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The title compound, [Cu
2(C
10H
8N
2O)
4(β-Mo
8O
26)]
n, is a one-dimensional coordination polymer containing octahedrally coordinated Cu
II atoms, each of which is bound to three O atoms and two N atoms from three distinct regioselectively oxidized 2,4′-bipyridinium ligands and one O atom from a centrosymmetric β-octamolybdate anion. The 4′-position N atoms within the ligands, as quaternary N atoms, are uncoordinated. [Cu
2(2′-O
−–2,4′-bpyH
+)
4]
4+ dimeric cations are linked through exobidentate β-octamolybdate anions into polymeric chains running along the [011] direction. N—H
O and C—H
O interactions connect adjacent chains into a three-dimensional network.
Supporting information
CCDC reference: 267715
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.013 Å
- R factor = 0.047
- wR factor = 0.132
- Data-to-parameter ratio = 20.9
checkCIF/PLATON results
No syntax errors found
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 ............ 2.00 Ratio
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ?
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 200 Deg.
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
6 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
4 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
1 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, 2001); cell refinement: SMART; data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CrystalMaker (Palmer, 2005); software used to prepare material for publication: SHELXL97.
poly[(µ-
β-octamolybdato-
κ2O:
O)bis[µ-4-(2-pyridyl)pyridinium-3-olato-
κ3N,
O:
O]bis[4-(2-pyridyl)pyridinium-3-olato-
κ2N:
O]dicopper(II)]
top
Crystal data top
[Cu2Mo8O26(C10H8N2O)4] | Z = 1 |
Mr = 1999.34 | F(000) = 962 |
Triclinic, P1 | Dx = 2.668 Mg m−3 |
a = 9.9620 (13) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.1592 (13) Å | Cell parameters from 15331 reflections |
c = 13.7049 (17) Å | θ = 1.6–28.3° |
α = 100.607 (2)° | µ = 2.89 mm−1 |
β = 107.197 (2)° | T = 173 K |
γ = 102.838 (2)° | Block, brown |
V = 1244.6 (3) Å3 | 0.40 × 0.12 × 0.10 mm |
Data collection top
Bruker SMART 1K diffractometer | 5925 independent reflections |
Radiation source: fine-focus sealed tube | 3211 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.082 |
ω scans | θmax = 28.3°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −13→13 |
Tmin = 0.475, Tmax = 0.749 | k = −13→13 |
15331 measured reflections | l = −18→17 |
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)] = 0.047 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.132 | w = 1/[σ2(Fo2) + (0.0592P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.95 | (Δ/σ)max < 0.001 |
5925 reflections | Δρmax = 1.24 e Å−3 |
284 parameters | Δρmin = −1.15 e Å−3 |
2 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0046 (4) |
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 | |
