107.7 (2) |
O9—Mo1—O8ii | 77.99 (10) | C5—N2—Co1 | 114.0 (3) |
O8—Mo1—O8ii | 75.67 (11) | O19—C1—O14 | 123.7 (4) |
O3—Mo2—O4 | 104.86 (15) | O19—C1—C2 | 120.4 (4) |
O3—Mo2—O2 | 103.50 (14) | O14—C1—C2 | 115.9 (4) |
O4—Mo2—O2 | 97.18 (14) | N1—C2—C1 | 111.7 (3) |
O3—Mo2—O5 | 102.42 (14) | N1—C2—H2A | 109.3 |
O4—Mo2—O5 | 97.99 (14) | C1—C2—H2A | 109.3 |
O2—Mo2—O5 | 145.35 (12) | N1—C2—H2B | 109.3 |
O3—Mo2—O13ii | 92.89 (12) | C1—C2—H2B | 109.3 |
O4—Mo2—O13ii | 162.22 (12) | H2A—C2—H2B | 107.9 |
O2—Mo2—O13ii | 77.27 (11) | C4—C3—C5 | 118.1 (4) |
O5—Mo2—O13ii | 78.84 (12) | C4—C3—H3A | 107.8 |
O3—Mo2—O8 | 162.32 (12) | C5—C3—H3A | 107.8 |
O4—Mo2—O8 | 92.79 (12) | C4—C3—H3B | 107.8 |
O2—Mo2—O8 | 74.68 (10) | C5—C3—H3B | 107.8 |
O5—Mo2—O8 | 73.63 (11) | H3A—C3—H3B | 107.1 |
O13ii—Mo2—O8 | 69.49 (10) | N1—C4—C3 | 115.5 (4) |
O7—Mo3—O6 | 105.39 (16) | N1—C4—H4A | 108.4 |
O7—Mo3—O5 | 100.17 (14) | C3—C4—H4A | 108.4 |
O6—Mo3—O5 | 101.07 (14) | N1—C4—H4B | 108.4 |
O7—Mo3—O9 | 100.97 (14) | C3—C4—H4B | 108.4 |
O6—Mo3—O9 | 97.32 (14) | H4A—C4—H4B | 107.5 |
O5—Mo3—O9 | 147.06 (12) | N2—C5—C3 | 113.8 (3) |
O7—Mo3—O8 | 159.88 (13) | N2—C5—H5A | 108.8 |
O6—Mo3—O8 | 94.60 (13) | C3—C5—H5A | 108.8 |
O5—Mo3—O8 | 77.73 (11) | N2—C5—H5B | 108.8 |
O9—Mo3—O8 | 73.74 (10) | C3—C5—H5B | 108.8 |
O7—Mo3—O11ii | 88.65 (13) | H5A—C5—H5B | 107.7 |
O6—Mo3—O11ii | 163.85 (13) | N2—C6—C7 | 111.6 (3) |
O5—Mo3—O11ii | 83.85 (11) | N2—C6—H6A | 109.3 |
O9—Mo3—O11ii | 71.72 (11) | C7—C6—H6A | 109.3 |
O8—Mo3—O11ii | 71.23 (10) | N2—C6—H6B | 109.3 |
O1—Mo4—O10 | 105.26 (15) | C7—C6—H6B | 109.3 |
O1—Mo4—O2 | 102.85 (14) | H6A—C6—H6B | 108.0 |
O10—Mo4—O2 | 99.54 (13) | O18—C7—O16 | 123.4 (4) |
O1—Mo4—O11 | 98.60 (13) | O18—C7—C6 | 120.3 (4) |
O10—Mo4—O11 | 97.38 (13) | O16—C7—C6 | 116.2 (4) |
O2—Mo4—O11 | 147.98 (12) | N1—C8—C9 | 109.0 (3) |
O1—Mo4—O9ii | 88.76 (13) | N1—C8—H8A | 109.9 |
O10—Mo4—O9ii | 163.83 (12) | C9—C8—H8A | 109.9 |
O2—Mo4—O9ii | 84.78 (11) | N1—C8—H8B | 109.9 |
O11—Mo4—O9ii | 72.13 (11) | C9—C8—H8B | 109.9 |
O1—Mo4—O8 | 160.59 (13) | H8A—C8—H8B | 108.3 |
