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The title compound, [Cu
4(β-Mo
8O
26)(C
10H
8N
2)
4]
n, is a two-dimensional 3,4-connected network coordination polymer containing two crystallographically distinct T-coordinated Cu
I atoms, each of which is bound to two N atoms from two bridging 2,4′-bipyridine ligands and a terminal O atom belonging to a centrosymmetric β-octamolybdate anion. Rippled cationic [Cu(2,4′-bpy)]
nn+ chain motifs are linked into `brick-wall' two-dimensional layers by
exo-tetradentate β-octamolybdate anions. The layers stack
via C—H
O interactions to form a three-dimensional structure.
Supporting information
CCDC reference: 636767
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (C-C) = 0.005 Å
- R factor = 0.023
- wR factor = 0.059
- Data-to-parameter ratio = 15.3
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.
| Author Response: CCD detector used
|
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) 300 Deg.
PLAT747_ALERT_1_C D...A Calc 3.073(4), Rep 3.07000 ...... Missing su
C4 -O5 1.555 1.445
PLAT747_ALERT_1_C D...A Calc 3.030(4), Rep 3.03000 ...... Missing su
C7 -O1 1.555 2.667
PLAT747_ALERT_1_C D...A Calc 3.252(4), Rep 3.25000 ...... Missing su
C10 -O4 1.555 2.666
PLAT747_ALERT_1_C D...A Calc 3.462(4), Rep 3.46000 ...... Missing su
C12 -O9 1.555 2.656
PLAT747_ALERT_1_C D...A Calc 3.116(4), Rep 3.12000 ...... Missing su
C14 -O10 1.555 2.766
PLAT747_ALERT_1_C D...A Calc 3.016(4), Rep 3.02000 ...... Missing su
C16 -O3 1.555 2.656
1 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
11 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
11 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
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[tetrakis(µ-2,4'-bipyridine-
κ2N:
N')(µ
4-
β-octamolybdato-
κ4-O:
O':
O'':
O''')tetracopper(I)]
top
Crystal data top
[Cu4Mo8O26(C10H8N2)4] | Z = 1 |
Mr = 2062.46 | F(000) = 988 |
Triclinic, P1 | Dx = 2.682 Mg m−3 |
a = 10.631 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.948 (2) Å | Cell parameters from 15119 reflections |
c = 12.701 (3) Å | θ = 1.8–28.3° |
α = 99.427 (3)° | µ = 3.62 mm−1 |
β = 114.082 (3)° | T = 173 K |
γ = 100.871 (3)° | Block, orange |
V = 1276.7 (5) Å3 | 0.40 × 0.20 × 0.16 mm |
Data collection top
Bruker SMART 1K diffractometer | 5945 independent reflections |
Radiation source: fine-focus sealed tube | 5371 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
ω scans | θmax = 28.3°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −14→14 |
Tmin = 0.412, Tmax = 0.560 | k = −14→14 |
15119 measured reflections | l = −16→16 |
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)] = 0.023 | H-atom parameters constrained |
wR(F2) = 0.059 | w = 1/[σ2(Fo2) + (0.026P)2 + 2.0526P] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max = 0.001 |