Cu1 | 0.42651 (11) | 0.13624 (11) | 0.03034 (8) | 0.0171 (3) | |
Mo1 | 0.42714 (8) | 0.40068 (8) | 0.27634 (5) | 0.01357 (19) | |
Mo2 | 0.68594 (8) | 0.52944 (7) | 0.50216 (5) | 0.01222 (19) | |
Mo3 | 0.42297 (8) | 0.19768 (8) | 0.45350 (6) | 0.01412 (19) | |
Mo4 | 0.30653 (8) | 0.67085 (8) | 0.31835 (6) | 0.0158 (2) | |
O1 | 0.5343 (6) | 0.0341 (6) | 0.1130 (4) | 0.0138 (13) | |
O2 | 0.3216 (6) | 0.2410 (6) | −0.0491 (5) | 0.0227 (14) | |
O3 | 0.5479 (6) | 0.4936 (6) | 0.2315 (4) | 0.0201 (14) | |
O4 | 0.3051 (6) | 0.3141 (5) | 0.3881 (4) | 0.0122 (12) | |
O5 | 0.3585 (6) | 0.2381 (6) | 0.1884 (4) | 0.0184 (13) | |
O6 | 0.2691 (6) | 0.4784 (6) | 0.2415 (4) | 0.0184 (14) | |
O7 | 0.5721 (6) | 0.3578 (6) | 0.3931 (4) | 0.0148 (13) | |
O8 | 0.3925 (6) | 0.0723 (6) | 0.3435 (4) | 0.0194 (14) | |
O9 | 0.7973 (6) | 0.6136 (6) | 0.4453 (4) | 0.0173 (13) | |
O10 | 0.7979 (6) | 0.4555 (6) | 0.5854 (4) | 0.0141 (13) | |
O11 | 0.3074 (6) | 0.1244 (6) | 0.5128 (4) | 0.0196 (14) | |
O12 | 0.6084 (6) | 0.1991 (6) | 0.5428 (4) | 0.0186 (14) | |
O13 | 0.4184 (7) | 0.7472 (6) | 0.2576 (5) | 0.0282 (16) | |
O14 | 0.4879 (6) | 0.5801 (6) | 0.4271 (4) | 0.0127 (12) | |
O15 | 0.1447 (7) | 0.7040 (6) | 0.2682 (5) | 0.0250 (15) | |
N1 | 0.2337 (8) | −0.0098 (7) | −0.0080 (5) | 0.0180 (8) | |
N2 | 0.1295 (8) | 0.1988 (8) | −0.3212 (6) | 0.0213 (8) | |
H2N | 0.161 (8) | 0.248 (7) | −0.362 (5) | 0.026* | |
N3 | 0.6166 (8) | 0.2841 (7) | 0.0642 (6) | 0.0207 (8) | |
N4 | 0.7357 (8) | 0.0963 (8) | 0.3858 (6) | 0.0168 (8) | |
H4N | 0.748 (9) | 0.060 (8) | 0.441 (4) | 0.020* | |
C1 | 0.2229 (9) | −0.0815 (9) | 0.0651 (7) | 0.0180 (8) | |
H1 | 0.3070 | −0.0650 | 0.1263 | 0.022* | |
C2 | 0.0918 (9) | −0.1785 (9) | 0.0529 (7) | 0.0180 (8) | |
H2 | 0.0856 | −0.2252 | 0.1062 | 0.022* | |
C3 | −0.0297 (9) | −0.2061 (9) | −0.0384 (6) | 0.0180 (8) | |
H3 | −0.1195 | −0.2730 | −0.0488 | 0.022* | |
C4 | −0.0183 (9) | −0.1349 (9) | −0.1138 (7) | 0.0180 (8) | |
H4 | −0.1002 | −0.1537 | −0.1768 | 0.022* | |
C5 | 0.1125 (9) | −0.0363 (9) | −0.0973 (7) | 0.0180 (8) | |
C6 | 0.1216 (10) | 0.0481 (10) | −0.1743 (7) | 0.0213 (8) | |
C7 | 0.2257 (10) | 0.1780 (10) | −0.1425 (7) | 0.0213 (8) | |
C8 | 0.2260 (10) | 0.2533 (10) | −0.2218 (7) | 0.0213 (8) | |
H8 | 0.2954 | 0.3429 | −0.2034 | 0.026* | |
C9 | 0.0224 (10) | −0.0015 (10) | −0.2775 (7) | 0.0213 (8) | |
H9 | −0.0494 | −0.0903 | −0.2987 | 0.026* | |
C10 | 0.0265 (10) | 0.0763 (9) | −0.3499 (7) | 0.0213 (8) | |
H10 | −0.0439 | 0.0425 | −0.4198 | 0.026* | |
C11 | 0.6258 (10) | 0.3562 (9) | −0.0102 (7) | 0.0207 (8) | |
H11 | 0.5408 | 0.3370 | −0.0712 | 0.025* | |
C12 | 0.7493 (9) | 0.4530 (9) | −0.0010 (7) | 0.0207 (8) | |
H12 | 0.7495 | 0.4997 | −0.0550 | 0.025* | |
C13 | 0.8757 (10) | 0.4843 (9) | 0.0865 (7) | 0.0207 (8) | |
H13 | 0.9632 | 0.5528 | 0.0942 | 0.025* | |
C14 | 0.8701 (10) | 0.4119 (9) | 0.1630 (7) | 0.0207 (8) | |
H14 | 0.9551 | 0.4298 | 0.2237 | 0.025* | |