O10—Mo4—O8 | 93.50 (13) | O22—C9—O15 | 124.0 (4) |
O2—Mo4—O8 | 78.37 (11) | O22—C9—C8 | 120.9 (4) |
O11—Mo4—O8 | 73.63 (10) | O15—C9—C8 | 115.1 (4) |
O9ii—Mo4—O8 | 71.99 (10) | N2—C10—C11 | 109.5 (3) |
Mo4—O2—Mo2 | 116.47 (14) | N2—C10—H10A | 109.8 |
Mo3—O5—Mo2 | 117.05 (14) | C11—C10—H10A | 109.8 |
Mo1—O8—Mo3 | 92.05 (10) | N2—C10—H10B | 109.8 |
Mo1—O8—Mo4 | 91.69 (10) | C11—C10—H10B | 109.8 |
Mo3—O8—Mo4 | 163.15 (13) | H10A—C10—H10B | 108.2 |
Mo1—O8—Mo1ii | 104.33 (11) | O21—C11—O17 | 123.3 (4) |
Mo3—O8—Mo1ii | 97.89 (10) | O21—C11—C10 | 122.4 (4) |
Mo4—O8—Mo1ii | 97.09 (10) | O17—C11—C10 | 114.3 (4) |
Mo1—O8—Mo2 | 164.17 (13) | | |
| | | |
O1—Mo4—O2—Mo2 | −178.96 (15) | O1—Mo4—O8—Mo1 | 85.5 (4) |
O10—Mo4—O2—Mo2 | −70.78 (18) | O10—Mo4—O8—Mo1 | −79.77 (13) |
O11—Mo4—O2—Mo2 | 50.2 (3) | O2—Mo4—O8—Mo1 | −178.80 (11) |
O8—Mo4—O2—Mo2 | 20.86 (14) | O11—Mo4—O8—Mo1 | 16.90 (10) |
O3—Mo2—O2—Mo4 | 178.23 (15) | O1—Mo4—O8—Mo3 | −171.7 (4) |
O4—Mo2—O2—Mo4 | 71.01 (18) | O10—Mo4—O8—Mo3 | 23.0 (4) |
O5—Mo2—O2—Mo4 | −44.4 (3) | O2—Mo4—O8—Mo3 | −76.0 (4) |
O8—Mo2—O2—Mo4 | −19.92 (13) | O11—Mo4—O8—Mo3 | 119.6 (4) |
O7—Mo3—O5—Mo2 | 179.68 (15) | O1—Mo4—O8—Mo2 | −110.1 (4) |
O6—Mo3—O5—Mo2 | 71.63 (18) | O10—Mo4—O8—Mo2 | 84.65 (12) |
O9—Mo3—O5—Mo2 | −51.1 (3) | O2—Mo4—O8—Mo2 | −14.37 (10) |
O8—Mo3—O5—Mo2 | −20.73 (14) | O11—Mo4—O8—Mo2 | −178.68 (10) |
O3—Mo2—O5—Mo3 | −178.04 (15) | O3—Mo2—O8—Mo1 | −179.2 (5) |
O4—Mo2—O5—Mo3 | −70.82 (18) | O4—Mo2—O8—Mo1 | −2.3 (5) |
O2—Mo2—O5—Mo3 | 44.3 (3) | O2—Mo2—O8—Mo1 | 94.4 (5) |
O8—Mo2—O5—Mo3 | 19.75 (13) | O5—Mo2—O8—Mo1 | −99.8 (5) |
O12—Mo1—O8—Mo3 | −80.01 (13) | O3—Mo2—O8—Mo3 | −93.8 (4) |
O13—Mo1—O8—Mo3 | 94.6 (3) | O4—Mo2—O8—Mo3 | 83.07 (12) |
O11—Mo1—O8—Mo3 | 179.15 (11) | O2—Mo2—O8—Mo3 | 179.75 (11) |
O9—Mo1—O8—Mo3 | 18.11 (10) | O5—Mo2—O8—Mo3 | −14.44 (10) |
O12—Mo1—O8—Mo4 | 83.56 (13) | O3—Mo2—O8—Mo4 | 101.0 (4) |
O13—Mo1—O8—Mo4 | −101.8 (3) | O4—Mo2—O8—Mo4 | −82.13 (12) |
O11—Mo1—O8—Mo4 | −17.28 (10) | O2—Mo2—O8—Mo4 | 14.55 (10) |
O9—Mo1—O8—Mo4 | −178.31 (11) | O5—Mo2—O8—Mo4 | −179.64 (11) |