5945 reflections | Δρmax = 1.61 e Å−3 |
389 parameters | Δρmin = −0.86 e Å−3 |
0 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: 0.00123 (13) |
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 | 0.92753 (4) | 0.15492 (4) | 0.54966 (3) | 0.02286 (9) | |
Cu2 | 0.44983 (4) | 0.64784 (4) | 0.55367 (4) | 0.02306 (9) | |
Mo1 | 0.82417 (2) | 0.49216 (2) | 0.98953 (2) | 0.01207 (6) | |
Mo2 | 0.82994 (3) | 0.69789 (2) | 0.80942 (2) | 0.01429 (6) | |
Mo3 | 0.88800 (2) | 0.22326 (2) | 0.92594 (2) | 0.01346 (6) | |
Mo4 | 0.91292 (2) | 0.43053 (2) | 0.74899 (2) | 0.01305 (6) | |
O1 | 0.7082 (2) | 0.4166 (2) | 1.03470 (19) | 0.0198 (4) | |
O2 | 0.9983 (2) | 0.58343 (18) | 0.92660 (17) | 0.0135 (4) | |
O3 | 0.7964 (2) | 0.35321 (19) | 0.85871 (17) | 0.0137 (4) | |
O4 | 0.7724 (2) | 0.52242 (19) | 0.71177 (17) | 0.0154 (4) | |
O5 | 0.9288 (2) | 0.7630 (2) | 0.7448 (2) | 0.0242 (5) | |
O6 | 0.9389 (2) | 0.80487 (19) | 0.96915 (18) | 0.0177 (4) | |
O7 | 0.7305 (2) | 0.58341 (19) | 0.90242 (17) | 0.0155 (4) | |
O8 | 0.6773 (2) | 0.7463 (2) | 0.75378 (19) | 0.0216 (5) | |
O9 | 0.7710 (2) | 0.1627 (2) | 0.97684 (19) | 0.0210 (4) | |
O10 | 1.0293 (2) | 0.5091 (2) | 0.70574 (19) | 0.0222 (5) | |
O11 | 0.8213 (2) | 0.2887 (2) | 0.63790 (18) | 0.0204 (4) | |
O12 | 1.0465 (2) | 0.36520 (19) | 0.87257 (17) | 0.0146 (4) | |
O13 | 0.8385 (2) | 0.1130 (2) | 0.79525 (19) | 0.0211 (4) | |
N1 | 0.0852 (3) | 0.1425 (2) | 0.6878 (2) | 0.0174 (5) | |
N2 | 0.7862 (2) | 0.1423 (2) | 0.3920 (2) | 0.0156 (5) | |
N3 | 0.3618 (3) | 0.5250 (2) | 0.6102 (2) | 0.0197 (5) | |
N4 | 0.5271 (3) | −0.2306 (2) | 0.4895 (2) | 0.0174 (5) | |
C1 | 0.2139 (3) | 0.2337 (3) | 0.7557 (3) | 0.0158 (6) | |
C2 | 0.3021 (3) | 0.2302 (3) | 0.8704 (3) | 0.0201 (6) | |
H2 | 0.3903 | 0.2924 | 0.9156 | 0.024* | |
C3 | 0.2599 (3) | 0.1350 (3) | 0.9178 (3) | 0.0221 (6) | |
H3 | 0.3162 | 0.1356 | 0.9965 | 0.027* | |
C4 | 0.1325 (3) | 0.0387 (3) | 0.8468 (3) | 0.0215 (6) | |
H4 | 0.1038 | −0.0292 | 0.8750 | 0.026* | |
C5 | 0.0495 (3) | 0.0459 (3) | 0.7333 (3) | 0.0206 (6) | |
H5 | −0.0358 | −0.0192 | 0.6852 | 0.025* | |
C6 | 0.4125 (3) | 0.5402 (3) | 0.7288 (3) | 0.0205 (6) | |
H6 | 0.4837 | 0.6155 | 0.7802 | 0.025* | |
C7 | 0.3649 (3) | 0.4508 (3) | 0.7779 (3) | 0.0187 (6) | |
H7 | 0.4028 | 0.4668 | 0.8607 | 0.022* | |
C8 | 0.2587 (3) | 0.3350 (3) | 0.7035 (3) | 0.0156 (5) | |
C9 | 0.2053 (3) | 0.3197 (3) | 0.5802 (3) | 0.0183 (6) | |
H9 | 0.1348 | 0.2448 | 0.5267 | 0.022* | |
C10 | 0.2572 (3) | 0.4153 (3) | 0.5377 (3) | 0.0207 (6) | |
H10 | 0.2183 | 0.4037 | 0.4554 | 0.025* | |
C11 | 0.6556 (3) | 0.0529 (3) | 0.3289 (3) | 0.0155 (5) | |
C12 | 0.5644 (3) | 0.0510 (3) | 0.2128 (3) | 0.0214 (6) | |
H12 | 0.4737 | −0.0081 | 0.1721 | 0.026* | |
C13 | 0.6090 (3) | 0.1375 (3) | 0.1576 (3) | 0.0232 (7) | |
H13 | 0.5510 | 0.1335 | 0.0783 | 0.028* | |