C15 | 0.7407 (10) | 0.3137 (9) | 0.1506 (7) | 0.0207 (8) | |
C16 | 0.7361 (9) | 0.2353 (9) | 0.2327 (7) | 0.0168 (8) | |
C17 | 0.6336 (9) | 0.1020 (9) | 0.2060 (7) | 0.0168 (8) | |
C18 | 0.6394 (9) | 0.0348 (9) | 0.2880 (6) | 0.0168 (8) | |
H18 | 0.5736 | −0.0558 | 0.2730 | 0.020* | |
C19 | 0.8346 (9) | 0.2946 (9) | 0.3366 (6) | 0.0168 (8) | |
H19 | 0.9030 | 0.3848 | 0.3550 | 0.020* | |
C20 | 0.8331 (9) | 0.2224 (9) | 0.4130 (7) | 0.0168 (8) | |
H20 | 0.9004 | 0.2621 | 0.4837 | 0.020* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0174 (6) | 0.0191 (6) | 0.0144 (5) | 0.0031 (4) | 0.0033 (4) | 0.0099 (4) |
Mo1 | 0.0166 (4) | 0.0147 (4) | 0.0084 (4) | 0.0023 (3) | 0.0036 (3) | 0.0048 (3) |
Mo2 | 0.0130 (4) | 0.0139 (4) | 0.0092 (4) | 0.0028 (3) | 0.0026 (3) | 0.0051 (3) |
Mo3 | 0.0167 (4) | 0.0132 (4) | 0.0117 (4) | 0.0030 (3) | 0.0034 (3) | 0.0059 (3) |
Mo4 | 0.0212 (4) | 0.0147 (4) | 0.0103 (4) | 0.0037 (3) | 0.0028 (3) | 0.0071 (3) |
O1 | 0.014 (3) | 0.016 (3) | 0.008 (3) | 0.001 (2) | 0.000 (2) | 0.005 (2) |
O2 | 0.023 (4) | 0.022 (4) | 0.023 (4) | 0.007 (3) | 0.005 (3) | 0.012 (3) |
O3 | 0.018 (3) | 0.027 (4) | 0.016 (3) | 0.003 (3) | 0.008 (3) | 0.010 (3) |
O4 | 0.014 (3) | 0.010 (3) | 0.009 (3) | −0.002 (2) | 0.002 (2) | 0.004 (2) |
O5 | 0.020 (3) | 0.017 (3) | 0.013 (3) | 0.002 (3) | 0.000 (3) | 0.002 (3) |
O6 | 0.022 (3) | 0.022 (4) | 0.007 (3) | 0.002 (3) | 0.002 (3) | 0.004 (3) |
O7 | 0.015 (3) | 0.013 (3) | 0.013 (3) | −0.001 (2) | 0.004 (3) | 0.002 (2) |
O8 | 0.024 (3) | 0.021 (3) | 0.011 (3) | 0.006 (3) | 0.003 (3) | 0.004 (3) |
O9 | 0.020 (3) | 0.021 (3) | 0.011 (3) | 0.005 (3) | 0.004 (3) | 0.009 (3) |
O10 | 0.018 (3) | 0.017 (3) | 0.012 (3) | 0.009 (3) | 0.007 (2) | 0.006 (3) |
O11 | 0.022 (3) | 0.019 (3) | 0.022 (3) | 0.006 (3) | 0.012 (3) | 0.008 (3) |
O12 | 0.027 (4) | 0.014 (3) | 0.014 (3) | 0.005 (3) | 0.006 (3) | 0.005 (3) |
O13 | 0.044 (4) | 0.020 (4) | 0.015 (3) | −0.003 (3) | 0.011 (3) | 0.006 (3) |
O14 | 0.014 (3) | 0.014 (3) | 0.011 (3) | 0.006 (2) | 0.002 (2) | 0.006 (2) |
O15 | 0.028 (4) | 0.024 (4) | 0.018 (3) | 0.009 (3) | 0.000 (3) | 0.005 (3) |
N1 | 0.0198 (18) | 0.018 (2) | 0.0165 (17) | 0.0045 (15) | 0.0055 (15) | 0.0081 (15) |
N2 | 0.023 (2) | 0.025 (2) | 0.0210 (19) | 0.0092 (16) | 0.0091 (16) | 0.0139 (17) |
N3 | 0.0235 (19) | 0.021 (2) | 0.0170 (18) | 0.0034 (16) | 0.0061 (15) | 0.0090 (15) |
N4 | 0.0172 (18) | 0.021 (2) | 0.0145 (17) | 0.0060 (15) | 0.0071 (15) | 0.0076 (15) |
C1 | 0.0198 (18) | 0.018 (2) | 0.0165 (17) | 0.0045 (15) | 0.0055 (15) | 0.0081 (15) |
C2 | 0.0198 (18) | 0.018 (2) | 0.0165 (17) | 0.0045 (15) | 0.0055 (15) | 0.0081 (15) |
C3 | 0.0198 (18) | 0.018 (2) | 0.0165 (17) | 0.0045 (15) | 0.0055 (15) | 0.0081 (15) |
C4 | 0.0198 (18) | 0.018 (2) | 0.0165 (17) | 0.0045 (15) | 0.0055 (15) | 0.0081 (15) |
C5 | 0.0198 (18) | 0.018 (2) | 0.0165 (17) | 0.0045 (15) | 0.0055 (15) | 0.0081 (15) |