O12—Mo1—O8—Mo2 | 4.6 (5) | O12—Mo1—O9—Mo3 | 72.68 (15) |
O13—Mo1—O8—Mo2 | 179.3 (4) | O13—Mo1—O9—Mo3 | −179.95 (13) |
O11—Mo1—O8—Mo2 | −96.2 (5) | O11—Mo1—O9—Mo3 | −61.9 (3) |
O9—Mo1—O8—Mo2 | 102.8 (5) | O8—Mo1—O9—Mo3 | −22.50 (12) |
O7—Mo3—O8—Mo1 | −95.4 (4) | O7—Mo3—O9—Mo1 | −178.51 (14) |
O6—Mo3—O8—Mo1 | 78.18 (13) | O6—Mo3—O9—Mo1 | −71.21 (16) |
O5—Mo3—O8—Mo1 | 178.53 (12) | O5—Mo3—O9—Mo1 | 52.4 (3) |
O9—Mo3—O8—Mo1 | −18.11 (10) | O8—Mo3—O9—Mo1 | 21.47 (12) |
O7—Mo3—O8—Mo4 | 161.9 (4) | O12—Mo1—O11—Mo4 | −73.60 (16) |
O6—Mo3—O8—Mo4 | −24.5 (4) | O13—Mo1—O11—Mo4 | 178.06 (13) |
O5—Mo3—O8—Mo4 | 75.8 (4) | O9—Mo1—O11—Mo4 | 60.5 (3) |
O9—Mo3—O8—Mo4 | −120.8 (4) | O8—Mo1—O11—Mo4 | 21.29 (12) |
O7—Mo3—O8—Mo2 | 100.4 (4) | O1—Mo4—O11—Mo1 | 177.92 (14) |
O6—Mo3—O8—Mo2 | −86.03 (13) | O10—Mo4—O11—Mo1 | 71.18 (16) |
O5—Mo3—O8—Mo2 | 14.31 (10) | O2—Mo4—O11—Mo1 | −50.3 (3) |
O9—Mo3—O8—Mo2 | 177.68 (11) | O8—Mo4—O11—Mo1 | −20.32 (12) |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x+1, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O23—H2···O10iii | 0.85 | 2.34 | 2.921 (5) | 126 |
O23—H3···O4 | 0.85 | 2.36 | 3.131 (5) | 151 |
O23—H1···O12iii | 0.85 | 2.47 | 2.947 (4) | 116 |
O23—H2···O4iii | 0.85 | 2.29 | 2.994 (5) | 141 |
O24—H4···O21iv | 0.89 | 1.92 | 2.814 (5) | 173 |
O24—H6···O22i | 0.92 | 1.91 | 2.826 (5) | 175 |
O24—H5···O7iii | 0.91 | 2.18 | 2.897 (5) | 135 |
O25—H7···O19v | 0.84 | 2.46 | 3.298 (6) | 170 |
O25—H8···O21 | 0.84 | 2.09 | 2.836 (6) | 147 |
O26—H9···O25 | 0.85 | 2.48 | 2.851 (8) | 107 |
O27—H12···O18 | 0.87 | 2.14 | 2.960 (5) | 158 |
O27—H12···O16 | 0.87 | 2.49 | 3.208 (5) | 140 |
O27—H11···O26 | 0.85 | 1.86 | 2.702 (5) | 177 |
O28—H14···O19iv | 0.89 | 1.96 | 2.848 (5) | 173 |
O28—H13···O15 | 0.85 | 2.14 | 2.950 (5) | 160 |
O29—H16···O14iv | 0.83 | 1.95 | 2.776 (4) | 178 |
O29—H15···O17i | 0.90 | 1.85 | 2.739 (4) | 172 |
O30—H18···O26iii | 0.85 | 2.36 | 2.904 (6) | 122 |
O30—H17···O5iv | 0.86 | 2.06 | 2.907 (5) | 170 |
Symmetry codes: (i) −x+1, −y+1, −z; (iii) −x+1, −y+1, −z+1; (iv) x+1, y, z; (v) −x, −y+1, −z. |