C14 | 0.7404 (3) | 0.2291 (3) | 0.2222 (3) | 0.0212 (6) | |
H14 | 0.7717 | 0.2893 | 0.1879 | 0.025* | |
C15 | 0.8246 (3) | 0.2301 (3) | 0.3388 (3) | 0.0190 (6) | |
H15 | 0.9117 | 0.2940 | 0.3829 | 0.023* | |
C16 | 0.4813 (3) | −0.2554 (3) | 0.3702 (3) | 0.0170 (6) | |
H16 | 0.4199 | −0.3364 | 0.3221 | 0.020* | |
C17 | 0.5210 (3) | −0.1666 (3) | 0.3166 (3) | 0.0176 (6) | |
H17 | 0.4865 | −0.1880 | 0.2339 | 0.021* | |
C18 | 0.6136 (3) | −0.0437 (3) | 0.3866 (3) | 0.0151 (5) | |
C19 | 0.6602 (3) | −0.0182 (3) | 0.5101 (3) | 0.0168 (6) | |
H19 | 0.7206 | 0.0624 | 0.5601 | 0.020* | |
C20 | 0.6168 (3) | −0.1124 (3) | 0.5580 (3) | 0.0181 (6) | |
H20 | 0.6505 | −0.0939 | 0.6405 | 0.022* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.01678 (18) | 0.0241 (2) | 0.01801 (19) | −0.00234 (15) | 0.00133 (15) | 0.00818 (16) |
Cu2 | 0.02266 (19) | 0.01944 (19) | 0.0292 (2) | 0.00161 (15) | 0.01384 (17) | 0.01121 (16) |
Mo1 | 0.00955 (11) | 0.01353 (12) | 0.01002 (11) | 0.00113 (9) | 0.00287 (9) | 0.00193 (9) |
Mo2 | 0.01283 (11) | 0.01307 (12) | 0.01159 (12) | −0.00015 (9) | 0.00239 (9) | 0.00252 (9) |
Mo3 | 0.01235 (11) | 0.01125 (12) | 0.01076 (12) | −0.00003 (9) | 0.00158 (9) | 0.00143 (9) |
Mo4 | 0.01278 (11) | 0.01352 (12) | 0.00906 (11) | 0.00109 (9) | 0.00302 (9) | 0.00162 (9) |
O1 | 0.0188 (10) | 0.0225 (11) | 0.0191 (10) | 0.0037 (8) | 0.0101 (9) | 0.0069 (9) |
O2 | 0.0120 (9) | 0.0128 (9) | 0.0110 (9) | 0.0006 (7) | 0.0031 (7) | 0.0004 (7) |
O3 | 0.0117 (9) | 0.0144 (9) | 0.0094 (9) | 0.0002 (7) | 0.0019 (7) | 0.0012 (7) |
O4 | 0.0130 (9) | 0.0163 (10) | 0.0107 (9) | 0.0017 (8) | 0.0008 (8) | 0.0029 (8) |
O5 | 0.0258 (11) | 0.0192 (11) | 0.0217 (11) | −0.0036 (9) | 0.0106 (9) | 0.0023 (9) |
O6 | 0.0161 (10) | 0.0143 (10) | 0.0152 (10) | 0.0032 (8) | 0.0015 (8) | 0.0015 (8) |
O7 | 0.0126 (9) | 0.0182 (10) | 0.0148 (10) | 0.0035 (8) | 0.0051 (8) | 0.0057 (8) |
O8 | 0.0190 (10) | 0.0195 (11) | 0.0192 (11) | 0.0033 (8) | 0.0025 (9) | 0.0067 (9) |
O9 | 0.0193 (10) | 0.0207 (11) | 0.0191 (11) | 0.0011 (8) | 0.0065 (9) | 0.0070 (9) |
O10 | 0.0197 (10) | 0.0258 (12) | 0.0204 (11) | 0.0015 (9) | 0.0100 (9) | 0.0072 (9) |
O11 | 0.0221 (11) | 0.0196 (11) | 0.0132 (10) | 0.0028 (9) | 0.0047 (9) | 0.0012 (8) |
O12 | 0.0138 (9) | 0.0136 (9) | 0.0123 (9) | 0.0031 (7) | 0.0033 (8) | 0.0013 (8) |
O13 | 0.0227 (11) | 0.0155 (10) | 0.0156 (10) | 0.0022 (8) | 0.0030 (9) | −0.0008 (8) |
N1 | 0.0155 (11) | 0.0167 (12) | 0.0165 (12) | 0.0019 (10) | 0.0047 (10) | 0.0052 (10) |
N2 | 0.0136 (11) | 0.0161 (12) | 0.0134 (11) | 0.0010 (9) | 0.0044 (9) | 0.0033 (9) |
N3 | 0.0173 (12) | 0.0199 (13) | 0.0224 (13) | 0.0037 (10) | 0.0087 (10) | 0.0095 (11) |
N4 | 0.0120 (11) | 0.0166 (12) | 0.0193 (12) | 0.0006 (9) | 0.0044 (10) | 0.0053 (10) |
C1 | 0.0149 (13) | 0.0169 (14) | 0.0161 (14) | 0.0042 (11) | 0.0080 (11) | 0.0040 (11) |