C6 | 0.023 (2) | 0.025 (2) | 0.0210 (19) | 0.0092 (16) | 0.0091 (16) | 0.0139 (17) |
C7 | 0.023 (2) | 0.025 (2) | 0.0210 (19) | 0.0092 (16) | 0.0091 (16) | 0.0139 (17) |
C8 | 0.023 (2) | 0.025 (2) | 0.0210 (19) | 0.0092 (16) | 0.0091 (16) | 0.0139 (17) |
C9 | 0.023 (2) | 0.025 (2) | 0.0210 (19) | 0.0092 (16) | 0.0091 (16) | 0.0139 (17) |
C10 | 0.023 (2) | 0.025 (2) | 0.0210 (19) | 0.0092 (16) | 0.0091 (16) | 0.0139 (17) |
C11 | 0.0235 (19) | 0.021 (2) | 0.0170 (18) | 0.0034 (16) | 0.0061 (15) | 0.0090 (15) |
C12 | 0.0235 (19) | 0.021 (2) | 0.0170 (18) | 0.0034 (16) | 0.0061 (15) | 0.0090 (15) |
C13 | 0.0235 (19) | 0.021 (2) | 0.0170 (18) | 0.0034 (16) | 0.0061 (15) | 0.0090 (15) |
C14 | 0.0235 (19) | 0.021 (2) | 0.0170 (18) | 0.0034 (16) | 0.0061 (15) | 0.0090 (15) |
C15 | 0.0235 (19) | 0.021 (2) | 0.0170 (18) | 0.0034 (16) | 0.0061 (15) | 0.0090 (15) |
C16 | 0.0172 (18) | 0.021 (2) | 0.0145 (17) | 0.0060 (15) | 0.0071 (15) | 0.0076 (15) |
C17 | 0.0172 (18) | 0.021 (2) | 0.0145 (17) | 0.0060 (15) | 0.0071 (15) | 0.0076 (15) |
C18 | 0.0172 (18) | 0.021 (2) | 0.0145 (17) | 0.0060 (15) | 0.0071 (15) | 0.0076 (15) |
C19 | 0.0172 (18) | 0.021 (2) | 0.0145 (17) | 0.0060 (15) | 0.0071 (15) | 0.0076 (15) |
C20 | 0.0172 (18) | 0.021 (2) | 0.0145 (17) | 0.0060 (15) | 0.0071 (15) | 0.0076 (15) |
Geometric parameters (Å, º) top
Cu1—O2 | 1.912 (6) | N3—C15 | 1.364 (11) |
Cu1—O1 | 1.930 (5) | N3—C11 | 1.371 (10) |
Cu1—N1 | 2.004 (7) | N4—C18 | 1.332 (10) |
Cu1—N3 | 2.005 (7) | N4—C20 | 1.334 (10) |
Cu1—O1i | 2.551 (5) | N4—H4N | 0.89 (6) |
Cu1—O5 | 2.564 (6) | C1—C2 | 1.394 (11) |
Mo1—O3 | 1.692 (5) | C1—H1 | 0.9500 |
Mo1—O5 | 1.710 (5) | C2—C3 | 1.391 (11) |
Mo1—O6 | 1.892 (6) | C2—H2 | 0.9500 |
Mo1—O7 | 2.002 (6) | C3—C4 | 1.382 (11) |
Mo1—O14 | 2.311 (5) | C3—H3 | 0.9500 |
Mo1—O4 | 2.391 (5) | C4—C5 | 1.384 (11) |
Mo2—O9 | 1.705 (5) | C4—H4 | 0.9500 |
Mo2—O10 | 1.745 (5) | C5—C6 | 1.488 (11) |
Mo2—O7 | 1.928 (5) | C6—C7 | 1.385 (12) |
Mo2—O4ii | 1.943 (5) | C6—C9 | 1.385 (12) |
Mo2—O14 | 2.159 (5) | C7—C8 | 1.439 (11) |
Mo2—O14ii | 2.390 (5) | C8—H8 | 0.9500 |
Mo3—O8 | 1.685 (6) | C9—C10 | 1.382 (11) |
Mo3—O11 | 1.713 (5) | C9—H9 | 0.9500 |
Mo3—O12 | 1.885 (6) | C10—H10 | 0.9500 |
Mo3—O4 | 1.992 (5) | C11—C12 | 1.350 (11) |
Mo3—O14ii | 2.335 (5) | C11—H11 | 0.9500 |
Mo3—O7 | 2.385 (5) | C12—C13 | 1.383 (12) |
Mo4—O15 | 1.690 (6) | C12—H12 | 0.9500 |
Mo4—O13 | 1.714 (6) | C13—C14 | 1.395 (11) |
Mo4—O12ii | 1.926 (6) | C13—H13 | 0.9500 |
Mo4—O6 | 1.938 (6) | C14—C15 | 1.387 (11) |
Mo4—O10ii | 2.305 (5) | C14—H14 | 0.9500 |
Mo4—O14 | 2.447 (5) | C15—C16 | 1.499 (11) |
O1—C17 | 1.306 (9) | C16—C19 | 1.395 (11) |
O2—C7 | 1.290 (10) | C16—C17 | 1.411 (11) |
N1—C1 | 1.357 (10) | C17—C18 | 1.412 (11) |
N1—C5 | 1.375 (10) | C18—H18 | 0.9500 |
N2—C10 | 1.330 (11) | C19—C20 | 1.387 (11) |
N2—C8 | 1.341 (11) | C19—H19 | 0.9500 |
N2—H2N | 0.89 (7) | C20—H20 | 0.9500 |
| | | |
O2—Cu1—O1 | 178.8 (3) | Mo3—O4—Mo1 | 104.2 (2) |
O2—Cu1—N1 | 88.0 (3) | Mo1—O5—Cu1 | 130.8 (3) |
O1—Cu1—N1 | 92.8 (3) | Mo1—O6—Mo4 | 116.5 (3) |
O2—Cu1—N3 | 90.3 (3) | Mo2—O7—Mo1 | 108.9 (3) |
O1—Cu1—N3 | 88.9 (3) | Mo2—O7—Mo3 | 112.2 (2) |
N1—Cu1—N3 | 178.1 (3) | Mo1—O7—Mo3 | 104.1 (2) |
O2—Cu1—O1i | 102.4 (2) | Mo2—O10—Mo4ii | 116.9 (3) |
O1—Cu1—O1i | 78.6 (2) | Mo3—O12—Mo4ii | 118.3 (3) |
N1—Cu1—O1i | 84.6 (2) | Mo2—O14—Mo1 | 91.3 (2) |
N3—Cu1—O1i | 94.9 (2) | Mo2—O14—Mo3ii | 91.26 (19) |
O2—Cu1—O5 | 89.0 (2) | Mo1—O14—Mo3ii | 161.8 (2) |
O1—Cu1—O5 | 90.2 (2) | Mo2—O14—Mo2ii | 104.5 (2) |
N1—Cu1—O5 | 82.6 (2) | Mo1—O14—Mo2ii | 97.91 (19) |
N3—Cu1—O5 | 98.3 (2) | Mo3ii—O14—Mo2ii | 98.85 (19) |
O1i—Cu1—O5 | 162.5 (2) | Mo2—O14—Mo4 | 164.0 (3) |
O3—Mo1—O5 | 104.6 (3) | Mo1—O14—Mo4 | 86.31 (17) |
O3—Mo1—O6 | 102.3 (3) | Mo3ii—O14—Mo4 | 86.29 (18) |
O5—Mo1—O6 | 103.2 (3) | Mo2ii—O14—Mo4 | 91.46 (18) |
O3—Mo1—O7 | 98.1 (2) | C1—N1—C5 | 118.8 (7) |
O5—Mo1—O7 | 98.5 (2) | C1—N1—Cu1 | 115.5 (6) |
O6—Mo1—O7 | 145.2 (2) | C5—N1—Cu1 | 125.6 (5) |
O3—Mo1—O14 | 93.1 (2) | C10—N2—C8 | 121.9 (8) |
O5—Mo1—O14 | 161.5 (2) | C10—N2—H2N | 129 (5) |
O6—Mo1—O14 | 77.6 (2) | C8—N2—H2N | 108 (5) |
O7—Mo1—O14 | 73.4 (2) | C15—N3—C11 | 116.8 (7) |
O3—Mo1—O4 | 163.3 (2) | C15—N3—Cu1 | 126.2 (6) |
O5—Mo1—O4 | 89.9 (2) | C11—N3—Cu1 | 116.8 (6) |
O6—Mo1—O4 | 81.9 (2) | C18—N4—C20 | 123.2 (7) |
O7—Mo1—O4 | 71.2 (2) | C18—N4—H4N | 127 (5) |
O14—Mo1—O4 | 71.81 (18) | C20—N4—H4N | 110 (5) |
O9—Mo2—O10 | 104.1 (3) | N1—C1—C2 | 121.8 (8) |
O9—Mo2—O7 | 102.7 (2) | N1—C1—H1 | 119.1 |
O10—Mo2—O7 | 96.5 (2) | C2—C1—H1 | 119.1 |
O9—Mo2—O4ii | 100.5 (2) | C3—C2—C1 | 119.0 (8) |
O10—Mo2—O4ii | 96.9 (2) | C3—C2—H2 | 120.5 |
O7—Mo2—O4ii | 149.3 (2) | C1—C2—H2 | 120.5 |
O9—Mo2—O14 | 99.1 (2) | C4—C3—C2 | 119.3 (8) |
O10—Mo2—O14 | 156.8 (2) | C4—C3—H3 | 120.4 |
O7—Mo2—O14 | 78.4 (2) | C2—C3—H3 | 120.4 |
O4ii—Mo2—O14 | 78.4 (2) | C3—C4—C5 | 120.0 (8) |
O9—Mo2—O14ii | 174.6 (2) | C3—C4—H4 | 120.0 |
O10—Mo2—O14ii | 81.3 (2) | C5—C4—H4 | 120.0 |
O7—Mo2—O14ii | 76.6 (2) | N1—C5—C4 | 121.1 (8) |
O4ii—Mo2—O14ii | 78.3 (2) | N1—C5—C6 | 118.8 (7) |
O14—Mo2—O14ii | 75.5 (2) | C4—C5—C6 | 120.0 (8) |
O9—Mo2—Mo3ii | 89.29 (19) | C7—C6—C9 | 119.9 (8) |
O10—Mo2—Mo3ii | 132.64 (18) | C7—C6—C5 | 120.3 (8) |
O7—Mo2—Mo3ii | 124.94 (17) | C9—C6—C5 | 119.7 (8) |
O4ii—Mo2—Mo3ii | 35.70 (16) | O2—C7—C6 | 127.5 (8) |
O14—Mo2—Mo3ii | 46.57 (14) | O2—C7—C8 | 115.8 (8) |
O14ii—Mo2—Mo3ii | 86.77 (13) | C6—C7—C8 | 116.7 (8) |
O8—Mo3—O11 | 105.3 (3) | N2—C8—C7 | 120.9 (8) |
O8—Mo3—O12 | 102.3 (3) | N2—C8—H8 | 119.6 |
O11—Mo3—O12 | 102.4 (3) | C7—C8—H8 | 119.6 |
O8—Mo3—O4 | 99.2 (2) | C10—C9—C6 | 120.8 (9) |
O11—Mo3—O4 | 98.0 (2) | C10—C9—H9 | 119.6 |
O12—Mo3—O4 | 145.1 (2) | C6—C9—H9 | 119.6 |
O8—Mo3—O14ii | 158.3 (2) | N2—C10—C9 | 119.7 (9) |
O11—Mo3—O14ii | 96.0 (2) | N2—C10—H10 | 120.2 |
O12—Mo3—O14ii | 76.6 (2) | C9—C10—H10 | 120.2 |