C2 | 0.0156 (14) | 0.0229 (15) | 0.0178 (14) | 0.0023 (12) | 0.0050 (12) | 0.0060 (12) |
C3 | 0.0195 (14) | 0.0291 (17) | 0.0170 (14) | 0.0076 (13) | 0.0057 (12) | 0.0103 (13) |
C4 | 0.0226 (15) | 0.0202 (15) | 0.0260 (16) | 0.0072 (12) | 0.0122 (13) | 0.0125 (13) |
C5 | 0.0193 (14) | 0.0183 (15) | 0.0209 (15) | 0.0020 (12) | 0.0074 (12) | 0.0051 (12) |
C6 | 0.0165 (14) | 0.0174 (14) | 0.0236 (15) | 0.0015 (11) | 0.0079 (12) | 0.0023 (12) |
C7 | 0.0166 (13) | 0.0203 (15) | 0.0148 (14) | 0.0015 (11) | 0.0057 (11) | 0.0019 (12) |
C8 | 0.0145 (13) | 0.0172 (14) | 0.0160 (14) | 0.0054 (11) | 0.0068 (11) | 0.0063 (11) |
C9 | 0.0153 (13) | 0.0196 (15) | 0.0139 (14) | 0.0000 (11) | 0.0035 (11) | 0.0030 (11) |
C10 | 0.0201 (14) | 0.0224 (15) | 0.0160 (14) | 0.0019 (12) | 0.0062 (12) | 0.0058 (12) |
C11 | 0.0129 (13) | 0.0164 (14) | 0.0153 (13) | 0.0023 (11) | 0.0061 (11) | 0.0020 (11) |
C12 | 0.0150 (13) | 0.0243 (16) | 0.0189 (15) | 0.0011 (12) | 0.0033 (12) | 0.0078 (13) |
C13 | 0.0190 (14) | 0.0299 (17) | 0.0174 (15) | 0.0055 (13) | 0.0035 (12) | 0.0123 (13) |
C14 | 0.0206 (15) | 0.0225 (15) | 0.0214 (15) | 0.0041 (12) | 0.0094 (12) | 0.0109 (13) |
C15 | 0.0165 (13) | 0.0168 (14) | 0.0205 (15) | −0.0003 (11) | 0.0076 (12) | 0.0048 (12) |
C16 | 0.0102 (12) | 0.0161 (14) | 0.0173 (14) | −0.0009 (10) | 0.0022 (11) | 0.0020 (11) |
C17 | 0.0130 (13) | 0.0197 (14) | 0.0145 (13) | 0.0009 (11) | 0.0034 (11) | 0.0020 (11) |
C18 | 0.0095 (12) | 0.0167 (14) | 0.0165 (13) | 0.0017 (10) | 0.0048 (11) | 0.0034 (11) |
C19 | 0.0137 (13) | 0.0157 (14) | 0.0156 (14) | −0.0011 (11) | 0.0041 (11) | 0.0037 (11) |
C20 | 0.0164 (13) | 0.0190 (14) | 0.0157 (14) | 0.0013 (11) | 0.0056 (11) | 0.0055 (12) |
Geometric parameters (Å, º) top
Cu1—N2 | 1.913 (2) | N4—C16 | 1.349 (4) |
Cu1—N1i | 1.916 (2) | N4—C20 | 1.353 (4) |
Cu1—O11 | 2.408 (2) | C1—C2 | 1.386 (4) |
Cu2—N3 | 1.895 (3) | C1—C8 | 1.482 (4) |
Cu2—N4ii | 1.897 (3) | C2—C3 | 1.378 (4) |
Cu2—O8 | 2.564 (2) | C2—H2 | 0.9300 |
Mo1—O1 | 1.697 (2) | C3—C4 | 1.383 (4) |
Mo1—O7 | 1.747 (2) | C3—H3 | 0.9300 |
Mo1—O12iii | 1.930 (2) | C4—C5 | 1.374 (4) |
Mo1—O3 | 1.940 (2) | C4—H4 | 0.9300 |
Mo1—O2iii | 2.149 (2) | C5—H5 | 0.9300 |
Mo1—O2 | 2.416 (2) | C6—C7 | 1.369 (4) |
Mo2—O5 | 1.703 (2) | C6—H6 | 0.9300 |
Mo2—O8 | 1.710 (2) | C7—C8 | 1.404 (4) |
Mo2—O6 | 1.903 (2) | C7—H7 | 0.9300 |
Mo2—O4 | 1.939 (2) | C8—C9 | 1.399 (4) |
Mo2—O7 | 2.256 (2) | C9—C10 | 1.378 (4) |
Mo2—O2 | 2.504 (2) | C9—H9 | 0.9300 |
Mo3—O13 | 1.697 (2) | C10—H10 | 0.9300 |
Mo3—O9 | 1.700 (2) | C11—C12 | 1.389 (4) |
Mo3—O6iii | 1.898 (2) | C11—C18 | 1.482 (4) |
Mo3—O3 | 1.986 (2) | C12—C13 | 1.390 (4) |
Mo3—O2iii | 2.310 (2) | C12—H12 | 0.9300 |
Mo3—O12 | 2.450 (2) | C13—C14 | 1.378 (4) |
Mo4—O10 | 1.697 (2) | C13—H13 | 0.9300 |
Mo4—O11 | 1.715 (2) | C14—C15 | 1.379 (4) |