O4—Mo3—O14ii | 73.3 (2) | C12—C11—N3 | 123.4 (8) |
O8—Mo3—O7 | 88.6 (2) | C12—C11—H11 | 118.3 |
O11—Mo3—O7 | 164.0 (2) | N3—C11—H11 | 118.3 |
O12—Mo3—O7 | 81.9 (2) | C11—C12—C13 | 120.3 (8) |
O4—Mo3—O7 | 71.4 (2) | C11—C12—H12 | 119.8 |
O14ii—Mo3—O7 | 69.79 (18) | C13—C12—H12 | 119.8 |
O8—Mo3—Mo2ii | 133.9 (2) | C12—C13—C14 | 117.6 (8) |
O11—Mo3—Mo2ii | 86.41 (19) | C12—C13—H13 | 121.2 |
O12—Mo3—Mo2ii | 118.79 (17) | C14—C13—H13 | 121.2 |
O4—Mo3—Mo2ii | 34.70 (15) | C15—C14—C13 | 120.2 (8) |
O14ii—Mo3—Mo2ii | 42.17 (13) | C15—C14—H14 | 119.9 |
O7—Mo3—Mo2ii | 78.11 (13) | C13—C14—H14 | 119.9 |
O15—Mo4—O13 | 105.8 (3) | N3—C15—C14 | 121.7 (8) |
O15—Mo4—O12ii | 102.3 (3) | N3—C15—C16 | 118.5 (7) |
O13—Mo4—O12ii | 100.0 (3) | C14—C15—C16 | 119.8 (8) |
O15—Mo4—O6 | 103.5 (3) | C19—C16—C17 | 119.7 (8) |
O13—Mo4—O6 | 96.9 (3) | C19—C16—C15 | 119.6 (8) |
O12ii—Mo4—O6 | 143.8 (2) | C17—C16—C15 | 120.7 (8) |
O15—Mo4—O10ii | 88.1 (2) | O1—C17—C16 | 126.7 (7) |
O13—Mo4—O10ii | 165.9 (3) | O1—C17—C18 | 116.6 (7) |
O12ii—Mo4—O10ii | 78.8 (2) | C16—C17—C18 | 116.7 (8) |
O6—Mo4—O10ii | 77.1 (2) | N4—C18—C17 | 121.1 (8) |
O15—Mo4—O14 | 158.4 (2) | N4—C18—H18 | 119.5 |
O13—Mo4—O14 | 95.8 (3) | C17—C18—H18 | 119.5 |
O12ii—Mo4—O14 | 73.2 (2) | C20—C19—C16 | 120.2 (8) |
O6—Mo4—O14 | 73.4 (2) | C20—C19—H19 | 119.9 |
O10ii—Mo4—O14 | 70.29 (18) | C16—C19—H19 | 119.9 |
C17—O1—Cu1 | 118.9 (5) | N4—C20—C19 | 119.0 (8) |
C7—O2—Cu1 | 119.3 (6) | N4—C20—H20 | 120.5 |
Mo2ii—O4—Mo3 | 109.6 (2) | C19—C20—H20 | 120.5 |
Mo2ii—O4—Mo1 | 109.4 (2) | | |
| | | |
N1—Cu1—O1—C17 | −135.0 (6) | O4ii—Mo2—O14—Mo4 | 99.6 (10) |
N3—Cu1—O1—C17 | 45.9 (6) | O14ii—Mo2—O14—Mo4 | −179.6 (11) |
O1i—Cu1—O1—C17 | 141.1 (6) | Mo3ii—Mo2—O14—Mo4 | 80.9 (9) |
O5—Cu1—O1—C17 | −52.4 (5) | O3—Mo1—O14—Mo2 | −78.3 (2) |
N1—Cu1—O2—C7 | −47.0 (6) | O5—Mo1—O14—Mo2 | 85.3 (7) |
N3—Cu1—O2—C7 | 132.1 (6) | O6—Mo1—O14—Mo2 | 179.8 (2) |
O1i—Cu1—O2—C7 | 37.0 (6) | O7—Mo1—O14—Mo2 | 19.24 (19) |
O5—Cu1—O2—C7 | −129.6 (6) | O4—Mo1—O14—Mo2 | 94.4 (2) |
O8—Mo3—O4—Mo2ii | 178.7 (3) | O3—Mo1—O14—Mo3ii | 19.7 (8) |
O11—Mo3—O4—Mo2ii | 71.8 (3) | O5—Mo1—O14—Mo3ii | −176.7 (7) |
O12—Mo3—O4—Mo2ii | −53.7 (5) | O6—Mo1—O14—Mo3ii | −82.1 (8) |
O14ii—Mo3—O4—Mo2ii | −22.2 (2) | O7—Mo1—O14—Mo3ii | 117.3 (8) |
O7—Mo3—O4—Mo2ii | −95.9 (3) | O4—Mo1—O14—Mo3ii | −167.6 (9) |
O8—Mo3—O4—Mo1 | −64.3 (3) | O3—Mo1—O14—Mo2ii | 176.8 (2) |
O11—Mo3—O4—Mo1 | −171.3 (2) | O5—Mo1—O14—Mo2ii | −19.5 (8) |
O12—Mo3—O4—Mo1 | 63.2 (4) | O6—Mo1—O14—Mo2ii | 75.0 (2) |
O14ii—Mo3—O4—Mo1 | 94.8 (2) | O7—Mo1—O14—Mo2ii | −85.6 (2) |
O7—Mo3—O4—Mo1 | 21.03 (18) | O4—Mo1—O14—Mo2ii | −10.49 (17) |
Mo2ii—Mo3—O4—Mo1 | 116.9 (3) | O3—Mo1—O14—Mo4 | 85.9 (2) |
O3—Mo1—O4—Mo2ii | 39.9 (10) | O5—Mo1—O14—Mo4 | −110.5 (7) |
O5—Mo1—O4—Mo2ii | −169.3 (3) | O6—Mo1—O14—Mo4 | −15.99 (19) |
O6—Mo1—O4—Mo2ii | −65.9 (3) | O7—Mo1—O14—Mo4 | −176.6 (2) |
O7—Mo1—O4—Mo2ii | 91.7 (3) | O4—Mo1—O14—Mo4 | −101.46 (19) |
O14—Mo1—O4—Mo2ii | 13.6 (2) | O15—Mo4—O14—Mo2 | −177.4 (8) |
O3—Mo1—O4—Mo3 | −77.2 (9) | O13—Mo4—O14—Mo2 | 2.2 (10) |
O5—Mo1—O4—Mo3 | 73.6 (3) | O12ii—Mo4—O14—Mo2 | −96.6 (10) |
O6—Mo1—O4—Mo3 | 177.0 (3) | O6—Mo4—O14—Mo2 | 97.7 (10) |
O7—Mo1—O4—Mo3 | −25.4 (2) | O10ii—Mo4—O14—Mo2 | 179.6 (10) |
O14—Mo1—O4—Mo3 | −103.5 (2) | O15—Mo4—O14—Mo1 | 100.8 (6) |
O3—Mo1—O5—Cu1 | 4.6 (4) | O13—Mo4—O14—Mo1 | −79.6 (2) |
O6—Mo1—O5—Cu1 | 111.3 (4) | O12ii—Mo4—O14—Mo1 | −178.4 (2) |
O7—Mo1—O5—Cu1 | −96.1 (4) | O6—Mo4—O14—Mo1 | 15.90 (19) |
O14—Mo1—O5—Cu1 | −158.4 (5) | O10ii—Mo4—O14—Mo1 | 97.81 (19) |
O4—Mo1—O5—Cu1 | −167.0 (3) | O15—Mo4—O14—Mo3ii | −95.8 (7) |
O2—Cu1—O5—Mo1 | −75.9 (4) | O13—Mo4—O14—Mo3ii | 83.8 (2) |
O1—Cu1—O5—Mo1 | 103.2 (4) | O12ii—Mo4—O14—Mo3ii | −15.0 (2) |
N1—Cu1—O5—Mo1 | −164.0 (4) | O6—Mo4—O14—Mo3ii | 179.3 (2) |
N3—Cu1—O5—Mo1 | 14.2 (4) | O10ii—Mo4—O14—Mo3ii | −98.81 (19) |
O1i—Cu1—O5—Mo1 | 152.8 (5) | O15—Mo4—O14—Mo2ii | 3.0 (7) |
O3—Mo1—O6—Mo4 | −67.7 (3) | O13—Mo4—O14—Mo2ii | −177.5 (2) |
O5—Mo1—O6—Mo4 | −176.1 (3) | O12ii—Mo4—O14—Mo2ii | 83.8 (2) |
O7—Mo1—O6—Mo4 | 56.8 (5) | O6—Mo4—O14—Mo2ii | −81.9 (2) |
O14—Mo1—O6—Mo4 | 22.8 (3) | O10ii—Mo4—O14—Mo2ii | −0.03 (17) |
O4—Mo1—O6—Mo4 | 95.8 (3) | O2—Cu1—N1—C1 | −148.8 (6) |
O15—Mo4—O6—Mo1 | −179.7 (3) | O1—Cu1—N1—C1 | 30.3 (6) |
O13—Mo4—O6—Mo1 | 72.1 (3) | O1i—Cu1—N1—C1 | 108.5 (6) |
O12ii—Mo4—O6—Mo1 | −45.4 (5) | O5—Cu1—N1—C1 | −59.5 (6) |
O10ii—Mo4—O6—Mo1 | −94.9 (3) | O2—Cu1—N1—C5 | 27.4 (7) |
O14—Mo4—O6—Mo1 | −21.9 (2) | O1—Cu1—N1—C5 | −153.6 (7) |
O9—Mo2—O7—Mo1 | −72.7 (3) | O1i—Cu1—N1—C5 | −75.3 (7) |
O10—Mo2—O7—Mo1 | −178.8 (3) | O5—Cu1—N1—C5 | 116.6 (7) |
O4ii—Mo2—O7—Mo1 | 65.7 (5) | O2—Cu1—N3—C15 | 153.6 (7) |
O14—Mo2—O7—Mo1 | 24.1 (2) | O1—Cu1—N3—C15 | −25.4 (7) |
O14ii—Mo2—O7—Mo1 | 101.7 (3) | O1i—Cu1—N3—C15 | −103.9 (7) |
Mo3ii—Mo2—O7—Mo1 | 25.5 (3) | O5—Cu1—N3—C15 | 64.6 (8) |
O9—Mo2—O7—Mo3 | 172.6 (3) | O2—Cu1—N3—C11 | −31.0 (7) |
O10—Mo2—O7—Mo3 | 66.5 (3) | O1—Cu1—N3—C11 | 150.0 (6) |
O4ii—Mo2—O7—Mo3 | −49.0 (5) | O1i—Cu1—N3—C11 | 71.5 (6) |
O14—Mo2—O7—Mo3 | −90.6 (3) | O5—Cu1—N3—C11 | −120.0 (6) |
O14ii—Mo2—O7—Mo3 | −12.9 (2) | C5—N1—C1—C2 | −1.4 (13) |
Mo3ii—Mo2—O7—Mo3 | −89.2 (2) | Cu1—N1—C1—C2 | 175.1 (7) |
O3—Mo1—O7—Mo2 | 67.9 (3) | N1—C1—C2—C3 | 2.2 (13) |
O5—Mo1—O7—Mo2 | 174.1 (3) | C1—C2—C3—C4 | −1.1 (13) |
O6—Mo1—O7—Mo2 | −57.7 (5) | C2—C3—C4—C5 | −0.8 (13) |
O14—Mo1—O7—Mo2 | −22.9 (2) | C1—N1—C5—C4 | −0.5 (13) |
O4—Mo1—O7—Mo2 | −98.9 (3) | Cu1—N1—C5—C4 | −176.6 (6) |
O3—Mo1—O7—Mo3 | −172.2 (2) | C1—N1—C5—C6 | 176.4 (8) |
O5—Mo1—O7—Mo3 | −66.1 (3) | Cu1—N1—C5—C6 | 0.4 (11) |
O6—Mo1—O7—Mo3 | 62.2 (5) | C3—C4—C5—N1 | 1.6 (13) |
O14—Mo1—O7—Mo3 | 96.9 (2) | C3—C4—C5—C6 | −175.3 (8) |
O4—Mo1—O7—Mo3 | 20.95 (18) | N1—C5—C6—C7 | −21.7 (13) |
O8—Mo3—O7—Mo2 | −167.6 (3) | C4—C5—C6—C7 | 155.3 (9) |
O11—Mo3—O7—Mo2 | 42.1 (10) | N1—C5—C6—C9 | 160.3 (8) |