Mo4—O4 | 1.901 (2) | C14—H14 | 0.9300 |
Mo4—O12 | 1.981 (2) | C15—H15 | 0.9300 |
Mo4—O2 | 2.288 (2) | C16—C17 | 1.372 (4) |
Mo4—O3 | 2.365 (2) | C16—H16 | 0.9300 |
N1—C5 | 1.350 (4) | C17—C18 | 1.401 (4) |
N1—C1 | 1.361 (4) | C17—H17 | 0.9300 |
N2—C15 | 1.355 (4) | C18—C19 | 1.399 (4) |
N2—C11 | 1.361 (4) | C19—C20 | 1.378 (4) |
N3—C6 | 1.345 (4) | C19—H19 | 0.9300 |
N3—C10 | 1.351 (4) | C20—H20 | 0.9300 |
| | | |
N2—Cu1—N1i | 166.67 (11) | Mo3iii—O6—Mo2 | 120.41 (11) |
N2—Cu1—O11 | 91.17 (9) | Mo1—O7—Mo2 | 119.82 (10) |
N1i—Cu1—O11 | 102.16 (9) | Mo2—O8—Cu2 | 129.30 (11) |
N3—Cu2—N4ii | 176.59 (11) | Mo4—O11—Cu1 | 125.50 (11) |
N3—Cu2—O8 | 94.60 (9) | Mo1iii—O12—Mo4 | 109.24 (9) |
N4ii—Cu2—O8 | 88.62 (9) | Mo1iii—O12—Mo3 | 109.26 (9) |
O1—Mo1—O7 | 104.13 (10) | Mo4—O12—Mo3 | 103.53 (8) |
O1—Mo1—O12iii | 103.31 (10) | C5—N1—C1 | 118.1 (3) |
O7—Mo1—O12iii | 96.53 (9) | C5—N1—Cu1iv | 113.7 (2) |
O1—Mo1—O3 | 100.14 (10) | C1—N1—Cu1iv | 126.6 (2) |
O7—Mo1—O3 | 97.28 (9) | C15—N2—C11 | 118.2 (2) |
O12iii—Mo1—O3 | 148.88 (8) | C15—N2—Cu1 | 115.35 (19) |
O1—Mo1—O2iii | 99.67 (9) | C11—N2—Cu1 | 126.5 (2) |
O7—Mo1—O2iii | 156.20 (8) | C6—N3—C10 | 116.9 (3) |
O12iii—Mo1—O2iii | 78.25 (8) | C6—N3—Cu2 | 119.3 (2) |
O3—Mo1—O2iii | 77.88 (8) | C10—N3—Cu2 | 123.5 (2) |
O1—Mo1—O2 | 174.83 (9) | C16—N4—C20 | 117.5 (3) |
O7—Mo1—O2 | 80.44 (8) | C16—N4—Cu2v | 119.9 (2) |
O12iii—Mo1—O2 | 78.32 (8) | C20—N4—Cu2v | 122.2 (2) |
O3—Mo1—O2 | 76.68 (7) | N1—C1—C2 | 120.5 (3) |
O2iii—Mo1—O2 | 75.76 (8) | N1—C1—C8 | 118.6 (3) |
O5—Mo2—O8 | 104.36 (11) | C2—C1—C8 | 120.9 (3) |
O5—Mo2—O6 | 99.98 (10) | C3—C2—C1 | 120.4 (3) |
O8—Mo2—O6 | 104.48 (10) | C3—C2—H2 | 119.8 |
O5—Mo2—O4 | 95.52 (10) | C1—C2—H2 | 119.8 |
O8—Mo2—O4 | 103.74 (9) | C2—C3—C4 | 119.0 (3) |
O6—Mo2—O4 | 143.10 (8) | C2—C3—H3 | 120.5 |
O5—Mo2—O7 | 167.53 (10) | C4—C3—H3 | 120.5 |
O8—Mo2—O7 | 87.49 (9) | C5—C4—C3 | 118.2 (3) |
O6—Mo2—O7 | 80.38 (8) | C5—C4—H4 | 120.9 |
O4—Mo2—O7 | 77.61 (8) | C3—C4—H4 | 120.9 |
O5—Mo2—O2 | 98.17 (9) | N1—C5—C4 | 123.5 (3) |
O8—Mo2—O2 | 157.44 (9) | N1—C5—H5 | 118.2 |
O6—Mo2—O2 | 72.29 (8) | C4—C5—H5 | 118.2 |
O4—Mo2—O2 | 72.49 (7) | N3—C6—C7 | 123.6 (3) |
O7—Mo2—O2 | 69.95 (7) | N3—C6—H6 | 118.2 |
O13—Mo3—O9 | 104.51 (11) | C7—C6—H6 | 118.2 |
O13—Mo3—O6iii | 102.70 (10) | C6—C7—C8 | 120.0 (3) |
O9—Mo3—O6iii | 102.48 (10) | C6—C7—H7 | 120.0 |
O13—Mo3—O3 | 98.40 (9) | C8—C7—H7 | 120.0 |
O9—Mo3—O3 | 98.37 (9) | C9—C8—C7 | 116.3 (3) |
O6iii—Mo3—O3 | 145.35 (8) | C9—C8—C1 | 123.2 (3) |
O13—Mo3—O2iii | 158.49 (9) | C7—C8—C1 | 120.4 (3) |
O9—Mo3—O2iii | 96.39 (9) | C10—C9—C8 | 120.1 (3) |
O6iii—Mo3—O2iii | 77.18 (8) | C10—C9—H9 | 120.0 |
O3—Mo3—O2iii | 73.23 (8) | C8—C9—H9 | 120.0 |
O13—Mo3—O12 | 87.46 (9) | N3—C10—C9 | 123.1 (3) |
O9—Mo3—O12 | 164.60 (9) | N3—C10—H10 | 118.5 |
O6iii—Mo3—O12 | 83.87 (8) | C9—C10—H10 | 118.5 |
O3—Mo3—O12 | 69.86 (7) | N2—C11—C12 | 120.9 (3) |
O2iii—Mo3—O12 | 71.10 (7) | N2—C11—C18 | 118.3 (2) |
O10—Mo4—O11 | 103.78 (11) | C12—C11—C18 | 120.7 (3) |
O10—Mo4—O4 | 101.69 (10) | C11—C12—C13 | 119.9 (3) |
O11—Mo4—O4 | 101.11 (9) | C11—C12—H12 | 120.0 |
O10—Mo4—O12 | 99.31 (10) | C13—C12—H12 | 120.0 |
O11—Mo4—O12 | 98.94 (9) | C14—C13—C12 | 118.9 (3) |
O4—Mo4—O12 | 146.43 (8) | C14—C13—H13 | 120.5 |
O10—Mo4—O2 | 94.67 (9) | C12—C13—H13 | 120.5 |
O11—Mo4—O2 | 161.16 (9) | C13—C14—C15 | 118.8 (3) |
O4—Mo4—O2 | 78.47 (8) | C13—C14—H14 | 120.6 |
O12—Mo4—O2 | 73.96 (8) | C15—C14—H14 | 120.6 |
O10—Mo4—O3 | 165.25 (9) | N2—C15—C14 | 123.1 (3) |
O11—Mo4—O3 | 89.49 (9) | N2—C15—H15 | 118.5 |
O4—Mo4—O3 | 81.66 (8) | C14—C15—H15 | 118.5 |
O12—Mo4—O3 | 71.85 (8) | N4—C16—C17 | 123.0 (3) |
O2—Mo4—O3 | 71.76 (7) | N4—C16—H16 | 118.5 |
Mo1iii—O2—Mo4 | 91.84 (7) | C17—C16—H16 | 118.5 |
Mo1iii—O2—Mo3iii | 91.42 (7) | C16—C17—C18 | 119.9 (3) |
Mo4—O2—Mo3iii | 161.75 (10) | C16—C17—H17 | 120.0 |
Mo1iii—O2—Mo1 | 104.24 (8) | C18—C17—H17 | 120.0 |
Mo4—O2—Mo1 | 97.94 (7) | C19—C18—C17 | 116.8 (3) |
Mo3iii—O2—Mo1 | 98.65 (7) | C19—C18—C11 | 123.1 (3) |
Mo1iii—O2—Mo2 | 165.98 (10) | C17—C18—C11 | 120.1 (3) |
Mo4—O2—Mo2 | 86.10 (6) | C20—C19—C18 | 120.1 (3) |
Mo3iii—O2—Mo2 | 86.40 (7) | C20—C19—H19 | 119.9 |
Mo1—O2—Mo2 | 89.78 (6) | C18—C19—H19 | 119.9 |
Mo1—O3—Mo3 | 108.88 (9) | N4—C20—C19 | 122.6 (3) |
Mo1—O3—Mo4 | 110.68 (9) | N4—C20—H20 | 118.7 |
Mo3—O3—Mo4 | 106.49 (8) | C19—C20—H20 | 118.7 |
Mo4—O4—Mo2 | 117.04 (10) | | |
| | | |
O10—Mo4—O2—Mo1iii | −80.59 (10) | O2—Mo2—O6—Mo3iii | 17.38 (10) |
O11—Mo4—O2—Mo1iii | 87.8 (3) | O1—Mo1—O7—Mo2 | −176.80 (11) |
O4—Mo4—O2—Mo1iii | 178.41 (9) | O12iii—Mo1—O7—Mo2 | 77.67 (12) |
O12—Mo4—O2—Mo1iii | 17.77 (7) | O3—Mo1—O7—Mo2 | −74.37 (12) |
O3—Mo4—O2—Mo1iii | 93.50 (8) | O2iii—Mo1—O7—Mo2 | 2.1 (3) |
O10—Mo4—O2—Mo3iii | 19.6 (3) | O2—Mo1—O7—Mo2 | 0.73 (10) |
O11—Mo4—O2—Mo3iii | −172.0 (3) | O5—Mo2—O7—Mo1 | 17.5 (5) |
O4—Mo4—O2—Mo3iii | −81.4 (3) | O8—Mo2—O7—Mo1 | 179.57 (13) |
O12—Mo4—O2—Mo3iii | 117.9 (3) | O6—Mo2—O7—Mo1 | −75.28 (12) |
O3—Mo4—O2—Mo3iii | −166.3 (3) | O4—Mo2—O7—Mo1 | 74.92 (12) |
Mo1iii—Mo4—O2—Mo3iii | 100.2 (3) | O2—Mo2—O7—Mo1 | −0.74 (10) |
O10—Mo4—O2—Mo1 | 174.76 (9) | O5—Mo2—O8—Cu2 | 82.41 (15) |
O11—Mo4—O2—Mo1 | −16.9 (3) | O6—Mo2—O8—Cu2 | −173.06 (12) |
O4—Mo4—O2—Mo1 | 73.76 (8) | O4—Mo2—O8—Cu2 | −17.07 (16) |
O12—Mo4—O2—Mo1 | −86.88 (8) | O7—Mo2—O8—Cu2 | −93.66 (14) |
O3—Mo4—O2—Mo1 | −11.15 (6) | O2—Mo2—O8—Cu2 | −94.4 (2) |
Mo1iii—Mo4—O2—Mo1 | −104.65 (9) | N3—Cu2—O8—Mo2 | 85.51 (16) |
O10—Mo4—O2—Mo2 | 85.53 (9) | N4ii—Cu2—O8—Mo2 | −95.62 (16) |
O11—Mo4—O2—Mo2 | −106.1 (3) | O10—Mo4—O11—Cu1 | 44.08 (15) |
O4—Mo4—O2—Mo2 | −15.47 (7) | O4—Mo4—O11—Cu1 | 149.19 (12) |
O12—Mo4—O2—Mo2 | −176.11 (8) | O12—Mo4—O11—Cu1 | −57.88 (14) |