O12—Mo3—O7—Mo2 | −64.9 (3) | C4—C5—C6—C9 | −22.6 (13) |
O4—Mo3—O7—Mo2 | 92.2 (3) | Cu1—O2—C7—C6 | 42.9 (12) |
O14ii—Mo3—O7—Mo2 | 13.7 (2) | Cu1—O2—C7—C8 | −138.4 (6) |
Mo2ii—Mo3—O7—Mo2 | 56.9 (2) | C9—C6—C7—O2 | 177.2 (9) |
O8—Mo3—O7—Mo1 | 74.8 (3) | C5—C6—C7—O2 | −0.7 (15) |
O11—Mo3—O7—Mo1 | −75.5 (9) | C9—C6—C7—C8 | −1.4 (13) |
O12—Mo3—O7—Mo1 | 177.5 (3) | C5—C6—C7—C8 | −179.4 (8) |
O4—Mo3—O7—Mo1 | −25.4 (2) | C10—N2—C8—C7 | 2.6 (13) |
O14ii—Mo3—O7—Mo1 | −103.9 (3) | O2—C7—C8—N2 | −178.9 (8) |
Mo2ii—Mo3—O7—Mo1 | −60.73 (18) | C6—C7—C8—N2 | −0.1 (13) |
O9—Mo2—O10—Mo4ii | 179.8 (3) | C7—C6—C9—C10 | 0.6 (14) |
O7—Mo2—O10—Mo4ii | −75.3 (3) | C5—C6—C9—C10 | 178.6 (8) |
O4ii—Mo2—O10—Mo4ii | 77.1 (3) | C8—N2—C10—C9 | −3.5 (13) |
O14—Mo2—O10—Mo4ii | 0.4 (7) | C6—C9—C10—N2 | 1.8 (14) |
O14ii—Mo2—O10—Mo4ii | 0.0 (2) | C15—N3—C11—C12 | −0.3 (13) |
Mo3ii—Mo2—O10—Mo4ii | 77.4 (3) | Cu1—N3—C11—C12 | −176.2 (7) |
O8—Mo3—O12—Mo4ii | 179.8 (3) | N3—C11—C12—C13 | 0.0 (14) |
O11—Mo3—O12—Mo4ii | −71.3 (3) | C11—C12—C13—C14 | 0.5 (14) |
O4—Mo3—O12—Mo4ii | 53.0 (5) | C12—C13—C14—C15 | −0.8 (13) |
O14ii—Mo3—O12—Mo4ii | 22.0 (3) | C11—N3—C15—C14 | 0.0 (13) |
O7—Mo3—O12—Mo4ii | 93.0 (3) | Cu1—N3—C15—C14 | 175.4 (7) |
Mo2ii—Mo3—O12—Mo4ii | 21.4 (4) | C11—N3—C15—C16 | −178.9 (8) |
O9—Mo2—O14—Mo1 | 81.7 (2) | Cu1—N3—C15—C16 | −3.5 (12) |
O10—Mo2—O14—Mo1 | −98.9 (6) | C13—C14—C15—N3 | 0.5 (14) |
O7—Mo2—O14—Mo1 | −19.55 (19) | C13—C14—C15—C16 | 179.4 (8) |
O4ii—Mo2—O14—Mo1 | −179.3 (2) | N3—C15—C16—C19 | −155.8 (8) |
O14ii—Mo2—O14—Mo1 | −98.5 (2) | C14—C15—C16—C19 | 25.2 (13) |
Mo3ii—Mo2—O14—Mo1 | 162.0 (3) | N3—C15—C16—C17 | 24.4 (12) |
O9—Mo2—O14—Mo3ii | −80.3 (2) | C14—C15—C16—C17 | −154.5 (9) |
O10—Mo2—O14—Mo3ii | 99.1 (6) | Cu1—O1—C17—C16 | −41.3 (11) |
O7—Mo2—O14—Mo3ii | 178.5 (2) | Cu1—O1—C17—C18 | 139.1 (6) |
O4ii—Mo2—O14—Mo3ii | 18.70 (19) | C19—C16—C17—O1 | 179.4 (8) |
O14ii—Mo2—O14—Mo3ii | 99.5 (2) | C15—C16—C17—O1 | −0.9 (14) |
O9—Mo2—O14—Mo2ii | −179.8 (2) | C19—C16—C17—C18 | −1.0 (12) |
O10—Mo2—O14—Mo2ii | −0.3 (7) | C15—C16—C17—C18 | 178.7 (8) |
O7—Mo2—O14—Mo2ii | 79.0 (2) | C20—N4—C18—C17 | −0.9 (13) |
O4ii—Mo2—O14—Mo2ii | −80.8 (2) | O1—C17—C18—N4 | −179.2 (7) |
O14ii—Mo2—O14—Mo2ii | 0.0 | C16—C17—C18—N4 | 1.1 (12) |
Mo3ii—Mo2—O14—Mo2ii | −99.5 (2) | C17—C16—C19—C20 | 0.7 (13) |
O9—Mo2—O14—Mo4 | 0.6 (10) | C15—C16—C19—C20 | −179.0 (8) |
O10—Mo2—O14—Mo4 | −180.0 (8) | C18—N4—C20—C19 | 0.5 (13) |
O7—Mo2—O14—Mo4 | −100.7 (10) | C16—C19—C20—N4 | −0.4 (13) |
Symmetry codes: (i) −x+1, −y, −z; (ii) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2N···O9iii | 0.89 (7) | 2.02 (7) | 2.892 (10) | 167 (7) |
N4—H4N···O11iv | 0.89 (6) | 2.10 (8) | 2.866 (10) | 144 (6) |
C4—H4···O5v | 0.95 | 2.47 | 3.100 (11) | 124 |
C10—H10···O11v | 0.95 | 2.58 | 3.335 (11) | 137 |
Symmetry codes: (iii) −x+1, −y+1, −z; (iv) −x+1, −y, −z+1; (v) −x, −y, −z. |
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