O3—Mo4—O2—Mo2 | −100.39 (7) | O2—Mo4—O11—Cu1 | −124.0 (2) |
Mo1iii—Mo4—O2—Mo2 | 166.12 (9) | O3—Mo4—O11—Cu1 | −129.41 (12) |
O7—Mo1—O2—Mo1iii | 179.45 (10) | Mo1iii—Mo4—O11—Cu1 | −55.35 (16) |
O12iii—Mo1—O2—Mo1iii | 80.67 (9) | N2—Cu1—O11—Mo4 | −132.28 (14) |
O3—Mo1—O2—Mo1iii | −80.65 (9) | N1i—Cu1—O11—Mo4 | 47.80 (15) |
O2iii—Mo1—O2—Mo1iii | 0.0 | O10—Mo4—O12—Mo1iii | 71.13 (12) |
O7—Mo1—O2—Mo4 | −86.60 (9) | O11—Mo4—O12—Mo1iii | 176.80 (10) |
O12iii—Mo1—O2—Mo4 | 174.62 (9) | O4—Mo4—O12—Mo1iii | −57.07 (18) |
O3—Mo1—O2—Mo4 | 13.31 (7) | O2—Mo4—O12—Mo1iii | −21.09 (9) |
O2iii—Mo1—O2—Mo4 | 93.95 (9) | O3—Mo4—O12—Mo1iii | −96.70 (10) |
O7—Mo1—O2—Mo3iii | 85.76 (9) | O10—Mo4—O12—Mo3 | −172.55 (9) |
O12iii—Mo1—O2—Mo3iii | −13.02 (8) | O11—Mo4—O12—Mo3 | −66.88 (10) |
O3—Mo1—O2—Mo3iii | −174.34 (9) | O4—Mo4—O12—Mo3 | 59.25 (17) |
O2iii—Mo1—O2—Mo3iii | −93.69 (9) | O2—Mo4—O12—Mo3 | 95.23 (8) |
O7—Mo1—O2—Mo2 | −0.57 (8) | O3—Mo4—O12—Mo3 | 19.61 (7) |
O12iii—Mo1—O2—Mo2 | −99.35 (7) | O13—Mo3—O12—Mo1iii | −167.66 (11) |
O3—Mo1—O2—Mo2 | 99.33 (7) | O9—Mo3—O12—Mo1iii | 50.8 (3) |
O2iii—Mo1—O2—Mo2 | 179.98 (10) | O6iii—Mo3—O12—Mo1iii | −64.59 (10) |
O5—Mo2—O2—Mo1iii | 4.3 (4) | O3—Mo3—O12—Mo1iii | 92.44 (10) |
O8—Mo2—O2—Mo1iii | −178.8 (3) | O2iii—Mo3—O12—Mo1iii | 13.93 (8) |
O6—Mo2—O2—Mo1iii | −93.6 (4) | O13—Mo3—O12—Mo4 | 76.04 (10) |
O4—Mo2—O2—Mo1iii | 97.5 (4) | O9—Mo3—O12—Mo4 | −65.5 (3) |
O7—Mo2—O2—Mo1iii | −179.6 (4) | O6iii—Mo3—O12—Mo4 | 179.11 (9) |
O5—Mo2—O2—Mo4 | −77.65 (9) | O3—Mo3—O12—Mo4 | −23.87 (8) |
O8—Mo2—O2—Mo4 | 99.2 (2) | O2iii—Mo3—O12—Mo4 | −102.37 (9) |
O6—Mo2—O2—Mo4 | −175.59 (9) | N1i—Cu1—N2—C15 | −86.4 (5) |
O4—Mo2—O2—Mo4 | 15.59 (7) | O11—Cu1—N2—C15 | 93.9 (2) |
O7—Mo2—O2—Mo4 | 98.44 (7) | N1i—Cu1—N2—C11 | 91.6 (5) |
O5—Mo2—O2—Mo3iii | 85.69 (9) | O11—Cu1—N2—C11 | −88.1 (2) |
O8—Mo2—O2—Mo3iii | −97.4 (2) | O8—Cu2—N3—C6 | 15.9 (2) |
O6—Mo2—O2—Mo3iii | −12.24 (8) | O8—Cu2—N3—C10 | −158.2 (2) |
O4—Mo2—O2—Mo3iii | 178.93 (8) | C5—N1—C1—C2 | −3.0 (4) |
O7—Mo2—O2—Mo3iii | −98.21 (7) | Cu1iv—N1—C1—C2 | 161.5 (2) |
O5—Mo2—O2—Mo1 | −175.63 (8) | C5—N1—C1—C8 | 175.8 (3) |
O8—Mo2—O2—Mo1 | 1.3 (2) | Cu1iv—N1—C1—C8 | −19.7 (4) |
O6—Mo2—O2—Mo1 | 86.43 (8) | N1—C1—C2—C3 | −0.8 (5) |
O4—Mo2—O2—Mo1 | −82.39 (8) | C8—C1—C2—C3 | −179.5 (3) |
O7—Mo2—O2—Mo1 | 0.46 (6) | C1—C2—C3—C4 | 4.0 (5) |
O1—Mo1—O3—Mo3 | −72.75 (11) | C2—C3—C4—C5 | −3.3 (5) |
O7—Mo1—O3—Mo3 | −178.59 (9) | C1—N1—C5—C4 | 3.7 (5) |
O12iii—Mo1—O3—Mo3 | 65.72 (19) | Cu1iv—N1—C5—C4 | −162.7 (3) |
O2iii—Mo1—O3—Mo3 | 25.07 (9) | C3—C4—C5—N1 | −0.5 (5) |
O2—Mo1—O3—Mo3 | 103.08 (9) | C10—N3—C6—C7 | 0.7 (5) |
O1—Mo1—O3—Mo4 | 170.53 (9) | Cu2—N3—C6—C7 | −173.8 (2) |
O7—Mo1—O3—Mo4 | 64.70 (10) | N3—C6—C7—C8 | 0.9 (5) |
O12iii—Mo1—O3—Mo4 | −51.00 (19) | C6—C7—C8—C9 | −1.2 (4) |
O2iii—Mo1—O3—Mo4 | −91.65 (9) | C6—C7—C8—C1 | 175.7 (3) |
O2—Mo1—O3—Mo4 | −13.63 (7) | N1—C1—C8—C9 | −22.9 (4) |
O13—Mo3—O3—Mo1 | 176.59 (10) | C2—C1—C8—C9 | 155.9 (3) |
O9—Mo3—O3—Mo1 | 70.46 (11) | N1—C1—C8—C7 | 160.5 (3) |
O6iii—Mo3—O3—Mo1 | −56.21 (18) | C2—C1—C8—C7 | −20.8 (4) |
O2iii—Mo3—O3—Mo1 | −23.73 (8) | C7—C8—C9—C10 | 0.1 (4) |
O12—Mo3—O3—Mo1 | −99.26 (10) | C1—C8—C9—C10 | −176.7 (3) |
O13—Mo3—O3—Mo4 | −64.05 (10) | C6—N3—C10—C9 | −1.9 (5) |
O9—Mo3—O3—Mo4 | −170.18 (9) | Cu2—N3—C10—C9 | 172.3 (2) |
O6iii—Mo3—O3—Mo4 | 63.15 (17) | C8—C9—C10—N3 | 1.5 (5) |
O2iii—Mo3—O3—Mo4 | 95.63 (8) | C15—N2—C11—C12 | 0.4 (4) |
O12—Mo3—O3—Mo4 | 20.10 (7) | Cu1—N2—C11—C12 | −177.5 (2) |
O10—Mo4—O3—Mo1 | 38.6 (4) | C15—N2—C11—C18 | 179.7 (3) |
O11—Mo4—O3—Mo1 | −167.07 (11) | Cu1—N2—C11—C18 | 1.7 (4) |
O4—Mo4—O3—Mo1 | −65.76 (10) | N2—C11—C12—C13 | 3.0 (5) |
O12—Mo4—O3—Mo1 | 93.35 (10) | C18—C11—C12—C13 | −176.2 (3) |
O2—Mo4—O3—Mo1 | 14.77 (8) | C11—C12—C13—C14 | −3.9 (5) |
Mo1iii—Mo4—O3—Mo1 | 58.02 (7) | C12—C13—C14—C15 | 1.4 (5) |
O10—Mo4—O3—Mo3 | −79.6 (4) | C11—N2—C15—C14 | −3.1 (4) |
O11—Mo4—O3—Mo3 | 74.75 (10) | Cu1—N2—C15—C14 | 175.1 (2) |
O4—Mo4—O3—Mo3 | 176.05 (9) | C13—C14—C15—N2 | 2.2 (5) |
O12—Mo4—O3—Mo3 | −24.84 (8) | C20—N4—C16—C17 | −0.3 (4) |
O2—Mo4—O3—Mo3 | −103.41 (9) | Cu2v—N4—C16—C17 | 173.0 (2) |
Mo1iii—Mo4—O3—Mo3 | −60.17 (7) | N4—C16—C17—C18 | 0.2 (4) |
O10—Mo4—O4—Mo2 | −69.74 (13) | C16—C17—C18—C19 | −0.5 (4) |
O11—Mo4—O4—Mo2 | −176.51 (11) | C16—C17—C18—C11 | −179.4 (3) |
O12—Mo4—O4—Mo2 | 57.89 (19) | N2—C11—C18—C19 | 30.6 (4) |
O2—Mo4—O4—Mo2 | 22.70 (10) | C12—C11—C18—C19 | −150.1 (3) |
O3—Mo4—O4—Mo2 | 95.67 (11) | N2—C11—C18—C17 | −150.5 (3) |
Mo1iii—Mo4—O4—Mo2 | 23.95 (13) | C12—C11—C18—C17 | 28.7 (4) |
O5—Mo2—O4—Mo4 | 75.61 (13) | C17—C18—C19—C20 | 1.0 (4) |
O8—Mo2—O4—Mo4 | −178.13 (11) | C11—C18—C19—C20 | 179.9 (3) |
O6—Mo2—O4—Mo4 | −39.1 (2) | C16—N4—C20—C19 | 0.9 (4) |
O7—Mo2—O4—Mo4 | −93.86 (11) | C18—C19—C20—N4 | −1.2 (5) |
O2—Mo2—O4—Mo4 | −21.24 (9) | C17—C18—C19—C20 | 1.0 (4) |
O5—Mo2—O6—Mo3iii | −78.09 (14) | C11—C18—C19—C20 | 179.9 (3) |
O8—Mo2—O6—Mo3iii | 174.12 (12) | C16—N4—C20—C19 | 0.9 (4) |
O4—Mo2—O6—Mo3iii | 35.3 (2) | C18—C19—C20—N4 | −1.2 (5) |
O7—Mo2—O6—Mo3iii | 89.26 (12) | | |
Symmetry codes: (i) x+1, y, z; (ii) x, y+1, z; (iii) −x+2, −y+1, −z+2; (iv) x−1, y, z; (v) x, y−1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C4—H4···O5vi | 0.93 | 2.46 | 3.07 | 124 |
C7—H7···O1vii | 0.93 | 2.47 | 3.03 | 119 |
C10—H10···O4viii | 0.93 | 2.42 | 3.25 | 148 |
C12—H12···O9ix | 0.93 | 2.55 | 3.46 | 168 |
C14—H14···O10x | 0.93 | 2.47 | 3.12 | 127 |
C16—H16···O3ix | 0.93 | 2.45 | 3.02 | 120 |
Symmetry codes: (vi) x−1, y−1, z; (vii) −x+1, −y+1, −z+2; (viii) −x+1, −y+1, −z+1; (ix) −x+1, −y, −z+1; (x) −x+2, −y+1, −z+1. |
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